Supplementary Material (ESI) for Journals of Materials Chemistry This journal is (C) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Chi, Yun' 'Carty, A.' 'Ching, Wei-Li' 'Chuang, Shiow-Huey' 'Hsu, Peng-Fu' 'Lee, Gene-Hsiang' 'Liu, Chao-Shiuan' 'Peng, Shie-ming' _publ_contact_author_name 'Prof Yun Chi' _publ_contact_author_address ; Department of Chemistry National Tsing Hua University Hsinchu 30013 TAIWAN ; _publ_contact_author_email 'YCHI@MX.NTHU.EDU.TW' _publ_section_title ; Fluorinated Aminoalkoxide CuII Complexes: New CVD Precursors for Deposition of Copper Metal ; data_ic6752 _database_code_CSD 187010 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H20 Cu F12 N2 O4' _chemical_formula_weight 571.86 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0215(2) _cell_length_b 12.7768(2) _cell_length_c 13.2584(1) _cell_angle_alpha 98.494(1) _cell_angle_beta 102.203(1) _cell_angle_gamma 114.022(1) _cell_volume 1608.65(4) _cell_formula_units_Z 3 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description column _exptl_crystal_colour blue _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method ? _exptl_crystal_F_000 861 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type 'empirical used sadabs' _exptl_absorpt_correction_T_min 0.7062 _exptl_absorpt_correction_T_max 0.8312 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Siemens SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22091 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6461 _reflns_number_observed 5331 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+1.1852P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6461 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_obs 0.0435 _refine_ls_wR_factor_all 0.1011 _refine_ls_wR_factor_obs 0.0932 _refine_ls_goodness_of_fit_all 1.013 _refine_ls_goodness_of_fit_obs 1.034 _refine_ls_restrained_S_all 1.013 _refine_ls_restrained_S_obs 1.034 _refine_ls_shift/esd_max -0.004 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cu1 Cu 0.56924(4) -0.42092(3) 0.83263(3) 0.03999(12) Uani 1 d . . Cu2 Cu 0.5000 0.0000 0.5000 0.03699(13) Uani 1 d S . O1 O 0.6433(2) -0.2182(2) 0.5752(2) 0.0572(6) Uani 1 d . . O2 O 0.4904(2) -0.3520(2) 0.92277(15) 0.0398(4) Uani 1 d . . O3 O 0.3181(2) -0.5975(2) 0.7412(2) 0.0583(6) Uani 1 d . . O4 O 0.6985(2) -0.4398(2) 0.7665(2) 0.0522(5) Uani 1 d . . O5 O 0.8502(3) -0.0069(3) 0.7710(2) 0.0835(8) Uani 1 d . . O6 O 0.6108(2) 0.0942(2) 0.4250(2) 0.0465(5) Uani 1 d . . N1 N 0.5418(3) -0.3206(2) 0.7365(2) 0.0405(5) Uani 1 d . . H1D H 0.6269(3) -0.2597(2) 0.7462(2) 0.049 Uiso 1 calc R . N2 N 0.5813(3) -0.5568(2) 0.8910(2) 0.0435(6) Uani 1 d . . H2C H 0.5621(3) -0.5549(2) 0.9545(2) 0.052 Uiso 1 calc R . N3 N 0.6807(2) 0.0298(2) 0.6036(2) 0.0390(5) Uani 1 d . . H3C H 0.6860(2) -0.0401(2) 0.5943(2) 0.047 Uiso 1 calc R . C1 C 0.7411(5) -0.2569(4) 0.5542(4) 0.0827(12) Uani 1 d . . H1A H 0.8318(5) -0.1902(4) 0.5760(4) 0.124 Uiso 1 calc R . H1B H 0.7148(5) -0.2928(4) 0.4791(4) 0.124 Uiso 1 calc R . H1C H 0.7429(5) -0.3140(4) 0.5934(4) 0.124 Uiso 1 calc R . C2 C 0.5046(3) -0.3080(3) 0.5470(2) 0.0508(8) Uani 1 d . . H2A H 0.4787(3) -0.3555(3) 0.4746(2) 0.061 Uiso 