Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'William Tolman' _publ_contact_author_address ; Department of Chemistry 139 Smith Hall University of Minnesota 207 Pleasant St. SE Minneapolis Minneapolis MN 55455 UNITED STATES OF AMERICA ; _publ_contact_author_email TOLMAN@CHEM.UMN.EDU _publ_section_title ; Modular Syntheses of Multidentate Ligands with Variable N-Donors: Applications to Tri- and Tetracopper(I) Complexes ; loop_ _publ_author_name 'William Tolman' 'Eric C Brown' 'Luigi Casella' 'Brandon Johnson' 'Benjamin E Kucera' 'Sara Palvicini' data_03229m _database_code_depnum_ccdc_archive 'CCDC 644162' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '03229-tricopper complex 15b' _chemical_melting_point ? _chemical_formula_moiety 'C41 H84 Cu3 N12, 2(C2 H3 N), 3(Cl2 Cu)' _chemical_formula_sum 'C45 H90 Cl6 Cu6 N14' _chemical_formula_weight 1421.25 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' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.4067(18) _cell_length_b 25.573(4) _cell_length_c 23.159(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.558(3) _cell_angle_gamma 90.00 _cell_volume 6661.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 983 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 23.32 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 _exptl_absorpt_coefficient_mu 2.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5184 _exptl_absorpt_correction_T_max 0.7375 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49536 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.08 _reflns_number_total 11821 _reflns_number_gt 8060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.0644P)^2^+11.8506P] 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 11821 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.56061(5) 0.45283(2) 0.30074(3) 0.03139(15) Uani 1 1 d . . . Cu2 Cu 0.61961(5) 0.63245(2) 0.16522(3) 0.03429(15) Uani 1 1 d . . . Cu3 Cu 0.44952(5) 0.65968(2) 0.38116(3) 0.03099(15) Uani 1 1 d . . . N1 N 0.4046(3) 0.47939(13) 0.26004(17) 0.0299(8) Uani 1 1 d . . . N2 N 0.5144(3) 0.36890(13) 0.29039(17) 0.0303(9) Uani 1 1 d . . . N3 N 0.6926(3) 0.43622(14) 0.24613(19) 0.0365(9) Uani 1 1 d . . . N4 N 0.6568(4) 0.46778(15) 0.37567(19) 0.0390(10) Uani 1 1 d . . . N5 N 0.4480(3) 0.61608(14) 0.15475(16) 0.0293(8) Uani 1 1 d . . . N6 N 0.6134(4) 0.66901(16) 0.07894(18) 0.0414(10) Uani 1 1 d . . . N7 N 0.6605(4) 0.70947(16) 0.20066(19) 0.0419(10) Uani 1 1 d . . . N8 N 0.7653(4) 0.59273(17) 0.1808(2) 0.0459(11) Uani 1 1 d . . . N9 N 0.3191(3) 0.63441(13) 0.32092(16) 0.0267(8) Uani 1 1 d . . . N10 N 0.3332(4) 0.69904(16) 0.43600(18) 0.0416(10) Uani 1 1 d . . . N11 N 0.4875(4) 0.60579(15) 0.45374(18) 0.0401(10) Uani 1 1 d . . . N12 N 0.5885(4) 0.70305(16) 0.38508(19) 0.0398(10) Uani 1 1 d . . . Cu4 Cu 0.14295(6) 0.72085(3) 0.10949(3) 0.0529(2) Uani 1 1 d . . . Cu5 Cu 0.99035(6) 0.57340(3) 0.37895(3) 0.0545(2) Uani 1 1 d . . . Cu6 Cu 0.26674(8) 0.44003(4) 0.09528(4) 0.0703(3) Uani 1 1 d . . . Cl1 Cl 0.2467(2) 0.76312(9) 0.05993(11) 0.1089(8) Uani 1 1 d . . . Cl2 Cl 0.03584(16) 0.67909(7) 0.15750(9) 0.0776(5) Uani 1 1 d . . . Cl3 Cl 1.10208(15) 0.51288(7) 0.36542(10) 0.0806(5) Uani 1 1 d . . . Cl4 Cl 0.8749(3) 0.63156(10) 0.39578(13) 0.1337(11) Uani 1 1 d . . . Cl5 Cl 0.36595(19) 0.37156(8) 0.10579(7) 0.0840(6) Uani 1 1 d . . . Cl6 Cl 0.16090(18) 0.50773(8) 0.08490(10) 0.0904(6) Uani 1 1 d . . . C1 C 0.5402(4) 0.58370(17) 0.2841(2) 0.0303(10) Uani 1 1 d . . . H1A H 0.5538 0.5586 0.3165 0.046 Uiso 1 1 calc R . . H1B H 0.5522 0.6193 0.2995 0.046 Uiso 1 1 calc R . . H1C H 0.5962 0.5768 0.2571 0.046 Uiso 1 1 calc R . . C2 C 0.4126(4) 0.57799(16) 0.25130(19) 0.0258(9) Uani 1 1 d . . . C3 C 0.3943(4) 0.52480(16) 0.2200(2) 0.0302(10) Uani 1 1 d . . . H3A H 0.3145 0.5243 0.1955 0.036 Uiso 1 1 calc R . . H3B H 0.4537 0.5211 0.1936 0.036 Uiso 1 1 calc R . . C4 C 0.3120(4) 0.45123(17) 0.2581(2) 0.0300(10) Uani 1 1 d . . . H4A H 0.2425 0.4620 0.2324 0.036 Uiso 1 1 calc R . . C5 C 0.3038(4) 0.40245(17) 0.2932(2) 0.0321(11) Uani 1 1 d . . . C6 C 0.1753(4) 0.3818(2) 0.2793(3) 0.0461(13) Uani 1 1 d . . . H6A H 0.1208 0.4079 0.2909 0.069 Uiso 1 1 calc R . . H6B H 0.1689 0.3493 0.3011 0.069 Uiso 1 1 calc R . . H6C H 0.1545 0.3749 0.2373 0.069 Uiso 1 1 calc R . . C7 C 0.3340(4) 0.41416(18) 0.3592(2) 0.0368(11) Uani 1 1 d . . . H7A H 0.2779 0.4400 0.3698 0.055 Uiso 1 1 calc R . . H7B H 0.4151 0.4280 0.3684 0.055 Uiso 1 1 calc R . . H7C H 0.3283 0.3819 0.3814 0.055 Uiso 1 1 calc R . . C8 C 0.3850(4) 0.35956(17) 0.2736(2) 0.0322(11) Uani 1 1 d . . . H8A H 0.3654 0.3257 0.2905 0.039 Uiso 1 1 calc R . . H8B H 0.3663 0.3563 0.2304 0.039 Uiso 1 1 calc R . . C9 C 0.5602(4) 0.33865(18) 0.3444(2) 0.0375(11) Uani 1 1 d . . . H9A H 0.5508 0.3012 0.3362 0.056 Uiso 1 1 calc R . . H9B H 0.5155 0.3482 0.3754 0.056 Uiso 1 1 calc R . . H9C H 0.6446 0.3467 0.3571 0.056 Uiso 1 1 calc R . . C10 C 0.5793(4) 0.35343(18) 0.2429(2) 0.0384(12) Uani 1 1 d . . . H10A H 0.5326 0.3639 0.2048 0.046 Uiso 1 1 calc R . . H10B H 0.5879 0.3149 0.2429 0.046 Uiso 1 1 calc R . . C11 C 0.7013(4) 0.37831(18) 0.2499(3) 0.0410(12) Uani 1 1 d . . . H11A H 0.7478 0.3683 0.2882 0.049 Uiso 1 1 calc R . . H11B H 0.7437 0.3652 0.2188 0.049 Uiso 1 1 calc R . . C12 C 0.6583(5) 0.4530(2) 0.1852(2) 0.0499(14) Uani 1 1 d . . . H12A H 0.7193 0.4421 0.1625 0.075 Uiso 1 1 calc R . . H12B H 0.6506 0.4912 0.1837 0.075 Uiso 1 1 calc R . . H12C H 0.5821 0.4370 0.1686 0.075 Uiso 1 1 calc R . . C13 C 0.8117(4) 0.4590(2) 0.2697(3) 0.0514(14) Uani 1 1 d . . . H13A H 0.8689 0.4488 0.2445 0.077 Uiso 1 1 calc R . . H13B H 0.8385 0.4458 0.3095 0.077 Uiso 1 1 calc R . . H13C H 0.8057 0.4972 0.2707 0.077 Uiso 1 1 calc R . . C14 C 0.7293(4) 0.47528(18) 0.4143(2) 0.0375(11) Uani 1 1 d . . . C15 C 0.8247(5) 0.4858(2) 0.4640(3) 0.0549(15) Uani 1 1 d . . . H15A H 0.8734 0.4543 0.4728 0.082 Uiso 0.50 1 calc PR . . H15B H 0.7896 0.4956 0.4983 0.082 Uiso 0.50 1 calc PR . . H15C H 0.8745 0.5145 0.4539 0.082 Uiso 0.50 1 calc PR . . H15D H 0.8183 0.5219 0.4772 0.082 Uiso 0.50 1 calc PR . . H15E H 0.9021 0.4807 0.4517 0.082 Uiso 0.50 1 calc PR . . H15F H 0.8172 0.4618 0.4961 0.082 Uiso 0.50 1 calc PR . . C16 C 0.3802(4) 0.62029(16) 0.2035(2) 0.0294(10) Uani 1 1 d . . . H16A H 0.2943 0.6177 0.1876 0.035 Uiso 1 1 calc R . . H16B H 0.3946 0.6552 0.2218 0.035 Uiso 1 1 calc R . . C17 C 0.3876(4) 0.60999(18) 0.1042(2) 0.0362(11) Uani 1 1 d . . . H17A H 0.3035 0.6087 0.1008 0.043 Uiso 1 1 calc R . . C18 C 0.4408(5) 0.6046(2) 0.0494(2) 0.0437(13) Uani 1 1 