Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year 2005 _journal_page_first 2547 _audit_creation_method Xtal3.6 _audit_creation_date 02-11-28 _audit_update_record ? _publ_contact_author_name 'Prof Peter Healy' _publ_contact_author_address ; School of Science Griffith University Nathan Campus Brisbane Queensland 4111 AUSTRALIA ; _publ_contact_author_email P.HEALY@GRIFFITH.EDU.AU _publ_section_title ; Structural and solid state 31P NMR studies of the four-coordinate copper(I) complexes [Cu(PPh3)3X] and [Cu(PPh3)3(CH3CN)]X ; _publ_section_references ; Sheldrick, G M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data. University of Gottingen, Germany. Siemens (1995). SMART and SAINT. Area-Detector Control and Integration Software. Siemens Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Hall, S.R., King, G.S.D., and Stewart., J.M. (1995). The Xtal 3.5 User's Manual. University of Western Australia, Lamb: Perth. ; loop_ _publ_author_name 'John V. Hanna' 'Sue E. Boyd' P.C.Healy G.A.Bowmanker 'Brian W. Skelton' 'A. H. White' data_6_H1187 _database_code_depnum_ccdc_archive 'CCDC 268666' # EXPERIMENTAL DATA #--------------------- _chemical_name_systematic ; Tris(triphenylphosphine)(acetonitrile)copper(I) perchlorate ; _chemical_formula_sum 'C56 H48 Cl1 Cu1 N1 O4 P3' _chemical_formula_moiety ? _chemical_formula_weight 990.92 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_b_c_a _symmetry_space_group_name_Hall -p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z _cell_length_a 17.6850(10) _cell_length_b 22.314(2) _cell_length_c 24.289(2) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 9585.0(13) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7884 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 30.94 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .66 _exptl_crystal_description prism _exptl_crystal_size_max .4 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .19 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .81 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 152360 _reflns_number_total 17060 _reflns_Friedel_coverage 0 _reflns_number_gt 11151 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 32.34 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .077 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .051 _refine_ls_wR_factor_ref .067 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_number_reflns 11151 _refine_ls_number_parameters 595 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .007 _refine_diff_density_min -.379 _refine_diff_density_max 1.356 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 448 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 384 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 8 .132 .159 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 8 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 32 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 24 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Cl1 Cl Uani 0.13073(4) 0.47487(3) 0.14595(3) 1.000 0.0340(2) . . O1 O Uani 0.10808(14) 0.42444(10) 0.11359(9) 1.000 0.0489(8) . . O2 O Uani 0.07271(15) 0.51907(12) 0.14427(12) 1.000 0.0643(10) . . O3 O Uani 0.14372(16) 0.45552(14) 0.20139(9) 1.000 0.0635(10) . . O4 O Uani 0.19888(15) 0.49889(14) 0.12398(13) 1.000 0.0685(11) . . Cu1 Cu Uani 0.44332(1) 0.24374(1) 0.35864(1) 1.000 0.0166(1) . . P1 P Uani 0.43091(3) 0.16611(3) 0.29621(2) 1.000 0.0173(1) . . P2 P Uani 0.45630(3) 0.21185(3) 0.44876(2) 1.000 0.0174(1) . . P3 P Uani 0.36675(3) 0.32768(2) 0.35018(2) 1.000 0.0175(2) . . N1 N Uani 0.55111(12) 0.27248(9) 0.34130(8) 1.000 0.0230(5) . . C1 C Uani 0.60998(14) 0.28976(11) 0.33257(10) 1.000 0.0229(6) . . C11 C Uani 0.68520(16) 0.31378(15) 0.32121(13) 1.000 0.0403(9) . . C111 C Uani 0.37259(13) 0.10436(10) 0.32129(9) 1.000 0.0186(5) . . C112 C Uani 0.31614(14) 0.11822(10) 0.35935(10) 1.000 0.0231(6) . . C113 C Uani 0.27021(14) 0.07414(12) 0.38131(10) 1.000 0.0278(7) . . C114 C Uani 0.27932(16) 0.01526(12) 0.36488(12) 1.000 0.0307(8) . . C115 C Uani 0.33524(17) 0.00112(11) 0.32646(12) 1.000 0.0329(8) . . C116 C Uani 0.38179(14) 0.04506(11) 0.30487(11) 1.000 0.0270(7) . . C121 C Uani 0.38847(12) 0.18653(10) 0.23022(9) 1.000 0.0196(6) . . C122 C Uani 0.40220(14) 0.24449(10) 0.21119(10) 1.000 0.0237(6) . . C123 C Uani 0.37383(17) 0.26356(12) 0.16082(11) 1.000 0.0312(8) . . C124 C Uani 0.33222(17) 0.22405(15) 0.12876(11) 1.000 0.0369(9) . . C125 C Uani 0.31888(16) 0.16649(14) 0.14705(10) 1.000 0.0341(8) . . C126 C Uani 0.34617(15) 0.14770(12) 0.19752(10) 1.000 0.0267(7) . . C131 C Uani 0.51939(13) 0.13072(10) 0.27554(9) 1.000 0.0190(6) . . C132 C Uani 0.57820(14) 0.12732(11) 0.31377(10) 1.000 0.0248(6) . . C133 C Uani 0.64578(14) 0.10004(13) 0.30027(11) 1.000 0.0297(7) . . C134 C Uani 0.65686(15) 0.07568(12) 0.24846(11) 1.000 0.0297(7) . . C135 C Uani 0.59894(15) 0.07856(12) 0.21012(10) 1.000 0.0283(7) . . C136 C Uani 0.53034(14) 0.10558(11) 0.22333(9) 1.000 0.0231(6) . . C211 C Uani 0.49392(13) 0.26961(9) 0.49462(9) 1.000 0.0190(5) . . C212 C Uani 0.52298(13) 0.32225(10) 0.47203(9) 1.000 0.0209(6) . . C213 C Uani 0.54977(14) 0.36741(11) 0.50604(10) 1.000 0.0241(6) . . C214 C Uani 0.54679(16) 0.36088(11) 0.56269(11) 1.000 0.0282(7) . . C215 C Uani 0.51750(18) 0.30910(12) 0.58557(10) 1.000 0.0320(8) . . C216 C Uani 0.49217(16) 0.26357(11) 0.55161(10) 1.000 0.0279(7) . . C221 C Uani 0.52317(14) 0.15007(11) 0.45708(9) 1.000 0.0243(6) . . C222 C Uani 0.50174(17) 0.09142(11) 0.44390(11) 1.000 0.0307(7) . . C223 C Uani 0.5532(2) 0.04520(14) 0.44657(13) 1.000 0.0463(10) . . C224 C Uani 0.6275(2) 0.05710(18) 0.46049(17) 1.000 0.0630(14) . . C225 C Uani 0.6498(2) 0.1141(2) 0.47297(18) 1.000 0.0663(16) . . C226 C Uani 0.59804(17) 0.16071(15) 0.47103(14) 1.000 0.0420(9) . . C231 C Uani 0.37264(13) 0.18464(10) 0.48494(9) 1.000 0.0195(6) . . C232 C Uani 0.30242(14) 0.20730(11) 0.46921(10) 1.000 0.0242(6) . . C233 C Uani 0.23631(14) 0.18799(12) 0.49446(10) 1.000 0.0289(7) . . C234 C Uani 0.23939(16) 0.14469(13) 0.53541(11) 1.000 0.0328(8) . . C235 C Uani 0.30854(18) 0.12184(13) 0.55162(11) 1.000 0.0338(8) . . C236 C Uani 0.37495(15) 0.14167(11) 0.52702(10) 1.000 0.0267(7) . . C311 C Uani 0.26559(13) 0.31148(10) 0.34627(9) 1.000 0.0210(6) . . C312 C Uani 0.24243(14) 0.26221(11) 0.31554(10) 1.000 0.0258(7) . . C313 C Uani 0.16603(16) 0.25030(13) 0.30722(12) 1.000 0.0340(8) . . C314 C Uani 0.11183(15) 0.28781(14) 0.32974(13) 1.000 0.0381(9) . . C315 C Uani 0.13426(15) 0.33604(14) 0.36148(14) 1.000 0.0383(9) . . C316 C Uani 0.21016(15) 0.34813(12) 0.36974(12) 1.000 0.0309(8) . . C321 C Uani 0.38316(13) 0.37315(10) 0.28857(9) 1.000 0.0200(6) . . C322 C Uani 0.45748(14) 0.38471(11) 0.27297(11) 1.000 0.0255(7) . . C323 C Uani 0.47318(15) 0.41882(12) 0.22649(11) 1.000 0.0298(7) . . C324 C Uani 0.41426(18) 0.44178(12) 0.19538(11) 1.000 0.0338(8) . . C325 C Uani 0.34052(16) 0.43089(12) 0.21027(10) 1.000 0.0310(8) . . C326 C Uani 0.32484(14) 0.39700(11) 0.25696(9) 1.000 0.0236(6) . . C331 C Uani 0.37519(13) 0.38272(10) 0.40551(9) 1.000 0.0201(6) . . C332 C Uani 0.34617(15) 0.37002(11) 0.45800(10) 1.000 0.0275(7) . . C333 C Uani 0.35571(16) 0.41003(12) 0.50116(11) 1.000 0.0329(8) . . C334 C Uani 0.39519(16) 0.46278(12) 0.49319(11) 1.000 0.0320(8) . . C335 C Uani 0.42614(16) 0.47514(11) 0.44206(11) 1.000 0.0293(7) . . C336 C Uani 0.41557(14) 0.43577(11) 0.39822(10) 1.000 0.0240(6) . . H11A H Uiso 0.71066 0.32356 0.35463 1.000 0.0600 . . H11B H Uiso 0.68183 0.34920 0.29918 1.000 0.0600 . . H11C H Uiso 0.71459 0.28499 0.30217 1.000 0.0600 . . H112 H Uiso 0.30977 0.15872 0.37094 1.000 0.0280 . . H113 H Uiso 0.23227 0.08439 0.40731 1.000 0.0340 . . H114 H Uiso 0.24778 -0.01525 0.38021 1.000 0.0380 . . H115 H Uiso 0.34116 -0.03968 0.31461 1.000 0.0400 . . H116 H Uiso 0.42107 0.03497 0.27890 1.000 0.0330 . . H122 H Uiso 0.43192 0.27173 0.23318 1.000 0.0290 . . H123 H Uiso 0.38216 0.30357 0.14835 1.000 0.0380 . . H124 H Uiso 0.31324 0.23673 0.09346 1.000 0.0440 . . H125 H Uiso 0.29101 0.13932 0.12433 1.000 0.0410 . . H126 H Uiso 0.33510 0.10760 0.21039 1.000 0.0320 . . H132 H Uiso 0.57047 0.14315 0.34982 1.000 0.0300 . . H133 H Uiso 0.68592 0.09794 0.32726 1.000 0.0360 . . H134 H Uiso 0.70407 0.05781 0.23852 1.000 0.0370 . . H135 H Uiso 0.60596 0.06164 0.17432 1.000 0.0350 . . H136 H Uiso 0.49066 0.10753 0.19632 1.000 0.0290 . . H212 H Uiso 0.52443 0.32741 0.43300 1.000 0.0260 . . H213 H Uiso 0.57146 0.40291 0.49009 1.000 0.0290 . . H214 H Uiso 0.56449 0.39265 0.58590 1.000 0.0350 . . H215 H Uiso 0.51505 0.30480 0.62470 1.000 0.0380 . . H216 H Uiso 0.47279 0.22704 0.56746 1.000 0.0330 . . H222 H Uiso 0.45073 0.08382 0.43316 1.000 0.0400 . . H223 H Uiso 0.53770 0.00512 0.43834 1.000 0.0560 . . H224 H Uiso 0.66322 0.02483 0.46269 1.000 0.0770 . . H225 H Uiso 0.70260 0.12264 0.48065 1.000 0.0810 . . H226 H Uiso 0.61285 0.20058 0.48084 1.000 0.0540 . . H232 H Uiso 0.29958 0.23643 0.44026 1.000 0.0310 . . H233 H Uiso 0.18852 0.20450 0.48372 1.000 0.0350 . . H234 H Uiso 0.19339 0.13079 0.55200 1.000 0.0410 . . H235 H Uiso 0.31074 0.09255 0.58043 1.000 0.0400 . . H236 H Uiso 0.42305 0.12554 0.53833 1.000 0.0340 . . H312 H Uiso 0.27957 0.23650 0.29967 1.000 0.0320 . . H313 H Uiso 0.15078 0.21595 0.28694 1.000 0.0420 . . H314 H Uiso 0.05975 0.28071 0.32312 1.000 0.0470 . . H315 H Uiso 0.09604 0.36177 0.37739 1.000 0.0470 . . H316 H Uiso 0.22567 0.38189 0.39159 1.000 0.0380 . . H322 H Uiso 0.49844 0.36918 0.29496 1.000 0.0320 . . H323 H Uiso 0.52434 0.42703 0.21614 1.000 0.0370 . . H324 H Uiso 0.42576 0.46506 0.16327 1.000 0.0410 . . H325 H Uiso 0.30019 0.44704 0.18848 1.000 0.0370 . . H326 H Uiso 0.27335 0.39066 0.26799 1.000 0.0300 . . H332 H Uiso 0.31828 0.33404 0.46372 1.000 0.0340 . . H333 H Uiso 0.33543 0.40098 0.53649 1.000 0.0400 . . H334 H Uiso 0.40098 0.49065 0.52245 1.000 0.0390 . . H335 H Uiso 0.45549 0.51029 0.43697 1.000 0.0360 . . H336 H Uiso 0.43537 0.44563 0.36265 1.000 0.0280 . . 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 Cl1 0.0304(3) 0.0404(4) 0.0313(3) -0.0117(3) -0.0013(3) 0.0044(3) O1 0.0572(14) 0.0458(13) 0.0438(12) -0.0245(10) -0.0159(10) 0.0168(11) O2 0.0494(15) 0.0526(15) 0.091(2) -0.0391(14) -0.0158(14) 0.0211(12) O3 0.0701(18) 0.095(2) 0.0254(11) -0.0101(13) -0.0019(11) 0.0029(16) O4 0.0414(15) 0.083(2) 0.081(2) 0.0235(17) 0.0021(14) -0.0095(14) Cu1 0.0183(1) 0.0160(1) 0.0155(1) -0.0009(1) 0.0004(1) -0.0014(1) P1 0.0198(3) 0.0166(2) 0.0154(2) -0.0014(2) 0.0007(2) -0.0017(2) P2 0.0207(3) 0.0166(2) 0.0149(2) 0.0001(2) 0.0009(2) -0.0009(2) P3 0.0177(3) 0.0148(2) 0.0200(3) 0.0007(2) 0.0005(2) -0.0015(2) N1 0.0243(10) 0.0219(9) 0.0227(9) 0.0000(8) 0.0013(8) -0.0012(8) C1 0.0242(11) 0.0247(11) 0.0198(10) -0.0022(9) -0.0003(8) 0.0015(9) C11 0.0242(13) 0.0554(18) 0.0414(16) -0.0102(14) 0.0070(11) -0.0121(13) C111 0.0215(10) 0.0181(9) 0.0162(9) 0.0012(8) -0.0006(8) -0.0020(8) C112 0.0256(11) 0.0223(10) 0.0213(10) -0.0034(8) 0.0020(9) -0.0010(9) C113 0.0263(12) 0.0317(13) 0.0254(12) 0.0004(10) 0.0061(9) -0.0033(10) C114 0.0328(13) 0.0235(12) 0.0357(14) 0.0056(10) 0.0085(11) -0.0062(10) C115 0.0398(15) 0.0186(11) 0.0404(15) -0.0021(10) 0.0077(12) -0.0023(10) C116 0.0279(12) 0.0216(11) 0.0314(13) -0.0016(10) 0.0067(10) -0.0011(9) C121 0.0211(10) 0.0221(10) 0.0157(9) -0.0009(8) 0.0010(8) 0.0010(8) C122 0.0289(12) 0.0212(11) 0.0211(10) -0.0009(8) 0.0052(9) 0.0005(9) C123 0.0399(15) 0.0272(12) 0.0264(12) 0.0067(10) 0.0057(11) 0.0068(11) C124 0.0326(14) 0.0564(18) 0.0217(12) 0.0080(12) -0.0051(10) 0.0070(13) C125 0.0329(14) 0.0506(17) 0.0187(11) -0.0020(11) -0.0047(10) -0.0093(12) C126 0.0298(12) 0.0313(12) 0.0191(10) -0.0006(9) -0.0021(9) -0.0063(10) C131 0.0204(10) 0.0175(9) 0.0192(10) -0.0020(8) 0.0032(8) -0.0012(8) C132 0.0243(11) 0.0290(12) 0.0210(10) -0.0037(9) -0.0004(9) -0.0022(9) C133 0.0224(11) 0.0379(14) 0.0287(12) -0.0030(11) -0.0034(9) 0.0000(10) C134 0.0261(12) 0.0329(13) 0.0300(12) 0.0008(10) 0.0062(10) 0.0043(10) C135 0.0342(13) 0.0283(12) 0.0224(11) -0.0024(9) 0.0058(10) 0.0037(10) C136 0.0258(11) 0.0243(11) 0.0192(10) -0.0030(8) -0.0003(8) 0.0029(9) C211 0.0209(10) 0.0182(9) 0.0178(9) -0.0020(8) -0.0009(8) 0.0008(8) C212 0.0227(11) 0.0207(10) 0.0194(10) -0.0010(8) 0.0006(8) -0.0014(8) C213 0.0265(12) 0.0204(10) 0.0254(11) 0.0002(9) -0.0010(9) -0.0050(9) C214 0.0359(14) 0.0242(11) 0.0245(11) -0.0050(9) -0.0071(10) 0.0013(10) C215 0.0517(17) 0.0268(12) 0.0175(11) -0.0017(9) -0.0037(11) -0.0024(12) C216 0.0419(15) 0.0221(11) 0.0197(10) 0.0014(9) -0.0010(10) -0.0043(10) C221 0.0286(12) 0.0275(11) 0.0167(10) -0.0001(9) 0.0009(9) 0.0038(9) C222 0.0439(15) 0.0219(11) 0.0263(12) -0.0004(9) 0.0059(11) 0.0048(11) C223 0.073(2) 0.0302(14) 0.0356(16) 0.0001(12) 0.0036(15) 0.0195(15) C224 0.076(3) 0.055(2) 0.058(2) -0.0130(18) -0.015(2) 0.044(2) C225 0.044(2) 0.077(3) 0.078(3) -0.033(2) -0.0242(19) 0.034(2) C226 0.0307(14) 0.0448(17) 0.0505(18) -0.0178(14) -0.0111(13) 0.0120(13) C231 0.0246(11) 0.0172(9) 0.0168(9) -0.0019(8) 0.0022(8) -0.0032(8) C232 0.0279(12) 0.0235(11) 0.0211(10) -0.0046(9) 0.0021(9) -0.0030(9) C233 0.0247(12) 0.0350(13) 0.0269(12) -0.0065(10) 0.0043(10) -0.0050(10) C234 0.0312(14) 0.0400(15) 0.0271(12) -0.0046(11) 0.0088(10) -0.0123(11) C235 0.0468(16) 0.0332(13) 0.0215(11) 0.0040(10) 0.0057(11) -0.0127(12) C236 0.0330(13) 0.0250(12) 0.0222(11) 0.0013(9) 0.0001(9) -0.0038(10) C311 0.0190(10) 0.0200(10) 0.0241(11) 0.0056(8) 0.0008(8) -0.0016(8) C312 0.0238(11) 0.0269(12) 0.0268(11) 0.0015(9) -0.0010(9) -0.0032(9) C313 0.0296(13) 0.0360(14) 0.0365(14) 0.0034(11) -0.0059(11) -0.0116(11) C314 0.0200(12) 0.0455(17) 0.0487(17) 0.0144(14) -0.0034(11) -0.0084(11) C315 0.0216(12) 0.0371(15) 0.0563(19) 0.0057(13) 0.0061(12) 0.0032(11) C316 0.0235(12) 0.0246(12) 0.0445(15) 0.0005(11) 0.0033(11) -0.0002(10) C321 0.0227(11) 0.0152(9) 0.0220(10) 0.0000(8) 0.0000(8) -0.0018(8) C322 0.0251(11) 0.0212(11) 0.0303(12) 0.0031(9) 0.0015(9) -0.0020(9) C323 0.0326(13) 0.0270(12) 0.0299(12) 0.0054(10) 0.0088(10) -0.0036(10) C324 0.0486(16) 0.0283(13) 0.0244(12) 0.0081(10) 0.0036(11) -0.0033(12) C325 0.0406(15) 0.0300(13) 0.0225(11) 0.0040(10) -0.0064(10) -0.0007(11) C326 0.0282(12) 0.0214(10) 0.0211(10) 0.0015(8) -0.0035(9) -0.0030(9) C331 0.0213(10) 0.0173(9) 0.0218(10) -0.0009(8) -0.0006(8) 0.0009(8) C332 0.0314(13) 0.0246(11) 0.0266(12) -0.0037(9) 0.0071(10) -0.0078(10) C333 0.0389(15) 0.0335(13) 0.0262(12) -0.0089(10) 0.0084(11) -0.0043(11) C334 0.0362(14) 0.0269(12) 0.0328(13) -0.0086(11) 0.0014(11) -0.0019(11) C335 0.0349(14) 0.0204(11) 0.0325(13) -0.0020(10) -0.0016(11) -0.0048(10) C336 0.0271(12) 0.0204(10) 0.0245(11) 0.0013(9) -0.0007(9) -0.0013(9) #=============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.055(2) . . yes Cu1 P1 2.3126(7) . . yes Cu1 P2 2.3131(6) . . yes Cu1 P3 2.3204(6) . . yes Cl1 O2 1.424(3) . . yes Cl1 O3 1.433(2) . . yes Cl1 O4 1.423(3) . . yes Cl1 O1 1.430(2) . . yes P1 C111 1.826(2) . . yes P1 C121 1.828(2) . . yes P1 C131 1.823(2) . . yes P2 C211 1.829(2) . . yes P2 C221 1.828(3) . . yes P2 C231 1.825(2) . . yes P3 C311 1.828(2) . . yes P3 C321 1.831(2) . . yes P3 C331 1.827(2) . . yes N1 C1 1.130(3) . . yes C1 C11 1.460(4) . . no C111 C112 1.395(3) . . no C111 C116 1.392(3) . . no C11 H11B 0.9563 . . no C11 H11C 0.9470 . . no C11 H11A 0.9536 . . no C112 C113 1.383(3) . . no C113 C114 1.383(4) . . no C114 C115 1.396(4) . . no C115 C116 1.383(4) . . no C121 C122 1.395(3) . . no C121 C126 1.393(3) . . no C122 C123 1.389(4) . . no C123 C124 1.387(4) . . no C124 C125 1.379(4) . . no C125 C126 1.383(4) . . no C131 C132 1.396(3) . . no C131 C136 1.400(3) . . no C132 C133 1.381(4) . . no C133 C134 1.385(4) . . no C134 C135 1.386(4) . . no C135 C136 1.392(4) . . no C211 C216 1.391(3) . . no C211 C212 1.395(3) . . no C212 C213 1.386(3) . . no C112 H112 0.9532 . . no C213 C214 1.385(4) . . no C113 H113 0.9494 . . no C214 C215 1.383(4) . . no C114 H114 0.9556 . . no C115 H115 0.9605 . . no C215 C216 1.383(4) . . no C116 H116 0.9650 . . no C221 C226 1.387(4) . . no C221 C222 1.400(4) . . no C122 H122 0.9649 . . no C222 C223 1.377(4) . . no C223 C224 1.383(5) . . no C123 H123 0.9542 . . no C224 C225 1.366(6) . . no C124 H124 0.9633 . . no C225 C226 1.386(5) . . no C125 H125 0.9566 . . no C126 H126 0.9678 . . no C231 C232 1.394(3) . . no C231 C236 1.402(3) . . no C232 C233 1.389(4) . . no C132 H132 0.9540 . . no C133 H133 0.9674 . . no C233 C234 1.388(4) . . no C134 H134 0.9562 . . no C234 C235 1.382(4) . . no C235 C236 1.390(4) . . no C135 H135 0.9561 . . no C136 H136 0.9616 . . no C311 C316 1.398(4) . . no C311 C312 1.391(3) . . no C212 H212 0.9553 . . no C312 C313 1.392(4) . . no C213 H213 0.9616 . . no C313 C314 1.385(4) . . no C214 H214 0.9583 . . no C314 C315 1.382(4) . . no C215 H215 0.9562 . . no C315 C316 1.384(4) . . no C216 H216 0.9644 . . no C321 C326 1.392(3) . . no C321 C322 1.392(3) . . no C222 H222 0.9543 . . no C322 C323 1.390(4) . . no C223 H223 0.9565 . . no C323 C324 1.385(4) . . no C324 C325 1.375(4) . . no C224 H224 0.9594 . . no C325 C326 1.391(3) . . no C225 H225 0.9711 . . no C226 H226 0.9575 . . no C331 C336 1.394(3) . . no C331 C332 1.403(3) . . no C332 C333 1.387(4) . . no C232 H232 0.9589 . . no C333 C334 1.382(4) . . no C233 H233 0.9582 . . no C234 H234 0.9594 . . no C334 C335 1.385(4) . . no C335 C336 1.393(4) . . no C235 H235 0.9583 . . no C236 H236 0.9636 . . no C312 H312 0.9535 . . no C313 H313 0.9502 . . no C314 H314 0.9483 . . no C315 H315 0.9674 . . no C316 H316 0.9615 . . no C322 H322 0.9644 . . no C323 H323 0.9567 . . no C324 H324 0.9589 . . no C325 H325 0.9585 . . no C326 H326 0.9597 . . no C332 H332 0.9525 . . no C333 H333 0.9517 . . no C334 H334 0.9499 . . no C335 H335 0.9486 . . no C336 H336 0.9578 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Cu1 P3 119.42(2) . . . yes P1 Cu1 N1 100.80(6) . . . yes P2 Cu1 P3 112.96(2) . . . yes P2 Cu1 N1 101.42(6) . . . yes P3 Cu1 N1 105.74(6) . . . yes P1 Cu1 P2 113.55(2) . . . yes O3 Cl1 O4 109.28(17) . . . yes O1 Cl1 O2 109.12(15) . . . yes O1 Cl1 O3 108.93(16) . . . yes O1 Cl1 O4 109.12(17) . . . yes O2 Cl1 O3 110.56(17) . . . yes O2 Cl1 O4 109.80(17) . . . yes Cu1 P1 C111 113.59(7) . . . yes Cu1 P1 C121 115.30(8) . . . yes Cu1 P1 C131 115.06(8) . . . yes C111 P1 C121 104.41(10) . . . yes C111 P1 C131 104.47(11) . . . yes C121 P1 C131 102.65(10) . . . yes Cu1 P2 C211 113.31(7) . . . yes Cu1 P2 C221 113.64(7) . . . yes Cu1 P2 C231 118.53(7) . . . yes C211 P2 C221 103.23(10) . . . yes C211 P2 C231 103.66(10) . . . yes C221 P2 C231 102.73(11) . . . yes Cu1 P3 C311 114.59(7) . . . yes Cu1 P3 C321 115.29(8) . . . yes Cu1 P3 C331 115.46(7) . . . yes C311 P3 C321 102.84(10) . . . yes C311 P3 C331 104.55(10) . . . yes C321 P3 C331 102.46(10) . . . yes Cu1 N1 C1 178.0(2) . . . yes N1 C1 C11 178.4(3) . . . yes P1 C111 C112 117.26(17) . . . yes P1 C111 C116 123.78(18) . . . yes C112 C111 C116 119.0(2) . . . no C1 C11 H11B 110.62 . . . no C1 C11 H11C 110.07 . . . no H11A C11 H11B 108.46 . . . no H11A C11 H11C 108.17 . . . no H11B C11 H11C 108.76 . . . no C1 C11 H11A 110.69 . . . no C111 C112 C113 121.2(2) . . . no C112 C113 C114 119.8(2) . . . no C113 C114 C115 119.4(2) . . . no C114 C115 C116 121.0(2) . . . no C111 C116 C115 119.7(2) . . . no P1 C121 C122 116.77(17) . . . yes P1 C121 C126 124.43(18) . . . yes C122 C121 C126 118.8(2) . . . no C121 C122 C123 120.9(2) . . . no C122 C123 C124 119.4(2) . . . no C123 C124 C125 120.1(3) . . . no C124 C125 C126 120.5(3) . . . no C121 C126 C125 120.3(2) . . . no C132 C131 C136 118.5(2) . . . no P1 C131 C136 122.80(18) . . . yes P1 C131 C132 118.66(17) . . . yes C131 C132 C133 120.7(2) . . . no C132 C133 C134 120.8(2) . . . no C133 C134 C135 119.2(2) . . . no C134 C135 C136 120.6(2) . . . no C131 C136 C135 120.2(2) . . . no P2 C211 C216 121.98(17) . . . yes P2 C211 C212 119.21(16) . . . yes C212 C211 C216 118.8(2) . . . no C111 C112 H112 119.36 . . . no C113 C112 H112 119.41 . . . no C211 C212 C213 120.2(2) . . . no C212 C213 C214 120.2(2) . . . no C112 C113 H113 120.03 . . . no C114 C113 H113 120.22 . . . no C115 C114 H114 120.86 . . . no C113 C114 H114 119.77 . . . no C213 C214 C215 120.1(2) . . . no C116 C115 H115 119.56 . . . no C114 C115 H115 119.46 . . . no C214 C215 C216 119.7(2) . . . no C111 C116 H116 119.56 . . . no C211 C216 C215 121.0(2) . . . no C115 C116 H116 120.72 . . . no P2 C221 C222 120.3(2) . . . yes P2 C221 C226 