#------------------------------------------------------------------------------ #$Date: 2020-09-05 02:46:25 +0300 (Sat, 05 Sep 2020) $ #$Revision: 255905 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705355.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_7705355 loop_ _publ_author_name 'Helling, Christoph' 'W\"olper, Christoph' 'Schulz, Stephan' _publ_section_title ; Synthesis of heteroleptic gallium-substituted antimony hydrides by stepwise \b-H elimination. ; _journal_issue 34 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 11835 _journal_page_last 11842 _journal_paper_doi 10.1039/d0dt01937b _journal_volume 49 _journal_year 2020 _chemical_formula_sum 'C35 H60 Cl Ga N3 Sb Si2' _chemical_formula_weight 805.96 _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 mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2020-05-27 deposited with the CCDC. 2020-07-14 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.101(14) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.861(3) _cell_length_b 19.979(6) _cell_length_c 20.390(6) _cell_measurement_reflns_used 8046 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 33.31 _cell_measurement_theta_min 2.59 _cell_volume 3913(2) _computing_cell_refinement 'BRUKER APEX2(v2009.5-1)' _computing_data_collection 'BRUKER APEX2(v2009.5-1)' _computing_data_reduction 'BRUKER APEX2(v2009.5-1)' _computing_molecular_graphics 'ORTEP/PLATON (Spek)' _computing_publication_material 'BRUKER AXS SHELXTL (c) 2008 / Vers. 2008/4' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'BRUKER APEX2(v2009.5-1)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker D8 KAPPA II (APEX II detector)' _diffrn_measurement_method 'Data collection strategy APEX 2/COSMO' _diffrn_radiation_monochromator 'Triumph Goebel mirror' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_unetI/netI 0.0258 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 146299 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.141 _diffrn_reflns_theta_min 1.446 _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.368 _exptl_crystal_description block _exptl_crystal_F_000 1672 _exptl_crystal_size_max 0.275 _exptl_crystal_size_mid 0.184 _exptl_crystal_size_min 0.078 _refine_diff_density_max 1.852 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.080 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 447 _refine_ls_number_reflns 14916 _refine_ls_number_restraints 31 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0292 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+3.0636P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.0825 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10070 _reflns_number_total 14916 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt01937b2.cif _cod_data_source_block ch_353m _cod_depositor_comments ; The following automatic conversions were performed: data item '_atom_sites_solution_secondary' value 'diffmap' was changed to 'difmap'. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7705355 _shelx_shelxl_version_number 2017/1 _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_min 0.678 _shelx_estimated_absorpt_t_max 0.890 _shelx_res_file ; TITL ch_353m in P2(1)/c ch_353m.res created by SHELXL-2017/1 at 10:03:27 on 21-Feb-2020 CELL 0.71073 9.8613 19.9793 20.3903 90.000 103.101 90.000 ZERR 4.00 0.0027 0.0060 0.0061 0.000 0.014 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N SI CL GA SB UNIT 140 240 12 8 4 4 4 