# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Sabiah Shahul Hameed' _publ_contact_author_email SABIAHS@GMAIL.COM _publ_section_title ; First Hexanuclear Copper(II)-Pyrophosphate through Hydrolysis of Phosphodiester with Dicopper ; loop_ _publ_author_name 'Sabiah Shahul Hameed' 'Narasimha. N Murthy' 'Babu Varghese' data_615835 _database_code_depnum_ccdc_archive 'CCDC 615835' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H132 Cl4 Cu6 N16 O36 P4' _chemical_formula_weight 3117.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.990(4) _cell_length_b 16.422(2) _cell_length_c 16.724(4) _cell_angle_alpha 105.052(12) _cell_angle_beta 103.96(2) _cell_angle_gamma 116.852(18) _cell_volume 3440.4(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 20 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1602 _exptl_absorpt_coefficient_mu 2.866 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8939 _exptl_absorpt_correction_T_max 0.9983 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 3 Theta correction was applied. Averaged transmission function was used. No Fourier smoothing was applied. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CAD4 Diffractometer' _diffrn_measurement_method '\w-2\t scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '1 hour' _diffrn_standards_decay_% 1 _diffrn_reflns_number 13014 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 67.94 _reflns_number_total 12527 _reflns_number_gt 9514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cad4 programs' _computing_cell_refinement 'cad4 programs' _computing_data_reduction 'xcad4 (wingx)' _computing_structure_solution 'SIR92 (WINGX)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (WINGX)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. A total of 56 restraints were used during refinement. The restraints were used on distances related to the anions(ClO4), acetonitrile and water molecules. These restraints were applied to maintain chemically meaningfull geometry to these moieties. Both anions in asymmetric unit are disordered and the refinement is carried out with sum of the disordered fragments constrained as 1. The oxygen atoms of the perchlorate anions were assigned only isotropic displacement parameters( anisotropic refinement isleading to bad standard deviations for thermal parameters). ; _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^)+(0.1075P)^2^+4.2717P] 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 SHELXL _refine_ls_extinction_coef 0.00036(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12527 _refine_ls_number_parameters 861 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1840 _refine_ls_wR_factor_gt 0.1683 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.090 _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 C1 C 0.7682(3) 0.2084(3) 0.2931(3) 0.0487(10) Uani 1 1 d . . . H1A H 0.7641 0.1888 0.3427 0.058 Uiso 1 1 calc R . . H1B H 0.7188 0.1487 0.2364 0.058 Uiso 1 1 calc R . . C2 C 0.7385(4) 0.2849(4) 0.2999(3) 0.0519(11) Uani 1 1 d . . . C3 C 0.6687(4) 0.2739(5) 0.2249(4) 0.0690(14) Uani 1 1 d . . . H3 H 0.6428 0.2219 0.1685 0.083 Uiso 1 1 calc R . . C4 C 0.6363(5) 0.3400(6) 0.2325(6) 0.090(2) Uani 1 1 d . . . H4 H 0.5883 0.3315 0.1814 0.108 Uiso 1 1 calc R . . C5 C 0.6749(6) 0.4179(6) 0.3153(7) 0.097(2) Uani 1 1 d . . . H5 H 0.6541 0.4628 0.3205 0.117 Uiso 1 1 calc R . . C6 C 0.7446(5) 0.4283(5) 0.3902(5) 0.0809(18) Uani 1 1 d . . . H6 H 0.7702 0.4805 0.4464 0.097 Uiso 1 1 calc R . . C7 C 0.7779(4) 0.3635(4) 0.3846(4) 0.0580(12) Uani 1 1 d . . . C8 C 0.8529(4) 0.3746(3) 0.4662(4) 0.0594(13) Uani 1 1 d . . . C9 C 0.8456(5) 0.4000(4) 0.5505(4) 0.083(2) Uani 1 1 d . . . H9 H 0.7946 0.4113 0.5549 0.100 Uiso 1 1 calc R . . C10 C 0.9118(7) 0.4081(5) 0.6254(5) 0.100(3) Uani 1 1 d . . . H10 H 0.9062 0.4253 0.6806 0.120 Uiso 1 1 calc R . . C11 C 0.9864(7) 0.3909(5) 0.6191(5) 0.104(3) Uani 1 1 d . . . H11 H 1.0309 0.3954 0.6700 0.125 Uiso 1 1 calc R . . C12 C 0.9968(5) 0.3670(4) 0.5381(5) 0.086(2) Uani 1 1 d . . . H12 H 1.0480 0.3555 0.5350 0.103 Uiso 1 1 calc R . . C13 C 0.9314(4) 0.3602(3) 0.4614(4) 0.0604(13) Uani 1 1 d . . . C14 C 0.9507(4) 0.3479(4) 0.3771(4) 0.0566(12) Uani 1 1 d . . . H14A H 1.0188 0.3597 0.3919 0.068 Uiso 1 1 calc R . . H14B H 0.9511 0.3997 0.3591 0.068 Uiso 1 1 calc R . . C15 C 0.8782(4) 0.2597(4) 0.2123(4) 0.0604(13) Uani 1 1 d . . . H15A H 0.8789 0.3196 0.2145 0.073 Uiso 1 1 calc R . . H15B H 0.8173 0.2020 0.1596 0.073 Uiso 1 1 calc R . . C16 C 0.9731(4) 0.2690(4) 0.2041(4) 0.0579(12) Uani 1 1 d . . . C17 C 1.0262(5) 0.3264(5) 0.1646(4) 0.0754(16) Uani 1 1 d . . . H17 H 1.0076 0.3666 0.1456 0.090 Uiso 1 1 calc R . . C18 C 1.1083(5) 0.3224(6) 0.1540(5) 0.085(2) Uani 1 1 d . . . H18 H 1.1450 0.3594 0.1270 0.102 Uiso 1 1 calc R . . C19 C 1.1341(5) 0.2638(6) 0.1836(5) 0.0821(19) Uani 1 1 d . . . H19 H 1.1880 0.2595 0.1761 0.098 Uiso 1 1 calc R . . C20 C 1.0799(4) 0.2108(5) 0.2245(4) 0.0695(15) Uani 1 1 d . . . H20 H 1.0984 0.1714 0.2451 0.083 Uiso 1 1 calc R . . C21 C 0.7886(4) -0.2598(5) 0.0996(3) 0.0633(13) Uani 1 1 d . . . H21A H 0.7479 -0.3258 0.0485 0.076 Uiso 1 1 calc R . . H21B H 0.7556 -0.2241 0.0892 0.076 Uiso 1 1 calc R . . C22 C 0.8940(5) -0.2033(5) 0.1007(3) 0.0646(14) Uani 1 1 d . . . C23 C 0.9323(6) -0.1096(5) 0.1017(4) 0.0823(18) Uani 1 1 d . . . H23 H 0.8982 -0.0773 0.1116 0.099 Uiso 1 1 calc R . . C24 C 1.0203(7) -0.0624(6) 0.0884(5) 0.099(2) Uani 1 1 d . . . H24 H 1.0448 0.0011 0.0889 0.119 Uiso 1 1 calc R . . C25 C 1.0726(6) -0.1088(7) 0.0744(5) 0.097(2) Uani 1 1 d . . . H25 H 1.1316 -0.0772 0.0644 0.117 Uiso 1 1 calc R . . C26 C 1.0366(5) -0.2027(6) 0.0752(4) 0.0837(19) Uani 1 1 d . . . H26 H 1.0719 -0.2338 0.0659 0.100 Uiso 1 1 calc R . . C27 C 0.9470(4) -0.2514(5) 0.0898(3) 0.0656(14) Uani 1 1 d . . . C28 C 0.9101(5) -0.3501(5) 0.0923(3) 0.0661(15) Uani 1 1 d . . . C29 C 0.9176(6) -0.4239(6) 0.0342(4) 0.086(2) Uani 1 1 d . . . H29 H 0.9484 -0.4091 -0.0051 0.103 Uiso 1 1 calc R . . C30 C 0.8801(7) -0.5169(6) 0.0352(4) 0.094(2) Uani 1 1 d . . . H30 H 0.8859 -0.5642 -0.0036 0.113 Uiso 1 1 calc R . . C31 C 0.8332(6) -0.5419(5) 0.0934(4) 0.092(2) Uani 1 1 d . . . H31 H 0.8065 -0.6054 0.0933 0.110 Uiso 1 1 calc R . . C32 C 0.8284(5) -0.4683(5) 0.1512(4) 0.0749(16) Uani 1 1 d . . . H32 H 0.7983 -0.4832 0.1909 0.090 Uiso 1 1 calc R . . C33 C 0.8662(4) -0.3741(4) 0.1523(3) 0.0605(13) Uani 1 1 d . . . C34 C 0.8661(4) -0.2941(4) 0.2221(3) 0.0550(12) Uani 1 1 d . . . H34A H 0.8551 -0.3148 0.2699 0.066 Uiso 1 1 calc R . . H34B H 0.9334 -0.2317 0.2496 0.066 Uiso 1 1 calc R . . C35 C 0.6812(4) -0.3600(4) 0.1614(3) 0.0596(12) Uani 1 1 d . . . H35A H 0.6824 -0.3817 0.2101 0.072 Uiso 1 1 calc R . . H35B H 0.6590 -0.4164 0.1060 0.072 Uiso 1 1 calc R . . C36 C 0.6072(4) -0.3269(4) 0.1483(3) 0.0555(11) Uani 1 1 d . . . C37 C 0.5034(4) -0.3897(5) 0.0895(4) 0.0741(16) Uani 1 1 d . . . H37 H 0.4747 -0.4572 0.0530 0.089 Uiso 1 1 calc R . . C38 C 0.4435(5) -0.3494(5) 0.0863(4) 0.0798(18) Uani 1 1 d . . . H38 H 0.3742 -0.3894 0.0460 0.096 Uiso 1 1 calc R . . C39 C 0.4861(5) -0.2516(5) 0.1420(4) 0.0727(15) Uani 1 1 d . . . H39 H 0.4462 -0.2243 0.1410 0.087 Uiso 1 1 calc R . . C40 C 0.5892(4) -0.1933(4) 0.2000(3) 0.0573(12) Uani 1 1 d . . . H40 H 0.6183 -0.1264 0.2385 0.069 Uiso 1 1 calc R . . C41 C 0.8023(3) 0.1841(3) 0.6481(3) 0.0435(9) Uani 1 1 d . . . H41A H 0.8126 0.1892 0.5943 0.052 Uiso 1 1 calc R . . H41B H 0.8697 0.2189 0.6977 0.052 Uiso 1 1 calc R . . C42 C 0.7479(4) 0.2359(3) 0.6723(3) 0.0462(10) Uani 1 1 d . . . C43 C 0.7817(5) 0.3028(4) 0.7607(3) 0.0616(13) Uani 1 1 d . . . H43 H 0.8383 0.3154 0.8067 0.074 Uiso 1 1 calc R . . C44 C 0.7329(6) 0.3508(5) 0.7819(4) 0.0788(17) Uani 1 1 d . . . H44 H 0.7564 0.3952 0.8418 0.095 Uiso 1 1 calc R . . C45 C 0.6485(5) 0.3330(5) 0.7138(4) 0.0755(16) Uani 1 1 d . . . H45 H 0.6152 0.3651 0.7279 0.091 Uiso 1 1 calc R . . C46 C 0.6146(4) 0.2683(4) 0.6261(4) 0.0608(12) Uani 1 1 d . . . H46 H 0.5585 0.2570 0.5806 0.073 Uiso 1 1 calc R . . C47 C 0.6634(3) 0.2182(3) 0.6033(3) 0.0456(10) Uani 1 1 d . . . C48 C 0.6270(3) 0.1483(3) 0.5083(3) 0.0446(9) Uani 1 1 d . . . C49 C 0.5997(4) 0.1725(4) 0.4364(3) 0.0541(11) Uani 1 1 d . . . H49 H 0.6048 0.2335 0.4485 0.065 Uiso 1 1 calc R . . C50 C 0.5649(4) 0.1066(4) 0.3468(3) 0.0572(12) Uani 1 1 d . . . H50 H 0.5462 0.1233 0.2994 0.069 Uiso 1 1 calc R . . C51 C 0.5581(4) 0.0166(4) 0.3288(3) 0.0571(12) Uani 1 1 d . . . H51 H 0.5365 -0.0270 0.2692 0.069 Uiso 1 1 calc R . . C52 C 0.5834(3) -0.0088(4) 0.3991(3) 0.0501(10) Uani 1 1 d . . . H52 H 0.5770 -0.0704 0.3862 0.060 Uiso 1 1 calc R . . C53 C 0.6185(3) 0.0564(3) 0.4895(3) 0.0429(9) Uani 1 1 d . . . C54 C 0.6336(3) 0.0225(3) 0.5637(3) 0.0412(9) Uani 1 1 d . . . H54A H 0.6053 -0.0492 0.5361 0.049 Uiso 1 1 calc R . . H54B H 0.5944 0.0322 0.5970 0.049 Uiso 1 1 calc R . . C55 C 0.7445(4) 0.0677(3) 0.7169(3) 0.0474(10) Uani 1 1 d . . . H55A H 0.6972 0.0828 0.7331 0.057 Uiso 1 1 calc R . . H55B H 0.8130 0.1164 0.7654 0.057 Uiso 1 1 calc R . . C56 C 0.7133(3) -0.0362(3) 0.7069(3) 0.0460(10) Uani 1 1 d . . . C57 C 0.6637(4) -0.0826(4) 0.7543(3) 0.0581(12) Uani 1 1 d . . . H57 H 0.6455 -0.0502 0.7943 0.070 Uiso 1 1 calc R . . C58 C 0.6418(5) -0.1766(5) 0.7416(4) 0.0713(15) Uani 1 1 d . . . H58 H 0.6078 -0.2093 0.7724 0.086 Uiso 1 1 calc R . . C59 C 0.6703(5) -0.2225(4) 0.6832(4) 0.0729(16) Uani 1 1 d . . . H59 H 0.6563 -0.2864 0.6744 0.087 Uiso 1 1 calc R . . C60 C 0.7198(4) -0.1732(4) 0.6377(4) 0.0602(13) Uani 1 1 d . . . H60 H 0.7387 -0.2046 0.5977 0.072 Uiso 1 1 calc R . . C61 C 0.7084(6) -0.0439(5) 0.0979(5) 0.0835(18) Uani 1 1 d . . . C62 C 0.6177(8) -0.1144(7) 0.0113(6) 0.133(4) Uani 1 1 d D . . H62A H 0.6285 -0.0916 -0.0348 0.199 Uiso 1 1 calc RD . . H62B H 0.5584 -0.1177 0.0179 0.199 Uiso 1 1 calc RD . . H62C H 0.6067 -0.1802 -0.0059 0.199 Uiso 1 1 calc RD . . N1 N 0.8746(3) 0.2470(3) 0.2967(3) 0.0473(8) Uani 1 1 d . . . N2 N 1.0013(3) 0.2144(3) 0.2356(3) 0.0573(10) Uani 1 1 d . . . N3 N 0.7863(3) -0.2743(3) 0.1845(2) 0.0515(9) Uani 1 1 d . . . N4 N 0.6488(3) -0.2304(3) 0.2025(2) 0.0497(9) Uani 1 1 d . . . N5 N 0.7438(3) 0.0759(2) 0.6305(2) 0.0394(7) Uani 1 1 d . . . N6 N 0.7412(3) -0.0813(3) 0.6496(3) 0.0479(8) Uani 1 1 d . . . N7 N 0.7774(4) 0.0103(4) 0.1652(4) 0.0779(14) Uani 1 1 d . . . O1 O 1.0082(3) 0.0973(3) 0.3270(2) 0.0612(9) Uani 1 1 d . . . O2 O 1.1247(2) 0.0729(2) 0.4348(2) 0.0426(6) Uani 1 1 d . . . O3 O 0.9468(2) -0.0743(2) 0.3234(2) 0.0523(8) Uani 1 1 d . . . O4 O 0.9752(2) 0.0648(2) 0.45721(17) 0.0374(6) Uani 1 1 d . . . O5 O 0.7862(2) -0.0585(2) 0.36213(19) 0.0465(7) Uani 1 1 d . . . O6 O 0.8493(2) 0.0738(2) 0.51698(19) 0.0417(6) Uani 1 1 d . . . O7 O 0.8677(2) 0.1241(2) 0.3903(2) 0.0469(7) Uani 1 1 d . . . O8 O 0.8123(4) -0.2269(3) 0.3843(3) 0.0782(11) Uani 1 1 d D . . O9 O 0.3408(3) 0.1525(3) 0.5598(2) 0.0613(9) Uani 1 1 d D . . O10 O 0.6075(8) 0.6447(5) 0.3879(6) 0.180(4) Uani 1 1 d . . . P1 P 1.01517(8) 0.03788(8) 0.38051(7) 0.0389(2) Uani 1 1 d . . . P2 P 0.86413(8) 0.05085(7) 0.43056(7) 0.0369(2) Uani 1 1 d . . . Cu1 Cu 0.92506(5) 0.15238(5) 0.30502(4) 0.04595(18) Uani 1 1 d . . . Cu2 Cu 0.79938(5) -0.15443(5) 0.27877(4) 0.04462(18) Uani 1 1 d . . . Cu3 Cu 0.80255(4) -0.00609(4) 0.58117(4) 0.03896(17) Uani 1 1 d . . . C63 C 0.3574(15) 0.5164(15) 0.3978(14) 0.238(8) Uiso 1 1 d D . . C64 C 0.3412(16) 0.4555(18) 0.4520(16) 0.288(11) Uiso 1 1 d D . . N8 N 0.285(2) 0.393(2) 0.4666(18) 0.401(14) Uiso 1 1 d D . . Cl1 Cl 0.40800(14) 0.40324(16) 0.16369(13) 0.0916(5) Uani 1 1 d D . . O11 O 0.3409(4) 0.4319(4) 0.1334(4) 0.1230(16) Uiso 1 1 d D A . O12 O 0.3445(7) 0.2914(5) 0.1175(7) 0.1230(16) Uiso 0.555(8) 1 d PD A 1 O13 O 0.4336(8) 0.4228(8) 0.2569(4) 0.1230(16) Uiso 0.555(8) 1 d PD A 1 O14 O 0.4924(6) 0.4383(8) 0.1441(8) 0.1230(16) Uiso 0.555(8) 1 d PD A 1 O12' O 0.3843(13) 0.3414(12) 0.2043(12) 0.227(11) Uiso 0.445(8) 1 d PD A 2 O13' O 0.5078(7) 0.5010(8) 0.2287(8) 0.151(6) Uiso 0.445(8) 1 d PD A 2 O14' O 0.4376(10) 0.3748(10) 0.0908(7) 0.115(4) Uiso 