121.0(2) . . . yes C222 C221 C226 118.3(3) . . . no C123 C122 H122 119.43 . . . no C221 C222 C223 120.7(3) . . . no C121 C122 H122 119.71 . . . no C122 C123 H123 120.69 . . . no C222 C223 C224 119.7(3) . . . no C124 C123 H123 119.88 . . . no C123 C124 H124 119.85 . . . no C125 C124 H124 120.04 . . . no C223 C224 C225 120.5(3) . . . no C224 C225 C226 120.0(3) . . . no C126 C125 H125 119.95 . . . no C124 C125 H125 119.50 . . . no C121 C126 H126 119.96 . . . no C221 C226 C225 120.7(3) . . . no C125 C126 H126 119.75 . . . no P2 C231 C232 118.00(17) . . . yes C232 C231 C236 118.3(2) . . . no P2 C231 C236 123.71(18) . . . yes C133 C132 H132 120.35 . . . no C131 C132 H132 118.91 . . . no C231 C232 C233 121.1(2) . . . no C132 C133 H133 119.71 . . . no C134 C133 H133 119.54 . . . no C232 C233 C234 120.0(2) . . . no C133 C134 H134 121.11 . . . no C233 C234 C235 119.7(3) . . . no C135 C134 H134 119.67 . . . no C234 C235 C236 120.5(3) . . . no C134 C135 H135 119.79 . . . no C136 C135 H135 119.59 . . . no C231 C236 C235 120.4(2) . . . no C135 C136 H136 119.89 . . . no C131 C136 H136 119.92 . . . no P3 C311 C316 123.33(18) . . . yes P3 C311 C312 118.20(17) . . . yes C312 C311 C316 118.3(2) . . . no C211 C212 H212 120.12 . . . no C213 C212 H212 119.63 . . . no C311 C312 C313 121.0(2) . . . no C312 C313 C314 119.9(3) . . . no C212 C213 H213 119.67 . . . no C214 C213 H213 120.15 . . . no C313 C314 C315 119.5(3) . . . no C213 C214 H214 119.62 . . . no C215 C214 H214 120.27 . . . no C216 C215 H215 120.29 . . . no C314 C315 C316 120.7(3) . . . no C214 C215 H215 120.02 . . . no C215 C216 H216 119.86 . . . no C311 C316 C315 120.5(3) . . . no C211 C216 H216 119.14 . . . no P3 C321 C322 118.35(18) . . . yes P3 C321 C326 123.05(18) . . . yes C322 C321 C326 118.6(2) . . . no C321 C322 C323 120.8(2) . . . no C223 C222 H222 120.30 . . . no C221 C222 H222 118.99 . . . no C224 C223 H223 120.20 . . . no C322 C323 C324 119.7(2) . . . no C222 C223 H223 120.07 . . . no C225 C224 H224 119.77 . . . no C223 C224 H224 119.69 . . . no C323 C324 C325 120.3(2) . . . no C224 C225 H225 120.20 . . . no C226 C225 H225 119.62 . . . no C324 C325 C326 120.0(2) . . . no C225 C226 H226 120.53 . . . no C221 C226 H226 118.74 . . . no C321 C326 C325 120.7(2) . . . no P3 C331 C332 120.18(17) . . . yes C332 C331 C336 118.3(2) . . . no P3 C331 C336 121.29(17) . . . yes C233 C232 H232 119.34 . . . no C331 C332 C333 120.8(2) . . . no C231 C232 H232 119.57 . . . no C232 C233 H233 120.20 . . . no C234 C233 H233 119.83 . . . no C332 C333 C334 120.2(2) . . . no C233 C234 H234 119.53 . . . no C235 C234 H234 120.75 . . . no C333 C334 C335 119.7(2) . . . no C234 C235 H235 119.70 . . . no C334 C335 C336 120.5(2) . . . no C236 C235 H235 119.78 . . . no C331 C336 C335 120.5(2) . . . no C231 C236 H236 119.27 . . . no C235 C236 H236 120.29 . . . no C311 C312 H312 119.33 . . . no C313 C312 H312 119.68 . . . no C312 C313 H313 120.32 . . . no C314 C313 H313 119.72 . . . no C313 C314 H314 120.28 . . . no C315 C314 H314 120.23 . . . no C314 C315 H315 118.98 . . . no C316 C315 H315 120.27 . . . no C311 C316 H316 118.90 . . . no C315 C316 H316 120.63 . . . no C321 C322 H322 119.46 . . . no C323 C322 H322 119.78 . . . no C322 C323 H323 120.48 . . . no C324 C323 H323 119.81 . . . no C323 C324 H324 118.98 . . . no C325 C324 H324 120.72 . . . no C324 C325 H325 119.61 . . . no C326 C325 H325 120.41 . . . no C321 C326 H326 119.53 . . . no C325 C326 H326 119.80 . . . no C331 C332 H332 119.48 . . . no C333 C332 H332 119.69 . . . no C332 C333 H333 119.93 . . . no C334 C333 H333 119.82 . . . no C333 C334 H334 120.48 . . . no C335 C334 H334 119.86 . . . no C334 C335 H335 119.85 . . . no C336 C335 H335 119.68 . . . no C331 C336 H336 119.80 . . . no C335 C336 H336 119.71 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Cu1 P1 C111 39.13(9) . . . . no P2 Cu1 P1 C121 159.57(8) . . . . no P2 Cu1 P1 C131 -81.20(8) . . . . no P3 Cu1 P1 C111 -98.11(8) . . . . no P3 Cu1 P1 C121 22.33(8) . . . . no P3 Cu1 P1 C131 141.56(8) . . . . no N1 Cu1 P1 C111 146.77(10) . . . . no N1 Cu1 P1 C121 -92.80(10) . . . . no N1 Cu1 P1 C131 26.43(10) . . . . no P1 Cu1 P2 C211 162.67(8) . . . . no P1 Cu1 P2 C221 45.25(9) . . . . no P1 Cu1 P2 C231 -75.53(9) . . . . no P3 Cu1 P2 C211 -57.29(8) . . . . no P3 Cu1 P2 C221 -174.71(9) . . . . no P3 Cu1 P2 C231 64.50(9) . . . . no N1 Cu1 P2 C211 55.42(10) . . . . no N1 Cu1 P2 C221 -62.00(11) . . . . no N1 Cu1 P2 C231 177.22(10) . . . . no P1 Cu1 P3 C311 52.74(8) . . . . no P1 Cu1 P3 C321 -66.38(8) . . . . no P1 Cu1 P3 C331 174.33(8) . . . . no P2 Cu1 P3 C311 -84.73(8) . . . . no P2 Cu1 P3 C321 156.15(8) . . . . no P2 Cu1 P3 C331 36.86(9) . . . . no N1 Cu1 P3 C311 165.22(10) . . . . no N1 Cu1 P3 C321 46.11(10) . . . . no N1 Cu1 P3 C331 -73.18(10) . . . . no Cu1 P1 C111 C112 28.5(2) . . . . no C121 P1 C111 C112 -97.88(19) . . . . no C131 P1 C111 C112 154.68(18) . . . . no Cu1 P1 C111 C116 -151.06(18) . . . . no C121 P1 C111 C116 82.5(2) . . . . no C131 P1 C111 C116 -24.9(2) . . . . no Cu1 P1 C131 C132 32.7(2) . . . . no Cu1 P1 C121 C122 31.8(2) . . . . no C111 P1 C121 C122 157.11(18) . . . . no C131 P1 C121 C122 -94.10(19) . . . . no Cu1 P1 C121 C126 -150.49(18) . . . . no C111 P1 C121 C126 -25.2(2) . . . . no C131 P1 C121 C126 83.6(2) . . . . no C121 P1 C131 C132 158.70(19) . . . . no Cu1 P1 C131 C136 -148.82(17) . . . . no C111 P1 C131 C132 -92.6(2) . . . . no C121 P1 C131 C136 -22.8(2) . . . . no C111 P1 C131 C136 86.0(2) . . . . no Cu1 P2 C231 C232 -28.2(2) . . . . no C231 P2 C221 C222 50.8(2) . . . . no C221 P2 C231 C232 -154.42(19) . . . . no C231 P2 C211 C212 -140.37(19) . . . . no C211 P2 C231 C232 98.34(19) . . . . no C221 P2 C231 C236 24.6(2) . . . . no Cu1 P2 C231 C236 150.82(17) . . . . no C211 P2 C231 C236 -82.6(2) . . . . no C221 P2 C211 C212 112.76(19) . . . . no Cu1 P2 C221 C226 94.9(2) . . . . no Cu1 P2 C211 C212 -10.6(2) . . . . no Cu1 P2 C221 C222 -78.5(2) . . . . no C211 P2 C221 C222 158.4(2) . . . . no Cu1 P2 C211 C216 167.21(18) . . . . no C231 P2 C221 C226 -135.8(2) . . . . no C221 P2 C211 C216 -69.4(2) . . . . no C231 P2 C211 C216 37.4(2) . . . . no C211 P2 C221 C226 -28.3(2) . . . . no C331 P3 C321 C322 83.1(2) . . . . no C321 P3 C331 C332 162.2(2) . . . . no Cu1 P3 C311 C312 -39.8(2) . . . . no C321 P3 C311 C312 86.1(2) . . . . no Cu1 P3 C331 C332 -71.6(2) . . . . no Cu1 P3 C311 C316 144.25(19) . . . . no Cu1 P3 C321 C322 -43.2(2) . . . . no C331 P3 C311 C312 -167.21(18) . . . . no C321 P3 C311 C316 -89.9(2) . . . . no Cu1 P3 C321 C326 137.32(18) . . . . no C311 P3 C321 C322 -168.63(19) . . . . no Cu1 P3 C331 C336 103.07(19) . . . . no C331 P3 C321 C326 -96.4(2) . . . . no C321 P3 C331 C336 -23.1(2) . . . . no C311 P3 C331 C332 55.2(2) . . . . no C331 P3 C311 C316 16.9(2) . . . . no C311 P3 C321 C326 11.9(2) . . . . no C311 P3 C331 C336 -130.1(2) . . . . no P2 C211 C212 C213 178.11(18) . . . . no C212 C211 C216 C215 1.1(4) . . . . no P1 C111 C112 H112 0.00 . . . . no C116 C111 C112 H112 179.60 . . . . no P1 C111 C116 H116 0.31 . . . . no C112 C111 C116 H116 -179.26 . . . . no P2 C211 C216 C215 -176.7(2) . . . . no C216 C211 C212 C213 0.2(3) . . . . no H112 C112 C113 C114 -179.73 . . . . no C111 C112 C113 H113 179.66 . . . . no H112 C112 C113 H113 0.86 . . . . no C211 C212 C213 C214 -1.0(4) . . . . no H113 C113 C114 H114 -0.95 . . . . no H113 C113 C114 C115 179.77 . . . . no C112 C113 C114 H114 179.64 . . . . no C212 C213 C214 C215 0.4(4) . . . . no H114 C114 C115 H115 1.61 . . . . no H114 C114 C115 C116 -178.94 . . . . no C213 C214 C215 C216 0.9(4) . . . . no C113 C114 C115 H115 -179.11 . . . . no H115 C115 C116 H116 -1.86 . . . . no C114 C115 C116 H116 178.70 . . . . no C214 C215 C216 C211 -1.6(4) . . . . no H115 C115 C116 C111 178.99 . . . . no P1 C121 C122 H122 -1.39 . . . . no C122 C121 C126 H126 -178.63 . . . . no C126 C121 C122 H122 -179.25 . . . . no P2 C221 C222 C223 175.7(2) . . . . no C226 C221 C222 C223 2.2(4) . . . . no P2 C221 C226 C225 -174.8(3) . . . . no C222 C221 C226 C225 -1.4(5) . . . . no P1 C121 C126 H126 3.68 . . . . no H122 C122 C123 H123 -1.90 . . . . no C221 C222 C223 C224 -2.3(5) . . . . no C121 C122 C123 H123 178.31 . . . . no H122 C122 C123 C124 178.87 . . . . no H123 C123 C124 C125 -178.85 . . . . no C122 C123 C124 H124 -178.76 . . . . no C222 C223 C224 C225 1.7(6) . . . . no H123 C123 C124 H124 2.00 . . . . no H124 C124 C125 H125 0.42 . . . . no C123 C124 C125 H125 -178.74 . . . . no C223 C224 C225 C226 -0.9(6) . . . . no H124 C124 C125 C126 179.67 . . . . no H125 C125 C126 H126 -2.65 . . . . no H125 C125 C126 C121 178.35 . . . . no C124 C125 C126 H126 178.10 . . . . no C224 C225 C226 C221 0.7(6) . . . . no P2 C231 C232 C233 179.12(19) . . . . no C236 C231 C232 C233 0.0(4) . . . . no C232 C231 C236 C235 0.9(4) . . . . no C132 C131 C136 H136 -179.79 . . . . no P2 C231 C236 C235 -178.1(2) . . . . no P1 C131 C136 H136 1.68 . . . . no C136 C131 C132 H132 -177.88 . . . . no P1 C131 C132 H132 0.71 . . . . no H132 C132 C133 C134 178.47 . . . . no C231 C232 C233 C234 -1.1(4) . . . . no C131 C132 C133 H133 -179.81 . . . . no H132 C132 C133 H133 -1.62 . . . . no C132 C133 C134 H134 178.10 . . . . no C232 C233 C234 C235 1.3(4) . . . . no H133 C133 C134 H134 -1.82 . . . . no H133 C133 C134 C135 179.64 . . . . no C133 C134 C135 H135 -179.61 . . . . no C233 C234 C235 C236 -0.3(4) . . . . no H134 C134 C135 C136 -178.56 . . . . no H134 C134 C135 H135 1.82 . . . . no H135 C135 C136 C131 -179.78 . . . . no C134 C135 C136 H136 179.63 . . . . no H135 C135 C136 H136 -0.75 . . . . no C234 C235 C236 C231 -0.8(4) . . . . no P3 C311 C312 H312 4.66 . . . . no C316 C311 C312 H312 -179.20 . . . . no P3 C311 C316 H316 -5.15 . . . . no C312 C311 C316 H316 178.92 . . . . no C311 C312 C313 H313 -178.40 . . . . no H312 C312 C313 C314 -179.39 . . . . no H312 C312 C313 H313 2.23 . . . . no C312 C313 C314 H314 177.77 . . . . no H313 C313 C314 C315 176.82 . . . . no H313 C313 C314 H314 -3.84 . . . . no C313 C314 C315 H315 -179.34 . . . . no H314 C314 C315 C316 -177.60 . . . . no H314 C314 C315 H315 1.32 . . . . no C314 C315 C316 H316 179.50 . . . . no H315 C315 C316 C311 -179.22 . . . . no H315 C315 C316 H316 0.59 . . . . no P3 C321 C322 H322 -0.84 . . . . no C326 C321 C322 H322 178.67 . . . . no P3 C321 C326 H326 1.80 . . . . no C322 C321 C326 H326 -177.69 . . . . no C321 C322 C323 H323 179.31 . . . . no H322 C322 C323 C324 -179.12 . . . . no H322 C322 C323 H323 0.00 . . . . no C322 C323 C324 H324 -179.64 . . . . no H323 C323 C324 C325 -179.18 . . . . no H323 C323 C324 H324 1.26 . . . . no C323 C324 C325 H325 179.91 . . . . no H324 C324 C325 C326 179.96 . . . . no H324 C324 C325 H325 -0.53 . . . . no C324 C325 C326 H326 177.80 . . . . no H325 C325 C326 C321 179.63 . . . . no H325 C325 C326 H326 -1.70 . . . . no P3 C331 C332 H332 -5.37 . . . . no C336 C331 C332 H332 179.78 . . . . no P3 C331 C336 H336 5.99 . . . . no C332 C331 C336 H336 -179.22 . . . . no C331 C332 C333 H333 179.56 . . . . no H332 C332 C333 C334 -179.12 . . . . no H332 C332 C333 H333 1.48 . . . . no C332 C333 C334 H334 178.75 . . . . no H333 C333 C334 C335 178.49 . . . . no H333 C333 C334 H334 -1.85 . . . . no C333 C334 C335 H335 -176.72 . . . . no H334 C334 C335 C336 -177.49 . . . . no H334 C334 C335 H335 3.61 . . . . no C334 C335 C336 H336 177.29 . . . . no H335 C335 C336 C331 177.41 . . . . no H335 C335 C336 H336 -3.81 . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu1 H132 3.1844 . . no Cu1 H212 2.9674 . . no Cu1 H232 3.2278 . . no Cu1 H312 3.2348 . . no Cu1 H322 3.3433 . . no Cu1 H112 3.0441 . . no Cu1 H122 3.1172 . . no Cl1 H334 3.1472 . 2_564 no P1 H312 3.1044 . . no O1 C234 3.373(4) . 8_554 no O1 C11 3.235(4) . 6_455 no O1 C213 3.336(3) . 6_455 no O1 C1 3.278(3) . 6_455 no O2 C136 3.276(4) . 7_555 no O3 C11 3.293(5) . 6_455 no O3 C115 3.225(4) . 7_555 no O3 C116 3.242(4) . 7_555 no O1 H213 2.6442 . 6_455 no O1 H212 2.8560 . 6_455 no O1 H334 2.9182 . 2_564 no O1 H234 2.4562 . 8_554 no O2 H136 2.5982 . 7_555 no O2 H335 2.8687 . 6_455 no O3 H11B 2.4663 . 6_455 no O3 H115 2.7650 . 7_555 no O3 H116 2.8285 . 7_555 no O3 H325 2.7913 . . no O4 H325 2.6463 . . no N1 C132 3.342(3) . . no N1 C212 3.400(3) . . no N1 C322 3.430(3) . . no N1 H132 2.9135 . . no N1 H212 2.5857 . . no N1 H322 2.6058 . . no C1 O1 3.278(3) . 6_555 no C11 C313 3.443(4) . 6_555 no C11 O3 3.293(5) . 6_555 no C11 O1 3.235(4) . 6_555 no C11 C123 3.546(4) . 6_555 no C11 C124 3.499(4) . 6_555 no C1 H322 2.8047 . . no C1 H212 2.9909 . . no C112 C232 3.336(3) . . no C112 C231 3.536(3) . . no C115 O3 3.225(4) . 7_545 no C116 C136 3.556(3) . . no C116 C126 3.527(4) . . no C116 O3 3.242(4) . 7_545 no C122 C321 3.448(3) . . no C123 C11 3.546(4) . 6_455 no C123 C216 3.433(4) . 8_554 no C123 C215 3.525(4) . 8_554 no C124 C216 3.404(4) . 8_554 no C124 C215 3.519(4) . 8_554 no C124 C11 3.499(4) . 6_455 no C126 C136 3.447(4) . . no C126 C116 3.527(4) . . no C132 N1 3.342(3) . . no C132 C222 3.530(4) . . no C134 C324 3.517(4) . 4_645 no C134 C325 3.383(4) . 4_645 no C136 C116 3.556(3) . . no C136 C126 3.447(4) . . no C136 O2 3.276(4) . 7_545 no C111 H222 3.0827 . . no C111 H126 2.7750 . . no C211 C332 3.555(3) . . no C212 C331 3.356(3) . . no C112 H222 3.0771 . . no C112 H312 3.0798 . . no C212 N1 3.400(3) . . no C212 C332 3.321(4) . . no C213 C233 3.523(4) . 3_556 no C213 O1 3.336(3) . 6_555 no C213 C334 3.478(4) . . no C213 C234 3.512(4) . 3_556 no C213 C333 3.563(4) . . no C114 H134 2.9967 . 6_455 no C114 H316 3.0472 . 7_545 no C115 H134 3.0777 . 6_455 no C215 C124 3.519(4) . 8_555 no C215 C123 3.525(4) . 8_555 no C215 C314 3.419(4) . 3_556 no C216 C226 3.550(4) . . no C216 C123 3.433(4) . 8_555 no C216 C236 3.472(4) . . no C216 C124 3.404(4) . 8_555 no C116 H126 2.8099 . . no C121 H136 2.6555 . . no C121 H312 2.7925 . . no C222 C132 3.530(4) . . no C122 H215 3.0993 . 8_554 no C122 H314 3.0184 . 6_555 no C122 H312 3.0584 . . no C222 C236 3.219(4) . . no C123 H215 3.0551 . 8_554 no C123 H216 2.8721 . 8_554 no C123 H11C 2.9946 . 6_455 no C124 H11C 2.9985 . 6_455 no C124 H216 3.0965 . 8_554 no C125 H333 3.0925 . 8_554 no C125 H133 2.8737 . 6_455 no C226 C216 3.550(4) . . no C126 H136 2.7081 . . no C231 C112 3.536(3) . . no C131 H116 2.7559 . . no C232 C112 3.336(3) . . no C233 C213 3.523(4) . 3_456 no C234 C213 3.512(4) . 3_456 no C234 O1 3.373(4) . 8_555 no C236 C222 3.219(4) . . no C136 H116 2.8352 . . no C236 C216 3.472(4) . . no C211 H226 2.6284 . . no C213 H335 3.0614 . 5_666 no C313 C11 3.443(4) . 6_455 no C213 H233 2.9424 . 3_556 no C213 H234 2.9052 . 3_556 no C214 H335 2.8750 . 5_666 no C314 C215 3.419(4) . 3_456 no C215 H314 3.0811 . 3_556 no C216 H226 3.0798 . . no C316 C332 3.259(4) . . no C316 C326 3.579(4) . . no C321 C122 3.448(3) . . no C221 H236 2.7073 . . no C221 H132 2.7406 . . no C222 H236 2.7887 . . no C322 C336 3.332(4) . . no C322 N1 3.430(3) . . no C222 H132 2.8340 . . no C324 C134 3.517(4) . 4_655 no C325 C134 3.383(4) . 4_655 no C326 C316 3.579(4) . . no C226 H132 3.0098 . . no C231 H222 2.9241 . . no C331 C212 3.356(3) . . no C231 H112 3.0394 . . no C231 H216 2.8372 . . no C332 C212 3.321(4) . . no C332 C211 3.555(3) . . no C232 H112 2.6247 . . no C332 C316 3.259(4) . . no C232 H332 2.8451 . . no C333 C213 3.563(4) . . no C234 H11A 2.8095 . 3_456 no C334 C213 3.478(4) . . no C236 H222 2.9427 . . no C236 H216 2.7546 . . no C336 C322 3.332(4) . . no C311 H326 2.5992 . . no C311 H332 3.0430 . . no C311 H232 2.8944 . . no C312 H112 2.9260 . . no C312 H11C 2.9453 . 6_455 no C313 H11C 2.8976 . 6_455 no C314 H215 2.9025 . 3_456 no C315 H115 3.0291 . 7_555 no C316 H332 2.9943 . . no C316 H326 2.8736 . . no C316 H115 2.9806 . 7_555 no C321 H336 2.5896 . . no C321 H122 2.7704 . . no C322 H122 2.7375 . . no C322 H336 2.5972 . . no C326 H11B 3.0649 . 6_455 no C331 H316 2.6659 . . no C331 H212 2.9891 . . no C332 H225 2.9486 . 3_456 no C332 H316 2.6858 . . no C333 H225 2.8388 . 3_456 no C334 H213 3.0814 . 5_666 no C335 H214 3.0318 . 5_666 no H11A C234 2.8095 . 3_556 no H11A H234 2.5048 . 3_556 no H11B O3 2.4663 . 6_555 no H11B C326 3.0649 . 6_555 no H11B H326 2.4774 . 6_555 no H11C C123 2.9946 . 6_555 no H11C C124 2.9985 . 6_555 no H11C C312 2.9453 . 6_555 no H11C C313 2.8976 . 6_555 no H112 Cu1 3.0441 . . no H112 C231 3.0394 . . no H112 C232 2.6247 . . no H112 C312 2.9260 . . no H112 H232 2.4237 . . no H112 H312 2.5088 . . no H114 H316 2.3590 . 7_545 no H115 O3 2.7650 . 7_545 no H115 C315 3.0291 . 7_545 no H115 C316 2.9806 . 7_545 no H116 C131 2.7559 . . no H116 C136 2.8352 . . no H116 H323 2.5976 . 4_645 no H116 O3 2.8285 . 7_545 no H122 Cu1 3.1172 . . no H122 C321 2.7704 . . no H122 C322 2.7375 . . no H125 H133 2.3852 . 6_455 no H125 H333 2.4450 . 8_554 no H126 C111 2.7750 . . no H126 C116 2.8099 . . no H132 Cu1 3.1844 . . no H132 N1 2.9135 . . no H132 C221 2.7406 . . no H132 C222 2.8340 . . no H132 C226 3.0098 . . no H133 C125 2.8737 . 6_555 no H133 H125 2.3852 . 6_555 no H134 C114 2.9967 . 6_555 no H134 C115 3.0777 . 6_555 no H135 H214 2.4881 . 8_554 no H136 C121 2.6555 . . no H136 C126 2.7081 . . no H136 O2 2.5982 . 7_545 no H212 Cu1 2.9674 . . no H212 N1 2.5857 . . no H212 C1 2.9909 . . no H212 C331 2.9891 . . no H212 O1 2.8560 . 6_555 no H213 H234 2.5021 . 3_556 no H213 C334 3.0814 . 5_666 no H213 H334 2.4437 . 5_666 no H213 O1 2.6442 . 6_555 no H214 C335 3.0318 . 5_666 no H214 H335 2.2636 . 5_666 no H214 H135 2.4881 . 8_555 no H215 C314 2.9025 . 3_556 no H215 H314 2.4232 . 3_556 no H215 C122 3.0993 . 8_555 no H215 C123 3.0551 . 8_555 no H216 C231 2.8372 . . no H216 C236 2.7546 . . no H216 H236 2.5306 . . no H216 C123 2.8721 . 8_555 no H216 C124 3.0965 . 8_555 no H222 C111 3.0827 . . no H222 C112 3.0771 . . no H222 C231 2.9241 . . no H222 C236 2.9427 . . no H225 C332 2.9486 . 3_556 no H225 C333 2.8388 . 3_556 no H225 H333 2.4432 . 3_556 no H226 C211 2.6284 . . no H226 C216 3.0798 . . no H232 Cu1 3.2278 . . no H232 C311 2.8944 . . no H232 H112 2.4237 . . no H232 H332 2.2755 . . no H233 C213 2.9424 . 3_456 no H234 C213 2.9052 . 3_456 no H234 H11A 2.5048 . 3_456 no H234 H213 2.5021 . 3_456 no H234 O1 2.4562 . 8_555 no H236 C221 2.7073 . . no H236 C222 2.7887 . . no H236 H216 2.5306 . . no H312 Cu1 3.2348 . . no H312 P1 3.1044 . . no H312 C112 3.0798 . . no H312 C121 2.7925 . . no H312 C122 3.0584 . . no H312 H112 2.5088 . . no H314 C215 3.0811 . 3_456 no H314 H215 2.4232 . 3_456 no H314 C122 3.0184 . 6_455 no H316 C331 2.6659 . . no H316 C332 2.6858 . . no H316 C114 3.0472 . 7_555 no H316 H114 2.3590 . 7_555 no H322 Cu1 3.3433 . . no H322 N1 2.6058 . . no H322 C1 2.8047 . . no H323 H116 2.5976 . 4_655 no H325 O3 2.7913 . . no H325 O4 2.6463 . . no H326 C311 2.5992 . . no H326 C316 2.8736 . . no H326 H11B 2.4774 . 6_455 no H332 C232 2.8451 . . no H332 C311 3.0430 . . no H332 C316 2.9943 . . no H332 H232 2.2755 . . no H333 H225 2.4432 . 3_456 no H333 C125 3.0925 . 8_555 no H333 H125 2.4450 . 8_555 no H334 Cl1 3.1472 . 2_565 no H334 O1 2.9182 . 2_565 no H334 H213 2.4437 . 5_666 no H335 C213 3.0614 . 5_666 no H335 C214 2.8750 . 5_666 no H335 H214 2.2636 . 5_666 no H335 O2 2.8687 . 6_555 no H336 C321 2.5896 . . no H336 C322 2.5972 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C11 H11B O3 0.9563 2.4663 3.293(5) 144.60 6_555 yes C136 H136 O2 0.9616 2.5982 3.276(4) 127.76 7_545 yes C212 H212 N1 0.9553 2.5857 3.400(3) 143.38 . yes C234 H234 O1 0.9594 2.4562 3.373(4) 159.87 8_555 yes C322 H322 N1 0.9644 2.6058 3.430(3) 143.63 . yes _exptl_crystal_F_000 4112 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 33 _reflns_limit_l_min 0 _reflns_limit_l_max 36 _reflns_number_observed ? _reflns_d_resolution_high .664 _reflns_d_resolution_low 12.115 _diffrn_reflns_av_sigmaI/netI .11 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .106 _refine_ls_wR_factor_all .079 _refine_ls_goodness_of_fit_all 1.021 _refine_ls_shift/su_mean .001 #========================================================================== data_7_H1052 _database_code_depnum_ccdc_archive 'CCDC 268667' # EXPERIMENTAL DATA #--------------------- _chemical_name_systematic ; Tris(triphenylphosphine)(acetonitrile)copper(I) tetrafluoroborate ; _chemical_formula_sum 'C56 H48 B1 Cu1 F4 N1 P3' _chemical_formula_moiety ? _chemical_formula_weight 978.28 _chemical_melting_point ? _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_b_c_a _symmetry_space_group_name_Hall -p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,+y,1/2-z 1/2-x,1/2+y,+z +x,1/2-y,1/2+z _cell_length_a 17.7300(10) _cell_length_b 22.2800(10) _cell_length_c 24.1850(10) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 9553.7(8) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.36 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7236 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.98 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .613 _exptl_crystal_description plate _exptl_crystal_size_max .32 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .09 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .91 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 126697 _reflns_number_total 9761 _reflns_Friedel_coverage 0 _reflns_number_gt 7132 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .097 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .047 _refine_ls_wR_factor_ref .064 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_number_reflns 7132 _refine_ls_number_parameters 595 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment noref _refine_ls_shift/su_max .006 _refine_diff_density_min -.298 _refine_diff_density_max .672 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 448 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 384 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' B ? 