#------------------------------------------------------------------------------ #$Date: 2021-08-19 01:12:36 +0300 (Thu, 19 Aug 2021) $ #$Revision: 268126 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564376.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_1564376 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 'C42 H68 N10 Si4 U2, 4(C5 H5 N), 2(C24 H20 B)' _chemical_formula_sum 'C110 H128 B2 N14 Si4 U2' _chemical_formula_weight 2256.30 _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 geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2020-12-14 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226) ; _audit_update_record ; 2021-07-16 deposited with the CCDC. 2021-08-13 downloaded from the CCDC. ; _cell_angle_alpha 103.7856(18) _cell_angle_beta 98.6207(18) _cell_angle_gamma 115.188(2) _cell_formula_units_Z 1 _cell_length_a 13.3639(3) _cell_length_b 14.7692(3) _cell_length_c 17.1055(4) _cell_measurement_reflns_used 19007 _cell_measurement_temperature 140.01(10) _cell_measurement_theta_max 76.1660 _cell_measurement_theta_min 3.6160 _cell_volume 2843.26(13) _computing_cell_refinement 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _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 (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 140.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2665 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.987 _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 -115.00 -13.00 1.00 2.50 -- -43.01 -66.00 -79.00 102 2 \w -60.00 22.00 1.00 2.50 -- -43.01 66.00 54.00 82 3 \w 137.00 178.00 1.00 10.00 -- 112.00 66.00 54.00 41 4 \w 113.00 140.00 1.00 10.00 -- 112.00 -66.00 -79.00 27 5 \w 40.00 72.00 1.00 10.00 -- 112.00 -66.00 -79.00 32 6 \w 93.00 118.00 1.00 10.00 -- 112.00 66.00 54.00 25 7 \w -114.00 -16.00 1.00 2.50 -- -43.01 -57.00-180.00 98 8 \w -21.00 15.00 1.00 2.50 -- 43.01 -77.00 150.00 36 9 \w -7.00 20.00 1.00 2.50 -- 43.01 -77.00 -60.00 27 10 \w 4.00 29.00 1.00 2.50 -- 43.01 -66.00 -79.00 25 11 \w 40.00 65.00 1.00 2.50 -- 43.01 66.00 54.00 25 12 \w 36.00 98.00 1.00 2.50 -- 43.01-125.00-180.00 62 13 \w 36.00 109.00 1.00 10.00 -- 112.00-111.00 120.00 73 14 \w 128.00 174.00 1.00 10.00 -- 112.00 30.00 0.00 46 15 \w 53.00 134.00 1.00 10.00 -- 112.00 -45.00 60.00 81 16 \w 105.00 178.00 1.00 10.00 -- 112.00 77.00 120.00 73 17 \w 41.00 109.00 1.00 10.00 -- 112.00-111.00 60.00 68 18 \w 85.00 110.00 1.00 10.00 -- 112.00 -77.00 120.00 25 19 \w 105.00 147.00 1.00 10.00 -- 112.00 111.00-180.00 42 20 \w 59.00 86.00 1.00 10.00 -- 112.00 -45.00 120.00 27 21 \w 37.00 108.00 1.00 10.00 -- 112.00-111.00 -60.00 71 22 \w 85.00 110.00 1.00 10.00 -- 112.00 30.00 0.00 25 23 \w 57.00 109.00 1.00 10.00 -- 112.00-111.00 0.00 52 24 \w 107.00 136.00 1.00 10.00 -- 112.00 77.00 150.00 29 25 \w 84.00 178.00 1.00 10.00 -- 112.00 30.00 -90.00 94 26 \w 55.00 92.00 1.00 10.00 -- 112.00-111.00 -90.00 37 27 \w 113.00 155.00 1.00 10.00 -- 112.00 111.00 90.00 42 28 \w 106.00 144.00 1.00 10.00 -- 112.00 77.00 30.00 38 29 \w 153.00 178.00 1.00 10.00 -- 112.00 77.00 30.00 25 30 \w 64.00 89.00 1.00 10.00 -- 112.00-111.00 -30.00 25 31 \w 38.00 63.00 1.00 10.00 -- 112.00-111.00 150.00 25 32 \w 75.00 106.00 1.00 10.00 -- 112.00-111.00 150.00 31 33 \w 52.00 96.00 1.00 10.00 -- 112.00-111.00 30.00 44 34 \w 109.00 144.00 1.00 10.00 -- 112.00 111.00 150.00 35 35 \w 131.00 177.00 1.00 10.00 -- 112.00 45.00 90.00 46 36 \w 65.00 104.00 1.00 10.00 -- 112.00-111.00 90.00 39 37 \w 87.00 113.00 1.00 10.00 -- 112.00 -45.00 120.00 26 38 \w 86.00 121.00 1.00 10.00 -- 112.00 45.00 90.00 35 39 \w 66.00 108.00 1.00 10.00 -- 112.00-102.00 164.26 42 40 \w 38.00 109.00 1.00 10.00 -- 112.00-111.00-120.00 71 ; _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 0.0597880000 _diffrn_orient_matrix_UB_12 0.1080646000 _diffrn_orient_matrix_UB_13 0.0715188000 _diffrn_orient_matrix_UB_21 0.1170948000 _diffrn_orient_matrix_UB_22 0.0206548000 _diffrn_orient_matrix_UB_23 -0.0157351000 _diffrn_orient_matrix_UB_31 -0.0196830000 _diffrn_orient_matrix_UB_32 0.0537771000 _diffrn_orient_matrix_UB_33 -0.0632672000 _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 0.0234 _diffrn_reflns_av_unetI/netI 0.0263 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 32842 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.529 _diffrn_reflns_theta_min 2.776 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 8.735 _exptl_absorpt_correction_T_max 0.600 _exptl_absorpt_correction_T_min 0.153 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark brown' _exptl_crystal_density_diffrn 1.318 _exptl_crystal_description prism _exptl_crystal_F_000 1136 _exptl_crystal_size_max 0.357 _exptl_crystal_size_mid 0.103 _exptl_crystal_size_min 0.078 _refine_diff_density_max 1.402 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 601 _refine_ls_number_reflns 11800 _refine_ls_number_restraints 491 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0298 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+2.0899P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.0814 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11293 _reflns_number_total 11800 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc03957a2.cif _cod_data_source_block mk-65-py _cod_original_cell_volume 2843.27(12) _cod_database_code 1564376 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C120 H138 B2 N16 Si4 U2' _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 0.549 _shelx_estimated_absorpt_t_min 0.147 _reflns_odcompleteness_completeness 99.81 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 74.33 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Aromatic/amide H refined with riding coordinates: N1(H1), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55) 3.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A, H5B,H5C), C6(H6A,H6B,H6C) ; _smtbx_masks_special_details ; A solvent mask was calculated and 83 electrons were found in a volume of 352\%A^3^ in 1 void per unit cell. This is consistent with the presence of 1[C5H5N] per Asymmetric Unit which account for 84 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL MK-65-py in P-1 mk-65-py.res created by SHELXL-2018/3 at 14:53:29 on 14-Dec-2020 CELL 1.54184 13.363927 14.769151 17.105492 103.7856 98.6207 115.1875 ZERR 1 0.000301 0.000305 0.000376 0.0018 0.0018 0.0021 LATT 1 SFAC C H B N Si U UNIT 110 128 2 14 4 2 RIGU L.S. 10 PLAN 20 SIZE 0.357 0.103 0.078 TEMP -133 CONF BOND LIST 4 MORE -1 BOND $H WPDB -2 fmap 2 acta ABIN REM REM REM WGHT 0.054000 2.089900 FVAR 3.37085 U1 6 0.478798 0.886835 0.421348 11.00000 0.03714 0.03821 = 0.03203 0.01125 0.01020 0.01753 SI1 5 0.754458 0.906486 0.470863 11.00000 0.04722 0.04850 = 0.05410 0.01070 0.01213 0.02292 SI2 5 0.557752 0.685904 0.374735 11.00000 0.05128 0.04588 = 0.05941 0.00961 0.00915 0.02345 N1 4 0.445495 1.018799 0.442502 11.00000 0.05663 0.04592 = 0.03513 0.01202 0.01224 0.03085 AFIX 43 H1 2 0.408542 1.033095 0.404245 11.00000 -1.20000 AFIX 0 N2 4 0.607392 0.821107 0.421467 11.00000 0.04928 0.04999 = 0.05112 0.01562 0.01418 0.02647 N3 4 0.308282 0.761619 0.465166 11.00000 0.04695 0.04410 = 0.04039 0.01344 0.01449 0.02128 N4 4 0.304409 0.799878 0.280230 11.00000 0.04752 