#------------------------------------------------------------------------------ #$Date: 2021-08-19 01:12:36 +0300 (Thu, 19 Aug 2021) $ #$Revision: 268126 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564377.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1564377 loop_ _publ_author_name 'Keener, Megan' 'Scopelliti, Rosario' 'Mazzanti, Marinella' _publ_section_title ; Nitride Protonation and NH3 Binding versus N--H Bond Cleavage in Uranium Nitrides ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC03957A _journal_year 2021 _chemical_formula_moiety 'C44 H100 N O14 Si3 U, C24 H20 B, 0.5(C4 H10 O)' _chemical_formula_sum 'C70 H125 B N O14.5 Si3 U' _chemical_formula_weight 1545.81 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2021-06-11 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-07-16 deposited with the CCDC. 2021-08-13 downloaded from the CCDC. ; _cell_angle_alpha 78.867(3) _cell_angle_beta 72.917(3) _cell_angle_gamma 73.341(3) _cell_formula_units_Z 2 _cell_length_a 13.6571(5) _cell_length_b 14.5356(5) _cell_length_c 22.7110(8) _cell_measurement_reflns_used 18656 _cell_measurement_temperature 140.00(10) _cell_measurement_theta_max 71.6240 _cell_measurement_theta_min 3.1260 _cell_volume 4099.4(3) _computing_cell_refinement 'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXT 2018/2 (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 140.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2665 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -82.00 2.00 1.00 4.00 -- -42.88 110.00 50.00 84 2 \w 21.00 79.00 1.00 4.00 -- 42.88-110.00 -44.00 58 3 \w 70.00 108.00 1.00 16.00 -- 102.23-110.00 -44.00 38 4 \w 124.00 159.00 1.00 16.00 -- 102.23 110.00 50.00 35 5 \w -47.00 -19.00 1.00 4.00 -- -42.88 -37.00 90.00 28 6 \w -114.00 -19.00 1.00 4.00 -- -42.88 -37.00-180.00 95 7 \w -105.00 -74.00 1.00 4.00 -- -42.88 -37.00 90.00 31 8 \w -116.00 -15.00 1.00 4.00 -- -42.88 -57.00 -60.00 101 9 \w 27.00 66.00 1.00 16.00 -- 102.23 -77.00 -60.00 39 10 \w 27.00 103.00 1.00 16.00 -- 102.23 -94.00 0.00 76 11 \w 35.00 106.00 1.00 16.00 -- 102.23 -94.00 90.00 71 12 \w 32.00 75.00 1.00 16.00 -- 102.23 -77.00 150.00 43 13 \w 103.00 163.00 1.00 16.00 -- 102.23 125.00 -30.00 60 14 \w 103.00 135.00 1.00 16.00 -- 102.23 -77.00 150.00 32 15 \w 75.00 163.00 1.00 16.00 -- 102.23 61.00-120.00 88 16 \w 103.00 130.00 1.00 16.00 -- 102.23 -77.00 -60.00 27 17 \w 104.00 177.00 1.00 16.00 -- 102.23 77.00 150.00 73 18 \w 81.00 112.00 1.00 16.00 -- 102.23-125.00-120.00 31 19 \w 73.00 158.00 1.00 16.00 -- 102.23 61.00 120.00 85 20 \w 105.00 148.00 1.00 16.00 -- 102.23 45.00 30.00 43 21 \w 80.00 112.00 1.00 16.00 -- 102.23 30.00 90.00 32 22 \w 136.00 168.00 1.00 16.00 -- 102.23 30.00 90.00 32 23 \w 76.00 112.00 1.00 16.00 -- 102.23-125.00 150.00 36 24 \w 81.00 106.00 1.00 16.00 -- 102.23 -94.00-180.00 25 25 \w 103.00 162.00 1.00 16.00 -- 102.23 77.00 -60.00 59 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0363109000 _diffrn_orient_matrix_UB_12 -0.0333140000 _diffrn_orient_matrix_UB_13 0.0698097000 _diffrn_orient_matrix_UB_21 -0.1066812000 _diffrn_orient_matrix_UB_22 0.0750118000 _diffrn_orient_matrix_UB_23 0.0033688000 _diffrn_orient_matrix_UB_31 -0.0460172000 _diffrn_orient_matrix_UB_32 -0.0753498000 _diffrn_orient_matrix_UB_33 -0.0149463000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_unetI/netI 0.0616 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 34513 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.750 _diffrn_reflns_theta_min 3.196 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 6.435 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_correction_T_min 0.507 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021) Numerical absorption correction based on Gaussian integration over a multifaceted crystal model. Empirical absorption correction using spherical harmonics as implemented in SCALE3 ABSPACK scaling algorithm ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.252 _exptl_crystal_description prism _exptl_crystal_F_000 1614 _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.04 _refine_diff_density_max 2.749 _refine_diff_density_min -2.248 _refine_diff_density_rms 0.116 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 876 _refine_ls_number_reflns 15595 _refine_ls_number_restraints 33 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0432 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1045 _refine_ls_wR_factor_ref 0.1117 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13556 _reflns_number_total 15595 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc03957a2.cif _cod_data_source_block mk-164 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Gaussian' was changed to 'gaussian' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_formula_sum 'C70 H125 B N O14.50 Si3 U' _cod_database_code 1564377 _shelx_shelxl_version_number 2018/3 _audit_contact_author 'Farzaneh Fadaei Tirani' _chemical_oxdiff_formula 'C70 H125 B N O14.50 Si3 U' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.783 _shelx_estimated_absorpt_t_min 0.408 _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, {H1A,H1B,H1C} of C84, All C(H,H) groups At 1.5 times of: {H84A,H84B,H84C} of C84, {H82A,H82B,H82C} of C82, {H32A,H32B,H32C} of C32, {H47A,H47B,H47C} of C47, {H28A,H28B,H28C} of C28, {H30A,H30B,H30C} of C30, {H43A,H43B,H43C} of C43, {H52A,H52B,H52C} of C52, {H26A,H26B,H26C} of C26, {H46A,H46B,H46C} of C46, {H31A,H31B,H31C} of C31, {H48A,H48B,H48C} of C48, {H50A,H50B,H50C} of C50, {H51A,H51B,H51C} of C51, {H42A,H42B,H42C} of C42, {H27A,H27B,H27C} of C27, {H44A,H44B,H44C} of C44, {H24A,H24B,H24C} of C24, {H2A,H2B,H2C} of C2, {H12A,H12B,H12C} of C12, {H22A,H22B,H22C} of C22, {H11A, H11B,H11C} of C11, {H23A,H23B,H23C} of C23, {H7A,H7B,H7C} of C7, {H8A,H8B, H8C} of C8, {H4A,H4B,H4C} of C4, {H3A,H3B,H3C} of C3, {H6A,H6B,H6C} of C6, {H10A,H10B,H10C} of C10 2. Restrained distances O81-C81 1.41 with sigma of 0.02 C83-C84 1.5 with sigma of 0.02 O81-C83 1.42 with sigma of 0.02 C82-C81 1.48 with sigma of 0.02 N1-H1A = N1-H1B = N1-H1C 1 with sigma of 0.02 O81-C82 = O81-C84 2.37 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints O81 \\sim C81 \\sim C82 \\sim C83 \\sim C84: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 4. Others Fixed Sof: O81(0.5) C81(0.5) H81A(0.5) H81B(0.5) C82(0.5) H82A(0.5) H82B(0.5) H82C(0.5) C83(0.5) H83A(0.5) H83B(0.5) C84(0.5) H84A(0.5) H84B(0.5) H84C(0.5) 5.a Secondary CH2 refined with riding coordinates: C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C71(H71A, H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C81(H81A,H81B), C83(H83A,H83B) 5.b Aromatic/amide H refined with riding coordinates: C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118), C120(H120), C121(H121), C122(H122), C123(H123), C124(H124) 5.c Idealised Me refined as rotating group: C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A, H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A, H12B,H12C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B, H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42(H42A,H42B,H42C), C43(H43A, H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B, H52C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C) ; _shelx_res_file ; TITL mk-164.res in P-1 mk-164.res created by SHELXL-2018/3 at 14:14:52 on 11-Jun-2021 CELL 1.54184 13.657114 14.53561 22.710963 78.8671 72.917 73.3409 ZERR 2 0.000466 0.000536 0.000777 0.003 0.003 0.0031 LATT 1 SFAC C H B N O Si U UNIT 140 250 2 2 29 6 2 DFIX 1.41 O81 C81 DANG 2.37 O81 C82 O81 C84 DFIX 1.5 C83 C84 SIMU 0.01 0.02 2 O81 > C84 DFIX 1.42 O81 C83 DFIX 1.48 C82 C81 DFIX 1 N1 H1a N1 H1b N1 H1c L.S. 20 PLAN 10 SIZE 0.04 0.1 0.17 TEMP -133.15 CONF WPDB -2 BOND $H MORE -1 fmap 2 acta REM REM REM WGHT 0.065200 FVAR 2.44059 U1 7 0.658294 0.225384 0.755304 11.00000 0.02866 0.02697 = 0.03720 -0.00333 -0.01194 -0.00767 SI1 6 0.516777 0.458255 0.815225 11.00000 0.03411 0.02777 = 0.04874 -0.00847 -0.00951 -0.00789 SI2 6 0.794723 0.047600 0.865210 11.00000 0.03619 0.03105 = 0.04272 -0.00080 -0.01698 -0.00917 SI3 6 0.437265 0.168982 0.722661 11.00000 0.03303 0.03567 = 0.04372 -0.00418 -0.01379 -0.01479 O1 5 0.583231 0.349941 0.804520 11.00000 0.04388 0.02872 = 0.04421 -0.01115 -0.01500 -0.00719 O2 5 0.488547 0.506146 0.748943 11.00000 0.04327 0.02876 = 0.05378 -0.00427 -0.01608 -0.00303 O3 5 0.582040 0.517599 0.836437 11.00000 0.04037 0.04362 = 0.06330 -0.01722 -0.00655 -0.01707 O4 5 0.405693 0.464496 0.867498 11.00000 0.03881 0.04237 = 0.05337 -0.01216 -0.01023 -0.01302 O21 5 0.723799 0.124431 0.823613 11.00000 0.03913 0.03982 = 0.04407 0.00238 -0.02162 -0.00669 O22 5 0.829587 0.098473 0.910990 11.00000 0.05143 0.04304 = 0.05120 -0.00686 -0.01861 -0.01262 O23 5 0.733562 -0.030837 0.908598 11.00000 0.05238 0.03974 = 0.05686 0.00073 -0.02043 -0.01572 O24 5 0.901703 0.002608 0.815371 11.00000 0.03968 0.04447 = 0.05567 -0.00946 -0.01653 -0.00688 O41 5 0.529819 0.173173 0.752930 11.00000 0.03620 0.03576 = 0.04637 0.00081 -0.01614 -0.01624 O42 5 0.324766 0.173728 0.773089 11.00000 0.03483 0.03710 = 0.04714 -0.00856 -0.00947 -0.01658 O43 5 0.463716 0.072909 0.689154 11.00000 0.04124 0.04811 = 0.05744 -0.01626 -0.00412 -0.02138 O44 5 0.437280 0.260154 0.667565 11.00000 0.04366 0.05258 = 0.04646 0.00287 -0.02206 -0.02281 O61 5 0.826270 0.277014 0.710061 11.00000 0.03537 0.04791 = 0.04743 -0.00307 -0.01324 -0.01803 O71 5 0.756366 0.129307 0.668710 11.00000 0.04259 0.04732 = 0.05059 -0.02262 -0.01249 -0.00566 N1 4 0.602728 0.349114 0.668244 11.00000 0.03777 0.04145 = 0.04337 -0.00126 -0.01813 -0.01214 C1 1 0.415369 0.596880 0.732966 11.00000 0.04589 0.02890 = 0.06615 0.00026 -0.01706 -0.00165 C2 1 0.305982 0.580253 0.749523 11.00000 0.04681 0.05115 = 0.07635 0.00325 -0.01909 -0.00702 AFIX 137 H2A 2 0.305669 0.531109 0.725539 11.00000 -1.50000 H2B 2 0.255851 0.640842 0.739866 11.00000 -1.50000 H2C 2 0.285330 0.558002 0.793928 11.00000 -1.50000 AFIX 0 C3 1 0.455522 0.620234 0.664195 11.00000 0.05844 0.04085 = 0.07402 0.00727 -0.01831 0.00111 AFIX 137 H3A 2 0.527045 0.629518 0.654909 11.00000 -1.50000 H3B 2 0.408727 0.679613 0.649636 11.00000 -1.50000 H3C 2 0.457003 0.566814 0.643150 11.00000 -1.50000 AFIX 0 C4 1 0.418277 0.675921 0.766922 11.00000 0.07095 0.03273 = 0.09644 -0.00735 -0.02879 -0.00484 AFIX 137 H4A 2 0.393122 0.659000 0.811728 11.00000 -1.50000 H4B 2 0.372664 0.737256 0.753754 11.00000 -1.50000 H4C 2 0.490924 0.682556 0.757214 11.00000 -1.50000 AFIX 0 C5 1 0.690377 0.524343 0.815639 11.00000 0.04484 0.05064 = 0.06799 -0.01531 -0.00806 -0.02408 C6 1 0.731712 0.522067 0.746933 11.00000 0.05141 0.05081 = 0.06283 -0.00262 -0.00211 -0.02167 AFIX 137 H6A 2 0.728204 0.461145 0.736201 11.00000 -1.50000 H6B 2 0.805227 0.527104 0.734198 11.00000 -1.50000 H6C 2 0.688733 0.576464 0.725474 11.00000 -1.50000 AFIX 0 C7 1 0.689628 0.620890 0.833450 11.00000 0.06381 0.06961 = 0.12450 -0.04520 -0.00326 -0.03840 AFIX 137 H7A 2 0.646270 0.673931 0.811349 11.00000 -1.50000 H7B 2 0.762033 0.628686 0.822130 11.00000 -1.50000 H7C 2 0.660100 0.621881 0.878276 11.00000 -1.50000 AFIX 0 C8 1 0.755422 0.441389 0.850905 11.00000 0.04913 0.07931 = 0.07765 -0.00345 -0.01763 -0.02573 AFIX 137 H8A 2 0.730601 0.447955 0.895348 11.00000 -1.50000 H8B 2 0.829999 0.443027 0.836231 11.00000 -1.50000 H8C 2 0.747558 0.379760 0.843850 11.00000 -1.50000 AFIX 0 C9 1 0.376762 0.466585 0.933480 11.00000 0.03898 0.05369 = 0.05236 -0.02036 -0.00842 -0.01276 C10 1 0.362408 0.570083 0.945278 11.00000 0.07522 0.07293 = 0.08262 -0.04442 0.00264 -0.02890 AFIX 137 H10A 2 0.430103 0.588094 0.929065 11.00000 -1.50000 H10B 2 0.337541 0.574518 0.989981 11.00000 -1.50000 H10C 2 0.310364 0.614095 0.924362 11.00000 -1.50000 AFIX 0 C11 1 0.459579 0.396993 0.962139 11.00000 0.04550 0.10013 = 0.06320 -0.00017 -0.01407 -0.01720 AFIX 137 H11A 2 0.465952 0.331192 0.954471 11.00000 -1.50000 H11B 2 0.439387 0.400323 1.006946 11.00000 -1.50000 H11C 2 0.527524 0.413980 0.943732 11.00000 -1.50000 AFIX 0 C12 1 0.272954 0.437747 0.957764 11.00000 0.04699 0.07758 = 0.06199 -0.01995 -0.00333 -0.02285 AFIX 137 H12A 2 0.250518 0.436190 1.003011 11.00000 -1.50000 H12B 2 0.281702 0.373500 0.946597 11.00000 -1.50000 H12C 2 0.219297 0.484843 0.939438 11.00000 -1.50000 AFIX 0 C21 1 0.780729 0.128024 0.971708 11.00000 0.05834 0.05346 = 0.05339 -0.01531 -0.01661 -0.01301 C22 1 0.666101 0.183021 0.974858 11.00000 0.05435 0.10140 = 0.09341 -0.04839 -0.01640 0.00069 AFIX 137 H22A 2 0.664154 0.237507 0.941845 11.00000 -1.50000 H22B 2 0.633535 0.207333 1.015272 11.00000 -1.50000 H22C 2 0.627079 0.139506 0.969479 11.00000 -1.50000 AFIX 0 C23 1 0.842596 0.195572 0.978131 11.00000 0.08504 0.06862 = 0.07745 -0.02603 -0.03133 -0.02017 AFIX 137 H23A 2 0.916592 0.160477 0.974577 11.00000 -1.50000 H23B 2 0.812474 0.219685 1.018702 11.00000 -1.50000 H23C 2 0.838677 0.250178 0.945263 11.00000 -1.50000 AFIX 0 C24 1 0.790136 0.041375 1.019823 11.00000 0.14253 0.08771 = 0.05987 0.00352 -0.04303 -0.04252 AFIX 137 H24A 2 0.746229 0.000452 1.016934 11.00000 -1.50000 H24B 2 0.766288 0.062751 1.061195 11.00000 -1.50000 H24C 2 0.864030 0.004375 1.012739 11.00000 -1.50000 AFIX 0 C25 1 0.670315 -0.086470 0.897217 11.00000 0.04878 0.04570 = 0.05701 0.00348 -0.02078 -0.02412 C26 1 0.557656 -0.021569 0.903160 11.00000 0.05427 0.07493 = 0.06712 -0.00985 -0.01842 -0.02267 AFIX 137 H26A 2 0.558499 0.032472 0.869837 11.00000 -1.50000 H26B 2 0.531855 0.003612 0.943426 11.00000 -1.50000 H26C 2 0.510903 -0.059478 0.899999 11.00000 -1.50000 AFIX 0 C27 1 0.671372 -0.171390 0.947619 11.00000 0.10062 0.06882 = 0.08944 0.02134 -0.04640 -0.04744 AFIX 137 H27A 2 0.623053 -0.208265 0.945254 11.00000 -1.50000 H27B 2 0.648658 -0.147699 0.988270 11.00000 -1.50000 H27C 2 0.743089 -0.213223 0.941989 11.00000 -1.50000 AFIX 0 C28 1 0.715384 -0.116731 0.832609 11.00000 0.05387 0.05470 = 0.07619 -0.02046 -0.01668 -0.01519 AFIX 137 H28A 2 0.673995 -0.157080 0.825977 11.00000 -1.50000 H28B 2 0.789004 -0.153635 0.828042 11.00000 -1.50000 H28C 2 0.712348 -0.059078 0.801955 11.00000 -1.50000 AFIX 0 C29 1 1.005175 -0.055170 0.822399 11.00000 0.03505 0.03994 = 0.07042 -0.01195 -0.02310 0.00244 C30 1 1.065651 0.010773 0.832153 11.00000 0.04882 0.06758 = 0.08592 -0.01431 -0.02410 -0.01731 AFIX 137 H30A 2 1.134131 -0.027737 0.838762 11.00000 -1.50000 H30B 2 1.025067 0.044339 0.868560 11.00000 -1.50000 H30C 2 1.076890 0.058391 0.795450 11.00000 -1.50000 AFIX 0 C31 1 0.991443 -0.133854 0.877259 11.00000 0.06447 0.05562 = 0.10923 0.01361 -0.03929 -0.00984 AFIX 137 H31A 2 1.060692 -0.176558 0.879351 11.00000 -1.50000 H31B 2 0.946308 -0.171617 0.871876 11.00000 -1.50000 H31C 2 0.958515 -0.103893 0.915766 11.00000 -1.50000 AFIX 0 C32 1 1.058035 -0.099451 0.762925 11.00000 0.05576 0.08331 = 0.09892 -0.04645 -0.02017 -0.00019 AFIX 137 H32A 2 1.069864 -0.048270 0.728518 11.00000 -1.50000 H32B 2 1.012758 -0.135104 0.755388 11.00000 -1.50000 H32C 2 1.125970 -0.143868 0.766066 11.00000 -1.50000 AFIX 0 C41 1 0.270693 0.231616 0.823905 11.00000 0.04183 0.04388 = 0.04042 -0.00808 -0.00810 -0.01701 C42 1 0.281853 0.334547 0.804688 11.00000 0.04318 0.03689 = 0.06316 -0.00931 -0.01947 -0.00613 AFIX 137 H42A 2 0.247010 0.372003 0.839957 11.00000 -1.50000 H42B 2 0.248834 0.363790 0.770363 11.00000 -1.50000 H42C 2 0.356940 0.334482 0.791302 11.00000 -1.50000 AFIX 0 C43 1 0.317203 0.185600 0.878572 11.00000 0.07161 0.05259 = 0.04703 -0.00222 -0.01704 -0.00811 AFIX 137 H43A 2 0.387940 0.196310 0.870173 11.00000 -1.50000 H43B 2 0.321978 0.115975 0.885071 11.00000 -1.50000 H43C 2 0.271801 0.214723 0.915864 11.00000 -1.50000 AFIX 0 C44 1 0.156233 0.227570 0.838233 11.00000 0.04459 0.05635 = 0.06710 -0.02179 0.00122 -0.02128 AFIX 137 H44A 2 0.113607 0.267868 0.871201 11.00000 -1.50000 H44B 2 0.150909 0.160580 0.851897 11.00000 -1.50000 H44C 2 0.130211 0.251645 0.800860 11.00000 -1.50000 AFIX 0 C45 1 0.438270 -0.019459 0.708589 11.00000 0.04872 0.04821 = 0.07169 -0.02059 -0.01252 -0.02120 C46 1 0.455097 -0.057310 0.771771 11.00000 0.17692 0.05033 = 0.12954 0.01755 -0.09833 -0.04480 AFIX 137 H46A 2 0.404124 -0.015596 0.801958 11.00000 -1.50000 H46B 2 0.527040 -0.057975 0.771801 11.00000 -1.50000 H46C 2 0.445168 -0.123195 0.783010 11.00000 -1.50000 AFIX 0 C47 1 0.324592 -0.007576 0.709991 11.00000 0.05729 0.05404 = 0.11210 -0.02564 -0.01093 -0.02830 AFIX 137 H47A 2 0.305187 -0.069246 0.726134 11.00000 -1.50000 H47B 2 0.315021 0.012542 0.667889 11.00000 -1.50000 H47C 2 0.279470 0.041720 0.736863 11.00000 -1.50000 AFIX 0 C48 1 0.508162 -0.082751 0.660408 11.00000 0.08504 0.06899 = 0.15799 -0.06837 0.04482 -0.03934 AFIX 137 H48A 2 0.499135 -0.148788 0.673297 11.00000 -1.50000 H48B 2 0.581981 -0.082967 0.655417 11.00000 -1.50000 H48C 2 0.489275 -0.058067 0.620864 11.00000 -1.50000 AFIX 0 C49 1 0.384021 0.291613 0.617538 11.00000 0.04973 0.05944 = 0.04717 0.00355 -0.02284 -0.02112 C50 1 0.280021 0.262699 0.634936 11.00000 0.05427 0.07164 = 0.07109 0.00756 -0.03590 -0.02624 AFIX 137 H50A 2 0.236688 0.286083 0.674418 11.00000 -1.50000 H50B 2 0.293688 0.192080 0.639150 11.00000 -1.50000 H50C 2 0.242462 0.291244 0.602486 11.00000 -1.50000 AFIX 0 C51 1 0.458218 0.254080 0.560032 11.00000 0.06336 0.11034 = 0.05668 -0.01659 -0.02157 -0.01450 AFIX 137 H51A 2 0.425516 0.279006 0.525206 11.00000 -1.50000 H51B 2 0.474485 0.183251 0.565632 11.00000 -1.50000 H51C 2 0.523555 0.275245 0.551355 11.00000 -1.50000 AFIX 0 C52 1 0.359382 0.402687 0.609705 11.00000 0.06611 0.06307 = 0.06315 0.01369 -0.03311 -0.02119 AFIX 137 H52A 2 0.319203 0.429020 0.578300 11.00000 -1.50000 H52B 2 0.425629 0.423356 0.596491 11.00000 -1.50000 H52C 2 0.317611 0.426477 0.649332 11.00000 -1.50000 AFIX 0 C61 1 0.915963 0.238619 0.737159 11.00000 0.03689 0.08054 = 0.06753 0.00660 -0.01627 -0.02231 AFIX 23 H61A 2 0.916186 0.172482 0.758629 11.00000 -1.20000 H61B 2 0.914379 0.280457 0.767208 11.00000 -1.20000 AFIX 0 C62 1 1.011391 0.237693 0.682659 11.00000 0.03456 0.08941 = 0.07473 -0.01213 -0.00256 -0.02420 AFIX 23 H62A 2 1.031271 0.178176 0.662375 11.00000 -1.20000 H62B 2 1.072644 0.243232 0.695411 11.00000 -1.20000 AFIX 0 C63 1 0.972194 0.326766 0.640342 11.00000 0.04754 0.07725 = 0.05488 -0.01189 0.00076 -0.03423 AFIX 23 H63A 2 0.974033 0.386580 0.654275 11.00000 -1.20000 H63B 2 1.014853 0.323065 0.596912 11.00000 -1.20000 AFIX 0 C64 1 0.860430 0.323029 0.646771 11.00000 0.04352 0.06276 = 0.04522 -0.00605 -0.00479 -0.02202 AFIX 23 H64A 2 0.814935 0.388929 0.640803 11.00000 -1.20000 H64B 2 0.857947 0.284408 0.616025 11.00000 -1.20000 AFIX 0 C71 1 0.839171 0.042659 0.676217 11.00000 0.05620 0.05847 = 0.05912 -0.01505 -0.01824 0.00875 AFIX 23 H71A 2 0.842927 0.026206 0.720010 11.00000 -1.20000 H71B 2 0.908791 0.050910 0.649854 11.00000 -1.20000 AFIX 0 C72 1 0.806303 -0.033668 0.655838 11.00000 0.11388 0.04978 = 0.06250 -0.01456 0.00659 -0.01914 AFIX 23 H72A 2 0.867319 -0.088546 0.643173 11.00000 -1.20000 H72B 2 0.751205 -0.058122 0.689155 11.00000 -1.20000 AFIX 0 C73 1 0.763946 0.019740 0.601882 11.00000 0.10876 0.07487 = 0.06278 -0.02544 -0.00353 -0.04447 AFIX 23 H73A 2 0.707356 -0.006938 0.598022 11.00000 -1.20000 H73B 2 0.820799 0.014466 0.562922 11.00000 -1.20000 AFIX 0 C74 1 0.720982 0.123240 0.614483 11.00000 0.05292 0.08395 = 0.04875 -0.02791 -0.01706 -0.00851 AFIX 23 H74A 2 0.749046 0.166960 0.578258 11.00000 -1.20000 H74B 2 0.642873 0.141200 0.623725 11.00000 -1.20000 AFIX 0 PART -1 O81 5 0.998618 0.501863 0.996877 10.50000 0.04991 0.04965 = 0.06125 -0.00580 -0.01079 -0.01595 C81 1 0.986773 0.593114 0.959726 10.50000 0.05262 0.06115 = 0.06615 -0.00687 -0.00953 -0.01547 AFIX 23 H81A 2 0.925456 0.606177 0.941880 10.50000 -1.20000 H81B 2 1.050969 0.594625 0.925385 10.50000 -1.20000 AFIX 0 C82 1 0.969782 0.666505 1.002221 10.50000 0.05507 0.05334 = 0.07622 -0.02130 0.00892 -0.01803 AFIX 137 H82A 2 0.958258 0.731457 0.979291 10.50000 -1.50000 H82B 2 1.032192 0.653924 1.018277 10.50000 -1.50000 H82C 2 0.907788 0.662111 1.036874 10.50000 -1.50000 AFIX 0 C83 1 1.002904 0.424564 0.965381 10.50000 0.05140 0.04976 = 0.07223 -0.01138 -0.00880 -0.01494 AFIX 23 H83A 2 1.067240 0.414186 0.930635 10.50000 -1.20000 H83B 2 0.940222 0.438968 0.948596 10.50000 -1.20000 AFIX 0 C84 1 1.004845 0.336391 1.012908 10.50000 0.08003 0.06542 = 0.09887 -0.00785 -0.00536 -0.01936 AFIX 137 H84A 2 1.005055 0.281226 0.993921 10.50000 -1.50000 H84B 2 0.942156 0.348825 1.047754 10.50000 -1.50000 H84C 2 1.068587 0.321789 1.027952 10.50000 -1.50000 AFIX 0 PART 0 H1A 2 0.553730 0.321416 0.656409 11.00000 -1.20000 H1B 2 0.568331 0.408307 0.688810 11.00000 -1.20000 H1C 2 0.660377 0.354022 0.630078 11.00000 -1.20000 C101 1 1.056206 0.274377 0.427610 11.00000 0.04050 0.02703 = 0.05426 -0.00996 -0.01690 -0.00701 C102 1 1.150201 0.284528 0.384496 11.00000 0.04229 0.03308 = 0.05972 -0.01026 -0.01078 -0.00676 AFIX 43 H102 2 1.147586 0.312552 0.343406 11.00000 -1.20000 AFIX 0 C103 1 1.247372 0.255626 0.398784 11.00000 0.04014 0.04155 = 0.07267 -0.01667 -0.00984 -0.00587 AFIX 43 H103 2 1.309411 0.264142 0.367907 11.00000 -1.20000 AFIX 0 C104 1 1.253614 0.213721 0.459098 11.00000 0.04385 0.03948 = 0.08283 -0.01742 -0.02532 -0.00395 AFIX 43 H104 2 1.319719 0.193573 0.469444 11.00000 -1.20000 AFIX 0 C105 1 1.162889 0.202291 0.502871 11.00000 0.05670 0.03403 = 0.06549 -0.00970 -0.03147 -0.00378 AFIX 43 H105 2 1.166176 0.173745 0.543785 11.00000 -1.20000 AFIX 0 C106 1 1.065815 0.232344 0.487659 11.00000 0.04314 0.03644 = 0.05230 -0.00999 -0.01561 -0.01091 AFIX 43 H106 2 1.003999 0.224196 0.518869 11.00000 -1.20000 AFIX 0 C107 1 0.858044 0.381734 0.463517 11.00000 0.04619 0.03103 = 0.04273 0.00162 -0.01548 -0.00786 C108 1 0.893143 0.452675 0.480398 11.00000 0.04406 0.03895 = 0.05075 -0.00719 -0.01046 -0.00915 AFIX 43 H108 2 0.965722 0.453024 0.465367 11.00000 -1.20000 AFIX 0 C109 1 0.826501 0.522015 0.517971 11.00000 0.05760 0.04228 = 0.05227 -0.01045 -0.01239 -0.00883 AFIX 43 H109 2 0.853434 0.569294 0.527450 11.00000 -1.20000 AFIX 0 C110 1 0.721363 0.522378 0.541536 11.00000 0.05209 0.04608 = 0.04913 -0.00633 -0.01204 0.00580 AFIX 43 H110 2 0.675234 0.569496 0.567439 11.00000 -1.20000 AFIX 0 C111 1 0.684069 0.453243 0.526939 11.00000 0.03922 0.05499 = 0.04580 0.00842 -0.00740 -0.00135 AFIX 43 H111 2 0.611606 0.452840 0.542878 11.00000 -1.20000 AFIX 0 C112 1 0.751376 0.384170 0.489161 11.00000 0.04054 0.03780 = 0.05017 0.00779 -0.01599 -0.01232 AFIX 43 H112 2 0.723653 0.336789 0.480472 11.00000 -1.20000 AFIX 0 C113 1 0.891631 0.215404 0.414706 11.00000 0.04026 0.03367 = 0.04855 -0.00644 -0.01376 -0.00725 C114 1 0.804918 0.227203 0.391104 11.00000 0.05407 0.03558 = 0.07227 0.00484 -0.03036 -0.01401 AFIX 43 H114 2 0.774073 0.289998 0.373853 11.00000 -1.20000 AFIX 0 C115 1 0.761553 0.151823 0.391585 11.00000 0.05769 0.04736 = 0.08102 0.00026 -0.03936 -0.01968 AFIX 43 H115 2 0.702156 0.163947 0.375014 11.00000 -1.20000 AFIX 0 C116 1 0.803761 0.059200 0.415906 11.00000 0.06240 0.03719 = 0.07201 -0.00148 -0.02420 -0.02327 AFIX 43 H116 2 0.773740 0.007310 0.416927 11.00000 -1.20000 AFIX 0 C117 1 0.891178 0.044331 0.438750 11.00000 0.05797 0.03436 = 0.06136 0.00031 -0.02334 -0.01174 AFIX 43 H117 2 0.923150 -0.019041 0.454604 11.00000 -1.20000 AFIX 0 C118 1 0.932679 0.121101 0.438742 11.00000 0.04628 0.03939 = 0.05179 -0.00238 -0.02010 -0.01317 AFIX 43 H118 2 0.991513 0.108802 0.455840 11.00000 -1.20000 AFIX 0 C119 1 0.951264 0.367671 0.341814 11.00000 0.03709 0.03680 = 0.05283 -0.00355 -0.01651 -0.01246 C120 1 0.991068 0.317494 0.289935 11.00000 0.06540 0.03872 = 0.05479 -0.00497 -0.01818 -0.01342 AFIX 43 H120 2 1.008216 0.248818 0.296455 11.00000 -1.20000 AFIX 0 C121 1 1.007004 0.362161 0.229441 11.00000 0.06688 0.05603 = 0.04762 -0.00749 -0.01489 -0.01524 AFIX 43 H121 2 1.035413 0.324349 0.195788 11.00000 -1.20000 AFIX 0 C122 1 0.981456 0.461853 0.218207 11.00000 0.04843 0.06058 = 0.05230 0.00736 -0.01842 -0.02375 AFIX 43 H122 2 0.990047 0.493643 0.177005 11.00000 -1.20000 AFIX 0 C123 1 0.943270 0.513942 0.268157 11.00000 0.04636 0.04375 = 0.06436 0.00693 -0.02055 -0.01509 AFIX 43 H123 2 0.927512 0.582571 0.261156 11.00000 -1.20000 AFIX 0 C124 1 0.927282 0.468453 0.328498 11.00000 0.03766 0.04076 = 0.05398 -0.00369 -0.01615 -0.01125 AFIX 43 H124 2 0.899177 0.506883 0.361843 11.00000 -1.20000 AFIX 0 B1 3 0.939066 0.308846 0.412807 11.00000 0.03781 0.02913 = 0.05214 -0.00877 -0.01346 -0.00564 HKLF 4 REM mk-164.res in P-1 REM wR2 = 0.1117, GooF = S = 1.030, Restrained GooF = 1.029 for all data REM R1 = 0.0432 for 13556 Fo > 4sig(Fo) and 0.0524 for all 15595 data REM 876 parameters refined using 33 restraints END WGHT 0.0652 0.0000 REM Highest difference peak 2.749, deepest hole -2.248, 1-sigma level 0.116 Q1 1 0.6389 0.2162 0.7999 11.00000 0.05 2.75 Q2 1 0.6768 0.2253 0.7106 11.00000 0.05 2.43 Q3 1 0.5949 0.2091 0.7727 11.00000 0.05 1.93 Q4 1 0.7218 0.2421 0.7362 11.00000 0.05 1.90 Q5 1 1.0221 0.3235 0.7352 11.00000 0.05 1.80 Q6 1 0.6457 0.2697 0.7258 11.00000 0.05 1.18 Q7 1 0.6659 0.2856 0.7718 11.00000 0.05 0.86 Q8 1 0.5578 0.1884 0.8758 11.00000 0.05 0.71 Q9 1 0.5892 0.3434 0.7683 11.00000 0.05 0.67 Q10 1 0.5603 0.1806 0.8543 11.00000 0.05 0.59 ; _shelx_res_checksum 35625 _shelx_hkl_file ; 0 0 2 525542. 5124.94 6 0 0 3 1050.71 475.778 6 0 0 4 157087. 3955.40 6 0 0 5 33637.0 2129.55 6 0 0 6 27829.8 2074.82 6 0 0 -7 3812.83 713.196 8 0 0 7 3799.78 976.497 6 0 0 -8 84950.5 3215.58 8 0 0 8 94621.4 4341.47 6 0 0 -9-318.671 481.676 8 0 0 9-780.017 883.370 6 0 0 -10 104832. 3860.81 8 0 0 10 106262. 5281.99 6 0 0 -11 2604.40 709.156 8 0 0 11 2882.29 1250.31 6 0 0 12 118184. 6198.91 6 0 0 13 1077.68 942.217 6 0 0 14 91025.9 6105.98 6 0 0 15 2104.31 1070.38 6 0 0 -15 3424.49 849.217 25 0 0 16 28616.5 3816.39 6 0 0 -16 24989.7 1909.14 25 0 0 17 13194.6 2700.18 6 0 0 -17 8263.50 1207.63 25 0 0 18 15959.9 3194.19 6 0 0 -18 12560.0 1416.69 25 0 0 19 29492.0 4263.21 6 0 0 -19 22693.5 1918.63 25 0 0 -20 4549.85 998.486 25 0 0 -21 16904.7 1612.24 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-6 1 9178.53 854.872 11 -15 -6 0 307.569 322.889 11 -15 -6 0-583.333 527.960 16 -15 -6 -1 15443.5 1252.59 11 -15 -6 -1 16315.2 1373.66 16 -15 -6 -2 234.456 423.558 11 -15 -6 -2-827.819 621.349 16 -15 -6 -3 17529.9 1440.42 11 -15 -6 -3 17728.6 1498.25 16 -15 -6 -4-297.511 502.183 11 -15 -6 -4-82.1939 555.300 16 -15 -6 -5 13231.6 1296.94 11 -15 -6 -5 11903.1 1238.50 16 -15 -6 -6 625.005 542.415 11 -15 -6 -7 19307.8 1558.41 11 -15 -6 -8 1671.33 701.409 11 -15 -6 -9 29648.1 1895.99 11 -15 -6 -10 1345.32 615.541 11 -15 -6 -11 33623.1 2003.55 11 -15 -6 -12 1659.25 562.246 11 -15 -6 -13 24988.8 1618.44 11 -15 -6 -14 1074.69 510.713 11 15 6 14 1223.40 399.894 19 -15 -6 -15 12623.5 1104.97 11 15 6 15 10426.4 851.220 19 -15 -6 -16 1909.18 430.135 11 15 6 16 1680.01 392.822 19 -15 -6 -17 14163.8 1014.66 11 -15 -6 -17 17032.6 1316.96 23 -15 -6 -18 325.829 378.515 23 -15 -7 1 969.766 308.985 11 -15 -7 1-577.782 444.712 16 -15 -7 0 10943.6 923.110 11 -15 -7 0 13678.9 1177.52 16 -15 -7 -1 2329.62 501.187 11 -15 -7 -1 3295.17 718.484 16 -15 -7 -2 13576.8 1170.78 11 -15 -7 -2 14001.1 1282.46 16 -15 -7 -3 1045.81 483.889 11 -15 -7 -3 260.793 522.137 16 -15 -7 -4 21390.9 1497.21 11 -15 -7 -4 19650.1 1532.47 16 -15 -7 -5 1006.59 538.820 11 -15 -7 -5 1294.59 577.899 16 -15 -7 -6 16956.6 1421.10 11 -15 -7 -6 14094.1 1231.92 23 -15 -7 -6 15609.4 1340.40 16 -15 -7 -7 3552.78 835.729 11 -15 -7 -7 3554.62 719.278 23 -15 -7 -7 2140.65 640.601 16 -15 -7 -8 34593.7 2042.25 11 -15 -7 -8 27853.1 1788.73 23 -15 -7 -9 1900.65 732.455 11 -15 -7 -10 35975.1 2080.91 11 -15 -7 -11-8.62228 494.693 11 -15 -7 -12 22155.5 