#------------------------------------------------------------------------------ #$Date: 2020-03-04 09:46:50 +0200 (Wed, 04 Mar 2020) $ #$Revision: 248752 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557450.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_1557450 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 'Cl7 Ga2, Cl4 Ga, 2(C H2 Cl2), C57 H76 N3 P' _chemical_formula_sum 'C59 H80 Cl15 Ga3 N3 P' _chemical_formula_weight 1603.14 _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 2019-08-27 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739) ; _audit_update_record ; 2019-09-05 deposited with the CCDC. 2020-01-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.5840(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.16275(15) _cell_length_b 13.46701(10) _cell_length_c 28.2924(2) _cell_measurement_reflns_used 76826 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 76.2540 _cell_measurement_theta_min 3.0950 _cell_volume 7277.92(9) _computing_cell_refinement 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.58a (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 100.0(1) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3114 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _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 -64.00 30.00 1.00 2.50 -- -38.50 57.00-120.00 94 2 \w -59.00 33.00 1.00 2.50 -- -38.50 38.00 60.00 92 3 \w 12.00 42.00 1.00 2.50 -- 42.70 80.00 31.89 30 4 \w 27.00 97.00 1.00 2.50 -- 42.70-125.00 90.00 70 5 \w 22.00 114.00 1.00 2.50 -- 42.70 38.00 -90.00 92 6 \w -28.00 63.00 1.00 2.50 -- 42.70 -38.00 60.00 91 7 \w 22.00 114.00 1.00 2.50 -- 42.70 38.00 120.00 92 8 \w 6.00 81.00 1.00 2.50 -- 42.70 -99.00 -60.00 75 9 \w 11.00 42.00 1.00 2.50 -- 42.70 81.00-144.67 31 10 \w 12.00 42.00 1.00 2.50 -- 42.70 78.00 69.28 30 11 \w 16.00 111.00 1.00 2.50 -- 42.70 63.00 147.36 95 12 \w 12.00 42.00 1.00 2.50 -- 42.70 80.00 -73.76 30 13 \w 13.00 42.00 1.00 2.50 -- 42.70 77.00-102.84 29 14 \w 11.00 42.00 1.00 2.50 -- 42.70 82.00 104.52 31 15 \w 22.00 114.00 1.00 2.50 -- 42.70 38.00 -30.00 92 16 \w 18.00 111.00 1.00 2.50 -- 42.70 57.00 0.00 93 17 \w 12.00 42.00 1.00 2.50 -- 42.70 79.00 -16.56 30 18 \w 11.00 42.00 1.00 2.50 -- 42.70 81.00 153.00 31 19 \w 85.00 178.00 1.00 10.00 -- 111.00 60.00-138.31 93 20 \w 86.00 178.00 1.00 10.00 -- 111.00 57.00 -98.41 92 21 \w 85.00 156.00 1.00 10.00 -- 111.00 61.00 -49.16 71 22 \w 82.00 108.00 1.00 10.00 -- 111.00 72.00 55.67 26 23 \w 86.00 162.00 1.00 10.00 -- 111.00 55.00 86.24 76 24 \w 82.00 109.00 1.00 10.00 -- 111.00 72.00 -85.23 27 25 \w 146.00 173.00 1.00 10.00 -- 111.00 72.00 55.67 27 26 \w 82.00 176.00 1.00 10.00 -- 111.00 72.00 36.97 94 27 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 -39.74 27 28 \w 82.00 109.00 1.00 10.00 -- 111.00 72.00 -30.57 27 29 \w 83.00 109.00 1.00 10.00 -- 111.00 68.00 -13.20 26 30 \w 44.00 136.00 1.00 10.00 -- 111.00 -61.00 0.00 92 31 \w 86.00 159.00 1.00 10.00 -- 111.00 61.00 -83.73 73 32 \w 85.00 158.00 1.00 10.00 -- 111.00 62.00 -66.44 73 33 \w 87.00 114.00 1.00 10.00 -- 111.00 53.00-152.47 27 34 \w 144.00 177.00 1.00 10.00 -- 111.00 57.00-122.94 33 35 \w 86.00 112.00 1.00 10.00 -- 111.00 57.00-122.94 26 36 \w 88.00 170.00 1.00 10.00 -- 111.00 47.00 30.60 82 37 \w 120.00 176.00 1.00 10.00 -- 111.00 58.00 137.18 56 38 \w 86.00 112.00 1.00 10.00 -- 111.00 58.00 137.18 26 39 \w 87.00 178.00 1.00 10.00 -- 111.00 50.00 154.95 91 40 \w 83.00 176.00 1.00 10.00 -- 111.00 67.00 170.59 93 41 \w 31.00 107.00 1.00 10.00 -- 111.00 -94.00-180.00 76 42 \w 31.00 105.00 1.00 10.00 -- 111.00 -94.00 0.00 74 43 \w 83.00 109.00 1.00 10.00 -- 111.00 69.00 -64.25 26 44 \w 61.00 107.00 1.00 10.00 -- 111.00-104.00 -34.71 46 45 \w 81.00 108.00 1.00 10.00 -- 111.00-103.00 -95.02 27 46 \w 123.00 178.00 1.00 10.00 -- 111.00 65.00 1.26 55 47 \w 82.00 109.00 1.00 10.00 -- 111.00 73.00 20.39 27 48 \w 83.00 113.00 1.00 10.00 -- 111.00 68.00 157.81 30 49 \w 85.00 177.00 1.00 10.00 -- 111.00 61.00-150.00 92 50 \w 43.00 134.00 1.00 10.00 -- 111.00 -61.00-180.00 91 51 \w 85.00 111.00 1.00 10.00 -- 111.00 61.00 90.00 26 52 \w 84.00 110.00 1.00 10.00 -- 111.00 64.00 24.00 26 53 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 -90.00 27 54 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 60.00 27 55 \w 83.00 109.00 1.00 10.00 -- 111.00-110.00 80.98 26 56 \w 86.00 113.00 1.00 10.00 -- 111.00 61.00-120.00 27 57 \w 152.00 178.00 1.00 10.00 -- 111.00 61.00-120.00 26 58 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 150.00 27 59 \w 84.00 110.00 1.00 10.00 -- 111.00 65.00 1.26 26 60 \w 85.00 112.00 1.00 10.00 -- 111.00 61.00 120.00 27 61 \w 42.00 113.00 1.00 10.00 -- 111.00-125.00-180.00 71 62 \w 39.00 66.00 1.00 10.00 -- 111.00-110.00 80.98 27 63 \w 85.00 178.00 1.00 10.00 -- 111.00 61.00 -30.00 93 64 \w 82.00 177.00 1.00 10.00 -- 111.00 74.00 90.37 95 65 \w 85.00 111.00 1.00 10.00 -- 111.00 60.00 117.47 26 66 \w 86.00 112.00 1.00 10.00 -- 111.00 55.00-162.16 26 ; _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 0.0669592000 _diffrn_orient_matrix_UB_12 0.0342859000 _diffrn_orient_matrix_UB_13 0.0292074000 _diffrn_orient_matrix_UB_21 0.0437088000 _diffrn_orient_matrix_UB_22 -0.0720993000 _diffrn_orient_matrix_UB_23 -0.0279082000 _diffrn_orient_matrix_UB_31 0.0103903000 _diffrn_orient_matrix_UB_32 0.0819262000 _diffrn_orient_matrix_UB_33 -0.0367911000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_unetI/netI 0.0265 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 160048 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.755 _diffrn_reflns_theta_min 3.134 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 6.866 _exptl_absorpt_correction_T_max 0.716 _exptl_absorpt_correction_T_min 0.169 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.58a (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 1.463 _exptl_crystal_description irregular _exptl_crystal_F_000 3272 _exptl_crystal_size_max 0.423 _exptl_crystal_size_mid 0.291 _exptl_crystal_size_min 0.205 _refine_diff_density_max 