0 8 0 .001 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 8 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 32 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 8 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 24 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Cu1 Cu Uani 0.43987(2) 0.24360(2) 0.35729(1) 1.000 0.0178(1) . . P1 P Uani 0.42816(4) 0.16582(3) 0.29450(3) 1.000 0.0184(2) . . P2 P Uani 0.45231(4) 0.21149(3) 0.44787(3) 1.000 0.0186(2) . . P3 P Uani 0.36310(4) 0.32761(3) 0.34913(3) 1.000 0.0190(2) . . N1 N Uani 0.54696(14) 0.27345(12) 0.34012(11) 1.000 0.0237(8) . . C1 C Uani 0.60498(18) 0.29244(14) 0.33191(13) 1.000 0.0241(9) . . C11 C Uani 0.6789(2) 0.31869(18) 0.32117(15) 1.000 0.0405(11) . . C111 C Uani 0.37076(16) 0.10355(13) 0.31953(12) 1.000 0.0211(9) . . C112 C Uani 0.31426(17) 0.11663(14) 0.35777(12) 1.000 0.0236(9) . . C113 C Uani 0.26920(18) 0.07167(15) 0.38000(13) 1.000 0.0289(10) . . C114 C Uani 0.27986(19) 0.01307(15) 0.36337(15) 1.000 0.0330(11) . . C115 C Uani 0.3351(2) -0.00029(15) 0.32478(15) 1.000 0.0366(11) . . C116 C Uani 0.38078(18) 0.04387(14) 0.30300(14) 1.000 0.0298(10) . . C121 C Uani 0.38528(16) 0.18611(14) 0.22830(12) 1.000 0.0214(9) . . C122 C Uani 0.39689(18) 0.24482(14) 0.20981(12) 1.000 0.0263(10) . . C123 C Uani 0.3672(2) 0.26404(16) 0.15996(15) 1.000 0.0364(11) . . C124 C Uani 0.3264(2) 0.22466(19) 0.12781(14) 1.000 0.0402(13) . . C125 C Uani 0.31492(19) 0.16653(19) 0.14552(14) 1.000 0.0378(13) . . C126 C Uani 0.34360(18) 0.14712(15) 0.19549(14) 1.000 0.0301(10) . . C131 C Uani 0.51681(16) 0.13097(13) 0.27363(12) 1.000 0.0214(8) . . C132 C Uani 0.57564(17) 0.12897(14) 0.31231(13) 1.000 0.0246(9) . . C133 C Uani 0.64345(17) 0.10197(16) 0.29885(14) 1.000 0.0302(10) . . C134 C Uani 0.65444(18) 0.07672(15) 0.24732(14) 1.000 0.0296(10) . . C135 C Uani 0.59653(19) 0.07796(15) 0.20912(13) 1.000 0.0290(10) . . C136 C Uani 0.52789(18) 0.10470(14) 0.22195(13) 1.000 0.0254(9) . . C211 C Uani 0.48904(16) 0.26944(13) 0.49416(12) 1.000 0.0209(8) . . C212 C Uani 0.51923(16) 0.32212(13) 0.47168(12) 1.000 0.0219(9) . . C213 C Uani 0.54535(17) 0.36752(14) 0.50609(13) 1.000 0.0253(9) . . C214 C Uani 0.54097(19) 0.36085(14) 0.56273(13) 1.000 0.0291(10) . . C215 C Uani 0.5108(2) 0.30898(15) 0.58537(13) 1.000 0.0334(10) . . C216 C Uani 0.4859(2) 0.26339(14) 0.55138(13) 1.000 0.0297(10) . . C221 C Uani 0.51924(18) 0.14960(14) 0.45648(12) 1.000 0.0247(9) . . C222 C Uani 0.4985(2) 0.09109(14) 0.44271(14) 1.000 0.0312(10) . . C223 C Uani 0.5499(2) 0.04489(16) 0.44587(16) 1.000 0.0433(14) . . C224 C Uani 0.6231(3) 0.0560(2) 0.4614(2) 1.000 0.0643(17) . . C225 C Uani 0.6451(3) 0.1138(2) 0.4739(2) 1.000 0.0657(17) . . C226 C Uani 0.5937(2) 0.16045(18) 0.47192(17) 1.000 0.0433(12) . . C231 C Uani 0.36851(16) 0.18361(13) 0.48411(12) 1.000 0.0215(8) . . C232 C Uani 0.29840(17) 0.20646(13) 0.46803(13) 1.000 0.0241(9) . . C233 C Uani 0.23293(17) 0.18685(15) 0.49304(14) 1.000 0.0293(10) . . C234 C Uani 0.23539(19) 0.14377(16) 0.53395(14) 1.000 0.0338(11) . . C235 C Uani 0.3043(2) 0.12069(15) 0.55031(13) 1.000 0.0328(11) . . C236 C Uani 0.37072(18) 0.14064(14) 0.52578(12) 1.000 0.0266(9) . . C311 C Uani 0.26225(16) 0.31092(13) 0.34557(12) 1.000 0.0210(8) . . C312 C Uani 0.23936(18) 0.26159(14) 0.31452(13) 1.000 0.0271(9) . . C313 C Uani 0.16363(19) 0.24892(15) 0.30652(15) 1.000 0.0334(11) . . C314 C Uani 0.10972(19) 0.28594(17) 0.32937(16) 1.000 0.0394(11) . . C315 C Uani 0.13083(18) 0.33428(17) 0.36156(16) 1.000 0.0382(11) . . C316 C Uani 0.20667(18) 0.34695(14) 0.36940(14) 1.000 0.0302(10) . . C321 C Uani 0.37828(16) 0.37383(13) 0.28742(12) 1.000 0.0223(9) . . C322 C Uani 0.45207(18) 0.38540(14) 0.27034(14) 1.000 0.0289(10) . . C323 C Uani 0.46576(19) 0.41952(15) 0.22397(15) 1.000 0.0341(11) . . C324 C Uani 0.4065(2) 0.44304(15) 0.19371(14) 1.000 0.0360(11) . . C325 C Uani 0.3331(2) 0.43186(15) 0.20955(14) 1.000 0.0341(11) . . C326 C Uani 0.31919(18) 0.39789(14) 0.25653(13) 1.000 0.0263(9) . . C331 C Uani 0.37194(16) 0.38256(13) 0.40520(12) 1.000 0.0214(8) . . C332 C Uani 0.34237(18) 0.37055(14) 0.45737(14) 1.000 0.0295(10) . . C333 C Uani 0.35200(19) 0.41042(16) 0.50076(14) 1.000 0.0333(11) . . C334 C Uani 0.39266(19) 0.46253(15) 0.49291(15) 1.000 0.0329(11) . . C335 C Uani 0.42434(19) 0.47440(14) 0.44186(14) 1.000 0.0300(10) . . C336 C Uani 0.41360(18) 0.43487(14) 0.39811(13) 1.000 0.0258(9) . . F1 F Uani 0.60778(16) 0.42750(11) 0.38856(10) 1.000 0.0635(9) . . F2 F Uani 0.57084(14) 0.51888(12) 0.36007(12) 1.000 0.0665(10) . . F3 F Uani 0.63182(17) 0.45561(13) 0.30132(10) 1.000 0.0713(10) . . F4 F Uani 0.69373(15) 0.49809(17) 0.37209(15) 1.000 0.0953(15) . . B1 B Uani 0.6259(3) 0.4752(2) 0.35507(18) 1.000 0.0413(14) . . H11A H Uiso 0.70102 0.33377 0.35414 1.000 0.0610 . . H11B H Uiso 0.67513 0.35097 0.29495 1.000 0.0610 . . H11C H Uiso 0.71192 0.28924 0.30555 1.000 0.0610 . . H112 H Uiso 0.30726 0.15741 0.36933 1.000 0.0290 . . H113 H Uiso 0.23056 0.08125 0.40662 1.000 0.0360 . . H114 H Uiso 0.24831 -0.01809 0.37810 1.000 0.0400 . . H115 H Uiso 0.34185 -0.04095 0.31283 1.000 0.0430 . . H116 H Uiso 0.41985 0.03407 0.27673 1.000 0.0350 . . H122 H Uiso 0.42658 0.27207 0.23197 1.000 0.0330 . . H123 H Uiso 0.37419 0.30480 0.14765 1.000 0.0460 . . H124 H Uiso 0.30582 0.23796 0.09287 1.000 0.0480 . . H125 H Uiso 0.28611 0.13933 0.12273 1.000 0.0470 . . H126 H Uiso 0.33496 0.10648 0.20776 1.000 0.0370 . . H132 H Uiso 0.56821 0.14550 0.34843 1.000 0.0310 . . H133 H Uiso 0.68339 0.10016 0.32610 1.000 0.0370 . . H134 H Uiso 0.70199 0.05854 0.23775 1.000 0.0360 . . H135 H Uiso 0.60397 0.06073 0.17325 1.000 0.0340 . . H136 H Uiso 0.48809 0.10500 0.19481 1.000 0.0310 . . H212 H Uiso 0.52203 0.32720 0.43210 1.000 0.0270 . . H213 H Uiso 0.56645 0.40360 0.49024 1.000 0.0310 . . H214 H Uiso 0.55965 0.39219 0.58634 1.000 0.0370 . . H215 H Uiso 0.50625 0.30507 0.62479 1.000 0.0410 . . H216 H Uiso 0.46620 0.22698 0.56735 1.000 0.0360 . . H222 H Uiso 0.44724 0.08290 0.43129 1.000 0.0390 . . H223 H Uiso 0.53497 0.00444 0.43663 1.000 0.0520 . . H224 H Uiso 0.65911 0.02411 0.46394 1.000 0.0770 . . H225 H Uiso 0.69682 0.12186 0.48318 1.000 0.0780 . . H226 H Uiso 0.60966 0.20028 0.48148 1.000 0.0520 . . H232 H Uiso 0.29658 0.23617 0.43900 1.000 0.0300 . . H233 H Uiso 0.18466 0.20332 0.48150 1.000 0.0360 . . H234 H Uiso 0.18922 0.12963 0.55082 1.000 0.0420 . . H235 H Uiso 0.30662 0.09063 0.57925 1.000 0.0390 . . H236 H Uiso 0.41873 0.12424 0.53707 1.000 0.0340 . . H312 H Uiso 0.27725 0.23615 0.29804 1.000 0.0340 . . H313 H Uiso 0.14835 0.21375 0.28596 1.000 0.0410 . . H314 H Uiso 0.05733 0.27871 0.32195 1.000 0.0480 . . H315 H Uiso 0.09252 0.35923 0.37771 1.000 0.0480 . . H316 H Uiso 0.22141 0.38086 0.39166 1.000 0.0360 . . H322 H Uiso 0.49357 0.36924 0.29141 1.000 0.0350 . . H323 H Uiso 0.51680 0.42706 0.21240 1.000 0.0410 . . H324 H Uiso 0.41672 0.46708 0.16153 1.000 0.0450 . . H325 H Uiso 0.29178 0.44753 0.18789 1.000 0.0400 . . H326 H Uiso 0.26807 0.39126 0.26816 1.000 0.0330 . . H332 H Uiso 0.31442 0.33450 0.46258 1.000 0.0360 . . H333 H Uiso 0.33065 0.40171 0.53638 1.000 0.0410 . . H334 H Uiso 0.39886 0.49062 0.52322 1.000 0.0410 . . H335 H Uiso 0.45393 0.50967 0.43608 1.000 0.0370 . . H336 H Uiso 0.43514 0.44353 0.36242 1.000 0.0310 . . 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 Cu1 0.0179(2) 0.0185(2) 0.0171(2) -0.0006(1) 0.0003(1) -0.0016(1) P1 0.0192(4) 0.0187(4) 0.0172(4) -0.0009(3) 0.0010(3) -0.0018(3) P2 0.0198(4) 0.0189(4) 0.0171(4) -0.0007(3) 0.0004(3) -0.0010(3) P3 0.0186(4) 0.0168(4) 0.0217(4) 0.0006(3) 0.0002(3) -0.0017(3) N1 0.0207(13) 0.0246(14) 0.0259(13) 0.0002(11) 0.0013(11) -0.0032(10) C1 0.0260(17) 0.0245(16) 0.0218(16) -0.0013(12) 0.0016(13) 0.0035(13) C11 0.0274(18) 0.054(2) 0.040(2) -0.0113(18) 0.0071(16) -0.0124(16) C111 0.0217(15) 0.0218(15) 0.0198(15) 0.0039(11) -0.0019(12) -0.0027(12) C112 0.0259(16) 0.0237(16) 0.0213(15) -0.0023(12) -0.0001(13) -0.0015(12) C113 0.0261(17) 0.0352(19) 0.0253(16) 0.0030(14) 0.0034(14) -0.0028(14) C114 0.0301(17) 0.0299(18) 0.039(2) 0.0071(15) 0.0067(15) -0.0085(14) C115 0.041(2) 0.0197(16) 0.049(2) -0.0019(15) 0.0061(17) -0.0034(14) C116 0.0279(17) 0.0250(17) 0.0366(19) -0.0036(14) 0.0051(14) -0.0019(13) C121 0.0202(15) 0.0303(17) 0.0138(14) -0.0007(12) 0.0005(12) 0.0022(12) C122 0.0338(18) 0.0239(16) 0.0211(16) -0.0028(12) 0.0055(13) 0.0031(13) C123 0.041(2) 0.037(2) 0.0312(18) 0.0092(15) 0.0086(16) 0.0136(16) C124 0.034(2) 0.066(3) 0.0207(17) 0.0085(17) -0.0025(15) 0.0069(19) C125 0.0266(18) 0.066(3) 0.0207(17) 0.0003(16) -0.0015(14) -0.0133(17) C126 0.0275(17) 0.0362(19) 0.0267(17) 0.0016(14) 0.0004(14) -0.0061(14) C131 0.0191(14) 0.0217(15) 0.0234(15) -0.0003(12) 0.0051(12) -0.0023(12) C132 0.0233(15) 0.0288(17) 0.0218(15) -0.0003(13) 0.0007(13) -0.0013(12) C133 0.0226(16) 0.039(2) 0.0291(17) -0.0008(14) -0.0040(14) -0.0005(14) C134 0.0249(16) 0.0337(18) 0.0303(17) 0.0021(14) 0.0058(14) 0.0056(14) C135 0.0373(19) 0.0267(17) 0.0229(16) -0.0015(13) 0.0046(14) 0.0058(14) C136 0.0283(16) 0.0238(16) 0.0240(16) -0.0010(13) -0.0011(13) 0.0009(13) C211 0.0203(15) 0.0198(14) 0.0227(15) -0.0028(12) -0.0009(12) 0.0030(11) C212 0.0197(14) 0.0257(16) 0.0203(15) -0.0025(12) -0.0001(12) 0.0009(12) C213 0.0219(15) 0.0241(16) 0.0298(17) -0.0001(13) -0.0007(13) -0.0019(12) C214 0.0366(18) 0.0262(17) 0.0246(16) -0.0038(13) -0.0077(14) 0.0009(14) C215 0.051(2) 0.0300(18) 0.0192(16) -0.0013(13) -0.0048(15) -0.0016(16) C216 0.0411(19) 0.0278(17) 0.0203(15) 0.0011(13) 0.0008(14) -0.0035(14) C221 0.0274(16) 0.0287(16) 0.0179(15) 0.0000(12) -0.0019(13) 0.0059(13) C222 0.041(2) 0.0253(17) 0.0274(17) 0.0021(13) 0.0056(15) 0.0032(14) C223 0.064(3) 0.029(2) 0.037(2) -0.0008(16) 0.004(2) 0.0151(18) C224 0.071(3) 0.063(3) 0.059(3) -0.015(2) -0.013(2) 0.043(3) C225 0.045(3) 0.075(3) 0.077(3) -0.030(3) -0.023(2) 0.027(2) C226 0.032(2) 0.045(2) 0.053(2) -0.0186(18) -0.0108(18) 0.0109(16) C231 0.0243(15) 0.0227(15) 0.0176(14) -0.0047(11) 0.0038(12) -0.0039(12) C232 0.0257(16) 0.0221(16) 0.0245(16) -0.0049(12) 0.0015(13) 0.0001(12) C233 0.0202(15) 0.0370(19) 0.0306(18) -0.0065(14) 0.0015(13) -0.0050(14) C234 0.0327(18) 0.042(2) 0.0266(17) -0.0048(15) 0.0078(14) -0.0131(15) C235 0.042(2) 0.0340(19) 0.0223(16) 0.0017(14) 0.0064(15) -0.0080(15) C236 0.0322(17) 0.0273(17) 0.0202(15) 0.0016(12) 0.0025(13) -0.0022(13) C311 0.0167(14) 0.0227(15) 0.0237(15) 0.0081(12) -0.0035(12) -0.0042(12) C312 0.0262(16) 0.0307(17) 0.0244(16) 0.0023(13) -0.0015(13) -0.0028(13) C313 0.0325(18) 0.0348(19) 0.0328(18) 0.0026(15) -0.0058(15) -0.0123(15) C314 0.0222(17) 0.048(2) 0.048(2) 0.0123(18) -0.0057(16) -0.0093(16) C315 0.0196(16) 0.040(2) 0.055(2) 0.0061(17) 0.0034(16) 0.0035(14) C316 0.0266(17) 0.0240(17) 0.040(2) 0.0000(14) 0.0023(15) 0.0015(13) C321 0.0249(16) 0.0163(14) 0.0257(16) -0.0005(12) 0.0023(13) -0.0038(12) C322 0.0297(17) 0.0242(17) 0.0329(18) 0.0019(14) 0.0020(14) 0.0008(13) C323 0.0349(19) 0.0293(18) 0.038(2) 0.0025(15) 0.0124(16) -0.0025(14) C324 0.054(2) 0.0277(18) 0.0263(17) 0.0042(14) 0.0061(17) -0.0046(16) C325 0.045(2) 0.0313(18) 0.0261(17) 0.0025(14) -0.0053(16) -0.0007(16) C326 0.0310(17) 0.0230(16) 0.0250(16) -0.0008(13) -0.0009(14) -0.0018(13) C331 0.0188(14) 0.0210(15) 0.0245(15) -0.0004(12) -0.0045(12) 0.0020(11) C332 0.0285(17) 0.0261(16) 0.0339(18) -0.0027(14) 0.0058(14) -0.0068(13) C333 0.0338(19) 0.039(2) 0.0272(17) -0.0059(15) 0.0059(15) -0.0017(15) C334 0.0350(19) 0.0286(18) 0.035(2) -0.0095(15) -0.0009(15) -0.0019(14) C335 0.0374(18) 0.0183(16) 0.0343(18) -0.0006(14) -0.0032(15) -0.0050(13) C336 0.0269(16) 0.0238(16) 0.0268(17) 0.0015(13) -0.0019(13) -0.0009(13) F1 0.0814(18) 0.0632(16) 0.0459(14) 0.0277(12) 0.0194(13) 0.0310(14) F2 0.0586(16) 0.0559(16) 0.085(2) 0.0324(14) 0.0148(14) 0.0223(12) F3 0.094(2) 0.088(2) 0.0319(13) 0.0145(13) 0.0011(14) 0.0086(16) F4 0.0438(16) 0.122(3) 0.120(3) -0.037(2) 0.0039(17) -0.0040(17) B1 0.034(2) 0.051(3) 0.039(2) 0.014(2) 0.0003(19) 0.010(2) #=============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P1 2.3135(8) . . yes Cu1 P2 2.3151(8) . . yes Cu1 P3 2.3227(8) . . yes Cu1 N1 2.054(3) . . yes P1 C111 1.824(3) . . yes P1 C121 1.829(3) . . yes P1 C131 1.824(3) . . yes P2 C211 1.829(3) . . yes P2 C221 1.831(3) . . yes P2 C231 1.833(3) . . yes P3 C311 1.828(3) . . yes P3 C321 1.833(3) . . yes P3 C331 1.834(3) . . yes F1 B1 1.374(5) . . yes F2 B1 1.384(6) . . yes F3 B1 1.375(5) . . yes F4 B1 1.370(6) . . yes N1 C1 1.130(4) . . yes C1 C11 1.458(5) . . no C111 C112 1.394(4) . . no C111 C116 1.400(4) . . no C11 H11A 0.9500 . . no C11 H11B 0.9612 . . no C11 H11C 0.9571 . . no C112 C113 1.390(4) . . no C113 C114 1.379(5) . . no C114 C115 1.385(5) . . no C115 C116 1.379(5) . . no C121 C122 1.398(4) . . no C121 C126 1.389(4) . . no C122 C123 1.383(5) . . no C123 C124 1.378(5) . . no C124 C125 1.379(6) . . no C125 C126 1.381(5) . . no C131 C132 1.402(4) . . no C131 C136 1.394(4) . . no C132 C133 1.383(4) . . no C133 C134 1.381(5) . . no C134 C135 1.381(5) . . no C135 C136 1.390(5) . . no C211 C216 1.392(4) . . no C211 C212 1.400(4) . . no C112 H112 0.9587 . . no C212 C213 1.389(4) . . no C113 H113 0.9640 . . no C213 C214 1.380(4) . . no C214 C215 1.386(5) . . no C114 H114 0.9601 . . no C215 C216 1.379(5) . . no C115 H115 0.9584 . . no C116 H116 0.9650 . . no C221 C226 1.393(5) . . no C221 C222 1.395(4) . . no C122 H122 0.9659 . . no C222 C223 1.377(5) . . no C223 C224 1.374(6) . . no C123 H123 0.9637 . . no C124 H124 0.9670 . . no C224 C225 1.379(6) . . no C225 C226 1.383(6) . . no C125 H125 0.9654 . . no C126 H126 0.9651 . . no C231 C236 1.391(4) . . no C231 C232 1.398(4) . . no C132 H132 0.9571 . . no C232 C233 1.380(4) . . no C133 H133 0.9682 . . no C233 C234 1.379(5) . . no C134 H134 0.9635 . . no C234 C235 1.383(5) . . no C235 C236 1.392(5) . . no C135 H135 0.9578 . . no C136 H136 0.9638 . . no C311 C316 1.396(4) . . no C311 C312 1.392(4) . . no C312 C313 1.386(5) . . no C212 H212 0.9652 . . no C313 C314 1.378(5) . . no C213 H213 0.9660 . . no C314 C315 1.381(5) . . no C214 H214 0.9609 . . no C315 C316 1.387(5) . . no C215 H215 0.9607 . . no C216 H216 0.9640 . . no C321 C322 1.396(4) . . no C321 C326 1.394(4) . . no C322 C323 1.376(5) . . no C222 H222 0.9672 . . no C223 H223 0.9655 . . no C323 C324 1.384(5) . . no C224 H224 0.9572 . . no C324 C325 1.379(5) . . no C325 C326 1.387(5) . . no C225 H225 0.9610 . . no C226 H226 0.9597 . . no C331 C332 1.392(4) . . no C331 C336 1.390(4) . . no C332 C333 1.385(5) . . no C232 H232 0.9655 . . no C333 C334 1.380(5) . . no C233 H233 0.9721 . . no C234 H234 0.9674 . . no C334 C335 1.382(5) . . no C235 H235 0.9696 . . no C335 C336 1.390(5) . . no C236 H236 0.9657 . . no C312 H312 0.9651 . . no C313 H313 0.9668 . . no C314 H314 0.9597 . . no C315 H315 0.9607 . . no C316 H316 0.9638 . . no C322 H322 0.9647 . . no C323 H323 0.9620 . . no C324 H324 0.9620 . . no C325 H325 0.9659 . . no C326 H326 0.9604 . . no C332 H332 0.9521 . . no C333 H333 0.9608 . . no C334 H334 0.9701 . . no C335 H335 0.9551 . . no C336 H336 0.9634 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Cu1 P2 113.47(3) . . . yes P1 Cu1 P3 119.69(3) . . . yes P1 Cu1 N1 101.11(8) . . . yes P2 Cu1 P3 112.66(3) . . . yes P2 Cu1 N1 101.73(8) . . . yes P3 Cu1 N1 105.28(8) . . . yes Cu1 P1 C111 113.70(10) . . . yes Cu1 P1 C121 115.26(10) . . . yes Cu1 P1 C131 115.03(10) . . . yes C111 P1 C121 104.27(13) . . . yes C111 P1 C131 104.41(13) . . . yes C121 P1 C131 102.77(13) . . . yes Cu1 P2 C211 113.27(10) . . . yes Cu1 P2 C221 113.71(10) . . . yes Cu1 P2 C231 118.68(10) . . . yes C211 P2 C221 103.37(14) . . . yes C211 P2 C231 103.60(13) . . . yes C221 P2 C231 102.46(14) . . . yes Cu1 P3 C311 114.41(10) . . . yes Cu1 P3 C321 115.84(10) . . . yes Cu1 P3 C331 115.16(10) . . . yes C311 P3 C321 102.68(13) . . . yes C311 P3 C331 104.73(13) . . . yes C321 P3 C331 102.38(13) . . . yes Cu1 N1 C1 176.6(3) . . . yes N1 C1 C11 178.3(3) . . . yes P1 C111 C112 117.5(2) . . . yes P1 C111 C116 123.8(2) . . . yes C112 C111 C116 118.6(3) . . . no C1 C11 H11B 110.80 . . . no C1 C11 H11C 110.19 . . . no H11A C11 H11B 108.53 . . . no H11A C11 H11C 108.74 . . . no H11B C11 H11C 107.16 . . . no C1 C11 H11A 111.30 . . . no C111 C112 C113 121.3(3) . . . no C112 C113 C114 119.4(3) . . . no C113 C114 C115 119.8(3) . . . no C114 C115 C116 121.3(3) . . . no C111 C116 C115 119.6(3) . . . no P1 C121 C122 116.8(2) . . . yes P1 C121 C126 124.5(2) . . . yes C122 C121 C126 118.7(3) . . . no C121 C122 C123 120.8(3) . . . no C122 C123 C124 119.6(3) . . . no C123 C124 C125 120.0(3) . . . no C124 C125 C126 120.8(3) . . . no C121 C126 C125 120.0(3) . . . no C132 C131 C136 118.7(3) . . . no P1 C131 C136 123.2(2) . . . yes P1 C131 C132 118.0(2) . . . yes C131 C132 C133 120.2(3) . . . no C132 C133 C134 120.8(3) . . . no C133 C134 C135 119.4(3) . . . no C134 C135 C136 120.7(3) . . . no C131 C136 C135 120.2(3) . . . no P2 C211 C216 121.7(2) . . . yes P2 C211 C212 119.4(2) . . . yes C212 C211 C216 118.9(3) . . . no C111 C112 H112 118.98 . . . no C113 C112 H112 119.73 . . . no C211 C212 C213 120.3(3) . . . no C212 C213 C214 119.8(3) . . . no C112 C113 H113 120.49 . . . no C114 C113 H113 120.11 . . . no C115 C114 H114 120.43 . . . no C113 C114 H114 119.77 . . . no C213 C214 C215 120.2(3) . . . no C116 C115 H115 119.07 . . . no C114 C115 H115 119.64 . . . no C214 C215 C216 120.1(3) . . . no C111 C116 H116 119.61 . . . no C211 C216 C215 120.6(3) . . . no C115 C116 H116 120.78 . . . no P2 C221 C222 120.4(2) . . . yes P2 C221 C226 120.9(3) . . . yes C222 C221 C226 118.4(3) . . . no C123 C122 H122 119.76 . . . no C221 C222 C223 120.7(3) . . . no C121 C122 H122 119.41 . . . no C122 C123 H123 120.80 . . . no C222 C223 C224 120.4(3) . . . no C124 C123 H123 119.56 . . . no C123 C124 H124 119.75 . . . no C125 C124 H124 120.23 . . . no C223 C224 C225 119.7(4) . . . no C224 C225 C226 120.5(5) . . . no C126 C125 H125 119.87 . . . no C124 C125 H125 119.36 . . . no C121 C126 H126 119.70 . . . no C221 C226 C225 120.2(4) . . . no C125 C126 H126 120.30 . . . no P2 C231 C232 117.6(2) . . . yes C232 C231 C236 118.5(3) . . . no P2 C231 C236 123.8(2) . . . yes C133 C132 H132 120.12 . . . no C131 C132 H132 119.63 . . . no C231 C232 C233 120.7(3) . . . no C132 C133 H133 119.58 . . . no C134 C133 H133 119.61 . . . no C232 C233 C234 120.5(3) . . . no C133 C134 H134 120.76 . . . no C233 C234 C235 119.5(3) . . . no C135 C134 H134 119.87 . . . no C234 C235 C236 120.4(3) . . . no C134 C135 H135 119.69 . . . no C136 C135 H135 119.64 . . . no C231 C236 C235 120.3(3) . . . no C135 C136 H136 119.47 . . . no C131 C136 H136 120.30 . . . no P3 C311 C316 123.7(2) . . . yes P3 C311 C312 118.1(2) . . . yes C312 C311 C316 118.1(3) . . . no C211 C212 H212 120.21 . . . no C213 C212 H212 119.44 . . . no C311 C312 C313 121.3(3) . . . no C312 C313 C314 119.6(3) . . . no C212 C213 H213 119.82 . . . no C214 C213 H213 120.35 . . . no C313 C314 C315 120.3(3) . . . no C213 C214 H214 119.49 . . . no C215 C214 H214 120.27 . . . no C216 C215 H215 119.85 . . . no C314 C315 C316 