# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email Koen.Binnemans@chem.kuleuven.be _publ_contact_author_name 'Koen Binnemans' _publ_author_name 'Koen Binnemans' data_kb16o _database_code_depnum_ccdc_archive 'CCDC 883549' #TrackingRef 'kb16o-[Cu-BuIm-4][Tf2N]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(N-methylimidazole)copper(II) bis(trifluoromethyl)sulfonylimide ; _chemical_name_common ; tetrakis(N-methylimidazole)copper(II) bistriflimide ; _chemical_melting_point 319 _chemical_formula_moiety 'C32 H48 Cu F12 N10 O8 S4' _chemical_formula_sum 'C32 H48 Cu F12 N10 O8 S4' _chemical_formula_weight 1120.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0369(6) _cell_length_b 24.0453(9) _cell_length_c 25.0434(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.651(2) _cell_angle_gamma 90.00 _cell_volume 9656.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9328 _cell_measurement_theta_min 2.548 _cell_measurement_theta_max 71.136 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4600 _exptl_absorpt_coefficient_mu 3.181 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.363 _exptl_absorpt_correction_T_max 0.742 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 81446 _diffrn_reflns_av_R_equivalents 0.0800 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 66.59 _reflns_number_total 17049 _reflns_number_gt 13480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ; A.L.Spek (2010) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+14.4485P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17049 _refine_ls_number_parameters 1302 _refine_ls_number_restraints 310 _refine_ls_R_factor_all 0.0764 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1365 _refine_ls_wR_factor_gt 0.1278 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.51304(3) 0.24123(2) 0.24790(2) 0.02295(12) Uani 1 1 d . . . Cu2 Cu 0.00114(3) 0.24496(2) 0.24289(2) 0.02630(13) Uani 1 1 d . A . N1 N 0.59543(19) 0.29238(12) 0.21507(12) 0.0248(6) Uani 1 1 d . . . C2 C 0.5913(2) 0.34778(15) 0.21439(14) 0.0255(8) Uani 1 1 d . . . H2 H 0.5489 0.3690 0.2309 0.031 Uiso 1 1 calc R . . N3 N 0.6552(2) 0.36943(12) 0.18717(12) 0.0259(7) Uani 1 1 d . . . C4 C 0.7021(2) 0.32557(15) 0.16870(15) 0.0272(8) Uani 1 1 d . . . H4 H 0.7508 0.3279 0.1476 0.033 Uiso 1 1 calc R . . C5 C 0.6652(2) 0.27856(15) 0.18635(15) 0.0283(8) Uani 1 1 d . . . H5 H 0.6844 0.2418 0.1800 0.034 Uiso 1 1 calc R . . C6 C 0.6656(2) 0.42848(15) 0.17357(16) 0.0301(8) Uani 1 1 d . . . H6A H 0.7238 0.4399 0.1813 0.036 Uiso 1 1 calc R . . H6B H 0.6283 0.4513 0.1960 0.036 Uiso 1 1 calc R . . C7 C 0.6455(2) 0.43893(16) 0.11480(16) 0.0304(8) Uani 1 1 d . . . H7A H 0.6509 0.4792 0.1074 0.036 Uiso 1 1 calc R . . H7B H 0.6868 0.4191 0.0927 0.036 Uiso 1 1 calc R . . C8 C 0.5584(3) 0.42003(17) 0.09843(15) 0.0323(9) Uani 1 1 d . . . H8A H 0.5169 0.4402 0.1200 0.039 Uiso 1 1 calc R . . H8B H 0.5526 0.3798 0.1062 0.039 Uiso 1 1 calc R . . C9 C 0.5399(3) 0.43009(19) 0.03956(16) 0.0393(10) Uani 1 1 d . . . H9A H 0.5780 0.4078 0.0179 0.059 Uiso 1 1 calc R . . H9B H 0.5476 0.4696 0.0314 0.059 Uiso 1 1 calc R . . H9C H 0.4823 0.4193 0.0314 0.059 Uiso 1 1 calc R . . N10 N 0.4204(2) 0.28794(13) 0.21959(12) 0.0255(6) Uani 1 1 d . . . C11 C 0.4021(2) 0.29693(15) 0.16852(15) 0.0277(8) Uani 1 1 d . . . H11 H 0.4315 0.2812 0.1395 0.033 Uiso 1 1 calc R . . N12 N 0.3368(2) 0.33106(13) 0.16330(12) 0.0286(7) Uani 1 1 d . . . C13 C 0.3123(3) 0.34538(17) 0.21370(16) 0.0331(9) Uani 1 1 d . . . H13 H 0.2679 0.3695 0.2229 0.040 Uiso 1 1 calc R . . C14 C 0.3641(2) 0.31827(17) 0.24751(15) 0.0326(9) Uani 1 1 d . . . H14 H 0.3616 0.3201 0.2854 0.039 Uiso 1 1 calc R . . C15 C 0.2977(3) 0.34833(17) 0.11263(16) 0.0348(9) Uani 1 1 d . . . H15A H 0.2370 0.3409 0.1142 0.042 Uiso 1 1 calc R . . H15B H 0.3207 0.3256 0.0834 0.042 Uiso 1 1 calc R . . C16 C 0.3108(2) 0.40878(16) 0.09995(15) 0.0292(8) Uani 1 1 d . . . H16A H 0.3714 0.4168 0.0995 0.035 Uiso 1 1 calc R . . H16B H 0.2855 0.4319 0.1282 0.035 Uiso 1 1 calc R . . C17 C 0.2722(3) 0.42421(17) 0.04601(16) 0.0369(9) Uani 1 1 d . . . H17A H 0.3001 0.4027 0.0176 0.044 Uiso 1 1 calc R . . H17B H 0.2125 0.4137 0.0457 0.044 Uiso 1 1 calc R . . C18 C 0.2798(3) 0.48562(19) 0.03379(18) 0.0469(11) Uani 1 1 d . . . H18A H 0.2551 0.4933 -0.0014 0.070 Uiso 1 1 calc R . . H18B H 0.3388 0.4962 0.0339 0.070 Uiso 1 1 calc R . . H18C H 0.2504 0.5071 0.0610 0.070 Uiso 1 1 calc R . . N19 N 0.42961(19) 0.19026(12) 0.28031(12) 0.0245(6) Uani 1 1 d . . . C20 C 0.4305(2) 0.17296(15) 0.33015(15) 0.0280(8) Uani 1 1 d . . . H20 H 0.4736 0.1810 0.3553 0.034 Uiso 1 1 calc R . . N21 N 0.3630(2) 0.14260(13) 0.34096(13) 0.0302(7) Uani 1 1 d . . . C22 C 0.3156(3) 0.14027(16) 0.29502(17) 0.0359(9) Uani 1 1 d . . . H22 H 0.2638 0.1216 0.2904 0.043 Uiso 1 1 calc R . . C23 C 0.3570(2) 0.16964(16) 0.25758(16) 0.0313(8) Uani 1 1 d . . . H23 H 0.3392 0.1752 0.2217 0.038 Uiso 1 1 calc R . . C24 C 0.3393(3) 0.12182(17) 0.39366(17) 0.0386(10) Uani 1 1 d . . . H24A H 0.3902 0.1124 0.4145 0.046 Uiso 1 1 calc R . . H24B H 0.3059 0.0875 0.3893 0.046 Uiso 1 1 calc R . . C25 C 0.2890(2) 0.16476(17) 0.42393(15) 0.0310(8) Uani 1 1 d . . . H25A H 0.2382 0.1739 0.4029 0.037 Uiso 1 1 calc R . . H25B H 0.3225 0.1992 0.4276 0.037 Uiso 1 1 calc R . . C26 C 0.2637(3) 0.14510(18) 0.47907(17) 0.0400(10) Uani 1 1 d . . . H26A H 0.2274 0.1120 0.4754 0.048 Uiso 1 1 calc R . . H26B H 0.3141 0.1341 0.4996 0.048 Uiso 1 1 calc R . . C27 C 0.2177(4) 0.1900(2) 0.50941(19) 0.0532(13) Uani 1 1 d . . . H27A H 0.1684 0.2017 0.4888 0.080 Uiso 1 1 calc R . . H27B H 0.2546 0.2220 0.5150 0.080 Uiso 1 1 calc R . . H27C H 0.2002 0.1754 0.5440 0.080 Uiso 1 1 calc R . . N28 N 0.60438(19) 0.19423(12) 0.27789(12) 0.0246(6) Uani 1 1 d . . . C29 C 0.6079(2) 0.13926(15) 0.27950(15) 0.0281(8) Uani 1 1 d . . . H29 H 0.5697 0.1153 0.2615 0.034 Uiso 1 1 calc R . . N30 N 0.67268(19) 0.12165(13) 0.30996(12) 0.0260(7) Uani 1 1 d . . . C31 C 0.7125(2) 0.16818(16) 0.32916(14) 0.0268(8) Uani 1 1 d . . . H31 H 0.7605 0.1691 0.3517 0.032 Uiso 1 1 calc R . . C32 C 0.6699(2) 0.21244(15) 0.30958(14) 0.0251(8) Uani 1 1 d . . . H32 H 0.6831 0.2503 0.3166 0.030 Uiso 1 1 calc R . . C33 C 0.6896(3) 0.06364(16) 0.32579(16) 0.0353(9) Uani 1 1 d . . . H33A H 0.7488 0.0548 0.3189 0.042 Uiso 1 1 calc R . . H33B H 0.6547 0.0383 0.3039 0.042 Uiso 1 1 calc R . . C34 C 0.6713(3) 0.05422(16) 0.38487(16) 0.0350(9) Uani 1 1 d . . . H34A H 0.6815 0.0146 0.3936 0.042 Uiso 1 1 calc R . . H34B H 0.7105 0.0768 0.4066 0.042 Uiso 1 1 calc R . . C35 C 0.5826(3) 0.06902(16) 0.40022(15) 0.0311(8) Uani 1 1 d . . . H35A H 0.5732 0.1091 0.3934 0.037 Uiso 1 1 calc R . . H35B H 0.5432 0.0479 0.3772 0.037 Uiso 1 1 calc R . . C36 C 0.5639(3) 0.05661(19) 0.45836(18) 0.0449(11) Uani 1 1 d . . . H36A H 0.5049 0.0639 0.4652 0.067 Uiso 1 1 calc R . . H36B H 0.5985 0.0804 0.4814 0.067 Uiso 1 1 calc R . . H36C H 0.5764 0.0175 0.4660 0.067 Uiso 1 1 calc R . . N37 N -0.0838(2) 0.27191(13) 0.29410(12) 0.0281(7) Uani 1 1 d . A . C38 C -0.1457(2) 0.30595(16) 0.28344(15) 0.0291(8) Uani 1 1 d . A . H38 H -0.1610 0.3178 0.2485 0.035 Uiso 1 1 calc R . . N39 N -0.1844(2) 0.32176(13) 0.32769(13) 0.0310(7) Uani 1 1 d D . . C40 C -0.1453(3) 0.2960(2) 0.36950(16) 0.0433(11) Uani 1 1 d . A . H40 H -0.1590 0.2989 0.4062 0.052 Uiso 1 1 calc R . . C41 C -0.0829(3) 0.2653(2) 0.34826(16) 0.0396(10) Uani 1 1 d . . . H41 H -0.0447 0.2428 0.3679 0.048 Uiso 1 1 calc R A . C42 C -0.2523(4) 0.3624(3) 0.3295(5) 0.0472(16) Uani 0.764(6) 1 d PDU A 1 H42A H -0.2814 0.3592 0.3641 0.057 Uiso 0.764(6) 1 calc PR A 1 H42B H -0.2932 0.3543 0.3006 0.057 Uiso 0.764(6) 1 calc PR A 1 C43 C -0.2200(4) 0.4203(2) 0.3232(3) 0.0532(15) Uani 0.764(6) 1 d PDU A 1 H43A H -0.1782 0.4279 0.3516 0.064 Uiso 0.764(6) 1 calc PR A 1 H43B H -0.1917 0.4235 0.2884 0.064 Uiso 0.764(6) 1 calc PR A 1 C44 C -0.2873(5) 0.4625(2) 0.3259(3) 0.0555(17) Uani 0.764(6) 1 d PDU A 1 H44A H -0.3116 0.4615 0.3620 0.067 Uiso 0.764(6) 1 calc PR A 1 H44B H -0.3319 0.4521 0.3001 0.067 Uiso 0.764(6) 1 calc PR A 1 C45 C -0.2605(6) 0.5203(3) 0.3144(3) 0.073(2) Uani 0.764(6) 1 d PDU A 1 H45A H -0.3085 0.5454 0.3168 0.110 Uiso 0.764(6) 1 calc PR A 1 H45B H -0.2376 0.5222 0.2783 0.110 Uiso 0.764(6) 1 calc PR A 1 H45C H -0.2176 0.5316 0.3404 0.110 Uiso 0.764(6) 1 calc PR A 1 C42' C -0.2554(12) 0.3591(12) 0.3359(18) 0.0472(16) Uani 0.236(6) 1 d PDU A 2 H42C H -0.3024 0.3372 0.3501 0.057 Uiso 0.236(6) 1 calc PR A 2 H42D H -0.2732 0.3745 0.3009 0.057 Uiso 0.236(6) 1 calc PR A 2 C43' C -0.2376(14) 0.4061(8) 0.3730(9) 0.059(3) Uani 0.236(6) 1 d PDU A 2 H43C H -0.2893 0.4277 0.3788 0.071 Uiso 0.236(6) 1 calc PR A 2 H43D H -0.2186 0.3913 0.4080 0.071 Uiso 0.236(6) 1 calc PR A 2 C44' C -0.1727(15) 0.4431(9) 0.3511(10) 0.066(3) Uani 0.236(6) 1 d PDU A 2 H44C H -0.1383 0.4194 0.3277 0.079 Uiso 0.236(6) 1 calc PR A 2 H44D H -0.1364 0.4535 0.3818 0.079 Uiso 0.236(6) 1 calc PR A 2 C45' C -0.188(2) 0.4955(11) 0.3208(13) 0.092(6) Uani 0.236(6) 1 d PDU A 2 H45D H -0.1352 0.5103 0.3080 0.138 Uiso 0.236(6) 1 calc PR A 2 H45E H -0.2147 0.5228 0.3442 0.138 Uiso 0.236(6) 1 calc PR A 2 H45F H -0.2252 0.4877 0.2903 0.138 Uiso 0.236(6) 1 calc PR A 2 N46 N 0.0916(2) 0.27403(13) 0.29036(13) 0.0290(7) Uani 1 1 d . . . C47 C 0.1059(2) 0.32618(16) 0.30342(15) 0.0298(8) Uani 1 1 d . . . H47 H 0.0710 0.3565 0.2935 0.036 Uiso 1 1 calc R . . N48 N 0.1765(2) 0.33103(13) 0.33272(13) 0.0297(7) Uani 1 1 d . . . C49 C 0.2084(3) 0.27845(17) 0.33889(17) 0.0348(9) Uani 1 1 d . . . H49 H 0.2576 0.2684 0.3580 0.042 Uiso 1 1 calc R . . C50 C 0.1561(3) 0.24394(17) 0.31248(17) 0.0359(9) Uani 1 1 d . . . H50 H 0.1628 0.2048 0.3096 0.043 Uiso 1 1 calc R . . C51 C 0.2128(3) 0.38250(17) 0.35432(16) 0.0342(9) Uani 1 1 d . . . H51A H 0.1787 0.4146 0.3424 0.041 Uiso 1 1 calc R . . H51B H 0.2697 0.3874 0.3401 0.041 Uiso 1 1 calc R . . C52 C 0.2170(3) 0.3815(2) 0.41544(17) 0.0444(11) Uani 1 1 d . . . H52A H 0.2552 0.3513 0.4268 0.053 Uiso 1 1 calc R . . H52B H 0.2415 0.4171 0.4280 0.053 Uiso 1 1 calc R . . C53 C 0.1345(4) 0.3733(2) 0.44249(19) 0.0552(13) Uani 1 1 d . . . H53A H 0.1090 0.3384 0.4291 0.066 Uiso 1 1 calc R . . H53B H 0.1445 0.3689 0.4813 0.066 Uiso 1 1 calc R . . C54 C 0.0736(4) 0.4202(3) 0.4337(3) 0.0717(17) Uani 1 1 d . . . H54A H 0.0603 0.4233 0.3956 0.107 Uiso 1 1 calc R . . H54B H 0.0985 0.4551 0.4463 0.107 Uiso 1 1 calc R . . H54C H 0.0225 0.4128 0.4536 0.107 Uiso 1 1 calc R . . N55 N -0.08722(19) 0.21316(13) 0.19581(12) 0.0257(7) Uani 1 1 d . . . C56 C -0.0890(2) 0.21251(16) 0.14286(15) 0.0275(8) Uani 1 1 d . . . H56 H -0.0487 0.2297 0.1208 0.033 Uiso 1 1 calc R . . N57 N -0.15553(19) 0.18417(13) 0.12480(12) 0.0258(6) Uani 1 1 d . . . C58 C -0.1975(2) 0.16423(15) 0.16853(14) 0.0252(7) Uani 1 1 d . . . H58 H -0.2464 0.1419 0.1683 0.030 Uiso 1 1 calc R . . C59 C -0.1549(2) 0.18302(16) 0.21193(14) 0.0270(8) Uani 1 1 d . . . H59 H -0.1697 0.1763 0.2480 0.032 Uiso 1 1 calc R . . C60 C -0.1720(3) 0.16988(17) 0.06858(15) 0.0325(9) Uani 1 1 d . . . H60A H -0.1372 0.1935 0.0453 0.039 Uiso 1 1 calc R . . H60B H -0.2313 0.1773 0.0597 0.039 Uiso 1 1 calc R . . C61 C -0.1527(3) 0.10939(18) 0.05827(16) 0.0387(10) Uani 1 1 d . . . H61A H -0.1618 0.1013 0.0199 0.046 Uiso 1 1 calc R . . H61B H -0.1917 0.0860 0.0788 0.046 Uiso 1 1 calc R . . C62 C -0.0633(3) 0.09381(18) 0.07371(17) 0.0406(10) Uani 1 1 d . . . H62A H -0.0244 0.1175 0.0534 0.049 Uiso 1 1 calc R . . H62B H -0.0544 0.1017 0.1121 0.049 Uiso 1 1 calc R . . C63 C -0.0433(4) 0.0336(2) 0.0632(2) 0.0589(14) Uani 1 1 d . . . H63A H -0.0552 0.0249 0.0256 0.088 Uiso 1 1 calc R . . H63B H -0.0776 0.0099 0.0861 0.088 Uiso 1 1 calc R . . H63C H 0.0158 0.0268 0.0710 0.088 Uiso 1 1 calc R . . N64 N 0.0879(2) 0.21925(13) 0.19297(13) 0.0281(7) Uani 1 1 d . . . C65 C 0.0986(3) 0.16762(18) 0.17748(19) 0.0417(11) Uani 1 1 d . . . H65 H 0.0625 0.1376 0.1860 0.050 Uiso 1 1 calc R . . N66 N 0.1678(2) 0.16304(15) 0.14785(15) 0.0423(9) Uani 1 1 d . . . C67 C 0.1996(3) 0.2146(2) 0.14215(17) 0.0423(11) Uani 1 1 d . . . H67 H 0.2472 0.2247 0.1221 0.051 Uiso 1 1 calc R . . C68 C 0.1505(3) 0.24904(19) 0.17044(17) 0.0408(10) Uani 1 1 d . . . H68 H 0.1584 0.2880 0.1741 0.049 Uiso 1 1 calc R . . C69 C 0.2005(5) 0.1106(2) 0.1260(3) 0.079(2) Uani 1 1 d . . . H69A H 0.1665 0.0795 0.1397 0.095 Uiso 1 1 calc R . . H69B H 0.2582 0.1053 0.1395 0.095 Uiso 1 1 calc R . . C70 C 0.2011(3) 0.1077(2) 0.0669(2) 0.0554(13) Uani 1 1 d . . . H70A H 0.2368 0.1378 0.0530 0.066 Uiso 1 1 calc R . . H70B H 0.1437 0.1138 0.0531 0.066 Uiso 1 1 calc R . . C71 C 0.2330(4) 0.0519(3) 0.0466(3) 0.0774(19) Uani 1 1 d . . . H71A H 0.2875 0.0438 0.0638 0.093 Uiso 1 1 calc R . . H71B H 0.1936 0.0223 0.0572 0.093 Uiso 1 1 calc R . . C72 C 0.2431(5) 0.0503(3) -0.0131(3) 0.106(3) Uani 1 1 d . . . H72A H 0.2269 0.0863 -0.0283 0.159 Uiso 1 1 calc R . . H72B H 0.2075 0.0210 -0.0282 0.159 Uiso 1 1 calc R . . H72C H 0.3015 0.0425 -0.0216 0.159 Uiso 1 1 calc R . . C73 C 0.1258(3) 0.01057(17) 0.24854(16) 0.0380(10) Uani 0.8911(19) 1 d PDU B 1 F74 F 0.1486(2) -0.01848(14) 0.29116(13) 0.0616(9) Uani 0.8911(19) 1 d PDU B 1 F75 F 0.1558(2) -0.01442(12) 0.20546(12) 0.0520(8) Uani 0.8911(19) 1 d PDU B 1 F76 F 0.15969(19) 0.06075(13) 0.25181(12) 0.0436(8) Uani 0.8911(19) 1 d PDU B 1 S77 S 0.01238(7) 0.01581(4) 0.24301(4) 0.0292(3) Uani 0.8911(19) 1 d PDU B 1 O78 O -0.0136(3) -0.04074(13) 0.23704(14) 0.0467(9) Uani 0.8911(19) 1 d PDU B 1 O79 O -0.0005(2) 0.05323(16) 0.19926(13) 0.0337(8) Uani 0.8911(19) 1 d PDU B 1 C73' C 0.0021(10) 0.0252(8) 0.2039(5) 0.034(5) Uani 0.1089(19) 1 d PDU B 2 F74' F -0.0625(14) -0.0092(9) 0.1974(9) 0.062(7) Uani 0.1089(19) 1 d PDU B 2 F75' F 0.0549(15) 0.0133(9) 0.1648(9) 0.062(7) Uani 0.1089(19) 1 d PDU B 2 F76' F -0.0257(15) 0.0764(7) 0.1942(9) 0.040(6) Uani 0.1089(19) 1 d PDU B 2 S77' S 0.0575(5) 0.0167(3) 0.2681(3) 0.0292(3) Uani 0.1089(19) 1 d PDU B 2 O78' O 0.1294(14) 0.0514(12) 0.2672(12) 0.036(6) Uani 0.1089(19) 1 d PDU B 2 O79' O 0.0561(18) -0.0423(5) 0.2745(11) 0.038(5) Uani 0.1089(19) 1 d PDU B 2 N80 N -0.0178(2) 0.03760(13) 0.29957(13) 0.0321(7) Uani 1 1 d D . . S81 S -0.02432(6) 0.09968(4) 0.31862(4) 0.02710(19) Uani 1 1 d . B . O82 O -0.10605(19) 0.11098(13) 0.33749(13) 0.0448(7) Uani 1 1 d . . . O83 O 0.01549(18) 0.14099(10) 0.28642(11) 0.0339(6) Uani 1 1 d . . . C84 C 0.0404(3) 0.09634(17) 0.37924(17) 0.0395(10) Uani 1 1 d . . . F85 F 0.11948(18) 0.08466(13) 0.36737(12) 0.0573(8) Uani 1 1 d . B . F86 F 0.0127(2) 0.05860(11) 0.41255(10) 0.0602(8) Uani 1 1 d . B . F87 F 0.0395(2) 