#------------------------------------------------------------------------------ #$Date: 2019-11-29 03:32:54 +0200 (Fri, 29 Nov 2019) $ #$Revision: 244791 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125617.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_7125617 loop_ _publ_author_name 'Khan, Shabana' 'Parvin, Nasrina' 'Hossain, Jabed' 'George, Anjana' 'Parameswaran, Pattiyil' _publ_section_title ; N-heterocyclic silylene stabilized monocordinated copper(I)-arene cationic complexes and their application in Click chemistry ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC09115G _journal_year 2019 _chemical_formula_moiety 'C28 H49 Cu N3 Si3, SbF6 ' _chemical_formula_sum 'C28 H49 Cu F6 N3 Sb Si3' _chemical_formula_weight 811.26 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-02-11 deposited with the CCDC. 2019-11-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.762(6) _cell_length_b 14.725(7) _cell_length_c 21.300(9) _cell_measurement_reflns_used 9469 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 21.83 _cell_measurement_theta_min 2.36 _cell_volume 3689(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0983 _diffrn_reflns_av_unetI/netI 0.0487 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 81475 _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 25.249 _diffrn_reflns_theta_min 2.216 _exptl_absorpt_coefficient_mu 1.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sheldrick, G. M. (2012) SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.461 _exptl_crystal_description block _exptl_crystal_F_000 1656 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max 0.1876 _exptl_transmission_factor_min 0.1564 _refine_diff_density_max 0.567 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.073 _refine_ls_abs_structure_details ; Flack x determined using 1819 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.071(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 392 _refine_ls_number_reflns 6657 _refine_ls_number_restraints 24 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0442 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+4.5547P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0931 _refine_ls_wR_factor_ref 0.1065 _reflns_Friedel_coverage 0.784 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 5034 _reflns_number_total 6657 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09115g2.cif _cod_data_source_block 4_a _cod_database_code 7125617 _shelx_shelxl_version_number 2014/7 _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_res_file ; 4_a.res created by SHELXL-2014/7 TITL 4_a.res in P2(1)2(1)2(1) CELL 0.71073 11.7622 14.7254 21.3005 90.000 90.000 90.000 ZERR 4.000 0.0055 0.0070 0.0094 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N F Si Cu Sb UNIT 112 196 12 24 12 4 4 OMIT -3 50.5 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 ISOR 0.001 C26 C28 ISOR 0.1 F4 F6 TEMP 23.000 WGHT 0.042200 4.554700 FVAR 0.26430 C1 1 0.699093 0.657458 0.249455 11.00000 0.03112 0.03472 = 0.04306 -0.00125 0.00255 0.00211 C2 1 0.698461 0.693227 0.184875 11.00000 0.05691 0.03236 = 0.03519 0.00148 -0.00496 0.00127 C3 1 0.753153 0.799634 0.312910 11.00000 0.04379 0.02971 = 0.04841 0.00243 -0.00029 -0.00421 C4 1 0.677605 0.486509 0.230242 11.00000 0.05252 0.03459 = 0.04098 -0.00773 -0.00065 0.00275 C5 1 0.799919 0.701431 0.151796 11.00000 0.06259 0.04383 = 0.03985 -0.00624 0.00691 -0.00738 AFIX 43 H5 2 0.868494 0.683773 0.169777 11.00000 -1.20000 AFIX 0 C6 1 0.796526 0.736520 0.091420 11.00000 0.09694 0.04806 = 0.04416 0.00090 0.01911 -0.01402 AFIX 43 H6 2 0.863404 0.742216 0.068464 11.00000 -1.20000 AFIX 0 C7 1 0.597619 0.718754 0.157802 11.00000 0.06188 0.04340 = 0.04462 0.00145 -0.00086 0.00159 AFIX 43 H7 2 0.530288 0.713405 0.180390 11.00000 -1.20000 AFIX 0 C8 1 0.592022 0.491165 0.176794 11.00000 0.08614 0.06207 = 0.06067 -0.01903 -0.01746 -0.00945 AFIX 137 H8A 2 0.519868 0.511012 0.192776 11.00000 -1.50000 H8B 2 0.583862 0.432107 0.158246 11.00000 -1.50000 H8C 2 0.618329 0.533314 0.145630 11.00000 -1.50000 AFIX 0 C9 1 0.641916 0.413009 0.275779 11.00000 0.09465 0.03274 = 0.05750 -0.00626 -0.00146 -0.01111 AFIX 137 H9A 2 0.698380 0.406983 0.308055 11.00000 -1.50000 H9B 2 0.634386 0.356437 0.253770 11.00000 -1.50000 H9C 2 0.570334 0.428964 0.294410 11.00000 -1.50000 AFIX 0 C10 1 0.689749 0.865180 0.270352 11.00000 0.08064 0.03344 = 0.09279 0.00419 -0.01927 0.00215 AFIX 137 H10A 2 0.712163 0.855117 0.227577 11.00000 -1.50000 H10B 2 0.707629 0.926458 0.282148 11.00000 -1.50000 H10C 2 0.609402 0.855369 0.274446 11.00000 -1.50000 AFIX 0 C11 1 0.595192 0.752527 0.096936 11.00000 0.09038 0.04722 = 0.05411 0.00516 -0.01711 0.00306 AFIX 43 H11 2 0.526555 0.767839 0.078022 11.00000 -1.20000 AFIX 0 C12 1 0.695328 0.762833 0.065389 11.00000 0.12643 0.03822 = 0.03414 0.00480 -0.00311 0.00008 AFIX 43 H12 2 0.694826 0.788234 0.025416 11.00000 -1.20000 AFIX 0 C13 1 0.878377 0.811163 0.301879 11.00000 0.06056 0.05118 = 0.10300 -0.00179 -0.00756 -0.01718 AFIX 137 H13A 2 0.919708 0.770244 0.328527 11.00000 -1.50000 H13B 2 0.899970 0.872539 0.311300 11.00000 -1.50000 H13C 2 0.895534 0.798079 0.258755 11.00000 -1.50000 AFIX 0 C14 1 1.079569 0.518359 0.331055 11.00000 0.07193 0.12808 = 0.06595 -0.00611 0.01507 0.05193 AFIX 43 H14 2 1.079806 0.497871 0.289756 11.00000 -1.20000 AFIX 0 C15 1 1.059377 0.496349 0.444325 11.00000 0.05178 0.14903 = 0.06815 0.02420 0.01363 0.03751 C16 1 0.727245 0.818477 0.381301 11.00000 0.11875 0.04943 = 0.06389 -0.01849 0.01968 -0.02966 AFIX 137 H16A 2 0.646453 0.817766 0.387674 11.00000 -1.50000 H16B 2 0.756853 0.876977 0.392631 11.00000 -1.50000 H16C 2 0.762000 0.772636 0.406965 11.00000 -1.50000 AFIX 0 C17 1 0.387660 0.507129 0.392439 11.00000 0.04358 0.06771 = 0.11333 -0.00236 0.00034 -0.00460 AFIX 137 H17A 2 0.324762 0.513892 0.364102 11.00000 -1.50000 H17B 2 0.359589 0.497237 0.434203 11.00000 -1.50000 H17C 2 0.433092 0.456165 0.379769 11.00000 -1.50000 AFIX 0 C18 1 0.427237 0.692721 0.452995 11.00000 0.08467 0.08810 = 0.10262 -0.03092 0.02754 0.02053 