119.9(3) . . . no C214 C215 H215 120.00 . . . no C215 C216 H216 119.80 . . . no C311 C316 C315 120.7(3) . . . no C211 C216 H216 119.64 . . . no P3 C321 C322 118.8(2) . . . yes P3 C321 C326 122.8(2) . . . yes C322 C321 C326 118.3(3) . . . no C321 C322 C323 120.6(3) . . . no C223 C222 H222 119.78 . . . no C221 C222 H222 119.49 . . . no C224 C223 H223 119.38 . . . no C322 C323 C324 120.4(3) . . . no C222 C223 H223 120.23 . . . no C225 C224 H224 119.37 . . . no C223 C224 H224 120.93 . . . no C323 C324 C325 120.1(3) . . . no C224 C225 H225 119.71 . . . no C226 C225 H225 119.76 . . . no C324 C325 C326 119.6(3) . . . no C225 C226 H226 119.49 . . . no C221 C226 H226 120.29 . . . no C321 C326 C325 121.0(3) . . . no P3 C331 C332 120.6(2) . . . yes C332 C331 C336 118.2(3) . . . no P3 C331 C336 120.9(2) . . . yes C233 C232 H232 120.51 . . . no C331 C332 C333 121.1(3) . . . no C231 C232 H232 118.79 . . . no C232 C233 H233 119.68 . . . no C234 C233 H233 119.77 . . . no C332 C333 C334 120.0(3) . . . no C233 C234 H234 120.16 . . . no C235 C234 H234 120.38 . . . no C333 C334 C335 119.8(3) . . . no C234 C235 H235 120.05 . . . no C334 C335 C336 120.2(3) . . . no C236 C235 H235 119.50 . . . no C331 C336 C335 120.7(3) . . . no C231 C236 H236 119.36 . . . no C235 C236 H236 120.30 . . . no C311 C312 H312 118.93 . . . no C313 C312 H312 119.81 . . . no C312 C313 H313 120.56 . . . no C314 C313 H313 119.80 . . . no C313 C314 H314 119.73 . . . no C315 C314 H314 119.92 . . . no C314 C315 H315 119.27 . . . no C316 C315 H315 120.80 . . . no C311 C316 H316 119.35 . . . no C315 C316 H316 119.92 . . . no C321 C322 H322 119.31 . . . no C323 C322 H322 120.13 . . . no C322 C323 H323 119.96 . . . no C324 C323 H323 119.63 . . . no C323 C324 H324 119.72 . . . no C325 C324 H324 120.20 . . . no C324 C325 H325 119.98 . . . no C326 C325 H325 120.43 . . . no C321 C326 H326 119.55 . . . no C325 C326 H326 119.44 . . . no C331 C332 H332 118.56 . . . no C333 C332 H332 120.32 . . . no C332 C333 H333 120.07 . . . no C334 C333 H333 119.95 . . . no C333 C334 H334 119.87 . . . no C335 C334 H334 120.37 . . . no C334 C335 H335 120.76 . . . no C336 C335 H335 119.03 . . . no C331 C336 H336 119.27 . . . no C335 C336 H336 120.06 . . . no F1 B1 F2 109.1(4) . . . yes F1 B1 F3 109.2(3) . . . yes F1 B1 F4 108.4(4) . . . yes F2 B1 F3 111.1(4) . . . yes F2 B1 F4 109.3(4) . . . yes F3 B1 F4 109.6(4) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Cu1 P1 C111 38.64(11) . . . . no P2 Cu1 P1 C121 158.97(10) . . . . no P2 Cu1 P1 C131 -81.68(11) . . . . no P3 Cu1 P1 C111 -98.32(11) . . . . no P3 Cu1 P1 C121 22.01(11) . . . . no P3 Cu1 P1 C131 141.36(11) . . . . no N1 Cu1 P1 C111 146.77(13) . . . . no N1 Cu1 P1 C121 -92.90(13) . . . . no N1 Cu1 P1 C131 26.45(13) . . . . no P1 Cu1 P2 C211 162.87(10) . . . . no P1 Cu1 P2 C221 45.24(12) . . . . no P1 Cu1 P2 C231 -75.33(11) . . . . no P3 Cu1 P2 C211 -57.10(11) . . . . no P3 Cu1 P2 C221 -174.73(11) . . . . no P3 Cu1 P2 C231 64.69(11) . . . . no N1 Cu1 P2 C211 55.13(13) . . . . no N1 Cu1 P2 C221 -62.50(14) . . . . no N1 Cu1 P2 C231 176.93(13) . . . . no P1 Cu1 P3 C311 53.04(11) . . . . no P1 Cu1 P3 C321 -66.14(11) . . . . no P1 Cu1 P3 C331 174.47(10) . . . . no P2 Cu1 P3 C311 -84.24(11) . . . . no P2 Cu1 P3 C321 156.58(11) . . . . no P2 Cu1 P3 C331 37.19(11) . . . . no N1 Cu1 P3 C311 165.73(13) . . . . no N1 Cu1 P3 C321 46.55(13) . . . . no N1 Cu1 P3 C331 -72.83(13) . . . . no Cu1 P1 C111 C112 28.6(3) . . . . no C121 P1 C111 C112 -97.8(2) . . . . no C131 P1 C111 C112 154.7(2) . . . . no Cu1 P1 C111 C116 -150.8(2) . . . . no C121 P1 C111 C116 82.9(3) . . . . no C131 P1 C111 C116 -24.6(3) . . . . no Cu1 P1 C131 C132 31.8(3) . . . . no Cu1 P1 C121 C122 30.4(3) . . . . no C111 P1 C121 C122 155.8(2) . . . . no C131 P1 C121 C122 -95.5(2) . . . . no Cu1 P1 C121 C126 -150.6(2) . . . . no C111 P1 C121 C126 -25.2(3) . . . . no C131 P1 C121 C126 83.5(3) . . . . no C121 P1 C131 C132 157.9(2) . . . . no Cu1 P1 C131 C136 -150.3(2) . . . . no C111 P1 C131 C132 -93.5(3) . . . . no C121 P1 C131 C136 -24.3(3) . . . . no C111 P1 C131 C136 84.4(3) . . . . no Cu1 P2 C231 C232 -28.5(3) . . . . no C231 P2 C221 C222 51.4(3) . . . . no C221 P2 C231 C232 -154.7(2) . . . . no C231 P2 C211 C212 -141.6(2) . . . . no C211 P2 C231 C232 98.1(2) . . . . no C221 P2 C231 C236 24.3(3) . . . . no Cu1 P2 C231 C236 150.5(2) . . . . no C211 P2 C231 C236 -83.0(3) . . . . no C221 P2 C211 C212 111.8(2) . . . . no Cu1 P2 C221 C226 96.1(3) . . . . no Cu1 P2 C211 C212 -11.7(3) . . . . no Cu1 P2 C221 C222 -77.9(3) . . . . no C211 P2 C221 C222 158.9(3) . . . . no Cu1 P2 C211 C216 166.4(2) . . . . no C231 P2 C221 C226 -134.6(3) . . . . no C221 P2 C211 C216 -70.1(3) . . . . no C231 P2 C211 C216 36.5(3) . . . . no C211 P2 C221 C226 -27.1(3) . . . . no C331 P3 C321 C322 84.1(3) . . . . no C321 P3 C331 C332 160.4(2) . . . . no Cu1 P3 C311 C312 -40.1(3) . . . . no C321 P3 C311 C312 86.2(3) . . . . no Cu1 P3 C331 C332 -73.0(3) . . . . no Cu1 P3 C311 C316 144.0(2) . . . . no Cu1 P3 C321 C322 -42.1(3) . . . . no C331 P3 C311 C312 -167.1(2) . . . . no C321 P3 C311 C316 -89.7(3) . . . . no Cu1 P3 C321 C326 137.7(2) . . . . no C311 P3 C321 C322 -167.5(2) . . . . no Cu1 P3 C331 C336 101.6(2) . . . . no C331 P3 C321 C326 -96.1(3) . . . . no C321 P3 C331 C336 -25.0(3) . . . . no C311 P3 C331 C332 53.6(3) . . . . no C331 P3 C311 C316 17.0(3) . . . . no C311 P3 C321 C326 12.3(3) . . . . no C311 P3 C331 C336 -131.9(3) . . . . no P2 C211 C212 C213 178.0(2) . . . . no C212 C211 C216 C215 1.2(5) . . . . no P1 C111 C112 H112 0.42 . . . . no C116 C111 C112 H112 179.79 . . . . no P1 C111 C116 H116 -0.30 . . . . no C112 C111 C116 H116 -179.63 . . . . no P2 C211 C216 C215 -177.0(3) . . . . no C216 C211 C212 C213 -0.2(4) . . . . no H112 C112 C113 C114 -179.68 . . . . no C111 C112 C113 H113 179.54 . . . . no H112 C112 C113 H113 0.75 . . . . no C211 C212 C213 C214 -0.5(4) . . . . no H113 C113 C114 H114 0.66 . . . . no H113 C113 C114 C115 179.50 . . . . no C112 C113 C114 H114 -178.91 . . . . no C212 C213 C214 C215 0.2(5) . . . . no H114 C114 C115 H115 -0.15 . . . . no H114 C114 C115 C116 179.76 . . . . no C213 C214 C215 C216 0.9(5) . . . . no C113 C114 C115 H115 -178.97 . . . . no H115 C115 C116 H116 -1.43 . . . . no C114 C115 C116 H116 178.66 . . . . no C214 C215 C216 C211 -1.6(5) . . . . no H115 C115 C116 C111 179.09 . . . . no P1 C121 C122 H122 0.20 . . . . no C122 C121 C126 H126 -179.79 . . . . no C126 C121 C122 H122 -178.85 . . . . no P2 C221 C222 C223 176.0(3) . . . . no C226 C221 C222 C223 1.9(5) . . . . no P2 C221 C226 C225 -174.7(3) . . . . no C222 C221 C226 C225 -0.6(5) . . . . no P1 C121 C126 H126 1.24 . . . . no H122 C122 C123 H123 -2.31 . . . . no C221 C222 C223 C224 -1.6(6) . . . . no C121 C122 C123 H123 178.49 . . . . no H122 C122 C123 C124 178.45 . . . . no H123 C123 C124 C125 -178.84 . . . . no C122 C123 C124 H124 -179.69 . . . . no C222 C223 C224 C225 0.0(7) . . . . no H123 C123 C124 H124 1.06 . . . . no H124 C124 C125 H125 -0.09 . . . . no C123 C124 C125 H125 179.81 . . . . no C223 C224 C225 C226 1.2(7) . . . . no H124 C124 C125 C126 -179.58 . . . . no H125 C125 C126 H126 -0.03 . . . . no H125 C125 C126 C121 179.80 . . . . no C124 C125 C126 H126 179.45 . . . . no C224 C225 C226 C221 -0.9(7) . . . . no P2 C231 C232 C233 179.1(2) . . . . no C236 C231 C232 C233 0.1(5) . . . . no C232 C231 C236 C235 0.6(4) . . . . no C132 C131 C136 H136 179.17 . . . . no P2 C231 C236 C235 -178.3(2) . . . . no P1 C131 C136 H136 1.29 . . . . no C136 C131 C132 H132 -177.70 . . . . no P1 C131 C132 H132 0.29 . . . . no H132 C132 C133 C134 178.54 . . . . no C231 C232 C233 C234 -0.8(5) . . . . no C131 C132 C133 H133 -178.84 . . . . no H132 C132 C133 H133 -0.42 . . . . no C132 C133 C134 H134 178.91 . . . . no C232 C233 C234 C235 0.7(5) . . . . no H133 C133 C134 H134 -2.13 . . . . no H133 C133 C134 C135 178.22 . . . . no C133 C134 C135 H135 179.62 . . . . no C233 C234 C235 C236 0.0(5) . . . . no H134 C134 C135 C136 -179.14 . . . . no H134 C134 C135 H135 -0.03 . . . . no H135 C135 C136 C131 -178.76 . . . . no C134 C135 C136 H136 -179.78 . . . . no H135 C135 C136 H136 1.11 . . . . no C234 C235 C236 C231 -0.7(5) . . . . no P3 C311 C312 H312 4.30 . . . . no C316 C311 C312 H312 -179.56 . . . . no P3 C311 C316 H316 -5.31 . . . . no C312 C311 C316 H316 178.78 . . . . no C311 C312 C313 H313 -177.83 . . . . no H312 C312 C313 C314 -178.93 . . . . no H312 C312 C313 H313 2.83 . . . . no C312 C313 C314 H314 176.08 . . . . no H313 C313 C314 C315 176.15 . . . . no H313 C313 C314 H314 -5.66 . . . . no C313 C314 C315 H315 -178.92 . . . . no H314 C314 C315 C316 -175.92 . . . . no H314 C314 C315 H315 2.90 . . . . no C314 C315 C316 H316 179.57 . . . . no H315 C315 C316 C311 -179.52 . . . . no H315 C315 C316 H316 0.77 . . . . no P3 C321 C322 H322 -0.55 . . . . no C326 C321 C322 H322 179.66 . . . . no P3 C321 C326 H326 1.77 . . . . no C322 C321 C326 H326 -178.45 . . . . no C321 C322 C323 H323 -179.64 . . . . no H322 C322 C323 C324 -179.72 . . . . no H322 C322 C323 H323 0.40 . . . . no C322 C323 C324 H324 179.53 . . . . no H323 C323 C324 C325 179.18 . . . . no H323 C323 C324 H324 -0.60 . . . . no C323 C324 C325 H325 -178.56 . . . . no H324 C324 C325 C326 -179.01 . . . . no H324 C324 C325 H325 1.22 . . . . no C324 C325 C326 H326 177.98 . . . . no H325 C325 C326 C321 178.48 . . . . no H325 C325 C326 H326 -2.25 . . . . no P3 C331 C332 H332 -4.37 . . . . no C336 C331 C332 H332 -179.10 . . . . no P3 C331 C336 H336 4.29 . . . . no C332 C331 C336 H336 179.01 . . . . no C331 C332 C333 H333 179.16 . . . . no H332 C332 C333 C334 179.91 . . . . no H332 C332 C333 H333 0.29 . . . . no C332 C333 C334 H334 179.29 . . . . no H333 C333 C334 C335 178.92 . . . . no H333 C333 C334 H334 -1.08 . . . . no C333 C334 C335 H335 -178.08 . . . . no H334 C334 C335 C336 -178.22 . . . . no H334 C334 C335 H335 1.92 . . . . no C334 C335 C336 H336 179.11 . . . . no H335 C335 C336 C331 178.91 . . . . no H335 C335 C336 H336 -1.03 . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu1 H112 3.0497 . . no Cu1 H122 3.1055 . . no Cu1 H132 3.1624 . . no Cu1 H212 2.9774 . . no Cu1 H232 3.2229 . . no Cu1 H312 3.2240 . . no Cu1 H322 3.3587 . . no P1 H312 3.1019 . . no F1 C213 3.330(4) . . no F1 C1 3.307(4) . . no F1 C234 3.340(4) . 3_556 no F1 C11 3.182(5) . . no F2 C136 3.264(4) . 4_655 no F3 C116 3.207(4) . 4_655 no F3 C115 3.257(4) . 4_655 no F3 C11 3.199(5) . . no F1 H11A 2.7905 . . no F1 H213 2.6207 . . no F1 H234 2.4196 . 3_556 no F1 H334 2.8096 . 5_666 no F2 H136 2.5564 . 4_655 no F2 H335 2.7781 . . no F3 H115 2.8010 . 4_655 no F3 H11B 2.4594 . . no F3 H116 2.7310 . 4_655 no F3 H325 2.8538 . 6_555 no F4 H325 2.5289 . 6_555 no N1 C132 3.328(4) . . no N1 C212 3.397(4) . . no N1 C322 3.450(4) . . no N1 H132 2.8825 . . no N1 H322 2.6151 . . no N1 H212 2.5648 . . no C1 F1 3.307(4) . . no C11 F1 3.182(5) . . no C11 C124 3.571(5) . 6_555 no C11 F3 3.199(5) . . no C11 C123 3.583(5) . 6_555 no C11 C326 3.582(5) . 6_555 no C11 C313 3.468(5) . 6_555 no C1 H212 2.9384 . . no C1 H322 2.7909 . . no C112 C231 3.534(4) . . no C112 C232 3.346(4) . . no C115 F3 3.257(4) . 4_645 no C116 C136 3.533(5) . . no C116 F3 3.207(4) . 4_645 no C116 C126 3.534(5) . . no C122 C321 3.449(4) . . no C122 C322 3.593(4) . . no C123 C215 3.519(5) . 8_554 no C123 C11 3.583(5) . 6_455 no C123 C216 3.420(5) . 8_554 no C124 C216 3.389(5) . 8_554 no C124 C11 3.571(5) . 6_455 no C124 C215 3.508(5) . 8_554 no C126 C116 3.534(5) . . no C126 C136 3.461(5) . . no C132 N1 3.328(4) . . no C132 C222 3.540(5) . . no C134 C324 3.475(5) . 4_645 no C134 C325 3.399(5) . 4_645 no C136 C126 3.461(5) . . no C136 F2 3.264(4) . 4_645 no C136 C116 3.533(5) . . no C111 H222 3.0588 . . no C211 C332 3.554(4) . . no C111 H126 2.7774 . . no C212 C332 3.334(4) . . no C212 C331 3.349(4) . . no C112 H222 3.0472 . . no C212 N1 3.397(4) . . no C112 H312 3.0997 . . no C213 C333 3.561(5) . . no C213 C234 3.515(5) . 3_556 no C213 F1 3.330(4) . . no C213 C334 3.451(5) . . no C213 C335 3.562(4) . . no C213 C233 3.540(4) . 3_556 no C114 H134 2.9855 . 6_455 no C114 H316 3.0241 . 7_545 no C215 C314 3.435(5) . 3_556 no C115 H134 3.0943 . 6_455 no C215 C123 3.519(5) . 8_555 no C215 C124 3.508(5) . 8_555 no C116 H126 2.8127 . . no C216 C124 3.389(5) . 8_555 no C216 C123 3.420(5) . 8_555 no C216 C226 3.551(5) . . no C216 C236 3.469(5) . . no C121 H136 2.6915 . . no C121 H312 2.7850 . . no C122 H314 3.0417 . 6_555 no C222 C132 3.540(5) . . no C222 C236 3.223(5) . . no C122 H312 3.0150 . . no C122 H215 3.0370 . 8_554 no C123 H215 3.0286 . 8_554 no C123 H216 2.8526 . 8_554 no C123 H11C 2.9310 . 6_455 no C124 H216 3.0729 . 8_554 no C124 H11C 2.9644 . 6_455 no C125 H133 2.8454 . 6_455 no C125 H333 3.0589 . 8_554 no C126 H133 3.0718 . 6_455 no C226 C216 3.551(5) . . no C126 H136 2.7283 . . no C231 C112 3.534(4) . . no C131 H116 2.7608 . . no C232 C112 3.346(4) . . no C233 C213 3.540(4) . 3_456 no C234 C213 3.515(5) . 3_456 no C234 F1 3.340(4) . 3_456 no C236 C216 3.469(5) . . no C236 C222 3.223(5) . . no C136 H116 2.8109 . . no C211 H226 2.6537 . . no C313 C11 3.468(5) . 6_455 no C213 H335 3.0730 . 5_666 no C213 H234 2.8992 . 3_556 no C213 H233 2.9465 . 3_556 no C214 H335 2.8864 . 5_666 no C314 C215 3.435(5) . 3_456 no C215 H314 3.0857 . 3_556 no C316 C326 3.566(5) . . no C316 C332 3.254(5) . . no C321 C122 3.449(4) . . no C221 H132 2.7552 . . no C221 H236 2.7007 . . no C322 N1 3.450(4) . . no C222 H236 2.7846 . . no C322 C122 3.593(4) . . no C222 H132 2.8629 . . no C322 C336 3.351(5) . . no C324 C134 3.475(5) . 4_655 no C325 C134 3.399(5) . 4_655 no C226 H132 3.0389 . . no C326 C316 3.566(5) . . no C326 C11 3.582(5) . 6_455 no C231 H222 2.9351 . . no C231 H112 3.0374 . . no C331 C212 3.349(4) . . no C231 H216 2.8260 . . no C332 C211 3.554(4) . . no C232 H112 2.6300 . . no C332 C316 3.254(5) . . no C232 H332 2.8699 . . no C332 C212 3.334(4) . . no C333 C213 3.561(5) . . no C334 C213 3.451(5) . . no C234 H11A 2.8191 . 3_456 no C335 C213 3.562(4) . . no C236 H216 2.7526 . . no C336 C322 3.351(5) . . no C236 H222 2.9526 . . no C311 H332 3.0232 . . no C311 H326 2.5922 . . no C311 H232 2.8723 . . no C312 H11C 3.0081 . 6_455 no C312 H112 2.9316 . . no C313 H11C 2.9810 . 6_455 no C314 H215 2.9506 . 3_456 no C315 H115 3.0580 . 7_555 no C316 H326 2.8557 . . no C316 H332 2.9673 . . no C316 H115 2.9749 . 7_555 no C321 H122 2.7698 . . no C321 H336 2.5919 . . no C322 H122 2.7278 . . no C322 H336 2.5936 . . no C326 H11B 3.0277 . 6_455 no C331 H316 2.6892 . . no C331 H212 3.0043 . . no C332 H316 2.6791 . . no C332 H225 2.9589 . 3_456 no C333 H225 2.8702 . 3_456 no C334 H213 3.0964 . 5_666 no C335 H214 3.0628 . 5_666 no C336 H114 3.0941 . 7_555 no H11A F1 2.7905 . . no H11A H234 2.4479 . 3_556 no H11A C234 2.8191 . 3_556 no H11B F3 2.4594 . . no H11B H326 2.4188 . 6_555 no H11B C326 3.0277 . 6_555 no H11C C123 2.9310 . 6_555 no H11C C124 2.9644 . 6_555 no H11C C313 2.9810 . 6_555 no H11C C312 3.0081 . 6_555 no H112 Cu1 3.0497 . . no H112 H312 2.5166 . . no H112 H232 2.4401 . . no H112 C312 2.9316 . . no H112 C231 3.0374 . . no H112 C232 2.6300 . . no H114 C336 3.0941 . 7_545 no H114 H316 2.3376 . 7_545 no H115 C315 3.0580 . 7_545 no H115 C316 2.9749 . 7_545 no H115 F3 2.8010 . 4_645 no H116 C131 2.7608 . . no H116 C136 2.8109 . . no H116 F3 2.7310 . 4_645 no H122 Cu1 3.1055 . . no H122 C322 2.7278 . . no H122 C321 2.7698 . . no H125 H133 2.3685 . 6_455 no H125 H333 2.4127 . 8_554 no H126 C116 2.8127 . . no H126 C111 2.7774 . . no H132 C221 2.7552 . . no H132 N1 2.8825 . . no H132 Cu1 3.1624 . . no H132 C222 2.8629 . . no H132 C226 3.0389 . . no H133 C125 2.8454 . 6_555 no H133 C126 3.0718 . 6_555 no H133 H125 2.3685 . 6_555 no H134 C115 3.0943 . 6_555 no H134 C114 2.9855 . 6_555 no H135 H214 2.4771 . 8_554 no H136 C121 2.6915 . . no H136 C126 2.7283 . . no H136 F2 2.5564 . 4_645 no H212 C331 3.0043 . . no H212 C1 2.9384 . . no H212 Cu1 2.9774 . . no H212 N1 2.5648 . . no H213 H234 2.5045 . 3_556 no H213 C334 3.0964 . 5_666 no H213 H334 2.4574 . 5_666 no H213 F1 2.6207 . . no H214 C335 3.0628 . 5_666 no H214 H335 2.2656 . 5_666 no H214 H135 2.4771 . 8_555 no H215 H314 2.4421 . 3_556 no H215 C122 3.0370 . 8_555 no H215 C123 3.0286 . 8_555 no H215 C314 2.9506 . 3_556 no H216 H236 2.5464 . . no H216 C123 2.8526 . 8_555 no H216 C124 3.0729 . 8_555 no H216 C231 2.8260 . . no H216 C236 2.7526 . . no H222 C231 2.9351 . . no H222 C111 3.0588 . . no H222 C112 3.0472 . . no H222 C236 2.9526 . . no H225 C333 2.8702 . 3_556 no H225 H333 2.4758 . 3_556 no H225 C332 2.9589 . 3_556 no H226 C211 2.6537 . . no H232 C311 2.8723 . . no H232 Cu1 3.2229 . . no H232 H332 2.2858 . . no H232 H112 2.4401 . . no H233 C213 2.9465 . 3_456 no H234 H213 2.5045 . 3_456 no H234 H11A 2.4479 . 3_456 no H234 C213 2.8991 . 3_456 no H234 F1 2.4196 . 3_456 no H236 C222 2.7846 . . no H236 H216 2.5464 . . no H236 C221 2.7007 . . no H312 C122 3.0150 . . no H312 H112 2.5166 . . no H312 C112 3.0997 . . no H312 Cu1 3.2240 . . no H312 P1 3.1019 . . no H312 C121 2.7850 . . no H314 C215 3.0857 . 3_456 no H314 C122 3.0417 . 6_455 no H314 H215 2.4421 . 3_456 no H316 H332 2.5939 . . no H316 C332 2.6791 . . no H316 C331 2.6892 . . no H316 C114 3.0241 . 7_555 no H316 H114 2.3376 . 7_555 no H322 Cu1 3.3587 . . no H322 N1 2.6151 . . no H322 C1 2.7909 . . no H325 F4 2.5289 . 6_455 no H325 F3 2.8538 . 6_455 no H326 C311 2.5922 . . no H326 C316 2.8557 . . no H326 H11B 2.4188 . 6_455 no H332 H316 2.5939 . . no H332 H232 2.2858 . . no H332 C232 2.8699 . . no H332 C311 3.0232 . . no H332 C316 2.9673 . . no H333 C125 3.0589 . 8_555 no H333 H125 2.4127 . 8_555 no H333 H225 2.4758 . 3_456 no H334 F1 2.8096 . 5_666 no H334 H213 2.4574 . 5_666 no H335 F2 2.7781 . . no H335 C213 3.0730 . 5_666 no H335 H214 2.2656 . 5_666 no H335 C214 2.8864 . 5_666 no H336 C321 2.5919 . . no H336 C322 2.5936 . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C11 H11B F3 0.9612 2.4594 3.199(5) 133.61 . yes C212 H212 N1 0.9652 2.5648 3.397(4) 144.52 . yes C234 H234 F1 0.9674 2.4196 3.340(4) 158.73 3_456 yes C322 H322 N1 0.9647 2.6151 3.450(4) 144.95 . yes C325 H325 F4 0.9659 2.5289 3.490(5) 173.44 6_455 yes _exptl_crystal_F_000 4048 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 30 _reflns_number_observed ? _reflns_d_resolution_high .8 _reflns_d_resolution_low 12.063 _diffrn_reflns_av_sigmaI/netI .074 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .079 _refine_ls_wR_factor_all .074 _refine_ls_goodness_of_fit_all 1.011 _refine_ls_shift/su_mean .0004 #========================================================================== data_H450_8 _database_code_depnum_ccdc_archive 'CCDC 268668' # EXPERIMENTAL DATA #--------------------- _chemical_name_systematic ; Tris(triphenylphosphine)(acetonitrile)copper(I) pentafluorosilicate acetonitrile solvate ; _chemical_formula_sum 'C58 H51 Cu1 F5 N2 P3 Si1' _chemical_formula_moiety ? _chemical_formula_weight 1055.6 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 10.485(2) _cell_length_b 13.189(2) _cell_length_c 19.451(4) _cell_angle_alpha 104.136(4) _cell_angle_beta 104.592(4) _cell_angle_gamma 93.839(5) _cell_volume 2500.5(8) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 7325 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 31.65 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .617 _exptl_crystal_description prism _exptl_crystal_size_max .42 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .26 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .91 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 51618 _reflns_number_total 17597 _reflns_Friedel_coverage 0 _reflns_number_gt 14031 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 32.21 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .044 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .043 _refine_ls_wR_factor_ref .055 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_number_reflns 14031 _refine_ls_number_parameters 835 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .01 _refine_diff_density_min -.469 _refine_diff_density_max .788 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 116 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 102 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 2 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 4 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 10 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 6 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' Si ? 