0.04933 = 0.03748 0.01408 0.00929 0.01775 N5 4 0.561268 0.951467 0.302729 11.00000 0.04438 0.05277 = 0.03962 0.01496 0.01437 0.02258 C1 1 0.792134 1.045655 0.476484 11.00000 0.05612 0.04505 = 0.06408 0.01539 0.02188 0.02260 AFIX 137 H1A 2 0.789215 1.051048 0.420270 11.00000 -1.50000 H1B 2 0.870100 1.094658 0.514261 11.00000 -1.50000 H1C 2 0.736828 1.064181 0.497868 11.00000 -1.50000 AFIX 0 C2 1 0.849926 0.872154 0.413066 11.00000 0.05388 0.07128 = 0.08226 0.00161 0.02122 0.02873 AFIX 137 H2A 2 0.839145 0.802081 0.412568 11.00000 -1.50000 H2B 2 0.930781 0.925642 0.441376 11.00000 -1.50000 H2C 2 0.829492 0.870888 0.355203 11.00000 -1.50000 AFIX 0 C3 1 0.799525 0.910255 0.580115 11.00000 0.06299 0.07055 = 0.05320 0.01465 0.00391 0.03470 AFIX 137 H3A 2 0.743191 0.915143 0.609174 11.00000 -1.50000 H3B 2 0.875542 0.972286 0.609746 11.00000 -1.50000 H3C 2 0.803646 0.845327 0.579129 11.00000 -1.50000 AFIX 0 C4 1 0.621935 0.626346 0.437944 11.00000 0.07498 0.05693 = 0.10544 0.02777 -0.00162 0.03082 AFIX 137 H4A 2 0.703644 0.653645 0.440362 11.00000 -1.50000 H4B 2 0.580985 0.548819 0.411598 11.00000 -1.50000 H4C 2 0.614817 0.645355 0.495001 11.00000 -1.50000 AFIX 0 C5 1 0.399107 0.610895 0.362399 11.00000 0.04308 0.04692 = 0.07759 0.00715 0.01387 0.01520 AFIX 137 H5A 2 0.386964 0.610006 0.417367 11.00000 -1.50000 H5B 2 0.367362 0.537793 0.324466 11.00000 -1.50000 H5C 2 0.360152 0.645716 0.338922 11.00000 -1.50000 AFIX 0 C6 1 0.578292 0.648955 0.267369 11.00000 0.06571 0.07371 = 0.06353 -0.00375 0.01463 0.03624 AFIX 137 H6A 2 0.538810 0.672483 0.230372 11.00000 -1.50000 H6B 2 0.545913 0.571657 0.244058 11.00000 -1.50000 H6C 2 0.660840 0.683498 0.271809 11.00000 -1.50000 AFIX 0 C7 1 0.339372 0.754645 0.540511 11.00000 0.05120 0.05382 = 0.04948 0.02138 0.01037 0.01511 AFIX 43 H7 2 0.419302 0.789553 0.569386 11.00000 -1.20000 AFIX 0 C8 1 0.261701 0.699471 0.578744 11.00000 0.06148 0.06347 = 0.05163 0.02664 0.01504 0.01563 AFIX 43 H8 2 0.288094 0.696338 0.632282 11.00000 -1.20000 AFIX 0 C9 1 0.144584 0.648689 0.537853 11.00000 0.05844 0.05220 = 0.05947 0.02222 0.02698 0.01648 AFIX 43 H9 2 0.088887 0.612823 0.563602 11.00000 -1.20000 AFIX 0 C10 1 0.111466 0.651901 0.458497 11.00000 0.04381 0.04403 = 0.06031 0.01545 0.01418 0.01333 AFIX 43 H10 2 0.032188 0.615919 0.427693 11.00000 -1.20000 AFIX 0 C11 1 0.194310 0.707601 0.424723 11.00000 0.05047 0.04286 = 0.04503 0.01359 0.01246 0.01917 AFIX 43 H11 2 0.170160 0.708213 0.369801 11.00000 -1.20000 AFIX 0 C12 1 0.305342 0.739812 0.208770 11.00000 0.06298 0.04794 = 0.04432 0.01176 0.01025 0.02171 AFIX 43 H12 2 0.350118 0.704426 0.211386 11.00000 -1.20000 AFIX 0 C13 1 0.243297 0.727269 0.130919 11.00000 0.09267 0.05239 = 0.03683 0.00884 0.00719 0.02376 AFIX 43 H13 2 0.246478 0.684532 0.081152 11.00000 -1.20000 AFIX 0 C14 1 0.177975 0.776268 0.126044 11.00000 0.07250 0.05596 = 0.04154 0.01809 -0.00718 0.01397 AFIX 43 H14 2 0.135271 0.768724 0.073050 11.00000 -1.20000 AFIX 0 C15 1 0.174696 0.836672 0.198724 11.00000 0.05936 0.06082 = 0.05727 0.02417 0.00056 0.02294 AFIX 43 H15 2 0.129825 0.872099 0.197396 11.00000 -1.20000 AFIX 0 C16 1 0.238023 0.845054 0.274085 11.00000 0.05460 0.06806 = 0.04555 0.01799 0.01106 0.02801 AFIX 43 H16 2 0.233773 0.885571 0.324493 11.00000 -1.20000 AFIX 0 C17 1 0.544740 1.024974 0.279232 11.00000 0.06939 0.06426 = 0.05101 0.02577 0.02699 0.03613 AFIX 43 H17 2 0.503602 1.054311 0.307252 11.00000 -1.20000 AFIX 0 C18 1 0.583835 1.061199 0.216507 11.00000 0.07222 0.06669 = 0.04914 0.02822 0.02065 0.02857 AFIX 43 H18 2 0.569014 1.113339 0.201817 11.00000 -1.20000 AFIX 0 C19 1 0.643675 1.020973 0.176371 11.00000 0.05813 0.08510 = 0.05954 0.03586 0.02933 0.02416 AFIX 43 H19 2 0.672714 1.045517 0.133819 11.00000 -1.20000 AFIX 0 C20 1 0.661237 0.946351 0.197487 11.00000 0.11004 0.14046 = 0.10313 0.06947 0.07866 0.08930 AFIX 43 H20 2 0.700595 0.915366 0.168775 11.00000 -1.20000 AFIX 0 C21 1 0.620771 0.914204 0.262723 11.00000 0.09549 0.10512 = 0.08155 0.05171 0.05271 0.07254 AFIX 43 H21 2 0.636800 0.863432 0.278894 11.00000 -1.20000 AFIX 0 N6 4 0.557510 0.795692 0.702657 11.00000 0.11276 0.10311 = 0.10194 0.00865 -0.00016 0.07029 C22 1 0.566195 0.713825 0.661896 11.00000 0.11577 0.09573 = 0.13936 0.04425 0.03547 0.06805 AFIX 43 H22 2 0.501824 0.660855 0.615870 11.00000 -1.20000 AFIX 0 C23 1 0.657993 0.696800 0.678688 11.00000 0.12352 0.09050 = 0.17050 0.05758 0.05302 0.06945 AFIX 43 H23 2 0.657834 0.634303 0.647261 11.00000 -1.20000 AFIX 0 C24 1 0.751715 0.776307 0.744485 11.00000 0.10738 0.11003 = 0.15437 0.06911 0.03822 0.06474 AFIX 43 H24 2 0.818198 0.768531 0.759775 11.00000 -1.20000 AFIX 0 C25 1 0.750028 0.862650 0.786225 11.00000 0.11793 0.15166 = 0.11502 0.05477 0.03140 0.08679 AFIX 43 H25 2 0.814640 0.917002 0.831467 11.00000 -1.20000 AFIX 0 C26 1 0.652705 0.873111 0.763234 11.00000 0.10793 0.11144 = 0.09323 0.03267 0.03061 0.06428 AFIX 43 H26 2 0.653322 0.937228 0.791271 11.00000 -1.20000 AFIX 0 N7 4 0.946880 0.915070 0.068405 11.00000 0.12804 0.10732 = 0.14267 0.06525 0.07270 0.07160 C27 1 0.907450 0.811356 0.053979 11.00000 0.08246 0.07876 = 0.06940 0.02452 0.02615 0.03916 AFIX 43 H27 2 0.901049 0.767031 0.001039 11.00000 -1.20000 AFIX 0 C28 1 0.876360 0.768309 0.113891 11.00000 0.07881 0.06719 = 0.07214 0.01768 0.01710 0.03122 AFIX 43 H28 2 0.848007 0.694169 0.102245 11.00000 -1.20000 AFIX 0 C29 1 0.885337 0.830390 0.190948 11.00000 0.08744 0.08318 = 0.07101 0.02822 0.02716 0.05280 AFIX 43 H29 2 0.864117 0.799279 0.232520 11.00000 -1.20000 AFIX 0 C30 1 0.922623 0.931278 0.207321 11.00000 0.09148 0.08350 = 0.09354 0.01341 0.02809 0.05816 AFIX 43 H30 2 0.927185 0.974028 0.260335 11.00000 -1.20000 AFIX 0 C31 1 0.955107 0.975577 0.148445 11.00000 0.12548 0.07335 = 0.15620 0.03730 0.06685 0.06007 AFIX 43 H31 2 0.984435 1.050057 0.161717 11.00000 -1.20000 AFIX 0 C32 1 1.065582 0.395694 0.140534 11.00000 0.04214 0.03518 = 0.04374 0.00911 0.01182 0.01605 C33 1 1.045718 0.419956 0.067229 11.00000 0.05300 0.04592 = 0.04500 0.01409 0.01515 0.02157 AFIX 43 H33 2 0.971479 0.410947 0.044225 11.00000 -1.20000 AFIX 0 C34 1 1.130005 0.456649 0.026717 11.00000 0.07849 0.05133 = 0.05559 0.02164 0.03184 0.02634 AFIX 43 H34 2 1.112720 0.472983 -0.022374 11.00000 -1.20000 AFIX 0 C35 1 1.237502 0.469365 0.057042 11.00000 0.06261 0.06001 = 0.07866 0.02177 0.04007 0.01862 AFIX 43 H35 2 1.295123 0.494484 0.029454 11.00000 -1.20000 AFIX 0 C36 1 1.260797 0.445311 0.127835 11.00000 0.04189 0.06835 = 0.07058 0.01078 0.01895 0.01932 AFIX 43 H36 2 1.334919 0.453042 0.149102 11.00000 -1.20000 AFIX 0 C37 1 1.176239 0.409345 0.169286 11.00000 0.04232 0.05489 = 0.05351 0.01249 0.01241 0.02116 AFIX 43 H37 2 1.194906 0.393776 0.218521 11.00000 -1.20000 AFIX 0 C38 1 1.002706 0.323192 0.266963 11.00000 0.04187 0.03806 = 0.03800 0.01059 0.01000 0.01950 C39 1 1.092705 0.405032 0.336972 11.00000 0.04738 0.04072 = 0.04450 0.00974 0.00448 0.01923 AFIX 43 H39 2 1.130497 0.474506 0.333955 11.00000 -1.20000 AFIX 0 C40 1 1.128427 0.388354 0.410152 11.00000 0.05459 0.05755 = 0.04488 0.01146 0.00398 0.02827 AFIX 43 H40 2 1.189960 0.445661 0.455806 11.00000 -1.20000 AFIX 0 C41 1 1.074170 0.287777 0.416664 11.00000 0.06792 0.06770 = 0.04627 0.02416 0.01415 