# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xian-He Bu' _publ_contact_author_email buxh@nankai.edu.cn _publ_author_name 'Xian-He Bu' data_1 _database_code_depnum_ccdc_archive 'CCDC 790269' #TrackingRef '- Crystal Data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum C94.4H58.4Cl31.2Cu6I6N24 _chemical_formula_weight 3777.66 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 20.799(4) _cell_length_b 20.799(4) _cell_length_c 47.180(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 17676(5) _cell_formula_units_Z 6 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 22143 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.9 _exptl_crystal_description Prism _exptl_crystal_colour dark-blue _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10008 _exptl_absorpt_coefficient_mu 3.325 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41085 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6944 _reflns_number_gt 6159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+548.5780P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6944 _refine_ls_number_parameters 361 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1525 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.003 _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 I1 I 0.60530(3) 0.75138(3) 1.013045(11) 0.03885(17) Uani 1 1 d . . . I4 I 0.57718(3) 0.92713(3) 0.843518(11) 0.03887(17) Uani 1 1 d . . . Cu1 Cu 0.51395(5) 0.89138(5) 0.892685(19) 0.0276(2) Uani 1 1 d . . . Cu2 Cu 0.55334(4) 0.70234(5) 0.962969(18) 0.0245(2) Uani 1 1 d . . . N1 N 0.5924(3) 0.9220(3) 0.92369(13) 0.0251(13) Uani 1 1 d . . . N2 N 0.4814(3) 0.7735(3) 0.95935(11) 0.0180(11) Uani 1 1 d . . . N3 N 0.4415(3) 0.6259(3) 0.96236(11) 0.0189(11) Uani 1 1 d . . . N4 N 0.5500(3) 0.5970(3) 0.96077(12) 0.0208(12) Uani 1 1 d . . . N5 N 0.6261(3) 0.7627(3) 0.93137(12) 0.0222(12) Uani 1 1 d . . . N6 N 0.4871(3) 0.7542(3) 0.89558(12) 0.0227(12) Uani 1 1 d . . . N7 N 0.4207(3) 0.5991(3) 0.89237(11) 0.0205(11) Uani 1 1 d . . . N8 N 0.4960(3) 0.5292(3) 0.89689(12) 0.0233(12) Uani 1 1 d . . . C1 C 0.6646(4) 0.9694(4) 0.91701(17) 0.0323(17) Uani 1 1 d . . . H1 H 0.6756 0.9888 0.8988 0.039 Uiso 1 1 calc R . . C2 C 0.7217(4) 0.9901(4) 0.93562(19) 0.0380(19) Uani 1 1 d . . . H2 H 0.7701 1.0235 0.9301 0.046 Uiso 1 1 calc R . . C3 C 0.7076(4) 0.9616(4) 0.96226(17) 0.0340(17) Uani 1 1 d . . . H3 H 0.7462 0.9748 0.9751 0.041 Uiso 1 1 calc R . . C4 C 0.6352(4) 0.9128(4) 0.97013(17) 0.0313(16) Uani 1 1 d . . . H4 H 0.6240 0.8917 0.9881 0.038 Uiso 1 1 calc R . . C5 C 0.5794(3) 0.8961(4) 0.95015(15) 0.0220(14) Uani 1 1 d . . . C6 C 0.4998(4) 0.8442(4) 0.95739(13) 0.0201(13) Uani 1 1 d . . . C7 C 0.4099(3) 0.7228(4) 0.96262(13) 0.0183(13) Uani 1 1 d . . . C8 C 0.3881(4) 0.6446(4) 0.96277(13) 0.0178(13) Uani 1 1 d . . . C9 C 0.4208(4) 0.5539(4) 0.96069(14) 0.0207(13) Uani 1 1 d . . . C10 C 0.4824(4) 0.5356(4) 0.96235(14) 0.0197(13) Uani 1 1 d . . . C11 C 0.4733(4) 0.4660(4) 0.96656(14) 0.0216(14) Uani 1 1 d . . . H11 H 0.4260 0.4247 0.9680 0.026 Uiso 1 1 calc R . . C12 C 0.5353(4) 0.4585(4) 0.96859(15) 0.0269(15) Uani 1 1 d . . . H12 H 0.5302 0.4120 0.9715 0.032 Uiso 1 1 calc R . . C13 C 0.6051(4) 0.5204(4) 0.96626(15) 0.0275(15) Uani 1 1 d . . . H13 H 0.6476 0.5163 0.9671 0.033 Uiso 1 1 calc R . . C14 C 0.6099(4) 0.5883(4) 0.96265(15) 0.0282(15) Uani 1 1 d . . . H14 H 0.6568 0.6303 0.9614 0.034 Uiso 1 1 calc R . . C15 C 0.6993(4) 0.8007(4) 0.93744(18) 0.0327(17) Uani 1 1 d . . . H15 H 0.7139 0.7980 0.9558 0.039 Uiso 1 1 calc R . . C16 C 0.7538(4) 0.8431(5) 0.91816(18) 0.0383(19) Uani 1 1 d . . . H16 H 0.8037 0.8662 0.9231 0.046 Uiso 1 1 calc R . . C17 C 0.7324(4) 0.8506(4) 0.89107(19) 0.0382(19) Uani 1 1 d . . . H17 H 0.7679 0.8798 0.8777 0.046 Uiso 1 1 calc R . . C18 C 0.6578(4) 0.8143(4) 0.88425(17) 0.0336(18) Uani 1 1 d . . . H18 H 0.6421 0.8201 0.8664 0.040 Uiso 1 1 calc R . . C19 C 0.6070(4) 0.7693(4) 0.90439(16) 0.0233(14) Uani 1 1 d . . . C20 C 0.5261(3) 0.7201(3) 0.89734(13) 0.0168(12) Uani 1 1 d . . . C21 C 0.4122(4) 0.7110(4) 0.89274(13) 0.0194(13) Uani 1 1 d . . . C22 C 0.3789(4) 0.6326(4) 0.89249(14) 0.0221(14) Uani 1 1 d . . . C23 C 0.4944(4) 0.6425(4) 0.89366(13) 0.0222(14) Uani 1 1 d . . . C24 C 0.5370(4) 0.6025(4) 0.89213(13) 0.0210(13) Uani 1 1 d U . . C25 C 0.6116(4) 0.6356(4) 0.88463(15) 0.0277(15) Uani 1 1 d . . . H25 H 0.6385 0.6858 0.8800 0.033 Uiso 1 1 calc R . . C26 C 0.6454(4) 0.5918(4) 0.88416(16) 0.0312(17) Uani 1 1 d . . . H26 H 0.6953 0.6126 0.8795 0.037 Uiso 1 1 calc R . . C27 C 0.6040(4) 0.5181(4) 0.89070(17) 0.0339(17) Uani 1 1 d . . . H27 H 0.6259 0.4886 0.8915 0.041 Uiso 1 1 calc R . . C28 C 0.5290(4) 0.4879(4) 0.89615(16) 0.0298(16) Uani 1 1 d . . . H28 H 0.5004 0.4372 0.8994 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.0482(3) 0.0313(3) 0.0375(3) -0.0024(2) -0.0161(2) 0.0203(2) I4 0.0342(3) 0.0508(3) 0.0352(3) 0.0174(2) 0.0153(2) 0.0239(3) Cu1 0.0192(4) 0.0297(5) 0.0307(5) 0.0069(4) 0.0052(3) 0.0099(4) Cu2 0.0162(4) 0.0214(4) 0.0315(5) 0.0015(3) -0.0025(3) 0.0062(3) N1 0.018(3) 0.020(3) 0.037(3) 0.001(2) 0.005(2) 0.010(2) N2 0.015(3) 0.013(3) 0.024(3) -0.002(2) -0.002(2) 0.005(2) N3 0.022(3) 0.017(3) 0.022(3) -0.002(2) -0.001(2) 0.012(2) N4 0.016(3) 0.018(3) 0.029(3) 0.001(2) 0.003(2) 0.009(2) N5 0.014(3) 0.015(3) 0.033(3) -0.006(2) -0.002(2) 0.003(2) N6 0.018(3) 0.025(3) 0.024(3) -0.002(2) 0.003(2) 0.010(2) N7 0.023(3) 0.021(3) 0.017(3) 0.003(2) 0.003(2) 0.010(2) N8 0.025(3) 0.012(3) 0.033(3) -0.001(2) 0.005(2) 0.010(2) C1 0.024(4) 0.018(3) 0.042(4) -0.002(3) 0.015(3) 0.001(3) C2 0.003(3) 0.037(4) 0.060(5) -0.009(4) -0.002(3) 0.000(3) C3 0.025(4) 0.025(4) 0.043(5) -0.011(3) -0.006(3) 0.005(3) C4 0.025(4) 0.023(4) 0.042(4) -0.006(3) -0.004(3) 0.010(3) C5 0.012(3) 0.017(3) 0.033(4) -0.007(3) -0.004(3) 0.004(3) C6 0.020(3) 0.016(3) 0.020(3) -0.002(2) -0.003(3) 0.006(3) C7 0.018(3) 0.021(3) 0.019(3) -0.005(3) -0.005(2) 0.012(3) C8 0.023(3) 0.018(3) 0.014(3) -0.001(2) -0.002(2) 0.012(3) C9 0.024(3) 0.022(3) 0.022(3) 0.002(3) 0.000(3) 0.016(3) C10 0.022(3) 0.018(3) 0.023(3) -0.001(3) 0.004(3) 0.013(3) C11 0.022(3) 0.021(3) 0.025(3) -0.001(3) 0.003(3) 0.013(3) C12 0.035(4) 0.023(4) 0.028(4) 0.002(3) 0.002(3) 0.019(3) C13 0.027(4) 0.035(4) 