1598.88 11 -15 -7 -13 1958.21 598.472 11 -15 -7 -14 16479.1 1286.99 11 15 7 14 13562.5 972.026 19 -15 -7 -14 16250.9 1431.07 23 -15 -7 -15 133.706 357.778 11 -15 -7 -15-24.0028 473.198 23 15 7 15 244.584 279.845 19 -15 -7 -16 8644.98 872.888 11 -15 -7 -16 8578.60 1019.76 23 -15 -7 -17 101.834 336.388 11 -15 -7 -17 1027.56 473.703 23 -15 -7 -18 7567.67 711.443 11 -15 -7 -18 9981.10 958.441 23 -15 -8 2 3102.03 516.852 16 -15 -8 1 8293.70 862.083 16 -15 -8 0 3366.28 646.066 16 -15 -8 -1 13419.5 979.482 11 -15 -8 -1 17707.2 1309.04 16 -15 -8 -2 4208.47 627.301 11 -15 -8 -2 5535.40 839.267 16 -15 -8 -3 16442.7 1247.14 11 -15 -8 -3 20499.1 1471.26 16 -15 -8 -4 2312.70 610.639 11 -15 -8 -4 2186.85 654.322 16 -15 -8 -5 21867.9 1480.27 11 -15 -8 -5 21535.2 1511.49 16 -15 -8 -6 2473.84 645.606 11 -15 -8 -6 2394.15 650.477 16 -15 -8 -7 15011.4 1281.51 11 -15 -8 -7 12707.5 1122.30 23 -15 -8 -7 16582.9 1284.39 16 -15 -8 -8 1510.15 587.672 11 -15 -8 -8 1725.05 607.426 23 -15 -8 -8 52.0116 382.733 16 -15 -8 -9 15868.7 1343.30 11 -15 -8 -9 13512.6 1293.60 23 -15 -8 -10-19.2514 428.632 11 -15 -8 -10 669.113 541.870 23 -15 -8 -11 21352.3 1533.73 11 -15 -8 -11 19356.7 1574.41 23 -15 -8 -12 347.770 519.207 11 -15 -8 -12 225.709 489.677 23 -15 -8 -13 14374.9 1236.73 11 -15 -8 -13 15146.0 1356.81 23 -15 -8 -14 2259.40 615.046 11 -15 -8 -14 2013.96 675.234 23 -15 -8 -15 9272.01 957.622 11 -15 -8 -15 11074.1 1122.06 23 -15 -8 -16 467.277 346.295 11 -15 -8 -16-487.443 454.610 23 -15 -8 -17 9303.65 859.313 11 -15 -8 -17 10779.1 1006.14 23 -15 -8 -18-567.322 337.964 11 -15 -8 -18 40.9421 353.139 23 -15 -9 1 2702.60 490.872 16 -15 -9 0 11140.7 932.439 16 -15 -9 -1 4491.22 675.190 16 -15 -9 -2 10530.4 983.692 16 -15 -9 -3 4733.77 640.929 11 -15 -9 -3 6183.58 843.553 16 -15 -9 -4 14105.4 1080.76 11 -15 -9 -4 15300.6 1220.51 16 -15 -9 -5 3566.86 632.585 11 -15 -9 -5 3577.75 722.452 16 -15 -9 -6 23278.0 1451.26 11 -15 -9 -6 22459.3 1439.74 16 -15 -9 -7 2246.88 640.936 11 -15 -9 -7 1251.27 433.971 23 -15 -9 -7 1951.15 569.339 16 -15 -9 -8 12054.1 1104.65 11 -15 -9 -8 9483.46 971.079 23 -15 -9 -8 10217.2 961.385 16 -15 -9 -9 3340.59 741.864 11 -15 -9 -9 3698.00 727.450 23 -15 -9 -9 2560.82 502.892 16 -15 -9 -10 9677.59 1024.50 11 -15 -9 -10 8710.30 1025.04 23 -15 -9 -11 5395.06 806.912 11 -15 -9 -11 4657.23 770.570 23 -15 -9 -12 11361.8 1064.58 11 -15 -9 -12 12596.0 1211.43 23 -15 -9 -13 4901.03 767.102 11 -15 -9 -13 3720.72 745.421 23 -15 -9 -14 21717.8 1414.32 11 -15 -9 -14 19906.1 1428.42 23 -15 -9 -15 1910.82 522.999 11 -15 -9 -15 1600.36 541.600 23 -15 -9 -16 18206.2 1189.50 11 -15 -9 -16 17910.9 1273.18 23 -15 -9 -17 2018.76 462.889 11 -15 -9 -17 2650.91 557.378 23 -15 -10 0 2395.24 439.419 16 -15 -10 -1 6795.38 721.108 16 -15 -10 -2 2306.25 468.855 16 -15 -10 -3 7166.14 797.697 16 -15 -10 -4 7371.27 806.386 16 -15 -10 -5 12410.6 928.957 11 -15 -10 -5 11874.7 996.551 16 -15 -10 -6 8452.38 829.973 11 -15 -10 -6 6101.55 762.619 16 -15 -10 -7 12554.0 1025.14 11 -15 -10 -7 11847.4 978.430 16 -15 -10 -8 8262.56 882.718 11 -15 -10 -8 7042.37 800.136 23 -15 -10 -8 7635.50 766.927 16 -15 -10 -9 9458.48 931.914 11 -15 -10 -9 8759.45 897.410 23 -15 -10 -10 8517.26 904.134 11 -15 -10 -10 6309.31 843.529 23 -15 -10 -11 10454.9 984.000 11 -15 -10 -11 11385.0 1063.30 23 -15 -10 -12 4692.04 714.881 11 -15 -10 -12 4648.27 737.050 23 -15 -10 -13 14194.3 1122.33 11 -15 -10 -13 13662.2 1165.21 23 -15 -10 -14 4027.24 622.763 11 -15 -10 -14 3736.82 663.219 23 -15 -10 -15 17291.8 1159.26 11 -15 -10 -15 17622.3 1241.28 23 -15 -10 -16 187.884 276.694 11 -15 -10 -16 92.1285 323.811 23 -15 -11 -3 3420.95 510.053 16 -15 -11 -4 7203.56 686.426 16 -15 -11 -5 7047.68 712.324 16 -15 -11 -6 2854.70 507.550 16 -15 -11 -7 11818.9 866.185 16 -15 -11 -8 5566.27 641.498 11 -15 -11 -9 12487.3 925.442 11 -15 -11 -10 6353.39 702.685 11 -15 -11 -10 5376.11 690.282 23 -15 -11 -11 3940.92 575.638 11 -15 -11 -11 3332.45 590.348 23 -15 -11 -12 8971.03 811.654 11 -15 -11 -12 8219.81 855.683 23 -15 -11 -13 2535.57 504.428 11 -15 -11 -13 1699.00 459.011 23 -15 -11 -14 3077.54 472.551 11 -15 -11 -14 3564.65 597.860 23 -15 -11 -15 543.293 363.707 23 -16 -1 -3 5044.82 592.831 11 -16 -1 -4 2155.91 449.104 11 -16 -1 -5 8637.38 788.833 11 16 1 5 7784.36 695.646 19 -16 -1 -6 666.485 275.695 11 16 1 6 1344.83 389.935 19 -16 -1 -7 7299.06 677.067 11 16 1 7 9714.01 786.188 19 16 1 8 1917.04 423.646 19 16 1 9 8978.38 764.867 19 16 1 10 3856.48 559.600 19 16 1 11 8349.51 713.795 19 16 1 12 498.362 294.646 19 -16 -2 -1 217.801 277.359 11 -16 -2 -2 12251.0 958.303 11 -16 -2 -3 678.219 357.748 11 -16 -2 -4 14155.9 1060.19 11 -16 -2 -5-370.525 339.504 11 -16 -2 -6 6253.57 731.440 11 -16 -2 -7-429.605 317.409 11 16 2 7 37.6153 343.628 19 -16 -2 -8 12607.5 964.835 11 16 2 8 14229.3 1009.03 19 -16 -2 -9 311.980 269.037 11 16 2 9 972.769 399.307 19 -16 -2 -10 15153.7 983.030 11 16 2 10 18835.7 1123.64 19 16 2 11 100.312 337.417 19 16 2 12 17799.1 1052.14 19 16 2 13 369.241 312.383 19 16 2 14 16300.5 943.135 19 -16 -3 0-438.374 279.498 11 -16 -3 -1 5227.68 620.960 11 -16 -3 -2 778.640 291.446 11 -16 -3 -3 16968.9 1164.75 11 -16 -3 -4-324.311 372.214 11 -16 -3 -5 24023.7 1407.24 11 -16 -3 -6 38.3123 410.363 11 -16 -3 -7 11088.3 983.829 11 -16 -3 -8 1288.02 453.625 11 -16 -3 -9 12739.9 1025.85 11 16 3 9 14628.1 1046.40 19 -16 -3 -10 1194.82 423.043 11 16 3 10 1025.72 462.888 19 -16 -3 -11 15303.2 1033.49 11 16 3 11 16510.7 1083.98 19 -16 -3 -12 118.516 249.404 11 16 3 12-252.713 358.105 19 16 3 13 18128.7 1067.61 19 16 3 14 94.3715 328.194 19 -16 -4 0 4126.37 547.269 11 -16 -4 -1 2498.98 475.459 11 -16 -4 -2 11123.3 924.846 11 -16 -4 -3 857.919 371.291 11 -16 -4 -4 15824.7 1146.51 11 -16 -4 -5 14.9218 353.895 11 -16 -4 -6 25489.7 1515.01 11 -16 -4 -7-35.5580 374.248 11 -16 -4 -8 14489.4 1138.16 11 -16 -4 -9-97.0880 356.398 11 -16 -4 -10 11557.8 982.113 11 -16 -4 -11 144.295 327.918 11 16 4 11 263.831 372.892 19 -16 -4 -12 11013.8 896.206 11 16 4 12 14338.0 1017.99 19 -16 -4 -13 1259.39 382.860 11 16 4 13-367.524 305.177 19 16 4 14 13239.3 904.934 19 -16 -5 -1 9826.30 834.297 11 -16 -5 -2 1845.72 433.508 11 -16 -5 -3 6580.77 756.518 11 -16 -5 -4 3741.72 614.507 11 -16 -5 -5 14563.2 1129.85 11 -16 -5 -6 3903.56 672.393 11 -16 -5 -7 15831.7 1216.17 11 -16 -5 -8 666.586 423.374 11 -16 -5 -9 9445.73 946.162 11 -16 -5 -10 1328.18 463.143 11 -16 -5 -11 7869.37 826.763 11 -16 -5 -12 2976.64 550.760 11 16 5 12 3068.37 532.556 19 -16 -5 -13 7531.16 751.899 11 16 5 13 7789.60 766.043 19 -16 -5 -14 1189.56 347.465 11 16 5 14 1368.74 370.967 19 -16 -5 -16 108.938 271.444 23 -16 -6 -2 8509.11 786.185 11 -16 -6 -3 3308.45 568.566 11 -16 -6 -4 5241.09 674.924 11 -16 -6 -5 6720.80 792.444 11 -16 -6 -6 12665.7 1074.08 11 -16 -6 -7 5465.65 759.743 11 -16 -6 -8 18911.8 1307.94 11 -16 -6 -8 15081.3 1128.30 23 -16 -6 -9 9908.00 988.292 11 -16 -6 -9 8817.78 906.181 23 -16 -6 -10 7607.72 857.842 11 -16 -6 -10 8572.79 909.983 23 -16 -6 -11 4215.47 663.385 11 -16 -6 -12 8973.55 867.450 11 16 6 12 7552.11 745.458 19 -16 -6 -12 8356.43 904.441 23 -16 -6 -13 2804.31 535.748 11 -16 -6 -13 3646.01 657.581 23 16 6 13 2673.00 470.109 19 -16 -6 -14 11776.3 901.815 11 16 6 14 10836.5 780.014 19 -16 -6 -14 11199.7 1021.37 23 -16 -6 -15 1741.20 499.700 23 -16 -6 -16 10893.5 930.739 23 -16 -7 -3 4103.14 549.389 11 -16 -7 -4 3702.53 560.303 11 -16 -7 -5 5101.29 644.489 11 -16 -7 -6 6028.10 734.592 11 -16 -7 -7 6929.01 800.427 11 -16 -7 -8 9257.32 906.979 11 -16 -7 -8 5343.86 635.368 23 -16 -7 -9 18824.2 1276.47 11 -16 -7 -9 15470.8 1123.38 23 -16 -7 -10 9145.00 937.795 11 -16 -7 -10 7693.21 855.677 23 -16 -7 -11 19856.9 1299.38 11 -16 -7 -11 17029.4 1240.95 23 -16 -7 -12 3368.53 587.770 11 -16 -7 -12 3031.25 615.655 23 16 7 12 3353.87 527.846 19 -16 -7 -13 5197.39 652.227 11 16 7 13 5829.28 598.482 19 -16 -7 -13 6254.11 792.067 23 -16 -7 -14 435.301 320.490 11 -16 -7 -14 341.662 369.200 23 -16 -7 -15 6519.37 673.596 11 -16 -7 -15 5785.65 703.595 23 -16 -8 -4 5763.61 617.056 11 -16 -8 -5 3705.86 513.329 11 -16 -8 -6 6342.31 714.962 11 -16 -8 -7 4484.74 623.016 11 -16 -8 -8 6764.93 761.788 11 -16 -8 -9 13747.5 1064.81 11 -16 -8 -9 10756.1 874.718 23 -16 -8 -10 9586.34 917.476 11 -16 -8 -10 8418.42 831.756 23 -16 -8 -11 6762.40 771.434 11 -16 -8 -11 6114.37 752.378 23 -16 -8 -12 4371.62 615.150 11 -16 -8 -12 5673.00 710.247 23 -16 -8 -13 2302.69 501.517 11 -16 -8 -13 2445.16 525.556 23 -16 -8 -14 6980.79 700.736 11 -16 -8 -14 7225.53 778.884 23 -16 -8 -15 1562.61 423.959 23 -16 -9 -7 7063.16 701.134 11 -16 -9 -8 6062.49 665.271 11 -16 -9 -9 3276.92 505.451 11 -16 -9 -10 5088.03 632.175 11 -16 -9 -11 896.622 375.573 11 -16 -9 -12 9707.77 818.308 11 -16 -9 -13 1669.51 384.924 11 0 0 0 0.00 0.00 0 TITL MK-164 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 13.657114 14.535610 22.710963 78.8671 72.9170 73.3409 ZERR 2.00 0.000466 0.000536 0.000777 0.0030 0.0030 0.0031 LATT 1 SFAC C H B N O Si U UNIT 140.00 250.00 2.00 2.00 29.00 6.00 2.00 REM CrysAlisPro recorded range (K): Min=140.0; max=140.0; aver:140.0 TEMP -133 SIZE 0.04 0.10 0.17 TREF HKLF 4 END ; _shelx_hkl_checksum 42702 _olex2_date_sample_data_collection 2021-02-26 