d . . . C19 C 0.3399(6) 0.5977(3) -0.0035(3) 0.0687(19) Uani 1 1 d . . . H19A H 0.2946 0.5660 0.0018 0.103 Uiso 1 1 calc R . . H19B H 0.3742 0.5946 -0.0395 0.103 Uiso 1 1 calc R . . H19C H 0.2869 0.6281 -0.0065 0.103 Uiso 1 1 calc R . . C20 C 0.5232(5) 0.5571(2) 0.0535(3) 0.0508(14) Uani 1 1 d . . . H20A H 0.4775 0.5253 0.0579 0.076 Uiso 1 1 calc R . . H20B H 0.5864 0.5609 0.0875 0.076 Uiso 1 1 calc R . . H20C H 0.5585 0.5547 0.0178 0.076 Uiso 1 1 calc R . . C21 C 0.5049(5) 0.6562(2) 0.0368(2) 0.0488(14) Uani 1 1 d . . . H21A H 0.5264 0.6537 -0.0028 0.059 Uiso 1 1 calc R . . H21B H 0.4479 0.6855 0.0363 0.059 Uiso 1 1 calc R . . C22 C 0.7209(5) 0.6540(2) 0.0538(2) 0.0534(15) Uani 1 1 d . . . H22A H 0.7207 0.6727 0.0169 0.080 Uiso 1 1 calc R . . H22B H 0.7200 0.6163 0.0466 0.080 Uiso 1 1 calc R . . H22C H 0.7925 0.6633 0.0815 0.080 Uiso 1 1 calc R . . C23 C 0.6167(5) 0.7254(2) 0.0938(2) 0.0502(14) Uani 1 1 d . . . H23A H 0.5359 0.7374 0.0977 0.060 Uiso 1 1 calc R . . H23B H 0.6429 0.7456 0.0617 0.060 Uiso 1 1 calc R . . C24 C 0.7009(5) 0.7357(2) 0.1504(2) 0.0490(14) Uani 1 1 d . . . H24A H 0.7812 0.7229 0.1468 0.059 Uiso 1 1 calc R . . H24B H 0.7062 0.7738 0.1577 0.059 Uiso 1 1 calc R . . C25 C 0.5613(5) 0.7381(2) 0.2188(3) 0.0563(15) Uani 1 1 d . . . H25A H 0.5853 0.7743 0.2280 0.084 Uiso 1 1 calc R . . H25B H 0.5391 0.7214 0.2535 0.084 Uiso 1 1 calc R . . H25C H 0.4930 0.7377 0.1869 0.084 Uiso 1 1 calc R . . C26 C 0.7592(5) 0.7074(2) 0.2505(3) 0.0570(16) Uani 1 1 d . . . H26A H 0.7833 0.7431 0.2626 0.085 Uiso 1 1 calc R . . H26B H 0.8268 0.6890 0.2387 0.085 Uiso 1 1 calc R . . H26C H 0.7334 0.6889 0.2832 0.085 Uiso 1 1 calc R . . C27 C 0.8566(5) 0.5735(2) 0.1849(3) 0.0576(16) Uani 1 1 d . . . C28 C 0.9729(6) 0.5477(3) 0.1886(4) 0.091(3) Uani 1 1 d . . . H28A H 0.9643 0.5161 0.1644 0.137 Uiso 1 1 calc R . . H28B H 1.0026 0.5382 0.2294 0.137 Uiso 1 1 calc R . . H28C H 1.0292 0.5716 0.1746 0.137 Uiso 1 1 calc R . . C29 C 0.3215(4) 0.58241(16) 0.2927(2) 0.0301(10) Uani 1 1 d . . . H29A H 0.2415 0.5749 0.2704 0.036 Uiso 1 1 calc R . . H29B H 0.3394 0.5555 0.3236 0.036 Uiso 1 1 calc R . . C30 C 0.2196(4) 0.65857(18) 0.3125(2) 0.0349(11) Uani 1 1 d . . . H30A H 0.1536 0.6417 0.2895 0.042 Uiso 1 1 calc R . . C31 C 0.2001(4) 0.71225(18) 0.3365(2) 0.0378(12) Uani 1 1 d . . . C32 C 0.2843(5) 0.75170(19) 0.3148(3) 0.0454(13) Uani 1 1 d . . . H32A H 0.3669 0.7414 0.3290 0.068 Uiso 1 1 calc R . . H32B H 0.2700 0.7866 0.3298 0.068 Uiso 1 1 calc R . . H32C H 0.2700 0.7523 0.2719 0.068 Uiso 1 1 calc R . . C33 C 0.0704(5) 0.7287(2) 0.3137(3) 0.0533(15) Uani 1 1 d . . . H33A H 0.0582 0.7316 0.2709 0.080 Uiso 1 1 calc R . . H33B H 0.0546 0.7626 0.3306 0.080 Uiso 1 1 calc R . . H33C H 0.0161 0.7024 0.3250 0.080 Uiso 1 1 calc R . . C34 C 0.2129(4) 0.7108(2) 0.4036(2) 0.0435(13) Uani 1 1 d . . . H34A H 0.1879 0.7452 0.4170 0.052 Uiso 1 1 calc R . . H34B H 0.1571 0.6843 0.4143 0.052 Uiso 1 1 calc R . . C35 C 0.3915(5) 0.7468(2) 0.4614(3) 0.0607(17) Uani 1 1 d . . . H35A H 0.3464 0.7612 0.4903 0.091 Uiso 1 1 calc R . . H35B H 0.3945 0.7725 0.4304 0.091 Uiso 1 1 calc R . . H35C H 0.4725 0.7385 0.4807 0.091 Uiso 1 1 calc R . . C36 C 0.3269(5) 0.6591(3) 0.4820(2) 0.0574(16) Uani 1 1 d . . . H36A H 0.2673 0.6323 0.4665 0.069 Uiso 1 1 calc R . . H36B H 0.3001 0.6760 0.5160 0.069 Uiso 1 1 calc R . . C37 C 0.4441(6) 0.6331(2) 0.5018(3) 0.0566(15) Uani 1 1 d . . . H37A H 0.5032 0.6597 0.5185 0.068 Uiso 1 1 calc R . . H37B H 0.4360 0.6077 0.5332 0.068 Uiso 1 1 calc R . . C38 C 0.6176(5) 0.5969(2) 0.4698(3) 0.0554(15) Uani 1 1 d . . . H38A H 0.6335 0.5751 0.5050 0.083 Uiso 1 1 calc R . . H38B H 0.6583 0.6305 0.4774 0.083 Uiso 1 1 calc R . . H38C H 0.6469 0.5791 0.4375 0.083 Uiso 1 1 calc R . . C39 C 0.4285(5) 0.5547(2) 0.4427(3) 0.0507(14) Uani 1 1 d . . . H39A H 0.4376 0.5348 0.4793 0.076 Uiso 1 1 calc R . . H39B H 0.4649 0.5354 0.4137 0.076 Uiso 1 1 calc R . . H39C H 0.3438 0.5601 0.4278 0.076 Uiso 1 1 calc R . . C40 C 0.6701(5) 0.7289(2) 0.3940(2) 0.0437(13) Uani 1 1 d . . . C41 C 0.7750(5) 0.7628(3) 0.4056(3) 0.0673(18) Uani 1 1 d . . . H41A H 0.7536 0.7982 0.3915 0.101 Uiso 1 1 calc R . . H41B H 0.8373 0.7490 0.3854 0.101 Uiso 1 1 calc R . . H41C H 0.8043 0.7639 0.4479 0.101 Uiso 1 1 calc R . . N13 N 0.1337(5) 0.6366(2) 0.5933(3) 0.085(2) Uani 1 1 d . . . C42 C 0.0362(6) 0.6298(2) 0.5777(3) 0.0553(15) Uani 1 1 d . . . C43 C -0.0870(5) 0.6200(3) 0.5571(4) 0.077(2) Uani 1 1 d . . . H43A H -0.1103 0.5872 0.5739 0.115 Uiso 1 1 calc R . . H43B H -0.1007 0.6173 0.5143 0.115 Uiso 1 1 calc R . . H43C H -0.1346 0.6488 0.5690 0.115 Uiso 1 1 calc R . . N14 N -0.0655(9) 0.3706(5) 0.1248(5) 0.159(5) Uani 1 1 d . . . C44 C -0.0440(8) 0.3748(4) 0.0800(6) 0.103(3) Uani 1 1 d . . . C45 C -0.0067(7) 0.3867(4) 0.0229(5) 0.113(3) Uani 1 1 d . . . H45A H -0.0429 0.3614 -0.0065 0.169 Uiso 1 1 calc R . . H45B H 0.0800 0.3846 0.0271 0.169 Uiso 1 1 calc R . . H45C H -0.0328 0.4221 0.0105 0.169 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 0.0258(3) 0.0232(3) 0.0422(4) -0.0014(2) -0.0029(2) -0.0007(2) Cu2 0.0281(3) 0.0339(3) 0.0405(4) 0.0013(3) 0.0046(3) -0.0071(2) Cu3 0.0265(3) 0.0272(3) 0.0382(3) -0.0019(2) 0.0023(2) 0.0037(2) N1 0.032(2) 0.0196(18) 0.036(2) 0.0000(16) 0.0000(17) 0.0016(15) N2 0.0239(19) 0.0227(18) 0.043(2) -0.0031(17) 0.0019(17) 0.0015(15) N3 0.029(2) 0.027(2) 0.052(3) 0.0014(18) 0.0039(19) -0.0035(16) N4 0.034(2) 0.031(2) 0.047(3) -0.0032(19) -0.008(2) 0.0002(17) N5 0.031(2) 0.0255(19) 0.030(2) 0.0016(16) 0.0039(17) -0.0051(15) N6 0.042(2) 0.042(2) 0.040(3) 0.0023(19) 0.004(2) -0.0142(19) N7 0.041(2) 0.036(2) 0.048(3) -0.0029(19) 0.007(2) -0.0118(19) N8 0.028(2) 0.045(3) 0.065(3) 0.009(2) 0.009(2) -0.005(2) N9 0.0245(19) 0.0243(18) 0.031(2) 0.0030(16) 0.0049(16) 0.0010(15) N10 0.044(3) 0.042(2) 0.038(2) -0.0036(19) 0.006(2) 0.0126(19) N11 0.041(2) 0.033(2) 0.043(3) 0.0038(19) -0.0031(19) 0.0114(18) N12 0.033(2) 0.036(2) 0.049(3) -0.0061(19) 0.004(2) -0.0012(19) Cu4 0.0475(4) 0.0481(4) 0.0626(5) 0.0014(3) 0.0076(3) 0.0007(3) Cu5 0.0445(4) 0.0534(4) 0.0684(5) 0.0123(4) 0.0175(3) 0.0102(3) Cu6 0.0663(5) 0.0872(6) 0.0548(5) -0.0049(4) 0.0022(4) -0.0273(4) Cl1 0.1135(18) 0.0992(16) 0.126(2) 0.0232(14) 0.0559(15) -0.0167(13) Cl2 0.0652(11) 0.0792(12) 0.0925(13) 0.0081(10) 0.0254(10) -0.0131(9) Cl3 0.0590(10) 0.0614(10) 0.1258(17) 0.0051(10) 0.0281(10) 0.0181(8) Cl4 0.153(2) 0.1104(18) 0.163(2) 0.0492(17) 0.098(2) 0.0816(17) Cl5 0.0940(14) 0.1057(15) 0.0475(10) 0.0018(9) -0.0028(9) -0.0080(11) Cl6 0.0825(13) 0.0840(13) 