#------------------------------------------------------------------------------ #$Date: 2020-03-04 09:46:50 +0200 (Wed, 04 Mar 2020) $ #$Revision: 248752 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557453.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_1557453 loop_ _publ_author_name 'Sharma, Mahendra K.' 'Blomeyer, Sebastian' 'Glodde, Timo' 'Neumann, Beate' 'Stammler, Hans-Georg' 'Hinz, Alexander' 'van Gastel, Maurice' 'Ghadwal, Rajendra S.' _publ_section_title ; Isolation of singlet carbene derived 2-phospha-1,3-butadienes and their sequential one-electron oxidation to radical cations and dications ; _journal_issue 7 _journal_name_full 'Chemical Science' _journal_page_first 1975 _journal_paper_doi 10.1039/C9SC05598C _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C54 H72 N3 P, Cl4 Ga' _chemical_formula_sum 'C54 H72 Cl4 Ga N3 P' _chemical_formula_weight 1005.63 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-04-10 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-08-28 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.7240(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.5123(2) _cell_length_b 12.8811(2) _cell_length_c 37.2397(5) _cell_measurement_reflns_used 60415 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 32.7800 _cell_measurement_theta_min 3.0020 _cell_volume 5472.21(15) _computing_cell_refinement 'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3114 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.940 _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 -87.00 12.00 1.00 81.50 -- -17.14 -77.00 -90.00 99 2 \w 17.00 91.00 1.00 81.50 -- 17.14-154.00-127.09 74 3 \w -8.00 82.00 1.00 81.50 -- 17.14 57.00-150.00 90 4 \w -4.00 83.00 1.00 81.50 -- 17.14 38.00 120.00 87 5 \w -4.00 88.00 1.00 81.50 -- 17.14 38.00 30.00 92 6 \w -53.00 28.00 1.00 81.50 -- 17.14 -38.00 -60.00 81 7 \w 6.00 75.00 1.00 81.50 -- 17.14-131.00 -95.76 69 8 \w -47.00 47.00 1.00 81.50 -- 17.14 -77.00 60.00 94 9 \w 47.00 74.00 1.00 81.50 -- 17.14-130.00 42.13 27 ; _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 -0.0151221000 _diffrn_orient_matrix_UB_12 -0.0199088000 _diffrn_orient_matrix_UB_13 0.0165089000 _diffrn_orient_matrix_UB_21 0.0553588000 _diffrn_orient_matrix_UB_22 -0.0248448000 _diffrn_orient_matrix_UB_23 0.0034246000 _diffrn_orient_matrix_UB_31 0.0239389000 _diffrn_orient_matrix_UB_32 0.0449363000 _diffrn_orient_matrix_UB_33 0.0092232000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_unetI/netI 0.0311 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.940 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_number 120621 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.788 _diffrn_reflns_theta_min 2.727 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.431 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.221 _exptl_crystal_description irregular _exptl_crystal_F_000 2124 _exptl_crystal_size_max 0.411 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.231 _refine_diff_density_max 0.689 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 584 _refine_ls_number_reflns 19071 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.174 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0544 _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^)+(0.0288P)^2^+4.9843P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1072 _refine_ls_wR_factor_ref 0.1106 _reflns_Friedel_coverage 0.000 _reflns_number_gt 16638 _reflns_number_total 19071 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05598c2.cif _cod_data_source_block compound6 _cod_database_code 1557453 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C54 H92 Cl4 Ga N3 P' _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 0.843 _shelx_estimated_absorpt_t_min 0.744 _diffrn_oxdiff_digest_frames ; 017d6918fea4acc13ab1afa85533e8547500476707a ; _diffrn_oxdiff_digest_hkl ; 015b83f5ac0d0b8e089321f4f3e997e0cac464 ; _reflns_odcompleteness_completeness 99.71 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 30.01 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C22(H22), C25(H25), C49(H49), C52(H52) 2.b Secondary CH2 refined with riding coordinates: C37(H37A,H37B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C45(H45), C46(H46), C47(H47) 2.d Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B, H53C), C54(H54A,H54B,H54C) ; _shelx_res_file ; TITL sharma29_a.res in P2(1)/c sharma29.res created by SHELXL-2018/3 at 09:24:24 on 10-Apr-2019 REM Old TITL sharma29 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.112, Rweak 0.141, Alpha 0.038 REM 2.043 for 498 systematic absences, Orientation as input REM Formula found by SHELXT: C54 N3 Cl5 Ga CELL 0.71073 11.5123 12.8811 37.2397 90 97.724 90 ZERR 4 0.0002 0.0002 0.0005 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Ga N P UNIT 216 288 16 4 12 4 L.S. 11 PLAN 5 SIZE 0.231 0.25 0.411 MORE -1 BOND $H CONF fmap 2 acta OMIT 0 0 12 OMIT -3 6 12 OMIT -3 6 3 REM REM REM WGHT 0.028800 4.984300 FVAR 0.27290 GA1 4 0.057677 0.819615 0.365821 11.00000 0.02084 0.01906 = 0.02606 -0.00101 0.00578 -0.00263 CL1 3 0.145582 0.967629 0.375215 11.00000 0.03539 0.02752 = 0.06167 -0.00313 0.00771 -0.01457 CL2 3 0.059289 0.732410 0.415832 11.00000 