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.170 SIZE 0.078 0.184 0.275 L.S. 16 ACTA FMAP 2 PLAN 20 DFIX 1.7 sb1 h1 !ohne 1.5 SADI si1 c30 si1 c31 si1 c32 si1' c30' si1' c31' si1' c32' SADI c30 c31 c31 c32 c32 c30 c30' c31' c31' c32' c32' c30' WGHT 0.029800 3.063600 FVAR 0.07142 0.49338 SB1 7 0.366666 0.248338 0.737151 11.00000 0.01373 0.05310 = 0.01311 0.00112 -0.00011 0.00075 GA1 6 0.333570 0.249815 0.862659 11.00000 0.01099 0.01245 = 0.01250 -0.00047 -0.00008 0.00093 CL1 5 0.114835 0.249019 0.872960 11.00000 0.01174 0.02117 = 0.03905 -0.00124 0.00470 0.00067 SI2 4 0.093023 0.327186 0.650856 11.00000 0.01701 0.02120 = 0.02420 0.00484 -0.00123 -0.00057 N1 3 0.419957 0.177020 0.921859 11.00000 0.01269 0.01295 = 0.01396 -0.00006 0.00225 0.00133 N2 3 0.422133 0.322535 0.920132 11.00000 0.01381 0.01295 = 0.01350 0.00014 0.00210 -0.00068 N3 3 0.164288 0.251993 0.683507 11.00000 0.01588 0.02077 = 0.01553 0.00034 -0.00304 -0.00110 C1 1 0.462364 0.187445 0.987631 11.00000 0.01522 0.01753 = 0.01392 0.00181 0.00302 0.00205 C2 1 0.467731 0.250859 1.017876 11.00000 0.02189 0.01774 = 0.01141 -0.00027 0.00282 0.00155 AFIX 43 H2 2 0.477317 0.251229 1.065297 11.00000 -1.20000 AFIX 0 C3 1 0.460699 0.313386 0.986758 11.00000 0.01491 0.01565 = 0.01422 -0.00291 0.00302 0.00007 C4 1 0.513322 0.130352 1.035071 11.00000 0.02905 0.01928 = 0.01756 0.00474 0.00180 0.00464 AFIX 137 H4A 2 0.540277 0.092796 1.009837 11.00000 -1.50000 H4B 2 0.438843 0.116104 1.056643 11.00000 -1.50000 H4C 2 0.593997 0.145010 1.069597 11.00000 -1.50000 AFIX 0 C5 1 0.503845 0.372910 1.031906 11.00000 0.02548 0.01962 = 0.01680 -0.00485 0.00223 -0.00180 AFIX 137 H5A 2 0.578656 0.397034 1.017536 11.00000 -1.50000 H5B 2 0.537073 0.357680 1.078471 11.00000 -1.50000 H5C 2 0.423899 0.402774 1.029109 11.00000 -1.50000 AFIX 0 C6 1 0.428474 0.111430 0.893297 11.00000 0.01455 0.01423 = 0.01411 -0.00017 0.00137 0.00396 C7 1 0.330204 0.061953 0.898464 11.00000 0.01479 0.01386 = 0.02234 0.00074 0.00256 0.00233 C8 1 0.338105 0.000696 0.866148 11.00000 0.02197 0.01438 = 0.02283 -0.00034 0.00174 0.00091 AFIX 43 H8 2 0.272161 -0.033304 0.868717 11.00000 -1.20000 AFIX 0 C9 1 0.439601 -0.011591 0.830535 11.00000 0.02734 0.01671 = 0.02014 -0.00175 0.00399 0.00518 AFIX 43 H9 2 0.442354 -0.053422 0.808723 11.00000 -1.20000 AFIX 0 C10 1 0.536981 0.037323 0.826860 11.00000 0.02244 0.02019 = 0.01743 -0.00053 0.00533 0.00649 AFIX 43 H10 2 0.607555 0.028332 0.803165 11.00000 -1.20000 AFIX 0 C11 1 0.533312 0.099546 0.857318 11.00000 0.01638 0.01838 = 0.01530 0.00157 0.00303 0.00550 C12 1 0.218247 0.070093 0.939070 11.00000 0.02034 0.01667 = 0.03662 -0.00223 0.01297 -0.00038 AFIX 13 H12 2 0.230024 0.115042 0.961209 11.00000 -1.20000 AFIX 0 C13 1 0.232265 0.016313 0.994216 11.00000 0.04182 0.02299 = 0.04349 0.00261 0.02616 -0.00051 AFIX 137 H13A 2 0.209863 -0.027659 0.973260 11.00000 -1.50000 H13B 2 0.167902 0.026367 1.023129 11.00000 -1.50000 H13C 2 0.327958 0.015977 1.021382 11.00000 -1.50000 AFIX 0 C14 1 0.072824 0.066144 0.894360 11.00000 0.01798 0.02926 = 0.06258 -0.00622 0.01158 -0.00082 AFIX 137 H14A 2 0.057572 0.104288 0.863338 11.00000 -1.50000 H14B 2 0.004099 0.067226 0.922335 11.00000 -1.50000 H14C 2 0.062854 0.024367 0.868524 11.00000 -1.50000 AFIX 0 C15 1 0.643307 0.151922 0.853562 11.00000 0.01535 0.02106 = 0.01954 0.00136 0.00517 0.00298 AFIX 13 H15 2 0.594520 0.196007 0.844871 11.00000 -1.20000 AFIX 0 C16 1 0.749777 0.157971 0.920319 11.00000 0.01561 0.03155 = 0.02465 0.00001 0.00188 