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 1.528 _oxdiff_exptl_absorpt_empirical_full_min 0.610 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group U1 U 0.65829(2) 0.22538(2) 0.75530(2) 0.03003(6) Uani 1 1 d . . . . . Si1 Si 0.51678(11) 0.45825(9) 0.81523(7) 0.0365(3) Uani 1 1 d . . . . . Si2 Si 0.79472(11) 0.04760(9) 0.86521(7) 0.0354(3) Uani 1 1 d . . . . . Si3 Si 0.43726(11) 0.16898(10) 0.72266(7) 0.0353(3) Uani 1 1 d . . . . . O1 O 0.5832(3) 0.3499(2) 0.80452(17) 0.0375(7) Uani 1 1 d . . . . . O2 O 0.4885(3) 0.5061(2) 0.74894(19) 0.0424(8) Uani 1 1 d . . . . . O3 O 0.5820(3) 0.5176(3) 0.8364(2) 0.0475(9) Uani 1 1 d . . . . . O4 O 0.4057(3) 0.4645(3) 0.86750(19) 0.0436(8) Uani 1 1 d . . . . . O21 O 0.7238(3) 0.1244(3) 0.82361(17) 0.0402(8) Uani 1 1 d . . . . . O22 O 0.8296(3) 0.0985(3) 0.91099(19) 0.0469(9) Uani 1 1 d . . . . . O23 O 0.7336(3) -0.0308(3) 0.9086(2) 0.0482(9) Uani 1 1 d . . . . . O24 O 0.9017(3) 0.0026(3) 0.8154(2) 0.0459(9) Uani 1 1 d . . . . . O41 O 0.5298(3) 0.1732(2) 0.75293(17) 0.0374(7) Uani 1 1 d . . . . . O42 O 0.3248(3) 0.1737(2) 0.77309(17) 0.0377(7) Uani 1 1 d . . . . . O43 O 0.4637(3) 0.0729(3) 0.6892(2) 0.0471(9) Uani 1 1 d . . . . . O44 O 0.4373(3) 0.2602(3) 0.66757(18) 0.0441(9) Uani 1 1 d . . . . . O61 O 0.8263(3) 0.2770(3) 0.71006(18) 0.0416(8) Uani 1 1 d . . . . . O71 O 0.7564(3) 0.1293(3) 0.66871(19) 0.0454(9) Uani 1 1 d . . . . . N1 N 0.6027(4) 0.3491(3) 0.6682(2) 0.0391(9) Uani 1 1 d D . . . . C1 C 0.4154(5) 0.5969(4) 0.7330(3) 0.0488(13) Uani 1 1 d . . . . . C2 C 0.3060(5) 0.5803(5) 0.7495(4) 0.0600(16) Uani 1 1 d . . . . . H2A H 0.305669 0.531109 0.725539 0.090 Uiso 1 1 calc R U . . . H2B H 0.255851 0.640842 0.739866 0.090 Uiso 1 1 calc R U . . . H2C H 0.285330 0.558002 0.793928 0.090 Uiso 1 1 calc R U . . . C3 C 0.4555(6) 0.6202(5) 0.6642(4) 0.0623(17) Uani 1 1 d . . . . . H3A H 0.527045 0.629518 0.654909 0.093 Uiso 1 1 calc R U . . . H3B H 0.408727 0.679613 0.649636 0.093 Uiso 1 1 calc R U . . . H3C H 0.457003 0.566814 0.643150 0.093 Uiso 1 1 calc R U . . . C4 C 0.4183(6) 0.6759(4) 0.7669(4) 0.0668(19) Uani 1 1 d . . . . . H4A H 0.393122 0.659000 0.811728 0.100 Uiso 1 1 calc R U . . . H4B H 0.372664 0.737256 0.753754 0.100 Uiso 1 1 calc R U . . . H4C H 0.490924 0.682556 0.757214 0.100 Uiso 1 1 calc R U . . . C5 C 0.6904(5) 0.5243(4) 0.8156(3) 0.0520(14) Uani 1 1 d . . . . . C6 C 0.7317(5) 0.5221(5) 0.7469(3) 0.0564(15) Uani 1 1 d . . . . . H6A H 0.728204 0.461145 0.736201 0.085 Uiso 1 1 calc R U . . . H6B H 0.805227 0.527104 0.734198 0.085 Uiso 1 1 calc R U . . . H6C H 0.688733 0.576464 0.725474 0.085 Uiso 1 1 calc R U . . . C7 C 0.6896(6) 0.6209(6) 0.8334(5) 0.081(3) Uani 1 1 d . . . . . H7A H 0.646270 0.673931 0.811349 0.121 Uiso 1 1 calc R U . . . H7B H 0.762033 0.628686 0.822130 0.121 Uiso 1 1 calc R U . . . H7C H 0.660100 0.621881 0.878276 0.121 Uiso 1 1 calc R U . . . C8 C 0.7554(6) 0.4414(6) 0.8509(4) 0.0670(18) Uani 1 1 d . . . . . H8A H 0.730601 0.447955 0.895348 0.101 Uiso 1 1 calc R U . . . H8B H 0.829999 0.443027 0.836231 0.101 Uiso 1 1 calc R U . . . H8C H 0.747558 0.379760 0.843850 0.101 Uiso 1 1 calc R U . . . C9 C 0.3768(5) 0.4666(4) 0.9335(3) 0.0467(13) Uani 1 1 d . . . . . C10 C 0.3624(7) 0.5701(6) 0.9453(4) 0.075(2) Uani 1 1 d . . . . . H10A H 0.430103 0.588094 0.929065 0.112 Uiso 1 1 calc R U . . . H10B H 0.337541 0.574518 0.989981 0.112 Uiso 1 1 calc R U . . . H10C H 0.310364 0.614095 0.924362 0.112 Uiso 1 1 calc R U . . . C11 C 0.4596(6) 0.3970(7) 0.9621(4) 0.071(2) Uani 1 1 d . . . . . H11A H 0.465952 0.331192 0.954471 0.107 Uiso 1 1 calc R U . . . H11B H 0.439387 0.400323 1.006946 0.107 Uiso 1 1 calc R U . . . H11C H 0.527524 0.413980 0.943732 0.107 Uiso 1 1 calc R U . . . C12 C 0.2730(5) 0.4377(6) 0.9578(3) 0.0612(17) Uani 1 1 d . . . . . H12A H 0.250518 0.436190 1.003011 0.092 Uiso 1 1 calc R U . . . H12B H 0.281702 0.373500 0.946597 0.092 Uiso 1 1 calc R U . . . H12C H 0.219297 0.484843 0.939438 0.092 Uiso 1 1 calc R U . . . C21 C 0.7807(6) 0.1280(5) 0.9717(3) 0.0534(14) Uani 1 1 d . . . . . C22 C 0.6661(6) 0.1830(7) 0.9749(5) 0.083(3) Uani 1 1 d . . . . . H22A H 0.664154 0.237507 0.941845 0.124 Uiso 1 1 calc R U . . . H22B H 0.633535 0.207333 1.015272 0.124 Uiso 1 1 calc R U . . . H22C H 0.627079 0.139506 0.969479 0.124 Uiso 1 1 calc R U . . . C23 C 0.8426(7) 0.1956(6) 0.9781(4) 0.072(2) Uani 1 1 d . . . . . H23A H 0.916592 0.160477 0.974577 0.108 Uiso 1 1 calc R U . . . H23B H 0.812474 0.219685 1.018702 0.108 Uiso 1 1 calc R U . . . H23C H 0.838677 0.250178 0.945263 0.108 Uiso 1 1 calc R U . . . C24 C 0.7901(10) 0.0414(7) 1.0198(4) 0.091(3) Uani 1 1 d . . . . . H24A H 0.746229 0.000452 1.016934 0.137 Uiso 1 1 calc R U . . . H24B H 0.766288 0.062751 1.061195 0.137 Uiso 1 1 calc R U . . . H24C H 0.864030 0.004375 1.012739 0.137 Uiso 1 1 calc R U . . . C25 C 0.6703(5) -0.0865(4) 0.8972(3) 0.0475(13) Uani 1 1 d . . . . . C26 C 0.5577(6) -0.0216(6) 0.9032(4) 0.0631(17) Uani 1 1 d . . . . . H26A H 0.558499 0.032472 0.869837 0.095 Uiso 1 1 calc R U . . . H26B H 0.531855 0.003612 0.943426 0.095 Uiso 1 1 calc R U . . . H26C H 0.510903 -0.059478 0.899999 0.095 Uiso 1 1 calc R U . . . C27 C 0.6714(8) -0.1714(6) 0.9476(4) 0.080(2) Uani 1 1 d . . . . . H27A H 0.623053 -0.208265 0.945254 0.120 Uiso 1 1 calc R U . . . H27B H 0.648658 -0.147699 0.988270 0.120 Uiso 1 1 calc R U . . . H27C H 0.743089 -0.213223 0.941989 0.120 Uiso 1 1 calc R U . . . C28 C 0.7154(6) -0.1167(5) 0.8326(3) 0.0593(16) Uani 1 1 d . . . . . H28A H 0.673995 -0.157080 0.825977 0.089 Uiso 1 1 calc R U . . . H28B H 0.789004 -0.153635 0.828042 0.089 Uiso 1 1 calc R U . . . H28C H 0.712348 -0.059078 0.801955 0.089 Uiso 1 1 calc R U . . . C29 C 1.0052(4) -0.0552(4) 0.8224(3) 0.0481(13) Uani 1 1 d . . . . . C30 C 1.0657(6) 0.0108(5) 0.8322(4) 0.0645(18) Uani 1 1 d . . . . . H30A H 1.134131 -0.027737 0.838762 0.097 Uiso 1 1 calc R U . . . H30B H 1.025067 0.044339 0.868560 0.097 Uiso 1 1 calc R U . . . H30C H 1.076890 0.058391 0.795450 0.097 Uiso 1 1 calc R U . . . C31 C 0.9914(7) -0.1339(5) 0.8773(5) 0.077(2) Uani 1 1 d . . . . . H31A H 1.060692 -0.176558 0.879351 0.115 Uiso 1 1 calc R U . . . H31B H 0.946308 -0.171617 0.871876 0.115 Uiso 1 1 calc R U . . . H31C H 0.958515 -0.103893 0.915766 0.115 Uiso 1 1 calc R U . . . C32 C 1.0580(6) -0.0995(6) 0.7629(4) 0.078(2) Uani 1 1 d . . . . . H32A H 1.069864 -0.048270 0.728518 0.117 Uiso 1 1 calc R U . . . H32B H 1.012758 -0.135104 0.755388 0.117 Uiso 1 1 calc R U . . . H32C H 1.125970 -0.143868 0.766066 0.117 Uiso 1 1 calc R U . . . C41 C 0.2707(4) 0.2316(4) 0.8239(3) 0.0407(11) Uani 1 1 d . . . . . C42 C 0.2819(5) 0.3345(4) 0.8047(3) 0.0467(13) Uani 1 1 d . . . . . H42A H 0.247010 0.372003 0.839957 0.070 Uiso 1 1 calc R U . . . H42B H 0.248834 0.363790 0.770363 0.070 Uiso 1 1 calc R U . . . H42C H 0.356940 0.334482 0.791302 0.070 Uiso 1 1 calc R U . . . C43 C 0.3172(6) 0.1856(5) 0.8786(3) 0.0587(16) Uani 1 1 d . . . . . H43A H 0.387940 0.196310 0.870173 0.088 Uiso 1 1 calc R U . . . H43B H 0.321978 0.115975 0.885071 0.088 Uiso 1 1 calc R U . . . H43C H 0.271801 0.214723 0.915864 0.088 Uiso 1 1 calc R U . . . C44 C 0.1562(5) 0.2276(5) 0.8382(3) 0.0554(15) Uani 1 1 d . . . . . H44A H 0.113607 0.267868 0.871201 0.083 Uiso 1 1 calc R U . . . H44B H 0.150909 0.160580 0.851897 0.083 Uiso 1 1 calc R U . . . H44C H 0.130211 0.251645 0.800860 0.083 Uiso 1 1 calc R U . . . C45 C 0.4383(5) -0.0195(4) 0.7086(3) 0.0529(15) Uani 1 1 d . . . . . C46 C 0.4551(11) -0.0573(6) 0.7718(5) 0.106(4) Uani 1 1 d . . . . . H46A H 0.404124 -0.015596 0.801958 0.159 Uiso 1 1 calc R U . . . H46B H 0.527040 -0.057975 0.771801 0.159 Uiso 1 1 calc R U . . . H46C H 0.445168 -0.123195 0.783010 0.159 Uiso 1 1 calc R U . . . C47 C 0.3246(6) -0.0076(5) 0.7100(4) 0.071(2) Uani 1 1 d . . . . . H47A H 0.305187 -0.069246 0.726134 0.107 Uiso 1 1 calc R U . . . H47B H 0.315021 0.012542 0.667889 0.107 Uiso 1 1 calc R U . . . H47C H 0.279470 0.041720 0.736863 0.107 Uiso 1 1 calc R U . . . C48 C 0.5082(8) -0.0828(6) 0.6604(6) 0.109(4) Uani 1 1 d . . . . . H48A H 0.499135 -0.148788 0.673297 0.163 Uiso 1 1 calc R U . . . H48B H 0.581981 -0.082967 0.655417 0.163 Uiso 1 1 calc R U . . . H48C H 0.489275 -0.058067 0.620864 0.163 Uiso 1 1 calc R U . . . C49 C 0.3840(5) 0.2916(5) 0.6175(3) 0.0495(13) Uani 1 1 d . . . . . C50 C 0.2800(6) 0.2627(5) 0.6349(4) 0.0612(17) Uani 1 1 d . . . . . H50A H 0.236688 0.286083 0.674418 0.092 Uiso 1 1 calc R U . . . H50B H 0.293688 0.192080 0.639150 0.092 Uiso 1 1 calc R U . . . H50C H 0.242462 0.291244 0.602486 0.092 Uiso 1 1 calc R U . . . C51 C 0.4582(7) 0.2541(7) 0.5600(4) 0.076(2) Uani 1 1 d . . . . . H51A H 0.425516 0.279006 0.525206 0.114 Uiso 1 1 calc R U . . . H51B H 0.474485 0.183251 0.565632 0.114 Uiso 1 1 calc R U . . . H51C H 0.523555 0.275245 0.551355 0.114 Uiso 1 1 calc R U . . . C52 C 0.3594(6) 0.4027(5) 0.6097(3) 0.0622(17) Uani 1 1 d . . . . . H52A H 0.319203 0.429020 0.578300 0.093 Uiso 1 1 calc R U . . . H52B H 0.425629 0.423356 0.596491 0.093 Uiso 1 1 calc R U . . . H52C H 0.317611 0.426477 0.649332 0.093 Uiso 1 1 calc R U . . . C61 C 0.9160(5) 0.2386(6) 0.7372(3) 0.0615(17) Uani 1 1 d . . . . . H61A H 0.916186 0.172482 0.758629 0.074 