1 calc R . H2B H 0.4429(3) -0.2714(3) 0.5483(2) 0.061 Uiso 1 calc R . C3 C 0.4862(3) -0.3870(3) 0.6214(2) 0.0484(7) Uani 1 d . . H3A H 0.3878(3) -0.4399(3) 0.6050(2) 0.058 Uiso 1 calc R . H3B H 0.5330(3) -0.4354(3) 0.6090(2) 0.058 Uiso 1 calc R . C4 C 0.4563(3) -0.2683(3) 0.7726(2) 0.0432(7) Uani 1 d . . H4A H 0.3585(3) -0.3195(3) 0.7350(2) 0.052 Uiso 1 calc R . H4B H 0.4811(3) -0.1915(3) 0.7576(2) 0.052 Uiso 1 calc R . C5 C 0.4832(3) -0.2543(2) 0.8950(2) 0.0408(6) Uani 1 d . . C6 C 0.6198(4) -0.1421(3) 0.9565(3) 0.0541(8) Uani 1 d . . C7 C 0.3596(4) -0.2415(3) 0.9216(3) 0.0539(8) Uani 1 d . . C8 C 0.1861(4) -0.5987(4) 0.7313(4) 0.0855(13) Uani 1 d . . H8A H 0.1797(4) -0.5407(4) 0.6948(4) 0.128 Uiso 1 calc R . H8B H 0.1766(4) -0.5802(4) 0.8012(4) 0.128 Uiso 1 calc R . H8C H 0.1133(4) -0.6760(4) 0.6913(4) 0.128 Uiso 1 calc R . C9 C 0.3330(4) -0.6816(3) 0.7945(3) 0.0592(9) Uani 1 d . . H9A H 0.2654(4) -0.7613(3) 0.7525(3) 0.071 Uiso 1 calc R . H9B H 0.3171(4) -0.6684(3) 0.8634(3) 0.071 Uiso 1 calc R . C10 C 0.4764(3) -0.6682(3) 0.8092(3) 0.0523(8) Uani 1 d . . H10A H 0.4970(3) -0.6675(3) 0.7416(3) 0.063 Uiso 1 calc R . H10B H 0.4821(3) -0.7356(3) 0.8311(3) 0.063 Uiso 1 calc R . C11 C 0.7257(3) -0.5408(3) 0.9050(3) 0.0519(8) Uani 1 d . . H11A H 0.7247(3) -0.6178(3) 0.8880(3) 0.062 Uiso 1 calc R . H11B H 0.7817(3) -0.5005(3) 0.9788(3) 0.062 Uiso 1 calc R . C12 C 0.7904(3) -0.4665(3) 0.8303(2) 0.0465(7) Uani 1 d . . C13 C 0.8393(4) -0.5356(4) 0.7579(3) 0.0669(10) Uani 1 d . . C14 C 0.9166(4) -0.3503(4) 0.9007(4) 0.0744(11) Uani 1 d . . C15 C 0.9819(5) 0.0099(6) 0.8336(4) 0.111(2) Uani 1 d . . H15A H 0.9917(5) -0.0610(6) 0.8144(4) 0.167 Uiso 1 calc R . H15B H 0.9879(5) 0.0271(6) 0.9080(4) 0.167 Uiso 1 calc R . H15C H 1.0547(5) 0.0750(6) 0.8207(4) 0.167 Uiso 1 calc R . C16 C 0.8281(4) 0.0926(4) 0.7947(3) 0.0656(10) Uani 1 d . . H16A H 0.9039(4) 0.1618(4) 0.7879(3) 0.079 Uiso 1 calc R . H16B H 0.8242(4) 0.1077(4) 0.8675(3) 0.079 Uiso 1 calc R . C17 C 0.6923(3) 0.0692(3) 0.7175(2) 0.0523(8) Uani 1 d . . H17A H 0.6165(3) 0.0089(3) 0.7338(2) 0.063 Uiso 1 calc R . H17B H 0.6814(3) 0.1413(3) 0.7283(2) 0.063 Uiso 1 calc R . C18 C 0.7962(3) 0.1143(3) 0.5727(2) 0.0433(7) Uani 1 d . . H18A H 0.8729(3) 0.0940(3) 0.5845(2) 0.052 Uiso 1 calc R . H18B H 0.8293(3) 0.1941(3) 0.6164(2) 0.052 Uiso 1 calc R . C19 C 0.7448(3) 0.1094(3) 0.4531(2) 0.0398(6) Uani 1 d . . C20 C 0.7529(4) 0.0073(3) 0.3831(3) 0.0628(9) Uani 1 d . . C21 C 0.8417(3) 0.2283(3) 0.4361(3) 0.0511(8) Uani 1 d . . F1 F 0.7265(2) -0.1487(2) 0.9285(2) 0.0712(6) Uani 1 d . . F2 F 0.6190(3) -0.0429(2) 0.9370(2) 0.0855(7) Uani 1 d . . F3 F 0.6520(2) -0.1266(2) 1.0616(2) 0.0830(7) Uani 1 d . . F4 F 0.3376(3) -0.1570(2) 0.8854(2) 0.0754(6) Uani 1 d . . F5 F 0.3772(2) -0.2145(2) 1.0269(2) 0.0718(6) Uani 1 d . . F6 F 0.2433(2) -0.3423(2) 0.8790(2) 0.0784(6) Uani 1 d . . F7 F 0.7314(3) -0.6373(2) 0.6965(2) 0.0910(8) Uani 1 d . . F8 F 0.9299(3) -0.5675(2) 0.8119(2) 0.0922(8) Uani 1 d . . F9 F 0.8979(4) -0.4775(3) 0.6934(3) 0.1177(11) Uani 1 d . . F10 F 1.0129(2) -0.3672(2) 0.9666(2) 0.0962(8) Uani 1 d . . F11 F 0.9810(3) -0.2799(2) 0.8456(3) 0.1232(11) Uani 1 d . . F12 F 