0.0976(15) -0.0071(11) -0.0058(11) -0.0211(10) C1 0.025(2) 0.027(2) 0.037(3) -0.001(2) 0.0000(19) 0.0015(18) C2 0.024(2) 0.022(2) 0.030(3) 0.0017(18) 0.0021(18) 0.0002(17) C3 0.029(2) 0.022(2) 0.036(3) 0.0006(19) -0.004(2) -0.0005(18) C4 0.024(2) 0.026(2) 0.036(3) -0.0012(19) -0.0062(19) 0.0021(19) C5 0.019(2) 0.028(2) 0.047(3) -0.001(2) -0.001(2) -0.0021(18) C6 0.029(3) 0.039(3) 0.069(4) 0.002(3) 0.004(3) -0.005(2) C7 0.030(3) 0.031(3) 0.050(3) 0.000(2) 0.009(2) 0.000(2) C8 0.026(2) 0.024(2) 0.044(3) -0.001(2) 0.000(2) -0.0011(18) C9 0.032(3) 0.028(2) 0.049(3) 0.003(2) -0.003(2) 0.006(2) C10 0.036(3) 0.026(2) 0.053(3) -0.009(2) 0.011(2) -0.002(2) C11 0.033(3) 0.034(3) 0.057(3) -0.003(2) 0.010(2) 0.002(2) C12 0.043(3) 0.055(3) 0.053(4) 0.005(3) 0.011(3) 0.002(3) C13 0.029(3) 0.048(3) 0.076(4) 0.002(3) 0.008(3) -0.010(2) C14 0.037(3) 0.029(2) 0.044(3) -0.003(2) 0.001(2) 0.001(2) C15 0.041(3) 0.060(4) 0.057(4) -0.009(3) -0.012(3) -0.002(3) C16 0.025(2) 0.022(2) 0.042(3) 0.0029(19) 0.006(2) 0.0026(17) C17 0.029(3) 0.033(3) 0.044(3) 0.004(2) 0.000(2) -0.006(2) C18 0.044(3) 0.047(3) 0.038(3) -0.003(2) 0.003(2) -0.016(2) C19 0.068(4) 0.093(5) 0.040(4) -0.002(3) -0.006(3) -0.032(4) C20 0.060(4) 0.042(3) 0.053(4) -0.012(3) 0.019(3) -0.012(3) C21 0.053(3) 0.053(3) 0.040(3) 0.006(3) 0.007(3) -0.014(3) C22 0.052(3) 0.068(4) 0.045(3) 0.002(3) 0.023(3) -0.021(3) C23 0.060(4) 0.042(3) 0.050(3) 0.011(3) 0.011(3) -0.014(3) C24 0.056(3) 0.035(3) 0.057(4) 0.000(3) 0.014(3) -0.017(2) C25 0.060(4) 0.039(3) 0.072(4) -0.012(3) 0.016(3) -0.011(3) C26 0.052(4) 0.058(4) 0.058(4) -0.006(3) 0.002(3) -0.024(3) C27 0.041(3) 0.051(3) 0.083(5) 0.019(3) 0.015(3) -0.009(3) C28 0.037(4) 0.081(5) 0.161(8) 0.035(5) 0.028(4) 0.010(3) C29 0.027(2) 0.023(2) 0.040(3) 0.0017(19) 0.003(2) -0.0037(18) C30 0.027(2) 0.036(3) 0.041(3) 0.005(2) 0.003(2) 0.002(2) C31 0.029(3) 0.032(3) 0.052(3) 0.006(2) 0.005(2) 0.011(2) C32 0.045(3) 0.032(3) 0.059(4) 0.008(2) 0.009(3) 0.009(2) C33 0.034(3) 0.053(3) 0.070(4) -0.001(3) 0.002(3) 0.018(2) C34 0.035(3) 0.043(3) 0.052(3) 0.001(2) 0.007(2) 0.016(2) C35 0.050(4) 0.060(4) 0.068(4) -0.030(3) 0.001(3) 0.016(3) C36 0.056(4) 0.079(4) 0.041(3) 0.011(3) 0.018(3) 0.023(3) C37 0.066(4) 0.061(4) 0.042(3) 0.007(3) 0.007(3) 0.018(3) C38 0.045(3) 0.057(4) 0.058(4) 0.007(3) -0.011(3) 0.009(3) C39 0.060(4) 0.035(3) 0.053(4) 0.014(2) -0.006(3) 0.002(2) C40 0.038(3) 0.041(3) 0.051(3) -0.007(2) 0.003(2) 0.005(2) C41 0.049(4) 0.072(4) 0.080(5) -0.021(4) 0.009(3) -0.024(3) N13 0.047(3) 0.061(4) 0.136(6) -0.005(3) -0.020(4) -0.003(3) C42 0.053(4) 0.038(3) 0.071(4) 0.002(3) 0.001(3) 0.003(3) C43 0.035(3) 0.085(5) 0.111(6) -0.009(4) 0.015(4) -0.004(3) N14 0.102(7) 0.252(14) 0.125(8) 0.027(9) 0.024(7) 0.020(7) C44 0.060(5) 0.112(7) 0.127(9) -0.025(7) -0.012(6) -0.005(5) C45 0.064(5) 0.100(7) 0.160(10) -0.029(7) -0.024(6) 0.001(5) _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 N4 1.931(4) . ? Cu1 N1 1.990(4) . ? Cu1 N3 2.163(4) . ? Cu1 N2 2.214(4) . ? Cu2 N8 1.930(4) . ? Cu2 N5 1.977(4) . ? Cu2 N7 2.155(4) . ? Cu2 N6 2.197(4) . ? Cu3 N12 1.925(4) . ? Cu3 N9 1.972(4) . ? Cu3 N11 2.161(4) . ? Cu3 N10 2.224(4) . ? N1 C4 1.273(6) . ? N1 C3 1.478(6) . ? N2 C10 1.477(6) . ? N2 C8 1.482(5) . ? N2 C9 1.489(6) . ? N3 C12 1.465(7) . ? N3 C11 1.486(6) . ? N3 C13 1.495(6) . ? N4 C14 1.129(6) . ? N5 C17 1.264(6) . ? N5 C16 1.474(6) . ? N6 C21 1.480(7) . ? N6 C23 1.483(7) . ? N6 C22 1.491(7) . ? N7 C25 1.467(7) . ? N7 C26 1.473(7) . ? N7 C24 1.481(7) . ? N8 C27 1.141(7) . ? N9 C30 1.278(6) . ? N9 C29 1.484(5) . ? N10 C35 1.466(7) . ? N10 C34 1.482(6) . ? N10 C36 1.487(7) . ? N11 C37 1.468(7) . ? N11 C39 1.471(6) . ? N11 C38 1.487(7) . ? N12 C40 1.133(6) . ? Cu4 Cl2 2.0785(18) . ? Cu4 Cl1 2.083(2) . ? Cu5 Cl3 2.0616(17) . ? Cu5 Cl4 2.066(2) . ? Cu6 Cl5 2.077(2) . ? Cu6 Cl6 2.101(2) . ? C1 C2 1.533(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C29 1.530(6) . ? C2 C3 1.539(6) . ? C2 C16 1.548(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.501(6) . ? C4 H4A 0.9500 . ? C5 C7 1.538(7) . ? C5 C6 1.541(6) . ? C5 C8 1.551(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.514(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.471(7) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15 H15D 0.9800 . ? C15 H15E 0.9800 . ? C15 H15F 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.502(7) . ? C17 H17A 0.9500 . ? C18 C20 1.529(8) . ? C18 C19 1.546(7) . ? C18 C21 1.559(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.515(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.472(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.512(7) . ? C30 H30A 0.9500 . ? C31 C32 1.534(7) . ? C31 C34 1.536(7) . ? C31 C33 1.544(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.496(8) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.465(8) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? N13 C42 1.125(7) . ? C42 C43 1.430(8) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N14 C44 1.111(13) . ? C44 C45 1.485(15) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? 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 N4 Cu1 N1 133.47(16) . . ? N4 Cu1 N3 102.56(17) . . ? N1 Cu1 N3 116.41(16) . . ? N4 Cu1 N2 112.26(15) . . ? N1 Cu1 N2 95.82(14) . . ? N3 Cu1 N2 85.57(14) . . ? N8 Cu2 N5 135.71(16) . . ? N8 Cu2 N7 106.54(18) . . ? N5 Cu2 N7 112.81(16) . . ? N8 Cu2 N6 106.91(18) . . ? N5 Cu2 N6 95.56(15) . . ? N7 Cu2 N6 85.96(16) . . ? N12 Cu3 N9 137.82(17) . . ? N12 Cu3 N11 105.89(17) . . ? N9 Cu3 N11 111.81(15) . . ? N12 Cu3 N10 106.09(17) . . ? N9 Cu3 N10 95.78(15) . . ? N11 Cu3 N10 84.60(16) . . ? C4 N1 C3 116.3(4) . . ? C4 N1 Cu1 119.7(3) . . ? C3 N1 Cu1 122.5(3) . . ? C10 N2 C8 111.2(4) . . ? C10 N2 C9 109.6(4) . . ? C8 N2 C9 109.4(4) . . ? C10 N2 Cu1 101.6(3) . . ? C8 N2 Cu1 113.2(2) . . ? C9 N2 Cu1 111.6(3) . . ? C12 N3 C11 110.7(4) . . ? C12 N3 C13 108.6(4) . . ? C11 N3 C13 108.6(4) . . ? C12 N3 Cu1 113.9(3) . . ? C11 N3 Cu1 102.0(3) . . ? C13 N3 Cu1 112.8(3) . . ? C14 N4 Cu1 167.8(4) . . ? C17 N5 C16 116.3(4) . . ? C17 N5 Cu2 121.0(3) . . ? C16 N5 Cu2 121.7(3) . . ? C21 N6 C23 110.8(4) . . ? C21 N6 C22 109.8(4) . . ? C23 N6 C22 110.5(4) . . ? C21 N6 Cu2 113.7(3) . . ? C23 N6 Cu2 102.0(3) . . ? C22 N6 Cu2 110.0(3) . . ? C25 N7 C26 108.6(5) . . ? C25 N7 C24 110.7(4) . . ? C26 N7 C24 109.5(4) . . ? C25 N7 Cu2 115.9(3) . . ? C26 N7 Cu2 110.8(3) . . ? C24 N7 Cu2 101.0(3) . . ? C27 N8 Cu2 171.0(5) . . ? C30 N9 C29 116.5(4) . . ? C30 N9 Cu3 119.8(3) . . ? C29 N9 Cu3 122.6(3) . . ? C35 N10 C34 110.7(4) . . ? C35 