Uiso 1 1 calc R U . . . H61B H 0.914379 0.280457 0.767208 0.074 Uiso 1 1 calc R U . . . C62 C 1.0114(5) 0.2377(6) 0.6827(4) 0.0665(19) Uani 1 1 d . . . . . H62A H 1.031271 0.178176 0.662375 0.080 Uiso 1 1 calc R U . . . H62B H 1.072644 0.243232 0.695411 0.080 Uiso 1 1 calc R U . . . C63 C 0.9722(5) 0.3268(5) 0.6403(3) 0.0583(16) Uani 1 1 d . . . . . H63A H 0.974033 0.386580 0.654275 0.070 Uiso 1 1 calc R U . . . H63B H 1.014853 0.323065 0.596912 0.070 Uiso 1 1 calc R U . . . C64 C 0.8604(5) 0.3230(5) 0.6468(3) 0.0500(13) Uani 1 1 d . . . . . H64A H 0.814935 0.388929 0.640803 0.060 Uiso 1 1 calc R U . . . H64B H 0.857947 0.284408 0.616025 0.060 Uiso 1 1 calc R U . . . C71 C 0.8392(6) 0.0427(5) 0.6762(3) 0.0609(17) Uani 1 1 d . . . . . H71A H 0.842927 0.026206 0.720010 0.073 Uiso 1 1 calc R U . . . H71B H 0.908791 0.050910 0.649854 0.073 Uiso 1 1 calc R U . . . C72 C 0.8063(8) -0.0337(5) 0.6558(4) 0.081(3) Uani 1 1 d . . . . . H72A H 0.867319 -0.088546 0.643173 0.097 Uiso 1 1 calc R U . . . H72B H 0.751205 -0.058122 0.689155 0.097 Uiso 1 1 calc R U . . . C73 C 0.7639(8) 0.0197(6) 0.6019(4) 0.079(2) Uani 1 1 d . . . . . H73A H 0.707356 -0.006938 0.598022 0.095 Uiso 1 1 calc R U . . . H73B H 0.820799 0.014466 0.562922 0.095 Uiso 1 1 calc R U . . . C74 C 0.7210(6) 0.1232(6) 0.6145(3) 0.0599(17) Uani 1 1 d . . . . . H74A H 0.749046 0.166960 0.578258 0.072 Uiso 1 1 calc R U . . . H74B H 0.642873 0.141200 0.623725 0.072 Uiso 1 1 calc R U . . . O81 O 0.999(8) 0.5019(17) 0.9969(19) 0.054(2) Uani 0.5 1 d D U P A -1 C81 C 0.9868(12) 0.5931(10) 0.9597(7) 0.061(3) Uani 0.5 1 d D U P A -1 H81A H 0.925456 0.606177 0.941880 0.073 Uiso 0.5 1 calc R U P A -1 H81B H 1.050969 0.594625 0.925385 0.073 Uiso 0.5 1 calc R U P A -1 C82 C 0.970(2) 0.6665(15) 1.0022(11) 0.064(5) Uani 0.5 1 d D U P A -1 H82A H 0.958258 0.731457 0.979291 0.096 Uiso 0.5 1 calc R U P A -1 H82B H 1.032192 0.653924 1.018277 0.096 Uiso 0.5 1 calc R U P A -1 H82C H 0.907788 0.662111 1.036874 0.096 Uiso 0.5 1 calc R U P A -1 C83 C 1.0029(11) 0.4246(9) 0.9654(7) 0.058(3) Uani 0.5 1 d D U P A -1 H83A H 1.067240 0.414186 0.930635 0.070 Uiso 0.5 1 calc R U P A -1 H83B H 0.940222 0.438968 0.948596 0.070 Uiso 0.5 1 calc R U P A -1 C84 C 1.005(3) 0.3364(16) 1.0129(12) 0.085(8) Uani 0.5 1 d D U P A -1 H84A H 1.005055 0.281226 0.993921 0.128 Uiso 0.5 1 calc R U P A -1 H84B H 0.942156 0.348825 1.047754 0.128 Uiso 0.5 1 calc R U P A -1 H84C H 1.068587 0.321789 1.027952 0.128 Uiso 0.5 1 calc R U P A -1 H1A H 0.554(7) 0.321(7) 0.656(5) 0.102 Uiso 1 1 d D U . . . H1B H 0.568(7) 0.408(4) 0.689(4) 0.102 Uiso 1 1 d D U . . . H1C H 0.660(6) 0.354(7) 0.630(3) 0.102 Uiso 1 1 d D U . . . C101 C 1.0562(4) 0.2744(3) 0.4276(3) 0.0391(11) Uani 1 1 d . . . . . C102 C 1.1502(5) 0.2845(4) 0.3845(3) 0.0454(12) Uani 1 1 d . . . . . H102 H 1.147586 0.312552 0.343406 0.054 Uiso 1 1 calc R U . . . C103 C 1.2474(5) 0.2556(4) 0.3988(3) 0.0519(14) Uani 1 1 d . . . . . H103 H 1.309411 0.264142 0.367907 0.062 Uiso 1 1 calc R U . . . C104 C 1.2536(5) 0.2137(4) 0.4591(3) 0.0532(15) Uani 1 1 d . . . . . H104 H 1.319719 0.193573 0.469444 0.064 Uiso 1 1 calc R U . . . C105 C 1.1629(5) 0.2023(4) 0.5029(3) 0.0496(14) Uani 1 1 d . . . . . H105 H 1.166176 0.173745 0.543785 0.059 Uiso 1 1 calc R U . . . C106 C 1.0658(5) 0.2323(4) 0.4877(3) 0.0423(12) Uani 1 1 d . . . . . H106 H 1.003999 0.224196 0.518869 0.051 Uiso 1 1 calc R U . . . C107 C 0.8580(5) 0.3817(4) 0.4635(3) 0.0403(11) Uani 1 1 d . . . . . C108 C 0.8931(5) 0.4527(4) 0.4804(3) 0.0449(12) Uani 1 1 d . . . . . H108 H 0.965722 0.453024 0.465367 0.054 Uiso 1 1 calc R U . . . C109 C 0.8265(5) 0.5220(4) 0.5180(3) 0.0511(14) Uani 1 1 d . . . . . H109 H 0.853434 0.569294 0.527450 0.061 Uiso 1 1 calc R U . . . C110 C 0.7214(5) 0.5224(4) 0.5415(3) 0.0530(14) Uani 1 1 d . . . . . H110 H 0.675234 0.569496 0.567439 0.064 Uiso 1 1 calc R U . . . C111 C 0.6841(5) 0.4532(5) 0.5269(3) 0.0517(14) Uani 1 1 d . . . . . H111 H 0.611606 0.452840 0.542878 0.062 Uiso 1 1 calc R U . . . C112 C 0.7514(4) 0.3842(4) 0.4892(3) 0.0431(12) Uani 1 1 d . . . . . H112 H 0.723653 0.336789 0.480472 0.052 Uiso 1 1 calc R U . . . C113 C 0.8916(4) 0.2154(4) 0.4147(3) 0.0404(11) Uani 1 1 d . . . . . C114 C 0.8049(5) 0.2272(4) 0.3911(3) 0.0517(14) Uani 1 1 d . . . . . H114 H 0.774073 0.289998 0.373853 0.062 Uiso 1 1 calc R U . . . C115 C 0.7616(6) 0.1518(4) 0.3916(3) 0.0568(16) Uani 1 1 d . . . . . H115 H 0.702156 0.163947 0.375014 0.068 Uiso 1 1 calc R U . . . C116 C 0.8038(6) 0.0592(4) 0.4159(3) 0.0539(15) Uani 1 1 d . . . . . H116 H 0.773740 0.007310 0.416927 0.065 Uiso 1 1 calc R U . . . C117 C 0.8912(5) 0.0443(4) 0.4387(3) 0.0502(14) Uani 1 1 d . . . . . H117 H 0.923150 -0.019041 0.454604 0.060 Uiso 1 1 calc R U . . . C118 C 0.9327(5) 0.1211(4) 0.4387(3) 0.0440(12) Uani 1 1 d . . . . . H118 H 0.991513 0.108802 0.455840 0.053 Uiso 1 1 calc R U . . . C119 C 0.9513(4) 0.3677(4) 0.3418(3) 0.0406(11) Uani 1 1 d . . . . . C120 C 0.9911(6) 0.3175(4) 0.2899(3) 0.0523(14) Uani 1 1 d . . . . . H120 H 1.008216 0.248818 0.296455 0.063 Uiso 1 1 calc R U . . . C121 C 1.0070(6) 0.3622(5) 0.2294(3) 0.0565(15) Uani 1 1 d . . . . . H121 H 1.035413 0.324349 0.195788 0.068 Uiso 1 1 calc R U . . . C122 C 0.9815(5) 0.4619(5) 0.2182(3) 0.0523(14) Uani 1 1 d . . . . . H122 H 0.990047 0.493643 0.177005 0.063 Uiso 1 1 calc R U . . . C123 C 0.9433(5) 0.5139(4) 0.2682(3) 0.0511(14) Uani 1 1 d . . . . . H123 H 0.927512 0.582571 0.261156 0.061 Uiso 1 1 calc R U . . . C124 C 0.9273(4) 0.4685(4) 0.3285(3) 0.0430(12) Uani 1 1 d . . . . . H124 H 0.899177 0.506883 0.361843 0.052 Uiso 1 1 calc R U . . . B1 B 0.9391(5) 0.3088(4) 0.4128(3) 0.0392(12) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.02866(9) 0.02697(8) 0.03720(9) -0.00333(5) -0.01194(6) -0.00767(6) Si1 0.0341(7) 0.0278(6) 0.0487(8) -0.0085(5) -0.0095(6) -0.0079(5) Si2 0.0362(7) 0.0310(6) 0.0427(7) -0.0008(5) -0.0170(6) -0.0092(5) Si3 0.0330(7) 0.0357(6) 0.0437(7) -0.0042(5) -0.0138(6) -0.0148(5) O1 0.044(2) 0.0287(16) 0.0442(19) -0.0111(14) -0.0150(16) -0.0072(14) O2 0.043(2) 0.0288(16) 0.054(2) -0.0043(15) -0.0161(17) -0.0030(15) O3 0.040(2) 0.044(2) 0.063(3) -0.0172(18) -0.0066(18) -0.0171(17) O4 0.039(2) 0.0424(19) 0.053(2) -0.0122(16) -0.0102(17) -0.0130(16) O21 0.0391(19) 0.0398(18) 0.044(2) 0.0024(15) -0.0216(16) -0.0067(15) O22 0.051(2) 0.043(2) 0.051(2) -0.0069(17) -0.0186(19) -0.0126(17) O23 0.052(2) 0.0397(19) 0.057(2) 0.0007(17) -0.0204(19) -0.0157(17) O24 0.040(2) 0.044(2) 0.056(2) -0.0095(17) -0.0165(18) -0.0069(16) O41 0.0362(18) 0.0358(17) 0.046(2) 0.0008(14) -0.0161(15) -0.0162(14) O42 0.0348(18) 0.0371(17) 0.047(2) -0.0086(15) -0.0095(15) -0.0166(14) O43 0.041(2) 0.048(2) 0.057(2) -0.0163(18) -0.0041(18) -0.0214(17) O44 0.044(2) 0.053(2) 0.046(2) 0.0029(16) -0.0221(17) -0.0228(17) O61 0.0354(19) 0.048(2) 0.047(2) -0.0031(16) -0.0132(16) -0.0180(16) O71 0.043(2) 0.047(2) 0.051(2) -0.0226(17) -0.0125(17) -0.0057(17) N1 0.038(2) 0.041(2) 0.043(2) -0.0013(18) -0.0181(19) -0.0121(19) C1 0.046(3) 0.029(2) 0.066(4) 0.000(2) -0.017(3) -0.002(2) C2 0.047(3) 0.051(3) 0.076(5) 0.003(3) -0.019(3) -0.007(3) C3 0.058(4) 0.041(3) 0.074(5) 0.007(3) -0.018(3) 0.001(3) C4 0.071(5) 0.033(3) 0.096(6) -0.007(3) -0.029(4) -0.005(3) C5 0.045(3) 0.051(3) 0.068(4) -0.015(3) -0.008(3) -0.024(3) C6 0.051(4) 0.051(3) 0.063(4) -0.003(3) -0.002(3) -0.022(3) C7 0.064(5) 0.070(5) 0.125(7) -0.045(5) -0.003(5) -0.038(4) C8 0.049(4) 0.079(5) 0.078(5) -0.003(4) -0.018(3) -0.026(3) C9 0.039(3) 0.054(3) 0.052(3) -0.020(3) -0.008(2) -0.013(2) C10 0.075(5) 0.073(5) 0.083(5) -0.044(4) 0.003(4) -0.029(4) C11 0.045(4) 0.100(6) 0.063(4) 0.000(4) -0.014(3) -0.017(4) C12 0.047(3) 0.078(5) 0.062(4) -0.020(3) -0.003(3) -0.023(3) C21 0.058(4) 0.053(3) 0.053(3) -0.015(3) -0.017(3) -0.013(3) C22 0.054(4) 0.101(6) 0.093(6) -0.048(5) -0.016(4) 0.001(4) C23 0.085(5) 0.069(4) 0.077(5) -0.026(4) -0.031(4) -0.020(4) C24 0.143(9) 0.088(6) 0.060(5) 0.004(4) -0.043(6) -0.043(6) C25 0.049(3) 0.046(3) 0.057(3) 0.003(2) -0.021(3) -0.024(3) C26 0.054(4) 0.075(4) 0.067(4) -0.010(3) -0.018(3) -0.023(3) C27 0.101(6) 0.069(5) 0.089(6) 0.021(4) -0.046(5) -0.047(5) C28 0.054(4) 0.055(4) 0.076(5) -0.020(3) -0.017(3) -0.015(3) C29 0.035(3) 0.040(3) 0.070(4) -0.012(3) -0.023(3) 0.002(2) C30 0.049(4) 0.068(4) 0.086(5) -0.014(4) -0.024(4) -0.017(3) C31 0.064(5) 0.056(4) 0.109(7) 0.014(4) -0.039(5) -0.010(3) C32 0.056(4) 0.083(5) 0.099(6) -0.046(5) -0.020(4) 0.000(4) C41 0.042(3) 0.044(3) 0.040(3) -0.008(2) -0.008(2) -0.017(2) C42 0.043(3) 0.037(3) 0.063(4) -0.009(2) -0.019(3) -0.006(2) C43 0.072(4) 0.053(3) 0.047(3) -0.002(3) -0.017(3) -0.008(3) C44 0.045(3) 0.056(3) 0.067(4) -0.022(3) 0.001(3) -0.021(3) C45 0.049(3) 0.048(3) 0.072(4) -0.021(3) -0.013(3) -0.021(3) C46 0.177(12) 0.050(4) 0.130(9) 0.018(5) -0.098(9) -0.045(6) C47 0.057(4) 0.054(4) 0.112(6) -0.026(4) -0.011(4) -0.028(3) C48 0.085(6) 0.069(5) 0.158(10) -0.068(6) 0.045(6) -0.039(5) C49 0.050(3) 0.059(3) 0.047(3) 0.004(3) -0.023(3) -0.021(3) C50 0.054(4) 0.072(4) 0.071(4) 0.008(3) -0.036(3) -0.026(3) C51 0.063(5) 0.110(6) 0.057(4) -0.017(4) -0.022(4) -0.015(4) C52 0.066(4) 0.063(4) 0.063(4) 0.014(3) -0.033(4) -0.021(3) C61 0.037(3) 0.081(5) 