0.680 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.075 _refine_ls_extinction_coef 0.000055(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 745 _refine_ls_number_reflns 15269 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.034 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0360 _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^+7.1390P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.0974 _reflns_Friedel_coverage 0.000 _reflns_number_gt 14273 _reflns_number_total 15269 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05598c2.cif _cod_data_source_block compound9 _cod_original_cell_volume 7277.92(10) _cod_database_code 1557450 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C236 H320 Cl60 Ga12 N12 P4 ' _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. ; _diffrn_oxdiff_digest_frames ; 01daf365e99f952ddea88f8f2f0b0a13620353757c2 ; _diffrn_oxdiff_digest_hkl ; 01b4283c6e2c41b5797aef955c991bd4411373 ; _reflns_odcompleteness_completeness 99.98 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _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: C20(H20), C23(H23), C32(H32), C35(H35), C50(H50), C53(H53) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C58(H58A,H58B), C59(H59A,H59B) 2.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C16(H16), C17(H17), C18(H18), C28(H28), C29(H29), C30(H30), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C46(H46), C47(H47), C48(H48) 2.d Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B, H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C37(H37A, H37B,H37C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C) ; _shelx_res_file ; TITL sharma53_a.res in P2(1)/c sharma53.res created by SHELXL-2018/3 at 11:11:11 on 27-Aug-2019 REM Old TITL Sharma53 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.095, Rweak 0.005, Alpha 0.024 REM 0.791 for 277 systematic absences, Orientation as input REM Formula found by SHELXT: C59 N3 Cl16 Ga3 CELL 1.54184 19.162745 13.467009 28.292392 90 94.584 90 ZERR 4 0.000149 0.000104 0.000224 0 0.0007 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Ga N P UNIT 236 320 60 12 12 4 L.S. 4 0 0 PLAN 5 TEMP -173.15(10) BOND $h more -1 list 4 fmap 2 53 acta REM REM REM WGHT 0.052900 7.139000 EXTI 0.000055 FVAR 1.71836 GA1 4 0.333337 0.037301 0.355465 11.00000 0.03392 0.02331 = 0.02581 -0.00114 -0.00407 -0.00135 GA2 4 0.386264 0.300596 0.394812 11.00000 0.02462 0.02428 = 0.02333 0.00330 0.00335 0.00134 GA3 4 0.000112 0.274500 0.613247 11.00000 0.02157 0.01879 = 0.02133 -0.00328 0.00545 -0.00154 CL1 3 0.255716 0.121903 0.314715 11.00000 0.05511 0.03636 = 0.05959 0.00064 -0.03114 0.00230 CL2 3 0.425808 0.013266 0.318690 11.00000 0.05505 0.03939 = 0.03007 -0.00267 0.01015 0.00540 CL3 3 0.296165 -0.092166 0.389367 11.00000 0.05481 0.03220 = 0.04162 0.00363 -0.00189 -0.01513 CL4 3 0.369932 0.138086 0.419395 11.00000 0.03443 0.02415 = 0.02024 -0.00032 0.00166 -0.00577 CL5 3 0.284771 0.365854 0.386259 11.00000 0.03296 0.04394 = 0.05003 0.00013 -0.00478 0.01435 CL6 3 0.443235 0.292712 0.333213 11.00000 0.06164 0.05263 = 0.03624 0.01424 0.02574 0.00811 CL7 3 0.446662 0.358962 0.455698 11.00000 0.04068 0.02676 = 0.04186 -0.00262 -0.00888 -0.00554 CL8 3 0.007334 0.308731 0.538504 11.00000 0.03605 0.04806 = 0.02077 -0.00270 0.00825 -0.00221 CL9 3 0.105396 0.274718 0.648437 11.00000 0.02325 0.02213 = 0.03318 -0.00405 0.00096 -0.00053 CL10 3 -0.057333 0.391665 0.646617 11.00000 0.02634 0.02145 = 0.02439 -0.00073 0.00896 0.00272 CL11 3 -0.052079 0.134061 0.621255 11.00000 0.03158 0.02123 = 0.04460 -0.00484 0.00749 -0.00722 CL12 3 0.204146 0.276565 0.540481 11.00000 0.03740 0.04170 = 0.04217 -0.00078 0.01000 -0.00038 CL13 3 0.356788 0.268159 0.555127 11.00000 0.03828 0.03594 = 0.05115 0.01318 0.01303 0.00670 CL14 3 0.517558 0.190097 0.607848 11.00000 0.04903 0.03617 = 0.05464 0.01690 -0.00210 -0.00980 CL15 3 0.545966 0.394446 0.580885 11.00000 0.04344 0.02573 = 0.03818 0.00149 0.01115 -0.00036 P1 6 0.740588 0.220328 0.338951 11.00000 0.01807 0.01279 = 0.01629 0.00158 -0.00089 -0.00173 N1 5 0.907911 0.351135 0.372029 11.00000 0.01830 0.01206 = 0.01737 -0.00200 0.00238 -0.00072 N2 5 0.818298 0.404949 0.407123 11.00000 0.01799 0.01061 = 0.01745 -0.00200 0.00250 -0.00027 N3 5 0.694347 0.033326 0.310766 11.00000 0.01879 0.01494 = 0.01524 0.00050 0.00198 -0.00362 C1 1 0.843913 0.326000 0.384277 11.00000 0.01684 0.01249 = 0.01409 -0.00047 0.00085 0.00089 C2 1 0.923814 0.446181 0.387772 11.00000 0.02082 0.01359 = 0.02552 -0.00277 0.00356 -0.00378 AFIX 43 H2 2 0.965753 0.481699 0.383724 11.00000 -1.20000 AFIX 0 C3 1 0.868353 0.479121 0.410049 11.00000 0.02295 0.01251 = 0.02449 -0.00363 0.00365 -0.00256 AFIX 43 H3 2 0.864501 0.541836 0.424993 11.00000 -1.20000 AFIX 0 C4 1 0.812901 0.226048 0.377274 11.00000 0.01686 0.01275 = 0.01470 -0.00142 0.00322 -0.00049 C5 1 0.704491 0.094158 0.346416 11.00000 0.01533 0.01491 = 0.01523 0.00159 -0.00031 0.00033 C6 1 0.655027 -0.061443 0.324144 11.00000 0.03109 0.01584 = 0.02090 -0.00084 0.00644 -0.01083 C7 1 0.619114 -0.022560 0.366910 11.00000 0.02505 0.02177 = 0.01944 0.00058 0.00469 -0.00685 AFIX 23 H7A 2 0.616131 -0.075829 0.390778 11.00000 -1.20000 H7B 2 0.571081 0.000199 0.356864 11.00000 -1.20000 AFIX 0 C8 1 0.663364 0.064772 0.388231 11.00000 0.01782 0.01683 = 0.01626 0.00096 0.00384 -0.00061 C9 1 0.709279 0.037179 0.433704 11.00000 0.02158 0.02589 = 0.01590 0.00141 0.00345 0.00137 AFIX 23 H9A 2 0.738331 -0.021356 0.427315 11.00000 -1.20000 H9B 2 0.741149 0.093081 0.442738 11.00000 -1.20000 AFIX 0 C10 1 0.664524 0.013631 0.475027 11.00000 0.03010 0.03156 = 0.01656 0.00332 0.00721 -0.00143 AFIX 23 H10A 2 0.636374 -0.046744 0.467393 11.00000 -1.20000 H10B 2 0.695635 -0.000095 0.503925 11.00000 -1.20000 AFIX 0 C11 1 0.615939 0.099191 0.484643 11.00000 0.03357 0.03629 = 0.02433 -0.00372 0.01429 -0.00312 AFIX 23 H11A 2 0.644069 0.157261 0.496152 11.00000 -1.20000 H11B 2 0.585494 0.079746 0.509758 11.00000 -1.20000 AFIX 0 C12 1 0.570683 0.127707 0.440019 11.00000 0.02630 