AFIX 137 H18A 2 0.444034 0.668212 0.493716 11.00000 -1.50000 H18B 2 0.346815 0.702450 0.449282 11.00000 -1.50000 H18C 2 0.466391 0.749418 0.447752 11.00000 -1.50000 AFIX 0 C19 1 0.795773 0.465024 0.204396 11.00000 0.08285 0.06318 = 0.08402 -0.03213 0.02071 0.01120 AFIX 137 H19A 2 0.819084 0.512514 0.176330 11.00000 -1.50000 H19B 2 0.793571 0.408361 0.182140 11.00000 -1.50000 H19C 2 0.848899 0.460699 0.238479 11.00000 -1.50000 AFIX 0 C20 1 0.765642 0.608134 0.513182 11.00000 0.08445 0.09301 = 0.04717 0.00218 -0.02105 -0.02017 AFIX 137 H20A 2 0.822352 0.628389 0.483949 11.00000 -1.50000 H20B 2 0.801539 0.575385 0.546734 11.00000 -1.50000 H20C 2 0.726019 0.659691 0.529978 11.00000 -1.50000 AFIX 0 C21 1 0.445183 0.670542 0.315897 11.00000 0.03307 0.10009 = 0.09583 0.02989 -0.00233 0.01137 AFIX 137 H21A 2 0.491940 0.723813 0.313004 11.00000 -1.50000 H21B 2 0.366529 0.687841 0.314538 11.00000 -1.50000 H21C 2 0.461669 0.630790 0.281355 11.00000 -1.50000 AFIX 0 C22 1 1.056833 0.457938 0.381563 11.00000 0.06438 0.10494 = 0.15579 0.01157 0.00535 0.04782 AFIX 43 H22 2 1.041109 0.396834 0.374745 11.00000 -1.20000 AFIX 0 C23 1 1.100745 0.606021 0.344608 11.00000 0.05265 0.13473 = 0.11336 0.00033 0.01090 0.02403 AFIX 43 H23 2 1.116357 0.645930 0.311886 11.00000 -1.20000 AFIX 0 C24 1 1.100150 0.637857 0.403489 11.00000 0.06663 0.14771 = 0.17066 0.00016 0.00701 0.01175 AFIX 43 H24 2 1.111513 0.699546 0.410430 11.00000 -1.20000 AFIX 0 C25 1 0.731248 0.421481 0.455601 11.00000 0.16071 0.05116 = 0.08743 0.03013 -0.03661 -0.01202 AFIX 137 H25A 2 0.674323 0.378070 0.443664 11.00000 -1.50000 H25B 2 0.769937 0.400494 0.492538 11.00000 -1.50000 H25C 2 0.784967 0.428495 0.422018 11.00000 -1.50000 AFIX 0 C26 1 0.547719 0.506949 0.527022 11.00000 0.11525 0.11949 = 0.11315 0.00528 0.00109 -0.00314 AFIX 137 H26A 2 0.518781 0.562568 0.544269 11.00000 -1.50000 H26B 2 0.576057 0.469283 0.560314 11.00000 -1.50000 H26C 2 0.487848 0.475684 0.505319 11.00000 -1.50000 AFIX 0 C27 1 1.083649 0.583064 0.452187 11.00000 0.07822 0.14689 = 0.12105 -0.02352 -0.00508 0.03189 AFIX 43 H27 2 1.089327 0.606320 0.492659 11.00000 -1.20000 AFIX 0 C28 1 1.042398 0.435214 0.500803 11.00000 0.16188 0.16482 = 0.16234 0.00431 0.00079 0.00219 AFIX 137 H28A 2 1.021025 0.471293 0.536438 11.00000 -1.50000 H28B 2 1.111946 0.403667 0.509787 11.00000 -1.50000 H28C 2 0.983470 0.391961 0.491954 11.00000 -1.50000 AFIX 0 SB1 7 0.320189 0.343975 0.646677 11.00000 0.06166 0.05763 = 0.06633 -0.01191 0.00551 -0.00734 CU1 6 0.906579 0.557905 0.364036 11.00000 0.02932 0.07865 = 0.07018 0.00370 -0.00987 0.01771 SI1 5 0.725981 0.598649 0.347741 11.00000 0.03273 0.03184 = 0.03495 0.00077 -0.00071 0.00085 SI2 5 0.475011 0.610892 0.390989 11.00000 0.03497 0.04315 = 0.05690 -0.00382 0.00594 0.00123 SI3 5 0.662745 0.532271 0.472173 11.00000 0.06212 0.05835 = 0.04013 0.01391 -0.00795 -0.01713 N1 3 0.716845 0.704854 0.302515 11.00000 0.02879 0.02935 = 0.04065 0.00039 -0.00332 0.00441 N3 3 0.619063 0.584106 0.400835 11.00000 0.03554 0.03189 = 