data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_contact_author_name 'Jian-Fang Ma' _publ_contact_author_address ; Key Lab of Polyoxometalate Science Department of Chemistry Northeast Normal University Changchun 130024 P.R.China ; _publ_contact_author_email jianfangma@yahoo.com.cn _publ_contact_author_fax +86-431-85098620 _publ_contact_author_phone +86-431-85098620 _publ_author_name 'Jian-Fang Ma' #============================================================================= data_Compound-1 _database_code_depnum_ccdc_archive 'CCDC 810538' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H25 Cd N7 O5, 2(H2 O)' _chemical_formula_sum 'C35 H29 Cd N7 O7' _chemical_formula_weight 772.05 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' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_space_group_name_hall '-P 2yn ' 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 10.0108(2) _cell_length_b 18.5140(4) _cell_length_c 18.8711(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.628(2) _cell_angle_gamma 90.00 _cell_volume 3474.19(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6002 _cell_measurement_theta_min 4.7 _cell_measurement_theta_max 67.2 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 5.527 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.428 _exptl_absorpt_correction_T_max 0.472 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15140 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.0982 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.72 _diffrn_reflns_theta_max 67.15 _reflns_number_total 6002 _reflns_number_gt 3568 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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. H atoms bonded to O atoms of hydroxy group and water molecules were located in difference Fourier maps and refined isotropically with distance restraints of O---H = 0.85+-0.02 \%A with U~iso~ = 1.5U~eq~(N). In order to restrict the angles of the water molecules, the distances of H1WB...HW1C and H2WA...H2WA were restrained to 1.35+-0.02 \%A. ; _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^)+(0.0977P)^2^+4.0520P] 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 6002 _refine_ls_number_parameters 466 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1330 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2049 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 Cd1 Cd 0.69963(5) 0.09506(3) 0.39921(3) 0.0447(2) Uani 1 1 d . . . C1 C 0.2938(8) 0.1291(5) 0.3091(5) 0.043(2) Uani 1 1 d . . . C2 C 0.1749(8) 0.1108(5) 0.3342(5) 0.049(2) Uani 1 1 d . . . H2 H 0.1751 0.0868 0.3775 0.059 Uiso 1 1 calc R . . C3 C 0.0540(8) 