N10 C36 110.9(5) . . ? C34 N10 C36 110.6(4) . . ? C35 N10 Cu3 109.4(3) . . ? C34 N10 Cu3 113.1(3) . . ? C36 N10 Cu3 101.7(3) . . ? C37 N11 C39 110.6(5) . . ? C37 N11 C38 109.4(4) . . ? C39 N11 C38 108.4(4) . . ? C37 N11 Cu3 103.8(3) . . ? C39 N11 Cu3 113.8(3) . . ? C38 N11 Cu3 110.8(3) . . ? C40 N12 Cu3 172.2(5) . . ? Cl2 Cu4 Cl1 178.64(10) . . ? Cl3 Cu5 Cl4 176.93(9) . . ? Cl5 Cu6 Cl6 177.95(9) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C29 C2 C1 111.8(4) . . ? C29 C2 C3 107.9(3) . . ? C1 C2 C3 111.2(3) . . ? C29 C2 C16 106.9(3) . . ? C1 C2 C16 112.4(3) . . ? C3 C2 C16 106.5(4) . . ? N1 C3 C2 114.1(4) . . ? N1 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? N1 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? N1 C4 C5 125.3(4) . . ? N1 C4 H4A 117.4 . . ? C5 C4 H4A 117.4 . . ? C4 C5 C7 110.6(4) . . ? C4 C5 C6 108.4(4) . . ? C7 C5 C6 108.8(4) . . ? C4 C5 C8 109.6(4) . . ? C7 C5 C8 112.5(4) . . ? C6 C5 C8 106.8(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C5 115.2(3) . . ? N2 C8 H8A 108.5 . . ? C5 C8 H8A 108.5 . . ? N2 C8 H8B 108.5 . . ? C5 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 111.9(4) . . ? N2 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? N2 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? N3 C11 C10 111.2(4) . . ? N3 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? N3 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? N3 C12 H12A 109.5 . . ? N3 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N3 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 179.0(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C15 H15D 109.5 . . ? H15A C15 H15D 141.1 . . ? H15B C15 H15D 56.3 . . ? H15C C15 H15D 56.3 . . ? C14 C15 H15E 109.5 . . ? H15A C15 H15E 56.3 . . ? H15B C15 H15E 141.1 . . ? H15C C15 H15E 56.3 . . ? H15D C15 H15E 109.5 . . ? C14 C15 H15F 109.5 . . ? H15A C15 H15F 56.3 . . ? H15B C15 H15F 56.3 . . ? H15C C15 H15F 141.1 . . ? H15D C15 H15F 109.5 . . ? H15E C15 H15F 109.5 . . ? N5 C16 C2 113.8(3) . . ? N5 C16 H16A 108.8 . . ? C2 C16 H16A 108.8 . . ? N5 C16 H16B 108.8 . . ? C2 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? N5 C17 C18 124.0(4) . . ? N5 C17 H17A 118.0 . . ? C18 C17 H17A 118.0 . . ? C17 C18 C20 110.5(4) . . ? C17 C18 C19 109.2(5) . . ? C20 C18 C19 109.1(5) . . ? C17 C18 C21 110.4(4) . . ? C20 C18 C21 112.4(4) . . ? C19 C18 C21 105.0(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N6 C21 C18 115.5(4) . . ? N6 C21 H21A 108.4 . . ? C18 C21 H21A 108.4 . . ? N6 C21 H21B 108.4 . . ? C18 C21 H21B 108.4 . . ? H21A C21 H21B 107.5 . . ? N6 C22 H22A 109.5 . . ? N6 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N6 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N6 C23 C24 110.9(4) . . ? N6 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? N6 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.0 . . ? N7 C24 C23 111.6(4) . . ? N7 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? N7 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? N7 C25 H25A 109.5 . . ? N7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N7 C26 H26A 109.5 . . ? N7 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N7 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N8 C27 C28 178.3(8) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N9 C29 C2 114.0(3) . . ? N9 C29 H29A 108.8 . . ? C2 C29 H29A 108.8 . . ? N9 C29 H29B 108.8 . . ? C2 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N9 C30 C31 124.3(4) . . ? N9 C30 H30A 117.8 . . ? C31 C30 H30A 117.8 . . ? C30 C31 C32 109.7(4) . . ? C30 C31 C34 110.9(4) . . ? C32 C31 C34 112.7(4) . . ? C30 C31 C33 108.2(4) . . ? C32 C31 C33 109.0(4) . . ? C34 C31 C33 106.1(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N10 C34 C31 116.2(4) . . ? N10 C34 H34A 108.2 . . ? C31 C34 H34A 108.2 . . ? N10 C34 H34B 108.2 . . ? C31 C34 H34B 108.2 . . ? H34A C34 H34B 107.4 . . ? N10 C35 H35A 109.5 . . ? N10 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N10 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N10 C36 C37 112.2(5) . . ? N10 C36 H36A 109.2 . . ? C37 C36 H36A 109.2 . . ? N10 C36 H36B 109.2 . . ? C37 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N11 C37 C36 112.0(5) . . ? N11 C37 H37A 109.2 . . ? C36 C37 H37A 109.2 . . ? N11 C37 H37B 109.2 . . ? C36 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? N11 C38 H38A 109.5 . . ? N11 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N11 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N11 C39 H39A 109.5 . . ? N11 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N11 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N12 C40 C41 179.5(6) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N13 C42 C43 178.5(8) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N14 C44 C45 172.5(13) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 N1 C4 -103.5(4) . . . . ? N3 Cu1 N1 C4 112.8(4) . . . . ? N2 Cu1 N1 C4 24.9(4) . . . . ? N4 Cu1 N1 C3 91.2(4) . . . . ? N3 Cu1 N1 C3 -52.5(4) . . . . ? N2 Cu1 N1 C3 -140.4(3) . . . . ? N4 Cu1 N2 C10 -113.8(3) . . . . ? N1 Cu1 N2 C10 104.1(3) . . . . ? N3 Cu1 N2 C10 -12.0(3) . . . . ? N4 Cu1 N2 C8 126.9(3) . . . . ? N1 Cu1 N2 C8 -15.1(3) . . . . ? N3 Cu1 N2 C8 -131.3(3) . . . . ? N4 Cu1 N2 C9 3.0(3) . . . . ? N1 Cu1 N2 C9 -139.1(3) . . . . ? N3 Cu1 N2 C9 104.7(3) . . . . ? N4 Cu1 N3 C12 -146.1(3) . . . . ? N1 Cu1 N3 C12 7.8(4) . . . . ? N2 Cu1 N3 C12 102.1(3) . . . . ? N4 Cu1 N3 C11 94.6(3) . . . . ? N1 Cu1 N3 C11 -111.5(3) . . . . ? N2 Cu1 N3 C11 -17.2(3) . . . . ? N4 Cu1 N3 C13 -21.6(3) . . . . ? N1 Cu1 N3 C13 132.2(3) . . . . ? N2 Cu1 N3 C13 -133.5(3) . . . . ? N1 Cu1 N4 C14 -144.4(18) . . . . ? N3 Cu1 N4 C14 2.7(19) . . . . ? N2 Cu1 N4 C14 93.0(19) . . . . ? N8 Cu2 N5 C17 -95.7(4) . . . . ? N7 Cu2 N5 C17 113.5(4) . . . . ? N6 Cu2 N5 C17 25.6(4) . . . . ? N8 Cu2 N5 C16 96.2(4) . . . . ? N7 Cu2 N5 C16 -54.6(3) . . . . ? N6 Cu2 N5 C16 -142.6(3) . . . . ? N8 Cu2 N6 C21 124.0(4) . . . . ? N5 Cu2 N6 C21 -17.4(4) . . . . ? N7 Cu2 N6 C21 -129.9(4) . . . . ? N8 Cu2 N6 C23 -116.7(3) . . . . ? N5 Cu2 N6 C23 101.9(3) . . . . ? N7 Cu2 N6 C23 -10.6(3) . . . . ? N8 Cu2 N6 C22 0.5(4) . . . . ? N5 Cu2 N6 C22 -140.9(3) . . . . ? N7 Cu2 N6 C22 106.6(3) . . . . ? N8 Cu2 N7 C25 -152.7(4) . . . . ? N5 Cu2 N7 C25 6.5(4) . . . . ? N6 Cu2 N7 C25 100.8(4) . . . . ? N8 Cu2 N7 C26 -28.4(4) . . . . ? N5 Cu2 N7 C26 130.8(3) . . . . ? N6 Cu2 N7 C26 -134.8(4) . . . . ? N8 Cu2 N7 C24 87.6(3) . . . . ? N5 Cu2 N7 C24 -113.2(3) . . . . ? N6 Cu2 N7 C24 -18.8(3) . . . . ? N5 Cu2 N8 C27 