0.03337 -0.00228 -0.00167 -0.00389 N2 3 0.681634 0.571256 0.267126 11.00000 0.04564 0.02978 = 0.03449 -0.00342 -0.00155 -0.00269 F1 4 0.196649 0.278415 0.619025 11.00000 0.08631 0.09665 = 0.19373 -0.03633 -0.02816 -0.02050 F2 4 0.442322 0.411971 0.674215 11.00000 0.10345 0.13600 = 0.12197 -0.04418 0.00661 -0.05029 F3 4 0.228028 0.407674 0.699997 11.00000 0.13763 0.15345 = 0.21711 -0.07835 0.08557 -0.00053 F4 4 0.414279 0.288855 0.591693 11.00000 0.09270 0.23890 = 0.17902 -0.12295 0.00679 0.02129 F5 4 0.290708 0.429842 0.586627 11.00000 0.16046 0.16763 = 0.18564 0.09347 -0.03271 -0.02092 F6 4 0.349174 0.261635 0.706700 11.00000 0.23215 0.14006 = 0.22655 0.08852 -0.10902 -0.06413 HKLF 4 REM 4_a.res in P2(1)2(1)2(1) REM R1 = 0.0442 for 5034 Fo > 4sig(Fo) and 0.0748 for all 6657 data REM 392 parameters refined using 24 restraints END WGHT 0.0426 4.4963 REM Highest difference peak 0.567, deepest hole -0.420, 1-sigma level 0.073 Q1 1 0.9051 0.5942 0.3884 11.00000 0.05 0.57 Q2 1 0.8677 0.5291 0.3691 11.00000 0.05 0.53 Q3 1 0.9291 0.5603 0.3417 11.00000 0.05 0.44 Q4 1 0.2418 0.3445 0.7030 11.00000 0.05 0.41 Q5 1 0.9431 0.5370 0.3670 11.00000 0.05 0.41 Q6 1 1.0153 0.4218 0.4184 11.00000 0.05 0.38 Q7 1 1.0734 0.5391 0.5250 11.00000 0.05 0.38 Q8 1 1.0563 0.5099 0.5224 11.00000 0.05 0.37 Q9 1 1.0737 0.4853 0.5129 11.00000 0.05 0.37 Q10 1 0.3837 0.2180 0.6526 11.00000 0.05 0.35 Q11 1 1.0185 0.4204 0.3454 11.00000 0.05 0.33 Q12 1 1.0383 0.4161 0.4889 11.00000 0.05 0.32 Q13 1 0.3246 0.3614 0.5745 11.00000 0.05 0.32 Q14 1 1.0086 0.3825 0.4657 11.00000 0.05 0.29 Q15 1 0.8232 0.6000 0.3244 11.00000 0.05 0.28 Q16 1 0.6756 0.8419 0.3816 11.00000 0.05 0.27 Q17 1 0.7227 0.9570 0.2880 11.00000 0.05 0.27 Q18 1 0.5961 0.4392 0.3974 11.00000 0.05 0.26 Q19 1 0.2972 0.3289 0.7142 11.00000 0.05 0.26 Q20 1 0.7380 0.9412 0.2251 11.00000 0.05 0.26 ; _shelx_res_checksum 50599 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp C1 C 0.6991(6) 0.6575(5) 0.2495(3) 0.0363(16) Uani 1 1 d . . C2 C 0.6985(7) 0.6932(5) 0.1849(3) 0.0415(19) Uani 1 1 d . . C3 C 0.7532(7) 0.7996(5) 0.3129(4) 0.0406(19) Uani 1 1 d . . C4 C 0.6776(7) 0.4865(5) 0.2302(3) 0.0427(18) Uani 1 1 d . . C5 C 0.7999(7) 0.7014(5) 0.1518(4) 0.049(2) Uani 1 1 d . . H5 H 0.8685 0.6838 0.1698 0.059 Uiso 1 1 calc R U C6 C 0.7965(10) 0.7365(6) 0.0914(4) 0.063(3) Uani 1 1 d . . H6 H 0.8634 0.7422 0.0685 0.076 Uiso 1 1 calc R U C7 C 0.5976(8) 0.7188(5) 0.1578(4) 0.050(2) Uani 1 1 d . . H7 H 0.5303 0.7134 0.1804 0.060 Uiso 1 1 calc R U C8 C 0.5920(9) 0.4912(7) 0.1768(4) 0.070(3) Uani 1 1 d . . H8A H 0.5199 0.5110 0.1928 0.104 Uiso 1 1 calc R U H8B H 0.5839 0.4321 0.1582 0.104 Uiso 1 1 calc R U H8C H 0.6183 0.5333 0.1456 0.104 Uiso 1 1 calc R U C9 C 0.6419(9) 0.4130(5) 0.2758(4) 0.062(3) Uani 1 1 d . . H9A H 0.6984 0.4070 0.3081 0.092 Uiso 1 1 calc R U H9B H 0.6344 0.3564 0.2538 0.092 Uiso 1 1 calc R U H9C H 0.5703 0.4290 0.2944 0.092 Uiso 1 1 calc R U C10 C 0.6897(9) 0.8652(5) 0.2704(5) 0.069(3) Uani 1 1 d . . H10A H 0.7122 0.8551 0.2276 0.103 