#------------------------------------------------------------------------------ #$Date: 2019-11-29 03:32:54 +0200 (Fri, 29 Nov 2019) $ #$Revision: 244791 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125616.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_7125616 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_sum 'C34 H44 Cu F6 N2 Sb' _chemical_formula_weight 780.00 _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 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 124.966(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 24.087(2) _cell_length_b 9.1915(9) _cell_length_c 19.165(3) _cell_measurement_reflns_used 9930 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 23.27 _cell_measurement_theta_min 2.20 _cell_volume 3477.1(7) _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.1028 _diffrn_reflns_av_unetI/netI 0.0789 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 43896 _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 25.248 _diffrn_reflns_theta_min 2.202 _exptl_absorpt_coefficient_mu 1.446 _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 1.490 _exptl_crystal_description block _exptl_crystal_F_000 1584 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max 0.7457 _exptl_transmission_factor_min 0.5817 _refine_diff_density_max 0.724 _refine_diff_density_min -0.446 _refine_diff_density_rms 0.085 _refine_ls_abs_structure_details ; Flack x determined using 1824 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.009(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 406 _refine_ls_number_reflns 6285 _refine_ls_number_restraints 8 _refine_ls_restrained_S_all 1.004 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0449 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+4.1641P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.0860 _reflns_Friedel_coverage 0.998 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 4635 _reflns_number_total 6285 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09115g2.cif _cod_data_source_block 1_a _cod_original_cell_volume 3477.2(7) _cod_original_sg_symbol_H-M 'C c' _cod_database_code 7125616 _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 ; 1_a.res created by SHELXL-2014/7 TITL 1_a.res in Cc CELL 0.71073 24.0875 9.1915 19.1647 90.000 124.966 90.000 ZERR 4.000 0.0023 0.0009 0.0031 0.000 0.002 0.000 LATT -7 SYMM X, -Y, 1/2+Z SFAC C H N F Cu Sb UNIT 136 176 8 24 4 4 OMIT -3 50.5 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 ISOR 0.001 C34 TEMP 23.000 WGHT 0.034500 4.164100 FVAR 0.27439 SB1 6 0.324511 0.591684 0.466514 11.00000 0.02939 0.04529 = 0.04898 -0.00650 0.02282 0.00070 CU1 5 0.581106 0.283611 0.431735 11.00000 0.05508 0.03676 = 0.03585 0.00635 0.03365 0.01906 N2 3 0.549079 0.379569 0.550954 11.00000 0.02510 0.02334 = 0.01799 0.00150 0.01403 0.00452 N1 3 0.541790 0.551388 0.471559 11.00000 0.02578 0.02928 = 0.01810 0.00764 