0.14567(11) 0.40334(11) 0.0549(7) Uani 1 1 d . B . C88 C 0.5115(4) 0.0826(2) 0.1202(2) 0.0636(16) Uani 1 1 d . . . F89 F 0.5414(3) 0.06547(15) 0.16738(15) 0.1016(15) Uani 1 1 d . . . F90 F 0.4292(3) 0.07898(18) 0.1207(2) 0.1090(16) Uani 1 1 d . . . F91 F 0.5403(3) 0.04971(13) 0.08321(14) 0.0817(11) Uani 1 1 d . . . S92 S 0.54246(6) 0.15478(4) 0.10981(4) 0.0305(2) Uani 1 1 d . . . O93 O 0.6309(2) 0.15107(16) 0.10946(14) 0.0525(8) Uani 1 1 d . . . O94 O 0.5040(2) 0.18524(13) 0.15209(11) 0.0401(7) Uani 1 1 d . . . N95 N 0.5101(2) 0.16614(18) 0.05195(13) 0.0440(9) Uani 1 1 d . . . S96 S 0.42508(6) 0.19284(4) 0.03441(4) 0.0339(2) Uani 1 1 d . . . O97 O 0.37069(18) 0.20930(13) 0.07622(11) 0.0400(7) Uani 1 1 d . . . O98 O 0.3906(2) 0.16319(14) -0.00980(12) 0.0475(8) Uani 1 1 d . . . C99 C 0.4613(3) 0.2588(2) 0.00609(17) 0.0438(11) Uani 1 1 d . . . F100 F 0.4976(2) 0.28960(13) 0.04310(11) 0.0606(8) Uani 1 1 d . . . F101 F 0.51415(19) 0.25039(12) -0.03336(10) 0.0540(7) Uani 1 1 d . . . F102 F 0.3954(2) 0.28648(13) -0.01364(13) 0.0646(8) Uani 1 1 d . . . C103 C 0.0865(3) 0.49646(18) 0.2460(2) 0.0463(11) Uani 1 1 d . . . F104 F 0.04471(19) 0.54395(11) 0.23848(12) 0.0537(7) Uani 1 1 d . . . F105 F 0.0461(2) 0.46666(12) 0.28274(12) 0.0590(8) Uani 1 1 d . . . F106 F 0.1611(2) 0.50927(14) 0.26637(15) 0.0732(10) Uani 1 1 d . . . S107 S 0.09618(6) 0.45826(4) 0.18414(5) 0.0374(2) Uani 1 1 d . . . O108 O 0.14204(19) 0.40955(13) 0.19834(15) 0.0506(9) Uani 1 1 d . . . O109 O 0.1320(2) 0.49715(14) 0.14850(15) 0.0576(10) Uani 1 1 d . . . N110 N 0.0014(2) 0.44927(15) 0.17005(16) 0.0413(9) Uani 1 1 d . . . S111 S -0.04633(6) 0.39284(4) 0.16963(4) 0.0315(2) Uani 1 1 d . B . O112 O -0.1325(2) 0.40355(15) 0.17884(14) 0.0500(8) Uani 1 1 d . . . O113 O -0.00864(19) 0.34642(12) 0.19651(11) 0.0381(7) Uani 1 1 d . . . C114 C -0.0439(4) 0.3745(2) 0.09892(19) 0.0543(13) Uani 1 1 d . . . F115 F 0.0337(3) 0.36557(17) 0.08445(13) 0.0861(12) Uani 1 1 d . B . F116 F -0.0879(3) 0.32828(12) 0.09052(13) 0.0799(11) Uani 1 1 d . B . F117 F -0.0758(3) 0.41393(13) 0.06881(12) 0.0722(10) Uani 1 1 d . B . C118 C 0.6474(3) 0.22953(18) 0.48646(16) 0.0376(10) Uani 1 1 d . . . F119 F 0.69321(18) 0.27458(13) 0.49125(12) 0.0577(8) Uani 1 1 d . . . F120 F 0.67958(19) 0.19624(13) 0.45052(11) 0.0571(8) Uani 1 1 d . . . F121 F 0.64971(19) 0.20246(13) 0.53281(11) 0.0597(8) Uani 1 1 d . . . S122 S 0.53789(6) 0.24643(4) 0.47150(4) 0.0302(2) Uani 1 1 d . . . O123 O 0.4981(2) 0.19491(12) 0.46119(12) 0.0421(7) Uani 1 1 d . . . O124 O 0.5106(2) 0.27921(14) 0.51487(13) 0.0486(8) Uani 1 1 d . . . N125 N 0.5573(2) 0.27940(15) 0.41742(14) 0.0358(8) Uani 1 1 d . . . S126 S 0.48858(6) 0.30741(4) 0.38270(4) 0.02673(19) Uani 1 1 d . . . O127 O 0.40413(18) 0.29162(12) 0.39184(11) 0.0368(6) Uani 1 1 d . . . O128 O 0.51738(19) 0.30758(12) 0.32808(11) 0.0368(7) Uani 1 1 d . . . C129 C 0.4927(3) 0.38100(17) 0.39957(16) 0.0341(9) Uani 1 1 d . . . F130 F 0.56684(18) 0.40213(11) 0.39180(12) 0.0535(7) Uani 1 1 d . . . F131 F 0.43853(19) 0.40913(11) 0.37103(12) 0.0564(7) Uani 1 1 d . . . F132 F 0.4744(2) 0.38789(12) 0.45102(11) 0.0647(9) Uani 1 1 d . . . 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 0.0237(3) 0.0209(3) 0.0242(3) 0.0034(2) -0.0018(2) 0.0030(2) Cu2 0.0231(3) 0.0278(3) 0.0280(3) -0.0039(2) -0.0002(2) -0.0012(2) N1 0.0280(17) 0.0215(15) 0.0247(15) -0.0013(12) -0.0020(12) 0.0027(13) C2 0.0264(19) 0.0227(18) 0.0273(18) 0.0021(14) -0.0022(15) 0.0020(15) N3 0.0290(17) 0.0214(15) 0.0272(15) 0.0021(12) -0.0016(13) -0.0001(13) C4 0.0257(19) 0.0245(18) 0.0315(19) 0.0026(15) 0.0019(15) 0.0049(15) C5 0.027(2) 0.0234(18) 0.034(2) 0.0016(15) 0.0019(16) 0.0065(15) C6 0.028(2) 0.0201(18) 0.042(2) 0.0018(16) 0.0021(17) -0.0018(15) C7 0.029(2) 0.0240(18) 0.038(2) 0.0071(16) 0.0054(16) 0.0009(16) C8 0.038(2) 0.031(2) 0.0283(19) 0.0028(16) 0.0034(17) 0.0002(17) C9 0.041(3) 0.044(2) 0.032(2) 0.0044(18) 0.0028(18) 0.008(2) N10 0.0287(17) 0.0248(15) 0.0229(15) 0.0019(12) -0.0020(12) 0.0041(13) C11 0.031(2) 0.0262(19) 0.0255(18) -0.0013(14) -0.0058(15) 0.0054(16) N12 0.0336(18) 0.0250(16) 0.0270(16) 0.0017(13) -0.0096(13) 0.0013(14) C13 0.029(2) 0.034(2) 0.036(2) -0.0017(17) -0.0054(16) 0.0102(17) C14 0.030(2) 0.040(2) 0.0275(19) 0.0005(16) -0.0037(16) 0.0087(18) C15 0.041(2) 0.030(2) 0.033(2) 0.0024(16) -0.0178(18) 0.0022(18) C16 0.030(2) 0.029(2) 0.0284(19) 0.0016(15) -0.0006(16) -0.0034(16) C17 0.046(3) 0.030(2) 0.035(2) 0.0038(17) -0.0118(18) -0.0024(18) C18 0.067(3) 0.038(2) 0.036(2) 0.0077(19) -0.008(2) -0.004(2) N19 0.0241(16) 0.0209(15) 0.0285(16) 0.0014(12) -0.0023(12) 0.0035(12) C20 0.027(2) 0.0241(18) 0.033(2) -0.0001(15) 0.0008(15) 0.0032(15) N21 0.0333(18) 0.0207(15) 0.0365(18) -0.0002(13) 0.0054(14) 0.0008(13) C22 0.031(2) 0.027(2) 0.050(2) -0.0062(18) 0.0015(19) -0.0004(17) C23 0.027(2) 0.0282(19) 0.038(2) -0.0029(16) -0.0054(16) 0.0009(16) C24 0.044(3) 0.027(2) 0.045(2) 0.0064(17) 0.013(2) 0.0030(18) C25 0.029(2) 0.032(2) 0.032(2) 0.0000(16) -0.0004(16) -0.0018(17) C26 0.047(3) 0.037(2) 0.036(2) 0.0055(18) 0.0034(19) -0.003(2) C27 0.074(4) 0.045(3) 0.041(3) -0.006(2) 0.015(2) -0.007(3) N28 0.0251(16) 0.0237(15) 0.0252(15) 0.0027(12) 0.0000(12) 0.0014(13) C29 0.031(2) 0.0221(18) 0.0308(19) 0.0008(15) -0.0041(16) 0.0027(15) N30 0.0265(17) 0.0239(16) 0.0277(15) 0.0035(12) 0.0012(13) 0.0060(13) C31 0.0248(19) 0.031(2) 0.0244(18) 0.0007(15) 0.0013(14) 0.0029(16) C32 0.0269(19) 0.0223(17) 0.0261(18) 0.0014(14) 0.0012(15) -0.0005(15) C33 0.040(2) 0.027(2) 0.039(2) 0.0018(17) 0.0022(18) 0.0128(18) C34 0.042(2) 0.0220(19) 0.041(2) 0.0079(16) -0.0035(18) 0.0049(17) C35 0.037(2) 0.0250(19) 0.031(2) 0.0003(15) -0.0057(16) -0.0051(17) C36 0.056(3) 0.035(2) 0.043(2) 0.0094(19) 0.002(2) 0.000(2) N37 0.0283(17) 0.0332(17) 0.0228(15) -0.0015(13) -0.0041(12) -0.0003(14) C38 0.031(2) 0.031(2) 0.0254(18) 0.0007(15) -0.0008(15) 0.0013(17) N39 0.0339(18) 0.0274(16) 0.0318(17) -0.0042(13) 0.0032(14) 0.0011(14) C40 0.051(3) 0.059(3) 0.0200(19) -0.0033(18) -0.0032(18) 0.008(2) C41 0.042(2) 0.053(3) 0.0240(19) -0.0009(18) -0.0046(17) 0.014(2) C42 0.054(3) 0.038(2) 0.049(4) -0.001(2) 0.009(2) 0.016(2) C43 0.062(3) 0.041(3) 0.056(3) -0.002(3) 0.003(3) 0.010(3) C44 0.067(4) 0.044(3) 0.056(4) -0.003(3) -0.001(3) 0.007(3) C45 0.094(6) 0.050(4) 0.076(5) 0.009(4) 0.026(5) 0.011(4) C42' 0.054(3) 0.038(2) 0.049(4) -0.001(2) 0.009(2) 0.016(2) C43' 0.065(5) 0.049(5) 0.062(5) -0.009(5) 0.004(5) 0.009(5) C44' 0.073(7) 0.060(6) 0.065(7) -0.008(6) -0.003(6) -0.002(6) C45' 0.075(12) 0.103(11) 0.099(12) 0.033(10) 0.008(11) -0.010(11) N46 0.0278(17) 0.0279(17) 0.0312(16) -0.0006(13) -0.0046(13) -0.0005(13) C47 0.026(2) 0.031(2) 0.032(2) 0.0013(16) -0.0048(16) 0.0027(16) N48 0.0311(18) 0.0272(16) 0.0306(16) 0.0002(13) -0.0051(13) -0.0016(14) C49 0.031(2) 0.031(2) 0.042(2) 0.0058(17) -0.0099(18) 0.0010(17) C50 0.032(2) 0.027(2) 0.049(2) 0.0033(18) -0.0079(18) 0.0016(17) C51 0.034(2) 0.031(2) 0.037(2) -0.0026(17) -0.0010(17) -0.0075(17) C52 0.052(3) 0.043(3) 0.037(2) -0.0036(19) -0.007(2) -0.005(2) C53 0.071(4) 0.058(3) 0.037(2) 0.006(2) 0.011(2) 0.003(3) C54 0.061(4) 0.084(4) 0.071(4) 0.012(3) 0.020(3) 0.009(3) N55 0.0259(17) 0.0247(15) 0.0266(16) -0.0029(12) 0.0013(13) 0.0003(13) C56 0.026(2) 0.0280(19) 0.0282(19) -0.0017(15) -0.0013(15) -0.0036(16) N57 0.0273(17) 0.0245(15) 0.0256(15) -0.0013(12) 0.0011(12) -0.0013(13) C58 0.0214(18) 0.0259(18) 0.0285(18) -0.0039(15) 0.0028(14) 0.0002(15) C59 0.0256(19) 0.0313(19) 0.0241(18) -0.0015(15) 0.0027(15) 0.0027(16) C60 0.036(2) 0.038(2) 0.0233(18) -0.0005(16) -0.0021(16) -0.0048(18) C61 0.050(3) 0.041(2) 0.0258(19) -0.0060(17) 0.0001(18) -0.004(2) C62 0.053(3) 0.034(2) 0.035(2) -0.0014(17) -0.0005(19) 0.002(2) C63 0.079(4) 0.040(3) 0.059(3) -0.004(2) 0.019(3) 0.009(3) N64 0.0250(17) 0.0273(16) 0.0321(16) 0.0023(13) 0.0027(13) -0.0048(13) C65 0.043(3) 0.027(2) 0.055(3) 0.0066(19) 0.023(2) 0.0017(19) N66 0.044(2) 0.0345(19) 0.049(2) 0.0102(16) 0.0190(17) 0.0125(17) C67 0.036(2) 0.053(3) 0.037(2) 0.002(2) 0.0115(19) -0.011(2) C68 0.047(3) 0.038(2) 0.038(2) -0.0025(18) 0.0134(19) -0.014(2) C69 0.100(5) 0.051(3) 0.087(4) 0.021(3) 0.054(4) 0.039(3) C70 0.042(3) 0.045(3) 0.079(4) -0.008(3) 0.003(3) -0.002(2) C71 0.065(4) 0.053(3) 0.114(6) -0.013(3) 0.024(4) -0.003(3) C72 0.090(6) 0.104(6) 0.123(7) -0.066(5) -0.009(5) -0.003(5) C73 0.041(3) 0.035(3) 0.037(2) -0.003(2) -0.004(2) 0.006(2) F74 0.073(2) 0.056(2) 0.0560(19) 0.0088(15) -0.0182(17) 0.0266(18) F75 0.0527(19) 0.0451(17) 0.0584(18) -0.0184(14) 0.0090(15) 0.0069(14) F76 0.0329(17) 0.0418(17) 0.056(2) -0.0107(14) -0.0034(14) -0.0029(14) S77 0.0392(6) 0.0224(5) 0.0261(5) 0.0026(4) 0.0007(4) -0.0072(4) O78 0.071(3) 0.0285(17) 0.0407(19) -0.0020(14) 0.0065(18) -0.0197(17) O79 0.042(2) 0.032(2) 0.0268(17) 0.0089(15) -0.0063(15) -0.0040(17) C73' 0.039(9) 0.034(9) 0.027(8) 0.004(8) 0.010(6) -0.005(7) F74' 0.079(15) 0.061(13) 0.046(13) -0.027(12) 0.004(9) -0.038(13) F75' 0.097(18) 0.050(14) 0.039(8) 0.009(11) 0.040(12) -0.005(12) F76' 0.056(17) 0.038(11) 0.026(11) -0.005(9) -0.015(9) -0.002(9) S77' 0.0392(6) 0.0224(5) 0.0261(5) 0.0026(4) 0.0007(4) -0.0072(4) O78' 0.033(9) 0.034(9) 0.040(10) 0.001(8) 0.018(7) -0.004(7) O79' 0.049(13) 0.016(7) 0.049(11) 0.001(8) 0.022(10) 0.010(8) N80 0.040(2) 0.0244(16) 0.0322(17) 0.0005(13) 0.0034(14) -0.0069(14) S81 0.0274(5) 0.0241(4) 0.0297(4) 0.0032(3) -0.0024(4) 0.0014(4) O82 0.0354(17) 0.0475(18) 0.0517(18) 0.0013(14) 0.0078(14) 0.0041(14) O83 0.0414(17) 0.0188(13) 0.0415(15) 0.0080(11) 0.0002(13) -0.0007(12) C84 0.053(3) 0.028(2) 0.037(2) 0.0011(17) -0.008(2) -0.0021(19) F85 0.0428(16) 0.0612(18) 0.0674(18) -0.0104(15) -0.0259(14) 0.0133(14) F86 0.106(3) 0.0414(15) 0.0327(13) 0.0113(11) -0.0143(14) -0.0066(16) F87 0.080(2) 0.0389(14) 0.0457(15) -0.0111(12) -0.0145(14) -0.0010(14) C88 0.094(5) 0.044(3) 0.054(3) -0.006(2) 0.012(3) -0.010(3) F89 0.188(5) 0.055(2) 0.062(2) 0.0220(17) 0.013(3) 0.005(3) F90 0.092(3) 0.087(3) 0.149(4) -0.025(3) 0.043(3) -0.056(3) F91 0.124(3) 0.0441(18) 0.077(2) -0.0253(16) 0.001(2) 0.0032(19) S92 0.0299(5) 0.0341(5) 0.0274(5) -0.0025(4) -0.0040(4) -0.0025(4) O93 0.0302(17) 0.066(2) 0.061(2) -0.0042(17) -0.0100(15) -0.0001(16) O94 0.0508(19) 0.0422(17) 0.0273(14) -0.0096(12) -0.0067(13) 0.0084(14) N95 0.038(2) 0.069(3) 0.0242(17) 0.0030(17) 0.0018(15) 0.0152(19) S96 0.0339(5) 0.0429(5) 0.0248(4) -0.0051(4) -0.0050(4) 0.0032(4) O97 0.0290(15) 0.0540(19) 0.0369(15) -0.0085(14) -0.0015(12) 0.0017(14) O98 0.063(2) 0.0466(18) 0.0323(15) -0.0070(13) -0.0176(14) 0.0002(16) C99 0.053(3) 0.044(3) 0.034(2) -0.0027(19) 0.000(2) 0.002(2) F100 0.078(2) 0.0598(18) 0.0448(15) -0.0150(13) 0.0090(14) -0.0228(16) F101 0.0694(19) 0.0603(18) 0.0325(13) 0.0031(12) 0.0095(12) -0.0012(15) F102 0.076(2) 0.0494(17) 0.069(2) 0.0104(15) -0.0025(17) 0.0158(16) C103 0.050(3) 0.028(2) 0.061(3) 0.012(2) -0.005(2) 0.001(2) F104 0.0601(18) 0.0309(13) 0.0703(18) 0.0039(12) 0.0036(14) 0.0097(13) F105 0.080(2) 0.0424(15) 0.0553(17) 0.0086(13) 0.0100(15) 0.0064(15) F106 0.060(2) 0.060(2) 0.098(3) 0.0012(18) -0.0335(18) -0.0086(16) S107 0.0264(5) 0.0285(5) 0.0575(6) 0.0109(4) 0.0077(4) 0.0017(4) O108 0.0300(17) 0.0328(16) 0.089(3) 0.0093(16) 0.0051(16) 0.0088(13) O109 0.054(2) 0.0419(19) 0.078(2) 0.0166(17) 0.0259(19) -0.0039(16) N110 0.037(2) 0.0285(18) 0.058(2) 0.0104(16) -0.0056(17) 0.0036(15) S111 0.0314(5) 0.0280(5) 0.0352(5) 0.0053(4) 0.0021(4) -0.0003(4) O112 0.0313(17) 0.057(2) 0.062(2) 0.0070(16) 0.0000(15) -0.0007(15) O113 0.0442(17) 0.0330(15) 0.0371(15) 0.0131(12) -0.0049(13) -0.0032(13) C114 0.086(4) 0.038(3) 0.038(3) 0.007(2) -0.001(3) 0.001(3) F115 0.108(3) 0.105(3) 0.0462(18) -0.0035(18) 0.0267(19) 0.029(2) F116 0.145(4) 0.0365(16) 0.0569(19) -0.0009(13) -0.036(2) -0.0086(19) F117 0.120(3) 0.0520(18) 0.0444(16) 0.0188(14) -0.0216(17) 0.0006(19) C118 0.041(2) 0.042(2) 0.029(2) -0.0064(17) -0.0024(18) 0.003(2) F119 0.0438(16) 0.0607(18) 0.0682(19) 0.0036(15) -0.0201(14) -0.0098(14) F120 0.0546(17) 0.0683(19) 0.0486(16) -0.0108(14) 0.0020(13) 0.0254(15) F121 0.0652(19) 0.072(2) 0.0421(15) 0.0145(14) -0.0170(13) 0.0208(16) S122 0.0324(5) 0.0285(5) 0.0296(5) 0.0044(4) -0.0018(4) 0.0042(4) O123 0.0486(19) 0.0351(16) 0.0426(17) 0.0057(13) -0.0056(14) -0.0046(14) O124 0.055(2) 0.0457(18) 0.0449(18) -0.0059(14) 0.0102(15) 0.0131(16) N125 0.0314(19) 0.041(2) 0.0347(18) 0.0042(15) -0.0009(14) 0.0075(15) S126 0.0288(5) 0.0211(4) 0.0301(4) -0.0002(3) -0.0070(4) 0.0004(4) O127 0.0350(16) 0.0356(15) 0.0396(15) 0.0033(12) -0.0025(12) -0.0037(13) O128 0.0462(18) 0.0345(15) 0.0297(14) -0.0073(12) 0.0029(12) 0.0024(13) C129 0.039(2) 0.030(2) 0.034(2) -0.0064(16) 0.0096(18) 0.0039(18) F130 0.0488(17) 0.0338(14) 0.078(2) -0.0109(13) 0.0068(14) -0.0135(12) F131 0.0618(19) 0.0347(14) 0.0725(19) 0.0094(13) -0.0043(15) 0.0144(13) F132 0.108(3) 0.0453(16) 0.0409(15) -0.0109(12) 0.0188(16) 0.0074(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N10 1.987(3) . ? Cu1 N1 1.990(3) . ? Cu1 N28 1.991(3) . ? Cu1 N19 1.994(3) . ? Cu1 O128 2.565(3) . ? Cu1 O94 2.754(3) . ? Cu2 N64 1.980(3) . ? Cu2 N55 1.986(3) . ? Cu2 N37 1.990(3) . ? Cu2 N46 1.992(3) . ? Cu2 O113 2.706(3) . ? Cu2 O83 2.736(3) . ? N1 C2 1.334(5) . ? N1 C5 1.377(5) . ? C2 N3 1.342(5) . ? N3 C4 1.378(5) . ? N3 C6 1.470(5) . ? C4 C5 1.352(5) . ? C6 C7 1.524(5) . ? C7 C8 1.520(6) . ? C8 C9 1.520(5) . ? N10 C11 1.327(5) . ? N10 C14 1.360(5) . ? C11 N12 1.335(5) . ? N12 C13 1.370(5) . ? N12 C15 1.469(5) . ? C13 C14 1.347(6) . ? C15 C16 1.503(5) . ? C16 C17 1.526(5) . ? C17 C18 1.513(6) . ? N19 C20 1.316(5) . ? N19 C23 1.382(5) . ? C20 N21 1.335(5) . ? N21 C22 1.373(6) . ? N21 C24 1.465(5) . ? C22 C23 1.354(6) . ? C24 C25 1.518(5) . ? C25 C26 1.520(5) . ? C26 C27 1.517(6) . ? N28 C29 1.324(5) . ? N28 C32 1.381(5) . ? C29 N30 1.350(5) . ? N30 C31 1.373(5) . ? N30 C33 1.475(5) . ? C31 C32 1.354(5) . ? C33 C34 1.529(6) . ? C34 C35 1.520(6) . ? C35 C36 1.519(6) . ? N37 C38 1.311(5) . ? N37 C41 1.366(5) . ? C38 N39 1.332(5) . ? N39 C40 1.363(5) . ? N39 C42 1.465(6) . ? N39 C42' 1.466(10) . ? C40 C41 1.357(6) . ? C42 C43 1.496(8) . ? C43 C44 1.484(7) . ? C44 C45 1.484(7) . ? C42' C43' 1.489(9) . ? C43' C44' 1.480(9) . ? C44' C45' 1.490(9) . ? N46 C47 1.315(5) . ? N46 C50 1.373(5) . ? C47 N48 1.347(5) . ? N48 C49 1.372(5) . ? N48 C51 1.468(5) . ? C49 C50 1.348(6) . ? C51 C52 1.532(6) . ? C52 C53 1.508(7) . ? C53 C54 1.506(8) . ? N55 C56 1.326(5) . ? N55 C59 1.370(5) . ? C56 N57 1.341(5) . ? N57 C58 1.378(5) . ? N57 C60 1.470(5) . ? C58 C59 1.355(5) . ? C60 