0.8720(3) -0.2911(2) 0.9635(3) 0.1148(11) Uani 1 d . . F13 F 0.6727(3) -0.0955(2) 0.4000(2) 0.0886(8) Uani 1 d . . F14 F 0.8799(3) 0.0147(3) 0.4030(3) 0.1116(10) Uani 1 d . . F15 F 0.7071(3) -0.0050(2) 0.2799(2) 0.0994(8) Uani 1 d . . F16 F 0.9752(2) 0.2541(2) 0.4720(2) 0.0807(7) Uani 1 d . . F17 F 0.8169(2) 0.2311(2) 0.3349(2) 0.0764(6) Uani 1 d . . F18 F 0.8273(3) 0.3171(2) 0.4879(2) 0.0839(7) Uani 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 0.0463(2) 0.0470(2) 0.0422(2) 0.0193(2) 0.0218(2) 0.0291(2) Cu2 0.0317(2) 0.0401(3) 0.0378(3) 0.0129(2) 0.0099(2) 0.0144(2) O1 0.0644(15) 0.0532(13) 0.0672(15) 0.0219(11) 0.0340(12) 0.0300(12) O2 0.0499(11) 0.0428(11) 0.0410(11) 0.0186(9) 0.0219(9) 0.0278(9) O3 0.0489(13) 0.0533(13) 0.071(2) 0.0175(11) 0.0166(11) 0.0215(11) O4 0.0596(13) 0.0745(15) 0.0562(13) 0.0363(11) 0.0345(11) 0.0474(12) O5 0.075(2) 0.098(2) 0.063(2) 0.023(2) -0.0084(14) 0.039(2) O6 0.0335(10) 0.0578(13) 0.0487(12) 0.0233(10) 0.0117(9) 0.0183(9) N1 0.0467(14) 0.0448(13) 0.0351(12) 0.0136(10) 0.0153(11) 0.0229(11) N2 0.0492(14) 0.0502(14) 0.0395(13) 0.0156(11) 0.0192(11) 0.0263(12) N3 0.0369(12) 0.0400(13) 0.0363(12) 0.0116(10) 0.0085(10) 0.0146(10) C1 0.089(3) 0.088(3) 0.106(3) 0.039(3) 0.053(3) 0.056(3) C2 0.062(2) 0.058(2) 0.039(2) 0.0144(14) 0.0155(15) 0.034(2) C3 0.059(2) 0.044(2) 0.039(2) 0.0074(13) 0.0146(14) 0.0214(15) C4 0.054(2) 0.046(2) 0.041(2) 0.0160(13) 0.0150(13) 0.0316(14) C5 0.051(2) 0.0403(15) 0.042(2) 0.0163(13) 0.0197(13) 0.0268(14) C6 0.070(2) 0.045(2) 0.044(2) 0.0102(14) 0.021(2) 0.022(2) C7 0.075(2) 0.061(2) 0.054(2) 0.024(2) 0.029(2) 0.049(2) C8 0.047(2) 0.086(3) 0.110(4) 0.017(3) 0.008(2) 0.028(2) C9 0.055(2) 0.050(2) 0.064(2) 0.016(2) 0.016(2) 0.016(2) C10 0.065(2) 0.044(2) 0.054(2) 0.0145(15) 0.022(2) 0.027(2) C11 0.051(2) 0.071(2) 0.055(2) 0.031(2) 0.024(2) 0.039(2) C12 0.047(2) 0.057(2) 0.053(2) 0.0215(15) 0.0242(14) 0.034(2) C13 0.079(3) 0.079(3) 0.073(3) 0.027(2) 0.039(2) 0.054(2) C14 0.055(2) 0.069(3) 0.100(3) 0.020(2) 0.027(2) 0.028(2) C15 0.073(3) 0.156(5) 0.100(4) 0.060(4) 0.003(3) 0.050(3) C16 0.059(2) 0.071(2) 0.039(2) 0.016(2) 0.005(2) 0.008(2) C17 0.052(2) 0.057(2) 0.039(2) 0.0134(14) 0.0157(14) 0.015(2) C18 0.0356(15) 0.052(2) 0.039(2) 0.0138(13) 0.0094(12) 0.0168(13) C19 0.0357(15) 0.048(2) 0.0374(15) 0.0132(12) 0.0121(12) 0.0199(13) C20 0.072(2) 0.067(2) 0.053(2) 0.011(2) 0.024(2) 0.034(2) C21 0.039(2) 0.064(2) 0.051(2) 0.022(2) 0.0170(14) 0.0206(15) F1 0.0541(12) 0.0681(13) 0.0717(14) 0.0049(11) 0.0210(10) 0.0125(10) F2 0.118(2) 0.0416(11) 0.091(2) 0.0178(11) 0.0327(14) 0.0307(12) F3 0.093(2) 0.0793(15) 0.0402(11) 0.0033(10) 0.0136(11) 0.0115(12) F4 0.113(2) 0.094(2) 0.0722(14) 0.0396(12) 0.0415(13) 0.0844(15) F5 0.104(2) 0.098(2) 0.0600(13) 0.0360(11) 0.0475(12) 0.0737(14) F6 0.0552(13) 0.083(2) 0.106(2) 0.0178(13) 0.0357(12) 0.0363(12) F7 0.105(2) 0.097(2) 0.080(2) -0.0033(14) 0.0232(14) 0.066(2) F8 0.090(2) 0.122(2) 0.112(2) 0.035(2) 0.0416(15) 0.085(2) F9 0.171(3) 0.145(3) 0.137(2) 0.082(2) 0.126(2) 0.112(2) F10 0.0531(13) 0.112(2) 0.106(2) 0.012(2) 0.0072(13) 0.0346(14) F11 0.091(2) 0.087(2) 0.187(3) 0.065(2) 0.053(2) 0.020(2) F12 0.090(2) 0.095(2) 