#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:04:42 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247593 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125619.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_7125619 loop_ _publ_author_name 'Parvin, Nasrina' 'Hossain, Jabed' 'George, Anjana' 'Parameswaran, Pattiyil' 'Khan, Shabana' _publ_section_title ; N-heterocyclic silylene stabilized monocordinated copper(i)-arene cationic complexes and their application in click chemistry. ; _journal_issue 2 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 273 _journal_page_last 276 _journal_paper_doi 10.1039/c9cc09115g _journal_volume 56 _journal_year 2019 _chemical_formula_moiety 'C29 H51 Cu F6 N3 Sb Si3' _chemical_formula_sum 'C29 H51 Cu F6 N3 Sb Si3' _chemical_formula_weight 825.29 _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_Hall 'P -2yac' _space_group_name_H-M_alt 'P 1 n 1' _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 98.414(18) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.226(7) _cell_length_b 11.541(9) _cell_length_c 18.052(14) _cell_measurement_reflns_used 5154 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 17.52 _cell_measurement_theta_min 2.28 _cell_volume 1901(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 0.2784 _diffrn_reflns_av_unetI/netI 0.2154 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 39863 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 24.000 _diffrn_reflns_theta_max 24.000 _diffrn_reflns_theta_min 2.232 _exptl_absorpt_coefficient_mu 1.416 _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 1.442 _exptl_crystal_description block _exptl_crystal_F_000 844 _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 0.1124 _refine_diff_density_max 0.959 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.111 _refine_ls_abs_structure_details ; Flack x determined using 977 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 403 _refine_ls_number_reflns 5967 _refine_ls_number_restraints 98 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.2138 _refine_ls_R_factor_gt 0.0841 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0805P)^2^+6.2600P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1605 _refine_ls_wR_factor_ref 0.2103 _reflns_Friedel_coverage 0.996 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 2797 _reflns_number_total 5967 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09115g2.cif _cod_data_source_block 4_b _cod_depositor_comments 'Adding full bibliography for 7125615--7125620.cif.' _cod_original_cell_volume 1901(2) _cod_original_sg_symbol_H-M 'P n' _cod_database_code 7125619 _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_b.res created by SHELXL-2014/7 TITL 4_b.res in Pn CELL 0.71073 9.2255 11.5411 18.0522 90.000 98.414 90.000 ZERR 2.000 0.0069 0.0088 0.0138 0.000 0.018 0.000 LATT -1 SYMM 1/2+X, -Y, 1/2+Z SFAC C H Cu F N Sb Si UNIT 58 102 2 12 6 2 6 OMIT -3 48 L.S. 1 ACTA BOND $H FMAP 2 PLAN 20 TWIN -1 0 0 0 1 0 0 0 -1 DELU 0.01 N2 C4 DELU 0.01 C6 C17 DELU 0.01 C10 C20 DELU 0.01 C10 C22 DELU 0.01 SI2 C26 