0.03363 = 0.03366 -0.00089 0.01389 0.00426 AFIX 23 H12A 2 0.540994 0.185291 0.446861 11.00000 -1.20000 H12B 2 0.539499 0.071597 0.430094 11.00000 -1.20000 AFIX 0 C13 1 0.616218 0.154182 0.399752 11.00000 0.02339 0.02288 = 0.02638 0.00137 0.00583 0.00417 AFIX 23 H13A 2 0.645973 0.212124 0.409121 11.00000 -1.20000 H13B 2 0.585875 0.172511 0.371116 11.00000 -1.20000 AFIX 0 C14 1 0.945792 0.298374 0.336977 11.00000 0.01937 0.01181 = 0.02009 -0.00179 0.00683 -0.00268 C15 1 0.920732 0.310682 0.289433 11.00000 0.02415 0.01587 = 0.02071 -0.00021 0.00530 -0.00364 C16 1 0.957343 0.261463 0.255652 11.00000 0.03452 0.02201 = 0.02046 -0.00183 0.00824 -0.00134 AFIX 43 H16 2 0.941866 0.267000 0.223012 11.00000 -1.20000 AFIX 0 C17 1 1.015763 0.204829 0.269046 11.00000 0.03368 0.02199 = 0.02724 -0.00396 0.01385 0.00043 AFIX 43 H17 2 1.039436 0.171011 0.245570 11.00000 -1.20000 AFIX 0 C18 1 1.040121 0.196851 0.316207 11.00000 0.02452 0.01827 = 0.02957 -0.00100 0.00872 0.00168 AFIX 43 H18 2 1.080879 0.158578 0.324608 11.00000 -1.20000 AFIX 0 C19 1 1.005844 0.244100 0.351762 11.00000 0.01851 0.01480 = 0.02425 -0.00070 0.00520 -0.00239 C20 1 0.861364 0.380951 0.273513 11.00000 0.02610 0.02156 = 0.02010 0.00332 0.00208 -0.00029 AFIX 13 H20 2 0.833165 0.392914 0.301217 11.00000 -1.20000 AFIX 0 C21 1 0.812310 0.338933 0.233159 11.00000 0.03381 0.03597 = 0.02489 0.00440 -0.00327 -0.00569 AFIX 137 H21A 2 0.836989 0.335539 0.204170 11.00000 -1.50000 H21B 2 0.771288 0.382140 0.227814 11.00000 -1.50000 H21C 2 0.797199 0.272177 0.241617 11.00000 -1.50000 AFIX 0 C22 1 0.892453 0.480519 0.259566 11.00000 0.03482 0.02296 = 0.03418 0.00848 0.00063 -0.00038 AFIX 137 H22A 2 0.922261 0.506979 0.286402 11.00000 -1.50000 H22B 2 0.854507 0.527503 0.250928 11.00000 -1.50000 H22C 2 0.920481 0.470778 0.232443 11.00000 -1.50000 AFIX 0 C23 1 1.035969 0.241073 0.402911 11.00000 0.02244 0.02211 = 0.02414 -0.00008 0.00146 0.00029 AFIX 13 H23 2 0.998090 0.259679 0.423594 11.00000 -1.20000 AFIX 0 C24 1 1.063444 0.138314 0.418000 11.00000 0.03226 0.02803 = 0.03411 0.00577 0.00304 0.00582 AFIX 137 H24A 2 1.026990 0.088547 0.410289 11.00000 -1.50000 H24B 2 1.076167 0.137957 0.452245 11.00000 -1.50000 H24C 2 1.104782 0.122585 0.401137 11.00000 -1.50000 AFIX 0 C25 1 1.094890 0.317933 0.410207 11.00000 0.03328 0.03404 = 0.04126 -0.00037 -0.00760 -0.00966 AFIX 137 H25A 2 1.132991 0.300204 0.390662 11.00000 -1.50000 H25B 2 1.112555 0.318959 0.443680 11.00000 -1.50000 H25C 2 1.076779 0.383756 0.400942 11.00000 -1.50000 AFIX 0 C26 1 0.750413 0.415049 0.426678 11.00000 0.01624 0.01278 = 0.02339 -0.00248 0.00329 0.00105 C27 1 0.693038 0.450076 0.397098 11.00000 0.02070 0.01492 = 0.02789 -0.00325 -0.00381 0.00026 C28 1 0.630003 0.460958 0.418427 11.00000 0.01938 0.02619 = 0.03909 -0.00439 -0.00167 0.00386 AFIX 43 H28 2 0.589404 0.481999 0.399621 11.00000 -1.20000 AFIX 0 C29 1 0.625182 0.441944 0.466091 11.00000 0.02381 0.03024 = 0.04008 -0.00226 0.01011 0.00021 AFIX 43 H29 2 0.581606 0.449841 0.479473 11.00000 -1.20000 AFIX 0 C30 1 0.683233 0.411607 0.494276 11.00000 0.02823 0.02655 = 0.02991 -0.00016 0.01092 0.00014 AFIX 43 H30 2 0.679578 0.400356 0.527134 11.00000 -1.20000 AFIX 0 C31 1 0.747350 0.397221 0.475095 11.00000 0.02314 0.01452 = 0.02376 -0.00175 0.00491 -0.00058 C32 1 0.697885 0.479875 0.345725 11.00000 0.03187 0.02079 = 0.02467 -0.00105 -0.00275 0.00703 AFIX 13 H32 2 0.725497 0.427980 0.330144 11.00000 -1.20000 AFIX 0 C33 1 0.735183 0.579578 0.341550 11.00000 0.06087 0.02977 = 0.03049 0.00648 -0.00248 -0.00873 AFIX 137 H33A 2 0.712507 0.629737 0.360208 11.00000 -1.50000 H33B 2 0.732574 0.600083 0.308221 11.00000 -1.50000 H33C 2 0.784355 0.572772 0.353548 11.00000 -1.50000 AFIX 0 C34 1 0.625961 0.487508 0.318481 11.00000 0.03818 0.05685 = 0.03492 -0.00244 -0.00926 0.01310 AFIX 137 H34A 2 0.598680 0.427750 0.324178 11.00000 -1.50000 H34B 2 0.631693 0.493610 0.284493 11.00000 -1.50000 H34C 2 0.601378 0.546061 0.329298 11.00000 -1.50000 AFIX 0 C35 1 0.810852 0.372630 0.508547 11.00000 0.02995 0.01943 = 0.01904 -0.00199 0.00205 0.00273 AFIX 13 H35 2 0.850464 0.356682 0.488863 11.00000 -1.20000 AFIX 0 C36 1 0.798470 0.282079 0.539424 11.00000 0.04217 0.02661 = 0.02316 0.00326 0.00607 0.00554 AFIX 137 H36A 2 0.841552 0.266326 0.559006 11.00000 -1.50000 H36B 2 0.784990 0.225215 0.519089 11.00000 -1.50000 H36C 2 0.760935 0.296682 0.559960 11.00000 -1.50000 AFIX 0 C37 1 0.831712 0.463976 0.538629 11.00000 0.04789 0.02501 = 0.03132 -0.00968 -0.00880 0.00607 AFIX 137 H37A 2 0.839562 0.520314 0.517780 11.00000 -1.50000 H37B 2 0.874803 0.449812 0.558511 11.00000 -1.50000 H37C 2 0.794125 0.480284 0.558856 11.00000 -1.50000 AFIX 0 C38 1 0.851489 0.144779 0.402721 11.00000 0.01528 0.01352 = 0.01800 -0.00002 0.00146 0.00017 C39 1 0.880421 0.156621 0.449273 11.00000 0.02221 0.01728 = 0.01830 -0.00175 0.00221 0.00156 AFIX 43 H39 2 0.880660 0.220337 0.463695 11.00000 -1.20000 AFIX 0 C40 1 0.908792 0.076125 0.474596 11.00000 0.02598 0.02659 = 0.02138 0.00512 -0.00011 0.00282 AFIX 43 H40 2 0.926518 0.084114 0.506697 11.00000 -1.20000 AFIX 0 C41 1 0.911252 -0.016412 0.452896 11.00000 0.02568 0.01998 = 0.03904 0.00863 -0.00097 0.00303 AFIX 43 H41 2 0.930106 -0.071830 0.470337 11.00000 -1.20000 AFIX 0 C42 1 0.886309 -0.027815 0.406011 11.00000 0.02518 0.01439 = 0.04541 -0.00454 -0.00301 0.00324 AFIX 43 H42 2 0.889530 -0.090500 0.390939 11.00000 -1.20000 AFIX 0 C43 1 0.856589 0.052171 0.380960 11.00000 0.02139 0.01651 = 0.02760 -0.00592 -0.00181 0.00134 AFIX 43 H43 2 0.839550 0.043961 0.348735 11.00000 -1.20000 AFIX 0 C44 1 0.710355 0.059206 0.262134 11.00000 0.02317 0.01911 = 0.01378 -0.00051 0.00235 -0.00796 C45 1 0.770676 0.022658 0.243002 11.00000 0.02531 0.02301 = 0.01785 -0.00308 0.00336 -0.00594 C46 1 0.782633 0.054383 0.197383 11.00000 0.03271 0.03604 = 0.01944 -0.00210 0.00826 -0.00528 AFIX 43 H46 2 0.823297 0.031806 0.183514 11.00000 -1.20000 AFIX 0 C47 1 0.737393 0.117268 0.171921 11.00000 0.03807 0.04069 = 0.01832 0.00495 0.00707 -0.00722 AFIX 43 H47 2 0.747641 0.138712 