C61 1.510(6) . ? C61 C62 1.527(6) . ? C62 C63 1.507(6) . ? N64 C65 1.312(5) . ? N64 C68 1.360(5) . ? C65 N66 1.346(5) . ? N66 C67 1.349(6) . ? N66 C69 1.473(6) . ? C67 C68 1.349(6) . ? C69 C70 1.482(8) . ? C70 C71 1.526(7) . ? C71 C72 1.505(10) . ? C73 F74 1.324(5) . ? C73 F76 1.326(5) . ? C73 F75 1.330(5) . ? C73 S77 1.827(5) . ? S77 O78 1.429(3) . ? S77 O79 1.431(3) . ? S77 N80 1.591(3) . ? C73' F76' 1.330(8) . ? C73' F75' 1.332(8) . ? C73' F74' 1.333(8) . ? C73' S77' 1.839(11) . ? S77' O78' 1.424(9) . ? S77' O79' 1.427(9) . ? S77' N80 1.534(7) . ? N80 S81 1.571(3) . ? S81 O82 1.425(3) . ? S81 O83 1.434(3) . ? S81 C84 1.831(4) . ? C84 F86 1.314(5) . ? C84 F87 1.331(5) . ? C84 F85 1.335(6) . ? C88 F91 1.305(6) . ? C88 F90 1.323(8) . ? C88 F89 1.336(7) . ? C88 S92 1.825(6) . ? S92 O93 1.421(3) . ? S92 O94 1.433(3) . ? S92 N95 1.558(4) . ? N95 S96 1.565(4) . ? S96 O98 1.423(3) . ? S96 O97 1.426(3) . ? S96 C99 1.834(5) . ? C99 F100 1.318(5) . ? C99 F101 1.324(5) . ? C99 F102 1.339(6) . ? C103 F106 1.332(6) . ? C103 F104 1.336(5) . ? C103 F105 1.339(5) . ? C103 S107 1.809(5) . ? S107 O109 1.419(3) . ? S107 O108 1.426(3) . ? S107 N110 1.571(4) . ? N110 S111 1.558(4) . ? S111 O112 1.427(3) . ? S111 O113 1.434(3) . ? S111 C114 1.825(5) . ? C114 F117 1.311(6) . ? C114 F115 1.318(7) . ? C114 F116 1.333(6) . ? C118 F119 1.314(5) . ? C118 F120 1.315(5) . ? C118 F121 1.331(5) . ? C118 S122 1.836(5) . ? S122 O124 1.415(3) . ? S122 O123 1.416(3) . ? S122 N125 1.603(3) . ? N125 S126 1.550(3) . ? S126 O127 1.428(3) . ? S126 O128 1.449(3) . ? S126 C129 1.820(4) . ? C129 F131 1.307(5) . ? C129 F130 1.310(5) . ? C129 F132 1.335(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N10 Cu1 N1 90.04(13) . . ? N10 Cu1 N28 178.63(12) . . ? N1 Cu1 N28 91.01(12) . . ? N10 Cu1 N19 89.43(13) . . ? N1 Cu1 N19 179.43(13) . . ? N28 Cu1 N19 89.52(12) . . ? N10 Cu1 O128 86.64(11) . . ? N1 Cu1 O128 85.80(11) . . ? N28 Cu1 O128 92.55(11) . . ? N19 Cu1 O128 94.36(11) . . ? N10 Cu1 O94 86.19(11) . . ? N1 Cu1 O94 88.32(11) . . ? N28 Cu1 O94 94.73(11) . . ? N19 Cu1 O94 91.45(11) . . ? O128 Cu1 O94 170.73(9) . . ? N64 Cu2 N55 90.39(13) . . ? N64 Cu2 N37 178.51(14) . . ? N55 Cu2 N37 91.08(13) . . ? N64 Cu2 N46 88.50(13) . . ? N55 Cu2 N46 177.86(13) . . ? N37 Cu2 N46 90.04(13) . . ? N64 Cu2 O113 92.76(11) . . ? N55 Cu2 O113 93.14(11) . . ? N37 Cu2 O113 86.92(11) . . ? N46 Cu2 O113 88.74(11) . . ? N64 Cu2 O83 84.82(11) . . ? N55 Cu2 O83 86.62(11) . . ? N37 Cu2 O83 95.50(11) . . ? N46 Cu2 O83 91.46(11) . . ? O113 Cu2 O83 177.57(9) . . ? C2 N1 C5 106.0(3) . . ? C2 N1 Cu1 126.1(3) . . ? C5 N1 Cu1 127.9(2) . . ? N1 C2 N3 110.8(3) . . ? C2 N3 C4 107.2(3) . . ? C2 N3 C6 125.6(3) . . ? C4 N3 C6 126.7(3) . . ? C5 C4 N3 106.7(3) . . ? C4 C5 N1 109.2(3) . . ? N3 C6 C7 111.1(3) . . ? C8 C7 C6 113.3(3) . . ? C7 C8 C9 112.5(3) . . ? C11 N10 C14 105.5(3) . . ? C11 N10 Cu1 126.3(3) . . ? C14 N10 Cu1 128.1(3) . . ? N10 C11 N12 111.0(3) . . ? C11 N12 C13 107.3(3) . . ? C11 N12 C15 125.8(3) . . ? C13 N12 C15 126.9(3) . . ? C14 C13 N12 106.0(3) . . ? C13 C14 N10 110.1(3) . . ? N12 C15 C16 113.3(3) . . ? C15 C16 C17 111.4(3) . . ? C18 C17 C16 112.6(3) . . ? C20 N19 C23 106.1(3) . . ? C20 N19 Cu1 125.5(3) . . ? C23 N19 Cu1 128.2(3) . . ? N19 C20 N21 111.5(3) . . ? C20 N21 C22 107.1(3) . . ? C20 N21 C24 126.0(4) . . ? C22 N21 C24 126.4(4) . . ? C23 C22 N21 106.7(4) . . ? C22 C23 N19 108.6(4) . . ? N21 C24 C25 111.3(3) . . ? C24 C25 C26 113.0(3) . . ? C27 C26 C25 111.8(4) . . ? C29 N28 C32 105.5(3) . . ? C29 N28 Cu1 127.5(3) . . ? C32 N28 Cu1 126.1(2) . . ? N28 C29 N30 111.2(3) . . ? C29 N30 C31 107.1(3) . . ? C29 N30 C33 125.9(3) . . ? C31 N30 C33 126.4(3) . . ? C32 C31 N30 106.4(3) . . ? C31 C32 N28 109.7(3) . . ? N30 C33 C34 111.3(3) . . ? C35 C34 C33 113.7(3) . . ? C36 C35 C34 113.1(4) . . ? C38 N37 C41 105.9(3) . . ? C38 N37 Cu2 126.4(3) . . ? C41 N37 Cu2 127.0(3) . . ? N37 C38 N39 111.6(3) . . ? C38 N39 C40 107.1(3) . . ? C38 N39 C42 124.8(6) . . ? C40 N39 C42 128.0(6) . . ? C38 N39 C42' 131.4(19) . . ? C40 N39 C42' 121.4(19) . . ? C41 C40 N39 106.3(4) . . ? C40 C41 N37 109.0(4) . . ? N39 C42 C43 111.0(6) . . ? C44 C43 C42 112.2(6) . . ? C43 C44 C45 114.7(7) . . ? N39 C42' C43' 114.2(16) . . ? C44' C43' C42' 111(2) . . ? C43' C44' C45' 126(2) . . ? C47 N46 C50 105.9(3) . . ? C47 N46 Cu2 127.3(3) . . ? C50 N46 Cu2 126.6(3) . . ? N46 C47 N48 111.2(3) . . ? C47 N48 C49 106.9(3) . . ? C47 N48 C51 126.9(3) . . ? C49 N48 C51 126.1(3) . . ? C50 C49 N48 106.4(4) . . ? C49 C50 N46 109.6(4) . . ? N48 C51 C52 111.6(3) . . ? C53 C52 C51 115.0(4) . . ? C54 C53 C52 114.0(4) . . ? C56 N55 C59 106.3(3) . . ? C56 N55 Cu2 127.2(3) . . ? C59 N55 Cu2 126.2(2) . . ? N55 C56 N57 110.6(3) . . ? C56 N57 C58 107.6(3) . . ? C56 N57 C60 125.1(3) . . ? C58 N57 C60 126.6(3) . . ? C59 C58 N57 106.0(3) . . ? C58 C59 N55 109.5(3) . . ? N57 C60 C61 110.7(3) . . ? C60 C61 C62 112.7(4) . . ? C63 C62 C61 113.1(4) . . ? C65 N64 C68 106.0(3) . . ? C65 N64 Cu2 125.2(3) . . ? C68 N64 Cu2 128.6(3) . . ? N64 C65 N66 110.6(4) . . ? C65 N66 C67 107.3(4) . . ? C65 N66 C69 125.0(4) . . ? C67 N66 C69 127.7(4) . . ? N66 C67 C68 106.6(4) . . ? C67 C68 N64 109.4(4) . . ? N66 C69 C70 114.6(5) . . ? C69 C70 C71 112.4(5) . . ? C72 C71 C70 113.3(6) . . ? F74 C73 F76 108.7(4) . . ? F74 C73 F75 108.4(4) . . ? F76 C73 F75 108.0(4) . . ? F74 C73 S77 111.3(3) . . ? F76 C73 S77 110.4(3) . . ? F75 C73 S77 109.8(3) . . ? O78 S77 O79 118.6(2) . . ? O78 S77 N80 108.36(19) . . ? O79 S77 N80 115.6(2) . . ? O78 S77 C73 103.3(2) . . ? O79 S77 C73 103.7(2) . . ? N80 S77 C73 105.56(19) . . ? F76' C73' F75' 106.3(12) . . ? F76' C73' F74' 107.0(12) . . ? F75' C73' F74' 106.1(12) . . ? F76' C73' S77' 114.8(16) . . ? F75' C73' S77' 108.3(15) . . ? F74' C73' S77' 113.8(15) . . ? O78' S77' O79' 126.7(19) . . ? O78' S77' N80 117.3(14) . . ? O79' S77' N80 104.7(11) . . ? O78' S77' C73' 107.8(15) . . ? O79' S77' C73' 101.6(15) . . ? N80 S77' C73' 92.2(7) . . ? S77' N80 S81 121.5(4) . . ? S81 N80 S77 127.2(2) . . ? O82 S81 O83 118.14(18) . . ? O82 S81 N80 110.26(19) . . ? O83 S81 N80 117.14(17) . . ? O82 S81 C84 104.4(2) . . ? O83 S81 C84 104.16(19) . . ? N80 S81 C84 99.86(19) . . ? S81 O83 Cu2 145.19(17) . . ? F86 C84 F87 108.8(4) . . ? F86 C84 F85 109.0(4) . . ? F87 C84 F85 107.7(4) . . ? F86 C84 S81 111.3(3) . . ? F87 C84 S81 109.1(3) . . ? F85 C84 S81 110.8(3) . . ? F91 C88 F90 109.2(5) . . ? F91 C88 F89 108.4(5) . . ? F90 C88 F89 108.5(5) . . ? F91 C88 S92 112.1(4) . . ? F90 C88 S92 109.7(4) . . ? F89 C88 S92 108.9(4) . . ? O93 S92 O94 118.3(2) . . ? O93 S92 N95 109.1(2) . . ? O94 S92 N95 117.12(19) . . ? O93 S92 C88 102.4(3) . . ? O94 S92 C88 105.1(2) . . ? N95 S92 C88 102.1(3) . . ? S92 O94 Cu1 151.03(19) . . ? S92 N95 S96 127.8(2) . . ? O98 S96 O97 118.3(2) . . ? O98 S96 N95 110.0(2) . . ? O97 S96 N95 116.46(18) . . ? O98 S96 C99 104.7(2) . . ? O97 S96 C99 104.1(2) . . ? N95 S96 C99 100.6(2) . . ? F100 C99 F101 109.2(4) . . ? F100 C99 F102 108.7(4) . . ? F101 C99 F102 108.0(4) . . ? F100 C99 S96 110.7(3) . . ? F101 C99 S96 111.4(3) . . ? F102 C99 S96 108.7(3) . . ? F106 C103 F104 107.6(4) . . ? F106 C103 F105 107.4(4) . . ? F104 C103 F105 108.0(4) . . ? F106 C103 S107 111.1(4) . . ? F104 C103 S107 111.2(3) . . ? F105 C103 S107 111.3(3) . . ? O109 S107 O108 119.1(2) . . ? O109 S107 N110 110.3(2) . . ? O108 S107 N110 115.97(19) . . ? O109 S107 C103 104.1(2) . . ? O108 S107 C103 104.6(2) . . ? N110 S107 C103 99.8(2) . . ? S111 N110 S107 126.5(2) . . ? O112 S111 O113 117.94(19) . . ? O112 S111 N110 108.6(2) . . ? O113 S111 N110 118.06(19) . . ? O112 S111 C114 103.4(3) . . ? O113 S111 C114 104.7(2) . . ? N110 S111 C114 101.6(2) . . ? S111 O113 Cu2 157.76(19) . . ? F117 C114 F115 108.9(4) . . ? F117 C114 F116 108.0(5) . . ? F115 C114 F116 108.7(5) . . ? F117 C114 S111 111.8(4) . . ? F115 C114 S111 109.7(4) . . ? F116 C114 S111 109.7(3) . . ? F119 C118 F120 109.9(4) . . ? F119 C118 F121 108.3(4) . . ? F120 C118 F121 107.0(4) . . ? F119 C118 S122 111.6(3) . . ? F120 C118 S122 112.2(3) . . ? F121 C118 S122 107.7(3) . . ? O124 S122 O123 119.0(2) . . ? O124 S122 N125 116.0(2) . . ? O123 S122 N125 111.72(19) . . ? O124 S122 C118 105.6(2) . . ? O123 S122 C118 105.8(2) . . ? N125 S122 C118 94.99(19) . . ? S126 N125 S122 123.0(2) . . ? O127 S126 O128 117.74(18) . . ? O127 S126 N125 117.68(18) . . ? O128 S126 N125 107.36(18) . . ? O127 S126 C129 104.66(18) . . ? O128 S126 C129 101.85(17) . . ? N125 S126 C129 105.6(2) . . ? S126 O128 Cu1 137.00(17) . . ? F131 C129 F130 108.5(4) . . ? F131 C129 F132 108.2(3) . . ? F130 C129 F132 107.7(4) . . ? F131 C129 S126 110.7(3) . . ? F130 C129 S126 111.9(3) . . ? F132 C129 S126 109.7(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 66.59 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.866 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.077 # Attachment 'kb20-[Cu-EtIm-4][Tf2N]2.cif' data_kb20 _database_code_depnum_ccdc_archive 'CCDC 883550' #TrackingRef 'kb20-[Cu-EtIm-4][Tf2N]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(N-methylimidazole)copper(II) bis(trifluoromethyl)sulfonylimide ; _chemical_name_common ; tetrakis(N-methylimidazole)copper(II) bistriflimide ; _chemical_melting_point 347 _chemical_formula_moiety 'C22 H32 Cu F6 N9 O4 S2, C2 F6 N O4 S2' _chemical_formula_sum 'C24 H32 Cu F12 N10 O8 S4' _chemical_formula_weight 1008.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.991(2) _cell_length_b 9.438(3) _cell_length_c 14.654(3) _cell_angle_alpha 89.594(15) _cell_angle_beta 72.209(13) _cell_angle_gamma 62.905(13) _cell_volume 1041.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1830 _cell_measurement_theta_min 3.207 _cell_measurement_theta_max 65.255 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 511 _exptl_absorpt_coefficient_mu 3.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.410 _exptl_absorpt_correction_T_max 0.532 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13995 _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_sigmaI/netI 0.0744 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 66.58 _reflns_number_total 3579 _reflns_number_gt 2607 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ; A.L.Spek (2010) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3579 _refine_ls_number_parameters 430 _refine_ls_number_restraints 366 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1745 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.5000 0.5000 0.0595(4) Uani 1 2 d S . . N1 N 0.5338(6) 0.6611(6) 0.5685(3) 0.0596(12) Uani 1 1 d . . . C2 C 0.4359(8) 0.8187(8) 0.5786(4) 0.0643(15) Uani 1 1 d . . . H2 H 0.3419 0.8706 0.5533 0.077 Uiso 1 1 calc R E . N3 N 0.4862(7) 0.8969(6) 0.6293(4) 0.0669(13) Uani 1 1 d . E . C3 C 0.6515(9) 0.6405(8) 0.6144(5) 0.0773(19) Uani 1 1 d . . . H3 H 0.7411 0.5390 0.6192 0.093 Uiso 1 1 calc R E . C4 C 0.6234(10) 0.7825(9) 0.6517(6) 0.084(2) Uani 1 1 d . E . H4 H 0.6876 0.7999 0.6873 0.100 Uiso 1 1 calc R . . C6 C 0.3992(12) 1.0717(8) 0.6596(6) 0.100(3) Uani 1 1 d . . . H6A H 0.3099 1.1256 0.6276 0.120 Uiso 1 1 calc R E . H6B H 0.4891 1.1091 0.6377 0.120 Uiso 1 1 calc R . . C7 C 0.3114(16) 1.1197(11) 0.7653(7) 0.146(4) Uani 1 1 d . . . H7A H 0.2588 1.2368 0.7816 0.220 Uiso 1 1 calc R . . H7B H 0.3989 1.0662 0.7976 0.220 Uiso 1 1 calc R . . H7C H 0.2178 1.0882 0.7872 0.220 Uiso 1 1 calc R . . N8 N 0.3087(6) 0.5214(6) 0.6205(3) 0.0601(12) Uani 1 1 d . E . C9 C 0.2984(8) 0.5500(8) 0.7111(4) 0.0670(16) Uani 1 1 d . . . H9 H 0.3866 0.5602 0.7289 0.080 Uiso 1 1 calc R E . N10 N 0.1499(7) 0.5626(7) 0.7739(4) 0.0684(14) Uani 1 1 d . . . C11 C 0.0577(9) 0.5400(9) 0.7237(5) 0.0777(19) Uani 1 1 d . . . H11 H -0.0535 0.5411 0.7499 0.093 Uiso 1 1 calc R E . C12 C 0.1551(8) 0.5150(9) 0.6277(5) 0.0765(19) Uani 1 1 d . E . H12 H 0.1228 0.4963 0.5748 0.092 Uiso 1 1 calc R . . C13 C 0.0939(11) 0.5947(11) 0.8822(5) 0.092(2) Uani 1 1 d . . . H13A H 0.0174 0.5456 0.9115 0.111 Uiso 1 1 calc R E . H13B H 0.2001 0.5445 0.9022 0.111 Uiso 1 1 calc R . . C14 C -0.0043(15) 0.7696(13) 0.9181(7) 0.145(4) Uani 1 1 d . . . H14A H -0.0419 0.7878 0.9890 0.217 Uiso 1 1 calc R . . H14B H -0.1091 0.8195 0.8979 0.217 Uiso 1 1 calc R . . H14C H 0.0729 0.8177 0.8910 0.217 Uiso 1 1 calc R . . C15 C 0.450(2) 0.776(2) 0.9927(11) 0.143(6) Uani 0.50 1 d PDU A -1 F16 F 0.452(3) 0.8845(17) 0.9354(12) 0.193(8) Uani 0.50 1 d PDU A -1 F17 F 0.283(2) 0.8244(16) 1.0449(12) 0.173(6) Uani 0.50 1 d PDU A -1 F18 F 0.539(3) 0.771(2) 1.0506(13) 0.180(8) Uani 0.50 1 d PDU A -1 S19 S 0.580(4) 0.575(4) 0.924(2) 0.081(3) Uani 0.50 1 d PU A -1 O20 O 0.5386(15) 0.4387(15) 1.1207(8) 0.097(3) Uani 0.50 1 d PU A -1 O21 O 0.265(2) 0.455(2) 1.1130(13) 0.130(5) Uani 0.50 1 d PU A -1 N22 N 0.4386(15) 0.5215(15) 0.9752(8) 0.080(2) Uani 0.50 1 d PU A -1 S23 S 0.437(4) 0.433(4) 1.067(2) 0.080(3) Uani 0.50 1 d PU A -1 O24 O 0.746(2) 0.495(2) 0.9351(11) 0.114(4) Uani 0.50 1 d PU A -1 O25 O 0.585(2) 0.5834(16) 0.8269(8) 0.118(4) Uani 0.50 1 d PU A -1 C26 C 0.515(2) 0.218(2) 1.0222(11) 0.140(6) Uani 0.50 1 d PDU A -1 F27 F 0.490(4) 0.185(5) 0.9426(17) 0.149(9) Uani 0.25 1 d PDU A -1 F28 F 0.686(2) 0.133(4) 1.009(2) 0.154(8) Uani 0.25 1 d PDU A -1 F29 F 0.422(4) 0.178(4) 1.0956(17) 0.140(9) Uani 0.25 1 d PDU A -1 F27' F 0.579(4) 0.169(4) 0.9279(12) 0.147(8) Uani 0.25 1 d PDU B -2 F28' F 0.650(3) 0.150(4) 1.055(2) 0.158(8) Uani 0.25 1 d PDU C -2 F29' F 0.401(4) 0.165(4) 1.0627(19) 0.136(7) Uani 0.25 1 d PDU D -2 C30 C -0.1244(13) 1.0869(12) 0.6814(10) 0.084(4) Uani 0.50 1 d PDU E -1 F31 F -0.2765(14) 1.0885(18) 0.7172(8) 0.114(3) Uani 0.50 1 d PDU E -1 F32 F -0.1204(19) 1.1916(16) 0.7361(8) 0.124(4) Uani 0.50 1 d PDU E -1 F33 F -0.0007(16) 0.9456(12) 0.6837(7) 0.118(4) Uani 0.50 1 d PDU E -1 S34 S -0.0645(13) 1.1673(10) 0.5629(8) 0.0641(16) Uani 0.50 1 d PU E -1 O35 O -0.217(2) 1.220(2) 0.5415(13) 0.088(4) Uani 0.50 1 d PU E -1 O36 O -0.0035(12) 1.2765(11) 0.5776(7) 0.082(2) Uani 0.50 1 d PU E -1 N37 N 0.0953(13) 1.0096(13) 0.4990(8) 0.067(2) Uani 0.50 1 d PU E -1 S38 S 0.0874(13) 0.8705(9) 0.4433(7) 0.0644(16) Uani 0.50 1 d PU E -1 O39 O -0.0813(14) 0.8725(12) 0.4687(7) 0.074(2) Uani 0.50 1 d PU E -1 O40 O 0.247(2) 0.7264(16) 0.4367(13) 0.088(4) Uani 0.50 1 d PU E -1 C41 C 0.1225(15) 0.8933(14) 0.3174(10) 0.099(5) Uani 0.50 1 d PDU E -1 F42 F -0.0107(17) 0.943(2) 0.2860(10) 0.141(4) Uani 0.50 1 d PDU E -1 F43 F 0.2585(19) 0.7673(14) 0.2592(8) 0.148(5) Uani 0.50 1 d PDU E -1 F44 F 0.165(2) 1.0074(17) 0.3167(8) 0.130(4) Uani 0.50 1 d PDU E -1 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 