0.00147 AFIX 137 H16A 2 0.790603 0.113938 0.933663 11.00000 -1.50000 H16B 2 0.703836 0.174663 0.954959 11.00000 -1.50000 H16C 2 0.823364 0.189201 0.915270 11.00000 -1.50000 AFIX 0 C17 1 0.718146 0.140143 0.796190 11.00000 0.02456 0.03269 = 0.02694 -0.00145 0.01301 0.00023 AFIX 137 H17A 2 0.649173 0.136426 0.753399 11.00000 -1.50000 H17B 2 0.772408 0.098681 0.804623 11.00000 -1.50000 H17C 2 0.780599 0.177807 0.793949 11.00000 -1.50000 AFIX 0 C18 1 0.448489 0.386659 0.892482 11.00000 0.01588 0.01377 = 0.01437 -0.00096 0.00216 -0.00211 C19 1 0.349549 0.437896 0.885233 11.00000 0.01790 0.01428 = 0.01785 -0.00076 0.00205 0.00007 C20 1 0.381359 0.499040 0.858576 11.00000 0.02564 0.01545 = 0.02067 0.00092 0.00388 -0.00005 AFIX 43 H20 2 0.314652 0.534138 0.852113 11.00000 -1.20000 AFIX 0 C21 1 0.507956 0.509501 0.841412 11.00000 0.03187 0.01762 = 0.01975 0.00144 0.00761 -0.00545 AFIX 43 H21 2 0.528089 0.551707 0.824368 11.00000 -1.20000 AFIX 0 C22 1 0.604488 0.458583 0.849118 11.00000 0.02425 0.02234 = 0.02375 -0.00118 0.00965 -0.00640 AFIX 43 H22 2 0.691147 0.466050 0.837383 11.00000 -1.20000 AFIX 0 C23 1 0.576682 0.396069 0.873969 11.00000 0.01927 0.01748 = 0.02130 -0.00217 0.00700 -0.00277 C24 1 0.210931 0.430017 0.905053 11.00000 0.01862 0.01644 = 0.02959 0.00187 0.00791 0.00168 AFIX 13 H24 2 0.211017 0.385835 0.928107 11.00000 -1.20000 AFIX 0 C25 1 0.186497 0.485068 0.953742 11.00000 0.03450 0.01981 = 0.04090 0.00070 0.02093 0.00471 AFIX 137 H25A 2 0.179034 0.528530 0.930922 11.00000 -1.50000 H25B 2 0.264748 0.485976 0.993151 11.00000 -1.50000 H25C 2 0.100128 0.475802 0.968199 11.00000 -1.50000 AFIX 0 C26 1 0.093736 0.429631 0.842182 11.00000 0.02025 0.03837 = 0.04188 0.00657 0.00122 -0.00112 AFIX 137 H26A 2 0.096795 0.471018 0.816762 11.00000 -1.50000 H26B 2 0.004097 0.426536 0.855115 11.00000 -1.50000 H26C 2 0.104706 0.391090 0.814109 11.00000 -1.50000 AFIX 0 C27 1 0.687186 0.341795 0.882327 11.00000 0.01783 0.02168 = 0.03024 -0.00033 0.00852 -0.00101 AFIX 13 H27 2 0.643856 0.298881 0.892427 11.00000 -1.20000 AFIX 0 C28 1 0.808628 0.357133 0.941312 11.00000 0.02757 0.04336 = 0.02816 -0.00137 0.00346 0.00847 AFIX 137 H28A 2 0.880583 0.322756 0.944045 11.00000 -1.50000 H28B 2 0.775760 0.357457 0.983208 11.00000 -1.50000 H28C 2 0.847649 0.401051 0.934620 11.00000 -1.50000 AFIX 0 C29 1 0.740229 0.331497 0.817757 11.00000 0.01773 0.03590 = 0.03072 -0.00995 0.00765 -0.00280 AFIX 137 H29A 2 0.662567 0.318050 0.780992 11.00000 -1.50000 H29B 2 0.811643 0.296465 0.825293 11.00000 -1.50000 H29C 2 0.780301 0.373411 0.805808 11.00000 -1.50000 AFIX 0 PART 1 21 SI1 4 0.096050 0.175815 0.654200 21.00000 0.01846 0.01987 = 0.02265 -0.00242 0.00304 -0.00223 C30 1 0.156599 0.109335 0.717900 21.00000 0.06027 0.03583 = 0.05993 0.00771 0.00216 -0.00765 AFIX 137 H30A 2 0.100491 0.068894 0.705322 21.00000 -1.50000 H30B 2 0.146575 0.124875 0.762142 21.00000 -1.50000 H30C 2 0.254650 0.099190 0.719814 21.00000 -1.50000 AFIX 0 C31 1 -0.097561 0.178386 0.639629 21.00000 0.02967 0.03963 = 0.03529 -0.01062 0.01077 -0.00829 AFIX 137 H31A 2 -0.133661 0.215411 0.609126 21.00000 -1.50000 H31B 2 -0.124179 0.185033 0.682650 21.00000 -1.50000 H31C 2 -0.136570 0.136064 0.619456 21.00000 -1.50000 AFIX 0 C32 1 0.145242 0.149568 0.574418 21.00000 0.03596 0.04732 = 0.04038 -0.02285 0.01326 -0.00153 AFIX 137 H32A 2 0.127511 0.186511 0.541979 21.00000 -1.50000 H32B 2 0.089628 0.110606 0.555429 21.00000 -1.50000 H32C 2 0.244301 0.137868 0.584139 21.00000 -1.50000 AFIX 0 PART 2 -21 SI1' 4 0.079273 0.175305 0.660997 -21.00000 0.02622 0.02215 = 0.02087 -0.00147 0.00037 -0.00744 C30' 1 0.110520 0.114269 0.732114 -21.00000 0.08924 0.02437 = 0.04233 0.01460 -0.01429 -0.02231 AFIX 137 H30E 2 0.052282 0.074584 0.718999 -21.00000 -1.50000 H30D 2 0.086877 0.135062 0.771604 -21.00000 -1.50000 H30F 2 0.208812 0.101108 0.743088 -21.00000 -1.50000 AFIX 0 C31' 1 -0.113161 0.187081 0.636423 -21.00000 0.02311 0.03975 = 0.04392 -0.01655 0.01332 -0.02040 AFIX 137 H31E 2 -0.137320 0.213451 0.594879 -21.00000 -1.50000 H31D 2 -0.144437 0.210686 0.672466 -21.00000 -1.50000 H31F 2 -0.158871 0.143296 0.629007 -21.00000 -1.50000 AFIX 0 C32' 1 0.141952 0.138252 0.589374 -21.00000 0.03437 0.03901 = 0.04445 -0.01325 0.00564 -0.00024 AFIX 137 H32E 2 0.110327 0.165912 0.549117 -21.00000 -1.20000 H32D 2 0.104573 0.092864 0.580572 -21.00000 -1.20000 H32F 2 0.243919 0.136493 0.600763 -21.00000 -1.20000 AFIX 0 PART 0 C33 1 -0.068579 0.346187 0.680878 11.00000 0.02177 0.03891 = 0.07570 -0.01494 0.00702 0.00538 AFIX 137 H33A 2 -0.079292 0.394780 0.683883 11.00000 -1.50000 H33B 2 -0.061563 0.326123 0.725380 11.00000 -1.50000 H33C 2 -0.149528 0.327611 0.649097 11.00000 -1.50000 AFIX 0 C34 1 0.214304 0.399159 0.675182 11.00000 0.03351 0.02785 = 0.04770 0.00167 0.00675 -0.00813 AFIX 137 H34A 2 0.295835 0.393120 0.655834 11.00000 -1.50000 H34B 2 0.244218 0.401380 0.724360 11.00000 -1.50000 H34C 2 0.166616 0.440813 0.658139 11.00000 -1.50000 AFIX 0 C35 1 0.050877 0.324286 0.556960 11.00000 0.06098 0.05071 = 0.02653 0.01751 -0.00925 -0.01131 AFIX 137 H35A 2 0.013156 0.367625 0.539005 11.00000 -1.50000 H35B 2 -0.018294 0.289183 0.541297 11.00000 -1.50000 H35C 2 0.135633 0.314528 0.541258 11.00000 -1.50000 AFIX 0 REM ##### H1 2 0.431637 0.325950 0.738571 11.00000 -1.20000 HKLF 4 REM ch_353m in P2(1)/c REM R1 = 0.0292 for 10070 Fo > 4sig(Fo) and 0.0555 for all 14916 data REM 447 parameters refined using 31 restraints END WGHT 0.0298 3.0638 REM Highest difference peak 1.852, deepest hole -0.607, 1-sigma level 0.080 Q1 1 0.3302 0.2163 0.7404 11.00000 0.05 1.85 Q2 1 0.3266 0.2738 0.7460 11.00000 0.05 1.17 Q3 1 0.3632 0.2485 0.7036 11.00000 0.05 0.66 Q4 1 0.4330 0.5104 0.8356 11.00000 0.05 0.63 Q5 1 0.4499 0.2200 0.9982 11.00000 0.05 0.62 Q6 1 0.4503 0.2803 0.9990 11.00000 0.05 0.59 Q7 1 0.3773 0.0864 0.8915 11.00000 0.05 0.59 Q8 1 0.4011 0.4191 0.8965 11.00000 0.05 0.58 Q9 1 0.4483 0.2704 0.7351 11.00000 0.05 0.55 Q10 1 0.4085 0.2426 0.7665 11.00000 0.05 0.53 Q11 1 0.2831 0.2504 0.8844 11.00000 0.05 0.52 Q12 1 0.3853 0.0014 0.8473 11.00000 0.05 0.50 Q13 1 0.7456 0.3425 0.9200 11.00000 0.05 0.47 Q14 1 0.3417 0.2512 0.8245 11.00000 0.05 0.47 Q15 1 0.4379 0.3225 0.9530 11.00000 0.05 0.46 Q16 1 0.6871 0.1535 0.8824 11.00000 0.05 0.46 Q17 1 0.4821 0.1600 1.0114 11.00000 0.05 0.46 Q18 1 0.5326 0.4702 0.8309 11.00000 0.05 0.46 Q19 1 0.5919 0.1295 0.8584 11.00000 0.05 0.45 Q20 1 0.5040 0.3896 0.8753 11.00000 0.05 0.45 ; _shelx_res_checksum 87652 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 Sb1 Sb 0.36667(2) 0.24834(2) 0.73715(2) 0.02715(4) Uani 1 1 d D . . . . Ga1 Ga 0.33357(2) 0.24982(2) 0.86266(2) 0.01241(4) Uani 1 1 d . . . . . Cl1 Cl 0.11484(4) 0.24902(2) 0.87296(2) 0.02415(8) Uani 1 1 d . . . . . Si2 Si 0.09302(5) 0.32719(2) 0.65086(2) 0.02174(10) Uani 1 1 d . . . . . N1 N 0.41996(12) 0.17702(6) 0.92186(6) 0.0133(2) Uani 1 1 d . . . . . N2 N 0.42213(12) 0.32253(6) 0.92013(6) 0.0136(2) Uani 1 1 d . . . . . N3 