0.141244 11.00000 -1.20000 AFIX 0 C48 1 0.677075 0.149388 0.190793 11.00000 0.03205 0.03259 = 0.02061 0.00682 -0.00040 -0.00445 AFIX 43 H48 2 0.645737 0.191872 0.172637 11.00000 -1.20000 AFIX 0 C49 1 0.661360 0.120320 0.236283 11.00000 0.02492 0.02462 = 0.01749 0.00199 0.00063 -0.00659 C50 1 0.821792 -0.052293 0.266319 11.00000 0.02615 0.03025 = 0.01807 -0.00488 0.00429 -0.00051 AFIX 13 H50 2 0.809318 -0.063062 0.299586 11.00000 -1.20000 AFIX 0 C51 1 0.813784 -0.151991 0.239772 11.00000 0.04801 0.03556 = 0.02351 -0.01013 0.00112 0.01177 AFIX 137 H51A 2 0.764252 -0.170878 0.236283 11.00000 -1.50000 H51B 2 0.840632 -0.203310 0.257795 11.00000 -1.50000 H51C 2 0.831373 -0.145225 0.208345 11.00000 -1.50000 AFIX 0 C52 1 0.897858 -0.017183 0.268221 11.00000 0.02558 0.06574 = 0.02820 0.00692 0.00369 -0.00584 AFIX 137 H52A 2 0.913676 -0.016852 0.236127 11.00000 -1.50000 H52B 2 0.927383 -0.062261 0.288314 11.00000 -1.50000 H52C 2 0.901262 0.050065 0.281440 11.00000 -1.50000 AFIX 0 C53 1 0.592453 0.156890 0.253282 11.00000 0.02342 0.03662 = 0.02192 0.00713 -0.00042 -0.00084 AFIX 13 H53 2 0.588182 0.131486 0.286138 11.00000 -1.20000 AFIX 0 C54 1 0.590297 0.270169 0.254279 11.00000 0.03022 0.03819 = 0.03884 0.00244 -0.00404 0.00863 AFIX 137 H54A 2 0.631406 0.295280 0.273435 11.00000 -1.50000 H54B 2 0.547662 0.292104 0.268165 11.00000 -1.50000 H54C 2 0.590438 0.295852 0.221878 11.00000 -1.50000 AFIX 0 C55 1 0.529707 0.118997 0.220998 11.00000 0.02759 0.05662 = 0.02972 0.00898 -0.00351 -0.01105 AFIX 137 H55A 2 0.529206 0.151688 0.190026 11.00000 -1.50000 H55B 2 0.486185 0.134130 0.235510 11.00000 -1.50000 H55C 2 0.533744 0.047025 0.216884 11.00000 -1.50000 AFIX 0 C56 1 0.604327 -0.095744 0.283642 11.00000 0.04264 0.03317 = 0.02512 -0.00545 0.00529 -0.02215 AFIX 137 H56A 2 0.568912 -0.044274 0.276443 11.00000 -1.50000 H56B 2 0.581387 -0.157125 0.292710 11.00000 -1.50000 H56C 2 0.629865 -0.108033 0.255558 11.00000 -1.50000 AFIX 0 C57 1 0.707660 -0.143437 0.338413 11.00000 0.04529 0.01583 = 0.03484 0.00112 0.01567 -0.00373 AFIX 137 H57A 2 0.729432 -0.166901 0.310283 11.00000 -1.50000 H57B 2 0.683455 -0.198744 0.352585 11.00000 -1.50000 H57C 2 0.743854 -0.117256 0.361525 11.00000 -1.50000 AFIX 0 C58 1 0.284562 0.305813 0.517305 11.00000 0.04296 0.05760 = 0.03670 0.01570 0.00996 0.00339 AFIX 23 H58A 2 0.286597 0.272923 0.486151 11.00000 -1.20000 H58B 2 0.287094 0.378418 0.512234 11.00000 -1.20000 AFIX 0 C59 1 0.546749 0.268888 0.564561 11.00000 0.05049 0.02802 = 0.03440 0.00015 0.00931 0.00043 AFIX 23 H59A 2 0.516620 0.259923 0.534780 11.00000 -1.20000 H59B 2 0.595037 0.249836 0.558268 11.00000 -1.20000 AFIX 0 HKLF 4 REM sharma53_a.res in P2(1)/c REM wR2 = 0.0974, GooF = S = 1.034, Restrained GooF = 1.034 for all data REM R1 = 0.0360 for 14273 Fo > 4sig(Fo) and 0.0384 for all 15269 data REM 745 parameters refined using 0 restraints END WGHT 0.0530 7.2037 REM Highest difference peak 0.680, deepest hole -0.771, 1-sigma level 0.075 Q1 1 0.2517 -0.0641 0.3942 11.00000 0.05 0.68 Q2 1 0.4221 -0.0527 0.3481 11.00000 0.05 0.53 Q3 1 0.4019 0.0937 0.4403 11.00000 0.05 0.50 Q4 1 0.3041 0.1080 0.3052 11.00000 0.05 0.48 Q5 1 0.2047 0.2172 0.5344 11.00000 0.05 0.43 ; _shelx_res_checksum 65402 _olex2_date_sample_data_collection 2019-08-26 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.332 _oxdiff_exptl_absorpt_empirical_full_min 0.377 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 0.33334(2) 0.03730(2) 0.35547(2) 0.02802(7) Uani 1 1 d . . . . . Ga2 Ga 0.38626(2) 0.30060(2) 0.39481(2) 0.02400(7) Uani 1 1 d . . . . . Ga3 Ga 0.00011(2) 0.27450(2) 0.61325(2) 0.02036(7) Uani 1 1 d . . . . . Cl1 Cl 0.25572(4) 0.12190(5) 0.31471(3) 0.05227(19) Uani 1 1 d . . . . . Cl2 Cl 0.42581(4) 0.01327(5) 0.31869(2) 0.04114(14) Uani 1 1 d . . . . . Cl3 Cl 0.29617(4) -0.09217(5) 0.38937(2) 0.04318(15) Uani 1 1 d . . . . . Cl4 Cl 0.36993(3) 0.13809(4) 0.41940(2) 0.02630(11) Uani 1 1 d . . . . . Cl5 Cl 0.28477(3) 0.36585(5) 0.38626(3) 0.04275(15) Uani 1 1 d . . . . . Cl6 Cl 0.44323(4) 0.29271(6) 0.33321(2) 0.04900(18) Uani 1 1 d . . . . . Cl7 Cl 0.44666(3) 0.35896(4) 0.45570(2) 0.03709(13) Uani 1 1 d . . . . . Cl8 Cl 0.00733(3) 0.30873(5) 0.53850(2) 0.03464(13) Uani 1 1 d . . . . . Cl9 Cl 0.10540(3) 0.27472(4) 0.64844(2) 0.02626(11) Uani 1 1 d . . . . . Cl10 Cl -0.05733(3) 0.39166(4) 0.64662(2) 0.02369(10) Uani 1 1 d . . . . . Cl11 Cl -0.05208(3) 0.13406(4) 0.62126(2) 0.03223(12) Uani 1 1 d . . . . . Cl12 Cl 0.20415(3) 0.27656(5) 0.54048(2) 0.04006(14) Uani 1 1 d . . . . . Cl13 Cl 0.35679(3) 0.26816(5) 0.55513(3) 0.04128(15) Uani 1 1 d . . . . . Cl14 Cl 0.51756(4) 0.19010(5) 0.60785(3) 0.04695(16) Uani 1 1 d . . . . . Cl15 Cl 0.54597(3) 0.39445(4) 0.58089(2) 0.03536(13) Uani 1 1 d . . . . . P1 P 0.74059(2) 0.22033(3) 0.33895(2) 0.01584(10) Uani 1 1 d . . . . . N1 N 0.90791(8) 0.35114(12) 0.37203(6) 0.0159(3) Uani 1 1 d . . . . . N2 N 0.81830(8) 0.40495(12) 0.40712(6) 0.0153(3) Uani 1 1 d . . . . . N3 N 0.69435(8) 0.03333(12) 0.31077(6) 0.0163(3) Uani 1 1 d . . . . . C1 C 0.84391(10) 0.32600(14) 0.38428(6) 0.0145(3) Uani 1 1 d . . . . . C2 C 0.92381(10) 0.44618(15) 0.38777(7) 0.0199(4) Uani 1 1 d . . . . . H2 H 0.965753 0.481699 0.383724 0.024 Uiso 1 1 calc R . . . . C3 C 0.86835(11) 0.47912(15) 0.41005(7) 0.0199(4) Uani 1 1 d . . . . . H3 H 0.864501 0.541836 0.424993 0.024 Uiso 1 1 calc R . . . . C4 C 0.81290(10) 0.22605(14) 0.37727(6) 0.0147(3) Uani 1 1 d . . . . . C5 C 0.70449(9) 0.09416(14) 0.34642(6) 0.0152(3) Uani 1 1 d . . . . . C6 C 0.65503(11) -0.06144(15) 0.32414(7) 0.0224(4) Uani 1 1 d . . . . . C7 C 0.61911(11) -0.02256(16) 0.36691(7) 0.0219(4) Uani 1 1 d . . . . . H7A H 0.616131 -0.075829 0.390778 0.026 Uiso 1 1 calc R . . . . H7B H 0.571081 0.000199 0.356864 0.026 Uiso 1 1 calc R . . . . C8 C 0.66336(10) 0.06477(15) 0.38823(7) 0.0168(4) Uani 1 1 d . . . . . C9 C 0.70928(11) 0.03718(16) 0.43370(7) 0.0210(4) Uani 1 1 d . . . . . H9A H 0.738331 -0.021356 0.427315 0.025 Uiso 1 1 calc R . . . . H9B H 0.741149 0.093081 0.442738 0.025 Uiso 1 