0.033(4) 0.003(3) 0.001(3) 0.024(3) C14 0.019(3) 0.031(4) 0.031(4) -0.003(3) -0.003(3) 0.010(3) C15 0.021(4) 0.028(4) 0.048(5) -0.006(3) -0.005(3) 0.012(3) C16 0.015(4) 0.042(5) 0.054(5) 0.003(4) 0.014(3) 0.012(3) C17 0.024(4) 0.030(4) 0.053(5) 0.012(4) 0.017(4) 0.007(3) C18 0.024(4) 0.028(4) 0.039(4) 0.011(3) 0.018(3) 0.005(3) C19 0.020(3) 0.013(3) 0.042(4) -0.004(3) 0.000(3) 0.012(3) C20 0.011(3) 0.019(3) 0.019(3) 0.002(2) 0.002(2) 0.006(3) C21 0.023(3) 0.017(3) 0.017(3) 0.001(2) 0.002(3) 0.009(3) C22 0.026(4) 0.019(3) 0.018(3) 0.003(3) 0.004(3) 0.009(3) C23 0.022(3) 0.027(4) 0.018(3) 0.001(3) 0.002(3) 0.013(3) C24 0.025(3) 0.023(3) 0.018(3) -0.003(2) 0.003(3) 0.015(3) C25 0.029(4) 0.024(4) 0.033(4) -0.003(3) 0.005(3) 0.016(3) C26 0.024(4) 0.035(4) 0.041(4) 0.005(3) 0.015(3) 0.020(3) C27 0.040(4) 0.033(4) 0.041(4) -0.005(3) 0.001(4) 0.027(4) C28 0.033(4) 0.022(4) 0.036(4) -0.008(3) -0.010(3) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Cu2 2.5861(10) . ? I4 Cu1 2.5856(10) . ? Cu1 N1 2.042(6) . ? Cu1 N7 2.055(6) 2_665 ? Cu1 N8 2.170(6) 2_665 ? Cu2 N5 2.046(6) . ? Cu2 N3 2.059(6) . ? Cu2 N4 2.160(6) . ? N1 C5 1.332(9) . ? N1 C1 1.359(9) . ? N2 C6 1.325(8) . ? N2 C7 1.335(8) . ? N3 C9 1.337(8) . ? N3 C8 1.349(8) . ? N4 C14 1.348(9) . ? N4 C10 1.349(9) . ? N5 C15 1.351(9) . ? N5 C19 1.360(9) . ? N6 C20 1.318(8) . ? N6 C21 1.362(9) . ? N7 C23 1.336(9) . ? N7 C22 1.360(9) . ? N7 Cu1 2.055(6) 3_565 ? N8 C28 1.341(9) . ? N8 C24 1.343(9) . ? N8 Cu1 2.170(6) 3_565 ? C1 C2 1.363(11) . ? C1 H1 0.9300 . ? C2 C3 1.358(12) . ? C2 H2 0.9300 . ? C3 C4 1.380(11) . ? C3 H3 0.9300 . ? C4 C5 1.398(10) . ? C4 H4 0.9300 . ? C5 C6 1.495(9) . ? C6 C9 1.422(9) 2_665 ? C7 C8 1.400(9) 2_665 ? C7 C8 1.453(9) . ? C8 C7 1.400(9) 3_565 ? C9 C6 1.422(10) 3_565 ? C9 C10 1.509(9) . ? C10 C11 1.377(9) . ? C11 C12 1.378(10) . ? C11 H11 0.9300 . ? C12 C13 1.382(11) . ? C12 H12 0.9300 . ? C13 C14 1.375(10) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.375(11) . ? C15 H15 0.9300 . ? C16 C17 1.387(12) . ? C16 H16 0.9300 . ? C17 C18 1.382(11) . ? C17 H17 0.9300 . ? C18 C19 1.382(10) . ? C18 H18 0.9300 . ? C19 C20 1.506(9) . ? C20 C23 1.418(9) . ? C21 C22 1.416(9) . ? C21 C22 1.446(9) 2_665 ? C22 C21 1.446(9) 3_565 ? C23 C24 1.491(9) . ? C24 C25 1.392(10) . ? C25 C26 1.402(10) . ? C25 H25 0.9300 . ? C26 C27 1.367(11) . ? C26 H26 0.9300 . ? C27 C28 1.384(11) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N7 132.8(2) . 2_665 ? N1 Cu1 N8 105.3(2) . 2_665 ? N7 Cu1 N8 76.8(2) 2_665 2_665 ? N1 Cu1 I4 109.94(17) . . ? N7 Cu1 I4 115.75(15) 2_665 . ? N8 Cu1 I4 102.05(15) 2_665 . ? N5 Cu2 N3 131.8(2) . . ? N5 Cu2 N4 103.1(2) . . ? N3 Cu2 N4 76.4(2) . . ? N5 Cu2 I1 112.87(16) . . ? N3 Cu2 I1 113.91(15) . . ? N4 Cu2 I1 103.83(15) . . ? C5 N1 C1 115.9(6) . . ? C5 N1 Cu1 125.2(4) . . ? C1 N1 Cu1 118.7(5) . . ? C6 N2 C7 118.3(6) . . ? C9 N3 C8 118.3(6) . . ? C9 N3 Cu2 118.2(4) . . ? C8 N3 Cu2 123.5(4) . . ? C14 N4 C10 117.8(6) . . ? C14 N4 Cu2 124.7(5) . . ? C10 N4 Cu2 116.5(4) . . ? C15 N5 C19 116.1(6) . . ? C15 N5 Cu2 118.4(5) . . ? C19 N5 Cu2 125.4(4) . . ? C20 N6 C21 117.4(6) . . ? C23 N7 C22 117.7(6) . . ? C23 N7 Cu1 118.1(5) . 3_565 ? C22 N7 Cu1 124.1(5) . 3_565 ? C28 N8 C24 118.9(6) . . ? C28 N8 Cu1 125.0(5) . 3_565 ? C24 N8 Cu1 113.6(4) . 3_565 ? N1 C1 C2 123.5(7) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 119.6(7) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.3(7) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 117.8(7) . . ? C3 C4 H4 121.1 . . ? C5 C4 H4 121.1 . . ? N1 C5 C4 123.8(6) . . ? N1 C5 C6 115.7(6) . . ? C4 C5 C6 120.5(6) . . ? N2 C6 C9 121.5(6) . 2_665 ? N2 C6 C5 114.7(6) . . ? C9 C6 C5 123.8(6) 2_665 . ? N2 C7 C8 120.8(6) . 2_665 ? N2 C7 C8 119.0(6) . . ? C8 C7 C8 119.8(6) 2_665 . ? N3 C8 C7 120.9(6) . 3_565 ? N3 C8 C7 118.9(6) . . ? C7 C8 C7 120.2(6) 3_565 . ? N3 C9 C6 119.6(6) . 3_565 ? N3 C9 C10 116.2(6) . . ? C6 C9 C10 124.2(6) 3_565 . ? N4 C10 C11 122.2(6) . . ? N4 C10 C9 111.9(5) . . ? C11 C10 C9 125.8(6) . . ? C10 C11 C12 119.0(6) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C11 C12 C13 119.8(6) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 118.0(6) . . ? C14 C13 H13 121.0 . . ? C12 C13 H13 121.0 . . ? N4 C14 C13 123.3(7) . . ? N4 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? N5 C15 C16 124.2(8) . . ? N5 C15 H15 117.9 . . ? C16 C15 H15 117.9 . . ? C15 C16 C17 118.3(7) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C18 C17 C16 119.3(7) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C19 C18 C17 118.7(8) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? N5 C19 C18 123.3(7) . . ? N5 C19 C20 115.0(6) . . ? C18 C19 C20 121.7(7) . . ? N6 C20 C23 122.9(6) . . ? N6 C20 C19 115.3(6) . . ? C23 C20 C19 121.7(6) . . ? N6 C21 C22 120.0(6) . . ? N6 C21 C22 118.8(6) . 2_665 ? C22 C21 C22 121.0(7) . 2_665 ? N7 C22 C21 121.3(6) . . ? N7 C22 C21 119.7(6) . 3_565 ? C21 C22 C21 119.0(7) . 3_565 ? N7 C23 C20 119.9(6) . . ? N7 C23 C24 115.0(6) . . ? C20 C23 C24 125.0(6) . . ? N8 C24 C25 121.6(6) . . ? N8 C24 C23 114.0(6) . . ? C25 C24 C23 124.3(6) . . ? C24 C25 C26 118.6(7) . . ? C24 C25 H25 120.7 . . ? C26 C25 H25 120.7 . . ? C27 C26 C25 119.1(7) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 119.0(7) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? N8 C28 C27 122.5(7) . . ? N8 C28 H28 118.7 . . ? C27 C28 H28 118.7 . . ? 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 N7 Cu1 N1 C5 2.6(7) 2_665 . . . ? N8 Cu1 N1 C5 88.6(6) 2_665 . . . ? I4 Cu1 N1 C5 -162.2(5) . . . . ? N7 Cu1 N1 C1 178.9(5) 2_665 . . . ? N8 Cu1 N1 C1 -95.1(5) 2_665 . . . ? I4 Cu1 N1 C1 14.1(6) . . . . ? N5 Cu2 N3 C9 94.8(5) . . . . ? N4 Cu2 N3 C9 -0.8(5) . . . . ? I1 Cu2 N3 C9 -100.1(5) . . . . ? N5 Cu2 N3 C8 -83.3(6) . . . . ? N4 Cu2 N3 C8 -178.9(5) . . . . ? I1 Cu2 N3 C8 81.8(5) . . . . ? N5 Cu2 N4 C14 56.0(6) . . . . ? N3 Cu2 N4 C14 -173.6(6) . . . . ? I1 Cu2 N4 C14 -61.9(6) . . . . ? N5 Cu2 N4 C10 -135.5(5) . . . . ? N3 Cu2 N4 C10 -5.1(5) . . . . ? I1 Cu2 N4 C10 106.6(5) . . . . ? N3 Cu2 N5 C15 -170.0(5) . . . . ? N4 Cu2 N5 C15 -86.7(5) . . . . ? I1 Cu2 N5 C15 24.7(5) . . . . ? N3 Cu2 N5 C19 11.1(6) . . . . ? N4 Cu2 N5 C19 94.5(5) . . . . ? I1 Cu2 N5 C19 -154.1(5) . . . . ? C5 N1 C1 C2 0.5(11) . . . . ? Cu1 N1 C1 C2 -176.2(6) . . . . ? N1 C1 C2 C3 1.2(13) . . . . ? C1 C2 C3 C4 -0.8(12) . . . . ? C2 C3 C4 C5 -1.2(11) . . . . ? C1 N1 C5 C4 -2.7(10) . . . . ? Cu1 N1 C5 C4 173.7(5) . . . . ? C1 N1 C5 C6 179.7(6) . . . . ? Cu1 N1 C5 C6 -3.9(8) . . . . ? C3 C4 C5 N1 3.1(11) . . . . ? C3 C4 C5 C6 -179.4(6) . . . . ? C7 N2 C6 C9 4.5(9) . . . 