0 2 .072 .071 'Int Tables Vol IV Tables 2.2B and 2.3.1' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Cu Cu Uani 0.29581(2) 0.14757(1) 0.25449(1) 1.000 0.0153(1) . . P1 P Uani 0.40152(4) 0.08662(3) 0.35428(2) 1.000 0.0161(1) . . P2 P Uani 0.26213(4) 0.32205(3) 0.26886(2) 1.000 0.0161(1) . . P3 P Uani 0.37041(4) 0.08193(3) 0.15293(2) 1.000 0.0158(1) . . N1 N Uani 0.09829(15) 0.08382(12) 0.23273(8) 1.000 0.0208(4) . . C11 C Uani -0.00396(18) 0.05535(14) 0.23632(10) 1.000 0.0226(5) . . C12 C Uani -0.1329(2) 0.0173(2) 0.24230(16) 1.000 0.0350(7) . . C111 C Uani 0.56170(16) 0.15868(13) 0.41325(9) 1.000 0.0178(4) . . C112 C Uani 0.58349(18) 0.26720(14) 0.42383(9) 1.000 0.0212(4) . . C113 C Uani 0.69762(19) 0.32747(15) 0.47425(10) 1.000 0.0251(5) . . C114 C Uani 0.7918(2) 0.27949(17) 0.51401(11) 1.000 0.0283(5) . . C115 C Uani 0.77167(19) 0.17127(17) 0.50306(11) 1.000 0.0282(5) . . C116 C Uani 0.65744(18) 0.11094(15) 0.45314(10) 1.000 0.0233(5) . . C121 C Uani 0.43620(17) -0.04877(13) 0.32976(9) 1.000 0.0199(4) . . C122 C Uani 0.5323(2) -0.06934(16) 0.29170(10) 1.000 0.0257(5) . . C123 C Uani 0.5591(2) -0.17121(18) 0.26815(11) 1.000 0.0335(6) . . C124 C Uani 0.4889(3) -0.25380(18) 0.28082(13) 1.000 0.0393(6) . . C125 C Uani 0.3948(2) -0.23437(16) 0.31833(13) 1.000 0.0359(6) . . C126 C Uani 0.3678(2) -0.13209(15) 0.34334(11) 1.000 0.0267(5) . . C131 C Uani 0.30489(16) 0.09193(13) 0.42059(9) 1.000 0.0183(4) . . C132 C Uani 0.17409(18) 0.04169(14) 0.39594(10) 1.000 0.0220(4) . . C133 C Uani 0.0915(2) 0.05698(16) 0.44227(11) 1.000 0.0272(5) . . C134 C Uani 0.1395(2) 0.12094(16) 0.51387(11) 1.000 0.0279(5) . . C135 C Uani 0.2706(2) 0.16752(15) 0.53965(10) 1.000 0.0255(5) . . C136 C Uani 0.35321(18) 0.15395(14) 0.49343(9) 1.000 0.0211(4) . . C211 C Uani 0.40732(16) 0.42230(13) 0.30932(9) 1.000 0.0191(4) . . C212 C Uani 0.50215(18) 0.42678(15) 0.27075(11) 1.000 0.0247(5) . . C213 C Uani 0.6211(2) 0.49328(16) 0.30318(13) 1.000 0.0301(5) . . C214 C Uani 0.6476(2) 0.55664(15) 0.37467(13) 1.000 0.0314(5) . . C215 C Uani 0.5540(2) 0.55454(16) 0.41287(12) 1.000 0.0307(5) . . C216 C Uani 0.43388(19) 0.48807(14) 0.38050(10) 1.000 0.0245(5) . . C221 C Uani 0.15119(16) 0.36411(13) 0.32565(9) 1.000 0.0185(4) . . C222 C Uani 0.1388(2) 0.31117(15) 0.37764(10) 1.000 0.0249(5) . . C223 C Uani 0.0544(2) 0.34067(17) 0.42142(11) 1.000 0.0302(5) . . C224 C Uani -0.0183(2) 0.42230(16) 0.41293(11) 1.000 0.0281(5) . . C225 C Uani -0.00555(18) 0.47584(15) 0.36203(11) 1.000 0.0249(5) . . C226 C Uani 0.07897(17) 0.44754(14) 0.31852(10) 1.000 0.0222(4) . . C231 C Uani 0.17813(16) 0.35066(13) 0.18283(9) 1.000 0.0181(4) . . C232 C Uani 0.08177(17) 0.27229(14) 0.13060(9) 1.000 0.0203(4) . . C233 C Uani 0.00801(18) 0.29112(15) 0.06614(10) 1.000 0.0244(5) . . C234 C Uani 0.0309(2) 0.38786(18) 0.05279(11) 1.000 0.0308(6) . . C235 C Uani 0.1274(2) 0.46580(17) 0.10406(12) 1.000 0.0341(6) . . C236 C Uani 0.2010(2) 0.44738(15) 0.16882(11) 1.000 0.0272(5) . . C311 C Uani 0.54096(16) 0.13820(13) 0.16608(9) 1.000 0.0181(4) . . C312 C Uani 0.61360(17) 0.19628(14) 0.23679(10) 1.000 0.0219(4) . . C313 C Uani 0.73891(19) 0.25032(16) 0.24936(11) 1.000 0.0282(5) . . C314 C Uani 0.7933(2) 0.24667(16) 0.19109(13) 1.000 0.0306(5) . . C315 C Uani 0.7231(2) 0.18790(17) 0.12075(12) 1.000 0.0298(6) . . C316 C Uani 0.59805(18) 0.13405(15) 0.10827(10) 1.000 0.0232(4) . . C321 C Uani 0.28500(16) 0.10619(14) 0.06543(9) 1.000 0.0190(4) . . C322 C Uani 0.31497(19) 0.20145(16) 0.05050(11) 1.000 0.0246(5) . . C323 C Uani 0.2451(2) 0.22104(18) -0.01447(12) 1.000 0.0308(6) . . C324 C Uani 0.1427(2) 0.1469(2) -0.06478(12) 1.000 0.0360(6) . . C325 C Uani 0.1113(2) 0.0537(2) -0.04969(11) 1.000 0.0360(6) . . C326 C Uani 0.1822(2) 0.03209(16) 0.01474(10) 1.000 0.0267(5) . . C331 C Uani 0.36419(17) -0.06083(13) 0.12770(9) 1.000 0.0188(4) . . C332 C Uani 0.26590(18) -0.11886(14) 0.14443(10) 1.000 0.0215(4) . . C333 C Uani 0.2533(2) -0.22799(15) 0.12577(11) 1.000 0.0263(5) . . C334 C Uani 0.3387(2) -0.28030(16) 0.09047(12) 1.000 0.0308(6) . . C335 C Uani 0.4362(2) -0.22308(16) 0.07370(12) 1.000 0.0305(6) . . C336 C Uani 0.4497(2) -0.11422(15) 0.09222(10) 1.000 0.0247(5) . . Si Si Uani -0.04556(6) -0.26707(5) 0.25806(3) 1.000 0.0308(2) . . F1 F Uani 0.03651(14) -0.17299(11) 0.23714(9) 1.000 0.0418(4) . . F2 F Uani -0.1299(2) -0.36003(18) 0.27644(14) 1.000 0.0844(9) . . F3 F Uani -0.17607(16) -0.25942(15) 0.19713(10) 1.000 0.0590(6) . . F4 F Uani 0.0552(2) -0.34348(16) 0.23740(18) 1.000 0.0978(12) . . F5 F Uani -0.0198(3) -0.1912(2) 0.33791(10) 1.000 0.0932(9) . . N2 N Uani -0.5295(4) -0.5421(3) 0.0791(2) 1.000 0.0847(14) . . C21 C Uani -0.4193(4) -0.5295(2) 0.08723(17) 1.000 0.0547(10) . . C22 C Uani -0.2769(4) -0.5146(4) 0.0965(3) 1.000 0.0727(14) . . H12A H Uiso -0.135(4) -0.045(3) 0.247(2) 1.000 0.073(11) . . H12B H Uiso -0.200(3) 0.027(2) 0.2046(18) 1.000 0.052(9) . . H12C H Uiso -0.143(4) 0.062(4) 0.280(3) 1.000 0.096(15) . . H112 H Uiso 0.524(2) 0.297(2) 0.4005(13) 1.000 0.027(6) . . H113 H Uiso 0.708(3) 0.399(2) 0.4784(14) 1.000 0.033(6) . . H114 H Uiso 0.870(3) 0.317(2) 0.5477(14) 1.000 0.030(6) . . H115 H Uiso 0.834(3) 0.140(2) 0.5304(15) 1.000 0.038(7) . . H116 H Uiso 0.646(3) 0.038(2) 0.4463(15) 1.000 0.037(7) . . H122 H Uiso 0.579(3) -0.011(2) 0.2825(14) 1.000 0.033(6) . . H123 H Uiso 0.621(3) -0.182(2) 0.2447(15) 1.000 0.034(7) . . H124 H Uiso 0.508(3) -0.325(2) 0.2604(16) 1.000 0.047(8) . . H125 H Uiso 0.346(3) -0.291(2) 0.3284(17) 1.000 0.051(8) . . H126 H Uiso 0.306(2) -0.1193(18) 0.3672(13) 1.000 0.021(5) . . H132 H Uiso 0.139(2) 0.0003(18) 0.3483(13) 1.000 0.022(5) . . H133 H Uiso -0.001(3) 0.021(2) 0.4226(15) 1.000 0.037(7) . . H134 H Uiso 0.083(3) 0.134(2) 0.5460(15) 1.000 0.034(7) . . H135 H Uiso 0.305(2) 0.209(2) 0.5860(14) 1.000 0.026(6) . . H136 H Uiso 0.441(2) 0.1859(18) 0.5101(13) 1.000 0.023(6) . . H212 H Uiso 0.484(2) 0.382(2) 0.2248(14) 1.000 0.026(6) . . H213 H Uiso 0.685(3) 0.491(2) 0.2765(15) 1.000 0.040(7) . . H214 H Uiso 0.723(3) 0.598(2) 0.3956(15) 1.000 0.036(7) . . H215 H Uiso 0.571(3) 0.596(2) 0.4598(18) 1.000 0.052(8) . . H216 H Uiso 0.370(2) 0.4878(19) 0.4073(13) 1.000 0.027(6) . . H222 H Uiso 0.186(2) 0.2507(19) 0.3805(13) 1.000 0.024(6) . . H223 H Uiso 0.045(3) 0.303(2) 0.4529(15) 1.000 0.034(7) . . H224 H Uiso -0.074(3) 0.439(2) 0.4416(15) 1.000 0.036(7) . . H225 H Uiso -0.051(3) 0.528(2) 0.3576(16) 1.000 0.047(8) . . H226 H Uiso 0.086(3) 0.482(2) 0.2843(14) 1.000 0.033(6) . . H232 H Uiso 0.066(3) 0.205(2) 0.1370(14) 1.000 0.034(7) . . H233 H Uiso -0.059(2) 0.240(2) 0.0294(13) 1.000 0.027(6) . . H234 H Uiso -0.015(3) 0.400(2) 0.0084(15) 1.000 0.036(7) . . H235 H Uiso 0.146(3) 0.534(3) 0.0940(17) 1.000 0.054(9) . . H236 H Uiso 0.275(3) 0.506(2) 0.2068(14) 1.000 0.035(7) . . H312 H Uiso 0.577(2) 0.1993(19) 0.2761(14) 1.000 0.027(6) . . H313 H Uiso 0.784(2) 0.286(2) 0.2944(14) 1.000 0.029(6) . . H314 H Uiso 0.880(3) 0.282(2) 0.1994(14) 1.000 0.036(7) . . H315 H Uiso 0.756(3) 0.188(2) 0.0788(15) 1.000 0.040(7) . . H316 H Uiso 0.553(2) 0.096(2) 0.0623(14) 1.000 0.031(6) . . H322 H Uiso 0.380(3) 0.253(2) 0.0845(15) 1.000 0.036(7) . . H323 H Uiso 0.267(2) 0.288(2) -0.0234(14) 1.000 0.030(6) . . H324 H Uiso 0.090(3) 0.160(2) -0.1099(17) 1.000 0.049(8) . . H325 H Uiso 0.037(3) 0.003(2) -0.0835(15) 1.000 0.036(7) . . H326 H Uiso 0.157(3) -0.031(2) 0.0251(14) 1.000 0.032(6) . . H332 H Uiso 0.208(3) -0.081(2) 0.1681(14) 1.000 0.031(6) . . H333 H Uiso 0.189(3) -0.261(2) 0.1378(14) 1.000 0.033(7) . . H334 H Uiso 0.336(2) -0.354(2) 0.0789(14) 1.000 0.031(6) . . H335 H Uiso 0.498(3) -0.260(2) 0.0523(16) 1.000 0.043(8) . . H336 H Uiso 0.519(2) -0.0743(19) 0.0835(13) 1.000 0.026(6) . . H22A H Uiso -0.246(5) -0.577(4) 0.079(3) 1.000 0.122(19) . . H22B H Uiso -0.240(5) -0.483(4) 0.142(3) 1.000 0.110(18) . . H22C H Uiso -0.271(5) -0.474(4) 0.058(3) 1.000 0.13(2) . . 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 Cu 0.0175(1) 0.0143(1) 0.0145(1) 0.0044(1) 0.0046(1) 0.0029(1) P1 0.0183(2) 0.0155(2) 0.0149(2) 0.0054(1) 0.0037(1) 0.0027(1) P2 0.0179(2) 0.0140(2) 0.0166(2) 0.0044(1) 0.0044(1) 0.0031(1) P3 0.0173(2) 0.0158(2) 0.0138(2) 0.0031(1) 0.0048(1) 0.0015(1) N1 0.0210(6) 0.0215(7) 0.0213(6) 0.0088(5) 0.0053(5) 0.0035(5) C11 0.0230(8) 0.0210(8) 0.0252(8) 0.0090(6) 0.0058(6) 0.0049(6) C12 0.0234(9) 0.0348(11) 0.0560(14) 0.0225(11) 0.0167(9) 0.0059(8) C111 0.0193(7) 0.0186(7) 0.0163(6) 0.0065(6) 0.0045(5) 0.0028(6) C112 0.0246(8) 0.0191(7) 0.0201(7) 0.0063(6) 0.0051(6) 0.0042(6) C113 0.0275(8) 0.0191(8) 0.0266(8) 0.0041(7) 0.0071(7) -0.0011(6) C114 0.0233(8) 0.0312(10) 0.0265(8) 0.0066(7) 0.0028(7) -0.0035(7) C115 0.0205(8) 0.0313(10) 0.0311(9) 0.0130(8) 0.0003(7) 0.0018(7) C116 0.0219(8) 0.0217(8) 0.0259(8) 0.0105(7) 0.0020(6) 0.0025(6) C121 0.0243(7) 0.0181(7) 0.0150(6) 0.0040(6) 0.0015(5) 0.0052(6) C122 0.0291(9) 0.0252(9) 0.0224(8) 0.0061(7) 0.0055(7) 0.0095(7) C123 0.0373(11) 0.0342(11) 0.0260(9) 0.0035(8) 0.0041(8) 0.0194(9) C124 0.0510(13) 0.0248(10) 0.0327(10) 0.0029(8) -0.0032(9) 0.0167(9) C125 0.0461(12) 0.0193(9) 0.0372(11) 0.0089(8) 0.0011(9) 0.0049(8) C126 0.0333(9) 0.0201(8) 0.0257(8) 0.0077(7) 0.0047(7) 0.0036(7) C131 0.0219(7) 0.0177(7) 0.0179(7) 0.0092(6) 0.0053(5) 0.0040(6) C132 0.0240(8) 0.0231(8) 0.0195(7) 0.0093(6) 0.0046(6) -0.0004(6) C133 0.0241(8) 0.0316(10) 0.0305(9) 0.0153(8) 0.0097(7) 0.0015(7) C134 0.0337(10) 0.0288(9) 0.0290(9) 0.0130(7) 0.0166(8) 0.0072(8) C135 0.0368(10) 0.0219(8) 0.0203(8) 0.0059(6) 0.0117(7) 0.0063(7) C136 0.0254(8) 0.0194(8) 0.0181(7) 0.0057(6) 0.0050(6) 0.0026(6) C211 0.0202(7) 0.0146(7) 0.0213(7) 0.0055(6) 0.0026(6) 0.0035(5) C212 0.0238(8) 0.0222(8) 0.0277(8) 0.0056(7) 0.0076(7) 0.0031(6) C213 0.0226(8) 0.0232(9) 0.0440(11) 0.0088(8) 0.0093(8) 0.0013(7) C214 0.0224(8) 0.0188(8) 0.0457(11) 0.0058(8) 0.0003(8) -0.0005(7) C215 0.0304(9) 0.0196(8) 0.0325(10) -0.0005(7) -0.0002(7) 0.0010(7) C216 0.0265(8) 0.0193(8) 0.0240(8) 0.0022(6) 0.0040(6) 0.0028(6) C221 0.0190(7) 0.0162(7) 0.0190(7) 0.0027(6) 0.0050(5) 0.0021(5) C222 0.0303(9) 0.0254(9) 0.0234(8) 0.0097(7) 0.0111(7) 0.0082(7) C223 0.0375(10) 0.0333(10) 0.0248(8) 0.0095(8) 0.0153(8) 0.0071(8) C224 0.0245(8) 0.0306(10) 0.0256(8) -0.0020(7) 0.0102(7) 0.0020(7) C225 0.0212(8) 0.0211(8) 0.0293(8) 0.0011(7) 0.0063(6) 0.0051(6) C226 0.0225(8) 0.0185(7) 0.0268(8) 0.0068(6) 0.0077(6) 0.0047(6) C231 0.0193(7) 0.0186(7) 0.0182(7) 0.0071(6) 0.0059(5) 0.0045(6) C232 0.0210(7) 0.0203(8) 0.0207(7) 0.0075(6) 0.0057(6) 0.0024(6) C233 0.0213(8) 0.0280(9) 0.0230(8) 0.0090(7) 0.0030(6) 0.0016(7) C234 0.0308(9) 0.0362(11) 0.0267(9) 0.0175(8) 0.0013(7) 0.0051(8) C235 0.0387(11) 0.0273(10) 0.0352(10) 0.0192(8) -0.0007(8) 0.0000(8) C236 0.0313(9) 0.0211(8) 0.0274(8) 0.0111(7) 0.0011(7) 0.0011(7) C311 0.0175(7) 0.0180(7) 0.0177(7) 0.0032(6) 0.0050(5) 0.0015(5) C312 0.0212(7) 0.0210(8) 0.0206(7) 0.0015(6) 0.0047(6) 0.0019(6) C313 0.0219(8) 0.0248(9) 0.0301(9) -0.0002(7) 0.0017(7) -0.0008(7) C314 0.0207(8) 0.0271(9) 0.0418(11) 0.0054(8) 0.0096(7) -0.0012(7) C315 0.0258(9) 0.0318(10) 0.0360(10) 0.0094(8) 0.0164(8) 0.0007(7) C316 0.0214(7) 0.0266(9) 0.0211(7) 0.0033(6) 0.0090(6) -0.0009(6) C321 0.0201(7) 0.0227(8) 0.0149(6) 0.0048(6) 0.0063(5) 0.0032(6) C322 0.0244(8) 0.0270(9) 0.0258(8) 0.0119(7) 0.0084(6) 0.0038(7) C323 0.0328(10) 0.0383(11) 0.0323(9) 0.0222(9) 0.0141(8) 0.0124(8) C324 0.0381(11) 0.0513(13) 0.0239(9) 0.0183(9) 0.0077(8) 0.0155(10) C325 0.0352(11) 0.0444(12) 0.0206(8) 0.0057(8) -0.0030(7) 0.0043(9) C326 0.0290(9) 0.0267(9) 0.0193(7) 0.0043(7) 0.0007(6) 0.0000(7) C331 0.0228(7) 0.0171(7) 0.0149(6) 0.0021(5) 0.0047(5) 0.0016(6) C332 0.0224(7) 0.0194(8) 0.0213(7) 0.0037(6) 0.0058(6) 0.0014(6) C333 0.0291(9) 0.0194(8) 0.0289(9) 0.0057(7) 0.0076(7) -0.0017(7) C334 0.0408(11) 0.0177(8) 0.0321(10) 0.0027(7) 0.0109(8) 0.0041(7) C335 0.0407(11) 0.0223(9) 0.0316(9) 0.0041(7) 0.0174(8) 0.0098(8) C336 0.0299(9) 0.0229(8) 0.0236(8) 0.0044(7) 0.0132(7) 0.0045(7) Si 0.0311(3) 0.0272(3) 0.0326(3) 0.0103(2) 0.0044(2) 0.0032(2) F1 0.0397(7) 0.0369(7) 0.0536(8) 0.0204(6) 0.0140(6) 0.0034(6) F2 0.0618(12) 0.0897(15) 0.1152(18) 0.0770(14) 0.0071(11) -0.0147(10) F3 0.0435(8) 0.0679(11) 0.0584(10) 0.0299(9) -0.0076(7) -0.0050(8) F4 0.0784(14) 0.0448(11) 0.192(3) 0.0396(14) 0.0624(17) 0.0332(10) F5 0.1048(18) 0.120(2) 0.0355(9) -0.0105(10) 0.0271(10) -0.0287(15) N2 0.081(2) 0.081(2) 0.102(3) 0.030(2) 0.041(2) -0.0021(18) C21 0.072(2) 0.0385(14) 0.0553(16) 0.0086(12) 0.0273(15) -0.0024(13) C22 0.067(2) 0.061(2) 0.076(3) -0.003(2) 0.018(2) -0.0009(18) #=============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu P1 2.3323(6) . . yes Cu P2 2.3115(7) . . yes Cu P3 2.3016(6) . . yes Cu N1 2.0800(17) . . yes P1 C111 1.8228(18) . . yes P1 C121 1.8184(19) . . yes P1 C131 1.8218(18) . . yes P2 C211 1.8176(18) . . yes P2 C221 1.8208(18) . . yes P2 C231 1.8244(18) . . yes P3 C311 1.8202(18) . . yes P3 C321 1.8269(18) . . yes P3 C331 1.8183(18) . . yes Si F5 1.575(2) . . yes Si F2 1.625(3) . . yes Si F3 1.5959(19) . . yes Si F1 1.6510(17) . . yes Si F4 1.566(2) . . yes N1 C11 1.137(3) . . yes N2 C21 1.121(6) . . yes C11 C12 1.453(3) . . no C111 C112 1.390(3) . . no C111 C116 1.392(3) . . no C12 H12B 0.92(3) . . no C112 C113 1.388(3) . . no C12 H12A 0.85(4) . . no C12 H12C 0.86(5) . . no C113 C114 1.383(3) . . no C114 C115 1.384(3) . . no C115 C116 1.385(3) . . no C121 C126 1.387(3) . . no C121 C122 1.397(3) . . no C122 C123 1.382(3) . . no C123 C124 1.380(4) . . no C124 C125 1.370(4) . . no C125 C126 1.392(3) . . no C131 C132 1.393(3) . . no C131 C136 1.396(2) . . no C132 C133 1.389(3) . . no C133 C134 1.386(3) . . no C134 C135 1.381(3) . . no C135 C136 1.387(3) . . no C211 C216 1.391(2) . . no C211 C212 1.394(3) . . no C112 H112 0.85(2) . . no C212 C213 1.382(3) . . no C213 C214 1.384(3) . . no C113 H113 0.92(3) . . no C114 H114 0.93(3) . . no C214 C215 1.375(3) . . no C215 C216 1.391(3) . . no C115 H115 0.92(3) . . no C116 H116 0.93(3) . . no C221 C222 1.388(3) . . no C221 C226 1.392(3) . . no C122 H122 0.96(3) . . no C222 C223 1.387(3) . . no C223 C224 1.379(3) . . no C123 H123 0.88(3) . . no C224 C225 1.376(3) . . no C124 H124 0.98(3) . . no C225 C226 1.382(3) . . no C125 H125 0.96(3) . . no C126 H126 0.89(2) . . no C231 C232 1.397(2) . . no C231 C236 1.386(3) . . no C132 H132 0.92(2) . . no C232 C233 1.386(3) . . no C233 C234 1.380(3) . . no C133 H133 0.99(3) . . no C134 H134 0.96(3) . . no C234 C235 1.388(3) . . no C235 C236 1.388(3) . . no C135 H135 0.90(3) . . no C136 H136 0.93(2) . . no C311 C316 1.393(3) . . no C311 C312 1.392(2) . . no C312 C313 1.386(3) . . no C212 H212 0.91(3) . . no C213 H213 0.94(3) . . no C313 C314 1.384(3) . . no C214 H214 0.87(3) . . no C314 C315 1.383(3) . . no C215 H215 0.91(3) . . no C315 C316 1.383(3) . . no C216 H216 0.95(2) . . no C321 C322 1.390(3) . . no C321 C326 1.393(3) . . no C322 C323 1.385(3) . . no C222 H222 0.97(2) . . no C323 C324 1.389(3) . . no C223 H223 0.90(3) . . no C224 H224 0.91(3) . . no C324 C325 1.370(4) . . no C225 H225 0.87(3) . . no C325 C326 1.392(3) . . no C226 H226 0.91(3) . . no C331 C332 1.392(3) . . no C331 C336 1.391(3) . . no C332 C333 1.384(3) . . no C232 H232 0.94(3) . . no C333 C334 1.382(3) . . no C233 H233 0.95(2) . . no C234 H234 0.93(3) . . no C334 C335 1.381(3) . . no C235 H235 0.98(4) . . no C335 C336 1.380(3) . . no C236 H236 1.05(3) . . no C312 H312 0.93(2) . . no C313 H313 0.88(3) . . no C314 H314 0.95(3) . . no C315 H315 0.96(3) . . no C316 H316 0.90(3) . . no C21 C22 1.452(6) . . no C322 H322 0.92(3) . . no C323 H323 0.96(3) . . no C324 H324 0.97(3) . . no C325 H325 0.97(3) . . no C326 H326 0.94(3) . . no C332 H332 0.95(3) . . no C333 H333 0.89(3) . . no C334 H334 0.94(3) . . no C335 H335 0.95(3) . . no C336 H336 0.94(2) . . no C22 H22A 0.92(5) . . no C22 H22B 0.86(6) . . no C22 H22C 1.03(6) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Cu P2 121.66(2) . . . yes P1 Cu P3 111.57(2) . . . yes P1 Cu N1 102.43(4) . . . yes P2 Cu P3 112.35(2) . . . yes P2 Cu N1 97.40(5) . . . yes P3 Cu N1 109.20(4) . . . yes Cu P1 C111 117.71(6) . . . yes Cu P1 C121 114.71(6) . . . yes Cu P1 C131 112.41(6) . . . yes C111 P1 C121 103.04(8) . . . yes C111 P1 C131 101.66(8) . . . yes C121 P1 C131 105.78(8) . . . yes Cu P2 C211 117.69(6) . . . yes Cu P2 C221 113.97(6) . . . yes Cu P2 C231 113.54(6) . . . yes C211 P2 C221 103.59(8) . . . yes C211 P2 C231 104.59(8) . . . yes C221 P2 C231 101.69(8) . . . yes Cu P3 C311 111.97(6) . . . yes Cu P3 C321 118.41(6) . . . yes Cu P3 C331 113.90(6) . . . yes C311 P3 C321 101.80(8) . . . yes C311 P3 C331 107.20(8) . . . yes C321 P3 C331 102.22(8) . . . yes F1 Si F5 88.20(12) . . . yes F2 Si F3 88.85(11) . . . yes F2 Si F4 90.73(12) . . . yes F2 Si F5 92.90(14) . . . yes F3 Si F4 120.69(14) . . . yes F3 Si F5 117.28(13) . . . yes F4 Si F5 121.96(16) . . . yes F1 Si F4 89.79(11) . . . yes F1 Si F2 178.30(11) . . . yes F1 Si F3 89.49(9) . . . yes Cu N1 C11 165.78(14) . . . yes N1 C11 C12 178.4(2) . . . yes P1 C111 C116 122.48(14) . . . yes P1 C111 C112 118.34(13) . . . yes C112 C111 C116 118.91(16) . . . no C11 C12 H12B 110(2) . . . no C11 C12 H12C 104(3) . . . no H12A C12 H12C 113(4) . . . no C11 C12 H12A 111(3) . . . no H12A C12 H12B 115(3) . . . no C111 C112 C113 120.70(17) . . . no H12B C12 H12C 102(4) . . . no C112 C113 C114 120.00(19) . . . no C113 C114 C115 119.64(19) . . . no C114 C115 C116 120.5(2) . . . no C111 C116 C115 120.22(19) . . . no P1 C121 C122 117.31(14) . . . yes P1 C121 C126 123.54(15) . . . yes C122 C121 C126 119.06(18) . . . no C121 C122 C123 120.45(19) . . . no C122 C123 C124 120.1(2) . . . no C123 C124 C125 119.9(2) . . . no C124 C125 C126 120.8(2) . . . no C121 C126 C125 119.72(19) . . . no C132 C131 C136 118.98(16) . . . no P1 C131 C136 121.78(14) . . . yes P1 C131 C132 118.89(13) . . . yes C131 C132 C133 120.35(17) . . . no C132 C133 C134 120.14(19) . . . no C133 C134 C135 119.82(19) . . . no C134 C135 C136 120.39(17) . . . no C131 C136 C135 120.23(17) . . . no P2 C211 C212 119.00(13) . . . yes C212 C211 C216 118.48(17) . . . no P2 C211 C216 122.22(14) . . . yes C211 C212 C213 120.73(19) . . . no C111 C112 H112 119.2(17) . . . no C113 C112 H112 120.0(17) . . . no C212 C213 C214 120.2(2) . . . no C114 C113 H113 122.8(18) . . . no C112 C113 H113 117.2(18) . . . no C113 C114 H114 122.5(17) . . . no C213 C214 C215 119.7(2) . . . no C115 C114 H114 117.8(17) . . . no C214 C215 C216 120.4(2) . . . no C116 C115 H115 120.3(18) . . . no C114 C115 H115 119.2(18) . . . no C111 C116 H116 120.6(18) . . . no C115 C116 H116 119.2(19) . . . no C211 C216 C215 120.45(18) . . . no P2 C221 C222 118.74(14) . . . yes P2 C221 C226 122.03(13) . . . yes C222 C221 C226 119.23(17) . . . no C123 C122 H122 121.2(17) . . . no C221 C222 C223 120.22(19) . . . no C121 C122 H122 118.4(17) . . . no C124 C123 H123 121.3(18) . . . no C122 C123 H123 118.7(18) . . . no C222 C223 C224 120.0(2) . . . no C123 C124 H124 116.8(18) . . . no C125 C124 H124 123.2(18) . . . no C223 C224 C225 120.15(19) . . . no C124 C125 H125 121.0(19) . . . no C224 C225 C226 120.32(19) . . . no C126 C125 H125 118.2(19) . . . no C221 C226 C225 120.10(17) . . . no C125 C126 H126 121.0(16) . . . no C121 C126 H126 119.3(16) . . . no P2 C231 C232 117.69(13) . . . yes P2 C231 C236 123.14(14) . . . yes C232 C231 C236 119.09(16) . . . no C133 C132 H132 118.3(14) . . . no C231 C232 C233 120.74(17) . . . no C131 C132 H132 121.3(14) . . . no C132 C133 H133 118.0(17) . . . no C134 C133 H133 121.8(17) . . . no C232 C233 C234 119.79(18) . . . no C133 C134 H134 121.1(17) . . . no C135 C134 H134 119.1(18) . . . no C233 C234 C235 119.82(19) . . . no C134 C135 H135 122.0(14) . . . no C234 C235 C236 120.5(2) . . . no C136 C135 H135 117.6(14) . . . no C131 C136 H136 118.9(14) . . . no C231 C236 C235 120.01(19) . . . no C135 C136 H136 120.9(14) . . . no P3 C311 C312 117.93(13) . . . yes P3 C311 C316 123.37(13) . . . yes C312 C311 C316 118.45(16) . . . no C213 C212 H212 122.0(15) . . . no C311 C312 C313 120.93(17) . . . no C211 C212 H212 117.2(15) . . . no C214 C213 H213 121.4(17) . . . no C312 C313 C314 119.86(19) . . . no C212 C213 H213 118.3(17) . . . no C213 C214 H214 120.6(19) . . . no C215 C214 H214 119.8(19) . . . no C313 C314 C315 119.8(2) . . . no C216 C215 H215 120(2) . . . no C214 C215 H215 120(2) . . . no C314 C315 C316 120.3(2) . . . no