DELU 0.01 C10 C23 ISOR 0.001 C6 C14 C16 C23 C28 C17 C18 C2 C27 C20 ISOR 0.01 SI3 ISOR 0.01 F6 F5 F2 F4 TEMP 23.000 WGHT 0.080500 6.260000 BASF 0.07673 FVAR 0.46177 F4 4 0.538076 0.923446 0.252621 11.00000 0.29628 0.18883 = 0.13287 -0.01747 0.12496 0.01942 C9 1 0.773230 0.087470 -0.138721 11.00000 0.09119 0.09066 = 0.10870 0.03991 0.01293 0.02791 AFIX 43 H9 2 0.831950 0.094855 -0.176169 11.00000 -1.20000 AFIX 0 C2 1 0.819707 0.015839 -0.082706 11.00000 0.08325 0.08326 = 0.08318 -0.00011 0.01232 0.00004 C18 1 0.753332 0.013771 -0.020360 11.00000 0.11964 0.11930 = 0.11950 -0.00007 0.01763 -0.00021 AFIX 43 H18 2 0.790072 -0.029743 0.021568 11.00000 -1.20000 AFIX 0 C17 1 0.618632 0.085062 -0.023041 11.00000 0.12079 0.12105 = 0.12092 0.00019 0.01774 -0.00013 AFIX 43 H17 2 0.569009 0.089257 0.018165 11.00000 -1.20000 AFIX 0 C6 1 0.568646 0.144912 -0.087882 11.00000 0.10808 0.10807 = 0.10841 0.00002 0.01601 0.00003 AFIX 43 H6 2 0.478640 0.182532 -0.092353 11.00000 -1.20000 AFIX 0 C29 1 0.649887 0.150000 -0.146341 11.00000 0.11718 0.07348 = 0.08523 0.02125 0.01164 -0.01749 C1 1 1.216408 0.507194 0.173530 11.00000 0.08773 0.04312 = 0.07699 -0.01313 0.01678 -0.02207 AFIX 137 H1A 2 1.249286 0.428377 0.179546 11.00000 -1.50000 H1B 2 1.132374 0.517986 0.198481 11.00000 -1.50000 H1C 2 1.293477 0.558281 0.194892 11.00000 -1.50000 AFIX 0 C3 1 0.976976 0.247934 0.269221 11.00000 0.06743 0.05023 = 0.05399 0.00043 -0.01110 -0.00093 C4 1 0.986126 0.289061 0.191186 11.00000 0.03174 0.04855 = 0.09491 -0.01633 -0.01031 0.00436 C5 1 0.876084 0.155602 0.278966 11.00000 0.09174 0.04641 = 0.09911 0.01151 0.03419 0.01025 AFIX 43 H5 2 0.815505 0.122915 0.238667 11.00000 -1.20000 AFIX 0 C7 1 0.949268 0.171188 0.413487 11.00000 0.11393 0.10049 = 0.06084 0.01703 0.02928 -0.00355 AFIX 43 H7 2 0.938565 0.148752 0.461870 11.00000 -1.20000 AFIX 0 C8 1 1.038322 0.256770 0.400011 11.00000 0.13568 0.08474 = 0.04279 -0.01370 -0.00413 0.03611 AFIX 43 H8 2 1.090691 0.294364 0.441014 11.00000 -1.20000 AFIX 0 C10 1 0.770957 0.425386 0.175316 11.00000 0.06733 0.07230 = 0.08999 -0.01373 0.02621 0.00305 C11 1 1.261985 0.170663 0.084276 11.00000 0.05523 0.10128 = 0.07567 0.02216 0.02045 0.01959 AFIX 137 H11A 2 1.190840 0.173531 0.039828 11.00000 -1.50000 H11B 2 1.324843 0.104895 0.081888 11.00000 -1.50000 H11C 2 1.319545 0.240281 0.088009 11.00000 -1.50000 AFIX 0 C12 1 1.101151 0.689369 0.067313 11.00000 0.12291 0.04948 = 0.10722 0.01283 -0.00632 -0.01464 AFIX 137 H12A 2 0.998442 0.690742 0.071083 11.00000 -1.50000 H12B 2 1.116783 0.722558 0.020364 11.00000 -1.50000 H12C 2 1.153878 0.733425 0.107645 11.00000 -1.50000 AFIX 0 C13 1 0.874643 0.118427 0.351830 11.00000 0.11217 0.08932 = 0.09550 0.03099 0.06276 0.01148 AFIX 43 H13 2 0.819177 0.053258 0.359165 11.00000 -1.20000 AFIX 0 C14 1 1.037927 0.589011 -0.111231 11.00000 0.12111 0.11950 = 0.11972 0.00051 0.01771 -0.00006 AFIX 137 H14A 2 1.138288 0.606521 -0.092394 11.00000 -1.50000 H14B 2 0.976000 0.649484 -0.097068 11.00000 -1.50000 H14C 2 1.026045 0.583346 -0.164834 11.00000 -1.50000 AFIX 0 C15 1 1.057737 0.292165 0.332754 11.00000 