0.04123 AFIX 43 H41 2 1.097699 0.275708 0.466685 11.00000 -1.20000 AFIX 0 C42 1 0.986218 0.206359 0.349762 11.00000 0.07327 0.04895 = 0.05344 0.02287 0.02240 0.03099 AFIX 43 H42 2 0.948416 0.137282 0.353522 11.00000 -1.20000 AFIX 0 C43 1 0.951549 0.223658 0.276270 11.00000 0.05152 0.03969 = 0.04259 0.01238 0.01255 0.01653 AFIX 43 H43 2 0.890736 0.165418 0.230765 11.00000 -1.20000 AFIX 0 C44 1 0.854249 0.244505 0.110414 11.00000 0.04276 0.04623 = 0.03599 0.01417 0.01090 0.01387 C45 1 0.872263 0.159420 0.071597 11.00000 0.04873 0.04683 = 0.03863 0.01184 0.01290 0.01485 AFIX 43 H45 2 0.946096 0.164915 0.089320 11.00000 -1.20000 AFIX 0 C46 1 0.786052 0.067794 0.008368 11.00000 0.06430 0.04682 = 0.04103 0.00507 0.01566 0.01029 AFIX 43 H46 2 0.801370 0.011866 -0.015899 11.00000 -1.20000 AFIX 0 C47 1 0.678569 0.057887 -0.019169 11.00000 0.05445 0.06271 = 0.04037 0.00395 0.00479 -0.00018 AFIX 43 H47 2 0.619278 -0.005115 -0.061893 11.00000 -1.20000 AFIX 0 C48 1 0.657534 0.139339 0.015347 11.00000 0.04052 0.07973 = 0.05200 0.01568 0.00165 0.00984 AFIX 43 H48 2 0.583933 0.133490 -0.004278 11.00000 -1.20000 AFIX 0 C49 1 0.744026 0.230987 0.079329 11.00000 0.04806 0.06256 = 0.04615 0.01530 0.00786 0.02045 AFIX 43 H49 2 0.727377 0.286317 0.102661 11.00000 -1.20000 AFIX 0 C50 1 0.922222 0.441161 0.219464 11.00000 0.03972 0.04261 = 0.03658 0.01392 0.00811 0.01887 C51 1 0.837924 0.418334 0.262938 11.00000 0.05173 0.05554 = 0.05388 0.02330 0.02090 0.02833 AFIX 43 H51 2 0.803102 0.350111 0.268629 11.00000 -1.20000 AFIX 0 C52 1 0.803645 0.491291 0.297776 11.00000 0.05754 0.07168 = 0.06137 0.02307 0.02632 0.03854 AFIX 43 H52 2 0.746432 0.472576 0.326613 11.00000 -1.20000 AFIX 0 C53 1 0.852641 0.591255 0.290591 11.00000 0.06692 0.06251 = 0.06413 0.01789 0.02104 0.04253 AFIX 43 H53 2 0.828693 0.641280 0.313474 11.00000 -1.20000 AFIX 0 C54 1 0.937001 0.617147 0.249575 11.00000 0.06135 0.04854 = 0.05912 0.01927 0.01360 0.02966 AFIX 43 H54 2 0.972093 0.686014 0.245075 11.00000 -1.20000 AFIX 0 C55 1 0.971238 0.543981 0.214837 11.00000 0.04825 0.04992 = 0.04456 0.01839 0.01383 0.02594 AFIX 43 H55 2 1.029598 0.564136 0.187105 11.00000 -1.20000 AFIX 0 B1 3 0.961518 0.350833 0.183968 11.00000 0.03938 0.04084 = 0.03808 0.01292 0.00990 0.01828 HKLF 4 REM MK-65-py in P-1 REM wR2 = 0.0814, GooF = S = 1.032, Restrained GooF = 1.014 for all data REM R1 = 0.0298 for 11293 Fo > 4sig(Fo) and 0.0311 for all 11800 data REM 601 parameters refined using 491 restraints END WGHT 0.0540 2.0899 REM Highest difference peak 1.402, deepest hole -1.062, 1-sigma level 0.090 Q1 1 0.4415 0.9183 0.4262 11.00000 0.05 1.40 Q2 1 0.7001 0.9416 0.4725 11.00000 0.05 1.21 Q3 1 0.4810 0.6914 0.3803 11.00000 0.05 1.12 Q4 1 0.5216 0.8449 0.4201 11.00000 0.05 1.09 Q5 1 0.7152 0.7780 0.8174 11.00000 0.05 0.87 Q6 1 0.4137 0.5156 0.3742 11.00000 0.05 0.80 Q7 1 0.4408 0.6647 0.2671 11.00000 0.05 0.72 Q8 1 0.7236 0.9091 0.5260 11.00000 0.05 0.70 Q9 1 0.5109 0.7496 0.7430 11.00000 0.05 0.70 Q10 1 0.4942 0.9717 0.4113 11.00000 0.05 0.68 Q11 1 0.5406 0.8603 0.3843 11.00000 0.05 0.66 Q12 1 0.5023 0.8879 0.4898 11.00000 0.05 0.55 Q13 1 0.5047 0.5139 0.3479 11.00000 0.05 0.55 Q14 1 0.4690 0.8046 0.4317 11.00000 0.05 0.51 Q15 1 0.4974 1.0416 0.4471 11.00000 0.05 0.50 Q16 1 0.4464 0.7216 0.4021 11.00000 0.05 0.44 Q17 1 0.9224 1.0564 0.5874 11.00000 0.05 0.44 Q18 1 0.5835 0.6105 0.3656 11.00000 0.05 0.43 Q19 1 0.5410 0.6892 0.4309 11.00000 0.05 0.41 Q20 1 0.5722 0.6267 0.3219 11.00000 0.05 0.41 ; 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11234.1 397.883 21 -11 16 -9 2526.36 189.279 30 -11 16 -9 2323.49 180.856 21 -11 16 -10 562.011 90.8099 21 -11 15 7 6985.47 272.342 27 11 -15 -7 7446.94 301.236 22 -11 15 6 7307.50 320.684 27 11 -15 -6 7494.29 340.764 22 -11 15 5 3770.08 208.647 16 -11 15 5 4403.77 279.739 27 11 -15 -5 4189.52 289.047 22 -11 15 4 580.057 102.676 5 -11 15 4 694.923 110.193 16 -11 15 4 868.136 157.959 27 11 -15 -4 656.243 157.675 22 -11 15 3 2642.63 224.318 5 11 -15 -3 3108.92 278.421 22 -11 15 2 9457.16 433.713 5 -11 15 2 10134.9 466.141 27 11 -15 -2 9207.79 476.055 22 -11 15 1 16467.5 609.073 5 -11 15 1 16988.6 633.596 27 -11 15 0 16360.8 620.434 5 -11 15 0 15772.7 609.239 27 -11 15 -1 8875.30 465.320 5 -11 15 -1 8377.67 453.591 27 -11 15 -2 310.672 173.402 5 -11 15 -2 380.814 160.601 27 -11 15 -3 3885.31 325.578 5 -11 15 -3 3346.44 289.949 27 -11 15 -3 3449.19 281.443 23 -11 15 -4 8416.99 455.141 5 -11 15 -4 7323.12 375.441 21 -11 15 -4 8677.21 416.625 23 -11 15 -5 8733.73 447.625 5 -11 15 -5 8604.16 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2825.75 229.406 26 -14 9 -5 3471.81 271.707 21 -14 9 -6 270.988 103.188 26 -14 9 -6 335.704 124.052 21 -14 9 -6 86.8370 126.330 29 -14 9 -7 2410.21 207.440 29 -14 9 -7 2025.68 180.439 26 -14 9 -7 2454.00 194.282 21 -14 9 -8 3528.49 207.302 26 -14 9 -8 3399.00 192.458 21 14 -8 -13 2078.92 138.278 25 -14 8 12 9463.33 345.610 35 14 -8 -12 8870.16 336.449 25 -14 8 11 15097.4 503.912 35 14 -8 -11 15282.0 497.088 25 -14 8 10 15235.5 550.887 35 14 -8 -10 14211.4 517.893 25 -14 8 9 10460.6 486.542 35 -14 8 9 9716.11 381.683 27 14 -8 -9 10397.3 474.634 25 -14 8 8 523.831 114.610 3 -14 8 8 581.045 177.317 35 14 -8 -8 672.809 170.107 25 -14 8 7 1543.95 212.739 3 -14 8 7 2007.79 271.535 35 14 -8 -7 1587.67 232.739 25 -14 8 6 10980.8 512.391 3 -14 8 6 11450.6 557.232 35 14 -8 -6 10763.3 530.307 25 -14 8 5 14982.9 616.360 3 -14 8 5 14696.8 641.884 35 14 -8 -5 14773.4 627.021 25 -14 8 4 14153.3 630.630 3 -14 8 4 12889.9 594.645 35 14 -8 -4 13020.1 596.350 25 -14 8 3 7210.11 466.887 3 -14 8 3 6507.96 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8525.25 510.600 25 -14 7 1 8890.35 516.405 29 -14 7 0 16109.4 675.566 3 14 -7 0 14919.3 654.848 25 -14 7 0 15914.5 703.515 29 -14 7 -1 19869.9 732.051 3 14 -7 1 18078.1 713.680 25 -14 7 -1 18788.2 746.851 29 -14 7 -2 2636.01 273.119 3 -14 7 -2 2560.47 302.018 29 -14 7 -2 2687.75 275.309 21 14 -7 2 2342.99 268.238 25 -14 7 -3 891.322 163.334 3 -14 7 -3 723.587 149.337 26 -14 7 -3 694.895 179.109 21 14 -7 3 739.855 162.157 25 -14 7 -3 928.844 226.781 29 -14 7 -4 2066.93 199.839 3 -14 7 -4 2177.20 222.125 26 14 -7 4 1973.76 214.056 25 -14 7 -4 2612.88 284.853 29 -14 7 -4 2467.02 246.556 21 -14 7 -5 6308.71 377.817 29 -14 7 -5 5630.71 324.955 26 -14 7 -5 6180.67 342.104 21 -14 7 -6 13881.2 513.497 29 -14 7 -6 13762.9 482.649 26 -14 7 -6 13420.0 457.288 21 -14 7 -7 14637.5 463.800 29 -14 7 -7 15479.7 468.899 26 -14 7 -8 6868.50 275.049 26 14 -6 -14 13973.9 371.865 25 -14 6 13 11288.3 372.001 35 14 -6 -13 11923.4 400.205 25 -14 6 12 2373.41 212.549 35 14 -6 -12 2674.55 217.829 25 -14 6 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1 6877.08 459.359 3 14 -5 -1 6493.54 470.151 25 -14 5 0 1214.84 227.652 3 14 -5 0 730.502 209.172 25 -14 5 -1 5506.88 389.349 3 14 -5 1 6158.45 434.000 25 -14 5 -2 17543.8 622.712 3 14 -5 2 17549.8 700.474 25 -14 5 -3 23014.5 662.084 3 -14 5 -3 25586.9 717.792 21 14 -5 3 24381.5 779.550 25 -14 5 -4 19534.7 590.371 21 14 -5 4 19780.5 658.031 25 -14 5 -4 20293.5 688.271 29 14 -5 5 12469.7 477.860 25 -14 5 -5 12893.6 425.756 21 -14 5 -5 13767.5 511.265 29 -14 5 -6 2605.19 202.227 29 -14 5 -6 2068.98 185.352 