N 0.16429(13) 0.25199(7) 0.68351(7) 0.0184(2) Uani 1 1 d . . . . . C1 C 0.46236(15) 0.18744(8) 0.98763(7) 0.0156(3) Uani 1 1 d . . . . . C2 C 0.46773(16) 0.25086(8) 1.01788(7) 0.0172(2) Uani 1 1 d . . . . . H2 H 0.477317 0.251229 1.065297 0.021 Uiso 1 1 calc R U . . . C3 C 0.46070(15) 0.31339(7) 0.98676(7) 0.0150(3) Uani 1 1 d . . . . . C4 C 0.51332(19) 0.13035(8) 1.03507(8) 0.0225(3) Uani 1 1 d . . . . . H4A H 0.540277 0.092796 1.009837 0.034 Uiso 1 1 calc R U . . . H4B H 0.438843 0.116104 1.056643 0.034 Uiso 1 1 calc R U . . . H4C H 0.593997 0.145010 1.069597 0.034 Uiso 1 1 calc R U . . . C5 C 0.50384(18) 0.37291(8) 1.03191(8) 0.0210(3) Uani 1 1 d . . . . . H5A H 0.578656 0.397034 1.017536 0.032 Uiso 1 1 calc R U . . . H5B H 0.537073 0.357680 1.078471 0.032 Uiso 1 1 calc R U . . . H5C H 0.423899 0.402774 1.029109 0.032 Uiso 1 1 calc R U . . . C6 C 0.42847(15) 0.11143(7) 0.89330(7) 0.0146(3) Uani 1 1 d . . . . . C7 C 0.33020(15) 0.06195(8) 0.89846(8) 0.0173(3) Uani 1 1 d . . . . . C8 C 0.33810(17) 0.00070(8) 0.86615(8) 0.0203(3) Uani 1 1 d . . . . . H8 H 0.272161 -0.033304 0.868717 0.024 Uiso 1 1 calc R U . . . C9 C 0.43960(18) -0.01159(8) 0.83054(8) 0.0216(3) Uani 1 1 d . . . . . H9 H 0.442354 -0.053422 0.808723 0.026 Uiso 1 1 calc R U . . . C10 C 0.53698(17) 0.03732(8) 0.82686(8) 0.0199(3) Uani 1 1 d . . . . . H10 H 0.607555 0.028332 0.803165 0.024 Uiso 1 1 calc R U . . . C11 C 0.53331(15) 0.09955(8) 0.85732(8) 0.0168(3) Uani 1 1 d . . . . . C12 C 0.21825(17) 0.07009(8) 0.93907(10) 0.0235(3) Uani 1 1 d . . . . . H12 H 0.230024 0.115042 0.961209 0.028 Uiso 1 1 calc R U . . . C13 C 0.2323(2) 0.01631(10) 0.99422(11) 0.0335(4) Uani 1 1 d . . . . . H13A H 0.209863 -0.027659 0.973260 0.050 Uiso 1 1 calc R U . . . H13B H 0.167902 0.026367 1.023129 0.050 Uiso 1 1 calc R U . . . H13C H 0.327958 0.015977 1.021382 0.050 Uiso 1 1 calc R U . . . C14 C 0.07282(19) 0.06614(10) 0.89436(12) 0.0362(5) Uani 1 1 d . . . . . H14A H 0.057572 0.104288 0.863338 0.054 Uiso 1 1 calc R U . . . H14B H 0.004099 0.067226 0.922335 0.054 Uiso 1 1 calc R U . . . H14C H 0.062854 0.024367 0.868524 0.054 Uiso 1 1 calc R U . . . C15 C 0.64331(16) 0.15192(8) 0.85356(8) 0.0185(3) Uani 1 1 d . . . . . H15 H 0.594520 0.196007 0.844871 0.022 Uiso 1 1 calc R U . . . C16 C 0.74978(17) 0.15797(9) 0.92032(9) 0.0244(3) Uani 1 1 d . . . . . H16A H 0.790603 0.113938 0.933663 0.037 Uiso 1 1 calc R U . . . H16B H 0.703836 0.174663 0.954959 0.037 Uiso 1 1 calc R U . . . H16C H 0.823364 0.189201 0.915270 0.037 Uiso 1 1 calc R U . . . C17 C 0.71815(19) 0.14014(10) 0.79619(9) 0.0269(4) Uani 1 1 d . . . . . H17A H 0.649173 0.136426 0.753399 0.040 Uiso 1 1 calc R U . . . H17B H 0.772408 0.098681 0.804623 0.040 Uiso 1 1 calc R U . . . H17C H 0.780599 0.177807 0.793949 0.040 Uiso 1 1 calc R U . . . C18 C 0.44849(15) 0.38666(7) 0.89248(7) 0.0149(3) Uani 1 1 d . . . . . C19 C 0.34955(16) 0.43790(8) 0.88523(8) 0.0170(3) Uani 1 1 d . . . . . C20 C 0.38136(18) 0.49904(8) 0.85858(8) 0.0208(3) Uani 1 1 d . . . . . H20 H 0.314652 0.534138 0.852113 0.025 Uiso 1 1 calc R U . . . C21 C 0.50796(19) 0.50950(8) 0.84141(8) 0.0228(3) Uani 1 1 d . . . . . H21 H 0.528089 0.551707 0.824368 0.027 Uiso 1 1 calc R U . . . C22 C 0.60449(18) 0.45858(9) 0.84912(9) 0.0228(3) Uani 1 1 d . . . . . H22 H 0.691147 0.466050 0.837383 0.027 Uiso 1 1 calc R U . . . C23 C 0.57668(16) 0.39607(8) 0.87397(8) 0.0190(3) Uani 1 1 d . . . . . C24 C 0.21093(16) 0.43002(8) 0.90505(9) 0.0212(3) Uani 1 1 