0.068(4) 0.007(3) -0.016(3) -0.022(3) C62 0.035(3) 0.089(5) 0.075(5) -0.012(4) -0.003(3) -0.024(3) C63 0.048(3) 0.077(4) 0.055(4) -0.012(3) 0.001(3) -0.034(3) C64 0.044(3) 0.063(4) 0.045(3) -0.006(3) -0.005(2) -0.022(3) C71 0.056(4) 0.058(4) 0.059(4) -0.015(3) -0.018(3) 0.009(3) C72 0.114(7) 0.050(4) 0.062(5) -0.015(3) 0.007(4) -0.019(4) C73 0.109(7) 0.075(5) 0.063(5) -0.025(4) -0.004(4) -0.044(5) C74 0.053(4) 0.084(5) 0.049(3) -0.028(3) -0.017(3) -0.009(3) O81 0.050(5) 0.050(3) 0.061(6) -0.006(3) -0.011(7) -0.016(4) C81 0.053(6) 0.061(6) 0.066(7) -0.007(5) -0.010(5) -0.015(5) C82 0.055(11) 0.053(9) 0.076(11) -0.021(7) 0.009(8) -0.018(7) C83 0.051(6) 0.050(5) 0.072(7) -0.011(5) -0.009(5) -0.015(5) C84 0.080(16) 0.065(11) 0.099(15) -0.008(10) -0.005(12) -0.019(10) C101 0.041(3) 0.027(2) 0.054(3) -0.010(2) -0.017(2) -0.007(2) C102 0.042(3) 0.033(2) 0.060(3) -0.010(2) -0.011(3) -0.007(2) C103 0.040(3) 0.042(3) 0.073(4) -0.017(3) -0.010(3) -0.006(2) C104 0.044(3) 0.039(3) 0.083(5) -0.017(3) -0.025(3) -0.004(2) C105 0.057(4) 0.034(3) 0.065(4) -0.010(2) -0.031(3) -0.004(2) C106 0.043(3) 0.036(3) 0.052(3) -0.010(2) -0.016(2) -0.011(2) C107 0.046(3) 0.031(2) 0.043(3) 0.002(2) -0.015(2) -0.008(2) C108 0.044(3) 0.039(3) 0.051(3) -0.007(2) -0.010(2) -0.009(2) C109 0.058(4) 0.042(3) 0.052(3) -0.010(2) -0.012(3) -0.009(3) C110 0.052(3) 0.046(3) 0.049(3) -0.006(3) -0.012(3) 0.006(3) C111 0.039(3) 0.055(3) 0.046(3) 0.008(3) -0.007(2) -0.001(3) C112 0.041(3) 0.038(3) 0.050(3) 0.008(2) -0.016(2) -0.012(2) C113 0.040(3) 0.034(2) 0.049(3) -0.006(2) -0.014(2) -0.007(2) C114 0.054(3) 0.036(3) 0.072(4) 0.005(3) -0.030(3) -0.014(2) C115 0.058(4) 0.047(3) 0.081(5) 0.000(3) -0.039(4) -0.020(3) C116 0.062(4) 0.037(3) 0.072(4) -0.001(3) -0.024(3) -0.023(3) C117 0.058(4) 0.034(3) 0.061(4) 0.000(2) -0.023(3) -0.012(3) C118 0.046(3) 0.039(3) 0.052(3) -0.002(2) -0.020(3) -0.013(2) C119 0.037(3) 0.037(3) 0.053(3) -0.004(2) -0.017(2) -0.012(2) C120 0.065(4) 0.039(3) 0.055(4) -0.005(2) -0.018(3) -0.013(3) C121 0.067(4) 0.056(3) 0.048(3) -0.007(3) -0.015(3) -0.015(3) C122 0.048(3) 0.061(4) 0.052(3) 0.007(3) -0.018(3) -0.024(3) C123 0.046(3) 0.044(3) 0.064(4) 0.007(3) -0.021(3) -0.015(3) C124 0.038(3) 0.041(3) 0.054(3) -0.004(2) -0.016(2) -0.011(2) B1 0.038(3) 0.029(3) 0.052(3) -0.009(2) -0.013(3) -0.006(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0100 0 0 1 0.0286 -1 0 0 0.0867 1 0 0 0.0545 -1 -1 -1 0.0370 1 1 1 0.0569 0 1 0 0.0429 0 -2 -1 0.0743 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 U1 O61 93.28(13) . . ? O1 U1 O71 159.40(14) . . ? O1 U1 N1 80.03(14) . . ? O21 U1 O1 101.22(14) . . ? O21 U1 O61 91.34(13) . . ? O21 U1 O71 95.39(14) . . ? O21 U1 N1 172.99(14) . . ? O41 U1 O1 103.53(14) . . ? O41 U1 O21 103.07(13) . . ? O41 U1 O61 155.05(14) . . ? O41 U1 O71 84.25(14) . . ? O41 U1 N1 83.21(13) . . ? O61 U1 N1 81.68(13) . . ? O71 U1 O61 74.09(13) . . ? O71 U1 N1 82.04(15) . . ? O1 Si1 O2 104.90(19) . . ? O1 Si1 O3 111.9(2) . . ? O1 Si1 O4 113.7(2) . . ? O3 Si1 O2 112.6(2) . . ? O4 Si1 O2 107.2(2) . . ? O4 Si1 O3 106.6(2) . . ? O21 Si2 O22 112.7(2) . . ? O21 Si2 O23 112.1(2) . . ? O21 Si2 O24 104.1(2) . . ? O23 Si2 O22 106.7(2) . . ? O23 Si2 O24 114.6(2) . . ? O24 Si2 O22 106.6(2) . . ? O41 Si3 O44 103.07(18) . . ? O42 Si3 O41 112.7(2) . . ? O42 Si3 O43 106.77(19) . . ? O42 Si3 O44 114.2(2) . . ? O43 Si3 O41 113.6(2) . . ? O43 Si3 O44 106.5(2) . . ? Si1 O1 U1 157.2(2) . . ? C1 O2 Si1 130.5(4) . . ? C5 O3 Si1 132.7(4) . . ? C9 O4 Si1 132.9(3) . . ? Si2 O21 U1 168.9(2) . . ? C21 O22 Si2 134.1(4) . . ? C25 O23 Si2 132.9(4) . . ? C29 O24 Si2 132.1(4) . . ? Si3 O41 U1 153.4(2) . . ? C41 O42 Si3 131.8(3) . . ? C45 O43 Si3 134.0(4) . . ? C49 O44 Si3 132.7(3) . . ? C61 O61 U1 121.7(3) . . ? C61 O61 C64 109.9(4) . . ? C64 O61 U1 126.0(3) . . ? C71 O71 U1 121.2(4) . . ? C71 O71 C74 107.3(5) . . ? C74 O71 U1 127.7(4) . . ? U1 N1 H1A 103(6) . . ? U1 N1 H1B 103(6) . . ? U1 N1 H1C 114(6) . . ? H1A N1 H1B 114(8) . . ? H1A N1 H1C 105(8) . . ? H1B N1 H1C 117(8) . . ? O2 C1 C2 108.6(5) . . ? O2 C1 C3 104.6(5) . . ? O2 C1 C4 110.2(5) . . ? C2 C1 C4 111.2(6) . . ? C3 C1 C2 111.5(6) . . ? C3 C1 C4 110.5(6) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 111.4(5) . . ? O3 C5 C7 105.3(5) . . ? O3 C5 C8 108.1(5) . . ? C6 C5 C7 110.7(6) . . ? C6 C5 C8 111.3(6) . . ? C8 C5 C7 109.8(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 C10 107.8(5) . . ? O4 C9 C11 110.5(5) . . ? O4 C9 C12 106.1(5) . . ? C11 C9 C10 111.4(6) . . ? C11 C9 C12 110.5(6) . . ? C12 C9 C10 110.2(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O22 C21 C22 109.0(6) . . ? O22 C21 C23 105.0(6) . . ? O22 C21 C24 109.8(6) . . ? C23 C21 C22 109.9(6) . . ? C24 C21 C22 112.7(8) . . ? C24 C21 C23 110.3(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O23 C25 C26 107.5(5) . . ? O23 C25 C27 105.5(5) . . ? O23 C25 C28 110.0(5) . . ? C27 C25 C26 110.7(6) . . ? C27 C25 C28 113.0(6) . . ? C28 C25 C26 109.8(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O24 C29 C30 108.8(5) . . ? O24 C29 C31 109.6(5) . . ? O24 C29 C32 105.4(5) . . ? C30 C29 C31 110.9(6) . . ? C32 C29 C30 111.5(6) . . ? C32 C29 C31 110.5(6) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O42 C41 C42 110.6(4) . . ? O42 C41 C43 108.4(5) . . ? O42 C41 C44 104.6(4) . . ? C42 C41 C44 111.1(5) . . ? C43 C41 C42 110.8(5) . . ? C43 C41 C44 111.1(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O43 C45 C46 109.7(5) . . ? O43 C45 C47 109.0(6) . . ? O43 C45 C48 105.8(6) . . ? C46 C45 C47 109.7(8) . . ? C48 C45 C46 112.9(9) . . ? C48 C45 C47 109.6(6) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O44 C49 C50 111.5(5) . . ? O44 C49 C51 108.5(5) . . ? O44 C49 C52 105.1(5) . . ? C50 C49 C52 107.9(6) . . ? C51 C49 C50 113.5(6) . . ? C51 C49 C52 110.0(6) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O61 C61 H61A 110.8 . . ? O61 C61 H61B 110.8 . . ? O61 C61 C62 104.6(6) . . ? H61A C61 H61B 108.9 . . ? C62 C61 H61A 110.8 . . ? C62 C61 H61B 110.8 . . ? C61 C62 H62A 111.4 . . ? C61 C62 H62B 111.4 . . ? C61 C62 C63 102.1(6) . . ? H62A C62 H62B 109.2 . . ? C63 C62 H62A 111.4 . . ? C63 C62 H62B 111.4 . . ? C62 C63 H63A 111.2 . . ? C62 C63 H63B 111.2 . . ? H63A C63 H63B 109.1 . . ? C64 C63 C62 102.7(5) . . ? C64 C63 H63A 111.2 . . ? C64 C63 H63B 111.2 . . ? O61 C64 C63 104.7(5) . . ? O61 C64 H64A 110.8 . . ? O61 C64 H64B 110.8 . . ? C63 C64 H64A 110.8 . . ? C63 C64 H64B 110.8 . . ? H64A C64 H64B 108.9 . . ? O71 C71 H71A 111.0 . . ? O71 C71 H71B 111.0 . . ? O71 C71 C72 103.6(6) . . ? H71A C71 H71B 109.0 . . ? C72 C71 H71A 111.0 . . ? C72 C71 H71B 111.0 . . ? C71 C72 H72A 111.3 . . ? C71 C72 H72B 111.3 . . ? H72A C72 H72B 109.2 . . ? C73 C72 C71 102.4(6) . . ? C73 C72 H72A 111.3 . . ? C73 C72 H72B 111.3 . . ? C72 C73 H73A 110.5 . . ? C72 C73 H73B 110.5 . . ? C72 C73 C74 106.2(6) . . ? H73A C73 H73B 108.7 . . ? C74 C73 H73A 110.5 . . ? C74 C73 H73B 110.5 . . ? O71 C74 C73 105.4(6) . . ? O71 C74 H74A 110.7 . . ? O71 C74 H74B 110.7 . . ? C73 C74 H74A 110.7 . . ? C73 C74 H74B 110.7 . . ? H74A C74 H74B 108.8 . . ? C81 O81 C83 113(2) . . ? O81 C81 H81A 110.5 . . ? O81 C81 H81B 110.5 . . ? O81 C81 C82 105.9(15) . . ? H81A C81 H81B 108.7 . . ? C82 C81 H81A 110.5 . . ? C82 C81 H81B 110.5 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82B 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O81 C83 H83A 110.5 . . ? O81 C83 H83B 110.5 . . ? O81 C83 C84 106.1(16) . . ? H83A C83 H83B 108.7 . . ? C84 C83 H83A 110.5 . . ? C84 C83 H83B 110.5 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84B 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C102 C101 C106 115.5(5) . . ? C102 C101 B1 124.6(5) . . ? C106 C101 B1 119.9(5) . . ? C101 C102 H102 118.5 . . ? C103 C102 C101 123.1(6) . . ? C103 C102 H102 118.5 . . ? C102 C103 H103 120.2 . . ? C102 C103 C104 119.7(6) . . ? C104 C103 H103 120.2 . . ? C103 C104 H104 120.5 . . ? C105 C104 C103 119.0(6) . . ? C105 C104 H104 120.5 . . ? C104 C105 H105 119.8 . . ? C104 C105 C106 120.4(6) . . ? C106 C105 H105 119.8 . . ? C101 C106 H106 118.8 . . ? C105 C106 C101 122.3(6) . . ? C105 C106 H106 118.8 . . ? C108 C107 B1 120.1(5) . . ? C112 C107 C108 114.9(5) . . ? C112 C107 B1 124.8(5) . . ? C107 C108 H108 118.5 . . ? C109 C108 C107 122.9(6) . . ? C109 C108 H108 118.5 . . ? C108 C109 H109 120.0 . . ? C110 C109 C108 120.0(6) . . ? C110 C109 H109 120.0 . . ? C109 C110 H110 120.5 . . ? C109 C110 C111 118.9(6) . . ? C111 C110 H110 120.5 . . ? C110 C111 H111 119.7 . . ? C110 C111 C112 120.7(6) . . ? C112 C111 H111 119.7 . . ? C107 C112 H112 118.8 . . ? C111 C112 C107 122.5(5) . . ? C111 C112 H112 118.8 . . ? C114 C113 C118 114.9(5) . . ? C114 C113 B1 120.5(5) . . ? C118 C113 B1 124.6(5) . . ? C113 C114 H114 118.4 . . ? C115 C114 C113 123.1(5) . . ? C115 C114 H114 118.4 . . ? C114 C115 H115 119.7 . . ? C116 C115 C114 120.6(6) . . ? C116 C115 H115 119.7 . . ? C115 C116 H116 121.1 . . ? C115 C116 C117 117.9(5) . . ? C117 C116 H116 121.1 . . ? C116 C117 H117 119.7 . . ? C116 C117 C118 120.7(5) . . ? C118 C117 H117 119.7 . . ? C113 C118 H118 118.6 . . ? C117 C118 C113 122.7(5) . . ? C117 C118 H118 118.6 . . ? C120 C119 C124 114.8(5) . . ? C120 C119 B1 120.8(5) . . ? C124 C119 B1 124.4(5) . . ? C119 