# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Uttam22 #TrackingRef '18844_web_deposit_cif_file_0_FrankR.Fronczek_1364243754.uttam22.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H36 Cl2 Cu2 N16, 2(Cl), 4(C3 H6 N O)' _chemical_formula_sum 'C56 H64 Cl4 Cu2 N20 O4' _chemical_formula_weight 1350.15 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall '-C 2bc 2 ' _symmetry_space_group_name_H-M 'C m c a ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 19.246(2) _cell_length_b 14.0507(15) _cell_length_c 22.037(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5959.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 90.0(5) _cell_measurement_reflns_used 9955 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 30.50 _exptl_crystal_description rhomb _exptl_crystal_colour blue _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8540 _exptl_absorpt_correction_T_max 0.9627 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'TRIUMPH curved graphite' _diffrn_measurement_device_type 'Bruker Kappa APEX-II DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45945 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 30.60 _reflns_number_total 4699 _reflns_number_gt 3418 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0524P)^2^+10.9299P] 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 4699 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 0.314485(17) 0.0000 0.5000 0.01358(10) Uani 1 2 d S . . Cl1 Cl 0.18619(3) 0.0000 0.5000 0.01923(15) Uani 1 2 d S . . N1 N 0.32089(8) 0.10262(12) 0.56495(8) 0.0152(3) Uani 1 1 d . . . N2 N 0.33516(8) 0.11193(12) 0.44831(8) 0.0154(3) Uani 1 1 d . . . N3 N 0.34488(9) 0.12441(13) 0.38982(8) 0.0182(4) Uani 1 1 d . . . N4 N 0.35501(9) 0.21796(13) 0.38291(8) 0.0183(4) Uani 1 1 d . . . C1 C 0.31016(11) 0.09049(16) 0.62476(10) 0.0194(4) Uani 1 1 d . . . H1 H 0.3042 0.0278 0.6401 0.023 Uiso 1 1 calc R . . C2 C 0.30757(11) 0.16608(16) 0.66445(10) 0.0221(4) Uani 1 1 d . . . H2 H 0.3001 0.1553 0.7065 0.027 Uiso 1 1 calc R . . C3 C 0.31593(11) 0.25822(15) 0.64272(11) 0.0216(5) Uani 1 1 d . . . H3 H 0.3138 0.3111 0.6695 0.026 Uiso 1 1 calc R . . C4 C 0.32744(10) 0.27145(15) 0.58122(10) 0.0189(4) Uani 1 1 d . . . H4 H 0.3337 0.3336 0.5651 0.023 Uiso 1 1 calc R . . C5 C 0.32959(9) 0.19234(14) 0.54369(10) 0.0146(4) Uani 1 1 d . . . C6 C 0.33923(9) 0.19633(14) 0.47812(10) 0.0153(4) Uani 1 1 d . . . C7 C 0.35198(10) 0.26528(15) 0.43569(10) 0.0182(4) Uani 1 1 d . . . H7 H 0.3575 0.3317 0.4422 0.022 Uiso 1 1 calc R . . C8 C 0.36906(11) 0.25391(16) 0.32106(11) 0.0233(5) Uani 1 1 d . . . H8A H 0.3708 0.3243 0.3217 0.028 Uiso 1 1 calc R . . H8B H 0.3310 0.2343 0.2935 0.028 Uiso 1 1 calc R . . C9 C 0.43726(10) 0.21521(16) 0.29784(10) 0.0193(4) Uani 1 1 d . . . C10 C 0.43753(11) 0.14032(17) 0.25669(11) 0.0235(5) Uani 1 1 d . . . H10 H 0.3948 0.1140 0.2431 0.028 Uiso 1 1 calc R . . C11 C 0.5000 0.2530(2) 0.31778(14) 0.0189(6) Uani 1 2 d S . . H11 H 0.5000 0.3051 0.3453 0.023 Uiso 1 2 calc SR . . C12 C 0.5000 0.1039(3) 0.23543(16) 0.0280(7) Uani 1 2 d S . . H12 H 0.5000 0.0541 0.2063 0.034 Uiso 1 2 calc SR . . Cl2 Cl 0.2500 0.05652(6) 0.2500 0.02617(18) Uani 1 2 d S . . O1 O 0.5000 0.1623(4) 0.5225(2) 0.0943(17) Uani 1 2 d S . . N5 N 0.5000 0.1059(2) 0.61655(16) 0.0369(8) Uani 1 2 d S . . C13 C 0.5000 0.1736(5) 0.5771(3) 0.0641(16) Uani 1 2 d S . . H13 H 0.5000 0.2371 0.5919 0.077 Uiso 1 2 calc SR . . C14 C 0.5000 0.0060(3) 0.6008(3) 0.0672(17) Uani 1 2 d S . . H14A H 0.4591 -0.0248 0.6186 0.101 Uiso 0.50 1 d PR . . H14B H 0.5422 -0.0240 0.6166 0.101 Uiso 0.50 1 d PR . . H14C H 0.5000 -0.0008 0.5565 0.101 Uiso 1 2 d SR . . C15 C 0.5000 0.1227(4) 0.6818(2) 0.0585(13) Uani 1 2 d S . . H15A H 0.4881 0.1893 0.6899 0.088 Uiso 0.50 1 d PR . . H15B H 0.5462 0.1089 0.6983 0.088 Uiso 0.50 1 d PR . . H15C H 0.4656 0.0811 0.7012 0.088 Uiso 0.50 1 d PR . . 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 0.01847(16) 0.01287(16) 0.00940(17) -0.00097(14) 0.000 0.000 Cl1 0.0164(3) 0.0153(3) 0.0260(4) -0.0013(3) 0.000 0.000 N1 0.0182(7) 0.0158(8) 0.0117(9) -0.0004(7) -0.0005(6) -0.0004(6) N2 0.0173(7) 0.0189(9) 0.0101(8) -0.0007(7) 0.0007(6) -0.0010(6) N3 0.0220(8) 0.0197(9) 0.0130(9) 0.0028(7) 0.0013(7) -0.0001(6) N4 0.0185(8) 0.0205(9) 0.0158(9) 0.0059(8) 0.0016(7) 0.0002(6) C1 0.0262(10) 0.0191(10) 0.0128(10) -0.0013(8) 0.0009(8) -0.0008(8) C2 0.0289(10) 0.0258(11) 0.0116(10) -0.0046(9) 0.0008(8) -0.0005(8) C3 0.0263(10) 0.0189(10) 0.0197(12) -0.0080(9) -0.0015(9) 0.0006(8) C4 0.0213(9) 0.0153(9) 0.0202(11) -0.0001(9) -0.0006(8) -0.0016(7) C5 0.0135(7) 0.0159(9) 0.0145(10) -0.0008(8) -0.0002(7) -0.0014(6) C6 0.0138(8) 0.0160(9) 0.0159(10) -0.0015(8) -0.0007(7) -0.0006(7) C7 0.0179(8) 0.0185(10) 0.0181(11) 0.0026(8) -0.0004(8) -0.0013(7) C8 0.0222(9) 0.0295(12) 0.0182(12) 0.0088(9) 0.0038(8) 0.0034(8) C9 0.0195(9) 0.0243(11) 0.0141(11) 0.0076(9) 0.0008(8) 0.0006(7) C10 0.0245(10) 0.0268(11) 0.0191(12) 0.0050(10) -0.0038(9) -0.0035(8) C11 0.0234(13) 0.0198(14) 0.0136(15) 0.0034(12) 0.000 0.000 C12 0.0340(16) 0.0257(17) 0.0243(19) -0.0046(14) 0.000 0.000 Cl2 0.0280(3) 0.0333(4) 0.0172(4) 0.000 -0.0055(3) 0.000 O1 0.0344(17) 0.200(6) 0.049(2) 0.013(3) 0.000 0.000 N5 0.0244(14) 0.0450(19) 0.041(2) -0.0163(17) 0.000 0.000 C13 0.029(2) 0.084(4) 0.080(4) 0.023(3) 0.000 0.000 C14 0.044(3) 0.046(3) 0.112(5) -0.015(3) 0.000 0.000 C15 0.055(3) 0.063(3) 0.057(3) -0.008(3) 0.000 0.000 _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 1.9823(17) 4_556 ? Cu1 N2 1.9823(18) . ? Cu1 N1 2.0355(17) . ? Cu1 N1 2.0355(17) 4_556 ? Cu1 Cl1 2.4692(8) . ? N1 C1 1.345(3) . ? N1 C5 1.355(3) . ? N2 N3 1.314(2) . ? N2 C6 1.358(3) . ? N3 N4 1.338(2) . ? N4 C7 1.341(3) . ? N4 C8 1.479(3) . ? C1 C2 1.377(3) . ? C1 H1 0.9500 . ? C2 C3 1.390(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.386(3) . ? C4 H4 0.9500 . ? C5 C6 1.458(3) . ? C6 C7 1.369(3) . ? C7 H7 0.9500 . ? C8 C9 1.510(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.389(3) . ? C9 C11 1.390(3) . ? C10 C12 1.388(3) . ? C10 H10 0.9500 . ? C11 C9 1.391(3) 12_655 ? C11 H11 0.9500 . ? C12 C10 1.388(3) 12_655 ? C12 H12 0.9500 . ? O1 C13 1.215(7) . ? N5 C13 1.288(6) . ? N5 C14 1.446(6) . ? N5 C15 1.458(6) . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9796 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 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 N2 Cu1 N2 156.85(10) 4_556 . ? N2 Cu1 N1 98.38(7) 4_556 . ? N2 Cu1 N1 80.21(7) . . ? N2 Cu1 N1 80.21(7) 4_556 4_556 ? N2 Cu1 N1 98.38(7) . 4_556 ? N1 Cu1 N1 173.05(9) . 4_556 ? N2 Cu1 Cl1 101.58(5) 4_556 . ? N2 Cu1 Cl1 101.58(5) . . ? N1 Cu1 Cl1 93.47(5) . . ? N1 Cu1 Cl1 93.47(5) 4_556 . ? C1 N1 C5 118.41(18) . . ? C1 N1 Cu1 126.16(14) . . ? C5 N1 Cu1 115.04(14) . . ? N3 N2 C6 110.47(17) . . ? N3 N2 Cu1 134.27(14) . . ? C6 N2 Cu1 115.24(14) . . ? N2 N3 N4 105.28(17) . . ? N3 N4 C7 112.47(18) . . ? N3 N4 C8 117.86(18) . . ? C7 N4 C8 129.66(19) . . ? N1 C1 C2 122.0(2) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 119.7(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 118.7(2) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 118.7(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.4(2) . . ? N1 C5 C6 113.21(18) . . ? C4 C5 C6 124.35(19) . . ? N2 C6 C7 107.34(19) . . ? N2 C6 C5 116.01(18) . . ? C7 C6 C5 136.65(19) . . ? N4 C7 C6 104.44(19) . . ? N4 C7 H7 127.8 . . ? C6 C7 H7 127.8 . . ? N4 C8 C9 110.38(18) . . ? N4 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? N4 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C11 119.5(2) . . ? C10 C9 C8 119.82(19) . . ? C11 C9 C8 120.7(2) . . ? C12 C10 C9 120.2(2) . . ? C12 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C9 C11 C9 120.5(3) . 12_655 ? C9 C11 H11 119.7 . . ? C9 C11 H11 119.7 12_655 . ? C10 C12 C10 120.0(3) 12_655 . ? C10 C12 H12 120.0 12_655 . ? C10 C12 H12 120.0 . . ? C13 N5 C14 123.7(5) . . ? C13 N5 C15 123.1(5) . . ? C14 N5 C15 113.2(4) . . ? O1 C13 N5 124.9(7) . . ? O1 C13 H13 117.6 . . ? N5 C13 H13 117.6 . . ? N5 C14 H14A 109.4 . . ? N5 C14 H14B 109.4 . . ? H14A C14 H14B 109.5 . . ? N5 C14 H14C 109.5 . . ? H14A C14 H14C 110.8 . . ? H14B C14 H14C 108.1 . . ? N5 C15 H15A 109.5 . . ? N5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.053 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.086 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 211 79 ' ' 2 0.500 0.000 0.000 211 79 ' ' 3 0.000 0.500 0.000 211 79 ' ' 4 0.500 0.500 0.500 211 79 ' ' _platon_squeeze_details ; The 318 electrons per cell removed by SQUEEZE correspond closely to 8 disordered dimethylformamide molecules per cell, or two per Cu dimer. These are included, in addition to the ordered DMF, in the formula, density, etc. ; _database_code_depnum_ccdc_archive 'CCDC 931039' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Uttam31 #TrackingRef '18845_web_deposit_cif_file_1_FrankR.Fronczek_1364243754.Uttam31.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H30 Cl4 Cu2 N10, 1.085(C3 H7 N O), 1.085(C4 H10 O)' _chemical_formula_sum 'C35.59 H48.44 Cl4 Cu2 N11.09 O2.17' _chemical_formula_weight 935.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1 ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.904(2) _cell_length_b 12.344(2) _cell_length_c 14.031(3) _cell_angle_alpha 92.315(9) _cell_angle_beta 91.163(9) _cell_angle_gamma 105.201(8) _cell_volume 1987.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(5) _cell_measurement_reflns_used 3594 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 67.81 _exptl_crystal_description fragment _exptl_crystal_colour 'yellowish green' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 966 _exptl_absorpt_coefficient_mu 4.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5910 _exptl_absorpt_correction_T_max 0.8500 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(5) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'I\mS microfocus' _diffrn_radiation_monochromator 'QUAZAR multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX-II DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7076 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 69.10 _reflns_number_total 7076 _reflns_number_gt 5569 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The crystal was a non-merohedral twin, with the second domain rotated from first domain by 7.6 degrees about reciprocal axis 1.000 0.937 -0.620 and real axis 1.000 0.899 -0.252. The structure was refined vs. a TWIN4 file prepared using TWINABS. ; _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^)+(0.0810P)^2^] 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 7076 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1164 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 0.25474(3) 0.51912(3) 0.13125(3) 0.01625(13) Uani 1 1 d . . . Cu2 Cu 0.69606(3) 0.97249(3) 0.21115(3) 0.01613(13) Uani 1 1 d . . . Cl1 Cl 0.31187(6) 0.48413(6) -0.02107(6) 0.02240(19) Uani 1 1 d . . . Cl2 Cl 0.29292(6) 0.42628(6) 0.26717(6) 0.02329(19) Uani 1 1 d . . . Cl3 Cl 0.79505(6) 0.95343(6) 0.07026(5) 0.01889(17) Uani 1 1 d . . . Cl4 Cl 0.75891(6) 0.90744(6) 0.35011(6) 0.02162(18) Uani 1 1 d . . . N1 N 0.1044(2) 0.4022(2) 0.10180(19) 0.0165(5) Uani 1 1 d . . . N2 N 0.1292(2) 0.6139(2) 0.15911(19) 0.0165(5) Uani 1 1 d . . . N3 N 0.1274(2) 0.7170(2) 0.1864(2) 0.0189(6) Uani 1 1 d . . . N4 N 0.0150(2) 0.7175(2) 0.18428(19) 0.0173(6) Uani 1 1 d . . . N5 N 0.4411(2) 1.1558(2) 0.1918(2) 0.0205(6) Uani 1 1 d . . . N6 N 0.4651(2) 1.0567(2) 0.1769(2) 0.0232(6) Uani 1 1 d . . . N7 N 0.5766(2) 1.0730(2) 0.2006(2) 0.0196(6) Uani 1 1 d . . . N8 N 0.7977(2) 1.1287(2) 0.24961(19) 0.0186(6) Uani 1 1 d . . . N9 N 0.39255(19) 0.6528(2) 0.15533(18) 0.0144(5) Uani 1 1 d . . . N10 N 0.5684(2) 0.8295(2) 0.18323(18) 0.0149(5) Uani 1 1 d . . . C1 C 0.1001(3) 0.2952(2) 0.0728(2) 0.0197(7) Uani 1 1 d . . . H1 H 0.1710 0.2738 0.0688 0.024 Uiso 1 1 calc R . . C2 C -0.0029(3) 0.2160(3) 0.0488(2) 0.0190(7) Uani 1 1 d . . . H2 H -0.0036 0.1406 0.0313 0.023 Uiso 1 1 calc R . . C3 C -0.1067(3) 0.2495(3) 0.0510(2) 0.0204(7) Uani 1 1 d . . . H3 H -0.1791 0.1972 0.0342 0.025 Uiso 1 1 calc R . . C4 C -0.1023(3) 0.3591(3) 0.0777(2) 0.0186(7) Uani 1 1 d . . . H4 H -0.1714 0.3839 0.0773 0.022 Uiso 1 1 calc R . . C5 C 0.0033(3) 0.4328(3) 0.1051(2) 0.0175(7) Uani 1 1 d . . . C6 C 0.0189(2) 0.5503(2) 0.1384(2) 0.0164(6) Uani 1 1 d . . . C7 C -0.0556(3) 0.6159(3) 0.1555(2) 0.0188(7) Uani 1 1 d . . . H7 H -0.1381 0.5950 0.1487 0.023 Uiso 1 1 calc R . . C8 C -0.0221(3) 0.8220(3) 0.2041(3) 0.0245(7) Uani 1 1 d . . . H8A H -0.0882 0.8052 0.2477 0.029 Uiso 1 1 calc R . . H8B H -0.0503 0.8457 0.1436 0.029 Uiso 1 1 calc R . . C9 C 0.0730(3) 0.9184(3) 0.2481(2) 0.0199(7) Uani 1 1 d . . . C10 C 0.0753(3) 0.9423(3) 0.3452(3) 0.0255(8) Uani 1 1 d . . . H10 H 0.0198 0.8952 0.3836 0.031 Uiso 1 1 calc R . . C11 C 0.1571(3) 1.0340(3) 0.3877(3) 0.0313(8) Uani 1 1 d . . . H11 H 0.1596 1.0487 0.4548 0.038 Uiso 1 1 calc R . . C12 C 0.2356(3) 1.1042(3) 0.3295(3) 0.0288(8) Uani 1 1 d . . . H12 H 0.2908 1.1681 0.3577 0.035 Uiso 1 1 calc R . . C13 C 0.2351(3) 1.0829(2) 0.2325(2) 0.0186(7) Uani 1 1 d . . . C14 C 0.1524(3) 0.9897(3) 0.1914(2) 0.0204(7) Uani 1 1 d . . . H14 H 0.1501 0.9748 0.1243 0.024 Uiso 1 1 calc R . . C15 C 0.3205(3) 1.1608(3) 0.1719(3) 0.0226(7) Uani 1 1 d . . . H15A H 0.2999 1.1400 0.1037 0.027 Uiso 1 1 calc R . . H15B H 0.3151 1.2387 0.1844 0.027 Uiso 1 1 calc R . . C16 C 0.5361(3) 1.2364(3) 0.2243(2) 0.0199(7) Uani 1 1 d . . . H16 H 0.5414 1.3132 0.2400 0.024 Uiso 1 1 calc R . . C17 C 0.6236(3) 1.1825(3) 0.2297(2) 0.0190(7) Uani 1 1 d . . . C18 C 0.7464(3) 1.2138(3) 0.2587(2) 0.0190(7) Uani 1 1 d . . . C19 C 0.8081(3) 1.3212(3) 0.2917(2) 0.0244(7) Uani 1 1 d . . . H19 H 0.7705 1.3800 0.2987 0.029 Uiso 1 1 calc R . . C20 C 0.9258(3) 1.3402(3) 0.3140(2) 0.0245(7) Uani 1 1 d . . . H20 H 0.9699 1.4125 0.3373 0.029 Uiso 1 1 calc R . . C21 C 0.9789(3) 1.2538(3) 0.3024(2) 0.0247(7) Uani 1 1 d . . . H21 H 1.0600 1.2666 0.3158 0.030 Uiso 1 1 calc R . . C22 C 0.9128(3) 1.1488(3) 0.2712(2) 0.0220(7) Uani 1 1 d . . . H22 H 0.9490 1.0889 0.2647 0.026 Uiso 1 1 calc R . . C23 C 0.3894(2) 0.7409(2) 0.0856(2) 0.0164(6) Uani 1 1 d . . . H23A H 0.3266 0.7770 0.1017 0.020 Uiso 1 1 calc R . . H23B H 0.3729 0.7059 0.0204 0.020 Uiso 1 1 calc R . . C24 C 0.5078(2) 0.8298(2) 0.0897(2) 0.0169(6) Uani 1 1 d . . . H24A H 0.5565 0.8131 0.0376 0.020 Uiso 1 1 calc R . . H24B H 0.4956 0.9050 0.0806 0.020 Uiso 1 1 calc R . . C25 C 0.4812(3) 0.8202(3) 0.2604(2) 0.0181(7) Uani 1 1 d . . . H25A H 0.4393 0.8792 0.2541 0.022 Uiso 1 1 calc R . . H25B H 0.5220 0.8318 0.3236 0.022 Uiso 1 1 calc R . . C26 C 0.3935(2) 0.7038(2) 0.2530(2) 0.0154(6) Uani 1 1 d . . . H26A H 0.4154 0.6547 0.3001 0.018 Uiso 1 1 calc R . . H26B H 0.3148 0.7112 0.2675 0.018 Uiso 1 1 calc R . . C27 C 0.5071(2) 0.6237(2) 0.1441(2) 0.0180(7) Uani 1 1 d . . . H27A H 0.5179 0.6061 0.0760 0.022 Uiso 1 1 calc R . . H27B H 0.5072 0.5565 0.1804 0.022 Uiso 1 1 calc R . . C28 C 0.6073(2) 0.7235(2) 0.1815(2) 0.0172(6) Uani 1 1 d . . . H28A H 0.6322 0.7098 0.2466 0.021 Uiso 1 1 calc R . . H28B H 0.6747 0.7314 0.1397 0.021 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 0.0110(2) 0.0137(2) 0.0233(3) -0.00219(18) -0.00073(17) 0.00258(18) Cu2 0.0126(2) 0.0144(2) 0.0204(3) -0.00151(18) -0.00150(17) 0.00215(18) Cl1 0.0131(3) 0.0264(4) 0.0266(5) -0.0095(3) -0.0001(3) 0.0049(3) Cl2 0.0240(4) 0.0165(4) 0.0290(5) 0.0026(3) -0.0041(3) 0.0048(3) Cl3 0.0168(3) 0.0181(3) 0.0201(4) 0.0001(3) 0.0009(3) 0.0018(3) Cl4 0.0185(3) 0.0242(4) 0.0202(4) 0.0017(3) -0.0039(3) 0.0024(3) N1 0.0121(12) 0.0153(12) 0.0205(15) 0.0000(11) -0.0015(10) 0.0007(10) N2 0.0119(12) 0.0141(12) 0.0244(16) -0.0021(11) -0.0009(10) 0.0053(10) N3 0.0121(12) 0.0158(12) 0.0293(17) -0.0037(11) -0.0028(10) 0.0054(11) N4 0.0126(12) 0.0166(12) 0.0238(16) -0.0040(11) 0.0001(10) 0.0067(11) N5 0.0198(13) 0.0145(12) 0.0291(17) 0.0004(11) -0.0025(11) 0.0084(11) N6 0.0185(13) 0.0142(13) 0.0379(18) -0.0042(12) -0.0036(11) 0.0073(11) N7 0.0159(12) 0.0128(12) 0.0303(17) -0.0026(11) -0.0028(11) 0.0048(11) N8 0.0170(12) 0.0183(13) 0.0182(15) 0.0002(11) -0.0017(10) 0.0011(11) N9 0.0095(11) 0.0154(12) 0.0184(15) -0.0031(10) -0.0022(9) 0.0042(10) N10 0.0131(12) 0.0155(12) 0.0160(14) -0.0022(10) -0.0008(10) 0.0040(10) C1 0.0174(15) 0.0150(14) 0.028(2) 0.0022(13) -0.0032(13) 0.0064(13) C2 0.0209(15) 0.0160(14) 0.0203(18) 0.0004(13) -0.0064(12) 0.0056(13) C3 0.0175(15) 