0.11415 0.10186 = 0.04171 0.00342 0.01813 -0.00922 AFIX 43 H15 2 1.127951 0.348542 0.328260 11.00000 -1.20000 AFIX 0 C16 1 1.067834 0.330449 -0.115303 11.00000 0.11590 0.11463 = 0.11439 -0.00060 0.01713 0.00015 AFIX 137 H16A 2 1.038157 0.258826 -0.095022 11.00000 -1.50000 H16B 2 1.172665 0.336797 -0.105763 11.00000 -1.50000 H16C 2 1.035707 0.332062 -0.168333 11.00000 -1.50000 AFIX 0 C19 1 1.185934 0.160297 0.150804 11.00000 0.08275 0.03359 = 0.09469 0.00109 0.01007 0.00244 C20 1 0.732561 0.518682 0.111544 11.00000 0.10366 0.10364 = 0.10415 -0.00071 0.01504 0.00164 AFIX 137 H20A 2 0.744933 0.485340 0.064152 11.00000 -1.50000 H20B 2 0.796602 0.584161 0.121566 11.00000 -1.50000 H20C 2 0.632792 0.543293 0.110122 11.00000 -1.50000 AFIX 0 C21 1 1.106441 0.045679 0.147556 11.00000 0.09459 0.05824 = 0.09983 0.00194 0.03751 0.03536 AFIX 137 H21A 2 1.176516 -0.016176 0.155817 11.00000 -1.50000 H21B 2 1.048476 0.036646 0.099222 11.00000 -1.50000 H21C 2 1.043773 0.043674 0.185562 11.00000 -1.50000 AFIX 0 C22 1 0.644801 0.340892 0.182867 11.00000 0.04408 0.08782 = 0.14846 -0.05963 0.03450 0.00892 AFIX 137 H22A 2 0.674411 0.288369 0.223505 11.00000 -1.50000 H22B 2 0.620900 0.297852 0.137206 11.00000 -1.50000 H22C 2 0.560432 0.383772 0.192598 11.00000 -1.50000 AFIX 0 C23 1 0.811772 0.487415 0.249247 11.00000 0.10252 0.10270 = 0.10239 -0.00227 0.01519 0.00043 AFIX 137 H23A 2 0.881096 0.547656 0.243638 11.00000 -1.50000 H23B 2 0.854613 0.433222 0.286487 11.00000 -1.50000 H23C 2 0.725508 0.520732 0.264532 11.00000 -1.50000 AFIX 0 C24 1 1.300234 0.169465 0.224422 11.00000 0.10086 0.06771 = 0.08638 0.03176 0.00154 0.02580 AFIX 137 H24A 2 1.350082 0.242579 0.225321 11.00000 -1.50000 H24B 2 1.370219 0.107697 0.225554 11.00000 -1.50000 H24C 2 1.250091 0.163707 0.267275 11.00000 -1.50000 AFIX 0 C25 1 0.784352 0.442405 -0.094973 11.00000 0.22214 0.08068 = 0.12660 0.00876 -0.04965 0.04303 AFIX 137 H25A 2 0.743530 0.518470 -0.091921 11.00000 -1.50000 H25B 2 0.746290 0.391922 -0.060189 11.00000 -1.50000 H25C 2 0.758499 0.412824 -0.144860 11.00000 -1.50000 AFIX 0 C26 1 1.339295 0.531274 0.030519 11.00000 0.07823 0.14901 = 0.10533 0.03282 0.00472 -0.01898 AFIX 137 H26A 2 1.338558 0.590121 -0.007119 11.00000 -1.50000 H26B 2 1.346329 0.456390 0.008167 11.00000 -1.50000 H26C 2 1.421832 0.542914 0.068809 11.00000 -1.50000 AFIX 0 C27 1 0.954211 -0.048981 -0.083755 11.00000 0.11706 0.11644 = 0.11716 -0.00035 0.01660 0.00098 AFIX 137 H27A 2 0.933222 -0.118688 -0.112332 11.00000 -1.50000 H27B 2 0.995888 -0.068489 -0.033431 11.00000 -1.50000 H27C 2 1.022487 -0.002638 -0.106196 11.00000 -1.50000 AFIX 0 C28 1 0.591150 0.213913 -0.211172 11.00000 0.13309 0.13262 = 0.13372 0.00008 0.01894 0.00021 AFIX 137 H28A 2 0.667664 0.230576 -0.240355 11.00000 -1.50000 H28B 2 0.550081 0.285188 -0.196338 11.00000 -1.50000 H28C 2 0.516050 0.169127 -0.240594 11.00000 -1.50000 AFIX 0 SB1 6 0.595514 0.859042 0.173277 11.00000 0.07115 0.05077 = 0.07306 -0.00371 0.01879 0.00505 CU1 3 0.816389 0.191816 0.004450 11.00000 0.09498 0.04103 = 0.06739 -0.01490 -0.01384 0.00294 SI1 7 0.959842 0.326484 0.068007 