0.04076 0.03032 = 0.02228 -0.00060 0.00021 -0.00815 CL3 3 -0.123355 0.849168 0.342061 11.00000 0.02312 0.02272 = 0.04663 0.00534 0.00224 0.00097 CL4 3 0.140755 0.724491 0.328083 11.00000 0.03839 0.03351 = 0.03786 0.00061 0.01990 0.00639 P1 6 0.671771 0.278220 0.391155 11.00000 0.01852 0.01747 = 0.01267 0.00029 0.00348 -0.00412 N1 5 0.724923 0.513268 0.372326 11.00000 0.01682 0.01591 = 0.01568 -0.00192 0.00453 -0.00220 N2 5 0.855661 0.473334 0.337166 11.00000 0.01435 0.01325 = 0.01509 -0.00039 0.00387 -0.00246 N3 5 0.588249 0.094377 0.408462 11.00000 0.01770 0.01849 = 0.01298 0.00293 0.00157 -0.00355 C1 1 0.765166 0.431957 0.353517 11.00000 0.01362 0.01663 = 0.01158 0.00063 0.00190 -0.00116 C2 1 0.790153 0.601858 0.367871 11.00000 0.02187 0.01469 = 0.02186 -0.00285 0.00589 -0.00320 AFIX 43 H2 2 0.780050 0.666698 0.377991 11.00000 -1.20000 AFIX 0 C3 1 0.870546 0.576931 0.346283 11.00000 0.01937 0.01404 = 0.02116 -0.00133 0.00526 -0.00459 AFIX 43 H3 2 0.926233 0.621436 0.338814 11.00000 -1.20000 AFIX 0 C4 1 0.620875 0.524718 0.390125 11.00000 0.01880 0.01769 = 0.01958 -0.00220 0.00802 -0.00129 C5 1 0.514655 0.547267 0.368621 11.00000 0.01952 0.02116 = 0.02513 -0.00106 0.00636 -0.00059 C6 1 0.420451 0.577284 0.386477 11.00000 0.02000 0.02822 = 0.03792 -0.00113 0.00958 0.00106 AFIX 43 H6 2 0.348229 0.592001 0.373071 11.00000 -1.20000 AFIX 0 C7 1 0.433746 0.585279 0.423912 11.00000 0.02955 0.03065 = 0.04075 -0.00704 0.02035 0.00017 AFIX 43 H7 2 0.370611 0.606079 0.435355 11.00000 -1.20000 AFIX 0 C8 1 0.539779 0.562680 0.444398 11.00000 0.03534 0.03198 = 0.02549 -0.00772 0.01635 -0.00222 AFIX 43 H8 2 0.546749 0.568031 0.469500 11.00000 -1.20000 AFIX 0 C9 1 0.637197 0.531808 0.428090 11.00000 0.02569 0.02174 = 0.01999 -0.00432 0.00807 -0.00369 C10 1 0.502243 0.545998 0.327467 11.00000 0.02081 0.03727 = 0.02412 0.00101 -0.00013 0.00399 AFIX 13 H10 2 0.566340 0.503992 0.320338 11.00000 -1.20000 AFIX 0 C11 1 0.514396 0.656341 0.312811 11.00000 0.04412 0.05543 = 0.03533 0.01690 -0.00556 -0.01446 AFIX 137 H11A 2 0.453762 0.699631 0.320056 11.00000 -1.50000 H11B 2 0.507399 0.654297 0.286841 11.00000 -1.50000 H11C 2 0.589623 0.684077 0.322376 11.00000 -1.50000 AFIX 0 C12 1 0.386475 0.497625 0.310284 11.00000 0.02940 0.03654 = 0.03827 -0.00303 -0.00630 0.00272 AFIX 137 H12A 2 0.376441 0.431241 0.321174 11.00000 -1.50000 H12B 2 0.387743 0.488923 0.284737 11.00000 -1.50000 H12C 2 0.322663 0.542385 0.314169 11.00000 -1.50000 AFIX 0 C13 1 0.754411 0.510192 0.450840 11.00000 0.03026 0.03398 = 0.01822 -0.00397 0.00522 -0.00315 AFIX 13 H13 2 0.806487 0.479703 0.434925 11.00000 -1.20000 AFIX 0 C14 1 0.811511 0.611019 0.466679 11.00000 0.04210 0.04376 = 0.03449 -0.00829 0.00255 -0.01411 AFIX 137 H14A 2 0.819044 0.658958 0.447390 11.00000 -1.50000 H14B 2 0.887696 0.595852 0.479455 11.00000 -1.50000 H14C 2 0.763454 0.641221 0.483087 11.00000 -1.50000 AFIX 0 C15 1 0.742782 0.432220 0.481286 11.00000 0.04656 0.04552 = 0.02167 0.00374 -0.00110 -0.00810 AFIX 137 H15A 2 0.694709 0.461495 0.497866 11.00000 -1.50000 H15B 2 0.819064 0.416847 0.493954 11.00000 -1.50000 H15C 2 0.707297 0.369520 0.471092 11.00000 -1.50000 AFIX 0 C16 1 0.931623 0.429426 0.312897 11.00000 0.01477 0.01414 = 0.01665 0.00024 0.00573 -0.00222 C17 1 0.906619 0.455398 0.276003 11.00000 0.02108 0.01457 = 0.01627 0.00078 0.00490 -0.00295 C18 1 0.987298 0.423367 0.253422 11.00000 0.03130 0.01746 = 0.01989 0.00075 0.01148 -0.00438 AFIX 43 H18 2 0.972902 0.437722 0.228750 11.00000 -1.20000 AFIX 0 C19 1 1.088291 0.370636 0.267134 11.00000 0.02744 0.01864 = 0.03049 -0.00168 0.01651 -0.00260 AFIX 43 H19 2 1.141823 0.351447 0.251732 11.00000 -1.20000 AFIX 0 C20 1 1.110187 0.346267 0.303581 11.00000 0.01835 0.01740 = 0.03223 0.00105 0.00887 0.00080 AFIX 43 H20 2 1.177905 0.309870 0.312296 11.00000 -1.20000 AFIX 0 C21 1 1.032205 0.375406 0.327644 11.00000 0.01561 0.01527 = 0.02132 0.00128 0.00384 -0.00218 C22 1 0.799333 0.517506 0.260734 11.00000 0.02444 0.01795 = 0.01809 0.00339 0.00161 -0.00059 AFIX 13 H22 2 0.742582 0.513949 0.278094 11.00000 -1.20000 AFIX 0 C23 1 0.831024 0.631988 0.256055 11.00000 0.03362 0.01798 = 0.02911 0.00393 -0.00084 -0.00037 AFIX 137 H23A 2 0.867671 0.659171 0.278794 11.00000 -1.50000 H23B 2 0.761111 0.670806 0.248091 11.00000 -1.50000 H23C 2 0.884113 0.637601 0.238354 11.00000 -1.50000 AFIX 0 C24 1 0.739936 0.475427 0.224297 11.00000 0.04310 0.02255 = 0.01947 0.00363 -0.00647 -0.00178 AFIX 137 H24A 2 0.787829 0.490640 0.205754 11.00000 -1.50000 H24B 2 0.664626 0.507654 0.218329 11.00000 -1.50000 H24C 2 0.730182 0.401655 0.226006 11.00000 -1.50000 AFIX 0 C25 1 1.057418 0.351827 0.367873 11.00000 0.01802 0.02168 = 0.02279 0.00263 0.00059 0.00007 AFIX 13 H25 2 0.982216 0.339459 0.376729 11.00000 -1.20000 AFIX 0 C26 1 1.116232 0.444673 0.388871 11.00000 0.03586 0.02866 = 0.02943 -0.00146 -0.00863 -0.00130 AFIX 137 H26A 2 1.191192 0.457448 0.381136 11.00000 -1.50000 H26B 2 1.126648 0.429568 0.414346 11.00000 -1.50000 H26C 2 1.067625 0.505048 0.384260 11.00000 -1.50000 AFIX 0 C27 1 1.133330 0.254896 0.376277 11.00000 0.02247 0.02743 = 0.03398 0.00745 -0.00191 0.00209 AFIX 137 H27A 2 1.099355 0.197727 0.362013 11.00000 -1.50000 H27B 2 1.137355 0.238247 0.401541 