0.0194(15) 0.0219(19) 0.0012(13) -0.0041(12) 0.0008(13) C4 0.0161(14) 0.0209(15) 0.0190(18) 0.0026(13) 0.0003(12) 0.0052(13) C5 0.0170(15) 0.0186(15) 0.0171(18) 0.0043(13) -0.0006(12) 0.0048(13) C6 0.0140(14) 0.0185(15) 0.0162(17) 0.0004(13) -0.0009(11) 0.0037(13) C7 0.0141(14) 0.0221(16) 0.0204(18) -0.0023(13) -0.0014(12) 0.0055(13) C8 0.0223(16) 0.0188(16) 0.034(2) -0.0065(14) -0.0025(14) 0.0106(14) C9 0.0138(14) 0.0199(15) 0.030(2) -0.0041(14) -0.0050(12) 0.0118(13) C10 0.0216(16) 0.0301(18) 0.026(2) 0.0010(15) -0.0001(13) 0.0087(15) C11 0.0325(19) 0.038(2) 0.022(2) -0.0075(16) -0.0044(14) 0.0082(17) C12 0.0259(17) 0.0230(17) 0.035(2) -0.0074(15) -0.0094(15) 0.0039(15) C13 0.0197(15) 0.0163(14) 0.0232(19) -0.0013(13) -0.0013(12) 0.0115(13) C14 0.0225(16) 0.0210(15) 0.0218(19) -0.0054(13) -0.0051(13) 0.0144(14) C15 0.0218(16) 0.0159(15) 0.031(2) -0.0017(14) -0.0071(13) 0.0081(13) C16 0.0243(16) 0.0139(14) 0.0214(19) -0.0031(13) -0.0022(13) 0.0055(13) C17 0.0233(16) 0.0185(15) 0.0161(18) -0.0005(13) 0.0024(12) 0.0071(13) C18 0.0204(15) 0.0179(15) 0.0181(18) -0.0005(13) 0.0025(12) 0.0038(13) C19 0.0277(17) 0.0208(16) 0.023(2) 0.0024(14) 0.0031(14) 0.0037(14) C20 0.0241(16) 0.0207(16) 0.0228(19) -0.0026(14) -0.0025(13) -0.0036(14) C21 0.0185(15) 0.0289(18) 0.024(2) 0.0033(14) -0.0023(13) 0.0014(14) C22 0.0170(15) 0.0227(16) 0.026(2) 0.0011(14) 0.0008(12) 0.0046(14) C23 0.0164(14) 0.0181(15) 0.0161(17) 0.0002(12) -0.0011(11) 0.0072(13) C24 0.0163(15) 0.0152(14) 0.0191(18) -0.0009(12) -0.0004(12) 0.0043(13) C25 0.0163(14) 0.0167(14) 0.0211(18) -0.0025(13) 0.0041(12) 0.0043(13) C26 0.0153(14) 0.0156(14) 0.0149(17) -0.0023(12) -0.0001(11) 0.0040(12) C27 0.0107(14) 0.0157(14) 0.0286(19) -0.0052(13) -0.0022(12) 0.0063(12) C28 0.0122(13) 0.0146(14) 0.0246(18) -0.0026(13) -0.0027(12) 0.0038(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 N1 2.006(2) . ? Cu1 N9 2.011(2) . ? Cu1 N2 2.158(2) . ? Cu1 Cl1 2.3142(10) . ? Cu1 Cl2 2.3603(10) . ? Cu2 N10 2.022(2) . ? Cu2 N8 2.034(3) . ? Cu2 N7 2.125(3) . ? Cu2 Cl4 2.3213(10) . ? Cu2 Cl3 2.3568(9) . ? N1 C5 1.353(4) . ? N1 C1 1.354(4) . ? N2 N3 1.320(3) . ? N2 C6 1.360(4) . ? N3 N4 1.338(3) . ? N4 C7 1.354(4) . ? N4 C8 1.487(4) . ? N5 N6 1.337(4) . ? N5 C16 1.352(4) . ? N5 C15 1.474(4) . ? N6 N7 1.323(4) . ? N7 C17 1.362(4) . ? N8 C18 1.350(4) . ? N8 C22 1.353(4) . ? N9 C26 1.484(4) . ? N9 C23 1.498(4) . ? N9 C27 1.509(3) . ? N10 C24 1.486(4) . ? N10 C28 1.497(4) . ? N10 C25 1.502(4) . ? C1 C2 1.379(4) . ? C1 H1 0.9500 . ? C2 C3 1.403(4) . ? C2 H2 0.9500 . ? C3 C4 1.377(4) . ? C3 H3 0.9500 . ? C4 C5 1.382(4) . ? C4 H4 0.9500 . ? C5 C6 1.468(4) . ? C6 C7 1.367(4) . ? C7 H7 0.9500 . ? C8 C9 1.513(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.379(5) . ? C9 C14 1.397(5) . ? C10 C11 1.389(5) . ? C10 H10 0.9500 . ? C11 C12 1.398(5) . ? C11 H11 0.9500 . ? C12 C13 1.376(5) . ? C12 H12 0.9500 . ? C13 C14 1.398(4) . ? C13 C15 1.506(4) . ? C14 H14 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.377(5) . ? C16 H16 0.9500 . ? C17 C18 1.456(4) . ? C18 C19 1.392(4) . ? C19 C20 1.386(5) . ? C19 H19 0.9500 . ? C20 C21 1.381(5) . ? C20 H20 0.9500 . ? C21 C22 1.377(5) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.541(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.536(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.539(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? 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 N9 171.52(10) . . ? N1 Cu1 N2 78.64(10) . . ? N9 Cu1 N2 93.83(9) . . ? N1 Cu1 Cl1 88.27(8) . . ? N9 Cu1 Cl1 92.62(8) . . ? N2 Cu1 Cl1 122.69(8) . . ? N1 Cu1 Cl2 91.79(8) . . ? N9 Cu1 Cl2 94.64(8) . . ? N2 Cu1 Cl2 111.66(8) . . ? Cl1 Cu1 Cl2 124.43(4) . . ? N10 Cu2 N8 168.33(10) . . ? N10 Cu2 N7 91.90(10) . . ? N8 Cu2 N7 77.71(10) . . ? N10 Cu2 Cl4 93.23(8) . . ? N8 Cu2 Cl4 88.84(8) . . ? N7 Cu2 Cl4 126.53(8) . . ? N10 Cu2 Cl3 94.15(7) . . ? N8 Cu2 Cl3 95.03(8) . . ? N7 Cu2 Cl3 114.81(8) . . ? Cl4 Cu2 Cl3 117.80(3) . . ? C5 N1 C1 118.4(3) . . ? C5 N1 Cu1 118.9(2) . . ? C1 N1 Cu1 122.6(2) . . ? N3 N2 C6 109.9(2) . . ? N3 N2 Cu1 139.01(19) . . ? C6 N2 Cu1 111.04(19) . . ? N2 N3 N4 105.9(2) . . ? N3 N4 C7 111.9(2) . . ? N3 N4 C8 121.9(2) . . ? C7 N4 C8 126.0(2) . . ? N6 N5 C16 111.7(3) . . ? N6 N5 C15 117.5(2) . . ? C16 N5 C15 130.9(3) . . ? N7 N6 N5 106.3(2) . . ? N6 N7 C17 109.9(3) . . ? N6 N7 Cu2 136.7(2) . . ? C17 N7 Cu2 113.3(2) . . ? C18 N8 C22 119.1(3) . . ? C18 N8 Cu2 118.3(2) . . ? C22 N8 Cu2 122.5(2) . . ? C26 N9 C23 108.0(2) . . ? C26 N9 C27 107.2(2) . . ? C23 N9 C27 107.0(2) . . ? C26 N9 Cu1 111.64(17) . . ? C23 N9 Cu1 110.07(18) . . ? C27 N9 Cu1 112.61(18) . . ? C24 N10 C28 106.0(2) . . ? C24 N10 C25 108.5(2) . . ? C28 N10 C25 106.9(2) . . ? C24 N10 Cu2 112.15(17) . . ? C28 N10 Cu2 115.20(17) . . ? C25 N10 Cu2 107.85(18) . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 118.2(3) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 121.9(3) . . ? N1 C5 C6 113.3(3) . . ? C4 C5 C6 124.8(3) . . ? N2 C6 C7 108.0(3) . . ? N2 C6 C5 117.9(3) . . ? C7 C6 C5 134.1(3) . . ? N4 C7 C6 104.3(3) . . ? N4 C7 H7 127.8 . . ? C6 C7 H7 127.8 . . ? N4 C8 C9 114.0(3) . . ? N4 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? N4 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C14 119.3(3) . . ? C10 C9 C8 119.3(3) . . ? C14 C9 C8 121.1(3) . . ? C9 C10 C11 121.2(3) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 118.5(3) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C13 C12 C11 121.6(3) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 118.8(3) . . ? C12 C13 C15 120.2(3) . . ? C14 C13 C15 121.0(3) . . ? C9 C14 C13 120.6(3) . . ? C9 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? N5 C15 C13 111.8(3) . . ? N5 C15 H15A 109.3 . . ? C13 C15 H15A 109.3 . . ? N5 C15 H15B 109.3 . . ? C13 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? N5 C16 C17 104.8(3) . . ? N5 C16 H16 127.6 . . ? C17 C16 H16 127.6 . . ? N7 C17 C16 107.4(3) . . ? N7 C17 C18 116.5(3) . . ? C16 C17 C18 136.1(3) . . ? N8 C18 C19 121.8(3) . . ? N8 C18 C17 113.8(3) . . ? C19 C18 C17 124.3(3) . . ? C20 C19 C18 118.2(3) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 119.2(3) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? N8 C22 C21 121.7(3) . . ? N8 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? N9 C23 C24 109.3(2) . . ? N9 C23 H23A 109.8 . . ? C24 C23 H23A 109.8 . . ? N9 C23 H23B 109.8 . . ? C24 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? N10 C24 C23 110.1(2) . . ? N10 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? N10 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.2 . . ? N10 C25 C26 110.2(2) . . ? N10 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? N10 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? N9 C26 C25 109.8(2) . . ? N9 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? N9 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? N9 C27 C28 109.6(2) . . ? N9 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? N9 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.2 . . ? N10 C28 C27 110.0(2) . . ? N10 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? N10 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? 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 N9 Cu1 N1 C5 -23.3(8) . . . . ? N2 Cu1 N1 C5 4.4(2) . . . . ? Cl1 Cu1 N1 C5 -119.5(2) . . . . ? Cl2 Cu1 N1 C5 116.1(2) . . . . ? N9 Cu1 N1 C1 152.4(6) . . . . ? N2 Cu1 N1 C1 -179.9(3) . . . . ? Cl1 Cu1 N1 C1 56.2(2) . . . . ? Cl2 Cu1 N1 C1 -68.2(2) . . . . ? N1 Cu1 N2 N3 -179.2(3) . . . . ? N9 Cu1 N2 N3 -3.2(3) . . . . ? Cl1 Cu1 N2 N3 -98.8(3) . . . . ? Cl2 Cu1 N2 N3 93.4(3) . . . . ? N1 Cu1 N2 C6 -3.2(2) . . . . ? N9 Cu1 N2 C6 172.9(2) . . . . ? Cl1 Cu1 N2 C6 77.3(2) . . . . ? Cl2 Cu1 N2 C6 -90.6(2) . . . . ? C6 N2 N3 N4 1.0(3) . . . . ? Cu1 N2 N3 N4 177.1(2) . . . . ? N2 N3 N4 C7 -0.3(3) . . . . ? N2 N3 N4 C8 -175.6(3) . . . . ? C16 N5 N6 N7 0.3(4) . . . . ? C15 N5 N6 N7 -179.2(3) . . . . ? N5 N6 N7 C17 -0.4(4) . . . . ? N5 N6 N7 Cu2 175.7(2) . . . . ? N10 Cu2 N7 N6 -5.6(3) . . . . ? N8 Cu2 N7 N6 179.7(3) . . . . ? Cl4 Cu2 N7 N6 -101.1(3) . . . . ? Cl3 Cu2 N7 N6 89.8(3) . . . . ? N10 Cu2 N7 C17 170.4(2) . . . . ? N8 Cu2 N7 C17 -4.3(2) . . . . ? Cl4 Cu2 N7 C17 75.0(2) . . . . ? Cl3 Cu2 N7 C17 -94.2(2) . . . . ? N10 Cu2 N8 C18 -21.9(7) . . . . ? N7 Cu2 N8 C18 5.6(2) . . . . ? Cl4 Cu2 N8 C18 -122.3(2) . . . . ? Cl3 Cu2 N8 C18 119.9(2) . . . . ? N10 Cu2 N8 C22 154.5(5) . . . . ? N7 Cu2 N8 C22 -178.1(3) . . . . ? Cl4 Cu2 N8 C22 54.1(2) . . . . ? Cl3 Cu2 N8 C22 -63.7(2) . . . . ? N1 Cu1 N9 C26 85.8(7) . . . . ? N2 Cu1 N9 C26 58.7(2) . . . . ? Cl1 Cu1 N9 C26 -178.30(18) . . . . ? Cl2 Cu1 N9 C26 -53.44(19) . . . . ? N1 Cu1 N9 C23 -34.1(8) . . . . ? N2 Cu1 N9 C23 -61.26(19) . . . . ? Cl1 Cu1 N9 C23 61.76(18) . . . . ? Cl2 Cu1 N9 C23 -173.38(17) . . . . ? N1 Cu1 N9 C27 -153.5(7) . . . . ? N2 Cu1 N9 C27 179.4(2) . . . . ? Cl1 Cu1 N9 C27 -57.6(2) . . . . ? Cl2 Cu1 N9 C27 67.3(2) . . . . ? N8 Cu2 N10 C24 85.3(6) . . . . ? N7 Cu2 N10 C24 58.5(2) . . . . ? Cl4 Cu2 N10 C24 -174.74(18) . . . . ? Cl3 Cu2 N10 C24 -56.54(19) . . . . ? N8 Cu2 N10 C28 -153.4(5) . . . . ? N7 Cu2 N10 C28 179.8(2) . . . . ? Cl4 Cu2 N10 C28 -53.4(2) . . . . ? Cl3 Cu2 N10 C28 64.8(2) . . . . ? N8 Cu2 N10 C25 -34.2(6) . . . . ? N7 Cu2 N10 C25 -61.0(2) . . . . ? Cl4 Cu2 N10 C25 65.80(19) . . . . ? Cl3 Cu2 N10 C25 -176.01(18) . . . . ? C5 N1 C1 C2 -1.6(5) . . . . ? Cu1 N1 C1 C2 -177.3(2) . . . . ? N1 C1 C2 C3 2.7(5) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C2 C3 C4 C5 -2.3(5) . . . . ? C1 N1 C5 C4 -1.6(4) . . . . ? Cu1 N1 C5 C4 174.3(2) . . . . ? C1 N1 C5 C6 179.5(3) . . . . ? Cu1 N1 C5 C6 -4.6(4) . . . . ? C3 C4 C5 N1 3.5(5) . . . . ? C3 C4 C5 C6 -177.7(3) . . . . ? N3 N2 C6 C7 -1.4(4) . . . . ? Cu1 N2 C6 C7 -178.6(2) . . . . ? N3 N2 C6 C5 179.1(3) . . . . ? Cu1 N2 C6 C5 1.8(3) . . . . ? N1 C5 C6 N2 1.6(4) . . . . ? C4 C5 C6 N2 -177.3(3) . . . . ? N1 C5 C6 C7 -177.8(3) . . . . ? C4 C5 C6 C7 3.3(6) . . . . ? N3 N4 C7 C6 -0.5(4) . . . . ? C8 N4 C7 C6 174.6(3) . . . . ? N2 C6 C7 N4 1.1(3) . . . . ? C5 C6 C7 N4 -179.4(3) . . . . ? N3 N4 C8 C9 -13.4(4) . . . . ? C7 N4 C8 C9 172.0(3) . . . . ? N4 C8 C9 C10 -100.6(4) . . . . ? N4 C8 C9 C14 85.1(4) . . . . ? C14 C9 C10 C11 -1.9(5) . . . . ? C8 C9 C10 C11 -176.3(3) . . . . ? C9 C10 C11 C12 1.9(5) . . . . ? C10 C11 C12 C13 -1.5(5) . . . . ? C11 C12 C13 C14 1.1(5) . . . . ? C11 C12 C13 C15 179.6(3) . . . . ? C10 C9 C14 C13 1.5(5) . . . . ? C8 C9 C14 C13 175.8(3) . . . . ? C12 C13 C14 C9 -1.1(5) . . . . ? C15 C13 C14 C9 -179.6(3) . . . . ? N6 N5 C15 C13 60.2(4) . . . . ? C16 N5 C15 C13 -119.3(4) . . . . ? C12 C13 C15 N5 67.9(4) . . . . ? C14 C13 C15 N5 -113.7(3) . . . . ? N6 N5 C16 C17 -0.1(4) . . . . ? C15 N5 C16 C17 179.4(3) . . . . ? N6 N7 C17 C16 0.4(4) . . . . ? Cu2 N7 C17 C16 -176.7(2) . . . . ? N6 N7 C17 C18 179.7(3) . . . . ? Cu2 N7 C17 C18 2.6(4) . . . . ? N5 C16 C17 N7 -0.1(3) . . . . ? N5 C16 C17 C18 -179.3(4) . . . . ? C22 N8 C18 C19 -1.4(5) . . . . ? Cu2 N8 C18 C19 175.1(2) . . . . ? C22 N8 C18 C17 177.7(3) . . . . ? Cu2 N8 C18 C17 -5.8(4) . . . . ? N7 C17 C18 N8 1.8(4) . . . . ? C16 C17 C18 N8 -179.0(4) . . . . ? N7 C17 C18 C19 -179.0(3) . . . . ? C16 C17 C18 C19 0.1(6) . . . . ? N8 C18 C19 C20 1.0(5) . . . . ? C17 C18 C19 C20 -178.0(3) . . . . ? C18 C19 C20 C21 0.6(5) . . . . ? C19 C20 C21 C22 -1.9(5) . . . . ? C18 N8 C22 C21 0.1(5) . . . . ? Cu2 N8 C22 C21 -176.2(2) . . . . ? C20 C21 C22 N8 1.5(5) . . . . ? C26 N9 C23 C24 70.6(3) . . . . ? C27 N9 C23 C24 -44.6(3) . . . . ? Cu1 N9 C23 C24 -167.25(19) . . . . ? C28 N10 C24 C23 71.9(3) . . . . ? C25 N10 C24 C23 -42.6(3) . . . . ? Cu2 N10 C24 C23 -161.62(19) . . . . ? N9 C23 C24 N10 -23.2(3) . . . . ? C24 N10 C25 C26 68.0(3) . . . . ? C28 N10 C25 C26 -45.8(3) . . . . ? Cu2 N10 C25 C26 -170.2(2) . . . . ? C23 N9 C26 C25 -45.2(3) . . . . ? C27 N9 C26 C25 69.8(3) . . . . ? Cu1 N9 C26 C25 -166.37(19) . . . . ? N10 C25 C26 N9 -20.9(3) . . . . ? C26 N9 C27 C28 -46.3(3) . . . . ? C23 N9 C27 C28 69.4(3) . . . . ? Cu1 N9 C27 C28 -169.5(2) . . . . ? C24 N10 C28 C27 -46.4(3) . . . . ? C25 N10 C28 C27 69.2(3) . . . . ? Cu2 N10 C28 C27 -171.0(2) . . . . ? N9 C27 C28 N10 -20.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 69.10 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.694 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.096 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.045 0.410 0.500 531 178 ' ' _platon_squeeze_details ; >From difference maps, the disordered solvents removed by SQUEEZE appeared to likely be both dimethylformamide and diethyl ether, in approximately equal amounts. The 178 electrons correspond to approximately 2.17 molecules of each per unit cell. The solvent molecules are included in the formula, density, etc., but are not in the model. ; # END OF CIF _database_code_depnum_ccdc_archive 'CCDC 931040' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Uttam29 #TrackingRef '18643_web_deposit_cif_file_0_FrankR.Fronczek_1363637732.uttam29.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H63 Cu2 N19 O4, 4 (P F6), 4(C3 H7 N O)' _chemical_formula_sum 'C73 H91 Cu2 F24 N23 O8 P4' _chemical_formula_weight 2125.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall ' -P 1 ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8788(14) _cell_length_b 13.7253(14) _cell_length_c 25.452(3) _cell_angle_alpha 83.482(7) _cell_angle_beta 87.955(8) _cell_angle_gamma 88.596(7) _cell_volume 4466.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 95.0(5) _cell_measurement_reflns_used 4893 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 58.35 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 2.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7695 _exptl_absorpt_correction_T_max 0.8372 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 95.0(5) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'I\mS microfocus' _diffrn_radiation_monochromator 'QUAZAR multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX-II DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12307 _diffrn_reflns_av_R_equivalents 0.0705 _diffrn_reflns_av_sigmaI/netI 0.1470 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 59.24 _reflns_number_total 12307 _reflns_number_gt 6796 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections, using a TWIN4 file generated using TWINABS. The crystal is a nonmerohedral twin, which can be described as the second domain rotated from first domain by 177.7 degrees about reciprocal axis 0.063 0.059 1.000 and real axis 0.181 -0.004 1.000 Twin matrix: -0.975 -0.039 0.127 0.064 -1.000 0.114 0.357 -0.002 0.977 ; _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^)+(0.1182P)^2^] 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 12307 _refine_ls_number_parameters 1279 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1474 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.2148 _refine_ls_wR_factor_gt 0.1869 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.21397(7) 0.68999(7) 0.24127(4) 0.0356(3) Uani 1 1 d . . . Cu2 Cu 0.77765(7) 0.37809(7) 0.25734(4) 0.0361(3) Uani 1 1 d . A . O1 O 0.0648(4) 0.7788(3) 0.2432(2) 0.0380(12) Uani 1 1 d D . . H1W H 0.059(6) 0.828(3) 0.222(2) 0.057 Uiso 1 1 d D . . H2W H 0.042(6) 0.793(5) 0.2715(16) 0.057 Uiso 1 1 d D . . O2 O 0.6210(5) 0.4542(5) 0.2645(3) 0.0653(19) Uani 1 1 d D . . O3 O 0.3694(4) 0.5940(4) 0.2457(3) 0.067(2) Uani 1 1 d . . . O4 O 0.9436(4) 0.2941(4) 0.2480(2) 0.0474(14) Uani 1 1 d . . . N1 N 0.1609(4) 0.5920(4) 0.3017(2) 0.0318(14) Uani 1 1 d . . . N2 N 0.1660(4) 0.5863(4) 0.1981(2) 0.0314(14) Uani 1 1 d . . . N3 N 0.1645(4) 0.5737(4) 0.1475(2) 0.0369(15) Uani 1 1 d . . . N4 N 0.1299(4) 0.4836(4) 0.1457(3) 0.0389(15) Uani 1 1 d . . . N5 N 0.6539(4) 0.2064(4) 0.1546(3) 0.0395(15) Uani 1 1 d . A . N6 N 0.7015(4) 0.2900(4) 0.1595(2) 0.0379(15) Uani 1 1 d . A . N7 N 0.7135(4) 0.2900(4) 0.2106(2) 0.0337(14) Uani 1 1 d . . . N8 N 0.7331(4) 0.2686(4) 0.3140(2) 0.0379(15) Uani 1 1 d . . . N9 N 0.2789(4) 0.7821(4) 0.1819(2) 0.0354(15) Uani 1 1 d . . . N10 N 0.2850(4) 0.7819(4) 0.2841(2) 0.0308(14) Uani 1 1 d . . . N11 N 0.2934(4) 0.7922(4) 0.3346(2) 0.0373(15) Uani 1 1 d . . . N12 N 0.3511(4) 0.8703(4) 0.3360(3) 0.0412(16) Uani 1 1 d . . . N13 N 0.8641(4) 0.5666(4) 0.3603(2) 0.0346(14) Uani 1 1 d . A . N14 N 0.8300(4) 0.4770(4) 0.3555(2) 0.0364(15) Uani 1 1 d . A . N15 N 0.8307(4) 0.4714(4) 0.3035(2) 