#------------------------------------------------------------------------------ #$Date: 2021-08-19 01:12:36 +0300 (Thu, 19 Aug 2021) $ #$Revision: 268126 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564372.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_1564372 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 'C72 H162 N4 O24 Si6 U2, 2[C4H8O]' _chemical_formula_sum 'C72 H172 N4 O24 Si6 U2' _chemical_formula_weight 2122.73 _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 2021-05-03 _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 106.7988(13) _cell_angle_beta 114.1561(17) _cell_angle_gamma 91.4673(12) _cell_formula_units_Z 1 _cell_length_a 14.2581(2) _cell_length_b 14.80263(18) _cell_length_c 15.5045(3) _cell_measurement_reflns_used 36457 _cell_measurement_temperature 140.00(10) _cell_measurement_theta_max 72.6060 _cell_measurement_theta_min 3.7170 _cell_volume 2819.33(9) _computing_cell_refinement 'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.105a (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 5.2817 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.984 _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 -78.00 4.00 1.00 1.00 -- -40.91 112.00 135.00 82 2 \w 18.00 84.00 1.00 1.00 -- 40.91-112.00 42.00 66 3 \w 108.00 142.00 1.00 4.00 -- 105.15 112.00 135.00 34 4 \w 46.00 105.00 1.00 4.00 -- 105.15-112.00 42.00 59 5 \w 1.00 29.00 1.00 1.00 -- 38.00 90.00 -89.10 28 6 \w -115.00 -16.00 1.00 1.00 -- -40.91 -38.00 150.00 99 7 \w -114.00 -16.00 1.00 1.00 -- -40.91 -38.00 -60.00 98 8 \w -112.00 -13.00 1.00 1.00 -- -40.91 -57.00 60.00 99 9 \w 9.00 34.00 1.00 1.00 -- 40.91 75.00 104.57 25 10 \w 6.00 82.00 1.00 1.00 -- 40.91 -99.00 -30.00 76 11 \w 16.00 41.00 1.00 1.00 -- 50.00 81.00 -38.42 25 12 \w 16.00 42.00 1.00 1.00 -- 50.00 81.00-154.98 26 13 \w 16.00 41.00 1.00 1.00 -- 50.00 82.00 73.24 25 14 \w 16.00 41.00 1.00 1.00 -- 50.00 82.00-117.79 25 15 \w 16.00 41.00 1.00 1.00 -- 50.00 82.00 10.24 25 16 \w 16.00 41.00 1.00 1.00 -- 50.00 82.00 -79.87 25 17 \w 16.00 41.00 1.00 1.00 -- 50.00 82.00 126.29 25 18 \w 31.00 57.00 1.00 1.00 -- 62.00 69.00 6.81 26 19 \w 78.00 105.00 1.00 1.00 -- 62.00 69.00 6.81 27 20 \w 36.00 61.00 1.00 1.00 -- 66.00 71.00 162.34 25 21 \w 102.00 131.00 1.00 1.00 -- 66.00 71.00 162.34 29 22 \w 37.00 64.00 1.00 1.00 -- 66.00 70.00 -96.71 27 23 \w 111.00 142.00 1.00 1.00 -- 70.00 71.00 56.95 31 24 \w 99.00 126.00 1.00 1.00 -- 70.00 71.00 -76.46 27 25 \w 40.00 67.00 1.00 1.00 -- 70.00 71.00 56.95 27 26 \w 39.00 65.00 1.00 1.00 -- 70.00 69.00 131.48 26 27 \w 40.00 65.00 1.00 1.00 -- 70.00 71.00 -76.46 25 28 \w 85.00 143.00 1.00 1.00 -- 70.00 69.00-131.95 58 29 \w 40.00 65.00 1.00 1.00 -- 70.00 69.00-131.95 25 30 \w 43.00 71.00 1.00 4.00 -- 74.00 71.00 83.95 28 31 \w 44.00 70.00 1.00 4.00 -- 74.00 66.00 -2.65 26 32 \w 43.00 70.00 1.00 4.00 -- 74.00 69.00-176.41 27 33 \w 47.00 73.00 1.00 4.00 -- 78.00 69.00 -48.13 26 34 \w 47.00 73.00 1.00 4.00 -- 78.00 69.00 20.87 26 35 \w 53.00 80.00 1.00 4.00 -- 82.00 59.00-103.64 27 36 \w 52.00 77.00 1.00 4.00 -- 82.00 70.00 -82.57 25 37 \w 125.00 152.00 1.00 4.00 -- 82.00 68.00 55.06 27 38 \w 53.00 83.00 1.00 4.00 -- 82.00 68.00 55.06 30 39 \w 56.00 99.00 1.00 4.00 -- 86.00 68.00 176.08 43 40 \w 56.00 104.00 1.00 4.00 -- 86.00 66.00 16.84 48 41 \w 109.00 159.00 1.00 4.00 -- 86.00 66.00 16.84 50 42 \w 56.00 100.00 1.00 4.00 -- 86.00 65.00 137.89 44 43 \w 64.00 133.00 1.00 4.00 -- 94.00 66.00 140.43 69 44 \w 77.00 126.00 1.00 4.00 -- 105.15 61.00 -90.00 49 45 \w 79.00 118.00 1.00 4.00 -- 105.15 45.00 90.00 39 46 \w 76.00 174.00 1.00 4.00 -- 105.15 61.00 -60.00 98 47 \w 96.00 137.00 1.00 4.00 -- 105.15 -77.00 -30.00 41 48 \w 75.00 106.00 1.00 4.00 -- 105.15 66.00 45.76 31 49 \w 36.00 68.00 1.00 4.00 -- 105.15 -77.00 -30.00 32 50 \w 78.00 176.00 1.00 4.00 -- 105.15 61.00-180.00 98 51 \w 63.00 106.00 1.00 4.00 -- 105.15-111.00 -30.00 43 52 \w 79.00 106.00 1.00 4.00 -- 105.15 61.00 150.00 27 53 \w 82.00 109.00 1.00 4.00 -- 105.15-111.00 90.00 27 54 \w 32.00 59.00 1.00 4.00 -- 105.15-111.00 90.00 27 55 \w 104.00 162.00 1.00 4.00 -- 105.15 111.00-120.00 58 56 \w 110.00 147.00 1.00 4.00 -- 105.15 61.00-120.00 37 57 \w 77.00 107.00 1.00 4.00 -- 105.15 61.00-120.00 30 58 \w 30.00 109.00 1.00 4.00 -- 105.15-111.00-150.00 79 59 \w 121.00 169.00 1.00 4.00 -- 105.15 61.00 30.00 48 60 \w 76.00 103.00 1.00 4.00 -- 105.15 61.00 30.00 27 61 \w 140.00 172.00 1.00 4.00 -- 105.15 66.00 45.76 32 62 \w 116.00 143.00 1.00 4.00 -- 105.15 61.00 -30.00 27 63 \w 34.00 132.00 1.00 4.00 -- 105.15 -61.00-180.00 98 64 \w 80.00 174.00 1.00 4.00 -- 105.15 61.00 0.00 94 65 \w 77.00 167.00 1.00 4.00 -- 105.15 61.00 120.00 90 66 \w 76.00 106.00 1.00 4.00 -- 105.15 61.00 -30.00 30 67 \w 76.00 177.00 1.00 4.00 -- 105.15 61.00-150.00 101 68 \w 76.00 175.00 1.00 4.00 -- 105.15 61.00 90.00 99 69 \w 131.00 156.00 1.00 4.00 -- 105.15 61.00 -90.00 25 70 \w 88.00 143.00 1.00 4.00 -- 105.15 178.00-120.00 55 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0359821000 _diffrn_orient_matrix_UB_12 0.0010234000 _diffrn_orient_matrix_UB_13 -0.0808853000 _diffrn_orient_matrix_UB_21 0.0411746000 _diffrn_orient_matrix_UB_22 0.1080786000 _diffrn_orient_matrix_UB_23 0.0520634000 _diffrn_orient_matrix_UB_31 0.1068820000 _diffrn_orient_matrix_UB_32 -0.0215877000 _diffrn_orient_matrix_UB_33 0.0635509000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_unetI/netI 0.0227 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 12820 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.719 _diffrn_reflns_theta_min 3.162 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 9.094 _exptl_absorpt_correction_T_max 0.618 _exptl_absorpt_correction_T_min 0.410 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.105a (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 'clear light blue' _exptl_crystal_density_diffrn 1.250 _exptl_crystal_description irregular _exptl_crystal_F_000 1092 _exptl_crystal_size_max 0.157 _exptl_crystal_size_mid 0.134 _exptl_crystal_size_min 0.107 _refine_diff_density_max 1.643 _refine_diff_density_min -1.117 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 524 _refine_ls_number_reflns 12820 _refine_ls_number_restraints 163 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0254 _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^)+(0.0529P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.0672 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12030 _reflns_number_total 12820 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 3.5714\% around [-0.15 0.99 -0.04] (reciprocal) or [-0.01 0.97 0.23] (direct) ; _cod_data_source_file d1sc03957a2.cif _cod_data_source_block mk-207_twin1_hklf5_sq _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_cell_volume 