1 calc R . . . . C10 C 0.66452(12) 0.01363(18) 0.47503(7) 0.0258(4) Uani 1 1 d . . . . . H10A H 0.636374 -0.046744 0.467393 0.031 Uiso 1 1 calc R . . . . H10B H 0.695635 -0.000095 0.503925 0.031 Uiso 1 1 calc R . . . . C11 C 0.61594(13) 0.09919(19) 0.48464(8) 0.0308(5) Uani 1 1 d . . . . . H11A H 0.644069 0.157261 0.496152 0.037 Uiso 1 1 calc R . . . . H11B H 0.585494 0.079746 0.509758 0.037 Uiso 1 1 calc R . . . . C12 C 0.57068(12) 0.12771(19) 0.44002(9) 0.0306(5) Uani 1 1 d . . . . . H12A H 0.540994 0.185291 0.446861 0.037 Uiso 1 1 calc R . . . . H12B H 0.539499 0.071597 0.430094 0.037 Uiso 1 1 calc R . . . . C13 C 0.61622(11) 0.15418(16) 0.39975(8) 0.0240(4) Uani 1 1 d . . . . . H13A H 0.645973 0.212124 0.409121 0.029 Uiso 1 1 calc R . . . . H13B H 0.585875 0.172511 0.371116 0.029 Uiso 1 1 calc R . . . . C14 C 0.94579(10) 0.29837(14) 0.33698(7) 0.0168(4) Uani 1 1 d . . . . . C15 C 0.92073(11) 0.31068(15) 0.28943(7) 0.0201(4) Uani 1 1 d . . . . . C16 C 0.95734(12) 0.26146(16) 0.25565(8) 0.0253(4) Uani 1 1 d . . . . . H16 H 0.941866 0.267000 0.223012 0.030 Uiso 1 1 calc R . . . . C17 C 1.01576(12) 0.20483(17) 0.26905(8) 0.0270(4) Uani 1 1 d . . . . . H17 H 1.039436 0.171011 0.245570 0.032 Uiso 1 1 calc R . . . . C18 C 1.04012(11) 0.19685(16) 0.31621(8) 0.0238(4) Uani 1 1 d . . . . . H18 H 1.080879 0.158578 0.324608 0.029 Uiso 1 1 calc R . . . . C19 C 1.00584(10) 0.24410(15) 0.35176(7) 0.0190(4) Uani 1 1 d . . . . . C20 C 0.86136(11) 0.38095(16) 0.27351(7) 0.0226(4) Uani 1 1 d . . . . . H20 H 0.833165 0.392914 0.301217 0.027 Uiso 1 1 calc R . . . . C21 C 0.81231(13) 0.3389(2) 0.23316(8) 0.0319(5) Uani 1 1 d . . . . . H21A H 0.836989 0.335539 0.204170 0.048 Uiso 1 1 calc GR . . . . H21B H 0.771288 0.382140 0.227814 0.048 Uiso 1 1 calc GR . . . . H21C H 0.797199 0.272177 0.241617 0.048 Uiso 1 1 calc GR . . . . C22 C 0.89245(13) 0.48052(18) 0.25957(9) 0.0308(5) Uani 1 1 d . . . . . H22A H 0.922261 0.506979 0.286402 0.046 Uiso 1 1 calc GR . . . . H22B H 0.854507 0.527503 0.250928 0.046 Uiso 1 1 calc GR . . . . H22C H 0.920481 0.470778 0.232443 0.046 Uiso 1 1 calc GR . . . . C23 C 1.03597(11) 0.24107(16) 0.40291(8) 0.0229(4) Uani 1 1 d . . . . . H23 H 0.998090 0.259679 0.423594 0.027 Uiso 1 1 calc R . . . . C24 C 1.06344(13) 0.13831(18) 0.41800(9) 0.0314(5) Uani 1 1 d . . . . . H24A H 1.026990 0.088547 0.410289 0.047 Uiso 1 1 calc GR . . . . H24B H 1.076167 0.137957 0.452245 0.047 Uiso 1 1 calc GR . . . . H24C H 1.104782 0.122585 0.401137 0.047 Uiso 1 1 calc GR . . . . C25 C 1.09489(14) 0.3179(2) 0.41021(10) 0.0368(6) Uani 1 1 d . . . . . H25A H 1.132991 0.300204 0.390662 0.055 Uiso 1 1 calc GR . . . . H25B H 1.112555 0.318959 0.443680 0.055 Uiso 1 1 calc GR . . . . H25C H 1.076779 0.383756 0.400942 0.055 Uiso 1 1 calc GR . . . . C26 C 0.75041(10) 0.41505(14) 0.42668(7) 0.0174(4) Uani 1 1 d . . . . . C27 C 0.69304(11) 0.45008(15) 0.39710(8) 0.0215(4) Uani 1 1 d . . . . . C28 C 0.63000(11) 0.46096(17) 0.41843(9) 0.0284(5) Uani 1 1 d . . . . . H28 H 0.589404 0.481999 0.399621 0.034 Uiso 1 1 calc R . . . . C29 C 0.62518(12) 0.44194(18) 0.46609(9) 0.0310(5) Uani 1 1 d . . . . . H29 H 0.581606 0.449841 0.479473 0.037 Uiso 1 1 calc R . . . . C30 C 0.68323(12) 0.41161(17) 0.49428(8) 0.0278(4) Uani 1 1 d . . . . . H30 H 0.679578 0.400356 0.527134 0.033 Uiso 1 1 calc R . . . . C31 C 0.74735(11) 0.39722(15) 0.47509(7) 0.0203(4) Uani 1 1 d . . . . . C32 C 0.69788(12) 0.47988(16) 0.34573(8) 0.0260(4) Uani 1 1 d . . . . . H32 H 0.725497 0.427980 0.330144 0.031 Uiso 1 1 calc R . . . . C33 C 0.73518(17) 0.5796(2) 0.34155(9) 0.0407(6) Uani 1 1 d . . . . . H33A H 0.712507 0.629737 0.360208 0.061 Uiso 1 1 calc GR . . . . H33B H 0.732574 0.600083 0.308221 0.061 Uiso 1 1 calc GR . . . . H33C H 0.784355 0.572772 0.353548 0.061 Uiso 1 1 calc GR . . . . C34 C 0.62596(15) 0.4875(3) 0.31848(10) 0.0440(7) Uani 1 1 d . . . . . H34A H 0.598680 0.427750 0.324178 0.066 Uiso 1 1 calc GR . . . . H34B H 0.631693 0.493610 0.284493 0.066 Uiso 1 1 calc GR . . . . H34C H 0.601378 0.546061 0.329298 0.066 Uiso 1 1 calc GR . . . . C35 C 0.81085(12) 0.37263(16) 0.50855(7) 0.0228(4) Uani 1 1 d . . . . . H35 H 0.850464 0.356682 0.488863 0.027 Uiso 1 1 calc R . . . . C36 C 0.79847(14) 0.28208(18) 0.53942(8) 0.0305(5) Uani 1 1 d . . . . . H36A H 0.841552 0.266326 0.559006 0.046 Uiso 1 1 calc GR . . . . H36B H 0.784990 0.225215 0.519089 0.046 Uiso 1 1 calc GR . . . . H36C H 0.760935 0.296682 0.559960 0.046 Uiso 1 1 calc GR . . . . C37 C 0.83171(15) 0.46398(18) 0.53863(9) 0.0354(5) Uani 1 1 d . . . . . H37A H 0.839562 0.520314 0.517780 0.053 Uiso 1 1 calc GR . . . . H37B H 0.874803 0.449812 0.558511 0.053 Uiso 1 1 calc GR . . . . H37C H 0.794125 0.480284 0.558856 0.053 Uiso 1 1 calc GR . . . . C38 C 0.85149(9) 0.14478(14) 0.40272(7) 0.0156(3) Uani 1 1 d . . . . . C39 C 0.88042(10) 0.15662(15) 0.44927(7) 0.0192(4) Uani 1 1 d . . . . . H39 H 0.880660 0.220337 0.463695 0.023 Uiso 1 1 calc R . . . . C40 C 0.90879(11) 0.07612(17) 0.47460(8) 0.0248(4) Uani 1 1 d . . . . . H40 H 0.926518 0.084114 0.506697 0.030 Uiso 1 1 calc R . . . . C41 C 0.91125(12) -0.01641(17) 0.45290(9) 0.0284(5) Uani 1 1 d . . . . . H41 H 0.930106 -0.071830 0.470337 0.034 Uiso 1 1 calc R . . . . C42 C 0.88631(12) -0.02781(16) 0.40601(9) 0.0286(5) Uani 1 1 d . . . . . H42 H 0.889530 -0.090500 0.390939 0.034 Uiso 1 1 calc R . . . . C43 C 0.85659(11) 0.05217(15) 0.38096(8) 0.0220(4) Uani 1 1 d . . . . . H43 H 0.839550 0.043961 0.348735 0.026 Uiso 1 1 calc R . . . . C44 C 0.71035(10) 0.05921(15) 0.26213(7) 0.0186(4) Uani 1 1 d . . . . . C45 C 0.77068(11) 0.02266(16) 0.24300(7) 0.0220(4) Uani 1 1 d . . . . . C46 C 0.78263(13) 0.05438(19) 0.19738(8) 0.0291(5) Uani 1 1 d . . . . . H46 H 0.823297 0.031806 0.183514 0.035 Uiso 1 1 calc R . . . . C47 C 0.73739(13) 0.1173(2) 0.17192(8) 0.0321(5) Uani 1 1 d . . . . . H47 H 0.747641 0.138712 0.141244 0.039 Uiso 1 1 calc R . . . . C48 C 0.67707(12) 0.14939(18) 0.19079(8) 0.0286(5) Uani 1 1 d . . . . . H48 H 0.645737 0.191872 0.172637 0.034 Uiso 1 1 calc