0.1287(6) 0.2939(5) 0.055(2) Uani 1 1 d . . . C4 C 0.0534(9) 0.1650(6) 0.2305(6) 0.062(3) Uani 1 1 d . . . H4 H -0.0278 0.1763 0.2037 0.074 Uiso 1 1 calc R . . C5 C 0.1744(9) 0.1850(6) 0.2061(5) 0.057(3) Uani 1 1 d . . . C6 C 0.2939(9) 0.1660(5) 0.2452(5) 0.051(2) Uani 1 1 d . . . H6 H 0.3750 0.1780 0.2287 0.061 Uiso 1 1 calc R . . C7 C -0.0770(9) 0.1080(6) 0.3221(6) 0.060(3) Uani 1 1 d . . . C8 C 0.4261(8) 0.1089(5) 0.3488(5) 0.046(2) Uani 1 1 d . . . C9 C 0.7131(13) 0.4730(6) 0.5614(6) 0.082(4) Uani 1 1 d . . . H9 H 0.6803 0.4769 0.6054 0.098 Uiso 1 1 calc R . . C10 C 0.6930(15) 0.4098(6) 0.5242(7) 0.088(4) Uani 1 1 d . . . H10 H 0.6447 0.3725 0.5422 0.106 Uiso 1 1 calc R . . C11 C 0.7449(12) 0.4015(6) 0.4595(6) 0.067(3) Uani 1 1 d . . . C12 C 0.8184(14) 0.4576(6) 0.4353(7) 0.087(4) Uani 1 1 d . . . H12 H 0.8567 0.4526 0.3929 0.104 Uiso 1 1 calc R . . C13 C 0.8356(14) 0.5219(6) 0.4741(6) 0.082(4) Uani 1 1 d . . . H13 H 0.8857 0.5592 0.4573 0.099 Uiso 1 1 calc R . . C14 C 0.7224(12) 0.2690(6) 0.4451(6) 0.071(3) Uani 1 1 d . . . H14 H 0.7351 0.2577 0.4934 0.085 Uiso 1 1 calc R . . C15 C 0.6885(15) 0.2608(7) 0.3328(7) 0.091(4) Uani 1 1 d . . . H15 H 0.6735 0.2411 0.2872 0.110 Uiso 1 1 calc R . . C16 C 0.6994(16) 0.3305(7) 0.3473(7) 0.095(5) Uani 1 1 d . . . H16 H 0.6923 0.3680 0.3143 0.114 Uiso 1 1 calc R . . C17 C 0.7820(12) 0.5994(6) 0.6475(5) 0.067(3) Uani 1 1 d . . . C18 C 0.6859(14) 0.6402(7) 0.6717(6) 0.084(4) Uani 1 1 d . . . H18 H 0.6329 0.6698 0.6400 0.101 Uiso 1 1 calc R . . C19 C 0.6640(13) 0.6392(7) 0.7433(5) 0.076(3) Uani 1 1 d . . . H19 H 0.5962 0.6672 0.7591 0.091 Uiso 1 1 calc R . . C20 C 0.7429(11) 0.5967(6) 0.7902(5) 0.065(3) Uani 1 1 d . . . C21 C 0.8475(11) 0.5571(7) 0.7678(6) 0.072(3) Uani 1 1 d . . . H21 H 0.9037 0.5302 0.8004 0.086 Uiso 1 1 calc R . . C22 C 0.8678(12) 0.5580(7) 0.6962(6) 0.074(3) Uani 1 1 d . . . H22 H 0.9376 0.5314 0.6805 0.089 Uiso 1 1 calc R . . C23 C 0.5899(11) 0.5773(6) 0.8835(6) 0.073(3) Uani 1 1 d . . . H23 H 0.5101 0.5699 0.8540 0.088 Uiso 1 1 calc R . . C24 C 0.6054(10) 0.5762(6) 0.9558(5) 0.066(3) Uani 1 1 d . . . H24 H 0.5382 0.5673 0.9848 0.079 Uiso 1 1 calc R . . C25 C 0.8010(10) 0.5992(6) 0.9224(5) 0.067(3) Uani 1 1 d . . . H25 H 0.8922 0.6093 0.9232 0.080 Uiso 1 1 calc R . . C26 C 0.7803(11) 0.6628(5) 0.5346(5) 0.058(3) Uani 1 1 d . . . C27 C 0.6820(13) 0.6682(6) 0.4782(7) 0.081(4) Uani 1 1 d . . . H27 H 0.6271 0.6288 0.4652 0.098 Uiso 1 1 calc R . . C28 C 0.8594(11) 0.7224(6) 0.5535(5) 0.066(3) Uani 1 1 d . . . H28 H 0.9265 0.7192 0.5919 0.079 Uiso 1 1 calc R . . C29 C 0.8407(11) 0.7864(6) 0.5165(5) 0.065(3) Uani 1 1 d . . . H29 H 0.8942 