11.00000 -1.50000 H27C 2 1.210848 0.267976 0.370543 11.00000 -1.50000 AFIX 0 C28 1 0.727616 0.325914 0.352682 11.00000 0.01363 0.01547 = 0.01356 0.00016 0.00188 -0.00185 C29 1 0.764525 0.259207 0.323768 11.00000 0.01548 0.01407 = 0.01530 -0.00076 0.00442 -0.00394 C30 1 0.721696 0.276650 0.287340 11.00000 0.02107 0.01512 = 0.01643 0.00040 0.00451 -0.00244 AFIX 43 H30 2 0.667982 0.329717 0.281109 11.00000 -1.20000 AFIX 0 C31 1 0.758900 0.215090 0.260278 11.00000 0.02744 0.01779 = 0.01709 -0.00047 0.00713 -0.00404 AFIX 43 H31 2 0.729178 0.226775 0.236142 11.00000 -1.20000 AFIX 0 C32 1 0.840007 0.136526 0.269180 11.00000 0.02822 0.01840 = 0.02335 -0.00479 0.01162 -0.00304 AFIX 43 H32 2 0.865806 0.096403 0.251053 11.00000 -1.20000 AFIX 0 C33 1 0.882589 0.118030 0.305362 11.00000 0.02076 0.01845 = 0.02732 -0.00142 0.00671 0.00034 AFIX 43 H33 2 0.936724 0.065201 0.311451 11.00000 -1.20000 AFIX 0 C34 1 0.844412 0.178328 0.332435 11.00000 0.01800 0.01720 = 0.02060 0.00041 0.00254 -0.00198 AFIX 43 H34 2 0.872309 0.164732 0.356584 11.00000 -1.20000 AFIX 0 C35 1 0.602235 0.156298 0.380153 11.00000 0.01457 0.01870 = 0.01284 0.00268 0.00162 -0.00095 C36 1 0.530126 0.111431 0.345634 11.00000 0.01653 0.01891 = 0.01328 0.00171 0.00132 -0.00499 C37 1 0.451991 0.031635 0.362307 11.00000 0.01904 0.02478 = 0.01710 0.00214 0.00149 -0.00967 AFIX 23 H37A 2 0.379263 0.063774 0.366936 11.00000 -1.20000 H37B 2 0.433580 -0.026439 0.345949 11.00000 -1.20000 AFIX 0 C38 1 0.522495 -0.005078 0.397745 11.00000 0.02210 0.02240 = 0.01571 0.00378 0.00067 -0.00802 C39 1 0.455809 0.198504 0.326038 11.00000 0.02029 0.02443 = 0.01942 0.00373 -0.00222 -0.00303 AFIX 137 H39A 2 0.410666 0.231591 0.342665 11.00000 -1.50000 H39B 2 0.403938 0.169733 0.306190 11.00000 -1.50000 H39C 2 0.506327 0.248663 0.317000 11.00000 -1.50000 AFIX 0 C40 1 0.600632 0.055864 0.318774 11.00000 0.02453 0.02093 = 0.01924 -0.00321 0.00637 -0.00840 AFIX 137 H40A 2 0.631600 0.106443 0.303676 11.00000 -1.50000 H40B 2 0.550101 0.009020 0.303931 11.00000 -1.50000 H40C 2 0.663979 0.017621 0.332037 11.00000 -1.50000 AFIX 0 C41 1 0.444852 -0.041045 0.425511 11.00000 0.03564 0.03063 = 0.01944 0.00474 0.00503 -0.01599 AFIX 137 H41A 2 0.491174 -0.047077 0.448856 11.00000 -1.50000 H41B 2 0.411199 -0.107305 0.418368 11.00000 -1.50000 H41C 2 0.383365 0.008631 0.426766 11.00000 -1.50000 AFIX 0 C42 1 0.609175 -0.093170 0.393303 11.00000 0.03529 0.02098 = 0.02750 0.00403 -0.00069 -0.00330 AFIX 137 H42A 2 0.666607 -0.069494 0.378720 11.00000 -1.50000 H42B 2 0.567581 -0.151339 0.381708 11.00000 -1.50000 H42C 2 0.647561 -0.113783 0.416703 11.00000 -1.50000 AFIX 0 C43 1 0.629533 0.121565 0.445708 11.00000 0.01822 0.02155 = 0.01197 0.00384 0.00143 -0.00454 C44 1 0.550480 0.170660 0.466074 11.00000 0.01823 0.02301 = 0.01521 0.00441 0.00262 -0.00369 C45 1 0.591026 0.196252 0.502022 11.00000 0.02483 0.02739 = 0.01489 0.00142 0.00512 -0.00282 AFIX 43 H45 2 0.540619 0.228787 0.516008 11.00000 -1.20000 AFIX 0 C46 1 0.704885 0.174139 0.517278 11.00000 0.02656 0.03295 = 0.01347 0.00402 0.00059 -0.00626 AFIX 43 H46 2 0.729917 0.190983 0.541360 11.00000 -1.20000 AFIX 0 C47 1 0.781140 0.127037 0.496659 11.00000 0.01899 0.03300 = 0.01766 0.00622 -0.00125 -0.00367 AFIX 43 H47 2 0.857497 0.112977 0.507104 11.00000 -1.20000 AFIX 0 C48 1 0.746154 0.100030 0.460458 11.00000 0.01823 0.02539 = 0.01517 0.00506 0.00150 -0.00236 C49 1 0.425929 0.201719 0.450701 11.00000 0.01737 0.02831 = 0.01816 0.00343 0.00380 -0.00068 AFIX 13 H49 2 0.407585 0.170158 0.426663 11.00000 -1.20000 AFIX 0 C50 1 0.416416 0.319652 0.446304 11.00000 0.02445 0.03015 = 0.02512 0.00260 0.00380 0.00396 AFIX 137 H50A 2 0.437858 0.352334 0.469413 11.00000 -1.50000 H50B 2 0.337247 0.337960 0.436992 11.00000 -1.50000 H50C 2 0.468176 0.342647 0.429750 11.00000 -1.50000 AFIX 0 C51 1 0.335777 0.161906 0.474638 11.00000 0.02118 0.04409 = 0.02647 0.00415 0.00843 -0.00193 AFIX 137 H51A 2 0.347115 0.088864 0.478873 11.00000 -1.50000 H51B 2 0.257921 0.173962 0.462553 11.00000 -1.50000 H51C 2 0.346238 0.198133 0.497372 11.00000 -1.50000 AFIX 0 C52 1 0.835747 0.051793 0.439025 11.00000 0.01877 0.03666 = 0.02000 0.00474 0.00193 0.00276 AFIX 13 H52 2 0.797923 0.039915 0.414186 11.00000 -1.20000 AFIX 0 C53 1 0.940172 0.125238 0.437546 11.00000 0.01952 0.05271 = 0.02692 0.00808 0.00415 -0.00104 AFIX 137 H53A 2 0.912321 0.190845 0.427627 11.00000 -1.50000 H53B 2 0.992925 0.095358 0.422516 11.00000 -1.50000 H53C 2 0.980511 0.135398 0.461572 11.00000 -1.50000 AFIX 0 C54 1 0.878847 -0.053291 0.455265 11.00000 0.03121 0.03867 = 0.03320 0.00458 0.00092 0.01130 AFIX 137 H54A 2 0.917060 -0.043129 0.479550 11.00000 -1.50000 H54B 2 0.933171 -0.083266 0.440785 11.00000 -1.50000 H54C 2 0.813223 -0.099098 0.455601 11.00000 -1.50000 AFIX 0 HKLF 4 REM sharma29_a.res in P2(1)/c REM wR2 = 0.1106, GooF = S = 1.174, Restrained GooF = 1.174 for all data REM R1 = 0.0544 for 16638 Fo > 4sig(Fo) and 0.0642 for all 19071 data REM 584 parameters refined using 0 restraints END WGHT 0.0288 4.9868 REM Highest difference peak 0.689, deepest hole -0.638, 1-sigma level 0.066 Q1 1 0.1210 0.8422 0.3731 11.00000 0.05 0.69 Q2 1 0.1966 0.7543 0.3384 11.00000 0.05 0.66 Q3 1 0.0917 0.8725 0.3668 