C211 C216 H216 120.0(14) . . . no C215 C216 H216 119.5(15) . . . no C311 C316 C315 120.67(17) . . . no P3 C321 C326 120.22(15) . . . yes P3 C321 C322 120.72(14) . . . yes C322 C321 C326 118.91(17) . . . no C321 C322 C323 120.25(19) . . . no C223 C222 H222 121.0(14) . . . no C221 C222 H222 118.7(14) . . . no C222 C223 H223 118(2) . . . no C322 C323 C324 120.6(2) . . . no C224 C223 H223 122(2) . . . no C225 C224 H224 121.8(18) . . . no C323 C324 C325 119.4(2) . . . no C223 C224 H224 118.1(18) . . . no C226 C225 H225 120(2) . . . no C224 C225 H225 119(2) . . . no C324 C325 C326 120.7(2) . . . no C221 C226 H226 119.6(19) . . . no C225 C226 H226 120.3(19) . . . no C321 C326 C325 120.2(2) . . . no P3 C331 C332 117.04(14) . . . yes P3 C331 C336 123.98(14) . . . yes C332 C331 C336 118.97(17) . . . no C233 C232 H232 117.5(17) . . . no C331 C332 C333 120.45(18) . . . no C231 C232 H232 121.7(17) . . . no C232 C233 H233 123.3(16) . . . no C234 C233 H233 116.9(16) . . . no C332 C333 C334 120.14(19) . . . no C333 C334 C335 119.6(2) . . . no C233 C234 H234 120.4(17) . . . no C235 C234 H234 119.7(18) . . . no C334 C335 C336 120.7(2) . . . no C234 C235 H235 120.0(18) . . . no C236 C235 H235 119.4(18) . . . no C331 C336 C335 120.17(19) . . . no C231 C236 H236 119.8(15) . . . no C235 C236 H236 120.2(14) . . . no C313 C312 H312 119.6(15) . . . no C311 C312 H312 119.4(15) . . . no C312 C313 H313 119.9(15) . . . no C314 C313 H313 120.2(15) . . . no C313 C314 H314 120.4(16) . . . no C315 C314 H314 119.7(16) . . . no C316 C315 H315 118.2(18) . . . no C314 C315 H315 121.4(18) . . . no C311 C316 H316 119.6(15) . . . no C315 C316 H316 119.7(15) . . . no N2 C21 C22 179.0(4) . . . yes C323 C322 H322 119.5(17) . . . no C321 C322 H322 120.2(17) . . . no C324 C323 H323 120.6(15) . . . no C322 C323 H323 118.8(15) . . . no C323 C324 H324 122.0(17) . . . no C325 C324 H324 118.6(17) . . . no C326 C325 H325 119.5(17) . . . no C324 C325 H325 119.7(17) . . . no C321 C326 H326 120.2(17) . . . no C325 C326 H326 119.5(17) . . . no C331 C332 H332 117.6(17) . . . no C333 C332 H332 121.9(17) . . . no C332 C333 H333 116.7(19) . . . no C334 C333 H333 123.2(19) . . . no C335 C334 H334 117.6(14) . . . no C333 C334 H334 122.7(14) . . . no C336 C335 H335 120.6(17) . . . no C334 C335 H335 118.6(17) . . . no C331 C336 H336 118.5(15) . . . no C335 C336 H336 121.3(15) . . . no C21 C22 H22A 112(3) . . . no C21 C22 H22B 107(4) . . . no C21 C22 H22C 102(3) . . . no H22A C22 H22B 115(5) . . . no H22A C22 H22C 103(5) . . . no H22B C22 H22C 118(5) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Cu P1 C111 -51.40(7) . . . . no P2 Cu P1 C121 -172.89(7) . . . . no P2 Cu P1 C131 66.22(7) . . . . no P3 Cu P1 C111 85.01(7) . . . . no P3 Cu P1 C121 -36.48(7) . . . . no P3 Cu P1 C131 -157.38(6) . . . . no N1 Cu P1 C111 -158.30(8) . . . . no N1 Cu P1 C121 80.21(8) . . . . no N1 Cu P1 C131 -40.69(8) . . . . no P1 Cu P2 C211 57.15(7) . . . . no P1 Cu P2 C221 -64.44(6) . . . . no P1 Cu P2 C231 179.74(6) . . . . no P3 Cu P2 C211 -78.95(6) . . . . no P3 Cu P2 C221 159.46(6) . . . . no P3 Cu P2 C231 43.64(7) . . . . no N1 Cu P2 C211 166.72(7) . . . . no N1 Cu P2 C221 45.13(7) . . . . no N1 Cu P2 C231 -70.68(8) . . . . no P1 Cu P3 C311 -69.88(6) . . . . no P1 Cu P3 C321 172.16(7) . . . . no P1 Cu P3 C331 51.97(7) . . . . no P2 Cu P3 C311 70.73(6) . . . . no P2 Cu P3 C321 -47.23(7) . . . . no P2 Cu P3 C331 -167.43(6) . . . . no N1 Cu P3 C311 177.62(8) . . . . no N1 Cu P3 C321 59.66(8) . . . . no N1 Cu P3 C331 -60.53(8) . . . . no Cu P1 C111 C112 33.15(16) . . . . no Cu P1 C111 C116 -152.91(13) . . . . no C121 P1 C111 C112 160.48(14) . . . . no C121 P1 C111 C116 -25.58(17) . . . . no C131 P1 C111 C112 -90.08(15) . . . . no C131 P1 C111 C116 83.86(16) . . . . no Cu P1 C121 C122 68.70(15) . . . . no Cu P1 C121 C126 -107.75(15) . . . . no C111 P1 C121 C122 -60.50(15) . . . . no C111 P1 C121 C126 123.05(16) . . . . no C131 P1 C121 C122 -166.82(14) . . . . no C131 P1 C121 C126 16.73(18) . . . . no Cu P1 C131 C132 54.79(16) . . . . no Cu P1 C131 C136 -118.31(14) . . . . no C111 P1 C131 C132 -178.44(15) . . . . no C111 P1 C131 C136 8.46(17) . . . . no C121 P1 C131 C132 -71.11(16) . . . . no C121 P1 C131 C136 115.79(16) . . . . no Cu P2 C211 C212 65.84(16) . . . . no Cu P2 C211 C216 -107.71(15) . . . . no C221 P2 C211 C212 -167.37(15) . . . . no C221 P2 C211 C216 19.08(17) . . . . no C231 P2 C211 C212 -61.22(16) . . . . no C231 P2 C211 C216 125.24(16) . . . . no Cu P2 C221 C222 25.33(16) . . . . no Cu P2 C221 C226 -154.78(13) . . . . no C211 P2 C221 C222 -103.77(15) . . . . no C211 P2 C221 C226 76.13(16) . . . . no C231 P2 C221 C222 147.89(15) . . . . no C231 P2 C221 C226 -32.21(17) . . . . no Cu P2 C231 C232 34.84(16) . . . . no Cu P2 C231 C236 -148.35(15) . . . . no C211 P2 C231 C232 164.41(14) . . . . no C211 P2 C231 C236 -18.78(18) . . . . no C221 P2 C231 C232 -88.03(15) . . . . no C221 P2 C231 C236 88.79(17) . . . . no Cu P3 C311 C312 11.40(16) . . . . no Cu P3 C311 C316 -162.72(14) . . . . no C321 P3 C311 C312 138.87(15) . . . . no C321 P3 C311 C316 -35.25(18) . . . . no C331 P3 C311 C312 -114.20(15) . . . . no C331 P3 C311 C316 71.68(17) . . . . no Cu P3 C321 C322 82.04(16) . . . . no Cu P3 C321 C326 -93.51(16) . . . . no C311 P3 C321 C322 -41.16(17) . . . . no C311 P3 C321 C326 143.29(16) . . . . no C331 P3 C321 C322 -151.92(16) . . . . no C331 P3 C321 C326 32.53(17) . . . . no Cu P3 C331 C332 29.39(15) . . . . no Cu P3 C331 C336 -151.58(14) . . . . no C311 P3 C331 C332 153.84(14) . . . . no C311 P3 C331 C336 -27.14(17) . . . . no C321 P3 C331 C332 -99.54(15) . . . . no C321 P3 C331 C336 79.49(17) . . . . no P2 C211 C212 C213 -172.30(16) . . . . no C216 C211 C212 C213 1.5(3) . . . . no P2 C211 C216 C215 171.87(15) . . . . no C212 C211 C216 C215 -1.7(3) . . . . no P1 C111 C116 H116 7(2) . . . . no C112 C111 C116 H116 -179(2) . . . . no P1 C111 C112 H112 -4.0(18) . . . . no C116 C111 C112 H112 -178.1(18) . . . . no C111 C112 C113 H113 179(2) . . . . no C211 C212 C213 C214 -0.1(3) . . . . no H112 C112 C113 C114 177.7(18) . . . . no H112 C112 C113 H113 -4(3) . . . . no C112 C113 C114 H114 179(2) . . . . no C212 C213 C214 C215 -1.2(3) . . . . no H113 C113 C114 C115 -178(2) . . . . no H113 C113 C114 H114 1(3) . . . . no C113 C114 C115 H115 -179(2) . . . . no H114 C114 C115 H115 2(3) . . . . no C213 C214 C215 C216 0.9(3) . . . . no H114 C114 C115 C116 -180(2) . . . . no H115 C115 C116 C111 178(2) . . . . no C114 C115 C116 H116 180(2) . . . . no C214 C215 C216 C211 0.5(3) . . . . no H115 C115 C116 H116 -2(3) . . . . no P2 C221 C222 C223 -179.52(15) . . . . no C226 C221 C222 C223 0.6(3) . . . . no C222 C221 C226 C225 -1.0(3) . . . . no C126 C121 C122 H122 179.9(18) . . . . no P1 C121 C126 H126 -3.0(17) . . . . no C122 C121 C126 H126 -179.4(17) . . . . no P1 C121 C122 H122 3.3(19) . . . . no P2 C221 C226 C225 179.06(14) . . . . no H122 C122 C123 C124 -178.8(19) . . . . no C121 C122 C123 H123 -179(2) . . . . no C221 C222 C223 C224 0.5(3) . . . . no H122 C122 C123 H123 1(3) . . . . no C222 C223 C224 C225 -1.2(3) . . . . no C122 C123 C124 H124 176(2) . . . . no H123 C123 C124 C125 179(2) . . . . no H123 C123 C124 H124 -3(3) . . . . no H124 C124 C125 H125 3(3) . . . . no H124 C124 C125 C126 -177(2) . . . . no C223 C224 C225 C226 0.7(3) . . . . no C123 C124 C125 H125 -179(2) . . . . no H125 C125 C126 H126 -1(3) . . . . no C224 C225 C226 C221 0.4(3) . . . . no C124 C125 C126 H126 179.2(17) . . . . no H125 C125 C126 C121 -180(2) . . . . no C236 C231 C232 C233 -1.2(3) . . . . no P2 C231 C236 C235 -175.92(16) . . . . no C232 C231 C236 C235 0.8(3) . . . . no C132 C131 C136 H136 178.4(17) . . . . no P1 C131 C136 H136 -8.5(17) . . . . no C136 C131 C132 H132 179.9(18) . . . . no P2 C231 C232 C233 175.79(14) . . . . no P1 C131 C132 H132 6.6(18) . . . . no H132 C132 C133 C134 -178.4(18) . . . . no H132 C132 C133 H133 2(3) . . . . no C231 C232 C233 C234 0.8(3) . . . . no C131 C132 C133 H133 179.0(19) . . . . no H133 C133 C134 C135 178.3(19) . . . . no C132 C133 C134 H134 178(2) . . . . no C232 C233 C234 C235 -0.2(3) . . . . no H133 C133 C134 H134 -2(3) . . . . no C233 C234 C235 C236 -0.1(3) . . . . no C133 C134 C135 H135 -179(2) . . . . no H134 C134 C135 C136 -177.1(19) . . . . no H134 C134 C135 H135 1(3) . . . . no C134 C135 C136 H136 179.0(17) . . . . no H135 C135 C136 C131 -179.0(19) . . . . no H135 C135 C136 H136 1(3) . . . . no C234 C235 C236 C231 -0.2(3) . . . . no P3 C311 C312 H312 6.1(18) . . . . no C316 C311 C312 H312 -179.5(18) . . . . no P3 C311 C316 H316 -7(2) . . . . no C312 C311 C316 H316 179(2) . . . . no C311 C312 C313 H313 -179(2) . . . . no H312 C312 C313 C314 -179.6(18) . . . . no H312 C312 C313 H313 1(3) . . . . no C312 C313 C314 H314 -178(2) . . . . no H313 C313 C314 C315 178(2) . . . . no H313 C313 C314 H314 1(3) . . . . no C313 C314 C315 H315 176(2) . . . . no H314 C314 C315 C316 178.5(19) . . . . no H314 C314 C315 H315 -7(3) . . . . no C314 C315 C316 H316 180.0(19) . . . . no H315 C315 C316 C311 -174.8(19) . . . . no H315 C315 C316 H316 5(3) . . . . no P3 C321 C322 H322 1(2) . . . . no C326 C321 C322 H322 177(2) . . . . no P3 C321 C326 H326 -1(2) . . . . no C322 C321 C326 H326 -176(2) . . . . no C321 C322 C323 H323 179.3(16) . . . . no H322 C322 C323 C324 -177(2) . . . . no H322 C322 C323 H323 1(3) . . . . no C322 C323 C324 H324 178(2) . . . . no H323 C323 C324 C325 -178.2(16) . . . . no H323 C323 C324 H324 0(3) . . . . no C323 C324 C325 H325 177(2) . . . . no H324 C324 C325 C326 -179(2) . . . . no H324 C324 C325 H325 -1(3) . . . . no C324 C325 C326 H326 177(2) . . . . no H325 C325 C326 C321 -177(2) . . . . no H325 C325 C326 H326 -1(3) . . . . no P3 C331 C332 H332 -0.2(18) . . . . no C336 C331 C332 H332 -179.3(18) . . . . no P3 C331 C336 H336 4.4(16) . . . . no C332 C331 C336 H336 -176.6(16) . . . . no C331 C332 C333 H333 179.9(19) . . . . no H332 C332 C333 C334 179.2(19) . . . . no H332 C332 C333 H333 -1(3) . . . . no C332 C333 C334 H334 177.0(18) . . . . no H333 C333 C334 C335 -180(2) . . . . no H333 C333 C334 H334 -3(3) . . . . no C333 C334 C335 H335 176(2) . . . . no H334 C334 C335 C336 -177.0(17) . . . . no H334 C334 C335 H335 -2(3) . . . . no C334 C335 C336 H336 176.4(17) . . . . no H335 C335 C336 C331 -176(2) . . . . no H335 C335 C336 H336 1(3) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu H112 3.30(2) . . no Cu H132 3.55(2) . . no Cu H222 3.03(2) . . no Cu H232 3.15(3) . . no Cu H312 2.88(2) . . no Cu H332 3.02(3) . . no P1 H312 3.17(2) . . no Si C12 3.985(3) . . no Si H12A 3.17(4) . . no Si H22B 3.34(5) . . no Si H324 3.45(3) . 2_555 no F1 C12 3.167(3) . . no F1 C11 3.073(3) . . no F2 C225 3.194(3) . 1_545 no F2 C213 3.366(3) . 1_445 no F3 C324 3.347(3) . 2_555 no F5 C132 3.340(3) . . no F5 C133 3.354(3) . . no F1 H324 2.55(3) . 2_555 no F1 H132 2.67(2) . . no F1 H332 2.87(3) . . no F1 H12A 2.56(4) . . no F2 H22B 2.64(5) . . no F2 H213 2.67(3) . 1_445 no F2 H225 2.45(3) . 1_545 no F3 H22B 2.85(5) . . no F3 H123 2.69(3) . 1_455 no F3 H324 2.67(3) . 2_555 no F3 H12A 2.72(4) . . no F4 H226 2.69(3) . 1_545 no F5 H115 2.70(3) . 2_656 no F5 H132 2.87(2) . . no F5 H133 2.85(3) . . no F5 H134 2.47(3) . 2_556 no N1 C132 3.266(2) . . no N1 H325 2.80(3) . 2_555 no N1 H132 2.69(2) . . no N1 H232 2.71(3) . . no N1 H332 2.71(3) . . no N2 H323 2.93(3) . 1_445 no N2 H334 2.93(3) . 1_455 no N2 H322 2.84(3) . 1_445 no C11 C314 3.538(3) . 1_455 no C11 F1 3.073(3) . . no C11 C132 3.249(3) . . no C11 C325 3.419(3) . 2_555 no C12 C324 3.572(4) . 2_555 no C12 Si 3.985(3) . . no C12 C313 3.422(3) . 1_455 no C12 C314 3.484(4) . 1_455 no C12 F1 3.167(3) . . no C11 H325 2.81(3) . 2_555 no C11 H132 2.61(2) . . no C112 C136 3.471(3) . . no C112 C216 3.578(3) . . no C116 C122 3.331(3) . . no C116 C136 3.521(3) . . no C121 C332 3.456(3) . . no C122 C332 3.353(3) . . no C122 C116 3.331(3) . . no C122 C331 3.266(3) . . no C123 C335 3.549(3) . . no C123 C334 3.529(3) . . no C123 C333 3.564(3) . . no C124 C333 3.489(3) . . no C124 C334 3.559(3) . . no C126 C132 3.309(3) . . no C132 C126 3.309(3) . . no C132 C11 3.249(3) . . no C132 F5 3.340(3) . . no C132 N1 3.266(2) . . no C133 F5 3.354(3) . . no C135 C214 3.557(3) . 2_666 no C136 C112 3.471(3) . . no C136 C116 3.521(3) . . no C111 H122 3.00(3) . . no C111 H136 2.49(2) . . no C111 H312 2.89(3) . . no C212 C313 3.546(3) . . no C112 H136 2.85(2) . . no C212 C312 3.306(3) . . no C212 C236 3.346(3) . . no C112 H312 2.77(3) . . no C113 H224 3.01(3) . 1_655 no C213 C313 3.526(3) . . no C213 F2 3.366(3) . 1_665 no C214 C135 3.557(3) . 2_666 no C115 H126 3.05(2) . 2_656 no C216 C226 3.570(3) . . no C216 C112 3.578(3) . . no C116 H136 2.90(2) . . no C121 H116 2.68(3) . . no C122 H116 2.89(3) . . no C123 H135 3.01(3) . 2_656 no C224 C224 3.416(3) . 2_566 no C124 H135 2.83(2) . 2_656 no C225 F2 3.194(3) . 1_565 no C226 C236 3.463(3) . . no C126 H132 3.07(2) . . no C226 C216 3.570(3) . . no C231 C322 3.510(3) . . no C131 H126 2.73(2) . . no C131 H222 2.68(3) . . no C132 H126 2.63(2) . . no C232 C314 3.535(3) . 1_455 no C232 C321 3.402(3) . . no C132 H222 2.84(3) . . no C132 H115 3.08(3) . 2_656 no C232 C322 3.285(3) . . no C133 H115 2.89(3) . 2_656 no C233 C323 3.325(3) . . no C233 C324 3.450(3) . . no C233 C322 3.560(3) . . no C234 C323 3.512(3) . . no C134 H133 2.97(3) . 2_556 no C134 H223 3.04(3) . . no C135 H214 3.03(3) . 2_666 no C135 H116 2.96(3) . 2_656 no C236 C212 3.346(3) . . no C236 C226 3.463(3) . . no C136 H116 3.04(3) . 2_656 no C136 H222 3.04(2) . . no C211 H112 2.83(3) . . no C211 H236 2.65(3) . . no C212 H236 2.79(3) . . no C312 C212 3.306(3) . . no C313 C213 3.526(3) . . no C213 H124 2.95(3) . 1_565 no C313 C212 3.546(3) . . no C313 C12 3.422(3) . 1_655 no C214 H135 2.97(3) . 2_666 no C314 C232 3.535(3) . 1_655 no C314 C11 3.538(3) . 1_655 no C314 C12 3.484(4) . 1_655 no C215 H113 3.02(3) . . no C316 C336 3.437(3) . . no C316 C322 3.166(3) . . no C216 H112 2.83(3) . . no C221 H216 2.62(2) . . no C321 C232 3.402(3) . . no C322 C233 3.560(3) . . no C322 C316 3.166(3) . . no C322 C232 3.285(3) . . no C222 H216 3.09(2) . . no C322 C231 3.510(3) . . no C323 C234 3.512(3) . . no C323 C233 3.325(3) . . no C324 F3 3.347(3) . 2_555 no C224 H224 2.85(3) . 2_566 no C224 H313 2.81(2) . 1_455 no C324 C233 3.450(3) . . no C324 C12 3.572(4) . 2_555 no C225 H114 2.91(3) . 2_666 no C325 C326 3.489(3) . 2_555 no C225 H313 3.01(3) . 1_455 no C325 C11 3.419(3) . 2_555 no C226 H216 3.04(2) . . no C326 C332 3.559(3) . . no C226 H314 3.00(3) . 1_455 no C326 C325 3.489(3) . 2_555 no C231 H226 2.71(3) . . no C231 H212 3.08(2) . . no C331 C122 3.266(3) . . no C332 C326 3.559(3) . . no C332 C121 3.456(3) . . no C232 H314 2.77(3) . 1_455 no C332 C122 3.353(3) . . no C333 C123 3.564(3) . . no C333 C124 3.489(3) . . no C233 H315 2.98(3) . 1_455 no C334 C123 3.529(3) . . no C334 C124 3.559(3) . . no C335 C123 3.549(3) . . no C336 C316 3.437(3) . . no C236 H226 2.77(3) . . no C311 H336 2.83(3) . . no C311 H322 2.80(3) . . no C312 H212 2.91(3) . . no C313 H12C 2.97(5) . 1_655 no C313 H12B 3.02(3) . 1_655 no C314 H12B 2.98(3) . 1_655 no C315 H12B 3.01(3) . 1_655 no C316 H336 2.71(3) . . no C316 H322 2.86(3) . . no C321 H316 2.84(2) . . no C322 H316 2.92(2) . . no C323 H335 3.01(3) . 2_655 no C325 H326 2.98(3) . 2_555 no C326 H325 3.00(3) . 2_555 no C331 H326 2.68(3) . . no C332 H326 2.86(3) . . no C334 H235 3.09(4) . 1_545 no C336 H316 3.07(3) . 2_655 no H12A F3 2.72(4) . . no H12A F1 2.56(4) . . no H12A Si 3.17(4) . . no H12B C313 3.02(3) . 1_455 no H12B C314 2.98(3) . 1_455 no H12B C315 3.01(3) . 1_455 no H12C C313 2.97(5) . 1_455 no H22B Si 3.34(5) . . no H22B F2 2.64(5) . . no H22B F3 2.85(5) . . no H112 Cu 3.30(2) . . no H112 C211 2.83(3) . . no H112 C216 2.83(3) . . no H113 C215 3.02(3) . . no H114 C225 2.91(3) . 2_666 no H115 H134 2.56(5) . 1_655 no H115 F5 2.70(3) . 2_656 no H115 C132 3.08(3) . 2_656 no H115 C133 2.89(3) . 2_656 no H116 C121 2.68(3) . . no H116 C122 2.89(3) . . no H116 C135 2.96(3) . 2_656 no H116 C136 3.04(3) . 2_656 no H122 C111 3.00(3) . . no H123 F3 2.69(3) . 1_655 no H124 C213 2.95(3) . 1_545 no H126 H132 2.45(3) . . no H126 C115 3.05(2) . 2_656 no H126 C132 2.63(2) . . no H126 C131 2.73(2) . . no H132 Cu 3.55(2) . . no H132 N1 2.69(2) . . no H132 F1 2.67(2) . . no H132 F5 2.87(2) . . no H132 H126 2.45(3) . . no H132 C11 2.61(2) . . no H132 C126 3.07(2) . . no H133 F5 2.85(3) . . no H133 C134 2.97(3) . 2_556 no H133 H134 2.44(4) . 2_556 no H134 H115 2.56(5) . 1_455 no H134 H133 2.44(4) . 2_556 no H134 F5 2.47(3) . 2_556 no H135 C124 2.83(2) . 2_656 no H135 C214 2.97(3) . 2_666 no H135 C123 3.01(3) . 2_656 no H135 H214 2.53(4) . 2_666 no H136 C112 2.85(2) . . no H136 C111 2.49(2) . . no H136 C116 2.90(2) . . no H212 C312 2.91(3) . . no H212 C231 3.08(2) . . no H213 F2 2.67(3) . 1_665 no H214 C135 3.03(3) . 2_666 no H214 H135 2.53(4) . 2_666 no H216 C221 2.62(2) . . no H216 C226 3.04(2) . . no H216 C222 3.09(2) . . no H222 C131 2.68(3) . . no H222 C132 2.84(3) . . no H222 C136 3.04(2) . . no H222 Cu 3.03(2) . . no H223 C134 3.04(3) . . no H224 C113 3.01(3) . 1_455 no H224 C224 2.85(3) . 2_566 no H224 H224 2.50(4) . 2_566 no H225 F2 2.45(3) . 1_565 no H226 F4 2.69(3) . 1_565 no H226 C231 2.71(3) . . no H226 C236 2.77(3) . . no H232 Cu 3.15(3) . . no H232 N1 2.71(3) . . no H233 H315 2.50(4) . 1_455 no H234 H235 2.50(4) . 2_565 no H235 H333 2.60(5) . 1_565 no H235 H334 2.52(4) . 1_565 no H235 C334 3.09(4) . 1_565 no H235 H234 2.50(4) . 2_565 no H236 C211 2.65(3) . . no H236 C212 2.79(3) . . no H312 P1 3.17(2) . . no H312 C111 2.89(3) . . no H312 C112 2.77(3) . . no H312 Cu 2.88(2) . . no H313 C225 3.01(3) . 1_655 no H313 C224 2.81(2) . 1_655 no H314 C226 3.00(3) . 1_655 no H314 C232 2.77(3) . 1_655 no H315 C233 2.98(3) . 1_655 no H315 H233 2.50(4) . 1_655 no H316 H336 2.40(4) . . no H316 C336 3.07(3) . 2_655 no H316 C322 2.92(2) . . no H316 C321 2.84(2) . . no H322 C316 2.86(3) . . no H322 N2 2.84(3) . 1_665 no H322 C311 2.80(3) . . no H323 N2 2.93(3) . 1_665 no H324 F1 2.55(3) . 2_555 no H324 F3 2.67(3) . 2_555 no H324 Si 3.45(3) . 2_555 no H325 C326 3.00(3) . 2_555 no H325 N1 2.80(3) . 2_555 no H325 C11 2.81(3) . 2_555 no H325 H326 2.57(4) . 2_555 no H326 C325 2.98(3) . 2_555 no H326 H325 2.57(4) . 2_555 no H326 C332 2.86(3) . . no H326 C331 2.68(3) . . no H332 N1 2.71(3) . . no H332 Cu 3.02(3) . . no H332 F1 2.87(3) . . no H333 H235 2.60(5) . 1_545 no H334 H235 2.52(4) . 1_545 no H334 N2 2.93(3) . 1_655 no H335 C323 3.01(3) . 2_655 no H336 H316 2.40(4) . . no H336 C311 2.83(3) . . no H336 C316 2.71(3) . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C134 H134 F5 0.96(3) 2.47(3) 3.379(3) 159(2) 2_556 yes C225 H225 F2 0.87(3) 2.45(3) 3.194(3) 144(3) 1_565 yes C324 H324 F1 0.97(3) 2.55(3) 3.516(3) 172(2) 2_555 yes _exptl_crystal_F_000 1092 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min -19 _reflns_limit_k_max 19 _reflns_limit_l_min -29 _reflns_limit_l_max 27 _reflns_number_observed ? _reflns_d_resolution_high .667 _reflns_d_resolution_low 18.057 _diffrn_reflns_av_sigmaI/netI .054 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .06 _refine_ls_wR_factor_all .059 _refine_ls_goodness_of_fit_all 1.034 _refine_ls_shift/su_mean .0004 #========================================================================== data_H1203_9 _database_code_depnum_ccdc_archive 'CCDC 268669' # EXPERIMENTAL DATA #--------------------- _chemical_name_systematic ; Tris(triphenylphosphine)(acetonitrile)copper(I) hexfluorophosphate acetonitrile solvate ; _chemical_formula_sum 'C58 H51 Cu1 F6 N2 P4' _chemical_formula_moiety ? _chemical_formula_weight 1077.49 _chemical_melting_point ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,-y,-z _cell_length_a 10.5757(8) _cell_length_b 13.2460(10) _cell_length_c 19.597(2) _cell_angle_alpha 104.180(2) _cell_angle_beta 104.139(2) _cell_angle_gamma 93.938(2) _cell_volume 2556.8(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.4 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _cell_measurement_reflns_used 8539 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 34.46 _cell_measurement_temperature 150 _exptl_absorpt_coefficient_mu .615 _exptl_crystal_description prism _exptl_crystal_size_max .38 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .19 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .94 _exptl_absorpt_correction_T_max 1 _diffrn_reflns_number 51243 _reflns_number_total 21697 _reflns_Friedel_coverage 0 _reflns_number_gt 16753 _reflns_threshold_expression 'F > 4.00 sig(F )' _diffrn_reflns_theta_max 34.65 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents .024 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .042 _refine_ls_wR_factor_ref .049 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_number_reflns 16753 _refine_ls_number_parameters 844 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment refall _refine_ls_shift/su_max .01 _refine_diff_density_min -.466 _refine_diff_density_max .673 _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? # Information for the "methods" section #----------------------------------------- _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 116 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 102 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' Cu ? 