2_665 ? C7 N2 C6 C5 -172.7(6) . . . . ? N1 C5 C6 N2 105.6(7) . . . . ? C4 C5 C6 N2 -72.1(8) . . . . ? N1 C5 C6 C9 -71.5(8) . . . 2_665 ? C4 C5 C6 C9 110.8(8) . . . 2_665 ? C6 N2 C7 C8 2.7(9) . . . 2_665 ? C6 N2 C7 C8 175.6(6) . . . . ? C9 N3 C8 C7 2.6(9) . . . 3_565 ? Cu2 N3 C8 C7 -179.3(4) . . . 3_565 ? C9 N3 C8 C7 -175.8(6) . . . . ? Cu2 N3 C8 C7 2.3(8) . . . . ? N2 C7 C8 N3 6.4(9) . . . . ? C8 C7 C8 N3 179.4(4) 2_665 . . . ? N2 C7 C8 C7 -172.1(4) . . . 3_565 ? C8 C7 C8 C7 1.0(12) 2_665 . . 3_565 ? C8 N3 C9 C6 4.4(9) . . . 3_565 ? Cu2 N3 C9 C6 -173.8(5) . . . 3_565 ? C8 N3 C9 C10 -175.9(6) . . . . ? Cu2 N3 C9 C10 5.9(7) . . . . ? C14 N4 C10 C11 1.8(10) . . . . ? Cu2 N4 C10 C11 -167.5(5) . . . . ? C14 N4 C10 C9 178.5(6) . . . . ? Cu2 N4 C10 C9 9.2(7) . . . . ? N3 C9 C10 N4 -9.9(8) . . . . ? C6 C9 C10 N4 169.8(6) 3_565 . . . ? N3 C9 C10 C11 166.7(6) . . . . ? C6 C9 C10 C11 -13.7(11) 3_565 . . . ? N4 C10 C11 C12 -1.5(10) . . . . ? C9 C10 C11 C12 -177.7(6) . . . . ? C10 C11 C12 C13 -0.3(10) . . . . ? C11 C12 C13 C14 1.6(10) . . . . ? C10 N4 C14 C13 -0.4(10) . . . . ? Cu2 N4 C14 C13 168.0(5) . . . . ? C12 C13 C14 N4 -1.3(11) . . . . ? C19 N5 C15 C16 -1.2(11) . . . . ? Cu2 N5 C15 C16 179.8(6) . . . . ? N5 C15 C16 C17 3.3(12) . . . . ? C15 C16 C17 C18 -1.3(12) . . . . ? C16 C17 C18 C19 -2.5(12) . . . . ? C15 N5 C19 C18 -2.9(10) . . . . ? Cu2 N5 C19 C18 175.9(5) . . . . ? C15 N5 C19 C20 173.8(6) . . . . ? Cu2 N5 C19 C20 -7.3(8) . . . . ? C17 C18 C19 N5 4.8(11) . . . . ? C17 C18 C19 C20 -171.7(7) . . . . ? C21 N6 C20 C23 6.3(9) . . . . ? C21 N6 C20 C19 -172.1(6) . . . . ? N5 C19 C20 N6 105.6(7) . . . . ? C18 C19 C20 N6 -77.6(8) . . . . ? N5 C19 C20 C23 -72.8(8) . . . . ? C18 C19 C20 C23 104.0(8) . . . . ? C20 N6 C21 C22 1.6(9) . . . . ? C20 N6 C21 C22 176.2(6) . . . 2_665 ? C23 N7 C22 C21 2.7(9) . . . . ? Cu1 N7 C22 C21 178.9(5) 3_565 . . . ? C23 N7 C22 C21 -176.5(6) . . . 3_565 ? Cu1 N7 C22 C21 -0.3(8) 3_565 . . 3_565 ? N6 C21 C22 N7 -6.2(9) . . . . ? C22 C21 C22 N7 179.2(4) 2_665 . . . ? N6 C21 C22 C21 173.0(4) . . . 3_565 ? C22 C21 C22 C21 -1.6(12) 2_665 . . 3_565 ? C22 N7 C23 C20 5.0(9) . . . . ? Cu1 N7 C23 C20 -171.5(5) 3_565 . . . ? C22 N7 C23 C24 -177.3(5) . . . . ? Cu1 N7 C23 C24 6.2(7) 3_565 . . . ? N6 C20 C23 N7 -10.0(10) . . . . ? C19 C20 C23 N7 168.3(6) . . . . ? N6 C20 C23 C24 172.6(6) . . . . ? C19 C20 C23 C24 -9.2(10) . . . . ? C28 N8 C24 C25 4.3(10) . . . . ? Cu1 N8 C24 C25 -158.5(5) 3_565 . . . ? C28 N8 C24 C23 -179.7(6) . . . . ? Cu1 N8 C24 C23 17.6(7) 3_565 . . . ? N7 C23 C24 N8 -16.0(8) . . . . ? C20 C23 C24 N8 161.5(6) . . . . ? N7 C23 C24 C25 159.9(6) . . . . ? C20 C23 C24 C25 -22.6(10) . . . . ? N8 C24 C25 C26 -4.8(11) . . . . ? C23 C24 C25 C26 179.6(7) . . . . ? C24 C25 C26 C27 0.8(11) . . . . ? C25 C26 C27 C28 3.4(12) . . . . ? C24 N8 C28 C27 0.1(11) . . . . ? Cu1 N8 C28 C27 160.8(6) 3_565 . . . ? C26 C27 C28 N8 -4.0(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 5.562 _refine_diff_density_min -2.773 _refine_diff_density_rms 0.158 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.114 -0.034 0.001 7445 3635 ' ' _platon_squeeze_details ;In order to subtract the contribution from the disordered solvent molecules, the SQUEEZE command was applied, which gave a new HKL file. The number of located electrons is 3635, is included in the formula, formula weight, calculated density, and F(000). These residual electron density were assigned to 10.4 chloroform molecules. So SQUEEZE 10.4 chloroform molecules per formula unit. This value calculated based upon electrons analysis. (One chloroform molecules would give 58 e). So the tentative formula for this compound is presented as in the text. See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake, L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun., 2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare.Chem. Commun. 2008, 5987; (c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang, and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650. ; data_2 _database_code_depnum_ccdc_archive 'CCDC 817852' #TrackingRef '- Crystal Data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum C266.5H195Cl29Cu12N96O84 _chemical_formula_weight 7876.86 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' '-x, -x+y, -z+1/2' 'x-y, -y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' 'x, x-y, z-1/2' '-x+y, y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' _cell_length_a 25.626(7) _cell_length_b 25.626(7) _cell_length_c 85.61(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 48687(25) _cell_formula_units_Z 6 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 45241 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.1 _exptl_crystal_description Prism _exptl_crystal_colour dark-brow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 23322 _exptl_absorpt_coefficient_mu 1.070 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(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 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 120649 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -101 _diffrn_reflns_limit_l_max 101 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9550 _reflns_number_gt 8689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+602.7534P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9550 _refine_ls_number_parameters 737 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.1737 _refine_ls_wR_factor_gt 0.1696 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.074 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.9957(3) 0.2774(2) 0.06737(7) 0.0369(13) Uani 1 1 d . . . H1 H 0.9797 0.2928 0.0746 0.044 Uiso 1 1 calc R . . C2 C 1.0390(3) 0.3162(2) 0.05710(7) 0.0420(14) Uani 1 1 d . . . H2 H 1.0524 0.3573 0.0574 0.050 Uiso 1 1 calc R . . C3 C 1.0622(3) 0.2936(3) 0.04646(8) 0.0483(16) Uani 1 1 d . . . H3 H 1.0907 0.3191 0.0393 0.058 Uiso 1 1 calc R . . C4 C 1.0432(3) 0.2328(2) 0.04637(8) 0.0437(15) Uani 1 1 d . . . H4 H 1.0596 0.2172 0.0393 0.052 Uiso 1 1 calc R . . C5 C 0.9993(2) 0.1952(2) 0.05692(6) 0.0286(11) Uani 1 1 d . . . C6 C 0.9792(2) 0.1293(2) 0.05745(6) 0.0246(10) Uani 1 1 d . . . C7 C 0.9190(2) 0.0815(2) 0.05719(5) 0.0245(10) Uani 1 1 d . . . C8 C 0.9522(2) 0.0137(2) 0.05685(6) 0.0247(10) Uani 1 1 d . . . C9 C 1.0120(2) 0.0607(2) 0.05697(6) 0.0278(11) Uani 1 1 d . . . C10 C 0.8051(2) 0.1271(3) 0.06478(7) 0.0363(12) Uani 1 1 d . . . H10A H 0.7991 0.1514 0.0718 0.044 Uiso 1 1 calc R . . C11 C 0.7618(2) 0.0957(3) 0.05375(7) 0.0402(13) Uani 1 1 d . . . H11A H 0.7275 0.0993 0.0532 0.048 Uiso 1 1 calc R . . C12 C 0.8212(2) 0.0547(2) 0.04455(6) 0.0312(11) Uani 1 1 d . . . H12A H 0.8271 0.0298 0.0378 0.037 Uiso 1 1 calc R . . C13 C 0.7696(2) 0.0589(2) 0.04364(6) 0.0354(12) Uani 1 1 d . . . H13A H 0.7403 0.0369 0.0362 0.042 Uiso 1 1 calc R . . C14 C 0.8638(2) 0.0882(2) 0.05576(6) 0.0254(10) Uani 1 1 d . . . C15 C 0.8394(2) 0.1807(2) -0.01823(7) 0.0338(12) Uani 1 1 d . . . H15A H 0.8457 0.1540 -0.0122 0.041 Uiso 1 1 calc R . . C16 C 0.8791(2) 0.2110(2) -0.03043(7) 0.0376(13) Uani 1 1 d . . . H16A H 0.9112 0.2048 -0.0326 0.045 Uiso 1 1 calc R . . C17 C 0.8696(2) 0.2506(2) -0.03928(7) 0.0361(12) Uani 1 1 d . . . H17A H 0.8946 0.2709 -0.0477 0.043 Uiso 1 1 calc R . . C18 C 0.8223(2) 0.2598(2) -0.03545(6) 0.0337(12) Uani 1 1 d . . . H18A H 0.8161 0.2873 -0.0411 0.040 Uiso 1 1 calc R . . C19 C 0.7844(2) 0.2280(2) -0.02327(6) 0.0273(10) Uani 1 1 d . . . C20 C 0.7104(2) 0.3141(2) -0.01646(6) 0.0276(11) Uani 1 1 d . . . C21 C 0.6489(2) 0.2709(2) -0.01640(5) 0.0265(11) Uani 1 1 d . . . C22 C 0.7348(2) 0.2396(2) -0.01921(6) 0.0265(11) Uani 1 1 d . . . C23 C 0.6726(2) 0.1957(2) -0.01873(6) 0.0268(10) Uani 1 1 d . . . C24 C 0.5790(2) 0.0425(2) -0.03598(6) 0.0321(12) Uani 1 1 d . . . H24A H 0.5479 0.0231 -0.0432 0.038 Uiso 1 1 calc R . . C25 C 0.6040(2) 0.0123(2) -0.02908(6) 0.0343(12) Uani 1 1 d . . . H25A H 0.5907 -0.0278 -0.0316 0.041 Uiso 1 1 calc R . . C26 C 0.6495(2) 0.0423(2) -0.01826(6) 0.0295(11) Uani 1 1 d . . . H26A H 0.6657 0.0213 -0.0133 0.035 Uiso 1 1 calc R . . C27 C 0.5858(2) 0.0429(2) 0.04261(6) 0.0339(12) Uani 1 1 d . . . H27A H 0.5585 0.0238 0.0507 0.041 Uiso 1 1 calc R . . C28 C 0.6035(2) 0.0110(2) 0.03323(6) 0.0316(12) Uani 1 1 d . . . H28A H 0.5874 -0.0302 0.0347 0.038 Uiso 1 1 calc R . . C29 C 0.6092(2) 0.1041(2) 0.03986(6) 0.0306(11) Uani 1 1 d . . . H29A H 0.5967 0.1263 0.0458 0.037 Uiso 1 1 calc R . . C30 C 0.6514(2) 0.1315(2) 0.02814(6) 0.0255(10) Uani 1 1 d . . . C31 C 0.6754(2) 0.1970(2) 0.02529(5) 0.0245(10) Uani 1 1 d . . . C32 C 0.7381(2) 0.2424(2) 0.02517(5) 0.0248(10) Uani 1 1 d . . . C33 C 0.7114(2) 0.3154(2) 0.02360(5) 0.0254(10) Uani 1 1 d . . . C34 C 0.6498(2) 0.2708(2) 0.02384(6) 0.0253(10) Uani 1 1 d . . . C35 C 0.8317(2) 0.2662(2) 0.03881(6) 0.0302(11) Uani 1 1 d . . . H35A H 0.8270 0.2942 0.0446 0.036 Uiso 1 1 calc R . . C36 C 0.8805(2) 0.2595(2) 0.04122(7) 0.0345(12) Uani 1 1 d . . . H36A H 0.9090 0.2823 0.0487 0.041 Uiso 1 1 calc R . . C37 C 0.8869(2) 0.2178(2) 0.03220(7) 0.0361(13) Uani 1 1 d . . . H37A H 0.9202 0.2127 0.0334 0.043 Uiso 1 1 calc R . . C38 C 0.8426(2) 0.1842(2) 0.02143(6) 0.0317(12) Uani 1 1 d . . . H38A H 0.8469 0.1563 0.0154 0.038 Uiso 1 1 calc R . . C43 C 0.6003(2) 0.1021(2) -0.03221(6) 0.0326(12) Uani 1 1 d . . . H43A H 0.5832 0.1231 -0.0367 0.039 Uiso 1 1 calc R . . C53 C 0.6474(2) 0.1304(2) -0.02172(6) 0.0269(11) Uani 1 1 d . . . C54 C 0.7889(2) 0.2312(2) 0.02761(6) 0.0249(10) Uani 1 1 d . . . C57 C 0.6454(2) 0.0410(2) 0.02167(6) 0.0282(11) Uani 1 1 d . . . H57A H 0.6567 0.0191 0.0153 0.034 Uiso 1 1 calc R . . Cu1 Cu 0.91411(3) 0.16746(3) 0.083263(7) 0.02983(18) Uani 1 1 d . . . Cu2 Cu 0.73410(3) 0.13962(3) 0.002334(7) 0.02655(17) Uani 1 1 d . . . N1 N 1.0081(3) 0.1821(3) 0.10127(7) 0.0639(17) Uani 1 1 d . . . N3 N 0.8429(2) 0.0690(2) 0.10051(6) 0.0449(12) Uani 1 1 d . . . N6 N 0.85607(18) 0.12419(18) 0.06587(5) 0.0258(9) Uani 1 1 d . A . N7 N 0.97573(18) 0.21759(18) 0.06735(5) 0.0289(9) Uani 1 1 d . A . N8 N 1.02535(18) 0.11895(17) 0.05684(5) 0.0268(9) Uani 1 1 d . . . N9 N 0.90584(17) 0.02436(17) 0.05663(5) 0.0239(9) Uani 1 1 d . . . N10 N 0.67064(17) 0.10082(17) 0.01927(5) 0.0244(9) Uani 1 1 d . B . N12 N 0.67099(17) 0.09978(17) -0.01471(5) 0.0251(9) Uani 1 1 d . B . N13 N 0.79249(18) 0.18817(18) -0.01472(5) 0.0277(9) Uani 1 1 d . B . N14 N 0.79388(17) 0.18953(17) 0.01916(5) 0.0249(9) Uani 1 1 d . B . N15 N 0.63083(19) 0.21160(18) -0.01731(5) 0.0287(9) Uani 1 1 d . . . N16 N 0.63255(18) 0.21219(17) 0.02447(5) 0.0254(9) Uani 1 1 d . . . N17 N 0.75325(19) 0.29861(18) -0.01789(5) 0.0300(9) Uani 1 1 d . . . N18 N 0.75462(18) 0.30027(18) 0.02429(4) 0.0242(9) Uani 1 1 d . . . O1 O 0.97402(19) 0.2050(2) 0.10017(5) 0.0499(11) Uani 1 1 d . A . O2 O 1.0037(3) 0.1443(3) 0.09147(7) 0.0779(16) Uani 1 1 d . A . O3 O 1.0448(2) 0.1998(4) 0.11201(6) 0.102(2) Uani 1 1 d . A . N2 N 0.8572(4) 0.2492(3) 0.09618(9) 0.050(3) Uani 0.689(11) 1 d PDU A 1 O4 O 0.8955(4) 0.2459(4) 0.08790(12) 0.079(3) Uani 0.689(11) 1 d PDU A 1 O5 O 0.8726(5) 0.2838(5) 0.10745(11) 0.089(5) Uani 0.689(11) 1 d PD A 1 O6 O 0.8025(3) 0.2170(4) 0.09303(10) 0.082(3) Uani 0.689(11) 1 d PD A 1 N2' N 0.8769(6) 0.2610(6) 0.09774(16) 0.037(6) Uani 0.311(11) 1 d PDU A 2 O4' O 0.8657(7) 0.2248(8) 0.0868(2) 0.062(6) Uani 0.311(11) 1 d PDU A 2 O5' O 0.9298(7) 0.3003(8) 0.1004(2) 0.108(9) Uani 0.311(11) 1 d PD A 2 O6' O 0.8353(8) 0.2576(11) 0.1059(3) 0.101(10) Uani 0.311(11) 1 d PD A 2 O7 O 0.85244(18) 0.12114(18) 0.09895(4) 0.0414(9) Uani 1 1 d . A . O8 O 0.8071(3) 0.0356(3) 0.11032(7) 0.091(2) Uani 1 1 d . A . O9 O 0.8694(3) 0.0498(2) 0.09152(6) 0.0741(16) Uani 1 1 d . A . N4 N 0.7705(8) 0.0234(10) -0.0005(2) 0.039(3) Uani 0.224(4) 1 d PD B 1 O10 O 0.7631(13) 0.0642(12) 0.0037(3) 0.0277(15) Uani 0.224(4) 1 d PDU B 1 O11 O 0.767(2) 0.0096(18) -0.0145(3) 0.17(2) Uani 0.224(4) 1 d PDU B 1 O12 O 0.7822(17) -0.0058(15) 0.0091(4) 0.112(13) Uani 0.224(4) 1 d PDU B 1 N4' N 0.7806(5) 0.0386(5) 0.00381(10) 0.039(3) Uani 0.392(8) 1 d PD B 2 O10' O 0.7580(5) 0.0670(5) -0.00052(13) 0.0277(15) Uani 0.392(8) 1 d PDU B 2 O11' O 0.8369(4) 0.0617(5) 0.0031(2) 0.087(6) Uani 