0.135(2) -0.030(2) 0.011(2) 0.050(2) F13 0.143(2) 0.0526(13) 0.0749(15) 0.0126(11) 0.0492(15) 0.0423(14) F14 0.105(2) 0.129(2) 0.134(2) 0.015(2) 0.053(2) 0.084(2) F15 0.153(2) 0.095(2) 0.0453(13) 0.0110(12) 0.0393(14) 0.049(2) F16 0.0358(10) 0.103(2) 0.097(2) 0.0482(14) 0.0194(10) 0.0182(11) F17 0.0718(14) 0.093(2) 0.0617(13) 0.0453(12) 0.0233(11) 0.0250(12) F18 0.098(2) 0.0501(12) 0.112(2) 0.0274(12) 0.0591(15) 0.0267(12) _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 O4 1.898(2) . ? Cu1 O2 1.926(2) . ? Cu1 N1 1.999(2) . ? Cu1 N2 2.043(2) . ? Cu2 O6 1.897(2) . ? Cu2 O6 1.897(2) 2_656 ? Cu2 N3 2.017(2) 2_656 ? Cu2 N3 2.018(2) . ? O1 C1 1.415(4) . ? O1 C2 1.413(4) . ? O2 C5 1.380(3) . ? O3 C9 1.414(4) . ? O3 C8 1.426(4) . ? O4 C12 1.365(3) . ? O5 C16 1.393(5) . ? O5 C15 1.423(5) . ? O6 C19 1.367(3) . ? N1 C4 1.473(4) . ? N1 C3 1.491(4) . ? N2 C10 1.487(4) . ? N2 C11 1.486(4) . ? N3 C18 1.478(4) . ? N3 C17 1.481(4) . ? C2 C3 1.498(4) . ? C4 C5 1.555(4) . ? C5 C6 1.538(4) . ? C5 C7 1.541(4) . ? C6 F3 1.325(4) . ? C6 F2 1.335(4) . ? C6 F1 1.335(4) . ? C7 F6 1.325(4) . ? C7 F4 1.332(3) . ? C7 F5 1.339(4) . ? C9 C10 1.484(5) . ? C11 C12 1.555(4) . ? C12 C13 1.532(4) . ? C12 C14 1.539(5) . ? C13 F9 1.315(4) . ? C13 F7 1.336(5) . ? C13 F8 1.339(4) . ? C14 F11 1.318(5) . ? C14 F12 1.340(5) . ? C14 F10 1.337(5) . ? C16 C17 1.508(5) . ? C18 C19 1.549(4) . ? C19 C20 1.531(5) . ? C19 C21 1.543(4) . ? C20 F15 1.315(4) . ? C20 F14 1.330(4) . ? C20 F13 1.335(4) . ? C21 F17 1.321(4) . ? C21 F18 1.322(4) . ? C21 F16 1.328(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 O4 Cu1 O2 161.12(10) . . ? O4 Cu1 N1 89.19(9) . . ? O2 Cu1 N1 86.85(8) . . ? O4 Cu1 N2 81.94(9) . . ? O2 Cu1 N2 105.74(9) . . ? N1 Cu1 N2 163.94(10) . . ? O6 Cu2 O6 179.998(1) . 2_656 ? O6 Cu2 N3 93.54(8) . 2_656 ? O6 Cu2 N3 86.46(8) 2_656 2_656 ? O6 Cu2 N3 86.46(8) . . ? O6 Cu2 N3 93.54(8) 2_656 . ? N3 Cu2 N3 180.0 2_656 . ? C1 O1 C2 115.5(3) . . ? C5 O2 Cu1 111.5(2) . . ? C9 O3 C8 111.8(3) . . ? C12 O4 Cu1 112.7(2) . . ? C16 O5 C15 112.8(4) . . ? C19 O6 Cu2 113.2(2) . . ? C4 N1 C3 114.5(2) . . ? C4 N1 Cu1 108.1(2) . . ? C3 N1 Cu1 112.2(2) . . ? C10 N2 C11 112.2(2) . . ? C10 N2 Cu1 106.1(2) . . ? C11 N2 Cu1 106.7(2) . . ? C18 N3 C17 112.4(2) . . ? C18 N3 Cu2 107.9(2) . . ? C17 N3 Cu2 114.4(2) . . ? O1 C2 C3 111.9(3) . . ? N1 C3 C2 113.4(2) . . ? N1 C4 C5 108.5(2) . . ? O2 C5 C6 109.5(2) . . ? O2 C5 C7 109.9(2) . . ? C6 C5 C7 109.9(3) . . ? O2 C5 C4 111.4(2) . . ? C6 C5 C4 109.8(2) . . ? C7 C5 C4 106.4(2) . . ? F3 C6 F2 107.3(3) . . ? F3 C6 F1 106.1(3) . . ? F2 C6 F1 106.2(3) . . ? F3 C6 C5 113.3(3) . . ? F2 C6 C5 113.1(3) . . ? F1 C6 C5 110.4(3) . . ? F6 C7 F4 107.5(3) . . ? F6 C7 F5 106.5(3) . . ? F4 C7 F5 106.4(2) . . ? F6 C7 C5 110.7(3) . . ? F4 C7 C5 112.6(3) . . ? F5 C7 C5 112.8(3) . . ? O3 C9 C10 108.4(3) . . ? C9 C10 N2 111.5(3) . . ? N2 C11 C12 109.7(2) . . ? O4 C12 C13 108.0(3) . . ? O4 C12 C14 109.1(3) . . ? C13 C12 C14 109.2(3) . . ? O4 C12 C11 112.7(2) . . ? C13 C12 C11 109.8(3) . . ? C14 C12 C11 108.1(3) . . ? F9 C13 F7 107.0(4) . . ? F9 C13 F8 106.9(3) . . ? F7 C13 F8 105.2(3) . . ? F9 C13 C12 113.6(3) . . ? F7 C13 C12 110.2(3) . . ? F8 C13 C12 