0.0302(14) Uani 1 1 d . . . N16 N 0.8339(4) 0.4813(4) 0.2002(2) 0.0318(14) Uani 1 1 d . . . N17 N 0.4972(7) 0.5712(6) 0.1784(3) 0.077(2) Uani 1 1 d . . . N19 N 0.9456(5) 0.1346(4) 0.2342(3) 0.0510(17) Uani 1 1 d . . . C1 C 0.1572(5) 0.6012(5) 0.3534(3) 0.0324(17) Uani 1 1 d . . . H1A H 0.1784 0.6611 0.3646 0.039 Uiso 1 1 calc R . . C2 C 0.1246(5) 0.5286(5) 0.3906(3) 0.0383(18) Uani 1 1 d . . . H2 H 0.1225 0.5381 0.4270 0.046 Uiso 1 1 calc R . . C3 C 0.0947(5) 0.4416(6) 0.3751(3) 0.0421(19) Uani 1 1 d . . . H3 H 0.0726 0.3899 0.4008 0.050 Uiso 1 1 calc R . . C4 C 0.0967(5) 0.4290(5) 0.3217(3) 0.0399(19) Uani 1 1 d . . . H4 H 0.0759 0.3694 0.3100 0.048 Uiso 1 1 calc R . . C5 C 0.1298(5) 0.5061(5) 0.2865(3) 0.0319(17) Uani 1 1 d . . . C6 C 0.1339(5) 0.5057(5) 0.2283(3) 0.0340(18) Uani 1 1 d . . . C7 C 0.1098(5) 0.4387(5) 0.1948(3) 0.0366(18) Uani 1 1 d . . . H7 H 0.0844 0.3745 0.2042 0.044 Uiso 1 1 calc R . . C8 C 0.1183(5) 0.4458(5) 0.0951(3) 0.0386(19) Uani 1 1 d . . . H8A H 0.0809 0.4954 0.0711 0.046 Uiso 1 1 calc R . . H8B H 0.0756 0.3862 0.1006 0.046 Uiso 1 1 calc R . . C9 C 0.2206(5) 0.4210(5) 0.0694(3) 0.0342(18) Uani 1 1 d . . . C10 C 0.2475(6) 0.4683(5) 0.0194(3) 0.046(2) Uani 1 1 d . . . H10 H 0.2008 0.5150 0.0021 0.055 Uiso 1 1 calc R . . C11 C 0.3405(6) 0.4478(5) -0.0046(3) 0.043(2) Uani 1 1 d . . . H11 H 0.3564 0.4798 -0.0389 0.052 Uiso 1 1 calc R . . C12 C 0.4132(6) 0.3813(5) 0.0194(3) 0.043(2) Uani 1 1 d . . . C13 C 0.5119(6) 0.3605(5) -0.0028(3) 0.048(2) Uani 1 1 d . . . H13 H 0.5306 0.3913 -0.0370 0.057 Uiso 1 1 calc R . . C14 C 0.5805(6) 0.2989(6) 0.0228(3) 0.048(2) Uani 1 1 d . . . H14 H 0.6469 0.2876 0.0069 0.057 Uiso 1 1 calc R . . C15 C 0.5541(5) 0.2506(5) 0.0734(3) 0.0385(19) Uani 1 1 d . . . C16 C 0.4583(5) 0.2666(5) 0.0965(3) 0.0378(18) Uani 1 1 d . . . H16 H 0.4409 0.2330 0.1302 0.045 Uiso 1 1 calc R . . C17 C 0.3853(5) 0.3321(5) 0.0708(3) 0.0370(18) Uani 1 1 d . . . C18 C 0.2883(5) 0.3542(5) 0.0943(3) 0.0336(17) Uani 1 1 d . . . H18 H 0.2694 0.3220 0.1282 0.040 Uiso 1 1 calc R . . C19 C 0.6326(5) 0.1813(5) 0.1017(3) 0.047(2) Uani 1 1 d . . . H19A H 0.6063 0.1137 0.1048 0.056 Uiso 1 1 calc R . . H19B H 0.6984 0.1827 0.0803 0.056 Uiso 1 1 calc R . . C20 C 0.6357(6) 0.1541(5) 0.2008(3) 0.046(2) Uani 1 1 d . . . H20 H 0.6025 0.0926 0.2073 0.055 Uiso 1 1 calc R A . C21 C 0.6753(5) 0.2085(5) 0.2374(3) 0.0378(18) Uani 1 1 d . A . C22 C 0.6843(5) 0.1942(5) 0.2945(3) 0.0380(19) Uani 1 1 d . A . C23 C 0.6517(6) 0.1131(6) 0.3267(3) 0.055(2) Uani 1 1 d . . . H23 H 0.6190 0.0616 0.3121 0.065 Uiso 1 1 calc R A . C24 C 0.6667(6) 0.1064(6) 0.3805(3) 0.062(2) Uani 1 1 d . A . H24 H 0.6438 0.0510 0.4035 0.074 Uiso 1 1 calc R . . C25 C 0.7154(6) 0.1818(6) 0.3998(3) 0.051(2) Uani 1 1 d . . . H25 H 0.7268 0.1788 0.4366 0.062 Uiso 1 1 calc R A . C26 C 0.7475(6) 0.2606(5) 0.3669(3) 0.0434(19) Uani 1 1 d . A . H26 H 0.7811 0.3120 0.3813 0.052 Uiso 1 1 calc R . . C27 C 0.2705(5) 0.7784(5) 0.1291(3) 0.0394(19) Uani 1 1 d . . . H27 H 0.2256 0.7316 0.1177 0.047 Uiso 1 1 calc R . . C28 C 0.3235(6) 0.8387(5) 0.0916(3) 0.046(2) Uani 1 1 d . . . H28 H 0.3169 0.8326 0.0551 0.055 Uiso 1 1 calc R . . C29 C 0.3867(6) 0.9085(6) 0.1076(3) 0.048(2) Uani 1 1 d . . . H29 H 0.4244 0.9510 0.0822 0.058 Uiso 1 1 calc R . . C30 C 0.3946(5) 0.9160(5) 0.1611(4) 0.045(2) Uani 1 1 d . . . H30 H 0.4372 0.9638 0.1732 0.054 Uiso 1 1 calc R . . C31 C 0.3388(5) 0.8522(5) 0.1961(3) 0.0369(18) Uani 1 1 d . . . C32 C 0.3379(5) 0.8516(5) 0.2537(3) 0.039(2) Uani 1 1 d . . . C33 C 0.3816(5) 0.9096(5) 0.2876(3) 0.043(2) Uani 1 1 d . . . H33 H 0.4239 0.9651 0.2786 0.052 Uiso 1 1 calc R . . C34 C 0.3797(6) 0.8998(5) 0.3875(3) 0.049(2) Uani 1 1 d . . . H34A H 0.3159 0.9135 0.4085 0.059 Uiso 1 1 calc R . . H34B H 0.4202 0.9607 0.3817 0.059 Uiso 1 1 calc R . . C35 C 0.4441(5) 0.8192(5) 0.4181(3) 0.0408(19) Uani 1 1 d . . . C36 C 0.3978(6) 0.7575(6) 0.4599(3) 0.046(2) Uani 1 1 d . . . H36 H 0.3274 0.7694 0.4703 0.055 Uiso 1 1 calc R . . C37 C 0.4523(6) 0.6803(6) 0.4860(3) 0.046(2) Uani 1 1 d . . . H37 H 0.4197 0.6392 0.5140 0.056 Uiso 1 1 calc R . . C38 C 0.5576(6) 0.6623(5) 0.4708(3) 0.0398(19) Uani 1 1 d . . . C39 C 0.6151(6) 0.5810(6) 0.4936(3) 0.048(2) Uani 1 1 d . . . H39 H 0.5848 0.5388 0.5219 0.058 Uiso 1 1 calc R . . C40 C 0.7145(6) 0.5616(5) 0.4757(3) 0.044(2) Uani 1 1 d . . . H40 H 0.7520 0.5057 0.4911 0.053 Uiso 1 1 calc R . . C41 C 0.7607(5) 0.6248(5) 0.4342(3) 0.0367(18) Uani 1 1 d . . . C42 C 0.7081(5) 0.7048(5) 0.4112(3) 0.0347(18) Uani 1 1 d . . . H42 H 0.7406 0.7469 0.3835 0.042 Uiso 1 1 calc R . . C43 C 0.6051(5) 0.7250(5) 0.4284(3) 0.0355(18) Uani 1 1 d . . . C44 C 0.5464(5) 0.8046(5) 0.4034(3) 0.0382(18) Uani 1 1 d . . . H44 H 0.5782 0.8484 0.3763 0.046 Uiso 1 1 calc R . . C45 C 0.8695(5) 0.5990(5) 0.4133(3) 0.0403(19) Uani 1 1 d . . . H45A H 0.9141 0.6571 0.4115 0.048 Uiso 1 1 calc R . . H45B H 0.9010 0.5460 0.4378 0.048 Uiso 1 1 calc R . . C46 C 0.8846(5) 0.6177(5) 0.3136(3) 0.0357(18) Uani 1 1 d . . . H46 H 0.9082 0.6832 0.3074 0.043 Uiso 1 1 calc R A . C47 C 0.8645(5) 0.5563(5) 0.2765(3) 0.0340(18) Uani 1 1 d . A . C48 C 0.8706(5) 0.5621(5) 0.2177(3) 0.0321(17) Uani 1 1 d . A . C49 C 0.9097(5) 0.6395(5) 0.1853(3) 0.0339(17) Uani 1 1 d . . . H49 H 0.9326 0.6962 0.1993 0.041 Uiso 1 1 calc R A . C50 C 0.9150(5) 0.6332(5) 0.1326(3) 0.0352(18) Uani 1 1 d . A . H50 H 0.9430 0.6852 0.1088 0.042 Uiso 1 1 calc R . . C51 C 0.8788(5) 0.5493(5) 0.1136(3) 0.0358(18) Uani 1 1 d . . . H51 H 0.8819 0.5441 0.0767 0.043 Uiso 1 1 calc R A . C52 C 0.8395(5) 0.4758(5) 0.1474(3) 0.0353(18) Uani 1 1 d . A . H52 H 0.8152 0.4190 0.1339 0.042 Uiso 1 1 calc R . . C53 C 0.4457(11) 0.6181(8) 0.2189(5) 0.111(4) Uani 1 1 d . . . H53 H 0.4757 0.6775 0.2261 0.133 Uiso 1 1 calc R . . C54 C 0.4608(10) 0.4874(7) 0.1620(4) 0.117(5) Uani 1 1 d . . . H54A H 0.4253 0.5035 0.1286 0.175 Uiso 1 1 calc R . . H54B H 0.4120 0.4566 0.1889 0.175 Uiso 1 1 calc R . . H54C H 0.5192 0.4420 0.1567 0.175 Uiso 1 1 calc R . . C55 C 0.5804(10) 0.6155(10) 0.1553(4) 0.137(5) Uani 1 1 d . . . H55A H 0.6406 0.5704 0.1585 0.206 Uiso 1 1 calc R . . H55B H 0.5944 0.6739 0.1725 0.206 Uiso 1 1 calc R . . H55C H 0.5676 0.6349 0.1178 0.206 Uiso 1 1 calc R . . N18A N 0.4848(15) 0.4662(16) 0.3301(8) 0.077(4) Uani 0.577(18) 1 d PD A 1 C56A C 0.5420(13) 0.4272(11) 0.2877(6) 0.072(7) Uani 0.577(18) 1 d PD A 1 H56A H 0.5129 0.3708 0.2760 0.086 Uiso 0.577(18) 1 calc PR A 1 C57A C 0.5287(17) 0.5478(16) 0.3493(7) 0.076(7) Uani 0.577(18) 1 d PD A 1 H57A H 0.5861 0.5721 0.3254 0.113 Uiso 0.577(18) 1 calc PR A 1 H57B H 0.5549 0.5283 0.3847 0.113 Uiso 0.577(18) 1 calc PR A 1 H57C H 0.4755 0.5998 0.3511 0.113 Uiso 0.577(18) 1 calc PR A 1 C58A C 0.3951(18) 0.4212(16) 0.3506(11) 0.092(6) Uani 0.577(18) 1 d PD A 1 H58A H 0.3835 0.3631 0.3327 0.138 Uiso 0.577(18) 1 calc PR A 1 H58B H 0.3359 0.4671 0.3452 0.138 Uiso 0.577(18) 1 calc PR A 1 H58C H 0.4021 0.4016 0.3886 0.138 Uiso 0.577(18) 1 calc PR A 1 N18B N 0.491(2) 0.495(2) 0.3275(12) 0.077(4) Uani 0.423(18) 1 d PD A 2 C56B C 0.5834(17) 0.5067(16) 0.2948(8) 0.116(15) Uani 0.423(18) 1 d PD A 2 H56B H 0.6207 0.5647 0.2976 0.140 Uiso 0.423(18) 1 calc PR A 2 C57B C 0.463(2) 0.5806(16) 0.3533(11) 0.075(9) Uani 0.423(18) 1 d PD A 2 H57D H 0.3867 0.5873 0.3559 0.113 Uiso 0.423(18) 1 calc PR A 2 H57E H 0.4914 0.6390 0.3327 0.113 Uiso 0.423(18) 1 calc PR A 2 H57F H 0.4905 0.5734 0.3889 0.113 Uiso 0.423(18) 1 calc PR A 2 C58B C 0.434(3) 0.412(2) 0.3314(15) 0.092(6) Uani 0.423(18) 1 d PD A 2 H58D H 0.4670 0.3607 0.3559 0.138 Uiso 0.423(18) 1 calc PR A 2 H58E H 0.4309 0.3885 0.2964 0.138 Uiso 0.423(18) 1 calc PR A 2 H58F H 0.3635 0.4255 0.3447 0.138 Uiso 0.423(18) 1 calc PR A 2 C59 C 0.9498(6) 0.2080(7) 0.2643(4) 0.054(2) Uani 1 1 d . A . H59 H 0.9584 0.1913 0.3012 0.065 Uiso 1 1 calc R . . C60 C 0.9390(7) 0.1543(6) 0.1786(3) 0.074(3) Uani 1 1 d . A . H60A H 0.9064 0.2191 0.1698 0.111 Uiso 1 1 calc R . . H60B H 0.8970 0.1043 0.1654 0.111 Uiso 1 1 calc R . . H60C H 1.0089 0.1532 0.1622 0.111 Uiso 1 1 calc R . . C61 C 0.9590(7) 0.0363(5) 0.2581(3) 0.070(3) Uani 1 1 d . A . H61A H 1.0280 0.0113 0.2482 0.105 Uiso 1 1 calc R . . H61B H 0.9057 -0.0048 0.2459 0.105 Uiso 1 1 calc R . . H61C H 0.9526 0.0348 0.2967 0.105 Uiso 1 1 calc R . . P1 P 0.68125(17) 0.85721(16) 0.24376(9) 0.0534(6) Uani 1 1 d . . . F5 F 0.6375(6) 0.8373(5) 0.1903(2) 0.123(2) Uani 1 1 d . . . F2 F 0.6065(5) 0.7777(3) 0.2729(2) 0.0978(19) Uani 1 1 d . . . F3 F 0.7207(5) 0.8796(5) 0.2990(2) 0.110(2) Uani 1 1 d . . . F1 F 0.7521(4) 0.9428(4) 0.2154(2) 0.0853(16) Uani 1 1 d . . . F4 F 0.5936(4) 0.9372(3) 0.2507(3) 0.111(2) Uani 1 1 d . . . F6 F 0.7668(6) 0.7819(5) 0.2384(4) 0.191(4) Uani 1 1 d . . . P2 P 0.93150(14) 0.27312(13) 0.01768(8) 0.0363(5) Uani 1 1 d . . . F7 F 0.8589(3) 0.3286(3) 0.05666(17) 0.0608(13) Uani 1 1 d . . . F8 F 0.8765(3) 0.1720(3) 0.03791(16) 0.0536(12) Uani 1 1 d . . . F9 F 1.0046(3) 0.2171(3) -0.02151(16) 0.0530(12) Uani 1 1 d . . . F10 F 0.9871(3) 0.3733(3) -0.00243(16) 0.0493(11) Uani 1 1 d . . . F11 F 0.8483(3) 0.2954(3) -0.02724(16) 0.0572(12) Uani 1 1 d . . . F12 F 1.0130(3) 0.2514(3) 0.06254(17) 0.0621(13) Uani 1 1 d . . . P3 P 1.2910(2) 0.17864(16) 0.25569(9) 0.0624(7) Uani 1 1 d . . . F13 F 1.2318(6) 0.2396(5) 0.2951(2) 0.157(3) Uani 1 1 d . . . F14 F 1.2297(4) 0.0827(4) 0.2740(2) 0.0973(19) Uani 1 1 d . . . F15 F 1.3557(3) 0.1196(3) 0.21442(18) 0.0679(14) Uani 1 1 d . . . F16 F 1.3567(5) 0.2726(4) 0.2332(3) 0.115(2) Uani 1 1 d . . . F17 F 1.2083(4) 0.2118(3) 0.21175(18) 0.0717(14) Uani 1 1 d . . . F18 F 1.3753(5) 0.1459(4) 0.2981(2) 0.112(2) Uani 1 1 d . . . P4 P 1.07086(15) 0.73057(14) 0.50422(8) 0.0414(5) Uani 1 1 d . . . F19 F 1.1238(3) 0.8355(3) 0.49918(16) 0.0520(11) Uani 1 1 d . . . F20 F 1.0405(3) 0.7409(3) 0.56530(15) 0.0487(11) Uani 1 1 d . . . F21 F 1.0184(3) 0.6253(3) 0.50983(16) 0.0554(12) Uani 1 1 d . . . F22 F 1.1008(3) 0.7210(3) 0.44400(15) 0.0565(12) Uani 1 1 d . . . F23 F 0.9631(3) 0.7808(3) 0.48719(17) 0.0616(13) Uani 1 1 d . . . F24 F 1.1787(3) 0.6795(3) 0.52221(16) 0.0525(12) Uani 1 1 d . . . O5 O 0.6123(4) 1.0281(4) 0.0277(2) 0.0586(15) Uani 1 1 d . . . N20 N 0.7089(5) 0.8913(4) 0.0518(2) 0.0446(16) Uani 1 1 d . . . C62 C 0.6290(6) 0.9415(6) 0.0295(3) 0.049(2) Uani 1 1 d . . . H62 H 0.5800 0.9048 0.0133 0.058 Uiso 1 1 calc R . . C63 C 0.7853(6) 0.9386(5) 0.0784(3) 0.056(2) Uani 1 1 d . . . H63A H 0.7900 1.0073 0.0632 0.084 Uiso 1 1 calc R . . H63B H 0.8528 0.9054 0.0742 0.084 Uiso 1 1 calc R . . H63C H 0.7656 0.9357 0.1161 0.084 Uiso 1 1 calc R . . C64 C 0.7212(7) 0.7860(6) 0.0530(4) 0.079(3) Uani 1 1 d . . . H64A H 0.6638 0.7604 0.0347 0.118 Uiso 1 1 calc R . . H64B H 0.7208 0.7560 0.0898 0.118 Uiso 1 1 calc R . . H64C H 0.7873 0.7703 0.0353 0.118 Uiso 1 1 calc R . . O6 O -0.0210(5) 0.8178(4) 0.3397(2) 0.0602(17) Uani 1 1 d . . . N21 N -0.0049(6) 0.9470(5) 0.3872(3) 0.0544(18) Uani 1 1 d . . . C65 C -0.0613(11) 0.8762(9) 0.3708(5) 0.038(4) Uiso 0.576(16) 1 d P B 1 H65 H -0.1319 0.8693 0.3824 0.046 Uiso 0.576(16) 1 calc PR B 1 C66 C 0.1033(10) 0.9531(11) 0.3717(6) 0.061(5) Uani 0.576(16) 1 d P B 1 H66A H 0.1183 0.9124 0.3430 0.092 Uiso 0.576(16) 1 calc PR B 1 H66B H 0.1456 0.9297 0.4021 0.092 Uiso 0.576(16) 1 calc PR B 1 H66C H 0.1200 1.0214 0.3596 0.092 Uiso 0.576(16) 1 calc PR B 1 C67 C -0.0472(15) 1.0108(11) 0.4243(7) 0.058(5) Uani 0.576(16) 1 d P B 1 H67A H -0.1231 1.0061 0.4264 0.087 Uiso 0.576(16) 1 calc PR B 1 H67B H -0.0281 1.0786 0.4125 0.087 Uiso 0.576(16) 1 calc PR B 1 H67C H -0.0192 0.9908 0.4593 0.087 Uiso 0.576(16) 1 calc PR B 1 C65A C 0.033(2) 0.8784(16) 0.3599(9) 0.074(10) Uani 0.424(16) 1 d P B 2 H65A H 0.1061 0.8738 0.3550 0.089 Uiso 0.424(16) 1 calc PR B 2 C66A C -0.115(2) 0.9486(18) 0.4012(11) 0.120(15) Uani 0.424(16) 1 d P B 2 H66D H -0.1550 0.9607 0.3690 0.181 Uiso 0.424(16) 1 calc PR B 2 H66E H -0.1304 1.0010 0.4237 0.181 Uiso 0.424(16) 1 calc PR B 2 H66F H -0.1343 0.8853 0.4205 0.181 Uiso 0.424(16) 1 calc PR B 2 C67A C 0.060(3) 1.0162(19) 0.4155(11) 0.128(15) Uani 0.424(16) 1 d P B 2 H67D H 0.0433 1.0059 0.4536 0.192 Uiso 0.424(16) 1 calc PR B 2 H67E H 0.0429 1.0843 0.4020 0.192 Uiso 0.424(16) 1 calc PR B 2 H67F H 0.1336 1.0025 0.4089 0.192 Uiso 0.424(16) 1 calc PR B 2 O7 O 0.6688(9) 0.9981(7) 0.4948(4) 0.158(4) Uani 1 1 d . . . N22 N 0.6815(7) 0.8587(5) 0.5482(3) 0.071(2) Uani 1 1 d . . . C68 C 0.704(2) 0.9282(11) 0.5136(6) 0.278(16) Uani 1 1 d . . . H68 H 0.7717 0.9182 0.4990 0.333 Uiso 1 1 calc R . . C69 C 0.5778(7) 0.8516(8) 0.5663(4) 0.105(4) Uani 1 1 d . . . H69A H 0.5357 0.9025 0.5463 0.158 Uiso 1 1 calc R . . H69B H 0.5729 0.8604 0.6039 0.158 Uiso 1 1 calc R . . H69C H 0.5520 0.7869 0.5612 0.158 Uiso 1 1 calc R . . C70 C 0.7480(8) 0.7794(8) 0.5676(4) 0.105(4) Uani 1 1 d . . . H70A H 0.8202 0.7952 0.5574 0.158 Uiso 1 1 calc R . . H70B H 0.7289 0.7199 0.5526 0.158 Uiso 1 1 calc R . . H70C H 0.7405 0.7685 0.6063 0.158 Uiso 1 1 calc R . . O8 O 0.0654(4) 0.9120(4) 0.1583(2) 0.0644(17) Uani 1 1 d . . . N23 N 0.1460(5) 1.0262(4) 0.1008(3) 0.0456(16) Uani 1 1 d . . . C71 C 0.1240(7) 0.9798(6) 0.1487(4) 0.058(2) Uani 1 1 d . . . H71 H 0.1572 1.0019 0.1778 0.070 Uiso 1 1 calc R . . C72 C 0.1006(6) 0.9977(5) 0.0536(3) 0.053(2) Uani 1 1 d . . . H72A H 0.0477 0.9484 0.0637 0.080 Uiso 1 1 calc R . . H72B H 0.1550 0.9701 0.0314 0.080 Uiso 1 1 calc R . . H72C H 0.0685 1.0554 0.0338 0.080 Uiso 1 1 calc R . . C73 C 0.2176(6) 1.1069(5) 0.0931(3) 0.055(2) Uani 1 1 d . . . H73A H 0.2442 1.1191 0.1273 0.082 Uiso 1 1 calc R . . H73B H 0.1813 1.1660 0.0771 0.082 Uiso 1 1 calc R . . H73C H 0.2757 1.0903 0.0695 0.082 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 0.0366(6) 0.0365(6) 0.0354(7) -0.0104(5) 0.0004(5) -0.0077(5) Cu2 0.0336(6) 0.0404(6) 0.0361(7) -0.0110(5) -0.0018(5) -0.0061(5) O1 0.036(3) 0.038(3) 0.039(4) -0.005(3) 0.004(3) -0.003(3) O2 0.036(3) 0.072(5) 0.095(5) -0.041(4) 0.002(3) -0.001(3) O3 0.028(3) 0.071(4) 0.102(5) -0.020(4) 0.023(3) -0.011(3) O4 0.035(3) 0.036(3) 0.070(4) 0.000(3) 0.000(3) -0.005(3) N1 0.032(3) 0.033(3) 0.030(4) -0.006(3) 0.006(3) -0.003(3) N2 0.031(3) 0.035(3) 0.031(4) -0.013(3) 0.000(3) -0.008(3) N3 0.037(4) 0.042(4) 0.035(4) -0.019(3) -0.007(3) -0.004(3) N4 0.032(4) 0.036(4) 0.051(5) -0.011(3) -0.003(3) -0.002(3) N5 0.031(3) 0.043(4) 0.049(5) -0.023(4) -0.006(3) 0.006(3) N6 0.033(4) 0.046(4) 0.038(4) -0.020(3) -0.004(3) -0.005(3) N7 0.027(3) 0.039(4) 0.037(4) -0.013(3) -0.003(3) 0.003(3) N8 0.023(3) 0.047(4) 0.044(4) -0.011(3) 0.009(3) -0.004(3) N9 0.037(4) 0.040(4) 0.031(4) -0.010(3) 0.003(3) 0.003(3) N10 0.030(3) 0.028(3) 0.037(4) -0.015(3) -0.007(3) 0.003(3) N11 0.030(3) 0.042(4) 0.044(4) -0.020(3) -0.007(3) 0.001(3) N12 0.031(4) 0.030(3) 0.066(5) -0.018(3) -0.014(3) 0.000(3) N13 0.024(3) 0.043(4) 0.039(4) -0.012(3) -0.008(3) 0.000(3) N14 0.034(4) 0.045(4) 0.033(4) -0.017(3) -0.006(3) -0.004(3) N15 0.027(3) 0.038(4) 0.028(4) -0.015(3) -0.008(3) 0.005(3) N16 0.021(3) 0.039(3) 0.036(4) -0.006(3) -0.003(3) 0.000(3) N17 0.084(6) 0.098(6) 0.055(5) -0.028(5) 0.003(5) -0.012(5) N19 0.060(5) 0.039(4) 0.053(5) -0.003(4) 0.005(4) 0.003(3) C1 0.031(4) 0.046(5) 0.021(4) -0.009(4) 0.004(3) 0.000(4) C2 0.033(4) 0.051(5) 0.031(5) -0.005(4) -0.006(4) 0.002(4) C3 0.036(5) 0.052(5) 0.035(5) 0.010(4) -0.001(4) -0.003(4) C4 0.032(4) 0.032(4) 0.054(6) 0.002(4) 0.002(4) -0.005(3) C5 0.025(4) 0.033(4) 0.041(5) -0.017(4) -0.009(3) 0.003(3) C6 0.028(4) 0.027(4) 0.048(5) -0.006(4) -0.001(4) 0.000(3) C7 0.026(4) 0.031(4) 0.055(6) -0.017(4) -0.002(4) -0.009(3) C8 0.039(4) 0.044(4) 0.039(5) -0.028(4) -0.008(4) 0.001(4) C9 0.025(4) 0.030(4) 0.051(5) -0.017(4) -0.007(4) -0.005(3) C10 0.043(5) 0.040(5) 0.058(6) -0.010(4) -0.013(4) 0.005(4) C11 0.050(5) 0.041(4) 0.039(5) -0.003(4) -0.007(4) -0.004(4) C12 0.044(5) 0.036(4) 0.051(6) -0.013(4) -0.008(4) 0.006(4) C13 0.045(5) 0.046(5) 0.052(5) -0.011(4) 0.009(4) 0.002(4) C14 0.032(5) 0.053(5) 0.061(6) -0.019(5) 0.011(4) -0.008(4) C15 0.033(5) 0.037(4) 0.050(5) -0.020(4) -0.010(4) -0.001(4) C16 0.033(4) 0.040(4) 0.044(5) -0.018(4) -0.003(4) -0.007(4) C17 0.032(4) 0.031(4) 0.051(5) -0.014(4) -0.006(4) -0.007(4) C18 0.028(4) 0.041(4) 0.033(4) -0.011(4) -0.003(4) -0.004(4) C19 0.030(4) 0.052(5) 0.064(6) -0.030(4) -0.005(4) 0.002(4) C20 0.041(5) 0.034(4) 0.063(6) -0.004(4) -0.004(4) -0.005(4) C21 0.034(4) 0.041(5) 0.041(5) -0.012(4) -0.007(4) 0.001(4) C22 0.031(4) 0.040(5) 0.044(5) -0.009(4) -0.007(4) -0.001(4) C23 0.070(6) 0.045(5) 0.049(6) 