0.01360 0.00535 F6 4 0.351158 0.479952 0.409803 11.00000 0.07392 0.05756 = 0.08224 -0.00119 0.05939 0.01721 F1 4 0.391117 0.727314 0.494848 11.00000 0.06674 0.04620 = 0.19510 -0.02497 0.07955 -0.02093 F2 4 0.263048 0.688967 0.365874 11.00000 0.07195 0.09307 = 0.08065 0.03223 0.05130 0.03669 F4 4 0.258698 0.456087 0.439627 11.00000 0.05698 0.08698 = 0.08966 -0.00317 0.04547 -0.01789 F3 4 0.295875 0.699828 0.521819 11.00000 0.06889 0.11853 = 0.06757 -0.02977 0.03520 0.01951 F5 4 0.387145 0.493606 0.567125 11.00000 0.06469 0.09142 = 0.05014 0.00387 0.01809 0.02411 C1 1 0.485039 0.641778 0.326837 11.00000 0.02823 0.02082 = 0.02841 0.00451 0.01580 0.00501 C2 1 0.556640 0.407976 0.487943 11.00000 0.02754 0.02000 = 0.02827 0.00542 0.01863 0.00077 C3 1 0.529667 0.500513 0.573372 11.00000 0.03698 0.03702 = 0.02275 0.00029 0.02259 0.00602 AFIX 43 H3 2 0.520949 0.506183 0.614704 11.00000 -1.20000 AFIX 0 C4 1 0.607383 0.671968 0.428076 11.00000 0.03659 0.02318 = 0.03143 0.00567 0.02191 0.00201 C5 1 0.516240 0.139944 0.569377 11.00000 0.04051 0.02353 = 0.02274 0.00477 0.02272 0.00735 C6 1 0.671609 0.664273 0.518956 11.00000 0.02859 0.05038 = 0.03281 0.01344 0.01184 -0.00161 AFIX 13 H6 2 0.663789 0.592744 0.550378 11.00000 -1.20000 AFIX 0 C7 1 0.525636 0.610038 0.523769 11.00000 0.02640 0.03326 = 0.02722 -0.00497 0.01595 0.01059 AFIX 43 H7 2 0.514180 0.706288 0.524719 11.00000 -1.20000 AFIX 0 C8 1 0.490061 0.700158 0.263699 11.00000 0.04388 0.02520 = 0.03198 0.00788 0.02326 0.00340 AFIX 43 H8 2 0.451334 0.709929 0.208569 11.00000 -1.20000 AFIX 0 C9 1 0.609750 0.731312 0.363141 11.00000 0.03584 0.02397 = 0.04788 -0.00125 0.03392 -0.00392 AFIX 43 H9 2 0.650937 0.762933 0.374774 11.00000 -1.20000 AFIX 0 C10 1 0.552094 0.743851 0.282075 11.00000 0.05877 0.02287 = 0.03252 0.00223 0.03553 -0.00421 AFIX 43 H10 2 0.554728 0.782037 0.239116 11.00000 -1.20000 AFIX 0 C11 1 0.537309 0.008810 0.614227 11.00000 0.06644 0.02429 = 0.04038 0.00328 0.03737 0.00802 AFIX 43 H11 2 0.505204 -0.063406 0.598965 11.00000 -1.20000 AFIX 0 C12 1 0.567357 0.241212 0.595277 11.00000 0.02974 0.03080 = 0.02532 0.00816 0.02291 0.01348 C13 1 0.580563 0.344676 0.291121 11.00000 0.04810 0.03545 = 0.05053 -0.00245 0.03780 0.00318 AFIX 43 H13 2 0.589530 0.433014 0.275796 11.00000 -1.20000 AFIX 0 C14 1 0.602762 -0.017692 0.679243 11.00000 0.06847 0.03927 = 0.04874 0.02115 0.04146 0.02581 AFIX 43 H14 2 0.614653 -0.106712 0.707354 11.00000 -1.20000 AFIX 0 C15 1 0.515280 0.291204 0.243241 11.00000 0.05259 0.04332 = 0.03204 0.00590 0.02615 0.00702 AFIX 43 H15 2 0.481961 0.341183 0.194695 11.00000 -1.20000 AFIX 0 C16 1 0.733163 0.617123 0.523112 11.00000 0.03357 0.08453 = 0.06439 -0.00768 0.01837 0.00864 AFIX 137 H16A 2 0.725011 0.523499 0.496686 11.00000 -1.50000 H16B 2 0.771271 0.611085 0.581547 11.00000 -1.50000 H16C 2 0.742538 0.686658 0.493756 11.00000 -1.50000 AFIX 0 C17 1 0.617520 0.141177 0.383578 