0 2 .263 1.266 'Int Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 4 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 12 .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .09 .095 'Int Tables Vol IV Tables 2.2B and 2.3.1' # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Cu Cu Uani 0.29163(2) 0.14833(1) 0.25400(1) 1.000 0.0161(1) . . P1 P Uani 0.39452(4) 0.08705(3) 0.35348(2) 1.000 0.0167(1) . . P2 P Uani 0.25748(4) 0.32338(3) 0.26796(2) 1.000 0.0168(1) . . P3 P Uani 0.36878(3) 0.08327(3) 0.15288(2) 1.000 0.0165(1) . . N1 N Uani 0.09449(13) 0.08358(10) 0.23141(7) 1.000 0.0212(3) . . C11 C Uani -0.00886(15) 0.05631(12) 0.23402(9) 1.000 0.0234(4) . . C12 C Uani -0.13920(19) 0.02046(17) 0.23912(14) 1.000 0.0366(6) . . C111 C Uani 0.55364(14) 0.15910(11) 0.41146(7) 1.000 0.0186(3) . . C112 C Uani 0.57617(15) 0.26776(12) 0.42143(8) 1.000 0.0215(4) . . C113 C Uani 0.69035(16) 0.32770(13) 0.47071(9) 1.000 0.0250(4) . . C114 C Uani 0.78348(16) 0.27958(14) 0.51043(9) 1.000 0.0274(4) . . C115 C Uani 0.76299(16) 0.17122(14) 0.49998(9) 1.000 0.0276(4) . . C116 C Uani 0.64858(15) 0.11084(13) 0.45108(9) 1.000 0.0238(4) . . C121 C Uani 0.42918(14) -0.04902(11) 0.32925(8) 1.000 0.0203(3) . . C122 C Uani 0.52666(16) -0.06981(13) 0.29212(9) 1.000 0.0252(4) . . C123 C Uani 0.55454(18) -0.17189(14) 0.26948(10) 1.000 0.0312(5) . . C124 C Uani 0.4838(2) -0.25465(14) 0.28265(10) 1.000 0.0354(5) . . C125 C Uani 0.3877(2) -0.23498(13) 0.31930(11) 1.000 0.0341(5) . . C126 C Uani 0.36022(17) -0.13228(12) 0.34293(9) 1.000 0.0258(4) . . C131 C Uani 0.29784(14) 0.09278(11) 0.42017(7) 1.000 0.0182(3) . . C132 C Uani 0.16621(15) 0.04424(12) 0.39549(8) 1.000 0.0214(3) . . C133 C Uani 0.08403(16) 0.05952(13) 0.44207(9) 1.000 0.0258(4) . . C134 C Uani 0.13229(18) 0.12155(13) 0.51379(9) 1.000 0.0267(4) . . C135 C Uani 0.26363(17) 0.16636(13) 0.53949(9) 1.000 0.0252(4) . . C136 C Uani 0.34622(15) 0.15275(12) 0.49306(8) 1.000 0.0216(4) . . C211 C Uani 0.40199(14) 0.42373(11) 0.30841(8) 1.000 0.0200(3) . . C212 C Uani 0.49785(16) 0.42710(12) 0.27021(9) 1.000 0.0247(4) . . C213 C Uani 0.61680(17) 0.49347(14) 0.30293(11) 1.000 0.0309(5) . . C214 C Uani 0.64178(17) 0.55684(13) 0.37419(12) 1.000 0.0332(5) . . C215 C Uani 0.54715(18) 0.55538(13) 0.41190(10) 1.000 0.0314(4) . . C216 C Uani 0.42713(16) 0.48960(12) 0.37952(9) 1.000 0.0252(4) . . C221 C Uani 0.14585(14) 0.36636(11) 0.32435(8) 1.000 0.0192(3) . . C222 C Uani 0.12979(17) 0.31240(13) 0.37540(9) 1.000 0.0251(4) . . C223 C Uani 0.04497(18) 0.34268(15) 0.41912(10) 1.000 0.0299(5) . . C224 C Uani -0.02429(16) 0.42661(13) 0.41162(9) 1.000 0.0263(4) . . C225 C Uani -0.00827(15) 0.48121(12) 0.36130(9) 1.000 0.0247(4) . . C226 C Uani 0.07666(15) 0.45159(12) 0.31779(9) 1.000 0.0223(4) . . C231 C Uani 0.17615(14) 0.35187(11) 0.18217(8) 1.000 0.0187(3) . . C232 C Uani 0.07962(14) 0.27366(12) 0.13053(8) 1.000 0.0208(3) . . C233 C Uani 0.00800(15) 0.29227(13) 0.06625(9) 1.000 0.0248(4) . . C234 C Uani 0.03256(18) 0.38886(15) 0.05224(10) 1.000 0.0308(5) . . C235 C Uani 0.1285(2) 0.46650(15) 0.10262(10) 1.000 0.0337(5) . . C236 C Uani 0.20070(17) 0.44843(13) 0.16736(9) 1.000 0.0269(4) . . C311 C Uani 0.53824(14) 0.14056(11) 0.16548(8) 1.000 0.0187(3) . . C312 C Uani 0.61043(15) 0.19813(12) 0.23585(8) 1.000 0.0224(3) . . C313 C Uani 0.73471(16) 0.25282(14) 0.24792(10) 1.000 0.0291(4) . . C314 C Uani 0.78847(17) 0.25083(14) 0.18967(11) 1.000 0.0318(5) . . C315 C Uani 0.71884(17) 0.19236(15) 0.11939(10) 1.000 0.0303(5) . . C316 C Uani 0.59477(15) 0.13734(13) 0.10715(9) 1.000 0.0244(4) . . C321 C Uani 0.28391(14) 0.10658(12) 0.06556(7) 1.000 0.0200(3) . . C322 C Uani 0.31280(16) 0.20213(13) 0.05016(9) 1.000 0.0252(4) . . C323 C Uani 0.24319(18) 0.22085(16) -0.01476(10) 1.000 0.0324(5) . . C324 C Uani 0.1429(2) 0.14603(18) -0.06415(10) 1.000 0.0370(6) . . C325 C Uani 0.1123(2) 0.05211(17) -0.04901(10) 1.000 0.0367(5) . . C326 C Uani 0.18279(17) 0.03175(14) 0.01535(9) 1.000 0.0276(4) . . C331 C Uani 0.36405(14) -0.05993(11) 0.12810(7) 1.000 0.0195(3) . . C332 C Uani 0.26549(15) -0.11874(12) 0.14414(8) 1.000 0.0224(3) . . C333 C Uani 0.25387(17) -0.22839(13) 0.12595(9) 1.000 0.0271(4) . . C334 C Uani 0.3413(2) -0.27983(13) 0.09147(10) 1.000 0.0313(5) . . C335 C Uani 0.4398(2) -0.22227(14) 0.07550(10) 1.000 0.0312(5) . . C336 C Uani 0.45159(17) -0.11253(13) 0.09355(9) 1.000 0.0251(4) . . P P Uani -0.05199(5) -0.26385(4) 0.26141(3) 1.000 0.0302(1) . . F1 F Uani 0.03929(12) -0.17744(10) 0.24318(7) 1.000 0.0395(3) . . F2 F Uani -0.14580(15) -0.34765(14) 0.27905(10) 1.000 0.0729(6) . . F3 F Uani -0.17382(11) -0.25198(10) 0.19784(7) 1.000 0.0399(4) . . F4 F Uani 0.06694(15) -0.27335(14) 0.32622(9) 1.000 0.0704(6) . . F5 F Uani -0.01099(16) -0.35460(12) 0.20524(11) 1.000 0.0742(6) . . F6 F Uani -0.09390(17) -0.16976(13) 0.31729(8) 1.000 0.0619(5) . . N2 N Uani -0.5282(3) -0.5450(3) 0.0792(2) 1.000 0.0858(11) . . C21 C Uani -0.4186(3) -0.5281(2) 0.08618(15) 1.000 0.0557(9) . . C22 C Uani -0.2791(4) -0.5104(3) 0.0928(3) 1.000 0.0758(11) . . H12A H Uiso -0.148(3) -0.044(3) 0.2385(19) 1.000 0.084(11) . . H12B H Uiso -0.206(3) 0.030(2) 0.1971(16) 1.000 0.062(8) . . H12C H Uiso -0.149(3) 0.065(3) 0.279(2) 1.000 0.078(11) . . H112 H Uiso 0.516(2) 0.3010(18) 0.3960(13) 1.000 0.038(6) . . H113 H Uiso 0.700(2) 0.399(2) 0.4787(13) 1.000 0.040(6) . . H114 H Uiso 0.858(2) 0.3188(19) 0.5444(13) 1.000 0.038(6) . . H115 H Uiso 0.828(2) 0.1360(18) 0.5265(13) 1.000 0.037(6) . . H116 H Uiso 0.637(2) 0.0403(19) 0.4437(12) 1.000 0.036(6) . . H122 H Uiso 0.575(2) -0.0116(16) 0.2819(11) 1.000 0.023(5) . . H123 H Uiso 0.621(2) -0.1847(18) 0.2464(12) 1.000 0.033(6) . . H124 H Uiso 0.507(2) -0.327(2) 0.2679(13) 1.000 0.043(6) . . H125 H Uiso 0.342(2) -0.293(2) 0.3311(14) 1.000 0.048(7) . . H126 H Uiso 0.296(2) -0.1186(17) 0.3682(12) 1.000 0.030(5) . . H132 H Uiso 0.1341(19) 0.0016(16) 0.3475(11) 1.000 0.022(5) . . H133 H Uiso -0.007(2) 0.0271(17) 0.4227(12) 1.000 0.032(6) . . H134 H Uiso 0.074(2) 0.135(2) 0.5458(14) 1.000 0.045(7) . . H135 H Uiso 0.300(2) 0.2049(17) 0.5862(12) 1.000 0.030(5) . . H136 H Uiso 0.439(2) 0.1838(16) 0.5124(11) 1.000 0.025(5) . . H212 H Uiso 0.4825(19) 0.3817(15) 0.2205(11) 1.000 0.020(5) . . H213 H Uiso 0.683(2) 0.4929(19) 0.2767(13) 1.000 0.040(6) . . H214 H Uiso 0.719(2) 0.5978(18) 0.3952(13) 1.000 0.035(6) . . H215 H Uiso 0.563(2) 0.596(2) 0.4575(13) 1.000 0.040(6) . . H216 H Uiso 0.363(2) 0.4913(17) 0.4063(12) 1.000 0.032(6) . . H222 H Uiso 0.173(2) 0.2523(18) 0.3796(12) 1.000 0.033(6) . . H223 H Uiso 0.034(2) 0.3054(18) 0.4511(13) 1.000 0.038(6) . . H224 H Uiso -0.082(2) 0.4458(18) 0.4378(13) 1.000 0.035(6) . . H225 H Uiso -0.053(2) 0.5402(18) 0.3555(12) 1.000 0.036(6) . . H226 H Uiso 0.087(2) 0.4876(16) 0.2841(11) 1.000 0.027(5) . . H232 H Uiso 0.064(2) 0.2091(16) 0.1391(11) 1.000 0.026(5) . . H233 H Uiso -0.056(2) 0.2388(18) 0.0310(12) 1.000 0.036(6) . . H234 H Uiso -0.013(2) 0.4003(17) 0.0088(12) 1.000 0.032(6) . . H235 H Uiso 0.148(3) 0.531(2) 0.0934(15) 1.000 0.054(8) . . H236 H Uiso 0.268(2) 0.5027(16) 0.2016(11) 1.000 0.026(5) . . H312 H Uiso 0.571(2) 0.2002(16) 0.2753(11) 1.000 0.027(5) . . H313 H Uiso 0.783(3) 0.288(2) 0.2950(14) 1.000 0.048(7) . . H314 H Uiso 0.870(2) 0.291(2) 0.1972(13) 1.000 0.044(7) . . H315 H Uiso 0.754(2) 0.190(2) 0.0790(14) 1.000 0.045(7) . . H316 H Uiso 0.545(2) 0.1019(16) 0.0605(11) 1.000 0.024(5) . . H322 H Uiso 0.379(2) 0.2535(17) 0.0846(12) 1.000 0.029(5) . . H323 H Uiso 0.264(2) 0.286(2) -0.0246(13) 1.000 0.041(6) . . H324 H Uiso 0.093(2) 0.160(2) -0.1073(14) 1.000 0.046(7) . . H325 H Uiso 0.040(2) 0.001(2) -0.0843(13) 1.000 0.040(6) . . H326 H Uiso 0.159(2) -0.033(2) 0.0254(13) 1.000 0.041(6) . . H332 H Uiso 0.210(2) -0.0828(17) 0.1686(12) 1.000 0.033(6) . . H333 H Uiso 0.188(2) -0.2648(18) 0.1376(12) 1.000 0.033(6) . . H334 H Uiso 0.337(2) -0.3570(19) 0.0781(13) 1.000 0.040(6) . . H335 H Uiso 0.501(2) -0.2564(19) 0.0532(13) 1.000 0.040(6) . . H336 H Uiso 0.522(2) -0.0725(17) 0.0842(11) 1.000 0.028(5) . . H22A H Uiso -0.232(5) -0.568(4) 0.096(3) 1.000 0.14(2) . . H22B H Uiso -0.250(5) -0.464(5) 0.130(3) 1.000 0.16(2) . . H22C H Uiso -0.268(3) -0.478(3) 0.053(2) 1.000 0.080(11) . . 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 Cu 0.0177(1) 0.0160(1) 0.0150(1) 0.0047(1) 0.0046(1) 0.0026(1) P1 0.0181(2) 0.0167(2) 0.0153(1) 0.0054(1) 0.0034(1) 0.0022(1) P2 0.0183(2) 0.0155(1) 0.0171(2) 0.0051(1) 0.0046(1) 0.0028(1) P3 0.0173(2) 0.0176(2) 0.0143(1) 0.0034(1) 0.0049(1) 0.0010(1) N1 0.0212(5) 0.0224(6) 0.0202(5) 0.0073(4) 0.0047(4) 0.0021(4) C11 0.0244(7) 0.0219(6) 0.0260(7) 0.0105(5) 0.0064(5) 0.0043(5) C12 0.0235(8) 0.0346(10) 0.0610(13) 0.0235(9) 0.0175(8) 0.0059(7) C111 0.0192(6) 0.0196(6) 0.0171(6) 0.0062(5) 0.0042(5) 0.0023(5) C112 0.0240(7) 0.0206(6) 0.0201(6) 0.0068(5) 0.0051(5) 0.0037(5) C113 0.0273(7) 0.0218(7) 0.0241(7) 0.0053(5) 0.0056(6) -0.0015(5) C114 0.0228(7) 0.0319(8) 0.0236(7) 0.0071(6) 0.0016(5) -0.0032(6) C115 0.0204(7) 0.0318(8) 0.0290(7) 0.0126(6) -0.0002(6) 0.0011(6) C116 0.0222(6) 0.0226(7) 0.0256(7) 0.0100(5) 0.0015(5) 0.0023(5) C121 0.0226(6) 0.0199(6) 0.0171(6) 0.0051(5) 0.0025(5) 0.0050(5) C122 0.0260(7) 0.0261(7) 0.0232(7) 0.0064(6) 0.0054(5) 0.0072(6) C123 0.0313(8) 0.0323(8) 0.0276(8) 0.0044(6) 0.0044(6) 0.0153(7) C124 0.0425(10) 0.0249(8) 0.0319(8) 0.0033(6) -0.0008(7) 0.0146(7) C125 0.0442(10) 0.0195(7) 0.0362(9) 0.0099(6) 0.0038(8) 0.0053(7) C126 0.0312(8) 0.0205(6) 0.0260(7) 0.0090(5) 0.0060(6) 0.0025(6) C131 0.0210(6) 0.0176(6) 0.0176(6) 0.0075(5) 0.0053(5) 0.0028(5) C132 0.0234(6) 0.0223(6) 0.0186(6) 0.0074(5) 0.0048(5) -0.0002(5) C133 0.0248(7) 0.0285(7) 0.0273(7) 0.0115(6) 0.0098(6) 0.0001(6) C134 0.0342(8) 0.0265(7) 0.0254(7) 0.0106(6) 0.0151(6) 0.0058(6) C135 0.0344(8) 0.0231(7) 0.0190(6) 0.0059(5) 0.0089(6) 0.0032(6) C136 0.0259(7) 0.0200(6) 0.0175(6) 0.0049(5) 0.0040(5) 0.0012(5) C211 0.0199(6) 0.0160(6) 0.0236(6) 0.0066(5) 0.0036(5) 0.0035(5) C212 0.0233(7) 0.0216(6) 0.0291(7) 0.0061(6) 0.0080(6) 0.0022(5) C213 0.0229(7) 0.0244(7) 0.0455(10) 0.0086(7) 0.0105(7) 0.0015(6) C214 0.0226(7) 0.0210(7) 0.0492(11) 0.0076(7) 0.0000(7) -0.0006(6) C215 0.0305(8) 0.0219(7) 0.0317(8) 0.0000(6) -0.0017(6) 0.0000(6) C216 0.0269(7) 0.0208(6) 0.0252(7) 0.0037(5) 0.0045(6) 0.0028(5) C221 0.0203(6) 0.0178(6) 0.0195(6) 0.0050(5) 0.0055(5) 0.0033(5) C222 0.0306(8) 0.0250(7) 0.0244(7) 0.0100(6) 0.0116(6) 0.0086(6) C223 0.0363(9) 0.0333(8) 0.0268(7) 0.0121(6) 0.0159(7) 0.0085(7) C224 0.0231(7) 0.0286(7) 0.0246(7) 0.0004(6) 0.0089(6) 0.0023(6) C225 0.0215(7) 0.0226(7) 0.0278(7) 0.0028(5) 0.0063(5) 0.0052(5) C226 0.0225(6) 0.0203(6) 0.0259(7) 0.0079(5) 0.0077(5) 0.0055(5) C231 0.0194(6) 0.0199(6) 0.0181(6) 0.0066(5) 0.0057(5) 0.0041(5) C232 0.0211(6) 0.0206(6) 0.0217(6) 0.0077(5) 0.0058(5) 0.0017(5) C233 0.0213(7) 0.0294(7) 0.0225(7) 0.0089(6) 0.0023(5) 0.0011(6) C234 0.0302(8) 0.0364(9) 0.0275(8) 0.0174(7) 0.0018(6) 0.0051(7) C235 0.0391(9) 0.0281(8) 0.0349(9) 0.0196(7) 0.0017(7) 0.0014(7) C236 0.0300(8) 0.0215(7) 0.0280(7) 0.0118(6) 0.0015(6) 0.0007(6) C311 0.0185(6) 0.0182(6) 0.0194(6) 0.0042(5) 0.0061(5) 0.0020(5) C312 0.0212(6) 0.0221(6) 0.0206(6) 0.0015(5) 0.0045(5) 0.0012(5) C313 0.0224(7) 0.0262(7) 0.0312(8) 0.0007(6) 0.0018(6) -0.0011(6) C314 0.0209(7) 0.0278(8) 0.0447(10) 0.0066(7) 0.0097(7) -0.0019(6) C315 0.0245(7) 0.0337(8) 0.0360(9) 0.0092(7) 0.0152(7) 0.0008(6) C316 0.0222(7) 0.0290(7) 0.0223(7) 0.0055(6) 0.0088(5) 0.0000(5) C321 0.0200(6) 0.0251(6) 0.0156(5) 0.0053(5) 0.0063(5) 0.0031(5) C322 0.0246(7) 0.0283(7) 0.0264(7) 0.0121(6) 0.0090(6) 0.0037(6) C323 0.0329(8) 0.0422(10) 0.0328(8) 0.0235(8) 0.0135(7) 0.0115(7) C324 0.0368(9) 0.0557(12) 0.0232(7) 0.0191(8) 0.0065(7) 0.0125(8) C325 0.0361(9) 0.0475(11) 0.0197(7) 0.0076(7) -0.0024(6) 0.0024(8) C326 0.0295(8) 0.0295(8) 0.0191(6) 0.0051(6) 0.0009(6) -0.0012(6) C331 0.0220(6) 0.0187(6) 0.0162(5) 0.0032(5) 0.0043(5) 0.0017(5) C332 0.0227(6) 0.0207(6) 0.0227(6) 0.0040(5) 0.0064(5) 0.0013(5) C333 0.0288(8) 0.0209(7) 0.0294(8) 0.0045(6) 0.0077(6) -0.0015(6) C334 0.0406(9) 0.0195(7) 0.0316(8) 0.0020(6) 0.0107(7) 0.0041(6) C335 0.0397(9) 0.0239(7) 0.0323(8) 0.0028(6) 0.0173(7) 0.0091(7) C336 0.0300(8) 0.0239(7) 0.0238(7) 0.0046(5) 0.0131(6) 0.0049(6) P 0.0291(2) 0.0273(2) 0.0316(2) 0.0130(2) -0.0005(2) -0.0011(2) F1 0.0366(6) 0.0413(6) 0.0422(6) 0.0170(5) 0.0102(5) -0.0026(5) F2 0.0494(8) 0.0753(11) 0.0989(13) 0.0659(10) -0.0058(8) -0.0194(7) F3 0.0328(6) 0.0452(7) 0.0394(6) 0.0176(5) -0.0005(5) 0.0050(5) F4 0.0469(8) 0.0820(11) 0.0758(11) 0.0539(9) -0.0221(7) -0.0128(7) F5 0.0605(10) 0.0417(8) 0.1006(13) -0.0122(8) 0.0140(9) 0.0187(7) F6 0.0822(11) 0.0659(10) 0.0365(7) 0.0013(7) 0.0283(7) 0.0041(8) N2 0.0731(19) 0.089(2) 0.107(2) 0.0374(19) 0.0377(18) 0.0005(16) C21 0.0673(17) 0.0431(12) 0.0560(15) 0.0095(11) 0.0225(13) -0.0035(11) C22 0.0589(19) 0.066(2) 0.082(2) -0.004(2) 0.0093(17) -0.0062(16) #=============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu P1 2.3460(5) . . yes Cu P2 2.3311(5) . . yes Cu P3 2.3206(5) . . yes Cu N1 2.0966(14) . . yes P1 C111 1.8297(15) . . yes P1 C121 1.8344(16) . . yes P1 C131 1.8369(15) . . yes P2 C211 1.8286(16) . . yes P2 C221 1.8332(16) . . yes P2 C231 1.8324(15) . . yes P3 C311 1.8314(16) . . yes P3 C321 1.8373(14) . . yes P3 C331 1.8331(16) . . yes P F6 1.6104(18) . . yes P F2 1.5938(19) . . yes P F3 1.6051(14) . . yes P F1 1.6083(15) . . yes P F5 1.5815(19) . . yes P F4 1.5908(18) . . yes N1 C11 1.144(2) . . yes N2 C21 1.133(5) . . yes C11 C12 1.462(3) . . no C111 C112 1.400(2) . . no C111 C116 1.404(2) . . no C112 C113 1.394(2) . . no C12 H12B 0.99(3) . . no C12 H12C 0.89(4) . . no C12 H12A 0.85(4) . . no C113 C114 1.392(2) . . no C114 C115 1.393(3) . . no C115 C116 1.395(2) . . no C121 C122 1.405(2) . . no C121 C126 1.396(2) . . no C122 C123 1.392(3) . . no C123 C124 1.396(3) . . no C124 C125 1.385(3) . . no C125 C126 1.400(3) . . no C131 C136 1.402(2) . . no C131 C132 1.407(2) . . no C132 C133 1.397(2) . . no C133 C134 1.392(2) . . no C134 C135 1.391(3) . . no C135 C136 1.397(2) . . no C211 C212 1.404(2) . . no C211 C216 1.402(2) . . no C112 H112 0.92(2) . . no C212 C213 1.394(3) . . no C213 C214 1.393(3) . . no C113 H113 0.91(3) . . no C214 C215 1.383(3) . . no C114 H114 0.92(2) . . no C115 H115 0.97(2) . . no C215 C216 1.399(3) . . no C116 H116 0.90(3) . . no C221 C222 1.399(2) . . no C221 C226 1.402(2) . . no C122 H122 0.98(2) . . no C222 C223 1.399(3) . . no C123 H123 0.93(2) . . no C223 C224 1.390(3) . . no C224 C225 1.392(2) . . no C124 H124 1.00(3) . . no C225 C226 1.395(2) . . no C125 H125 0.98(3) . . no C126 H126 0.94(2) . . no C231 C232 1.406(2) . . no C231 C236 1.400(2) . . no C232 C233 1.390(2) . . no C132 H132 0.94(2) . . no C133 H133 0.97(2) . . no C233 C234 1.393(3) . . no C134 H134 0.98(2) . . no C234 C235 1.390(3) . . no C235 C236 1.397(3) . . no C135 H135 0.90(2) . . no C136 H136 0.98(2) . . no C311 C312 1.399(2) . . no C311 C316 1.407(2) . . no C312 C313 1.393(2) . . no C212 H212 0.98(2) . . no C313 C314 1.390(3) . . no C213 H213 0.96(2) . . no C214 H214 0.89(2) . . no C314 C315 1.394(3) . . no C215 H215 0.89(2) . . no C315 C316 1.393(3) . . no C216 H216 0.95(2) . . no C321 C326 1.399(2) . . no C321 C322 1.402(2) . . no C322 C323 1.394(3) . . no C222 H222 0.96(2) . . no C323 C324 1.389(3) . . no C223 H223 0.91(2) . . no C324 C325 1.383(3) . . no C224 H224 0.90(2) . . no C225 H225 0.96(2) . . no C325 C326 1.398(3) . . no C226 H226 0.93(2) . . no C331 C336 1.402(2) . . no C331 C332 1.400(2) . . no C332 C333 1.397(2) . . no C232 H232 0.92(2) . . no C333 C334 1.394(3) . . no C233 H233 0.95(2) . . no C234 H234 0.92(2) . . no C334 C335 1.390(3) . . no C335 C336 1.398(3) . . no C235 H235 0.94(3) . . no C236 H236 0.97(2) . . no C312 H312 0.96(2) . . no C313 H313 0.93(3) . . no C314 H314 0.94(2) . . no C315 H315 0.95(2) . . no C316 H316 0.92(2) . . no C21 C22 1.447(6) . . no C322 H322 0.94(2) . . no C323 H323 0.95(3) . . no C324 H324 0.95(3) . . no C325 H325 0.98(2) . . no C326 H326 0.96(3) . . no C332 H332 0.93(2) . . no C333 H333 0.92(2) . . no C334 H334 0.99(3) . . no C335 H335 0.95(2) . . no C336 H336 0.96(2) . . no C22 H22A 0.95(6) . . no C22 H22B 0.81(6) . . no C22 H22C 1.00(4) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Cu P2 121.89(2) . . . yes P1 Cu P3 111.67(2) . . . yes P1 Cu N1 102.39(4) . . . yes P2 Cu P3 112.07(2) . . . yes P2 Cu N1 97.49(4) . . . yes P3 Cu N1 109.08(4) . . . yes Cu P1 C111 117.18(5) . . . yes Cu P1 C121 114.86(5) . . . yes Cu P1 C131 112.86(5) . . . yes C111 P1 C121 102.95(7) . . . yes C111 P1 C131 101.76(6) . . . yes C121 P1 C131 105.68(7) . . . yes Cu P2 C211 117.45(5) . . . yes Cu P2 C221 114.34(5) . . . yes Cu P2 C231 113.61(5) . . . yes C211 P2 C221 103.42(7) . . . yes C211 P2 C231 104.49(7) . . . yes C221 P2 C231 101.74(7) . . . yes Cu P3 C311 112.43(5) . . . yes Cu P3 C321 118.24(5) . . . yes Cu P3 C331 113.69(5) . . . yes C311 P3 C321 101.75(7) . . . yes C311 P3 C331 107.19(7) . . . yes C321 P3 C331 102.19(7) . . . yes F1 P F5 90.40(8) . . . yes F1 P F6 88.57(8) . . . yes F2 P F3 89.10(8) . . . yes F2 P F4 90.55(10) . . . yes F2 P F5 90.59(10) . . . yes F2 P F6 90.42(10) . . . yes F3 P F4 178.23(9) . . . yes F3 P F5 90.59(9) . . . yes F3 P F6 88.54(8) . . . yes F4 P F5 91.14(10) . . . yes F4 P F6 89.73(9) . . . yes F5 P F6 178.65(10) . . . yes F1 P F2 178.40(9) . . . yes F1 P F3 89.63(7) . . . yes F1 P F4 90.69(8) . . . yes Cu N1 C11 166.10(13) . . . yes N1 C11 C12 178.41(19) . . . yes P1 C111 C112 118.50(11) . . . yes P1 C111 C116 122.20(12) . . . yes C112 C111 C116 119.06(14) . . . no C111 C112 C113 120.64(15) . . . no C11 C12 H12B 108.7(19) . . . no C11 C12 H12C 105(2) . . . no H12A C12 H12B 108(3) . . . no H12A C12 H12C 115(3) . . . no H12B C12 H12C 107(3) . . . no C11 C12 H12A 112(2) . . . no C112 C113 C114 120.04(16) . . . no C113 C114 C115 119.74(16) . . . no C114 C115 C116 120.51(16) . . . no C111 C116 C115 119.99(16) . . . no P1 C121 C122 117.38(12) . . . yes P1 C121 C126 123.46(12) . . . yes C122 C121 C126 119.10(15) . . . no C121 C122 C123 120.53(16) . . . no C122 C123 C124 119.84(18) . . . no C123 C124 C125 120.07(18) . . . no C124 C125 C126 120.34(17) . . . no C121 C126 C125 120.10(17) . . . no P1 C131 C136 122.14(12) . . . yes C132 C131 C136 118.79(14) . . . no P1 C131 C132 118.74(10) . . . yes C131 C132 C133 120.40(14) . . . no C132 C133 C134 120.23(16) . . . no C133 C134 C135 119.73(17) . . . no C134 C135 C136 120.47(15) . . . no C131 C136 C135 120.30(15) . . . no C212 C211 C216 118.79(14) . . . no P2 C211 C216 122.04(12) . . . yes P2 C211 C212 118.79(11) . . . yes C111 C112 H112 120.7(15) . . . no C113 C112 H112 118.6(15) . . . no C211 C212 C213 120.55(15) . . . no C114 C113 H113 120.9(15) . . . no C212 C213 C214 120.11(17) . . . no C112 C113 H113 119.0(14) . . . no C115 C114 H114 119.5(16) . . . no C113 C114 H114 120.8(16) . . . no C213 C214 C215 119.81(18) . . . no C114 C115 H115 120.9(14) . . . no C116 C115 H115 118.6(14) . . . no C214 C215 C216 120.61(17) . . . no C115 C116 H116 120.0(14) . . . no C211 C216 C215 120.11(16) . . . no C111 C116 H116 120.0(14) . . . no P2 C221 C222 118.82(12) . . . yes P2 C221 C226 121.89(12) . . . yes C222 C221 C226 119.30(15) . . . no C123 C122 H122 120.0(13) . . . no C221 C222 C223 120.39(16) . . . no C121 C122 H122 119.5(13) . . . no C122 C123 H123 120.0(15) . . . no C222 C223 C224 119.85(17) . . . no C124 C123 H123 120.1(15) . . . no C123 C124 H124 119.1(14) . . . no C125 C124 H124 120.7(14) . . . no