0.445(8) 1 d PD A 2 Cl2 Cl 0.68476(17) 0.14567(15) 0.95522(10) 0.0949(6) Uani 1 1 d D . . O15 O 0.6542(5) 0.1909(5) 1.0130(4) 0.145(2) Uiso 1 1 d D B . O16 O 0.7002(12) 0.0755(9) 0.9780(9) 0.138(6) Uiso 0.472(12) 1 d PD B 1 O17 O 0.6410(8) 0.1183(8) 0.8651(4) 0.105(4) Uiso 0.472(12) 1 d PD B 1 O18 O 0.7956(6) 0.2354(8) 0.9874(9) 0.149(6) Uiso 0.472(12) 1 d PD B 1 O16' O 0.7475(8) 0.1160(9) 0.9909(7) 0.114(4) Uiso 0.528(12) 1 d PD B 2 O17' O 0.5834(7) 0.0481(7) 0.8889(7) 0.156(6) Uiso 0.528(12) 1 d PD B 2 O18' O 0.7135(10) 0.1938(9) 0.9000(8) 0.148(6) Uiso 0.528(12) 1 d PD B 2 H9B H 0.381(4) 0.2236(9) 0.587(3) 0.09(2) Uiso 1 1 d D . . H9A H 0.312(5) 0.130(4) 0.599(3) 0.09(2) Uiso 1 1 d D . . H8B H 0.753(3) -0.277(3) 0.385(4) 0.09(2) Uiso 1 1 d D . . H8A H 0.842(6) -0.169(3) 0.439(4) 0.17(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.046(2) 0.049(2) 0.051(2) 0.026(2) 0.022(2) 0.023(2) C2 0.052(3) 0.054(3) 0.063(3) 0.034(2) 0.033(2) 0.029(2) C3 0.066(3) 0.083(4) 0.077(4) 0.046(3) 0.034(3) 0.046(3) C4 0.080(4) 0.119(6) 0.114(6) 0.076(5) 0.047(4) 0.069(5) C5 0.098(5) 0.090(5) 0.141(7) 0.057(5) 0.058(5) 0.069(5) C6 0.080(4) 0.057(3) 0.112(5) 0.030(3) 0.052(4) 0.040(3) C7 0.053(3) 0.050(3) 0.072(3) 0.029(2) 0.034(3) 0.024(2) C8 0.060(3) 0.038(2) 0.061(3) 0.020(2) 0.029(2) 0.013(2) C9 0.088(4) 0.045(3) 0.070(4) 0.013(3) 0.039(3) 0.007(3) C10 0.114(6) 0.053(3) 0.056(4) 0.015(3) 0.032(4) -0.004(4) C11 0.117(6) 0.054(4) 0.053(4) 0.022(3) 0.000(4) 0.002(4) C12 0.073(4) 0.054(3) 0.081(4) 0.027(3) 0.003(3) 0.014(3) C13 0.058(3) 0.036(2) 0.057(3) 0.020(2) 0.012(2) 0.010(2) C14 0.049(3) 0.048(3) 0.075(3) 0.033(2) 0.030(2) 0.022(2) C15 0.064(3) 0.078(3) 0.063(3) 0.051(3) 0.035(3) 0.042(3) C16 0.061(3) 0.075(3) 0.059(3) 0.044(3) 0.034(2) 0.039(3) C17 0.079(4) 0.100(5) 0.077(4) 0.064(4) 0.046(3) 0.050(4) C18 0.072(4) 0.119(5) 0.088(4) 0.075(4) 0.052(4) 0.044(4) C19 0.077(4) 0.125(6) 0.090(4) 0.074(4) 0.061(4) 0.061(4) C20 0.069(3) 0.099(4) 0.077(4) 0.057(3) 0.048(3) 0.053(3) C21 0.067(3) 0.081(4) 0.042(2) 0.019(2) 0.022(2) 0.046(3) C22 0.080(4) 0.082(4) 0.039(2) 0.022(2) 0.026(2) 0.051(3) C23 0.101(5) 0.094(5) 0.061(3) 0.033(3) 0.040(3) 0.057(4) C24 0.113(6) 0.096(5) 0.071(4) 0.035(4) 0.041(4) 0.044(5) C25 0.072(4) 0.123(7) 0.063(4) 0.029(4) 0.030(3) 0.035(4) C26 0.075(4) 0.116(6) 0.054(3) 0.026(3) 0.028(3) 0.053(4) C27 0.066(3) 0.087(4) 0.038(2) 0.013(2) 0.020(2) 0.045(3) C28 0.074(3) 0.085(4) 0.036(2) 0.008(2) 0.015(2) 0.055(3) C29 0.109(5) 0.122(6) 0.046(3) 0.019(3) 0.031(3) 0.089(5) C30 0.133(6) 0.106(5) 0.053(3) 0.011(3) 0.021(4) 0.095(5) C31 0.113(5) 0.081(4) 0.062(4) 0.003(3) 0.006(4) 0.068(4) C32 0.082(4) 0.069(4) 0.056(3) 0.006(3) 0.013(3) 0.047(3) C33 0.064(3) 0.065(3) 0.038(2) 0.003(2) 0.008(2) 0.041(3) C34 0.058(3) 0.060(3) 0.038(2) 0.008(2) 0.015(2) 0.035(2) C35 0.057(3) 0.046(3) 0.049(3) 0.003(2) 0.013(2) 0.022(2) C36 0.051(3) 0.053(3) 0.042(2) 0.010(2) 0.016(2) 0.022(2) C37 0.054(3) 0.068(3) 0.057(3) 0.001(3) 0.010(2) 0.022(3) C38 0.050(3) 0.090(4) 0.063(3) 0.013(3) 0.008(3) 0.030(3) C39 0.062(3) 0.090(4) 0.066(3) 0.028(3) 0.022(3) 0.047(3) C40 0.053(3) 0.058(3) 0.054(3) 0.018(2) 0.021(2) 0.030(2) C41 0.043(2) 0.037(2) 0.044(2) 0.0143(18) 0.0202(18) 0.0179(18) C42 0.053(3) 0.040(2) 0.046(2) 0.0183(19) 0.027(2) 0.023(2) C43 0.076(3) 0.053(3) 0.047(3) 0.014(2) 0.025(2) 0.034(3) C44 0.112(5) 0.068(4) 0.059(3) 0.014(3) 0.041(4) 0.056(4) C45 0.097(5) 0.070(4) 0.084(4) 0.029(3) 0.053(4) 0.058(4) C46 0.070(3) 0.060(3) 0.068(3) 0.030(3) 0.037(3) 0.042(3) C47 0.047(2) 0.039(2) 0.053(2) 0.0204(19) 0.026(2) 0.0222(19) C48 0.039(2) 0.044(2) 0.048(2) 0.0216(19) 0.0216(19) 0.0182(18) C49 0.049(3) 0.053(3) 0.061(3) 0.030(2) 0.024(2) 0.025(2) C50 0.045(2) 0.076(3) 0.050(3) 0.035(3) 0.023(2) 0.027(2) C51 0.049(3) 0.071(3) 0.042(2) 0.017(2) 0.021(2) 0.028(2) C52 0.045(2) 0.051(2) 0.046(2) 0.014(2) 0.021(2) 0.022(2) C53 0.036(2) 0.043(2) 0.042(2) 0.0155(18) 0.0197(18) 0.0167(18) C54 0.038(2) 0.040(2) 0.045(2) 0.0165(18) 0.0229(18) 0.0184(18) C55 0.057(3) 0.052(2) 0.039(2) 0.0202(19) 0.027(2) 0.030(2) C56 0.048(2) 0.054(2) 0.042(2) 0.023(2) 0.0243(19) 0.028(2) C57 0.068(3) 0.073(3) 0.056(3) 0.040(3) 0.041(3) 0.041(3) C58 0.087(4) 0.077(4) 0.080(4) 0.054(3) 0.057(3) 0.044(3) C59 0.096(4) 0.062(3) 0.092(4) 0.049(3) 0.061(4) 0.046(3) C60 0.074(3) 0.054(3) 0.078(3) 0.038(3) 0.050(3) 0.039(3) C61 0.095(5) 0.074(4) 0.070(4) 0.031(3) 0.031(4) 0.038(4) C62 0.130(8) 0.105(6) 0.090(6) 0.027(5) 0.008(5) 0.037(6) N1 0.046(2) 0.050(2) 0.051(2) 0.0292(17) 0.0245(17) 0.0245(17) N2 0.060(2) 0.072(3) 0.059(2) 0.042(2) 0.036(2) 0.037(2) N3 0.054(2) 0.055(2) 0.0372(18) 0.0099(17) 0.0153(17) 0.0313(19) N4 0.047(2) 0.048(2) 0.0415(19) 0.0110(16) 0.0159(16) 0.0224(17) N5 0.0431(18) 0.0395(17) 0.0371(17) 0.0160(14) 0.0214(15) 0.0215(15) N6 0.056(2) 0.051(2) 0.052(2) 0.0299(18) 0.0342(18) 0.0307(18) N7 0.084(4) 0.074(3) 0.066(3) 0.028(3) 0.032(3) 0.038(3) O1 0.081(2) 0.094(3) 0.067(2) 0.057(2) 0.056(2) 0.065(2) O2 0.0411(15) 0.0423(15) 0.0481(16) 0.0196(13) 0.0234(13) 0.0229(13) O3 0.0434(16) 0.0475(17) 0.0504(17) 0.0045(14) 0.0235(14) 0.0204(14) O4 0.0420(15) 0.0387(14) 0.0355(14) 0.0175(12) 0.0221(12) 0.0213(12) O5 0.0438(16) 0.0434(16) 0.0427(16) 0.0096(13) 0.0216(13) 0.0199(13) O6 0.0524(16) 0.0410(15) 0.0405(15) 0.0199(12) 0.0293(13) 0.0258(13) O7 0.0576(18) 0.0546(17) 0.0543(17) 0.0336(15) 0.0353(15) 0.0379(15) O8 0.099(3) 0.071(3) 0.061(2) 0.025(2) 0.034(2) 0.046(3) O9 0.057(2) 0.063(2) 0.063(2) 0.0255(18) 0.0317(18) 0.0300(18) O10 0.228(9) 0.096(5) 0.208(8) 0.062(5) 0.121(7) 0.070(5) P1 0.0414(5) 0.0420(5) 0.0384(5) 0.0186(4) 0.0229(4) 0.0228(5) P2 0.0418(5) 0.0373(5) 0.0368(5) 0.0175(4) 0.0230(4) 0.0213(4) Cu1 0.0529(4) 0.0533(4) 0.0492(4) 0.0319(3) 0.0314(3) 0.0315(3) Cu2 0.0429(3) 0.0409(3) 0.0384(3) 0.0079(3) 0.0174(3) 0.0190(3) Cu3 0.0432(3) 0.0408(3) 0.0406(3) 0.0202(3) 0.0260(3) 0.0229(3) Cl1 0.0877(11) 0.1202(14) 0.0942(12) 0.0665(11) 0.0505(10) 0.0596(11) Cl2 0.1482(17) 0.1211(14) 0.0528(8) 0.0346(9) 0.0440(9) 0.1013(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.501(6) . ? C1 C2 1.518(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.370(7) . ? C2 C7 1.399(7) . ? C3 C4 1.390(9) . ? C3 H3 0.9300 . ? C4 C5 1.374(11) . ? C4 H4 0.9300 . ? C5 C6 1.373(11) . ? C5 H5 0.9300 . ? C6 C7 1.382(8) . ? C6 H6 0.9300 . ? C7 C8 1.488(8) . ? C8 C13 1.395(8) . ? C8 C9 1.411(8) . ? C9 C10 1.361(11) . ? C9 H9 0.9300 . ? C10 C11 1.366(12) . ? C10 H10 0.9300 . ? C11 C12 1.381(11) . ? C11 H11 0.9300 . ? C12 C13 1.388(8) . ? C12 H12 0.9300 . ? C13 C14 1.497(7) . ? C14 N1 1.505(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N1 1.490(6) . ? C15 C16 1.499(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N2 1.335(6) . ? C16 C17 1.385(7) . ? C17 C18 1.395(9) . ? C17 H17 0.9300 . ? C18 C19 1.359(9) . ? C18 H18 0.9300 . ? C19 C20 1.376(7) . ? C19 H19 0.9300 . ? C20 N2 1.338(7) . ? C20 H20 0.9300 . ? C21 C22 1.504(8) . ? C21 N3 1.505(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.369(9) . ? C22 C27 1.408(8) . ? C23 C24 1.373(10) . ? C23 H23 0.9300 . ? C24 C25 1.383(11) . ? C24 H24 0.9300 . ? C25 C26 1.386(11) . ? C25 H25 0.9300 . ? C26 C27 1.410(9) . ? C26 H26 0.9300 . ? C27 C28 1.469(9) . ? C28 C33 1.396(8) . ? C28 C29 1.416(7) . ? C29 C30 1.372(11) . ? C29 H29 0.9300 . ? C30 C31 1.401(11) . ? C30 H30 0.9300 . ? C31 C32 1.383(8) . ? C31 H31 0.9300 . ? C32 C33 1.377(8) . ? C32 H32 0.9300 . ? C33 C34 1.516(6) . ? C34 N3 1.491(6) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N3 1.491(6) . ? C35 C36 1.504(7) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N4 1.336(6) . ? C36 C37 1.387(7) . ? C37 C38 1.387(9) . ? C37 H37 0.9300 . ? C38 C39 1.357(9) . ? C38 H38 0.9300 . ? C39 C40 1.377(8) . ? C39 H39 0.9300 . ? C40 N4 1.342(6) . ? C40 H40 0.9300 . ? C41 N5 1.488(5) . ? C41 C42 1.518(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.386(6) . ? C42 C47 1.400(7) . ? C43 C44 1.379(8) . ? C43 H43 0.9300 . ? C44 C45 1.391(9) . ? C44 H44 0.9300 . ? C45 C46 1.365(8) . ? C45 H45 0.9300 . ? C46 C47 1.410(6) . ? C46 H46 0.9300 . ? C47 C48 1.478(6) . ? C48 C53 1.394(6) . ? C48 C49 1.395(6) . ? C49 C50 1.391(7) . ? C49 H49 0.9300 . ? C50 C51 1.378(8) . ? C50 H50 0.9300 . ? C51 C52 1.377(7) . ? C51 H51 0.9300 . ? C52 C53 1.397(6) . ? C52 H52 0.9300 . ? C53 C54 1.499(6) . ? C54 N5 1.507(5) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 N5 1.483(5) . ? C55 C56 1.493(6) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 N6 1.344(6) . ? C56 C57 1.381(6) . ? C57 C58 1.362(8) . ? C57 H57 0.9300 . ? C58 C59 1.367(8) . ? C58 H58 0.9300 . ? C59 C60 1.377(7) . ? C59 H59 0.9300 . ? C60 N6 1.332(6) . ? C60 H60 0.9300 . ? C61 N7 1.127(8) . ? C61 C62 1.463(11) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? N1 Cu1 2.069(4) . ? N2 Cu1 2.011(4) . ? N3 Cu2 2.063(4) . ? N4 Cu2 1.990(4) . ? N5 Cu3 2.077(3) . ? N6 Cu3 1.995(3) . ? N7 Cu1 2.452(6) . ? O1 P1 1.507(3) . ? O1 Cu1 1.935(3) . ? O2 P1 1.508(3) . ? O2 Cu3 1.944(3) 2_756 ? O3 P1 1.505(3) . ? O3 Cu2 1.920(3) . ? O4 P2 1.614(3) . ? O4 P1 1.614(3) . ? O5 P2 1.520(3) . ? O5 Cu2 1.941(3) . ? O6 P2 1.500(3) . ? O6 Cu3 1.915(3) . ? O7 P2 1.510(3) . ? O7 Cu1 1.919(3) . ? O8 Cu2 2.390(4) . ? O8 H8B 0.940(11) . ? O8 H8A 0.944(11) . ? O9 H9B 0.942(11) . ? O9 H9A 0.946(11) . ? Cu3 O2 1.944(3) 2_756 ? C63 C64 1.496(10) . ? C64 N8 1.157(7) . ? Cl1 O12' 1.330(7) . ? Cl1 O14 1.367(6) . ? Cl1 O11 1.395(5) . ? Cl1 O13 1.419(6) . ? Cl1 O14' 1.452(7) . ? Cl1 O12 1.483(6) . ? Cl1 O13' 1.499(7) . ? Cl2 O17 1.348(6) . ? Cl2 O16' 1.379(6) . ? Cl2 O15 1.382(5) . ? Cl2 O18' 1.394(7) . ? Cl2 O16 1.404(7) . ? Cl2 O17' 1.513(7) . ? Cl2 O18 1.539(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 113.6(4) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C7 119.8(5) . . ? C3 C2 C1 120.6(5) . . ? C7 C2 C1 119.5(4) . . ? C2 C3 C4 120.4(6) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.3(7) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 118.9(6) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 122.0(7) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C2 118.5(6) . . ? C6 C7 C8 121.7(5) . . ? C2 C7 C8 119.7(5) . . ? C13 C8 C9 118.5(6) . . ? C13 C8 C7 121.1(5) . . ? C9 C8 C7 120.4(6) . . ? C10 C9 C8 121.4(8) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 119.5(7) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C12 121.0(7) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C13 120.4(8) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C8 119.2(6) . . ? C12 C13 C14 120.7(6) . . ? C8 C13 C14 119.8(5) . . ? C13 C14 N1 115.9(4) . . ? C13 C14 H14A 108.3 . . ? N1 C14 H14A 108.3 . . ? C13 C14 H14B 108.3 . . ? N1 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? N1 C15 C16 109.6(4) . . ? N1 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? N1 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? N2 C16 C17 121.9(5) . . ? N2 C16 C15 114.5(4) . . ? C17 C16 C15 123.6(5) . . ? C16 C17 C18 118.3(6) . . ? C16 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C19 C18 C17 119.2(5) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 119.6(6) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? N2 C20 C19 121.9(6) . . ? N2 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C22 C21 N3 115.7(4) . . ? C22 C21 H21A 108.4 . . ? N3 C21 H21A 108.4 . . ? C22 C21 H21B 108.4 . . ? N3 C21 H21B 108.4 . . ? H21A C21 H21B 107.4 . . ? C23 C22 C27 120.3(6) . . ? C23 C22 C21 119.5(6) . . ? C27 C22 C21 119.9(6) . . ? C22 C23 C24 121.1(7) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C25 120.3(8) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 119.7(7) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C27 120.6(7) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C22 C27 C26 118.0(6) . . ? C22 C27 C28 121.4(5) . . ? C26 C27 C28 120.5(6) . . ? C33 C28 C29 117.8(6) . . ? C33 C28 C27 120.9(5) . . ? C29 C28 C27 121.3(6) . . ? C30 C29 C28 120.8(7) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 121.3(6) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C32 