2819.32(9) _cod_database_code 1564372 _shelx_shelxl_version_number 2018/3 _audit_contact_author 'Farzaneh Fadaei Tirani' _chemical_oxdiff_formula 'C72 H162 N4 O24 Si6 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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.5851(9) 0.4149(9) 2. Fixed Uiso At 1.2 times of: All N(H,H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances N1-H1B \\sim N1-H1A with sigma of 0.02 4. Uiso/Uaniso restraints and constraints C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A 5.a Idealised Me refined as rotating group: N2(H2A,H2B,H2C), C2(H2D,H2E,H2F), 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) ; _shelx_res_file ; TITL mk-207_twin1_hklf5.res in P-1 mk-207_twin1_hklf5_sq.res created by SHELXL-2018/3 at 18:42:32 on 03-May-2021 CELL 1.54184 14.258071 14.802626 15.50449 106.7988 114.1561 91.4673 ZERR 1 0.000246 0.000175 0.000282 0.0013 0.0017 0.0012 LATT 1 SFAC C H N O Si U UNIT 72 172 4 24 6 2 SADI N1 H1b N1 H1a SIMU 0.005 0.01 2 $C L.S. 30 0 44 PLAN 10 TEMP -133.15 CONF WPDB -2 MORE -1 BOND $H ABIN fmap 2 acta REM REM REM WGHT 0.052900 BASF 0.41495 FVAR 3.69378 U1 6 0.599079 0.590004 0.630664 11.00000 0.02395 0.01758 = 0.02166 0.00498 0.00822 0.00175 SI1 5 0.478000 0.760963 0.757082 11.00000 0.03135 0.02619 = 0.02440 0.00523 0.01161 0.00612 SI2 5 0.829722 0.758753 0.694104 11.00000 0.02643 0.02301 = 0.02775 0.00490 0.00906 -0.00138 SI3 5 0.656157 0.423506 0.777137 11.00000 0.03042 0.02178 = 0.02559 0.00820 0.00862 0.00396 O1 4 0.554264 0.690397 0.733017 11.00000 0.03603 0.02699 = 0.02681 0.00512 0.01451 0.00757 O2 4 0.373078 0.707423 0.749409 11.00000 0.03093 0.04041 = 0.03005 0.01168 0.01221 0.00530 O3 4 0.437047 0.809388 0.668129 11.00000 0.03883 0.03125 = 0.03332 0.01223 0.01726 0.01217 O4 4 0.534566 0.840677 0.867984 11.00000 0.03797 0.03321 = 0.02858 0.00079 0.01456 0.00383 O21 4 0.750293 0.666601 0.670615 11.00000 0.02280 0.02444 = 0.03409 0.00697 0.00964 -0.00115 O22 4 0.755114 0.834316 0.654213 11.00000 0.03583 0.02164 = 0.03229 0.00646 0.00955 -0.00176 O23 4 0.903750 0.811879 0.812503 11.00000 0.03180 0.03024 = 0.02824 0.00500 0.00559 0.00098 O24 4 0.907561 0.733559 0.640393 11.00000 0.03046 0.03535 = 0.03499 0.00486 0.01358 -0.00340 O41 4 0.636742 0.479994 0.698682 11.00000 0.03458 0.03267 = 0.03470 0.01733 0.01068 0.00568 O42 4 0.646072 0.483602 0.877854 11.00000 0.03310 0.03556 = 0.03078 0.00211 0.01099 0.00127 O43 4 0.771349 0.393894 0.816139 11.00000 0.03566 0.03126 = 0.03182 0.00941 0.00936 0.01011 O44 4 0.562966 0.331079 0.717613 11.00000 0.03935 0.02494 = 0.02864 0.00776 0.01067 -0.00074 N1 3 0.414592 0.515695 0.529745 11.00000 0.03145 0.02997 = 0.03099 0.00550 0.01678 0.00270 H1A 2 0.395010 0.482146 0.561299 11.00000 0.04937 H1B 2 0.367959 0.556701 0.523617 11.00000 0.07460 N2 3 0.535198 0.706931 0.528841 11.00000 0.03386 0.02615 = 0.03013 0.00958 0.01152 0.00396 AFIX 137 H2A 2 0.502032 0.672907 0.462380 11.00000 -1.20000 H2B 2 0.590883 0.748207 0.540714 11.00000 -1.20000 H2C 2 0.490387 0.740480 0.547899 11.00000 -1.20000 AFIX 0 C1 1 0.349747 0.653996 0.804575 11.00000 0.03946 0.04453 = 0.03350 0.01454 0.01889 0.00482 C2 1 0.396907 0.563121 0.793003 11.00000 0.06086 0.04324 = 0.04775 0.01862 0.02445 0.01055 AFIX 137 H2D 2 0.367275 0.524325 0.722054 11.00000 -1.50000 H2E 2 0.381336 0.526682 0.830555 11.00000 -1.50000 H2F 2 0.472588 0.579625 0.818921 11.00000 -1.50000 AFIX 0 C3 1 0.230562 0.628596 0.754559 11.00000 0.04078 0.07252 = 0.05521 0.02604 0.02130 0.00178 AFIX 137 H3A 2 0.200276 0.687488 0.760607 11.00000 -1.50000 H3B 2 0.208832 0.590529 0.787464 11.00000 -1.50000 H3C 2 0.206396 0.591534 0.683635 11.00000 -1.50000 AFIX 0 C4 1 0.389379 0.714556 0.913580 11.00000 0.06209 0.05572 = 0.03434 0.01045 0.02497 0.00454 AFIX 137 H4A 2 0.465080 0.733719 0.942863 11.00000 -1.50000 H4B 2 0.372587 0.677372 0.949910 11.00000 -1.50000 H4C 2 0.356101 0.771744 0.918467 11.00000 -1.50000 AFIX 0 C5 1 0.346847 0.852779 0.631754 11.00000 0.05321 0.06588 = 0.04056 0.02676 0.02019 0.03461 C6 1 0.254369 0.773228 0.561848 11.00000 0.04183 0.10758 = 0.06521 0.05282 0.00955 0.00812 AFIX 137 H6A 2 0.193056 0.801072 0.530042 11.00000 -1.50000 H6B 2 0.239976 0.737058 0.600192 11.00000 -1.50000 H6C 2 0.270484 0.730294 0.510266 11.00000 -1.50000 AFIX 0 C7 1 0.368688 0.910866 0.574123 11.00000 0.06467 0.04434 = 0.05276 0.02437 0.01207 0.01755 AFIX 137 H7A 2 0.309424 0.943183 0.547850 11.00000 -1.50000 H7B 2 0.379204 0.868323 0.518463 11.00000 -1.50000 H7C 2 0.431571 0.958688 0.618756 11.00000 -1.50000 AFIX 0 C8 1 0.327358 0.915149 0.718267 11.00000 0.10367 0.10438 = 0.05973 0.03031 0.03878 0.07662 AFIX 137 H8A 2 0.388627 0.964441 0.764173 11.00000 -1.50000 H8B 2 0.314394 0.875311 0.754179 11.00000 -1.50000 H8C 2 0.266542 0.945729 0.691978 11.00000 -1.50000 AFIX 0 C9 1 0.630389 0.907375 0.922169 11.00000 0.04203 0.03202 = 0.03640 0.00034 0.01510 0.00000 C10 1 0.609838 0.996116 0.890577 11.00000 0.07944 0.05232 = 0.10150 0.02182 0.02048 0.00564 AFIX 137 H10A 2 0.597613 0.980526 0.820560 11.00000 -1.50000 H10B 2 0.670390 1.046958 0.933058 11.00000 -1.50000 H10C 2 0.548303 1.017893 0.897812 11.00000 -1.50000 AFIX 0 C11 1 0.652578 0.934597 1.028690 11.00000 0.08656 0.12736 = 0.04839 -0.01416 0.02026 -0.04463 AFIX 137 H11A 2 0.594428 0.962290 1.038260 11.00000 -1.50000 H11B 2 0.716601 0.981831 1.068912 11.00000 -1.50000 H11C 2 0.661463 0.877775 1.049744 11.00000 -1.50000 AFIX 0 C12 1 0.715611 0.867333 0.899980 11.00000 0.04740 0.05256 = 0.10958 -0.00430 0.02653 -0.00017 AFIX 137 H12A 2 0.728116 0.809931 0.919689 11.00000 -1.50000 H12B 2 0.779330 0.915090 0.937483 11.00000 -1.50000 H12C 2 0.695599 0.850564 0.828130 11.00000 -1.50000 AFIX 0 C21 1 0.776312 0.932389 0.659823 11.00000 0.04838 0.02336 = 0.03937 0.01037 0.01066 -0.00139 C22 1 0.670937 0.965347 0.626425 11.00000 0.06405 0.03338 = 0.04821 0.01533 0.01978 0.01473 AFIX 137 H22A 2 0.640157 0.960888 0.671457 11.00000 -1.50000 H22B 2 0.624760 0.924571 0.558039 11.00000 -1.50000 H22C 2 0.679954 1.031833 0.628245 11.00000 -1.50000 AFIX 0 C23 1 0.848734 0.994305 0.766298 11.00000 0.07959 0.02772 = 0.04292 0.00704 0.00303 -0.00789 AFIX 137 H23A 2 0.917825 0.975344 0.785322 11.00000 -1.50000 H23B 2 0.820572 0.985840 0.811992 11.00000 -1.50000 H23C 2 0.854469 1.061623 0.770185 11.00000 -1.50000 AFIX 0 C24 1 0.823261 0.934915 0.588654 11.00000 0.05834 0.04132 = 0.06350 0.02481 0.02452 0.00171 AFIX 137 H24A 2 0.836953 1.001099 0.591262 11.00000 -1.50000 H24B 2 0.774474 0.896000 0.520390 11.00000 -1.50000 H24C 2 0.888733 0.909280 0.608263 11.00000 -1.50000 AFIX 0 C25 1 1.001661 0.795522 0.880036 11.00000 0.03529 0.03645 = 0.03406 0.00626 0.00255 0.00170 C26 1 1.008151 0.841134 0.983667 11.00000 0.06787 0.05298 = 0.03191 0.00368 0.00278 0.01359 