113.5(3) . . ? F11 C14 F12 108.0(4) . . ? F11 C14 F10 106.8(3) . . ? F12 C14 F10 106.0(4) . . ? F11 C14 C12 113.6(4) . . ? F12 C14 C12 108.4(3) . . ? F10 C14 C12 113.6(3) . . ? O5 C16 C17 108.3(3) . . ? N3 C17 C16 114.2(3) . . ? N3 C18 C19 109.6(2) . . ? O6 C19 C20 109.3(3) . . ? O6 C19 C21 109.4(2) . . ? C20 C19 C21 109.4(3) . . ? O6 C19 C18 111.3(2) . . ? C20 C19 C18 109.9(3) . . ? C21 C19 C18 107.5(2) . . ? F15 C20 F14 107.1(3) . . ? F15 C20 F13 105.6(3) . . ? F14 C20 F13 106.0(3) . . ? F15 C20 C19 113.7(3) . . ? F14 C20 C19 114.1(3) . . ? F13 C20 C19 109.7(3) . . ? F17 C21 F18 106.4(3) . . ? F17 C21 F16 106.7(3) . . ? F18 C21 F16 106.6(3) . . ? F17 C21 C19 113.5(3) . . ? F18 C21 C19 110.9(2) . . ? F16 C21 C19 112.4(3) . . ? _refine_diff_density_max 0.393 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.051 #===END data_ic7850 _database_code_CSD 187011 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H26 Cu F12 N2 O3' _chemical_formula_weight 585.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9469(4) _cell_length_b 10.7389(4) _cell_length_c 12.8240(5) _cell_angle_alpha 65.919(1) _cell_angle_beta 74.578(1) _cell_angle_gamma 83.479(1) _cell_volume 1205.58(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 5890 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 27.50 _exptl_crystal_description columnar _exptl_crystal_colour pink _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 1.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7454 _exptl_absorpt_correction_T_max 0.8621 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Bruker SMART 1K CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 16682 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5522 _reflns_number_gt 3934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0286P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5522 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.0000 0.5000 0.5000 0.02026(8) Uani 1 2 d S . . Cu2 Cu 0.0000 1.0000 0.0000 0.02140(9) Uani 1 2 d S . . O1 O 0.11847(13) 0.63987(12) 0.47512(10) 0.0240(3) Uani 1 1 d . . . O2 O 0.08036(13) 1.04313(12) 0.09867(10) 0.0261(3) Uani 1 1 d . . . N1 N -0.09237(15) 0.51120(15) 0.65632(12) 0.0222(3) Uani 1 1 d . . . H1A H -0.0657 0.4339 0.7144 0.027 Uiso 1 1 calc R . . N2 N 0.17445(15) 1.08054(15) -0.12753(12) 0.0227(3) Uani 1 1 d . . . H2A H 0.1481 1.1581 -0.1856 0.027 Uiso 1 1 calc R . . C1 C -0.2890(2) 0.3723(3) 0.90123(19) 0.0553(7) Uani 1 1 d . . . H1B H -0.1884 0.3664 0.8951 0.083 Uiso 1 1 calc R . . H1C H -0.3184 0.2943 0.8917 0.083 Uiso 1 1 calc R . . H1D H -0.3387 0.3712 0.9786 0.083 Uiso 1 1 calc R . . C2 C -0.4794(2) 0.5151(3) 0.8141(2) 0.0480(6) Uani 1 1 d . . . H2B H -0.4996 0.6009 0.7527 0.072 Uiso 1 1 calc R . . H2C H -0.5294 0.5134 0.8916 0.072 Uiso 1 1 calc R . . H2D H -0.5096 0.4383 0.8034 0.072 Uiso 1 1 calc R . . C3 C -0.3224(2) 0.5035(2) 0.80583(17) 0.0342(5) Uani 1 1 d . . . H3A H -0.2930 0.5823 0.8172 0.041 Uiso 1 1 calc R . . C4 C -0.24706(18) 0.5121(2) 0.68304(16) 0.0272(4) Uani 1 1 d . . . H4A H -0.2771 0.4344 0.6721 0.033 Uiso 1 1 calc R . . H4B H -0.2775 0.5968 0.6248 0.033 Uiso 1 1 calc R . . C5 C -0.03559(19) 0.63068(19) 