11.00000 0.07506 0.03728 = 0.06155 0.00165 0.00189 0.01668 SI2 7 1.166492 0.539826 0.072729 11.00000 0.09751 0.05399 = 0.07715 0.00522 0.00071 -0.00616 SI3 7 0.986937 0.450140 -0.071667 11.00000 0.15474 0.05574 = 0.07246 0.00201 -0.00099 -0.00626 N3 5 1.039215 0.439839 0.026694 11.00000 0.10665 0.03789 = 0.02169 -0.00303 0.00108 -0.01335 N1 5 1.080020 0.257552 0.144680 11.00000 0.05518 0.03835 = 0.06722 -0.02634 -0.00657 0.02520 N2 5 0.890066 0.358766 0.154747 11.00000 0.09103 0.08729 = 0.03648 0.01455 0.02444 0.06979 F5 4 0.505595 0.723873 0.189979 11.00000 0.21132 0.12728 = 0.10633 0.00600 0.03468 -0.09951 F2 4 0.668050 0.792431 0.093146 11.00000 0.23381 0.10953 = 0.14197 0.02783 0.11343 0.05496 F3 4 0.448135 0.906584 0.102918 11.00000 0.17556 0.23624 = 0.23317 0.08816 -0.04007 0.03541 F1 4 0.743596 0.812890 0.234875 11.00000 0.11288 0.38890 = 0.15633 0.03218 -0.08333 0.01930 F6 4 0.688168 0.992012 0.152469 11.00000 0.29450 0.18079 = 0.12148 -0.03296 0.02671 -0.13588 HKLF 4 REM 4_b.res in Pn REM R1 = 0.0841 for 2797 Fo > 4sig(Fo) and 0.2138 for all 5967 data REM 403 parameters refined using 98 restraints END WGHT 0.0882 5.0233 REM Highest difference peak 0.959, deepest hole -0.528, 1-sigma level 0.111 Q1 1 0.7782 0.8550 0.1520 11.00000 0.05 0.96 Q2 1 0.4135 0.8572 0.1991 11.00000 0.05 0.92 Q3 1 0.9946 0.1884 -0.0006 11.00000 0.05 0.50 Q4 1 0.5352 0.8402 0.0813 11.00000 0.05 0.49 Q5 1 0.6414 0.1816 0.0175 11.00000 0.05 0.48 Q6 1 0.6573 0.8793 0.2825 11.00000 0.05 0.47 Q7 1 0.7940 0.2848 0.1492 11.00000 0.05 0.45 Q8 1 1.0340 0.5350 0.1006 11.00000 0.05 0.44 Q9 1 0.6405 0.1018 0.0183 11.00000 0.05 0.43 Q10 1 0.6759 0.0444 -0.0717 11.00000 0.05 0.43 Q11 1 0.7782 0.1884 -0.1105 11.00000 0.05 0.41 Q12 1 1.0860 0.4804 -0.0575 11.00000 0.05 0.41 Q13 1 0.7826 0.1443 0.0003 11.00000 0.05 0.40 Q14 1 0.6201 0.7115 0.2190 11.00000 0.05 0.40 Q15 1 0.5881 1.0197 0.1564 11.00000 0.05 0.40 Q16 1 0.6088 0.7636 0.0966 11.00000 0.05 0.40 Q17 1 0.8222 0.2075 -0.0506 11.00000 0.05 0.39 Q18 1 0.9019 -0.1370 -0.1608 11.00000 0.05 0.37 Q19 1 0.6204 0.2560 0.0174 11.00000 0.05 0.37 Q20 1 0.9686 0.5990 -0.1075 11.00000 0.05 0.36 ; _shelx_res_checksum 39592 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y, 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 F4 F 0.538(4) 0.923(3) 0.2526(14) 0.197(12) Uani 1 1 d . U C9 C 0.773(4) 0.087(3) -0.139(2) 0.097(11) Uani 1 1 d . . H9 H 0.8320 0.0949 -0.1762 0.116 Uiso 1 1 calc R U C2 C 0.820(4) 0.016(3) -0.083(2) 0.083(9) Uani 1 1 d . U C18 C 0.753(4) 0.014(4) -0.020(2) 0.119(13) Uani 1 1 d . U H18 H 0.7901 -0.0297 0.0216 0.143 Uiso 1 1 calc R U C17 C 0.619(4) 0.085(4) -0.023(2) 0.121(11) Uani 1 1 d . U H17 H 0.5690 0.0893 0.0182 0.145 Uiso 1 1 calc R U C6 C 0.569(4) 0.145(3) -0.088(2) 0.108(10) Uani 1 1 d . U H6 H 0.4786 0.1825 -0.0924 0.130 Uiso 1 1 calc R U C29 C 0.650(4) 0.150(3) -0.1463(19) 0.092(10) Uani 1 1 d . . C1 C 1.216(3) 0.507(2) 0.1735(14) 0.069(8) Uani 1 1 d . . H1A H 1.2493 0.4284 0.1795 0.103 Uiso 1 1 calc R U H1B H 1.1324 0.5180 0.1985 0.103 Uiso 1 1 calc R U H1C H 1.2935 0.5583 0.1949 0.103 