d . . . . . H24 H 0.211017 0.385835 0.928107 0.025 Uiso 1 1 calc R U . . . C25 C 0.1865(2) 0.48507(9) 0.95374(10) 0.0298(4) Uani 1 1 d . . . . . H25A H 0.179034 0.528530 0.930922 0.045 Uiso 1 1 calc R U . . . H25B H 0.264748 0.485976 0.993151 0.045 Uiso 1 1 calc R U . . . H25C H 0.100128 0.475802 0.968199 0.045 Uiso 1 1 calc R U . . . C26 C 0.09374(19) 0.42963(11) 0.84218(11) 0.0344(4) Uani 1 1 d . . . . . H26A H 0.096795 0.471018 0.816762 0.052 Uiso 1 1 calc R U . . . H26B H 0.004097 0.426536 0.855115 0.052 Uiso 1 1 calc R U . . . H26C H 0.104706 0.391090 0.814109 0.052 Uiso 1 1 calc R U . . . C27 C 0.68719(17) 0.34179(9) 0.88233(9) 0.0228(3) Uani 1 1 d . . . . . H27 H 0.643856 0.298881 0.892427 0.027 Uiso 1 1 calc R U . . . C28 C 0.8086(2) 0.35713(11) 0.94131(10) 0.0335(4) Uani 1 1 d . . . . . H28A H 0.880583 0.322756 0.944045 0.050 Uiso 1 1 calc R U . . . H28B H 0.775760 0.357457 0.983208 0.050 Uiso 1 1 calc R U . . . H28C H 0.847649 0.401051 0.934620 0.050 Uiso 1 1 calc R U . . . C29 C 0.74023(18) 0.33150(10) 0.81776(10) 0.0278(4) Uani 1 1 d . . . . . H29A H 0.662567 0.318050 0.780992 0.042 Uiso 1 1 calc R U . . . H29B H 0.811643 0.296465 0.825293 0.042 Uiso 1 1 calc R U . . . H29C H 0.780301 0.373411 0.805808 0.042 Uiso 1 1 calc R U . . . Si1 Si 0.0961(9) 0.1758(5) 0.6542(5) 0.0206(8) Uani 0.49(3) 1 d D . P A 1 C30 C 0.1566(14) 0.1093(6) 0.7179(8) 0.054(2) Uani 0.49(3) 1 d D . P A 1 H30A H 0.100491 0.068894 0.705322 0.081 Uiso 0.49(3) 1 calc R U P A 1 H30B H 0.146575 0.124875 0.762142 0.081 Uiso 0.49(3) 1 calc R U P A 1 H30C H 0.254650 0.099190 0.719814 0.081 Uiso 0.49(3) 1 calc R U P A 1 C31 C -0.0976(11) 0.1784(10) 0.6396(9) 0.034(2) Uani 0.49(3) 1 d D . P A 1 H31A H -0.133661 0.215411 0.609126 0.051 Uiso 0.49(3) 1 calc R U P A 1 H31B H -0.124179 0.185033 0.682650 0.051 Uiso 0.49(3) 1 calc R U P A 1 H31C H -0.136570 0.136064 0.619456 0.051 Uiso 0.49(3) 1 calc R U P A 1 C32 C 0.1452(19) 0.1496(9) 0.5744(7) 0.040(3) Uani 0.49(3) 1 d D . P A 1 H32A H 0.127511 0.186511 0.541979 0.061 Uiso 0.49(3) 1 calc R U P A 1 H32B H 0.089628 0.110606 0.555429 0.061 Uiso 0.49(3) 1 calc R U P A 1 H32C H 0.244301 0.137868 0.584139 0.061 Uiso 0.49(3) 1 calc R U P A 1 Si1' Si 0.0793(12) 0.1753(5) 0.6610(5) 0.0239(10) Uani 0.51(3) 1 d D . P A 2 C30' C 0.111(2) 0.1143(5) 0.7321(6) 0.057(4) Uani 0.51(3) 1 d D . P A 2 H30E H 0.052282 0.074584 0.718999 0.085 Uiso 0.51(3) 1 calc R U P A 2 H30D H 0.086877 0.135062 0.771604 0.085 Uiso 0.51(3) 1 calc R U P A 2 H30F H 0.208812 0.101108 0.743088 0.085 Uiso 0.51(3) 1 calc R U P A 2 C31' C -0.1132(12) 0.1871(10) 0.6364(9) 0.035(2) Uani 0.51(3) 1 d D . P A 2 H31E H -0.137320 0.213451 0.594879 0.052 Uiso 0.51(3) 1 calc R U P A 2 H31D H -0.144437 0.210686 0.672466 0.052 Uiso 0.51(3) 1 calc R U P A 2 H31F H -0.158871 0.143296 0.629007 0.052 Uiso 0.51(3) 1 calc R U P A 2 C32' C 0.1420(18) 0.1383(8) 0.5894(8) 0.040(2) Uani 0.51(3) 1 d D . P A 2 H32E H 0.110327 0.165912 0.549117 0.048 Uiso 0.51(3) 1 calc R U P A 2 H32D H 0.104573 0.092864 0.580572 0.048 Uiso 0.51(3) 1 calc R U P A 2 H32F H 0.243919 0.136493 0.600763 0.048 Uiso 0.51(3) 1 calc R U P A 2 C33 C -0.0686(2) 0.34619(12) 0.68088(14) 0.0461(6) Uani 1 1 d . . . . . H33A H -0.079292 0.394780 0.683883 0.069 Uiso 1 1 calc R U . . . H33B H -0.061563 0.326123 0.725380 0.069 Uiso 1 1 calc R U . . . H33C H -0.149528 0.327611 0.649097 0.069 Uiso 1 1 calc R U . . . C34 C 0.2143(2) 0.39916(10) 0.67518(12) 0.0367(5) Uani 1 1 d . . . . . H34A H 