0.8263 0.5299 0.077 Uiso 1 1 calc R . . C30 C 0.7403(11) 0.7906(6) 0.4585(5) 0.062(3) Uani 1 1 d . . . C31 C 0.6640(13) 0.7324(6) 0.4404(7) 0.085(4) Uani 1 1 d . . . H31 H 0.5976 0.7352 0.4017 0.102 Uiso 1 1 calc R . . C32 C 0.7154(14) 0.8609(7) 0.3447(6) 0.082(4) Uani 1 1 d . . . H32 H 0.7174 0.8234 0.3120 0.098 Uiso 1 1 calc R . . C33 C 0.7113(10) 0.9220(6) 0.4423(5) 0.060(3) Uani 1 1 d . . . H33 H 0.7117 0.9332 0.4904 0.072 Uiso 1 1 calc R . . C34 C 0.7038(12) 0.9325(6) 0.3300(6) 0.069(3) Uani 1 1 d . . . H34 H 0.7000 0.9526 0.2846 0.083 Uiso 1 1 calc R . . C35 C 0.7794(13) 0.5310(6) 0.5367(5) 0.069(3) Uani 1 1 d . . . N1 N 0.7989(11) 0.5974(5) 0.5738(5) 0.071(3) Uani 1 1 d . . . N2 N 0.7227(10) 0.3369(5) 0.4193(5) 0.068(3) Uani 1 1 d . . . N3 N 0.7026(9) 0.2217(4) 0.3951(5) 0.063(2) Uani 1 1 d . . . N4 N 0.7136(8) 0.5913(5) 0.8620(4) 0.059(2) Uani 1 1 d . . . N5 N 0.7394(7) 0.5908(5) 0.9791(4) 0.057(2) Uani 1 1 d . . . N6 N 0.7236(8) 0.8550(4) 0.4175(4) 0.056(2) Uani 1 1 d . . . N7 N 0.6987(7) 0.9705(4) 0.3909(4) 0.0443(17) Uani 1 1 d . . . O1 O 0.1699(7) 0.2243(5) 0.1440(4) 0.079(2) Uani 1 1 d D . . O2 O -0.1802(6) 0.1055(5) 0.2804(5) 0.086(3) Uani 1 1 d . . . O3 O -0.0732(7) 0.0983(5) 0.3878(4) 0.075(2) Uani 1 1 d . . . O4 O 0.4356(6) 0.0958(4) 0.4141(4) 0.070(2) Uani 1 1 d . . . O5 O 0.5258(5) 0.1046(4) 0.3137(3) 0.0572(17) Uani 1 1 d . . . O1W O 0.5934(10) 0.1173(9) 0.1776(5) 0.127(4) Uani 1 1 d D . . O2W O 0.4356(10) 0.2305(8) 0.1092(6) 0.128(4) Uani 1 1 d D . . H1 H 0.245(9) 0.234(11) 0.129(9) 0.192 Uiso 1 1 d D . . H1WB H 0.667(11) 0.139(10) 0.191(9) 0.192 Uiso 1 1 d D . . H1WC H 0.559(17) 0.109(11) 0.216(5) 0.192 Uiso 1 1 d D . . H2WA H 0.493(16) 0.197(8) 0.121(9) 0.192 Uiso 1 1 d D . . H2WB H 0.457(18) 0.247(9) 0.070(6) 0.192 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 Cd1 0.0398(3) 0.0497(4) 0.0431(3) 0.0005(4) -0.0018(2) 0.0012(3) C1 0.036(4) 0.047(5) 0.046(5) 0.004(4) 0.002(4) 0.006(4) C2 0.043(4) 0.057(6) 0.048(5) 0.003(4) 0.004(4) 0.001(4) C3 0.037(4) 0.063(6) 0.062(6) 0.003(5) -0.001(4) 0.002(4) C4 0.038(4) 0.083(8) 0.062(6) 0.011(6) -0.008(4) 0.013(5) C5 0.055(5) 0.068(7) 0.048(5) 0.007(5) 0.000(4) 0.011(5) C6 0.045(4) 0.060(6) 0.048(5) 0.008(5) 0.004(4) 0.000(4) C7 0.043(5) 0.066(7) 0.073(7) -0.004(6) 0.010(5) -0.005(5) C8 0.043(4) 0.046(6) 0.047(5) 0.004(4) -0.002(4) 0.006(4) C9 0.130(10) 0.053(7) 0.068(7) 0.000(6) 0.034(7) -0.025(7) C10 0.146(12) 0.043(7) 0.079(8) -0.004(7) 0.025(8) -0.018(7) C11 0.107(8) 0.035(6) 0.062(6) 0.002(6) 0.025(6) -0.015(6) C12 0.134(11) 0.057(8) 0.072(8) -0.010(6) 0.023(8) 0.000(7) C13 0.129(10) 0.054(7) 0.067(7) -0.001(6) 