0.0609(7) 0.0644(8) 0.0529(7) -0.0039(5) -0.0157(5) -0.0316(6) N1 0.062(3) 0.056(3) 0.064(3) -0.001(2) -0.025(2) -0.028(2) C2 0.072(4) 0.068(4) 0.059(3) 0.014(3) -0.034(3) -0.032(3) N3 0.091(4) 0.051(3) 0.067(3) 0.009(2) -0.039(3) -0.032(3) C3 0.079(4) 0.056(4) 0.099(5) 0.002(3) -0.049(4) -0.021(3) C4 0.094(5) 0.073(5) 0.107(6) 0.012(4) -0.066(5) -0.039(4) C6 0.140(7) 0.054(4) 0.113(6) 0.017(4) -0.069(6) -0.036(5) C7 0.219(12) 0.078(6) 0.099(7) -0.017(5) -0.067(7) -0.028(7) N8 0.056(3) 0.063(3) 0.057(3) 0.000(2) -0.016(2) -0.027(2) C9 0.066(4) 0.071(4) 0.056(3) 0.003(3) -0.020(3) -0.026(3) N10 0.066(3) 0.076(4) 0.056(3) 0.012(3) -0.017(2) -0.029(3) C11 0.064(4) 0.093(5) 0.074(4) 0.016(4) -0.021(3) -0.038(4) C12 0.068(4) 0.103(6) 0.061(4) 0.010(4) -0.023(3) -0.042(4) C13 0.104(6) 0.114(7) 0.051(4) 0.012(4) -0.017(4) -0.051(5) C14 0.169(10) 0.120(8) 0.083(6) -0.028(6) -0.010(6) -0.039(7) C15 0.238(14) 0.085(8) 0.106(10) 0.032(7) -0.062(9) -0.074(9) F16 0.291(18) 0.078(8) 0.144(11) 0.050(8) -0.036(12) -0.059(11) F17 0.209(12) 0.085(8) 0.133(10) 0.012(7) -0.019(9) -0.021(8) F18 0.286(15) 0.104(12) 0.141(12) -0.028(8) -0.097(11) -0.070(11) S19 0.104(7) 0.088(4) 0.070(6) 0.024(3) -0.033(5) -0.058(5) O20 0.117(8) 0.120(8) 0.074(6) 0.013(6) -0.037(6) -0.068(7) O21 0.098(8) 0.151(12) 0.132(12) 0.016(9) 0.006(9) -0.079(8) N22 0.089(5) 0.091(5) 0.076(5) 0.016(5) -0.024(4) -0.058(5) S23 0.093(5) 0.091(6) 0.066(5) 0.014(4) -0.019(3) -0.055(4) O24 0.094(7) 0.151(11) 0.112(10) 0.038(8) -0.030(7) -0.074(7) O25 0.186(11) 0.115(8) 0.062(6) 0.027(5) -0.041(6) -0.079(8) C26 0.175(11) 0.093(7) 0.130(11) -0.009(8) -0.020(9) -0.066(8) F27 0.195(17) 0.094(13) 0.119(13) -0.035(11) -0.008(12) -0.064(13) F28 0.175(13) 0.089(11) 0.129(15) -0.014(13) -0.005(12) -0.036(10) F29 0.188(14) 0.093(11) 0.128(14) 0.013(12) -0.038(12) -0.066(11) F27' 0.181(14) 0.095(10) 0.124(12) -0.021(9) -0.010(11) -0.057(10) F28' 0.174(13) 0.098(10) 0.143(14) -0.006(11) -0.009(11) -0.047(10) F29' 0.179(13) 0.087(9) 0.141(13) -0.011(10) -0.027(11) -0.079(9) C30 0.089(8) 0.099(9) 0.073(8) 0.006(7) -0.029(7) -0.051(7) F31 0.110(7) 0.140(10) 0.082(7) 0.004(6) -0.008(5) -0.068(7) F32 0.133(8) 0.143(10) 0.088(6) -0.026(7) -0.034(7) -0.061(8) F33 0.132(8) 0.098(7) 0.077(6) 0.039(5) -0.029(6) -0.019(7) S34 0.067(3) 0.055(4) 0.069(2) 0.004(3) -0.029(2) -0.024(2) O35 0.058(7) 0.082(11) 0.098(9) -0.015(7) -0.036(6) -0.005(7) O36 0.081(6) 0.064(5) 0.104(7) 0.005(5) -0.034(5) -0.036(5) N37 0.065(5) 0.060(5) 0.069(5) 0.008(4) -0.027(4) -0.020(4) S38 0.069(3) 0.048(3) 0.071(3) 0.011(2) -0.031(2) -0.019(2) O39 0.071(6) 0.059(6) 0.090(6) 0.017(5) -0.029(5) -0.027(5) O40 0.083(7) 0.042(6) 0.091(8) 0.005(5) -0.032(6) 0.010(5) C41 0.131(11) 0.109(10) 0.063(8) 0.016(7) -0.037(7) -0.060(8) F42 0.156(10) 0.167(12) 0.100(8) 0.039(8) -0.065(7) -0.064(9) F43 0.162(10) 0.128(9) 0.069(6) -0.011(6) 0.010(7) -0.032(8) F44 0.174(11) 0.130(9) 0.080(7) 0.022(6) -0.014(8) -0.087(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N8 1.988(5) . ? Cu1 N8 1.988(5) 2_666 ? Cu1 N1 2.010(4) . ? Cu1 N1 2.010(4) 2_666 ? Cu1 O40 2.725(17) . ? Cu1 O35 2.938(17) 1_645 ? N1 C2 1.319(7) . ? N1 C3 1.363(7) . ? C2 N3 1.348(7) . ? N3 C4 1.351(8) . ? N3 C6 1.467(8) . ? C3 C4 1.333(9) . ? C6 C7 1.471(12) . ? N8 C9 1.323(7) . ? N8 C12 1.382(7) . ? C9 N10 1.323(7) . ? N10 C11 1.345(8) . ? N10 C13 1.499(8) . ? C11 C12 1.366(9) . ? C13 C14 1.477(12) . ? C15 F17 1.318(9) . ? C15 F18 1.319(9) . ? C15 F16 1.320(9) . ? C15 S19 1.81(4) . ? S19 O24 1.40(4) . ? S19 O25 1.41(4) . ? S19 N22 1.56(3) . ? O20 S23 1.38(4) . ? O21 S23 1.40(4) . ? N22 S23 1.58(4) . ? S23 C26 1.87(4) . ? C26 F28 1.316(9) . ? C26 F29 1.320(9) . ? C26 F27 1.322(9) . ? C30 F32 1.297(8) . ? C30 F33 1.299(8) . ? C30 F31 1.299(8) . ? C30 S34 1.915(18) . ? S34 O35 1.36(2) . ? S34 O36 1.414(11) . ? S34 N37 1.551(14) . ? N37 S38 1.591(13) . ? S38 O40 1.436(18) . ? S38 O39 1.438(13) . ? S38 C41 1.802(18) . ? C41 F44 1.297(8) . ? C41 F42 1.298(8) . ? C41 F43 1.300(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Cu1 N8 179.999(1) . 2_666 ? N8 Cu1 N1 89.3(2) . . ? N8 Cu1 N1 90.7(2) 2_666 . ? N8 Cu1 N1 90.7(2) . 2_666 ? N8 Cu1 N1 89.3(2) 2_666 2_666 ? N1 Cu1 N1 179.999(1) . 2_666 ? N8 Cu1 O40 88.9(4) . . ? N8 Cu1 O40 91.1(4) 2_666 . ? N1 Cu1 O40 94.5(4) . . ? N1 Cu1 O40 85.5(4) 2_666 . ? N8 Cu1 O35 95.0(4) . 1_645 ? N8 Cu1 O35 85.0(4) 2_666 1_645 ? N1 Cu1 O35 94.0(4) . 1_645 ? N1 Cu1 O35 86.0(4) 2_666 1_645 ? O40 Cu1 O35 170.7(5) . 1_645 ? C2 N1 C3 104.5(5) . . ? C2 N1 Cu1 124.3(4) . . ? C3 N1 Cu1 131.1(4) . . ? N1 C2 N3 111.4(5) . . ? C2 N3 C4 106.6(5) . . ? C2 N3 C6 126.1(6) . . ? C4 N3 C6 127.2(6) . . ? C4 C3 N1 110.6(6) . . ? C3 C4 N3 106.8(5) . . ? N3 C6 C7 113.0(7) . . ? C9 N8 C12 105.2(5) . . ? C9 N8 Cu1 127.4(4) . . ? C12 N8 Cu1 127.4(4) . . ? N10 C9 N8 111.5(6) . . ? C9 N10 C11 108.2(5) . . ? C9 N10 C13 126.2(6) . . ? C11 N10 C13 125.6(6) . . ? N10 C11 C12 106.6(6) . . ? C11 C12 N8 108.4(6) . . ? C14 C13 N10 110.9(7) . . ? F17 C15 F18 109.4(13) . . ? F17 C15 F16 107.0(11) . . ? F18 C15 F16 109.2(12) . . ? F17 C15 S19 118.1(16) . . ? F18 C15 S19 102.1(16) . . ? F16 C15 S19 110.9(15) . . ? O24 S19 O25 115(2) . . ? O24 S19 N22 118(2) . . ? O25 S19 N22 107(3) . . ? O24 S19 C15 111(3) . . ? O25 S19 C15 109(2) . . ? N22 S19 C15 94.2(17) . . ? S19 N22 S23 124(3) . . ? O20 S23 O21 121(3) . . ? O20 S23 N22 118(3) . . ? O21 S23 N22 108(2) . . ? O20 S23 C26 109(2) . . ? O21 S23 C26 90(2) . . ? N22 S23 C26 106(2) . . ? F28 C26 F29 110.4(14) . . ? F28 C26 F27 107.6(13) . . ? F29 C26 F27 108.7(13) . . ? F28 C26 S23 110(2) . . ? F29 C26 S23 102(2) . . ? F27 C26 S23 118(2) . . ? F32 C30 F33 107.5(10) . . ? F32 C30 F31 109.2(10) . . ? F33 C30 F31 108.2(10) . . ? F32 C30 S34 96.1(9) . . ? F33 C30 S34 113.2(9) . . ? F31 C30 S34 121.2(10) . . ? O35 S34 O36 120.2(12) . . ? O35 S34 N37 115.3(9) . . ? O36 S34 N37 109.1(9) . . ? O35 S34 C30 101.0(11) . . ? O36 S34 C30 108.9(7) . . ? N37 S34 C30 99.7(7) . . ? S34 N37 S38 126.9(9) . . ? O40 S38 O39 121.8(11) . . ? O40 S38 N37 105.1(10) . . ? O39 S38 N37 117.4(8) . . ? O40 S38 C41 101.5(10) . . ? O39 S38 C41 99.3(7) . . ? N37 S38 C41 110.1(7) . . ? S38 O40 Cu1 157.3(11) . . ? F44 C41 F42 107.4(11) . . ? F44 C41 F43 108.0(11) . . ? F42 C41 F43 110.2(11) . . ? F44 C41 S38 98.1(9) . . ? F42 C41 S38 119.3(11) . . ? F43 C41 S38 112.5(10) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.602 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.088 # Attachment 'kb3n-[Cu-MeIm-4][Tf2N]2.cif' data_kb3n _database_code_depnum_ccdc_archive 'CCDC 883551' #TrackingRef 'kb3n-[Cu-MeIm-4][Tf2N]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(N-methylimidazole)copper(II) bis(trifluoromethyl)sulfonylimide ; _chemical_name_common ; tetrakis(N-methylimidazole)copper(II) bistriflimide ; _chemical_melting_point 362 _chemical_formula_moiety 'C20 H24 Cu F12 N10 O8 S4' _chemical_formula_sum 'C20 H24 Cu F12 N10 O8 S4' _chemical_formula_weight 952.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1104(5) _cell_length_b 9.6323(5) _cell_length_c 10.6590(7) _cell_angle_alpha 68.139(4) _cell_angle_beta 85.255(5) _cell_angle_gamma 87.828(4) _cell_volume 865.11(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2790 _cell_measurement_theta_min 4.871 _cell_measurement_theta_max 70.529 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 479 _exptl_absorpt_coefficient_mu 4.312 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.358 _exptl_absorpt_correction_T_max 0.412 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12483 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.48 _diffrn_reflns_theta_max 66.58 _reflns_number_total 2998 _reflns_number_gt 2543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ; A.L.Spek (2010) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+1.3454P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2998 _refine_ls_number_parameters 321 _refine_ls_number_restraints 537 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1520 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.5000 1.0000 0.0289(3) Uani 1 2 d S . . N1 N 0.5506(3) 0.2923(3) 1.1268(4) 0.0325(8) Uani 1 1 d . . . C2 C 0.5820(4) 0.1811(4) 1.0844(5) 0.0331(9) Uani 1 1 d . . . H2 H 0.5747 0.1869 0.9942 0.040 Uiso 1 1 calc R . . N3 N 0.6259(3) 0.0584(3) 1.1866(4) 0.0338(8) Uani 1 1 d . . . C4 C 0.6205(5) 0.0924(5) 1.2997(5) 0.0415(11) Uani 1 1 d . . . H4 H 0.6437 0.0280 1.3879 0.050 Uiso 1 1 calc R . . C5 C 0.5748(5) 0.2386(5) 1.2605(5) 0.0410(10) Uani 1 1 d . . . H5 H 0.5620 0.2940 1.3181 0.049 Uiso 1 1 calc R . . C6 C 0.6721(4) -0.0848(4) 1.1766(5) 0.0386(10) Uani 1 1 d . . . H6A H 0.6617 -0.0802 1.0844 0.058 Uiso 1 1 calc R . . H6B H 0.6103 -0.1650 1.2412 0.058 Uiso 1 1 calc R . . H6C H 0.7753 -0.1049 1.1977 0.058 Uiso 1 1 calc R . . N7 N 0.3148(3) 0.4202(3) 0.9634(4) 0.0280(7) Uani 1 1 d . . . C8 C 0.2065(4) 0.3603(4) 1.0576(4) 0.0305(9) Uani 1 1 d . . . H8 H 0.2117 0.3399 1.1514 0.037 Uiso 1 1 calc R . . N9 N 0.0893(3) 0.3324(3) 1.0038(4) 0.0311(8) Uani 1 1 d . . . C10 C 0.1233(5) 0.3757(5) 0.8668(5) 0.0359(9) Uani 1 1 d . . . H10 H 0.0616 0.3692 0.8016 0.043 Uiso 1 1 calc R . . C11 C 0.2631(4) 0.4300(4) 0.8428(5) 0.0343(9) Uani 1 1 d . . . H11 H 0.3163 0.4684 0.7565 0.041 Uiso 1 1 calc R . . C12 C -0.0507(4) 0.2686(5) 1.0753(5) 0.0389(10) Uani 1 1 d . . . H12A H -0.0634 0.1704 1.0700 0.058 Uiso 1 1 calc R . . H12B H -0.1317 0.3352 1.0334 0.058 Uiso 1 1 calc R . . H12C H -0.0508 0.2575 1.1706 0.058 Uiso 1 1 calc R . . C13 C 0.7632(19) 0.5917(18) 0.5612(14) 0.031(2) Uani 0.50 1 d PD A 1 F14 F 0.8058(9) 0.5685(14) 0.4494(12) 0.0485(17) Uani 0.50 1 d PD A 1 F15 F 0.6667(19) 0.703(2) 0.532(2) 0.051(2) Uani 0.50 1 d PDU A 1 F16 F 0.878(3) 0.629(4) 0.609(3) 0.039(3) Uani 0.50 1 d PD A 1 S17 S 0.6889(10) 0.4128(19) 0.6862(13) 0.0331(5) Uani 0.50 1 d PDU A 1 O18 O 0.5539(9) 0.3896(11) 0.6350(11) 0.0438(17) Uani 0.50 1 d PDU A 1 O19 O 0.6182(10) 0.4641(14) 0.7840(9) 0.0371(16) Uani 0.50 1 d PDU A 1 N20 N 0.8216(18) 0.2994(14) 0.7274(15) 0.0299(12) Uani 0.50 1 d PDU A 1 S21 S 0.8155(12) 0.1242(14) 0.7734(10) 0.0293(8) Uani 0.50 1 d PDU A 1 O22 O 0.9231(11) 0.0613(12) 0.8719(8) 0.0443(17) Uani 0.50 1 d PDU A 1 O23 O 0.6693(16) 0.068(3) 0.8106(14) 0.035(2) Uani 0.50 1 d PDU A 1 C24 C 0.8866(8) 0.0809(7) 0.6254(7) 0.0436(18) Uani 0.50 1 d PDU A 1 F25 F 0.8168(10) 0.1631(9) 0.5194(8) 0.066(2) Uani 0.50 1 d PDU A 1 F26 F 1.0288(6) 0.1048(6) 0.6010(6) 0.0510(13) Uani 0.50 1 d PDU A 1 F27 F 0.8615(9) -0.0625(7) 0.6554(11) 0.054(2) Uani 0.50 1 d PDU A 1 C13' C 0.7967(18) 0.5715(18) 0.5616(14) 0.031(2) Uani 0.50 1 d PDU B 2 F14' F 0.8629(9) 0.5457(14) 0.4576(12) 0.0485(17) Uani 0.50 1 d PDU B 2 F15' F 0.7025(19) 0.684(2) 0.516(2) 0.051(2) Uani 0.50 1 d PDU B 2 F16' F 0.897(3) 0.611(4) 0.625(3) 0.039(3) Uani 0.50 1 d PDU B 2 S17' S 0.6803(10) 0.4170(19) 0.6802(13) 0.0331(5) Uani 0.50 1 d PDU B 2 O18' O 0.5965(9) 0.3667(11) 0.5962(10) 0.0438(17) Uani 0.50 1 d PDU B 2 O19' O 0.6553(10) 0.4559(15) 0.8046(10) 0.0371(16) Uani 0.50 1 d PU B 2 N20' N 0.8236(18) 0.3175(14) 0.7025(15) 0.0299(12) Uani 0.50 1 d PDU B 2 S21' S 0.8111(12) 0.1418(14) 0.7627(10) 0.0293(8) Uani 0.50 1 d PDU B 2 O22' O 0.9487(10) 0.0771(12) 0.8119(9) 0.0443(17) Uani 0.50 1 d PDU B 2 O23' O 0.6807(17) 0.077(3) 0.8434(13) 0.035(2) Uani 0.50 1 d PDU B 2 C24' C 0.7895(8) 0.0966(8) 0.6110(8) 0.0512(19) Uani 0.50 1 d PDU B 2 F25' F 0.8947(10) 0.1569(11) 0.5142(10) 0.085(3) Uani 0.50 1 d PDU B 2 F26' F 0.7939(9) -0.0498(7) 0.6399(11) 0.057(2) Uani 0.50 1 d PDU B 2 F27' F 0.6629(8) 0.1473(7) 0.5539(6) 0.0656(17) Uani 0.50 1 d PDU B 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 Cu1 0.0159(4) 0.0139(4) 0.0489(5) -0.0026(3) -0.0016(3) 0.0000(3) N1 0.0176(15) 0.0155(15) 0.055(2) -0.0017(14) -0.0065(15) 0.0010(11) C2 0.0206(18) 0.0199(18) 0.051(3) -0.0034(17) -0.0044(18) -0.0047(14) N3 0.0215(16) 0.0169(15) 0.053(2) -0.0016(14) -0.0037(15) 0.0012(12) C4 0.040(2) 0.022(2) 0.055(3) -0.0038(18) -0.013(2) 0.0041(17) C5 0.038(2) 0.024(2) 0.058(3) -0.0103(19) -0.010(2) 0.0055(17) C6 0.029(2) 0.0191(19) 0.061(3) -0.0063(18) -0.008(2) 0.0037(15) N7 0.0185(15) 0.0165(14) 0.0445(19) -0.0061(13) -0.0013(14) -0.0008(11) C8 0.0229(19) 0.0195(17) 0.045(2) -0.0078(16) -0.0016(18) -0.0012(14) N9 0.0215(16) 0.0210(15) 0.050(2) -0.0138(15) 0.0028(15) -0.0028(12) C10 0.029(2) 0.033(2) 0.051(3) -0.0212(19) -0.0019(19) -0.0027(17) C11 0.026(2) 0.028(2) 0.049(3) -0.0164(18) 0.0035(19) -0.0026(16) C12 0.0216(19) 0.028(2) 0.065(3) -0.016(2) 0.008(2) -0.0034(16) C13 0.026(7) 0.025(4) 0.035(2) -0.002(2) -0.003(3) 0.002(4) F14 0.049(6) 0.059(4) 0.0292(19) -0.008(2) 0.002(4) 0.001(4) F15 0.041(7) 0.026(4) 0.064(5) 0.008(2) -0.008(5) 0.009(4) F16 0.035(5) 0.028(7) 0.046(5) -0.005(6) -0.004(3) -0.008(4) S17 0.0253(9) 0.0227(8) 0.0412(9) 0.0016(8) -0.0096(7) -0.0026(8) O18 0.033(4) 0.030(3) 0.064(5) -0.010(2) -0.019(3) 0.004(3) O19 0.021(3) 0.0294(17) 0.048(3) -0.003(2) 0.009(2) 0.010(2) N20 0.0262(15) 0.022(2) 0.040(3) -0.010(2) -0.002(2) -0.0005(17) S21 0.0282(7) 0.018(2) 0.0437(12) -0.0137(14) -0.0036(7) 0.0006(10) O22 0.031(3) 0.030(2) 0.073(5) -0.019(4) -0.006(4) 0.007(2) O23 0.034(2) 0.027(2) 0.039(5) -0.007(4) -0.005(3) -0.0033(18) C24 0.061(4) 0.026(3) 0.048(4) -0.019(3) -0.002(4) -0.002(4) F25 0.102(5) 0.062(4) 0.047(4) -0.032(3) -0.033(4) 0.013(5) F26 0.058(3) 0.041(3) 0.051(3) -0.019(2) 0.024(3) -0.009(2) F27 0.077(6) 0.032(3) 0.064(4) -0.030(3) 0.001(5) -0.004(3) C13' 0.026(7) 0.025(4) 0.035(2) -0.002(2) -0.003(3) 0.002(4) F14' 0.049(6) 0.059(4) 0.0292(19) -0.008(2) 0.002(4) 0.001(4) F15' 0.041(7) 0.026(4) 0.064(5) 0.008(2) -0.008(5) 0.009(4) F16' 0.035(5) 0.028(7) 0.046(5) -0.005(6) -0.004(3) -0.008(4) S17' 0.0253(9) 0.0227(8) 0.0412(9) 0.0016(8) -0.0096(7) -0.0026(8) O18' 0.033(4) 0.030(3) 0.064(5) -0.010(2) -0.019(3) 0.004(3) O19' 0.021(3) 0.0294(17) 0.048(3) -0.003(2) 0.009(2) 0.010(2) N20' 0.0262(15) 0.022(2) 0.040(3) -0.010(2) -0.002(2) -0.0005(17) S21' 0.0282(7) 0.018(2) 0.0437(12) -0.0137(14) -0.0036(7) 0.0006(10) O22' 0.031(3) 0.030(2) 0.073(5) -0.019(4) -0.006(4) 0.007(2) O23' 0.034(2) 0.027(2) 0.039(5) -0.007(4) -0.005(3) -0.0033(18) C24' 0.073(5) 0.034(4) 0.049(4) -0.022(3) 0.012(4) -0.007(4) F25' 0.113(6) 0.066(4) 0.079(5) -0.040(4) 0.059(5) -0.038(5) F26' 0.074(5) 0.033(3) 0.073(5) -0.032(3) 0.004(5) -0.004(3) F27' 0.102(5) 0.055(3) 0.052(3) -0.030(3) -0.029(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N7 2.005(3) . ? Cu1 N7 2.005(3) 2_667 ? Cu1 N1 2.015(3) 2_667 ? Cu1 N1 2.015(3) . ? N1 C2 1.322(6) . ? N1 C5 1.357(6) . ? C2 N3 1.350(5) . ? N3 C4 1.358(6) . ? N3 C6 1.466(5) . ? C4 C5 1.370(6) . ? N7 C8 1.327(5) . ? N7 C11 1.375(6) . ? C8 N9 1.334(5) . ? N9 C10 1.372(6) . ? N9 C12 1.461(5) . ? C10 C11 1.363(6) . ? C13 F14 1.318(7) . ? C13 F16 1.319(7) . ? C13 F15 1.323(6) . ? C13 S17 1.852(7) . ? S17 O19 1.412(8) . ? S17 O18 1.443(6) . ? S17 N20 1.574(6) . ? N20 S21 1.574(6) . ? S21 O23 1.424(6) . ? S21 O22 1.443(6) . ? S21 C24 1.839(9) . ? C24 F26 1.312(6) . ? C24 F25 1.312(6) . ? C24 F27 1.321(6) . ? C13' F14' 1.318(6) . ? C13' F16' 1.321(6) . ? C13' F15' 1.322(7) . ? C13' S17' 1.852(7) . ? S17' O18' 1.443(6) . ? S17' O19' 1.506(11) . ? S17' N20' 1.571(6) . ? N20' S21' 1.575(6) . ? S21' O23' 1.424(6) . ? S21' O22' 1.429(6) . ? S21' C24' 1.851(14) . ? C24' F25' 1.324(7) . ? C24' F26' 1.327(6) . ? C24' F27' 1.339(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Cu1 N7 180.0(2) . 