11.00000 0.05499 0.04851 = 0.04425 -0.00021 0.03402 0.03194 AFIX 43 H17 2 0.652134 0.088007 0.429331 11.00000 -1.20000 AFIX 0 C18 1 0.443583 0.166283 0.496105 11.00000 0.04366 0.04046 = 0.03111 0.00609 0.01860 -0.00794 AFIX 13 H18 2 0.438697 0.270327 0.482608 11.00000 -1.20000 AFIX 0 C19 1 0.544421 0.626255 0.406903 11.00000 0.03318 0.01802 = 0.02479 -0.00231 0.02069 0.00102 C20 1 0.631842 0.273026 0.359462 11.00000 0.04822 0.05216 = 0.05479 -0.00511 0.03690 0.01231 AFIX 43 H20 2 0.675703 0.309903 0.389990 11.00000 -1.20000 AFIX 0 C21 1 0.498457 0.164705 0.266076 11.00000 0.04916 0.03477 = 0.04048 -0.00730 0.03212 0.00605 C22 1 0.633880 0.219607 0.662045 11.00000 0.03117 0.04260 = 0.02596 0.01538 0.01892 0.01586 C23 1 0.687738 0.335609 0.689940 11.00000 0.03101 0.07852 = 0.03379 0.02462 0.01536 0.01320 AFIX 13 H23 2 0.664777 0.422497 0.655541 11.00000 -1.20000 AFIX 0 C24 1 0.416748 0.602048 0.308269 11.00000 0.03074 0.03410 = 0.02982 0.00417 0.01607 -0.00176 AFIX 13 H24 2 0.424993 0.573210 0.362700 11.00000 -1.20000 AFIX 0 C25 1 0.650870 0.085667 0.703251 11.00000 0.04744 0.06245 = 0.03802 0.02058 0.02604 0.02269 AFIX 43 H25 2 0.695608 0.066708 0.747675 11.00000 -1.20000 AFIX 0 C26 1 0.551118 0.091471 0.338255 11.00000 0.07576 0.02795 = 0.04736 -0.00644 0.04664 0.00601 AFIX 43 H26 2 0.541343 0.007404 0.356271 11.00000 -1.20000 AFIX 0 C27 1 0.392773 0.127701 0.516521 11.00000 0.05285 0.06619 = 0.05721 -0.00006 0.03803 -0.00217 AFIX 137 H27A 2 0.392842 0.024366 0.523854 11.00000 -1.50000 H27B 2 0.348314 0.158482 0.470559 11.00000 -1.50000 H27C 2 0.405180 0.175965 0.568003 11.00000 -1.50000 AFIX 0 C28 1 0.683641 0.810471 0.561932 11.00000 0.05549 0.09911 = 0.04994 -0.02679 0.00768 0.00955 AFIX 137 H28A 2 0.719501 0.801840 0.621345 11.00000 -1.50000 H28B 2 0.642963 0.841672 0.555649 11.00000 -1.50000 H28C 2 0.696086 0.880556 0.536037 11.00000 -1.50000 AFIX 0 C29 1 0.722011 0.378345 0.783831 11.00000 0.07440 0.10241 = 0.05325 -0.00725 0.02899 -0.04087 AFIX 137 H29A 2 0.747577 0.297303 0.819712 11.00000 -1.50000 H29B 2 0.688016 0.405088 0.792792 11.00000 -1.50000 H29C 2 0.751806 0.459289 0.797526 11.00000 -1.50000 AFIX 0 C30 1 0.428675 0.105286 0.215429 11.00000 0.06594 0.04767 = 0.04926 -0.01165 0.03184 -0.00910 AFIX 137 H30A 2 0.400437 0.164594 0.165862 11.00000 -1.50000 H30B 2 0.411013 0.105186 0.249380 11.00000 -1.50000 H30C 2 0.429365 0.007585 0.198234 11.00000 -1.50000 AFIX 0 C31 1 0.370950 0.728254 0.277750 11.00000 0.04504 0.08403 = 0.13788 0.01211 0.04639 0.01425 AFIX 137 H31A 2 0.358340 0.755275 0.222057 11.00000 -1.50000 H31B 2 0.393562 0.808377 0.316177 11.00000 -1.50000 H31C 2 0.331068 0.703449 0.275107 11.00000 -1.50000 AFIX 0 C32 1 0.427041 0.083065 0.416988 11.00000 0.07144 0.15795 = 0.03631 -0.03789 0.03253 -0.03278 AFIX 137 H32A 2 0.460800 0.103946 0.406665 11.00000 -1.50000 H32B 2 0.383378 0.112636 0.368641 11.00000 -1.50000 H32C 2 