0.295835 0.393120 0.655834 0.055 Uiso 1 1 calc R U . . . H34B H 0.244218 0.401380 0.724360 0.055 Uiso 1 1 calc R U . . . H34C H 0.166616 0.440813 0.658139 0.055 Uiso 1 1 calc R U . . . C35 C 0.0509(3) 0.32429(13) 0.55696(11) 0.0491(6) Uani 1 1 d . . . . . H35A H 0.013156 0.367625 0.539005 0.074 Uiso 1 1 calc R U . . . H35B H -0.018294 0.289183 0.541297 0.074 Uiso 1 1 calc R U . . . H35C H 0.135633 0.314528 0.541258 0.074 Uiso 1 1 calc R U . . . H1 H 0.432(3) 0.3260(9) 0.7386(14) 0.059 Uiso 1 1 d D U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.01373(5) 0.05310(8) 0.01311(5) 0.00112(5) -0.00011(3) 0.00075(5) Ga1 0.01099(6) 0.01245(7) 0.01250(7) -0.00047(6) -0.00008(5) 0.00093(6) Cl1 0.01174(14) 0.02117(17) 0.0390(2) -0.00124(17) 0.00470(13) 0.00067(14) Si2 0.0170(2) 0.0212(2) 0.0242(2) 0.00484(18) -0.00123(17) -0.00057(16) N1 0.0127(5) 0.0129(6) 0.0140(5) -0.0001(4) 0.0023(4) 0.0013(4) N2 0.0138(5) 0.0130(6) 0.0135(5) 0.0001(4) 0.0021(4) -0.0007(4) N3 0.0159(5) 0.0208(6) 0.0155(5) 0.0003(5) -0.0030(4) -0.0011(5) C1 0.0152(6) 0.0175(7) 0.0139(6) 0.0018(5) 0.0030(5) 0.0020(5) C2 0.0219(6) 0.0177(6) 0.0114(6) -0.0003(6) 0.0028(5) 0.0016(6) C3 0.0149(6) 0.0157(7) 0.0142(6) -0.0029(5) 0.0030(5) 0.0001(5) C4 0.0290(8) 0.0193(8) 0.0176(7) 0.0047(6) 0.0018(6) 0.0046(6) C5 0.0255(8) 0.0196(8) 0.0168(7) -0.0048(6) 0.0022(6) -0.0018(6) C6 0.0145(6) 0.0142(6) 0.0141(6) -0.0002(5) 0.0014(5) 0.0040(5) C7 0.0148(6) 0.0139(6) 0.0223(7) 0.0007(5) 0.0026(5) 0.0023(5) C8 0.0220(7) 0.0144(7) 0.0228(8) -0.0003(6) 0.0017(6) 0.0009(5) C9 0.0273(8) 0.0167(7) 0.0201(7) -0.0017(6) 0.0040(6) 0.0052(6) C10 0.0224(7) 0.0202(7) 0.0174(7) -0.0005(6) 0.0053(6) 0.0065(6) C11 0.0164(6) 0.0184(7) 0.0153(7) 0.0016(5) 0.0030(5) 0.0055(5) C12 0.0203(7) 0.0167(7) 0.0366(10) -0.0022(6) 0.0130(7) -0.0004(6) C13 0.0418(11) 0.0230(9) 0.0435(11) 0.0026(8) 0.0262(9) -0.0005(8) C14 0.0180(8) 0.0293(10) 0.0626(14) -0.0062(9) 0.0116(8) -0.0008(7) C15 0.0154(6) 0.0211(7) 0.0195(7) 0.0014(6) 0.0052(5) 0.0030(5) C16 0.0156(7) 0.0316(9) 0.0247(8) 0.0000(7) 0.0019(6) 0.0015(6) C17 0.0246(8) 0.0327(9) 0.0269(9) -0.0015(7) 0.0130(7) 0.0002(7) C18 0.0159(6) 0.0138(6) 0.0144(6) -0.0010(5) 0.0022(5) -0.0021(5) C19 0.0179(7) 0.0143(7) 0.0179(7) -0.0008(5) 0.0021(5) 0.0001(5) C20 0.0256(8) 0.0155(7) 0.0207(7) 0.0009(6) 0.0039(6) 0.0000(6) C21 0.0319(9) 0.0176(7) 0.0198(7) 0.0014(6) 0.0076(6) -0.0055(6) C22 0.0242(8) 0.0223(8) 0.0237(8) -0.0012(6) 0.0096(6) -0.0064(6) C23 0.0193(7) 0.0175(7) 0.0213(7) -0.0022(6) 0.0070(6) -0.0028(5) C24 0.0186(7) 0.0164(7) 0.0296(9) 0.0019(6) 0.0079(6) 0.0017(5) C25 0.0345(9) 0.0198(8) 0.0409(11) 0.0007(7) 0.0209(8) 0.0047(7) C26 0.0203(8) 0.0384(11) 0.0419(11) 0.0066(9) 0.0012(7) -0.0011(7) C27 0.0178(7) 0.0217(8) 0.0302(9) -0.0003(6) 0.0085(6) -0.0010(6) C28 0.0276(9) 0.0434(11) 0.0282(9) -0.0014(8) 0.0035(7) 0.0085(8) C29 0.0177(7) 0.0359(10) 0.0307(9) -0.0099(8) 0.0077(6) -0.0028(7) Si1 0.0185(12) 0.0199(11) 0.0227(17) -0.0024(10) 0.0030(9) -0.0022(9) C30 0.060(5) 0.036(3) 0.060(5) 0.008(3) 0.002(4) -0.008(3) C31 0.030(4) 0.040(5) 0.035(4) -0.011(3) 0.011(3) -0.008(3) C32 0.036(3) 0.047(6) 0.040(5) -0.023(4) 0.013(4) -0.002(4) Si1' 0.026(2) 0.0221(10) 0.0209(14) -0.0015(9) 0.0004(12) -0.0074(13) C30' 0.089(8) 0.024(3) 0.042(4) 0.015(3) -0.014(4) -0.022(4) C31' 0.023(3) 0.040(5) 0.044(5) -0.017(3) 0.013(3) -0.020(3) C32' 0.034(3) 0.039(4) 0.044(5) -0.013(4) 0.006(4) 0.000(3) C33 0.0218(9) 0.0389(12) 0.0757(18) -0.0149(12) 0.0070(10) 