2_667 ? N7 Cu1 N1 90.69(12) . 2_667 ? N7 Cu1 N1 89.31(12) 2_667 2_667 ? N7 Cu1 N1 89.31(12) . . ? N7 Cu1 N1 90.69(12) 2_667 . ? N1 Cu1 N1 179.998(1) 2_667 . ? C2 N1 C5 106.1(3) . . ? C2 N1 Cu1 122.6(3) . . ? C5 N1 Cu1 131.0(3) . . ? N1 C2 N3 110.8(4) . . ? C2 N3 C4 107.5(3) . . ? C2 N3 C6 126.1(4) . . ? C4 N3 C6 126.4(4) . . ? N3 C4 C5 106.0(4) . . ? N1 C5 C4 109.6(4) . . ? C8 N7 C11 105.8(3) . . ? C8 N7 Cu1 123.6(3) . . ? C11 N7 Cu1 130.2(3) . . ? N7 C8 N9 111.5(4) . . ? C8 N9 C10 107.3(3) . . ? C8 N9 C12 127.1(4) . . ? C10 N9 C12 125.6(4) . . ? C11 C10 N9 106.4(4) . . ? C10 C11 N7 109.0(4) . . ? F14 C13 F16 109.4(9) . . ? F14 C13 F15 108.5(8) . . ? F16 C13 F15 108.9(9) . . ? F14 C13 S17 107.2(11) . . ? F16 C13 S17 109(2) . . ? F15 C13 S17 113.8(15) . . ? O19 S17 O18 94.7(7) . . ? O19 S17 N20 118.9(11) . . ? O18 S17 N20 126.6(12) . . ? O19 S17 C13 99.9(10) . . ? O18 S17 C13 105.5(13) . . ? N20 S17 C13 107.6(8) . . ? S17 N20 S21 126.9(14) . . ? O23 S21 O22 117.1(11) . . ? O23 S21 N20 112.4(13) . . ? O22 S21 N20 107.6(9) . . ? O23 S21 C24 108.0(9) . . ? O22 S21 C24 104.8(7) . . ? N20 S21 C24 106.1(9) . . ? F26 C24 F25 110.2(7) . . ? F26 C24 F27 109.1(6) . . ? F25 C24 F27 110.4(7) . . ? F26 C24 S21 110.9(6) . . ? F25 C24 S21 109.4(6) . . ? F27 C24 S21 106.8(8) . . ? F14' C13' F16' 108.8(9) . . ? F14' C13' F15' 108.8(8) . . ? F16' C13' F15' 108.6(9) . . ? F14' C13' S17' 115.1(11) . . ? F16' C13' S17' 111.6(19) . . ? F15' C13' S17' 103.7(15) . . ? O18' S17' O19' 138.8(8) . . ? O18' S17' N20' 104.7(10) . . ? O19' S17' N20' 105.1(10) . . ? O18' S17' C13' 105.8(11) . . ? O19' S17' C13' 103.7(9) . . ? N20' S17' C13' 86.9(8) . . ? S17' N20' S21' 119.9(13) . . ? O23' S21' O22' 117.3(12) . . ? O23' S21' N20' 118.2(13) . . ? O22' S21' N20' 109.5(9) . . ? O23' S21' C24' 100.5(8) . . ? O22' S21' C24' 105.9(7) . . ? N20' S21' C24' 103.0(9) . . ? F25' C24' F26' 107.2(7) . . ? F25' C24' F27' 105.4(7) . . ? F26' C24' F27' 106.9(6) . . ? F25' C24' S21' 111.9(8) . . ? F26' C24' S21' 111.7(8) . . ? F27' C24' S21' 113.4(6) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.678 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.100 # Attachment 'nam3-[Co-MeIm-6][Tf2N]2.cif' data_nam3 _database_code_depnum_ccdc_archive 'CCDC 883552' #TrackingRef 'nam3-[Co-MeIm-6][Tf2N]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis(N-methylimidazole)cobalt(II) bis(trifluoromethyl)sulfonylimide ; _chemical_name_common ; hexakis(N-methylimidazole)cobalt(II) bistriflimide ; _chemical_melting_point 410 _chemical_formula_moiety 'C24 H36 Co N12, 2(C2 F6 N O4 S2)' _chemical_formula_sum 'C28 H36 Co F12 N14 O8 S4' _chemical_formula_weight 1111.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2207(2) _cell_length_b 20.3211(4) _cell_length_c 27.0612(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.363(2) _cell_angle_gamma 90.00 _cell_volume 4516.83(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15625 _cell_measurement_theta_min 3.170 _cell_measurement_theta_max 29.170 _exptl_crystal_description needle _exptl_crystal_colour 'pale pink' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.584 _exptl_absorpt_correction_T_max 0.764 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26973 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8851 _reflns_number_gt 7041 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ; A.L.Spek (2010) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8851 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.51971(3) 0.252735(11) 0.594605(8) 0.01508(7) Uani 1 1 d . . . N1 N 0.36499(16) 0.21423(7) 0.53436(5) 0.0185(3) Uani 1 1 d . . . C2 C 0.3904(2) 0.21711(9) 0.48661(6) 0.0223(4) Uani 1 1 d . . . H2 H 0.4832 0.2369 0.4730 0.027 Uiso 1 1 calc R . . N3 N 0.26860(18) 0.18861(8) 0.45963(5) 0.0247(4) Uani 1 1 d . . . C4 C 0.1582(2) 0.16614(10) 0.49201(7) 0.0283(4) Uani 1 1 d . . . H4 H 0.0591 0.1438 0.4840 0.034 Uiso 1 1 calc R . . C5 C 0.2181(2) 0.18205(9) 0.53780(7) 0.0258(4) Uani 1 1 d . . . H5 H 0.1668 0.1725 0.5678 0.031 Uiso 1 1 calc R . . C6 C 0.2595(3) 0.18105(11) 0.40569(7) 0.0377(5) Uani 1 1 d . . . H6A H 0.1580 0.1586 0.3956 0.057 Uiso 0.50 1 calc PR . . H6B H 0.3524 0.1550 0.3953 0.057 Uiso 0.50 1 calc PR . . H6C H 0.2620 0.2245 0.3901 0.057 Uiso 0.50 1 calc PR . . H6D H 0.3570 0.2002 0.3917 0.057 Uiso 0.50 1 calc PR . . H6E H 0.1625 0.2037 0.3920 0.057 Uiso 0.50 1 calc PR . . H6F H 0.2530 0.1342 0.3973 0.057 Uiso 0.50 1 calc PR . . N7 N 0.67845(16) 0.16828(7) 0.58943(5) 0.0207(3) Uani 1 1 d . . . C8 C 0.6572(2) 0.11712(9) 0.55977(7) 0.0245(4) Uani 1 1 d . . . H8 H 0.5721 0.1139 0.5350 0.029 Uiso 1 1 calc R . . N9 N 0.76969(18) 0.07027(8) 0.56861(6) 0.0278(4) Uani 1 1 d . . . C10 C 0.8695(2) 0.09264(11) 0.60688(8) 0.0356(5) Uani 1 1 d . . . H10 H 0.9603 0.0703 0.6218 0.043 Uiso 1 1 calc R . . C11 C 0.8136(2) 0.15231(10) 0.61903(7) 0.0303(5) Uani 1 1 d . . . H11 H 0.8603 0.1796 0.6443 0.036 Uiso 1 1 calc R . . C12 C 0.7808(3) 0.00699(11) 0.54338(9) 0.0447(6) Uani 1 1 d . . . H12A H 0.8745 -0.0176 0.5573 0.067 Uiso 0.50 1 calc PR . . H12B H 0.7944 0.0144 0.5080 0.067 Uiso 0.50 1 calc PR . . H12C H 0.6810 -0.0183 0.5479 0.067 Uiso 0.50 1 calc PR . . H12D H 0.6921 0.0033 0.5182 0.067 Uiso 0.50 1 calc PR . . H12E H 0.7721 -0.0287 0.5675 0.067 Uiso 0.50 1 calc PR . . H12F H 0.8856 0.0039 0.5275 0.067 Uiso 0.50 1 calc PR . . N13 N 0.66253(16) 0.30565(7) 0.54240(5) 0.0204(3) Uani 1 1 d . . . C14 C 0.6527(2) 0.36915(9) 0.53221(6) 0.0241(4) Uani 1 1 d . . . H14 H 0.5816 0.3988 0.5478 0.029 Uiso 1 1 calc R . . N15 N 0.75543(18) 0.38663(8) 0.49719(5) 0.0278(4) Uani 1 1 d . . . C16 C 0.8360(2) 0.33091(11) 0.48435(7) 0.0347(5) Uani 1 1 d . . . H16 H 0.9163 0.3274 0.4602 0.042 Uiso 1 1 calc R . . C17 C 0.7800(2) 0.28172(10) 0.51244(7) 0.0297(4) Uani 1 1 d . . . H17 H 0.8161 0.2373 0.5117 0.036 Uiso 1 1 calc R . . C18 C 0.7720(3) 0.45216(11) 0.47513(8) 0.0440(6) Uani 1 1 d . . . H18A H 0.8565 0.4510 0.4506 0.066 Uiso 0.50 1 calc PR . . H18B H 0.8025 0.4840 0.5011 0.066 Uiso 0.50 1 calc PR . . H18C H 0.6681 0.4652 0.4590 0.066 Uiso 0.50 1 calc PR . . H18D H 0.6949 0.4825 0.4898 0.066 Uiso 0.50 1 calc PR . . H18E H 0.7489 0.4495 0.4394 0.066 Uiso 0.50 1 calc PR . . H18F H 0.8833 0.4683 0.4815 0.066 Uiso 0.50 1 calc PR . . N19 N 0.67637(16) 0.29148(7) 0.65462(5) 0.0203(3) Uani 1 1 d . . . C20 C 0.6616(2) 0.28485(9) 0.70262(6) 0.0231(4) Uani 1 1 d . . . H20 H 0.5691 0.2661 0.7172 0.028 Uiso 1 1 calc R . . N21 N 0.79234(17) 0.30764(8) 0.72865(5) 0.0240(3) Uani 1 1 d . . . C22 C 0.8982(2) 0.33054(10) 0.69537(7) 0.0290(4) Uani 1 1 d . . . H22 H 1.0020 0.3497 0.7025 0.035 Uiso 1 1 calc R . . C23 C 0.8263(2) 0.32066(10) 0.65008(7) 0.0291(5) Uani 1 1 d . . . H23 H 0.8725 0.3322 0.6196 0.035 Uiso 1 1 calc R . . C24 C 0.8169(2) 0.30692(12) 0.78248(7) 0.0394(6) Uani 1 1 d . . . H24A H 0.9227 0.3266 0.7917 0.059 Uiso 0.50 1 calc PR . . H24B H 0.8143 0.2614 0.7944 0.059 Uiso 0.50 1 calc PR . . H24C H 0.7303 0.3323 0.7974 0.059 Uiso 0.50 1 calc PR . . H24D H 0.7221 0.2869 0.7973 0.059 Uiso 0.50 1 calc PR . . H24E H 0.8306 0.3521 0.7946 0.059 Uiso 0.50 1 calc PR . . H24F H 0.9146 0.2813 0.7916 0.059 Uiso 0.50 1 calc PR . . N25 N 0.35674(16) 0.33473(7) 0.59993(5) 0.0181(3) Uani 1 1 d . . . C26 C 0.3555(2) 0.37770(9) 0.63642(7) 0.0237(4) Uani 1 1 d . . . H26 H 0.4348 0.3790 0.6629 0.028 Uiso 1 1 calc R . . N27 N 0.22971(17) 0.41928(7) 0.63183(5) 0.0226(3) Uani 1 1 d . . . C28 C 0.1434(2) 0.40237(9) 0.58929(6) 0.0231(4) Uani 1 1 d . . . H28 H 0.0476 0.4231 0.5760 0.028 Uiso 1 1 calc R . . C29 C 0.2211(2) 0.35067(9) 0.57010(6) 0.0203(4) Uani 1 1 d . . . H29 H 0.1880 0.3284 0.5405 0.024 Uiso 1 1 calc R . . C30 C 0.1963(3) 0.47376(10) 0.66535(8) 0.0364(5) Uani 1 1 d . . . H30A H 0.0970 0.4966 0.6537 0.055 Uiso 0.50 1 calc PR . . H30B H 0.2879 0.5046 0.6661 0.055 Uiso 0.50 1 calc PR . . H30C H 0.1815 0.4565 0.6987 0.055 Uiso 0.50 1 calc PR . . H30D H 0.2806 0.4752 0.6920 0.055 Uiso 0.50 1 calc PR . . H30E H 0.0897 0.4672 0.6795 0.055 Uiso 0.50 1 calc PR . . H30F H 0.1961 0.5153 0.6470 0.055 Uiso 0.50 1 calc PR . . N31 N 0.38178(16) 0.20198(7) 0.64883(5) 0.0188(3) Uani 1 1 d . . . C32 C 0.4366(2) 0.15380(9) 0.67784(6) 0.0208(4) Uani 1 1 d . . . H32 H 0.5390 0.1329 0.6747 0.025 Uiso 1 1 calc R . . N33 N 0.33021(17) 0.13804(8) 0.71221(5) 0.0227(3) Uani 1 1 d . . . C34 C 0.1985(2) 0.17824(10) 0.70483(7) 0.0267(4) Uani 1 1 d . . . H34 H 0.1027 0.1787 0.7233 0.032 Uiso 1 1 calc R . . C35 C 0.2311(2) 0.21735(10) 0.66608(6) 0.0237(4) Uani 1 1 d . . . H35 H 0.1607 0.2505 0.6527 0.028 Uiso 1 1 calc R . . C36 C 0.3530(2) 0.08796(10) 0.75047(7) 0.0333(5) Uani 1 1 d . . . H36A H 0.2570 0.0867 0.7708 0.050 Uiso 0.50 1 calc PR . . H36B H 0.4495 0.0986 0.7714 0.050 Uiso 0.50 1 calc PR . . H36C H 0.3678 0.0449 0.7350 0.050 Uiso 0.50 1 calc PR . . H36D H 0.4592 0.0668 0.7473 0.050 Uiso 0.50 1 calc PR . . H36E H 0.2667 0.0549 0.7467 0.050 Uiso 0.50 1 calc PR . . H36F H 0.3484 0.1086 0.7831 0.050 Uiso 0.50 1 calc PR . . C37 C 0.6699(2) 0.00415(11) 0.38277(8) 0.0343(5) Uani 1 1 d . . . F38 F 0.69020(17) -0.03791(6) 0.41998(5) 0.0589(4) Uani 1 1 d . . . F39 F 0.51912(14) -0.00256(6) 0.36403(5) 0.0492(3) Uani 1 1 d . . . F40 F 0.77322(14) -0.01180(7) 0.34840(5) 0.0505(3) Uani 1 1 d . . . S41 S 0.70700(6) 0.08801(2) 0.404794(18) 0.02797(12) Uani 1 1 d . . . O42 O 0.57958(18) 0.09889(7) 0.43813(5) 0.0430(4) Uani 1 1 d . . . O43 O 0.87092(16) 0.08693(7) 0.42446(5) 0.0394(4) Uani 1 1 d . . . N44 N 0.67136(18) 0.12926(8) 0.35665(6) 0.0315(4) Uani 1 1 d . . . S45 S 0.80339(6) 0.15191(3) 0.319201(18) 0.02938(12) Uani 1 1 d . . . O46 O 0.73173(17) 0.15261(8) 0.27050(5) 0.0474(4) Uani 1 1 d . . . O47 O 0.96270(15) 0.12562(7) 0.32679(5) 0.0367(3) Uani 1 1 d . . . C48 C 0.8246(3) 0.23863(11) 0.33563(9) 0.0399(5) Uani 1 1 d . . . F49 F 0.87489(17) 0.24510(6) 0.38263(5) 0.0553(4) Uani 1 1 d . . . F50 F 0.68586(16) 0.27108(7) 0.32882(6) 0.0614(4) Uani 1 1 d . . . F51 F 0.93497(17) 0.26697(7) 0.30781(6) 0.0610(4) Uani 1 1 d . . . C52 C 0.6882(3) 0.61926(12) 0.58465(8) 0.0403(5) Uani 1 1 d . . . F53 F 0.57035(17) 0.65488(7) 0.60247(5) 0.0614(4) Uani 1 1 d . . . F54 F 0.82248(17) 0.65536(7) 0.58635(6) 0.0647(4) Uani 1 1 d . . . F55 F 0.64902(19) 0.60719(8) 0.53724(5) 0.0685(4) Uani 1 1 d . . . S56 S 0.71814(5) 0.54112(2) 0.617301(17) 0.02613(12) Uani 1 1 d . . . O57 O 0.56370(16) 0.50942(7) 0.61246(5) 0.0365(3) Uani 1 1 d . . . O58 O 0.85174(17) 0.51254(8) 0.59309(5) 0.0433(4) Uani 1 1 d . . . N59 N 0.77906(17) 0.56272(8) 0.67058(6) 0.0282(4) Uani 1 1 d . . . S60 S 0.66232(6) 0.58110(3) 0.713499(17) 0.02870(12) Uani 1 1 d . . . O61 O 0.74472(18) 0.62628(8) 0.74611(5) 0.0441(4) Uani 1 1 d . . . O62 O 0.49674(16) 0.59367(8) 0.69863(5) 0.0410(4) Uani 1 1 d . . . C63 C 0.6563(3) 0.50513(12) 0.74948(8) 0.0394(5) Uani 1 1 d . . . F64 F 0.59748(17) 0.45547(6) 0.72222(5) 0.0515(3) Uani 1 1 d . . . F65 F 0.5581(2) 0.51391(8) 0.78656(5) 0.0703(5) Uani 1 1 d . . . F66 F 0.80095(17) 0.48803(8) 0.76728(5) 0.0680(5) Uani 1 1 d . . . 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 Co1 0.01422(12) 0.01772(13) 0.01328(12) -0.00035(9) 0.00053(9) 0.00015(9) N1 0.0179(7) 0.0184(8) 0.0190(7) -0.0015(6) -0.0015(6) 0.0018(6) C2 0.0234(9) 0.0244(10) 0.0187(9) -0.0029(8) -0.0032(7) 0.0046(8) N3 0.0270(8) 0.0260(9) 0.0204(8) -0.0052(7) -0.0072(7) 0.0058(7) C4 0.0221(10) 0.0286(11) 0.0337(11) -0.0074(9) -0.0056(8) -0.0011(8) C5 0.0243(10) 0.0270(10) 0.0261(10) -0.0041(8) -0.0002(8) -0.0034(8) C6 0.0485(13) 0.0447(13) 0.0188(10) -0.0075(9) -0.0112(9) 0.0062(11) N7 0.0173(7) 0.0255(9) 0.0193(7) 0.0021(7) 0.0029(6) 0.0024(6) C8 0.0233(9) 0.0239(10) 0.0262(10) 0.0012(8) -0.0004(8) 0.0060(8) N9 0.0295(9) 0.0242(9) 0.0301(9) 0.0032(7) 0.0058(7) 0.0096(7) C10 0.0244(10) 0.0441(13) 0.0381(12) 0.0065(10) -0.0001(9) 0.0152(9) C11 0.0210(10) 0.0394(12) 0.0300(10) -0.0019(9) -0.0046(8) 0.0060(9) C12 0.0564(14) 0.0283(12) 0.0498(14) -0.0045(10) 0.0061(11) 0.0170(11) N13 0.0199(7) 0.0252(9) 0.0162(7) -0.0019(6) 0.0013(6) -0.0015(6) C14 0.0259(10) 0.0280(11) 0.0185(9) 0.0009(8) 0.0024(7) -0.0020(8) N15 0.0315(9) 0.0320(10) 0.0200(8) 0.0045(7) 0.0026(7) -0.0093(7) C16 0.0327(11) 0.0451(14) 0.0274(10) -0.0029(10) 0.0147(9) -0.0080(10) C17 0.0282(10) 0.0322(11) 0.0294(10) -0.0032(9) 0.0112(8) 0.0009(9) C18 0.0585(14) 0.0374(13) 0.0365(12) 0.0119(10) 0.0068(11) -0.0178(11) N19 0.0159(7) 0.0255(8) 0.0195(8) -0.0010(6) 0.0001(6) -0.0021(6) C20 0.0185(9) 0.0325(11) 0.0185(9) -0.0025(8) 0.0013(7) -0.0050(8) N21 0.0215(8) 0.0361(9) 0.0141(7) -0.0039(7) -0.0024(6) -0.0004(7) C22 0.0180(9) 0.0426(12) 0.0263(10) -0.0044(9) -0.0012(8) -0.0085(9) C23 0.0226(10) 0.0435(12) 0.0213(10) 0.0015(9) 0.0031(8) -0.0101(9) C24 0.0326(11) 0.0668(16) 0.0183(10) -0.0054(10) -0.0037(8) -0.0053(11) N25 0.0173(7) 0.0193(8) 0.0178(7) -0.0005(6) 0.0014(6) -0.0002(6) C26 0.0224(9) 0.0228(10) 0.0257(10) -0.0065(8) -0.0020(8) 0.0014(8) N27 0.0216(8) 0.0199(8) 0.0266(8) -0.0072(7) 0.0049(6) 0.0010(6) C28 0.0205(9) 0.0230(10) 0.0256(10) 0.0026(8) 0.0009(7) 0.0023(8) C29 0.0217(9) 0.0214(10) 0.0177(9) 0.0006(7) 0.0005(7) 0.0020(8) C30 0.0376(11) 0.0297(12) 0.0421(12) -0.0159(10) 0.0051(10) 0.0083(9) N31 0.0159(7) 0.0226(8) 0.0178(7) -0.0005(6) -0.0007(6) -0.0010(6) C32 0.0190(9) 0.0230(10) 0.0205(9) 0.0028(8) 0.0026(7) -0.0007(7) N33 0.0208(8) 0.0259(9) 0.0215(8) 0.0060(7) 0.0037(6) -0.0017(7) C34 0.0189(9) 0.0359(11) 0.0257(10) 0.0029(9) 0.0064(7) 0.0012(8) C35 0.0168(9) 0.0294(11) 0.0252(10) 0.0029(8) 0.0025(7) 0.0026(8) C36 0.0317(11) 0.0384(12) 0.0303(11) 0.0181(9) 0.0072(9) 0.0010(9) C37 0.0308(11) 