R . . . . C49 C 0.66136(11) 0.12032(16) 0.23628(7) 0.0224(4) Uani 1 1 d . . . . . C50 C 0.82179(11) -0.05229(17) 0.26632(7) 0.0247(4) Uani 1 1 d . . . . . H50 H 0.809318 -0.063062 0.299586 0.030 Uiso 1 1 calc R . . . . C51 C 0.81378(15) -0.1520(2) 0.23977(8) 0.0358(5) Uani 1 1 d . . . . . H51A H 0.764252 -0.170878 0.236283 0.054 Uiso 1 1 calc GR . . . . H51B H 0.840632 -0.203310 0.257795 0.054 Uiso 1 1 calc GR . . . . H51C H 0.831373 -0.145225 0.208345 0.054 Uiso 1 1 calc GR . . . . C52 C 0.89786(13) -0.0172(2) 0.26822(9) 0.0398(6) Uani 1 1 d . . . . . H52A H 0.913676 -0.016852 0.236127 0.060 Uiso 1 1 calc GR . . . . H52B H 0.927383 -0.062261 0.288314 0.060 Uiso 1 1 calc GR . . . . H52C H 0.901262 0.050065 0.281440 0.060 Uiso 1 1 calc GR . . . . C53 C 0.59245(11) 0.15689(19) 0.25328(8) 0.0274(4) Uani 1 1 d . . . . . H53 H 0.588182 0.131486 0.286138 0.033 Uiso 1 1 calc R . . . . C54 C 0.59030(13) 0.2702(2) 0.25428(10) 0.0361(5) Uani 1 1 d . . . . . H54A H 0.631406 0.295280 0.273435 0.054 Uiso 1 1 calc GR . . . . H54B H 0.547662 0.292104 0.268165 0.054 Uiso 1 1 calc GR . . . . H54C H 0.590438 0.295852 0.221878 0.054 Uiso 1 1 calc GR . . . . C55 C 0.52971(13) 0.1190(2) 0.22100(9) 0.0383(6) Uani 1 1 d . . . . . H55A H 0.529206 0.151688 0.190026 0.057 Uiso 1 1 calc GR . . . . H55B H 0.486185 0.134130 0.235510 0.057 Uiso 1 1 calc GR . . . . H55C H 0.533744 0.047025 0.216884 0.057 Uiso 1 1 calc GR . . . . C56 C 0.60433(14) -0.09574(19) 0.28364(8) 0.0335(5) Uani 1 1 d . . . . . H56A H 0.568912 -0.044274 0.276443 0.050 Uiso 1 1 calc GR . . . . H56B H 0.581387 -0.157125 0.292710 0.050 Uiso 1 1 calc GR . . . . H56C H 0.629865 -0.108033 0.255558 0.050 Uiso 1 1 calc GR . . . . C57 C 0.70766(14) -0.14344(16) 0.33841(9) 0.0313(5) Uani 1 1 d . . . . . H57A H 0.729432 -0.166901 0.310283 0.047 Uiso 1 1 calc GR . . . . H57B H 0.683455 -0.198744 0.352585 0.047 Uiso 1 1 calc GR . . . . H57C H 0.743854 -0.117256 0.361525 0.047 Uiso 1 1 calc GR . . . . C58 C 0.28456(15) 0.3058(3) 0.51730(10) 0.0454(7) Uani 1 1 d . . . . . H58A H 0.286597 0.272923 0.486151 0.054 Uiso 1 1 calc R . . . . H58B H 0.287094 0.378418 0.512234 0.054 Uiso 1 1 calc R . . . . C59 C 0.54675(16) 0.26889(19) 0.56456(10) 0.0373(6) Uani 1 1 d . . . . . H59A H 0.516620 0.259923 0.534780 0.045 Uiso 1 1 calc R . . . . H59B H 0.595037 0.249836 0.558268 0.045 Uiso 1 1 calc R . . . . 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 0.03392(15) 0.02331(14) 0.02581(14) -0.00114(10) -0.00407(11) -0.00135(11) Ga2 0.02462(13) 0.02428(14) 0.02333(13) 0.00330(10) 0.00335(10) 0.00134(10) Ga3 0.02157(13) 0.01879(13) 0.02133(13) -0.00328(9) 0.00545(9) -0.00154(9) Cl1 0.0551(4) 0.0364(3) 0.0596(4) 0.0006(3) -0.0311(3) 0.0023(3) Cl2 0.0551(4) 0.0394(3) 0.0301(3) -0.0027(2) 0.0101(3) 0.0054(3) Cl3 0.0548(4) 0.0322(3) 0.0416(3) 0.0036(2) -0.0019(3) -0.0151(3) Cl4 0.0344(3) 0.0241(2) 0.0202(2) -0.00032(17) 0.00166(18) -0.00577(19) Cl5 0.0330(3) 0.0439(4) 0.0500(4) 0.0001(3) -0.0048(3) 0.0144(3) Cl6 0.0616(4) 0.0526(4) 0.0362(3) 0.0142(3) 0.0257(3) 0.0081(3) Cl7 0.0407(3) 0.0268(3) 0.0419(3) -0.0026(2) -0.0089(2) -0.0055(2) Cl8 0.0360(3) 0.0481(3) 0.0208(2) -0.0027(2) 0.0082(2) -0.0022(2) Cl9 0.0233(2) 0.0221(2) 0.0332(3) -0.00405(19) 0.00096(19) -0.00053(18) Cl10 0.0263(2) 0.0214(2) 0.0244(2) -0.00073(17) 0.00896(18) 0.00272(18) Cl11 0.0316(3) 0.0212(2) 0.0446(3) -0.0048(2) 0.0075(2) -0.0072(2) Cl12 0.0374(3) 0.0417(3) 0.0422(3) -0.0008(3) 0.0100(2) -0.0004(2) Cl13 0.0383(3) 0.0359(3) 0.0512(4) 0.0132(3) 0.0130(3) 0.0067(2) Cl14 0.0490(4) 0.0362(3) 0.0546(4) 0.0169(3) -0.0021(3) -0.0098(3) Cl15 0.0434(3) 0.0257(3) 0.0382(3) 0.0015(2) 0.0111(2) -0.0004(2) P1 0.0181(2) 0.0128(2) 0.0163(2) 0.00158(16) -0.00089(17) -0.00173(16) N1 0.0183(7) 0.0121(7) 0.0174(7) -0.0020(6) 0.0024(6) -0.0007(6) N2 0.0180(7) 0.0106(7) 0.0174(7) -0.0020(6) 0.0025(6) -0.0003(6) N3 0.0188(7) 0.0149(8) 0.0152(7) 0.0005(6) 0.0020(6) -0.0036(6) C1 0.0168(8) 0.0125(9) 0.0141(8) -0.0005(6) 0.0008(6) 0.0009(7) C2 0.0208(9) 0.0136(9) 0.0255(10) -0.0028(7) 0.0036(7) -0.0038(7) C3 0.0230(9) 0.0125(9) 0.0245(9) -0.0036(7) 0.0037(7) -0.0026(7) C4 0.0169(8) 0.0128(9) 0.0147(8) -0.0014(6) 0.0032(6) -0.0005(7) C5 0.0153(8) 0.0149(9) 0.0152(8) 0.0016(7) -0.0003(6) 0.0003(7) C6 0.0311(10) 0.0158(9) 0.0209(9) -0.0008(7) 0.0064(8) -0.0108(8) C7 0.0250(10) 0.0218(10) 0.0194(9) 0.0006(7) 0.0047(7) -0.0068(8) C8 0.0178(8) 0.0168(9) 0.0163(8) 0.0010(7) 0.0038(7) -0.0006(7) C9 0.0216(9) 0.0259(10) 0.0159(9) 0.0014(7) 0.0035(7) 0.0014(8) C10 0.0301(10) 0.0316(11) 0.0166(9) 0.0033(8) 0.0072(8) -0.0014(9) C11 0.0336(12) 0.0363(13) 0.0243(10) -0.0037(9) 0.0143(9) -0.0031(10) C12 0.0263(11) 0.0336(12) 0.0337(12) -0.0009(9) 0.0139(9) 0.0043(9) C13 0.0234(10) 0.0229(10) 0.0264(10) 0.0014(8) 0.0058(8) 0.0042(8) C14 0.0194(9) 0.0118(8) 0.0201(9) -0.0018(7) 0.0068(7) -0.0027(7) C15 0.0241(9) 0.0159(9) 0.0207(9) -0.0002(7) 0.0053(7) -0.0036(7) C16 0.0345(11) 0.0220(10) 0.0205(10) -0.0018(8) 0.0082(8) -0.0013(9) C17 0.0337(11) 0.0220(10) 0.0272(11) -0.0040(8) 0.0139(9) 0.0004(9) C18 0.0245(10) 0.0183(10) 0.0296(11) -0.0010(8) 0.0087(8) 0.0017(8) C19 0.0185(9) 0.0148(9) 0.0242(10) -0.0007(7) 0.0052(7) -0.0024(7) C20 0.0261(10) 0.0216(10) 0.0201(9) 0.0033(8) 0.0021(8) -0.0003(8) C21 0.0338(12) 0.0360(13) 0.0249(11) 0.0044(9) -0.0033(9) -0.0057(10) C22 0.0348(12) 0.0230(11) 0.0342(12) 0.0085(9) 0.0006(9) -0.0004(9) C23 0.0224(9) 0.0221(10) 0.0241(10) -0.0001(8) 0.0015(8) 0.0003(8) C24 0.0323(12) 0.0280(12) 0.0341(12) 0.0058(9) 0.0030(9) 0.0058(9) C25 0.0333(12) 0.0340(13) 0.0413(14) -0.0004(10) -0.0076(10) -0.0097(10) C26 0.0162(8) 0.0128(8) 0.0234(9) -0.0025(7) 0.0033(7) 0.0010(7) C27 0.0207(9) 0.0149(9) 0.0279(10) -0.0033(7) -0.0038(8) 0.0003(7) C28 0.0194(10) 0.0262(11) 0.0391(12) -0.0044(9) -0.0017(9) 0.0039(8) C29 0.0238(10) 0.0302(12) 0.0401(13) -0.0023(10) 0.0101(9) 0.0002(9) C30 0.0282(11) 0.0266(11) 0.0299(11) -0.0002(9) 0.0109(9) 0.0001(9) C31 0.0231(9) 0.0145(9) 0.0238(10) -0.0018(7) 0.0049(8) -0.0006(7) C32 0.0319(11) 0.0208(10) 