0.392(8) 1 d PD B 2 O12' O 0.7510(7) -0.0134(5) 0.00904(18) 0.071(5) Uani 0.392(8) 1 d PDU B 2 N4" N 0.7586(5) 0.0292(5) -0.00066(12) 0.039(3) Uani 0.384(8) 1 d PD B 3 O10" O 0.7593(7) 0.0686(6) 0.00665(14) 0.0277(15) Uani 0.384(8) 1 d PDU B 3 O11" O 0.7943(8) 0.0381(6) -0.01143(18) 0.090(6) Uani 0.384(8) 1 d PDU B 3 O12" O 0.7207(7) -0.0247(5) 0.0022(2) 0.086(5) Uani 0.384(8) 1 d PDU B 3 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 0.041(3) 0.026(3) 0.046(3) -0.008(2) -0.012(3) 0.018(3) C2 0.040(3) 0.023(3) 0.063(4) -0.003(3) -0.010(3) 0.016(3) C3 0.035(3) 0.027(3) 0.077(5) 0.021(3) 0.019(3) 0.011(3) C4 0.040(3) 0.030(3) 0.065(4) 0.009(3) 0.020(3) 0.020(3) C5 0.023(3) 0.022(3) 0.045(3) -0.002(2) -0.004(2) 0.014(2) C6 0.023(2) 0.023(2) 0.027(2) 0.0024(19) 0.0016(19) 0.010(2) C7 0.026(3) 0.021(2) 0.028(2) 0.002(2) 0.000(2) 0.014(2) C8 0.020(2) 0.020(2) 0.034(3) 0.000(2) -0.0025(19) 0.010(2) C9 0.021(2) 0.024(3) 0.036(3) -0.001(2) 0.004(2) 0.010(2) C10 0.035(3) 0.040(3) 0.043(3) 0.001(2) 0.006(2) 0.026(3) C11 0.031(3) 0.050(4) 0.051(3) -0.004(3) -0.008(3) 0.029(3) C12 0.032(3) 0.031(3) 0.032(3) -0.006(2) -0.003(2) 0.017(2) C13 0.031(3) 0.039(3) 0.039(3) -0.006(2) -0.014(2) 0.019(3) C14 0.024(3) 0.023(2) 0.031(3) 0.004(2) 0.002(2) 0.013(2) C15 0.025(3) 0.028(3) 0.049(3) -0.006(2) -0.009(2) 0.014(2) C16 0.026(3) 0.030(3) 0.057(4) -0.005(3) -0.003(3) 0.015(2) C17 0.025(3) 0.030(3) 0.045(3) 0.001(2) 0.004(2) 0.008(2) C18 0.028(3) 0.026(3) 0.042(3) 0.003(2) 0.002(2) 0.010(2) C19 0.024(3) 0.023(2) 0.033(3) -0.002(2) -0.003(2) 0.010(2) C20 0.027(3) 0.026(3) 0.033(3) -0.002(2) -0.004(2) 0.016(2) C21 0.030(3) 0.024(3) 0.027(2) 0.005(2) 0.000(2) 0.014(2) C22 0.025(3) 0.023(3) 0.031(3) -0.002(2) -0.003(2) 0.012(2) C23 0.023(3) 0.027(3) 0.032(3) 0.000(2) -0.001(2) 0.014(2) C24 0.031(3) 0.030(3) 0.029(3) -0.005(2) -0.005(2) 0.010(2) C25 0.034(3) 0.024(3) 0.035(3) -0.007(2) 0.001(2) 0.008(2) C26 0.025(3) 0.026(3) 0.035(3) 0.003(2) -0.001(2) 0.011(2) C27 0.026(3) 0.039(3) 0.037(3) 0.011(2) 0.000(2) 0.016(2) C28 0.027(3) 0.024(3) 0.042(3) 0.004(2) -0.009(2) 0.011(2) C29 0.028(3) 0.029(3) 0.037(3) 0.002(2) -0.004(2) 0.016(2) C30 0.022(2) 0.020(2) 0.034(3) 0.002(2) -0.007(2) 0.010(2) C31 0.024(2) 0.029(3) 0.022(2) 0.0003(19) -0.0003(19) 0.014(2) C32 0.024(3) 0.022(2) 0.029(2) -0.0011(19) -0.003(2) 0.012(2) C33 0.026(3) 0.029(3) 0.027(2) -0.002(2) 0.0006(19) 0.017(2) C34 0.023(2) 0.024(3) 0.030(3) 0.000(2) -0.002(2) 0.013(2) C35 0.031(3) 0.027(3) 0.033(3) -0.003(2) -0.007(2) 0.015(2) C36 0.026(3) 0.022(3) 0.047(3) 0.001(2) -0.014(2) 0.005(2) C37 0.021(3) 0.034(3) 0.056(3) 0.005(3) -0.008(2) 0.015(2) C38 0.028(3) 0.027(3) 0.040(3) 0.000(2) 0.001(2) 0.014(2) C43 0.029(3) 0.038(3) 0.031(3) 0.004(2) 0.000(2) 0.017(2) C53 0.025(3) 0.030(3) 0.027(2) 0.000(2) -0.002(2) 0.014(2) C54 0.023(2) 0.018(2) 0.031(2) 0.0041(19) -0.002(2) 0.009(2) C57 0.028(3) 0.022(3) 0.034(3) 0.002(2) -0.008(2) 0.011(2) Cu1 0.0318(4) 0.0296(3) 0.0292(3) -0.0050(3) -0.0035(3) 0.0161(3) Cu2 0.0240(3) 0.0226(3) 0.0310(3) -0.0008(2) -0.0045(2) 0.0101(3) N1 0.048(3) 0.090(5) 0.041(3) 0.001(3) -0.012(3) 0.024(4) N3 0.046(3) 0.057(3) 0.038(3) 0.019(2) 0.015(2) 0.031(3) N6 0.023(2) 0.025(2) 0.034(2) 0.0004(17) -0.0001(17) 0.0153(18) N7 0.026(2) 0.025(2) 0.036(2) -0.0050(18) -0.0098(18) 0.0135(19) N8 0.026(2) 0.017(2) 0.038(2) 0.0011(17) 0.0017(18) 0.0117(18) N9 0.023(2) 0.020(2) 0.029(2) 0.0000(16) 0.0001(16) 0.0110(17) N10 0.022(2) 0.019(2) 0.029(2) 0.0013(16) -0.0085(17) 0.0089(17) N12 0.021(2) 0.022(2) 0.030(2) -0.0023(17) -0.0025(17) 0.0088(18) N13 0.022(2) 0.022(2) 0.037(2) -0.0029(18) -0.0033(18) 0.0099(18) N14 0.020(2) 0.018(2) 0.035(2) -0.0002(17) -0.0055(17) 0.0079(17) N15 0.032(2) 0.026(2) 0.027(2) 0.0045(17) 0.0022(18) 0.0128(19) N16 0.026(2) 0.021(2) 0.029(2) 0.0012(17) -0.0019(17) 0.0114(18) N17 0.029(2) 0.023(2) 0.035(2) 0.0003(18) -0.0037(18) 0.0114(19) N18 0.025(2) 0.026(2) 0.025(2) -0.0031(16) -0.0010(16) 0.0162(18) O1 0.043(2) 0.056(3) 0.037(2) -0.0080(19) -0.0050(19) 0.015(2) O2 0.093(4) 0.092(4) 0.075(4) -0.010(3) -0.034(3) 0.066(4) O3 0.054(3) 0.196(7) 0.043(3) -0.011(4) -0.018(3) 0.054(4) N2 0.055(6) 0.050(6) 0.056(5) -0.003(4) 0.002(5) 0.035(5) O4 0.076(6) 0.058(5) 0.118(6) 0.002(4) 0.042(5) 0.044(5) O5 0.137(11) 0.092(8) 0.071(6) -0.050(6) -0.050(8) 0.082(9) O6 0.066(6) 0.083(6) 0.097(7) -0.008(5) 0.005(5) 0.037(5) N2' 0.039(9) 0.021(8) 0.048(9) -0.009(6) 0.009(7) 0.013(6) O4' 0.060(9) 0.063(9) 0.083(9) -0.022(7) -0.010(7) 0.045(7) O5' 0.108(18) 0.084(15) 0.098(16) -0.050(12) 0.015(13) 0.022(13) O6' 0.088(17) 0.13(2) 0.091(19) -0.032(15) 0.036(15) 0.059(18) O7 0.041(2) 0.038(2) 0.042(2) -0.0042(18) 0.0048(18) 0.0176(19) O8 0.115(5) 0.086(4) 0.095(4) 0.050(3) 0.060(4) 0.068(4) O9 0.103(4) 0.077(4) 0.074(3) 0.026(3) 0.035(3) 0.069(3) N4 0.030(6) 0.050(6) 0.039(5) 0.004(4) 0.002(5) 0.022(5) O10 0.029(2) 0.026(2) 0.024(3) 0.000(2) -0.014(2) 0.0109(16) O11 0.17(2) 0.17(2) 0.16(2) -0.003(7) -0.001(7) 0.081(12) O12 0.113(16) 0.117(16) 0.116(16) 0.011(9) -0.005(10) 0.065(11) N4' 0.030(6) 0.050(6) 0.039(5) 0.004(4) 0.002(5) 0.022(5) O10' 0.029(2) 0.026(2) 0.024(3) 0.000(2) -0.014(2) 0.0109(16) O11' 0.059(9) 0.062(9) 0.159(16) 0.002(9) 0.005(9) 0.045(8) O12' 0.081(9) 0.053(7) 0.069(8) 0.014(6) 0.006(7) 0.026(6) N4" 0.030(6) 0.050(6) 0.039(5) 0.004(4) 0.002(5) 0.022(5) O10" 0.029(2) 0.026(2) 0.024(3) 0.000(2) -0.014(2) 0.0109(16) O11" 0.113(10) 0.069(8) 0.073(8) 0.006(6) 0.041(7) 0.035(7) O12" 0.082(9) 0.064(8) 0.106(9) 0.009(7) -0.004(7) 0.033(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N7 1.351(6) . ? C1 C2 1.375(8) . ? C1 H1 0.9300 . ? C2 C3 1.364(9) . ? C2 H2 0.9300 . ? C3 C4 1.380(8) . ? C3 H3 0.9300 . ? C4 C5 1.387(7) . ? C4 H4 0.9300 . ? C5 N7 1.356(6) . ? C5 C6 1.502(7) . ? C6 N8 1.334(6) . ? C6 C7 1.412(7) . ? C7 N9 1.330(6) . ? C7 C14 1.511(6) . ? C8 N9 1.344(6) . ? C8 C9 1.397(7) . ? C8 C9 1.465(6) 2_645 ? C9 N8 1.354(6) . ? C9 C8 1.465(6) 3_765 ? C10 N6 1.349(6) . ? C10 C11 1.371(8) . ? C10 H10A 0.9300 . ? C11 C13 1.365(8) . ? C11 H11A 0.9300 . ? C12 C14 1.383(7) . ? C12 C13 1.383(7) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 N6 1.351(6) . ? C15 N13 1.343(6) . ? C15 C16 1.393(8) . ? C15 H15A 0.9300 . ? C16 C17 