0.65956(16) 0.0274(4) Uani 1 1 d . . . H5A H -0.0280 0.6102 0.7404 0.033 Uiso 1 1 calc R . . H5B H -0.0992 0.7098 0.6370 0.033 Uiso 1 1 calc R . . C6 C 0.10983(19) 0.66553(18) 0.57337(15) 0.0230(4) Uani 1 1 d . . . C7 C 0.2224(2) 0.5818(2) 0.63564(17) 0.0318(5) Uani 1 1 d . . . C8 C 0.1360(2) 0.8190(2) 0.53289(18) 0.0358(5) Uani 1 1 d . . . C9 C 0.3322(2) 1.1561(2) -0.39240(18) 0.0451(6) Uani 1 1 d . . . H9A H 0.4166 1.1895 -0.4557 0.068 Uiso 1 1 calc R . . H9B H 0.2885 1.2307 -0.3696 0.068 Uiso 1 1 calc R . . H9C H 0.2668 1.1225 -0.4200 0.068 Uiso 1 1 calc R . . C10 C 0.4421(2) 0.9237(2) -0.31935(19) 0.0384(5) Uani 1 1 d . . . H10A H 0.4672 0.8514 -0.2504 0.058 Uiso 1 1 calc R . . H10B H 0.5266 0.9575 -0.3824 0.058 Uiso 1 1 calc R . . H10C H 0.3784 0.8873 -0.3465 0.058 Uiso 1 1 calc R . . C11 C 0.3708(2) 1.0403(2) -0.28623(16) 0.0297(4) Uani 1 1 d . . . H11A H 0.4376 1.0765 -0.2595 0.036 Uiso 1 1 calc R . . C12 C 0.24337(19) 0.98510(19) -0.18361(16) 0.0264(4) Uani 1 1 d . . . H12A H 0.1736 0.9570 -0.2121 0.032 Uiso 1 1 calc R . . H12B H 0.2721 0.9023 -0.1224 0.032 Uiso 1 1 calc R . . C13 C 0.26912(19) 1.1243(2) -0.07670(16) 0.0281(4) Uani 1 1 d . . . H13A H 0.3111 1.2134 -0.1335 0.034 Uiso 1 1 calc R . . H13B H 0.3454 1.0567 -0.0609 0.034 Uiso 1 1 calc R . . C14 C 0.18591(19) 1.13679(19) 0.03918(15) 0.0247(4) Uani 1 1 d . . . C15 C 0.2869(2) 1.1114(2) 0.11814(18) 0.0363(5) Uani 1 1 d . . . C16 C 0.1222(2) 1.2806(2) 0.01220(17) 0.0334(5) Uani 1 1 d . . . F1 F 0.19214(12) 0.44741(11) 0.68035(10) 0.0408(3) Uani 1 1 d . . . F2 F 0.34912(12) 0.59614(14) 0.56451(11) 0.0508(3) Uani 1 1 d . . . F3 F 0.23046(13) 0.61065(13) 0.72578(10) 0.0461(3) Uani 1 1 d . . . F4 F 0.11171(13) 0.85737(12) 0.62378(10) 0.0454(3) Uani 1 1 d . . . F5 F 0.05211(14) 0.89226(11) 0.46433(11) 0.0508(4) Uani 1 1 d . . . F6 F 0.26629(14) 0.85547(12) 0.47052(11) 0.0533(4) Uani 1 1 d . . . F7 F 0.22983(13) 1.13804(14) 0.21392(10) 0.0499(3) Uani 1 1 d . . . F8 F 0.32766(14) 0.98160(13) 0.15602(11) 0.0540(4) Uani 1 1 d . . . F9 F 0.40316(12) 1.18676(14) 0.06178(11) 0.0526(4) Uani 1 1 d . . . F10 F 0.21659(14) 1.37903(12) -0.02936(11) 0.0510(3) Uani 1 1 d . . . F11 F 0.03201(13) 1.29334(13) 0.10489(10) 0.0482(3) Uani 1 1 d . . . F12 F 0.05047(12) 1.30963(12) -0.07069(10) 0.0411(3) Uani 1 1 d . . . O3 O 0.03444(16) 0.78359(16) 0.26746(14) 0.0325(3) Uani 1 1 d . . . H3B H 0.064(2) 0.762(2) 0.3246(19) 0.043(7) Uiso 1 1 d . . . H3C H 0.065(2) 0.857(2) 0.229(2) 0.046(8) Uiso 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 0.02369(18) 0.01948(17) 0.01849(17) -0.00796(14) -0.00484(13) -0.00233(13) Cu2 0.02114(18) 0.02580(19) 0.01684(17) -0.00625(14) -0.00540(13) -0.00509(14) O1 0.0310(7) 0.0231(7) 0.0195(6) -0.0090(5) -0.0052(5) -0.0064(5) O2 0.0282(7) 0.0317(7) 0.0172(6) -0.0049(6) -0.0062(5) -0.0119(6) N1 0.0215(8) 0.0247(8) 0.0211(8) -0.0097(7) -0.0042(6) -0.0023(6) N2 0.0235(8) 0.0260(8) 0.0182(8) -0.0071(7) -0.0062(6) -0.0026(6) C1 0.0417(14) 0.0784(19) 0.0294(12) -0.0140(12) 0.0019(11) 0.0090(13) C2 0.0261(12) 0.0632(16) 0.0572(15) -0.0317(13) -0.0021(11) 0.0015(11) C3 0.0234(11) 0.0461(13) 0.0371(12) -0.0232(10) -0.0020(9) -0.0015(9) C4 0.0220(10) 