0.0247(10) -0.0011(8) -0.0027(8) 0.0070(8) C33 0.0609(17) 0.0298(13) 0.0305(12) 0.0065(10) -0.0025(11) -0.0087(12) C34 0.0382(14) 0.0569(18) 0.0349(13) -0.0024(12) -0.0093(11) 0.0131(13) C35 0.0300(10) 0.0194(10) 0.0190(9) -0.0020(7) 0.0021(8) 0.0027(8) C36 0.0422(13) 0.0266(11) 0.0232(10) 0.0033(8) 0.0061(9) 0.0055(9) C37 0.0479(14) 0.0250(12) 0.0313(12) -0.0097(9) -0.0088(10) 0.0061(10) C38 0.0153(8) 0.0135(9) 0.0180(9) 0.0000(7) 0.0015(7) 0.0002(7) C39 0.0222(9) 0.0173(9) 0.0183(9) -0.0017(7) 0.0022(7) 0.0016(7) C40 0.0260(10) 0.0266(11) 0.0214(9) 0.0051(8) -0.0001(8) 0.0028(8) C41 0.0257(10) 0.0200(10) 0.0390(12) 0.0086(9) -0.0010(9) 0.0030(8) C42 0.0252(10) 0.0144(10) 0.0454(13) -0.0045(9) -0.0030(9) 0.0032(8) C43 0.0214(9) 0.0165(9) 0.0276(10) -0.0059(8) -0.0018(8) 0.0013(7) C44 0.0232(9) 0.0191(9) 0.0138(8) -0.0005(7) 0.0024(7) -0.0080(7) C45 0.0253(10) 0.0230(10) 0.0178(9) -0.0031(7) 0.0034(7) -0.0059(8) C46 0.0327(11) 0.0360(13) 0.0194(10) -0.0021(9) 0.0083(8) -0.0053(9) C47 0.0381(12) 0.0407(13) 0.0183(10) 0.0050(9) 0.0071(9) -0.0072(10) C48 0.0321(11) 0.0326(12) 0.0206(10) 0.0068(9) -0.0004(8) -0.0044(9) C49 0.0249(10) 0.0246(10) 0.0175(9) 0.0020(8) 0.0006(7) -0.0066(8) C50 0.0261(10) 0.0303(11) 0.0181(9) -0.0049(8) 0.0043(8) -0.0005(9) C51 0.0480(14) 0.0356(13) 0.0235(11) -0.0101(9) 0.0011(10) 0.0118(11) C52 0.0256(11) 0.0657(19) 0.0282(12) 0.0069(12) 0.0037(9) -0.0058(11) C53 0.0234(10) 0.0366(12) 0.0219(10) 0.0071(9) -0.0004(8) -0.0008(9) C54 0.0302(12) 0.0382(14) 0.0388(13) 0.0024(10) -0.0040(10) 0.0086(10) C55 0.0276(11) 0.0566(17) 0.0297(12) 0.0090(11) -0.0035(9) -0.0110(11) C56 0.0426(13) 0.0332(13) 0.0251(11) -0.0054(9) 0.0053(9) -0.0222(10) C57 0.0453(13) 0.0158(10) 0.0348(12) 0.0011(8) 0.0157(10) -0.0037(9) C58 0.0430(15) 0.0576(18) 0.0367(14) 0.0157(13) 0.0100(11) 0.0034(13) C59 0.0505(15) 0.0280(13) 0.0344(13) 0.0002(10) 0.0093(11) 0.0004(11) 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 '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' P P 0.2955 0.4335 '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 -11 3 7 0.1027 11 -3 -7 0.1027 10 0 -12 0.0937 0 -8 7 0.1903 0 8 -7 0.1903 -12 0 -4 0.1033 12 0 4 0.1033 1 -6 13 0.1754 7 6 -10 0.1613 -3 6 -13 0.1769 -7 2 15 0.1034 7 -2 -15 0.1034 6 2 -17 0.0983 -3 -5 14 0.1776 -7 6 11 0.1164 -1 2 -18 0.1083 5 5 13 0.1278 2 -1 18 0.1611 -4 -4 -15 0.1566 2 -3 -17 0.1212 -1 8 8 0.1363 -3 -1 18 0.1383 -2 6 14 0.1166 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 112.60(3) . . ? Cl1 Ga1 Cl3 115.73(3) . . ? Cl1 Ga1 Cl4 105.20(3) . . ? Cl2 Ga1 Cl4 104.80(3) . . ? Cl3 Ga1 Cl2 114.28(3) . . ? Cl3 Ga1 Cl4 102.57(2) . . ? Cl5 Ga2 Cl4 106.19(3) . . ? Cl5 Ga2 Cl6 116.76(3) . . ? Cl5 Ga2 Cl7 111.65(3) . . ? Cl6 Ga2 Cl4 106.72(3) . . ? Cl6 Ga2 Cl7 113.32(3) . . ? Cl7 Ga2 Cl4 100.46(2) . . ? Cl8 Ga3 Cl10 109.90(2) . . ? Cl9 Ga3 Cl8 108.36(2) . . ? Cl9 Ga3 Cl10 106.40(2) . . ? Cl11 Ga3 Cl8 110.66(3) . . ? Cl11 Ga3 Cl9 111.91(2) . . ? Cl11 Ga3 Cl10 109.52(2) . . ? Ga1 Cl4 Ga2 110.87(2) . . ? C4 P1 C5 105.24(9) . . ? C1 N1 C2 109.42(16) . . ? C1 N1 C14 124.48(16) . . ? C2 N1 C14 124.15(16) . . ? C1 N2 C3 108.61(16) . . ? C1 N2 C26 128.38(16) . . ? C3 N2 C26 123.01(16) . . ? C5 N3 C6 112.07(15) . . ? C5 N3 C44 123.00(16) . . ? C44 N3 C6 124.45(15) . . ? N1 C1 N2 107.33(16) . . ? N1 C1 C4 124.06(16) . . ? N2 C1 C4 128.36(17) . . ? N1 C2 H2 126.5 . . ? C3 C2 N1 107.02(17) . . ? C3 C2 H2 126.5 . . ? N2 C3 H3 126.2 . . ? C2 C3 N2 107.59(17) . . ? C2 C3 H3 126.2 . . ? C1 C4 P1 115.30(13) . . ? C38 C4 P1 129.18(14) . . ? C38 C4 C1 115.44(16) . . ? N3 C5 P1 121.51(14) . . ? N3 C5 C8 112.54(16) . . ? C8 C5 P1 123.17(14) . . ? C7 C6 N3 99.78(15) . . ? C56 C6 N3 111.27(17) . . ? C56 C6 C7 113.62(19) . . ? C56 C6 C57 110.5(2) . . ? C57 C6 N3 109.71(17) . . ? C57 C6 C7 111.54(18) . . ? C6 C7 H7A 110.2 . . ? C6 C7 H7B 110.2 . . ? C6 C7 C8 107.56(16) . . ? H7A C7 H7B 108.5 . . ? C8 C7 H7A 110.2 . . ? C8 C7 H7B 110.2 . . ? C5 C8 C7 101.32(15) . . ? C5 C8 C9 114.40(15) . . ? C5 C8 C13 107.85(16) . . ? C7 C8 C9 113.61(17) . . ? C7 C8 C13 111.19(16) . . ? C9 C8 C13 108.26(16) . . ? C8 C9 H9A 109.3 . . ? C8 C9 H9B 109.3 . . ? H9A C9 H9B 108.0 . . ? C10 C9 C8 111.58(17) . . ? C10 C9 H9A 109.3 . . ? C10 C9 H9B 109.3 . . ? C9 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C11 C10 C9 111.52(18) . . ? C11 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C10 C11 C12 111.06(19) . . ? H11A C11 H11B 108.0 . . ? C12 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 C13 110.79(19) . . ? H12A C12 H12B 108.1 . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? C12 C13 C8 110.53(18) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? C15 C14 N1 116.34(17) . . ? C19 C14 N1 119.55(17) . . ? C19 C14 C15 124.02(18) . . ? C14 C15 C20 123.29(18) . . ? C16 C15 C14 116.63(19) . . ? C16 C15 C20 119.83(19) . . ? C15 C16 H16 119.5 . . ? C17 C16 C15 120.9(2) . . ? C17 C16 H16 119.5 . . ? C16 C17 H17 119.6 . . ? C18 C17 C16 120.7(2) . . ? C18 C17 H17 119.6 . . ? C17 C18 H18 119.4 . . ? C17 C18 C19 121.2(2) . . ? C19 C18 H18 119.4 . . ? C14 C19 C23 122.77(18) . . ? C18 C19 C14 116.45(19) . . ? C18 C19 C23 120.67(19) . . ? C15 C20 H20 107.9 . . ? C15 C20 C21 113.07(19) . . ? C15 C20 C22 108.91(18) . . ? C21 C20 H20 107.9 . . ? C21 C20 C22 111.12(18) . . ? C22 C20 H20 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23 108.3 . . ? C19 C23 C24 112.79(18) . . ? C19 C23 C25 109.31(18) . . ? C24 C23 H23 108.3 . . ? C24 C23 C25 109.87(19) . . ? C25 C23 H23 108.