1.383(8) . ? C16 H16A 0.9300 . ? C17 C18 1.384(8) . ? C17 H17A 0.9300 . ? C18 C19 1.379(7) . ? C18 H18A 0.9300 . ? C19 N13 1.354(6) . ? C19 C22 1.483(7) . ? C20 N17 1.347(6) . ? C20 C21 1.401(7) . ? C20 C21 1.460(7) 2_655 ? C21 N15 1.351(6) . ? C21 C20 1.460(7) 3_665 ? C22 N17 1.345(6) . ? C22 C23 1.420(7) . ? C23 N15 1.328(6) . ? C23 C53 1.485(7) . ? C24 C25 1.361(8) . ? C24 C43 1.380(7) . ? C24 H24A 0.9300 . ? C25 C26 1.383(7) . ? C25 H25A 0.9300 . ? C26 N12 1.325(6) . ? C26 H26A 0.9300 . ? C27 C28 1.374(8) . ? C27 C29 1.392(7) . ? C27 H27A 0.9300 . ? C28 C57 1.377(7) . ? C28 H28A 0.9300 . ? C29 C30 1.382(7) . ? C29 H29A 0.9300 . ? C30 N10 1.352(6) . ? C30 C31 1.489(7) . ? C31 N16 1.339(6) . ? C31 C32 1.438(7) . ? C32 N18 1.325(6) . ? C32 C54 1.482(6) . ? C33 N18 1.345(6) . ? C33 C34 1.412(7) . ? C33 C34 1.456(7) 2_655 ? C34 N16 1.338(6) . ? C34 C33 1.456(7) 3_665 ? C35 C36 1.359(7) . ? C35 C54 1.394(7) . ? C35 H35A 0.9300 . ? C36 C37 1.393(8) . ? C36 H36A 0.9300 . ? C37 C38 1.379(7) . ? C37 H37A 0.9300 . ? C38 N14 1.338(6) . ? C38 H38A 0.9300 . ? C43 C53 1.384(7) . ? C43 H43A 0.9300 . ? C53 N12 1.346(6) . ? C54 N14 1.347(6) . ? C57 N10 1.349(6) . ? C57 H57A 0.9300 . ? Cu1 O7 1.958(4) . ? Cu1 O1 1.975(4) . ? Cu1 N7 1.993(4) . ? Cu1 N6 2.002(4) . ? Cu1 O4 2.319(8) . ? Cu1 O4' 2.367(17) . ? Cu2 N13 2.014(4) . ? Cu2 N14 2.025(4) . ? Cu2 N10 2.029(4) . ? Cu2 N12 2.034(4) . ? Cu2 O10" 2.244(14) . ? Cu2 O10' 2.245(11) . ? Cu2 O10 2.40(2) . ? N1 O3 1.229(7) . ? N1 O2 1.243(8) . ? N1 O1 1.274(8) . ? N3 O8 1.222(6) . ? N3 O7 1.241(6) . ? N3 O9 1.275(7) . ? N2 O5 1.234(8) . ? N2 O4 1.249(8) . ? N2 O6 1.249(8) . ? N2' O6' 1.242(9) . ? N2' O5' 1.242(9) . ? N2' O4' 1.250(9) . ? N4 O10 1.206(9) . ? N4 O11 1.244(9) . ? N4 O12 1.244(9) . ? N4' O10' 1.193(9) . ? N4' O12' 1.241(9) . ? N4' O11' 1.257(9) . ? N4" O10" 1.182(9) . ? N4" O11" 1.237(9) . ? N4" O12" 1.252(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 C1 C2 122.1(5) . . ? N7 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 119.0(5) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 119.0(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N7 C5 C4 120.9(5) . . ? N7 C5 C6 118.8(4) . . ? C4 C5 C6 120.2(5) . . ? N8 C6 C7 121.4(4) . . ? N8 C6 C5 112.5(4) . . ? C7 C6 C5 125.9(4) . . ? N9 C7 C6 121.3(4) . . ? N9 C7 C14 112.7(4) . . ? C6 C7 C14 125.7(4) . . ? N9 C8 C9 121.7(4) . . ? N9 C8 C9 118.8(4) . 2_645 ? C9 C8 C9 119.5(5) . 2_645 ? N8 C9 C8 120.9(4) . . ? N8 C9 C8 118.6(4) . 3_765 ? C8 C9 C8 120.5(5) . 3_765 ? N6 C10 C11 122.5(5) . . ? N6 C10 H10A 118.8 . . ? C11 C10 H10A 118.8 . . ? C13 C11 C10 119.2(5) . . ? C13 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C14 C12 C13 118.7(5) . . ? C14 C12 H12A 120.7 . . ? C13 C12 H12A 120.7 . . ? C11 C13 C12 119.6(5) . . ? C11 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? N6 C14 C12 121.9(4) . . ? N6 C14 C7 119.4(4) . . ? C12 C14 C7 118.6(4) . . ? N13 C15 C16 123.0(5) . . ? N13 C15 H15A 118.5 . . ? C16 C15 H15A 118.5 . . ? C17 C16 C15 118.2(5) . . ? C17 C16 H16A 120.9 . . ? C15 C16 H16A 120.9 . . ? C16 C17 C18 119.1(5) . . ? C16 C17 H17A 120.5 . . ? C18 C17 H17A 120.5 . . ? C19 C18 C17 119.8(5) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? N13 C19 C18 121.8(5) . . ? N13 C19 C22 119.6(4) . . ? C18 C19 C22 118.6(5) . . ? N17 C20 C21 121.9(4) . . ? N17 C20 C21 118.2(4) . 2_655 ? C21 C20 C21 119.7(5) . 2_655 ? N15 C21 C20 120.4(4) . . ? N15 C21 C20 119.2(4) . 3_665 ? C20 C21 C20 120.3(5) . 3_665 ? N17 C22 C23 120.8(4) . . ? N17 C22 C19 113.0(4) . . ? C23 C22 C19 125.7(4) . . ? N15 C23 C22 121.2(4) . . ? N15 C23 C53 113.5(4) . . ? C22 C23 C53 124.9(4) . . ? C25 C24 C43 119.3(5) . . ? C25 C24 H24A 120.3 . . ? C43 C24 H24A 120.3 . . ? C24 C25 C26 118.7(5) . . ? C24 C25 H25A 120.6 . . ? C26 C25 H25A 120.6 . . ? N12 C26 C25 122.5(5) . . ? N12 C26 H26A 118.8 . . ? C25 C26 H26A 118.8 . . ? C28 C27 C29 119.1(5) . . ? C28 C27 H27A 120.4 . . ? C29 C27 H27A 120.4 . . ? C27 C28 C57 119.1(5) . . ? C27 C28 H28A 120.5 . . ? C57 C28 H28A 120.5 . . ? C30 C29 C27 118.9(5) . . ? C30 C29 H29A 120.6 . . ? C27 C29 H29A 120.6 . . ? N10 C30 C29 122.2(4) . . ? N10 C30 C31 119.9(4) . . ? C29 C30 C31 118.0(4) . . ? N16 C31 C32 120.7(4) . . ? N16 C31 C30 113.5(4) . . ? C32 C31 C30 125.3(4) . . ? N18 C32 C31 120.6(4) . . ? N18 C32 C54 113.9(4) . . ? C31 C32 C54 125.2(4) . . ? N18 C33 C34 121.0(4) . . ? N18 C33 C34 118.6(4) . 2_655 ? C34 C33 C34 120.3(5) . 2_655 ? N16 C34 C33 121.1(4) . . ? N16 C34 C33 119.2(4) . 3_665 ? C33 C34 C33 119.7(5) . 3_665 ? C36 C35 C54 120.0(5) . . ? C36 C35 H35A 120.0 . . ? C54 C35 H35A 120.0 . . ? C35 C36 C37 118.8(5) . . ? C35 C36 H36A 120.6 . . ? C37 C36 H36A 120.6 . . ? C38 C37 C36 118.3(5) . . ? C38 C37 H37A 120.9 . . ? C36 C37 H37A 120.9 . . ? N14 C38 C37 123.5(5) . . ? N14 C38 H38A 118.3 . . ? C37 C38 H38A 118.3 . . ? C24 C43 C53 119.4(5) . . ? C24 C43 H43A 120.3 . . ? C53 C43 H43A 120.3 . . ? N12 C53 C43 120.8(5) . . ? N12 C53 C23 120.7(4) . . ? C43 C53 C23 118.4(4) . . ? N14 C54 C35 121.6(4) . . ? N14 C54 C32 121.2(4) . . ? C35 C54 C32 117.2(4) . . ? N10 C57 C28 122.7(5) . . ? N10 C57 H57A 118.7 . . ? C28 C57 H57A 118.7 . . ? O7 Cu1 O1 89.31(17) . . ? O7 Cu1 N7 177.27(17) . . ? O1 Cu1 N7 90.84(17) . . ? O7 Cu1 N6 91.34(17) . . ? O1 Cu1 N6 174.83(18) . . ? N7 Cu1 N6 88.76(16) . . ? O7 Cu1 O4 87.4(2) . . ? O1 Cu1 O4 84.2(3) . . ? N7 Cu1 O4 89.9(2) . . ? N6 Cu1 O4 100.9(3) . . ? O7 Cu1 O4' 77.0(5) . . ? O1 Cu1 O4' 97.3(4) . . ? N7 Cu1 O4' 100.3(5) . . ? N6 Cu1 O4' 87.9(3) . . ? O4 Cu1 O4' 16.8(4) . . ? N13 Cu2 N14 91.83(16) . . ? N13 Cu2 N10 170.53(16) . . ? N14 Cu2 N10 88.22(16) . . ? N13 Cu2 N12 87.05(16) . . ? N14 Cu2 N12 171.24(16) . . ? N10 Cu2 N12 91.46(16) . . ? N13 Cu2 O10" 101.2(4) . . ? N14 Cu2 O10" 87.8(3) . . ? N10 Cu2 O10" 88.3(4) . . ? N12 Cu2 O10" 101.0(3) . . ? N13 Cu2 O10' 90.4(3) . . ? N14 Cu2 O10' 99.6(3) . . ? N10 Cu2 O10' 99.0(3) . . ? N12 Cu2 O10' 89.1(3) . . ? O10" Cu2 O10' 15.8(3) . . ? N13 Cu2 O10 95.7(7) . . ? N14 Cu2 O10 91.9(6) . . ? N10 Cu2 O10 93.7(7) . . ? N12 Cu2 O10 96.9(6) . . ? O10" Cu2 O10 6.7(7) . . ? O10' Cu2 O10 9.3(6) . . ? O3 N1 O2 123.1(7) . . ? O3 N1 O1 117.4(7) . . ? O2 N1 O1 119.5(5) . . ? O8 N3 O7 120.2(5) . . ? O8 N3 O9 120.2(6) . . ? O7 N3 O9 