26 14 -5 6 2129.22 178.713 25 -14 5 -7 602.941 103.672 26 14 -4 -14 430.215 84.2029 25 -14 4 13 4306.89 248.565 35 14 -4 -13 4697.94 260.419 25 -14 4 12 6897.06 347.471 35 14 -4 -12 6404.46 342.178 25 -14 4 11 9245.19 440.210 35 14 -4 -11 9290.65 440.124 25 -14 4 10 15648.6 510.559 3 14 -4 -10 18888.1 656.897 25 -14 4 9 9910.24 452.199 3 14 -4 -9 11475.1 540.280 25 -14 4 8 2557.84 260.841 3 14 -4 -8 2358.44 292.050 25 -14 4 7 697.930 198.348 3 14 -4 -7 476.680 191.412 25 14 -4 -6 6785.29 467.521 25 14 -4 -5 25763.9 896.239 25 14 -4 -4 33066.3 1050.12 25 14 -4 -3 10968.5 608.221 25 14 -4 -2 4271.60 393.829 25 14 -4 -1 869.813 228.147 25 -14 4 0 15274.8 636.012 3 14 -4 0 14098.3 657.989 25 -14 4 -1 32077.6 892.261 3 14 -4 1 31797.9 961.956 25 -14 4 -2 22168.5 677.502 3 14 -4 2 23416.5 784.564 25 -14 4 -3 18375.1 574.352 21 14 -4 3 17998.7 664.784 25 14 -4 4 5564.50 343.540 25 -14 4 -4 5783.51 285.708 21 -14 4 -5-79.0487 68.6196 21 14 -4 5-49.5718 97.3843 25 -14 4 -5-76.3251 109.548 29 14 -4 6 1205.25 134.245 25 -14 4 -6 930.562 113.884 29 14 -3 -14 1450.95 139.664 31 -14 3 13 7416.70 322.719 35 14 -3 -13 7684.30 323.033 25 -14 3 12 12934.4 482.073 35 14 -3 -12 13499.2 481.791 25 14 -3 -11 11792.2 406.940 13 14 -3 -11 14755.8 549.280 25 -14 3 10 8373.54 377.014 3 14 -3 -10 9012.06 464.663 25 -14 3 9 269.355 120.585 3 14 -3 -9 314.773 164.714 25 14 -3 -8 3641.38 328.067 25 14 -3 -7 10893.3 559.565 25 14 -3 -6 18315.5 730.512 25 14 -3 -5 12375.6 631.484 25 14 -3 -4 6452.16 459.692 25 -14 3 3 119.147 163.524 28 14 -3 -3 102.923 210.492 25 -14 3 2 3668.58 392.364 28 14 -3 -2 3522.27 356.806 25 -14 3 1 16163.6 767.669 28 14 -3 -1 15819.9 699.413 25 -14 3 0 27853.9 972.630 28 14 -3 0 25125.8 855.735 25 -14 3 -1 18096.6 620.256 3 14 -3 1 18043.0 705.434 25 -14 3 -2 5173.19 294.274 3 14 -3 2 5233.36 376.740 25 -14 3 -3 1156.82 141.025 21 14 -3 3 1220.04 191.957 25 -14 3 -4-137.016 67.2701 21 14 -3 4-60.3765 111.273 25 14 -3 5 4061.42 246.117 25 -14 3 -5 4086.17 228.975 29 -14 3 -6 5500.56 225.146 26 14 -2 -14 10541.6 344.092 31 -14 2 13 11824.7 400.214 35 14 -2 -13 11233.0 370.347 25 14 -2 -12 5943.63 258.711 13 14 -2 -12 7083.55 334.973 25 14 -2 -11 3340.89 227.327 13 14 -2 -11 3359.54 259.665 25 -14 2 10 209.908 108.907 3 14 -2 -10-131.288 135.091 25 14 -2 -9 6932.65 403.771 25 -14 2 8 19041.4 754.867 38 14 -2 -8 19429.5 707.140 25 -14 2 7 17805.5 755.716 38 14 -2 -7 19206.6 717.649 25 -14 2 6 9593.67 551.215 38 14 -2 -6 9074.38 515.654 25 -14 2 5 755.596 191.139 38 -14 2 5 1154.89 229.295 28 14 -2 -5 1268.34 244.449 25 -14 2 4 809.420 182.920 38 -14 2 4 1035.90 219.851 28 14 -2 -4 1154.09 236.918 25 -14 2 3 6113.73 473.965 28 14 -2 -3 5571.74 414.126 25 -14 2 2 11507.4 639.320 28 14 -2 -2 11382.2 577.886 25 -14 2 1 20428.2 844.292 28 14 -2 -1 20698.6 763.561 25 -14 2 0 16155.9 719.916 28 14 -2 0 15383.4 636.152 25 -14 2 -1 1635.60 183.014 3 14 -2 1 1789.01 236.707 25 14 -2 2 1080.89 188.376 25 14 -2 3 421.418 138.172 25 14 -2 4 4248.92 257.472 25 -14 2 -4 4563.13 249.831 29 14 -1 -13 2852.44 181.277 31 -14 1 13 3503.43 209.135 35 14 -1 -12 470.014 90.2606 13 14 -1 -12 535.702 104.084 25 14 -1 -11 1609.65 168.560 13 14 -1 -11 1636.27 173.988 25 -14 1 10 8739.83 383.468 3 14 -1 -10 8864.26 409.560 25 -14 1 9 12539.2 580.822 38 14 -1 -9 11695.5 497.250 25 -14 1 8 17869.4 708.186 38 14 -1 -8 17149.0 633.783 25 -14 1 7 4257.78 369.463 38 14 -1 -7 4280.74 339.851 25 -14 1 6 150.660 160.866 38 14 -1 -6 79.0101 149.890 25 -14 1 5 540.295 168.321 38 -14 1 5 689.698 165.129 28 14 -1 -5 796.709 200.305 25 -14 1 4 5124.42 361.895 38 -14 1 4 4984.50 422.843 28 14 -1 -4 6015.19 401.540 25 -14 1 3 13001.2 657.536 28 14 -1 -3 13369.9 600.972 25 -14 1 2 24612.8 892.797 28 14 -1 -2 24669.6 791.975 25 -14 1 1 10269.1 563.659 28 14 -1 -1 10583.1 507.900 25 -14 1 0 3923.39 349.110 28 14 -1 0 4516.70 333.705 25 -14 1 -1-113.065 76.6002 3 14 -1 1-95.4434 131.065 25 14 -1 2 3161.32 244.457 25 14 -1 3 11442.0 411.259 25 -14 0 13 218.420 71.8779 35 14 0 -12 2520.58 172.957 13 14 0 -11 7367.47 324.169 13 14 0 -11 6186.94 269.227 25 14 0 -10 11947.2 425.063 25 -14 0 9 8226.37 454.735 38 14 0 -9 7913.71 372.726 25 -14 0 8 2398.48 266.313 38 14 0 -8 2582.29 238.259 25 -14 0 7 778.427 182.190 38 14 0 -7 827.606 152.068 25 -14 0 6 1611.00 232.187 38 -14 0 6 1603.58 215.054 28 14 0 -6 1720.45 220.146 25 -14 0 5 7028.22 423.128 38 -14 0 5 6533.02 425.985 28 14 0 -5 6861.39 401.425 25 -14 0 4 14813.9 562.359 38 -14 0 4 15664.1 676.068 28 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163.536 3 -16 5 8 3605.79 201.642 35 16 -5 -8 3741.28 216.087 25 -16 5 7 87.0851 68.0559 3 -16 5 7 67.7921 75.1522 35 16 -5 -7 214.993 94.4062 25 -16 5 6 1726.87 160.691 3 -16 5 6 1485.31 140.330 35 16 -5 -6 1644.74 173.045 25 -16 5 5 6132.59 289.288 3 16 -5 -5 5286.73 283.790 25 -16 5 4 9715.36 373.175 3 16 -5 -4 9327.41 382.647 25 -16 5 3 9734.39 364.852 3 16 -5 -3 9518.38 378.779 25 -16 5 2 9416.60 348.799 3 -16 5 2 8283.08 320.805 29 -16 5 2 8760.73 322.759 21 16 -5 -2 8920.58 363.434 25 -16 5 1 2535.91 173.187 3 -16 5 1 2422.11 176.395 29 -16 5 1 2716.66 176.676 21 16 -5 -1 2672.07 193.014 25 -16 5 0-13.0645 64.0361 21 16 -5 0-111.105 73.0209 25 -16 5 0 38.7707 69.8853 29 -16 5 -1 1358.49 126.612 29 -16 5 -1 1263.86 108.313 21 -16 4 9 1392.24 120.078 35 16 -4 -9 1291.81 117.415 25 -16 4 8-16.7129 66.9264 35 16 -4 -8 32.7074 67.0197 25 -16 4 7 1726.12 142.641 3 -16 4 7 1594.87 134.873 35 16 -4 -7 1825.63 161.731 25 -16 4 6 6601.44 279.958 3 16 -4 -6 5890.85 285.536 25 -16 4 5 14832.5 437.636 3 16 -4 -5 14230.8 453.266 25 -16 4 4 14066.3 424.186 3 16 -4 -4 12753.0 430.846 25 -16 4 3 8034.16 313.929 3 16 -4 -3 7974.65 332.009 25 -16 4 2 679.858 103.162 3 -16 4 2 541.955 91.9645 21 16 -4 -2 644.738 116.972 25 -16 4 2 619.899 97.6110 29 -16 4 1 356.086 76.9830 21 16 -4 -1 259.996 79.2486 25 -16 4 1 199.095 74.9766 29 -16 3 7 11242.0 329.599 3 16 -3 -7 11059.1 348.594 25 -16 3 6 12750.1 371.026 3 16 -3 -6 12414.4 383.972 25 -16 3 5 11861.3 363.808 3 16 -3 -5 11218.0 372.500 25 -16 3 4 1826.29 146.700 3 16 -3 -4 1868.14 158.624 25 -16 3 3 212.586 69.0541 3 16 -3 -3 77.2597 66.5461 25 16 -3 -2 2360.79 160.571 25 0 0 0 0.00 0.00 0 TITL mk-65-pyma in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 13.363927 14.769151 17.105492 103.7856 98.6207 115.1875 ZERR 1.00 0.000301 0.000305 0.000376 0.0018 0.0018 0.0021 LATT 1 SFAC C H B N Si U UNIT 120.00 138.00 2.00 16.00 4.00 2.00 TREF HKLF 4 END ; _shelx_hkl_checksum 38944 _shelx_fab_file ; -16 3 2 0.0992 -0.9613 -16 3 3 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12 1 1 0.0861 0.3901 12 1 2 0.2227 0.6314 12 1 3 0.0342 0.4435 12 1 4 -0.1677 -0.2072 12 1 5 -0.0722 -0.7619 12 1 6 0.2295 -0.9024 12 2 0 0.3690 0.3133 12 2 1 0.2640 0.2565 12 2 2 0.1541 -0.1624 12 2 3 0.2651 -0.4742 12 2 4 0.4797 -0.0354 12 2 5 0.5109 0.8008 12 3 0 0.1436 0.8172 12 3 1 -0.0493 0.4912 12 3 2 -0.1566 0.3169 12 3 3 -0.2227 0.5392 12 4 0 -0.3391 0.4404 12 4 1 -0.3288 0.3531 13 -16 0 0.3945 0.4517 13 -16 1 0.3602 0.1606 13 -16 2 0.2276 -0.2506 13 -16 3 0.0523 -0.5863 13 -16 4 -0.0225 -0.3935 13 -16 5 0.0005 0.2520 13 -16 6 -0.0109 0.7841 13 -15 0 -0.5182 -0.9960 13 -15 1 -0.5973 -0.9712 13 -15 2 -0.4158 -0.6025 13 -15 3 -0.0858 -0.0190 13 -15 4 0.0566 0.2785 13 -15 5 -0.0816 0.0793 13 -15 6 -0.2033 -0.2312 13 -15 7 -0.1355 -0.3233 13 -15 8 -0.0486 -0.3474 13 -14 0 0.0734 -1.1134 13 -14 1 0.3736 -0.9643 13 -14 2 0.5480 -0.4775 13 -14 3 0.3067 -0.0183 13 -14 4 -0.1152 0.2880 13 -14 5 -0.2315 0.5039 13 -14 6 -0.0216 0.5248 13 -14 7 0.1792 0.2868 13 -14 8 0.2589 0.1181 13 -14 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14 -2 1 0.1128 -0.5693 14 -2 2 0.0702 -0.0564 14 -2 3 0.0324 0.4044 14 -2 4 0.1002 0.2514 14 -1 0 0.1820 -0.6406 14 -1 1 0.1781 -0.6600 14 -1 2 0.1773 -0.6654 14 -1 3 0.2783 -0.6159 14 0 0 0.0133 -0.3655 14 0 1 -0.0543 0.3257 14 0 2 0.0311 0.7876 14 1 0 -0.2875 0.9661 15 -14 0 0.0464 -1.5236 15 -14 1 0.0299 -1.1961 15 -14 2 0.0154 -0.3926 15 -14 3 -0.0781 0.4282 15 -13 0 -0.3865 -1.2055 15 -13 1 -0.3322 -0.7370 15 -13 2 -0.2090 -0.2809 15 -13 3 -0.0380 0.0425 15 -13 4 0.0130 0.3009 15 -13 5 -0.1864 0.4140 15 -12 0 0.3442 0.3285 15 -12 1 0.2530 0.4799 15 -12 2 0.0485 0.4724 15 -12 3 -0.1686 0.3779 15 -12 4 -0.2949 0.0973 15 -12 5 -0.1739 -0.2624 15 -12 6 0.0992 -0.4869 15 -11 0 0.1786 0.6667 15 -11 1 0.2712 0.8340 15 -11 2 0.1688 0.7335 15 -11 3 0.0046 0.2914 15 -11 4 -0.0036 -0.2239 15 -11 5 0.0531 -0.5906 15 -11 6 -0.0284 -0.7482 15 -10 0 -0.1695 1.0561 15 -10 1 -0.5452 0.9756 15 -10 2 -0.4275 0.5717 15 -10 3 -0.0633 0.1418 15 -10 4 0.0814 -0.2233 15 -10 5 -0.0495 -0.4544 15 -10 6 -0.1522 -0.4223 15 -9 0 -0.3253 0.5023 15 -9 1 0.1584 0.3294 15 -9 2 0.3272 0.1223 15 -9 3 0.1770 -0.1249 15 -9 4 0.0540 -0.2134 15 -9 5 0.0961 -0.0658 15 -9 6 0.1147 0.1058 15 -8 0 0.1089 -0.0824 15 -8 1 -0.1332 -0.4357 15 -8 2 -0.3122 -0.5400 15 -8 3 -0.1768 -0.3258 15 -8 4 0.0536 -0.0000 15 -8 5 0.0923 0.2963 15 -8 6 0.0152 0.5814 15 -7 0 0.2015 -0.4249 15 -7 1 0.4656 -0.6381 15 -7 2 0.6955 -0.7003 15 -7 3 0.4903 -0.5342 15 -7 4 -0.0060 -0.0371 15 -7 5 -0.2777 0.5517 15 -6 0 0.1597 -0.8517 15 -6 1 -0.1299 -0.5872 15 -6 2 -0.5767 -0.1042 15 -6 3 -0.7116 0.3758 15 -6 4 -0.3502 0.4189 15 -6 5 0.1399 -0.0601 15 -5 0 -0.4361 -0.8585 15 -5 1 -0.4416 -0.7763 15 -5 2 -0.0720 -0.4876 15 -5 3 0.4086 -0.2605 15 -5 4 0.5774 -0.0588 15 -4 0 0.4672 0.4391 15 -4 1 0.6610 0.6290 15 -4 2 0.6017 0.4266 15 -4 3 0.2741 0.2101 15 -4 4 -0.0803 0.1707 15 -3 0 -0.1755 -0.4067 15 -3 1 -0.1979 -0.0401 15 -3 2 -0.1934 0.3253 15 -3 3 -0.1077 0.2473 15 -2 0 0.1162 0.4836 15 -2 1 0.0264 0.2211 15 -1 0 -0.2070 1.1300 16 -12 0 -0.1391 0.0130 16 -12 1 -0.0531 -0.0885 16 -11 0 -0.2072 -0.4293 16 -11 1 -0.1983 -0.6022 16 -11 2 -0.0384 -0.4809 16 -11 3 0.0680 -0.1205 16 -10 0 0.2879 -1.0684 16 -10 1 0.4486 -0.8964 16 -10 2 0.2896 -0.5578 16 -10 3 0.1246 -0.1808 16 -9 0 -0.0949 -0.8858 16 -9 1 -0.3246 -0.7059 16 -9 2 -0.2266 -0.3712 16 -9 3 -0.0424 0.0077 16 -8 0 0.4057 -0.3279 16 -8 1 0.5817 -0.0260 16 -8 2 0.4168 0.1675 16 -8 3 0.0050 0.1969 16 -7 0 -0.2564 0.2720 16 -7 1 -0.5249 0.5252 16 -7 2 -0.5331 0.6007 16 -7 3 -0.0992 0.3813 16 -6 0 -0.2676 0.6735 16 -6 1 -0.0285 0.3699 16 -6 2 0.3014 -0.1073 16 -5 0 0.2634 1.1593 16 -5 1 0.2761 0.9159 0 0 0 0.0 0.0 ; _shelx_fab_checksum 66169 _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 1.571 _oxdiff_exptl_absorpt_empirical_full_min 0.753 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 0.47880(2) 0.88683(2) 0.42135(2) 0.03610(5) Uani 1 1 d . . . . . Si1 Si 0.75446(10) 0.90649(9) 0.47086(7) 0.0516(2) Uani 1 1 d . . . . . Si2 Si 0.55775(10) 0.68590(9) 0.37474(8) 0.0546(2) Uani 1 1 d . . . . . N1 N 0.4455(3) 1.0188(2) 0.44250(18) 0.0439(6) Uani 1 1 d . . . . . H1 H 0.408542 1.033095 0.404245 0.053 Uiso 1 1 calc R U . . . N2 N 0.6074(3) 0.8211(3) 0.4215(2) 0.0494(7) Uani 1 1 d . . . . . N3 N 0.3083(3) 0.7616(2) 0.46517(19) 0.0440(6) Uani 1 1 d . . . . . N4 N 0.3044(3) 0.7999(3) 0.28023(19) 0.0474(7) Uani 1 1 d . . . . . N5 N 0.5613(3) 0.9515(3) 0.30273(19) 0.0457(6) Uani 1 1 d . . . . . C1 C 0.7921(4) 1.0457(3) 0.4765(3) 0.0558(9) Uani 1 1 d . . . . . H1A H 0.789215 1.051048 0.420270 0.084 Uiso 1 1 calc R U . . . H1B H 0.870100 1.094658 0.514261 0.084 Uiso 1 1 calc R U . . . H1C H 0.736828 1.064181 0.497868 0.084 Uiso 1 1 calc R U . . . C2 C 0.8499(4) 0.8722(4) 0.4131(4) 0.0743(14) Uani 1 1 d . . . . . H2A H 0.839145 0.802081 0.412568 0.111 Uiso 1 1 calc R U . . . H2B H 0.930781 0.925642 0.441376 0.111 Uiso 1 1 calc R U . . . H2C H 0.829492 0.870888 0.355203 0.111 Uiso 1 1 calc R U . . . C3 C 0.7995(4) 0.9103(4) 0.5801(3) 0.0641(11) Uani 1 1 d . . . . . H3A H 0.743191 0.915143 0.609174 0.096 Uiso 1 1 calc R U . . . H3B H 0.875542 0.972286 0.609746 0.096 Uiso 1 1 calc R U . . . H3C H 0.803646 0.845327 0.579129 0.096 Uiso 1 1 calc R U . . . C4 C 0.6219(5) 0.6263(4) 0.4379(4) 0.0828(17) Uani 1 1 d . . . . . H4A H 0.703644 0.653645 0.440362 0.124 Uiso 1 1 calc R U . . . H4B H 0.580985 0.548819 0.411598 0.124 Uiso 1 1 calc R U . . . H4C H 0.614817 0.645355 0.495001 0.124 Uiso 1 1 calc R U . . . C5 C 0.3991(4) 0.6109(3) 0.3624(3) 0.0615(11) Uani 1 1 d . . . . . H5A H 0.386964 0.610006 0.417367 0.092 Uiso 1 1 calc R U . . . H5B H 0.367362 0.537793 0.324466 0.092 Uiso 1 1 calc R U . . . H5C H 0.360152 0.645716 0.338922 0.092 Uiso 1 1 calc R U . . . C6 C 0.5783(5) 0.6490(4) 0.2674(3) 0.0725(14) Uani 1 1 d . . . . . H6A H 0.538810 0.672483 0.230372 0.109 Uiso 1 1 calc R U . . . H6B H 0.545913 0.571657 0.244058 0.109 Uiso 1 1 calc R U . . . H6C H 0.660840 0.683498 0.271809 0.109 Uiso 1 1 calc R U . . . C7 C 0.3394(4) 0.7546(3) 0.5405(3) 0.0551(9) Uani 1 1 d . . . . . H7 H 0.419302 0.789553 0.569386 0.066 Uiso 1 1 calc R U . . . C8 C 0.2617(4) 0.6995(4) 0.5787(3) 0.0631(11) Uani 1 1 d . . . . . H8 H 0.288094 0.696338 0.632282 0.076 Uiso 1 1 calc R U . . . C9 C 0.1446(4) 0.6487(4) 0.5379(3) 0.0587(10) Uani 1 1 d . . . . . H9 H 0.088887 0.612823 0.563602 0.070 Uiso 1 1 calc R U . . . C10 C 0.1115(4) 0.6519(3) 0.4585(3) 0.0529(9) Uani 1 1 d . . . . . H10 H 0.032188 0.615919 0.427693 0.063 Uiso 1 1 calc R U . . . C11 C 0.1943(3) 0.7076(3) 0.4247(2) 0.0478(8) Uani 1 1 d . . . . . H11 H 0.170160 0.708213 0.369801 0.057 Uiso 1 1 calc R U . . . C12 C 0.3053(4) 0.7398(3) 0.2088(3) 0.0550(9) Uani 1 1 d . . . . . H12 H 0.350118 0.704426 0.211386 0.066 Uiso 1 1 calc R U . . . C13 C 0.2433(5) 0.7273(4) 0.1309(3) 0.0675(12) Uani 1 1 d . . . . . H13 H 0.246478 0.684532 0.081152 0.081 Uiso 1 1 calc R U . . . C14 C 0.1780(5) 0.7763(4) 0.1260(3) 0.0657(12) Uani 1 1 d . . . . . H14 H 0.135271 0.768724 0.073050 0.079 Uiso 1 1 calc R U . . . C15 C 0.1747(4) 0.8367(4) 0.1987(3) 0.0626(11) Uani 1 1 d . . . . . H15 H 0.129825 0.872099 0.197396 0.075 Uiso 1 1 calc R U . . . C16 C 0.2380(4) 0.8451(4) 0.2741(3) 0.0573(9) Uani 1 1 d . . . . . H16 H 0.233773 0.885571 0.324493 0.069 Uiso 1 1 calc R U . . . C17 C 0.5447(4) 1.0250(4) 0.2792(3) 0.0575(10) Uani 1 1 d . . . . . H17 H 0.503602 1.054311 0.307252 0.069 Uiso 1 1 calc R U . . . C18 C 0.5838(5) 1.0612(4) 0.2165(3) 0.0624(11) Uani 1 1 d . . . . . H18 H 0.569014 1.113339 0.201817 0.075 Uiso 1 1 calc R U . . . C19 C 0.6437(4) 1.0210(5) 0.1764(3) 0.0677(12) Uani 1 1 d . . . . . H19 H 0.672714 1.045517 0.133819 0.081 Uiso 1 1 calc R U . . . C20 C 0.6612(6) 0.9464(7) 0.1975(5) 0.095(2) Uani 1 1 d . . . . . H20 H 0.700595 