AFIX 137 H26A 2 0.949316 0.810785 0.988360 11.00000 -1.50000 H26B 2 1.005675 0.909606 0.996012 11.00000 -1.50000 H26C 2 1.073662 0.832525 1.033679 11.00000 -1.50000 AFIX 0 C27 1 1.088038 0.845622 0.868312 11.00000 0.03392 0.05693 = 0.07191 0.01347 0.00437 -0.00841 AFIX 137 H27A 2 1.083150 0.913767 0.881399 11.00000 -1.50000 H27B 2 1.080724 0.817061 0.799983 11.00000 -1.50000 H27C 2 1.155885 0.838315 0.916003 11.00000 -1.50000 AFIX 0 C28 1 1.005882 0.689856 0.858587 11.00000 0.04943 0.04010 = 0.04358 0.00953 0.00954 0.00969 AFIX 137 H28A 2 1.004624 0.662508 0.792447 11.00000 -1.50000 H28B 2 0.945591 0.657917 0.859800 11.00000 -1.50000 H28C 2 1.070170 0.680582 0.909596 11.00000 -1.50000 AFIX 0 C29 1 0.894177 0.663266 0.548251 11.00000 0.04236 0.04156 = 0.03561 0.00679 0.01988 0.00671 C30 1 0.986082 0.691989 0.530182 11.00000 0.04398 0.07171 = 0.05255 0.01751 0.02845 0.00846 AFIX 137 H30A 2 0.983570 0.755699 0.523163 11.00000 -1.50000 H30B 2 0.982515 0.645598 0.468814 11.00000 -1.50000 H30C 2 1.051328 0.693161 0.586935 11.00000 -1.50000 AFIX 0 C31 1 0.897002 0.564590 0.560010 11.00000 0.06251 0.03796 = 0.04770 0.00683 0.02767 0.01351 AFIX 137 H31A 2 0.962600 0.565370 0.616184 11.00000 -1.50000 H31B 2 0.891913 0.517349 0.498440 11.00000 -1.50000 H31C 2 0.838311 0.547555 0.572973 11.00000 -1.50000 AFIX 0 C32 1 0.791624 0.665030 0.463235 11.00000 0.04100 0.04742 = 0.03591 0.00355 0.01378 0.00259 AFIX 137 H32A 2 0.733807 0.651910 0.478959 11.00000 -1.50000 H32B 2 0.782634 0.616123 0.401066 11.00000 -1.50000 H32C 2 0.792458 0.728190 0.454987 11.00000 -1.50000 AFIX 0 C41 1 0.721915 0.551727 0.970353 11.00000 0.03944 0.04261 = 0.03115 -0.00300 0.01032 0.00136 C42 1 0.659222 0.610619 1.017473 11.00000 0.05107 0.10575 = 0.06089 -0.03482 0.01858 0.00416 AFIX 137 H42A 2 0.615607 0.643153 0.972445 11.00000 -1.50000 H42B 2 0.706748 0.658284 1.081364 11.00000 -1.50000 H42C 2 0.614791 0.568485 1.029067 11.00000 -1.50000 AFIX 0 C43 1 0.790083 0.614915 0.950078 11.00000 0.05239 0.03623 = 0.03949 0.00632 0.00333 -0.00650 AFIX 137 H43A 2 0.832227 0.576186 0.922397 11.00000 -1.50000 H43B 2 0.836084 0.664997 1.012705 11.00000 -1.50000 H43C 2 0.746065 0.644465 0.902006 11.00000 -1.50000 AFIX 0 C44 1 0.787805 0.497478 1.037606 11.00000 0.06918 0.06723 = 0.03082 0.01634 0.00662 -0.00397 AFIX 137 H44A 2 0.742491 0.457717 1.050619 11.00000 -1.50000 H44B 2 0.838819 0.543272 1.101083 11.00000 -1.50000 H44C 2 0.824356 0.456658 1.004243 11.00000 -1.50000 AFIX 0 C45 1 0.837241 0.354020 0.770962 11.00000 0.04135 0.04146 = 0.04985 0.01115 0.02183 0.01448 C46 1 0.856996 0.416024 0.715760 11.00000 0.09533 0.05330 = 0.11682 0.02298 0.08096 0.01481 AFIX 137 H46A 2 0.899205 0.386229 0.682417 11.00000 -1.50000 H46B 2 0.894242 0.479371 0.763456 11.00000 -1.50000 H46C 2 0.790328 0.422607 0.665677 11.00000 -1.50000 AFIX 0 C47 1 0.935774 0.350005 0.856709 11.00000 0.05741 0.15895 = 0.07127 0.00992 0.01415 0.05364 AFIX 137 H47A 2 0.919819 0.308143 0.889362 11.00000 -1.50000 H47B 2 0.965836 0.414490 0.905178 11.00000 -1.50000 H47C 2 0.985812 0.324768 0.831412 11.00000 -1.50000 AFIX 0 C48 1 0.786143 0.253944 0.699476 11.00000 0.08478 0.04317 = 0.07110 -0.00201 0.04922 0.00563 AFIX 137 H48A 2 0.721442 0.256926 0.644459 11.00000 -1.50000 H48B 2 0.770352 0.215379 0.735152 11.00000 -1.50000 H48C 2 0.833532 0.224697 0.672507 11.00000 -1.50000 AFIX 0 C49 1 0.523617 0.267039 0.754569 11.00000 0.04670 0.02858 = 0.04257 0.01262 0.02053 -0.00050 C50 1 0.612781 0.236540 0.830622 11.00000 0.06441 0.04198 = 0.05014 0.02572 0.02504 0.01058 AFIX 137 H50A 2 0.656136 0.293159 0.887341 11.00000 -1.50000 H50B 2 0.655203 0.203794 0.799062 11.00000 -1.50000 H50C 2 0.584364 0.193047 0.854389 11.00000 -1.50000 AFIX 0 C51 1 0.459157 0.180828 0.662630 11.00000 0.07065 0.03223 = 0.05360 0.00681 0.02398 -0.01322 AFIX 137 H51A 2 0.430228 0.133971 0.682567 11.00000 -1.50000 H51B 2 0.503600 0.151560 0.631778 11.00000 -1.50000 H51C 2 0.402184 0.201502 0.614410 11.00000 -1.50000 AFIX 0 C52 1 0.454889 0.316070 0.801028 11.00000 0.05257 0.04140 = 0.06362 0.01586 0.03216 0.00336 AFIX 137 H52A 2 0.398738 0.336195 0.751517 11.00000 -1.50000 H52B 2 0.496872 0.372227 0.859071 11.00000 -1.50000 H52C 2 0.424818 0.271351 0.822402 11.00000 -1.50000 AFIX 0 HKLF 5 REM mk-207_twin1_hklf5.res in P-1 REM wR2 = 0.0672, GooF = S = 1.011, Restrained GooF = 1.040 for all data REM R1 = 0.0254 for 12030 Fo > 4sig(Fo) and 0.0270 for all 12820 data REM 524 parameters refined using 163 restraints END WGHT 0.0529 0.0000 REM Highest difference peak 1.643, deepest hole -1.117, 1-sigma level 0.088 Q1 1 0.6320 0.5853 0.6902 11.00000 0.05 1.64 Q2 1 0.5607 0.5964 0.5724 11.00000 0.05 1.31 Q3 1 0.6380 0.5738 0.6011 11.00000 0.05 1.14 Q4 1 0.5578 0.5990 0.6621 11.00000 0.05 1.12 Q5 1 0.6629 0.9436 0.8523 11.00000 0.05 1.00 Q6 1 0.7165 0.8469 0.9713 11.00000 0.05 0.95 Q7 1 0.6227 0.9922 0.9956 11.00000 0.05 0.81 Q8 1 0.5819 0.6603 0.6978 11.00000 0.05 0.74 Q9 1 0.7967 0.7696 0.8938 11.00000 0.05 0.65 Q10 1 0.3977 0.4779 0.4504 11.00000 0.05 0.63 ; _shelx_res_checksum 89138 _shelx_hkl_file ; 0 0 1 145761. 962.885 1 0 0 -1 254811. 2113.05 -2 0 0 -1 254811. 2113.05 1 0 0 2 207782. 1648.77 1 0 0 -2 353108. 2952.01 -2 0 0 -2 353108. 2952.01 1 0 0 -3 166753. 1833.50 1 0 0 4 71148.6 1363.01 1 0 0 5 26527.3 672.372 1 0 0 6 10685.5 524.325 1 0 0 7 95236.7 1168.46 1 0 0 8 95744.8 1970.99 1 0 0 -9 902.101 306.247 1 0 0 10 19330.9 405.011 1 0 0 11 36841.6 595.483 1 0 0 -12 55161.7 686.983 1 0 0 13 7061.25 310.405 1 0 0 14 3561.92 224.109 1 0 0 -15 30346.6 488.592 1 0 0 -16 19090.7 571.714 1 0 -1 16 18273.7 601.182 1 0 1 -15 7209.18 264.226 1 0 -1 14 489.530 178.321 1 0 1 -13 22052.5 473.036 1 0 1 -12 78379.8 916.600 1 0 1 -11 24475.7 578.002 1 0 1 -10 1036.09 253.739 1 0 1 -9 88819.4 1215.44 1 0 1 -8 114109. 1577.85 1 0 1 -7 20333.4 707.027 1 0 1 -6 1576.85 303.637 1 0 -1 5 103092. 1674.23 1 0 1 -4 33198.1 884.956 1 0 -1 3 84127.8 1096.51 1 0 1 -3 154990. 2380.42 -2 0 1 -3 154990. 2380.42 1 0 -1 2 68322.2 704.348 1 0 1 -2 129265. 1872.16 -2 0 1 -2 129265. 1872.16 1 0 -1 1 431813. 1807.71 1 0 1 0 470543. 2293.37 -2 0 1 0 470543. 2293.37 1 0 1 1 67342.3 958.624 1 0 -1 -1 112914. 1624.94 -2 0 -1 -1 112914. 1624.94 1 0 -1 -2 120504. 1447.65 1 0 -1 -2 210925. 2496.81 -2 0 -1 -2 210925. 2496.81 1 0 1 3 222952. 2314.46 1 0 1 4 3251.90 326.990 1 0 1 5 948.455 288.590 1 0 -1 -6 38785.3 1246.00 1 0 -1 -7 97092.1 1324.67 1 0 -1 -8 10436.2 504.983 1 0 -1 -9 11055.3 490.133 1 0 -1 -10 30516.7 488.462 1 0 -1 -11 30930.7 518.722 1 0 -1 -12 27304.4 546.899 1 0 -1 -13 168.167 218.173 1 0 -1 -14 19150.2 433.406 1 0 -1 -15 36522.4 533.429 1 0 1 16 1550.24 332.202 1 0 2 -17 19798.7 859.977 1 0 2 -16 5741.18 306.051 1 0 2 -15 387.108 173.692 1 0 -2 14 4778.36 251.384 1 0 -2 13 26718.0 511.892 1 0 -2 12 51863.0 771.497 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43490.3 565.774 1 3 -2 -10 973.280 176.834 1 -3 2 9 51301.6 899.760 1 -3 2 8 98691.8 1083.40 1 3 -2 -7 11026.6 345.322 1 -3 2 6 18357.5 530.165 1 -3 2 5 322220. 