0.426588 -0.019496 0.426118 11.00000 -1.50000 AFIX 0 C33 1 0.740374 0.291708 0.674092 11.00000 0.06226 0.13365 = 0.12948 0.01987 0.06981 0.01052 AFIX 137 H33A 2 0.770368 0.220718 0.715586 11.00000 -1.50000 H33B 2 0.765900 0.375770 0.678603 11.00000 -1.50000 H33C 2 0.718144 0.250869 0.618063 11.00000 -1.50000 AFIX 0 C34 1 0.386509 0.478524 0.252504 11.00000 0.12237 0.12637 = 0.13110 -0.00737 0.07502 -0.00143 AFIX 137 H34A 2 0.344640 0.454496 0.245076 11.00000 -1.50000 H34B 2 0.416824 0.397038 0.276970 11.00000 -1.50000 H34C 2 0.377884 0.501608 0.198252 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1_a.res in Cc REM R1 = 0.0449 for 4635 Fo > 4sig(Fo) and 0.0840 for all 6285 data REM 406 parameters refined using 8 restraints END WGHT 0.0241 4.7600 REM Highest difference peak 0.724, deepest hole -0.446, 1-sigma level 0.085 Q1 1 0.3655 0.5242 0.2146 11.00000 0.05 0.72 Q2 1 0.3746 0.6807 0.1892 11.00000 0.05 0.41 Q3 1 0.2798 0.4872 0.2187 11.00000 0.05 0.40 Q4 1 0.7444 0.9016 0.6404 11.00000 0.05 0.39 Q5 1 0.3071 0.6248 0.4307 11.00000 0.05 0.37 Q6 1 0.5319 0.8296 0.2169 11.00000 0.05 0.37 Q7 1 0.6465 0.9369 0.3316 11.00000 0.05 0.35 Q8 1 0.3880 0.5498 0.5424 11.00000 0.05 0.34 Q9 1 0.5488 0.3156 0.5709 11.00000 0.05 0.34 Q10 1 0.3390 0.6388 0.5070 11.00000 0.05 0.33 Q11 1 0.3408 -0.1017 0.4383 11.00000 0.05 0.33 Q12 1 0.2878 0.7013 0.2217 11.00000 0.05 0.33 Q13 1 0.3699 0.7422 0.5083 11.00000 0.05 0.33 Q14 1 0.7898 0.2748 0.7864 11.00000 0.05 0.32 Q15 1 0.3143 0.7416 0.3537 11.00000 0.05 0.32 Q16 1 0.7193 0.4701 0.6718 11.00000 0.05 0.32 Q17 1 0.7729 0.2538 0.9017 11.00000 0.05 0.32 Q18 1 0.5206 0.8561 0.5138 11.00000 0.05 0.31 Q19 1 0.6789 0.5993 0.7591 11.00000 0.05 0.31 Q20 1 0.3114 0.4644 0.1999 11.00000 0.05 0.31 ; _shelx_res_checksum 72544 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -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 Sb1 Sb 0.32451(3) 0.59168(6) 0.46651(3) 0.04101(19) Uani 1 1 d . . Cu1 Cu 0.58111(6) 0.28361(12) 0.43174(6) 0.0382(3) Uani 1 1 d . . N2 N 0.5491(3) 0.3796(6) 0.5510(4) 0.0212(15) Uani 1 1 d . . N1 N 0.5418(3) 0.5514(7) 0.4716(4) 0.0238(16) Uani 1 1 d . . F6 F 0.3512(3) 0.4800(6) 0.4098(4) 0.0629(17) Uani 1 1 d . . F1 F 0.3911(4) 0.7273(7) 0.4948(6) 0.100(3) Uani 1 1 d . . F2 F 0.2630(3) 0.6890(7) 0.3659(4) 0.078(2) Uani 1 1 d . . F4 F 0.2587(3) 0.4561(7) 0.4396(5) 0.076(2) Uani 1 1 d . . F3 F 0.2959(4) 0.6998(8) 0.5218(4) 0.087(2) Uani 1 1 d . . F5 F 0.3871(3) 0.4936(7) 0.5671(4) 0.077(2) Uani 1 1 d . . C1 C 0.4850(4) 0.6418(8) 0.3268(5) 0.026(2) Uani 1 1 d . . C2 C 0.5566(4) 0.4080(9) 0.4879(5) 0.0238(18) Uani 1 1 d . . C3 C 0.5297(4) 0.5005(9) 0.5734(5) 0.029(2) Uani 1 1 d . . H3 H 0.5209 0.5062 0.6147 0.035 Uiso 1 1 calc R U C4 C 0.6074(4) 0.6720(9) 0.4281(5) 0.029(2) Uani 1 1 d . . C5 C 0.5162(5) 0.1399(9) 0.5694(5) 0.026(2) Uani 1 1 d . . C6 C 0.6716(5) 0.6643(10) 0.5190(6) 0.041(2) Uani 1 