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 N2 118.87(18) . . ? C31 C26 N2 117.66(17) . . ? C31 C26 C27 123.25(18) . . ? C26 C27 C32 123.56(19) . . ? C28 C27 C26 116.0(2) . . ? C28 C27 C32 120.39(19) . . ? C27 C28 H28 119.1 . . ? C29 C28 C27 121.9(2) . . ? C29 C28 H28 119.1 . . ? C28 C29 H29 119.8 . . ? C30 C29 C28 120.4(2) . . ? C30 C29 H29 119.8 . . ? C29 C30 H30 119.6 . . ? C29 C30 C31 120.7(2) . . ? C31 C30 H30 119.6 . . ? C26 C31 C35 123.70(18) . . ? C30 C31 C26 117.7(2) . . ? C30 C31 C35 118.35(19) . . ? C27 C32 H32 108.2 . . ? C27 C32 C33 111.76(19) . . ? C27 C32 C34 112.3(2) . . ? C33 C32 H32 108.2 . . ? C34 C32 H32 108.2 . . ? C34 C32 C33 108.1(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35 107.8 . . ? C31 C35 C36 112.15(19) . . ? C31 C35 C37 109.40(18) . . ? C36 C35 H35 107.8 . . ? C36 C35 C37 111.63(19) . . ? C37 C35 H35 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C4 121.40(17) . . ? C39 C38 C43 118.74(18) . . ? C43 C38 C4 119.79(17) . . ? C38 C39 H39 119.7 . . ? C40 C39 C38 120.52(19) . . ? C40 C39 H39 119.7 . . ? C39 C40 H40 120.1 . . ? C39 C40 C41 119.9(2) . . ? C41 C40 H40 120.1 . . ? C40 C41 H41 119.9 . . ? C42 C41 C40 120.1(2) . . ? C42 C41 H41 119.9 . . ? C41 C42 H42 120.0 . . ? C41 C42 C43 120.0(2) . . ? C43 C42 H42 120.0 . . ? C38 C43 H43 119.7 . . ? C42 C43 C38 120.6(2) . . ? C42 C43 H43 119.7 . . ? C45 C44 N3 121.05(18) . . ? C45 C44 C49 122.67(18) . . ? C49 C44 N3 116.28(17) . . ? C44 C45 C50 125.97(18) . . ? C46 C45 C44 116.8(2) . . ? C46 C45 C50 117.19(19) . . ? C45 C46 H46 119.0 . . ? C47 C46 C45 122.0(2) . . ? C47 C46 H46 119.0 . . ? C46 C47 H47 119.9 . . ? C46 C47 C48 120.2(2) . . ? C48 C47 H47 119.9 . . ? C47 C48 H48 119.5 . . ? C47 C48 C49 121.0(2) . . ? C49 C48 H48 119.5 . . ? C44 C49 C53 125.72(18) . . ? C48 C49 C44 117.2(2) . . ? C48 C49 C53 117.1(2) . . ? C45 C50 H50 108.1 . . ? C45 C50 C51 109.37(18) . . ? C45 C50 C52 112.9(2) . . ? C51 C50 H50 108.1 . . ? C52 C50 H50 108.1 . . ? C52 C50 C51 110.1(2) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53 108.7 . . ? C49 C53 C54 110.76(19) . . ? C49 C53 C55 111.2(2) . . ? C54 C53 H53 108.7 . . ? C54 C53 C55 108.8(2) . . ? C55 C53 H53 108.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C6 C56 H56A 109.5 . . ? C6 C56 H56B 109.5 . . ? C6 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C6 C57 H57A 109.5 . . ? C6 C57 H57B 109.5 . . ? C6 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? Cl12 C58 H58A 109.2 . . ? Cl12 C58 H58B 109.2 . . ? Cl13 C58 Cl12 112.21(15) . . ? Cl13 C58 H58A 109.2 . . ? Cl13 C58 H58B 109.2 . . ? H58A C58 H58B 107.9 . . ? Cl14 C59 Cl15 113.04(15) . . ? Cl14 C59 H59A 109.0 . . ? Cl14 C59 H59B 109.0 . . ? Cl15 C59 H59A 109.0 . . ? Cl15 C59 H59B 109.0 . . ? H59A C59 H59B 107.8 . . ? 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 2.1367(7) . ? Ga1 Cl2 2.1499(7) . ? Ga1 Cl3 2.1393(7) . ? Ga1 Cl4 2.3244(6) . ? Ga2 Cl4 2.3251(6) . ? Ga2 Cl5 2.1303(6) . ? Ga2 Cl6 2.1318(7) . ? Ga2 Cl7 2.1462(6) . ? Ga3 Cl8 2.1795(6) . ? Ga3 Cl9 2.1773(6) . ? Ga3 Cl10 2.1815(5) . ? Ga3 Cl11 2.1598(6) . ? Cl12 C58 1.767(3) . ? Cl13 C58 1.755(3) . ? Cl14 C59 1.746(3) . ? Cl15 C59 1.753(3) . ? P1 C4 1.6916(19) . ? P1 C5 1.8530(19) . ? N1 C1 1.344(2) . ? N1 C2 1.381(2) . ? N1 C14 1.460(2) . ? N2 C1 1.356(2) . ? N2 C3 1.383(2) . ? N2 C26 1.460(2) . ? N3 C5 1.302(2) . ? N3 C6 1.544(2) . ? N3 C44 1.475(2) . ? C1 C4 1.478(2) . ? C2 H2 0.9500 . ? C2 C3 1.353(3) . ? C3 H3 0.9500 . ? C4 C38 1.476(3) . ? C5 C8 1.525(2) . ? C6 C7 1.531(3) . ? C6 C56 1.514(3) . ? C6 C57 1.528(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.544(3) . ? C8 C9 1.545(3) . ? C8 C13 1.555(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.537(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.520(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.523(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.531(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.402(3) . ? C14 C19 1.399(3) . ? C15 C16 1.397(3) . ? C15 C20 1.520(3) . ? C16 H16 0.9500 . ? C16 C17 1.382(3) . ? C17 H17 0.9500 . ? C17 C18 1.382(3) . ? C18 H18 0.9500 . ? C18 C19 1.398(3) . ? C19 C23 1.515(3) . ? C20 H20 1.0000 . ? C20 C21 1.528(3) . ? C20 C22 1.532(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23 1.0000 . ? C23 C24 1.529(3) . ? C23 C25 1.533(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.409(3) . ? C26 C31 1.397(3) . ? C27 C28 1.400(3) . ? C27 C32 1.518(3) . ? C28 H28 0.9500 . ? C28 C29 1.383(4) . ? C29 H29 0.9500 . ? C29 C30 1.378(3) . ? C30 H30 0.9500 . ? C30 C31 1.396(3) . ? C31 C35 1.517(3) . ? C32 H32 1.0000 . ? C32 C33 1.530(3) . ? C32 C34 1.528(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35 1.0000 . ? C35 C36 1.530(3) . ? C35 C37 1.531(3) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C39 1.397(3) . ? C38 C43 1.398(3) . ? C39 H39 0.9500 . ? C39 C40 1.386(3) . ? C40 H40 0.9500 . ? C40 C41 1.392(3) . ? C41 H41 0.9500 . ? C41 C42 1.382(3) . ? C42 H42 0.9500 . ? C42 C43 1.387(3) . ? C43 H43 0.9500 . ? C44 C45 1.404(3) . ? C44 C49 1.409(3) . ? C45 C46 1.396(3) . ? C45 C50 1.520(3) . ? C46 H46 0.9500 . ? C46 C47 1.374(4) . ? C47 H47 0.9500 . ? C47 C48 1.381(4) . ? C48 H48 0.9500 . ? C48 C49 1.401(3) . ? C49 C53 1.523(3) . ? C50 H50 1.0000 . ? C50 C51 1.540(3) . ? C50 C52 1.529(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53 1.0000 . ? C53 C54 1.526(4) . ? C53 C55 1.538(3) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? 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 -11.0186 2.8425 7.3667 -0.4252 -0.8921 -0.1526 11.0186 -2.8425 -7.3667 0.4252 0.8921 0.1526 10.2751 0.2361 -11.5253 0.3595 0.7537 0.5501 0.0146 -8.0837 6.9631 -0.0728 0.3891 -0.9183 -0.0146 8.0837 -6.9631 0.0728 -0.3891 0.9183 -11.8134 -0.1726 -4.3328 -0.9235 -0.3830 0.0225 11.8134 0.1726 4.3328 0.9235 0.3830 -0.0225 1.1277 -5.9270 13.2145 0.2583 0.1078 -0.9600 7.0412 5.8217 -9.7344 0.3868 0.1597 0.9082 -2.7406 5.5957 -13.1432 -0.3755 -0.1564 0.9135 -6.8275 2.3957 15.2618 0.0707 -0.8971 -0.4362 6.8275 -2.3957 -15.2618 -0.0707 0.8971 0.4362 5.6855 1.6656 -16.5750 -0.0463 0.5910 0.8053 -3.2263 -5.3495 14.0574 0.0111 -0.1476 -0.9890 -6.5270 5.5518 11.1456 0.0788 -0.9966 -0.0230 -1.2042 1.5117 -17.7956 -0.5486 0.3350 0.7661 4.6074 5.1709 12.5660 0.8528 -0.5221 0.0092 1.7128 -0.6816 17.8680 0.6132 -0.3747 -0.6954 -4.1362 -3.9820 -14.6264 -0.8407 0.5145 0.1689 2.4397 -3.2216 -16.9196 -0.4413 0.8111 0.3839 -0.8757 7.7807 8.3470 0.4519 -0.8322 0.3212 -2.8290 -0.6988 18.0972 0.3152 -0.5783 -0.7525 -1.8018 5.7901 13.6664 0.4770 -0.8776 -0.0472