3233.90 1 -3 2 4 307728. 3324.99 1 3 -2 -3 3547.63 462.624 1 3 -2 -2 182880. 2961.42 1 -3 2 2 307636. 3651.62 -2 -3 2 2 307636. 3651.62 1 3 -2 -1 262017. 2283.29 1 -3 2 1 434022. 4001.26 -2 -3 2 1 434022. 4001.26 1 3 -2 0 2882.15 236.250 1 -3 2 0 5783.32 609.875 -2 -3 2 0 5783.32 609.875 1 -3 2 -1 1487.44 239.004 1 3 -2 2 3162.69 299.288 1 -3 2 -3 50647.8 848.079 1 3 -2 4 69782.2 1093.14 1 -3 2 -5-128.161 328.067 1 -3 2 -6 79921.7 2022.93 1 -3 2 -7 110459. 2271.81 1 3 -2 8 25456.7 653.607 1 -3 2 -9 1078.69 200.957 1 3 -2 10 40922.2 671.991 1 -3 2 -11 53884.5 844.369 1 -3 2 -12 4038.78 263.065 1 3 -2 13 9625.61 340.797 1 -3 2 -14 24133.1 634.066 1 3 -2 15 21567.8 723.465 1 -3 1 17 18997.9 437.292 1 -3 1 16 14857.8 396.875 1 3 -1 -15 745.646 209.525 1 3 -1 -14 14015.8 423.545 1 3 -1 -13 45052.8 685.711 1 3 -1 -12 56301.6 671.255 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579.871 1 -3 0 7 116075. 1310.39 1 3 0 -6 55769.2 1382.43 1 -3 0 5 3636.15 352.051 1 -3 0 4 126408. 1579.52 1 -3 0 3 97898.1 1365.52 1 3 0 -2 16884.3 457.110 1 -3 0 1 111360. 959.681 1 -3 0 0 15106.1 662.999 1 3 0 1 13052.7 564.067 1 -3 0 -2 271598. 2535.78 1 -3 0 -3 44944.0 897.738 1 -3 0 -4 23027.1 872.622 1 -3 0 -5 97242.0 1880.53 1 -3 0 -6 30110.5 777.015 1 3 0 7 7461.96 1007.73 1 3 0 8 18495.6 788.869 1 -3 0 -9 57589.6 1072.30 1 3 0 10 67739.9 1293.57 1 -3 0 -11 630.144 257.905 1 3 0 12 27068.1 568.182 1 -3 0 -13 42248.3 762.949 1 3 0 14 8446.51 395.644 1 3 1 -17 6310.92 244.068 1 -3 -1 16 356.453 210.889 1 -3 -1 15 29155.8 816.126 1 -3 -1 14 59470.5 746.042 1 3 1 -13 7126.18 331.818 1 -3 -1 12 41184.9 565.523 1 -3 -1 11 37501.8 559.825 1 -3 -1 10 16408.5 481.340 1 -3 -1 9 27157.0 499.374 1 3 1 -8 43004.8 740.015 1 -3 -1 7 139660. 1502.39 1 -3 -1 6 66630.8 953.301 1 -3 -1 5 5418.69 395.697 1 3 1 -4 17729.2 638.764 1 -3 -1 3 67847.6 918.846 1 -3 -1 2 440723. 2658.39 1 3 1 -2 770515. 4878.68 -2 3 1 -2 770515. 4878.68 1 -3 -1 1 2142.62 201.542 1 3 1 -1 3238.67 702.286 -2 3 1 -1 3238.67 702.286 1 -3 -1 0 101486. 1307.76 1 -3 -1 -1 366624. 3600.95 1 -3 -1 -2 92400.5 976.506 1 -3 -1 -3 1499.06 280.265 1 3 1 4 135611. 1428.97 1 -3 -1 -5 150701. 1714.71 1 -3 -1 -6 6782.15 494.538 1 -3 -1 -7 6630.00 497.098 1 3 1 8 52117.3 811.364 1 -3 -1 -9 49956.0 854.937 1 -3 -1 -10 3032.88 325.574 1 -3 -1 -11 9867.21 395.799 1 3 1 12 32363.6 609.640 1 -3 -1 -13 25344.2 489.352 1 3 1 14 1310.28 259.644 1 3 2 -18 12377.3 698.539 1 -3 -2 17 64.7242 159.636 1 -3 -2 16 20654.9 542.753 1 -3 -2 15 45205.8 734.621 1 -3 -2 14 22243.8 521.660 1 -3 -2 13 4215.16 292.723 1 -3 -2 12 59710.6 714.180 1 -3 -2 11 45962.1 568.543 1 3 2 -10 3509.57 279.164 1 3 2 -9 3650.44 269.309 1 3 2 -8 61252.8 729.698 1 -3 -2 7 171197. 2610.22 1 -3 -2 6 36537.1 615.335 1 3 2 -5 18278.3 535.919 1 3 2 -4 6544.99 400.120 1 3 2 -4 12227.2 570.710 -2 3 2 -4 12227.2 570.710 1 3 2 -3 183550. 2108.92 1 3 2 -3 304649. 2777.05 -2 3 2 -3 304649. 2777.05 1 -3 -2 2 58353.0 1964.22 1 3 2 -2 91550.9 1898.37 -2 3 2 -2 91550.9 1898.37 1 -3 -2 1 101653. 1640.07 1 -3 -2 0 405468. 2805.15 1 -3 -2 -1 247761. 2703.95 1 -3 -2 -2 8692.59 384.324 1 -3 -2 -3 116752. 1359.51 1 -3 -2 -4 220516. 2446.97 1 -3 -2 -5 28106.2 786.192 1 -3 -2 -6 144.811 471.739 1 -3 -2 -7 23743.1 556.915 1 -3 -2 -8 90517.2 1035.66 1 3 2 9 5735.12 328.508 1 -3 -2 -10 12130.3 459.742 1 3 2 11 29294.1 653.260 1 3 2 12 24121.4 621.727 1 -3 -2 -13 9699.16 294.066 1 3 2 14 276.256 195.798 1 -3 -3 18 717.413 225.267 1 -3 -3 17 7489.47 281.679 1 3 3 -16 37814.2 801.445 1 -3 -3 15 26600.8 684.005 1 -3 -3 14 723.271 244.779 1 -3 -3 13 26021.8 503.391 1 3 3 -12 47297.6 675.959 1 -3 -3 11 46008.6 666.113 1 -3 -3 10 13528.7 412.609 1 -3 -3 9 103118. 1045.89 1 3 3 -8 156859. 1626.28 1 3 3 -7 36299.7 768.557 1 -3 -3 6 2853.63 288.720 1 -3 -3 5 128304. 1510.17 1 -3 -3 4 139408. 1896.87 1 -3 -3 3 47545.3 923.768 1 -3 -3 2 90557.4 1456.78 1 -3 -3 2 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1 9 28078.9 994.756 1 17 -1 -8 23613.7 886.495 1 -17 1 7 22633.3 968.213 -2 -17 1 8 22633.3 968.213 1 17 -1 -7 1468.57 430.543 1 -17 1 6 6556.04 573.403 -2 -17 1 7 6556.04 573.403 1 17 -1 -6 8836.77 621.059 1 17 -1 -5 15436.1 705.252 1 17 -1 -4 8223.33 530.770 1 17 0 -12 8828.83 365.802 1 17 0 -11 492.533 247.377 1 17 0 -10 7055.13 405.066 1 17 0 -9 16666.4 768.870 1 -17 0 8 21169.5 905.170 -2 -17 0 9 21169.5 905.170 1 17 0 -8 10926.8 656.258 1 -17 0 7 10736.3 720.472 -2 -17 0 8 10736.3 720.472 1 17 0 -7 855.493 402.891 1 -17 0 6 9118.09 576.735 -2 -17 0 7 9118.09 576.735 1 17 0 -6 12625.7 655.061 1 -17 0 5 10836.9 417.450 1 17 0 -4 1812.74 334.036 1 17 1 -12 83.5419 226.521 1 17 1 -11 7675.81 392.102 1 17 1 -10 18128.2 753.745 1 -17 -1 9 26312.4 923.727 -2 -17 -1 10 26312.4 923.727 1 17 1 -9 9959.98 618.635 1 -17 -1 8 9847.81 703.587 -2 -17 -1 9 9847.81 703.587 1 17 1 -8 259.542 347.357 1 -17 -1 7 2577.24 487.896 -2 -17 -1 8 2577.24 487.896 1 17 1 -7 3217.90 325.582 1 -17 -1 6 12254.9 443.835 1 17 1 -5 7323.73 460.532 1 17 1 -4-33.3712 305.034 1 17 2 -12 661.526 225.959 1 -17 -2 11 16385.5 404.729 1 17 2 -10 20828.4 726.489 1 -17 -2 9 21229.8 835.245 -2 -17 -2 10 21229.8 835.245 1 17 2 -9 1100.01 344.040 1 -17 -2 8 2512.24 497.973 -2 -17 -2 9 2512.24 497.973 1 17 2 -8 1968.44 383.206 1 -17 -2 7 7461.44 407.145 -2 -17 -2 8 7461.44 407.145 1 -17 -2 7 8308.42 389.499 1 -17 -2 6 12492.9 405.830 1 17 2 -5 1202.05 361.164 1 -17 -3 11 17422.7 505.414 1 17 3 -10 5834.40 413.600 1 -17 -3 9 8068.79 426.322 -2 -17 -3 10 8068.79 426.322 1 17 3 -9 1370.79 320.770 1 -17 -3 8 5706.03 429.508 -2 -17 -3 9 5706.03 429.508 1 17 3 -8 7627.87 452.391 1 -17 -3 7 16836.4 738.848 -2 -17 -3 8 16836.4 738.848 1 -17 -3 7 13984.1 666.263 1 -17 -4 9 4493.05 479.958 -2 -17 -4 10 4493.05 479.958 1 -17 -4 8 16380.9 737.432 -2 -17 -4 9 16380.9 737.432 1 0 0 0 0.00000 0.00000 0 TITL MK-207_twin1_hklf4 in P-1 REM P-1 (#2 in standard setting) CELL 1.54184 14.258071 14.802626 15.504490 106.7988 114.1561 91.4673 ZERR 2.00 0.000246 0.000175 0.000282 0.0013 0.0017 0.0012 LATT 1 SFAC C H N O Si U UNIT 144.00 324.00 8.00 48.00 12.00 4.00 REM CrysAlisPro recorded range (K): Min=140.0; max=140.0; aver:140.0 TEMP -133 TREF HKLF 5 BASF 0.39485 END ; _shelx_hkl_checksum 87089 _shelx_fab_file ; -8 -6 19 0.17 0.00 -6 -7 19 0.26 0.00 -7 -7 19 -0.13 0.00 -8 -7 19 -0.21 0.00 -10 -1 18 -0.06 0.00 -3 -2 18 0.20 0.00 -8 -2 18 0.19 0.00 -10 -2 18 -0.36 0.00 -11 -2 18 -0.61 0.00 -2 -3 18 0.26 0.00 -11 -3 18 -0.07 0.00 -12 -3 18 0.19 0.00 -9 -4 18 0.03 0.00 -10 -4 18 0.03 0.00 -11 -4 