140(3) . . . . ? N7 Cu2 N8 C27 -68(3) . . . . ? N6 Cu2 N8 C27 23(3) . . . . ? N12 Cu3 N9 C30 -96.3(4) . . . . ? N11 Cu3 N9 C30 112.0(3) . . . . ? N10 Cu3 N9 C30 25.5(4) . . . . ? N12 Cu3 N9 C29 96.4(4) . . . . ? N11 Cu3 N9 C29 -55.4(3) . . . . ? N10 Cu3 N9 C29 -141.9(3) . . . . ? N12 Cu3 N10 C35 -0.8(4) . . . . ? N9 Cu3 N10 C35 -144.3(4) . . . . ? N11 Cu3 N10 C35 104.2(4) . . . . ? N12 Cu3 N10 C34 123.2(3) . . . . ? N9 Cu3 N10 C34 -20.4(4) . . . . ? N11 Cu3 N10 C34 -131.8(4) . . . . ? N12 Cu3 N10 C36 -118.1(4) . . . . ? N9 Cu3 N10 C36 98.3(3) . . . . ? N11 Cu3 N10 C36 -13.1(3) . . . . ? N12 Cu3 N11 C37 90.2(4) . . . . ? N9 Cu3 N11 C37 -109.1(3) . . . . ? N10 Cu3 N11 C37 -15.0(3) . . . . ? N12 Cu3 N11 C39 -149.5(4) . . . . ? N9 Cu3 N11 C39 11.2(4) . . . . ? N10 Cu3 N11 C39 105.3(4) . . . . ? N12 Cu3 N11 C38 -27.0(4) . . . . ? N9 Cu3 N11 C38 133.7(3) . . . . ? N10 Cu3 N11 C38 -132.3(4) . . . . ? N9 Cu3 N12 C40 163(3) . . . . ? N11 Cu3 N12 C40 -45(3) . . . . ? N10 Cu3 N12 C40 44(3) . . . . ? C4 N1 C3 C2 117.9(4) . . . . ? Cu1 N1 C3 C2 -76.3(4) . . . . ? C29 C2 C3 N1 -57.4(5) . . . . ? C1 C2 C3 N1 65.5(5) . . . . ? C16 C2 C3 N1 -171.8(4) . . . . ? C3 N1 C4 C5 177.8(4) . . . . ? Cu1 N1 C4 C5 11.6(6) . . . . ? N1 C4 C5 C7 58.8(6) . . . . ? N1 C4 C5 C6 178.0(5) . . . . ? N1 C4 C5 C8 -65.8(6) . . . . ? C10 N2 C8 C5 -140.5(4) . . . . ? C9 N2 C8 C5 98.3(4) . . . . ? Cu1 N2 C8 C5 -26.9(5) . . . . ? C4 C5 C8 N2 70.6(5) . . . . ? C7 C5 C8 N2 -52.9(5) . . . . ? C6 C5 C8 N2 -172.2(4) . . . . ? C8 N2 C10 C11 161.1(4) . . . . ? C9 N2 C10 C11 -77.8(5) . . . . ? Cu1 N2 C10 C11 40.4(4) . . . . ? C12 N3 C11 C10 -76.7(5) . . . . ? C13 N3 C11 C10 164.1(4) . . . . ? Cu1 N3 C11 C10 44.8(5) . . . . ? N2 C10 C11 N3 -62.8(6) . . . . ? Cu1 N4 C14 C15 57(39) . . . . ? C17 N5 C16 C2 121.2(4) . . . . ? Cu2 N5 C16 C2 -70.1(4) . . . . ? C29 C2 C16 N5 -171.0(3) . . . . ? C1 C2 C16 N5 66.1(5) . . . . ? C3 C2 C16 N5 -55.9(5) . . . . ? C16 N5 C17 C18 -179.6(4) . . . . ? Cu2 N5 C17 C18 11.6(6) . . . . ? N5 C17 C18 C20 59.8(6) . . . . ? N5 C17 C18 C19 179.8(5) . . . . ? N5 C17 C18 C21 -65.2(6) . . . . ? C23 N6 C21 C18 -137.5(5) . . . . ? C22 N6 C21 C18 100.3(5) . . . . ? Cu2 N6 C21 C18 -23.4(6) . . . . ? C17 C18 C21 N6 68.0(6) . . . . ? C20 C18 C21 N6 -55.9(6) . . . . ? C19 C18 C21 N6 -174.4(5) . . . . ? C21 N6 C23 C24 160.4(4) . . . . ? C22 N6 C23 C24 -77.7(5) . . . . ? Cu2 N6 C23 C24 39.1(5) . . . . ? C25 N7 C24 C23 -76.4(6) . . . . ? C26 N7 C24 C23 163.8(5) . . . . ? Cu2 N7 C24 C23 46.9(5) . . . . ? N6 C23 C24 N7 -63.4(6) . . . . ? Cu2 N8 C27 C28 -91(24) . . . . ? C30 N9 C29 C2 122.2(4) . . . . ? Cu3 N9 C29 C2 -70.1(4) . . . . ? C1 C2 C29 N9 64.2(5) . . . . ? C3 C2 C29 N9 -173.3(3) . . . . ? C16 C2 C29 N9 -59.1(5) . . . . ? C29 N9 C30 C31 -178.7(4) . . . . ? Cu3 N9 C30 C31 13.2(6) . . . . ? N9 C30 C31 C32 58.1(6) . . . . ? N9 C30 C31 C34 -67.1(6) . . . . ? N9 C30 C31 C33 176.9(5) . . . . ? C35 N10 C34 C31 103.2(5) . . . . ? C36 N10 C34 C31 -133.4(5) . . . . ? Cu3 N10 C34 C31 -20.1(5) . . . . ? C30 C31 C34 N10 66.3(6) . . . . ? C32 C31 C34 N10 -57.1(6) . . . . ? C33 C31 C34 N10 -176.4(4) . . . . ? C35 N10 C36 C37 -75.9(6) . . . . ? C34 N10 C36 C37 160.8(5) . . . . ? Cu3 N10 C36 C37 40.4(6) . . . . ? C39 N11 C37 C36 -80.0(6) . . . . ? C38 N11 C37 C36 160.7(5) . . . . ? Cu3 N11 C37 C36 42.4(6) . . . . ? N10 C36 C37 N11 -60.6(7) . . . . ? Cu3 N12 C40 C41 -64(95) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.924 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.094 #===END data_04305a _database_code_depnum_ccdc_archive 'CCDC 644163' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '04305-complex 19' _chemical_melting_point ? _chemical_formula_moiety 'C18 H36 Cu N4, F6 P' _chemical_formula_sum 'C18 H36 Cu F6 N4 P' _chemical_formula_weight 517.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 13.5564(5) _cell_length_b 13.5564(5) _cell_length_c 13.5564(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2491.34(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2635 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6356 _exptl_absorpt_correction_T_max 0.6356 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1472 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 1 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1472 _reflns_number_gt 1340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.0374P)^2^+0.6413P] 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_abs_structure_details 'Flack H D (1983), 636 Friedel Pairs, Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 1472 _refine_ls_number_parameters 118 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.022 _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 0.49991(1) 0.49991(1) 0.49991(1) 0.0253(1) Uani 1 3 d S . . N1 N 0.40514(11) 0.40514(11) 0.40514(11) 0.0309(6) Uani 1 3 d S . . C1 C 0.46378(15) 0.31545(14) 0.39280(15) 0.0359(4) Uani 1 1 d . . . H1A H 0.5100 0.3243 0.3370 0.043 Uiso 1 1 calc R . . H1B H 0.4195 0.2597 0.3767 0.043 Uiso 1 1 calc R . . C2 C 0.52223(15) 0.29096(13) 0.48624(15) 0.0370(4) Uani 1 1 d . . . H2A H 0.4764 0.2698 0.5390 0.044 Uiso 1 1 calc R . . H2B H 0.5682 0.2359 0.4727 0.044 Uiso 1 1 calc R . . N2 N 0.57831(11) 0.37819(11) 0.51924(11) 0.0304(3) Uani 1 1 d . . . C3 C 0.66641(15) 0.36798(15) 0.54836(16) 0.0383(5) Uani 1 1 d . . . H3A H 0.6961 0.3047 0.5441 0.046 Uiso 1 1 calc R . . C4 C 0.72522(15) 0.45116(15) 0.58897(18) 0.0436(5) Uani 1 1 d . . . H4A H 0.6856 0.5130 0.5822 0.052 Uiso 1 1 calc R . . C5 C 0.82141(19) 0.4642(2) 0.5320(2) 0.0675(8) Uani 1 1 d . . . H5A H 0.8594 0.5185 0.5609 0.101 Uiso 1 1 calc R . . H5B H 0.8066 0.4793 0.4629 0.101 Uiso 1 1 calc R . . H5C H 0.8600 0.4032 0.5356 0.101 Uiso 1 1 calc R . . C6 C 0.74440(19) 0.43304(19) 0.69862(19) 0.0589(7) Uani 1 1 d . . . H6A H 0.7805 0.4892 0.7264 0.088 Uiso 1 1 calc R . . H6B H 0.7836 0.3728 0.7066 0.088 Uiso 1 1 calc R . . H6C H 0.6814 0.4255 0.7332 0.088 Uiso 1 1 calc R . . P1 P 0.2480(2) 0.2547(2) 0.7464(2) 0.0405(7) Uani 0.33333 1 d PD A -1 F1 F 0.3179(5) 0.1855(7) 0.8093(8) 0.0632(9) Uani 0.33333 1 d PD A -1 F6 F 0.1773(5) 0.3252(6) 0.6842(7) 0.0632(9) Uani 0.33333 1 d PD A -1 F2 F 0.255(2) 0.1811(9) 0.6556(5) 0.075(3) Uani 0.33333 1 d PD A -1 F3 F 0.1547(4) 0.1962(12) 0.7857(16) 0.072(2) Uani 0.33333 1 d PD A -1 F5 F 0.241(2) 0.3293(8) 0.8363(6) 0.075(3) Uani 0.33333 1 d PD A -1 F4 F 0.3414(4) 0.3127(13) 0.7053(17) 0.072(2) Uani 0.33333 1 d PD A -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 0.02530(13) 0.02530(13) 