119.6(5) . . ? C10 N6 C14 118.1(4) . . ? C10 N6 Cu1 119.5(4) . . ? C14 N6 Cu1 122.2(3) . . ? C1 N7 C5 118.9(5) . . ? C1 N7 Cu1 117.3(4) . . ? C5 N7 Cu1 123.7(3) . . ? C6 N8 C9 117.2(4) . . ? C7 N9 C8 117.4(4) . . ? C57 N10 C30 118.0(4) . . ? C57 N10 Cu2 118.5(3) . . ? C30 N10 Cu2 123.5(3) . . ? C26 N12 C53 119.2(4) . . ? C26 N12 Cu2 120.4(3) . . ? C53 N12 Cu2 120.2(3) . . ? C15 N13 C19 118.2(4) . . ? C15 N13 Cu2 121.0(4) . . ? C19 N13 Cu2 120.8(3) . . ? C38 N14 C54 117.8(4) . . ? C38 N14 Cu2 119.3(3) . . ? C54 N14 Cu2 122.8(3) . . ? C23 N15 C21 118.3(4) . . ? C34 N16 C31 118.1(4) . . ? C22 N17 C20 117.3(4) . . ? C32 N18 C33 118.5(4) . . ? N1 O1 Cu1 112.0(4) . . ? O5 N2 O4 120.8(8) . . ? O5 N2 O6 119.6(7) . . ? O4 N2 O6 119.5(7) . . ? N2 O4 Cu1 131.8(6) . . ? O6' N2' O5' 120.2(8) . . ? O6' N2' O4' 120.2(8) . . ? O5' N2' O4' 119.6(8) . . ? N2' O4' Cu1 124.0(11) . . ? N3 O7 Cu1 113.1(3) . . ? O10 N4 O11 120.7(9) . . ? O10 N4 O12 120.9(9) . . ? O11 N4 O12 118.4(9) . . ? N4 O10 Cu2 158.5(16) . . ? O10' N4' O12' 123.0(8) . . ? O10' N4' O11' 119.4(8) . . ? O12' N4' O11' 117.6(8) . . ? N4' O10' Cu2 152.7(8) . . ? O10" N4" O11" 122.9(9) . . ? O10" N4" O12" 120.8(8) . . ? O11" N4" O12" 116.3(8) . . ? N4" O10" Cu2 136.0(9) . . ? 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 N7 C1 C2 C3 0.6(9) . . . . ? C1 C2 C3 C4 -1.6(9) . . . . ? C2 C3 C4 C5 1.8(10) . . . . ? C3 C4 C5 N7 -0.8(9) . . . . ? C3 C4 C5 C6 -178.0(5) . . . . ? N7 C5 C6 N8 -132.9(5) . . . . ? C4 C5 C6 N8 44.3(7) . . . . ? N7 C5 C6 C7 52.6(7) . . . . ? C4 C5 C6 C7 -130.2(6) . . . . ? N8 C6 C7 N9 1.3(7) . . . . ? C5 C6 C7 N9 175.4(5) . . . . ? N8 C6 C7 C14 -171.8(5) . . . . ? C5 C6 C7 C14 2.3(8) . . . . ? N9 C8 C9 N8 0.0(8) . . . . ? N9 C8 C9 C8 -178.6(3) . . . 3_765 ? C9 C8 C9 C8 1.3(10) 2_645 . . 3_765 ? N6 C10 C11 C13 1.3(9) . . . . ? C10 C11 C13 C12 -0.8(9) . . . . ? C14 C12 C13 C11 -0.2(8) . . . . ? C13 C12 C14 N6 0.7(8) . . . . ? C13 C12 C14 C7 177.5(5) . . . . ? N9 C7 C14 N6 132.6(5) . . . . ? C6 C7 C14 N6 -53.8(7) . . . . ? N9 C7 C14 C12 -44.3(6) . . . . ? C6 C7 C14 C12 129.3(5) . . . . ? N13 C15 C16 C17 0.1(8) . . . . ? C15 C16 C17 C18 1.7(8) . . . . ? C16 C17 C18 C19 -2.1(8) . . . . ? C17 C18 C19 N13 0.7(8) . . . . ? C17 C18 C19 C22 178.8(5) . . . . ? N17 C20 C21 N15 2.1(8) . . . . ? C21 C20 C21 N15 176.4(3) 2_655 . . . ? N17 C20 C21 C20 -173.6(3) . . . 3_665 ? C21 C20 C21 C20 0.7(10) 2_655 . . 3_665 ? N13 C19 C22 N17 129.6(5) . . . . ? C18 C19 C22 N17 -48.5(6) . . . . ? N13 C19 C22 C23 -58.7(7) . . . . ? C18 C19 C22 C23 123.2(6) . . . . ? N17 C22 C23 N15 1.5(8) . . . . ? C19 C22 C23 N15 -169.6(5) . . . . ? N17 C22 C23 C53 173.3(5) . . . . ? C19 C22 C23 C53 2.2(8) . . . . ? C43 C24 C25 C26 1.0(8) . . . . ? C24 C25 C26 N12 -2.1(8) . . . . ? C29 C27 C28 C57 2.0(7) . . . . ? C28 C27 C29 C30 -2.4(7) . . . . ? C27 C29 C30 N10 -0.1(7) . . . . ? C27 C29 C30 C31 179.3(4) . . . . ? N10 C30 C31 N16 132.1(4) . . . . ? C29 C30 C31 N16 -47.3(6) . . . . ? N10 C30 C31 C32 -55.0(7) . . . . ? C29 C30 C31 C32 125.5(5) . . . . ? N16 C31 C32 N18 0.1(7) . . . . ? C30 C31 C32 N18 -172.3(4) . . . . ? N16 C31 C32 C54 173.5(4) . . . . ? C30 C31 C32 C54 1.1(8) . . . . ? N18 C33 C34 N16 -1.1(7) . . . . ? C34 C33 C34 N16 -176.4(3) 2_655 . . . ? N18 C33 C34 C33 178.0(3) . . . 3_665 ? C34 C33 C34 C33 2.7(9) 2_655 . . 3_665 ? C54 C35 C36 C37 0.7(8) . . . . ? C35 C36 C37 C38 -1.4(8) . . . . ? C36 C37 C38 N14 0.1(8) . . . . ? C25 C24 C43 C53 1.2(8) . . . . ? C24 C43 C53 N12 -2.6(8) . . . . ? C24 C43 C53 C23 175.5(5) . . . . ? N15 C23 C53 N12 -139.6(5) . . . . ? C22 C23 C53 N12 48.1(7) . . . . ? N15 C23 C53 C43 42.4(6) . . . . ? C22 C23 C53 C43 -130.0(5) . . . . ? C36 C35 C54 N14 1.2(8) . . . . ? C36 C35 C54 C32 -177.8(5) . . . . ? N18 C32 C54 N14 -133.9(5) . . . . ? C31 C32 C54 N14 52.3(7) . . . . ? N18 C32 C54 C35 45.1(6) . . . . ? C31 C32 C54 C35 -128.7(5) . . . . ? C27 C28 C57 N10 0.9(7) . . . . ? C11 C10 N6 C14 -0.8(8) . . . . ? C11 C10 N6 Cu1 -175.9(4) . . . . ? C12 C14 N6 C10 -0.2(7) . . . . ? C7 C14 N6 C10 -177.0(4) . . . . ? C12 C14 N6 Cu1 174.8(4) . . . . ? C7 C14 N6 Cu1 -2.0(6) . . . . ? O7 Cu1 N6 C10 59.5(4) . . . . ? O1 Cu1 N6 C10 156.7(18) . . . . ? N7 Cu1 N6 C10 -117.7(4) . . . . ? O4 Cu1 N6 C10 -28.1(4) . . . . ? O4' Cu1 N6 C10 -17.4(6) . . . . ? O7 Cu1 N6 C14 -115.4(4) . . . . ? O1 Cu1 N6 C14 -18(2) . . . . ? N7 Cu1 N6 C14 67.4(4) . . . . ? O4 Cu1 N6 C14 157.0(4) . . . . ? O4' Cu1 N6 C14 167.7(6) . . . . ? C2 C1 N7 C5 0.3(8) . . . . ? C2 C1 N7 Cu1 178.7(4) . . . . ? C4 C5 N7 C1 -0.2(7) . . . . ? C6 C5 N7 C1 177.0(4) . . . . ? C4 C5 N7 Cu1 -178.5(4) . . . . ? C6 C5 N7 Cu1 -1.2(6) . . . . ? O7 Cu1 N7 C1 24(4) . . . . ? O1 Cu1 N7 C1 -68.8(4) . . . . ? N6 Cu1 N7 C1 116.4(4) . . . . ? O4 Cu1 N7 C1 15.4(4) . . . . ? O4' Cu1 N7 C1 28.7(5) . . . . ? O7 Cu1 N7 C5 -158(3) . . . . ? O1 Cu1 N7 C5 109.5(4) . . . . ? N6 Cu1 N7 C5 -65.3(4) . . . . ? O4 Cu1 N7 C5 -166.3(5) . . . . ? O4' Cu1 N7 C5 -153.0(5) . . . . ? C7 C6 N8 C9 -4.1(7) . . . . ? C5 C6 N8 C9 -178.8(4) . . . . ? C8 C9 N8 C6 3.4(7) . . . . ? C8 C9 N8 C6 -177.9(4) 3_765 . . . ? C6 C7 N9 C8 2.2(7) . . . . ? C14 C7 N9 C8 176.1(4) . . . . ? C9 C8 N9 C7 -2.8(7) . . . . ? C9 C8 N9 C7 177.3(4) 2_645 . . . ? C28 C57 N10 C30 -3.4(7) . . . . ? C28 C57 N10 Cu2 177.8(4) . . . . ? C29 C30 N10 C57 2.9(7) . . . . ? C31 C30 N10 C57 -176.5(4) . . . . ? C29 C30 N10 Cu2 -178.3(3) . . . . ? C31 C30 N10 Cu2 2.3(6) . . . . ? N13 Cu2 N10 C57 152.0(9) . . . . ? N14 Cu2 N10 C57 -117.5(3) . . . . ? N12 Cu2 N10 C57 71.2(3) . . . . ? O10" Cu2 N10 C57 -29.7(5) . . . . ? O10' Cu2 N10 C57 -18.0(4) . . . . ? O10 Cu2 N10 C57 -25.8(7) . . . . ? N13 Cu2 N10 C30 -26.8(12) . . . . ? N14 Cu2 N10 C30 63.7(4) . . . . ? N12 Cu2 N10 C30 -107.5(4) . . . . ? O10" Cu2 N10 C30 151.5(5) . . . . ? O10' Cu2 N10 C30 163.2(4) . . . . ? O10 Cu2 N10 C30 155.4(7) . . . . ? C25 C26 N12 C53 0.8(7) . . . . ? C25 C26 N12 Cu2 175.9(4) . . . . ? C43 C53 N12 C26 1.6(7) . . . . ? C23 C53 N12 C26 -176.5(5) . . . . ? C43 C53 N12 Cu2 -173.6(4) . . . . ? C23 C53 N12 Cu2 8.4(6) . . . . ? N13 Cu2 N12 C26 111.4(4) . . . . ? N14 Cu2 N12 C26 -165.8(9) . . . . ? N10 Cu2 N12 C26 -78.0(4) . . . . ? O10" Cu2 N12 C26 10.5(5) . . . . ? O10' Cu2 N12 C26 20.9(5) . . . . ? O10 Cu2 N12 C26 