Uiso 1 1 calc R U H10B H 0.7076 0.9265 0.2821 0.103 Uiso 1 1 calc R U H10C H 0.6094 0.8554 0.2744 0.103 Uiso 1 1 calc R U C11 C 0.5952(10) 0.7525(6) 0.0969(4) 0.064(3) Uani 1 1 d . . H11 H 0.5266 0.7678 0.0780 0.077 Uiso 1 1 calc R U C12 C 0.6953(12) 0.7628(6) 0.0654(4) 0.066(3) Uani 1 1 d . . H12 H 0.6948 0.7882 0.0254 0.080 Uiso 1 1 calc R U C13 C 0.8784(8) 0.8112(6) 0.3019(5) 0.072(3) Uani 1 1 d . . H13A H 0.9197 0.7702 0.3285 0.107 Uiso 1 1 calc R U H13B H 0.9000 0.8725 0.3113 0.107 Uiso 1 1 calc R U H13C H 0.8955 0.7981 0.2588 0.107 Uiso 1 1 calc R U C14 C 1.0796(10) 0.5184(11) 0.3311(5) 0.089(4) Uani 1 1 d . . H14 H 1.0798 0.4979 0.2898 0.106 Uiso 1 1 calc R U C15 C 1.0594(10) 0.4963(13) 0.4443(6) 0.090(4) Uani 1 1 d . . C16 C 0.7272(10) 0.8185(6) 0.3813(4) 0.077(3) Uani 1 1 d . . H16A H 0.6465 0.8178 0.3877 0.116 Uiso 1 1 calc R U H16B H 0.7569 0.8770 0.3926 0.116 Uiso 1 1 calc R U H16C H 0.7620 0.7726 0.4070 0.116 Uiso 1 1 calc R U C17 C 0.3877(8) 0.5071(6) 0.3924(5) 0.075(3) Uani 1 1 d . . H17A H 0.3248 0.5139 0.3641 0.112 Uiso 1 1 calc R U H17B H 0.3596 0.4972 0.4342 0.112 Uiso 1 1 calc R U H17C H 0.4331 0.4562 0.3798 0.112 Uiso 1 1 calc R U C18 C 0.4272(10) 0.6927(7) 0.4530(6) 0.092(4) Uani 1 1 d . . H18A H 0.4440 0.6682 0.4937 0.138 Uiso 1 1 calc R U H18B H 0.3468 0.7024 0.4493 0.138 Uiso 1 1 calc R U H18C H 0.4664 0.7494 0.4478 0.138 Uiso 1 1 calc R U C19 C 0.7958(9) 0.4650(7) 0.2044(5) 0.077(3) Uani 1 1 d . . H19A H 0.8191 0.5125 0.1763 0.115 Uiso 1 1 calc R U H19B H 0.7936 0.4084 0.1821 0.115 Uiso 1 1 calc R U H19C H 0.8489 0.4607 0.2385 0.115 Uiso 1 1 calc R U C20 C 0.7656(9) 0.6081(7) 0.5132(4) 0.075(3) Uani 1 1 d . . H20A H 0.8224 0.6284 0.4839 0.112 Uiso 1 1 calc R U H20B H 0.8015 0.5754 0.5467 0.112 Uiso 1 1 calc R U H20C H 0.7260 0.6597 0.5300 0.112 Uiso 1 1 calc R U C21 C 0.4452(8) 0.6705(8) 0.3159(5) 0.076(3) Uani 1 1 d . . H21A H 0.4919 0.7238 0.3130 0.114 Uiso 1 1 calc R U H21B H 0.3665 0.6878 0.3145 0.114 Uiso 1 1 calc R U H21C H 0.4617 0.6308 0.2814 0.114 Uiso 1 1 calc R U C22 C 1.0568(10) 0.4579(10) 0.3816(8) 0.108(5) Uani 1 1 d . . H22 H 1.0411 0.3968 0.3747 0.130 Uiso 1 1 calc R U C23 C 1.1007(10) 0.6060(12) 0.3446(8) 0.100(4) Uani 1 1 d . . H23 H 1.1164 0.6459 0.3119 0.120 Uiso 1 1 calc R U C24 C 1.1001(12) 0.6379(13) 0.4035(12) 0.128(5) Uani 1 1 d . . H24 H 1.1115 0.6995 0.4104 0.154 Uiso 1 1 calc R U C25 C 0.7312(12) 0.4215(6) 0.4556(5) 0.100(4) Uani 1 1 d . . H25A H 0.6743 0.3781 0.4437 0.150 Uiso 1 1 calc R U H25B H 0.7699 0.4005 0.4925 0.150 Uiso 1 1 calc R U H25C H 0.7850 0.4285 0.4220 0.150 Uiso 1 1 calc R U C26 C 0.5477(12) 0.5069(10) 0.5270(7) 0.116(5) Uani 1 1 d . U H26A H 0.5188 0.5626 0.5443 0.174 Uiso 1 1 calc R U H26B H 0.5761 0.4693 0.5603 0.174 Uiso 1 1 calc R U H26C H 0.4878 0.4757 0.5053 0.174 Uiso 1 1 calc R U C27 C 1.0836(13) 0.5831(15) 0.4522(9) 0.115(5) Uani 1 1 d . . H27 H 1.0893 0.6063 0.4927 0.138 Uiso 1 1 calc R U C28 C 1.0424(16) 0.4352(13) 0.5008(8) 0.163(7) Uani 1 1 d . U H28A H 1.0210 0.4713 0.5364 0.245 Uiso 