1 d . . H6 H 0.6638 0.5927 0.5504 0.049 Uiso 1 1 calc R U C7 C 0.5256(5) 0.6100(10) 0.5238(5) 0.029(2) Uani 1 1 d . . H7 H 0.5142 0.7063 0.5247 0.034 Uiso 1 1 calc R U C8 C 0.4901(5) 0.7002(9) 0.2637(6) 0.033(2) Uani 1 1 d . . H8 H 0.4513 0.7099 0.2086 0.039 Uiso 1 1 calc R U C9 C 0.6098(5) 0.7313(9) 0.3631(6) 0.030(2) Uani 1 1 d . . H9 H 0.6509 0.7629 0.3748 0.036 Uiso 1 1 calc R U C10 C 0.5521(5) 0.7439(9) 0.2821(6) 0.033(2) Uani 1 1 d . . H10 H 0.5547 0.7820 0.2391 0.039 Uiso 1 1 calc R U C11 C 0.5373(6) 0.0088(10) 0.6142(6) 0.040(3) Uani 1 1 d . . H11 H 0.5052 -0.0634 0.5990 0.048 Uiso 1 1 calc R U C12 C 0.5674(5) 0.2412(9) 0.5953(5) 0.025(2) Uani 1 1 d . . C13 C 0.5806(5) 0.3447(10) 0.2911(6) 0.039(2) Uani 1 1 d . . H13 H 0.5895 0.4330 0.2758 0.047 Uiso 1 1 calc R U C14 C 0.6028(6) -0.0177(11) 0.6792(7) 0.048(3) Uani 1 1 d . . H14 H 0.6147 -0.1067 0.7074 0.057 Uiso 1 1 calc R U C15 C 0.5153(5) 0.2912(10) 0.2432(6) 0.042(2) Uani 1 1 d . . H15 H 0.4820 0.3412 0.1947 0.050 Uiso 1 1 calc R U C16 C 0.7332(6) 0.6171(13) 0.5231(8) 0.066(4) Uani 1 1 d . . H16A H 0.7250 0.5235 0.4967 0.100 Uiso 1 1 calc R U H16B H 0.7713 0.6111 0.5815 0.100 Uiso 1 1 calc R U H16C H 0.7425 0.6867 0.4938 0.100 Uiso 1 1 calc R U C17 C 0.6175(7) 0.1412(13) 0.3836(7) 0.046(3) Uani 1 1 d . . H17 H 0.6521 0.0880 0.4293 0.055 Uiso 1 1 calc R U C18 C 0.4436(5) 0.1663(10) 0.4961(5) 0.040(2) Uani 1 1 d . . H18 H 0.4387 0.2703 0.4826 0.048 Uiso 1 1 calc R U C19 C 0.5444(4) 0.6263(8) 0.4069(5) 0.0230(19) Uani 1 1 d . . C20 C 0.6318(6) 0.2730(11) 0.3595(7) 0.048(3) Uani 1 1 d . . H20 H 0.6757 0.3099 0.3900 0.057 Uiso 1 1 calc R U C21 C 0.4985(5) 0.1647(10) 0.2661(6) 0.038(2) Uani 1 1 d . . C22 C 0.6339(5) 0.2196(11) 0.6620(5) 0.032(2) Uani 1 1 d . . C23 C 0.6877(5) 0.3356(13) 0.6899(6) 0.050(3) Uani 1 1 d . . H23 H 0.6648 0.4225 0.6555 0.060 Uiso 1 1 calc R U C24 C 0.4167(4) 0.6020(9) 0.3083(5) 0.032(2) Uani 1 1 d . . H24 H 0.4250 0.5732 0.3627 0.039 Uiso 1 1 calc R U C25 C 0.6509(5) 0.0857(12) 0.7033(6) 0.048(3) Uani 1 1 d . . H25 H 0.6956 0.0667 0.7477 0.058 Uiso 1 1 calc R U C26 C 0.5511(6) 0.0915(10) 0.3383(6) 0.044(3) Uani 1 1 d . . H26 H 0.5413 0.0074 0.3563 0.053 Uiso 1 1 calc R U C27 C 0.3928(5) 0.1277(11) 0.5165(7) 0.055(3) Uani 1 1 d . . H27A H 0.3928 0.0244 0.5239 0.083 Uiso 1 1 calc R U H27B H 0.3483 0.1585 0.4706 0.083 Uiso 1 1 calc R U H27C H 0.4052 0.1760 0.5680 0.083 Uiso 1 1 calc R U C28 C 0.6836(6) 0.8105(14) 0.5619(7) 0.081(4) Uani 1 1 d . . H28A H 0.7195 0.8018 0.6213 0.121 Uiso 1 1 calc R U H28B H 0.6430 0.8417 0.5556 0.121 Uiso 1 1 calc R U H28C H 0.6961 0.8806 0.5360 0.121 Uiso 1 1 calc R U C29 C 0.7220(7) 0.3783(14) 0.7838(7) 0.081(4) Uani 1 1 d . . H29A H 0.7476 0.2973 0.8197 0.122 Uiso 1 1 calc R U H29B H 0.6880 0.4051 0.7928 0.122 Uiso 1 1 calc R U H29C H 0.7518 0.4593 0.7975 0.122 Uiso 1 1 calc R U C30 C 0.4287(5) 0.1053(11) 0.2154(7) 0.055(3) Uani 1 1 