Uiso 1 1 calc R U C3 C 0.977(3) 0.248(2) 0.2692(18) 0.059(8) Uani 1 1 d . . C4 C 0.986(3) 0.289(2) 0.1912(19) 0.060(8) Uani 1 1 d . U C5 C 0.876(4) 0.156(2) 0.279(2) 0.077(11) Uani 1 1 d . . H5 H 0.8155 0.1229 0.2387 0.092 Uiso 1 1 calc R U C7 C 0.949(5) 0.171(4) 0.413(2) 0.090(12) Uani 1 1 d . . H7 H 0.9386 0.1488 0.4619 0.108 Uiso 1 1 calc R U C8 C 1.038(5) 0.257(3) 0.4000(19) 0.089(11) Uani 1 1 d . . H8 H 1.0907 0.2944 0.4410 0.107 Uiso 1 1 calc R U C10 C 0.771(3) 0.425(3) 0.1753(18) 0.075(7) Uani 1 1 d . U C11 C 1.262(3) 0.171(3) 0.0843(17) 0.076(11) Uani 1 1 d . . H11A H 1.1908 0.1735 0.0398 0.114 Uiso 1 1 calc R U H11B H 1.3248 0.1049 0.0819 0.114 Uiso 1 1 calc R U H11C H 1.3195 0.2403 0.0880 0.114 Uiso 1 1 calc R U C12 C 1.101(4) 0.689(2) 0.0673(18) 0.096(11) Uani 1 1 d . . H12A H 0.9984 0.6907 0.0711 0.143 Uiso 1 1 calc R U H12B H 1.1168 0.7226 0.0204 0.143 Uiso 1 1 calc R U H12C H 1.1539 0.7334 0.1076 0.143 Uiso 1 1 calc R U C13 C 0.875(4) 0.118(3) 0.352(2) 0.094(12) Uani 1 1 d . . H13 H 0.8192 0.0533 0.3592 0.113 Uiso 1 1 calc R U C14 C 1.038(4) 0.589(3) -0.111(2) 0.120(13) Uani 1 1 d . U H14A H 1.1383 0.6065 -0.0924 0.180 Uiso 1 1 calc R U H14B H 0.9760 0.6495 -0.0971 0.180 Uiso 1 1 calc R U H14C H 1.0260 0.5833 -0.1648 0.180 Uiso 1 1 calc R U C15 C 1.058(4) 0.292(3) 0.3328(19) 0.085(10) Uani 1 1 d . . H15 H 1.1280 0.3485 0.3283 0.102 Uiso 1 1 calc R U C16 C 1.068(4) 0.330(3) -0.115(2) 0.115(13) Uani 1 1 d . U H16A H 1.0382 0.2588 -0.0950 0.172 Uiso 1 1 calc R U H16B H 1.1727 0.3368 -0.1058 0.172 Uiso 1 1 calc R U H16C H 1.0357 0.3321 -0.1683 0.172 Uiso 1 1 calc R U C19 C 1.186(3) 0.160(2) 0.1508(19) 0.071(9) Uani 1 1 d . . C20 C 0.733(4) 0.519(3) 0.1115(19) 0.104(11) Uani 1 1 d . U H20A H 0.7449 0.4853 0.0642 0.156 Uiso 1 1 calc R U H20B H 0.7966 0.5842 0.1216 0.156 Uiso 1 1 calc R U H20C H 0.6328 0.5433 0.1101 0.156 Uiso 1 1 calc R U C21 C 1.106(4) 0.046(2) 0.1476(17) 0.082(10) Uani 1 1 d . . H21A H 1.1765 -0.0162 0.1558 0.123 Uiso 1 1 calc R U H21B H 1.0485 0.0366 0.0992 0.123 Uiso 1 1 calc R U H21C H 1.0438 0.0437 0.1856 0.123 Uiso 1 1 calc R U C22 C 0.645(2) 0.341(3) 0.183(2) 0.091(12) Uani 1 1 d . U H22A H 0.6744 0.2884 0.2235 0.137 Uiso 1 1 calc R U H22B H 0.6209 0.2979 0.1372 0.137 Uiso 1 1 calc R U H22C H 0.5604 0.3838 0.1926 0.137 Uiso 1 1 calc R U C23 C 0.812(4) 0.487(3) 0.2492(19) 0.103(11) Uani 1 1 d . U H23A H 0.8811 0.5477 0.2436 0.154 Uiso 1 1 calc R U H23B H 0.8546 0.4332 0.2865 0.154 Uiso 1 1 calc R U H23C H 0.7255 0.5207 0.2645 0.154 Uiso 1 1 calc R U C24 C 1.300(3) 0.169(2) 0.2244(18) 0.086(10) Uani 1 1 d . . H24A H 1.3501 0.2426 0.2253 0.129 Uiso 1 1 calc R U H24B H 1.3702 0.1077 0.2256 0.129 Uiso 1 1 calc R U H24C H 1.2501 0.1637 0.2673 0.129 Uiso 1 1 calc R U C25 C 0.784(5) 0.442(3) -0.095(2) 0.151(19) Uani 1 1 d . . H25A H 0.7435 0.5185 -0.0919 0.226 Uiso 1 1 calc R U H25B H 0.7463 0.3919 -0.0602 0.226 Uiso 1 1 calc R U H25C H 0.7585 0.4128 -0.1449 0.226 Uiso 1 1 calc R U C26 C 1.339(3) 0.531(3) 0.031(2) 0.112(13) Uani 1 1 d . U H26A H 1.3386 0.5901 -0.0071 0.168 Uiso 1 1 calc R U H26B H 1.3463 0.4564 