15.9(8) . . . . ? N13 Cu2 N12 C53 -73.5(4) . . . . ? N14 Cu2 N12 C53 9.3(13) . . . . ? N10 Cu2 N12 C53 97.1(4) . . . . ? O10" Cu2 N12 C53 -174.3(5) . . . . ? O10' Cu2 N12 C53 -163.9(5) . . . . ? O10 Cu2 N12 C53 -168.9(7) . . . . ? C16 C15 N13 C19 -1.4(7) . . . . ? C16 C15 N13 Cu2 176.7(4) . . . . ? C18 C19 N13 C15 1.0(7) . . . . ? C22 C19 N13 C15 -177.0(4) . . . . ? C18 C19 N13 Cu2 -177.1(4) . . . . ? C22 C19 N13 Cu2 4.9(6) . . . . ? N14 Cu2 N13 C15 75.4(4) . . . . ? N10 Cu2 N13 C15 165.6(8) . . . . ? N12 Cu2 N13 C15 -113.3(4) . . . . ? O10" Cu2 N13 C15 -12.7(5) . . . . ? O10' Cu2 N13 C15 -24.3(5) . . . . ? O10 Cu2 N13 C15 -16.6(7) . . . . ? N14 Cu2 N13 C19 -106.5(4) . . . . ? N10 Cu2 N13 C19 -16.4(12) . . . . ? N12 Cu2 N13 C19 64.8(4) . . . . ? O10" Cu2 N13 C19 165.4(5) . . . . ? O10' Cu2 N13 C19 153.8(4) . . . . ? O10 Cu2 N13 C19 161.4(7) . . . . ? C37 C38 N14 C54 1.8(7) . . . . ? C37 C38 N14 Cu2 177.6(4) . . . . ? C35 C54 N14 C38 -2.5(7) . . . . ? C32 C54 N14 C38 176.5(4) . . . . ? C35 C54 N14 Cu2 -178.1(4) . . . . ? C32 C54 N14 Cu2 0.9(6) . . . . ? N13 Cu2 N14 C38 -70.5(4) . . . . ? N10 Cu2 N14 C38 118.9(4) . . . . ? N12 Cu2 N14 C38 -153.0(10) . . . . ? O10" Cu2 N14 C38 30.6(5) . . . . ? O10' Cu2 N14 C38 20.1(5) . . . . ? O10 Cu2 N14 C38 25.3(7) . . . . ? N13 Cu2 N14 C54 105.0(4) . . . . ? N10 Cu2 N14 C54 -65.5(4) . . . . ? N12 Cu2 N14 C54 22.5(13) . . . . ? O10" Cu2 N14 C54 -153.9(5) . . . . ? O10' Cu2 N14 C54 -164.3(5) . . . . ? O10 Cu2 N14 C54 -159.2(7) . . . . ? C22 C23 N15 C21 0.3(7) . . . . ? C53 C23 N15 C21 -172.4(4) . . . . ? C20 C21 N15 C23 -2.0(7) . . . . ? C20 C21 N15 C23 173.8(4) 3_665 . . . ? C33 C34 N16 C31 1.6(7) . . . . ? C33 C34 N16 C31 -177.5(4) 3_665 . . . ? C32 C31 N16 C34 -1.1(7) . . . . ? C30 C31 N16 C34 172.1(4) . . . . ? C23 C22 N17 C20 -1.5(7) . . . . ? C19 C22 N17 C20 170.7(4) . . . . ? C21 C20 N17 C22 -0.3(7) . . . . ? C21 C20 N17 C22 -174.7(4) 2_655 . . . ? C31 C32 N18 C33 0.5(7) . . . . ? C54 C32 N18 C33 -173.7(4) . . . . ? C34 C33 N18 C32 0.0(7) . . . . ? C34 C33 N18 C32 175.4(4) 2_655 . . . ? O3 N1 O1 Cu1 -176.0(5) . . . . ? O2 N1 O1 Cu1 5.3(8) . . . . ? O7 Cu1 O1 N1 102.8(4) . . . . ? N7 Cu1 O1 N1 -79.9(4) . . . . ? N6 Cu1 O1 N1 6(2) . . . . ? O4 Cu1 O1 N1 -169.7(5) . . . . ? O4' Cu1 O1 N1 179.6(6) . . . . ? O5 N2 O4 Cu1 116.3(9) . . . . ? O6 N2 O4 Cu1 -63.4(9) . . . . ? O7 Cu1 O4 N2 -5.5(9) . . . . ? O1 Cu1 O4 N2 -95.0(9) . . . . ? N7 Cu1 O4 N2 174.1(9) . . . . ? N6 Cu1 O4 N2 85.4(9) . . . . ? O4' Cu1 O4 N2 45.7(19) . . . . ? O6' N2' O4' Cu1 -128.3(17) . . . . ? O5' N2' O4' Cu1 51.6(17) . . . . ? O7 Cu1 O4' N2' 81.1(13) . . . . ? O1 Cu1 O4' N2' -6.5(14) . . . . ? N7 Cu1 O4' N2' -98.7(13) . . . . ? N6 Cu1 O4' N2' 173.0(14) . . . . ? O4 Cu1 O4' N2' -45.9(15) . . . . ? O8 N3 O7 Cu1 177.3(5) . . . . ? O9 N3 O7 Cu1 -4.8(7) . . . . ? O1 Cu1 O7 N3 -98.5(4) . . . . ? N7 Cu1 O7 N3 168(11) . . . . ? N6 Cu1 O7 N3 76.4(4) . . . . ? O4 Cu1 O7 N3 177.3(5) . . . . ? O4' Cu1 O7 N3 163.9(5) . . . . ? O11 N4 O10 Cu2 14(5) . . . . ? O12 N4 O10 Cu2 -166(5) . . . . ? N13 Cu2 O10 N4 -63(5) . . . . ? N14 Cu2 O10 N4 -155(5) . . . . ? N10 Cu2 O10 N4 116(5) . . . . ? N12 Cu2 O10 N4 25(5) . . . . ? O10" Cu2 O10 N4 152(13) . . . . ? O10' Cu2 O10 N4 -8(3) . . . . ? O12' N4' O10' Cu2 104.1(18) . . . . ? O11' N4' O10' Cu2 -76.0(18) . . . . ? N13 Cu2 O10' N4' 110.3(18) . . . . ? N14 Cu2 O10' N4' 18.3(18) . . . . ? N10 Cu2 O10' N4' -71.4(18) . . . . ? N12 Cu2 O10' N4' -162.7(18) . . . . ? O10" Cu2 O10' N4' -23.4(18) . . . . ? O10 Cu2 O10' N4' -15(5) . . . . ? O11" N4" O10" Cu2 72.4(14) . . . . ? O12" N4" O10" Cu2 -107.4(14) . . . . ? N13 Cu2 O10" N4" -63.3(13) . . . . ? N14 Cu2 O10" N4" -154.8(13) . . . . ? N10 Cu2 O10" N4" 116.9(13) . . . . ? N12 Cu2 O10" N4" 25.8(13) . . . . ? O10' Cu2 O10" N4" -15.9(13) . . . . ? O10 Cu2 O10" N4" -27(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.826 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.092 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 445 109 ' ' 2 0.000 0.500 0.000 181 78 ' ' 3 -0.333 0.333 0.083 1215 300 ' ' 4 0.000 0.000 0.108 132 43 ' ' 5 -0.167 0.667 0.167 182 78 ' ' 6 0.000 0.000 0.250 1211 300 ' ' 7 0.167 0.833 0.333 182 78 ' ' 8 0.000 0.000 0.392 132 43 ' ' 9 0.333 0.667 0.417 1215 300 ' ' 10 0.000 0.000 0.500 445 109 ' ' 11 0.000 0.500 0.500 181 78 ' ' 12 -0.333 0.333 0.583 1215 300 ' ' 13 0.000 0.000 0.608 132 43 ' ' 14 -0.167 0.167 0.667 182 78 ' ' 15 0.000 0.000 0.750 1211 300 ' ' 16 0.167 0.333 0.833 182 78 ' ' 17 0.000 0.000 0.892 132 43 ' ' 18 0.333 0.667 0.917 1215 300 ' ' 19 0.167 0.333 0.333 182 78 ' ' 20 0.167 0.833 0.833 181 78 ' ' 21 0.333 0.667 0.167 459 109 ' ' 22 0.333 0.667 0.667 459 109 ' ' 23 0.333 0.167 0.167 182 78 ' ' 24 0.333 0.167 0.667 182 78 ' ' 25 0.333 0.667 0.058 129 42 ' ' 26 0.333 0.667 0.558 129 42 ' ' 27 0.333 0.667 0.275 132 43 ' ' 28 0.333 0.667 0.775 132 43 ' ' 29 0.500 0.500 0.000 182 78 ' ' 30 0.500 1.000 0.500 181 78 ' ' 31 0.500 0.000 0.000 181 78 ' ' 32 0.500 0.500 0.500 182 78 ' ' 33 0.667 0.333 0.333 459 109 ' ' 34 0.667 0.333 0.833 459 109 ' ' 35 0.667 0.833 0.333 182 78 ' ' 36 0.667 0.833 0.833 182 78 ' ' 37 0.667 0.333 0.225 132 43 ' ' 38 0.667 0.333 0.725 132 43 ' ' 39 0.667 0.333 0.442 129 42 ' ' 40 0.667 0.333 0.942 129 42 ' ' 41 0.833 1.167 0.167 181 78 ' ' 42 0.833 0.667 0.667 182 78 ' ' _platon_squeeze_details ;In order to subtract the contribution from the disordered solvent molecules, the SQUEEZE command was applied, which gave a new HKL file. The number of located electrons is 4370, is included in the formula, formula weight, calculated density, and F(000). These residual electron density were assigned to 12 water molecules and 14.5 dichloromethane molecules. So SQUEEZE 12 water molecules and 14.5 dichloromethane molecules per formula unit. This value calculated based upon electrons analysis. (One water molecule would give 10 e; one dichloromethane molecule would give 42 e). So the tentative formula for this compound is presented as in the text. See refs. (a) C. H Tan, S. H Yang, N. R. Champness, X. Lin, A. J. Blake, W. Lewis and M. Schroder, Chem. Commun., 2011, 47, 4487; (b) A. L. Spek, Acta Crystallogr.Sect.D, 2009, 65, 148. Z before the SQUEEZE is 6 and after the SQUEEZE is 12 ;