1 1 calc R U H28B H 1.1119 0.4037 0.5098 0.245 Uiso 1 1 calc R U H28C H 0.9835 0.3920 0.4920 0.245 Uiso 1 1 calc R U Sb1 Sb 0.32019(6) 0.34398(4) 0.64668(3) 0.0619(2) Uani 1 1 d . . Cu1 Cu 0.90658(8) 0.55790(8) 0.36404(5) 0.0594(3) Uani 1 1 d . . Si1 Si 0.72598(16) 0.59865(12) 0.34774(10) 0.0332(4) Uani 1 1 d . . Si2 Si 0.47501(18) 0.61089(16) 0.39099(11) 0.0450(6) Uani 1 1 d . . Si3 Si 0.6627(2) 0.53227(17) 0.47217(10) 0.0535(6) Uani 1 1 d . . N1 N 0.7168(5) 0.7049(4) 0.3025(3) 0.0329(14) Uani 1 1 d . . N3 N 0.6191(5) 0.5841(4) 0.4008(3) 0.0336(14) Uani 1 1 d . . N2 N 0.6816(6) 0.5713(4) 0.2671(3) 0.0366(14) Uani 1 1 d . . F1 F 0.1966(6) 0.2784(5) 0.6190(4) 0.126(3) Uani 1 1 d . . F2 F 0.4423(6) 0.4120(5) 0.6742(4) 0.120(3) Uani 1 1 d . . F3 F 0.2280(8) 0.4077(6) 0.7000(5) 0.169(4) Uani 1 1 d . . F4 F 0.4143(7) 0.2889(8) 0.5917(5) 0.170(4) Uani 1 1 d . U F5 F 0.2907(9) 0.4298(7) 0.5866(5) 0.171(4) Uani 1 1 d . . F6 F 0.3492(11) 0.2616(7) 0.7067(6) 0.200(6) Uani 1 1 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 C1 0.031(4) 0.035(4) 0.043(4) -0.001(4) 0.003(3) 0.002(3) C2 0.057(5) 0.032(4) 0.035(4) 0.001(3) -0.005(4) 0.001(4) C3 0.044(5) 0.030(4) 0.048(5) 0.002(4) 0.000(4) -0.004(3) C4 0.053(5) 0.035(4) 0.041(4) -0.008(3) -0.001(4) 0.003(4) C5 0.063(6) 0.044(4) 0.040(5) -0.006(4) 0.007(5) -0.007(4) C6 0.097(9) 0.048(5) 0.044(5) 0.001(4) 0.019(6) -0.014(5) C7 0.062(5) 0.043(4) 0.045(5) 0.001(4) -0.001(4) 0.002(4) C8 0.086(7) 0.062(6) 0.061(6) -0.019(5) -0.017(6) -0.009(6) C9 0.095(8) 0.033(5) 0.058(6) -0.006(4) -0.001(5) -0.011(4) C10 0.081(7) 0.033(5) 0.093(7) 0.004(4) -0.019(6) 0.002(5) C11 0.090(8) 0.047(5) 0.054(6) 0.005(5) -0.017(6) 0.003(5) C12 0.126(10) 0.038(5) 0.034(5) 0.005(4) -0.003(6) 0.000(6) C13 0.061(7) 0.051(6) 0.103(8) -0.002(6) -0.008(6) -0.017(5) C14 0.072(8) 0.128(11) 0.066(7) -0.006(8) 0.015(6) 0.052(8) C15 0.052(7) 0.149(13) 0.068(8) 0.024(9) 0.014(6) 0.038(8) C16 0.119(9) 0.049(6) 0.064(6) -0.018(5) 0.020(6) -0.030(6) C17 0.044(6) 0.068(6) 0.113(9) -0.002(6) 0.000(6) -0.005(5) C18 0.085(8) 0.088(8) 0.103(9) -0.031(7) 0.028(7) 0.021(6) C19 0.083(8) 0.063(6) 0.084(7) -0.032(5) 0.021(6) 0.011(6) C20 0.084(7) 0.093(7) 0.047(6) 0.002(5) -0.021(5) -0.020(6) C21 0.033(5) 0.100(8) 0.096(7) 0.030(7) -0.002(5) 0.011(5) C22 0.064(7) 0.105(10) 0.156(14) 0.012(10) 0.005(8) 0.048(7) C23 0.053(7) 0.135(13) 0.113(12) 0.000(10) 0.011(7) 0.024(8) C24 0.067(8) 0.148(15) 0.171(17) 0.000(16) 0.007(11) 0.012(10) C25 0.161(13) 0.051(6) 0.087(8) 0.030(6) -0.037(8) -0.012(7) C26 0.115(5) 0.119(5) 0.113(5) 0.005(3) 0.001(3) -0.003(3) C27 0.078(10) 0.147(15) 0.121(14) -0.024(12) -0.005(9) 0.032(10) C28 0.162(7) 0.165(7) 0.162(7) 0.004(3) 0.001(3) 0.002(3) Sb1 0.0617(4) 0.0576(3) 0.0663(4) -0.0119(3) 0.0055(4) -0.0073(3) Cu1 0.0293(5) 0.0787(7) 0.0702(7) 0.0037(6) -0.0099(5) 0.0177(5) Si1 0.0327(10) 0.0318(10) 0.0350(11) 0.0008(10) -0.0007(9) 0.0009(8) Si2 0.0350(12) 0.0431(12) 0.0569(15) -0.0038(11) 0.0059(10) 0.0012(10) Si3 0.0621(16) 0.0584(15) 0.0401(12) 