0.000(4) -0.016(5) -0.020(4) C24 0.069(6) 0.061(6) 0.053(6) 0.012(5) -0.016(5) -0.024(5) C25 0.064(6) 0.048(5) 0.040(5) 0.007(4) -0.012(4) 0.000(5) C26 0.049(5) 0.050(5) 0.030(5) -0.001(4) -0.003(4) -0.002(4) C27 0.042(5) 0.034(4) 0.041(5) -0.001(4) 0.011(4) -0.002(4) C28 0.055(5) 0.050(5) 0.033(5) -0.005(4) 0.007(4) 0.006(4) C29 0.033(5) 0.052(5) 0.058(6) 0.001(5) 0.004(4) 0.010(4) C30 0.022(4) 0.039(5) 0.074(7) -0.010(4) 0.003(4) -0.007(4) C31 0.027(4) 0.039(4) 0.048(6) -0.019(4) -0.005(4) -0.002(4) C32 0.025(4) 0.019(4) 0.075(7) -0.005(4) -0.009(4) -0.005(3) C33 0.032(4) 0.034(4) 0.063(6) -0.001(4) -0.001(4) -0.008(4) C34 0.045(5) 0.043(5) 0.067(6) -0.028(4) -0.025(4) 0.006(4) C35 0.030(4) 0.048(5) 0.049(5) -0.024(4) -0.009(4) 0.007(4) C36 0.033(5) 0.059(5) 0.051(6) -0.029(5) -0.001(4) -0.004(4) C37 0.043(5) 0.054(5) 0.044(5) -0.015(4) 0.008(4) -0.005(4) C38 0.043(5) 0.041(5) 0.037(5) -0.011(4) -0.010(4) 0.000(4) C39 0.038(5) 0.058(5) 0.049(5) -0.007(4) 0.004(4) -0.001(4) C40 0.055(5) 0.041(5) 0.038(5) -0.003(4) -0.017(4) 0.004(4) C41 0.041(5) 0.040(4) 0.032(5) -0.016(4) -0.010(4) -0.002(4) C42 0.035(4) 0.042(4) 0.029(4) -0.010(4) -0.004(4) -0.005(4) C43 0.033(4) 0.038(4) 0.037(5) -0.013(4) -0.004(4) 0.000(4) C44 0.034(5) 0.044(4) 0.039(5) -0.010(4) -0.012(4) -0.004(4) C45 0.041(5) 0.052(5) 0.031(5) -0.017(4) -0.010(4) 0.000(4) C46 0.019(4) 0.031(4) 0.058(6) -0.011(4) -0.003(4) 0.000(3) C47 0.030(4) 0.029(4) 0.046(5) -0.017(4) -0.005(4) 0.001(3) C48 0.031(4) 0.036(4) 0.032(5) -0.011(4) -0.006(3) 0.004(4) C49 0.033(4) 0.036(4) 0.033(5) -0.007(4) -0.005(4) 0.001(3) C50 0.024(4) 0.046(5) 0.034(5) 0.003(4) -0.001(3) -0.006(3) C51 0.028(4) 0.050(5) 0.031(5) -0.015(4) -0.005(3) 0.004(4) C52 0.033(4) 0.051(5) 0.022(5) -0.008(4) 0.006(3) -0.007(4) C53 0.142(13) 0.076(8) 0.119(12) -0.023(8) -0.048(10) 0.026(9) C54 0.202(14) 0.096(8) 0.061(7) -0.023(6) -0.016(8) -0.083(9) C55 0.130(11) 0.220(15) 0.074(9) -0.060(9) 0.017(8) -0.089(11) N18A 0.098(7) 0.100(14) 0.035(5) -0.015(8) 0.019(5) -0.029(8) C56A 0.100(17) 0.054(11) 0.056(13) 0.022(9) -0.031(12) 0.003(11) C57A 0.097(17) 0.096(16) 0.044(11) -0.050(11) 0.015(12) -0.034(14) C58A 0.094(18) 0.094(10) 0.096(19) -0.058(11) 0.052(11) -0.025(12) N18B 0.098(7) 0.100(14) 0.035(5) -0.015(8) 0.019(5) -0.029(8) C56B 0.16(3) 0.07(2) 0.12(3) 0.02(2) -0.07(3) -0.05(2) C57B 0.10(2) 0.062(16) 0.071(19) -0.036(14) 0.024(18) -0.011(16) C58B 0.094(18) 0.094(10) 0.096(19) -0.058(11) 0.052(11) -0.025(12) C59 0.041(5) 0.061(6) 0.061(6) -0.008(5) 0.005(4) -0.004(5) C60 0.086(7) 0.075(6) 0.063(7) -0.017(5) -0.008(6) 0.032(6) C61 0.093(7) 0.046(5) 0.068(7) 0.009(5) 0.002(5) -0.010(5) P1 0.0492(14) 0.0583(14) 0.0522(15) -0.0060(12) -0.0030(12) 0.0080(12) F5 0.179(7) 0.137(5) 0.058(4) -0.013(4) -0.023(4) -0.052(5) F2 0.146(5) 0.059(3) 0.088(4) -0.005(3) 0.009(4) -0.033(3) F3 0.124(5) 0.144(5) 0.061(4) 0.005(4) -0.017(3) -0.049(4) F1 0.064(3) 0.106(4) 0.081(4) 0.011(3) 0.012(3) -0.026(3) F4 0.065(4) 0.053(3) 0.214(7) -0.018(4) 0.027(4) -0.004(3) F6 0.120(6) 0.153(6) 0.290(11) -0.022(7) 0.046(7) 0.084(5) P2 0.0357(11) 0.0368(11) 0.0374(12) -0.0077(9) -0.0018(10) -0.0063(9) F7 0.079(3) 0.049(3) 0.055(3) -0.018(2) 0.020(2) 0.005(2) F8 0.055(3) 0.048(3) 0.059(3) -0.012(2) 0.016(2) -0.020(2) F9 0.054(3) 0.045(2) 0.059(3) -0.010(2) 0.015(2) 0.006(2) F10 0.060(3) 0.036(2) 0.051(3) 0.002(2) 0.003(2) -0.014(2) F11 0.052(3) 0.066(3) 0.057(3) -0.018(2) -0.021(2) 0.003(2) F12 0.076(3) 0.051(3) 0.061(3) -0.002(2) -0.036(3) -0.007(2) P3 0.0891(18) 0.0474(14) 0.0519(16) -0.0127(12) -0.0097(14) 0.0170(14) F13 0.272(9) 0.144(5) 0.055(4) -0.042(4) -0.022(5) 0.147(6) F14 0.082(4) 0.085(4) 0.110(5) 0.039(3) 0.029(3) 0.026(3) F15 0.072(3) 0.061(3) 0.072(3) -0.015(3) 0.004(3) 0.009(3) F16 0.151(6) 0.058(3) 0.141(6) -0.013(4) -0.053(5) -0.008(4) F17 0.093(4) 0.061(3) 0.061(3) -0.005(3) -0.022(3) 0.026(3) F18 0.151(6) 0.107(4) 0.085(4) -0.040(4) -0.071(4) 0.050(4) P4 0.0402(12) 0.0475(12) 0.0372(13) -0.0074(10) 0.0004(10) -0.0025(10) F19 0.061(3) 0.042(2) 0.052(3) -0.001(2) -0.002(2) -0.011(2) F20 0.060(3) 0.053(3) 0.035(3) -0.015(2) 0.007(2) -0.006(2) F21 0.072(3) 0.052(3) 0.044(3) -0.012(2) -0.005(2) -0.021(2) F22 0.074(3) 0.064(3) 0.032(3) -0.013(2) 0.010(2) -0.004(2) F23 0.044(3) 0.077(3) 0.063(3) -0.002(3) -0.006(2) 0.009(2) F24 0.049(3) 0.053(3) 0.055(3) -0.006(2) 0.003(2) 0.006(2) O5 0.059(4) 0.052(4) 0.069(4) -0.023(3) -0.016(3) 0.005(3) N20 0.045(4) 0.043(4) 0.047(4) -0.005(3) 0.000(3) -0.014(3) C62 0.040(5) 0.054(6) 0.055(6) -0.014(5) 0.001(4) -0.006(5) C63 0.054(5) 0.049(5) 0.068(6) -0.013(5) -0.001(5) -0.012(4) C64 0.090(7) 0.042(5) 0.103(8) 0.003(5) -0.010(6) -0.012(5) O6 0.094(5) 0.042(3) 0.047(4) -0.012(3) -0.006(3) -0.004(3) N21 0.068(5) 0.044(4) 0.051(5) -0.007(4) -0.008(4) 0.007(4) C66 0.030(9) 0.067(11) 0.091(13) -0.019(10) -0.009(8) -0.016(8) C67 0.076(13) 0.040(9) 0.062(11) -0.028(8) 0.017(10) 0.011(9) C65A 0.10(2) 0.053(16) 0.066(17) 0.013(13) 0.003(15) 0.056(17) C66A 0.17(3) 0.058(18) 0.11(3) 0.034(18) 0.07(2) 0.06(2) C67A 0.22(4) 0.09(2) 0.08(2) -0.046(18) -0.05(3) 0.05(3) O7 0.261(12) 0.103(7) 0.105(7) 0.031(6) -0.011(7) -0.059(8) N22 0.104(7) 0.056(5) 0.050(5) 0.007(4) -0.007(5) 0.006(5) C68 0.67(5) 0.067(10) 0.097(13) 0.010(10) 0.04(2) -0.100(19) C69 0.058(7) 0.152(11) 0.122(10) -0.084(9) -0.013(7) 0.006(7) C70 0.077(8) 0.135(10) 0.106(9) -0.029(8) 0.003(7) 0.025(8) O8 0.064(4) 0.051(4) 0.073(4) 0.009(3) 0.019(3) 0.001(3) N23 0.044(4) 0.044(4) 0.046(5) 0.005(4) 0.001(3) 0.003(3) C71 0.054(6) 0.048(6) 0.073(7) -0.011(5) -0.002(5) 0.022(5) C72 0.069(6) 0.045(5) 0.048(5) -0.012(4) -0.012(5) -0.007(4) C73 0.058(5) 0.047(5) 0.060(6) -0.009(4) -0.005(5) -0.008(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 N10 2.014(5) . ? Cu1 N2 2.016(5) . ? Cu1 N9 2.027(6) . ? Cu1 N1 2.035(5) . ? Cu1 O1 2.252(5) . ? Cu1 O3 2.368(6) . ? Cu2 N15 1.983(5) . ? Cu2 N7 2.000(6) . ? Cu2 N16 2.039(5) . ? Cu2 N8 2.040(6) . ? Cu2 O2 2.259(5) . ? Cu2 O4 2.421(5) . ? O1 H1W 0.82(2) . ? O1 H2W 0.81(2) . ? O2 C56B 1.197(18) . ? O2 C56A 1.203(15) . ? O3 C53 1.208(14) . ? O4 C59 1.209(9) . ? N1 C1 1.334(8) . ? N1 C5 1.356(8) . ? N2 N3 1.318(7) . ? N2 C6 1.339(8) . ? N3 N4 1.331(7) . ? N4 C7 1.350(8) . ? N4 C8 1.456(8) . ? N5 C20 1.322(9) . ? N5 N6 1.334(7) . ? N5 C19 1.464(9) . ? N6 N7 1.316(7) . ? N7 C21 1.338(8) . ? N8 C26 1.357(8) . ? N8 C22 1.360(8) . ? N9 C31 1.337(8) . ? N9 C27 1.359(8) . ? N10 N11 1.317(7) . ? N10 C32 1.344(8) . ? N11 N12 1.324(7) . ? N12 C33 1.335(9) . ? N12 C34 1.478(9) . ? N13 C46 1.330(8) . ? N13 N14 1.335(7) . ? N13 C45 1.473(8) . ? N14 N15 1.333(7) . ? N15 C47 1.358(8) . ? N16 C48 1.344(8) . ? N16 C52 1.354(8) . ? N17 C55 1.331(12) . ? N17 C54 1.367(10) . ? N17 C53 1.412(13) . ? N19 C59 1.337(9) . ? N19 C60 1.415(10) . ? N19 C61 1.425(9) . ? C1 C2 1.358(9) . ? C1 H1A 0.9500 . ? C2 C3 1.367(9) . ? C2 H2 0.9500 . ? C3 C4 1.387(9) . ? C3 H3 0.9500 . ? C4 C5 1.373(9) . ? C4 H4 0.9500 . ? C5 C6 1.482(9) . ? C6 C7 1.370(9) . ? C7 H7 0.9500 . ? C8 C9 1.499(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C18 1.368(9) . ? C9 C10 1.396(9) . ? C10 C11 1.363(10) . ? C10 H10 0.9500 . ? C11 C12 1.399(9) . ? C11 H11 0.9500 . ? C12 C13 1.408(10) . ? C12 C17 1.441(10) . ? C13 C14 1.341(10) . ? C13 H13 0.9500 . ? C14 C15 1.414(10) . ? C14 H14 0.9500 . ? C15 C16 1.371(9) . ? C15 C19 1.516(9) . ? C16 C17 1.410(9) . ? C16 H16 0.9500 . ? C17 C18 1.407(9) . ? C18 H18 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.376(9) . ? C20 H20 0.9500 . ? C21 C22 1.455(10) . ? C22 C23 1.370(10) . ? C23 C24 1.382(10) . ? C23 H23 0.9500 . ? C24 C25 1.370(10) . ? C24 H24 0.9500 . ? C25 C26 1.354(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.364(9) . ? C27 H27 0.9500 . ? C28 C29 1.377(10) . ? C28 H28 0.9500 . ? C29 C30 1.385(10) . ? C29 H29 0.9500 . ? C30 C31 1.373(9) . ? C30 H30 0.9500 . ? C31 C32 1.464(10) . ? C32 C33 1.381(9) . ? C33 H33 0.9500 . ? C34 C35 1.524(9) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C44 1.374(9) . ? C35 C36 1.407(10) . ? C36 C37 1.376(10) . ? C36 H36 0.9500 . ? C37 C38 1.420(10) . ? C37 H37 0.9500 . ? C38 C39 1.405(10) . ? C38 C43 1.431(9) . ? C39 C40 1.373(10) . ? C39 H39 0.9500 . ? C40 C41 1.413(9) . ? C40 H40 0.9500 . ? C41 C42 1.361(9) . ? C41 C45 1.529(9) . ? C42 C43 1.414(9) . ? C42 H42 0.9500 . ? C43 C44 1.416(9) . ? C44 H44 0.9500 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.371(9) . ? C46 H46 0.9500 . ? C47 C48 1.488(9) . ? C48 C49 1.364(9) . ? C49 C50 1.354(9) . ? C49 H49 0.9500 . ? C50 C51 1.394(9) . ? C50 H50 0.9500 . ? C51 C52 1.346(9) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53 0.9500 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? N18A C58A 1.382(13) . ? N18A C57A 1.411(16) . ? N18A C56A 1.43(2) . ? C56A H56A 0.9500 . ? C57A H57A 0.9800 . ? C57A H57B 0.9800 . ? C57A H57C 0.9800 . ? C58A H58A 0.9800 . ? C58A H58B 0.9800 . ? C58A H58C 0.9800 . ? N18B C58B 1.37(2) . ? N18B C56B 1.43(2) . ? N18B C57B 1.44(3) . ? C56B H56B 0.9500 . ? C57B H57D 0.9800 . ? C57B H57E 0.9800 . ? C57B H57F 0.9800 . ? C58B H58D 0.9800 . ? C58B H58E 0.9800 . ? C58B H58F 0.9800 . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? P1 F6 1.505(6) . ? P1 F5 1.547(6) . ? P1 F4 1.575(5) . ? P1 F2 1.576(5) . ? P1 F3 1.576(6) . ? P1 F1 1.596(5) . ? P2 F12 1.577(4) . ? P2 F7 1.584(4) . ? P2 F10 1.590(4) . ? P2 F11 1.594(4) . ? P2 F9 1.594(4) . ? P2 F8 1.598(4) . ? P3 F13 1.547(5) . ? P3 F14 1.569(6) . ? P3 F18 1.579(5) . ? P3 F17 1.593(5) . ? P3 F15 1.598(5) . ? P3 F16 1.599(6) . ? P4 F22 1.586(4) . ? P4 F23 1.587(4) . ? P4 F24 1.598(4) . ? P4 F19 1.599(4) . ? P4 F21 1.599(4) . ? P4 F20 1.611(4) . ? O5 C62 1.199(8) . ? N20 C62 1.332(9) . ? N20 C63 1.424(9) . ? N20 C64 1.447(9) . ? C62 H62 0.9500 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? O6 C65A 1.26(3) . ? O6 C65 1.277(14) . ? N21 C65A 1.31(2) . ? N21 C65 1.340(14) . ? N21 C66 1.437(14) . ? N21 C67 1.443(15) . ? N21 C66A 1.45(3) . ? N21 C67A 1.53(3) . ? C65 H65 0.9500 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C65A H65A 0.9500 . ? C66A H66D 0.9800 . ? C66A H66E 0.9800 . ? C66A H66F 0.9800 . ? C67A H67D 0.9800 . ? C67A H67E 0.9800 . ? C67A H67F 0.9800 . ? O7 C68 1.116(19) . ? N22 C68 1.254(15) . ? N22 C69 1.399(11) . ? N22 C70 1.423(11) . ? C68 H68 0.9500 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? O8 C71 1.210(9) . ? N23 C71 1.333(10) . ? N23 C73 1.450(9) . ? N23 C72 1.453(9) . ? C71 H71 0.9500 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 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 N10 Cu1 N2 170.5(2) . . ? N10 Cu1 N9 80.3(2) . . ? N2 Cu1 N9 98.7(2) . . ? N10 Cu1 N1 98.7(2) . . ? N2 Cu1 N1 81.6(2) . . ? N9 Cu1 N1 175.1(2) . . ? N10 Cu1 O1 91.42(19) . . ? N2 Cu1 O1 98.1(2) . . ? N9 Cu1 O1 93.4(2) . . ? N1 Cu1 O1 91.38(19) . . ? N10 Cu1 O3 86.9(2) . . ? N2 Cu1 O3 83.6(2) . . ? N9 Cu1 O3 89.9(2) . . ? N1 Cu1 O3 85.3(2) . . ? O1 Cu1 O3 176.0(2) . . ? N15 Cu2 N7 175.5(2) . . ? N15 Cu2 N16 81.2(2) . . ? N7 Cu2 N16 98.6(2) . . ? N15 Cu2 N8 99.2(2) . . ? N7 Cu2 N8 81.4(2) . . ? N16 Cu2 N8 175.2(2) . . ? N15 Cu2 O2 87.3(2) . . ? N7 Cu2 O2 88.2(2) . . ? N16 Cu2 O2 94.1(2) . . ? N8 Cu2 O2 90.7(2) . . ? N15 Cu2 O4 94.20(19) . . ? N7 Cu2 O4 90.29(19) . . ? N16 Cu2 O4 85.95(19) . . ? N8 Cu2 O4 89.22(19) . . ? O2 Cu2 O4 178.5(2) . . ? Cu1 O1 H1W 118(6) . . ? Cu1 O1 H2W 119(5) . . ? H1W O1 H2W 107(8) . . ? C56B O2 C56A 63.3(14) . . ? C56B O2 Cu2 133.7(11) . . ? C56A O2 Cu2 130.9(8) . . ? C53 O3 Cu1 121.6(7) . . ? C59 O4 Cu2 118.1(5) . . ? C1 N1 C5 117.6(6) . . ? C1 N1 Cu1 128.0(5) . . ? C5 N1 Cu1 114.4(5) . . ? N3 N2 C6 110.6(5) . . ? N3 N2 Cu1 136.7(5) . . ? C6 N2 Cu1 112.4(5) . . ? N2 N3 N4 106.1(6) . . ? N3 N4 C7 110.9(6) . . ? N3 N4 C8 120.5(6) . . ? C7 N4 C8 128.6(6) . . ? C20 N5 N6 112.4(6) . . ? C20 N5 C19 128.3(7) . . ? N6 N5 C19 119.2(7) . . ? N7 N6 N5 105.2(6) . . ? N6 N7 C21 110.6(6) . . ? N6 N7 Cu2 136.4(5) . . ? C21 N7 Cu2 113.0(5) . . ? C26 N8 C22 117.7(6) . . ? C26 N8 Cu2 128.6(5) . . ? C22 N8 Cu2 113.6(5) . . ? C31 N9 C27 116.5(6) . . ? C31 N9 Cu1 116.6(5) . . ? C27 N9 Cu1 126.9(5) . . ? N11 N10 C32 110.7(6) . . ? N11 N10 Cu1 136.8(5) . . ? C32 N10 Cu1 112.5(5) . . ? N10 N11 N12 105.8(6) . . ? N11 N12 C33 112.2(6) . . ? N11 N12 C34 119.6(7) . . ? C33 N12 C34 128.0(6) . . ? C46 N13 N14 112.4(6) . . ? C46 N13 C45 128.2(6) . . ? N14 N13 C45 119.4(6) . . ? N15 N14 N13 104.9(5) . . ? N14 N15 C47 110.5(5) . . ? N14 N15 Cu2 135.4(5) . . ? C47 N15 Cu2 113.4(5) . . ? C48 N16 C52 117.7(6) . . ? C48 N16 Cu2 115.4(5) . . ? C52 N16 Cu2 126.9(5) . . ? C55 N17 C54 121.5(10) . . ? C55 N17 C53 116.5(10) . . ? C54 N17 C53 121.9(10) . . ? C59 N19 C60 120.6(7) . . ? C59 N19 C61 119.0(7) . . ? C60 N19 C61 120.1(7) . . ? N1 C1 C2 122.8(7) . . ? N1 C1 H1A 118.6 . . ? C2 C1 H1A 118.6 . . ? C1 C2 C3 119.4(7) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C2 C3 C4 119.8(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 117.5(7) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? N1 C5 C4 123.0(7) . . ? N1 C5 C6 112.7(6) . . ? C4 C5 C6 124.3(6) . . ? N2 C6 C7 107.1(6) . . ? N2 C6 C5 118.5(6) . . ? C7 C6 C5 134.4(7) . . ? N4 C7 C6 105.2(6) . . ? N4 C7 H7 127.4 . . ? C6 C7 H7 127.4 . . ? N4 C8 C9 112.6(5) . . ? N4 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? N4 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C18 C9 C10 119.8(6) . . ? C18 C9 C8 121.1(7) . . ? C10 C9 C8 119.1(6) . . ? C11 C10 C9 120.3(7) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 122.4(7) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C13 124.6(8) . . ? C11 C12 C17 117.3(7) . . ? C13 C12 C17 118.1(7) . . ? C14 C13 C12 122.3(8) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C13 C14 C15 120.1(7) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.1(7) . . ? C16 C15 C19 120.5(7) . . ? C14 C15 C19 119.4(7) . . ? C15 C16 C17 121.0(7) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C18 C17 C16 122.6(7) . . ? C18 C17 C12 118.9(7) . . ? C16 C17 C12 118.4(6) . . ? C9 C18 C17 121.3(7) . . ? C9 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? N5 C19 C15 112.9(6) . . ? N5 C19 H19A 109.0 . . ? C15 C19 H19A 109.0 . . ? N5 C19 H19B 109.0 . . ? C15 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? N5 C20 C21 104.7(6) . . ? N5 C20 H20 127.6 . . ? C21 C20 H20 127.6 . . ? N7 C21 C20 107.1(7) . . ? N7 C21 C22 118.5(7) . . ? C20 C21 C22 134.4(7) . . ? N8 C22 C23 121.6(7) . . ? N8 C22 C21 113.4(6) . . ? C23 C22 C21 124.9(7) . . ? C22 C23 C24 119.9(7) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 118.1(8) . . ? C25 C24 H24 121.0 . . ? C23 C24 H24 121.0 . . ? C26 C25 C24 120.6(8) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 N8 122.1(7) . . ? C25 C26 H26 119.0 . . ? N8 C26 H26 119.0 . . ? N9 C27 C28 123.1(7) . . ? N9 C27 H27 118.5 . . ? C28 C27 H27 118.5 . . ? C27 C28 C29 119.0(7) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C28 C29 C30 119.3(7) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C31 C30 C29 117.9(7) . . ? C31 C30 H30 121.1 . . ? C29 C30 H30 121.1 . . ? N9 C31 C30 124.2(7) . . ? N9 C31 C32 111.4(7) . . ? C30 C31 C32 124.4(7) . . ? N10 C32 C33 106.6(7) . . ? N10 C32 C31 119.0(6) . . ? C33 C32 C31 134.3(7) . . ? N12 C33 C32 104.7(6) . . ? N12 C33 H33 127.6 . . ? C32 C33 H33 127.6 . . ? N12 C34 C35 110.7(5) . . ? N12 C34 H34A 109.5 . . ? C35 C34 H34A 109.5 . . ? N12 C34 H34B 109.5 . . ? C35 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C44 C35 C36 120.1(7) . . ? C44 C35 C34 119.7(7) . . ? C36 C35 C34 120.2(7) . . ? C37 C36 C35 121.3(7) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 119.7(7) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? C39 C38 C37 122.3(7) . . ? C39 C38 C43 118.4(7) . . ? C37 C38 C43 119.1(7) . . ? C40 C39 C38 121.0(7) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C41 119.8(7) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C42 C41 C40 121.1(7) . . ? C42 C41 C45 120.0(7) . . ? C40 C41 C45 118.7(6) . . ? C41 C42 C43 119.9(7) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C42 C43 C44 121.2(7) . . ? C42 C43 C38 119.6(6) . . ? C44 C43 C38 119.1(6) . . ? C35 C44 C43 120.5(7) . . ? C35 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? N13 C45 C41 110.2(5) . . ? N13 C45 H45A 109.6 . . ? C41 C45 H45A 109.6 . . ? N13 C45 H45B 109.6 . . ? C41 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? N13 C46 C47 105.7(6) . . ? N13 C46 H46 127.2 . . ? C47 C46 H46 127.2 . . ? N15 C47 