11.00000 0.05 0.57 Q4 1 -0.0556 0.8439 0.3306 11.00000 0.05 0.54 Q5 1 0.6459 0.2081 0.3858 11.00000 0.05 0.49 ; _shelx_res_checksum 65051 _olex2_date_sample_data_collection 2019-04-08 _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 ; _oxdiff_exptl_absorpt_empirical_full_max 1.208 _oxdiff_exptl_absorpt_empirical_full_min 0.841 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Ga1 Ga 0.05768(2) 0.81961(2) 0.36582(2) 0.02175(5) Uani 1 1 d . . . . . Cl1 Cl 0.14558(5) 0.96763(4) 0.37522(2) 0.04142(13) Uani 1 1 d . . . . . Cl2 Cl 0.05929(5) 0.73241(4) 0.41583(2) 0.03149(10) Uani 1 1 d . . . . . Cl3 Cl -0.12335(4) 0.84917(4) 0.34206(2) 0.03105(10) Uani 1 1 d . . . . . Cl4 Cl 0.14075(5) 0.72449(4) 0.32808(2) 0.03523(11) Uani 1 1 d . . . . . P1 P 0.67177(4) 0.27822(3) 0.39116(2) 0.01609(8) Uani 1 1 d . . . . . N1 N 0.72492(12) 0.51327(11) 0.37233(4) 0.0159(2) Uani 1 1 d . . . . . N2 N 0.85566(11) 0.47333(10) 0.33717(4) 0.0141(2) Uani 1 1 d . . . . . N3 N 0.58825(12) 0.09438(11) 0.40846(4) 0.0164(3) Uani 1 1 d . . . . . C1 C 0.76517(13) 0.43196(12) 0.35352(4) 0.0139(3) Uani 1 1 d . . . . . C2 C 0.79015(15) 0.60186(13) 0.36787(5) 0.0192(3) Uani 1 1 d . . . . . H2 H 0.780050 0.666698 0.377991 0.023 Uiso 1 1 calc R . . . . C3 C 0.87055(15) 0.57693(12) 0.34628(5) 0.0180(3) Uani 1 1 d . . . . . H3 H 0.926233 0.621436 0.338814 0.022 Uiso 1 1 calc R . . . . C4 C 0.62087(15) 0.52472(13) 0.39013(5) 0.0182(3) Uani 1 1 d . . . . . C5 C 0.51465(15) 0.54727(14) 0.36862(5) 0.0216(3) Uani 1 1 d . . . . . C6 C 0.42045(17) 0.57728(16) 0.38648(6) 0.0282(4) Uani 1 1 d . . . . . H6 H 0.348229 0.592001 0.373071 0.034 Uiso 1 1 calc R . . . . C7 C 0.43375(18) 0.58528(16) 0.42391(6) 0.0322(4) Uani 1 1 d . . . . . H7 H 0.370611 0.606079 0.435355 0.039 Uiso 1 1 calc R . . . . C8 C 0.53978(18) 0.56268(16) 0.44440(6) 0.0298(4) Uani 1 1 d . . . . . H8 H 0.546749 0.568031 0.469500 0.036 Uiso 1 1 calc R . . . . C9 C 0.63720(16) 0.53181(14) 0.42809(5) 0.0220(3) Uani 1 1 d . . . . . C10 C 0.50224(17) 0.54600(17) 0.32747(5) 0.0277(4) Uani 1 1 d . . . . . H10 H 0.566340 0.503992 0.320338 0.033 Uiso 1 1 calc R . . . . C11 C 0.5144(2) 0.6563(2) 0.31281(7) 0.0460(6) Uani 1 1 d . . . . . H11A H 0.453762 0.699631 0.320056 0.069 Uiso 1 1 calc GR . . . . H11B H 0.507399 0.654297 0.286841 0.069 Uiso 1 1 calc GR . . . . H11C H 0.589623 0.684077 0.322376 0.069 Uiso 1 1 calc GR . . . . C12 C 0.38648(19) 0.49763(18) 0.31028(6) 0.0357(5) Uani 1 1 d . . . . . H12A H 0.376441 0.431241 0.321174 0.054 Uiso 1 1 calc GR . . . . H12B H 0.387743 0.488923 0.284737 0.054 Uiso 1 1 calc GR . . . . H12C H 0.322663 0.542385 0.314169 0.054 Uiso 1 1 calc GR . . . . C13 C 0.75441(18) 0.51019(16) 0.45084(5) 0.0273(4) Uani 1 1 d . . . . . H13 H 0.806487 0.479703 0.434925 0.033 Uiso 1 1 calc R . . . . C14 C 0.8115(2) 0.61102(19) 0.46668(7) 0.0404(5) Uani 1 1 d . . . . . H14A H 0.819044 0.658958 0.447390 0.061 Uiso 1 1 calc GR . . . . H14B H 0.887696 0.595852 0.479455 0.061 Uiso 1 1 calc GR . . . . H14C H 0.763454 0.641221 0.483087 0.061 Uiso 1 1 calc GR . . . . C15 C 0.7428(2) 0.43222(19) 0.48129(6) 0.0384(5) Uani 1 1 d . . . . . H15A H 0.694709 0.461495 0.497866 0.058 Uiso 1 1 calc GR . . . . H15B H 0.819064 0.416847 0.493954 0.058 Uiso 1 1 calc GR . . . . H15C H 0.707297 0.369520 0.471092 0.058 Uiso 1 1 calc GR . . . . C16 C 0.93162(13) 0.42943(12) 0.31290(4) 0.0149(3) Uani 1 1 d . . . . . C17 C 0.90662(15) 0.45540(12) 0.27600(4) 0.0171(3) Uani 1 1 d . . . . . C18 C 0.98730(16) 0.42337(13) 0.25342(5) 0.0222(3) Uani 1 1 d . . . . . H18 H 0.972902 0.437722 0.228750 0.027 Uiso 1 1 calc R . . . . C19 C 1.08829(17) 0.37064(14) 0.26713(5) 0.0244(4) Uani 1 1 d . . . . . H19 H 1.141823 0.351447 0.251732 0.029 Uiso 1 1 calc R . . . . C20 C 1.11019(15) 0.34627(13) 0.30358(5) 0.0222(3) Uani 1 1 d . . . . . H20 H 1.177905 0.309870 0.312296 0.027 Uiso 1 1 calc R . . . . C21 C 1.03221(14) 0.37541(12) 0.32764(5) 0.0173(3) Uani 1 1 d . . . . . C22 C 0.79933(16) 0.51751(13) 0.26073(5) 0.0203(3) Uani 1 1 d . . . . . H22 H 0.742582 0.513949 0.278094 0.024 Uiso 1 1 calc R . . . . C23 C 0.83102(18) 0.63199(14) 0.25606(6) 0.0274(4) Uani 1 1 d . . . . . H23A H 0.867671 0.659171 0.278794 0.041 Uiso 1 1 calc GR . . . . H23B H 0.761111 0.670806 0.248091 0.041 Uiso 1 1 calc GR . . . . H23C H 0.884113 0.637601 0.238354 0.041 Uiso 1 1 calc GR . . . . C24 C 0.7399(2) 0.47543(15) 0.22430(5) 0.0293(4) Uani 1 1 d . . . . . H24A H 0.787829 0.490640 0.205754 0.044 Uiso 1 1 calc GR . . . . H24B H 0.664626 0.507654 0.218329 0.044 Uiso 1 1 calc GR . . . . H24C H 0.730182 0.401655 0.226006 0.044 Uiso 1 1 calc GR . . . . C25 C 1.05742(15) 0.35183(14) 0.36787(5) 0.0210(3) Uani 1 1 d . . . . . H25 H 0.982216 0.339459 0.376729 0.025 Uiso 1 1 calc R . . . . C26 C 1.11623(19) 0.44467(16) 0.38887(6) 0.0325(4) Uani 1 1 d . . . . . H26A H 1.191192 0.457448 0.381136 0.049 Uiso 1 1 calc GR . . . . H26B H 1.126648 0.429568 0.414346 0.049 Uiso 1 1 calc GR . . . . H26C H 1.067625 0.505048 0.384260 0.049 Uiso 1 1 calc GR . . . . C27 C 1.13333(17) 0.25490(16) 0.37628(6) 0.0285(4) Uani 1 1 d . . . . . H27A H 1.099355 0.197727 0.362013 0.043 Uiso 1 1 calc GR . . . . H27B H 1.137355 0.238247 0.401541 0.043 Uiso 1 1 calc GR . . . . H27C H 1.210848 0.267976 0.370543 0.043 Uiso 1 1 calc GR . . . . C28 C 0.72762(13) 0.32591(12) 0.35268(4) 0.0142(3) Uani 1 1 d . . . . . C29 C 0.76452(14) 0.25921(12) 0.32377(4) 0.0147(3) Uani 1 1 d . . . . . C30 C 0.72170(15) 0.27665(13) 0.28734(4) 0.0174(3) Uani 1 1 d . . . . . H30 H 0.667982 0.329717 0.281109 0.021 Uiso 1 1 calc R . . . . C31 C 0.75890(16) 0.21509(13) 0.26028(5) 0.0204(3) Uani 1 1 d . . . . . H31 H 0.729178 0.226775 0.236142 0.024 Uiso 1 1 calc R . . . . C32 C 0.84001(16) 0.13653(13) 0.26918(5) 0.0226(3) Uani 1 1 d . . . . . H32 H 0.865806 0.096403 0.251053 0.027 Uiso 1 1 calc R . . . . C33 C 0.88259(15) 0.11803(14) 0.30536(5) 0.0219(3) Uani 1 1 d . . . . . H33 H 0.936724 0.065201 0.311451 0.026 Uiso 1 1 calc R . . . . C34 C 0.84441(14) 0.17833(13) 0.33244(5) 0.0186(3) Uani 1 1 d . . . . . H34 H 0.872309 0.164732 0.356584 0.022 Uiso 1 1 calc R . . . . C35 C 0.60224(13) 0.15630(12) 0.38015(4) 0.0154(3) Uani 1 1 d . . . . . C36 C 0.53013(14) 0.11143(13) 0.34563(4) 0.0163(3) Uani 1 1 d . . . . . C37 C 0.45199(15) 0.03164(14) 0.36231(5) 0.0204(3) Uani 1 1 d . . . . . H37A H 0.379263 0.063774 0.366936 0.024 Uiso 1 1 calc R . . . . H37B H 0.433580 -0.026439 0.345949 0.024 Uiso 1 1 calc R . . . . C38 C 0.52250(15) -0.00508(14) 0.39775(5) 0.0202(3) Uani 1 1 d . . . . . C39 C 0.45581(15) 0.19850(14) 0.32604(5) 0.0218(3) Uani 1 1 d . . . . . H39A H 0.410666 0.231591 0.342665 0.033 Uiso 1 1 calc GR . . . . H39B H 0.403938 0.169733 0.306190 0.033 Uiso 1 1 calc GR . . . . H39C H 0.506327 0.248663 0.317000 0.033 Uiso 1 1 calc GR . . . . C40 C 0.60063(16) 0.05586(14) 0.31877(5) 0.0213(3) Uani 1 1 d . . . . . H40A H 0.631600 0.106443 0.303676 0.032 Uiso 1 1 calc GR . . . . H40B H 0.550101 0.009020 0.303931 0.032 Uiso 1 1 calc GR . . . . H40C H 0.663979 0.017621 0.332037 0.032 Uiso 1 1 calc GR . . . . C41 C 0.44485(18) -0.04105(16) 0.42551(5) 0.0284(4) Uani 1 1 d . . . . . H41A H 0.491174 -0.047077 0.448856 0.043 Uiso 1 1 calc GR . . . . H41B H 0.411199 -0.107305 0.418368 0.043 Uiso 1 1 calc GR . . . . H41C H 0.383365 0.008631 0.426766 0.043 Uiso 1 1 calc GR . . . . C42 C 0.60918(18) -0.09317(15) 0.39330(6) 0.0284(4) Uani 1 1 d . . . . . H42A H 0.666607 -0.069494 0.378720 0.043 Uiso 1 1 calc GR . . . . H42B H 0.567581 -0.151339 0.381708 0.043 Uiso 1 1 calc GR . . . . H42C H 0.647561 -0.113783 0.416703 0.043 Uiso 1 1 calc GR . . . . C43 C 0.62953(14) 0.12157(13) 0.44571(4) 0.0173(3) Uani 1 1 d . . . . . C44 C 0.55048(14) 0.17066(13) 0.46607(4) 0.0188(3) Uani 1 1 d . . . . . C45 C 0.59103(16) 0.19625(14) 0.50202(5) 0.0221(3) Uani 1 1 d . . . . . H45 H 0.540619 0.228787 0.516008 0.027 Uiso 1 1 calc R . . . . C46 C 0.70489(16) 0.17414(15) 0.51728(5) 0.0245(4) Uani 1 1 d . . . . . H46 H 0.729917 0.190983 0.541360 0.029 Uiso 1 1 calc R . . . . C47 C 0.78114(16) 0.12704(15) 0.49666(5) 0.0236(3) Uani 1 1 d . . . . . H47 H 0.857497 0.112977 0.507104 0.028 Uiso 1 1 calc R . . . . C48 C 0.74615(15) 0.10003(14) 0.46046(4) 0.0197(3) Uani 1 1 d . . . . . C49 C 0.42593(15) 0.20172(14) 0.45070(5) 0.0212(3) Uani 1 1 d . . . . . H49 H 0.407585 0.170158 0.426663 0.025 Uiso 1 1 calc R . . . . C50 C 0.41642(17) 0.31965(15) 0.44630(5) 0.0265(4) Uani 1 1 d . . . . . H50A H 0.437858 0.352334 0.469413 0.040 Uiso 1 1 calc GR . . . . H50B H 0.337247 0.337960 0.436992 0.040 Uiso 1 1 calc GR . . . . H50C H 0.468176 0.342647 0.429750 0.040 Uiso 1 1 calc GR . . . . C51 C 0.33578(17) 0.16191(18) 0.47464(5) 0.0301(4) Uani 1 1 d . . . . . H51A H 0.347115 0.088864 0.478873 0.045 Uiso 1 1 calc GR . . . . H51B H 0.257921 0.173962 0.462553 0.045 Uiso 1 1 calc GR . . . . H51C H 0.346238 0.198133 0.497372 0.045 Uiso 1 1 calc GR . . . . C52 C 0.83575(16) 0.05179(16) 0.43903(5) 0.0252(4) Uani 1 1 d . . . . . H52 H 0.797923 0.039915 0.414186 0.030 Uiso 1 1 calc R . . . . C53 C 0.94017(17) 0.12524(19) 0.43755(6) 0.0330(4) Uani 1 1 d . . . . . H53A H 0.912321 0.190845 0.427627 0.049 Uiso 1 1 calc GR . . . . H53B H 0.992925 0.095358 0.422516 0.049 Uiso 1 1 calc GR . . . . H53C H 0.980511 0.135398 0.461572 0.049 Uiso 1 1 calc GR . . . . C54 C 0.87885(19) -0.05329(18) 0.45526(6) 0.0347(5) Uani 1 1 d . . . . . H54A H 0.917060 -0.043129 0.479550 0.052 Uiso 1 1 calc GR . . . . H54B H 0.933171 -0.083266 0.440785 0.052 Uiso 1 1 calc GR . . . . H54C H 0.813223 -0.099098 0.455601 0.052 Uiso 1 1 calc GR . . . . 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 Ga1 0.02084(9) 0.01906(9) 0.02606(10) -0.00101(7) 0.00578(7) -0.00263(7) Cl1 0.0354(3) 0.0275(2) 0.0617(4) -0.0031(2) 0.0077(3) -0.0146(2) Cl2 0.0408(3) 0.0303(2) 0.0223(2) -0.00060(17) 0.00021(18) -0.0081(2) Cl3 0.0231(2) 0.0227(2) 0.0466(3) 0.00534(19) 0.00224(19) 0.00097(16) Cl4 0.0384(3) 0.0335(2) 0.0379(3) 0.0006(2) 0.0199(2) 0.0064(2) P1 0.01852(19) 0.01747(18) 0.01267(17) 0.00029(14) 0.00348(14) -0.00412(15) N1 0.0168(6) 0.0159(6) 0.0157(6) -0.0019(5) 0.0045(5) -0.0022(5) N2 0.0143(6) 0.0133(6) 0.0151(6) -0.0004(5) 0.0039(5) -0.0025(5) N3 0.0177(6) 0.0185(6) 0.0130(6) 0.0029(5) 0.0016(5) -0.0036(5) C1 0.0136(6) 0.0166(7) 0.0116(6) 0.0006(5) 0.0019(5) -0.0012(5) C2 0.0219(8) 0.0147(7) 0.0219(8) -0.0028(6) 0.0059(6) -0.0032(6) C3 0.0194(7) 0.0140(7) 0.0212(7) -0.0013(6) 0.0053(6) -0.0046(6) C4 