0.0054(8) C34 0.0335(10) 0.0279(10) 0.0477(12) 0.0017(9) 0.0067(9) -0.0081(8) C35 0.0610(15) 0.0507(14) 0.0265(10) 0.0175(10) -0.0092(10) -0.0113(12) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N3 Sb1 Ga1 101.35(4) . . ? N2 Ga1 N1 96.33(6) . . ? N2 Ga1 Cl1 105.20(4) . . ? N1 Ga1 Cl1 103.49(4) . . ? N2 Ga1 Sb1 116.94(4) . . ? N1 Ga1 Sb1 117.08(4) . . ? Cl1 Ga1 Sb1 115.279(19) . . ? N3 Si2 C34 112.83(9) . . ? N3 Si2 C35 110.19(10) . . ? C34 Si2 C35 106.10(11) . . ? N3 Si2 C33 110.66(10) . . ? C34 Si2 C33 107.40(11) . . ? C35 Si2 C33 109.51(13) . . ? C1 N1 C6 121.06(12) . . ? C1 N1 Ga1 119.98(10) . . ? C6 N1 Ga1 118.85(9) . . ? C3 N2 C18 118.81(12) . . ? C3 N2 Ga1 119.69(10) . . ? C18 N2 Ga1 121.50(10) . . ? Si1 N3 Si2 123.0(3) . . ? Si2 N3 Si1' 122.0(3) . . ? Si1 N3 Sb1 114.3(3) . . ? Si2 N3 Sb1 119.94(7) . . ? Si1' N3 Sb1 117.3(3) . . ? N1 C1 C2 123.84(14) . . ? N1 C1 C4 120.85(14) . . ? C2 C1 C4 115.29(13) . . ? C3 C2 C1 127.92(13) . . ? N2 C3 C2 123.87(13) . . ? N2 C3 C5 119.28(14) . . ? C2 C3 C5 116.82(13) . . ? C7 C6 C11 121.17(14) . . ? C7 C6 N1 120.27(13) . . ? C11 C6 N1 118.48(13) . . ? C8 C7 C6 117.82(14) . . ? C8 C7 C12 118.10(14) . . ? C6 C7 C12 124.05(14) . . ? C9 C8 C7 121.69(15) . . ? C10 C9 C8 119.73(15) . . ? C9 C10 C11 121.15(15) . . ? C10 C11 C6 118.42(15) . . ? C10 C11 C15 120.01(14) . . ? C6 C11 C15 121.53(14) . . ? C14 C12 C7 111.64(16) . . ? C14 C12 C13 108.60(16) . . ? C7 C12 C13 111.38(14) . . ? C11 C15 C16 111.36(13) . . ? C11 C15 C17 113.83(14) . . ? C16 C15 C17 109.86(13) . . ? C19 C18 C23 121.32(14) . . ? C19 C18 N2 120.44(13) . . ? C23 C18 N2 118.23(13) . . ? C18 C19 C20 117.84(15) . . ? C18 C19 C24 122.98(14) . . ? C20 C19 C24 119.19(14) . . ? C21 C20 C19 121.52(15) . . ? C22 C21 C20 119.88(15) . . ? C21 C22 C23 120.92(15) . . ? C22 C23 C18 118.49(15) . . ? C22 C23 C27 118.92(14) . . ? C18 C23 C27 122.55(14) . . ? C19 C24 C26 109.54(15) . . ? C19 C24 C25 112.34(14) . . ? C26 C24 C25 110.37(15) . . ? C23 C27 C28 111.13(15) . . ? C23 C27 C29 111.98(15) . . ? C28 C27 C29 110.12(14) . . ? N3 Si1 C30 110.6(6) . . ? N3 Si1 C31 109.7(8) . . ? C30 Si1 C31 106.6(6) . . ? N3 Si1 C32 113.1(7) . . ? C30 Si1 C32 107.5(6) . . ? C31 Si1 C32 109.0(7) . . ? N3 Si1' C32' 109.1(7) . . ? N3 Si1' C31' 110.9(7) . . ? C32' Si1' C31' 109.7(6) . . ? N3 Si1' C30' 112.5(6) . . ? C32' Si1' C30' 108.9(6) . . ? C31' Si1' C30' 105.7(6) . . ? 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 Sb1 N3 2.0482(14) . ? Sb1 Ga1 2.6524(8) . ? Ga1 N2 1.9450(13) . ? Ga1 N1 1.9575(13) . ? Ga1 Cl1 2.2141(7) . ? Si2 N3 1.7268(15) . ? Si2 C34 1.864(2) . ? Si2 C35 1.866(2) . ? Si2 C33 1.871(2) . ? N1 C1 1.3276(19) . ? N1 C6 1.4442(19) . ? N2 C3 1.3377(19) . ? N2 C18 1.4468(19) . ? N3 Si1 1.716(11) . ? N3 Si1' 1.757(11) . ? C1 C2 1.405(2) . ? C1 C4 1.506(2) . ? C2 C3 1.396(2) . ? C3 C5 1.505(2) . ? C6 C7 1.405(2) . ? C6 C11 1.417(2) . ? C7 C8 1.401(2) . ? C7 C12 1.531(2) . ? C8 C9 1.385(2) . ? C9 C10 1.384(2) . ? C10 C11 1.394(2) . ? C11 C15 1.522(2) . ? C12 C14 1.517(3) . ? C12 C13 1.539(3) . ? C15 C16 1.524(2) . ? C15 C17 1.536(2) . ? C18 C19 1.399(2) . ? C18 C23 1.411(2) . ? C19 C20 1.401(2) . ? C19 C24 1.519(2) . ? C20 C21 1.387(2) . ? C21 C22 1.378(3) . ? C22 C23 1.398(2) . ? C23 C27 1.519(2) . ? C24 C26 1.519(3) . ? C24 C25 1.537(2) . ? C27 C28 1.524(3) . ? C27 C29 1.537(2) . ? Si1 C30 1.859(9) . ? Si1 C31 1.865(10) . ? Si1 C32 1.875(9) . ? Si1' C32' 1.863(9) . ? Si1' C31' 1.865(9) . ? Si1' C30' 1.866(8) . ?