C46 106.5(6) . . ? N15 C47 C48 117.4(6) . . ? C46 C47 C48 136.1(7) . . ? N16 C48 C49 123.7(6) . . ? N16 C48 C47 112.0(6) . . ? C49 C48 C47 124.3(6) . . ? C50 C49 C48 118.2(7) . . ? C50 C49 H49 120.9 . . ? C48 C49 H49 120.9 . . ? C49 C50 C51 119.0(7) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? C52 C51 C50 120.3(7) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C51 C52 N16 121.1(7) . . ? C51 C52 H52 119.4 . . ? N16 C52 H52 119.4 . . ? O3 C53 N17 129.8(11) . . ? O3 C53 H53 115.1 . . ? N17 C53 H53 115.1 . . ? N17 C54 H54A 109.5 . . ? N17 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N17 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N17 C55 H55A 109.5 . . ? N17 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N17 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C58A N18A C57A 124.6(15) . . ? C58A N18A C56A 119.7(16) . . ? C57A N18A C56A 115.7(15) . . ? O2 C56A N18A 130.5(14) . . ? O2 C56A H56A 114.8 . . ? N18A C56A H56A 114.8 . . ? C58B N18B C56B 122(2) . . ? C58B N18B C57B 124.4(17) . . ? C56B N18B C57B 113.6(19) . . ? O2 C56B N18B 130(2) . . ? O2 C56B H56B 115.1 . . ? N18B C56B H56B 115.1 . . ? N18B C57B H57D 109.5 . . ? N18B C57B H57E 109.5 . . ? H57D C57B H57E 109.5 . . ? N18B C57B H57F 109.5 . . ? H57D C57B H57F 109.5 . . ? H57E C57B H57F 109.5 . . ? N18B C58B H58D 109.5 . . ? N18B C58B H58E 109.5 . . ? H58D C58B H58E 109.5 . . ? N18B C58B H58F 109.5 . . ? H58D C58B H58F 109.5 . . ? H58E C58B H58F 109.5 . . ? O4 C59 N19 124.7(8) . . ? O4 C59 H59 117.7 . . ? N19 C59 H59 117.7 . . ? N19 C60 H60A 109.5 . . ? N19 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N19 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N19 C61 H61A 109.5 . . ? N19 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N19 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? F6 P1 F5 90.8(5) . . ? F6 P1 F4 178.3(5) . . ? F5 P1 F4 90.9(4) . . ? F6 P1 F2 91.8(4) . . ? F5 P1 F2 89.3(3) . . ? F4 P1 F2 88.7(3) . . ? F6 P1 F3 91.7(5) . . ? F5 P1 F3 177.4(4) . . ? F4 P1 F3 86.7(4) . . ? F2 P1 F3 89.7(3) . . ? F6 P1 F1 91.6(4) . . ? F5 P1 F1 91.5(3) . . ? F4 P1 F1 87.9(3) . . ? F2 P1 F1 176.5(3) . . ? F3 P1 F1 89.4(3) . . ? F12 P2 F7 89.7(3) . . ? F12 P2 F10 90.2(2) . . ? F7 P2 F10 89.9(2) . . ? F12 P2 F11 179.4(3) . . ? F7 P2 F11 89.8(2) . . ? F10 P2 F11 90.0(2) . . ? F12 P2 F9 90.3(2) . . ? F7 P2 F9 179.9(3) . . ? F10 P2 F9 90.2(2) . . ? F11 P2 F9 90.2(2) . . ? F12 P2 F8 89.5(2) . . ? F7 P2 F8 90.4(2) . . ? F10 P2 F8 179.6(3) . . ? F11 P2 F8 90.3(2) . . ? F9 P2 F8 89.5(2) . . ? F13 P3 F14 94.0(4) . . ? F13 P3 F18 90.7(3) . . ? F14 P3 F18 89.6(3) . . ? F13 P3 F17 90.5(3) . . ? F14 P3 F17 91.2(3) . . ? F18 P3 F17 178.5(4) . . ? F13 P3 F15 177.4(4) . . ? F14 P3 F15 88.5(3) . . ? F18 P3 F15 88.9(3) . . ? F17 P3 F15 89.9(3) . . ? F13 P3 F16 90.2(4) . . ? F14 P3 F16 175.7(4) . . ? F18 P3 F16 91.3(4) . . ? F17 P3 F16 87.8(3) . . ? F15 P3 F16 87.3(3) . . ? F22 P4 F23 89.9(2) . . ? F22 P4 F24 90.9(2) . . ? F23 P4 F24 179.2(3) . . ? F22 P4 F19 90.1(2) . . ? F23 P4 F19 90.4(2) . . ? F24 P4 F19 89.8(2) . . ? F22 P4 F21 90.3(2) . . ? F23 P4 F21 89.9(2) . . ? F24 P4 F21 89.8(2) . . ? F19 P4 F21 179.4(3) . . ? F22 P4 F20 179.7(3) . . ? F23 P4 F20 90.0(2) . . ? F24 P4 F20 89.2(2) . . ? F19 P4 F20 89.6(2) . . ? F21 P4 F20 90.0(2) . . ? C62 N20 C63 121.2(6) . . ? C62 N20 C64 122.9(7) . . ? C63 N20 C64 115.8(7) . . ? O5 C62 N20 126.9(8) . . ? O5 C62 H62 116.6 . . ? N20 C62 H62 116.6 . . ? N20 C63 H63A 109.5 . . ? N20 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N20 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N20 C64 H64A 109.5 . . ? N20 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N20 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C65A O6 C65 58.2(11) . . ? C65A N21 C65 55.5(14) . . ? C65A N21 C66 63.7(14) . . ? C65 N21 C66 119.1(11) . . ? C65A N21 C67 170.9(12) . . ? C65 N21 C67 121.6(12) . . ? C66 N21 C67 119.0(11) . . ? C65A N21 C66A 119.1(19) . . ? C65 N21 C66A 63.6(14) . . ? C66 N21 C66A 175.7(12) . . ? C67 N21 C66A 58.9(13) . . ? C65A N21 C67A 125(2) . . ? C65 N21 C67A 169.6(14) . . ? C66 N21 C67A 63.7(15) . . ? C67 N21 C67A 55.5(13) . . ? C66A N21 C67A 114.4(19) . . ? O6 C65 N21 120.6(12) . . ? O6 C65 H65 119.7 . . ? N21 C65 H65 119.7 . . ? N21 C66 H66A 109.5 . . ? N21 C66 H66B 109.5 . . ? N21 C66 H66C 109.5 . . ? N21 C67 H67A 109.5 . . ? N21 C67 H67B 109.5 . . ? N21 C67 H67C 109.5 . . ? O6 C65A N21 125(2) . . ? O6 C65A H65A 117.6 . . ? N21 C65A H65A 117.6 . . ? N21 C66A H66D 109.5 . . ? N21 C66A H66E 109.5 . . ? H66D C66A H66E 109.5 . . ? N21 C66A H66F 109.5 . . ? H66D C66A H66F 109.5 . . ? H66E C66A H66F 109.5 . . ? N21 C67A H67D 109.5 . . ? N21 C67A H67E 109.5 . . ? H67D C67A H67E 109.5 . . ? N21 C67A H67F 109.5 . . ? H67D C67A H67F 109.5 . . ? H67E C67A H67F 109.5 . . ? C68 N22 C69 117.5(15) . . ? C68 N22 C70 126.9(16) . . ? C69 N22 C70 115.3(9) . . ? O7 C68 N22 140(3) . . ? O7 C68 H68 110.2 . . ? N22 C68 H68 110.2 . . ? N22 C69 H69A 109.5 . . ? N22 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N22 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N22 C70 H70A 109.5 . . ? N22 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N22 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C71 N23 C73 121.9(7) . . ? C71 N23 C72 121.7(7) . . ? C73 N23 C72 116.4(6) . . ? O8 C71 N23 125.7(9) . . ? O8 C71 H71 117.2 . . ? N23 C71 H71 117.2 . . ? N23 C72 H72A 109.5 . . ? N23 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N23 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N23 C73 H73A 109.5 . . ? N23 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? N23 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 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 N15 Cu2 O2 C56B -18.4(17) . . . . ? N7 Cu2 O2 C56B 162.1(17) . . . . ? N16 Cu2 O2 C56B -99.4(17) . . . . ? N8 Cu2 O2 C56B 80.8(17) . . . . ? O4 Cu2 O2 C56B 169(9) . . . . ? N15 Cu2 O2 C56A -108.7(12) . . . . ? N7 Cu2 O2 C56A 71.8(12) . . . . ? N16 Cu2 O2 C56A 170.3(12) . . . . ? N8 Cu2 O2 C56A -9.6(12) . . . . ? O4 Cu2 O2 C56A 79(9) . . . . ? N10 Cu1 O3 C53 -76.1(9) . . . . ? N2 Cu1 O3 C53 103.0(9) . . . . ? N9 Cu1 O3 C53 4.2(9) . . . . ? N1 Cu1 O3 C53 -175.0(9) . . . . ? O1 Cu1 O3 C53 -141(3) . . . . ? N15 Cu2 O4 C59 117.9(6) . . . . ? N7 Cu2 O4 C59 -62.6(6) . . . . ? N16 Cu2 O4 C59 -161.2(6) . . . . ? N8 Cu2 O4 C59 18.8(6) . . . . ? O2 Cu2 O4 C59 -69(9) . . . . ? N10 Cu1 N1 C1 12.3(6) . . . . ? N2 Cu1 N1 C1 -177.3(6) . . . . ? N9 Cu1 N1 C1 90(3) . . . . ? O1 Cu1 N1 C1 -79.3(5) . . . . ? O3 Cu1 N1 C1 98.5(5) . . . . ? N10 Cu1 N1 C5 -164.9(4) . . . . ? N2 Cu1 N1 C5 5.5(4) . . . . ? N9 Cu1 N1 C5 -88(3) . . . . ? O1 Cu1 N1 C5 103.4(4) . . . . ? O3 Cu1 N1 C5 -78.8(4) . . . . ? N10 Cu1 N2 N3 -87.3(16) . . . . ? N9 Cu1 N2 N3 -4.3(6) . . . . ? N1 Cu1 N2 N3 -179.4(6) . . . . ? O1 Cu1 N2 N3 90.4(6) . . . . ? O3 Cu1 N2 N3 -93.3(6) . . . . ? N10 Cu1 N2 C6 86.7(15) . . . . ? N9 Cu1 N2 C6 169.7(4) . . . . ? N1 Cu1 N2 C6 -5.4(4) . . . . ? O1 Cu1 N2 C6 -95.6(4) . . . . ? O3 Cu1 N2 C6 80.8(4) . . . . ? C6 N2 N3 N4 0.5(7) . . . . ? Cu1 N2 N3 N4 174.6(4) . . . . ? N2 N3 N4 C7 -0.2(7) . . . . ? N2 N3 N4 C8 179.8(5) . . . . ? C20 N5 N6 N7 0.0(7) . . . . ? C19 N5 N6 N7 -177.4(5) . . . . ? N5 N6 N7 C21 0.4(7) . . . . ? N5 N6 N7 Cu2 178.0(4) . . . . ? N15 Cu2 N7 N6 85(3) . . . . ? N16 Cu2 N7 N6 -2.3(6) . . . . ? N8 Cu2 N7 N6 -177.4(6) . . . . ? O2 Cu2 N7 N6 91.6(6) . . . . ? O4 Cu2 N7 N6 -88.3(6) . . . . ? N15 Cu2 N7 C21 -97(3) . . . . ? N16 Cu2 N7 C21 175.3(4) . . . . ? N8 Cu2 N7 C21 0.2(4) . . . . ? O2 Cu2 N7 C21 -90.8(5) . . . . ? O4 Cu2 N7 C21 89.3(4) . . . . ? N15 Cu2 N8 C26 -6.1(6) . . . . ? N7 Cu2 N8 C26 178.4(6) . . . . ? N16 Cu2 N8 C26 88(3) . . . . ? O2 Cu2 N8 C26 -93.5(6) . . . . ? O4 Cu2 N8 C26 88.0(6) . . . . ? N15 Cu2 N8 C22 175.0(4) . . . . ? N7 Cu2 N8 C22 -0.4(4) . . . . ? N16 Cu2 N8 C22 -91(3) . . . . ? O2 Cu2 N8 C22 87.7(5) . . . . ? O4 Cu2 N8 C22 -90.8(4) . . . . ? N10 Cu1 N9 C31 3.5(5) . . . . ? N2 Cu1 N9 C31 -166.9(5) . . . . ? N1 Cu1 N9 C31 -75(3) . . . . ? O1 Cu1 N9 C31 94.3(5) . . . . ? O3 Cu1 N9 C31 -83.4(5) . . . . ? N10 Cu1 N9 C27 -178.7(6) . . . . ? N2 Cu1 N9 C27 10.9(6) . . . . ? N1 Cu1 N9 C27 103(3) . . . . ? O1 Cu1 N9 C27 -87.8(5) . . . . ? O3 Cu1 N9 C27 94.5(5) . . . . ? N2 Cu1 N10 N11 -97.0(15) . . . . ? N9 Cu1 N10 N11 178.5(6) . . . . ? N1 Cu1 N10 N11 -6.3(6) . . . . ? O1 Cu1 N10 N11 85.3(6) . . . . ? O3 Cu1 N10 N11 -91.1(6) . . . . ? N2 Cu1 N10 C32 83.1(15) . . . . ? N9 Cu1 N10 C32 -1.4(4) . . . . ? N1 Cu1 N10 C32 173.8(4) . . . . ? O1 Cu1 N10 C32 -94.6(4) . . . . ? O3 Cu1 N10 C32 89.0(4) . . . . ? C32 N10 N11 N12 1.0(7) . . . . ? Cu1 N10 N11 N12 -178.9(4) . . . . ? N10 N11 N12 C33 -1.2(7) . . . . ? N10 N11 N12 C34 -177.2(5) . . . . ? C46 N13 N14 N15 1.0(7) . . . . ? C45 N13 N14 N15 177.8(5) . . . . ? N13 N14 N15 C47 -0.2(7) . . . . ? N13 N14 N15 Cu2 -170.1(4) . . . . ? N7 Cu2 N15 N14 89(3) . . . . ? N16 Cu2 N15 N14 176.5(6) . . . . ? N8 Cu2 N15 N14 -8.4(6) . . . . ? O2 Cu2 N15 N14 81.9(6) . . . . ? O4 Cu2 N15 N14 -98.3(6) . . . . ? N7 Cu2 N15 C47 -81(3) . . . . ? N16 Cu2 N15 C47 6.7(4) . . . . ? N8 Cu2 N15 C47 -178.2(4) . . . . ? O2 Cu2 N15 C47 -87.9(5) . . . . ? O4 Cu2 N15 C47 91.9(4) . . . . ? N15 Cu2 N16 C48 -4.6(4) . . . . ? N7 Cu2 N16 C48 170.8(4) . . . . ? N8 Cu2 N16 C48 -100(3) . . . . ? O2 Cu2 N16 C48 82.0(5) . . . . ? O4 Cu2 N16 C48 -99.5(4) . . . . ? N15 Cu2 N16 C52 174.0(5) . . . . ? N7 Cu2 N16 C52 -10.5(5) . . . . ? N8 Cu2 N16 C52 79(3) . . . . ? O2 Cu2 N16 C52 -99.3(5) . . . . ? O4 Cu2 N16 C52 79.1(5) . . . . ? C5 N1 C1 C2 0.4(9) . . . . ? Cu1 N1 C1 C2 -176.7(5) . . . . ? N1 C1 C2 C3 0.5(10) . . . . ? C1 C2 C3 C4 -0.9(10) . . . . ? C2 C3 C4 C5 0.3(10) . . . . ? C1 N1 C5 C4 -1.0(9) . . . . ? Cu1 N1 C5 C4 176.5(5) . . . . ? C1 N1 C5 C6 178.0(5) . . . . ? Cu1 N1 C5 C6 -4.4(7) . . . . ? C3 C4 C5 N1 0.6(10) . . . . ? C3 C4 C5 C6 -178.3(6) . . . . ? N3 N2 C6 C7 -0.6(7) . . . . ? Cu1 N2 C6 C7 -176.2(4) . . . . ? N3 N2 C6 C5 -179.7(5) . . . . ? Cu1 N2 C6 C5 4.7(7) . . . . ? N1 C5 C6 N2 -0.2(8) . . . . ? C4 C5 C6 N2 178.8(6) . . . . ? N1 C5 C6 C7 -179.0(7) . . . . ? C4 C5 C6 C7 0.0(12) . . . . ? N3 N4 C7 C6 -0.1(7) . . . . ? C8 N4 C7 C6 179.9(6) . . . . ? N2 C6 C7 N4 0.4(7) . . . . ? C5 C6 C7 N4 179.3(7) . . . . ? N3 N4 C8 C9 73.2(8) . . . . ? C7 N4 C8 C9 -106.8(8) . . . . ? N4 C8 C9 C18 58.5(8) . . . . ? N4 C8 C9 C10 -120.5(7) . . . . ? C18 C9 C10 C11 0.4(10) . . . . ? C8 C9 C10 C11 179.4(6) . . . . ? C9 C10 C11 C12 -1.4(11) . . . . ? C10 C11 C12 C13 -177.3(7) . . . . ? C10 C11 C12 C17 1.6(10) . . . . ? C11 C12 C13 C14 177.4(7) . . . . ? C17 C12 C13 C14 -1.5(11) . . . . ? C12 C13 C14 C15 1.3(11) . . . . ? C13 C14 C15 C16 0.0(10) . . . . ? C13 C14 C15 C19 -179.9(6) . . . . ? C14 C15 C16 C17 -1.0(10) . . . . ? C19 C15 C16 C17 178.9(6) . . . . ? C15 C16 C17 C18 -176.7(6) . . . . ? C15 C16 C17 C12 0.6(10) . . . . ? C11 C12 C17 C18 -1.0(10) . . . . ? C13 C12 C17 C18 178.0(6) . . . . ? C11 C12 C17 C16 -178.4(6) . . . . ? C13 C12 C17 C16 0.6(10) . . . . ? C10 C9 C18 C17 0.3(10) . . . . ? C8 C9 C18 C17 -178.7(6) . . . . ? C16 C17 C18 C9 177.4(6) . . . . ? C12 C17 C18 C9 0.0(10) . . . . ? C20 N5 C19 C15 116.6(8) . . . . ? N6 N5 C19 C15 -66.4(8) . . . . ? C16 C15 C19 N5 -54.8(9) . . . . ? C14 C15 C19 N5 125.1(7) . . . . ? N6 N5 C20 C21 -0.4(8) . . . . ? C19 N5 C20 C21 176.8(6) . . . . ? N6 N7 C21 C20 -0.6(7) . . . . ? Cu2 N7 C21 C20 -178.9(4) . . . . ? N6 N7 C21 C22 178.3(5) . . . . ? Cu2 N7 C21 C22 0.1(8) . . . . ? N5 C20 C21 N7 0.6(8) . . . . ? N5 C20 C21 C22 -178.1(7) . . . . ? C26 N8 C22 C23 -0.9(10) . . . . ? Cu2 N8 C22 C23 178.0(6) . . . . ? C26 N8 C22 C21 -178.4(6) . . . . ? Cu2 N8 C22 C21 0.6(7) . . . . ? N7 C21 C22 N8 -0.5(9) . . . . ? C20 C21 C22 N8 178.2(7) . . . . ? N7 C21 C22 C23 -177.8(7) . . . . ? C20 C21 C22 C23 0.8(13) . . . . ? N8 C22 C23 C24 1.2(12) . . . . ? C21 C22 C23 C24 178.3(7) . . . . ? C22 C23 C24 C25 -0.8(12) . . . . ? C23 C24 C25 C26 0.2(12) . . . . ? C24 C25 C26 N8 0.0(12) . . . . ? C22 N8 C26 C25 0.3(10) . . . . ? Cu2 N8 C26 C25 -178.4(5) . . . . ? C31 N9 C27 C28 3.2(9) . . . . ? Cu1 N9 C27 C28 -174.6(5) . . . . ? N9 C27 C28 C29 -1.7(10) . . . . ? C27 C28 C29 C30 -0.2(10) . . . . ? C28 C29 C30 C31 0.4(10) . . . . ? C27 N9 C31 C30 -3.0(9) . . . . ? Cu1 N9 C31 C30 175.1(5) . . . . ? C27 N9 C31 C32 177.4(5) . . . . ? Cu1 N9 C31 C32 -4.5(7) . . . . ? C29 C30 C31 N9 1.3(10) . . . . ? C29 C30 C31 C32 -179.2(6) . . . . ? N11 N10 C32 C33 -0.5(7) . . . . ? Cu1 N10 C32 C33 179.5(4) . . . . ? N11 N10 C32 C31 179.5(5) . . . . ? Cu1 N10 C32 C31 -0.6(7) . . . . ? N9 C31 C32 N10 3.4(9) . . . . ? C30 C31 C32 N10 -176.2(6) . . . . ? N9 C31 C32 C33 -176.7(7) . . . . ? C30 C31 C32 C33 3.7(12) . . . . ? N11 N12 C33 C32 0.9(7) . . . . ? C34 N12 C33 C32 176.5(6) . . . . ? N10 C32 C33 N12 -0.2(7) . . . . ? C31 C32 C33 N12 179.8(7) . . . . ? N11 N12 C34 C35 61.4(8) . . . . ? C33 N12 C34 C35 -113.9(8) . . . . ? N12 C34 C35 C44 75.3(8) . . . . ? N12 C34 C35 C36 -102.3(8) . . . . ? C44 C35 C36 C37 -1.7(10) . . . . ? C34 C35 C36 C37 175.9(6) . . . . ? C35 C36 C37 C38 0.3(11) . . . . ? C36 C37 C38 C39 -175.8(7) . . . . ? C36 C37 C38 C43 -0.1(10) . . . . ? C37 C38 C39 C40 175.4(7) . . . . ? C43 C38 C39 C40 -0.3(11) . . . . ? C38 C39 C40 C41 1.0(11) . . . . ? C39 C40 C41 C42 -0.5(10) . . . . ? C39 C40 C41 C45 -177.3(6) . . . . ? C40 C41 C42 C43 -0.7(10) . . . . ? C45 C41 C42 C43 176.1(6) . . . . ? C41 C42 C43 C44 -176.6(6) . . . . ? C41 C42 C43 C38 1.3(10) . . . . ? C39 C38 C43 C42 -0.9(10) . . . . ? C37 C38 C43 C42 -176.7(6) . . . . ? C39 C38 C43 C44 177.1(6) . . . . ? C37 C38 C43 C44 1.3(10) . . . . ? C36 C35 C44 C43 2.9(10) . . . . ? C34 C35 C44 C43 -174.7(6) . . . . ? C42 C43 C44 C35 175.3(6) . . . . ? C38 C43 C44 C35 -2.7(10) . . . . ? C46 N13 C45 C41 100.8(8) . . . . ? N14 N13 C45 C41 -75.5(7) . . . . ? C42 C41 C45 N13 -68.5(8) . . . . ? C40 C41 C45 N13 108.4(7) . . . . ? N14 N13 C46 C47 -1.4(7) . . . . ? C45 N13 C46 C47 -177.9(6) . . . . ? N14 N15 C47 C46 -0.6(7) . . . . ? Cu2 N15 C47 C46 171.7(4) . . . . ? N14 N15 C47 C48 179.7(5) . . . . ? Cu2 N15 C47 C48 -8.0(7) . . . . ? N13 C46 C47 N15 1.2(7) . . . . ? N13 C46 C47 C48 -179.2(7) . . . . ? C52 N16 C48 C49 2.3(9) . . . . ? Cu2 N16 C48 C49 -178.9(5) . . . . ? C52 N16 C48 C47 -177.1(5) . . . . ? Cu2 N16 C48 C47 1.7(7) . . . . ? N15 C47 C48 N16 4.1(8) . . . . ? C46 C47 C48 N16 -175.4(7) . . . . ? N15 C47 C48 C49 -175.2(6) . . . . ? C46 C47 C48 C49 5.2(12) . . . . ? N16 C48 C49 C50 -2.3(10) . . . . ? C47 C48 C49 C50 177.0(6) . . . . ? C48 C49 C50 C51 1.2(9) . . . . ? C49 C50 C51 C52 -0.2(10) . . . . ? C50 C51 C52 N16 0.2(10) . . . . ? C48 N16 C52 C51 -1.2(9) . . . . ? Cu2 N16 C52 C51 -179.8(5) . . . . ? Cu1 O3 C53 N17 -115.9(11) . . . . ? C55 N17 C53 O3 179.8(12) . . . . ? C54 N17 C53 O3 2.8(18) . . . . ? C56B O2 C56A N18A -8(2) . . . . ? Cu2 O2 C56A N18A 118.2(17) . . . . ? C58A N18A C56A O2 -179.7(18) . . . . ? C57A N18A C56A O2 -2(3) . . . . ? C56A O2 C56B N18B 0(2) . . . . ? Cu2 O2 C56B N18B -123(2) . . . . ? C58B N18B C56B O2 6(3) . . . . ? C57B N18B C56B O2 -172(2) . . . . ? Cu2 O4 C59 N19 99.2(8) . . . . ? C60 N19 C59 O4 3.7(12) . . . . ? C61 N19 C59 O4 177.0(8) . . . . ? C63 N20 C62 O5 1.8(12) . . . . ? C64 N20 C62 O5 178.6(8) . . . . ? C65A O6 C65 N21 7.3(12) . . . . ? C65A N21 C65 O6 -7.3(12) . . . . ? C66 N21 C65 O6 -3.5(16) . . . . ? C67 N21 C65 O6 -177.0(11) . . . . ? C66A N21 C65 O6 172.6(17) . . . . ? C67A N21 C65 O6 -106(9) . . . . ? C65 O6 C65A N21 -7.9(13) . . . . ? C65 N21 C65A O6 7.7(13) . . . . ? C66 N21 C65A O6 -169(2) . . . . ? C67 N21 C65A O6 82(11) . . . . ? C66A N21 C65A O6 8(3) . . . . ? C67A N21 C65A O6 175.1(18) . . . . ? C69 N22 C68 O7 12(3) . . . . ? C70 N22 C68 O7 -175(2) . . . . ? C73 N23 C71 O8 -179.9(7) . . . . ? C72 N23 C71 O8 -0.7(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H2W O6 0.81(2) 1.95(2) 2.761(7) 175(8) . O1 H1W O8 0.82(2) 1.88(3) 2.667(7) 162(8) . _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 59.24 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.784 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.094 _database_code_depnum_ccdc_archive 'CCDC 929880' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Uttam27 #TrackingRef '18644_web_deposit_cif_file_1_FrankR.Fronczek_1363637732.Uttam27.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C61 H61 Cu2 N19 O2, 4(F6 P), 5.55(C3 H7 N O)' _chemical_formula_sum 'C77.65 H99.85 Cu2 F24 N24.55 O7.55 P4' _chemical_formula_weight 2204.