0.0188(7) 0.0177(7) 0.0196(7) -0.0022(6) 0.0080(6) -0.0013(6) C5 0.0195(8) 0.0212(8) 0.0251(8) -0.0011(6) 0.0064(6) -0.0006(6) C6 0.0200(8) 0.0282(9) 0.0379(11) -0.0011(8) 0.0096(7) 0.0011(7) C7 0.0296(10) 0.0307(10) 0.0407(11) -0.0070(8) 0.0203(9) 0.0002(8) C8 0.0353(10) 0.0320(10) 0.0255(9) -0.0077(8) 0.0163(8) -0.0022(8) C9 0.0257(8) 0.0217(8) 0.0200(8) -0.0043(6) 0.0081(6) -0.0037(7) C10 0.0208(8) 0.0373(10) 0.0241(9) 0.0010(8) -0.0001(7) 0.0040(7) C11 0.0441(13) 0.0554(15) 0.0353(12) 0.0169(11) -0.0056(10) -0.0145(11) C12 0.0294(10) 0.0365(11) 0.0383(12) -0.0030(9) -0.0063(9) 0.0027(9) C13 0.0303(9) 0.0340(10) 0.0182(8) -0.0040(7) 0.0052(7) -0.0031(8) C14 0.0421(12) 0.0438(13) 0.0345(11) -0.0083(10) 0.0026(10) -0.0141(10) C15 0.0466(13) 0.0455(13) 0.0217(9) 0.0037(9) -0.0011(9) -0.0081(10) C16 0.0148(7) 0.0141(6) 0.0166(7) 0.0002(5) 0.0057(5) -0.0022(5) C17 0.0211(7) 0.0146(7) 0.0163(7) 0.0008(5) 0.0049(6) -0.0029(6) C18 0.0313(9) 0.0175(7) 0.0199(8) 0.0007(6) 0.0115(7) -0.0044(7) C19 0.0274(9) 0.0186(8) 0.0305(9) -0.0017(7) 0.0165(7) -0.0026(7) C20 0.0184(7) 0.0174(7) 0.0322(9) 0.0011(6) 0.0089(7) 0.0008(6) C21 0.0156(7) 0.0153(7) 0.0213(7) 0.0013(6) 0.0038(6) -0.0022(5) C22 0.0244(8) 0.0179(7) 0.0181(7) 0.0034(6) 0.0016(6) -0.0006(6) C23 0.0336(10) 0.0180(8) 0.0291(9) 0.0039(7) -0.0008(8) -0.0004(7) C24 0.0431(11) 0.0226(8) 0.0195(8) 0.0036(7) -0.0065(8) -0.0018(8) C25 0.0180(7) 0.0217(8) 0.0228(8) 0.0026(6) 0.0006(6) 0.0001(6) C26 0.0359(11) 0.0287(10) 0.0294(10) -0.0015(8) -0.0086(8) -0.0013(8) C27 0.0225(9) 0.0274(9) 0.0340(10) 0.0075(8) -0.0019(7) 0.0021(7) C28 0.0136(6) 0.0155(7) 0.0136(6) 0.0002(5) 0.0019(5) -0.0019(5) C29 0.0155(7) 0.0141(6) 0.0153(7) -0.0008(5) 0.0044(5) -0.0039(5) C30 0.0211(7) 0.0151(7) 0.0164(7) 0.0004(5) 0.0045(6) -0.0024(6) C31 0.0274(8) 0.0178(7) 0.0171(7) -0.0005(6) 0.0071(6) -0.0040(6) C32 0.0282(9) 0.0184(8) 0.0233(8) -0.0048(6) 0.0116(7) -0.0030(6) C33 0.0208(8) 0.0185(7) 0.0273(9) -0.0014(6) 0.0067(7) 0.0003(6) C34 0.0180(7) 0.0172(7) 0.0206(7) 0.0004(6) 0.0025(6) -0.0020(6) C35 0.0146(7) 0.0187(7) 0.0128(6) 0.0027(5) 0.0016(5) -0.0010(5) C36 0.0165(7) 0.0189(7) 0.0133(6) 0.0017(5) 0.0013(5) -0.0050(6) C37 0.0190(7) 0.0248(8) 0.0171(7) 0.0021(6) 0.0015(6) -0.0097(6) C38 0.0221(8) 0.0224(8) 0.0157(7) 0.0038(6) 0.0007(6) -0.0080(6) C39 0.0203(8) 0.0244(8) 0.0194(8) 0.0037(6) -0.0022(6) -0.0030(6) C40 0.0245(8) 0.0209(8) 0.0192(8) -0.0032(6) 0.0064(6) -0.0084(6) C41 0.0356(10) 0.0306(10) 0.0194(8) 0.0047(7) 0.0050(7) -0.0160(8) C42 0.0353(10) 0.0210(8) 0.0275(9) 0.0040(7) -0.0007(8) -0.0033(7) C43 0.0182(7) 0.0216(7) 0.0120(6) 0.0038(6) 0.0014(5) -0.0045(6) C44 0.0182(7) 0.0230(8) 0.0152(7) 0.0044(6) 0.0026(6) -0.0037(6) C45 0.0248(8) 0.0274(9) 0.0149(7) 0.0014(6) 0.0051(6) -0.0028(7) C46 0.0266(9) 0.0330(9) 0.0135(7) 0.0040(7) 0.0006(6) -0.0063(7) C47 0.0190(8) 0.0330(9) 0.0177(8) 0.0062(7) -0.0013(6) -0.0037(7) C48 0.0182(7) 0.0254(8) 0.0152(7) 0.0051(6) 0.0015(6) -0.0024(6) C49 0.0174(7) 0.0283(9) 0.0182(7) 0.0034(6) 0.0038(6) -0.0007(6) C50 0.0245(9) 0.0302(9) 0.0251(9) 0.0026(7) 0.0038(7) 0.0040(7) C51 0.0212(8) 0.0441(12) 0.0265(9) 0.0041(8) 0.0084(7) -0.0019(8) C52 0.0188(8) 0.0367(10) 0.0200(8) 0.0047(7) 0.0019(6) 0.0028(7) C53 0.0195(8) 0.0527(13) 0.0269(9) 0.0081(9) 0.0042(7) -0.0010(8) C54 0.0312(10) 0.0387(11) 0.0332(11) 0.0046(9) 0.0009(8) 0.0113(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 -4 -16 -16 0.1601 -6 4 49 0.1651 5 -2 -1 0.1254 1 5 5 0.1595 0 1 -1 0.0842 4 -9 43 0.1251 -1 0 1 0.1030 4 -15 -30 0.1378 1 0 -1 0.1471 0 1 2 0.1608 5 -14 27 0.1054 -4 -1 -48 0.2102 -1 -1 2 0.1210 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 Cl1 Ga1 Cl2 111.52(2) . . ? Cl1 Ga1 Cl3 108.16(2) . . ? Cl1 Ga1 Cl4 111.29(2) . . ? Cl2 Ga1 Cl3 109.57(2) . . ? Cl2 Ga1 Cl4 107.94(2) . . ? Cl4 Ga1 Cl3 108.30(2) . . ? C28 P1 C35 108.79(7) . . ? C1 N1 C2 109.92(13) . . ? C1 N1 C4 131.69(13) . . ? C2 N1 C4 117.62(13) . . ? C1 N2 C16 132.51(13) . . ? C3 N2 C1 109.88(13) . . ? C3 N2 C16 117.60(13) . . ? C35 N3 C38 113.73(13) . . ? C35 N3 C43 123.20(14) . . ? C43 N3 C38 123.06(13) . . ? N1 C1 N2 104.85(13) . . ? N1 C1 C28 128.06(14) . . ? N2 C1 C28 126.98(14) . . ? N1 C2 H2 126.2 . . ? C3 C2 N1 107.59(14) . . ? C3 C2 H2 126.2 . . ? N2 C3 H3 126.1 . . ? C2 C3 N2 107.76(14) . . ? C2 C3 H3 126.1 . . ? C5 C4 N1 118.09(15) . . ? C5 C4 C9 123.45(15) . . ? C9 C4 N1 117.34(15) . . ? C4 C5 C6 117.29(17) . . ? C4 C5 C10 122.09(15) . . ? C6 C5 C10 120.52(17) . . ? C5 C6 H6 119.7 . . ? C7 C6 C5 120.68(19) . . ? C7 C6 H6 119.7 . . ? C6 C7 H7 119.7 . . ? C8 C7 C6 120.67(17) . . ? C8 C7 H7 119.7 . . ? C7 C8 H8 119.4 . . ? C7 C8 C9 121.29(18) . . ? C9 C8 H8 119.4 . . ? C4 C9 C13 122.56(15) . . ? C8 C9 C4 116.60(17) . . ? C8 C9 C13 120.82(17) . . ? C5 C10 H10 107.9 . . ? C5 C10 C11 110.34(18) . . ? C5 C10 C12 112.60(17) . . ? C11 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C12 C10 C11 110.11(18) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13 107.8 . . ? C9 C13 C14 111.17(18) . . ? C9 C13 C15 111.90(17) . . ? C14 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C15 C13 C14 110.18(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 N2 116.98(14) . . ? C21 C16 N2 