18 0.28 0.00 -12 -4 18 0.12 0.00 -4 -5 18 -0.07 0.00 -11 -5 18 0.04 0.00 -12 -5 18 -0.04 0.00 -2 -6 18 -0.63 0.00 -3 -6 18 -0.26 0.00 -5 -6 18 0.01 0.00 -6 -6 18 -0.32 0.00 -7 -6 18 -0.61 0.00 -11 -6 18 -0.07 0.00 -3 -7 18 -0.48 0.00 -5 -7 18 -0.28 0.00 -6 -7 18 -0.06 0.00 -7 -7 18 0.03 0.00 -10 -7 18 -0.07 0.00 -11 -7 18 -0.29 0.00 -2 -8 18 -0.48 0.00 -4 -8 18 -0.37 0.00 -5 -8 18 -0.02 0.00 -6 -8 18 0.20 0.00 -7 -8 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12 -0.11 0.00 7 0 12 0.10 0.00 -17 1 12 -0.27 0.00 6 2 12 0.03 0.00 5 4 12 0.21 0.00 -15 6 12 0.21 0.00 1 8 12 -0.08 0.00 -12 9 12 0.29 0.00 -11 9 12 -0.09 0.00 -10 10 12 0.08 0.00 -4 10 12 0.13 0.00 -3 10 12 0.12 0.00 -9 -15 13 -0.18 0.00 4 -13 13 -0.13 0.00 6 -11 13 0.58 0.00 7 -7 13 0.19 0.00 -16 -6 13 0.18 0.00 7 -6 13 -0.04 0.00 7 -5 13 0.28 0.00 7 -4 13 0.16 0.00 5 2 13 0.28 0.00 -16 3 13 0.02 0.00 -15 5 13 -0.18 0.00 -14 6 13 0.13 0.00 -13 7 13 0.06 0.00 -12 8 13 -0.26 0.00 -10 9 13 -0.01 0.00 -4 9 13 -0.24 0.00 -4 -16 14 -0.20 0.00 -3 -16 14 0.03 0.00 -8 -15 14 0.05 0.00 2 -14 14 0.04 0.00 -11 -13 14 -0.35 0.00 3 -13 14 -0.24 0.00 -12 -12 14 -0.17 0.00 4 -12 14 0.03 0.00 -13 -11 14 0.00 0.00 -15 -8 14 -0.13 0.00 -15 -7 14 -0.30 0.00 -16 -5 14 0.13 0.00 -16 -4 14 0.32 0.00 5 -1 14 -0.44 0.00 -16 1 14 -0.05 0.00 4 1 14 -0.41 0.00 2 4 14 -0.18 0.00 -14 5 14 -0.03 0.00 1 5 14 -0.18 0.00 -13 6 14 0.33 0.00 -2 7 14 -0.06 0.00 -9 8 14 0.30 0.00 -5 8 14 0.06 0.00 -6 -15 15 0.23 0.00 -5 -15 15 -0.03 0.00 -4 -15 15 -0.25 0.00 -3 -15 15 -0.28 0.00 -2 -15 15 -0.07 0.00 2 -12 15 -0.07 0.00 3 -11 15 0.14 0.00 -14 -9 15 -0.35 0.00 4 -9 15 0.46 0.00 -15 -7 15 -0.36 0.00 -15 -6 15 -0.50 0.00 4 -5 15 0.49 0.00 4 -4 15 0.29 0.00 4 -3 15 0.15 0.00 3 0 15 0.31 0.00 -15 2 15 0.37 0.00 1 3 15 0.11 0.00 0 4 15 0.25 0.00 -11 6 15 -0.13 0.00 -3 6 15 0.44 0.00 -8 7 15 -0.16 0.00 -7 7 15 -0.03 0.00 -7 -14 16 -0.01 0.00 -6 -14 16 0.01 0.00 -5 -14 16 -0.01 0.00 -4 -14 16 0.14 0.00 -3 -14 16 0.27 0.00 -9 -13 16 0.25 0.00 2 -10 16 -0.18 0.00 3 -7 16 -0.13 0.00 3 -6 16 -0.26 0.00 3 -5 16 -0.34 0.00 -15 -4 16 -0.60 0.00 -15 -3 16 0.11 0.00 -15 -2 16 -0.12 0.00 -15 -1 16 0.05 0.00 -14 1 16 -0.10 0.00 -13 3 16 0.17 0.00 -12 4 16 0.22 0.00 -3 4 16 -0.29 0.00 -10 5 16 -0.03 0.00 -5 5 16 -0.58 0.00 -6 -13 17 0.05 0.00 -5 -13 17 -0.38 0.00 -4 -13 17 -0.47 0.00 -9 -12 17 -0.27 0.00 -2 -12 17 0.00 0.00 -1 -11 17 -0.20 0.00 0 -10 17 0.51 0.00 1 -8 17 0.08 0.00 1 -7 17 0.31 0.00 1 -6 17 0.59 0.00 -14 -5 17 0.24 0.00 1 -5 17 0.39 0.00 -14 -4 17 -0.20 0.00 1 -4 17 0.31 0.00 -14 -3 17 0.18 0.00 -14 -2 17 0.10 0.00 -1 0 17 -0.35 0.00 -2 1 17 -0.22 0.00 -12 2 17 0.03 0.00 -3 2 17 -0.14 0.00 -10 3 17 0.27 0.00 -9 3 17 0.14 0.00 -5 3 17 0.13 0.00 -8 -11 18 0.06 0.00 -7 -11 18 -0.01 0.00 -6 -11 18 -0.13 0.00 -5 -11 18 -0.17 0.00 -4 -11 18 -0.12 0.00 -9 -10 18 0.03 0.00 -12 -7 18 -0.30 0.00 -1 -7 18 -0.48 0.00 -12 -6 18 -0.22 0.00 -1 -6 18 -0.66 0.00 -1 -5 18 -0.26 0.00 -12 -2 18 -0.36 0.00 -2 -2 18 0.27 0.00 -12 -1 18 -0.31 0.00 -3 -1 18 -0.09 0.00 -11 0 18 -0.05 0.00 -4 0 18 -0.40 0.00 -10 1 18 -0.01 0.00 -9 1 18 -0.12 0.00 -8 1 18 -0.34 0.00 -6 1 18 -0.55 0.00 -8 -8 19 -0.30 0.00 -7 -8 19 -0.57 0.00 -6 -8 19 -0.21 0.00 -5 -8 19 0.29 0.00 -9 -7 19 0.03 0.00 -5 -7 19 0.39 0.00 -10 -6 19 0.39 0.00 -9 -6 19 0.43 0.00 -10 -5 19 0.11 0.00 -9 -5 19 -0.17 0.00 -8 -5 19 -0.57 0.00 -10 -4 19 -0.32 0.00 -9 -4 19 -0.60 0.00 -5 -4 19 0.96 0.00 -9 -3 19 -0.24 0.00 -8 -3 19 0.50 0.00 -6 -3 19 1.31 0.00 -8 -2 19 0.72 0.00 -7 -2 19 0.92 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 180320) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 372 79 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL mk-207_twin1_hklfP -1 R = 0.04 CELL 14.2581 14.8026 15.5045 106.80 114.16 91.47 SPGR P-1 # Solvent Accessible Volume = 374 # Electrons Found in S.A.V. = 78 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.890 0.766 0.219 ! 3.05 eA-3 C102 0.912 0.860 0.213 ! 3.05 eA-3 C103 0.887 0.936 0.277 ! 2.99 eA-3 C104 0.877 0.779 0.297 ! 2.61 eA-3 C105 0.902 0.956 0.373 ! 2.19 eA-3 C106 0.843 0.875 0.323 ! 1.98 eA-3 C107 0.967 0.897 0.404 ! 1.77 eA-3 C108 0.971 0.829 0.339 ! 1.75 eA-3 Q109 0.371 0.407 0.319 ! 1.73 eA-3 Q110 0.436 0.411 0.419 ! 1.38 eA-3 Q111 0.359 0.428 0.390 ! 1.22 eA-3 Q112 0.440 0.401 0.341 ! 1.19 eA-3 Q113 0.330 0.066 0.133 ! 1.00 eA-3 C114 0.838 0.856 0.257 ! 0.99 eA-3 Q115 0.284 0.152 0.030 ! 0.96 eA-3 Q116 0.433 0.348 0.315 ! 0.73 eA-3 Q117 0.492 0.693 0.454 ! 0.73 eA-3 Q118 0.507 0.258 0.455 ! 0.73 eA-3 Q119 0.296 0.421 0.026 ! 0.69 eA-3 Q120 0.375 1.003 0.005 ! 0.68 eA-3 Q121 0.614 0.531 0.445 ! 0.68 eA-3 Q122 0.450 0.313 0.451 ! 0.65 eA-3 Q123 0.629 0.437 0.469 ! 0.61 eA-3 Q124 0.400 0.487 0.455 ! 0.61 eA-3 Q125 0.681 0.606 0.015 ! 0.60 eA-3 Q126 0.202 0.234 0.107 ! 0.59 eA-3 Q127 0.527 0.423 0.421 ! 0.57 eA-3 Q128 0.419 0.246 0.472 ! 0.57 eA-3 Q129 0.172 0.572 0.311 ! 0.51 eA-3 Q130 0.515 0.414 0.499 ! 0.51 eA-3 Q131 0.296 0.379 0.389 ! 0.50 eA-3 ) ; _shelx_fab_checksum 87464 _platon_squeeze_void_probe_radius 1.20 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 3.755 _oxdiff_exptl_absorpt_empirical_full_min 0.490 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 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 0.59908(2) 0.59000(2) 0.63066(2) 0.02204(4) Uani 1 1 d . . . . . Si1 Si 0.47800(7) 0.76096(6) 0.75708(6) 0.02820(17) Uani 1 1 d . . . . . Si2 Si 0.82972(7) 0.75875(6) 0.69410(6) 0.02762(17) Uani 1 1 d . . . . . Si3 Si 0.65616(7) 0.42351(5) 0.77714(6) 0.02709(17) Uani 1 1 d . . . . . O1 O 0.55426(19) 0.69040(15) 0.73302(17) 0.0305(5) Uani 1 1 d . . . . . O2 O 0.37308(19) 0.70742(17) 0.74941(18) 0.0342(5) Uani 1 1 d . . . . . O3 O 0.4370(2) 0.80939(16) 0.66813(18) 0.0334(5) Uani 1 1 d . . . . . O4 O 0.5346(2) 0.84068(16) 0.86798(18) 0.0355(5) Uani 1 1 d . . . . . O21 O 0.75029(17) 0.66660(15) 0.67061(17) 0.0288(5) Uani 1 1 d . . . . . O22 O 0.75511(19) 0.83432(15) 0.65421(17) 0.0325(5) Uani 1 1 d . . . . . O23 O 0.90375(19) 0.81188(16) 0.81250(18) 0.0339(5) Uani 1 1 d . . . . . O24 O 0.90756(19) 0.73356(17) 0.64039(19) 0.0356(5) Uani 1 1 d . . . . . O41 O 0.63674(19) 0.47999(17) 0.69868(18) 0.0340(5) Uani 1 1 d . . . . . O42 O 0.6461(2) 0.48360(17) 0.87785(18) 0.0363(5) Uani 1 1 d . . . . . O43 O 0.77135(19) 0.39389(16) 0.81614(18) 0.0349(5) Uani 1 1 d . . . . . O44 O 0.5630(2) 0.33108(15) 0.71761(17) 0.0328(5) Uani 1 1 d . . . . . N1 N 0.4146(2) 0.51570(19) 0.5297(2) 0.0308(6) Uani 1 1 d D . . . . H1A H 0.395(4) 0.482(3) 0.561(3) 0.049(13) Uiso 1 1 d D . . . . H1B H 0.368(4) 0.557(4) 0.524(4) 0.075(18) Uiso 1 1 d D . . . . N2 N 0.5352(2) 0.70693(19) 0.5288(2) 0.0308(6) Uani 1 1 d . . . . . H2A H 0.502032 0.672907 0.462380 0.037 Uiso 1 1 calc R U . . . H2B H 0.590883 0.748207 