0.0139(11) -0.0079(11) -0.0171(13) N1 0.029(3) 0.029(3) 0.041(4) 0.000(3) -0.003(3) 0.004(3) N3 0.036(3) 0.032(3) 0.033(3) -0.002(3) -0.002(3) -0.004(3) N2 0.046(4) 0.030(3) 0.034(3) -0.003(3) -0.002(3) -0.003(3) F1 0.086(5) 0.097(5) 0.194(8) -0.036(5) -0.028(5) -0.021(4) F2 0.103(5) 0.136(6) 0.122(6) -0.044(5) 0.007(4) -0.050(5) F3 0.138(7) 0.153(8) 0.217(10) -0.078(7) 0.086(7) -0.001(6) F4 0.093(6) 0.239(11) 0.179(8) -0.123(8) 0.007(6) 0.021(6) F5 0.160(9) 0.168(8) 0.186(9) 0.093(7) -0.033(7) -0.021(7) F6 0.232(12) 0.140(8) 0.227(11) 0.089(8) -0.109(10) -0.064(8) 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' F F 0.0171 0.0103 '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' Cu Cu 0.3201 1.2651 '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 N2 C1 N1 106.2(6) N2 C1 C2 126.9(6) N1 C1 C2 126.9(6) N2 C1 Si1 53.5(3) N1 C1 Si1 53.5(3) C2 C1 Si1 172.2(5) C7 C2 C5 120.3(7) C7 C2 C1 119.7(7) C5 C2 C1 120.0(7) N1 C3 C13 111.5(7) N1 C3 C16 105.0(6) C13 C3 C16 109.1(8) N1 C3 C10 111.7(6) C13 C3 C10 108.4(8) C16 C3 C10 111.0(8) N2 C4 C9 105.8(6) N2 C4 C8 112.4(6) C9 C4 C8 109.2(7) N2 C4 C19 109.7(7) C9 C4 C19 109.6(7) C8 C4 C19 110.0(7) C6 C5 C2 118.5(9) C6 C5 H5 120.7 C2 C5 H5 120.7 C12 C6 C5 120.4(9) C12 C6 H6 119.8 C5 C6 H6 119.8 C2 C7 C11 120.6(9) C2 C7 H7 119.7 C11 C7 H7 119.7 C4 C8 H8A 109.5 C4 C8 H8B 109.5 H8A C8 H8B 109.5 C4 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C4 C9 H9A 109.5 C4 C9 H9B 109.5 H9A C9 H9B 109.5 C4 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 C3 C10 H10A 109.5 C3 C10 H10B 109.5 H10A C10 H10B 109.5 C3 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C12 C11 C7 118.8(9) C12 C11 H11 120.6 C7 C11 H11 120.6 C11 C12 C6 121.3(8) C11 C12 H12 119.3 C6 C12 H12 119.3 C3 C13 H13A 109.5 C3 C13 H13B 109.5 H13A C13 H13B 109.5 C3 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C23 C14 C22 118.2(12) C23 C14 Cu1 81.4(7) C22 C14 Cu1 75.7(6) C23 C14 H14 120.9 C22 C14 H14 120.9 Cu1 C14 H14 112.7 C27 C15 C22 119.9(14) C27 C15 C28 120.2(17) C22 C15 C28 119.8(16) C3 C16 H16A 109.5 C3 C16 H16B 109.5 H16A C16 H16B 109.5 C3 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 Si2 C17 H17A 109.5 Si2 C17 H17B 109.5 H17A C17 H17B 109.5 Si2 C17 H17C 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 Si2 C18 H18A 109.5 Si2 C18 H18B 109.5 H18A C18 H18B 109.5 Si2 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C4 C19 H19A 109.5 C4 C19 H19B 109.5 H19A C19 H19B 109.5 C4 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 Si3 C20 H20A 109.5 Si3 C20 H20B 109.5 H20A C20 H20B 109.5 Si3 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 Si2 C21 H21A 109.5 Si2 C21 H21B 109.5 H21A C21 H21B 109.5 Si2 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C14 C22 C15 116.7(13) C14 C22 Cu1 68.0(6) C15 C22 Cu1 85.2(7) C14 C22 H22 121.7 C15 C22 H22 121.7 Cu1 C22 H22 115.8 C24 C23 C14 122.4(16) C24 C23 Cu1 86.4(9) C14 C23 Cu1 65.3(7) C24 C23 H23 118.8 C14 C23 H23 118.8 Cu1 C23 H23 119.9 C27 C24 C23 121.3(19) C27 C24 H24 119.3 C23 C24 H24 119.3 