0.0082 0.168 Uiso 1 1 calc R U H26C H 1.4218 0.5429 0.0688 0.168 Uiso 1 1 calc R U C27 C 0.954(4) -0.049(3) -0.084(2) 0.117(13) Uani 1 1 d . U H27A H 0.9332 -0.1187 -0.1123 0.175 Uiso 1 1 calc R U H27B H 0.9959 -0.0685 -0.0334 0.175 Uiso 1 1 calc R U H27C H 1.0225 -0.0026 -0.1062 0.175 Uiso 1 1 calc R U C28 C 0.591(5) 0.214(4) -0.211(3) 0.133(14) Uani 1 1 d . U H28A H 0.6677 0.2306 -0.2404 0.200 Uiso 1 1 calc R U H28B H 0.5501 0.2852 -0.1963 0.200 Uiso 1 1 calc R U H28C H 0.5160 0.1691 -0.2406 0.200 Uiso 1 1 calc R U Sb1 Sb 0.59551(15) 0.85904(15) 0.17328(11) 0.0642(7) Uani 1 1 d . . Cu1 Cu 0.8164(4) 0.1918(3) 0.0045(2) 0.0704(12) Uani 1 1 d . . Si1 Si 0.9598(9) 0.3265(6) 0.0680(4) 0.059(2) Uani 1 1 d . . Si2 Si 1.1665(10) 0.5398(8) 0.0727(5) 0.077(3) Uani 1 1 d . U Si3 Si 0.9869(13) 0.4501(8) -0.0717(5) 0.096(3) Uani 1 1 d . U N3 N 1.039(2) 0.4398(16) 0.0267(10) 0.056(6) Uani 1 1 d . . N1 N 1.080(2) 0.2576(16) 0.1447(11) 0.055(6) Uani 1 1 d . . N2 N 0.890(2) 0.3588(19) 0.1547(11) 0.070(7) Uani 1 1 d . U F5 F 0.506(3) 0.724(2) 0.1900(12) 0.147(8) Uani 1 1 d . U F2 F 0.668(3) 0.7924(19) 0.0931(13) 0.153(9) Uani 1 1 d . U F3 F 0.448(4) 0.907(3) 0.1029(19) 0.222(15) Uani 1 1 d . . F1 F 0.744(3) 0.813(3) 0.2349(17) 0.230(16) Uani 1 1 d . . F6 F 0.688(4) 0.992(2) 0.1525(14) 0.199(11) 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 F4 0.30(3) 0.19(2) 0.133(18) -0.017(16) 0.125(18) 0.02(2) C9 0.09(3) 0.09(3) 0.11(3) 0.04(2) 0.01(2) 0.03(2) C2 0.083(9) 0.083(9) 0.083(9) -0.0001(15) 0.012(2) 0.0000(15) C18 0.120(13) 0.119(13) 0.120(13) -0.0001(15) 0.018(2) -0.0002(15) C17 0.121(11) 0.121(11) 0.121(11) 0.0002(15) 0.018(2) -0.0001(15) C6 0.108(10) 0.108(10) 0.108(10) 0.0000(15) 0.016(2) 0.0000(15) C29 0.12(3) 0.07(2) 0.09(3) 0.02(2) 0.01(2) -0.02(2) C1 0.09(2) 0.043(16) 0.08(2) -0.013(15) 0.017(17) -0.022(15) C3 0.07(2) 0.050(19) 0.05(2) 0.000(17) -0.011(18) -0.001(16) C4 0.032(18) 0.049(17) 0.09(3) -0.016(16) -0.010(16) 0.004(13) C5 0.09(3) 0.05(2) 0.10(3) 0.012(18) 0.03(2) 0.010(19) C7 0.11(3) 0.10(3) 0.06(3) 0.02(2) 0.03(2) 0.00(2) C8 0.14(4) 0.08(3) 0.04(2) -0.01(2) 0.00(2) 0.04(3) C10 0.07(2) 0.072(19) 0.090(17) -0.014(12) 0.026(17) 0.003(14) C11 0.06(2) 0.10(3) 0.08(3) 0.02(2) 0.020(19) 0.02(2) C12 0.12(3) 0.049(19) 0.11(3) 0.013(18) -0.01(2) -0.015(18) C13 0.11(3) 0.09(3) 0.10(3) 0.03(3) 0.06(3) 0.01(2) C14 0.121(13) 0.120(13) 0.120(13) 0.001(3) 0.018(3) 0.000(3) C15 0.11(3) 0.10(3) 0.04(2) 0.00(2) 0.02(2) -0.01(2) C16 0.116(13) 0.115(13) 0.114(13) -0.001(3) 0.017(3) 0.000(3) C19 0.08(2) 0.034(19) 0.09(3) 0.001(16) 0.01(2) 0.002(16) C20 0.104(11) 0.104(11) 0.104(11) -0.001(3) 0.015(3) 0.002(3) C21 0.09(2) 0.06(2) 0.10(3) 0.002(16) 0.04(2) 0.035(19) C22 0.04(2) 0.09(2) 0.15(3) -0.06(2) 0.03(2) 0.009(13) C23 0.103(11) 0.103(11) 0.102(11) -0.002(3) 0.015(3) 0.000(3) C24 0.10(3) 0.07(2) 0.09(2) 0.032(17) 0.00(2) 0.026(18) C25 0.22(5) 0.08(3) 0.13(4) 0.01(2) -0.05(3) 0.04(3) C26 0.08(2) 0.15(3) 0.11(3) 0.03(2) 0.005(19) -0.02(2) C27 0.117(13) 0.116(13) 0.117(13) 0.000(3) 0.017(4) 0.001(3) C28 0.133(14) 0.133(14) 0.134(14) 0.000(3) 0.019(4) 