119.01(14) . . ? C21 C16 C17 123.52(14) . . ? C16 C17 C22 122.78(14) . . ? C18 C17 C16 116.93(16) . . ? C18 C17 C22 120.28(15) . . ? C17 C18 H18 119.4 . . ? C19 C18 C17 121.12(17) . . ? C19 C18 H18 119.4 . . ? C18 C19 H19 119.8 . . ? C20 C19 C18 120.46(16) . . ? C20 C19 H19 119.8 . . ? C19 C20 H20 119.4 . . ? C19 C20 C21 121.24(16) . . ? C21 C20 H20 119.4 . . ? C16 C21 C20 116.73(16) . . ? C16 C21 C25 121.71(14) . . ? C20 C21 C25 121.55(15) . . ? C17 C22 H22 108.0 . . ? C17 C22 C23 110.82(15) . . ? C17 C22 C24 112.89(15) . . ? C23 C22 H22 108.0 . . ? C24 C22 H22 108.0 . . ? C24 C22 C23 108.88(15) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25 107.7 . . ? C21 C25 C26 111.07(15) . . ? C21 C25 C27 113.13(15) . . ? C26 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C27 C25 C26 109.29(15) . . ? 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 . . ? C1 C28 P1 117.26(11) . . ? C1 C28 C29 116.95(13) . . ? C29 C28 P1 124.11(11) . . ? C30 C29 C28 120.87(14) . . ? C30 C29 C34 118.62(15) . . ? C34 C29 C28 120.50(14) . . ? C29 C30 H30 119.8 . . ? C31 C30 C29 120.50(16) . . ? C31 C30 H30 119.8 . . ? C30 C31 H31 119.8 . . ? C32 C31 C30 120.31(16) . . ? C32 C31 H31 119.8 . . ? C31 C32 H32 120.2 . . ? C31 C32 C33 119.66(16) . . ? C33 C32 H32 120.2 . . ? C32 C33 H33 119.9 . . ? C34 C33 C32 120.15(16) . . ? C34 C33 H33 119.9 . . ? C29 C34 H34 119.6 . . ? C33 C34 C29 120.74(16) . . ? C33 C34 H34 119.6 . . ? N3 C35 P1 115.96(12) . . ? N3 C35 C36 108.77(13) . . ? C36 C35 P1 133.95(11) . . ? C35 C36 C37 100.99(12) . . ? C35 C36 C40 116.18(13) . . ? C39 C36 C35 108.97(13) . . ? C39 C36 C37 111.03(14) . . ? C39 C36 C40 109.78(14) . . ? C40 C36 C37 109.61(14) . . ? C36 C37 H37A 110.5 . . ? C36 C37 H37B 110.5 . . ? H37A C37 H37B 108.6 . . ? C38 C37 C36 106.36(13) . . ? C38 C37 H37A 110.5 . . ? C38 C37 H37B 110.5 . . ? N3 C38 C37 98.89(13) . . ? N3 C38 C41 113.31(14) . . ? N3 C38 C42 110.17(14) . . ? C37 C38 C42 114.41(15) . . ? C41 C38 C37 112.79(15) . . ? C41 C38 C42 107.28(15) . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 N3 118.12(14) . . ? C48 C43 N3 119.94(15) . . ? C48 C43 C44 121.93(15) . . ? C43 C44 C49 123.93(15) . . ? C45 C44 C43 117.68(15) . . ? C45 C44 C49 118.32(15) . . ? C44 C45 H45 119.3 . . ? C46 C45 C44 121.34(17) . . ? C46 C45 H45 119.3 . . ? C45 C46 H46 120.0 . . ? C47 C46 C45 119.92(16) . . ? C47 C46 H46 120.0 . . ? C46 C47 H47 119.2 . . ? C46 C47 C48 121.52(16) . . ? C48 C47 H47 119.2 . . ? C43 C48 C52 123.69(15) . . ? C47 C48 C43 117.59(16) . . ? C47 C48 C52 118.71(15) . . ? C44 C49 H49 108.1 . . ? C44 C49 C50 110.55(15) . . ? C44 C49 C51 111.56(15) . . ? C50 C49 H49 108.1 . . ? C50 C49 C51 110.34(15) . . ? C51 C49 H49 108.1 . . ? 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 . . ? C48 C52 H52 108.2 . . ? C48 C52 C53 110.90(17) . . ? C48 C52 C54 111.07(15) . . ? C53 C52 H52 108.2 . . ? C53 C52 C54 110.09(16) . . ? C54 C52 H52 108.2 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 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 Ga1 Cl1 2.1648(5) . ? Ga1 Cl2 2.1729(5) . ? Ga1 Cl3 2.1853(5) . ? Ga1 Cl4 2.1800(5) . ? P1 C28 1.7581(15) . ? P1 C35 1.7852(17) . ? N1 C1 1.375(2) . ? N1 C2 1.388(2) . ? N1 C4 1.452(2) . ? N2 C1 1.3823(19) . ? N2 C3 1.382(2) . ? N2 C16 1.4539(19) . ? N3 C35 1.349(2) . ? N3 C38 1.514(2) . ? N3 C43 1.447(2) . ? C1 C28 1.432(2) . ? C2 H2 0.9300 . ? C2 C3 1.344(2) . ? C3 H3 0.9300 . ? C4 C5 1.399(2) . ? C4 C9 1.404(2) . ? C5 C6 1.401(2) . ? C5 C10 1.520(3) . ? C6 H6 0.9300 . ? C6 C7 1.386(3) . ? C7 H7 0.9300 . ? C7 C8 1.381(3) . ? C8 H8 0.9300 . ? C8 C9 1.403(2) . ? C9 C13 1.519(3) . ? C10 H10 0.9800 . ? C10 C11 1.536(3) . ? C10 C12 1.531(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13 0.9800 . ? C13 C14 1.537(3) . ? C13 C15 1.534(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.406(2) . ? C16 C21 1.398(2) . ? C17 C18 1.396(2) . ? C17 C22 1.517(2) . ? C18 H18 0.9300 . ? C18 C19 1.384(3) . ? C19 H19 0.9300 . ? C19 C20 1.383(3) . ? C20 H20 0.9300 . ? C20 C21 1.402(2) . ? C21 C25 1.518(2) . ? C22 H22 0.9800 . ? C22 C23 1.535(2) . ? C22 C24 1.534(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25 0.9800 . ? C25 C26 1.536(3) . ? C25 C27 1.532(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.484(2) . ? C29 C30 1.398(2) . ? C29 C34 1.398(2) . ? C30 H30 0.9300 . ? C30 C31 1.394(2) . ? C31 H31 0.9300 . ? C31 C32 1.387(3) . ? C32 H32 0.9300 . ? C32 C33 1.391(3) . ? C33 H33 0.9300 . ? C33 C34 1.390(2) . ? C34 H34 0.9300 . ? C35 C36 1.546(2) . ? C36 C37 1.550(2) . ? C36 C39 1.534(2) . ? C36 C40 1.546(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 C38 1.528(2) . ? C38 C41 1.527(2) . ? C38 C42 1.535(3) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.410(2) . ? C43 C48 1.408(2) . ? C44 C45 1.397(2) . ? C44 C49 1.524(2) . ? C45 H45 0.9300 . ? C45 C46 1.386(3) . ? C46 H46 0.9300 . ? C46 C47 1.382(3) . ? C47 H47 0.9300 . ? C47 C48 1.398(2) . ? C48 C52 1.519(2) . ? C49 H49 0.9800 . ? C49 C50 1.530(3) . ? C49 C51 1.544(2) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52 0.9800 . ? C52 C53 1.537(3) . ? C52 C54 1.537(3) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? 