0.540714 0.037 Uiso 1 1 calc R U . . . H2C H 0.490387 0.740480 0.547899 0.037 Uiso 1 1 calc R U . . . C1 C 0.3497(3) 0.6540(3) 0.8046(3) 0.0377(8) Uani 1 1 d . U . . . C2 C 0.3969(4) 0.5631(3) 0.7930(3) 0.0494(10) Uani 1 1 d . U . . . H2D H 0.367275 0.524325 0.722054 0.074 Uiso 1 1 calc R U . . . H2E H 0.381336 0.526682 0.830555 0.074 Uiso 1 1 calc R U . . . H2F H 0.472588 0.579625 0.818921 0.074 Uiso 1 1 calc R U . . . C3 C 0.2306(3) 0.6286(4) 0.7546(4) 0.0550(11) Uani 1 1 d . U . . . H3A H 0.200276 0.687488 0.760607 0.082 Uiso 1 1 calc R U . . . H3B H 0.208832 0.590529 0.787464 0.082 Uiso 1 1 calc R U . . . H3C H 0.206396 0.591534 0.683635 0.082 Uiso 1 1 calc R U . . . C4 C 0.3894(4) 0.7146(3) 0.9136(3) 0.0505(10) Uani 1 1 d . U . . . H4A H 0.465080 0.733719 0.942863 0.076 Uiso 1 1 calc R U . . . H4B H 0.372587 0.677372 0.949910 0.076 Uiso 1 1 calc R U . . . H4C H 0.356101 0.771744 0.918467 0.076 Uiso 1 1 calc R U . . . C5 C 0.3468(4) 0.8528(3) 0.6318(3) 0.0506(10) Uani 1 1 d . U . . . C6 C 0.2544(4) 0.7732(5) 0.5618(4) 0.0707(14) Uani 1 1 d . U . . . H6A H 0.193056 0.801072 0.530042 0.106 Uiso 1 1 calc R U . . . H6B H 0.239976 0.737058 0.600192 0.106 Uiso 1 1 calc R U . . . H6C H 0.270484 0.730294 0.510266 0.106 Uiso 1 1 calc R U . . . C7 C 0.3687(4) 0.9109(3) 0.5741(4) 0.0565(11) Uani 1 1 d . U . . . H7A H 0.309424 0.943183 0.547850 0.085 Uiso 1 1 calc R U . . . H7B H 0.379204 0.868323 0.518463 0.085 Uiso 1 1 calc R U . . . H7C H 0.431571 0.958688 0.618756 0.085 Uiso 1 1 calc R U . . . C8 C 0.3274(6) 0.9151(5) 0.7183(4) 0.0861(19) Uani 1 1 d . U . . . H8A H 0.388627 0.964441 0.764173 0.129 Uiso 1 1 calc R U . . . H8B H 0.314394 0.875311 0.754179 0.129 Uiso 1 1 calc R U . . . H8C H 0.266542 0.945729 0.691978 0.129 Uiso 1 1 calc R U . . . C9 C 0.6304(3) 0.9074(3) 0.9222(3) 0.0402(8) Uani 1 1 d . U . . . C10 C 0.6098(5) 0.9961(4) 0.8906(6) 0.0853(19) Uani 1 1 d . U . . . H10A H 0.597613 0.980526 0.820560 0.128 Uiso 1 1 calc R U . . . H10B H 0.670390 1.046958 0.933058 0.128 Uiso 1 1 calc R U . . . H10C H 0.548303 1.017893 0.897812 0.128 Uiso 1 1 calc R U . . . C11 C 0.6526(6) 0.9346(6) 1.0287(4) 0.102(2) Uani 1 1 d . U . . . H11A H 0.594428 0.962290 1.038260 0.153 Uiso 1 1 calc R U . . . H11B H 0.716601 0.981831 1.068912 0.153 Uiso 1 1 calc R U . . . H11C H 0.661463 0.877775 1.049744 0.153 Uiso 1 1 calc R U . . . C12 C 0.7156(4) 0.8673(4) 0.9000(5) 0.0800(18) Uani 1 1 d . U . . . H12A H 0.728116 0.809931 0.919689 0.120 Uiso 1 1 calc R U . . . H12B H 0.779330 0.915090 0.937483 0.120 Uiso 1 1 calc R U . . . H12C H 0.695599 0.850564 0.828130 0.120 Uiso 1 1 calc R U . . . C21 C 0.7763(3) 0.9324(2) 0.6598(3) 0.0401(8) Uani 1 1 d . U . . . C22 C 0.6709(4) 0.9653(3) 0.6264(3) 0.0496(10) Uani 1 1 d . U . . . H22A H 0.640157 0.960888 0.671457 0.074 Uiso 1 1 calc R U . . . H22B H 0.624760 0.924571 0.558039 0.074 Uiso 1 1 calc R U . . . H22C H 0.679954 1.031833 0.628245 0.074 Uiso 1 1 calc R U . . . C23 C 0.8487(4) 0.9943(3) 0.7663(3) 0.0598(13) Uani 1 1 d . U . . . H23A H 0.917825 0.975344 0.785322 0.090 Uiso 1 1 calc R U . . . H23B H 0.820572 0.985840 0.811992 0.090 Uiso 1 1 calc R U . . . H23C H 0.854469 1.061623 0.770185 0.090 Uiso 1 1 calc R U . . . C24 C 0.8233(4) 0.9349(3) 0.5887(4) 0.0534(10) Uani 1 1 d . U . . . H24A H 0.836953 1.001099 0.591262 0.080 Uiso 1 1 calc R U . . . H24B H 0.774474 0.896000 0.520390 0.080 Uiso 1 1 calc R U . . . H24C H 0.888733 0.909280 0.608263 0.080 Uiso 1 1 calc R U . . . C25 C 1.0017(3) 0.7955(3) 0.8800(3) 0.0410(8) Uani 1 1 d . U . . . C26 C 1.0082(4) 0.8411(3) 0.9837(3) 0.0599(13) Uani 1 1 d . U . . . H26A H 0.949316 0.810785 0.988360 0.090 Uiso 1 1 calc R U . . . H26B H 1.005675 0.909606 0.996012 0.090 Uiso 1 1 calc R U . . . H26C H 1.073662 0.832525 1.033679 0.090 Uiso 1 1 calc R U . . . C27 C 1.0880(3) 0.8456(4) 0.8683(4) 0.0630(13) Uani 1 1 d . U . . . H27A H 1.083150 0.913767 0.881399 0.094 Uiso 1 1 calc R U . . . H27B H 1.080724 0.817061 0.799983 0.094 Uiso 1 1 calc R U . . . H27C H 1.155885 0.838315 0.916003 0.094 Uiso 1 1 calc R U . . . C28 C 1.0059(4) 0.6899(3) 0.8586(3) 0.0491(10) Uani 1 1 d . U . . . H28A H 1.004624 0.662508 0.792447 0.074 Uiso 1 1 calc R U . . . H28B H 0.945591 0.657917 0.859800 0.074 Uiso 1 1 calc R U . . . H28C H 1.070170 0.680582 0.909596 0.074 Uiso 1 1 calc R U . . . C29 C 0.8942(3) 0.6633(3) 0.5483(3) 0.0402(8) Uani 1 1 d . U . . . C30 C 0.9861(4) 0.6920(4) 0.5302(4) 0.0542(10) Uani 1 1 d . U . . . H30A H 0.983570 0.755699 0.523163 0.081 Uiso 1 1 calc R U . . . H30B H 0.982515 0.645598 0.468814 0.081 Uiso 1 1 calc R U . . . H30C H 1.051328 0.693161 0.586935 0.081 Uiso 1 1 calc R U . . . C31 C 0.8970(4) 0.5646(3) 0.5600(3) 0.0497(10) Uani 1 1 d . U . . . H31A H 0.962600 0.565370 0.616184 0.075 Uiso 1 1 calc R U . . . H31B H 0.891913 0.517349 0.498440 0.075 Uiso 1 1 calc R U . . . H31C H 0.838311 0.547555 0.572973 0.075 Uiso 1 1 calc R U . . . C32 C 0.7916(3) 0.6650(3) 0.4632(3) 0.0450(9) Uani 1 1 d . U . . . H32A H 0.733807 0.651910 0.478959 0.067 Uiso 1 1 calc R U . . . H32B H 0.782634 0.616123 0.401066 0.067 Uiso 1 1 calc R U . . . H32C H 0.792458 0.728190 0.454987 0.067 Uiso 1 1 calc R U . . . C41 C 0.7219(3) 0.5517(3) 0.9704(3) 0.0432(9) Uani 1 1 d . U . . . C42 C 0.6592(4) 0.6106(5) 1.0175(4) 0.090(2) Uani 1 1 d . U . . . H42A H 0.615607 0.643153 0.972445 0.134 Uiso 1 1 calc R U . . . H42B H 0.706748 0.658284 1.081364 0.134 Uiso 1 1 calc R U . . . H42C H 0.614791 0.568485 1.029067 0.134 Uiso 1 1 calc R U . . . C43 C 0.7901(4) 0.6149(3) 0.9501(3) 0.0503(10) Uani 1 1 d . U . . . H43A H 0.832227 0.576186 0.922397 0.075 Uiso 1 1 calc R U . . . H43B H 0.836084 0.664997 1.012705 0.075 Uiso 1 1 calc R U . . . H43C H 0.746065 0.644465 0.902006 0.075 Uiso 1 1 calc R U . . . C44 C 0.7878(4) 0.4975(4) 1.0376(3) 0.0613(12) Uani 1 1 d . U . . . H44A H 0.742491 0.457717 1.050619 0.092 Uiso 1 1 calc R U . . . H44B H 0.838819 0.543272 1.101083 0.092 Uiso 1 1 calc R U . . . H44C H 0.824356 0.456658 1.004243 0.092 Uiso 1 1 calc R U . . . C45 C 0.8372(3) 0.3540(3) 0.7710(3) 0.0443(9) Uani 1 1 d . U . . . C46 C 0.8570(5) 0.4160(4) 0.7158(5) 0.0774(16) Uani 1 1 d . U . . . H46A H 0.899205 0.386229 0.682417 0.116 Uiso 1 1 calc R U . . . H46B H 0.894242 0.479371 0.763456 0.116 Uiso 1 1 calc R U . . . H46C H 0.790328 0.422607 0.665677 0.116 Uiso 1 1 calc R U . . . C47 C 0.9358(5) 0.3500(6) 0.8567(5) 0.107(3) Uani 1 1 d . U . . . H47A H 0.919819 0.308143 0.889362 0.160 Uiso 1 1 calc R U . . . H47B H 0.965836 0.414490 0.905178 0.160 Uiso 1 1 calc R U . . . H47C H 0.985812 0.324768 0.831412 0.160 Uiso 1 1 calc R U . . . C48 C 0.7861(5) 0.2539(3) 0.6995(4) 0.0660(13) Uani 1 1 d . U . . . H48A H 0.721442 0.256926 0.644459 0.099 Uiso 1 1 calc R U . . . H48B H 0.770352 0.215379 0.735152 0.099 Uiso 1 1 calc R U . . . H48C H 0.833532 0.224697 0.672507 0.099 Uiso 1 1 calc R U . . . C49 C 0.5236(3) 0.2670(2) 0.7546(3) 0.0388(8) Uani 1 1 d . U . . . C50 C 0.6128(4) 0.2365(3) 0.8306(3) 0.0496(10) Uani 1 1 d . U . . . H50A H 0.656136 0.293159 0.887341 0.074 Uiso 1 1 calc R U . . . H50B H 0.655203 0.203794 0.799062 0.074 Uiso 1 1 calc R U . . . H50C H 0.584364 0.193047 0.854389 0.074 Uiso 1 1 calc R U . . . C51 C 0.4592(4) 0.1808(3) 0.6626(3) 0.0554(11) Uani 1 1 d . U . . . H51A H 0.430228 0.133971 0.682567 0.083 Uiso 1 1 calc R U . . . H51B H 0.503600 0.151560 0.631778 0.083 Uiso 1 1 calc R U . . . H51C H 0.402184 0.201502 0.614410 0.083 Uiso 1 1 calc R U . . . C52 C 0.4549(4) 0.3161(3) 0.8010(4) 0.0505(10) Uani 1 1 d . U . . . H52A H 0.398738 0.336195 0.751517 0.076 Uiso 1 1 calc R U . . . H52B H 0.496872 0.372227 0.859071 0.076 Uiso 1 1 calc R U . . . H52C H 0.424818 0.271351 0.822402 0.076 Uiso 1 1 calc R U . . . 