d . . H30A H 0.4004 0.1646 0.1659 0.082 Uiso 1 1 calc R U H30B H 0.4110 0.1052 0.2494 0.082 Uiso 1 1 calc R U H30C H 0.4294 0.0076 0.1982 0.082 Uiso 1 1 calc R U C31 C 0.3710(6) 0.7283(14) 0.2778(10) 0.092(5) Uani 1 1 d . . H31A H 0.3583 0.7553 0.2221 0.139 Uiso 1 1 calc R U H31B H 0.3936 0.8084 0.3162 0.139 Uiso 1 1 calc R U H31C H 0.3311 0.7034 0.2751 0.139 Uiso 1 1 calc R U C32 C 0.4270(7) 0.0831(16) 0.4170(7) 0.088(5) Uani 1 1 d . . H32A H 0.4608 0.1039 0.4067 0.131 Uiso 1 1 calc R U H32B H 0.3834 0.1126 0.3686 0.131 Uiso 1 1 calc R U H32C H 0.4266 -0.0195 0.4261 0.131 Uiso 1 1 calc R U C33 C 0.7404(7) 0.2917(16) 0.6741(10) 0.100(5) Uani 1 1 d . . H33A H 0.7704 0.2207 0.7156 0.150 Uiso 1 1 calc R U H33B H 0.7659 0.3758 0.6786 0.150 Uiso 1 1 calc R U H33C H 0.7181 0.2509 0.6181 0.150 Uiso 1 1 calc R U C34 C 0.3865(9) 0.4785(18) 0.2525(11) 0.125(6) Uani 1 1 d . U H34A H 0.3446 0.4545 0.2451 0.188 Uiso 1 1 calc R U H34B H 0.4168 0.3970 0.2770 0.188 Uiso 1 1 calc R U H34C H 0.3779 0.5016 0.1983 0.188 Uiso 1 1 calc R 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 0.0294(3) 0.0453(3) 0.0490(4) -0.0065(4) 0.0228(3) 0.0007(4) Cu1 0.0551(8) 0.0368(6) 0.0358(7) 0.0063(6) 0.0336(7) 0.0191(6) N2 0.025(4) 0.023(4) 0.018(4) 0.001(3) 0.014(3) 0.005(3) N1 0.026(4) 0.029(4) 0.018(4) 0.008(3) 0.014(3) 0.005(3) F6 0.074(5) 0.058(4) 0.082(5) -0.001(4) 0.059(4) 0.017(4) F1 0.067(5) 0.046(4) 0.195(8) -0.025(5) 0.080(6) -0.021(4) F2 0.072(5) 0.093(5) 0.081(5) 0.032(4) 0.051(4) 0.037(4) F4 0.057(4) 0.087(5) 0.090(5) -0.003(4) 0.045(4) -0.018(4) F3 0.069(5) 0.119(7) 0.068(5) -0.030(5) 0.035(4) 0.020(5) F5 0.065(5) 0.091(5) 0.050(4) 0.004(4) 0.018(4) 0.024(4) C1 0.028(5) 0.021(5) 0.028(5) 0.005(4) 0.016(5) 0.005(4) C2 0.028(5) 0.020(4) 0.028(5) 0.005(4) 0.019(4) 0.001(4) C3 0.037(6) 0.037(5) 0.023(5) 0.000(4) 0.023(5) 0.006(5) C4 0.037(6) 0.023(5) 0.031(5) 0.006(4) 0.022(5) 0.002(4) C5 0.041(6) 0.024(5) 0.023(5) 0.005(4) 0.023(5) 0.007(4) C6 0.029(6) 0.050(6) 0.033(6) 0.013(5) 0.012(5) -0.002(5) C7 0.026(5) 0.033(5) 0.027(5) -0.005(4) 0.016(5) 0.011(4) C8 0.044(7) 0.025(5) 0.032(5) 0.008(4) 0.023(5) 0.003(5) C9 0.036(6) 0.024(5) 0.048(6) -0.001(5) 0.034(6) -0.004(5) C10 0.059(7) 0.023(5) 0.033(6) 0.002(4) 0.036(6) -0.004(5) C11 0.066(8) 0.024(5) 0.040(6) 0.003(5) 0.037(6) 0.008(5) C12 0.030(6) 0.031(5) 0.025(5) 0.008(4) 0.023(5) 0.013(4) C13 0.048(7) 0.035(5) 0.051(7) -0.002(5) 0.038(6) 0.003(5) C14 0.068(8) 0.039(6) 0.049(7) 0.021(5) 0.041(7) 0.026(6) C15 0.053(7) 0.043(6) 0.032(6) 0.006(5) 0.026(6) 0.007(5) C16 0.034(7) 0.085(9) 0.064(9) -0.008(7) 0.018(7) 0.009(6) C17 0.055(8) 0.049(7) 0.044(7) 0.000(6) 0.034(7) 0.032(6) C18 0.044(7) 0.040(6) 0.031(6) 0.006(4) 0.019(5) -0.008(5) C19 0.033(5) 0.018(5) 0.025(5) -0.002(4) 0.021(5) 0.001(4) C20 0.048(7) 0.052(7) 0.055(7) -0.005(6) 0.037(7) 0.012(6) C21 0.049(7) 0.035(5) 0.040(6) -0.007(5) 0.032(6) 0.006(5) C22 