0.0320(12) 0.0398(12) -0.0042(10) -0.0025(9) 0.0012(9) F38 0.0760(10) 0.0332(8) 0.0663(9) 0.0121(7) -0.0110(8) -0.0029(7) F39 0.0349(7) 0.0493(8) 0.0626(9) -0.0104(7) -0.0092(6) -0.0107(6) F40 0.0461(8) 0.0441(8) 0.0616(9) -0.0227(7) 0.0054(7) 0.0075(6) S41 0.0281(3) 0.0271(3) 0.0283(3) -0.0030(2) -0.0043(2) 0.0027(2) O42 0.0506(9) 0.0451(9) 0.0340(8) -0.0041(7) 0.0103(7) 0.0098(8) O43 0.0355(8) 0.0425(9) 0.0388(8) 0.0027(7) -0.0162(6) -0.0037(7) N44 0.0220(8) 0.0357(10) 0.0364(9) 0.0063(8) -0.0029(7) 0.0029(7) S45 0.0247(2) 0.0346(3) 0.0284(3) -0.0025(2) -0.0040(2) 0.0018(2) O46 0.0416(8) 0.0695(12) 0.0303(8) -0.0004(8) -0.0088(7) -0.0035(8) O47 0.0256(7) 0.0423(9) 0.0421(8) -0.0057(7) 0.0012(6) 0.0054(6) C48 0.0363(12) 0.0357(13) 0.0478(14) 0.0031(11) 0.0031(10) 0.0022(10) F49 0.0658(9) 0.0447(8) 0.0549(9) -0.0197(7) -0.0025(7) -0.0034(7) F50 0.0527(8) 0.0427(8) 0.0893(11) 0.0132(8) 0.0090(8) 0.0195(7) F51 0.0583(9) 0.0463(8) 0.0797(11) 0.0120(8) 0.0202(8) -0.0091(7) C52 0.0348(12) 0.0483(14) 0.0388(13) 0.0115(11) 0.0121(10) 0.0082(11) F53 0.0603(9) 0.0504(9) 0.0759(10) 0.0271(7) 0.0309(7) 0.0308(7) F54 0.0544(9) 0.0547(9) 0.0867(11) 0.0205(8) 0.0237(8) -0.0102(7) F55 0.0876(11) 0.0828(11) 0.0350(8) 0.0224(7) 0.0001(7) 0.0162(9) S56 0.0253(2) 0.0304(3) 0.0228(2) -0.0011(2) 0.00220(19) 0.0071(2) O57 0.0371(8) 0.0399(9) 0.0322(8) -0.0033(7) -0.0033(6) -0.0070(7) O58 0.0436(9) 0.0556(10) 0.0313(8) -0.0045(7) 0.0089(7) 0.0247(8) N59 0.0183(8) 0.0411(10) 0.0252(8) -0.0030(8) 0.0024(6) 0.0017(7) S60 0.0264(3) 0.0343(3) 0.0259(3) -0.0062(2) 0.0059(2) -0.0023(2) O61 0.0539(9) 0.0437(9) 0.0350(8) -0.0140(7) 0.0063(7) -0.0138(8) O62 0.0270(7) 0.0543(10) 0.0425(9) -0.0051(7) 0.0108(6) 0.0084(7) C63 0.0426(13) 0.0483(14) 0.0270(11) -0.0013(10) -0.0017(10) -0.0107(11) F64 0.0711(9) 0.0378(8) 0.0446(8) -0.0015(6) -0.0075(7) -0.0155(7) F65 0.1001(12) 0.0723(11) 0.0410(8) -0.0004(7) 0.0331(8) -0.0247(9) F66 0.0653(9) 0.0726(11) 0.0635(10) 0.0264(8) -0.0286(8) -0.0109(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N25 2.1467(14) . ? Co1 N31 2.1541(14) . ? Co1 N13 2.1604(15) . ? Co1 N7 2.1640(15) . ? Co1 N1 2.1718(13) . ? Co1 N19 2.1779(13) . ? N1 C2 1.319(2) . ? N1 C5 1.380(2) . ? C2 N3 1.346(2) . ? N3 C4 1.366(2) . ? N3 C6 1.466(2) . ? C4 C5 1.354(2) . ? N7 C8 1.321(2) . ? N7 C11 1.381(2) . ? C8 N9 1.342(2) . ? N9 C10 1.372(3) . ? N9 C12 1.461(3) . ? C10 C11 1.342(3) . ? N13 C14 1.321(2) . ? N13 C17 1.375(2) . ? C14 N15 1.343(2) . ? N15 C16 1.364(3) . ? N15 C18 1.468(3) . ? C16 C17 1.348(3) . ? N19 C20 1.316(2) . ? N19 C23 1.378(2) . ? C20 N21 1.343(2) . ? N21 C22 1.360(2) . ? N21 C24 1.463(2) . ? C22 C23 1.353(2) . ? N25 C26 1.318(2) . ? N25 C29 1.388(2) . ? C26 N27 1.337(2) . ? N27 C28 1.371(2) . ? N27 C30 1.464(2) . ? C28 C29 1.345(2) . ? N31 C32 1.322(2) . ? N31 C35 1.377(2) . ? C32 N33 1.341(2) . ? N33 C34 1.365(2) . ? N33 C36 1.458(2) . ? C34 C35 1.351(3) . ? C37 F40 1.326(2) . ? C37 F38 1.326(2) . ? C37 F39 1.327(2) . ? C37 S41 1.827(2) . ? S41 O42 1.4275(15) . ? S41 O43 1.4285(13) . ? S41 N44 1.5666(16) . ? N44 S45 1.5835(17) . ? S45 O46 1.4213(14) . ? S45 O47 1.4215(13) . ? S45 C48 1.824(2) . ? C48 F50 1.323(2) . ? C48 F49 1.328(3) . ? C48 F51 1.334(3) . ? C52 F53 1.317(2) . ? C52 F54 1.324(3) . ? C52 F55 1.332(3) . ? C52 S56 1.829(2) . ? S56 O57 1.4248(14) . ? S56 O58 1.4256(14) . ? S56 N59 1.5693(16) . ? N59 S60 1.5816(16) . ? S60 O61 1.4251(15) . ? S60 O62 1.4265(14) . ? S60 C63 1.827(2) . ? C63 F66 1.311(2) . ? C63 F65 1.326(2) . ? C63 F64 1.329(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N25 Co1 N31 88.76(5) . . ? N25 Co1 N13 90.86(5) . . ? N31 Co1 N13 177.89(5) . . ? N25 Co1 N7 178.44(5) . . ? N31 Co1 N7 90.01(5) . . ? N13 Co1 N7 90.40(5) . . ? N25 Co1 N1 88.98(5) . . ? N31 Co1 N1 91.74(5) . . ? N13 Co1 N1 90.32(5) . . ? N7 Co1 N1 90.10(5) . . ? N25 Co1 N19 91.19(5) . . ? N31 Co1 N19 88.67(5) . . ? N13 Co1 N19 89.26(5) . . ? N7 Co1 N19 89.73(5) . . ? N1 Co1 N19 179.55(5) . . ? C2 N1 C5 105.17(14) . . ? C2 N1 Co1 127.44(12) . . ? C5 N1 Co1 127.39(11) . . ? N1 C2 N3 111.60(17) . . ? C2 N3 C4 107.15(15) . . ? C2 N3 C6 126.25(17) . . ? C4 N3 C6 126.57(15) . . ? C5 C4 N3 106.35(16) . . ? C4 C5 N1 109.73(17) . . ? C8 N7 C11 104.50(15) . . ? C8 N7 Co1 126.78(11) . . ? C11 N7 Co1 128.43(12) . . ? N7 C8 N9 112.18(15) . . ? C8 N9 C10 106.60(16) . . ? C8 N9 C12 126.68(16) . . ? C10 N9 C12 126.70(16) . . ? C11 C10 N9 106.52(16) . . ? C10 C11 N7 110.20(17) . . ? C14 N13 C17 105.12(15) . . ? C14 N13 Co1 126.31(12) . . ? C17 N13 Co1 128.56(13) . . ? N13 C14 N15 111.75(17) . . ? C14 N15 C16 106.63(16) . . ? C14 N15 C18 126.76(18) . . ? C16 N15 C18 126.54(17) . . ? C17 C16 N15 106.92(17) . . ? C16 C17 N13 109.56(18) . . ? C20 N19 C23 104.55(14) . . ? C20 N19 Co1 128.54(12) . . ? C23 N19 Co1 126.35(11) . . ? N19 C20 N21 112.20(16) . . ? C20 N21 C22 106.91(14) . . ? C20 N21 C24 126.42(16) . . ? C22 N21 C24 126.66(15) . . ? C23 C22 N21 106.36(15) . . ? C22 C23 N19 109.98(16) . . ? C26 N25 C29 104.48(14) . . ? C26 N25 Co1 126.06(11) . . ? C29 N25 Co1 129.12(11) . . ? N25 C26 N27 112.27(15) . . ? C26 N27 C28 106.92(14) . . ? C26 N27 C30 125.77(15) . . ? C28 N27 C30 127.28(15) . . ? C29 C28 N27 106.40(15) . . ? C28 C29 N25 109.93(15) . . ? C32 N31 C35 104.81(15) . . ? C32 N31 Co1 125.66(11) . . ? C35 N31 Co1 128.93(12) . . ? N31 C32 N33 111.88(15) . . ? C32 N33 C34 106.96(15) . . ? C32 N33 C36 126.21(15) . . ? C34 N33 C36 126.83(15) . . ? C35 C34 N33 106.49(16) . . ? C34 C35 N31 109.87(16) . . ? F40 C37 F38 108.10(17) . . ? F40 C37 F39 108.80(16) . . ? F38 C37 F39 108.08(18) . . ? F40 C37 S41 110.72(14) . . ? F38 C37 S41 109.84(14) . . ? F39 C37 S41 111.20(14) . . ? O42 S41 O43 118.19(9) . . ? O42 S41 N44 109.01(9) . . ? O43 S41 N44 117.34(9) . . ? O42 S41 C37 103.51(10) . . ? O43 S41 C37 104.45(9) . . ? N44 S41 C37 101.82(9) . . ? S41 N44 S45 125.32(10) . . ? O46 S45 O47 118.81(9) . . ? O46 S45 N44 109.12(9) . . ? O47 S45 N44 116.74(9) . . ? O46 S45 C48 104.36(10) . . ? O47 S45 C48 104.46(9) . . ? N44 S45 C48 100.71(10) . . ? F50 C48 F49 108.46(19) . . ? F50 C48 F51 107.98(18) . . ? F49 C48 F51 107.80(18) . . ? F50 C48 S45 111.98(15) . . ? F49 C48 S45 110.61(15) . . ? F51 C48 S45 109.87(16) . . ? F53 C52 F54 107.9(2) . . ? F53 C52 F55 107.54(17) . . ? F54 C52 F55 107.68(18) . . ? F53 C52 S56 112.74(14) . . ? F54 C52 S56 111.65(14) . . ? F55 C52 S56 109.13(16) . . ? O57 S56 O58 118.29(9) . . ? O57 S56 N59 117.41(8) . . ? O58 S56 N59 108.27(8) . . ? O57 S56 C52 104.28(9) . . ? O58 S56 C52 102.85(10) . . ? N59 S56 C52 103.44(10) . . ? S56 N59 S60 124.09(9) . . ? O61 S60 O62 118.88(10) . . ? O61 S60 N59 108.64(9) . . ? O62 S60 N59 115.85(8) . . ? O61 S60 C63 103.70(9) . . ? O62 S60 C63 104.78(10) . . ? N59 S60 C63 102.85(10) . . ? F66 C63 F65 109.22(18) . . ? F66 C63 F64 107.8(2) . . ? F65 C63 F64 107.64(18) . . ? F66 C63 S60 112.07(15) . . ? F65 C63 S60 108.68(16) . . ? F64 C63 S60 111.28(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.315 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.048 # Attachment 'nam6-[Ni-MeIm-6][Tf2N]2.cif' data_nam6 _database_code_depnum_ccdc_archive 'CCDC 883553' #TrackingRef 'nam6-[Ni-MeIm-6][Tf2N]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis(N-methylimidazole)nickel(II) bis(trifluoromethyl)sulfonylimide ; _chemical_name_common ; hexakis(N-methylimidazole)nickel(II) bistriflimide ; _chemical_melting_point 420 _chemical_formula_moiety 'C24 H36 N12 Ni, 2(C2 F6 N O4 S2)' _chemical_formula_sum 'C28 H36 F12 N14 Ni O8 S4' _chemical_formula_weight 1111.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2018(2) _cell_length_b 20.3183(5) _cell_length_c 26.9380(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.341(3) _cell_angle_gamma 90.00 _cell_volume 4485.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5633 _cell_measurement_theta_min 3.121 _cell_measurement_theta_max 29.251 _exptl_crystal_description needle _exptl_crystal_colour 'pale purple' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14425 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9720 _reflns_number_gt 8083 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ; A.L.Spek (2010) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9836 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1225 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.47967(6) 0.25358(2) 0.404840(18) 0.01332(12) Uani 1 1 d . . . N1 N 0.3398(4) 0.30547(16) 0.45640(12) 0.0183(8) Uani 1 1 d . . . C2 C 0.3500(5) 0.3689(2) 0.46710(16) 0.0229(10) Uani 1 1 d . . . H2 H 0.4222 0.3986 0.4520 0.027 Uiso 1 1 calc R . . N3 N 0.2456(4) 0.38602(19) 0.50201(13) 0.0257(9) Uani 1 1 d . . . C4 C 0.1629(6) 0.3307(2) 0.51407(17) 0.0317(11) Uani 1 1 d . . . H4 H 0.0806 0.3272 0.5378 0.038 Uiso 1 1 calc R . . C5 C 0.2204(5) 0.2818(2) 0.48586(17) 0.0270(10) Uani 1 1 d . . . H5 H 0.1836 0.2375 0.4863 0.032 Uiso 1 1 calc R . . C6 C 0.2299(7) 0.4510(2) 0.5245(2) 0.0403(13) Uani 1 1 d . . . H6A H 0.3029 0.4820 0.5086 0.060 Uiso 0.50 1 calc PR . . H6B H 0.2593 0.4483 0.5601 0.060 Uiso 0.50 1 calc PR . . H6C H 0.1169 0.4663 0.5200 0.060 Uiso 0.50 1 calc PR . . H6D H 0.1498 0.4490 0.5505 0.060 Uiso 0.50 1 calc PR . . H6E H 0.1935 0.4827 0.4991 0.060 Uiso 0.50 1 calc PR . . H6F H 0.3358 0.4648 0.5392 0.060 Uiso 0.50 1 calc PR . . N7 N 0.3252(4) 0.29186(17) 0.34586(12) 0.0177(8) Uani 1 1 d . . . C8 C 0.3386(5) 0.2835(2) 0.29740(17) 0.0250(10) Uani 1 1 d . . . H8 H 0.4294 0.2633 0.2828 0.030 Uiso 1 1 calc R . . N9 N 0.2090(4) 0.30697(18) 0.27156(13) 0.0211(8) Uani 1 1 d . . . C10 C 0.1042(5) 0.3321(2) 0.30470(17) 0.0272(11) Uani 1 1 d . . . H10 H 0.0012 0.3520 0.2974 0.033 Uiso 1 1 calc R . . C11 C 0.1769(5) 0.3227(2) 0.35005(17) 0.0245(10) Uani 1 1 d . . . H11 H 0.1321 0.3356 0.3805 0.029 Uiso 1 1 calc R . . C12 C 0.1832(6) 0.3045(3) 0.21753(17) 0.0351(12) Uani 1 1 d . . . H12A H 0.0778 0.3247 0.2081 0.053 Uiso 0.50 1 calc PR . . H12B H 0.1838 0.2586 0.2064 0.053 Uiso 0.50 1 calc PR . . H12C H 0.2708 0.3287 0.2018 0.053 Uiso 0.50 1 calc PR . . H12D H 0.2771 0.2833 0.2028 0.053 Uiso 0.50 1 calc PR . . H12E H 0.1711 0.3494 0.2045 0.053 Uiso 0.50 1 calc PR . . H12F H 0.0842 0.2793 0.2091 0.053 Uiso 0.50 1 calc PR . . N13 N 0.3240(4) 0.17046(16) 0.40952(13) 0.0179(8) Uani 1 1 d . . . C14 C 0.3473(5) 0.1184(2) 0.43855(17) 0.0234(10) Uani 1 1 d . . . H14 H 0.4355 0.1141 0.4623 0.028 Uiso 1 1 calc R . . N15 N 0.2318(4) 0.07267(18) 0.43042(14) 0.0275(9) Uani 1 1 d . . . C16 C 0.1291(6) 0.0968(2) 0.39360(18) 0.0329(12) Uani 1 1 d . . . H16 H 0.0354 0.0754 0.3794 0.039 Uiso 1 1 calc R . . C17 C 0.1854(5) 0.1568(2) 0.38104(17) 0.0264(10) Uani 1 1 d . . . H17 H 0.1370 0.1850 0.3565 0.032 Uiso 1 1 calc R . . C18 C 0.2220(7) 0.0086(2) 0.4552(2) 0.0441(14) Uani 1 1 d . . . H18A H 0.1255 -0.0152 0.4421 0.066 Uiso 0.50 1 calc PR . . H18B H 0.2138 0.0152 0.4910 0.066 Uiso 0.50 1 calc PR . . H18C H 0.3202 -0.0171 0.4489 0.066 Uiso 0.50 1 calc PR . . H18D H 0.3142 0.0038 0.4792 0.066 Uiso 0.50 1 calc PR . . H18E H 0.2259 -0.0266 0.4303 0.066 Uiso 0.50 1 calc PR . . H18F H 0.1195 0.0057 0.4725 0.066 Uiso 0.50 1 calc PR . . N19 N 0.6162(4) 0.20343(16) 0.35184(12) 0.0165(7) Uani 1 1 d . . . C20 C 0.5640(5) 0.1535(2) 0.32355(15) 0.0195(9) Uani 1 1 d . . . H20 H 0.4629 0.1316 0.3273 0.023 Uiso 1 1 calc R . . N21 N 0.6706(4) 0.13786(17) 0.28911(13) 0.0206(8) Uani 1 1 d . . . C22 C 0.8006(5) 0.1791(2) 0.29564(16) 0.0258(10) Uani 1 1 d . . . H22 H 0.8965 0.1797 0.2770 0.031 Uiso 1 1 calc R . . C23 C 0.7657(5) 0.2195(2) 0.33420(16) 0.0220(10) Uani 1 1 d . . . H23 H 0.8346 0.2536 0.3470 0.026 Uiso 1 1 calc R . . C24 C 0.6508(6) 0.0867(2) 0.25162(18) 0.0316(11) Uani 1 1 d . . . H24A H 0.7472 0.0857 0.2313 0.047 Uiso 0.50 1 calc PR . . H24B H 0.5537 0.0960 0.2304 0.047 Uiso 0.50 1 calc PR . . H24C H 0.6382 0.0440 0.2679 0.047 Uiso 0.50 1 calc PR . . H24D H 0.5455 0.0648 0.2551 0.047 Uiso 0.50 1 calc PR . . H24E H 0.7391 0.0545 0.2560 0.047 Uiso 0.50 1 calc PR . . H24F H 0.6545 0.1065 0.2185 0.047 Uiso 0.50 1 calc PR . . N25 N 0.6314(4) 0.21579(16) 0.46401(12) 0.0171(7) Uani 1 1 d . . . C26 C 0.6072(5) 0.2193(2) 0.51249(16) 0.0204(9) Uani 1 1 d . . . H26 H 0.5159 0.2400 0.5264 0.024 Uiso 1 1 calc R . . N27 N 0.7273(4) 0.18985(17) 0.53921(13) 0.0231(8) Uani 1 1 d . . . C28 C 0.8373(6) 0.1671(2) 0.50702(18) 0.0300(11) Uani 1 1 d . . . H28 H 0.9368 0.1450 0.5152 0.036 Uiso 1 1 calc R . . C29 C 0.7764(5) 0.1825(2) 0.46039(17) 0.0233(10) Uani 1 1 d . . . H29 H 0.8265 0.1718 0.4302 0.028 Uiso 1 1 calc R . . C30 C 0.7376(6) 0.1824(2) 0.59349(17) 0.0353(12) Uani 1 1 d . . . H30A H 0.8381 0.1589 0.6033 0.053 Uiso 0.50 1 calc PR . . H30B H 0.6432 0.1573 0.6042 0.053 Uiso 0.50 1 calc PR . . H30C H 0.7384 0.2259 0.6091 0.053 Uiso 0.50 1 calc PR . . H30D H 0.6417 0.2026 0.6078 0.053 Uiso 0.50 1 calc PR . . H30E H 0.8366 0.2041 0.6069 0.053 Uiso 0.50 1 calc PR . . H30F H 0.7414 0.1355 0.6020 0.053 Uiso 0.50 1 calc PR . . N31 N 0.6389(4) 0.33427(16) 0.39963(13) 0.0170(7) Uani 1 1 d . . . C32 C 0.6399(5) 0.3769(2) 0.36277(16) 0.0206(9) Uani 1 1 d . . . H32 H 0.5608 0.3779 0.3360 0.025 Uiso 1 1 calc R . . N33 N 0.7660(4) 0.41876(17) 0.36757(13) 0.0219(8) Uani 1 1 d . . . C34 C 0.8517(5) 0.4025(2) 0.41048(16) 0.0211(9) Uani 1 1 d . . . H34 H 0.9468 0.4236 0.4240 0.025 Uiso 1 1 calc R . . C35 C 0.7740(5) 0.3504(2) 0.42966(15) 0.0185(9) Uani 1 1 d . . . H35 H 0.8072 0.3282 0.4594 0.022 Uiso 1 1 calc R . . C36 C 0.7996(6) 0.4733(2) 0.3338(2) 0.0361(12) Uani 1 1 d . . . H36A H 0.8985 0.4964 0.3457 0.054 Uiso 0.50 1 calc PR . . H36B H 0.7073 0.5039 0.3327 0.054 Uiso 0.50 1 calc PR . . H36C H 0.8155 0.4559 0.3004 0.054 Uiso 0.50 1 calc PR . . H36D H 0.7157 0.4744 0.3068 0.054 Uiso 0.50 1 calc PR . . H36E H 0.9069 0.4669 0.3198 0.054 Uiso 0.50 1 calc PR . . H36F H 0.7987 0.5149 0.3521 0.054 Uiso 0.50 1 calc PR . . C37 C 0.6900(6) 0.3815(3) 0.5851(2) 0.0373(13) Uani 1 1 d . . . F38 F 0.8257(4) 0.34561(17) 0.58700(14) 0.0652(11) Uani 1 1 d . . . F39 F 0.5722(4) 0.34629(15) 0.60337(13) 0.0582(10) Uani 1 1 d . . . F40 F 0.6515(5) 0.39341(19) 0.53776(12) 0.0678(11) Uani 1 1 d . . . S41 S 0.72024(13) 0.46000(6) 0.61796(4) 0.0243(3) Uani 1 1 d . . . O42 O 0.8534(4) 0.48895(18) 0.59354(13) 0.0406(9) Uani 1 1 d . . . O43 O 0.5638(4) 0.49103(16) 0.61314(12) 0.0343(8) Uani 1 1 d . . . N44 N 0.7820(4) 0.43832(19) 0.67170(14) 0.0282(9) Uani 1 1 d . . . S45 S 0.66587(14) 0.41986(6) 0.71466(4) 0.0266(3) Uani 1 1 d . . . O46 O 0.4995(4) 0.40664(18) 0.70005(13) 0.0384(9) Uani 1 1 d . . . O47 O 0.7503(5) 0.37464(17) 0.74721(13) 0.0405(9) Uani 1 1 d . . . C48 C 0.6588(6) 0.4963(3) 0.75083(18) 0.0383(13) Uani 1 1 d . . . F49 F 0.5618(5) 0.48704(18) 0.78865(12) 0.0697(11) Uani 1 1 d . . . F50 F 0.5992(4) 0.54529(14) 0.72371(11) 0.0483(8) Uani 1 1 d . . . F51 F 0.8052(4) 0.51346(19) 0.76822(14) 0.0674(11) Uani 1 1 d . . . C52 C 1.1752(6) 0.2403(2) 0.6640(2) 0.0364(12) Uani 1 1 d . . . F53 F 1.3146(4) 0.27246(16) 0.67044(14) 0.0571(9) Uani 1 1 d . . . F54 F 1.0647(4) 0.26849(16) 0.69235(13) 0.0581(10) Uani 1 1 d . . . F55 F 1.1229(4) 0.24697(15) 0.61723(12) 0.0536(9) Uani 1 1 d . . . S56 S 1.19573(14) 0.15351(6) 0.68031(4) 0.0270(3) Uani 1 1 d . . . O57 O 1.2696(4) 0.15405(19) 0.72938(13) 0.0440(9) Uani 1 1 d . . . O58 O 1.0359(4) 0.12734(16) 0.67306(13) 0.0339(8) Uani 1 1 d . . . N59 N 1.3277(4) 0.13102(19) 0.64224(15) 0.0293(9) Uani 1 1 d . . . S60 S 1.29021(14) 0.08958(5) 0.59390(4) 0.0261(2) Uani 1 1 d . . . O61 O 1.4178(4) 0.09997(18) 0.56031(13) 0.0420(9) Uani 1 1 d . . . O62 O 1.1256(4) 0.08878(17) 0.57455(13) 0.0385(9) Uani 1 1 d . . . C63 C 1.3262(6) 0.0052(2) 0.61602(19) 0.0317(11) Uani 1 1 d . . . F64 F 1.2223(4) -0.01010(15) 0.65080(12) 0.0477(8) Uani 1 1 d . . . F65 F 1.4769(3) -0.00142(15) 0.63494(12) 0.0453(8) Uani 1 1 d . . . F66 F 1.3039(4) -0.03669(15) 0.57877(13) 0.0559(9) Uani 1 1 d . . . 