0.027(7) -0.018(7) C14 0.116(9) 0.034(7) 0.061(6) -0.010(5) 0.000(6) -0.005(6) C15 0.155(13) 0.056(8) 0.058(7) 0.004(6) -0.012(8) 0.000(8) C16 0.176(15) 0.049(8) 0.059(7) 0.001(6) 0.007(8) 0.002(8) C17 0.109(8) 0.045(6) 0.048(5) 0.004(5) 0.011(5) 0.008(6) C18 0.126(10) 0.068(8) 0.057(7) -0.004(6) 0.005(7) 0.034(8) C19 0.101(8) 0.079(8) 0.047(6) -0.005(6) 0.005(6) 0.030(7) C20 0.081(6) 0.071(7) 0.041(5) 0.001(6) 0.000(5) 0.018(6) C21 0.076(7) 0.081(8) 0.058(6) 0.023(6) 0.006(5) 0.001(6) C22 0.098(8) 0.076(8) 0.052(6) 0.016(6) 0.019(6) 0.018(7) C23 0.070(6) 0.097(9) 0.049(6) -0.001(6) -0.007(5) -0.008(6) C24 0.052(5) 0.092(9) 0.055(6) 0.000(6) 0.007(4) -0.016(5) C25 0.064(5) 0.088(8) 0.046(5) -0.002(6) -0.008(4) 0.010(6) C26 0.092(7) 0.032(6) 0.048(5) -0.006(4) 0.003(5) -0.004(5) C27 0.112(9) 0.040(7) 0.085(8) -0.005(6) -0.018(7) -0.024(6) C28 0.087(7) 0.058(7) 0.049(5) 0.005(5) -0.008(5) 0.003(6) C29 0.087(7) 0.052(6) 0.052(6) -0.002(5) -0.003(5) -0.003(5) C30 0.087(7) 0.051(7) 0.049(5) -0.001(5) 0.004(5) -0.004(6) C31 0.103(9) 0.062(8) 0.081(8) 0.005(7) -0.028(7) -0.025(7) C32 0.135(11) 0.066(9) 0.043(6) -0.009(6) 0.005(6) 0.007(7) C33 0.072(6) 0.063(8) 0.046(5) -0.006(5) 0.008(5) 0.000(5) C34 0.117(9) 0.045(6) 0.045(6) 0.004(5) 0.002(6) 0.003(6) C35 0.121(9) 0.039(6) 0.049(6) -0.003(5) 0.021(6) -0.003(6) N1 0.129(8) 0.033(5) 0.052(4) 0.004(4) 0.009(5) -0.009(5) N2 0.108(7) 0.040(5) 0.058(5) -0.008(4) 0.014(5) 0.000(5) N3 0.076(5) 0.040(5) 0.073(5) 0.001(5) 0.003(4) 0.003(4) N4 0.063(5) 0.064(5) 0.047(4) 0.008(4) 0.002(3) 0.005(4) N5 0.050(4) 0.075(6) 0.043(4) 0.001(4) -0.002(3) 0.000(4) N6 0.076(5) 0.045(5) 0.046(5) -0.003(4) 0.000(4) 0.004(4) N7 0.049(4) 0.036(4) 0.048(4) 0.003(4) 0.003(3) 0.012(3) O1 0.073(4) 0.107(6) 0.057(4) 0.034(5) 0.001(4) 0.007(5) O2 0.035(3) 0.128(7) 0.094(6) -0.009(5) 0.000(3) -0.003(4) O3 0.054(4) 0.110(6) 0.066(4) 0.016(5) 0.019(3) -0.002(4) O4 0.053(3) 0.099(6) 0.056(4) 0.020(4) -0.002(3) 0.014(4) O5 0.037(3) 0.082(5) 0.052(3) 0.002(4) 0.001(3) 0.006(3) O1W 0.081(6) 0.239(14) 0.062(5) -0.009(7) 0.009(4) 0.018(8) O2W 0.101(7) 0.191(13) 0.097(7) 0.050(8) 0.035(6) -0.019(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Cd1 O5 2.239(5) . ? Cd1 N5 2.309(7) 2_646 ? Cd1 O3 2.310(6) 1_655 ? Cd1 N7 2.312(7) 1_545 ? Cd1 N3 2.346(8) . ? C1 C2 1.372(12) . ? C1 C6 1.387(12) . ? C1 C8 1.492(11) . ? C2 C3 1.394(12) . ? C2 H2 0.9300 . ? C3 C4 1.372(14) . ? C3 C7 1.521(13) . ? C4 C5 1.395(14) . ? C4 H4 0.9300 . ? C5 C6 1.376(12) . ? C5 O1 1.376(12) . ? C6 H6 0.9300 . ? C7 O2 1.225(12) . ? C7 O3 1.249(13) . ? C8 O4 1.249(11) . ? C8 O5 1.262(10) . ? C9 C10 1.366(15) . ? C9 C35 1.373(15) . ? C9 