0.915366 0.168775 0.114 Uiso 1 1 calc R U . . . C21 C 0.6208(6) 0.9142(5) 0.2627(4) 0.0773(15) Uani 1 1 d . . . . . H21 H 0.636800 0.863432 0.278894 0.093 Uiso 1 1 calc R U . . . N6 N 0.5575(6) 0.7957(5) 0.7027(4) 0.108(2) Uani 1 1 d . . . . . C22 C 0.5662(8) 0.7138(7) 0.6619(6) 0.110(2) Uani 1 1 d . . . . . H22 H 0.501824 0.660855 0.615870 0.131 Uiso 1 1 calc R U . . . C23 C 0.6580(8) 0.6968(7) 0.6787(7) 0.117(3) Uani 1 1 d . . . . . H23 H 0.657834 0.634303 0.647261 0.141 Uiso 1 1 calc R U . . . C24 C 0.7517(8) 0.7763(7) 0.7445(7) 0.114(2) Uani 1 1 d . . . . . H24 H 0.818198 0.768531 0.759775 0.137 Uiso 1 1 calc R U . . . C25 C 0.7500(9) 0.8626(9) 0.7862(6) 0.118(3) Uani 1 1 d . . . . . H25 H 0.814640 0.917002 0.831467 0.142 Uiso 1 1 calc R U . . . C26 C 0.6527(7) 0.8731(7) 0.7632(5) 0.100(2) Uani 1 1 d . . . . . H26 H 0.653322 0.937228 0.791271 0.120 Uiso 1 1 calc R U . . . N7 N 0.9469(7) 0.9151(6) 0.0684(5) 0.111(2) Uani 1 1 d . . . . . C27 C 0.9074(5) 0.8114(5) 0.0540(4) 0.0763(13) Uani 1 1 d . . . . . H27 H 0.901049 0.767031 0.001039 0.092 Uiso 1 1 calc R U . . . C28 C 0.8764(5) 0.7683(5) 0.1139(4) 0.0759(13) Uani 1 1 d . . . . . H28 H 0.848007 0.694169 0.102245 0.091 Uiso 1 1 calc R U . . . C29 C 0.8853(5) 0.8304(5) 0.1909(4) 0.0750(13) Uani 1 1 d . . . . . H29 H 0.864117 0.799279 0.232520 0.090 Uiso 1 1 calc R U . . . C30 C 0.9226(6) 0.9313(5) 0.2073(5) 0.0864(16) Uani 1 1 d . . . . . H30 H 0.927185 0.974028 0.260335 0.104 Uiso 1 1 calc R U . . . C31 C 0.9551(8) 0.9756(6) 0.1484(6) 0.111(2) Uani 1 1 d . . . . . H31 H 0.984435 1.050057 0.161717 0.133 Uiso 1 1 calc R U . . . C32 C 1.0656(3) 0.3957(3) 0.1405(2) 0.0422(7) Uani 1 1 d . . . . . C33 C 1.0457(4) 0.4200(3) 0.0672(2) 0.0489(8) Uani 1 1 d . . . . . H33 H 0.971479 0.410947 0.044225 0.059 Uiso 1 1 calc R U . . . C34 C 1.1300(5) 0.4566(4) 0.0267(3) 0.0614(10) Uani 1 1 d . . . . . H34 H 1.112720 0.472983 -0.022374 0.074 Uiso 1 1 calc R U . . . C35 C 1.2375(5) 0.4694(4) 0.0570(4) 0.0691(12) Uani 1 1 d . . . . . H35 H 1.295123 0.494484 0.029454 0.083 Uiso 1 1 calc R U . . . C36 C 1.2608(4) 0.4453(4) 0.1278(3) 0.0652(11) Uani 1 1 d . . . . . H36 H 1.334919 0.453042 0.149102 0.078 Uiso 1 1 calc R U . . . C37 C 1.1762(3) 0.4093(3) 0.1693(3) 0.0524(8) Uani 1 1 d . . . . . H37 H 1.194906 0.393776 0.218521 0.063 Uiso 1 1 calc R U . . . C38 C 1.0027(3) 0.3232(3) 0.2670(2) 0.0398(7) Uani 1 1 d . . . . . C39 C 1.0927(3) 0.4050(3) 0.3370(2) 0.0469(8) Uani 1 1 d . . . . . H39 H 1.130497 0.474506 0.333955 0.056 Uiso 1 1 calc R U . . . C40 C 1.1284(4) 0.3884(4) 0.4102(3) 0.0543(9) Uani 1 1 d . . . . . H40 H 1.189960 0.445661 0.455806 0.065 Uiso 1 1 calc R U . . . C41 C 1.0742(4) 0.2878(4) 0.4167(3) 0.0566(9) Uani 1 1 d . . . . . H41 H 1.097699 0.275708 0.466685 0.068 Uiso 1 1 calc R U . . . C42 C 0.9862(4) 0.2064(3) 0.3498(3) 0.0563(9) Uani 1 1 d . . . . . H42 H 0.948416 0.137282 0.353522 0.068 Uiso 1 1 calc R U . . . C43 C 0.9515(4) 0.2237(3) 0.2763(2) 0.0471(8) Uani 1 1 d . . . . . H43 H 0.890736 0.165418 0.230765 0.056 Uiso 1 1 calc R U . . . C44 C 0.8542(3) 0.2445(3) 0.1104(2) 0.0445(7) Uani 1 1 d . . . . . C45 C 0.8723(4) 0.1594(3) 0.0716(2) 0.0483(8) Uani 1 1 d . . . . . H45 H 0.946096 0.164915 0.089320 0.058 Uiso 1 1 calc R U . . . C46 C 0.7861(4) 0.0678(3) 0.0084(3) 0.0589(10) Uani 1 1 d . . . . . H46 H 0.801370 0.011866 -0.015899 0.071 Uiso 1 1 calc R U . . . C47 C 0.6786(4) 0.0579(4) -0.0192(3) 0.0672(12) Uani 1 1 d . . . . . H47 H 0.619278 -0.005115 -0.061893 0.081 Uiso 1 1 calc R U . . . C48 C 0.6575(4) 0.1393(4) 0.0153(3) 0.0675(12) Uani 1 1 d . . . . . H48 H 0.583933 0.133490 -0.004278 0.081 Uiso 1 1 calc R U . . . C49 C 0.7440(4) 0.2310(4) 0.0793(3) 0.0559(9) Uani 1 1 d . . . . . H49 H 0.727377 0.286317 0.102661 0.067 Uiso 1 1 calc R U . . . C50 C 0.9222(3) 0.4412(3) 0.2195(2) 0.0402(7) Uani 1 1 d . . . . . C51 C 0.8379(4) 0.4183(3) 0.2629(3) 0.0510(8) Uani 1 1 d . . . . . H51 H 0.803102 0.350111 0.268629 0.061 Uiso 1 1 calc R U . . . C52 C 0.8036(4) 0.4913(4) 0.2978(3) 0.0594(10) Uani 1 1 d . . . . . H52 H 0.746432 0.472576 0.326613 0.071 Uiso 1 1 calc R U . . . C53 C 0.8526(4) 0.5913(4) 0.2906(3) 0.0605(10) Uani 1 1 d . . . . . H53 H 0.828693 0.641280 0.313474 0.073 Uiso 1 1 calc R U . . . C54 C 0.9370(4) 0.6171(3) 0.2496(3) 0.0553(9) Uani 1 1 d . . . . . H54 H 0.972093 0.686014 0.245075 0.066 Uiso 1 1 calc R U . . . C55 C 0.9712(3) 0.5440(3) 0.2148(2) 0.0461(7) Uani 1 1 d . . . . . H55 H 1.029598 0.564136 0.187105 0.055 Uiso 1 1 calc R U . . . B1 B 0.9615(3) 0.3508(3) 0.1840(2) 0.0400(7) 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 0.03714(7) 0.03821(7) 0.03203(6) 0.01125(4) 0.01020(4) 0.01753(5) Si1 0.0472(5) 0.0485(5) 0.0541(6) 0.0107(4) 0.0121(4) 0.0229(4) Si2 0.0513(6) 0.0459(5) 0.0594(6) 0.0096(5) 0.0091(5) 0.0235(5) N1 0.0566(18) 0.0459(15) 0.0351(14) 0.0120(12) 0.0122(12) 0.0309(14) N2 0.0493(17) 0.0500(17) 0.0511(17) 0.0156(14) 0.0142(14) 0.0265(14) N3 0.0470(15) 0.0441(15) 0.0404(15) 0.0134(12) 0.0145(12) 0.0213(13) N4 0.0475(16) 0.0493(16) 0.0375(14) 0.0141(12) 0.0093(12) 0.0177(13) N5 0.0444(15) 0.0528(17) 0.0396(15) 0.0150(13) 0.0144(12) 0.0226(14) C1 0.056(2) 0.045(2) 0.064(2) 0.0154(18) 0.0219(19) 0.0226(18) C2 0.054(2) 0.071(3) 0.082(3) 0.002(3) 0.021(2) 0.029(2) C3 0.063(3) 0.071(3) 0.053(2) 0.015(2) 0.004(2) 0.035(2) C4 0.075(3) 0.057(3) 0.105(4) 0.028(3) -0.002(3) 0.031(3) C5 0.043(2) 0.047(2) 0.078(3) 0.007(2) 0.0139(19) 0.0152(17) C6 0.066(3) 0.074(3) 0.064(3) -0.004(2) 0.015(2) 0.036(3) C7 0.051(2) 0.054(2) 0.049(2) 0.0214(18) 0.0104(17) 0.0151(18) C8 0.061(2) 0.063(3) 0.052(2) 0.027(2) 0.0150(19) 0.016(2) C9 0.058(2) 0.052(2) 0.059(2) 0.0222(19) 0.0270(19) 0.0165(19) C10 0.0438(19) 0.0440(19) 0.060(2) 0.0154(17) 0.0142(17) 0.0133(16) C11 0.0505(19) 0.0429(18) 0.0450(19) 0.0136(15) 0.0125(15) 0.0192(15) C12 0.063(2) 0.048(2) 0.0443(19) 0.0118(16) 0.0102(17) 0.0217(18) C13 0.093(3) 0.052(2) 0.0368(19) 0.0088(17) 0.007(2) 0.024(2) C14 0.073(3) 0.056(2) 0.042(2) 0.0181(18) -0.0072(19) 0.014(2) C15 0.059(2) 0.061(2) 0.057(2) 0.024(2) 0.0006(19) 0.023(2) C16 0.055(2) 0.068(3) 0.046(2) 0.0180(19) 0.0111(17) 0.028(2) C17 0.069(3) 0.064(2) 0.051(2) 0.0258(19) 0.027(2) 0.036(2) C18 0.072(3) 0.067(3) 0.049(2) 0.028(2) 0.021(2) 0.029(2) C19 0.058(2) 0.085(3) 0.060(3) 0.036(2) 0.029(2) 0.024(2) C20 0.110(5) 0.140(6) 0.103(5) 0.069(4) 0.079(4) 0.089(5) C21 0.095(4) 0.105(4) 0.082(3) 0.052(3) 0.053(3) 0.073(4) N6 0.113(5) 0.103(4) 0.102(4) 0.009(3) 0.000(3) 0.070(4) C22 0.116(6) 0.096(5) 0.139(7) 0.044(4) 0.035(5) 0.068(5) C23 0.124(6) 0.091(5) 0.171(8) 0.058(5) 0.053(5) 0.069(4) C24 0.107(5) 0.110(5) 0.154(7) 0.069(5) 0.038(5) 0.065(5) C25 0.118(6) 0.152(7) 0.115(6) 0.055(5) 0.031(5) 0.087(6) C26 0.108(5) 0.111(5) 0.093(5) 0.033(4) 0.031(4) 0.064(4) N7 0.128(5) 0.107(4) 0.143(5) 0.065(4) 0.073(5) 0.072(4) C27 0.082(4) 0.079(3) 0.069(3) 0.025(3) 0.026(3) 0.039(3) C28 0.079(3) 0.067(3) 0.072(3) 0.018(2) 0.017(3) 0.031(3) C29 0.087(4) 0.083(3) 0.071(3) 0.028(3) 0.027(3) 0.053(3) C30 0.091(4) 0.083(4) 0.094(4) 0.013(3) 0.028(3) 0.058(3) C31 0.125(6) 0.073(4) 0.156(7) 0.037(4) 0.067(6) 0.060(4) C32 0.0421(17) 0.0352(15) 0.0437(17) 0.0091(13) 0.0118(14) 0.0160(13) C33 0.053(2) 0.0459(19) 