C223 C224 C225 120.16(16) . . . no C224 C225 C226 120.20(15) . . . no C126 C125 H125 119.9(15) . . . no C124 C125 H125 119.7(15) . . . no C121 C126 H126 119.3(14) . . . no C221 C226 C225 120.09(15) . . . no C125 C126 H126 120.6(14) . . . no P2 C231 C232 117.49(11) . . . yes P2 C231 C236 123.48(12) . . . yes C232 C231 C236 118.96(14) . . . no C131 C132 H132 119.4(13) . . . no C231 C232 C233 120.64(15) . . . no C133 C132 H132 120.2(13) . . . no C232 C233 C234 119.95(16) . . . no C132 C133 H133 118.2(13) . . . no C134 C133 H133 121.6(13) . . . no C233 C234 C235 119.92(17) . . . no C135 C134 H134 119.9(15) . . . no C133 C134 H134 120.4(15) . . . no C134 C135 H135 122.7(14) . . . no C136 C135 H135 116.8(14) . . . no C234 C235 C236 120.45(18) . . . no C231 C236 C235 120.07(16) . . . no C131 C136 H136 120.4(12) . . . no C135 C136 H136 119.3(12) . . . no P3 C311 C316 123.19(12) . . . yes P3 C311 C312 117.97(11) . . . yes C312 C311 C316 118.59(14) . . . no C213 C212 H212 119.2(12) . . . no C211 C212 H212 120.2(12) . . . no C311 C312 C313 120.85(15) . . . no C212 C213 H213 119.6(14) . . . no C214 C213 H213 120.3(15) . . . no C312 C313 C314 120.06(16) . . . no C313 C314 C315 119.82(17) . . . no C215 C214 H214 120.6(15) . . . no C213 C214 H214 119.6(15) . . . no C216 C215 H215 119.5(15) . . . no C314 C315 C316 120.27(17) . . . no C214 C215 H215 119.9(15) . . . no C215 C216 H216 118.9(14) . . . no C211 C216 H216 121.0(13) . . . no C311 C316 C315 120.38(15) . . . no P3 C321 C322 120.81(11) . . . yes C322 C321 C326 118.78(14) . . . no P3 C321 C326 120.26(13) . . . yes C223 C222 H222 118.6(13) . . . no C221 C222 H222 121.0(13) . . . no C321 C322 C323 120.26(16) . . . no C222 C223 H223 119.1(15) . . . no C322 C323 C324 120.43(19) . . . no C224 C223 H223 121.0(15) . . . no C225 C224 H224 118.4(16) . . . no C223 C224 H224 121.4(16) . . . no C323 C324 C325 119.78(18) . . . no C224 C225 H225 122.3(13) . . . no C226 C225 H225 117.5(13) . . . no C324 C325 C326 120.31(19) . . . no C225 C226 H226 120.3(13) . . . no C221 C226 H226 119.6(13) . . . no C321 C326 C325 120.42(17) . . . no P3 C331 C332 117.17(11) . . . yes C332 C331 C336 119.10(14) . . . no P3 C331 C336 123.72(12) . . . yes C233 C232 H232 119.6(13) . . . no C331 C332 C333 120.72(15) . . . no C231 C232 H232 119.8(13) . . . no C232 C233 H233 120.5(15) . . . no C234 C233 H233 119.5(15) . . . no C332 C333 C334 119.67(16) . . . no C233 C234 H234 119.9(14) . . . no C235 C234 H234 120.2(14) . . . no C333 C334 C335 120.13(17) . . . no C234 C235 H235 121.0(18) . . . no C334 C335 C336 120.35(18) . . . no C236 C235 H235 118.5(18) . . . no C331 C336 C335 120.04(17) . . . no C231 C236 H236 120.3(13) . . . no C235 C236 H236 119.6(13) . . . no C313 C312 H312 121.1(13) . . . no C311 C312 H312 118.1(13) . . . no C312 C313 H313 119.9(19) . . . no C314 C313 H313 120.0(19) . . . no C315 C314 H314 119.9(15) . . . no C313 C314 H314 120.2(15) . . . no C314 C315 H315 121.0(15) . . . no C316 C315 H315 118.7(15) . . . no C311 C316 H316 118.2(14) . . . no C315 C316 H316 121.3(14) . . . no N2 C21 C22 177.7(4) . . . yes C321 C322 H322 118.9(14) . . . no C323 C322 H322 120.8(14) . . . no C322 C323 H323 119.4(14) . . . no C324 C323 H323 120.2(14) . . . no C325 C324 H324 119.8(16) . . . no C323 C324 H324 120.4(16) . . . no C326 C325 H325 121.4(16) . . . no C324 C325 H325 118.3(16) . . . no C321 C326 H326 120.4(14) . . . no C325 C326 H326 119.1(14) . . . no C333 C332 H332 121.0(14) . . . no C331 C332 H332 118.2(14) . . . no C332 C333 H333 118.5(15) . . . no C334 C333 H333 121.8(15) . . . no C335 C334 H334 117.6(13) . . . no C333 C334 H334 122.2(13) . . . no C334 C335 H335 120.7(16) . . . no C336 C335 H335 118.9(16) . . . no C331 C336 H336 119.6(13) . . . no C335 C336 H336 120.3(13) . . . no C21 C22 H22A 117(3) . . . no C21 C22 H22B 104(4) . . . no C21 C22 H22C 107.5(19) . . . no H22A C22 H22B 108(5) . . . no H22A C22 H22C 114(4) . . . no H22B C22 H22C 105(5) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Cu P1 C111 -52.09(6) . . . . no P2 Cu P1 C121 -173.14(6) . . . . no P2 Cu P1 C131 65.63(6) . . . . no P3 Cu P1 C111 84.24(6) . . . . no P3 Cu P1 C121 -36.81(6) . . . . no P3 Cu P1 C131 -158.04(5) . . . . no N1 Cu P1 C111 -159.18(7) . . . . no N1 Cu P1 C121 79.77(7) . . . . no N1 Cu P1 C131 -41.46(7) . . . . no P1 Cu P2 C211 57.34(6) . . . . no P1 Cu P2 C221 -64.13(6) . . . . no P1 Cu P2 C231 179.67(6) . . . . no P3 Cu P2 C211 -78.83(6) . . . . no P3 Cu P2 C221 159.70(5) . . . . no P3 Cu P2 C231 43.50(6) . . . . no N1 Cu P2 C211 167.02(7) . . . . no N1 Cu P2 C221 45.55(7) . . . . no N1 Cu P2 C231 -70.65(7) . . . . no P1 Cu P3 C311 -70.51(6) . . . . no P1 Cu P3 C321 171.34(6) . . . . no P1 Cu P3 C331 51.52(5) . . . . no P2 Cu P3 C311 70.24(6) . . . . no P2 Cu P3 C321 -47.91(6) . . . . no P2 Cu P3 C331 -167.73(5) . . . . no N1 Cu P3 C311 177.05(7) . . . . no N1 Cu P3 C321 58.90(7) . . . . no N1 Cu P3 C331 -60.93(7) . . . . no Cu P1 C111 C112 33.03(13) . . . . no Cu P1 C111 C116 -152.69(11) . . . . no C121 P1 C111 C112 160.13(12) . . . . no C121 P1 C111 C116 -25.60(14) . . . . no C131 P1 C111 C112 -90.54(12) . . . . no C131 P1 C111 C116 83.73(13) . . . . no Cu P1 C121 C122 69.20(13) . . . . no Cu P1 C121 C126 -107.91(13) . . . . no C111 P1 C121 C122 -59.35(13) . . . . no C111 P1 C121 C126 123.54(14) . . . . no C131 P1 C121 C122 -165.72(12) . . . . no C131 P1 C121 C126 17.17(15) . . . . no Cu P1 C131 C132 53.69(13) . . . . no Cu P1 C131 C136 -119.61(12) . . . . no C111 P1 C131 C132 -179.85(12) . . . . no C111 P1 C131 C136 6.84(15) . . . . no C121 P1 C131 C132 -72.62(14) . . . . no C121 P1 C131 C136 114.08(13) . . . . no Cu P2 C211 C212 65.24(13) . . . . no Cu P2 C211 C216 -107.60(13) . . . . no C221 P2 C211 C212 -167.78(13) . . . . no C221 P2 C211 C216 19.37(15) . . . . no C231 P2 C211 C212 -61.66(14) . . . . no C231 P2 C211 C216 125.50(13) . . . . no Cu P2 C221 C222 23.82(14) . . . . no Cu P2 C221 C226 -156.29(11) . . . . no C211 P2 C221 C222 -105.09(13) . . . . no C211 P2 C221 C226 74.80(14) . . . . no C231 P2 C221 C222 146.71(13) . . . . no C231 P2 C221 C226 -33.40(15) . . . . no Cu P2 C231 C232 35.96(13) . . . . no Cu P2 C231 C236 -147.24(13) . . . . no C211 P2 C231 C232 165.20(12) . . . . no C211 P2 C231 C236 -18.00(16) . . . . no C221 P2 C231 C232 -87.43(13) . . . . no C221 P2 C231 C236 89.37(15) . . . . no Cu P3 C311 C312 12.27(14) . . . . no Cu P3 C311 C316 -161.92(12) . . . . no C321 P3 C311 C312 139.77(13) . . . . no C321 P3 C311 C316 -34.42(15) . . . . no C331 P3 C311 C312 -113.36(13) . . . . no C331 P3 C311 C316 72.45(15) . . . . no Cu P3 C321 C322 82.39(14) . . . . no Cu P3 C321 C326 -93.23(13) . . . . no C311 P3 C321 C322 -41.26(14) . . . . no C311 P3 C321 C326 143.12(13) . . . . no C331 P3 C321 C322 -151.98(13) . . . . no C331 P3 C321 C326 32.40(15) . . . . no Cu P3 C331 C332 29.88(12) . . . . no Cu P3 C331 C336 -151.05(11) . . . . no C311 P3 C331 C332 154.76(11) . . . . no C311 P3 C331 C336 -26.17(14) . . . . no C321 P3 C331 C332 -98.68(12) . . . . no C321 P3 C331 C336 80.39(14) . . . . no P2 C211 C212 C213 -171.99(14) . . . . no C216 C211 C212 C213 1.1(2) . . . . no P2 C211 C216 C215 171.38(13) . . . . no C212 C211 C216 C215 -1.5(2) . . . . no P1 C111 C116 H116 8.5(16) . . . . no C112 C111 C116 H116 -177.3(16) . . . . no P1 C111 C112 H112 -6.0(17) . . . . no C116 C111 C112 H112 179.6(17) . . . . no C111 C112 C113 H113 -175.6(17) . . . . no C211 C212 C213 C214 0.3(3) . . . . no H112 C112 C113 C114 179.7(17) . . . . no H112 C112 C113 H113 4(2) . . . . no C112 C113 C114 H114 -177.8(16) . . . . no C212 C213 C214 C215 -1.3(3) . . . . no H113 C113 C114 C115 176.6(17) . . . . no H113 C113 C114 H114 -2(2) . . . . no C113 C114 C115 H115 178.6(16) . . . . no H114 C114 C115 H115 -3(2) . . . . no C213 C214 C215 C216 1.0(3) . . . . no H114 C114 C115 C116 177.4(16) . . . . no H115 C115 C116 C111 -179.3(15) . . . . no C114 C115 C116 H116 178.4(16) . . . . no C214 C215 C216 C211 0.5(3) . . . . no H115 C115 C116 H116 -2(2) . . . . no P2 C221 C222 C223 -179.70(14) . . . . no C226 C221 C222 C223 0.4(2) . . . . no C222 C221 C226 C225 -0.7(2) . . . . no C126 C121 C122 H122 179.4(14) . . . . no P1 C121 C126 H126 -3.7(16) . . . . no C122 C121 C126 H126 179.2(15) . . . . no P1 C121 C122 H122 2.2(14) . . . . no P2 C221 C226 C225 179.43(12) . . . . no H122 C122 C123 C124 -178.6(14) . . . . no C121 C122 C123 H123 -177.9(16) . . . . no C221 C222 C223 C224 0.3(3) . . . . no H122 C122 C123 H123 2(2) . . . . no C222 C223 C224 C225 -0.7(3) . . . . no C122 C123 C124 H124 -177.7(16) . . . . no H123 C123 C124 C125 177.8(16) . . . . no H123 C123 C124 H124 1(2) . . . . no H124 C124 C125 H125 0(2) . . . . no H124 C124 C125 C126 176.9(16) . . . . no C223 C224 C225 C226 0.4(3) . . . . no C123 C124 C125 H125 -176.2(17) . . . . no H125 C125 C126 H126 -3(2) . . . . no C224 C225 C226 C221 0.3(2) . . . . no C124 C125 C126 H126 -179.3(16) . . . . no H125 C125 C126 C121 177.0(17) . . . . no C236 C231 C232 C233 -1.0(2) . . . . no P2 C231 C236 C235 -175.82(14) . . . . no C232 C231 C236 C235 0.9(3) . . . . no C132 C131 C136 H136 176.3(15) . . . . no P1 C131 C136 H136 -10.4(15) . . . . no C136 C131 C132 H132 -177.3(15) . . . . no P2 C231 C232 C233 175.91(12) . . . . no P1 C131 C132 H132 9.2(15) . . . . no H132 C132 C133 C134 179.0(16) . . . . no H132 C132 C133 H133 -2(2) . . . . no C231 C232 C233 C234 0.6(2) . . . . no C131 C132 C133 H133 177.7(16) . . . . no H133 C133 C134 C135 179.8(16) . . . . no C132 C133 C134 H134 177.2(19) . . . . no C232 C233 C234 C235 -0.1(3) . . . . no H133 C133 C134 H134 -2(2) . . . . no C233 C234 C235 C236 0.0(3) . . . . no C133 C134 C135 H135 -177.3(17) . . . . no H134 C134 C135 C136 -176.3(18) . . . . no H134 C134 C135 H135 4(3) . . . . no C134 C135 C136 H136 -178.8(15) . . . . no H135 C135 C136 C131 179.1(16) . . . . no H135 C135 C136 H136 1(2) . . . . no C234 C235 C236 C231 -0.4(3) . . . . no P3 C311 C312 H312 5.2(15) . . . . no C316 C311 C312 H312 179.7(15) . . . . no P3 C311 C316 H316 -2.9(16) . . . . no C312 C311 C316 H316 -177.1(16) . . . . no C311 C312 C313 H313 -177(2) . . . . no H312 C312 C313 C314 -178.4(15) . . . . no H312 C312 C313 H313 4(3) . . . . no C312 C313 C314 H314 176.2(18) . . . . no H313 C313 C314 C315 176(2) . . . . no H313 C313 C314 H314 -7(3) . . . . no C313 C314 C315 H315 -179.9(18) . . . . no H314 C314 C315 C316 -176.4(18) . . . . no H314 C314 C315 H315 3(3) . . . . no C314 C315 C316 H316 175.8(16) . . . . no H315 C315 C316 C311 -178.8(18) . . . . no H315 C315 C316 H316 -3(2) . . . . no P3 C321 C322 H322 2.4(15) . . . . no C326 C321 C322 H322 178.0(15) . . . . no P3 C321 C326 H326 -2.0(16) . . . . no C322 C321 C326 H326 -177.7(16) . . . . no C321 C322 C323 H323 -179.8(16) . . . . no H322 C322 C323 C324 -177.9(16) . . . . no H322 C322 C323 H323 1(2) . . . . no C322 C323 C324 H324 177.2(17) . . . . no H323 C323 C324 C325 -179.2(16) . . . . no H323 C323 C324 H324 -2(2) . . . . no C323 C324 C325 H325 178.9(16) . . . . no H324 C324 C325 C326 -178.3(17) . . . . no H324 C324 C325 H325 1(2) . . . . no C324 C325 C326 H326 178.7(16) . . . . no H325 C325 C326 C321 -178.8(16) . . . . no H325 C325 C326 H326 -1(2) . . . . no P3 C331 C332 H332 -3.1(15) . . . . no C336 C331 C332 H332 177.8(15) . . . . no P3 C331 C336 H336 3.6(14) . . . . no C332 C331 C336 H336 -177.4(14) . . . . no C331 C332 C333 H333 179.6(16) . . . . no H332 C332 C333 C334 -177.9(16) . . . . no H332 C332 C333 H333 2(2) . . . . no C332 C333 C334 H334 179.5(16) . . . . no H333 C333 C334 C335 -179.4(16) . . . . no H333 C333 C334 H334 0(2) . . . . no C333 C334 C335 H335 178.4(17) . . . . no H334 C334 C335 C336 -179.6(16) . . . . no H334 C334 C335 H335 -1(2) . . . . no C334 C335 C336 H336 177.6(14) . . . . no H335 C335 C336 C331 -178.6(17) . . . . no H335 C335 C336 H336 -1(2) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cu H112 3.29(2) . . no Cu H132 3.56(2) . . no Cu H222 3.10(2) . . no Cu H232 3.17(2) . . no Cu H312 2.89(2) . . no Cu H332 3.06(2) . . no P1 H312 3.20(2) . . no F1 C12 3.339(3) . . no F1 C11 3.213(2) . . no F2 C213 3.359(3) . 1_445 no F2 C225 3.309(3) . 1_545 no F3 C324 3.331(3) . 2_555 no F4 C114 3.230(2) . 2_656 no F4 C115 3.329(2) . 2_656 no F5 C22 3.327(5) . . no F6 C12 3.259(3) . . no F6 C134 3.345(2) . 2_556 no F1 H132 2.67(2) . . no F1 H324 2.76(3) . 2_555 no F1 H12A 2.74(4) . . no F2 H22B 2.85(6) . . no F2 H225 2.45(2) . 1_545 no F2 H213 2.67(2) . 1_445 no F3 H22B 2.76(6) . . no F3 H123 2.70(2) . 1_455 no F3 H12A 2.65(4) . . no F3 H324 2.65(3) . 2_555 no F4 H114 2.69(2) . 2_656 no F5 H22B 2.70(6) . . no F6 H12A 2.54(4) . . no F6 H134 2.56(3) . 2_556 no F6 H133 2.83(2) . . no N1 C132 3.297(2) . . no N1 H232 2.72(2) . . no N1 H132 2.71(2) . . no N1 H332 2.76(2) . . no N1 H325 2.79(2) . 2_555 no N2 H322 2.82(2) . 1_445 no C11 F1 3.213(2) . . no C11 C132 3.300(2) . . no C11 C314 3.596(3) . 1_455 no C11 C325 3.421(2) . 2_555 no C12 C314 3.499(3) . 1_455 no C12 F6 3.259(3) . . no C12 C313 3.420(3) . 1_455 no C12 F1 3.339(3) . . no C12 C324 3.583(3) . 2_555 no C22 F5 3.327(5) . . no C11 H325 2.77(2) . 2_555 no C11 H132 2.66(2) . . no C112 C136 3.523(2) . . no C114 F4 3.230(2) . 2_656 no C115 F4 3.329(2) . 2_656 no C116 C136 3.538(2) . . no C116 C122 3.325(2) . . no C121 C332 3.476(2) . . no C122 C332 3.373(2) . . no C122 C331 3.293(2) . . no C122 C116 3.325(2) . . no C123 C333 3.585(3) . . no C123 C335 3.572(3) . . no C123 C334 3.545(3) . . no C124 C333 3.529(3) . . no C126 C132 3.354(2) . . no C132 N1 3.297(2) . . no C132 C126 3.354(2) . . no C132 C11 3.300(2) . . no C134 F6 3.345(2) . 2_556 no C135 C214 3.597(3) . 2_666 no C136 C112 3.523(2) . . no C136 C116 3.538(2) . . no C111 H136 2.53(2) . . no C111 H312 2.90(2) . . no C111 H122 3.02(2) . . no C112 H312 2.77(2) . . no C112 H136 2.92(2) . . no C212 C312 3.310(2) . . no C212 C236 3.365(2) . . no C212 C313 3.554(3) . . no C213 F2 3.359(3) . 1_665 no C113 H224 3.07(2) . 1_655 no C213 C313 3.521(3) . . no C214 C135 3.597(3) . 2_666 no C115 H126 3.03(2) . 2_656 no C116 H136 2.88(2) . . no C216 C226 3.565(2) . . no C121 H116 2.68(2) . . no C122 H116 2.87(2) . . no C123 H135 3.02(2) . 2_656 no C124 H135 2.89(2) . 2_656 no C224 C224 3.426(2) . 2_566 no C225 F2 3.309(3) . 1_565 no C226 C236 3.500(2) . . no C226 C216 3.565(2) . . no C126 H132 3.08(2) . . no C131 H126 2.73(2) . . no C231 C322 3.524(2) . . no C131 H222 2.74(2) . . no C232 C322 3.309(2) . . no C232 C314 3.564(2) . 1_455 no C232 C321 3.436(2) . . no C132 H222 2.85(2) . . no C132 H126 2.65(2) . . no C233 C323 3.334(3) . . no C133 H115 2.96(2) . 2_656 no C133 H134 3.06(3) . 2_556 no C233 C322 3.572(2) . . no C233 C324 3.472(3) . . no C234 C323 3.510(3) . . no C134 H133 2.97(2) . 2_556 no C135 H116 3.06(3) . 2_656 no C135 H214 3.05(2) . 2_666 no C236 C212 3.365(2) . . no C236 C226 3.500(2) . . no C211 H112 2.77(2) . . no C211 H236 2.70(2) . . no C212 H236 2.85(2) . . no C312 C212 3.310(2) . . no C313 C213 3.521(3) . . no C313 C212 3.554(3) . . no C213 H124 2.87(3) . 1_565 no C313 C12 3.420(3) . 1_655 no C214 H135 3.04(2) . 2_666 no C314 C232 3.564(2) . 1_655 no C214 H124 3.03(3) . 1_565 no C314 C12 3.499(3) . 1_655 no C314 C11 3.596(3) . 1_655 no C215 H113 3.06(3) . . no C316 C336 3.464(3) . . no C216 H112 2.79(2) . . no C316 C322 3.173(2) . . no C321 C232 3.436(2) . . no C221 H216 2.64(2) . . no C322 C232 3.309(2) . . no C322 C316 3.173(2) . . no C322 C233 3.572(2) . . no C322 C231 3.524(2) . . no C323 C234 3.510(3) . . no C323 C233 3.334(3) . . no C324 F3 3.331(3) . 2_555 no C324 C233 3.472(3) . . no C324 C12 3.583(3) . 2_555 no C224 H224 2.92(2) . 2_566 no C224 H313 2.81(3) . 1_455 no C225 H313 3.05(3) . 1_455 no C325 C11 3.421(2) . 2_555 no C225 H114 2.92(2) . 2_666 no C325 C326 3.507(3) . 2_555 no C226 H216 3.04(2) . . no C326 C332 3.569(2) . . no C226 H314 3.04(2) . 1_455 no C326 C325 3.507(3) . 2_555 no C231 H226 2.74(2) . . no C331 C122 3.293(2) . . no C232 H314 2.83(2) . 1_455 no C332 C122 3.373(2) . . no C332 C326 3.569(2) . . no C332 C121 3.476(2) . . no C333 C124 3.529(3) . . no C333 C123 3.585(3) . . no C233 H315 3.02(2) . 1_455 no C334 C123 3.545(3) . . no C335 C123 3.572(3) . . no C236 H226 2.79(2) . . no C336 C316 3.464(3) . . no C311 H336 2.85(2) . . no C311 H322 2.79(2) . . no C312 H212 2.91(2) . . no C313 H12B 3.04(3) . 1_655 no C313 H12C 2.98(4) . 1_655 no C314 H12B 2.97(3) . 1_655 no C315 H12B 2.97(3) . 1_655 no C316 H336 2.73(2) . . no C316 H12B 3.06(3) . 1_655 no C316 H322 2.84(2) . . no C321 H316 2.79(2) . . no C322 H316 2.86(2) . . no C323 H335 3.02(2) . 2_655 no C325 H326 3.02(2) . 2_555 no C326 H325 3.04(2) . 2_555 no C331 H326 2.68(2) . . no C332 H326 2.86(3) . . no C336 H316 3.07(2) . 2_655 no H12A F1 2.74(4) . . no H12A F6 2.54(4) . . no H12A F3 2.65(4) . . no H12B C315 2.97(3) . 1_455 no H12B C316 3.06(3) . 1_455 no H12B C314 2.97(3) . 1_455 no H12B C313 3.04(3) . 1_455 no H12C C313 2.98(4) . 1_455 no H22B F2 2.85(6) . . no H22B F5 2.70(6) . . no H22B F3 2.76(6) . . no H112 C211 2.77(2) . . no H112 Cu 3.29(2) . . no H112 C216 2.79(2) . . no H113 C215 3.06(3) . . no H114 C225 2.92(2) . 2_666 no H114 F4 2.69(2) . 2_656 no H115 H134 2.54(3) . 1_655 no H115 C133 2.96(2) . 2_656 no H116 C121 2.68(2) . . no H116 C122 2.87(2) . . no H116 C135 3.06(3) . 2_656 no H122 C111 3.02(2) . . no H123 F3 2.70(2) . 1_655 no H124 C213 2.87(3) . 1_545 no H124 C214 3.03(3) . 1_545 no H126 C132 2.65(2) . . no H126 C131 2.73(2) . . no H126 H132 2.45(3) . . no H126 C115 3.03(2) . 2_656 no H132 F1 2.67(2) . . no H132 Cu 3.56(2) . . no H132 C126 3.08(2) . . no H132 N1 2.71(2) . . no H132 C11 2.66(2) . . no H132 H126 2.45(3) . . no H133 H134 2.48(4) . 2_556 no H133 F6 2.83(2) . . no H133 C134 2.97(2) . 2_556 no H134 F6 2.56(3) . 2_556 no H134 H115 2.54(3) . 1_455 no H134 H133 2.48(4) . 2_556 no H134 C133 3.06(3) . 2_556 no H135 C123 3.02(2) . 2_656 no H135 H214 2.58(3) . 2_666 no H135 C124 2.89(2) . 2_656 no H135 C214 3.04(2) . 2_666 no H136 C111 2.53(2) . . no H136 C116 2.88(2) . . no H136 C112 2.92(2) . . no H212 C312 2.91(2) . . no H213 F2 2.67(2) . 1_665 no H214 H135 2.58(3) . 2_666 no H214 C135 3.05(2) . 2_666 no H216 C226 3.04(2) . . no H216 C221 2.64(2) . . no H222 C131 2.74(2) . . no H222 C132 2.85(2) . . no H222 Cu 3.10(2) . . no H224 C224 2.92(2) . 2_566 no H224 C113 3.07(2) . 1_455 no H225 F2 2.45(2) . 1_565 no H226 C231 2.74(2) . . no H226 C236 2.79(2) . . no H232 Cu 3.17(2) . . no H232 N1 2.72(2) . . no H233 H315 2.53(3) . 1_455 no H234 H235 2.56(4) . 2_565 no H235 H334 2.53(4) . 1_565 no H235 H234 2.56(4) . 2_565 no H236 C211 2.70(2) . . no H236 C212 2.85(2) . . no H312 Cu 2.89(2) . . no H312 C112 2.77(2) . . no H312 P1 3.20(2) . . no H312 C111 2.90(2) . . no H313 C224 2.81(3) . 1_655 no H313 C225 3.05(3) . 1_655 no H314 C232 2.83(2) . 1_655 no H314 C226 3.04(2) . 1_655 no H315 C233 3.02(2) . 1_655 no H315 H233 2.53(3) . 1_655 no H316 C321 2.79(2) . . no H316 C336 3.07(2) . 2_655 no H316 C322 2.86(2) . . no H316 H336 2.47(3) . . no H322 C311 2.79(2) . . no H322 N2 2.82(2) . 1_665 no H322 C316 2.84(2) . . no H324 F3 2.65(3) . 2_555 no H324 F1 2.76(3) . 2_555 no H325 C326 3.04(2) . 2_555 no H325 N1 2.79(2) . 2_555 no H325 C11 2.77(2) . 2_555 no H326 C331 2.68(2) . . no H326 C332 2.86(3) . . no H326 C325 3.02(2) . 2_555 no H332 Cu 3.06(2) . . no H332 N1 2.76(2) . . no H334 H235 2.53(4) . 1_545 no H335 C323 3.02(2) . 2_655 no H336 H316 2.47(3) . . no H336 C311 2.85(2) . . no H336 C316 2.73(2) . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C12 H12A F6 0.85(4) 2.54(4) 3.259(3) 143(3) . yes C225 H225 F2 0.96(2) 2.45(2) 3.309(3) 149.8(18) 1_565 yes #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? _exptl_crystal_F_000 1112 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min -21 _reflns_limit_k_max 21 _reflns_limit_l_min -31 _reflns_limit_l_max 29 _reflns_number_observed ? _reflns_d_resolution_high .625 _reflns_d_resolution_low 12.69 _diffrn_reflns_av_sigmaI/netI .062 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_reduction_process ? _diffrn_ambient_temperature 150 _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'CCD area detector' _refine_ls_extinction_expression ? _refine_ls_matrix_type full _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .062 _refine_ls_wR_factor_all .053 _refine_ls_goodness_of_fit_all .988 _refine_ls_shift/su_mean .0003 #==========================================================================