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1 ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0571(11) _cell_length_b 14.5591(12) _cell_length_c 24.932(2) _cell_angle_alpha 88.774(3) _cell_angle_beta 86.565(3) _cell_angle_gamma 81.906(3) _cell_volume 4683.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 90.0(5) _cell_measurement_reflns_used 9882 _cell_measurement_theta_min 4.79 _cell_measurement_theta_max 68.20 _exptl_crystal_description parallelepiped _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 2.221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6651 _exptl_absorpt_correction_T_max 0.7765 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90.0(5) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'I\mS microfocus' _diffrn_radiation_monochromator 'QUAZAR multilayer optics' _diffrn_measurement_device_type 'Bruker Kappa APEX-II DUO' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61972 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 68.24 _reflns_number_total 16478 _reflns_number_gt 15083 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker (2006) Apex-II' _computing_cell_refinement 'Bruker (2006) Apex-II ' _computing_data_reduction 'Bruker (2006) Apex-II ' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2008)' _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^)+(0.1196P)^2^+12.0416P] 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 16478 _refine_ls_number_parameters 1242 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.2136 _refine_ls_wR_factor_gt 0.2100 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.058 _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 0.21299(4) 0.62319(3) 0.754542(19) 0.02349(15) Uani 1 1 d . . . Cu2 Cu 0.75398(4) 0.36015(4) 0.74139(2) 0.02850(16) Uani 1 1 d . . . N1 N 0.1523(2) 0.5278(2) 0.80382(12) 0.0251(6) Uani 1 1 d . . . N2 N 0.1644(2) 0.5435(2) 0.69895(12) 0.0243(6) Uani 1 1 d . . . N3 N 0.1697(2) 0.5407(2) 0.64608(12) 0.0269(6) Uani 1 1 d . . . N4 N 0.1334(2) 0.4625(2) 0.63365(12) 0.0276(6) Uani 1 1 d . . . N5 N 0.6948(3) 0.2459(2) 0.59908(14) 0.0371(8) Uani 1 1 d . . . N6 N 0.7241(3) 0.3186(2) 0.62297(14) 0.0362(8) Uani 1 1 d . . . N7 N 0.7226(2) 0.2982(2) 0.67469(13) 0.0304(7) Uani 1 1 d . . . N8 N 0.7063(2) 0.2432(2) 0.77536(14) 0.0296(7) Uani 1 1 d . . . N9 N 0.2457(2) 0.7317(2) 0.70653(12) 0.0260(6) Uani 1 1 d . . . N10 N 0.2568(2) 0.7054(2) 0.81056(12) 0.0246(6) Uani 1 1 d . . . N11 N 0.2629(2) 0.7020(2) 0.86309(12) 0.0264(6) Uani 1 1 d . . . N12 N 0.2916(2) 0.7834(2) 0.87604(12) 0.0263(6) Uani 1 1 d . . . N13 N 0.8075(2) 0.4845(2) 0.88310(14) 0.0324(7) Uani 1 1 d . . . N14 N 0.7727(2) 0.4117(2) 0.86083(13) 0.0306(7) Uani 1 1 d . . . N15 N 0.7838(2) 0.4257(2) 0.80838(13) 0.0287(7) Uani 1 1 d . . . N16 N 0.8174(2) 0.4688(2) 0.70671(13) 0.0291(7) Uani 1 1 d . . . N17 N 0.3844(2) 0.5332(2) 0.74686(11) 0.0228(6) Uani 1 1 d . . . N18 N 0.5719(2) 0.4440(2) 0.74255(12) 0.0243(6) Uani 1 1 d . . . C1 C 0.1435(3) 0.5278(3) 0.85781(15) 0.0285(8) Uani 1 1 d . . . H1 H 0.1682 0.5760 0.8762 0.034 Uiso 1 1 calc R . . C2 C 0.1001(3) 0.4607(3) 0.88748(16) 0.0325(8) Uani 1 1 d . . . H2 H 0.0950 0.4630 0.9256 0.039 Uiso 1 1 calc R . . C3 C 0.0640(3) 0.3895(3) 0.86124(16) 0.0334(8) Uani 1 1 d . . . H3 H 0.0344 0.3422 0.8810 0.040 Uiso 1 1 calc R . . C4 C 0.0721(3) 0.3890(3) 0.80526(16) 0.0297(8) Uani 1 1 d . . . H4 H 0.0478 0.3415 0.7860 0.036 Uiso 1 1 calc R . . C5 C 0.1158(3) 0.4588(2) 0.77822(14) 0.0249(7) Uani 1 1 d . . . C6 C 0.1256(3) 0.4682(2) 0.71988(15) 0.0253(7) Uani 1 1 d . . . C7 C 0.1048(3) 0.4153(3) 0.67777(15) 0.0286(8) Uani 1 1 d . . . H7 H 0.0767 0.3585 0.6795 0.034 Uiso 1 1 calc R . . C8 C 0.1247(3) 0.4403(3) 0.57673(15) 0.0342(8) Uani 1 1 d . . . H8A H 0.0757 0.4895 0.5603 0.041 Uiso 1 1 calc R . . H8B H 0.0963 0.3810 0.5747 0.041 Uiso 1 1 calc R . . C9 C 0.2282(3) 0.4325(3) 0.54528(15) 0.0314(8) Uani 1 1 d . . . C10 C 0.2351(3) 0.4792(3) 0.49478(16) 0.0369(9) Uani 1 1 d . . . H10 H 0.1758 0.5171 0.4823 0.044 Uiso 1 1 calc R . . C11 C 0.3248(4) 0.4702(3) 0.46427(17) 0.0399(9) Uani 1 1 d . . . H11 H 0.3274 0.5005 0.4302 0.048 Uiso 1 1 calc R . . C12 C 0.4162(3) 0.4156(3) 0.48280(16) 0.0350(9) Uani 1 1 d . . . C13 C 0.5126(4) 0.4065(3) 0.45286(17) 0.0425(10) Uani 1 1 d . . . H13 H 0.5179 0.4370 0.4189 0.051 Uiso 1 1 calc R . . C14 C 0.5980(4) 0.3547(3) 0.47214(17) 0.0429(10) Uani 1 1 d . . . H14 H 0.6622 0.3499 0.4517 0.052 Uiso 1 1 calc R . . C15 C 0.5922(3) 0.3076(3) 0.52236(17) 0.0380(9) Uani 1 1 d . . . C16 C 0.5003(3) 0.3155(3) 0.55232(16) 0.0352(9) Uani 1 1 d . . . H16 H 0.4968 0.2842 0.5861 0.042 Uiso 1 1 calc R . . C17 C 0.4101(3) 0.3699(3) 0.53370(15) 0.0322(8) Uani 1 1 d . . . C18 C 0.3142(3) 0.3792(3) 0.56412(15) 0.0327(8) Uani 1 1 d . . . H18 H 0.3093 0.3484 0.5979 0.039 Uiso 1 1 calc R . . C19 C 0.6891(4) 0.2489(4) 0.54026(18) 0.0456(11) Uani 1 1 d . . . H19A H 0.6913 0.1850 0.5271 0.055 Uiso 1 1 calc R . . H19B H 0.7504 0.2742 0.5239 0.055 Uiso 1 1 calc R . . C20 C 0.6737(3) 0.1795(3) 0.63452(19) 0.0397(10) Uani 1 1 d . . . H20 H 0.6518 0.1217 0.6273 0.048 Uiso 1 1 calc R . . C21 C 0.6911(3) 0.2138(3) 0.68374(17) 0.0312(8) Uani 1 1 d . . . C22 C 0.6840(3) 0.1812(3) 0.73944(17) 0.0327(8) Uani 1 1 d . . . C23 C 0.6556(4) 0.0956(3) 0.7553(2) 0.0428(10) Uani 1 1 d . . . H23 H 0.6393 0.0536 0.7295 0.051 Uiso 1 1 calc R . . C24 C 0.6517(4) 0.0732(3) 0.8096(2) 0.0502(12) Uani 1 1 d . . . H24 H 0.6327 0.0152 0.8215 0.060 Uiso 1 1 calc R . . C25 C 0.6758(4) 0.1359(3) 0.8463(2) 0.0459(11) Uani 1 1 d . . . H25 H 0.6737 0.1215 0.8836 0.055 Uiso 1 1 calc R . . C26 C 0.7029(3) 0.2202(3) 0.82756(17) 0.0350(9) Uani 1 1 d . . . H26 H 0.7197 0.2631 0.8527 0.042 Uiso 1 1 calc R . . C27 C 0.2334(3) 0.7411(3) 0.65314(15) 0.0314(8) Uani 1 1 d . . . H27 H 0.2124 0.6914 0.6345 0.038 Uiso 1 1 calc R . . C28 C 0.2502(4) 0.8202(3) 0.62496(17) 0.0424(10) Uani 1 1 d . . . H28 H 0.2409 0.8249 0.5875 0.051 Uiso 1 1 calc R . . C29 C 0.2809(4) 0.8932(3) 0.65181(19) 0.0470(11) Uani 1 1 d . . . H29 H 0.2929 0.9483 0.6329 0.056 Uiso 1 1 calc R . . C30 C 0.2938(4) 0.8848(3) 0.70654(18) 0.0415(10) Uani 1 1 d . . . H30 H 0.3150 0.9338 0.7258 0.050 Uiso 1 1 calc R . . C31 C 0.2750(3) 0.8033(2) 0.73261(15) 0.0289(8) Uani 1 1 d . . . C32 C 0.2810(3) 0.7872(2) 0.79038(15) 0.0277(8) Uani 1 1 d . . . C33 C 0.3043(3) 0.8382(2) 0.83257(16) 0.0302(8) Uani 1 1 d . . . H33 H 0.3247 0.8983 0.8314 0.036 Uiso 1 1 calc R . . C34 C 0.2981(3) 0.8060(3) 0.93297(15) 0.0296(8) Uani 1 1 d . . . H34A H 0.2288 0.8070 0.9516 0.035 Uiso 1 1 calc R . . H34B H 0.3181 0.8688 0.9352 0.035 Uiso 1 1 calc R . . C35 C 0.3753(3) 0.7377(3) 0.96168(15) 0.0290(8) Uani 1 1 d . . . C36 C 0.3535(3) 0.7166(3) 1.01629(16) 0.0328(8) Uani 1 1 d . . . H36 H 0.2904 0.7440 1.0339 0.039 Uiso 1 1 calc R . . C37 C 0.4223(3) 0.6571(3) 1.04429(16) 0.0337(8) Uani 1 1 d . . . H37 H 0.4060 0.6434 1.0810 0.040 Uiso 1 1 calc R . . C38 C 0.5175(3) 0.6156(3) 1.01934(15) 0.0320(8) Uani 1 1 d . . . C39 C 0.5900(3) 0.5515(3) 1.04679(16) 0.0348(9) Uani 1 1 d . . . H39 H 0.5752 0.5359 1.0833 0.042 Uiso 1 1 calc R . . C40 C 0.6799(3) 0.5127(3) 1.02133(16) 0.0356(9) Uani 1 1 d . . . H40 H 0.7277 0.4707 1.0403 0.043 Uiso 1 1 calc R . . C41 C 0.7032(3) 0.5345(3) 0.96643(17) 0.0333(8) Uani 1 1 d . . . C42 C 0.6346(3) 0.5945(3) 0.93905(16) 0.0323(8) Uani 1 1 d . . . H42 H 0.6503 0.6082 0.9023 0.039 Uiso 1 1 calc R . . C43 C 0.5398(3) 0.6369(3) 0.96458(15) 0.0300(8) Uani 1 1 d . . . C44 C 0.4666(3) 0.6982(3) 0.93642(16) 0.0305(8) Uani 1 1 d . . . H44 H 0.4811 0.7122 0.8996 0.037 Uiso 1 1 calc R . . C45 C 0.8062(3) 0.4891(3) 0.94185(17) 0.0382(9) Uani 1 1 d . . . H45A H 0.8614 0.5245 0.9519 0.046 Uiso 1 1 calc R . . H45B H 0.8216 0.4254 0.9568 0.046 Uiso 1 1 calc R . . C46 C 0.8392(3) 0.5437(3) 0.84586(18) 0.0348(9) Uani 1 1 d . . . H46 H 0.8663 0.5996 0.8517 0.042 Uiso 1 1 calc R . . C47 C 0.8241(3) 0.5060(3) 0.79755(17) 0.0304(8) Uani 1 1 d . . . C48 C 0.8447(3) 0.5301(3) 0.74144(17) 0.0316(8) Uani 1 1 d . . . C49 C 0.8902(3) 0.6072(3) 0.7247(2) 0.0401(10) Uani 1 1 d . . . H49 H 0.9087 0.6487 0.7502 0.048 Uiso 1 1 calc R . . C50 C 0.9079(3) 0.6226(3) 0.6702(2) 0.0459(11) Uani 1 1 d . . . H50 H 0.9384 0.6750 0.6575 0.055 Uiso 1 1 calc R . . C51 C 0.8802(3) 0.5603(3) 0.6347(2) 0.0443(10) Uani 1 1 d . . . H51 H 0.8919 0.5694 0.5971 0.053 Uiso 1 1 calc R . . C52 C 0.8355(3) 0.4847(3) 0.65389(17) 0.0370(9) Uani 1 1 d . . . H52 H 0.8169 0.4424 0.6289 0.044 Uiso 1 1 calc R . . C53 C 0.4561(3) 0.5865(3) 0.71564(15) 0.0288(8) Uani 1 1 d . . . H53A H 0.4568 0.6469 0.7330 0.035 Uiso 1 1 calc R . . H53B H 0.4316 0.5989 0.6790 0.035 Uiso 1 1 calc R . . C54 C 0.5671(3) 0.5325(3) 0.71183(16) 0.0305(8) Uani 1 1 d . . . H54A H 0.5888 0.5196 0.6737 0.037 Uiso 1 1 calc R . . H54B H 0.6157 0.5710 0.7262 0.037 Uiso 1 1 calc R . . C55 C 0.4991(3) 0.3883(3) 0.71950(17) 0.0325(8) Uani 1 1 d . . . H55A H 0.4986 0.3296 0.7403 0.039 Uiso 1 1 calc R . . H55B H 0.5228 0.3725 0.6819 0.039 Uiso 1 1 calc R . . C56 C 0.3878(3) 0.4423(3) 0.72072(17) 0.0314(8) Uani 1 1 d . . . H56A H 0.3653 0.4522 0.6836 0.038 Uiso 1 1 calc R . . H56B H 0.3394 0.4055 0.7407 0.038 Uiso 1 1 calc R . . C57 C 0.4228(3) 0.5155(3) 0.80121(14) 0.0292(8) Uani 1 1 d . . . H57A H 0.3774 0.4771 0.8222 0.035 Uiso 1 1 calc R . . H57B H 0.4200 0.5752 0.8199 0.035 Uiso 1 1 calc R . . C58 C 0.5353(3) 0.4651(3) 0.79836(15) 0.0306(8) Uani 1 1 d . . . H58A H 0.5811 0.5047 0.8141 0.037 Uiso 1 1 calc R . . H58B H 0.5387 0.4067 0.8197 0.037 Uiso 1 1 calc R . . O1 O 0.9239(2) 0.2751(2) 0.73880(16) 0.0482(8) Uani 1 1 d D . . H1W H 0.929(5) 0.249(4) 0.7698(11) 0.072 Uiso 1 1 d D . . H2W H 0.939(5) 0.227(3) 0.7170(17) 0.072 Uiso 1 1 d D . . O2 O 0.0466(2) 0.7293(2) 0.76561(15) 0.0510(8) Uani 1 1 d . . . N20 N -0.0599(4) 0.8554(4) 0.7872(3) 0.103(3) Uani 1 1 d . . . C59 C 0.0064(4) 0.7858(4) 0.7956(2) 0.0562(13) Uani 1 1 d . . . H59 H 0.0268 0.7781 0.8316 0.067 Uiso 1 1 calc R . . C60 C -0.0827(12) 0.8795(9) 0.7317(6) 0.173(6) Uani 1 1 d . . . H60A H -0.0239 0.8540 0.7077 0.260 Uiso 1 1 calc R . . H60B H -0.0949 0.9472 0.7274 0.260 Uiso 1 1 calc R . . H60C H -0.1447 0.8535 0.7227 0.260 Uiso 1 1 calc R . . C61 C -0.1193(6) 0.9064(7) 0.8347(5) 0.132(4) Uani 1 1 d . . . H61A H -0.1863 0.8839 0.8412 0.197 Uiso 1 1 calc R . . H61B H -0.1305 0.9731 0.8267 0.197 Uiso 1 1 calc R . . H61C H -0.0792 0.8948 0.8668 0.197 Uiso 1 1 calc R . . P1 P 0.97873(9) 0.27656(8) 0.48582(5) 0.0430(3) Uani 1 1 d . . . F1 F 0.9331(2) 0.18032(19) 0.49421(13) 0.0544(7) Uani 1 1 d . . . F2 F 0.9241(2) 0.3131(2) 0.54166(12) 0.0554(7) Uani 1 1 d . . . F3 F 1.0232(2) 0.3739(2) 0.47768(12) 0.0546(7) Uani 1 1 d . . . F4 F 1.0334(3) 0.2418(2) 0.42952(14) 0.0699(9) Uani 1 1 d . . . F5 F 1.0797(2) 0.2361(2) 0.51584(16) 0.0704(9) Uani 1 1 d . . . F6 F 0.8775(2) 0.31872(19) 0.45590(11) 0.0504(6) Uani 1 1 d . . . P2 P 0.61757(10) 0.78179(8) 0.78495(6) 0.0502(3) Uani 1 1 d . . . F7 F 0.7181(3) 0.7541(2) 0.81853(18) 0.0840(12) Uani 1 1 d . . . F8 F 0.6723(2) 0.72263(19) 0.73524(14) 0.0585(8) Uani 1 1 d . . . F9 F 0.5161(2) 0.8070(2) 0.75140(13) 0.0642(8) Uani 1 1 d . . . F10 F 0.5630(3) 0.8418(3) 0.83394(16) 0.0863(12) Uani 1 1 d . . . F11 F 0.5730(3) 0.6912(2) 0.80907(12) 0.0635(8) Uani 1 1 d . . . F12 F 0.6614(3) 0.8715(2) 0.76129(18) 0.0793(11) Uani 1 1 d . . . P3 P 0.30885(14) 0.16847(9) 0.69676(8) 0.0700(5) Uani 1 1 d . . . F13 F 0.2544(3) 0.2410(3) 0.73970(16) 0.0848(11) Uani 1 1 d . . . F14 F 0.2232(4) 0.1009(3) 0.7077(2) 0.1149(17) Uani 1 1 d . . . F15 F 0.3583(4) 0.0977(3) 0.6525(3) 0.133(2) Uani 1 1 d . . . F16 F 0.3820(3) 0.2389(2) 0.67481(16) 0.0786(10) Uani 1 1 d . . . F17 F 0.3805(8) 0.1233(6) 0.7383(3) 0.229(5) Uani 1 1 d . . . F18 F 0.2277(3) 0.2208(3) 0.65235(19) 0.0927(12) Uani 1 1 d . . . P4 P 1.00760(9) 0.29108(8) 1.02599(5) 0.0407(3) Uani 1 1 d D . . F19 F 0.9530(4) 0.2740(3) 0.97244(16) 0.0995(14) Uani 1 1 d D A . F20 F 1.0596(4) 0.3132(3) 1.07842(16) 0.1030(17) Uani 1 1 d D A . F21 F 1.0735(8) 0.1914(6) 1.0154(4) 0.077(3) Uani 0.458(13) 1 d PD A 1 F22 F 1.0805(13) 0.3379(11) 0.9881(4) 0.127(7) Uani 0.458(13) 1 d PD A 1 F23 F 0.9292(14) 0.3767(9) 1.0389(4) 0.129(9) Uani 0.458(13) 1 d PD A 1 F24 F 0.9395(6) 0.2350(10) 1.0682(3) 0.085(4) Uani 0.458(13) 1 d PD A 1 F25 F 1.1181(6) 0.2697(11) 0.9996(7) 0.167(7) Uani 0.542(13) 1 d PD A 2 F26 F 1.0076(6) 0.4011(4) 1.0083(3) 0.055(2) Uani 0.542(13) 1 d PD A 2 F27 F 0.8922(5) 0.3233(7) 1.0447(4) 0.078(3) Uani 0.542(13) 1 d PD A 2 F28 F 0.9989(14) 0.1920(5) 1.0433(5) 0.130(7) Uani 0.542(13) 1 d PD A 2 O3 O 0.3409(3) 0.0231(2) 0.88496(15) 0.0517(8) Uani 1 1 d . . . N21 N 0.3467(4) 0.1770(3) 0.87571(19) 0.0545(11) Uani 1 1 d . . . C62 C 0.3763(4) 0.0899(3) 0.8651(2) 0.0485(11) Uani 1 1 d . . . H62 H 0.4319 0.0769 0.8388 0.058 Uiso 1 1 calc R . . C63 C 0.2535(9) 0.2057(5) 0.9089(5) 0.127(4) Uani 1 1 d . . . H63A H 0.1950 0.2217 0.8860 0.190 Uiso 1 1 calc R . . H63B H 0.2627 0.2599 0.9297 0.190 Uiso 1 1 calc R . . H63C H 0.2396 0.1548 0.9334 0.190 Uiso 1 1 calc R . . C64 C 0.3903(6) 0.2529(4) 0.8489(3) 0.082(2) Uani 1 1 d . . . H64A H 0.4149 0.2916 0.8757 0.122 Uiso 1 1 calc R . . H64B H 0.3371 0.2903 0.8286 0.122 Uiso 1 1 calc R . . H64C H 0.4485 0.2280 0.8243 0.122 Uiso 1 1 calc R . . O4 O 0.9391(3) 0.2034(3) 0.84343(16) 0.0620(10) Uani 1 1 d . . . N22 N 1.0389(4) 0.0760(4) 0.8728(2) 0.0712(14) Uani 1 1 d . . . C65 C 0.9616(4) 0.1429(3) 0.8772(2) 0.0500(11) Uani 1 1 d . . . H65 H 0.9189 0.1449 0.9095 0.060 Uiso 1 1 calc R . . C66 C 1.1032(6) 0.0638(7) 0.8195(4) 0.102(3) Uani 1 1 d . . . H66A H 1.0723 0.1080 0.7928 0.154 Uiso 1 1 calc R . . H66B H 1.1044 0.0004 0.8068 0.154 Uiso 1 1 calc R . . H66C H 1.1741 0.0751 0.8248 0.154 Uiso 1 1 calc R . . C67 C 1.0666(7) 0.0095(6) 0.9155(4) 0.113(3) Uani 1 1 d . . . H67A H 1.0187 0.0235 0.9470 0.170 Uiso 1 1 calc R . . H67B H 1.1375 0.0133 0.9252 0.170 Uiso 1 1 calc R . . H67C H 1.0622 -0.0533 0.9032 0.170 Uiso 1 1 calc R . . O5 O 0.9281(4) 0.1373(4) 0.6713(2) 0.0937(16) Uani 1 1 d . . . N23 N 1.0013(5) 0.0508(4) 0.6028(2) 0.0813(16) Uani 1 1 d . . . C68 C 0.9984(5) 0.1115(6) 0.6394(3) 0.087(2) Uani 1 1 d . . . H68 H 1.0593 0.1397 0.6416 0.104 Uiso 1 1 calc R . . C69 C 0.9097(7) 0.0104(5) 0.5923(4) 0.095(2) Uani 1 1 d . . . H69A H 0.8591 0.0212 0.6230 0.142 Uiso 1 1 calc R . . H69B H 0.9284 -0.0565 0.5870 0.142 Uiso 1 1 calc R . . H69C H 0.8794 0.0391 0.5599 0.142 Uiso 1 1 calc R . . C70 C 1.0915(7) 0.0273(5) 0.5656(3) 0.089(2) Uani 1 1 d . . . H70A H 1.0735 0.0471 0.5291 0.134 Uiso 1 1 calc R . . H70B H 1.1132 -0.0399 0.5665 0.134 Uiso 1 1 calc R . . H70C H 1.1483 0.0591 0.5763 0.134 Uiso 1 1 calc R . . O6 O 0.2467(6) -0.0590(3) 1.03202(17) 0.108(2) Uani 1 1 d . . . N24 N 0.3308(10) 0.0664(5) 1.0445(4) 0.160(5) Uani 1 1 d . . . C72 C 0.4407(12) 0.0224(18) 1.0547(11) 0.37(2) Uani 1 1 d . . . H72A H 0.4413 -0.0094 1.0898 0.556 Uiso 1 1 calc R . . H72B H 0.4860 0.0707 1.0545 0.556 Uiso 1 1 calc R . . H72C H 0.4657 -0.0225 1.0265 0.556 Uiso 1 1 calc R . . C71 C 0.2668(6) 0.0178(4) 1.0310(3) 0.0716(18) Uani 1 1 d . . . H71 H 0.2141 0.0564 1.0131 0.086 Uiso 1 1 calc R . . C73 C 0.3362(9) 0.1616(6) 1.0411(5) 0.127(4) Uani 1 1 d . . . H73A H 0.2774 0.1927 1.0219 0.191 Uiso 1 1 calc R . . H73B H 0.4011 0.1720 1.0216 0.191 Uiso 1 1 calc R . . H73C H 0.3338 0.1868 1.0773 0.191 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 0.0246(3) 0.0242(3) 0.0226(3) -0.0046(2) -0.0003(2) -0.0066(2) Cu2 0.0286(3) 0.0259(3) 0.0320(3) -0.0090(2) 0.0042(2) -0.0085(2) N1 0.0205(14) 0.0276(15) 0.0269(15) -0.0037(12) 0.0009(11) -0.0029(11) N2 0.0221(14) 0.0250(15) 0.0254(15) -0.0035(12) -0.0006(11) -0.0015(11) N3 0.0267(15) 0.0282(15) 0.0260(15) -0.0066(12) 0.0002(12) -0.0045(12) N4 0.0265(15) 0.0297(16) 0.0274(16) -0.0082(12) -0.0007(12) -0.0058(12) N5 0.0329(17) 0.0412(19) 0.0365(18) -0.0167(15) 0.0017(14) -0.0023(14) N6 0.0324(17) 0.0400(19) 0.0359(18) -0.0130(15) 0.0068(14) -0.0054(14) N7 0.0228(15) 0.0300(16) 0.0376(18) -0.0081(13) 0.0033(13) -0.0017(12) N8 0.0254(15) 0.0217(15) 0.0414(18) -0.0040(13) -0.0043(13) 0.0000(12) N9 0.0264(15) 0.0215(14) 0.0295(15) -0.0035(12) -0.0031(12) 0.0004(11) N10 0.0201(14) 0.0247(15) 0.0283(15) -0.0054(12) -0.0010(11) 0.0001(11) N11 0.0232(14) 0.0295(16) 0.0270(15) -0.0090(12) -0.0017(12) -0.0041(12) N12 0.0253(15) 0.0227(15) 0.0303(16) -0.0087(12) -0.0049(12) 0.0013(12) N13 0.0248(15) 0.0287(16) 