Si3 C25 H25A 109.5 Si3 C25 H25B 109.5 H25A C25 H25B 109.5 Si3 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 Si3 C26 H26A 109.5 Si3 C26 H26B 109.5 H26A C26 H26B 109.5 Si3 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C15 C27 C24 121.4(17) C15 C27 H27 119.3 C24 C27 H27 119.3 C15 C28 H28A 109.5 C15 C28 H28B 109.5 H28A C28 H28B 109.5 C15 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 F6 Sb1 F4 92.4(6) F6 Sb1 F3 91.0(6) F4 Sb1 F3 175.9(5) F6 Sb1 F5 178.8(5) F4 Sb1 F5 88.5(6) F3 Sb1 F5 88.1(5) F6 Sb1 F1 91.4(4) F4 Sb1 F1 92.3(4) F3 Sb1 F1 90.0(4) F5 Sb1 F1 89.4(4) F6 Sb1 F2 89.6(4) F4 Sb1 F2 88.5(4) F3 Sb1 F2 89.2(4) F5 Sb1 F2 89.7(4) F1 Sb1 F2 178.8(4) C14 Cu1 Si1 152.7(3) C14 Cu1 C22 36.2(4) Si1 Cu1 C22 156.3(4) C14 Cu1 C23 33.3(4) Si1 Cu1 C23 142.2(4) C22 Cu1 C23 59.9(5) N3 Si1 N2 112.5(3) N3 Si1 N1 114.3(3) N2 Si1 N1 71.4(3) N3 Si1 Cu1 124.4(2) N2 Si1 Cu1 110.8(2) N1 Si1 Cu1 111.4(2) N3 Si1 C1 123.6(3) N2 Si1 C1 35.8(3) N1 Si1 C1 36.0(3) Cu1 Si1 C1 112.04(19) N3 Si2 C17 110.5(4) N3 Si2 C21 113.1(4) C17 Si2 C21 107.5(5) N3 Si2 C18 110.5(5) C17 Si2 C18 110.8(5) C21 Si2 C18 104.2(5) N3 Si3 C26 114.9(5) N3 Si3 C25 109.9(4) C26 Si3 C25 105.3(6) N3 Si3 C20 109.3(4) C26 Si3 C20 107.7(6) C25 Si3 C20 109.5(5) C1 N1 C3 131.4(6) C1 N1 Si1 90.5(4) C3 N1 Si1 135.1(5) Si1 N3 Si2 127.3(4) Si1 N3 Si3 114.1(3) Si2 N3 Si3 118.6(3) C1 N2 C4 131.0(6) C1 N2 Si1 90.6(4) C4 N2 Si1 133.8(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N2 1.340(9) C1 N1 1.345(9) C1 C2 1.473(10) C1 Si1 2.288(7) C2 C7 1.371(11) C2 C5 1.391(11) C3 N1 1.476(9) C3 C13 1.501(12) C3 C16 1.514(11) C3 C10 1.520(11) C4 N2 1.475(9) C4 C9 1.513(11) C4 C8 1.521(12) C4 C19 1.528(12) C5 C6 1.387(12) C5 H5 0.9300 C6 C12 1.369(14) C6 H6 0.9300 C7 C11 1.389(12) C7 H7 0.9300 C8 H8A 0.9600 C8 H8B 0.9600 C8 H8C 0.9600 C9 H9A 0.9600 C9 H9B 0.9600 C9 H9C 0.9600 C10 H10A 0.9600 C10 H10B 0.9600 C10 H10C 0.9600 C11 C12 1.364(14) C11 H11 0.9300 C12 H12 0.9300 C13 H13A 0.9600 C13 H13B 0.9600 C13 H13C 0.9600 C14 C23 1.346(17) C14 C22 1.421(17) C14 Cu1 2.230(10) C14 H14 0.9300 C15 C27 1.319(19) C15 C22 1.452(18) C15 C28 1.52(2) C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C17 Si2 1.842(9) C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 C18 Si2 1.874(10) C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 C19 H19A 0.9600 C19 H19B 0.9600 C19 H19C 0.9600 C20 Si3 1.864(9) C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600 C21 Si2 1.858(10) C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C22 Cu1 2.330(11) C22 H22 0.9300 C23 C24 1.34(2) C23 Cu1 2.427(13) C23 H23 0.9300 C24 C27 1.33(2) C24 H24 0.9300 C25 Si3 1.853(11) C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C26 Si3 1.826(14) C26 H26A 0.9600 C26 H26B 0.9600 C26 H26C 0.9600 C27 H27 0.9300 C28 H28A 0.9600 C28 H28B 0.9600 C28 H28C 0.9600 Sb1 F6 1.795(9) Sb1 F4 1.804(8) Sb1 F3 1.829(7) Sb1 F5 1.832(8) Sb1 F1 1.841(6) Sb1 F2 1.847(7) Cu1 Si1 2.234(2) Si1 N3 1.705(6) Si1 N2 1.839(6) Si1 N1 1.840(6) Si2 N3 1.752(6) Si3 N3 1.776(6)