0.02530(13) -0.00064(8) -0.00064(8) -0.00064(8) N1 0.0309(6) 0.0309(6) 0.0309(6) -0.0039(6) -0.0039(6) -0.0039(6) C1 0.0405(11) 0.0293(10) 0.0380(11) -0.0078(8) -0.0018(9) -0.0041(8) C2 0.0412(10) 0.0260(9) 0.0437(11) -0.0026(8) -0.0012(9) -0.0002(8) N2 0.0327(8) 0.0275(8) 0.0309(8) 0.0003(6) -0.0006(7) 0.0012(6) C3 0.0375(11) 0.0305(10) 0.0468(12) 0.0024(9) -0.0022(9) 0.0079(9) C4 0.0350(11) 0.0353(11) 0.0604(13) 0.0030(10) -0.0109(10) 0.0062(9) C5 0.0478(14) 0.0610(15) 0.094(2) 0.0123(15) 0.0038(14) -0.0104(13) C6 0.0578(15) 0.0565(15) 0.0625(16) -0.0010(13) -0.0200(12) -0.0046(12) P1 0.044(6) 0.056(5) 0.022(4) 0.000(5) 0.009(4) 0.019(4) F1 0.064(9) 0.060(9) 0.065(5) 0.008(6) -0.003(6) 0.029(3) F6 0.064(9) 0.060(9) 0.065(5) 0.008(6) -0.003(6) 0.029(3) F2 0.127(8) 0.052(4) 0.045(3) -0.018(3) -0.008(5) 0.013(5) F3 0.056(3) 0.069(5) 0.093(7) 0.025(4) 0.007(5) 0.000(4) F5 0.127(8) 0.052(4) 0.045(3) -0.018(3) -0.008(5) 0.013(5) F4 0.056(3) 0.069(5) 0.093(7) 0.025(4) 0.007(5) 0.000(4) _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 N2 1.9802(15) . ? Cu1 N2 1.9802(15) 9 ? Cu1 N2 1.9803(15) 5 ? Cu1 N1 2.225(3) . ? N1 C1 1.462(2) . ? N1 C1 1.462(2) 9 ? N1 C1 1.462(2) 5 ? C1 C2 1.530(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.475(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N2 C3 1.265(3) . ? C3 C4 1.487(3) . ? C3 H3A 0.9500 . ? C4 C5 1.526(3) . ? C4 C6 1.529(3) . ? C4 H4A 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? P1 F1 1.584(2) . ? P1 F3 1.586(3) . ? P1 F5 1.586(3) . ? P1 F2 1.587(3) . ? P1 F4 1.590(3) . ? P1 F6 1.595(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 N2 Cu1 N2 119.111(14) . 9 ? N2 Cu1 N2 119.113(14) . 5 ? N2 Cu1 N2 119.111(14) 9 5 ? N2 Cu1 N1 84.56(4) . . ? N2 Cu1 N1 84.56(4) 9 . ? N2 Cu1 N1 84.56(4) 5 . ? C1 N1 C1 114.78(9) . 9 ? C1 N1 C1 114.78(9) . 5 ? C1 N1 C1 114.78(9) 9 5 ? C1 N1 Cu1 103.43(12) . . ? C1 N1 Cu1 103.43(12) 9 . ? C1 N1 Cu1 103.43(12) 5 . ? N1 C1 C2 111.54(16) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C1 110.12(15) . . ? N2 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.2 . . ? C3 N2 C2 119.56(16) . . ? C3 N2 Cu1 129.72(14) . . ? C2 N2 Cu1 110.56(11) . . ? N2 C3 C4 122.59(18) . . ? N2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? C3 C4 C5 111.0(2) . . ? C3 C4 C6 109.23(19) . . ? C5 C4 C6 111.4(2) . . ? C3 C4 H4A 108.3 . . ? C5 C4 H4A 108.3 . . ? C6 C4 H4A 108.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? F1 P1 F3 89.94(19) . . ? F1 P1 F5 90.03(19) . . ? F3 P1 F5 90.67(19) . . ? F1 P1 F2 90.61(19) . . ? F3 P1 F2 89.51(19) . . ? F5 P1 F2 179.34(18) . . ? F1 P1 F4 90.3(2) . . ? F3 P1 F4 179.1(2) . . ? F5 P1 F4 90.18(19) . . ? F2 P1 F4 89.65(19) . . ? F1 P1 F6 179.3(3) . . ? F3 P1 F6 89.88(19) . . ? F5 P1 F6 89.29(19) . . ? F2 P1 F6 90.07(19) . . ? F4 P1 F6 89.87(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 N1 C1 -11.89(9) . . . . ? N2 Cu1 N1 C1 -131.88(9) 9 . . . ? N2 Cu1 N1 C1 108.12(9) 5 . . . ? N2 Cu1 N1 C1 108.12(9) . . . 9 ? N2 Cu1 N1 C1 -11.88(9) 9 . . 9 ? N2 Cu1 N1 C1 -131.88(9) 5 . . 9 ? N2 Cu1 N1 C1 -131.88(9) . . . 5 ? N2 Cu1 N1 C1 108.12(9) 9 . . 5 ? N2 Cu1 N1 C1 -11.88(9) 5 . . 5 ? C1 N1 C1 C2 -76.4(3) 9 . . . ? C1 N1 C1 C2 147.39(19) 5 . . . ? Cu1 N1 C1 C2 35.48(15) . . . . ? N1 C1 C2 N2 -51.2(2) . . . . ? C1 C2 N2 C3 -137.4(2) . . . . ? C1 C2 N2 Cu1 38.41(18) . . . . ? N2 Cu1 N2 C3 -118.69(18) 9 . . . ? N2 Cu1 N2 C3 80.0(2) 5 . . . ? N1 Cu1 N2 C3 160.63(19) . . . . ? N2 Cu1 N2 C2 66.10(15) 9 . . . ? N2 Cu1 N2 C2 -95.25(12) 5 . . . ? N1 Cu1 N2 C2 -14.57(12) . . . . ? C2 N2 C3 C4 -175.78(19) . . . . ? Cu1 N2 C3 C4 9.4(3) . . . . ? N2 C3 C4 C5 -124.2(2) . . . . ? N2 C3 C4 C6 112.5(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.178 _refine_diff_density_min -0.550 _refine_diff_density_rms 0.045 #===END data_05006m _database_code_depnum_ccdc_archive 'CCDC 644164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '05006-complex 21' _chemical_melting_point ? _chemical_formula_moiety 'C27 H30 Cu N4, F6 P' _chemical_formula_sum 'C27 H30 Cu F6 N4 P' _chemical_formula_weight 619.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 10.4705(12) _cell_length_b 11.0935(13) _cell_length_c 12.0139(14) _cell_angle_alpha 83.962(2) _cell_angle_beta 84.970(2) _cell_angle_gamma 83.927(2) _cell_volume 1375.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3006 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 24.95 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 0.917 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6571 _exptl_absorpt_correction_T_max 0.8747 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13962 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0398 _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 -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4868 _reflns_number_gt 4170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _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^)+(0.0317P)^2^+0.6850P] 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 4868 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.22967(2) 0.24040(2) 0.73843(2) 0.02235(9) Uani 1 1 d . . . P1 P 0.54581(6) 0.69349(6) 0.74603(5) 0.02973(15) Uani 1 1 d . . . N3 N 0.23971(16) 0.36165(15) 0.60289(14) 0.0218(4) Uani 1 1 d . . . F6 F 0.59044(15) 0.77642(14) 0.63541(12) 0.0485(4) Uani 1 1 d . . . N2 N 0.25170(17) 0.07225(16) 0.68711(15) 0.0269(4) Uani 1 1 d . . . N1 N 0.25031(17) 0.26400(17) 0.89626(15) 0.0286(4) Uani 1 1 d . . . F2 F 0.69004(14) 0.67422(14) 0.78008(14) 0.0530(4) Uani 1 1 d . . . N4 N 0.44347(16) 0.22860(16) 0.71543(15) 0.0252(4) Uani 1 1 d . . . F3 F 0.50109(16) 0.61178(15) 0.85592(13) 0.0556(4) Uani 1 1 d . . . F5 F 0.52107(17) 0.81176(14) 0.81181(13) 0.0574(4) Uani 1 1 d . . . F4 F 0.57261(17) 0.57524(15) 0.67953(14) 0.0607(5) Uani 1 1 d . . . C22 C 0.05207(19) 0.34472(18) 0.50185(17) 0.0230(4) Uani 1 1 d . . . C21 C 0.1780(2) 0.38561(19) 0.51502(18) 0.0244(5) Uani 1 1 d . . . H21A H 0.2165 0.4336 0.4535 0.029 Uiso 1 1 calc R . . C3 C 0.1734(2) 0.2926(2) 0.97929(19) 0.0327(5) Uani 1 1 d . . . H3A H 0.2072 0.2896 1.0505 0.039 Uiso 1 1 calc R . . C20 C 0.3631(2) 0.4149(2) 0.60236(19) 0.0276(5) Uani 1 1 d . . . H20A H 0.3588 0.4679 0.6642 0.033 Uiso 1 1 calc R . . H20B H 0.3793 0.4655 0.5306 0.033 Uiso 1 1 calc R . . C19 C 0.4727(2) 0.3139(2) 0.61681(19) 0.0280(5) Uani 1 1 d . . . H19A H 0.4861 0.2693 0.5489 0.034 Uiso 1 1 calc R . . H19B H 0.5533 0.3500 0.6257 0.034 Uiso 1 1 calc R . . C24 C -0.1210(2) 0.3399(2) 0.38311(19) 0.0313(5) Uani 1 1 d . . . H24A H -0.1548 0.3569 0.3117 0.038 Uiso 1 1 calc R . . F1 F 0.40195(14) 0.71357(18) 0.70970(14) 0.0647(5) Uani 1 1 d . . . C10 C 0.4798(2) 0.1005(2) 0.6979(2) 0.0319(5) Uani 1 1 d . . . H10A H 0.4840 0.0513 0.7714 0.038 Uiso 1 1 calc R . . H10B H 0.5663 0.0919 0.6573 0.038 Uiso 1 1 calc R . . C25 C -0.1937(2) 0.2856(2) 0.4722(2) 0.0313(5) Uani 1 1 d . . . H25A H -0.2782 0.2667 0.4625 0.038 Uiso 1 1 calc R . . C23 C 0.0009(2) 0.36953(19) 0.39779(18) 0.0273(5) Uani 1 1 d . . . H23A H 0.0504 0.4072 0.3363 0.033 Uiso 1 1 calc R . . C12 C 0.1748(2) -0.0076(2) 0.6796(2) 0.0370(6) Uani 1 1 d . . . H12A H 0.2048 -0.0737 0.6369 0.044 Uiso 1 1 calc R . . C26 C -0.1435(2) 0.2588(2) 0.5756(2) 0.0318(5) Uani 1 1 d . . . H26A H -0.1929 0.2201 0.6366 0.038 Uiso 1 1 calc R . . C4 C 0.0354(2) 0.3301(2) 0.97199(18) 0.0317(5) Uani 1 1 d . . . C27 C -0.0218(2) 0.2883(2) 0.59018(18) 0.0281(5) Uani 1 1 d . . . H27A H 0.0121 0.2697 0.6615 0.034 Uiso 1 1 calc R . . C1 C 0.4784(2) 0.2665(2) 0.82150(19) 0.0323(5) Uani 1 1 d . . . H1A H 0.4762 0.3564 0.8155 0.039 Uiso 1 1 calc R . . H1B H 0.5673 0.2319 0.8354 0.039 Uiso 1 1 calc R . . C2 C 0.3861(2) 0.2241(2) 0.91973(19) 0.0373(6) Uani 1 1 d . . . H2A H 0.3978 0.1341 0.9331 0.045 Uiso 1 1 calc R . . H2B H 0.4061 0.2581 0.9885 0.045 Uiso 1 1 calc R . . C13 C 0.0431(2) -0.0041(2) 0.7325(2) 0.0355(6) Uani 1 1 d . . . C6 C -0.1460(2) 0.4164(2) 0.8710(2) 0.0406(6) Uani 1 1 d . . . H6A H -0.1797 0.4540 0.8036 0.049 Uiso 1 1 calc R . . C5 C -0.0154(2) 0.3849(2) 0.8743(2) 0.0342(5) Uani 1 1 d . . . H5A H 0.0405 0.4009 0.8090 0.041 Uiso 1 1 calc R . . C7 C -0.2282(2) 0.3932(2) 0.9657(2) 0.0438(6) Uani 1 1 d . . . H7A H -0.3182 0.4146 0.9633 0.053 Uiso 1 1 calc R . . C18 C -0.0476(2) -0.0623(2) 0.6848(3) 0.0442(7) Uani 1 1 d . . . H18A H -0.0236 -0.1021 0.6187 0.053 Uiso 1 1 calc R . . C9 C -0.0478(2) 0.3089(3) 1.0671(2) 0.0439(6) Uani 1 1 d . . . H9A H -0.0142 0.2734 1.1352 0.053 Uiso 1 1 calc R . . C11 C 0.3822(2) 0.0536(2) 0.6303(2) 0.0322(5) Uani 1 1 d . . . H11A H 0.3839 0.0975 0.5541 0.039 Uiso 1 1 calc R . . H11B H 0.4051 -0.0342 0.6226 0.039 Uiso 1 1 calc R . . C15 C -0.1185(2) 0.0527(3) 0.8779(2) 0.0468(7) Uani 1 1 d . . . H15A H -0.1435 0.0925 0.9437 0.056 Uiso 1 1 calc R . . C17 C -0.1723(3) -0.0623(2) 0.7334(3) 0.0507(8) Uani 1 1 d . . . H17A H -0.2341 -0.1011 0.7003 0.061 Uiso 1 1 calc R . . C16 C -0.2066(3) -0.0063(3) 0.8296(3) 0.0519(8) Uani 1 1 d . . . H16A H -0.2919 -0.0080 0.8635 0.062 Uiso 1 1 calc R . . C14 C 0.0069(2) 0.0532(2) 0.8292(2) 0.0391(6) Uani 1 1 d . . . H14A H 0.0681 0.0929 0.8623 0.047 Uiso 1 1 calc R . . C8 C -0.1790(3) 0.3390(3) 1.0634(2) 0.0494(7) Uani 1 1 d . . . H8A H -0.2354 0.3223 1.1283 0.059 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 0.01923(14) 0.02600(15) 0.02231(15) -0.00326(10) -0.00273(10) -0.00271(10) P1 0.0290(3) 0.0358(3) 0.0262(3) -0.0045(3) -0.0056(2) -0.0069(3) N3 0.0182(9) 0.0207(9) 0.0267(9) -0.0028(7) -0.0023(7) -0.0021(7) F6 0.0537(9) 0.0586(10) 0.0333(8) 0.0055(7) -0.0033(7) -0.0154(8) N2 0.0261(10) 0.0240(10) 0.0313(10) -0.0035(8) -0.0044(8) -0.0030(8) N1 0.0293(10) 0.0332(10) 0.0241(10) -0.0031(8) -0.0038(8) -0.0050(8) F2 0.0371(8) 0.0518(9) 0.0718(11) 0.0028(8) -0.0230(8) -0.0059(7) N4 0.0210(9) 0.0285(10) 0.0269(10) -0.0045(8) -0.0050(7) -0.0015(7) F3 0.0623(10) 0.0573(10) 0.0427(9) 0.0109(8) 0.0066(8) -0.0104(8) F5 0.0886(13) 0.0419(9) 0.0414(9) -0.0132(7) -0.0125(8) 0.0106(8) F4 0.0700(11) 0.0541(10) 0.0648(11) -0.0313(8) 0.0145(9) -0.0275(9) C22 0.0226(11) 0.0197(10) 0.0266(11) -0.0048(8) -0.0022(9) 0.0015(8) C21 0.0245(11) 0.0225(11) 0.0255(11) -0.0007(9) 0.0004(9) -0.0022(9) C3 0.0390(13) 0.0382(13) 0.0220(12) -0.0057(10) -0.0031(10) -0.0057(11) C20 0.0217(11) 0.0266(12) 0.0354(13) 0.0005(9) -0.0040(9) -0.0080(9) C19 0.0175(10) 0.0347(12) 0.0327(12) -0.0041(10) -0.0005(9) -0.0075(9) C24 0.0293(12) 0.0364(13) 0.0294(12) -0.0117(10) -0.0102(10) 0.0060(10) F1 0.0316(9) 0.1070(15) 0.0564(10) 0.0002(10) -0.0139(7) -0.0108(9) C10 0.0206(11) 0.0313(12) 0.0430(14) -0.0040(10) -0.0045(10) 0.0028(9) C25 0.0202(11) 0.0342(13) 0.0416(14) -0.0145(11) -0.0066(10) 0.0013(9) C23 0.0286(12) 0.0266(11) 0.0263(12) -0.0040(9) -0.0021(9) 0.0006(9) C12 0.0340(13) 0.0264(12) 0.0524(16) -0.0100(11) -0.0063(11) -0.0028(10) C26 0.0252(12) 0.0326(13) 0.0374(13) -0.0017(10) -0.0005(10) -0.0058(9) C4 0.0363(13) 0.0351(13) 0.0242(12) -0.0088(10) 0.0011(10) -0.0029(10) C27 0.0260(11) 0.0314(12) 0.0269(12) 0.0006(9) -0.0057(9) -0.0031(9) C1 0.0215(11) 0.0435(14) 0.0333(13) -0.0057(11) -0.0094(9) -0.0021(10) C2 0.0314(13) 0.0553(16) 0.0258(12) -0.0039(11) -0.0107(10) 0.0003(11) C13 0.0298(12) 0.0217(12) 0.0555(16) 0.0004(11) -0.0075(11) -0.0054(9) C6 0.0380(14) 0.0450(15) 0.0361(14) -0.0015(11) -0.0009(11) 0.0045(11) C5 0.0372(13) 0.0318(13) 0.0312(13) -0.0032(10) 0.0057(10) 0.0009(10) C7 0.0325(14) 0.0537(17) 0.0451(16) -0.0117(13) 0.0035(11) -0.0019(12) C18 0.0371(14) 0.0269(13) 0.0714(19) -0.0059(12) -0.0137(13) -0.0076(11) C9 0.0434(15) 0.0640(18) 0.0239(13) -0.0046(12) -0.0005(11) -0.0050(13) C11 0.0288(12) 0.0280(12) 0.0400(14) -0.0094(10) 0.0021(10) -0.0007(9) C15 0.0389(15) 0.0477(16) 0.0508(16) 0.0092(13) 0.0025(12) -0.0086(12) C17 0.0346(15) 0.0318(14) 0.088(2) 0.0061(15) -0.0193(15) -0.0115(11) C16 0.0287(14) 0.0475(17) 0.075(2) 0.0209(16) -0.0042(13) -0.0103(12) C14 0.0329(13) 0.0365(14) 0.0481(16) 0.0055(12) -0.0063(11) -0.0105(11) C8 0.0399(15) 0.076(2) 0.0321(14) -0.0098(13) 0.0079(12) -0.0110(14) _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 N1 1.9746(18) . ? Cu1 N3 2.0027(17) . ? Cu1 N2 2.0097(18) . ? Cu1 N4 2.2231(17) . ? P1 F3 1.5855(15) . ? P1 F2 1.5860(15) . ? P1 F5 1.5885(16) . ? P1 F1 1.5915(16) . ? P1 F4 1.5941(16) . ? P1 F6 1.5987(15) . ? N3 C21 1.276(3) . ? N3 C20 1.476(3) . ? N2 C12 1.273(3) . ? N2 C11 1.477(3) . ? N1 C3 1.272(3) . ? N1 C2 1.486(3) . ? N4 C10 1.464(3) . ? N4 C19 1.468(3) . ? N4 C1 1.470(3) . ? C22 C27 1.391(3) . ? C22 C23 1.393(3) . ? C22 C21 1.465(3) . ? C21 H21A 0.9500 . ? C3 C4 1.468(3) . ? C3 H3A 0.9500 . ? C20 C19 1.525(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C24 C23 1.381(3) . ? C24 C25 1.381(3) . ? C24 H24A 0.9500 . ? C10 C11 1.523(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C25 C26 1.382(3) . ? C25 H25A 0.9500 . ? C23 H23A 0.9500 . ? C12 C13 1.466(3) . ? C12 H12A 0.9500 . ? C26 C27 1.379(3) . ? C26 H26A 0.9500 . ? C4 C5 1.385(3) . ? C4 C9 1.390(3) . ? C27 H27A 0.9500 . ? C1 C2 1.526(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C13 C14 1.388(4) . ? C13 C18 1.397(3) . ? C6 C5 1.379(3) . ? C6 C7 1.383(3) . ? C6 H6A 0.9500 . ? C5 H5A 0.9500 . ? C7 C8 1.377(4) . ? C7 H7A 0.9500 . ? C18 C17 1.383(4) . ? C18 H18A 0.9500 . ? C9 C8 1.383(4) . ? C9 H9A 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C15 C16 1.385(4) . ? C15 C14 1.390(3) . ? C15 H15A 0.9500 . ? C17 C16 1.371(4) . ? C17 H17A 0.9500 . ? C16 H16A 0.9500 . ? C14 H14A 0.9500 . ? C8 H8A 0.9500 . ? 