C31 C30 117.2(7) . . ? C32 C31 H31 121.4 . . ? C30 C31 H31 121.4 . . ? C33 C32 C31 122.8(7) . . ? C33 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? C32 C33 C28 120.1(5) . . ? C32 C33 C34 120.2(5) . . ? C28 C33 C34 119.6(5) . . ? N3 C34 C33 114.3(4) . . ? N3 C34 H34A 108.7 . . ? C33 C34 H34A 108.7 . . ? N3 C34 H34B 108.7 . . ? C33 C34 H34B 108.7 . . ? H34A C34 H34B 107.6 . . ? N3 C35 C36 109.4(4) . . ? N3 C35 H35A 109.8 . . ? C36 C35 H35A 109.8 . . ? N3 C35 H35B 109.8 . . ? C36 C35 H35B 109.8 . . ? H35A C35 H35B 108.2 . . ? N4 C36 C37 121.4(5) . . ? N4 C36 C35 113.9(4) . . ? C37 C36 C35 124.6(5) . . ? C38 C37 C36 118.4(5) . . ? C38 C37 H37 120.8 . . ? C36 C37 H37 120.8 . . ? C39 C38 C37 119.9(5) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 119.1(6) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? N4 C40 C39 121.8(5) . . ? N4 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? N5 C41 C42 112.8(3) . . ? N5 C41 H41A 109.0 . . ? C42 C41 H41A 109.0 . . ? N5 C41 H41B 109.0 . . ? C42 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? C43 C42 C47 119.0(4) . . ? C43 C42 C41 121.6(4) . . ? C47 C42 C41 119.4(4) . . ? C44 C43 C42 121.3(5) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 119.9(5) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 119.7(5) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C47 121.0(5) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C42 C47 C46 119.0(4) . . ? C42 C47 C48 119.9(4) . . ? C46 C47 C48 121.1(4) . . ? C53 C48 C49 119.2(4) . . ? C53 C48 C47 120.1(4) . . ? C49 C48 C47 120.8(4) . . ? C50 C49 C48 120.9(5) . . ? C50 C49 H49 119.5 . . ? C48 C49 H49 119.5 . . ? C51 C50 C49 119.6(5) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C52 C51 C50 119.9(4) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C51 C52 C53 121.3(5) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C48 C53 C52 119.1(4) . . ? C48 C53 C54 120.1(4) . . ? C52 C53 C54 120.4(4) . . ? C53 C54 N5 115.1(3) . . ? C53 C54 H54A 108.5 . . ? N5 C54 H54A 108.5 . . ? C53 C54 H54B 108.5 . . ? N5 C54 H54B 108.5 . . ? H54A C54 H54B 107.5 . . ? N5 C55 C56 110.3(3) . . ? N5 C55 H55A 109.6 . . ? C56 C55 H55A 109.6 . . ? N5 C55 H55B 109.6 . . ? C56 C55 H55B 109.6 . . ? H55A C55 H55B 108.1 . . ? N6 C56 C57 121.4(4) . . ? N6 C56 C55 114.3(4) . . ? C57 C56 C55 124.3(4) . . ? C58 C57 C56 119.1(5) . . ? C58 C57 H57 120.4 . . ? C56 C57 H57 120.4 . . ? C57 C58 C59 119.5(5) . . ? C57 C58 H58 120.3 . . ? C59 C58 H58 120.3 . . ? C58 C59 C60 119.4(5) . . ? C58 C59 H59 120.3 . . ? C60 C59 H59 120.3 . . ? N6 C60 C59 121.4(5) . . ? N6 C60 H60 119.3 . . ? C59 C60 H60 119.3 . . ? N7 C61 C62 179.0(9) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C15 N1 C1 110.3(4) . . ? C15 N1 C14 108.5(4) . . ? C1 N1 C14 109.7(4) . . ? C15 N1 Cu1 105.3(3) . . ? C1 N1 Cu1 114.6(3) . . ? C14 N1 Cu1 108.2(3) . . ? C16 N2 C20 119.1(4) . . ? C16 N2 Cu1 114.8(3) . . ? C20 N2 Cu1 125.9(4) . . ? C35 N3 C34 110.9(4) . . ? C35 N3 C21 108.5(4) . . ? C34 N3 C21 110.3(4) . . ? C35 N3 Cu2 102.6(3) . . ? C34 N3 Cu2 112.8(3) . . ? C21 N3 Cu2 111.4(3) . . ? C36 N4 C40 119.4(4) . . ? C36 N4 Cu2 114.2(3) . . ? C40 N4 Cu2 126.4(3) . . ? C55 N5 C41 109.6(3) . . ? C55 N5 C54 108.5(3) . . ? C41 N5 C54 110.6(3) . . ? C55 N5 Cu3 104.8(3) . . ? C41 N5 Cu3 115.7(2) . . ? C54 N5 Cu3 107.3(2) . . ? C60 N6 C56 119.2(4) . . ? C60 N6 Cu3 125.5(3) . . ? C56 N6 Cu3 115.1(3) . . ? C61 N7 Cu1 169.5(6) . . ? P1 O1 Cu1 133.22(19) . . ? P1 O2 Cu3 130.06(18) . 2_756 ? P1 O3 Cu2 125.51(19) . . ? P2 O4 P1 121.45(17) . . ? P2 O5 Cu2 131.83(18) . . ? P2 O6 Cu3 132.21(17) . . ? P2 O7 Cu1 127.31(18) . . ? Cu2 O8 H8B 121(4) . . ? Cu2 O8 H8A 99(6) . . ? H8B O8 H8A 105.4(16) . . ? H9B O9 H9A 107.9(16) . . ? O3 P1 O1 112.9(2) . . ? O3 P1 O2 112.79(18) . . ? O1 P1 O2 112.84(19) . . ? O3 P1 O4 107.73(16) . . ? O1 P1 O4 105.95(16) . . ? O2 P1 O4 103.85(16) . . ? O6 P2 O7 112.25(17) . . ? O6 P2 O5 112.18(16) . . ? O7 P2 O5 112.55(18) . . ? O6 P2 O4 106.64(16) . . ? O7 P2 O4 106.97(16) . . ? O5 P2 O4 105.70(16) . . ? O7 Cu1 O1 95.71(13) . . ? O7 Cu1 N2 167.16(16) . . ? O1 Cu1 N2 89.18(15) . . ? O7 Cu1 N1 90.72(13) . . ? O1 Cu1 N1 164.58(16) . . ? N2 Cu1 N1 81.79(16) . . ? O7 Cu1 N7 98.19(16) . . ? O1 Cu1 N7 99.95(18) . . ? N2 Cu1 N7 92.63(18) . . ? N1 Cu1 N7 92.96(17) . . ? O3 Cu2 O5 97.27(13) . . ? O3 Cu2 N4 164.18(15) . . ? O5 Cu2 N4 88.87(14) . . ? O3 Cu2 N3 92.68(14) . . ? O5 Cu2 N3 169.84(15) . . ? N4 Cu2 N3 82.03(16) . . ? O3 Cu2 O8 90.35(16) . . ? O5 Cu2 O8 89.86(14) . . ? N4 Cu2 O8 104.28(17) . . ? N3 Cu2 O8 88.02(15) . . ? O6 Cu3 O2 97.26(12) . 2_756 ? O6 Cu3 N6 171.69(14) . . ? O2 Cu3 N6 91.02(14) 2_756 . ? O6 Cu3 N5 90.24(12) . . ? O2 Cu3 N5 166.46(13) 2_756 . ? N6 Cu3 N5 81.77(14) . . ? N8 C64 C63 149(2) . . ? O12' Cl1 O14 124.9(8) . . ? O12' Cl1 O11 119.5(7) . . ? O14 Cl1 O11 115.5(5) . . ? O12' Cl1 O13 48.6(8) . . ? O14 Cl1 O13 113.0(5) . . ? O11 Cl1 O13 110.8(5) . . ? O12' Cl1 O14' 115.2(7) . . ? O14 Cl1 O14' 40.6(5) . . ? O11 Cl1 O14' 107.4(5) . . ? O13 Cl1 O14' 141.2(6) . . ? O12' Cl1 O12 54.0(8) . . ? O14 Cl1 O12 109.1(5) . . ? O11 Cl1 O12 104.8(4) . . ? O13 Cl1 O12 102.5(5) . . ? O14' Cl1 O12 73.5(6) . . ? O12' Cl1 O13' 108.9(7) . . ? O14 Cl1 O13' 58.4(6) . . ? O11 Cl1 O13' 104.2(5) . . ? O13 Cl1 O13' 65.3(6) . . ? O14' Cl1 O13' 99.1(6) . . ? O12 Cl1 O13' 150.9(6) . . ? O17 Cl2 O16' 122.1(6) . . ? O17 Cl2 O15 119.7(5) . . ? O16' Cl2 O15 117.3(5) . . ? O17 Cl2 O18' 47.5(6) . . ? O16' Cl2 O18' 115.1(6) . . ? O15 Cl2 O18' 112.8(5) . . ? O17 Cl2 O16 114.9(6) . . ? O16' Cl2 O16 28.0(7) . . ? O15 Cl2 O16 112.5(5) . . ? O18' Cl2 O16 133.2(7) . . ? O17 Cl2 O17' 55.4(6) . . ? O16' Cl2 O17' 104.7(6) . . ? O15 Cl2 O17' 101.5(5) . . ? O18' Cl2 O17' 102.9(6) . . ? O16 Cl2 O17' 79.2(7) . . ? O17 Cl2 O18 104.4(6) . . ? O16' Cl2 O18 74.8(7) . . ? O15 Cl2 O18 99.3(5) . . ? O18' Cl2 O18 58.5(7) . . ? O16 Cl2 O18 102.7(6) . . ? O17' Cl2 O18 156.5(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 106.9(5) . . . . ? N1 C1 C2 C7 -77.2(5) . . . . ? C7 C2 C3 C4 -0.4(8) . . . . ? C1 C2 C3 C4 175.6(5) . . . . ? C2 C3 C4 C5 0.7(10) . . . . ? C3 C4 C5 C6 -0.9(11) . . . . ? C4 C5 C6 C7 0.7(11) . . . . ? C5 C6 C7 C2 -0.3(9) . . . . ? C5 C6 C7 C8 -179.5(6) . . . . ? C3 C2 C7 C6 0.2(7) . . . . ? C1 C2 C7 C6 -175.8(5) . . . . ? C3 C2 C7 C8 179.3(5) . . . . ? C1 C2 C7 C8 3.4(7) . . . . ? C6 C7 C8 C13 -140.0(5) . . . . ? C2 C7 C8 C13 40.8(7) . . . . ? C6 C7 C8 C9 40.1(7) . . . . ? C2 C7 C8 C9 -139.0(5) . . . . ? C13 C8 C9 C10 -1.5(8) . . . . ? C7 C8 C9 C10 178.4(5) . . . . ? C8 C9 C10 C11 -0.4(9) . . . . ? C9 C10 C11 C12 1.1(10) . . . . ? C10 C11 C12 C13 0.1(10) . . . . ? C11 C12 C13 C8 -2.0(8) . . . . ? C11 C12 C13 C14 171.9(5) . . . . ? C9 C8 C13 C12 2.6(7) . . . . ? C7 C8 C13 C12 -177.2(5) . . . . ? C9 C8 C13 C14 -171.3(4) . . . . ? C7 C8 C13 C14 8.9(7) . . . . ? C12 C13 C14 N1 110.6(5) . . . . ? C8 C13 C14 N1 -75.6(6) . . . . ? N1 C15 C16 N2 34.2(7) . . . . ? N1 C15 C16 C17 -147.8(6) . . . . ? N2 C16 C17 C18 3.2(10) . . . . ? C15 C16 C17 C18 -174.7(6) . . . . ? C16 C17 C18 C19 -0.8(11) . . . . ? C17 C18 C19 C20 -1.0(11) . . . . ? C18 C19 C20 N2 0.6(11) . . . . ? N3 C21 C22 C23 -112.1(6) . . . . ? N3 C21 C22 C27 75.3(6) . . . . ? C27 C22 C23 C24 2.8(9) . . . . ? C21 C22 C23 C24 -169.7(6) . . . . ? C22 C23 C24 C25 -0.5(11) . . . . ? C23 C24 C25 C26 -1.0(11) . . . . ? C24 C25 C26 C27 0.2(10) . . . . ? C23 C22 C27 C26 -3.5(8) . . . . ? C21 C22 C27 C26 169.0(5) . . . . ? C23 C22 C27 C28 177.4(5) . . . . ? C21 C22 C27 C28 -10.1(7) . . . . ? C25 C26 C27 C22 2.0(8) . . . . ? C25 C26 C27 C28 -178.9(5) . . . . ? C22 C27 C28 C33 -37.7(7) . . . . ? C26 C27 C28 C33 143.2(5) . . . . ? C22 C27 C28 C29 142.4(6) . . . . ? C26 C27 C28 C29 -36.7(8) . . . . ? C33 C28 C29 C30 2.0(9) . . . . ? C27 C28 C29 C30 -178.1(6) . . . . ? C28 C29 C30 C31 0.0(10) . . . . ? C29 C30 C31 C32 -1.3(10) . . . . ? C30 C31 C32 C33 0.7(9) . . . . ? C31 C32 C33 C28 1.3(9) . . . . ? C31 C32 C33 C34 -175.3(5) . . . . ? C29 C28 C33 C32 -2.6(8) . . . . ? C27 C28 C33 C32 177.5(5) . . . . ? C29 C28 C33 C34 174.0(5) . . . . ? C27 C28 C33 C34 -6.0(7) . . . . ? C32 C33 C34 N3 -106.0(6) . . . . ? C28 C33 C34 N3 77.4(6) . . . . ? N3 C35 C36 N4 -34.2(6) . . . . ? N3 C35 C36 C37 149.0(5) . . . . ? N4 C36 C37 C38 1.6(9) . . . . ? C35 C36 C37 C38 178.1(6) . . . . ? C36 C37 C38 C39 -2.0(10) . . . . ? C37 C38 C39 C40 1.0(10) . . . . ? C38 C39 C40 N4 0.4(9) . . . . ? N5 C41 C42 C43 105.6(5) . . . . ? N5 C41 C42 C47 -76.2(5) . . . . ? C47 C42 C43 C44 0.8(8) . . . . ? C41 C42 C43 C44 178.9(5) . . . . ? C42 C43 C44 C45 -0.3(9) . . . . ? C43 C44 C45 C46 -0.3(10) . . . . ? C44 C45 C46 C47 0.5(9) . . . . ? C43 C42 C47 C46 -0.5(7) . . . . ? C41 C42 C47 C46 -178.7(4) . . . . ? C43 C42 C47 C48 179.2(4) . . . . ? C41 C42 C47 C48 1.0(6) . . . . ? C45 C46 C47 C42 -0.1(7) . . . . ? C45 C46 C47 C48 -179.8(5) . . . . ? C42 C47 C48 C53 43.8(6) . . . . ? C46 C47 C48 C53 -136.5(5) . . . . ? C42 C47 C48 C49 -137.0(4) . . . . ? C46 C47 C48 C49 42.7(6) . . . . ? C53 C48 C49 C50 -0.4(7) . . . . ? C47 C48 C49 C50 -179.6(4) . . . . ? C48 C49 C50 C51 -0.6(7) . . . . ? C49 C50 C51 C52 1.6(7) . . . . ? C50 C51 C52 C53 -1.6(7) . . . . ? C49 C48 C53 C52 0.4(6) . . . . ? C47 C48 C53 C52 179.6(4) . . . . ? C49 C48 C53 C54 -171.7(4) . . . . ? C47 C48 C53 C54 7.5(6) . . . . ? C51 C52 C53 C48 0.6(6) . . . . ? C51 C52 C53 C54 172.7(4) . . . . ? C48 C53 C54 N5 -75.0(5) . . . . ? C52 C53 C54 N5 112.9(4) . . . . ? N5 C55 C56 N6 32.1(5) . . . . ? N5 C55 C56 C57 -150.5(5) . . . . ? N6 C56 C57 C58 -0.7(8) . . . . ? C55 C56 C57 C58 -178.0(5) . . . . ? C56 C57 C58 C59 0.7(9) . . . . ? C57 C58 C59 C60 -0.6(10) . . . . ? C58 C59 C60 N6 0.4(10) . . . . ? C16 C15 N1 C1 -163.8(4) . . . . ? C16 C15 N1 C14 76.0(5) . . . . ? C16 C15 N1 Cu1 -39.7(5) . . . . ? C2 C1 N1 C15 -69.2(5) . . . . ? C2 C1 N1 C14 50.2(5) . . . . ? C2 C1 N1 Cu1 172.2(3) . . . . ? C13 C14 N1 C15 157.6(4) . . . . ? C13 C14 N1 C1 37.1(5) . . . . ? C13 C14 N1 Cu1 -88.6(4) . . . . ? C17 C16 N2 C20 -3.5(9) . . . . ? C15 C16 N2 C20 174.5(5) . . . . ? C17 C16 N2 Cu1 172.1(5) . . . . ? C15 C16 N2 Cu1 -9.9(6) . . . . ? C19 C20 N2 C16 1.6(9) . . . . ? C19 C20 N2 Cu1 -173.5(5) . . . . ? C36 C35 N3 C34 164.8(4) . . . . ? C36 C35 N3 C21 -73.9(5) . . . . ? C36 C35 N3 Cu2 44.1(4) . . . . ? C33 C34 N3 C35 71.8(5) . . . . ? C33 C34 N3 C21 -48.4(6) . . . . ? C33 C34 N3 Cu2 -173.7(4) . . . . ? C22 C21 N3 C35 -159.6(5) . . . . ? C22 C21 N3 C34 -37.9(6) . . . . ? C22 C21 N3 Cu2 88.2(5) . . . . ? C37 C36 N4 C40 -0.2(8) . . . . ? C35 C36 N4 C40 -177.1(4) . . . . ? C37 C36 N4 Cu2 -178.7(4) . . . . ? C35 C36 N4 Cu2 4.5(5) . . . . ? C39 C40 N4 C36 -0.8(8) . . . . ? C39 C40 N4 Cu2 177.4(4) . . . . ? C56 C55 N5 C41 -164.0(4) . . . . ? C56 C55 N5 C54 75.1(4) . . . . ? C56 C55 N5 Cu3 -39.3(4) . . . . ? C42 C41 N5 C55 -69.3(5) . . . . ? C42 C41 N5 C54 50.4(4) . . . . ? C42 C41 N5 Cu3 172.6(3) . . . . ? C53 C54 N5 C55 156.8(3) . . . . ? C53 C54 N5 C41 36.6(4) . . . . ? C53 C54 N5 Cu3 -90.4(3) . . . . ? C59 C60 N6 C56 -0.4(8) . . . . ? C59 C60 N6 Cu3 -175.0(5) . . . . ? C57 C56 N6 C60 0.6(7) . . . . ? C55 C56 N6 C60 178.1(4) . . . . ? C57 C56 N6 Cu3 175.7(4) . . . . ? C55 C56 N6 Cu3 -6.8(5) . . . . ? C62 C61 N7 Cu1 -87(48) . . . . ? Cu2 O3 P1 O1 -73.2(3) . . . . ? Cu2 O3 P1 O2 157.5(2) . . . . ? Cu2 O3 P1 O4 43.4(3) . . . . ? Cu1 O1 P1 O3 93.0(3) . . . . ? Cu1 O1 P1 O2 -137.7(3) . . . . ? Cu1 O1 P1 O4 -24.7(4) . . . . ? Cu3 O2 P1 O3 18.4(3) 2_756 . . . ? Cu3 O2 P1 O1 -111.0(2) 2_756 . . . ? Cu3 O2 P1 O4 134.7(2) 2_756 . . . ? P2 O4 P1 O3 -66.5(2) . . . . ? P2 O4 P1 O1 54.5(3) . . . . ? P2 O4 P1 O2 173.64(19) . . . . ? Cu3 O6 P2 O7 160.6(2) . . . . ? Cu3 O6 P2 O5 32.7(3) . . . . ? Cu3 O6 P2 O4 -82.6(3) . . . . ? Cu1 O7 P2 O6 159.6(2) . . . . ? Cu1 O7 P2 O5 -72.7(3) . . . . ? Cu1 O7 P2 O4 42.9(3) . . . . ? Cu2 O5 P2 O6 -140.7(2) . . . . ? Cu2 O5 P2 O7 91.5(3) . . . . ? Cu2 O5 P2 O4 -24.9(3) . . . . ? P1 O4 P2 O6 174.98(18) . . . . ? P1 O4 P2 O7 -64.7(2) . . . . ? P1 