C120 H120 118.2 . . ? C121 C120 C119 123.7(6) . . ? C121 C120 H120 118.2 . . ? C120 C121 H121 120.1 . . ? C122 C121 C120 119.8(6) . . ? C122 C121 H121 120.1 . . ? C121 C122 H122 120.8 . . ? C123 C122 C121 118.3(6) . . ? C123 C122 H122 120.8 . . ? C122 C123 H123 119.3 . . ? C122 C123 C124 121.4(6) . . ? C124 C123 H123 119.3 . . ? C119 C124 H124 119.0 . . ? C123 C124 C119 122.0(6) . . ? C123 C124 H124 119.0 . . ? C101 B1 C107 108.9(4) . . ? C101 B1 C113 111.7(4) . . ? C101 B1 C119 108.5(5) . . ? C107 B1 C113 110.7(5) . . ? C107 B1 C119 109.5(4) . . ? C113 B1 C119 107.5(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 O1 2.150(3) . ? U1 O21 2.132(3) . ? U1 O41 2.120(3) . ? U1 O61 2.487(3) . ? U1 O71 2.460(4) . ? U1 N1 2.539(4) . ? Si1 O1 1.600(4) . ? Si1 O2 1.638(4) . ? Si1 O3 1.620(4) . ? Si1 O4 1.620(4) . ? Si2 O21 1.609(4) . ? Si2 O22 1.626(4) . ? Si2 O23 1.612(4) . ? Si2 O24 1.616(4) . ? Si3 O41 1.626(3) . ? Si3 O42 1.616(4) . ? Si3 O43 1.618(4) . ? Si3 O44 1.638(4) . ? O2 C1 1.464(6) . ? O3 C5 1.441(7) . ? O4 C9 1.437(7) . ? O22 C21 1.434(8) . ? O23 C25 1.442(6) . ? O24 C29 1.459(7) . ? O42 C41 1.450(6) . ? O43 C45 1.438(7) . ? O44 C49 1.457(7) . ? O61 C61 1.452(7) . ? O61 C64 1.464(7) . ? O71 C71 1.452(8) . ? O71 C74 1.474(7) . ? N1 H1A 0.99(2) . ? N1 H1B 0.99(2) . ? N1 H1C 0.99(2) . ? C1 C2 1.508(9) . ? C1 C3 1.501(10) . ? C1 C4 1.517(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.499(9) . ? C5 C7 1.530(8) . ? C5 C8 1.522(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.526(9) . ? C9 C11 1.499(10) . ? C9 C12 1.511(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 C22 1.528(11) . ? C21 C23 1.517(9) . ? C21 C24 1.502(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.540(10) . ? C25 C27 1.513(9) . ? C25 C28 1.513(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.514(9) . ? C29 C31 1.527(10) . ? C29 C32 1.502(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 C42 1.514(8) . ? C41 C43 1.514(8) . ? C41 C44 1.516(8) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.494(11) . ? C45 C47 1.503(10) . ? C45 C48 1.492(10) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.516(9) . ? C49 C51 1.487(10) . ? C49 C52 1.538(9) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C61 C62 1.510(10) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C62 C63 1.520(11) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C63 C64 1.506(8) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C71 C72 1.501(11) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C72 C73 1.493(13) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C73 C74 1.500(11) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? O81 C81 1.422(19) . ? O81 C83 1.423(19) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C81 C82 1.499(17) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C83 C84 1.507(18) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C101 C102 1.394(8) . ? C101 C106 1.410(8) . ? C101 B1 1.648(8) . ? C102 H102 0.9500 . ? C102 C103 1.387(9) . ? C103 H103 0.9500 . ? C103 C104 1.404(10) . ? C104 H104 0.9500 . ? C104 C105 1.372(10) . ? C105 H105 0.9500 . ? C105 C106 1.395(8) . ? C106 H106 0.9500 . ? C107 C108 1.409(8) . ? C107 C112 1.394(8) . ? C107 B1 1.650(8) . ? C108 H108 0.9500 . ? C108 C109 1.386(8) . ? C109 H109 0.9500 . ? C109 C110 1.376(10) . ? C110 H110 0.9500 . ? C110 C111 1.379(10) . ? C111 H111 0.9500 . ? C111 C112 1.389(9) . ? C112 H112 0.9500 . ? C113 C114 1.393(8) . ? C113 C118 1.393(8) . ? C113 B1 1.653(7) . ? C114 H114 0.9500 . ? C114 C115 1.384(8) . ? C115 H115 0.9500 . ? C115 C116 1.380(9) . ? C116 H116 0.9500 . ? C116 C117 1.383(9) . ? C117 H117 0.9500 . ? C117 C118 1.389(8) . ? C118 H118 0.9500 . ? C119 C120 1.394(9) . ? C119 C124 1.399(8) . ? C119 B1 1.658(9) . ? C120 H120 0.9500 . ? C120 C121 1.385(9) . ? C121 H121 0.9500 . ? C121 C122 1.381(9) . ? C122 H122 0.9500 . ? C122 C123 1.375(10) . ? C123 H123 0.9500 . ? C123 C124 1.386(9) . ? C124 H124 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag U1 O61 C61 C62 148.0(4) . . . . ? U1 O61 C64 C63 -172.5(4) . . . . ? U1 O71 C71 C72 125.6(5) . . . . ? U1 O71 C74 C73 -142.6(5) . . . . ? Si1 O2 C1 C2 -83.5(6) . . . . ? Si1 O2 C1 C3 157.4(4) . . . . ? Si1 O2 C1 C4 38.6(7) . . . . ? Si1 O3 C5 C6 36.4(8) . . . . ? Si1 O3 C5 C7 156.4(6) . . . . ? Si1 O3 C5 C8 -86.2(7) . . . . ? Si1 O4 C9 C10 81.3(6) . . . . ? Si1 O4 C9 C11 -40.8(7) . . . . ? Si1 O4 C9 C12 -160.6(4) . . . . ? Si2 O22 C21 C22 -46.4(8) . . . . ? Si2 O22 C21 C23 -164.1(5) . . . . ? Si2 O22 C21 C24 77.4(8) . . . . ? Si2 O23 C25 C26 -82.8(7) . . . . ? Si2 O23 C25 C27 159.0(6) . . . . ? Si2 O23 C25 C28 36.8(8) . . . . ? Si2 O24 C29 C30 -77.6(7) . . . . ? Si2 O24 C29 C31 43.8(7) . . . . ? Si2 O24 C29 C32 162.7(5) . . . . ? Si3 O42 C41 C42 41.2(6) . . . . ? Si3 O42 C41 C43 -80.5(6) . . . . ? Si3 O42 C41 C44 160.9(4) . . . . ? Si3 O43 C45 C46 -44.9(9) . . . . ? Si3 O43 C45 C47 75.3(7) . . . . ? Si3 O43 C45 C48 -166.9(6) . . . . ? Si3 O44 C49 C50 29.1(8) . . . . ? Si3 O44 C49 C51 -96.6(7) . . . . ? Si3 O44 C49 C52 145.7(5) . . . . ? O1 Si1 O2 C1 168.4(4) . . . . ? O1 Si1 O3 C5 42.9(6) . . . . ? O1 Si1 O4 C9 89.4(5) . . . . ? O2 Si1 O1 U1 -1.7(6) . . . . ? O2 Si1 O3 C5 -74.9(6) . . . . ? O2 Si1 O4 C9 -155.1(5) . . . . ? O3 Si1 O1 U1 -124.1(6) . . . . ? O3 Si1 O2 C1 -69.6(5) . . . . ? O3 Si1 O4 C9 -34.3(5) . . . . ? O4 Si1 O1 U1 115.0(6) . . . . ? O4 Si1 O2 C1 47.3(5) . . . . ? O4 Si1 O3 C5 167.8(5) . . . . ? O21 Si2 O22 C21 85.4(6) . . . . ? O21 Si2 O23 C25 44.5(6) . . . . ? O21 Si2 O24 C29 165.8(4) . . . . ? O22 Si2 O21 U1 94.5(12) . . . . ? O22 Si2 O23 C25 168.3(5) . . . . ? O22 Si2 O24 C29 46.4(5) . . . . ? O23 Si2 O21 U1 -145.1(11) . . . . ? O23 Si2 O22 C21 -38.0(6) . . . . ? O23 Si2 O24 C29 -71.4(5) . . . . ? O24 Si2 O21 U1 -20.6(12) . . . . ? O24 Si2 O22 C21 -160.9(5) . . . . ? O24 Si2 O23 C25 -73.9(6) . . . . ? O41 Si3 O42 C41 41.6(5) . . . . ? O41 Si3 O43 C45 95.2(6) . . . . ? O41 Si3 O44 C49 171.3(5) . . . . ? O42 Si3 O41 U1 -133.0(5) . . . . ? O42 Si3 O43 C45 -29.7(6) . . . . ? O42 Si3 O44 C49 -66.1(6) . . . . ? O43 Si3 O41 U1 105.4(5) . . . . ? O43 Si3 O42 C41 167.0(4) . . . . ? O43 Si3 O44 C49 51.5(6) . . . . ? O44 Si3 O41 U1 -9.4(6) . . . . ? O44 Si3 O42 C41 -75.6(5) . . . . ? O44 Si3 O43 C45 -152.1(5) . . . . ? O61 C61 C62 C63 34.1(7) . . . . ? O71 C71 C72 C73 38.8(8) . . . . ? C61 O61 C64 C63 -9.9(7) . . . . ? C61 C62 C63 C64 -39.9(7) . . . . ? C62 C63 C64 O61 30.9(7) . . . . ? C64 O61 C61 C62 -15.4(7) . . . . ? C71 O71 C74 C73 15.1(7) . . . . ? C71 C72 C73 C74 -29.7(9) . . . . ? C72 C73 C74 O71 9.7(9) . . . . ? C74 O71 C71 C72 -33.9(7) . . . . ? C81 O81 C83 C84 -175(5) . . . . ? C83 O81 C81 C82 173(5) . . . . ? C101 C102 C103 C104 0.2(8) . . . . ? C102 C101 C106 C105 -0.4(7) . . . . ? C102 C101 B1 C107 -125.5(5) . . . . ? C102 C101 B1 C113 111.9(6) . . . . ? C102 C101 B1 C119 -6.4(6) . . . . ? C102 C103 C104 C105 -0.1(8) . . . . ? C103 C104 C105 C106 -0.3(8) . . . . ? C104 C105 C106 C101 0.6(8) . . . . ? C106 C101 C102 C103 0.0(7) . . . . ? C106 C101 B1 C107 53.7(6) . . . . ? C106 C101 B1 C113 -68.9(6) . . . . ? C106 C101 B1 C119 172.8(4) . . . . ? C107 C108 C109 C110 1.3(10) . . . . ? C108 C107 C112 C111 1.9(8) . . . . ? C108 C107 B1 C101 41.7(7) . . . . ? C108 C107 B1 C113 164.9(5) . . . . ? C108 C107 B1 C119 -76.7(6) . . . . ? C108 C109 C110 C111 -0.2(9) . . . . ? C109 C110 C111 C112 0.1(9) . . . . ? C110 C111 C112 C107 -1.0(9) . . . . ? C112 C107 C108 C109 -2.1(8) . . . . ? C112 C107 B1 C101 -143.1(5) . . . . ? C112 C107 B1 C113 -19.9(7) . . . . ? C112 C107 B1 C119 98.4(6) . . . . ? C113 C114 C115 C116 -0.3(12) . . . . ? C114 C113 C118 C117 0.6(9) . . . . ? C114 C113 B1 C101 -166.6(6) . . . . ? C114 C113 B1 C107 71.9(7) . . . . ? C114 C113 B1 C119 -47.7(7) . . . . ? C114 C115 C116 C117 -0.9(11) . . . . ? C115 C116 C117 C118 1.9(11) . . . . ? C116 C117 C118 C113 -1.8(10) . . . . ? C118 C113 C114 C115 0.4(10) . . . . ? C118 C113 B1 C101 13.2(8) . . . . ? C118 C113 B1 C107 -108.4(6) . . . . ? C118 C113 B1 C119 132.0(6) . . . . ? C119 C120 C121 C122 -1.0(11) . . . . ? C120 C119 C124 C123 -0.6(8) . . . . ? C120 C119 B1 C101 78.8(6) . . . . ? C120 C119 B1 C107 -162.5(5) . . . . ? C120 C119 B1 C113 -42.2(7) . . . . ? C120 C121 C122 C123 1.8(10) . . . . ? C121 C122 C123 C124 -2.0(9) . . . . ? C122 C123 C124 C119 1.5(9) . . . . ? C124 C119 C120 C121 0.4(9) . . . . ? C124 C119 B1 C101 -98.9(6) . . . . ? C124 C119 B1 C107 19.8(7) . . . . ? C124 C119 B1 C113 140.2(5) . . . . ? B1 C101 C102 C103 179.3(5) . . . . ? B1 C101 C106 C105 -179.7(5) . . . . ? B1 C107 C108 C109 173.6(5) . . . . ? B1 C107 C112 C111 -173.5(5) . . . . ? B1 C113 C114 C115 -179.8(6) . . . . ? B1 C113 C118 C117 -179.2(6) . . . . ? B1 C119 C120 C121 -177.5(6) . . . . ? B1 C119 C124 C123 177.1(5) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0000 0.0000 -0.9999 -0.0698 -0.0034 0.0149 -0.0000 -0.0000 0.9999 0.0698 0.0034 -0.0149 -1.0001 -0.0000 -0.0000 0.0363 0.1067 0.0460 1.0001 0.0000 0.0000 -0.0363 -0.1067 -0.0460 -1.0000 -1.0000 -1.0000 -0.0002 0.0283 0.1363 1.0000 1.0000 1.0000 0.0002 -0.0283 -0.1363 0.0000 1.0000 0.0000 -0.0333 0.0750 -0.0754 -0.0000 -2.0000 -1.0000 -0.0032 -0.1534 0.1656