0.031(6) 0.043(6) 0.026(5) 0.015(5) 0.019(5) 0.016(5) C23 0.031(6) 0.079(8) 0.034(6) 0.025(5) 0.015(5) 0.013(6) C24 0.031(5) 0.034(5) 0.030(5) 0.004(4) 0.016(4) -0.002(5) C25 0.047(7) 0.062(7) 0.038(6) 0.021(6) 0.026(5) 0.023(6) C26 0.076(8) 0.028(5) 0.047(6) -0.006(5) 0.047(7) 0.006(6) C27 0.053(7) 0.066(7) 0.057(7) 0.000(6) 0.038(6) -0.002(6) C28 0.055(8) 0.099(10) 0.050(8) -0.027(7) 0.008(7) 0.010(7) C29 0.074(9) 0.102(10) 0.053(8) -0.007(7) 0.029(7) -0.041(8) C30 0.066(8) 0.048(6) 0.049(6) -0.012(5) 0.032(6) -0.009(6) C31 0.045(8) 0.084(10) 0.138(13) 0.012(9) 0.046(9) 0.014(7) C32 0.071(11) 0.158(14) 0.036(8) -0.038(8) 0.033(8) -0.033(9) C33 0.062(9) 0.134(12) 0.129(13) 0.020(10) 0.070(10) 0.011(9) C34 0.122(6) 0.126(6) 0.131(6) -0.007(3) 0.075(4) -0.001(3) 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' 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 F4 Sb1 F1 179.3(4) F4 Sb1 F2 89.4(3) F1 Sb1 F2 91.2(4) F4 Sb1 F3 88.9(3) F1 Sb1 F3 90.9(3) F2 Sb1 F3 90.0(3) F4 Sb1 F6 89.6(3) F1 Sb1 F6 90.7(3) F2 Sb1 F6 89.7(3) F3 Sb1 F6 178.4(4) F4 Sb1 F5 91.1(3) F1 Sb1 F5 88.3(4) F2 Sb1 F5 179.1(3) F3 Sb1 F5 90.8(3) F6 Sb1 F5 89.5(3) C2 Cu1 C17 173.5(4) C2 Cu1 C20 144.5(4) C17 Cu1 C20 37.0(4) C2 Cu1 C26 147.6(4) C17 Cu1 C26 36.4(4) C20 Cu1 C26 62.8(4) C2 N2 C3 111.8(6) C2 N2 C12 122.9(6) C3 N2 C12 124.9(6) C2 N1 C7 111.1(7) C2 N1 C19 121.7(6) C7 N1 C19 127.2(7) C19 C1 C8 117.1(8) C19 C1 C24 122.0(7) C8 C1 C24 120.8(8) N2 C2 N1 104.1(7) N2 C2 Cu1 130.0(6) N1 C2 Cu1 125.9(6) C7 C3 N2 106.5(7) C7 C3 H3 126.7 N2 C3 H3 126.7 C9 C4 C19 117.0(8) C9 C4 C6 120.2(8) C19 C4 C6 122.7(7) C12 C5 C11 115.1(9) C12 C5 C18 122.9(8) C11 C5 C18 122.0(9) C16 C6 C28 110.6(9) C16 C6 C4 113.4(8) C28 C6 C4 109.3(8) C16 C6 H6 107.8 C28 C6 H6 107.8 C4 C6 H6 107.8 C3 C7 N1 106.5(7) C3 C7 H7 126.7 N1 C7 H7 126.7 C10 C8 C1 120.7(9) C10 C8 H8 119.7 C1 C8 H8 119.7 C10 C9 C4 120.8(8) C10 C9 H9 119.6 C4 C9 H9 119.6 C9 C10 C8 120.6(8) C9 C10 H10 119.7 C8 C10 H10 119.7 C14 C11 C5 122.7(10) C14 C11 H11 118.6 C5 C11 H11 118.6 C22 C12 C5 123.8(8) C22 C12 N2 118.2(8) C5 C12 N2 118.0(8) C20 C13 C15 122.2(10) C20 C13 H13 118.9 C15 C13 H13 118.9 C25 C14 C11 120.1(9) C25 C14 H14 120.0 C11 C14 H14 120.0 C13 C15 C21 121.2(9) C13 C15 H15 119.4 C21 C15 H15 119.4 C6 C16 H16A 109.5 C6 C16 H16B 109.5 H16A C16 H16B 109.5 C6 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C20 C17 C26 119.3(11) C20 C17 Cu1 81.2(6) C26 C17 Cu1 81.7(6) C20 C17 H17 120.4 C26 C17 H17 120.4 Cu1 C17 H17 107.0 C5 C18 C27 113.4(7) C5 C18 C32 110.2(9) C27 C18 C32 110.2(9) C5 C18 H18 107.6 C27 C18 H18 107.6 C32 C18 H18 107.6 C1 C19 C4 123.7(7) C1 C19 N1 118.3(7) C4 C19 N1 117.9(7) C13 C20 C17 118.6(11) C13 C20 Cu1 93.3(6) C17 C20 Cu1 61.8(5) C13 C20 H20 120.7 C17 C20 H20 120.7 Cu1 C20 H20 114.0 C15 C21 C26 116.9(9) C15 C21 C30 122.1(9) C26 C21 C30 121.0(9) C12 C22 C25 117.5(9) C12 C22 C23 122.0(8) C25 C22 C23 120.5(9) C33 