0.0427(19) -0.0117(14) -0.0073(13) 0.0037(13) N14 0.0262(15) 0.0299(16) 0.0347(17) -0.0095(13) -0.0033(13) 0.0010(12) N15 0.0213(14) 0.0249(15) 0.0392(18) -0.0076(13) -0.0019(12) -0.0001(12) N16 0.0188(14) 0.0306(16) 0.0378(17) -0.0068(13) 0.0043(12) -0.0044(12) N17 0.0218(14) 0.0229(14) 0.0236(14) -0.0027(11) 0.0007(11) -0.0030(11) N18 0.0230(14) 0.0221(14) 0.0281(15) -0.0028(12) 0.0003(12) -0.0042(11) C1 0.0257(18) 0.0334(19) 0.0264(18) -0.0060(15) 0.0005(14) -0.0049(15) C2 0.0299(19) 0.040(2) 0.0282(19) -0.0032(16) 0.0022(15) -0.0080(16) C3 0.0307(19) 0.033(2) 0.037(2) 0.0034(16) 0.0022(16) -0.0077(16) C4 0.0265(18) 0.0276(18) 0.036(2) -0.0060(15) 0.0012(15) -0.0060(14) C5 0.0201(16) 0.0261(17) 0.0279(18) -0.0061(14) -0.0016(13) -0.0002(13) C6 0.0221(16) 0.0254(17) 0.0285(18) -0.0047(14) -0.0002(14) -0.0032(13) C7 0.0274(18) 0.0272(18) 0.0322(19) -0.0075(15) -0.0004(15) -0.0070(14) C8 0.035(2) 0.040(2) 0.0280(19) -0.0115(16) -0.0008(16) -0.0075(17) C9 0.037(2) 0.0309(19) 0.0276(18) -0.0107(15) 0.0037(15) -0.0105(16) C10 0.046(2) 0.032(2) 0.032(2) -0.0050(16) -0.0020(17) -0.0035(17) C11 0.053(3) 0.037(2) 0.030(2) -0.0012(17) 0.0038(18) -0.0095(19) C12 0.047(2) 0.032(2) 0.0269(19) -0.0045(15) 0.0070(17) -0.0102(17) C13 0.052(3) 0.046(2) 0.030(2) -0.0051(18) 0.0107(18) -0.011(2) C14 0.044(2) 0.051(3) 0.034(2) -0.0146(19) 0.0152(18) -0.014(2) C15 0.039(2) 0.042(2) 0.034(2) -0.0175(17) 0.0055(17) -0.0088(18) C16 0.040(2) 0.037(2) 0.0283(19) -0.0073(16) 0.0030(16) -0.0068(17) C17 0.040(2) 0.0310(19) 0.0271(18) -0.0091(15) 0.0046(16) -0.0100(16) C18 0.039(2) 0.035(2) 0.0249(18) -0.0060(15) 0.0020(16) -0.0084(16) C19 0.041(2) 0.058(3) 0.036(2) -0.019(2) 0.0045(18) -0.001(2) C20 0.033(2) 0.034(2) 0.052(3) -0.0185(19) -0.0060(18) -0.0003(17) C21 0.0250(18) 0.0235(18) 0.045(2) -0.0094(16) -0.0043(16) -0.0011(14) C22 0.0289(19) 0.0221(18) 0.047(2) -0.0084(16) -0.0097(16) 0.0008(14) C23 0.046(2) 0.026(2) 0.058(3) -0.0031(18) -0.012(2) -0.0063(17) C24 0.058(3) 0.026(2) 0.067(3) 0.005(2) -0.011(2) -0.0062(19) C25 0.056(3) 0.032(2) 0.049(3) 0.0064(19) -0.009(2) -0.0019(19) C26 0.036(2) 0.0260(19) 0.043(2) -0.0011(16) -0.0101(17) -0.0003(16) C27 0.037(2) 0.0264(18) 0.0303(19) -0.0025(15) -0.0061(16) -0.0015(15) C28 0.063(3) 0.031(2) 0.032(2) 0.0021(17) -0.010(2) -0.0036(19) C29 0.071(3) 0.026(2) 0.046(3) 0.0082(18) -0.013(2) -0.010(2) C30 0.057(3) 0.0235(19) 0.046(2) -0.0009(17) -0.012(2) -0.0090(18) C31 0.0333(19) 0.0209(17) 0.0311(19) -0.0048(14) -0.0063(15) 0.0033(14) C32 0.0255(17) 0.0211(17) 0.036(2) -0.0042(14) -0.0041(15) 0.0008(13) C33 0.0311(19) 0.0203(17) 0.039(2) -0.0058(15) -0.0065(16) 0.0005(14) C34 0.0306(19) 0.0278(18) 0.0298(19) -0.0107(15) -0.0062(15) 0.0009(15) C35 0.0295(18) 0.0249(18) 0.0330(19) -0.0085(15) -0.0076(15) -0.0015(14) C36 0.033(2) 0.033(2) 0.033(2) -0.0111(16) -0.0027(16) -0.0038(16) C37 0.040(2) 0.033(2) 0.0283(19) -0.0065(15) -0.0026(16) -0.0042(16) C38 0.039(2) 0.0282(19) 0.0294(19) -0.0095(15) -0.0097(16) -0.0037(16) C39 0.044(2) 0.033(2) 0.0288(19) -0.0055(15) -0.0116(17) -0.0049(17) C40 0.041(2) 0.031(2) 0.036(2) -0.0070(16) -0.0173(17) 0.0001(17) C41 0.0309(19) 0.0307(19) 0.039(2) -0.0123(16) -0.0105(16) -0.0021(15) C42 0.032(2) 0.032(2) 0.0319(19) -0.0078(15) -0.0083(16) -0.0004(16) C43 0.0308(19) 0.0283(18) 0.0316(19) -0.0081(15) -0.0086(15) -0.0023(15) C44 0.0318(19) 0.0303(19) 0.0295(19) -0.0070(15) -0.0064(15) -0.0015(15) C45 0.032(2) 0.042(2) 0.039(2) -0.0111(18) -0.0137(17) 0.0045(17) C46 0.0273(19) 0.0284(19) 0.049(2) -0.0112(17) -0.0088(17) -0.0010(15) C47 0.0214(17) 0.0245(18) 0.045(2) -0.0073(16) -0.0041(15) -0.0008(14) C48 0.0185(17) 0.0275(19) 0.048(2) -0.0057(16) -0.0008(15) -0.0017(14) C49 0.027(2) 0.030(2) 0.064(3) -0.0023(19) -0.0017(19) -0.0089(16) C50 0.028(2) 0.040(2) 0.070(3) 0.003(2) 0.007(2) -0.0106(17) C51 0.029(2) 0.050(3) 0.053(3) 0.001(2) 0.0113(19) -0.0078(18) C52 0.0264(19) 0.043(2) 0.041(2) -0.0051(18) 0.0066(16) -0.0056(16) C53 0.0243(18) 0.0273(18) 0.0332(19) 0.0029(15) 0.0032(14) -0.0006(14) C54 0.0247(18) 0.0290(19) 0.036(2) 0.0031(15) 0.0045(15) -0.0003(14) C55 0.0253(18) 0.0280(19) 0.044(2) -0.0117(16) -0.0011(16) -0.0027(15) C56 0.0240(18) 0.0281(19) 0.042(2) -0.0094(16) -0.0038(15) -0.0027(15) C57 0.0273(18) 0.0340(19) 0.0245(18) -0.0017(15) -0.0017(14) 0.0028(15) C58 0.0241(18) 0.036(2) 0.0297(19) -0.0026(15) -0.0008(14) 0.0025(15) O1 0.0348(16) 0.0392(17) 0.071(2) -0.0148(15) -0.0100(16) -0.0016(13) O2 0.0327(16) 0.0434(18) 0.077(2) -0.0183(17) -0.0141(15) 0.0018(13) N20 0.065(3) 0.077(4) 0.167(7) -0.059(4) -0.062(4) 0.021(3) C59 0.037(2) 0.067(3) 0.067(3) -0.027(3) -0.007(2) -0.010(2) C60 0.213(15) 0.119(9) 0.189(13) 0.020(9) -0.110(12) 0.015(9) C61 0.058(4) 0.129(7) 0.207(11) -0.109(8) -0.012(5) 0.007(4) P1 0.0378(6) 0.0383(6) 0.0519(7) -0.0023(5) 0.0105(5) -0.0074(5) F1 0.0536(16) 0.0409(15) 0.0694(19) 0.0001(13) 0.0047(14) -0.0123(12) F2 0.0565(17) 0.0614(18) 0.0494(16) -0.0043(13) 0.0109(13) -0.0169(14) F3 0.0575(17) 0.0501(16) 0.0579(17) -0.0011(13) 0.0117(13) -0.0200(13) F4 0.072(2) 0.0604(19) 0.073(2) -0.0170(16) 0.0366(17) -0.0070(16) F5 0.0443(16) 0.0629(19) 0.105(3) 0.0126(18) -0.0086(16) -0.0106(14) F6 0.0543(16) 0.0453(15) 0.0505(15) -0.0024(12) -0.0009(12) -0.0030(12) P2 0.0487(7) 0.0352(6) 0.0675(8) -0.0143(5) -0.0143(6) -0.0020(5) F7 0.078(2) 0.057(2) 0.122(3) -0.006(2) -0.056(2) -0.0047(17) F8 0.0523(16) 0.0370(14) 0.085(2) -0.0106(14) 0.0092(15) -0.0067(12) F9 0.0469(16) 0.077(2) 0.0657(19) -0.0092(16) -0.0114(14) 0.0067(15) F10 0.111(3) 0.069(2) 0.075(2) -0.0336(19) -0.017(2) 0.012(2) F11 0.084(2) 0.0642(19) 0.0476(16) -0.0078(14) -0.0051(15) -0.0254(16) F12 0.090(3) 0.0333(15) 0.118(3) -0.0066(17) -0.017(2) -0.0158(16) P3 0.0837(11) 0.0296(6) 0.0946(12) -0.0006(7) 0.0201(9) -0.0114(6) F13 0.103(3) 0.066(2) 0.079(2) -0.0082(18) 0.009(2) 0.004(2) F14 0.115(4) 0.058(2) 0.168(5) 0.003(3) 0.032(3) -0.015(2) F15 0.125(4) 0.064(3) 0.209(6) -0.063(3) 0.068(4) -0.036(3) F16 0.097(3) 0.058(2) 0.086(2) -0.0060(17) 0.003(2) -0.0332(19) F17 0.275(10) 0.232(9) 0.130(5) -0.002(5) -0.072(6) 0.160(8) F18 0.092(3) 0.086(3) 0.102(3) -0.006(2) -0.024(2) -0.011(2) P4 0.0424(6) 0.0391(6) 0.0382(6) -0.0086(5) 0.0037(5) 0.0007(5) F19 0.153(4) 0.078(3) 0.070(2) -0.027(2) -0.037(3) -0.007(3) F20 0.173(4) 0.075(2) 0.084(3) 0.033(2) -0.083(3) -0.068(3) F21 0.083(6) 0.052(5) 0.085(6) -0.004(4) 0.006(5) 0.024(5) F22 0.198(17) 0.143(14) 0.055(5) 0.040(7) 0.018(8) -0.090(13) F23 0.209(19) 0.085(9) 0.063(6) -0.033(7) -0.050(9) 0.109(11) F24 0.046(4) 0.161(12) 0.055(5) -0.014(6) 0.010(3) -0.046(6) F25 0.046(5) 0.169(14) 0.271(18) -0.084(12) 0.046(7) 0.023(7) F26 0.076(5) 0.044(3) 0.051(4) 0.005(3) -0.016(3) -0.024(3) F27 0.053(4) 0.097(7) 0.085(5) -0.034(5) 0.028(4) -0.027(5) F28 0.25(2) 0.033(4) 0.123(10) 0.031(5) -0.094(12) -0.051(7) O3 0.059(2) 0.0279(15) 0.069(2) -0.0023(15) -0.0027(17) -0.0112(14) N21 0.076(3) 0.0262(19) 0.064(3) 0.0014(17) -0.016(2) -0.0130(18) C62 0.033(2) 0.039(2) 0.074(3) 0.000(2) -0.003(2) -0.0065(18) C63 0.155(9) 0.049(4) 0.163(9) -0.011(5) 0.049(8) 0.008(5) C64 0.105(5) 0.052(3) 0.100(5) 0.023(3) -0.035(4) -0.044(3) O4 0.060(2) 0.069(2) 0.057(2) 0.0101(19) -0.0109(18) -0.0084(18) N22 0.054(3) 0.063(3) 0.098(4) 0.008(3) -0.025(3) -0.007(2) C65 0.053(3) 0.046(3) 0.051(3) 0.001(2) -0.005(2) -0.011(2) C66 0.065(4) 0.126(7) 0.109(6) -0.010(5) 0.014(4) 0.005(4) C67 0.110(6) 0.082(5) 0.156(9) 0.054(5) -0.069(6) -0.026(5) O5 0.103(4) 0.078(3) 0.098(4) -0.040(3) 0.001(3) -0.002(3) N23 0.084(4) 0.082(4) 0.074(4) -0.016(3) -0.009(3) 0.007(3) C68 0.053(3) 0.125(6) 0.082(5) -0.056(5) 0.003(3) -0.004(4) C69 0.115(6) 0.074(5) 0.101(6) -0.028(4) -0.011(5) -0.025(4) C70 0.111(6) 0.073(4) 0.076(4) -0.016(3) -0.017(4) 0.025(4) O6 0.240(7) 0.037(2) 0.043(2) -0.0023(17) -0.016(3) -0.007(3) N24 0.289(13) 0.076(5) 0.131(7) 0.043(5) -0.139(8) -0.039(6) C72 0.113(11) 0.44(4) 0.52(4) 0.37(3) 0.031(17) 0.043(16) C71 0.096(5) 0.047(3) 0.077(4) 0.011(3) -0.047(4) -0.012(3) C73 0.141(8) 0.091(6) 0.167(10) -0.004(6) -0.075(8) -0.050(6) _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 2.012(3) . ? Cu1 N10 2.018(3) . ? Cu1 N9 2.040(3) . ? Cu1 N1 2.046(3) . ? Cu1 N17 2.428(3) . ? Cu2 N7 2.000(3) . ? Cu2 N15 2.026(3) . ? Cu2 N16 2.040(3) . ? Cu2 N8 2.044(3) . ? Cu2 O1 2.381(3) . ? N1 C1 1.344(5) . ? N1 C5 1.357(5) . ? N2 N3 1.317(4) . ? N2 C6 1.354(5) . ? N3 N4 1.344(4) . ? N4 C7 1.346(5) . ? N4 C8 1.476(5) . ? N5 N6 1.338(5) . ? N5 C20 1.342(6) . ? N5 C19 1.472(6) . ? N6 N7 1.317(5) . ? N7 C21 1.359(5) . ? N8 C26 1.336(5) . ? N8 C22 1.357(5) . ? N9 C31 1.352(5) . ? N9 C27 1.352(5) . ? N10 N11 1.316(4) . ? N10 C32 1.354(5) . ? N11 N12 1.344(4) . ? N12 C33 1.348(5) . ? N12 C34 1.474(5) . ? N13 C46 1.340(6) . ? N13 N14 1.352(5) . ? N13 C45 1.466(5) . ? N14 N15 1.321(5) . ? N15 C47 1.363(5) . ? N16 C52 1.345(5) . ? N16 C48 1.354(5) . ? N17 C53 1.474(5) . ? N17 C57 1.477(5) . ? N17 C56 1.482(5) . ? N18 C58 1.468(5) . ? N18 C54 1.481(5) . ? N18 C55 1.481(5) . ? C1 C2 1.377(6) . ? C1 H1 0.9500 . ? C2 C3 1.389(6) . ? C2 H2 0.9500 . ? C3 C4 1.393(6) . ? C3 H3 0.9500 . ? C4 C5 1.379(5) . ? C4 H4 0.9500 . ? C5 C6 1.458(5) . ? C6 C7 1.377(5) . ? C7 H7 0.9500 . ? C8 C9 1.512(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C18 1.373(6) . ? C9 C10 1.422(6) . ? C10 C11 1.350(6) . ? C10 H10 0.9500 . ? C11 C12 1.433(6) . ? C11 H11 0.9500 . ? C12 C13 1.416(6) . ? C12 C17 1.424(6) . ? C13 C14 1.362(7) . ? C13 H13 0.9500 . ? C14 C15 1.417(6) . ? C14 H14 0.9500 . ? C15 C16 1.366(6) . ? C15 C19 1.509(6) . ? C16 C17 1.420(6) . ? C16 H16 0.9500 . ? C17 C18 1.417(6) . ? C18 H18 0.9500 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.378(6) . ? C20 H20 0.9500 . ? C21 C22 1.460(6) . ? C22 C23 1.392(6) . ? C23 C24 1.385(7) . ? C23 H23 0.9500 . ? C24 C25 1.387(7) . ? C24 H24 0.9500 . ? C25 C26 1.389(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.374(6) . ? C27 H27 0.9500 . ? C28 C29 1.385(6) . ? C28 H28 0.9500 . ? C29 C30 1.386(6) . ? C29 H29 0.9500 . ? C30 C31 1.385(6) . ? C30 H30 0.9500 . ? C31 C32 1.459(5) . ? C32 C33 1.373(5) . ? C33 H33 0.9500 . ? C34 C35 1.513(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C44 1.371(5) . ? C35 C36 1.410(6) . ? C36 C37 1.369(6) . ? C36 H36 0.9500 . ? C37 C38 1.417(6) . ? C37 H37 0.9500 . ? C38 C43 1.416(6) . ? C38 C39 1.427(6) . ? C39 C40 1.356(6) . ? C39 H39 0.9500 . ? C40 C41 1.423(6) . ? C40 H40 0.9500 . ? C41 C42 1.364(6) . ? C41 C45 1.513(6) . ? C42 C43 1.423(5) . ? C42 H42 0.9500 . ? C43 C44 1.420(5) . ? C44 H44 0.9500 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.370(6) . ? C46 H46 0.9500 . ? C47 C48 1.454(6) . ? C48 C49 1.387(6) . ? C49 C50 1.383(7) . ? C49 H49 0.9500 . ? C50 C51 1.378(7) . ? C50 H50 0.9500 . ? C51 C52 1.381(6) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.548(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.551(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.546(5) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? O1 H1W 0.86(2) . ? O1 H2W 0.89(2) . ? O2 C59 1.170(6) . ? N20 C59 1.260(8) . ? N20 C60 1.458(14) . ? N20 C61 1.524(11) . ? C59 H59 0.9500 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? P1 F5 1.590(3) . ? P1 F2 1.593(3) . ? P1 F4 1.595(3) . ? P1 F6 1.597(3) . ? P1 F1 1.603(3) . ? P1 F3 1.610(3) . ? P2 F12 1.587(4) . ? P2 F10 1.590(4) . ? P2 F7 1.598(3) . ? P2 F8 1.598(3) . ? P2 F9 1.604(3) . ? P2 F11 1.606(3) . ? P3 F17 1.514(6) . ? P3 F16 1.565(4) . ? P3 F15 1.573(5) . ? P3 F13 1.585(4) . ? P3 F14 1.599(5) . ? P3 F18 1.675(5) . ? P4 F28 1.514(6) . ? P4 F22 1.519(8) . ? P4 F23 1.525(7) . ? P4 F25 1.543(8) . ? P4 F27 1.560(7) . ? P4 F20 1.568(3) . ? P4 F19 1.591(4) . ? P4 F21 1.598(7) . ? P4 F24 1.618(8) . ? P4 F26 1.652(5) . ? O3 C62 1.218(6) . ? N21 C62 1.301(6) . ? N21 C63 1.446(10) . ? N21 C64 1.446(7) . ? C62 H62 0.9500 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? O4 C65 1.223(6) . ? N22 C65 1.302(7) . ? N22 C67 1.452(9) . ? N22 C66 1.527(10) . ? C65 H65 0.9500 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? O5 C68 1.202(8) . ? N23 C68 1.279(8) . ? N23 C69 1.444(10) . ? N23 C70 1.459(10) . ? C68 H68 0.9500 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? O6 C71 1.184(7) . ? N24 C71 1.234(11) . ? N24 C73 1.398(11) . ? N24 C72 1.521(17) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C71 H71 0.9500 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 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 N2 Cu1 N10 178.07(11) . . ? N2 Cu1 N9 99.29(12) . . ? N10 Cu1 N9 80.55(12) . . ? N2 Cu1 N1 80.30(12) . . ? N10 Cu1 N1 99.48(12) . . ? N9 Cu1 N1 169.11(12) . . ? N2 Cu1 N17 90.22(11) . . ? N10 Cu1 N17 91.72(11) . . ? N9 Cu1 N17 96.98(11) . . ? N1 Cu1 N17 93.91(11) . . ? N7 Cu2 N15 178.66(13) . . ? N7 Cu2 N16 98.85(13) . . ? N15 Cu2 N16 80.40(13) . . ? N7 Cu2 N8 80.90(13) . . ? N15 Cu2 N8 99.97(13) . . ? N16 Cu2 N8 173.71(12) . . ? N7 Cu2 O1 90.83(12) . . ? N15 Cu2 O1 90.25(12) . . ? N16 Cu2 O1 87.79(12) . . ? N8 Cu2 O1 85.93(12) . . ? C1 N1 C5 117.8(3) . . ? C1 N1 Cu1 127.0(3) . . ? C5 N1 Cu1 115.2(2) . . ? N3 N2 C6 110.1(3) . . ? N3 N2 Cu1 135.8(2) . . ? C6 N2 Cu1 113.7(2) . . ? N2 N3 N4 105.8(3) . . ? N3 N4 C7 112.0(3) . . ? N3 N4 C8 119.6(3) . . ? C7 N4 C8 128.3(3) . . ? N6 N5 C20 112.2(3) . . ? N6 N5 C19 118.2(4) . . ? C20 N5 C19 129.6(4) . . ? N7 N6 N5 105.9(3) . . ? N6 N7 C21 110.2(3) . . ? N6 N7 Cu2 136.0(3) . . ? C21 N7 Cu2 113.9(3) . . ? C26 N8 C22 118.7(3) . . ? C26 N8 Cu2 126.7(3) . . ? C22 N8 Cu2 114.3(3) . . ? C31 N9 C27 118.2(3) . . ? C31 N9 Cu1 115.0(2) . . ? C27 N9 Cu1 126.6(3) . . ? N11 N10 C32 110.6(3) . . ? N11 N10 Cu1 135.9(2) . . ? C32 N10 Cu1 113.4(2) . . ? N10 N11 N12 105.3(3) . . ? N11 N12 C33 112.2(3) . . ? N11 N12 C34 119.7(3) . . ? C33 N12 C34 127.9(3) . . ? C46 N13 N14 112.0(3) . . ? C46 N13 C45 129.3(3) . . ? N14 N13 C45 118.7(3) . . ? N15 N14 N13 105.2(3) . . ? N14 N15 C47 110.4(3) . . ? N14 N15 Cu2 136.4(3) . . ? C47 N15 Cu2 113.2(3) . . ? C52 N16 C48 117.7(3) . . ? C52 N16 Cu2 127.0(3) . . ? C48 N16 Cu2 115.3(3) . . ? C53 N17 C57 108.4(3) . . ? C53 N17 C56 108.0(3) . . ? C57 N17 C56 107.7(3) . . ? C53 N17 Cu1 109.6(2) . . ? C57 N17 Cu1 108.9(2) . . ? C56 N17 Cu1 114.1(2) . . ? C58 N18 C54 108.2(3) . . ? C58 N18 C55 108.0(3) . . ? C54 N18 C55 107.8(3) . . ? N1 C1 C2 122.6(3) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 119.5(4) . . ? C1 C2 H2 120.2 . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 118.4(4) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 122.8(3) . . ? N1 C5 C6 112.9(3) . . ? C4 C5 C6 124.3(3) . . ? N2 C6 C7 107.8(3) . . ? N2 C6 C5 117.7(3) . . ? C7 C6 C5 134.5(3) . . ? N4 C7 C6 104.2(3) . . ? N4 C7 H7 127.9 . . ? C6 C7 H7 127.9 . . ? N4 C8 C9 112.0(3) . . ? N4 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N4 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C18 C9 C10 119.9(4) . . ? C18 C9 C8 121.0(4) . . ? C10 C9 C8 119.1(4) . . ? C11 C10 C9 120.9(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C17 118.8(4) . . ? C13 C12 C11 122.6(4) . . ? C17 C12 C11 118.6(4) . . ? C14 C13 C12 120.8(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.8(4) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 119.8(4) . . ? C16 C15 C19 122.4(4) . . ? C14 C15 C19 117.8(4) . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 121.9(4) . . ? C18 C17 C12 119.1(4) . . ? C16 C17 C12 119.0(4) . . ? C9 C18 C17 120.7(4) . . ? C9 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? N5 C19 C15 112.7(3) . . ? N5 C19 H19A 109.1 . . ? C15 C19 H19A 109.1 . . ? N5 C19 H19B 109.1 . . ? C15 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? N5 C20 C21 104.5(4) . . ? N5 C20 H20 127.7 . . ? C21 C20 H20 127.7 . . ? N7 C21 C20 107.3(4) . . ? N7 C21 C22 117.1(3) . . ? C20 C21 C22 135.6(4) . . ? N8 C22 C23 122.2(4) . . ? N8 C22 C21 113.6(3) . . ? C23 C22 C21 124.2(4) . . ? C24 C23 C22 118.4(4) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 119.5(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C26 118.9(4) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? N8 C26 C25 122.3(4) . . ? N8 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? N9 C27 C28 122.2(4) . . ? N9 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? C27 C28 C29 119.3(4) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C30 119.3(4) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 118.5(4) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? N9 C31 C30 122.4(4) . . ? N9 C31 C32 113.5(3) . . ? C30 C31 C32 124.1(3) . . ? N10 C32 C33 107.7(3) . . ? N10 C32 C31 117.5(3) . . ? C33 C32 C31 134.8(4) . . ? N12 C33 C32 104.2(3) . . ? N12 C33 H33 127.9 . . ? C32 C33 H33 127.9 . . ? N12 C34 C35 113.1(3) . . ? N12 C34 H34A 109.0 . . ? C35 C34 H34A 109.0 . . ? N12 C34 H34B 109.0 . . ? C35 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? C44 C35 C36 119.5(4) . . ? C44 C35 C34 121.7(4) . . ? C36 C35 C34 118.7(3) . . ? C37 C36 C35 120.8(4) . . ? C37 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C36 C37 C38 121.0(4) . . ? C36 C37 H37 119.5 . . ? C38 C37 H37 119.5 . . ? C43 C38 C37 118.4(4) . . ? C43 C38 C39 119.0(4) . . ? C37 C38 C39 122.6(4) . . ? C40 C39 C38 120.8(4) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C41 120.5(4) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C42 C41 C40 119.9(4) . . ? C42 C41 C45 123.5(4) . . ? C40 C41 C45 116.6(4) . . ? C41 C42 C43 121.1(4) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C38 C43 C44 119.4(4) . . ? C38 C43 C42 118.7(4) . . ? C44 C43 C42 121.9(4) . . ? C35 C44 C43 120.9(4) . . ? C35 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? N13 C45 C41 112.6(3) . . ? N13 C45 H45A 109.1 . . ? C41 C45 H45A 109.1 . . ? N13 C45 H45B 109.1 . . ? C41 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? N13 C46 C47 105.1(3) . . ? N13 C46 H46 127.5 . . ? C47 C46 H46 127.5 . . ? N15 C47 C46 107.3(4) . . ? N15 C47 C48 117.5(3) . . ? C46 C47 C48 135.2(4) . . ? N16 C48 C49 122.8(4) . . ? N16 C48 C47 113.6(3) . . ? C49 C48 C47 123.6(4) . . ? C50 C49 C48 118.7(4) . . ? C50 C49 H49 120.6 . . ? C48 C49 H49 120.6 . . ? C51 C50 C49 118.6(4) . . ? C51 C50 H50 120.7 . . ? C49 C50 H50 120.7 . . ? C50 C51 C52 119.9(4) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? N16 C52 C51 122.2(4) . . ? N16 C52 H52 118.9 . . ? C51 C52 H52 118.9 . . ? N17 C53 C54 110.9(3) . . ? N17 C53 H53A 109.5 . . ? C54 C53 H53A 109.5 . . ? N17 C53 H53B 109.5 . . ? C54 C53 H53B 109.5 . . ? H53A C53 H53B 108.0 . . ? N18 C54 C53 110.9(3) . . ? N18 C54 H54A 109.5 . . ? C53 C54 H54A 109.5 . . ? N18 C54 H54B 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 108.1 . . ? N18 C55 C56 111.0(3) . . ? N18 C55 H55A 109.4 . . ? C56 C55 H55A 109.4 . . ? N18 C55 H55B 109.4 . . ? C56 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? N17 C56 C55 110.5(3) . . ? N17 C56 H56A 109.5 . . ? C55 C56 H56A 109.5 . . ? N17 C56 H56B 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 108.1 . . ? N17 C57 C58 111.0(3) . . ? N17 C57 H57A 109.4 . . ? C58 C57 H57A 109.4 . . ? N17 C57 H57B 109.4 . . ? C58 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? N18 C58 C57 110.9(3) . . ? N18 C58 H58A 109.5 . . ? C57 C58 H58A 109.5 . . ? N18 C58 H58B 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 108.0 . . ? Cu2 O1 H1W 105(4) . . ? Cu2 O1 H2W 119(4) . . ? H1W O1 H2W 102(3) . . ? C59 N20 C60 118.0(8) . . ? C59 N20 C61 119.5(8) . . ? C60 N20 C61 122.3(8) . . ? O2 C59 N20 129.5(6) . . ? O2 C59 H59 115.3 . . ? N20 C59 H59 115.3 . . ? N20 C60 H60A 109.5 . . ? N20 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N20 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N20 C61 H61A 109.5 . . ? N20 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N20 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? F5 P1 F2 89.69(19) . . ? F5 P1 F4 90.8(2) . . ? F2 P1 F4 178.96(18) . . ? F5 P1 F6 179.17(19) . . ? F2 P1 F6 89.94(16) . . ? F4 P1 F6 89.58(18) . . ? F5 P1 F1 91.09(17) . . ? F2 P1 F1 90.70(16) . . ? F4 P1 F1 90.22(17) . . ? F6 P1 F1 89.66(16) . . ? F5 P1 F3 89.35(18) . . ? F2 P1 F3 88.78(16) . . ? F4 P1 F3 90.31(17) . . ? F6 P1 F3 89.90(16) . . ? F1 P1 F3 179.32(18) . . ? F12 P2 F10 89.0(2) . . ? F12 P2 F7 91.1(2) . . ? F10 P2 F7 90.0(2) . . ? F12 P2 F8 90.3(2) . . ? F10 P2 F8 179.3(2) . . ? F7 P2 F8 90.4(2) . . ? F12 P2 F9 90.2(2) . . ? F10 P2 F9 90.5(2) . . ? F7 P2 F9 178.6(2) . . ? F8 P2 F9 89.11(18) . . ? F12 P2 F11 179.8(2) . . ? F10 P2 F11 90.8(2) . . ? F7 P2 F11 88.9(2) . . ? F8 P2 F11 89.86(16) . . ? F9 P2 F11 89.79(19) . . ? F17 P3 F16 95.8(5) . . ? F17 P3 F15 92.1(4) . . ? F16 P3 F15 89.4(2) . . ? F17 P3 F13 90.5(3) . . ? F16 P3 F13 91.1(2) . . ? F15 P3 F13 177.3(3) . . ? F17 P3 F14 95.3(5) . . ? F16 P3 F14 168.2(3) . . ? F15 P3 F14 86.3(3) . . ? F13 P3 F14 92.7(3) . . ? F17 P3 F18 178.2(3) . . ? F16 P3 F18 84.3(2) . . ? F15 P3 F18 89.8(3) . . ? F13 P3 F18 87.6(2) . . ? F14 P3 F18 84.7(3) . . ? F28 P4 F23 126.8(11) . . ? F22 P4 F23 97.5(10) . . ? F28 P4 F25 95.6(9) . . ? F28 P4 F27 91.4(8) . . ? F22 P4 F27 130.1(8) . . ? F25 P4 F27 170.7(9) . . ? F28 P4 F20 93.6(4) . . ? F22 P4 F20 95.1(5) . . ? F23 P4 F20 86.0(5) . . ? F25 P4 F20 86.9(6) . . ? F27 P4 F20 98.7(4) . . ? F28 P4 F19 89.0(4) . . ? F22 P4 F19 83.8(5) . . ? F23 P4 F19 91.6(5) . . ? F25 P4 F19 93.9(7) . . ? F27 P4 F19 80.1(4) . . ? F20 P4 F19 177.2(2) . . ? F22 P4 F21 91.7(8) . . ? F23 P4 F21 170.0(10) . . ? F27 P4 F21 133.1(6) . . ? F20 P4 F21 97.2(4) . . ? F19 P4 F21 85.5(4) . . ? F22 P4 F24 174.6(8) . . ? F23 P4 F24 86.9(8) . . ? F25 P4 F24 133.5(9) . . ? F20 P4 F24 82.2(4) . . ? F19 P4 F24 99.2(4) . . ? F21 P4 F24 84.1(6) . . ? F28 P4 F26 175.7(8) . . ? F25 P4 F26 88.7(7) . . ? F27 P4 F26 84.3(4) . . ? F20 P4 F26 87.4(2) . . ? F19 P4 F26 89.9(3) . . ? C62 N21 C63 120.9(5) . . ? C62 N21 C64 124.2(6) . . ? C63 N21 C64 114.0(6) . . ? O3 C62 N21 127.5(5) . . ? O3 C62 H62 116.3 . . ? N21 C62 H62 116.3 . . ? N21 C63 H63A 109.5 . . ? N21 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N21 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N21 C64 H64A 109.5 . . ? N21 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N21 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C65 N22 C67 123.6(7) . . ? C65 N22 C66 119.2(6) . . ? C67 N22 C66 117.2(7) . . ? O4 C65 N22 125.7(6) . . ? O4 C65 H65 117.2 . . ? N22 C65 H65 117.2 . . ? N22 C66 H66A 109.5 . . ? N22 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N22 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N22 C67 H67A 109.5 . . ? N22 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N22 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C68 N23 C69 120.5(6) . . ? C68 N23 C70 122.4(7) . . ? C69 N23 C70 116.6(6) . . ? O5 C68 N23 128.1(7) . . ? O5 C68 H68 116.0 . . ? N23 C68 H68 116.0 . . ? N23 C69 H69A 109.5 . . ? N23 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? N23 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? N23 C70 H70A 109.5 . . ? N23 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N23 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C71 N24 C73 133.4(9) . . ? C71 N24 C72 120.1(14) . . ? C73 N24 C72 104.5(13) . . ? N24 C72 H72A 109.5 . . ? N24 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N24 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O6 C71 N24 143.3(7) . . ? O6 C71 H71 108.4 . . ? N24 C71 H71 108.4 . . ? N24 C73 H73A 109.5 . . ? N24 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? N24 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 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 N2 Cu1 N1 C1 -175.7(3) . . . . ? N10 Cu1 N1 C1 2.3(3) . . . . ? N9 Cu1 N1 C1 -87.0(7) . . . . ? N17 Cu1 N1 C1 94.7(3) . . . . ? N2 Cu1 N1 C5 3.0(2) . . . . ? N10 Cu1 N1 C5 -178.9(2) . . . . ? N9 Cu1 N1 C5 91.8(7) . . . . ? N17 Cu1 N1 C5 -86.5(2) . . . . ? N9 Cu1 N2 N3 14.9(3) . . . . ? N1 Cu1 N2 N3 -176.1(3) . . . . ? N17 Cu1 N2 N3 -82.2(3) . . . . ? N9 Cu1 N2 C6 -173.3(2) . . . . ? N1 Cu1 N2 C6 -4.3(2) . . . . ? N17 Cu1 N2 C6 89.6(2) . . . . ? C6 N2 N3 N4 0.2(4) . . . . ? Cu1 N2 N3 N4 172.2(2) . . . . ? N2 N3 N4 C7 0.1(4) . . . . ? N2 N3 N4 C8 177.4(3) . . . . ? C20 N5 N6 N7 0.5(4) . . . . ? C19 N5 N6 N7 180.0(3) . . . . ? N5 N6 N7 C21 -0.9(4) . . . . ? N5 N6 N7 Cu2 179.4(3) . . . . ? N16 Cu2 N7 N6 -8.9(4) . . . . ? N8 Cu2 N7 N6 177.5(4) . . . . ? O1 Cu2 N7 N6 -96.8(4) . . . . ? N16 Cu2 N7 C21 171.5(2) . . . . ? N8 Cu2 N7 C21 -2.1(2) . . . . ? O1 Cu2 N7 C21 83.6(3) . . . . ? N7 Cu2 N8 C26 178.4(3) . . . . ? N15 Cu2 N8 C26 -2.6(3) . . . . ? O1 Cu2 N8 C26 86.9(3) . . . . ? N7 Cu2 N8 C22 3.6(3) . . . . ? N15 Cu2 N8 C22 -177.4(2) . . . . ? O1 Cu2 N8 C22 -87.9(3) . . . . ? N2 Cu1 N9 C31 175.8(2) . . . . ? N10 Cu1 N9 C31 -2.3(2) . . . . ? N1 Cu1 N9 C31 88.8(7) . . . . ? N17 Cu1 N9 C31 -92.9(3) . . . . ? N2 Cu1 N9 C27 1.2(3) . . . . ? N10 Cu1 N9 C27 -176.9(3) . . . . ? N1 Cu1 N9 C27 -85.8(7) . . . . ? N17 Cu1 N9 C27 92.5(3) . . . . ? N9 Cu1 N10 N11 177.6(3) . . . . ? N1 Cu1 N10 N11 8.6(3) . . . . ? N17 Cu1 N10 N11 -85.6(3) . . . . ? N9 Cu1 N10 C32 2.0(2) . . . . ? N1 Cu1 N10 C32 -167.0(2) . . . . ? N17 Cu1 N10 C32 98.8(2) . . . . ? C32 N10 N11 N12 -0.1(4) . . . . ? Cu1 N10 N11 N12 -175.7(2) . . . . ? N10 N11 N12 C33 -0.3(4) . . . . ? N10 N11 N12 C34 175.3(3) . . . . ? C46 N13 N14 N15 0.5(4) . . . . ? C45 N13 N14 N15 -179.5(3) . . . . ? N13 N14 N15 C47 -0.5(4) . . . . ? N13 N14 N15 Cu2 -179.0(3) . . . . ? N16 Cu2 N15 N14 -178.9(4) . . . . ? N8 Cu2 N15 N14 -5.2(4) . . . . ? O1 Cu2 N15 N14 -91.2(3) . . . . ? N16 Cu2 N15 C47 2.6(2) . . . . ? N8 Cu2 N15 C47 176.2(2) . . . . ? O1 Cu2 N15 C47 90.3(2) . . . . ? N7 Cu2 N16 C52 -3.6(3) . . . . ? N15 Cu2 N16 C52 177.5(3) . . . . ? O1 Cu2 N16 C52 86.9(3) . . . . ? N7 Cu2 N16 C48 177.2(2) . . . . ? N15 Cu2 N16 C48 -1.7(2) . . . . ? O1 Cu2 N16 C48 -92.3(3) . . . . ? N2 Cu1 N17 C53 104.2(2) . . . . ? N10 Cu1 N17 C53 -75.9(2) . . . . ? N9 Cu1 N17 C53 4.8(2) . . . . ? N1 Cu1 N17 C53 -175.6(2) . . . . ? N2 Cu1 N17 C57 -137.4(2) . . . . ? N10 Cu1 N17 C57 42.5(2) . . . . ? N9 Cu1 N17 C57 123.2(2) . . . . ? N1 Cu1 N17 C57 -57.1(2) . . . . ? N2 Cu1 N17 C56 -17.1(3) . . . . ? N10 Cu1 N17 C56 162.9(3) . . . . ? N9 Cu1 N17 C56 -116.4(3) . . . . ? N1 Cu1 N17 C56 63.2(3) . . . . ? C5 N1 C1 C2 0.5(5) . . . . ? Cu1 N1 C1 C2 179.2(3) . . . . ? N1 C1 C2 C3 0.3(6) . . . . ? C1 C2 C3 C4 -0.6(6) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C1 N1 C5 C4 -0.9(5) . . . . ? Cu1 N1 C5 C4 -179.8(3) . . . . ? C1 N1 C5 C6 177.6(3) . . . . ? Cu1 N1 C5 C6 -1.3(4) . . . . ? C3 C4 C5 N1 0.5(5) . . . . ? C3 C4 C5 C6 -177.8(3) . . . . ? N3 N2 C6 C7 -0.3(4) . . . . ? Cu1 N2 C6 C7 -174.3(2) . . . . ? N3 N2 C6 C5 179.0(3) . . . . ? Cu1 N2 C6 C5 5.1(4) . . . . ? N1 C5 C6 N2 -2.5(4) . . . . ? C4 C5 C6 N2 176.0(3) . . . . ? N1 C5 C6 C7 176.6(4) . . . . ? C4 C5 C6 C7 -4.9(6) . . . . ? N3 N4 C7 C6 -0.3(4) . . . . ? C8 N4 C7 C6 -177.3(3) . . . . ? N2 C6 C7 N4 0.4(4) . . . . ? C5 C6 C7 N4 -178.8(4) . . . . ? N3 N4 C8 C9 59.3(5) . . . . ? C7 N4 C8 C9 -123.8(4) . . . . ? N4 C8 C9 C18 49.2(5) . . . . ? N4 C8 C9 C10 -132.5(4) . . . . ? C18 C9 C10 C11 1.6(6) . . . . ? C8 C9 C10 C11 -176.8(4) . . . . ? C9 C10 C11 C12 -1.9(6) . . . . ? C10 C11 C12 C13 -178.1(4) . . . . ? C10 C11 C12 C17 0.9(6) . . . . ? C17 C12 C13 C14 0.4(6) . . . . ? C11 C12 C13 C14 179.4(4) . . . . ? C12 C13 C14 C15 0.7(7) . . . . ? C13 C14 C15 C16 -1.1(6) . . . . ? C13 C14 C15 C19 178.1(4) . . . . ? C14 C15 C16 C17 0.4(6) . . . . ? C19 C15 C16 C17 -178.7(4) . . . . ? C15 C16 C17 C18 -179.8(4) . . . . ? C15 C16 C17 C12 0.7(6) . . . . ? C13 C12 C17 C18 179.5(4) . . . . ? C11 C12 C17 C18 0.4(6) . . . . ? C13 C12 C17 C16 -1.1(6) . . . . ? C11 C12 C17 C16 179.9(4) . . . . ? C10 C9 C18 C17 -0.2(6) . . . . ? C8 C9 C18 C17 178.1(3) . . . . ? C16 C17 C18 C9 179.8(4) . . . . ? C12 C17 C18 C9 -0.7(6) . . . . ? N6 N5 C19 C15 -78.5(5) . . . . ? C20 N5 C19 C15 100.8(5) . . . . ? C16 C15 C19 N5 -32.2(6) . . . . ? C14 C15 C19 N5 148.7(4) . . . . ? N6 N5 C20 C21 0.1(4) . . . . ? C19 N5 C20 C21 -179.3(4) . . . . ? N6 N7 C21 C20 1.0(4) . . . . ? Cu2 N7 C21 C20 -179.3(2) . . . . ? N6 N7 C21 C22 -179.3(3) . . . . ? Cu2 N7 C21 C22 0.4(4) . . . . ? N5 C20 C21 N7 -0.7(4) . . . . ? N5 C20 C21 C22 179.7(4) . . . . ? C26 N8 C22 C23 1.3(6) . . . . ? Cu2 N8 C22 C23 176.6(3) . . . . ? C26 N8 C22 C21 -179.5(3) . . . . ? Cu2 N8 C22 C21 -4.3(4) . . . . ? N7 C21 C22 N8 2.6(5) . . . . ? C20 C21 C22 N8 -177.8(4) . . . . ? N7 C21 C22 C23 -178.3(4) . . . . ? C20 C21 C22 C23 1.3(7) . . . . ? N8 C22 C23 C24 -0.9(6) . . . . ? C21 C22 C23 C24 -179.9(4) . . . . ? C22 C23 C24 C25 0.1(7) . . . . ? C23 C24 C25 C26 0.2(7) . . . . ? C22 N8 C26 C25 -1.0(6) . . . . ? Cu2 N8 C26 C25 -175.6(3) . . . . ? C24 C25 C26 N8 0.2(7) . . . . ? C31 N9 C27 C28 0.4(6) . . . . ? Cu1 N9 C27 C28 174.9(3) . . . . ? N9 C27 C28 C29 0.0(7) . . . . ? C27 C28 C29 C30 -0.1(7) . . . . ? C28 C29 C30 C31 -0.2(7) . . . . ? C27 N9 C31 C30 -0.8(6) . . . . ? Cu1 N9 C31 C30 -175.9(3) . . . . ? C27 N9 C31 C32 177.2(3) . . . . ? Cu1 N9 C31 C32 2.1(4) . . . . ? C29 C30 C31 N9 0.7(7) . . . . ? C29 C30 C31 C32 -177.1(4) . . . . ? N11 N10 C32 C33 0.3(4) . . . . ? Cu1 N10 C32 C33 177.0(2) . . . . ? N11 N10 C32 C31 -178.2(3) . . . . ? Cu1 N10 C32 C31 -1.5(4) . . . . ? N9 C31 C32 N10 -0.4(5) . . . . ? C30 C31 C32 N10 177.6(4) . . . . ? N9 C31 C32 C33 -178.5(4) . . . . ? C30 C31 C32 C33 -0.5(7) . . . . ? N11 N12 C33 C32 0.5(4) . . . . ? C34 N12 C33 C32 -174.7(3) . . . . ? N10 C32 C33 N12 -0.5(4) . . . . ? C31 C32 C33 N12 177.7(4) . . . . ? N11 N12 C34 C35 60.4(4) . . . . ? C33 N12 C34 C35 -124.7(4) . . . . ? N12 C34 C35 C44 36.4(5) . . . . ? N12 C34 C35 C36 -145.5(3) . . . . ? C44 C35 C36 C37 -0.2(6) . . . . ? C34 C35 C36 C37 -178.3(4) . . . . ? C35 C36 C37 C38 0.5(6) . . . . ? C36 C37 C38 C43 -0.2(6) . . . . ? C36 C37 C38 C39 -178.5(4) . . . . ? C43 C38 C39 C40 1.1(6) . . . . ? C37 C38 C39 C40 179.5(4) . . . . ? C38 C39 C40 C41 -0.6(6) . . . . ? C39 C40 C41 C42 -0.3(6) . . . . ? C39 C40 C41 C45 178.9(4) . . . . ? C40 C41 C42 C43 0.7(6) . . . . ? C45 C41 C42 C43 -178.5(4) . . . . ? C37 C38 C43 C44 -0.4(5) . . . . ? C39 C38 C43 C44 178.0(4) . . . . ? C37 C38 C43 C42 -179.1(4) . . . . ? C39 C38 C43 C42 -0.8(5) . . . . ? C41 C42 C43 C38 -0.1(6) . . . . ? C41 C42 C43 C44 -178.9(4) . . . . ? C36 C35 C44 C43 -0.4(6) . . . . ? C34 C35 C44 C43 177.7(3) . . . . ? C38 C43 C44 C35 0.6(6) . . . . ? C42 C43 C44 C35 179.4(4) . . . . ? C46 N13 C45 C41 93.9(5) . . . . ? N14 N13 C45 C41 -86.1(4) . . . . ? C42 C41 C45 N13 -23.3(6) . . . . ? C40 C41 C45 N13 157.5(4) . . . . ? N14 N13 C46 C47 -0.4(4) . . . . ? C45 N13 C46 C47 179.7(3) . . . . ? N14 N15 C47 C46 0.2(4) . . . . ? Cu2 N15 C47 C46 179.2(2) . . . . ? N14 N15 C47 C48 177.9(3) . . . . ? Cu2 N15 C47 C48 -3.1(4) . . . . ? N13 C46 C47 N15 0.1(4) . . . . ? N13 C46 C47 C48 -177.0(4) . . . . ? C52 N16 C48 C49 -0.2(5) . . . . ? Cu2 N16 C48 C49 179.1(3) . . . . ? C52 N16 C48 C47 -178.8(3) . . . . ? Cu2 N16 C48 C47 0.5(4) . . . . ? N15 C47 C48 N16 1.8(5) . . . . ? C46 C47 C48 N16 178.6(4) . . . . ? N15 C47 C48 C49 -176.8(3) . . . . ? C46 C47 C48 C49 0.0(7) . . . . ? N16 C48 C49 C50 0.4(6) . . . . ? C47 C48 C49 C50 178.8(4) . . . . ? C48 C49 C50 C51 -0.4(6) . . . . ? C49 C50 C51 C52 0.2(6) . . . . ? C48 N16 C52 C51 0.0(6) . . . . ? Cu2 N16 C52 C51 -179.2(3) . . . . ? C50 C51 C52 N16 0.0(6) . . . . ? C57 N17 C53 C54 59.1(4) . . . . ? C56 N17 C53 C54 -57.3(4) . . . . ? Cu1 N17 C53 C54 177.9(2) . . . . ? C58 N18 C54 C53 -56.9(4) . . . . ? C55 N18 C54 C53 59.7(4) . . . . ? N17 C53 C54 N18 -2.4(4) . . . . ? C58 N18 C55 C56 59.8(4) . . . . ? C54 N18 C55 C56 -56.8(4) . . . . ? C53 N17 C56 C55 60.0(4) . . . . ? C57 N17 C56 C55 -56.8(4) . . . . ? Cu1 N17 C56 C55 -177.8(2) . . . . ? N18 C55 C56 N17 -2.5(5) . . . . ? C53 N17 C57 C58 -56.3(4) . . . . ? C56 N17 C57 C58 60.3(4) . . . . ? Cu1 N17 C57 C58 -175.5(2) . . . . ? C54 N18 C58 C57 59.8(4) . . . . ? C55 N18 C58 C57 -56.6(4) . . . . ? N17 C57 C58 N18 -3.0(4) . . . . ? C60 N20 C59 O2 -9.2(13) . . . . ? C61 N20 C59 O2 165.8(6) . . . . ? C63 N21 C62 O3 -9.3(10) . . . . ? C64 N21 C62 O3 -177.7(5) . . . . ? C67 N22 C65 O4 175.7(6) . . . . ? C66 N22 C65 O4 -6.1(9) . . . . ? C69 N23 C68 O5 6.2(14) . . . . ? C70 N23 C68 O5 178.6(8) . . . . ? C73 N24 C71 O6 -176.1(12) . . . . ? C72 N24 C71 O6 23(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1W O4 0.86(2) 1.94(2) 2.796(5) 173(5) . O1 H2W O5 0.89(2) 1.77(3) 2.638(6) 162(6) . _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.787 _refine_diff_density_min -1.191 _refine_diff_density_rms 0.132 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.500 415 124 ' ' _platon_squeeze_details ; The 124 electrons removed by SQUEEZE correspond to 3.1 molecules of DMF per unit cell, or 1.55 molecules per Cu dimer. This solvent is included in the formula, FW, density, etc., but is not in the model. ; # END OF CIF _database_code_depnum_ccdc_archive 'CCDC 929881'