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 Ni1 0.0130(2) 0.0149(2) 0.0119(2) 0.0000(2) -0.0001(2) -0.0002(2) N1 0.0193(18) 0.0208(19) 0.0146(18) -0.0010(15) -0.0008(15) 0.0030(15) C2 0.021(2) 0.029(2) 0.018(2) 0.0010(19) -0.0028(19) 0.004(2) N3 0.027(2) 0.033(2) 0.0173(19) 0.0003(17) 0.0040(17) 0.0099(17) C4 0.032(3) 0.041(3) 0.023(3) 0.002(2) 0.013(2) 0.006(2) C5 0.024(2) 0.029(2) 0.028(3) 0.001(2) 0.004(2) -0.003(2) C6 0.053(3) 0.032(3) 0.036(3) -0.010(2) 0.007(3) 0.015(3) N7 0.0188(17) 0.0208(18) 0.0134(18) 0.0019(15) 0.0011(15) -0.0002(15) C8 0.023(2) 0.030(2) 0.022(2) 0.000(2) 0.002(2) 0.004(2) N9 0.0172(18) 0.033(2) 0.0132(18) 0.0045(15) -0.0028(15) 0.0013(16) C10 0.018(2) 0.038(3) 0.025(3) 0.004(2) -0.0014(19) 0.010(2) C11 0.018(2) 0.035(3) 0.021(2) -0.005(2) 0.0009(18) 0.010(2) C12 0.029(2) 0.059(3) 0.017(2) 0.003(2) -0.004(2) 0.007(3) N13 0.0159(17) 0.0198(18) 0.0181(19) -0.0033(15) 0.0029(15) -0.0009(14) C14 0.023(2) 0.025(2) 0.022(2) -0.0039(19) -0.0021(19) -0.004(2) N15 0.028(2) 0.023(2) 0.031(2) -0.0080(17) 0.0064(18) -0.0103(17) C16 0.020(2) 0.041(3) 0.037(3) -0.007(2) -0.006(2) -0.015(2) C17 0.019(2) 0.036(3) 0.024(2) 0.001(2) -0.0049(19) -0.005(2) C18 0.054(3) 0.030(3) 0.048(3) 0.001(3) 0.005(3) -0.017(3) N19 0.0141(16) 0.0211(18) 0.0142(17) -0.0023(15) -0.0014(14) 0.0026(14) C20 0.017(2) 0.023(2) 0.018(2) -0.0020(18) 0.0041(17) 0.0025(18) N21 0.0203(19) 0.0205(19) 0.0210(19) -0.0056(15) 0.0017(16) 0.0032(15) C22 0.024(2) 0.035(3) 0.019(2) -0.003(2) 0.0073(19) -0.003(2) C23 0.018(2) 0.025(2) 0.024(2) -0.0001(19) 0.0031(19) -0.0041(19) C24 0.031(3) 0.035(3) 0.029(3) -0.018(2) 0.011(2) -0.003(2) N25 0.0158(17) 0.0181(18) 0.0174(19) 0.0025(15) 0.0007(15) -0.0019(15) C26 0.020(2) 0.023(2) 0.018(2) 0.0044(18) -0.0014(18) -0.0013(18) N27 0.0251(19) 0.024(2) 0.0198(19) 0.0087(16) -0.0065(16) -0.0026(17) C28 0.020(2) 0.035(3) 0.034(3) 0.013(2) -0.008(2) -0.001(2) C29 0.022(2) 0.020(2) 0.027(2) 0.0009(19) -0.0028(19) 0.0026(19) C30 0.046(3) 0.042(3) 0.017(2) 0.003(2) -0.009(2) -0.008(2) N31 0.0175(17) 0.0161(17) 0.0173(18) 0.0047(15) 0.0009(15) 0.0009(15) C32 0.021(2) 0.020(2) 0.021(2) 0.0023(18) 0.0009(18) -0.0013(19) N33 0.0213(18) 0.0219(19) 0.0226(19) 0.0070(16) 0.0032(16) 0.0018(16) C34 0.018(2) 0.020(2) 0.026(2) 0.0009(19) 0.0017(19) -0.0021(18) C35 0.022(2) 0.019(2) 0.015(2) -0.0042(17) -0.0016(17) 0.0006(18) C36 0.038(3) 0.029(3) 0.041(3) 0.019(2) 0.000(2) -0.008(2) C37 0.037(3) 0.039(3) 0.037(3) -0.006(2) 0.015(2) -0.007(2) F38 0.056(2) 0.058(2) 0.084(3) -0.019(2) 0.026(2) 0.0150(18) F39 0.062(2) 0.0439(19) 0.071(2) -0.0244(17) 0.0278(19) -0.0326(17) F40 0.088(3) 0.082(3) 0.033(2) -0.0219(18) 0.0004(18) -0.019(2) S41 0.0250(6) 0.0270(6) 0.0209(6) 0.0011(5) 0.0022(5) -0.0073(5) O42 0.0388(19) 0.053(2) 0.031(2) 0.0028(17) 0.0069(17) -0.0252(18) O43 0.0378(19) 0.0356(19) 0.0291(19) 0.0040(15) -0.0034(15) 0.0087(16) N44 0.0175(19) 0.042(2) 0.025(2) 0.0028(18) 0.0018(16) -0.0017(17) S45 0.0255(6) 0.0302(6) 0.0245(6) 0.0063(5) 0.0059(5) 0.0024(5) O46 0.0263(18) 0.050(2) 0.039(2) 0.0070(17) 0.0097(15) -0.0088(16) O47 0.052(2) 0.039(2) 0.0309(19) 0.0116(16) 0.0028(17) 0.0148(18) C48 0.044(3) 0.047(3) 0.024(3) 0.001(2) 0.000(2) 0.011(3) F49 0.106(3) 0.067(2) 0.039(2) 0.0007(17) 0.033(2) 0.023(2) F50 0.067(2) 0.0390(17) 0.0384(18) 0.0036(14) -0.0075(16) 0.0177(17) F51 0.064(2) 0.074(3) 0.061(2) -0.028(2) -0.028(2) 0.010(2) C52 0.036(3) 0.028(3) 0.045(3) -0.001(2) 0.000(2) -0.003(2) F53 0.0517(19) 0.0425(19) 0.077(3) -0.0088(18) 0.0035(18) -0.0180(17) F54 0.059(2) 0.0451(19) 0.071(2) -0.0110(17) 0.0194(19) 0.0077(17) F55 0.063(2) 0.048(2) 0.050(2) 0.0193(16) -0.0024(16) 0.0078(18) S56 0.0242(6) 0.0308(6) 0.0255(6) 0.0033(5) -0.0038(5) -0.0007(5) O57 0.040(2) 0.063(3) 0.0278(19) 0.0009(18) -0.0128(16) 0.0040(19) O58 0.0256(17) 0.0360(19) 0.040(2) 0.0093(16) 0.0002(15) -0.0063(15) N59 0.021(2) 0.033(2) 0.033(2) -0.0056(18) -0.0066(17) -0.0010(17) S60 0.0280(6) 0.0233(6) 0.0268(6) 0.0023(5) -0.0044(5) -0.0019(5) O61 0.051(2) 0.044(2) 0.032(2) 0.0032(16) 0.0114(18) -0.0132(18) O62 0.0350(19) 0.042(2) 0.038(2) -0.0012(17) -0.0122(16) 0.0052(17) C63 0.033(3) 0.026(3) 0.036(3) 0.007(2) -0.006(2) -0.001(2) F64 0.0467(18) 0.0421(18) 0.055(2) 0.0216(16) 0.0065(16) -0.0102(15) F65 0.0337(16) 0.0451(18) 0.057(2) 0.0121(15) -0.0061(15) 0.0111(14) F66 0.077(2) 0.0290(17) 0.061(2) -0.0140(16) -0.0093(18) 0.0019(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N31 2.104(3) . ? Ni1 N19 2.112(3) . ? Ni1 N1 2.118(3) . ? Ni1 N13 2.124(3) . ? Ni1 N25 2.125(3) . ? Ni1 N7 2.138(3) . ? N1 C2 1.322(5) . ? N1 C5 1.373(5) . ? C2 N3 1.343(5) . ? N3 C4 1.359(6) . ? N3 C6 1.461(6) . ? C4 C5 1.348(7) . ? N7 C8 1.325(5) . ? N7 C11 1.377(5) . ? C8 N9 1.334(5) . ? N9 C10 1.364(5) . ? N9 C12 1.463(6) . ? C10 C11 1.351(6) . ? N13 C14 1.325(6) . ? N13 C17 1.373(5) . ? C14 N15 1.339(5) . ? N15 C16 1.366(6) . ? N15 C18 1.466(6) . ? C16 C17 1.352(6) . ? N19 C20 1.329(5) . ? N19 C23 1.372(5) . ? C20 N21 1.339(5) . ? N21 C22 1.362(5) . ? N21 C24 1.453(5) . ? C22 C23 1.362(6) . ? N25 C26 1.331(5) . ? N25 C29 1.375(5) . ? C26 N27 1.337(5) . ? N27 C28 1.358(6) . ? N27 C30 1.469(6) . ? C28 C29 1.369(6) . ? N31 C32 1.318(5) . ? N31 C35 1.385(5) . ? C32 N33 1.341(5) . ? N33 C34 1.369(5) . ? N33 C36 1.467(5) . ? C34 C35 1.348(6) . ? C37 F39 1.315(5) . ? C37 F40 1.323(6) . ? C37 F38 1.330(6) . ? C37 S41 1.836(5) . ? S41 O42 1.425(3) . ? S41 O43 1.431(3) . ? S41 N44 1.577(4) . ? N44 S45 1.574(4) . ? S45 O47 1.429(3) . ? S45 O46 1.430(3) . ? S45 C48 1.835(5) . ? C48 F50 1.318(6) . ? C48 F51 1.318(6) . ? C48 F49 1.331(6) . ? C52 F55 1.321(6) . ? C52 F53 1.322(6) . ? C52 F54 1.337(6) . ? C52 S56 1.824(5) . ? S56 O58 1.421(3) . ? S56 O57 1.431(3) . ? S56 N59 1.588(4) . ? N59 S60 1.571(4) . ? S60 O61 1.427(3) . ? S60 O62 1.428(3) . ? S60 C63 1.835(5) . ? C63 F66 1.323(6) . ? C63 F65 1.324(5) . ? C63 F64 1.329(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Ni1 N19 89.05(13) . . ? N31 Ni1 N1 90.57(13) . . ? N19 Ni1 N1 178.42(13) . . ? N31 Ni1 N13 178.49(13) . . ? N19 Ni1 N13 89.61(13) . . ? N1 Ni1 N13 90.79(13) . . ? N31 Ni1 N25 89.16(13) . . ? N19 Ni1 N25 91.28(13) . . ? N1 Ni1 N25 90.24(13) . . ? N13 Ni1 N25 90.20(13) . . ? N31 Ni1 N7 91.00(13) . . ? N19 Ni1 N7 89.28(12) . . ? N1 Ni1 N7 89.20(13) . . ? N13 Ni1 N7 89.65(13) . . ? N25 Ni1 N7 179.42(13) . . ? C2 N1 C5 104.8(4) . . ? C2 N1 Ni1 126.7(3) . . ? C5 N1 Ni1 128.5(3) . . ? N1 C2 N3 111.7(4) . . ? C2 N3 C4 106.9(4) . . ? C2 N3 C6 126.5(4) . . ? C4 N3 C6 126.5(4) . . ? C5 C4 N3 106.6(4) . . ? C4 C5 N1 110.0(4) . . ? C8 N7 C11 104.3(4) . . ? C8 N7 Ni1 128.0(3) . . ? C11 N7 Ni1 127.1(3) . . ? N7 C8 N9 111.9(4) . . ? C8 N9 C10 107.6(4) . . ? C8 N9 C12 125.9(4) . . ? C10 N9 C12 126.5(4) . . ? C11 C10 N9 105.8(4) . . ? C10 C11 N7 110.4(4) . . ? C14 N13 C17 105.4(4) . . ? C14 N13 Ni1 126.6(3) . . ? C17 N13 Ni1 127.8(3) . . ? N13 C14 N15 111.9(4) . . ? C14 N15 C16 106.3(4) . . ? C14 N15 C18 126.4(4) . . ? C16 N15 C18 127.3(4) . . ? C17 C16 N15 107.4(4) . . ? C16 C17 N13 109.0(4) . . ? C20 N19 C23 104.7(3) . . ? C20 N19 Ni1 126.1(3) . . ? C23 N19 Ni1 128.7(3) . . ? N19 C20 N21 112.0(4) . . ? C20 N21 C22 107.1(3) . . ? C20 N21 C24 126.4(4) . . ? C22 N21 C24 126.5(4) . . ? C23 C22 N21 106.3(4) . . ? C22 C23 N19 109.9(4) . . ? C26 N25 C29 105.1(4) . . ? C26 N25 Ni1 127.6(3) . . ? C29 N25 Ni1 127.3(3) . . ? N25 C26 N27 111.6(4) . . ? C26 N27 C28 107.6(4) . . ? C26 N27 C30 126.4(4) . . ? C28 N27 C30 126.0(4) . . ? N27 C28 C29 106.3(4) . . ? C28 C29 N25 109.4(4) . . ? C32 N31 C35 104.7(3) . . ? C32 N31 Ni1 125.8(3) . . ? C35 N31 Ni1 129.1(3) . . ? N31 C32 N33 111.9(4) . . ? C32 N33 C34 107.2(3) . . ? C32 N33 C36 125.6(4) . . ? C34 N33 C36 127.1(4) . . ? C35 C34 N33 106.2(4) . . ? C34 C35 N31 110.0(4) . . ? F39 C37 F40 108.1(4) . . ? F39 C37 F38 108.2(5) . . ? F40 C37 F38 107.7(4) . . ? F39 C37 S41 112.3(3) . . ? F40 C37 S41 109.2(4) . . ? F38 C37 S41 111.2(4) . . ? O42 S41 O43 118.5(2) . . ? O42 S41 N44 108.4(2) . . ? O43 S41 N44 117.4(2) . . ? O42 S41 C37 103.1(2) . . ? O43 S41 C37 103.6(2) . . ? N44 S41 C37 103.4(2) . . ? S45 N44 S41 124.1(2) . . ? O47 S45 O46 118.7(2) . . ? O47 S45 N44 108.2(2) . . ? O46 S45 N44 116.2(2) . . ? O47 S45 C48 104.1(2) . . ? O46 S45 C48 104.7(2) . . ? N44 S45 C48 102.8(2) . . ? F50 C48 F51 108.0(5) . . ? F50 C48 F49 108.1(4) . . ? F51 C48 F49 109.2(4) . . ? F50 C48 S45 111.4(3) . . ? F51 C48 S45 111.4(4) . . ? F49 C48 S45 108.7(4) . . ? F55 C52 F53 108.7(4) . . ? F55 C52 F54 107.5(4) . . ? F53 C52 F54 108.4(4) . . ? F55 C52 S56 110.6(3) . . ? F53 C52 S56 112.0(4) . . ? F54 C52 S56 109.5(4) . . ? O58 S56 O57 118.9(2) . . ? O58 S56 N59 116.9(2) . . ? O57 S56 N59 108.9(2) . . ? O58 S56 C52 104.7(2) . . ? O57 S56 C52 104.3(2) . . ? N59 S56 C52 100.4(2) . . ? S60 N59 S56 125.1(2) . . ? O61 S60 O62 118.5(2) . . ? O61 S60 N59 108.8(2) . . ? O62 S60 N59 117.3(2) . . ? O61 S60 C63 103.4(2) . . ? O62 S60 C63 104.2(2) . . ? N59 S60 C63 102.0(2) . . ? F66 C63 F65 108.9(4) . . ? F66 C63 F64 108.1(4) . . ? F65 C63 F64 108.7(4) . . ? F66 C63 S60 109.8(3) . . ? F65 C63 S60 110.8(3) . . ? F64 C63 S60 110.4(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.445 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.085 # Attachment 'wg299n-[Cu-MeIm-6][Tf2N-]2.cif' data_wg299n _database_code_depnum_ccdc_archive 'CCDC 883554' #TrackingRef 'wg299n-[Cu-MeIm-6][Tf2N-]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis(N-methylimidazole)copper(II) bis(trifluoromethyl)sulfonylimide ; _chemical_name_common ; hexakis(N-methylimidazole)copper(II) bistriflimide ; _chemical_melting_point 325 _chemical_formula_moiety 'C24 H36 Cu N12, 2(C2 F6 N O4 S2)' _chemical_formula_sum 'C28 H36 Cu F12 N14 O8 S4' _chemical_formula_weight 1116.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2933(3) _cell_length_b 11.1971(3) _cell_length_c 24.1682(7) _cell_angle_alpha 91.145(1) _cell_angle_beta 93.419(1) _cell_angle_gamma 92.945(2) _cell_volume 2236.73(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6756 _cell_measurement_theta_min 4.321 _cell_measurement_theta_max 71.241 _exptl_crystal_description needle _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1134 _exptl_absorpt_coefficient_mu 3.462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.338 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'crossed G\"obel mirrors' _diffrn_measurement_device_type 'SMART 6000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38817 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 66.59 _reflns_number_total 7871 _reflns_number_gt 7131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAINT' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ; A.L.Spek (2010) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+1.3571P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7871 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.0000 1.0000 1.0000 0.01499(11) Uani 1 2 d S . . Cu2 Cu 0.5000 0.5000 0.5000 0.01506(11) Uani 1 2 d S . . C1 C 0.3536(3) 0.2098(2) 0.24482(10) 0.0326(5) Uani 1 1 d . . . F2 F 0.4613(2) 0.23207(17) 0.20725(7) 0.0555(5) Uani 1 1 d . . . F3 F 0.2134(2) 0.25009(15) 0.22665(8) 0.0534(5) Uani 1 1 d . . . F4 F 0.4020(2) 0.26860(13) 0.29144(6) 0.0421(4) Uani 1 1 d . . . S5 S 0.33584(6) 0.04782(5) 0.25495(2) 0.02318(13) Uani 1 1 d . . . O6 O 0.4970(2) 0.01591(17) 0.26914(7) 0.0325(4) Uani 1 1 d . . . O7 O 0.2569(2) 0.00207(17) 0.20399(7) 0.0360(4) Uani 1 1 d . . . N8 N 0.2128(2) 0.03476(18) 0.30217(7) 0.0241(4) Uani 1 1 d . . . S9 S 0.26515(6) 0.02755(5) 0.36568(2) 0.02138(12) Uani 1 1 d . . . O10 O 0.4176(2) 0.08440(15) 0.38389(7) 0.0319(4) Uani 1 1 d . . . O11 O 0.1273(2) 0.04857(17) 0.39655(7) 0.0367(4) Uani 1 1 d . . . C12 C 0.2931(3) -0.1324(2) 0.37569(10) 0.0272(5) Uani 1 1 d . . . F13 F 0.4142(2) -0.16990(13) 0.34861(8) 0.0455(4) Uani 1 1 d . . . F14 F 0.3251(2) -0.14973(15) 0.42935(7) 0.0490(4) Uani 1 1 d . . . F15 F 0.1610(2) -0.19819(14) 0.35947(8) 0.0455(4) Uani 1 1 d . . . C16 C 0.7446(3) 0.7085(2) 0.25358(10) 0.0332(5) Uani 1 1 d . . . F17 F 0.7036(2) 0.76378(14) 0.20734(7) 0.0439(4) Uani 1 1 d . . . F18 F 0.6367(2) 0.73080(18) 0.29052(7) 0.0575(5) Uani 1 1 d . . . F19 F 0.8884(2) 0.75221(17) 0.27312(8) 0.0552(5) Uani 1 1 d . . . S20 S 0.74542(6) 0.54685(5) 0.24088(2) 0.02471(13) Uani 1 1 d . . . O22 O 0.5814(2) 0.51123(16) 0.22442(7) 0.0333(4) Uani 1 1 d . . . O23 O 0.8147(2) 0.50265(19) 0.29145(7) 0.0419(5) Uani 1 1 d . . . N23 N 0.8720(2) 0.54059(18) 0.19504(8) 0.0262(4) Uani 1 1 d . . . S24 S 0.82804(6) 0.52394(4) 0.13099(2) 0.02060(12) Uani 1 1 d . . . O25 O 0.9563(2) 0.57639(16) 0.10124(7) 0.0339(4) Uani 1 1 d . . . O26 O 0.6649(2) 0.54378(16) 0.11206(7) 0.0311(4) Uani 1 1 d . . . C27 C 0.8478(3) 0.3629(2) 0.12082(10) 0.0275(5) Uani 1 1 d . . . F28 F 0.99498(17) 0.33184(13) 0.13652(6) 0.0359(3) Uani 1 1 d . . . F29 F 0.8190(2) 0.33397(15) 0.06762(7) 0.0482(4) Uani 1 1 d . . . F30 F 0.74133(19) 0.30189(13) 0.14956(8) 0.0448(4) Uani 1 1 d . . . N31 N 0.8201(2) 1.13975(15) 0.95313(7) 0.0188(3) Uani 1 1 d . . . C32 C 0.8376(3) 1.18347(19) 0.90350(8) 0.0208(4) Uani 1 1 d . . . H32 H 0.9280 1.1707 0.8821 0.025 Uiso 1 1 calc R . . N33 N 0.7120(2) 