0.0450(18) 0.0141(15) 0.0151(16) 0.0216(16) C34 0.078(3) 0.051(2) 0.056(2) 0.0216(19) 0.032(2) 0.026(2) C35 0.063(3) 0.060(3) 0.079(3) 0.022(2) 0.040(2) 0.019(2) C36 0.042(2) 0.068(3) 0.071(3) 0.011(2) 0.0189(19) 0.0193(19) C37 0.0423(18) 0.055(2) 0.054(2) 0.0125(17) 0.0124(16) 0.0212(17) C38 0.0419(16) 0.0381(16) 0.0380(16) 0.0106(13) 0.0100(13) 0.0195(14) C39 0.0474(19) 0.0407(17) 0.0445(18) 0.0097(15) 0.0045(15) 0.0192(15) C40 0.055(2) 0.058(2) 0.0449(19) 0.0115(17) 0.0040(16) 0.0283(18) C41 0.068(3) 0.068(2) 0.046(2) 0.0242(18) 0.0141(18) 0.041(2) C42 0.073(3) 0.049(2) 0.053(2) 0.0229(17) 0.0224(19) 0.031(2) C43 0.052(2) 0.0397(17) 0.0426(18) 0.0124(14) 0.0125(15) 0.0165(15) C44 0.0428(17) 0.0462(18) 0.0360(16) 0.0142(14) 0.0109(13) 0.0139(15) C45 0.0487(19) 0.0468(19) 0.0386(17) 0.0118(15) 0.0129(15) 0.0148(16) C46 0.064(2) 0.047(2) 0.0410(19) 0.0051(16) 0.0157(17) 0.0103(18) C47 0.054(2) 0.063(3) 0.040(2) 0.0040(18) 0.0048(17) -0.0002(19) C48 0.041(2) 0.080(3) 0.052(2) 0.016(2) 0.0016(17) 0.010(2) C49 0.048(2) 0.063(2) 0.046(2) 0.0153(18) 0.0079(16) 0.0204(18) C50 0.0397(16) 0.0426(16) 0.0366(16) 0.0139(13) 0.0081(13) 0.0189(14) C51 0.052(2) 0.056(2) 0.054(2) 0.0233(18) 0.0209(17) 0.0283(18) C52 0.058(2) 0.072(3) 0.061(2) 0.023(2) 0.026(2) 0.039(2) C53 0.067(3) 0.063(2) 0.064(3) 0.018(2) 0.021(2) 0.043(2) C54 0.061(2) 0.049(2) 0.059(2) 0.0193(18) 0.0136(18) 0.0297(19) C55 0.0483(19) 0.0499(19) 0.0446(18) 0.0184(15) 0.0138(15) 0.0259(16) B1 0.0394(18) 0.0408(18) 0.0381(18) 0.0129(14) 0.0099(14) 0.0183(15) 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' 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 1 2 -1 0.1724 1 -1 2 0.0315 1 1 0 0.1660 -1 -1 2 0.1461 -1 0 1 0.1140 0 -1 2 0.0944 0 1 -2 0.1115 2 -2 -1 0.0347 0 0 -1 0.0466 0 0 1 0.0571 -3 3 -5 0.0455 -5 -2 -2 0.1454 0 1 -1 0.1373 5 -3 -3 0.0625 -3 5 -4 0.0835 -1 1 0 0.0509 -5 4 1 0.0508 -3 2 5 0.0473 3 -2 -5 0.0557 -2 5 0 0.0974 -5 2 9 0.0493 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 N1 U1 U1 37.02(8) . 2_676 ? N1 U1 U1 35.44(8) 2_676 2_676 ? N1 U1 N1 72.47(13) . 2_676 ? N1 U1 N2 150.08(13) . . ? N1 U1 N2 93.05(12) 2_676 . ? N1 U1 N3 98.21(11) . . ? N1 U1 N3 85.34(11) 2_676 . ? N1 U1 N4 149.59(11) 2_676 . ? N1 U1 N4 84.52(11) . . ? N1 U1 N5 84.22(11) . . ? N1 U1 N5 124.05(11) 2_676 . ? N2 U1 U1 124.11(9) . 2_676 ? N2 U1 N3 106.74(11) . . ? N2 U1 N4 116.11(12) . . ? N2 U1 N5 82.69(11) . . ? N3 U1 U1 92.03(7) . 2_676 ? N3 U1 N4 78.42(10) . . ? N3 U1 N5 149.23(10) . . ? N4 U1 U1 119.12(8) . 2_676 ? N5 U1 U1 107.00(7) . 2_676 ? N5 U1 N4 71.26(10) . . ? N2 Si1 C1 110.39(19) . . ? N2 Si1 C2 113.3(2) . . ? N2 Si1 C3 112.9(2) . . ? C1 Si1 C2 105.6(2) . . ? C3 Si1 C1 106.9(2) . . ? C3 Si1 C2 107.2(3) . . ? N2 Si2 C4 114.8(2) . . ? N2 Si2 C5 109.46(19) . . ? N2 Si2 C6 113.9(2) . . ? C4 Si2 C5 104.0(3) . . ? C4 Si2 C6 106.9(3) . . ? C5 Si2 C6 107.1(2) . . ? U1 N1 U1 107.53(13) . 2_676 ? U1 N1 H1 126.2 2_676 . ? U1 N1 H1 126.2 . . ? Si1 N2 U1 120.13(17) . . ? Si2 N2 U1 120.04(18) . . ? Si2 N2 Si1 119.82(19) . . ? C7 N3 U1 114.1(3) . . ? C7 N3 C11 116.4(3) . . ? C11 N3 U1 129.4(2) . . ? C12 N4 U1 121.7(3) . . ? C16 N4 U1 117.4(3) . . ? C16 N4 C12 117.1(4) . . ? C17 N5 U1 120.9(3) . . ? C21 N5 U1 123.3(3) . . ? C21 N5 C17 115.7(4) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 H7 118.2 . . ? N3 C7 C8 123.6(4) . . ? C8 C7 H7 118.2 . . ? C7 C8 H8 120.5 . . ? C7 C8 C9 119.0(4) . . ? C9 C8 H8 120.5 . . ? C8 C9 H9 121.0 . . ? C10 C9 C8 117.9(4) . . ? C10 C9 H9 121.0 . . ? C9 C10 H10 120.4 . . ? C11 C10 C9 119.2(4) . . ? C11 C10 H10 120.4 . . ? N3 C11 C10 123.6(4) . . ? N3 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? N4 C12 H12 118.9 . . ? N4 C12 C13 122.2(5) . . ? C13 C12 H12 118.9 . . ? C12 C13 H13 120.2 . . ? C14 C13 C12 119.7(5) . . ? C14 C13 H13 120.2 . . ? C13 C14 H14 120.6 . . ? C13 C14 C15 118.8(4) . . ? C15 C14 H14 120.6 . . ? C14 C15 H15 120.8 . . ? C14 C15 C16 118.5(5) . . ? C16 C15 H15 120.8 . . ? N4 C16 C15 123.8(4) . . ? N4 C16 H16 118.1 . . ? C15 C16 H16 118.1 . . ? N5 C17 H17 118.0 . . ? N5 C17 C18 124.0(4) . . ? C18 C17 H17 118.0 . . ? C17 C18 H18 120.6 . . ? C19 C18 C17 118.8(5) . . ? C19 C18 H18 120.6 . . ? C18 C19 H19 120.5 . . ? C20 C19 C18 119.1(4) . . ? C20 C19 H19 120.5 . . ? C19 C20 H20 120.4 . . ? C19 C20 C21 119.2(5) . . ? C21 C20 H20 120.4 . . ? N5 C21 C20 123.1(5) . . ? N5 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? C22 N6 C26 115.6(7) . . ? N6 C22 H22 116.7 . . ? N6 C22 C23 126.5(10) . . ? C23 C22 H22 116.7 . . ? C22 C23 H23 122.2 . . ? C22 C23 C24 115.6(8) . . ? C24 C23 H23 122.2 . . ? C23 C24 H24 119.6 . . ? C25 C24 C23 120.8(9) . . ? C25 C24 H24 119.6 . . ? C24 C25 H25 120.5 . . ? C24 C25 C26 119.0(10) . . ? C26 C25 H25 120.5 . . ? N6 C26 C25 122.2(8) . . ? N6 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C27 N7 C31 116.2(6) . . ? N7 C27 H27 119.6 . . ? N7 C27 C28 120.9(6) . . ? C28 C27 H27 119.6 . . ? C27 C28 H28 119.6 . . ? C27 C28 C29 120.8(6) . . ? C29 C28 H28 119.6 . . ? C28 C29 H29 119.9 . . ? C30 C29 C28 120.2(6) . . ? C30 C29 H29 119.9 . . ? C29 C30 H30 120.2 . . ? C29 C30 C31 119.6(6) . . ? C31 C30 H30 120.2 . . ? N7 C31 H31 118.9 . . ? C30 C31 N7 122.2(7) . . ? C30 C31 H31 118.9 . . ? C33 C32 B1 120.2(3) . . ? C37 C32 C33 114.9(4) . . ? C37 C32 B1 124.9(3) . . ? C32 C33 H33 118.6 . . ? C34 C33 C32 122.9(4) . . ? C34 C33 H33 118.6 . . ? C33 C34 H34 119.8 . . ? C35 C34 C33 120.5(5) . . ? C35 C34 H34 119.8 . . ? C34 C35 H35 120.5 . . ? C34 C35 C36 118.9(4) . . ? C36 C35 H35 120.5 . . ? C35 C36 H36 119.7 . . ? C35 C36 C37 120.7(5) . . ? C37 C36 H36 119.7 . . ? C32 C37 C36 122.2(4) . . ? C32 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C39 C38 B1 119.6(3) . . ? C43 C38 C39 115.2(3) . . ? C43 C38 B1 125.1(3) . . ? C38 C39 H39 118.7 . . ? C40 C39 C38 122.7(4) . . ? C40 C39 H39 118.7 . . ? C39 C40 H40 120.0 . . ? C39 C40 C41 120.0(4) . . ? C41 C40 H40 120.0 . . ? C40 C41 H41 120.6 . . ? C42 C41 C40 118.9(4) . . ? C42 C41 H41 120.6 . . ? C41 C42 H42 119.6 . . ? C41 C42 C43 120.8(4) . . ? C43 C42 H42 119.6 . . ? C38 C43 H43 118.8 . . ? C42 C43 C38 122.5(4) . . ? C42 C43 H43 118.8 . . ? C45 C44 B1 119.3(3) . . ? C49 C44 C45 115.1(4) . . ? C49 C44 B1 125.5(4) . . ? C44 C45 H45 118.8 . . ? C46 C45 C44 122.4(4) . . ? C46 C45 H45 118.8 . . ? C45 C46 H46 119.9 . . ? C47 C46 C45 120.1(5) . . ? C47 C46 H46 119.9 . . ? C46 C47 H47 120.2 . . ? C48 C47 C46 119.6(4) . . ? C48 C47 H47 120.2 . . ? C47 C48 H48 119.9 . . ? C47 C48 C49 120.1(5) . . ? C49 C48 H48 119.9 . . ? C44 C49 H49 118.7 . . ? C48 C49 C44 122.5(5) . . ? C48 C49 H49 118.7 . . ? C51 C50 B1 119.1(3) . . ? C55 C50 C51 115.4(3) . . ? C55 C50 B1 125.3(3) . . ? C50 C51 H51 118.6 . . ? C52 C51 C50 122.7(4) . . ? C52 C51 H51 118.6 . . ? C51 C52 H52 120.0 . . ? C53 C52 C51 120.1(4) . . ? C53 C52 H52 120.0 . . ? C52 C53 H53 120.6 . . ? C54 C53 C52 118.9(4) . . ? C54 C53 H53 120.6 . . ? C53 C54 H54 119.5 . . ? C53 C54 C55 120.9(4) . . ? C55 C54 H54 119.5 . . ? C50 C55 H55 119.0 . . ? C54 C55 C50 122.0(4) . . ? C54 C55 H55 119.0 . . ? C32 B1 C38 111.8(3) . . ? C32 B1 C44 106.0(3) . . ? C32 B1 C50 111.3(3) . . ? C38 B1 C50 105.0(3) . . ? C44 B1 C38 111.6(3) . . ? C44 B1 C50 111.2(3) . . ? 