O4 P2 O5 55.4(2) . . . . ? P2 O7 Cu1 O1 -18.2(3) . . . . ? P2 O7 Cu1 N2 -130.2(6) . . . . ? P2 O7 Cu1 N1 175.8(3) . . . . ? P2 O7 Cu1 N7 82.7(3) . . . . ? P1 O1 Cu1 O7 8.4(4) . . . . ? P1 O1 Cu1 N2 176.5(4) . . . . ? P1 O1 Cu1 N1 122.6(5) . . . . ? P1 O1 Cu1 N7 -90.9(4) . . . . ? C16 N2 Cu1 O7 -65.6(8) . . . . ? C20 N2 Cu1 O7 109.7(8) . . . . ? C16 N2 Cu1 O1 -178.2(4) . . . . ? C20 N2 Cu1 O1 -3.0(5) . . . . ? C16 N2 Cu1 N1 -10.8(4) . . . . ? C20 N2 Cu1 N1 164.5(5) . . . . ? C16 N2 Cu1 N7 81.8(4) . . . . ? C20 N2 Cu1 N7 -102.9(5) . . . . ? C15 N1 Cu1 O7 -162.8(3) . . . . ? C1 N1 Cu1 O7 -41.4(3) . . . . ? C14 N1 Cu1 O7 81.4(3) . . . . ? C15 N1 Cu1 O1 82.4(6) . . . . ? C1 N1 Cu1 O1 -156.3(5) . . . . ? C14 N1 Cu1 O1 -33.5(7) . . . . ? C15 N1 Cu1 N2 27.7(3) . . . . ? C1 N1 Cu1 N2 149.0(3) . . . . ? C14 N1 Cu1 N2 -88.2(3) . . . . ? C15 N1 Cu1 N7 -64.6(3) . . . . ? C1 N1 Cu1 N7 56.8(3) . . . . ? C14 N1 Cu1 N7 179.6(3) . . . . ? C61 N7 Cu1 O7 113(3) . . . . ? C61 N7 Cu1 O1 -150(3) . . . . ? C61 N7 Cu1 N2 -60(3) . . . . ? C61 N7 Cu1 N1 22(3) . . . . ? P1 O3 Cu2 O5 -18.4(3) . . . . ? P1 O3 Cu2 N4 93.8(5) . . . . ? P1 O3 Cu2 N3 163.7(3) . . . . ? P1 O3 Cu2 O8 -108.3(3) . . . . ? P2 O5 Cu2 O3 8.6(3) . . . . ? P2 O5 Cu2 N4 -156.7(3) . . . . ? P2 O5 Cu2 N3 176.9(7) . . . . ? P2 O5 Cu2 O8 99.0(3) . . . . ? C36 N4 Cu2 O3 88.6(6) . . . . ? C40 N4 Cu2 O3 -89.7(6) . . . . ? C36 N4 Cu2 O5 -158.1(3) . . . . ? C40 N4 Cu2 O5 23.6(4) . . . . ? C36 N4 Cu2 N3 17.3(3) . . . . ? C40 N4 Cu2 N3 -161.0(4) . . . . ? C36 N4 Cu2 O8 -68.5(4) . . . . ? C40 N4 Cu2 O8 113.1(4) . . . . ? C35 N3 Cu2 O3 161.7(3) . . . . ? C34 N3 Cu2 O3 42.3(3) . . . . ? C21 N3 Cu2 O3 -82.4(3) . . . . ? C35 N3 Cu2 O5 -6.7(10) . . . . ? C34 N3 Cu2 O5 -126.0(8) . . . . ? C21 N3 Cu2 O5 109.2(8) . . . . ? C35 N3 Cu2 N4 -33.3(3) . . . . ? C34 N3 Cu2 N4 -152.7(3) . . . . ? C21 N3 Cu2 N4 82.6(3) . . . . ? C35 N3 Cu2 O8 71.4(3) . . . . ? C34 N3 Cu2 O8 -48.0(3) . . . . ? C21 N3 Cu2 O8 -172.7(3) . . . . ? P2 O6 Cu3 O2 40.8(3) . . . 2_756 ? P2 O6 Cu3 N6 -134.5(9) . . . . ? P2 O6 Cu3 N5 -150.5(3) . . . . ? C60 N6 Cu3 O6 145.7(9) . . . . ? C56 N6 Cu3 O6 -29.1(12) . . . . ? C60 N6 Cu3 O2 -29.7(4) . . . 2_756 ? C56 N6 Cu3 O2 155.5(3) . . . 2_756 ? C60 N6 Cu3 N5 161.8(4) . . . . ? C56 N6 Cu3 N5 -13.0(3) . . . . ? C55 N5 Cu3 O6 -153.9(3) . . . . ? C41 N5 Cu3 O6 -33.1(3) . . . . ? C54 N5 Cu3 O6 90.9(2) . . . . ? C55 N5 Cu3 O2 -30.0(7) . . . 2_756 ? C41 N5 Cu3 O2 90.8(6) . . . 2_756 ? C54 N5 Cu3 O2 -145.2(5) . . . 2_756 ? C55 N5 Cu3 N6 28.4(3) . . . . ? C41 N5 Cu3 N6 149.2(3) . . . . ? C54 N5 Cu3 N6 -86.8(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 67.94 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.415 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.081 _vrf_PLAT306_sabiah ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O10 RESPONSE: Water hydrogens could not be located in difference Fourier map. ; _vrf_PLAT780_sabiah ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: The coordinates shown in cif is the asymmetric unit which forms only half of the molecule. ; # end Validation Reply Form ############################################################### data_615836 _database_code_depnum_ccdc_archive 'CCDC 615836' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H55 Cl2 Cu2 N6 O14 P' _chemical_formula_weight 1265.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4129(3) _cell_length_b 26.9168(5) _cell_length_c 14.6457(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.0740(10) _cell_angle_gamma 90.00 _cell_volume 5625.47(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9675 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 29.2 _exptl_crystal_description rectangular _exptl_crystal_colour blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 0.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.710 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS(Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker axs kappa apex2 CCD Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 64588 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9880 _reflns_number_gt 8432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'SIR92 (WinGX)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP2 (WinGX)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0727P)^2^+7.3065P] 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 SHELXL _refine_ls_extinction_coef 0.0043(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9880 _refine_ls_number_parameters 766 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1398 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.147 _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 C1 C 0.3381(2) 0.16703(12) 0.0161(2) 0.0285(7) Uani 1 1 d . . . H1A H 0.3662 0.1673 0.0803 0.034 Uiso 1 1 calc R . . H1B H 0.3883 0.1708 -0.0211 0.034 Uiso 1 1 calc R . . C2 C 0.2733(2) 0.21109(12) -0.0009(2) 0.0307(7) Uani 1 1 d . . . C3 C 0.2822(3) 0.24414(14) -0.0721(3) 0.0400(9) Uani 1 1 d . . . H3 H 0.3231 0.2369 -0.1140 0.048 Uiso 1 1 calc R . . C4 C 0.2312(3) 0.28747(15) -0.0811(3) 0.0513(11) Uani 1 1 d . . . H4 H 0.2380 0.3094 -0.1288 0.062 Uiso 1 1 calc R . . C5 C 0.1703(3) 0.29836(15) -0.0197(3) 0.0524(11) Uani 1 1 d . . . H5 H 0.1360 0.3277 -0.0259 0.063 Uiso 1 1 calc R . . C6 C 0.1597(3) 0.26605(14) 0.0510(3) 0.0450(10) Uani 1 1 d . . . H6 H 0.1182 0.2738 0.0921 0.054 Uiso 1 1 calc R . . C7 C 0.2104(3) 0.22182(13) 0.0616(2) 0.0332(8) Uani 1 1 d . . . C8 C 0.1979(3) 0.18665(14) 0.1369(2) 0.0338(8) Uani 1 1 d . . . C9 C 0.1909(3) 0.20396(16) 0.2254(3) 0.0450(10) Uani 1 1 d . . . H9 H 0.1932 0.2379 0.2371 0.054 Uiso 1 1 calc R . . C10 C 0.1805(3) 0.17120(18) 0.2960(3) 0.0529(11) Uani 1 1 d . . . H10 H 0.1755 0.1832 0.3547 0.063 Uiso 1 1 calc R . . C11 C 0.1776(3) 0.12076(18) 0.2794(3) 0.0502(11) Uani 1 1 d . . . H11 H 0.1719 0.0987 0.3273 0.060 Uiso 1 1 calc R . . C12 C 0.1829(3) 0.10276(14) 0.1918(3) 0.0388(9) Uani 1 1 d . . . H12 H 0.1793 0.0687 0.1808 0.047 Uiso 1 1 calc R . . C13 C 0.1937(2) 0.13527(13) 0.1196(2) 0.0316(8) Uani 1 1 d . . . C14 C 0.1965(2) 0.11592(13) 0.0236(2) 0.0300(7) Uani 1 1 d . . . H14A H 0.1737 0.0820 0.0201 0.036 Uiso 1 1 calc R . . H14B H 0.1543 0.1356 -0.0195 0.036 Uiso 1 1 calc R . . C15 C 0.3526(2) 0.07856(12) 0.0470(2) 0.0286(7) Uani 1 1 d . . . H15A H 0.3188 0.0473 0.0463 0.034 Uiso 1 1 calc R . . H15B H 0.3693 0.0889 0.1107 0.034 Uiso 1 1 calc R . . C16 C 0.4394(2) 0.07195(11) 0.0028(2) 0.0264(7) Uani 1 1 d . . . C17 C 0.5266(3) 0.06104(13) 0.0510(2) 0.0340(8) Uani 1 1 d . . . H17 H 0.5342 0.0573 0.1148 0.041 Uiso 1 1 calc R . . C18 C 0.6019(3) 0.05580(14) 0.0034(3) 0.0379(9) Uani 1 1 d . . . H18 H 0.6611 0.0486 0.0348 0.045 Uiso 1 1 calc R . . C19 C 0.5889(3) 0.06134(14) -0.0912(3) 0.0361(8) Uani 1 1 d . . . H19 H 0.6388 0.0577 -0.1245 0.043 Uiso 1 1 calc R . . C20 C 0.5004(2) 0.07238(13) -0.1353(2) 0.0296(7) Uani 1 1 d . . . H20 H 0.4915 0.0763 -0.1990 0.036 Uiso 1 1 calc R . . C21 C 0.3609(2) -0.03014(12) -0.2848(2) 0.0245(7) Uani 1 1 d . . . H21A H 0.3149 -0.0423 -0.2478 0.029 Uiso 1 1 calc R . . H21B H 0.3949 -0.0032 -0.2511 0.029 Uiso 1 1 calc R . . C22 C 0.4290(2) -0.07164(12) -0.2968(2) 0.0272(7) Uani 1 1 d . . . C23 C 0.4093(3) -0.12033(13) -0.2720(2) 0.0354(8) Uani 1 1 d . . . H23 H 0.3524 -0.1275 -0.2519 0.042 Uiso 1 1 calc R . . C24 C 0.4737(3) -0.15798(15) -0.2772(3) 0.0484(10) Uani 1 1 d . . . H24 H 0.4599 -0.1902 -0.2607 0.058 Uiso 1 1 calc R . . C25 C 0.5581(3) -0.14774(16) -0.3068(3) 0.0512(11) Uani 1 1 d . . . H25 H 0.6012 -0.1731 -0.3104 0.061 Uiso 1 1 calc R . . C26 C 0.5790(3) -0.09980(16) -0.3314(3) 0.0433(9) Uani 1 1 d . . . H26 H 0.6361 -0.0934 -0.3519 0.052 Uiso 1 1 calc R . . C27 C 0.5156(2) -0.06080(13) -0.3259(2) 0.0304(7) Uani 1 1 d . . . C28 C 0.5389(2) -0.00876(14) -0.3456(2) 0.0310(8) Uani 1 1 d . . . C29 C 0.6275(3) 0.01053(16) -0.3123(3) 0.0389(9) Uani 1 1 d . . . H29 H 0.6727 -0.0100 -0.2803 0.047 Uiso 1 1 calc R . . C30 C 0.6485(3) 0.05954(17) -0.3265(3) 0.0467(10) Uani 1 1 d . . . H30 H 0.7076 0.0718 -0.3039 0.056 Uiso 1 1 calc R . . C31 C 0.5827(3) 0.09048(16) -0.3738(3) 0.0462(10) Uani 1 1 d . . . H31 H 0.5970 0.1237 -0.3825 0.055 Uiso 1 1 calc R . . C32 C 0.4947(3) 0.07199(14) -0.4088(3) 0.0364(8) Uani 1 1 d . . . H32 H 0.4508 0.0929 -0.4418 0.044 Uiso 1 1 calc R . . C33 C 0.4718(2) 0.02258(13) -0.3949(2) 0.0284(7) Uani 1 1 d . . . C34 C 0.3794(2) 0.00167(13) -0.4395(2) 0.0276(7) Uani 1 1 d . . . H34A H 0.3914 -0.0284 -0.4723 0.033 Uiso 1 1 calc R . . H34B H 0.3505 0.0254 -0.4846 0.033 Uiso 1 1 calc R . . C35 C 0.2431(2) -0.04775(12) -0.4166(2) 0.0298(7) Uani 1 1 d . . . H35A H 0.2110 -0.0629 -0.3697 0.036 Uiso 1 1 calc R . . H35B H 0.2762 -0.0737 -0.4448 0.036 Uiso 1 1 calc R . . C36 C 0.1730(2) -0.02379(13) -0.4883(2) 0.0285(7) Uani 1 1 d . . . C37 C 0.1288(3) -0.04817(15) -0.5651(3) 0.0390(9) Uani 1 1 d . . . H37 H 0.1436 -0.0810 -0.5762 0.047 Uiso 1 1 calc R . . C38 C 0.0622(3) -0.02327(16) -0.6253(3) 0.0421(9) Uani 1 1 d . . . H38 H 0.0314 -0.0391 -0.6773 0.051 Uiso 1 1 calc R . . C39 C 0.0423(2) 0.02531(16) -0.6069(2) 0.0391(9) Uani 1 1 d . . . H39 H -0.0020 0.0428 -0.6468 0.047 Uiso 1 1 calc R . . C40 C 0.0886(2) 0.04820(14) -0.5285(2) 0.0321(8) Uani 1 1 d . . . H40 H 0.0745 0.0810 -0.5161 0.038 Uiso 1 1 calc R . . C41 C 0.1377(3) 0.22609(15) -0.3699(3) 0.0430(9) Uani 1 1 d . . . C42 C 0.0720(3) 0.21377(17) -0.4445(3) 0.0551(11) Uani 1 1 d . . . H42 H 0.0399 0.1837 -0.4465 0.066 Uiso 1 1 calc R . . C43 C 0.0555(4) 0.2474(2) -0.5157(4) 0.0647(13) Uani 1 1 d . . . H43 H 0.0113 0.2399 -0.5664 0.078 Uiso 1 1 calc R . . C44 C 0.1028(4) 0.2916(2) -0.5137(4) 0.0741(16) Uani 1 1 d . . . H44 H 0.0913 0.3135 -0.5631 0.089 Uiso 1 1 calc R . . C45 C 0.1670(4) 0.3034(2) -0.4389(4) 0.0740(15) Uani 1 1 d . . . H45 H 0.1981 0.3338 -0.4367 0.089 Uiso 1 1 calc R . . C46 C 0.1853(4) 0.27053(17) -0.3671(4) 0.0581(12) Uani 1 1 d . . . H46 H 0.2297 0.2782 -0.3167 0.070 Uiso 1 1 calc R . . C47 C -0.0333(3) 0.16855(14) -0.2181(3) 0.0431(9) Uani 1 1 d . . . C48 C -0.1292(3) 0.15953(19) -0.2303(4) 0.0598(12) Uani 1 1 d . . . H48 H -0.1560 0.1387 -0.2775 0.072 Uiso 1 1 calc R . . C49 C -0.1839(4) 0.1815(2) -0.1724(5) 0.0757(16) Uani 1 1 d . . . H49 H -0.2481 0.1755 -0.1804 0.091 Uiso 1 1 calc R . . C50 C -0.1451(4) 0.2123(2) -0.1026(5) 0.0749(16) Uani 1 1 d . . . H50 H -0.1827 0.2270 -0.0635 0.090 Uiso 1 1 calc R . . C51 C -0.0502(3) 0.22139(18) -0.0907(4) 0.0606(12) Uani 1 1 d . . . H51 H -0.0241 0.2423 -0.0435 0.073 Uiso 1 1 calc R . . C52 C 0.0070(3) 0.19973(15) -0.1483(3) 0.0490(10) Uani 1 1 d . . . H52 H 0.0711 0.2060 -0.1403 0.059 Uiso 1 1 calc R . . C53 C 0.9502(4) 0.0775(2) 0.9548(4) 0.0679(14) Uani 1 1 d D . . C54 C 0.8733(3) 0.04837(18) 0.9095(4) 0.0573(12) Uani 1 1 d . . . C55 C 0.9455(5) 0.1517(2) 0.1801(5) 0.087(2) Uani 1 1 d D . . C56 C 0.9295(5) 0.1425(2) 0.2748(7) 0.091(2) Uani 1 1 d . . . N1 N 0.29206(19) 0.11711(10) -0.00505(18) 0.0249(6) Uani 1 1 d . . . N2 N 0.42640(19) 0.07768(10) -0.08940(18) 0.0260(6) Uani 1 1 d . . . N3 N 0.31087(18) -0.01025(10) -0.37353(17) 0.0231(6) Uani 1 1 d . . . N4 N 0.15310(18) 0.02393(10) -0.47036(18) 0.0265(6) Uani 1 1 d . . . N5 N 0.8129(3) 0.0255(2) 0.8742(4) 0.0864(15) Uani 1 1 d . . . N6 N 0.9158(5) 0.1349(2) 0.3483(6) 0.124(3) Uani 1 1 d . . . O1 O 0.31697(16) 0.08004(8) -0.26419(15) 0.0264(5) Uani 1 1 d D . . O2 O 0.17382(17) 0.12729(9) -0.18247(16) 0.0346(6) Uani 1 1 d . . . O3 O 0.13955(18) 0.10823(9) -0.35467(18) 0.0402(6) Uani 1 1 d . . . O4 O 0.01678(19) 0.14366(10) -0.27909(19) 0.0447(7) Uani 1 1 d . . . O5 O 0.1596(2) 0.19599(10) -0.29205(18) 0.0448(6) Uani 1 1 d . . . O6 O 0.2261(2) 0.02072(10) -0.10967(18) 0.0503(8) Uani 1 1 d . . . O7 O 0.14629(17) 0.00246(10) -0.25635(17) 0.0399(6) Uani 1 1 d . . . O8 O 0.1844(2) -0.06035(10) -0.1471(2) 0.0581(8) Uani 1 1 d . . . O9 O 0.0678(2) -0.00306(19) -0.1290(3) 0.0931(15) Uani 1 1 d . . . O10 O 0.5502(3) 0.1946(3) 0.7463(4) 0.148(3) Uani 1 1 d . . . O11 O 0.4244(7) 0.24863(17) 0.7465(5) 0.183(4) Uani 