0.0329(12) 0.0296(11) -0.0146(9) -0.0064(9) -0.0018(8) C5 0.0257(10) 0.0327(11) 0.0298(10) -0.0189(9) -0.0052(8) -0.0012(8) C6 0.0261(10) 0.0228(10) 0.0220(9) -0.0087(8) -0.0082(8) -0.0021(8) C7 0.0302(12) 0.0355(12) 0.0296(11) -0.0112(9) -0.0080(9) -0.0041(9) C8 0.0484(14) 0.0280(12) 0.0364(12) -0.0139(10) -0.0150(11) -0.0051(10) C9 0.0477(14) 0.0423(14) 0.0296(12) -0.0088(10) 0.0068(10) 0.0004(11) C10 0.0299(12) 0.0480(14) 0.0433(13) -0.0264(11) -0.0063(10) 0.0026(10) C11 0.0239(10) 0.0368(12) 0.0316(11) -0.0185(9) -0.0021(8) -0.0041(9) C12 0.0266(11) 0.0267(11) 0.0256(10) -0.0107(9) -0.0052(9) -0.0006(8) C13 0.0216(10) 0.0384(12) 0.0267(10) -0.0146(9) -0.0043(8) -0.0070(8) C14 0.0244(10) 0.0301(11) 0.0202(9) -0.0081(8) -0.0062(8) -0.0074(8) C15 0.0354(13) 0.0452(14) 0.0291(11) -0.0101(10) -0.0113(10) -0.0125(10) C16 0.0373(12) 0.0374(13) 0.0275(11) -0.0134(10) -0.0060(9) -0.0092(10) F1 0.0439(7) 0.0276(7) 0.0464(7) -0.0065(6) -0.0186(6) 0.0039(5) F2 0.0247(7) 0.0663(9) 0.0541(8) -0.0179(7) -0.0070(6) -0.0005(6) F3 0.0523(8) 0.0575(8) 0.0402(7) -0.0204(6) -0.0281(6) -0.0007(6) F4 0.0672(9) 0.0368(7) 0.0480(8) -0.0273(6) -0.0208(7) -0.0039(6) F5 0.0837(10) 0.0247(6) 0.0532(8) -0.0132(6) -0.0387(8) 0.0083(6) F6 0.0589(9) 0.0406(8) 0.0541(8) -0.0148(6) 0.0014(7) -0.0272(7) F7 0.0535(8) 0.0764(10) 0.0289(7) -0.0236(7) -0.0141(6) -0.0148(7) F8 0.0579(9) 0.0518(9) 0.0599(9) -0.0140(7) -0.0418(7) 0.0056(7) F9 0.0369(7) 0.0783(10) 0.0440(8) -0.0162(7) -0.0141(6) -0.0266(7) F10 0.0591(9) 0.0342(7) 0.0567(8) -0.0129(6) -0.0092(7) -0.0202(6) F11 0.0578(9) 0.0517(8) 0.0396(7) -0.0285(6) -0.0025(6) 0.0008(7) F12 0.0486(8) 0.0405(7) 0.0397(7) -0.0169(6) -0.0222(6) 0.0102(6) O3 0.0435(9) 0.0247(8) 0.0289(8) -0.0030(7) -0.0188(7) -0.0045(7) _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 O1 1.8861(11) . ? Cu1 O1 1.8861(11) 2_566 ? Cu1 N1 2.0173(14) 2_566 ? Cu1 N1 2.0173(14) . ? Cu2 O2 1.8854(11) . ? Cu2 O2 1.8854(11) 2_575 ? Cu2 N2 2.0276(14) . ? Cu2 N2 2.0276(14) 2_575 ? O1 C6 1.375(2) . ? O1 H3B 2.02(2) . ? O2 C14 1.372(2) . ? O2 H3C 2.01(2) . ? N1 C5 1.479(2) . ? N1 C4 1.485(2) . ? N1 H1A 0.9300 . ? N2 C13 1.486(2) . ? N2 C12 1.489(2) . ? N2 H2A 0.9300 . ? C1 C3 1.515(3) . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 C3 1.531(3) . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C2 H2D 0.9800 . ? C3 C4 1.523(2) . ? C3 H3A 1.0000 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.546(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.536(3) . ? C6 C8 1.543(3) . ? C7 F2 1.328(2) . ? C7 F3 1.337(2) . ? C7 F1 1.354(2) . ? C8 F5 1.329(2) . ? C8 F6 1.335(2) . ? C8 F4 1.344(2) . ? C9 C11 1.528(3) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.524(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.529(2) . ? C11 H11A 1.0000 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.547(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.537(3) . ? C14 C16 1.538(3) . ? C15 F8 1.329(2) . ? C15 F7 1.339(2) . ? C15 F9 1.344(2) . ? C16 F11 1.332(2) . ? C16 F10 1.335(2) . ? C16 F12 1.349(2) . ? O3 H3B 0.80(2) . ? O3 H3C 0.78(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 O1 Cu1 O1 180.000(1) . 