0.000(3) Sb1 0.0712(13) 0.0508(11) 0.0731(13) -0.0037(13) 0.0188(10) 0.0050(14) Cu1 0.095(3) 0.041(2) 0.067(3) -0.0149(18) -0.014(2) 0.0029(19) Si1 0.075(6) 0.037(4) 0.062(5) 0.002(4) 0.002(4) 0.017(4) Si2 0.098(8) 0.054(5) 0.077(7) 0.005(5) 0.001(5) -0.006(5) Si3 0.155(9) 0.056(5) 0.072(6) 0.002(5) -0.001(6) -0.006(6) N3 0.107(18) 0.038(13) 0.022(12) -0.003(9) 0.001(12) -0.013(12) N1 0.055(14) 0.038(13) 0.067(17) -0.026(11) -0.007(14) 0.025(12) N2 0.091(17) 0.087(17) 0.036(13) 0.015(12) 0.024(12) 0.070(14) F5 0.211(19) 0.127(15) 0.106(14) 0.006(12) 0.035(14) -0.100(14) F2 0.23(2) 0.110(15) 0.142(17) 0.028(13) 0.113(16) 0.055(14) F3 0.18(3) 0.24(3) 0.23(4) 0.09(3) -0.04(2) 0.04(2) F1 0.11(2) 0.39(5) 0.16(3) 0.03(3) -0.083(19) 0.02(3) F6 0.29(2) 0.181(19) 0.121(17) -0.033(15) 0.027(16) -0.136(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' Cu Cu 0.3201 1.2651 '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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 '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 C2 C9 C29 126(4) C2 C9 H9 116.9 C29 C9 H9 116.9 C9 C2 C18 121(4) C9 C2 C27 119(4) C18 C2 C27 119(4) C2 C18 C17 116(4) C2 C18 Cu1 91(3) C17 C18 Cu1 71(2) C2 C18 H18 122.0 C17 C18 H18 122.0 Cu1 C18 H18 106.8 C6 C17 C18 119(4) C6 C17 Cu1 94(3) C18 C17 Cu1 69(2) C6 C17 H17 120.7 C18 C17 H17 120.7 Cu1 C17 H17 106.2 C17 C6 C29 121(4) C17 C6 H6 119.4 C29 C6 H6 119.4 C9 C29 C6 117(3) C9 C29 C28 125(4) C6 C29 C28 118(4) Si2 C1 H1A 109.5 Si2 C1 H1B 109.5 H1A C1 H1B 109.5 Si2 C1 H1C 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 C15 C3 C5 117(3) C15 C3 C4 125(3) C5 C3 C4 118(3) N2 C4 N1 108(3) N2 C4 C3 123(3) N1 C4 C3 129(3) N2 C4 Si1 54.1(15) N1 C4 Si1 54.4(15) C3 C4 Si1 168(2) C13 C5 C3 116(3) C13 C5 H5 121.9 C3 C5 H5 121.9 C8 C7 C13 116(4) C8 C7 H7 122.1 C13 C7 H7 122.1 C15 C8 C7 125(4) C15 C8 H8 117.6 C7 C8 H8 117.6 N2 C10 C23 112(3) N2 C10 C22 108(2) C23 C10 C22 108(2) N2 C10 C20 106(2) C23 C10 C20 109(3) C22 C10 C20 114(3) C19 C11 H11A 109.5 C19 C11 H11B 109.5 H11A C11 H11B 109.5 C19 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 Si2 C12 H12A 109.5 Si2 C12 H12B 109.5 H12A C12 H12B 109.5 Si2 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C7 C13 C5 124(4) C7 C13 H13 117.9 C5 C13 H13 117.9 Si3 C14 H14A 109.5 Si3 C14 H14B 109.5 H14A C14 H14B 109.5 Si3 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C8 C15 C3 122(3) C8 C15 H15 119.2 C3 C15 H15 119.2 Si3 C16 H16A 109.5 Si3 C16 H16B 109.5 H16A C16 H16B 109.5 Si3 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 N1 C19 C11 105(2) N1 C19 C21 110(2) C11 C19 C21 109(2) N1 C19 C24 111(2) C11 C19 C24 110(3) C21 C19 C24 111(2) C10 C20 H20A 109.5 C10 C20 H20B 109.5 H20A C20 H20B 109.5 C10 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 C19 C21 H21A 109.5 C19 C21 H21B 109.5 H21A C21 H21B 109.5 C19 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C10 C22 H22A 109.5 C10 C22 H22B 109.5 H22A C22 H22B 109.5 C10 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C10 C23 H23A 109.5 C10 C23 H23B 109.5 H23A C23 H23B 109.5 C10 