1 1 d . . . O12 O 0.4107(4) 0.17235(16) 0.7881(5) 0.137(3) Uani 1 1 d . . . O13 O 0.4227(6) 0.1876(4) 0.6381(5) 0.243(6) Uani 1 1 d . . . O14 O 0.2819(3) 0.1299(2) 0.5252(3) 0.0993(15) Uani 1 1 d D . . P1 P 0.12740(7) 0.14065(3) -0.27631(7) 0.0343(2) Uani 1 1 d . . . Cu1 Cu 0.29710(3) 0.098579(14) -0.14157(3) 0.02528(13) Uani 1 1 d . . . Cu2 Cu 0.22940(3) 0.052352(14) -0.35892(3) 0.02387(13) Uani 1 1 d . . . Cl1 Cl 0.15466(6) -0.00993(3) -0.16003(6) 0.0323(2) Uani 1 1 d . . . Cl2 Cl 0.45136(10) 0.20152(4) 0.72795(10) 0.0699(4) Uani 1 1 d . . . H53B H 0.920(2) 0.1067(8) 0.964(3) 0.12(3) Uiso 1 1 d D . . H53A H 0.996(2) 0.0836(15) 0.919(3) 0.10(2) Uiso 1 1 d D . . H55A H 0.964(2) 0.1236(9) 0.152(3) 0.12(3) Uiso 1 1 d D . . H55B H 0.9905(19) 0.1760(9) 0.180(4) 0.14(3) Uiso 1 1 d D . . H53C H 0.977(3) 0.0648(18) 1.0109(16) 0.12(3) Uiso 1 1 d D . . H55C H 0.8895(19) 0.1630(14) 0.149(3) 0.14(3) Uiso 1 1 d D . . H1 H 0.339(3) 0.1055(9) -0.288(3) 0.036(11) Uiso 1 1 d D . . H142 H 0.311(3) 0.1588(9) 0.517(6) 0.14(4) Uiso 1 1 d D . . H141 H 0.225(3) 0.1341(18) 0.543(6) 0.147 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0283(17) 0.0294(17) 0.0280(18) -0.0041(14) 0.0049(14) 0.0012(14) C2 0.0340(19) 0.0304(17) 0.0282(18) -0.0012(14) 0.0060(14) 0.0023(14) C3 0.046(2) 0.039(2) 0.037(2) 0.0024(16) 0.0149(17) 0.0021(17) C4 0.069(3) 0.041(2) 0.047(2) 0.0142(19) 0.019(2) 0.011(2) C5 0.069(3) 0.036(2) 0.054(3) 0.0043(19) 0.014(2) 0.020(2) C6 0.056(3) 0.039(2) 0.042(2) -0.0032(17) 0.0152(19) 0.0151(18) C7 0.040(2) 0.0327(18) 0.0276(18) -0.0037(14) 0.0071(15) 0.0039(15) C8 0.0339(19) 0.0392(19) 0.0293(19) -0.0001(15) 0.0086(15) 0.0095(15) C9 0.053(2) 0.049(2) 0.036(2) -0.0036(18) 0.0156(18) 0.0117(19) C10 0.062(3) 0.074(3) 0.026(2) -0.0003(19) 0.0168(19) 0.015(2) C11 0.051(3) 0.069(3) 0.034(2) 0.020(2) 0.0172(19) 0.013(2) C12 0.033(2) 0.044(2) 0.041(2) 0.0088(17) 0.0124(17) 0.0055(16) C13 0.0268(18) 0.0406(19) 0.0284(18) 0.0025(15) 0.0079(14) 0.0061(15) C14 0.0277(18) 0.0313(17) 0.0306(18) -0.0002(14) 0.0028(14) 0.0024(14) C15 0.0318(18) 0.0326(17) 0.0203(16) -0.0010(13) -0.0005(14) 0.0051(14) C16 0.0325(18) 0.0243(15) 0.0206(16) -0.0018(13) -0.0030(13) 0.0030(13) C17 0.038(2) 0.0381(19) 0.0226(17) -0.0024(14) -0.0076(15) 0.0087(16) C18 0.0305(19) 0.043(2) 0.036(2) -0.0051(16) -0.0093(16) 0.0097(16) C19 0.0264(18) 0.045(2) 0.036(2) -0.0066(16) 0.0006(15) 0.0070(15) C20 0.0280(18) 0.0356(18) 0.0242(17) -0.0031(14) 0.0001(14) 0.0046(14) C21 0.0218(16) 0.0342(17) 0.0171(15) -0.0003(13) 0.0013(12) 0.0038(13) C22 0.0256(17) 0.0351(18) 0.0189(16) -0.0048(13) -0.0036(13) 0.0031(14) C23 0.037(2) 0.0357(19) 0.0326(19) -0.0035(15) -0.0001(15) -0.0002(16) C24 0.059(3) 0.034(2) 0.049(2) 0.0000(18) -0.002(2) 0.0085(19) C25 0.049(3) 0.047(2) 0.056(3) -0.006(2) 0.001(2) 0.021(2) C26 0.032(2) 0.058(3) 0.040(2) -0.0024(18) 0.0044(17) 0.0131(18) C27 0.0266(18) 0.0436(19) 0.0194(16) -0.0048(14) -0.0019(13) 0.0079(15) C28 0.0254(17) 0.047(2) 0.0215(16) -0.0056(15) 0.0051(13) 0.0007(15) C29 0.0275(19) 0.061(2) 0.0279(19) -0.0035(17) 0.0022(15) -0.0028(17) C30 0.033(2) 0.072(3) 0.036(2) -0.013(2) 0.0073(17) -0.019(2) C31 0.052(3) 0.051(2) 0.039(2) -0.0072(18) 0.0178(19) -0.018(2) C32 0.040(2) 0.042(2) 0.0294(19) 0.0005(16) 0.0122(16) -0.0006(16) C33 0.0237(17) 0.0426(19) 0.0203(16) -0.0028(14) 0.0077(13) -0.0002(14) C34 0.0236(17) 0.0428(19) 0.0167(15) 0.0004(14) 0.0039(13) 0.0038(14) C35 0.0272(18) 0.0313(17) 0.0296(18) -0.0074(14) -0.0004(14) -0.0019(14) C36 0.0218(17) 0.0383(18) 0.0252(17) -0.0050(14) 0.0028(13) -0.0040(14) C37 0.032(2) 0.049(2) 0.034(2) -0.0124(17) -0.0013(16) -0.0058(16) C38 0.033(2) 0.064(3) 0.0273(19) -0.0077(18) -0.0054(16) -0.0102(18) C39 0.0254(18) 0.062(3) 0.0266(19) 0.0105(17) -0.0076(14) -0.0076(17) C40 0.0264(18) 0.0414(19) 0.0274(18) 0.0064(15) 0.0001(14) -0.0026(15) C41 0.047(2) 0.044(2) 0.039(2) 0.0039(17) 0.0092(18) 0.0103(18) C42 0.053(3) 0.052(2) 0.058(3) 0.011(2) -0.001(2) 0.008(2) C43 0.060(3) 0.071(3) 0.060(3) 0.018(3) -0.002(2) 0.018(3) C44 0.081(4) 0.073(4) 0.072(4) 0.035(3) 0.021(3) 0.023(3) C45 0.082(4) 0.058(3) 0.084(4) 0.019(3) 0.019(3) -0.002(3) C46 0.064(3) 0.049(3) 0.063(3) 0.004(2) 0.015(2) -0.001(2) C47 0.038(2) 0.039(2) 0.051(2) 0.0074(18) 0.0038(18) 0.0109(17) C48 0.039(2) 0.061(3) 0.076(3) 0.004(2) 0.000(2) 0.003(2) C49 0.044(3) 0.076(4) 0.111(5) 0.003(3) 0.024(3) 0.005(3) C50 0.056(3) 0.075(4) 0.100(4) 0.002(3) 0.033(3) 0.015(3) C51 0.060(3) 0.056(3) 0.069(3) -0.006(2) 0.018(2) 0.006(2) C52 0.042(2) 0.046(2) 0.060(3) 0.004(2) 0.010(2) 0.0054(19) C53 0.069(3) 0.067(3) 0.066(4) 0.007(3) 0.002(3) -0.018(3) C54 0.043(3) 0.057(3) 0.070(3) 0.006(2) 0.004(2) 0.006(2) C55 0.078(4) 0.060(3) 0.127(6) -0.027(4) 0.035(4) -0.017(3) C56 0.081(4) 0.045(3) 0.158(7) -0.018(4) 0.058(5) -0.011(3) N1 0.0271(14) 0.0265(13) 0.0206(13) -0.0023(11) 0.0020(11) 0.0037(11) N2 0.0276(15) 0.0299(14) 0.0194(14) -0.0033(11) -0.0003(11) 0.0038(11) N3 0.0179(13) 0.0326(14) 0.0180(13) -0.0029(11) 0.0000(10) 0.0010(11) N4 0.0189(13) 0.0395(16) 0.0202(14) 0.0019(11) -0.0006(11) -0.0025(12) N5 0.051(3) 0.080(3) 0.122(5) -0.011(3) -0.009(3) 0.000(2) N6 0.136(6) 0.062(3) 0.193(8) 0.005(4) 0.094(6) 0.000(3) O1 0.0284(12) 0.0309(12) 0.0183(11) -0.0021(9) -0.0023(9) -0.0006(10) O2 0.0351(13) 0.0404(13) 0.0267(13) -0.0011(10) -0.0016(10) 0.0137(11) O3 0.0383(15) 0.0413(14) 0.0365(14) -0.0037(11) -0.0099(11) 0.0137(11) O4 0.0363(15) 0.0493(16) 0.0459(16) -0.0003(13) -0.0031(12) 0.0086(12) O5 0.0503(17) 0.0438(15) 0.0376(15) 0.0031(12) -0.0035(12) -0.0038(13) O6 0.077(2) 0.0354(14) 0.0320(15) 0.0007(11) -0.0158(14) -0.0103(14) O7 0.0309(14) 0.0616(17) 0.0253(13) 0.0011(12) -0.0023(10) -0.0088(12) O8 0.067(2) 0.0346(15) 0.067(2) 0.0040(14) -0.0114(16) -0.0083(14) O9 0.046(2) 0.171(4) 0.069(2) 0.041(3) 0.0340(18) 0.038(2) O10 0.077(3) 0.251(7) 0.126(4) -0.080(5) 0.053(3) -0.069(4) O11 0.345(11) 0.047(3) 0.182(6) 0.012(3) 0.126(7) 0.010(4) O12 0.104(4) 0.073(3) 0.255(8) 0.054(4) 0.098(4) -0.006(2) O13 0.175(7) 0.401(14) 0.133(6) -0.163(8) -0.044(5) 0.109(8) O14 0.070(3) 0.148(5) 0.082(3) 0.012(3) 0.016(2) 0.025(3) P1 0.0320(5) 0.0365(5) 0.0322(5) -0.0004(4) -0.0037(4) 0.0082(4) Cu1 0.0254(2) 0.0312(2) 0.0176(2) -0.00282(15) -0.00276(15) 0.00696(16) Cu2 0.0205(2) 0.0311(2) 0.0186(2) -0.00174(15) -0.00204(15) 0.00156(15) Cl1 0.0247(4) 0.0432(5) 0.0286(4) 0.0028(3) 0.0029(3) -0.0006(3) Cl2 0.0860(9) 0.0513(7) 0.0787(9) -0.0224(6) 0.0340(7) -0.0221(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 C1 C2 1.509(5) . ? C1 N1 1.511(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.390(5) . ? C2 C7 1.405(5) . ? C3 C4 1.375(6) . ? C3 H3 0.9300 . ? C4 C5 1.374(6) . ? C4 H4 0.9300 . ? C5 C6 1.377(6) . ? C5 H5 0.9300 . ? C6 C7 1.394(5) . ? C6 H6 0.9300 . ? C7 C8 1.483(5) . ? C8 C9 1.395(5) . ? C8 C13 1.406(5) . ? C9 C10 1.384(6) . ? C9 H9 0.9300 . ? C10 C11 1.379(7) . ? C10 H10 0.9300 . ? C11 C12 1.384(6) . ? C11 H11 0.9300 . ? C12 C13 1.398(5) . ? C12 H12 0.9300 . ? C13 C14 1.505(5) . ? C14 N1 1.496(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N1 1.494(4) . ? C15 C16 1.499(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N2 1.345(4) . ? C16 C17 1.384(5) . ? C17 C18 1.378(5) . ? C17 H17 0.9300 . ? C18 C19 1.380(5) . ? C18 H18 0.9300 . ? C19 C20 1.379(5) . ? C19 H19 0.9300 . ? C20 N2 1.345(4) . ? C20 H20 0.9300 . ? C21 N3 1.494(4) . ? C21 C22 1.513(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.400(5) . ? C22 C27 1.405(5) . ? C23 C24 1.383(5) . ? C23 H23 0.9300 . ? C24 C25 1.375(6) . ? C24 H24 0.9300 . ? C25 C26 1.384(6) . ? C25 H25 0.9300 . ? C26 C27 1.402(5) . ? C26 H26 0.9300 . ? C27 C28 1.478(5) . ? C28 C29 1.401(5) . ? C28 C33 1.405(5) . ? C29 C30 1.376(6) . ? C29 H29 0.9300 . ? C30 C31 1.374(6) . ? C30 H30 0.9300 . ? C31 C32 1.391(6) . ? C31 H31 0.9300 . ? C32 C33 1.392(5) . ? C32 H32 0.9300 . ? C33 C34 1.507(5) . ? C34 N3 1.510(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N3 1.483(4) . ? C35 C36 1.497(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N4 1.350(4) . ? C36 C37 1.378(5) . ? C37 C38 1.382(6) . ? C37 H37 0.9300 . ? C38 C39 1.373(6) . ? C38 H38 0.9300 . ? C39 C40 1.389(5) . ? C39 H39 0.9300 . ? C40 N4 1.339(4) . ? C40 H40 0.9300 . ? C41 C46 1.377(6) . ? C41 C42 1.382(6) . ? C41 O5 1.398(5) . ? C42 C43 1.375(6) . ? C42 H42 0.9300 . ? C43 C44 1.370(8) . ? C43 H43 0.9300 . ? C44 C45 1.369(9) . ? C44 H44 0.9300 . ? C45 C46 1.372(7) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C52 1.386(6) . ? C47 C48 1.389(6) . ? C47 O4 1.396(5) . ? C48 C49 1.371(7) . ? C48 H48 0.9300 . ? C49 C50 1.373(8) . ? C49 H49 0.9300 . ? C50 C51 1.376(7) . ? C50 H50 0.9300 . ? C51 C52 1.388(6) . ? C51 H51 0.9300 . ? C52 H52 0.9300 . ? C53 C54 1.442(7) . ? C53 H53B 0.91(4) . ? C53 H53A 0.92(4) . ? C53 H53C 0.92(3) . ? C54 N5 1.130(6) . ? C55 C56 1.458(10) . ? C55 H55A 0.92(3) . ? C55 H55B 0.92(3) . ? C55 H55C 0.92(3) . ? C56 N6 1.140(10) . ? N1 Cu1 2.072(3) . ? N2 Cu1 1.993(3) . ? N3 Cu2 2.082(3) . ? N4 Cu2 1.989(3) . ? O1 Cu2 1.892(2) . ? O1 Cu1 1.924(2) . ? O1 H1 0.85(3) . ? O2 P1 1.486(2) . ? O2 Cu1 1.953(2) . ? O3 P1 1.472(3) . ? O3 Cu2 1.991(2) . ? O4 P1 1.591(3) . ? O5 P1 1.586(3) . ? O6 Cl1 1.439(3) . ? O6 Cu1 2.407(3) . ? O7 Cl1 1.438(3) . ? O8 Cl1 1.428(3) . ? O9 Cl1 1.403(3) . ? O10 Cl2 1.424(6) . ? O11 Cl2 1.365(5) . ? O12 Cl2 1.372(4) . ? O13 Cl2 1.375(6) . ? O14 H142 0.90(3) . ? O14 H141 0.90(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 114.9(3) . . ? C2 C1 H1A 108.5 . . ? N1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? N1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C3 C2 C7 119.5(3) . . ? C3 C2 C1 120.4(3) . . ? C7 C2 C1 119.7(3) . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C5 C4 C3 120.0(4) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 120.8(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 118.6(3) . . ? C6 C7 C8 120.8(3) . . ? C2 C7 C8 120.6(3) . . ? C9 C8 C13 119.3(3) . . ? C9 C8 C7 120.7(3) . . ? C13 C8 C7 120.0(3) . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C11 C10 C9 120.0(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.3(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.6(4) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 119.1(3) . . ? C12 C13 C14 120.7(3) . . ? C8 C13 C14 120.2(3) . . ? N1 C14 C13 113.6(3) . . ? N1 C14 H14A 108.8 . . ? C13 C14 H14A 108.8 . . ? N1 C14 H14B 108.8 . . ? C13 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N1 C15 C16 108.9(3) . . ? N1 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? N1 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? N2 C16 C17 121.7(3) . . ? N2 C16 C15 114.4(3) . . ? C17 C16 C15 123.9(3) . . ? C18 C17 C16 119.1(3) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 119.4(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 118.7(3) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? N2 C20 C19 122.4(3) . . ? N2 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? N3 C21 C22 113.9(2) . . ? N3 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N3 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C27 119.6(3) . . ? C23 C22 C21 120.2(3) . . ? C27 C22 C21 120.0(3) . . ? C24 C23 C22 120.7(4) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.2(4) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C27 121.0(4) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C22 118.5(3) . . ? C26 C27 C28 122.0(3) . . ? C22 C27 C28 119.5(3) . . ? C29 C28 C33 119.0(3) . . ? C29 C28 C27 120.3(3) . . ? C33 C28 C27 120.7(3) . . ? C30 C29 C28 120.8(4) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C31 C30 C29 120.5(4) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 119.8(4) . . ? C30 C31 H31 120.1 . . ? C32 C31 H31 120.1 . . ? C31 C32 C33 120.7(4) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C28 119.2(3) . . ? C32 C33 C34 120.4(3) . . ? C28 C33 C34 120.1(3) . . ? C33 C34 N3 114.8(3) . . ? C33 C34 H34A 108.6 . . ? N3 C34 H34A 108.6 . . ? C33 C34 H34B 108.6 . . ? N3 C34 H34B 108.6 . . ? H34A C34 H34B 