2_566 ? O1 Cu1 N1 93.57(5) . 2_566 ? O1 Cu1 N1 86.43(5) 2_566 2_566 ? O1 Cu1 N1 86.43(5) . . ? O1 Cu1 N1 93.57(5) 2_566 . ? N1 Cu1 N1 180.0 2_566 . ? O2 Cu2 O2 180.0 . 2_575 ? O2 Cu2 N2 86.08(5) . . ? O2 Cu2 N2 93.92(5) 2_575 . ? O2 Cu2 N2 93.92(5) . 2_575 ? O2 Cu2 N2 86.08(5) 2_575 2_575 ? N2 Cu2 N2 180.0 . 2_575 ? C6 O1 Cu1 114.40(10) . . ? C6 O1 H3B 128.8(6) . . ? Cu1 O1 H3B 91.7(6) . . ? C14 O2 Cu2 114.00(10) . . ? C14 O2 H3C 133.5(7) . . ? Cu2 O2 H3C 97.2(6) . . ? C5 N1 C4 112.81(14) . . ? C5 N1 Cu1 108.27(11) . . ? C4 N1 Cu1 113.64(10) . . ? C5 N1 H1A 107.3 . . ? C4 N1 H1A 107.3 . . ? Cu1 N1 H1A 107.3 . . ? C13 N2 C12 112.58(14) . . ? C13 N2 Cu2 108.71(10) . . ? C12 N2 Cu2 112.28(11) . . ? C13 N2 H2A 107.7 . . ? C12 N2 H2A 107.7 . . ? Cu2 N2 H2A 107.7 . . ? C3 C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C3 C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 C2 H2D 109.5 . . ? H2B C2 H2D 109.5 . . ? H2C C2 H2D 109.5 . . ? C1 C3 C4 112.09(17) . . ? C1 C3 C2 110.33(18) . . ? C4 C3 C2 108.32(16) . . ? C1 C3 H3A 108.7 . . ? C4 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? N1 C4 C3 115.91(15) . . ? N1 C4 H4A 108.3 . . ? C3 C4 H4A 108.3 . . ? N1 C4 H4B 108.3 . . ? C3 C4 H4B 108.3 . . ? H4A C4 H4B 107.4 . . ? N1 C5 C6 109.51(14) . . ? N1 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? N1 C5 H5B 109.8 . . ? C6 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? O1 C6 C7 109.06(15) . . ? O1 C6 C8 108.06(14) . . ? C7 C6 C8 109.57(15) . . ? O1 C6 C5 111.94(14) . . ? C7 C6 C5 109.83(15) . . ? C8 C6 C5 108.33(15) . . ? F2 C7 F3 107.51(16) . . ? F2 C7 F1 106.10(16) . . ? F3 C7 F1 106.73(15) . . ? F2 C7 C6 113.58(16) . . ? F3 C7 C6 113.02(16) . . ? F1 C7 C6 109.45(15) . . ? F5 C8 F6 106.85(17) . . ? F5 C8 F4 107.44(17) . . ? F6 C8 F4 107.16(16) . . ? F5 C8 C6 109.95(16) . . ? F6 C8 C6 112.78(17) . . ? F4 C8 C6 112.36(16) . . ? C11 C9 H9A 109.5 . . ? C11 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C11 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C11 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C10 C11 C9 110.87(17) . . ? C10 C11 C12 109.08(16) . . ? C9 C11 C12 111.97(17) . . ? C10 C11 H11A 108.3 . . ? C9 C11 H11A 108.3 . . ? C12 C11 H11A 108.3 . . ? N2 C12 C11 116.07(15) . . ? N2 C12 H12A 108.3 . . ? C11 C12 H12A 108.3 . . ? N2 C12 H12B 108.3 . . ? C11 C12 H12B 108.3 . . ? H12A C12 H12B 107.4 . . ? N2 C13 C14 109.61(14) . . ? N2 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N2 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O2 C14 C15 108.50(14) . . ? O2 C14 C16 108.59(15) . . ? C15 C14 C16 109.76(16) . . ? O2 C14 C13 111.99(15) . . ? C15 C14 C13 108.17(16) . . ? C16 C14 C13 109.80(15) . . ? F8 C15 F7 106.73(16) . . ? F8 C15 F9 106.70(18) . . ? F7 C15 F9 106.76(16) . . ? F8 C15 C14 110.56(16) . . ? F7 C15 C14 112.95(18) . . ? F9 C15 C14 112.74(16) . . ? F11 C16 F10 106.93(16) . . ? F11 C16 F12 106.29(16) . . ? F10 C16 F12 106.69(15) . . ? F11 C16 C14 113.39(16) . . ? F10 C16 C14 113.81(16) . . ? F12 C16 C14 109.27(15) . . ? H3B O3 H3C 102(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.324 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.051 #===END