C23 C22 112.7(10) C33 C23 C29 110.6(10) C22 C23 C29 111.6(8) C33 C23 H23 107.2 C22 C23 H23 107.2 C29 C23 H23 107.2 C34 C24 C31 112.4(11) C34 C24 C1 112.6(10) C31 C24 C1 111.7(8) C34 C24 H24 106.5 C31 C24 H24 106.5 C1 C24 H24 106.5 C14 C25 C22 120.7(9) C14 C25 H25 119.7 C22 C25 H25 119.7 C21 C26 C17 121.7(10) C21 C26 Cu1 95.8(5) C17 C26 Cu1 61.9(5) C21 C26 H26 119.1 C17 C26 H26 119.1 Cu1 C26 H26 112.3 C18 C27 H27A 109.5 C18 C27 H27B 109.5 H27A C27 H27B 109.5 C18 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C6 C28 H28A 109.5 C6 C28 H28B 109.5 H28A C28 H28B 109.5 C6 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C23 C29 H29A 109.5 C23 C29 H29B 109.5 H29A C29 H29B 109.5 C23 C29 H29C 109.5 H29A C29 H29C 109.5 H29B C29 H29C 109.5 C21 C30 H30A 109.5 C21 C30 H30B 109.5 H30A C30 H30B 109.5 C21 C30 H30C 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 C24 C31 H31A 109.5 C24 C31 H31B 109.5 H31A C31 H31B 109.5 C24 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 C18 C32 H32A 109.5 C18 C32 H32B 109.5 H32A C32 H32B 109.5 C18 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 C23 C33 H33A 109.5 C23 C33 H33B 109.5 H33A C33 H33B 109.5 C23 C33 H33C 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C24 C34 H34A 109.5 C24 C34 H34B 109.5 H34A C34 H34B 109.5 C24 C34 H34C 109.5 H34A C34 H34C 109.5 H34B C34 H34C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Sb1 F4 1.843(6) Sb1 F1 1.851(6) Sb1 F2 1.854(6) Sb1 F3 1.851(6) Sb1 F6 1.857(5) Sb1 F5 1.863(6) Cu1 C2 1.882(8) Cu1 C17 2.065(9) Cu1 C20 2.316(9) Cu1 C26 2.317(9) N2 C2 1.346(10) N2 C3 1.367(10) N2 C12 1.451(10) N1 C2 1.355(10) N1 C7 1.375(10) N1 C19 1.450(10) C1 C19 1.380(11) C1 C8 1.391(11) C1 C24 1.515(11) C3 C7 1.349(12) C3 H3 0.9300 C4 C9 1.390(12) C4 C19 1.391(11) C4 C6 1.531(12) C5 C12 1.389(12) C5 C11 1.396(12) C5 C18 1.509(12) C6 C16 1.502(14) C6 C28 1.515(14) C6 H6 0.9800 C7 H7 0.9300 C8 C10 1.384(12) C8 H8 0.9300 C9 C10 1.372(13) C9 H9 0.9300 C10 H10 0.9300 C11 C14 1.359(14) C11 H11 0.9300 C12 C22 1.376(12) C13 C20 1.349(13) C13 C15 1.379(13) C13 H13 0.9300 C14 C25 1.359(14) C14 H14 0.9300 C15 C21 1.382(12) C15 H15 0.9300 C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C17 C20 1.409(15) C17 C26 1.389(16) C17 H17 0.9300 C18 C27 1.525(12) C18 C32 1.533(14) C18 H18 0.9800 C20 H20 0.9300 C21 C26 1.402(13) C21 C30 1.482(13) C22 C25 1.392(13) C22 C23 1.520(14) C23 C33 1.518(14) C23 C29 1.540(14) C23 H23 0.9800 C24 C34 1.439(17) C24 C31 1.471(14) C24 H24 0.9800 C25 H25 0.9300 C26 H26 0.9300 C27 H27A 0.9600 C27 H27B 0.9600 C27 H27C 0.9600 C28 H28A 0.9600 C28 H28B 0.9600 C28 H28C 0.9600 C29 H29A 0.9600 C29 H29B 0.9600 C29 H29C 0.9600 C30 H30A 0.9600 C30 H30B 0.9600 C30 H30C 0.9600 C31 H31A 0.9600 C31 H31B 0.9600 C31 H31C 0.9600 C32 H32A 0.9600 C32 H32B 0.9600 C32 H32C 0.9600 C33 H33A 0.9600 C33 H33B 0.9600 C33 H33C 0.9600 C34 H34A 0.9600 C34 H34B 0.9600 C34 H34C 0.9600