107.5 . . ? N3 C35 C36 110.2(3) . . ? N3 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? N3 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? N4 C36 C37 121.7(3) . . ? N4 C36 C35 114.5(3) . . ? C37 C36 C35 123.8(3) . . ? C36 C37 C38 119.3(4) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C39 C38 C37 118.8(3) . . ? C39 C38 H38 120.6 . . ? C37 C38 H38 120.6 . . ? C38 C39 C40 119.7(3) . . ? C38 C39 H39 120.2 . . ? C40 C39 H39 120.2 . . ? N4 C40 C39 121.3(3) . . ? N4 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C46 C41 C42 121.0(4) . . ? C46 C41 O5 115.1(4) . . ? C42 C41 O5 123.8(4) . . ? C43 C42 C41 117.9(5) . . ? C43 C42 H42 121.1 . . ? C41 C42 H42 121.1 . . ? C44 C43 C42 121.5(5) . . ? C44 C43 H43 119.2 . . ? C42 C43 H43 119.2 . . ? C45 C44 C43 119.9(5) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 119.9(5) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 119.8(5) . . ? C45 C46 H46 120.1 . . ? C41 C46 H46 120.1 . . ? C52 C47 C48 120.5(4) . . ? C52 C47 O4 124.1(4) . . ? C48 C47 O4 115.3(4) . . ? C49 C48 C47 119.5(5) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 120.7(5) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C49 C50 C51 119.7(5) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C50 C51 C52 120.9(5) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C47 C52 C51 118.6(4) . . ? C47 C52 H52 120.7 . . ? C51 C52 H52 120.7 . . ? C54 C53 H53B 100(2) . . ? C54 C53 H53A 114(3) . . ? H53B C53 H53A 109(3) . . ? C54 C53 H53C 114(3) . . ? H53B C53 H53C 110(4) . . ? H53A C53 H53C 109(4) . . ? N5 C54 C53 179.8(7) . . ? C56 C55 H55A 113(3) . . ? C56 C55 H55B 109(4) . . ? H55A C55 H55B 109(4) . . ? C56 C55 H55C 107(4) . . ? H55A C55 H55C 110(3) . . ? H55B C55 H55C 110(3) . . ? N6 C56 C55 179.0(8) . . ? C15 N1 C14 109.7(2) . . ? C15 N1 C1 107.7(2) . . ? C14 N1 C1 110.9(2) . . ? C15 N1 Cu1 103.20(18) . . ? C14 N1 Cu1 115.1(2) . . ? C1 N1 Cu1 109.77(19) . . ? C20 N2 C16 118.7(3) . . ? C20 N2 Cu1 127.1(2) . . ? C16 N2 Cu1 114.1(2) . . ? C35 N3 C21 109.6(3) . . ? C35 N3 C34 108.9(2) . . ? C21 N3 C34 110.7(2) . . ? C35 N3 Cu2 104.31(19) . . ? C21 N3 Cu2 114.26(18) . . ? C34 N3 Cu2 108.85(19) . . ? C40 N4 C36 119.2(3) . . ? C40 N4 Cu2 126.1(2) . . ? C36 N4 Cu2 114.7(2) . . ? Cu2 O1 Cu1 127.97(12) . . ? Cu2 O1 H1 105(3) . . ? Cu1 O1 H1 107(3) . . ? P1 O2 Cu1 130.65(15) . . ? P1 O3 Cu2 128.42(15) . . ? C47 O4 P1 127.9(3) . . ? C41 O5 P1 128.7(3) . . ? Cl1 O6 Cu1 133.84(16) . . ? H142 O14 H141 113(4) . . ? O3 P1 O2 119.37(14) . . ? O3 P1 O5 111.98(16) . . ? O2 P1 O5 105.00(15) . . ? O3 P1 O4 103.82(15) . . ? O2 P1 O4 110.81(15) . . ? O5 P1 O4 105.11(15) . . ? O1 Cu1 O2 93.71(10) . . ? O1 Cu1 N2 91.77(10) . . ? O2 Cu1 N2 172.12(10) . . ? O1 Cu1 N1 173.40(10) . . ? O2 Cu1 N1 92.69(10) . . ? N2 Cu1 N1 81.70(10) . . ? O1 Cu1 O6 94.50(10) . . ? O2 Cu1 O6 90.62(11) . . ? N2 Cu1 O6 94.58(11) . . ? N1 Cu1 O6 87.07(10) . . ? O1 Cu2 N4 171.20(10) . . ? O1 Cu2 O3 92.83(10) . . ? N4 Cu2 O3 91.66(11) . . ? O1 Cu2 N3 93.80(10) . . ? N4 Cu2 N3 81.91(11) . . ? O3 Cu2 N3 173.28(10) . . ? O9 Cl1 O8 110.3(2) . . ? O9 Cl1 O7 109.40(19) . . ? O8 Cl1 O7 109.44(19) . . ? O9 Cl1 O6 111.4(3) . . ? O8 Cl1 O6 107.27(18) . . ? O7 Cl1 O6 108.98(16) . . ? O11 Cl2 O12 104.2(4) . . ? O11 Cl2 O13 112.8(6) . . ? O12 Cl2 O13 111.1(6) . . ? O11 Cl2 O10 112.9(5) . . ? O12 Cl2 O10 108.1(4) . . ? O13 Cl2 O10 107.7(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -111.4(4) . . . . ? N1 C1 C2 C7 75.6(4) . . . . ? C7 C2 C3 C4 0.9(6) . . . . ? C1 C2 C3 C4 -172.1(4) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? C3 C4 C5 C6 -0.1(7) . . . . ? C4 C5 C6 C7 0.0(7) . . . . ? C5 C6 C7 C2 0.5(6) . . . . ? C5 C6 C7 C8 -179.1(4) . . . . ? C3 C2 C7 C6 -1.0(6) . . . . ? C1 C2 C7 C6 172.0(3) . . . . ? C3 C2 C7 C8 178.6(4) . . . . ? C1 C2 C7 C8 -8.4(5) . . . . ? C6 C7 C8 C9 -42.2(6) . . . . ? C2 C7 C8 C9 138.2(4) . . . . ? C6 C7 C8 C13 138.2(4) . . . . ? C2 C7 C8 C13 -41.3(5) . . . . ? C13 C8 C9 C10 0.5(6) . . . . ? C7 C8 C9 C10 -179.1(4) . . . . ? C8 C9 C10 C11 0.4(7) . . . . ? C9 C10 C11 C12 -1.4(7) . . . . ? C10 C11 C12 C13 1.6(6) . . . . ? C11 C12 C13 C8 -0.7(6) . . . . ? C11 C12 C13 C14 -178.1(3) . . . . ? C9 C8 C13 C12 -0.3(5) . . . . ? C7 C8 C13 C12 179.3(3) . . . . ? C9 C8 C13 C14 177.1(3) . . . . ? C7 C8 C13 C14 -3.4(5) . . . . ? C12 C13 C14 N1 -106.6(4) . . . . ? C8 C13 C14 N1 76.1(4) . . . . ? N1 C15 C16 N2 -33.9(4) . . . . ? N1 C15 C16 C17 145.9(3) . . . . ? N2 C16 C17 C18 -0.2(5) . . . . ? C15 C16 C17 C18 -179.9(3) . . . . ? C16 C17 C18 C19 -0.2(5) . . . . ? C17 C18 C19 C20 0.5(6) . . . . ? C18 C19 C20 N2 -0.3(5) . . . . ? N3 C21 C22 C23 -109.7(3) . . . . ? N3 C21 C22 C27 75.4(4) . . . . ? C27 C22 C23 C24 -1.0(5) . . . . ? C21 C22 C23 C24 -175.9(3) . . . . ? C22 C23 C24 C25 0.1(6) . . . . ? C23 C24 C25 C26 0.1(7) . . . . ? C24 C25 C26 C27 0.6(6) . . . . ? C25 C26 C27 C22 -1.5(6) . . . . ? C25 C26 C27 C28 175.7(4) . . . . ? C23 C22 C27 C26 1.6(5) . . . . ? C21 C22 C27 C26 176.5(3) . . . . ? C23 C22 C27 C28 -175.6(3) . . . . ? C21 C22 C27 C28 -0.7(5) . . . . ? C26 C27 C28 C29 -42.5(5) . . . . ? C22 C27 C28 C29 134.7(3) . . . . ? C26 C27 C28 C33 139.9(4) . . . . ? C22 C27 C28 C33 -43.0(4) . . . . ? C33 C28 C29 C30 0.8(5) . . . . ? C27 C28 C29 C30 -176.9(3) . . . . ? C28 C29 C30 C31 -0.1(6) . . . . ? C29 C30 C31 C32 -0.9(6) . . . . ? C30 C31 C32 C33 1.2(5) . . . . ? C31 C32 C33 C28 -0.5(5) . . . . ? C31 C32 C33 C34 -174.9(3) . . . . ? C29 C28 C33 C32 -0.5(5) . . . . ? C27 C28 C33 C32 177.2(3) . . . . ? C29 C28 C33 C34 173.9(3) . . . . ? C27 C28 C33 C34 -8.4(4) . . . . ? C32 C33 C34 N3 -110.5(3) . . . . ? C28 C33 C34 N3 75.2(4) . . . . ? N3 C35 C36 N4 -31.5(4) . . . . ? N3 C35 C36 C37 150.8(3) . . . . ? N4 C36 C37 C38 -0.1(5) . . . . ? C35 C36 C37 C38 177.3(3) . . . . ? C36 C37 C38 C39 0.3(6) . . . . ? C37 C38 C39 C40 -0.4(6) . . . . ? C38 C39 C40 N4 0.4(5) . . . . ? C46 C41 C42 C43 -0.1(7) . . . . ? O5 C41 C42 C43 178.4(4) . . . . ? C41 C42 C43 C44 0.4(7) . . . . ? C42 C43 C44 C45 -1.0(8) . . . . ? C43 C44 C45 C46 1.4(9) . . . . ? C44 C45 C46 C41 -1.2(8) . . . . ? C42 C41 C46 C45 0.6(7) . . . . ? O5 C41 C46 C45 -178.1(4) . . . . ? C52 C47 C48 C49 -0.4(7) . . . . ? O4 C47 C48 C49 178.6(4) . . . . ? C47 C48 C49 C50 0.1(8) . . . . ? C48 C49 C50 C51 0.2(9) . . . . ? C49 C50 C51 C52 -0.1(8) . . . . ? C48 C47 C52 C51 0.5(6) . . . . ? O4 C47 C52 C51 -178.5(4) . . . . ? C50 C51 C52 C47 -0.2(7) . . . . ? C16 C15 N1 C14 166.9(3) . . . . ? C16 C15 N1 C1 -72.3(3) . . . . ? C16 C15 N1 Cu1 43.8(3) . . . . ? C13 C14 N1 C15 71.0(3) . . . . ? C13 C14 N1 C1 -47.9(4) . . . . ? C13 C14 N1 Cu1 -173.2(2) . . . . ? C2 C1 N1 C15 -158.8(3) . . . . ? C2 C1 N1 C14 -38.8(4) . . . . ? C2 C1 N1 Cu1 89.5(3) . . . . ? C19 C20 N2 C16 -0.1(5) . . . . ? C19 C20 N2 Cu1 174.9(3) . . . . ? C17 C16 N2 C20 0.3(5) . . . . ? C15 C16 N2 C20 -179.9(3) . . . . ? C17 C16 N2 Cu1 -175.3(3) . . . . ? C15 C16 N2 Cu1 4.5(3) . . . . ? C36 C35 N3 C21 162.7(3) . . . . ? C36 C35 N3 C34 -76.1(3) . . . . ? C36 C35 N3 Cu2 40.0(3) . . . . ? C22 C21 N3 C35 70.4(3) . . . . ? C22 C21 N3 C34 -49.6(4) . . . . ? C22 C21 N3 Cu2 -172.9(2) . . . . ? C33 C34 N3 C35 -157.3(3) . . . . ? C33 C34 N3 C21 -36.8(4) . . . . ? C33 C34 N3 Cu2 89.6(3) . . . . ? C39 C40 N4 C36 -0.3(5) . . . . ? C39 C40 N4 Cu2 177.0(2) . . . . ? C37 C36 N4 C40 0.2(5) . . . . ? C35 C36 N4 C40 -177.5(3) . . . . ? C37 C36 N4 Cu2 -177.4(3) . . . . ? C35 C36 N4 Cu2 4.9(3) . . . . ? C52 C47 O4 P1 7.0(6) . . . . ? C48 C47 O4 P1 -172.0(3) . . . . ? C46 C41 O5 P1 -172.5(3) . . . . ? C42 C41 O5 P1 8.8(6) . . . . ? Cu2 O3 P1 O2 -11.6(3) . . . . ? Cu2 O3 P1 O5 111.6(2) . . . . ? Cu2 O3 P1 O4 -135.5(2) . . . . ? Cu1 O2 P1 O3 38.4(3) . . . . ? Cu1 O2 P1 O5 -88.1(2) . . . . ? Cu1 O2 P1 O4 158.91(19) . . . . ? C41 O5 P1 O3 47.5(4) . . . . ? C41 O5 P1 O2 178.5(3) . . . . ? C41 O5 P1 O4 -64.5(3) . . . . ? C47 O4 P1 O3 177.9(3) . . . . ? C47 O4 P1 O2 48.6(3) . . . . ? C47 O4 P1 O5 -64.3(3) . . . . ? Cu2 O1 Cu1 O2 -41.06(16) . . . . ? Cu2 O1 Cu1 N2 144.60(16) . . . . ? Cu2 O1 Cu1 N1 153.3(8) . . . . ? Cu2 O1 Cu1 O6 49.86(16) . . . . ? P1 O2 Cu1 O1 -13.5(2) . . . . ? P1 O2 Cu1 N2 120.5(7) . . . . ? P1 O2 Cu1 N1 164.9(2) . . . . ? P1 O2 Cu1 O6 -108.0(2) . . . . ? C20 N2 Cu1 O1 21.0(3) . . . . ? C16 N2 Cu1 O1 -163.8(2) . . . . ? C20 N2 Cu1 O2 -113.1(8) . . . . ? C16 N2 Cu1 O2 62.1(9) . . . . ? C20 N2 Cu1 N1 -158.0(3) . . . . ? C16 N2 Cu1 N1 17.2(2) . . . . ? C20 N2 Cu1 O6 115.7(3) . . . . ? C16 N2 Cu1 O6 -69.1(2) . . . . ? C15 N1 Cu1 O1 -42.0(10) . . . . ? C14 N1 Cu1 O1 -161.4(8) . . . . ? C1 N1 Cu1 O1 72.6(9) . . . . ? C15 N1 Cu1 O2 152.3(2) . . . . ? C14 N1 Cu1 O2 32.9(2) . . . . ? C1 N1 Cu1 O2 -93.0(2) . . . . ? C15 N1 Cu1 N2 -33.2(2) . . . . ? C14 N1 Cu1 N2 -152.6(2) . . . . ? C1 N1 Cu1 N2 81.4(2) . . . . ? C15 N1 Cu1 O6 61.9(2) . . . . ? C14 N1 Cu1 O6 -57.6(2) . . . . ? C1 N1 Cu1 O6 176.5(2) . . . . ? Cl1 O6 Cu1 O1 -46.8(3) . . . . ? Cl1 O6 Cu1 O2 46.9(3) . . . . ? Cl1 O6 Cu1 N2 -139.0(3) . . . . ? Cl1 O6 Cu1 N1 139.6(3) . . . . ? Cu1 O1 Cu2 N4 176.8(6) . . . . ? Cu1 O1 Cu2 O3 56.18(16) . . . . ? Cu1 O1 Cu2 N3 -122.72(15) . . . . ? C40 N4 Cu2 O1 -101.3(7) . . . . ? C36 N4 Cu2 O1 76.1(8) . . . . ? C40 N4 Cu2 O3 19.4(3) . . . . ? C36 N4 Cu2 O3 -163.2(2) . . . . ? C40 N4 Cu2 N3 -162.5(3) . . . . ? C36 N4 Cu2 N3 14.8(2) . . . . ? P1 O3 Cu2 O1 -27.2(2) . . . . ? P1 O3 Cu2 N4 160.3(2) . . . . ? P1 O3 Cu2 N3 143.4(8) . . . . ? C35 N3 Cu2 O1 157.9(2) . . . . ? C21 N3 Cu2 O1 38.2(2) . . . . ? C34 N3 Cu2 O1 -86.1(2) . . . . ? C35 N3 Cu2 N4 -29.9(2) . . . . ? C21 N3 Cu2 N4 -149.5(2) . . . . ? C34 N3 Cu2 N4 86.2(2) . . . . ? C35 N3 Cu2 O3 -12.8(10) . . . . ? C21 N3 Cu2 O3 -132.4(9) . . . . ? C34 N3 Cu2 O3 103.3(9) . . . . ? Cu1 O6 Cl1 O9 -100.2(3) . . . . ? Cu1 O6 Cl1 O8 139.0(3) . . . . ? Cu1 O6 Cl1 O7 20.6(3) . . . . ? 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 H1 O12 0.90(5) 2.29(3) 2.880(6) 127(3) 1_554 O14 H141 O3 0.90(5) 2.19(4) 2.943(6) 141(6) 1_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.997 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.153 _vrf_PLAT220_sab ; PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min) ... 9.20 Ratio RESPONSE: This is due to the large librational motion of perchlorate moieties. ; _vrf_PLAT222_sab ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.07 Ratio RESPONSE: This is due to large libration of the peripheral parts of the molecule as compared to the center. ; _vrf_PLAT242_sab ; PROBLEM: Check Low Ueq as Compared to Neighbors for Cl2 RESPONSE: This is due to the large librational motion of perchlorate moiety. ; _vrf_PLAT780_sab ; PROBLEM: Coordinates do not Form a Properly Connected Set ? RESPONSE: The perchlorate (Cl2 O10 O11 O12 O13) is only very weakly coordinated to the metals. Hence it is represented with an equivalent sufficiently away from the metal center in the asymmetric unit for the sake of clarity. ; # end Validation Reply Form #======================================================================= data_615837 _database_code_depnum_ccdc_archive 'CCDC 615837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H38 Cl2 Cu2 N4 O10' _chemical_formula_weight 932.72 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' O O 0.0106 0.0060 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.2323(8) _cell_length_b 9.1681(4) _cell_length_c 20.8139(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.760(2) _cell_angle_gamma 90.00 _cell_volume 3841.