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 P1 C28 C29 C30 128.18(14) . . . . ? P1 C28 C29 C34 -52.7(2) . . . . ? P1 C35 C36 C37 -152.31(14) . . . . ? P1 C35 C36 C39 -35.4(2) . . . . ? P1 C35 C36 C40 89.23(19) . . . . ? N1 C1 C28 P1 -28.2(2) . . . . ? N1 C1 C28 C29 165.91(15) . . . . ? N1 C2 C3 N2 0.1(2) . . . . ? N1 C4 C5 C6 -168.24(16) . . . . ? N1 C4 C5 C10 8.1(2) . . . . ? N1 C4 C9 C8 168.08(16) . . . . ? N1 C4 C9 C13 -10.4(2) . . . . ? N2 C1 C28 P1 147.36(14) . . . . ? N2 C1 C28 C29 -18.5(2) . . . . ? N2 C16 C17 C18 172.71(14) . . . . ? N2 C16 C17 C22 -5.8(2) . . . . ? N2 C16 C21 C20 -172.02(14) . . . . ? N2 C16 C21 C25 6.5(2) . . . . ? N3 C35 C36 C37 13.58(17) . . . . ? N3 C35 C36 C39 130.53(14) . . . . ? N3 C35 C36 C40 -104.88(16) . . . . ? N3 C43 C44 C45 179.78(15) . . . . ? N3 C43 C44 C49 -3.2(2) . . . . ? N3 C43 C48 C47 -179.42(15) . . . . ? N3 C43 C48 C52 2.1(3) . . . . ? C1 N1 C2 C3 0.3(2) . . . . ? C1 N1 C4 C5 -79.7(2) . . . . ? C1 N1 C4 C9 112.0(2) . . . . ? C1 N2 C3 C2 -0.55(19) . . . . ? C1 N2 C16 C17 103.0(2) . . . . ? C1 N2 C16 C21 -84.7(2) . . . . ? C1 C28 C29 C30 -67.0(2) . . . . ? C1 C28 C29 C34 112.06(17) . . . . ? C2 N1 C1 N2 -0.63(18) . . . . ? C2 N1 C1 C28 175.73(16) . . . . ? C2 N1 C4 C5 89.11(19) . . . . ? C2 N1 C4 C9 -79.2(2) . . . . ? C3 N2 C1 N1 0.72(17) . . . . ? C3 N2 C1 C28 -175.69(15) . . . . ? C3 N2 C16 C17 -75.51(19) . . . . ? C3 N2 C16 C21 96.71(18) . . . . ? C4 N1 C1 N2 168.81(16) . . . . ? C4 N1 C1 C28 -14.8(3) . . . . ? C4 N1 C2 C3 -170.80(15) . . . . ? C4 C5 C6 C7 0.8(3) . . . . ? C4 C5 C10 C11 -97.0(2) . . . . ? C4 C5 C10 C12 139.55(18) . . . . ? C4 C9 C13 C14 107.7(2) . . . . ? C4 C9 C13 C15 -128.60(19) . . . . ? C5 C4 C9 C8 0.4(3) . . . . ? C5 C4 C9 C13 -178.04(17) . . . . ? C5 C6 C7 C8 -0.7(3) . . . . ? C6 C5 C10 C11 79.3(2) . . . . ? C6 C5 C10 C12 -44.2(3) . . . . ? C6 C7 C8 C9 0.5(3) . . . . ? C7 C8 C9 C4 -0.3(3) . . . . ? C7 C8 C9 C13 178.20(19) . . . . ? C8 C9 C13 C14 -70.7(2) . . . . ? C8 C9 C13 C15 53.0(2) . . . . ? C9 C4 C5 C6 -0.7(3) . . . . ? C9 C4 C5 C10 175.70(17) . . . . ? C10 C5 C6 C7 -175.62(19) . . . . ? C16 N2 C1 N1 -177.92(15) . . . . ? C16 N2 C1 C28 5.7(3) . . . . ? C16 N2 C3 C2 178.32(14) . . . . ? C16 C17 C18 C19 -1.5(2) . . . . ? C16 C17 C22 C23 99.27(19) . . . . ? C16 C17 C22 C24 -138.29(17) . . . . ? C16 C21 C25 C26 -83.4(2) . . . . ? C16 C21 C25 C27 153.27(16) . . . . ? C17 C16 C21 C20 -0.3(2) . . . . ? C17 C16 C21 C25 178.14(15) . . . . ? C17 C18 C19 C20 1.5(3) . . . . ? C18 C17 C22 C23 -79.2(2) . . . . ? C18 C17 C22 C24 43.2(2) . . . . ? C18 C19 C20 C21 -1.0(3) . . . . ? C19 C20 C21 C16 0.4(2) . . . . ? C19 C20 C21 C25 -178.11(16) . . . . ? C20 C21 C25 C26 95.0(2) . . . . ? C20 C21 C25 C27 -28.3(2) . . . . ? C21 C16 C17 C18 0.9(2) . . . . ? C21 C16 C17 C22 -177.66(15) . . . . ? C22 C17 C18 C19 177.12(16) . . . . ? C28 P1 C35 N3 159.59(12) . . . . ? C28 P1 C35 C36 -35.29(18) . . . . ? C28 C29 C30 C31 178.52(15) . . . . ? C28 C29 C34 C33 -177.61(15) . . . . ? C29 C30 C31 C32 -0.8(2) . . . . ? C30 C29 C34 C33 1.5(2) . . . . ? C30 C31 C32 C33 1.2(3) . . . . ? C31 C32 C33 C34 -0.3(3) . . . . ? C32 C33 C34 C29 -1.1(3) . . . . ? C34 C29 C30 C31 -0.6(2) . . . . ? C35 P1 C28 C1 167.46(12) . . . . ? C35 P1 C28 C29 -27.79(15) . . . . ? C35 N3 C38 C37 -25.75(18) . . . . ? C35 N3 C38 C41 -145.37(16) . . . . ? C35 N3 C38 C42 94.45(17) . . . . ? C35 N3 C43 C44 93.93(19) . . . . ? C35 N3 C43 C48 -85.3(2) . . . . ? C35 C36 C37 C38 -29.52(17) . . . . ? C36 C37 C38 N3 32.92(16) . . . . ? C36 C37 C38 C41 152.93(15) . . . . ? C36 C37 C38 C42 -84.09(17) . . . . ? C38 N3 C35 P1 176.57(11) . . . . ? C38 N3 C35 C36 7.83(18) . . . . ? C38 N3 C43 C44 -84.4(2) . . . . ? C38 N3 C43 C48 96.37(19) . . . . ? C39 C36 C37 C38 -144.94(15) . . . . ? C40 C36 C37 C38 93.60(16) . . . . ? C43 N3 C35 P1 -1.9(2) . . . . ? C43 N3 C35 C36 -170.66(14) . . . . ? C43 N3 C38 C37 152.74(15) . . . . ? C43 N3 C38 C41 33.1(2) . . . . ? C43 N3 C38 C42 -87.06(18) . . . . ? C43 C44 C45 C46 -0.1(3) . . . . ? C43 C44 C49 C50 -107.51(19) . . . . ? C43 C44 C49 C51 129.32(18) . . . . ? C43 C48 C52 C53 118.96(19) . . . . ? C43 C48 C52 C54 -118.28(19) . . . . ? C44 C43 C48 C47 1.4(2) . . . . ? C44 C43 C48 C52 -177.12(16) . . . . ? C44 C45 C46 C47 0.8(3) . . . . ? C45 C44 C49 C50 69.5(2) . . . . ? C45 C44 C49 C51 -53.6(2) . . . . ? C45 C46 C47 C48 -0.4(3) . . . . ? C46 C47 C48 C43 -0.6(3) . . . . ? C46 C47 C48 C52 177.95(17) . . . . ? C47 C48 C52 C53 -59.5(2) . . . . ? C47 C48 C52 C54 63.2(2) . . . . ? C48 C43 C44 C45 -1.0(2) . . . . ? C48 C43 C44 C49 176.02(16) . . . . ? C49 C44 C45 C46 -177.33(16) . . . . ? 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 -4.0774 -16.4149 -16.1841 0.1213 0.1267 -0.9845 -6.3382 4.3142 49.0311 0.8194 -0.2901 0.4944 5.0101 -2.0128 -1.0026 -0.0522 0.3239 0.0202 1.0092 5.0136 5.0644 -0.0315 -0.0514 0.2962 0.0014 1.0042 -0.9944 -0.0364 -0.0283 0.0360 3.7160 -8.5193 42.7814 0.8197 0.5639 0.1007 -1.0026 0.0006 0.9996 0.0317 -0.0521 -0.0148 3.6062 -14.7310 -29.6881 -0.2514 0.4640 -0.8494 1.0026 -0.0006 -0.9996 -0.0317 0.0521 0.0148 0.0013 1.0023 2.0155 0.0133 -0.0179 0.0637 4.5846 -14.1188 27.2715 0.6620 0.6980 -0.2732 -4.3572 -0.6396 -48.1927 -0.7170 -0.3904 -0.5775 -1.0039 -1.0036 1.9941 0.0681 -0.0238 -0.0507