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 U1 3.5184(2) 2_676 ? U1 N1 2.222(3) 2_676 ? U1 N1 2.140(3) . ? U1 N2 2.306(3) . ? U1 N3 2.600(3) . ? U1 N4 2.683(3) . ? U1 N5 2.635(3) . ? Si1 N2 1.747(4) . ? Si1 C1 1.870(4) . ? Si1 C2 1.885(5) . ? Si1 C3 1.855(5) . ? Si2 N2 1.738(4) . ? Si2 C4 1.870(5) . ? Si2 C5 1.877(4) . ? Si2 C6 1.883(5) . ? N1 H1 0.8800 . ? N3 C7 1.335(5) . ? N3 C11 1.350(5) . ? N4 C12 1.334(5) . ? N4 C16 1.324(6) . ? N5 C17 1.332(6) . ? N5 C21 1.327(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? 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 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7 0.9500 . ? C7 C8 1.381(6) . ? C8 H8 0.9500 . ? C8 C9 1.387(7) . ? C9 H9 0.9500 . ? C9 C10 1.382(7) . ? C10 H10 0.9500 . ? C10 C11 1.371(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C12 C13 1.384(6) . ? C13 H13 0.9500 . ? C13 C14 1.356(8) . ? C14 H14 0.9500 . ? C14 C15 1.365(8) . ? C15 H15 0.9500 . ? C15 C16 1.379(6) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C17 C18 1.384(6) . ? C18 H18 0.9500 . ? C18 C19 1.356(8) . ? C19 H19 0.9500 . ? C19 C20 1.336(9) . ? C20 H20 0.9500 . ? C20 C21 1.406(8) . ? C21 H21 0.9500 . ? N6 C22 1.305(10) . ? N6 C26 1.342(10) . ? C22 H22 0.9500 . ? C22 C23 1.357(12) . ? C23 H23 0.9500 . ? C23 C24 1.382(13) . ? C24 H24 0.9500 . ? C24 C25 1.316(13) . ? C25 H25 0.9500 . ? C25 C26 1.384(11) . ? C26 H26 0.9500 . ? N7 C27 1.334(9) . ? N7 C31 1.405(11) . ? C27 H27 0.9500 . ? C27 C28 1.357(8) . ? C28 H28 0.9500 . ? C28 C29 1.369(8) . ? C29 H29 0.9500 . ? C29 C30 1.294(9) . ? C30 H30 0.9500 . ? C30 C31 1.354(11) . ? C31 H31 0.9500 . ? C32 C33 1.402(5) . ? C32 C37 1.397(6) . ? C32 B1 1.639(5) . ? C33 H33 0.9500 . ? C33 C34 1.391(6) . ? C34 H34 0.9500 . ? C34 C35 1.367(8) . ? C35 H35 0.9500 . ? C35 C36 1.370(8) . ? C36 H36 0.9500 . ? C36 C37 1.404(6) . ? C37 H37 0.9500 . ? C38 C39 1.408(5) . ? C38 C43 1.394(5) . ? C38 B1 1.649(5) . ? C39 H39 0.9500 . ? C39 C40 1.387(6) . ? C40 H40 0.9500 . ? C40 C41 1.390(6) . ? C41 H41 0.9500 . ? C41 C42 1.369(7) . ? C42 H42 0.9500 . ? C42 C43 1.393(6) . ? C43 H43 0.9500 . ? C44 C45 1.409(6) . ? C44 C49 1.399(6) . ? C44 B1 1.645(5) . ? C45 H45 0.9500 . ? C45 C46 1.389(5) . ? C46 H46 0.9500 . ? C46 C47 1.375(8) . ? C47 H47 0.9500 . ? C47 C48 1.369(8) . ? C48 H48 0.9500 . ? C48 C49 1.396(6) . ? C49 H49 0.9500 . ? C50 C51 1.408(5) . ? C50 C55 1.403(5) . ? C50 B1 1.652(5) . ? C51 H51 0.9500 . ? C51 C52 1.386(6) . ? C52 H52 0.9500 . ? C52 C53 1.383(7) . ? C53 H53 0.9500 . ? C53 C54 1.381(7) . ? C54 H54 0.9500 . ? C54 C55 1.388(6) . ? C55 H55 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 N3 C7 C8 174.7(4) . . . . ? U1 N3 C11 C10 -173.4(3) . . . . ? U1 N4 C12 C13 -155.3(4) . . . . ? U1 N4 C16 C15 155.8(4) . . . . ? U1 N5 C17 C18 -178.8(4) . . . . ? U1 N5 C21 C20 177.8(6) . . . . ? N3 C7 C8 C9 -0.5(8) . . . . ? N4 C12 C13 C14 -0.7(8) . . . . ? N5 C17 C18 C19 -0.6(8) . . . . ? C1 Si1 N2 U1 -24.4(3) . . . . ? C1 Si1 N2 Si2 157.2(2) . . . . ? C2 Si1 N2 U1 -142.7(3) . . . . ? C2 Si1 N2 Si2 39.0(3) . . . . ? C3 Si1 N2 U1 95.2(2) . . . . ? C3 Si1 N2 Si2 -83.2(3) . . . . ? C4 Si2 N2 U1 -135.0(3) . . . . ? C4 Si2 N2 Si1 43.4(4) . . . . ? C5 Si2 N2 U1 -18.5(3) . . . . ? C5 Si2 N2 Si1 159.8(2) . . . . ? C6 Si2 N2 U1 101.4(3) . . . . ? C6 Si2 N2 Si1 -80.3(3) . . . . ? C7 N3 C11 C10 3.2(6) . . . . ? C7 C8 C9 C10 2.9(8) . . . . ? C8 C9 C10 C11 -2.3(7) . . . . ? C9 C10 C11 N3 -0.8(7) . . . . ? C11 N3 C7 C8 -2.5(7) . . . . ? C12 N4 C16 C15 -2.7(7) . . . . ? C12 C13 C14 C15 -0.4(8) . . . . ? C13 C14 C15 C16 -0.1(7) . . . . ? C14 C15 C16 N4 1.7(8) . . . . ? C16 N4 C12 C13 2.2(7) . . . . ? C17 N5 C21 C20 -2.1(9) . . . . ? C17 C18 C19 C20 1.2(9) . . . . ? C18 C19 C20 C21 -2.2(11) . . . . ? C19 C20 C21 N5 2.8(12) . . . . ? C21 N5 C17 C18 1.1(7) . . . . ? N6 C22 C23 C24 -1.7(16) . . . . ? C22 N6 C26 C25 -5.7(14) . . . . ? C22 C23 C24 C25 -0.9(15) . . . . ? C23 C24 C25 C26 -0.1(15) . . . . ? C24 C25 C26 N6 3.6(15) . . . . ? C26 N6 C22 C23 4.9(15) . . . . ? N7 C27 C28 C29 -0.4(10) . . . . ? C27 N7 C31 C30 -1.4(13) . . . . ? C27 C28 C29 C30 0.8(10) . . . . ? C28 C29 C30 C31 -1.4(11) . . . . ? C29 C30 C31 N7 1.8(13) . . . . ? C31 N7 C27 C28 0.7(11) . . . . ? C32 C33 C34 C35 0.9(7) . . . . ? C33 C32 C37 C36 0.4(6) . . . . ? C33 C32 B1 C38 177.7(3) . . . . ? C33 C32 B1 C44 55.9(4) . . . . ? C33 C32 B1 C50 -65.2(4) . . . . ? C33 C34 C35 C36 0.1(8) . . . . ? C34 C35 C36 C37 -0.7(8) . . . . ? C35 C36 C37 C32 0.5(7) . . . . ? C37 C32 C33 C34 -1.1(6) . . . . ? C37 C32 B1 C38 0.1(5) . . . . ? C37 C32 B1 C44 -121.7(4) . . . . ? C37 C32 B1 C50 117.2(4) . . . . ? C38 C39 C40 C41 -0.5(7) . . . . ? C39 C38 C43 C42 0.5(6) . . . . ? C39 C38 B1 C32 62.4(4) . . . . ? C39 C38 B1 C44 -179.1(3) . . . . ? C39 C38 B1 C50 -58.4(4) . . . . ? C39 C40 C41 C42 0.4(7) . . . . ? C40 C41 C42 C43 0.1(7) . . . . ? C41 C42 C43 C38 -0.6(7) . . . . ? C43 C38 C39 C40 0.1(6) . . . . ? C43 C38 B1 C32 -120.7(4) . . . . ? C43 C38 B1 C44 -2.2(5) . . . . ? C43 C38 B1 C50 118.4(4) . . . . ? C44 C45 C46 C47 0.6(6) . . . . ? C45 C44 C49 C48 0.9(6) . . . . ? C45 C44 B1 C32 57.8(4) . . . . ? C45 C44 B1 C38 -64.1(4) . . . . ? C45 C44 B1 C50 178.9(3) . . . . ? C45 C46 C47 C48 0.8(7) . . . . ? C46 C47 C48 C49 -1.3(7) . . . . ? C47 C48 C49 C44 0.5(7) . . . . ? C49 C44 C45 C46 -1.4(6) . . . . ? C49 C44 B1 C32 -119.8(4) . . . . ? C49 C44 B1 C38 118.3(4) . . . . ? C49 C44 B1 C50 1.4(5) . . . . ? C50 C51 C52 C53 0.0(7) . . . . ? C51 C50 C55 C54 -1.1(6) . . . . ? C51 C50 B1 C32 -176.6(3) . . . . ? C51 C50 B1 C38 -55.4(4) . . . . ? C51 C50 B1 C44 65.5(4) . . . . ? C51 C52 C53 C54 -1.1(7) . . . . ? C52 C53 C54 C55 1.0(7) . . . . ? C53 C54 C55 C50 0.1(7) . . . . ? C55 C50 C51 C52 1.1(6) . . . . ? C55 C50 B1 C32 -0.8(5) . . . . ? C55 C50 B1 C38 120.4(4) . . . . ? C55 C50 B1 C44 -118.8(4) . . . . ? B1 C32 C33 C34 -178.9(4) . . . . ? B1 C32 C37 C36 178.1(4) . . . . ? B1 C38 C39 C40 177.2(4) . . . . ? B1 C38 C43 C42 -176.5(4) . . . . ? B1 C44 C45 C46 -179.2(3) . . . . ? B1 C44 C49 C48 178.5(4) . . . . ? B1 C50 C51 C52 177.2(4) . . . . ? B1 C50 C55 C54 -177.0(4) . . . . ? 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 1.0000 2.0000 -1.0000 0.2044 0.1741 0.1511 1.0000 -1.0000 2.0000 0.0948 0.0650 -0.2000 1.0000 1.0000 -0.0000 0.1679 0.1377 0.0341 -1.0000 -1.0000 2.0000 -0.0248 -0.1692 -0.1606 -1.0000 -0.0000 1.0000 0.0117 -0.1328 -0.0436 -0.0000 -1.0000 2.0000 0.0350 -0.0521 -0.1803 0.0000 1.0000 -2.0000 -0.0350 0.0521 0.1803 2.0000 -2.0000 -1.0000 -0.1681 0.2086 -0.0837 0.0000 -0.0000 -1.0000 -0.0715 0.0157 0.0633 -0.0000 0.0000 1.0000 0.0715 -0.0157 -0.0633 -3.0000 3.0000 -5.0000 -0.2128 -0.2106 0.5367 -5.0000 -2.0000 -2.0000 -0.6581 -0.5953 0.1174 -0.0000 1.0000 -1.0000 0.0365 0.0364 0.1170 5.0000 -3.0000 -3.0000 -0.2398 0.5707 -0.0699 -3.0000 5.0000 -4.0000 0.0749 -0.1851 0.5810 -1.0000 1.0000 -0.0000 0.0483 -0.0964 0.0735 -5.0000 4.0000 1.0000 0.2048 -0.5186 0.2503 -3.0000 2.0000 5.0000 0.3944 -0.3887 -0.1497 3.0000 -2.0000 -5.0000 -0.3944 0.3887 0.1497 -2.0000 5.0000 -0.0000 0.4207 -0.1309 0.3083 -5.1480 2.2064 9.3925 0.6024 -0.7050 -0.3743 loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.500 0.500 1.000 351.7 82.7 '2 py'