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C19 C24 H24A 109.5 C19 C24 H24B 109.5 H24A C24 H24B 109.5 C19 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 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 Si2 C26 H26A 109.5 Si2 C26 H26B 109.5 H26A C26 H26B 109.5 Si2 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C2 C27 H27A 109.5 C2 C27 H27B 109.5 H27A C27 H27B 109.5 C2 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C29 C28 H28A 109.5 C29 C28 H28B 109.5 H28A C28 H28B 109.5 C29 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 F1 Sb1 F4 84.8(16) F1 Sb1 F3 175.7(19) F4 Sb1 F3 99.1(17) F1 Sb1 F5 88.0(16) F4 Sb1 F5 91.6(12) F3 Sb1 F5 93.6(13) F1 Sb1 F6 92.4(15) F4 Sb1 F6 91.0(14) F3 Sb1 F6 85.8(16) F5 Sb1 F6 177.3(12) F1 Sb1 F2 91.9(14) F4 Sb1 F2 176.3(15) F3 Sb1 F2 84.1(15) F5 Sb1 F2 90.0(11) F6 Sb1 F2 87.4(12) C18 Cu1 C17 39.8(13) C18 Cu1 Si1 152.1(11) C17 Cu1 Si1 155.7(12) N3 Si1 N2 116.4(11) N3 Si1 N1 114.2(11) N2 Si1 N1 71.8(10) N3 Si1 C4 125.8(10) N2 Si1 C4 35.5(9) N1 Si1 C4 36.7(9) N3 Si1 Cu1 124.1(7) N2 Si1 Cu1 109.0(9) N1 Si1 Cu1 109.5(7) C4 Si1 Cu1 110.1(7) N3 Si2 C12 113.6(13) N3 Si2 C1 112.5(10) C12 Si2 C1 106.1(14) N3 Si2 C26 108.8(15) C12 Si2 C26 108.8(16) C1 Si2 C26 106.6(14) N3 Si3 C16 108.4(14) N3 Si3 C14 113.5(15) C16 Si3 C14 110.6(17) N3 Si3 C25 109.9(15) C16 Si3 C25 109.3(17) C14 Si3 C25 105.0(17) Si1 N3 Si2 126.1(11) Si1 N3 Si3 114.4(11) Si2 N3 Si3 119.5(11) C4 N1 C19 130(2) C4 N1 Si1 88.9(18) C19 N1 Si1 135.1(18) C4 N2 C10 134(2) C4 N2 Si1 90.5(18) C10 N2 Si1 135.6(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance F4 Sb1 1.76(2) C9 C2 1.33(4) C9 C29 1.34(4) C9 H9 0.9300 C2 C18 1.36(5) C2 C27 1.45(4) C18 C17 1.49(5) C18 Cu1 2.16(4) C18 H18 0.9300 C17 C6 1.38(5) C17 Cu1 2.20(4) C17 H17 0.9300 C6 C29 1.38(4) C6 H6 0.9300 C29 C28 1.42(5) C1 Si2 1.85(3) C1 H1A 0.9600 C1 H1B 0.9600 C1 H1C 0.9600 C3 C15 1.37(4) C3 C5 1.44(4) C3 C4 1.50(4) C4 N2 1.30(3) C4 N1 1.34(3) C4 Si1 2.24(3) C5 C13 1.39(4) C5 H5 0.9300 C7 C8 1.33(5) C7 C13 1.36(5) C7 H7 0.9300 C8 C15 1.32(4) C8 H8 0.9300 C10 N2 1.43(3) C10 C23 1.51(4) C10 C22 1.54(4) C10 C20 1.58(4) C11 C19 1.48(4) C11 H11A 0.9600 C11 H11B 0.9600 C11 H11C 0.9600 C12 Si2 1.83(3) C12 H12A 0.9600 C12 H12B 0.9600 C12 H12C 0.9600 C13 H13 0.9300 C14 Si3 1.84(4) C14 H14A 0.9600 C14 H14B 0.9600 C14 H14C 0.9600 C15 H15 0.9300 C16 Si3 1.80(3) C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C19 N1 1.48(3) C19 C21 1.51(3) C19 C24 1.57(4) C20 H20A 0.9600 C20 H20B 0.9600 C20 H20C 0.9600 C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C22 H22A 0.9600 C22 H22B 0.9600 C22 H22C 0.9600 C23 H23A 0.9600 C23 H23B 0.9600 C23 H23C 0.9600 C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 C25 Si3 1.86(4) C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C26 Si2 1.87(3) C26 H26A 0.9600 C26 H26B 0.9600 C26 H26C 0.9600 C27 H27A 0.9600 C27 H27B 0.9600 C27 H27C 0.9600 C28 H28A 0.9600 C28 H28B 0.9600 C28 H28C 0.9600 Sb1 F1 1.72(2) Sb1 F3 1.80(3) Sb1 F5 1.813(18) Sb1 F6 1.82(2) Sb1 F2 1.848(19) Cu1 Si1 2.245(8) Si1 N3 1.72(2) Si1 N2 1.82(2) Si1 N1 1.82(2) Si2 N3 1.77(2) Si3 N3 1.77(2)