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 0.02395(6) 0.01758(6) 0.02166(6) 0.00498(4) 0.00822(4) 0.00175(4) Si1 0.0314(4) 0.0262(4) 0.0244(4) 0.0052(3) 0.0116(4) 0.0061(3) Si2 0.0264(4) 0.0230(4) 0.0278(4) 0.0049(3) 0.0091(3) -0.0014(3) Si3 0.0304(4) 0.0218(3) 0.0256(4) 0.0082(3) 0.0086(3) 0.0040(3) O1 0.0360(12) 0.0270(10) 0.0268(11) 0.0051(9) 0.0145(10) 0.0076(9) O2 0.0309(12) 0.0404(12) 0.0301(12) 0.0117(10) 0.0122(10) 0.0053(10) O3 0.0388(13) 0.0313(11) 0.0333(12) 0.0122(10) 0.0173(11) 0.0122(10) O4 0.0380(13) 0.0332(11) 0.0286(12) 0.0008(9) 0.0146(11) 0.0038(10) O21 0.0228(11) 0.0244(10) 0.0341(12) 0.0070(9) 0.0096(9) -0.0012(8) O22 0.0358(13) 0.0216(10) 0.0323(12) 0.0065(9) 0.0095(10) -0.0018(9) O23 0.0318(12) 0.0302(11) 0.0282(11) 0.0050(9) 0.0056(10) 0.0010(9) O24 0.0305(12) 0.0353(11) 0.0350(13) 0.0049(10) 0.0136(10) -0.0034(10) O41 0.0346(13) 0.0327(11) 0.0347(12) 0.0173(10) 0.0107(10) 0.0057(10) O42 0.0331(13) 0.0356(12) 0.0308(12) 0.0021(10) 0.0110(10) 0.0013(10) O43 0.0357(13) 0.0313(11) 0.0318(12) 0.0094(9) 0.0094(10) 0.0101(10) O44 0.0393(13) 0.0249(10) 0.0286(11) 0.0078(9) 0.0107(10) -0.0007(9) N1 0.0315(15) 0.0300(13) 0.0310(14) 0.0055(11) 0.0168(12) 0.0027(11) N2 0.0339(15) 0.0261(12) 0.0301(14) 0.0096(11) 0.0115(12) 0.0040(11) C1 0.0395(19) 0.0445(18) 0.0335(17) 0.0145(15) 0.0189(15) 0.0048(15) C2 0.061(3) 0.0432(19) 0.048(2) 0.0186(17) 0.024(2) 0.0105(19) C3 0.041(2) 0.073(3) 0.055(2) 0.026(2) 0.021(2) 0.002(2) C4 0.062(3) 0.056(2) 0.0343(19) 0.0105(17) 0.0250(19) 0.005(2) C5 0.053(2) 0.066(2) 0.041(2) 0.0268(18) 0.0202(18) 0.035(2) C6 0.042(2) 0.108(4) 0.065(3) 0.053(3) 0.010(2) 0.008(3) C7 0.065(3) 0.044(2) 0.053(2) 0.0244(19) 0.012(2) 0.018(2) C8 0.104(4) 0.104(4) 0.060(3) 0.030(3) 0.039(3) 0.077(4) C9 0.042(2) 0.0320(16) 0.0364(18) 0.0003(14) 0.0151(16) 0.0000(14) C10 0.079(4) 0.052(3) 0.102(4) 0.022(3) 0.020(3) 0.006(3) C11 0.087(4) 0.127(5) 0.048(3) -0.014(3) 0.020(3) -0.045(4) C12 0.047(3) 0.053(3) 0.110(4) -0.004(3) 0.027(3) 0.000(2) C21 0.048(2) 0.0234(14) 0.0394(18) 0.0104(13) 0.0107(16) -0.0014(14) C22 0.064(3) 0.0334(17) 0.048(2) 0.0153(16) 0.020(2) 0.0147(18) C23 0.080(3) 0.0277(17) 0.043(2) 0.0070(16) 0.003(2) -0.0079(19) C24 0.058(3) 0.0413(19) 0.064(3) 0.0248(19) 0.025(2) 0.0017(18) C25 0.0353(18) 0.0365(17) 0.0341(18) 0.0063(14) 0.0025(15) 0.0017(14) C26 0.068(3) 0.053(2) 0.032(2) 0.0037(18) 0.003(2) 0.014(2) C27 0.034(2) 0.057(2) 0.072(3) 0.013(2) 0.004(2) -0.0084(19) C28 0.049(2) 0.0401(19) 0.044(2) 0.0095(16) 0.0095(18) 0.0097(17) C29 0.042(2) 0.0416(18) 0.0356(18) 0.0068(15) 0.0199(16) 0.0067(15) C30 0.044(2) 0.072(3) 0.053(2) 0.018(2) 0.028(2) 0.008(2) C31 0.063(3) 0.0380(18) 0.048(2) 0.0068(17) 0.028(2) 0.0135(18) C32 0.041(2) 0.047(2) 0.0359(19) 0.0036(16) 0.0138(17) 0.0026(17) C41 0.0394(19) 0.0426(18) 0.0312(17) -0.0030(15) 0.0103(15) 0.0014(16) C42 0.051(3) 0.106(4) 0.061(3) -0.035(3) 0.019(2) 0.004(3) C43 0.052(2) 0.0362(18) 0.039(2) 0.0063(16) 0.0033(18) -0.0065(17) C44 0.069(3) 0.067(3) 0.031(2) 0.0163(19) 0.007(2) -0.004(2) C45 0.041(2) 0.0415(18) 0.050(2) 0.0112(16) 0.0218(17) 0.0145(16) C46 0.095(4) 0.053(3) 0.117(4) 0.023(3) 0.081(4) 0.015(3) C47 0.057(3) 0.159(6) 0.071(4) 0.010(4) 0.014(3) 0.054(4) C48 0.085(3) 0.043(2) 0.071(3) -0.002(2) 0.049(3) 0.006(2) C49 0.047(2) 0.0286(15) 0.0426(18) 0.0126(14) 0.0205(16) -0.0005(14) C50 0.064(3) 0.0420(19) 0.050(2) 0.0257(17) 0.025(2) 0.0106(18) C51 0.071(3) 0.0322(18) 0.054(2) 0.0068(17) 0.024(2) -0.0132(19) C52 0.053(2) 0.0414(19) 0.064(3) 0.0159(19) 0.032(2) 0.0034(18) 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' 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 1 2 -2 0.0535 0 -1 1 0.0578 -1 -1 1 0.0686 1 0 0 0.0723 -1 0 0 0.0766 0 1 0 0.0563 0 -1 0 0.0507 0 1 1 0.0507 1 -2 -2 0.0628 2 -1 2 0.0613 0 0 1 0.0517 -2 1 1 0.0672 -2 1 0 0.0547 1 1 -2 0.0530 2 1 -2 0.0563 1 1 0 0.0655 -1 -1 2 0.0608 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 U1 124.28(6) . 2_666 ? O1 U1 O21 99.83(9) . . ? O1 U1 N1 158.05(10) . 2_666 ? O1 U1 N1 88.70(9) . . ? O1 U1 N2 82.08(9) . . ? O21 U1 U1 128.39(6) . 2_666 ? O21 U1 N1 93.28(9) . 2_666 ? O21 U1 N1 159.37(10) . . ? O21 U1 N2 82.03(9) . . ? O41 U1 U1 93.50(6) . 2_666 ? O41 U1 O1 101.39(9) . . ? O41 U1 O21 103.42(9) . . ? O41 U1 N1 92.49(10) . 2_666 ? O41 U1 N1 93.12(10) . . ? O41 U1 N2 172.79(9) . . ? N1 U1 U1 36.65(6) . 2_666 ? N1 U1 U1 36.85(7) 2_666 2_666 ? N1 U1 N1 73.51(11) 2_666 . ? N1 U1 N2 82.40(9) 2_666 . ? N1 U1 N2 80.58(9) . . ? N2 U1 U1 79.36(6) . 2_666 ? O1 Si1 O2 114.30(13) . . ? O1 Si1 O3 105.85(12) . . ? O1 Si1 O4 112.62(13) . . ? O2 Si1 O3 104.82(14) . . ? O2 Si1 O4 106.75(13) . . ? O4 Si1 O3 112.34(13) . . ? O21 Si2 O22 104.80(12) . . ? O21 Si2 O23 114.06(13) . . ? O21 Si2 O24 112.58(12) . . ? O23 Si2 O22 106.89(12) . . ? O23 Si2 O24 106.43(13) . . ? O24 Si2 O22 112.04(14) . . ? O41 Si3 O42 114.12(14) . . ? O41 Si3 O43 112.78(14) . . ? O41 Si3 O44 104.56(13) . . ? O42 Si3 O44 107.40(13) . . ? O43 Si3 O42 105.23(13) . . ? O43 Si3 O44 112.82(13) . . ? Si1 O1 U1 152.18(15) . . ? C1 O2 Si1 135.4(2) . . ? C5 O3 Si1 130.9(2) . . ? C9 O4 Si1 134.5(2) . . ? Si2 O21 U1 154.41(14) . . ? C21 O22 Si2 133.3(2) . . ? C25 O23 Si2 132.3(2) . . ? C29 O24 Si2 132.1(2) . . ? Si3 O41 U1 160.51(16) . . ? C41 O42 Si3 130.7(2) . . ? C45 O43 Si3 135.8(2) . . ? C49 O44 Si3 130.6(2) . . ? U1 N1 U1 106.50(11) 2_666 . ? U1 N1 H1A 111(3) 2_666 . ? U1 N1 H1A 110(3) . . ? U1 N1 H1B 114(4) 2_666 . ? U1 N1 H1B 116(4) . . ? H1A N1 H1B 100(5) . . ? U1 N2 H2A 109.5 . . ? U1 N2 H2B 109.5 . . ? U1 N2 H2C 109.5 . . ? H2A N2 H2B 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? O2 C1 C2 109.2(3) . . ? O2 C1 C3 104.9(3) . . ? O2 C1 C4 110.5(3) . . ? C2 C1 C3 109.7(4) . . ? C4 C1 C2 111.6(4) . . ? C4 C1 C3 110.8(4) . . ? C1 C2 H2D 109.5 . . ? C1 C2 H2E 109.5 . . ? C1 C2 H2F 109.5 . . ? H2D C2 H2E 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 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 107.9(4) . . ? O3 C5 C7 105.7(4) . . ? O3 C5 C8 110.7(4) . . ? C6 C5 C8 110.3(5) . . ? C7 C5 C6 110.2(4) . . ? C7 C5 C8 111.8(4) . . ? 