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9422 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 32.8 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 1.312 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7602 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; Blessing, R.H. (1995) Acta Cryst. A51, 33-38. Sheldrick, G.M. (2004) SADABS, University of G\:ottingen, Germany ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker axs kappa Apex2' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85833 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6755 _reflns_number_gt 6051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)' _computing_structure_solution 'SIR92 (WinGX)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP2 (WinGX)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0429P)^2^+9.3125P] 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 6755 _refine_ls_number_parameters 531 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 1.171 _refine_ls_restrained_S_all 1.248 _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 C1 C 0.25982(16) 0.0801(4) 0.20691(15) 0.0185(7) Uani 1 1 d . . . H1A H 0.2806 -0.0017 0.1872 0.022 Uiso 1 1 calc R . . H1B H 0.2271 0.0411 0.2333 0.022 Uiso 1 1 calc R . . C2 C 0.31189(17) 0.1608(4) 0.24966(16) 0.0217(7) Uani 1 1 d . . . C3 C 0.30059(18) 0.1996(4) 0.31218(17) 0.0281(8) Uani 1 1 d . . . H3 H 0.2600 0.1772 0.3272 0.034 Uiso 1 1 calc R . . C4 C 0.3486(2) 0.2706(5) 0.35234(19) 0.0400(10) Uani 1 1 d . . . H4 H 0.3404 0.2958 0.3941 0.048 Uiso 1 1 calc R . . C5 C 0.4089(2) 0.3041(5) 0.3302(2) 0.0432(11) Uani 1 1 d . . . H5 H 0.4413 0.3524 0.3571 0.052 Uiso 1 1 calc R . . C6 C 0.42126(18) 0.2662(5) 0.26828(19) 0.0341(9) Uani 1 1 d . . . H6 H 0.4622 0.2881 0.2540 0.041 Uiso 1 1 calc R . . C7 C 0.37296(17) 0.1954(4) 0.22689(17) 0.0243(7) Uani 1 1 d . . . C8 C 0.38613(17) 0.1564(4) 0.15992(17) 0.0252(8) Uani 1 1 d . . . C9 C 0.44754(19) 0.1013(5) 0.1467(2) 0.0354(9) Uani 1 1 d . . . H9 H 0.4807 0.0859 0.1803 0.042 Uiso 1 1 calc R . . C10 C 0.4595(2) 0.0692(5) 0.0837(2) 0.0464(12) Uani 1 1 d . . . H10 H 0.5010 0.0348 0.0753 0.056 Uiso 1 1 calc R . . C11 C 0.4103(2) 0.0879(5) 0.0335(2) 0.0434(11) Uani 1 1 d . . . H11 H 0.4182 0.0641 -0.0085 0.052 Uiso 1 1 calc R . . C12 C 0.3495(2) 0.1420(4) 0.04599(18) 0.0320(9) Uani 1 1 d . . . H12 H 0.3164 0.1551 0.0121 0.038 Uiso 1 1 calc R . . C13 C 0.33684(17) 0.1773(4) 0.10849(17) 0.0226(7) Uani 1 1 d . . . C14 C 0.27374(16) 0.2562(4) 0.11912(16) 0.0224(7) Uani 1 1 d . . . H14A H 0.2853 0.3451 0.1429 0.027 Uiso 1 1 calc R . . H14B H 0.2519 0.2845 0.0774 0.027 Uiso 1 1 calc R . . C15 C 0.18264(16) 0.2840(4) 0.18289(17) 0.0210(7) Uani 1 1 d . . . H15A H 0.1758 0.3660 0.1535 0.025 Uiso 1 1 calc R . . H15B H 0.2052 0.3195 0.2232 0.025 Uiso 1 1 calc R . . C16 C 0.11699(16) 0.2212(4) 0.19498(15) 0.0188(7) Uani 1 1 d . . . C17 C 0.08028(17) 0.2692(4) 0.24370(16) 0.0215(7) Uani 1 1 d . . . H17 H 0.0982 0.3350 0.2747 0.026 Uiso 1 1 calc R . . C18 C 0.01641(17) 0.2166(4) 0.24489(17) 0.0244(8) Uani 1 1 d . . . H18 H -0.0098 0.2487 0.2763 0.029 Uiso 1 1 calc R . . C19 C -0.00831(16) 0.1166(4) 0.19948(17) 0.0240(8) Uani 1 1 d . . . H19 H -0.0515 0.0819 0.1994 0.029 Uiso 1 1 calc R . . C20 C 0.03177(17) 0.0684(4) 0.15406(17) 0.0222(7) Uani 1 1 d . . . H20 H 0.0156 -0.0018 0.1243 0.027 Uiso 1 1 calc R . . C21 C 0.25118(16) -0.3989(4) -0.03344(16) 0.0207(7) Uani 1 1 d . . . H21A H 0.2635 -0.4647 -0.0667 0.025 Uiso 1 1 calc R . . H21B H 0.2163 -0.4455 -0.0121 0.025 Uiso 1 1 calc R . . C22 C 0.31055(16) -0.3754(4) 0.01522(16) 0.0195(7) Uani 1 1 d . . . C23 C 0.30465(17) -0.3906(4) 0.08092(16) 0.0222(7) Uani 1 1 d . . . H23 H 0.2631 -0.4084 0.0948 0.027 Uiso 1 1 calc R . . C24 C 0.35981(19) -0.3795(4) 0.12594(17) 0.0286(8) Uani 1 1 d . . . H24 H 0.3551 -0.3899 0.1697 0.034 Uiso 1 1 calc R . . C25 C 0.42153(19) -0.3530(4) 0.10582(18) 0.0310(8) Uani 1 1 d . . . H25 H 0.4586 -0.3463 0.1359 0.037 Uiso 1 1 calc R . . C26 C 0.42834(17) -0.3365(4) 0.04024(18) 0.0273(8) Uani 1 1 d . . . H26 H 0.4700 -0.3180 0.0269 0.033 Uiso 1 1 calc R . . C27 C 0.37326(17) -0.3473(4) -0.00553(16) 0.0217(7) Uani 1 1 d . . . C28 C 0.37936(16) -0.3306(4) -0.07549(16) 0.0225(7) Uani 1 1 d . . . C29 C 0.42905(18) -0.4018(4) -0.10482(18) 0.0293(8) Uani 1 1 d . . . H29 H 0.4606 -0.4567 -0.0798 0.035 Uiso 1 1 calc R . . C30 C 0.4321(2) -0.3918(5) -0.17053(19) 0.0345(9) Uani 1 1 d . . . H30 H 0.4649 -0.4419 -0.1897 0.041 Uiso 1 1 calc R . . C31 C 0.3865(2) -0.3079(5) -0.20803(18) 0.0332(9) Uani 1 1 d . . . H31 H 0.3886 -0.3012 -0.2524 0.040 Uiso 1 1 calc R . . C32 C 0.33789(18) -0.2340(4) -0.17928(17) 0.0265(8) Uani 1 1 d . . . H32 H 0.3077 -0.1762 -0.2045 0.032 Uiso 1 1 calc R . . C33 C 0.33309(16) -0.2442(4) -0.11336(16) 0.0221(7) Uani 1 1 d . . . C34 C 0.27994(16) -0.1634(4) -0.08144(16) 0.0209(7) Uani 1 1 d . . . H34A H 0.3001 -0.1172 -0.0424 0.025 Uiso 1 1 calc R . . H34B H 0.2617 -0.0871 -0.1102 0.025 Uiso 1 1 calc R . . C35 C 0.18042(16) -0.2999(4) -0.12410(16) 0.0232(7) Uani 1 1 d . . . H35A H 0.2007 -0.3779 -0.1468 0.028 Uiso 1 1 calc R . . H35B H 0.1754 -0.2161 -0.1526 0.028 Uiso 1 1 calc R . . C36 C 0.11340(16) -0.3480(4) -0.10721(16) 0.0203(7) Uani 1 1 d . . . C37 C 0.07297(17) -0.4436(4) -0.14383(17) 0.0229(7) Uani 1 1 d . . . H37 H 0.0877 -0.4886 -0.1798 0.027 Uiso 1 1 calc R . . C38 C 0.01009(17) -0.4718(4) -0.12625(17) 0.0249(8) Uani 1 1 d . . . H38 H -0.0179 -0.5366 -0.1502 0.030 Uiso 1 1 calc R . . C39 C -0.01073(17) -0.4026(4) -0.07270(16) 0.0223(7) Uani 1 1 d . . . H39 H -0.0532 -0.4188 -0.0606 0.027 Uiso 1 1 calc R . . C40 C 0.03236(17) -0.3096(4) -0.03760(16) 0.0225(7) Uani 1 1 d . . . H40 H 0.0187 -0.2636 -0.0014 0.027 Uiso 1 1 calc R . . O1 O 0.22534(11) -0.0595(3) 0.05268(11) 0.0222(5) Uani 1 1 d D . . O2 O 0.09934(14) -0.0859(4) 0.04987(15) 0.0560(10) Uani 1 1 d D . . O3 O 0.13228(17) -0.1723(3) 0.2051(2) 0.0721(13) Uani 1 1 d . . . O4 O 0.23295(13) -0.2775(4) 0.19267(14) 0.0444(8) Uani 1 1 d . . . O5 O 0.1544(3) -0.4085(4) 0.2419(2) 0.0893(17) Uani 1 1 d . . . O6 O 0.14013(16) -0.3663(3) 0.13014(19) 0.0579(10) Uani 1 1 d . . . O7 O 0.17280(18) 0.2922(4) -0.0967(2) 0.0654(11) Uani 1 1 d . . . O8 O 0.06714(14) 0.2100(3) -0.08472(16) 0.0447(7) Uani 1 1 d . . . O9 O 0.15420(18) 0.0447(3) -0.07777(14) 0.0504(9) Uani 1 1 d . . . O10 O 0.1444(2) 0.2181(4) 0.00548(14) 0.0644(12) Uani 1 1 d . . . Cl1 Cl 0.16459(4) -0.30669(9) 0.19265(5) 0.0291(2) Uani 1 1 d . . . Cl2 Cl 0.13559(4) 0.19194(10) -0.06332(4) 0.0258(2) Uani 1 1 d . . . Cu1 Cu 0.160616(19) 0.04035(4) 0.098664(18) 0.01816(12) Uani 1 1 d D . . Cu2 Cu 0.161476(19) -0.16277(4) -0.005149(18) 0.01902(12) Uani 1 1 d D . . N1 N 0.22500(13) 0.1727(3) 0.15459(13) 0.0170(6) Uani 1 1 d . . . N2 N 0.09352(13) 0.1205(3) 0.15176(13) 0.0186(6) Uani 1 1 d . . . N3 N 0.22454(13) -0.2607(3) -0.06466(13) 0.0185(6) Uani 1 1 d . . . N4 N 0.09382(13) -0.2834(3) -0.05442(13) 0.0189(6) Uani 1 1 d . . . H1 H 0.2550(14) -0.114(4) 0.0783(3) 0.069(17) Uiso 1 1 d D . . H2 H 0.0754(3) -0.1515(6) 0.0708(3) 0.45(13) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0185(16) 0.0181(16) 0.0190(16) 0.0005(13) 0.0027(12) 0.0012(13) C2 0.0207(17) 0.0235(18) 0.0207(17) -0.0026(14) 0.0008(13) 0.0024(14) C3 0.0233(18) 0.037(2) 0.0240(18) -0.0039(16) 0.0022(14) 0.0002(16) C4 0.036(2) 0.061(3) 0.0224(19) -0.0159(19) -0.0003(16) -0.001(2) C5 0.030(2) 0.062(3) 0.035(2) -0.019(2) -0.0072(17) -0.009(2) C6 0.0199(18) 0.048(3) 0.034(2) -0.0074(19) 0.0012(15) -0.0044(17) C7 0.0185(17) 0.030(2) 0.0239(18) -0.0039(15) 0.0010(13) 0.0016(14) C8 0.0213(17) 0.0290(19) 0.0260(18) -0.0023(15) 0.0064(14) -0.0022(15) C9 0.0239(19) 0.046(2) 0.037(2) -0.0012(19) 0.0070(16) 0.0059(18) C10 0.038(2) 0.055(3) 0.050(3) 0.002(2) 0.027(2) 0.017(2) C11 0.054(3) 0.049(3) 0.030(2) -0.003(2) 0.0185(19) 0.007(2) C12 0.039(2) 0.034(2) 0.0244(19) -0.0011(16) 0.0101(16) -0.0027(17) C13 0.0212(17) 0.0224(18) 0.0248(18) -0.0011(14) 0.0058(14) -0.0044(14) C14 0.0200(17) 0.0229(18) 0.0242(17) 0.0026(14) 0.0022(13) -0.0018(14) C15 0.0196(17) 0.0156(16) 0.0272(18) -0.0041(14) -0.0012(13) 0.0031(13) C16 0.0200(16) 0.0157(16) 0.0199(16) 0.0036(13) -0.0026(13) 0.0044(13) C17 0.0239(17) 0.0203(17) 0.0200(16) 0.0006(14) 0.0005(13) 0.0055(14) C18 0.0255(18) 0.0221(18) 0.0267(18) 0.0091(15) 0.0084(14) 0.0085(15) C19 0.0153(16) 0.0228(18) 0.0342(19) 0.0110(15) 0.0036(14) 0.0012(14) C20 0.0219(17) 0.0195(17) 0.0244(17) 0.0041(14) -0.0012(13) -0.0023(14) C21 0.0175(16) 0.0175(17) 0.0266(17) -0.0027(14) -0.0006(13) 0.0023(13) C22 0.0181(16) 0.0152(16) 0.0251(17) -0.0019(13) 0.0013(13) 0.0039(13) C23 0.0212(17) 0.0214(18) 0.0244(17) -0.0007(14) 0.0042(13) 0.0026(14) C24 0.033(2) 0.034(2) 0.0193(17) -0.0016(15) 0.0036(15) 0.0019(16) C25 0.0257(19) 0.040(2) 0.0259(19) 0.0001(17) -0.0066(15) 0.0027(17) C26 0.0138(16) 0.038(2) 0.0291(19) 0.0012(16) -0.0005(14) 0.0023(15) C27 0.0206(17) 0.0221(18) 0.0223(17) -0.0015(14) 0.0018(13) 0.0055(14) C28 0.0169(16) 0.0283(19) 0.0221(17) -0.0012(14) 0.0012(13) 0.0011(14) C29 0.0219(18) 0.038(2) 0.0281(19) 0.0039(16) 0.0045(14) 0.0081(16) C30 0.034(2) 0.039(2) 0.033(2) 0.0012(18) 0.0154(17) 0.0080(18) C31 0.039(2) 0.040(2) 0.0212(18) 0.0012(16) 0.0056(16) -0.0011(18) C32 0.0266(18) 0.0280(19) 0.0241(18) 0.0031(15) -0.0018(14) 0.0002(15) C33 0.0196(17) 0.0226(18) 0.0234(17) -0.0017(14) -0.0007(13) -0.0025(14) C34 0.0178(16) 0.0188(17) 0.0253(17) -0.0011(14) -0.0018(13) 0.0022(13) C35 0.0193(17) 0.0294(19) 0.0197(17) -0.0094(14) -0.0037(13) 0.0031(14) C36 0.0190(16) 0.0198(17) 0.0206(16) -0.0008(13) -0.0047(13) 0.0069(13) C37 0.0265(18) 0.0177(17) 0.0229(17) -0.0042(14) -0.0046(14) 0.0036(14) C38 0.0252(18) 0.0191(18) 0.0283(19) 0.0012(14) -0.0081(14) -0.0029(14) C39 0.0195(16) 0.0203(17) 0.0259(17) 0.0062(14) -0.0032(13) 0.0008(14) C40 0.0226(17) 0.0242(18) 0.0205(17) 0.0020(14) 0.0006(13) 0.0053(14) O1 0.0206(12) 0.0202(12) 0.0242(12) -0.0081(10) -0.0056(9) 0.0027(10) O2 0.0248(14) 0.096(3) 0.0493(18) -0.0573(19) 0.0113(13) -0.0206(16) O3 0.043(2) 0.0242(17) 0.149(4) -0.017(2) 0.012(2) 0.0109(14) O4 0.0238(14) 0.071(2) 0.0386(16) -0.0221(15) 0.0044(12) -0.0080(14) O5 0.179(5) 0.0216(17) 0.083(3) -0.0084(17) 0.095(3) -0.016(2) O6 0.0500(19) 0.0276(16) 0.086(3) -0.0071(16) -0.0407(18) -0.0046(14) O7 0.058(2) 0.053(2) 0.093(3) -0.032(2) 0.047(2) -0.0291(18) O8 0.0302(15) 0.0443(18) 0.059(2) -0.0127(15) 0.0031(14) 0.0018(13) O9 0.084(2) 0.0376(18) 0.0281(15) -0.0041(13) -0.0006(15) 0.0366(17) O10 0.098(3) 0.063(2) 0.0263(16) -0.0169(15) -0.0199(16) 0.052(2) Cl1 0.0195(4) 0.0172(4) 0.0522(6) 0.0006(4) 0.0118(4) -0.0004(3) Cl2 0.0282(4) 0.0258(4) 0.0227(4) -0.0023(3) 0.0000(3) 0.0080(3) Cu1 0.0173(2) 0.0202(2) 0.0164(2) -0.00294(16) -0.00064(15) -0.00114(16) Cu2 0.0168(2) 0.0217(2) 0.0176(2) -0.00554(16) -0.00276(15) 0.00180(16) N1 0.0165(13) 0.0150(14) 0.0192(13) 0.0003(11) 0.0013(10) 0.0022(11) N2 0.0196(14) 0.0185(14) 0.0172(13) 0.0021(11) -0.0013(11) -0.0016(11) N3 0.0130(13) 0.0192(14) 0.0220(14) -0.0038(11) -0.0050(11) 0.0019(11) N4 0.0191(14) 0.0185(14) 0.0181(13) -0.0005(11) -0.0036(11) 0.0034(11) _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 C1 N1 1.500(4) . ? C1 C2 1.504(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.390(5) . ? C2 C7 1.403(5) . ? C3 C4 1.380(5) . ? C3 H3 0.9300 . ? C4 C5 1.382(6) . ? C4 H4 0.9300 . ? C5 C6 1.382(6) . ? C5 H5 0.9300 . ? C6 C7 1.396(5) . ? C6 H6 0.9300 . ? C7 C8 1.489(5) . ? C8 C9 1.394(5) . ? C8 C13 1.401(5) . ? C9 C10 1.388(6) . ? C9 H9 0.9300 . ? C10 C11 1.381(7) . ? C10 H10 0.9300 . ? C11 C12 1.375(6) . ? C11 H11 0.9300 . ? C12 C13 1.389(5) . ? C12 H12 0.9300 . ? C13 C14 1.503(5) . ? C14 N1 1.500(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N1 1.491(4) . ? C15 C16 1.492(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N2 1.342(4) . ? C16 C17 1.387(5) . ? C17 C18 1.382(5) . ? C17 H17 0.9300 . ? C18 C19 1.374(5) . ? C18 H18 0.9300 . ? C19 C20 1.378(5) . ? C19 H19 0.9300 . ? C20 N2 1.343(4) . ? C20 H20 0.9300 . ? C21 N3 1.500(4) . ? C21 C22 1.507(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.392(5) . ? C22 C27 1.405(5) . ? C23 C24 1.387(5) . ? C23 H23 0.9300 . ? C24 C25 1.378(5) . ? C24 H24 0.9300 . ? C25 C26 1.394(5) . ? C25 H25 0.9300 . ? C26 C27 1.395(5) . ? C26 H26 0.9300 . ? C27 C28 1.481(5) . ? C28 C29 1.390(5) . ? C28 C33 1.407(5) . ? C29 C30 1.378(5) . ? C29 H29 0.9300 . ? C30 C31 1.381(6) . ? C30 H30 0.9300 . ? C31 C32 1.379(5) . ? C31 H31 0.9300 . ? C32 C33 1.388(5) . ? C32 H32 0.9300 . ? C33 C34 1.513(5) . ? C34 N3 1.501(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 N3 1.495(4) . ? C35 C36 1.501(5) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 N4 1.343(4) . ? C36 C37 1.376(5) . ? C37 C38 1.383(5) . ? C37 H37 0.9300 . ? C38 C39 1.385(5) . ? C38 H38 0.9300 . ? C39 C40 1.376(5) . ? C39 H39 0.9300 . ? C40 N4 1.347(4) . ? C40 H40 0.9300 . ? O1 Cu2 1.924(2) . ? O1 Cu1 1.929(2) . ? O1 H1 0.91(3) . ? O2 Cu1 1.912(3) . ? O2 Cu2 1.918(3) . ? O2 H2 0.9100(11) . ? O3 Cl1 1.431(3) . ? O4 Cl1 1.409(3) . ? O5 Cl1 1.416(4) . ? O6 Cl1 1.452(3) . ? O7 Cl2 1.414(3) . ? O8 Cl2 1.421(3) . ? O9 Cl2 1.441(3) . ? O9 Cu2 2.425(3) . ? O10 Cl2 1.445(3) . ? Cu1 N2 1.976(3) . ? Cu1 N1 2.054(3) . ? Cu1 Cu2 2.8539(5) . ? Cu2 N4 1.966(3) . ? Cu2 N3 2.070(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 113.6(3) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C7 119.4(3) . . ? C3 C2 C1 120.6(3) . . ? C7 C2 C1 120.0(3) . . ? C4 C3 C2 121.1(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.2(4) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C7 120.8(4) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 118.8(3) . . ? C6 C7 C8 120.6(3) . . ? C2 C7 C8 120.6(3) . . ? C9 C8 C13 118.6(3) . . ? C9 C8 C7 121.2(3) . . ? C13 C8 C7 120.1(3) . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.5(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.5(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 120.9(4) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C8 120.0(3) . . ? C12 C13 C14 119.3(3) . . ? C8 C13 C14 120.2(3) . . ? N1 C14 C13 115.9(3) . . ? N1 C14 H14A 108.3 . . ? C13 C14 H14A 108.3 . . ? N1 C14 H14B 108.3 . . ? C13 C14 H14B 108.3 . . ? H14A C14 H14B 107.4 . . ? N1 C15 C16 111.1(3) . . ? N1 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? N1 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? N2 C16 C17 121.9(3) . . ? N2 C16 C15 114.4(3) . . ? C17 C16 C15 123.5(3) . . ? C18 C17 C16 118.2(3) . . ? C18 C17 H17 120.9 . . ? C16 C17 H17 120.9 . . ? C19 C18 C17 119.8(3) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 119.1(3) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? N2 C20 C19 121.6(3) . . ? N2 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? N3 C21 C22 113.4(3) . . ? N3 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? N3 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C27 119.3(3) . . ? C23 C22 C21 120.3(3) . . ? C27 C22 C21 120.2(3) . . ? C24 C23 C22 120.9(3) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 119.9(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C25 C26 C27 120.7(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 119.2(3) . . ? C26 C27 C28 121.6(3) . . ? C22 C27 C28 119.2(3) . . ? C29 C28 C33 119.2(3) . . ? C29 C28 C27 121.2(3) . . ? C33 C28 C27 119.5(3) . . ? C30 C29 C28 120.7(3) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 120.3(4) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 119.6(3) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 121.3(3) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C32 C33 C28 118.9(3) . . ? C32 C33 C34 121.6(3) . . ? C28 C33 C34 119.5(3) . . ? N3 C34 C33 113.1(3) . . ? N3 C34 H34A 109.0 . . ? C33 C34 H34A 109.0 . . ? N3 C34 H34B 109.0 . . ? C33 C34 H34B 109.0 . . ? H34A C34 H34B 107.8 . . ? N3 C35 C36 110.8(3) . . ? N3 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? N4 C36 C37 121.8(3) . . ? N4 C36 C35 114.2(3) . . ? C37 C36 C35 123.9(3) . . ? C36 C37 C38 119.0(3) . . ? C36 C37 H37 120.5 . . ? C38 C37 H37 120.5 . . ? C37 C38 C39 119.3(3) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C40 C39 C38 118.9(3) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? N4 C40 C39 121.6(3) . . ? N4 C40 H40 119.2 . . ? C39 C40 H40 119.2 . . ? Cu2 O1 Cu1 95.58(10) . . ? Cu2 O1 H1 117(3) . . ? Cu1 O1 H1 114.2(2) . . ? Cu1 O2 Cu2 96.36(13) . . ? Cu1 O2 H2 119.6(3) . . ? Cu2 O2 H2 117.1(3) . . ? Cl2 O9 Cu2 127.26(17) . . ? O4 Cl1 O5 109.8(3) . . ? O4 Cl1 O3 107.6(2) . . ? O5 Cl1 O3 109.5(2) . . ? O4 Cl1 O6 108.5(2) . . ? O5 Cl1 O6 109.8(2) . . ? O3 Cl1 O6 111.5(2) . . ? O7 Cl2 O8 108.7(2) . . ? O7 Cl2 O9 110.1(2) . . ? O8 Cl2 O9 108.1(2) . . ? O7 Cl2 O10 111.1(2) . . ? O8 Cl2 O10 108.1(2) . . ? O9 Cl2 O10 110.69(18) . . ? O2 Cu1 O1 83.43(11) . . ? O2 Cu1 N2 94.42(12) . . ? O1 Cu1 N2 173.06(11) . . ? O2 Cu1 N1 177.58(13) . . ? O1 Cu1 N1 97.93(10) . . ? N2 Cu1 N1 84.00(11) . . ? O2 Cu1 Cu2 41.90(8) . . ? O1 Cu1 Cu2 42.16(7) . . ? N2 Cu1 Cu2 136.29(8) . . ? N1 Cu1 Cu2 139.71(8) . . ? O2 Cu2 O1 83.39(11) . . ? O2 Cu2 N4 93.12(11) . . ? O1 Cu2 N4 172.55(11) . . ? O2 Cu2 N3 175.60(13) . . ? O1 Cu2 N3 99.92(10) . . ? N4 Cu2 N3 83.26(11) . . ? O2 Cu2 O9 94.68(15) . . ? O1 Cu2 O9 89.93(11) . . ? N4 Cu2 O9 96.92(12) . . ? N3 Cu2 O9 88.26(11) . . ? O2 Cu2 Cu1 41.75(8) . . ? O1 Cu2 Cu1 42.27(7) . . ? N4 Cu2 Cu1 134.83(8) . . ? N3 Cu2 Cu1 141.90(7) . . ? O9 Cu2 Cu1 87.45(7) . . ? C15 N1 C14 106.1(3) . . ? C15 N1 C1 110.3(2) . . ? C14 N1 C1 111.2(2) . . ? C15 N1 Cu1 105.73(19) . . ? C14 N1 Cu1 115.7(2) . . ? C1 N1 Cu1 107.55(19) . . ? C16 N2 C20 119.2(3) . . ? C16 N2 Cu1 114.5(2) . . ? C20 N2 Cu1 125.6(2) . . ? C35 N3 C21 108.3(3) . . ? C35 N3 C34 110.4(3) . . ? C21 N3 C34 111.0(2) . . ? C35 N3 Cu2 104.30(19) . . ? C21 N3 Cu2 108.9(2) . . ? C34 N3 Cu2 113.7(2) . . ? C36 N4 C40 119.4(3) . . ? C36 N4 Cu2 115.3(2) . . ? C40 N4 Cu2 125.2(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 N1 C1 C2 C3 106.3(4) . . . . ? N1 C1 C2 C7 -74.8(4) . . . . ? C7 C2 C3 C4 -0.4(6) . . . . ? C1 C2 C3 C4 178.5(4) . . . . ? C2 C3 C4 C5 0.1(7) . . . . ? C3 C4 C5 C6 -0.3(7) . . . . ? C4 C5 C6 C7 0.9(7) . . . . ? C5 C6 C7 C2 -1.2(6) . . . . ? C5 C6 C7 C8 179.2(4) . . . . ? C3 C2 C7 C6 1.0(6) . . . . ? C1 C2 C7 C6 -177.9(3) . . . . ? C3 C2 C7 C8 -179.4(3) . . . . ? C1 C2 C7 C8 1.7(5) . . . . ? C6 C7 C8 C9 40.9(6) . . . . ? C2 C7 C8 C9 -138.7(4) . . . . ? C6 C7 C8 C13 -138.0(4) . . . . ? C2 C7 C8 C13 42.4(5) . . . . ? C13 C8 C9 C10 0.6(6) . . . . ? C7 C8 C9 C10 -178.3(4) . . . . ? C8 C9 C10 C11 -1.7(7) . . . . ? C9 C10 C11 C12 1.5(7) . . . . ? C10 C11 C12 C13 -0.4(7) . . . . ? C11 C12 C13 C8 -0.7(6) . . . . ? C11 C12 C13 C14 171.1(4) . . . . ? C9 C8 C13 C12 0.5(6) . . . . ? C7 C8 C13 C12 179.5(3) . . . . ? C9 C8 C13 C14 -171.2(3) . . . . ? C7 C8 C13 C14 7.8(5) . . . . ? C12 C13 C14 N1 114.1(4) . . . . ? C8 C13 C14 N1 -74.1(4) . . . . ? N1 C15 C16 N2 -33.9(4) . . . . ? N1 C15 C16 C17 150.7(3) . . . . ? N2 C16 C17 C18 -3.6(5) . . . . ? C15 C16 C17 C18 171.5(3) . . . . ? C16 C17 C18 C19 1.6(5) . . . . ? C17 C18 C19 C20 1.2(5) . . . . ? C18 C19 C20 N2 -2.3(5) . . . . ? N3 C21 C22 C23 108.2(4) . . . . ? N3 C21 C22 C27 -76.0(4) . . . . ? C27 C22 C23 C24 -0.5(5) . . . . ? C21 C22 C23 C24 175.4(3) . . . . ? C22 C23 C24 C25 0.0(6) . . . . ? C23 C24 C25 C26 0.5(6) . . . . ? C24 C25 C26 C27 -0.4(6) . . . . ? C25 C26 C27 C22 -0.1(6) . . . . ? C25 C26 C27 C28 -179.8(3) . . . . ? C23 C22 C27 C26 0.5(5) . . . . ? C21 C22 C27 C26 -175.4(3) . . . . ? C23 C22 C27 C28 -179.8(3) . . . . ? C21 C22 C27 C28 4.3(5) . . . . ? C26 C27 C28 C29 46.4(5) . . . . ? C22 C27 C28 C29 -133.2(4) . . . . ? C26 C27 C28 C33 -135.2(4) . . . . ? C22 C27 C28 C33 45.2(5) . . . . ? C33 C28 C29 C30 -2.0(6) . . . . ? C27 C28 C29 C30 176.5(4) . . . . ? C28 C29 C30 C31 1.5(6) . . . . ? C29 C30 C31 C32 0.0(6) . . . . ? C30 C31 C32 C33 -1.1(6) . . . . ? C31 C32 C33 C28 0.7(5) . . . . ? C31 C32 C33 C34 180.0(3) . . . . ? C29 C28 C33 C32 0.9(5) . . . . ? C27 C28 C33 C32 -177.6(3) . . . . ? C29 C28 C33 C34 -178.5(3) . . . . ? C27 C28 C33 C34 3.1(5) . . . . ? C32 C33 C34 N3 104.2(4) . . . . ? C28 C33 C34 N3 -76.5(4) . . . . ? N3 C35 C36 N4 31.3(4) . . . . ? N3 C35 C36 C37 -152.2(3) . . . . ? N4 C36 C37 C38 1.1(5) . . . . ? C35 C36 C37 C38 -175.2(3) . . . . ? C36 C37 C38 C39 0.4(5) . . . . ? C37 C38 C39 C40 -1.3(5) . . . . ? C38 C39 C40 N4 0.6(5) . . . . ? Cu2 O9 Cl2 O7 144.2(3) . . . . ? Cu2 O9 Cl2 O8 -97.2(3) . . . . ? Cu2 O9 Cl2 O10 21.0(4) . . . . ? Cu2 O2 Cu1 O1 -8.50(15) . . . . ? Cu2 O2 Cu1 N2 178.12(15) . . . . ? Cu2 O2 Cu1 N1 -133(3) . . . . ? Cu2 O1 Cu1 O2 8.46(15) . . . . ? Cu2 O1 Cu1 N2 80.7(9) . . . . ? Cu2 O1 Cu1 N1 -173.55(10) . . . . ? Cu1 O2 Cu2 O1 8.52(15) . . . . ? Cu1 O2 Cu2 N4 -178.08(16) . . . . ? Cu1 O2 Cu2 N3 147.3(16) . . . . ? Cu1 O2 Cu2 O9 -80.86(17) . . . . ? Cu1 O1 Cu2 O2 -8.43(15) . . . . ? Cu1 O1 Cu2 N4 -70.7(8) . . . . ? Cu1 O1 Cu2 N3 174.51(10) . . . . ? Cu1 O1 Cu2 O9 86.29(11) . . . . ? Cl2 O9 Cu2 O2 25.0(3) . . . . ? Cl2 O9 Cu2 O1 -58.3(3) . . . . ? Cl2 O9 Cu2 N4 118.7(3) . . . . ? Cl2 O9 Cu2 N3 -158.3(3) . . . . ? Cl2 O9 Cu2 Cu1 -16.1(3) . . . . ? O1 Cu1 Cu2 O2 167.4(2) . . . . ? N2 Cu1 Cu2 O2 -2.7(2) . . . . ? N1 Cu1 Cu2 O2 177.3(2) . . . . ? O2 Cu1 Cu2 O1 -167.4(2) . . . . ? N2 Cu1 Cu2 O1 -170.07(16) . . . . ? N1 Cu1 Cu2 O1 9.90(16) . . . . ? O2 Cu1 Cu2 N4 2.7(2) . . . . ? O1 Cu1 Cu2 N4 170.06(16) . . . . ? N2 Cu1 Cu2 N4 0.00(16) . . . . ? N1 Cu1 Cu2 N4 179.97(16) . . . . ? O2 Cu1 Cu2 N3 -176.1(2) . . . . ? O1 Cu1 Cu2 N3 -8.79(17) . . . . ? N2 Cu1 Cu2 N3 -178.86(17) . . . . ? N1 Cu1 Cu2 N3 1.11(18) . . . . ? O2 Cu1 Cu2 O9 99.9(2) . . . . ? O1 Cu1 Cu2 O9 -92.70(14) . . . . ? N2 Cu1 Cu2 O9 97.23(14) . . . . ? N1 Cu1 Cu2 O9 -82.80(15) . . . . ? C16 C15 N1 C14 156.2(3) . . . . ? C16 C15 N1 C1 -83.1(3) . . . . ? C16 C15 N1 Cu1 32.9(3) . . . . ? C13 C14 N1 C15 157.2(3) . . . . ? C13 C14 N1 C1 37.2(4) . . . . ? C13 C14 N1 Cu1 -85.9(3) . . . . ? C2 C1 N1 C15 -68.6(3) . . . . ? C2 C1 N1 C14 48.9(4) . . . . ? C2 C1 N1 Cu1 176.5(2) . . . . ? O2 Cu1 N1 C15 -69(3) . . . . ? O1 Cu1 N1 C15 167.0(2) . . . . ? N2 Cu1 N1 C15 -19.7(2) . . . . ? Cu2 Cu1 N1 C15 160.34(15) . . . . ? O2 Cu1 N1 C14 174(3) . . . . ? O1 Cu1 N1 C14 49.9(2) . . . . ? N2 Cu1 N1 C14 -136.8(2) . . . . ? Cu2 Cu1 N1 C14 43.2(3) . . . . ? O2 Cu1 N1 C1 49(3) . . . . ? O1 Cu1 N1 C1 -75.1(2) . . . . ? N2 Cu1 N1 C1 98.2(2) . . . . ? Cu2 Cu1 N1 C1 -81.8(2) . . . . ? C17 C16 N2 C20 2.6(5) . . . . ? C15 C16 N2 C20 -172.9(3) . . . . ? C17 C16 N2 Cu1 -168.1(2) . . . . ? C15 C16 N2 Cu1 16.4(3) . . . . ? C19 C20 N2 C16 0.4(5) . . . . ? C19 C20 N2 Cu1 170.0(2) . . . . ? O2 Cu1 N2 C16 -179.4(2) . . . . ? O1 Cu1 N2 C16 109.0(8) . . . . ? N1 Cu1 N2 C16 2.5(2) . . . . ? Cu2 Cu1 N2 C16 -177.54(17) . . . . ? O2 Cu1 N2 C20 10.7(3) . . . . ? O1 Cu1 N2 C20 -61.0(9) . . . . ? N1 Cu1 N2 C20 -167.5(3) . . . . ? Cu2 Cu1 N2 C20 12.5(3) . . . . ? C36 C35 N3 C21 79.1(3) . . . . ? C36 C35 N3 C34 -159.2(3) . . . . ? C36 C35 N3 Cu2 -36.7(3) . . . . ? C22 C21 N3 C35 163.5(3) . . . . ? C22 C21 N3 C34 42.2(4) . . . . ? C22 C21 N3 Cu2 -83.7(3) . . . . ? C33 C34 N3 C35 -74.8(3) . . . . ? C33 C34 N3 C21 45.3(4) . . . . ? C33 C34 N3 Cu2 168.4(2) . . . . ? O2 Cu2 N3 C35 60.9(18) . . . . ? O1 Cu2 N3 C35 -160.7(2) . . . . ? N4 Cu2 N3 C35 26.1(2) . . . . ? O9 Cu2 N3 C35 -71.1(2) . . . . ? Cu1 Cu2 N3 C35 -154.75(17) . . . . ? O2 Cu2 N3 C21 -54.6(18) . . . . ? O1 Cu2 N3 C21 83.8(2) . . . . ? N4 Cu2 N3 C21 -89.4(2) . . . . ? O9 Cu2 N3 C21 173.5(2) . . . . ? Cu1 Cu2 N3 C21 89.8(2) . . . . ? O2 Cu2 N3 C34 -179(100) . . . . ? O1 Cu2 N3 C34 -40.5(2) . . . . ? N4 Cu2 N3 C34 146.3(2) . . . . ? O9 Cu2 N3 C34 49.1(2) . . . . ? Cu1 Cu2 N3 C34 -34.5(3) . . . . ? C37 C36 N4 C40 -1.8(5) . . . . ? C35 C36 N4 C40 174.8(3) . . . . ? C37 C36 N4 Cu2 175.4(3) . . . . ? C35 C36 N4 Cu2 -8.0(4) . . . . ? C39 C40 N4 C36 0.9(5) . . . . ? C39 C40 N4 Cu2 -175.9(2) . . . . ? O2 Cu2 N4 C36 171.5(3) . . . . ? O1 Cu2 N4 C36 -126.8(8) . . . . ? N3 Cu2 N4 C36 -11.0(2) . . . . ? O9 Cu2 N4 C36 76.4(2) . . . . ? Cu1 Cu2 N4 C36 169.68(18) . . . . ? O2 Cu2 N4 C40 -11.5(3) . . . . ? O1 Cu2 N4 C40 50.2(9) . . . . ? N3 Cu2 N4 C40 165.9(3) . . . . ? O9 Cu2 N4 C40 -106.6(3) . . . . ? Cu1 Cu2 N4 C40 -13.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.750 _refine_diff_density_min -0.666 _refine_diff_density_rms 0.096 _vrf_PLAT222_ssoh ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE: There is some amount of disorder for hydrogen H2 which could not be accounted. This led to bad thermal parameter for this hydrogen. ; # end Validation Reply Form