1.24865(16) 0.88656(7) 0.0216(4) Uani 1 1 d . . . C34 C 0.6067(3) 1.24611(19) 0.92790(9) 0.0237(4) Uani 1 1 d . . . H34 H 0.5064 1.2834 0.9281 0.028 Uiso 1 1 calc R . . C35 C 0.6743(3) 1.17952(19) 0.96869(9) 0.0212(4) Uani 1 1 d . . . H35 H 0.6279 1.1628 1.0029 0.025 Uiso 1 1 calc R . . C36 C 0.6943(3) 1.3085(2) 0.83361(10) 0.0346(6) Uani 1 1 d . . . H36A H 0.7966 1.3513 0.8263 0.052 Uiso 1 1 calc R . . H36B H 0.6088 1.3656 0.8351 0.052 Uiso 1 1 calc R . . H36C H 0.6657 1.2490 0.8039 0.052 Uiso 1 1 calc R . . N37 N 1.1233(2) 0.98990(15) 0.93024(7) 0.0160(3) Uani 1 1 d . . . C38 C 1.0639(2) 0.95457(18) 0.88034(8) 0.0174(4) Uani 1 1 d . . . H38 H 0.9560 0.9239 0.8723 0.021 Uiso 1 1 calc R . . N39 N 1.1749(2) 0.96733(16) 0.84258(7) 0.0189(3) Uani 1 1 d . . . C40 C 1.3156(3) 1.0125(2) 0.86967(9) 0.0218(4) Uani 1 1 d . . . H40 H 1.4160 1.0300 0.8539 0.026 Uiso 1 1 calc R . . C41 C 1.2824(2) 1.02697(19) 0.92370(8) 0.0209(4) Uani 1 1 d . . . H41 H 1.3570 1.0578 0.9525 0.025 Uiso 1 1 calc R . . C42 C 1.1496(3) 0.9381(2) 0.78317(9) 0.0282(5) Uani 1 1 d . . . H42A H 1.1331 0.8513 0.7778 0.042 Uiso 1 1 calc R . . H42B H 1.2447 0.9665 0.7640 0.042 Uiso 1 1 calc R . . H42C H 1.0540 0.9772 0.7680 0.042 Uiso 1 1 calc R . . N43 N 0.8452(2) 0.86062(15) 0.97157(7) 0.0167(3) Uani 1 1 d . . . C44 C 0.8551(2) 0.74789(19) 0.98572(8) 0.0187(4) Uani 1 1 d . . . H44 H 0.9354 0.7199 1.0112 0.022 Uiso 1 1 calc R . . N45 N 0.7371(2) 0.67763(16) 0.95948(7) 0.0204(4) Uani 1 1 d . . . C46 C 0.6464(3) 0.7494(2) 0.92634(8) 0.0227(4) Uani 1 1 d . . . H46 H 0.5547 0.7251 0.9026 0.027 Uiso 1 1 calc R . . C47 C 0.7129(2) 0.86203(19) 0.93401(8) 0.0208(4) Uani 1 1 d . . . H47 H 0.6746 0.9311 0.9164 0.025 Uiso 1 1 calc R . . C48 C 0.7146(3) 0.5475(2) 0.96342(10) 0.0296(5) Uani 1 1 d . . . H48A H 0.7975 0.5089 0.9432 0.044 Uiso 1 1 calc R . . H48B H 0.6071 0.5212 0.9472 0.044 Uiso 1 1 calc R . . H48C H 0.7240 0.5253 1.0024 0.044 Uiso 1 1 calc R . . N49 N 0.3631(2) 0.36149(15) 0.52992(7) 0.0176(3) Uani 1 1 d . . . C50 C 0.3685(3) 0.24782(19) 0.51491(8) 0.0208(4) Uani 1 1 d . . . H50 H 0.4363 0.2189 0.4879 0.025 Uiso 1 1 calc R . . N51 N 0.2661(2) 0.17821(17) 0.54272(7) 0.0242(4) Uani 1 1 d . . . C52 C 0.1894(3) 0.2514(2) 0.57749(9) 0.0272(5) Uani 1 1 d . . . H52 H 0.1101 0.2278 0.6025 0.033 Uiso 1 1 calc R . . C53 C 0.2491(3) 0.3641(2) 0.56919(9) 0.0240(4) Uani 1 1 d . . . H53 H 0.2173 0.4342 0.5876 0.029 Uiso 1 1 calc R . . C54 C 0.2461(3) 0.0475(2) 0.53881(11) 0.0365(6) Uani 1 1 d . . . H54A H 0.2614 0.0205 0.5007 0.055 Uiso 1 1 calc R . . H54B H 0.1371 0.0220 0.5489 0.055 Uiso 1 1 calc R . . H54C H 0.3263 0.0125 0.5642 0.055 Uiso 1 1 calc R . . N55 N 0.6501(2) 0.50321(15) 0.57019(7) 0.0168(3) Uani 1 1 d . . . C56 C 0.6223(2) 0.46299(18) 0.62010(8) 0.0186(4) Uani 1 1 d . . . H56 H 0.5226 0.4257 0.6297 0.022 Uiso 1 1 calc R . . N57 N 0.7525(2) 0.48158(16) 0.65536(7) 0.0190(3) Uani 1 1 d . . . C58 C 0.8725(3) 0.5360(2) 0.62644(9) 0.0243(4) Uani 1 1 d . . . H58 H 0.9792 0.5598 0.6402 0.029 Uiso 1 1 calc R . . C59 C 0.8075(3) 0.5488(2) 0.57423(9) 0.0232(4) Uani 1 1 d . . . H59 H 0.8627 0.5840 0.5448 0.028 Uiso 1 1 calc R . . C60 C 0.7663(3) 0.4489(2) 0.71360(9) 0.0266(5) Uani 1 1 d . . . H60A H 0.6580 0.4340 0.7270 0.040 Uiso 1 1 calc R . . H60B H 0.8232 0.5143 0.7356 0.040 Uiso 1 1 calc R . . H60C H 0.8270 0.3763 0.7173 0.040 Uiso 1 1 calc R . . N61 N 0.3286(2) 0.64007(15) 0.54241(7) 0.0197(4) Uani 1 1 d . . . C62 C 0.3423(3) 0.68187(19) 0.59401(9) 0.0221(4) Uani 1 1 d . . . H62 H 0.4293 0.6657 0.6197 0.026 Uiso 1 1 calc R . . N63 N 0.2201(2) 0.74963(15) 0.60626(7) 0.0196(4) Uani 1 1 d . . . C64 C 0.1202(2) 0.75304(18) 0.55888(9) 0.0200(4) Uani 1 1 d . . . H64 H 0.0233 0.7944 0.5542 0.024 Uiso 1 1 calc R . . C65 C 0.1879(3) 0.68554(18) 0.52031(8) 0.0195(4) Uani 1 1 d . . . H65 H 0.1448 0.6715 0.4833 0.023 Uiso 1 1 calc R . . C66 C 0.1990(3) 0.8086(2) 0.65963(9) 0.0295(5) Uani 1 1 d . . . H66A H 0.2103 0.7506 0.6893 0.044 Uiso 1 1 calc R . . H66B H 0.0912 0.8407 0.6593 0.044 Uiso 1 1 calc R . . H66C H 0.2814 0.8741 0.6661 0.044 Uiso 1 1 calc R . . 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 0.0154(2) 0.0174(2) 0.01174(19) 0.00011(14) 0.00068(14) -0.00250(16) Cu2 0.0144(2) 0.0178(2) 0.01253(19) 0.00227(15) -0.00156(14) -0.00143(16) C1 0.0394(13) 0.0332(12) 0.0233(11) 0.0087(9) -0.0077(10) -0.0080(11) F2 0.0684(12) 0.0579(11) 0.0385(9) 0.0149(8) 0.0086(8) -0.0237(9) F3 0.0583(11) 0.0394(9) 0.0598(11) 0.0169(8) -0.0258(9) 0.0035(8) F4 0.0612(10) 0.0298(7) 0.0323(8) 0.0017(6) -0.0145(7) -0.0069(7) S5 0.0226(3) 0.0297(3) 0.0168(2) 0.00064(19) 0.00055(19) -0.0018(2) O6 0.0233(8) 0.0449(10) 0.0304(8) 0.0033(7) 0.0078(6) 0.0039(7) O7 0.0439(10) 0.0431(10) 0.0195(8) -0.0038(7) -0.0017(7) -0.0074(8) N8 0.0184(8) 0.0335(10) 0.0205(9) 0.0041(7) -0.0008(7) 0.0028(8) S9 0.0240(3) 0.0237(3) 0.0173(2) 0.00235(18) 0.00237(19) 0.0079(2) O10 0.0379(9) 0.0324(9) 0.0238(8) 0.0011(6) -0.0067(7) -0.0021(7) O11 0.0406(10) 0.0426(10) 0.0305(9) 0.0062(7) 0.0139(7) 0.0212(8) C12 0.0277(11) 0.0247(11) 0.0309(12) 0.0078(9) 0.0089(9) 0.0064(9) F13 0.0437(9) 0.0294(7) 0.0686(11) 0.0122(7) 0.0307(8) 0.0171(7) F14 0.0644(11) 0.0467(9) 0.0385(8) 0.0238(7) 0.0057(8) 0.0158(8) F15 0.0395(8) 0.0322(8) 0.0648(11) 0.0009(7) 0.0111(8) -0.0061(7) C16 0.0342(13) 0.0374(13) 0.0286(12) -0.0073(10) -0.0013(10) 0.0141(11) F17 0.0561(10) 0.0307(7) 0.0450(9) 0.0058(6) -0.0043(7) 0.0091(7) F18 0.0607(11) 0.0682(12) 0.0468(10) -0.0146(8) 0.0143(8) 0.0291(10) F19 0.0493(10) 0.0527(10) 0.0604(11) -0.0250(9) -0.0132(8) 0.0015(8) S20 0.0219(3) 0.0332(3) 0.0199(2) 0.0060(2) -0.00042(19) 0.0096(2) O22 0.0240(8) 0.0407(10) 0.0360(9) 0.0102(7) 0.0037(7) 0.0046(7) O23 0.0391(10) 0.0622(13) 0.0263(9) 0.0151(8) -0.0016(7) 0.0201(9) N23 0.0191(9) 0.0355(10) 0.0239(9) -0.0035(8) -0.0030(7) 0.0054(8) S24 0.0213(3) 0.0210(2) 0.0194(2) 0.00092(18) -0.00141(18) 0.0038(2) O25 0.0389(10) 0.0312(9) 0.0322(9) 0.0064(7) 0.0082(7) -0.0025(8) O26 0.0294(9) 0.0377(9) 0.0262(8) 0.0008(7) -0.0081(6) 0.0119(7) C27 0.0269(11) 0.0232(11) 0.0321(12) -0.0019(9) -0.0032(9) 0.0042(9) F28 0.0297(7) 0.0318(7) 0.0465(8) -0.0019(6) -0.0043(6) 0.0130(6) F29 0.0574(10) 0.0439(9) 0.0414(9) -0.0220(7) -0.0136(7) 0.0124(8) F30 0.0381(8) 0.0257(7) 0.0708(11) 0.0089(7) 0.0061(8) -0.0047(6) N31 0.0189(8) 0.0188(8) 0.0181(8) 0.0030(6) -0.0036(6) -0.0012(7) C32 0.0212(10) 0.0215(10) 0.0195(10) 0.0032(8) -0.0027(8) 0.0025(8) N33 0.0225(9) 0.0182(8) 0.0232(9) 0.0056(7) -0.0077(7) 0.0007(7) C34 0.0178(10) 0.0197(10) 0.0333(12) 0.0018(9) -0.0045(8) 0.0045(8) C35 0.0196(10) 0.0198(10) 0.0239(10) -0.0001(8) 0.0007(8) -0.0009(8) C36 0.0374(13) 0.0360(13) 0.0292(12) 0.0152(10) -0.0126(10) 0.0010(11) N37 0.0164(8) 0.0170(8) 0.0147(8) 0.0015(6) 0.0009(6) 0.0008(6) C38 0.0155(9) 0.0194(9) 0.0173(9) 0.0021(7) 0.0007(7) 0.0014(8) N39 0.0192(8) 0.0232(9) 0.0146(8) 0.0008(6) 0.0012(6) 0.0019(7) C40 0.0163(9) 0.0287(11) 0.0202(10) 0.0028(8) 0.0018(8) -0.0018(8) C41 0.0169(10) 0.0277(11) 0.0177(10) 0.0030(8) -0.0011(7) -0.0020(8) C42 0.0278(11) 0.0420(13) 0.0143(10) -0.0039(9) 0.0023(8) -0.0028(10) N43 0.0158(8) 0.0203(8) 0.0138(7) 0.0007(6) 0.0010(6) -0.0011(7) C44 0.0186(9) 0.0214(10) 0.0157(9) 0.0006(8) -0.0001(7) -0.0014(8) N45 0.0223(9) 0.0207(9) 0.0177(8) 0.0002(7) 0.0007(7) -0.0037(7) C46 0.0181(10) 0.0300(11) 0.0191(10) -0.0009(8) -0.0027(8) -0.0034(9) C47 0.0181(10) 0.0245(11) 0.0194(10) 0.0026(8) -0.0023(8) 0.0008(8) C48 0.0363(13) 0.0193(11) 0.0322(12) -0.0003(9) 0.0002(10) -0.0067(10) N49 0.0159(8) 0.0214(8) 0.0149(8) 0.0031(6) -0.0023(6) -0.0009(7) C50 0.0208(10) 0.0225(10) 0.0188(9) 0.0026(8) 0.0001(8) -0.0007(8) N51 0.0270(9) 0.0226(9) 0.0219(9) 0.0055(7) -0.0033(7) -0.0059(8) C52 0.0230(11) 0.0359(13) 0.0226(10) 0.0074(9) 0.0027(8) -0.0049(10) C53 0.0201(10) 0.0301(11) 0.0219(10) 0.0016(8) 0.0030(8) -0.0007(9) C54 0.0469(15) 0.0223(12) 0.0388(13) 0.0094(10) -0.0011(11) -0.0102(11) N55 0.0170(8) 0.0182(8) 0.0150(8) 0.0015(6) -0.0017(6) 0.0014(7) C56 0.0179(9) 0.0211(10) 0.0170(9) 0.0027(8) 0.0003(7) 0.0019(8) N57 0.0187(8) 0.0239(9) 0.0145(8) 0.0019(7) -0.0010(6) 0.0048(7) C58 0.0186(10) 0.0325(12) 0.0208(10) 0.0022(9) -0.0035(8) -0.0032(9) C59 0.0189(10) 0.0298(11) 0.0203(10) 0.0045(8) -0.0010(8) -0.0039(9) C60 0.0267(11) 0.0386(13) 0.0148(10) 0.0059(9) -0.0017(8) 0.0072(10) N61 0.0189(8) 0.0204(8) 0.0196(8) -0.0011(7) 0.0008(7) 0.0014(7) C62 0.0207(10) 0.0247(10) 0.0203(10) -0.0028(8) -0.0020(8) 0.0024(9) N63 0.0205(9) 0.0194(8) 0.0188(8) -0.0029(7) 0.0024(7) 0.0004(7) C64 0.0162(9) 0.0194(10) 0.0244(10) 0.0009(8) 0.0003(8) 0.0019(8) C65 0.0207(10) 0.0198(10) 0.0178(9) 0.0027(8) -0.0012(8) -0.0002(8) C66 0.0325(12) 0.0331(12) 0.0232(11) -0.0100(9) 0.0024(9) 0.0069(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N37 2.0276(16) . ? Cu1 N37 2.0276(16) 2_777 ? Cu1 N43 2.0496(17) 2_777 ? Cu1 N43 2.0496(17) . ? Cu1 N31 2.4633(17) 2_777 ? Cu1 N31 2.4633(17) . ? Cu2 N55 2.0419(16) 2_666 ? Cu2 N55 2.0419(16) . ? Cu2 N49 2.0443(17) . ? Cu2 N49 2.0443(17) 2_666 ? Cu2 N61 2.4229(17) . ? Cu2 N61 2.4229(17) 2_666 ? C1 F3 1.323(3) . ? C1 F4 1.324(3) . ? C1 F2 1.330(3) . ? C1 S5 1.834(3) . ? S5 O6 1.4254(18) . ? S5 O7 1.4325(17) . ? S5 N8 1.5795(18) . ? N8 S9 1.5749(18) . ? S9 O10 1.4274(18) . ? S9 O11 1.4287(18) . ? S9 C12 1.836(2) . ? C12 F13 1.313(3) . ? C12 F15 1.324(3) . ? C12 F14 1.328(3) . ? C16 F19 1.322(3) . ? C16 F17 1.324(3) . ? C16 F18 1.330(3) . ? C16 S20 1.830(3) . ? S20 O23 1.4278(17) . ? S20 O22 1.4289(18) . ? S20 N23 1.574(2) . ? N23 S24 1.5743(19) . ? S24 O25 1.4272(18) . ? S24 O26 1.4319(17) . ? S24 C27 1.832(2) . ? C27 F28 1.322(3) . ? C27 F29 1.324(3) . ? C27 F30 1.326(3) . ? N31 C32 1.318(3) . ? N31 C35 1.380(3) . ? C32 N33 1.351(3) . ? N33 C34 1.365(3) . ? N33 C36 1.460(3) . ? C34 C35 1.360(3) . ? N37 C38 1.320(3) . ? N37 C41 1.382(3) . ? C38 N39 1.339(3) . ? N39 C40 1.371(3) . ? N39 C42 1.466(3) . ? C40 C41 1.359(3) . ? N43 C44 1.320(3) . ? N43 C47 1.383(3) . ? C44 N45 1.344(3) . ? N45 C46 1.367(3) . ? N45 C48 1.465(3) . ? C46 C47 1.355(3) . ? N49 C50 1.320(3) . ? N49 C53 1.380(3) . ? C50 N51 1.342(3) . ? N51 C52 1.368(3) . ? N51 C54 1.465(3) . ? C52 C53 1.355(3) . ? N55 C56 1.325(3) . ? N55 C59 1.375(3) . ? C56 N57 1.340(3) . ? N57 C58 1.374(3) . ? N57 C60 1.461(3) . ? C58 C59 1.356(3) . ? N61 C62 1.320(3) . ? N61 C65 1.379(3) . ? C62 N63 1.340(3) . ? N63 C64 1.375(3) . ? N63 C66 1.461(3) . ? C64 C65 1.354(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N37 Cu1 N37 179.999(1) . 2_777 ? N37 Cu1 N43 89.39(7) . 2_777 ? N37 Cu1 N43 90.61(7) 2_777 2_777 ? N37 Cu1 N43 90.61(7) . . ? N37 Cu1 N43 89.39(7) 2_777 . ? N43 Cu1 N43 179.998(1) 2_777 . ? N37 Cu1 N31 90.98(6) . 2_777 ? N37 Cu1 N31 89.02(6) 2_777 2_777 ? N43 Cu1 N31 89.17(6) 2_777 2_777 ? N43 Cu1 N31 90.83(6) . 2_777 ? N37 Cu1 N31 89.02(6) . . ? N37 Cu1 N31 90.98(6) 2_777 . ? N43 Cu1 N31 90.83(6) 2_777 . ? N43 Cu1 N31 89.17(6) . . ? N31 Cu1 N31 179.999(1) 2_777 . ? N55 Cu2 N55 180.00(9) 2_666 . ? N55 Cu2 N49 89.62(7) 2_666 . ? N55 Cu2 N49 90.38(7) . . ? N55 Cu2 N49 90.38(7) 2_666 2_666 ? N55 Cu2 N49 89.62(7) . 2_666 ? N49 Cu2 N49 180.0 . 2_666 ? N55 Cu2 N61 89.33(6) 2_666 . ? N55 Cu2 N61 90.67(6) . . ? N49 Cu2 N61 89.52(6) . . ? N49 Cu2 N61 90.48(6) 2_666 . ? N55 Cu2 N61 90.67(6) 2_666 2_666 ? N55 Cu2 N61 89.33(6) . 2_666 ? N49 Cu2 N61 90.48(6) . 2_666 ? N49 Cu2 N61 89.52(6) 2_666 2_666 ? N61 Cu2 N61 179.999(1) . 2_666 ? F3 C1 F4 108.3(2) . . ? F3 C1 F2 108.7(2) . . ? F4 C1 F2 108.8(2) . . ? F3 C1 S5 110.89(17) . . ? F4 C1 S5 111.59(15) . . ? F2 C1 S5 108.56(19) . . ? O6 S5 O7 118.83(11) . . ? O6 S5 N8 116.10(10) . . ? O7 S5 N8 108.47(10) . . ? O6 S5 C1 104.50(11) . . ? O7 S5 C1 103.54(11) . . ? N8 S5 C1 103.28(11) . . ? S9 N8 S5 123.96(12) . . ? O10 S9 O11 118.82(11) . . ? O10 S9 N8 116.93(10) . . ? O11 S9 N8 108.10(10) . . ? O10 S9 C12 104.19(11) . . ? O11 S9 C12 102.83(11) . . ? N8 S9 C12 103.72(11) . . ? F13 C12 F15 108.5(2) . . ? F13 C12 F14 108.2(2) . . ? F15 C12 F14 108.17(19) . . ? F13 C12 S9 111.86(16) . . ? F15 C12 S9 111.45(16) . . ? F14 C12 S9 108.54(17) . . ? F19 C16 F17 108.9(2) . . ? F19 C16 F18 108.7(2) . . ? F17 C16 F18 108.3(2) . . ? F19 C16 S20 111.10(17) . . ? F17 C16 S20 110.64(16) . . ? F18 C16 S20 109.1(2) . . ? O23 S20 O22 118.54(11) . . ? O23 S20 N23 109.08(11) . . ? O22 S20 N23 116.91(10) . . ? O23 S20 C16 103.93(12) . . ? O22 S20 C16 104.78(11) . . ? N23 S20 C16 101.02(12) . . ? S20 N23 S24 124.96(12) . . ? O25 S24 O26 118.38(11) . . ? O25 S24 N23 109.08(11) . . ? O26 S24 N23 116.95(10) . . ? O25 S24 C27 103.60(11) . . ? O26 S24 C27 104.75(11) . . ? N23 S24 C27 101.56(11) . . ? F28 C27 F29 108.6(2) . . ? F28 C27 F30 108.96(19) . . ? F29 C27 F30 108.4(2) . . ? F28 C27 S24 111.21(16) . . ? F29 C27 S24 109.33(16) . . ? F30 C27 S24 110.28(16) . . ? C32 N31 C35 104.82(17) . . ? C32 N31 Cu1 125.48(14) . . ? C35 N31 Cu1 129.38(13) . . ? N31 C32 N33 112.02(19) . . ? C32 N33 C34 106.93(17) . . ? C32 N33 C36 125.6(2) . . ? C34 N33 C36 127.46(19) . . ? C35 C34 N33 106.20(18) . . ? C34 C35 N31 110.03(19) . . ? C38 N37 C41 105.48(17) . . ? C38 N37 Cu1 126.71(14) . . ? C41 N37 Cu1 127.63(14) . . ? N37 C38 N39 111.53(18) . . ? C38 N39 C40 107.46(17) . . ? C38 N39 C42 125.95(18) . . ? C40 N39 C42 126.59(18) . . ? C41 C40 N39 106.15(18) . . ? C40 C41 N37 109.38(18) . . ? C44 N43 C47 105.48(17) . . ? C44 N43 Cu1 125.65(14) . . ? C47 N43 Cu1 128.86(14) . . ? N43 C44 N45 111.46(18) . . ? C44 N45 C46 107.23(18) . . ? C44 N45 C48 126.44(18) . . ? C46 N45 C48 126.26(18) . . ? C47 C46 N45 106.57(18) . . ? C46 C47 N43 109.26(19) . . ? C50 N49 C53 105.44(18) . . ? C50 N49 Cu2 125.59(14) . . ? C53 N49 Cu2 128.97(15) . . ? N49 C50 N51 111.43(19) . . ? C50 N51 C52 107.33(18) . . ? C50 N51 C54 126.4(2) . . ? C52 N51 C54 126.2(2) . . ? C53 C52 N51 106.34(19) . . ? C52 C53 N49 109.5(2) . . ? C56 N55 C59 105.31(17) . . ? C56 N55 Cu2 129.50(14) . . ? C59 N55 Cu2 125.18(14) . . ? N55 C56 N57 111.46(18) . . ? C56 N57 C58 107.33(17) . . ? C56 N57 C60 126.70(18) . . ? C58 N57 C60 125.96(18) . . ? C59 C58 N57 105.97(18) . . ? C58 C59 N55 109.92(19) . . ? C62 N61 C65 104.41(17) . . ? C62 N61 Cu2 127.03(14) . . ? C65 N61 Cu2 128.33(13) . . ? N61 C62 N63 112.63(18) . . ? C62 N63 C64 106.61(17) . . ? C62 N63 C66 126.30(19) . . ? C64 N63 C66 127.09(18) . . ? C65 C64 N63 106.07(18) . . ? C64 C65 N61 110.28(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 66.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.441 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.072