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 107.1(4) . . ? O4 C9 C11 106.3(4) . . ? O4 C9 C12 111.8(3) . . ? C11 C9 C10 107.8(5) . . ? C11 C9 C12 113.8(5) . . ? C12 C9 C10 109.7(5) . . ? 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 105.4(3) . . ? O22 C21 C23 110.9(3) . . ? O22 C21 C24 108.9(3) . . ? C22 C21 C23 110.2(4) . . ? C24 C21 C22 110.3(4) . . ? C24 C21 C23 111.0(4) . . ? 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 105.3(3) . . ? O23 C25 C27 107.8(3) . . ? O23 C25 C28 111.2(3) . . ? C26 C25 C27 110.6(4) . . ? C28 C25 C26 110.9(4) . . ? C28 C25 C27 110.8(4) . . ? 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 105.4(3) . . ? O24 C29 C31 109.6(3) . . ? O24 C29 C32 110.1(3) . . ? C30 C29 C31 110.3(4) . . ? C30 C29 C32 110.6(4) . . ? C31 C29 C32 110.7(3) . . ? 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 105.5(3) . . ? O42 C41 C43 110.5(3) . . ? O42 C41 C44 108.9(3) . . ? C42 C41 C44 110.5(4) . . ? C43 C41 C42 110.6(4) . . ? C43 C41 C44 110.7(4) . . ? 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 110.4(3) . . ? O43 C45 C47 104.9(4) . . ? O43 C45 C48 109.4(4) . . ? C47 C45 C46 112.1(5) . . ? C47 C45 C48 109.8(5) . . ? C48 C45 C46 110.1(4) . . ? 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 110.9(3) . . ? O44 C49 C51 105.2(3) . . ? O44 C49 C52 109.5(3) . . ? C50 C49 C51 110.4(3) . . ? C52 C49 C50 110.6(4) . . ? C52 C49 C51 110.3(4) . . ? 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 . . ? 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 3.9375(2) 2_666 ? U1 O1 2.156(2) . ? U1 O21 2.166(2) . ? U1 O41 2.151(2) . ? U1 N1 2.463(3) . ? U1 N1 2.451(3) 2_666 ? U1 N2 2.608(3) . ? Si1 O1 1.606(2) . ? Si1 O2 1.618(3) . ? Si1 O3 1.640(3) . ? Si1 O4 1.626(2) . ? Si2 O21 1.604(2) . ? Si2 O22 1.639(2) . ? Si2 O23 1.625(2) . ? Si2 O24 1.632(3) . ? Si3 O41 1.606(2) . ? Si3 O42 1.624(2) . ? Si3 O43 1.623(3) . ? Si3 O44 1.632(2) . ? O2 C1 1.442(4) . ? O3 C5 1.429(5) . ? O4 C9 1.435(4) . ? O22 C21 1.446(4) . ? O23 C25 1.439(5) . ? O24 C29 1.438(4) . ? O42 C41 1.443(4) . ? O43 C45 1.432(5) . ? O44 C49 1.446(4) . ? N1 H1A 0.90(4) . ? N1 H1B 0.91(4) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? C1 C2 1.516(6) . ? C1 C3 1.533(6) . ? C1 C4 1.515(5) . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C2 H2F 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 1.521(7) . ? C5 C7 1.514(6) . ? C5 C8 1.527(6) . ? 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 1.525(7) . ? C9 C11 1.474(7) . ? C9 C12 1.486(7) . ? 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 1.520(6) . ? C21 C23 1.521(5) . ? C21 C24 1.515(6) . ? 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 1.515(6) . ? C25 C27 1.521(6) . ? C25 C28 1.510(5) . ? 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 1.522(5) . ? C29 C31 1.523(6) . ? C29 C32 1.523(6) . ? 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 1.516(6) . ? C41 C43 1.514(6) . ? C41 C44 1.528(7) . ? 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 1.514(7) . ? C45 C47 1.505(7) . ? C45 C48 1.513(6) . ? 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 1.523(6) . ? C49 C51 1.524(5) . ? C49 C52 1.522(6) . ? 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 . ? 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 Si1 O2 C1 C2 -64.6(4) . . . . ? Si1 O2 C1 C3 177.9(3) . . . . ? Si1 O2 C1 C4 58.5(5) . . . . ? Si1 O3 C5 C6 -79.6(4) . . . . ? Si1 O3 C5 C7 162.5(3) . . . . ? Si1 O3 C5 C8 41.2(6) . . . . ? Si1 O4 C9 C10 84.1(5) . . . . ? Si1 O4 C9 C11 -160.8(4) . . . . ? Si1 O4 C9 C12 -36.0(6) . . . . ? Si2 O22 C21 C22 -168.9(3) . . . . ? Si2 O22 C21 C23 -49.6(5) . . . . ? Si2 O22 C21 C24 72.8(4) . . . . ? Si2 O23 C25 C26 -158.5(3) . . . . ? Si2 O23 C25 C27 83.3(4) . . . . ? Si2 O23 C25 C28 -38.3(5) . . . . ? Si2 O24 C29 C30 167.4(3) . . . . ? Si2 O24 C29 C31 -73.9(4) . . . . ? Si2 O24 C29 C32 48.0(5) . . . . ? Si3 O42 C41 C42 158.4(4) . . . . ? Si3 O42 C41 C43 38.8(5) . . . . ? Si3 O42 C41 C44 -83.0(4) . . . . ? Si3 O43 C45 C46 57.2(5) . . . . ? Si3 O43 C45 C47 178.1(4) . . . . ? Si3 O43 C45 C48 -64.1(5) . . . . ? Si3 O44 C49 C50 -45.3(4) . . . . ? Si3 O44 C49 C51 -164.7(3) . . . . ? Si3 O44 C49 C52 76.9(4) . . . . ? O1 Si1 O2 C1 67.0(3) . . . . ? O1 Si1 O3 C5 158.0(3) . . . . ? O1 Si1 O4 C9 50.5(4) . . . . ? O2 Si1 O1 U1 79.1(3) . . . . ? O2 Si1 O3 C5 36.8(4) . . . . ? O2 Si1 O4 C9 176.7(3) . . . . ? O3 Si1 O1 U1 -35.8(3) . . . . ? O3 Si1 O2 C1 -177.6(3) . . . . ? O3 Si1 O4 C9 -68.9(4) . . . . ? O4 Si1 O1 U1 -158.9(3) . . . . ? O4 Si1 O2 C1 -58.2(3) . . . . ? O4 Si1 O3 C5 -78.7(4) . . . . ? O21 Si2 O22 C21 174.2(3) . . . . ? O21 Si2 O23 C25 85.5(3) . . . . ? O21 Si2 O24 C29 31.3(4) . . . . ? O22 Si2 O21 U1 -13.8(4) . . . . ? O22 Si2 O23 C25 -159.2(3) . . . . ? O22 Si2 O24 C29 -86.5(3) . . . . ? O23 Si2 O21 U1 102.8(3) . . . . ? O23 Si2 O22 C21 52.8(3) . . . . ? O23 Si2 O24 C29 157.0(3) . . . . ? O24 Si2 O21 U1 -135.8(3) . . . . ? O24 Si2 O22 C21 -63.4(3) . . . . ? O24 Si2 O23 C25 -39.3(3) . . . . ? O41 Si3 O42 C41 -86.1(3) . . . . ? O41 Si3 O43 C45 -44.0(4) . . . . ? O41 Si3 O44 C49 -163.3(3) . . . . ? O42 Si3 O41 U1 -4.6(5) . . . . ? O42 Si3 O43 C45 -169.0(3) . . . . ? O42 Si3 O44 C49 -41.7(3) . . . . ? O43 Si3 O41 U1 -124.7(4) . . . . ? O43 Si3 O42 C41 38.1(4) . . . . ? O43 Si3 O44 C49 73.8(3) . . . . ? O44 Si3 O41 U1 112.4(5) . . . . ? O44 Si3 O42 C41 158.5(3) . . . . ? O44 Si3 O43 C45 74.2(4) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 372 79 '2 thf' loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.5851(9) 47938 7016 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.4149(9) 0 7016 nmt 1.0268 0.0064 0.0647 0.0184 1.0029 0.0085 -0.0752 -0.0123 0.9662 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 0.9103 2.0061 -2.0317 0.1991 0.1485 -0.0751 0.0583 -0.9941 0.9783 -0.0780 -0.0541 0.0899 -0.9685 -1.0121 1.0534 -0.1211 -0.0944 -0.0147 1.0268 0.0180 -0.0752 0.0430 0.0403 0.1046 -1.0268 -0.0180 0.0752 -0.0430 -0.0403 -0.1046 0.0064 1.0027 -0.0123 0.0023 0.1080 -0.0217 -0.0064 -1.0027 0.0123 -0.0023 -0.1080 0.0217 0.0710 1.0113 0.9536 -0.0735 0.1619 0.0464 0.8847 -2.0047 -1.9825 0.1901 -0.2835 0.0118 2.1765 -0.9494 1.7939 -0.0678 0.0804 0.3671 0.0647 0.0086 0.9660 -0.0758 0.0539 0.0681 -1.9826 0.9753 1.1040 -0.1596 0.0813 -0.1628 -2.0472 0.9667 0.1380 -0.0838 0.0274 -0.2309 0.9039 1.0034 -2.0194 0.1969 0.0405 -0.0534 1.9307 1.0214 -2.0946 0.2399 0.0808 0.0512 1.0332 1.0207 -0.0875 0.0453 0.1483 0.0828 -0.9039 -1.0034 2.0194 -0.1969 -0.0405 0.0534