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 N1 Cu1 N3 128.64(7) . . ? N1 Cu1 N2 120.37(8) . . ? N3 Cu1 N2 108.47(7) . . ? N1 Cu1 N4 85.85(7) . . ? N3 Cu1 N4 83.71(7) . . ? N2 Cu1 N4 84.58(7) . . ? F3 P1 F2 90.42(9) . . ? F3 P1 F5 90.47(9) . . ? F2 P1 F5 89.97(9) . . ? F3 P1 F1 90.53(9) . . ? F2 P1 F1 179.01(10) . . ? F5 P1 F1 90.32(10) . . ? F3 P1 F4 89.99(9) . . ? F2 P1 F4 89.38(9) . . ? F5 P1 F4 179.21(10) . . ? F1 P1 F4 90.32(10) . . ? F3 P1 F6 179.73(10) . . ? F2 P1 F6 89.73(9) . . ? F5 P1 F6 89.30(9) . . ? F1 P1 F6 89.33(9) . . ? F4 P1 F6 90.24(9) . . ? C21 N3 C20 117.20(18) . . ? C21 N3 Cu1 135.02(14) . . ? C20 N3 Cu1 106.61(13) . . ? C12 N2 C11 117.32(19) . . ? C12 N2 Cu1 133.96(17) . . ? C11 N2 Cu1 107.77(13) . . ? C3 N1 C2 116.81(19) . . ? C3 N1 Cu1 134.55(17) . . ? C2 N1 Cu1 108.20(14) . . ? C10 N4 C19 114.01(18) . . ? C10 N4 C1 115.60(18) . . ? C19 N4 C1 114.04(17) . . ? C10 N4 Cu1 103.29(12) . . ? C19 N4 Cu1 105.25(12) . . ? C1 N4 Cu1 102.67(12) . . ? C27 C22 C23 118.5(2) . . ? C27 C22 C21 122.94(19) . . ? C23 C22 C21 118.49(19) . . ? N3 C21 C22 124.91(19) . . ? N3 C21 H21A 117.5 . . ? C22 C21 H21A 117.5 . . ? N1 C3 C4 124.0(2) . . ? N1 C3 H3A 118.0 . . ? C4 C3 H3A 118.0 . . ? N3 C20 C19 109.95(17) . . ? N3 C20 H20A 109.7 . . ? C19 C20 H20A 109.7 . . ? N3 C20 H20B 109.7 . . ? C19 C20 H20B 109.7 . . ? H20A C20 H20B 108.2 . . ? N4 C19 C20 110.76(17) . . ? N4 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C23 C24 C25 120.0(2) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? N4 C10 C11 110.42(17) . . ? N4 C10 H10A 109.6 . . ? C11 C10 H10A 109.6 . . ? N4 C10 H10B 109.6 . . ? C11 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? C24 C25 C26 119.9(2) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C24 C23 C22 120.7(2) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? N2 C12 C13 124.3(2) . . ? N2 C12 H12A 117.9 . . ? C13 C12 H12A 117.9 . . ? C27 C26 C25 120.0(2) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C5 C4 C9 118.7(2) . . ? C5 C4 C3 122.8(2) . . ? C9 C4 C3 118.5(2) . . ? C26 C27 C22 120.9(2) . . ? C26 C27 H27A 119.6 . . ? C22 C27 H27A 119.6 . . ? N4 C1 C2 111.18(18) . . ? N4 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N4 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N1 C2 C1 110.76(18) . . ? N1 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C14 C13 C18 119.4(2) . . ? C14 C13 C12 121.9(2) . . ? C18 C13 C12 118.7(2) . . ? C5 C6 C7 120.1(2) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C5 C4 120.7(2) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C8 C7 C6 119.8(2) . . ? C8 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C17 C18 C13 120.2(3) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? C8 C9 C4 120.6(2) . . ? C8 C9 H9A 119.7 . . ? C4 C9 H9A 119.7 . . ? N2 C11 C10 110.00(18) . . ? N2 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? N2 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C16 C15 C14 119.5(3) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C16 C17 C18 119.9(3) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C17 C16 C15 120.8(3) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C13 C14 C15 120.2(2) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C7 C8 C9 120.1(2) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 N3 C21 -140.61(19) . . . . ? N2 Cu1 N3 C21 57.7(2) . . . . ? N4 Cu1 N3 C21 139.8(2) . . . . ? N1 Cu1 N3 C20 52.63(16) . . . . ? N2 Cu1 N3 C20 -109.05(13) . . . . ? N4 Cu1 N3 C20 -26.92(13) . . . . ? N1 Cu1 N2 C12 91.9(2) . . . . ? N3 Cu1 N2 C12 -104.6(2) . . . . ? N4 Cu1 N2 C12 173.9(2) . . . . ? N1 Cu1 N2 C11 -99.98(15) . . . . ? N3 Cu1 N2 C11 63.48(15) . . . . ? N4 Cu1 N2 C11 -18.03(14) . . . . ? N3 Cu1 N1 C3 92.7(2) . . . . ? N2 Cu1 N1 C3 -107.5(2) . . . . ? N4 Cu1 N1 C3 171.2(2) . . . . ? N3 Cu1 N1 C2 -95.51(16) . . . . ? N2 Cu1 N1 C2 64.28(17) . . . . ? N4 Cu1 N1 C2 -16.96(15) . . . . ? N1 Cu1 N4 C10 110.66(14) . . . . ? N3 Cu1 N4 C10 -119.71(14) . . . . ? N2 Cu1 N4 C10 -10.41(14) . . . . ? N1 Cu1 N4 C19 -129.49(14) . . . . ? N3 Cu1 N4 C19 0.14(13) . . . . ? N2 Cu1 N4 C19 109.44(14) . . . . ? N1 Cu1 N4 C1 -9.88(14) . . . . ? N3 Cu1 N4 C1 119.75(14) . . . . ? N2 Cu1 N4 C1 -130.95(14) . . . . ? C20 N3 C21 C22 -177.60(19) . . . . ? Cu1 N3 C21 C22 16.7(3) . . . . ? C27 C22 C21 N3 8.8(3) . . . . ? C23 C22 C21 N3 -174.9(2) . . . . ? C2 N1 C3 C4 -177.9(2) . . . . ? Cu1 N1 C3 C4 -6.7(4) . . . . ? C21 N3 C20 C19 -119.4(2) . . . . ? Cu1 N3 C20 C19 50.16(19) . . . . ? C10 N4 C19 C20 138.90(18) . . . . ? C1 N4 C19 C20 -85.3(2) . . . . ? Cu1 N4 C19 C20 26.43(19) . . . . ? N3 C20 C19 N4 -52.3(2) . . . . ? C19 N4 C10 C11 -77.2(2) . . . . ? C1 N4 C10 C11 147.72(19) . . . . ? Cu1 N4 C10 C11 36.4(2) . . . . ? C23 C24 C25 C26 -1.2(3) . . . . ? C25 C24 C23 C22 0.3(3) . . . . ? C27 C22 C23 C24 0.7(3) . . . . ? C21 C22 C23 C24 -175.78(19) . . . . ? C11 N2 C12 C13 178.9(2) . . . . ? Cu1 N2 C12 C13 -13.9(4) . . . . ? C24 C25 C26 C27 1.1(3) . . . . ? N1 C3 C4 C5 -27.0(4) . . . . ? N1 C3 C4 C9 152.6(2) . . . . ? C25 C26 C27 C22 -0.1(3) . . . . ? C23 C22 C27 C26 -0.8(3) . . . . ? C21 C22 C27 C26 175.5(2) . . . . ? C10 N4 C1 C2 -77.1(2) . . . . ? C19 N4 C1 C2 147.83(19) . . . . ? Cu1 N4 C1 C2 34.5(2) . . . . ? C3 N1 C2 C1 -145.0(2) . . . . ? Cu1 N1 C2 C1 41.6(2) . . . . ? N4 C1 C2 N1 -53.3(3) . . . . ? N2 C12 C13 C14 -27.2(4) . . . . ? N2 C12 C13 C18 154.1(2) . . . . ? C7 C6 C5 C4 -0.1(4) . . . . ? C9 C4 C5 C6 -0.9(4) . . . . ? C3 C4 C5 C6 178.8(2) . . . . ? C5 C6 C7 C8 0.2(4) . . . . ? C14 C13 C18 C17 0.3(4) . . . . ? C12 C13 C18 C17 179.1(2) . . . . ? C5 C4 C9 C8 1.7(4) . . . . ? C3 C4 C9 C8 -177.9(2) . . . . ? C12 N2 C11 C10 -145.7(2) . . . . ? Cu1 N2 C11 C10 43.9(2) . . . . ? N4 C10 C11 N2 -56.2(2) . . . . ? C13 C18 C17 C16 -0.8(4) . . . . ? C18 C17 C16 C15 1.3(4) . . . . ? C14 C15 C16 C17 -1.2(4) . . . . ? C18 C13 C14 C15 -0.1(4) . . . . ? C12 C13 C14 C15 -178.9(2) . . . . ? C16 C15 C14 C13 0.6(4) . . . . ? C6 C7 C8 C9 0.6(4) . . . . ? C4 C9 C8 C7 -1.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.371 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.055 #===END