H9 0.9300 . ? C10 C11 1.390(16) . ? C10 H10 0.9300 . ? C11 C12 1.382(16) . ? C11 N2 1.419(13) . ? C12 C13 1.397(16) . ? C12 H12 0.9300 . ? C13 C35 1.376(15) . ? C13 H13 0.9300 . ? C14 N3 1.285(12) . ? C14 N2 1.348(13) . ? C14 H14 0.9300 . ? C15 C16 1.320(16) . ? C15 N3 1.375(14) . ? C15 H15 0.9300 . ? C16 N2 1.358(15) . ? C16 H16 0.9300 . ? C17 C18 1.344(16) . ? C17 C22 1.410(15) . ? C17 N1 1.421(14) . ? C18 C19 1.394(15) . ? C18 H18 0.9300 . ? C19 C20 1.365(14) . ? C19 H19 0.9300 . ? C20 C21 1.383(15) . ? C20 N4 1.423(12) . ? C21 C22 1.390(15) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.355(14) . ? C23 N4 1.372(14) . ? C23 H23 0.9300 . ? C24 N5 1.389(11) . ? C24 H24 0.9300 . ? C25 N5 1.303(13) . ? C25 N4 1.363(12) . ? C25 H25 0.9300 . ? C26 C27 1.368(14) . ? C26 C28 1.380(14) . ? C26 N1 1.420(13) . ? C27 C31 1.388(16) . ? C27 H27 0.9300 . ? C28 C29 1.377(14) . ? C28 H28 0.9300 . ? C29 C30 1.401(13) . ? C29 H29 0.9300 . ? C30 C31 1.342(15) . ? C30 N6 1.420(13) . ? C31 H31 0.9300 . ? C32 C34 1.357(16) . ? C32 N6 1.372(13) . ? C32 H32 0.9300 . ? C33 N7 1.316(12) . ? C33 N6 1.337(13) . ? C33 H33 0.9300 . ? C34 N7 1.354(12) . ? C34 H34 0.9300 . ? C35 N1 1.417(13) . ? N5 Cd1 2.309(7) 2_656 ? N7 Cd1 2.312(7) 1_565 ? O1 H1 0.85(2) . ? O3 Cd1 2.310(6) 1_455 ? O1W H1WB 0.85(2) . ? O1W H1WC 0.85(2) . ? O2W H2WA 0.85(2) . ? O2W H2WB 0.85(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cd1 N5 144.4(2) . 2_646 ? O5 Cd1 O3 128.5(2) . 1_655 ? N5 Cd1 O3 86.8(3) 2_646 1_655 ? O5 Cd1 N7 91.9(2) . 1_545 ? N5 Cd1 N7 91.8(3) 2_646 1_545 ? O3 Cd1 N7 90.9(3) 1_655 1_545 ? O5 Cd1 N3 84.8(3) . . ? N5 Cd1 N3 93.7(3) 2_646 . ? O3 Cd1 N3 87.4(3) 1_655 . ? N7 Cd1 N3 174.2(3) 1_545 . ? C2 C1 C6 120.6(8) . . ? C2 C1 C8 121.4(8) . . ? C6 C1 C8 118.0(8) . . ? C1 C2 C3 119.1(9) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 120.6(9) . . ? C4 C3 C7 120.8(8) . . ? C2 C3 C7 118.6(9) . . ? C3 C4 C5 120.0(8) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 O1 122.2(9) . . ? C6 C5 C4 119.3(9) . . ? O1 C5 C4 118.5(8) . . ? C5 C6 C1 120.3(8) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? O2 C7 O3 124.0(9) . . ? O2 C7 C3 118.8(10) . . ? O3 C7 C3 117.1(9) . . ? O4 C8 O5 122.0(7) . . ? O4 C8 C1 120.3(8) . . ? O5 C8 C1 117.6(8) . . ? C10 C9 C35 122.9(11) . . ? C10 C9 H9 118.5 . . ? C35 C9 H9 118.5 . . ? C9 C10 C11 119.9(11) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 118.3(11) . . ? C12 C11 N2 120.9(10) . . ? C10 C11 N2 120.8(10) . . ? C11 C12 C13 120.4(12) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C35 C13 C12 121.1(11) . . ? C35 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? N3 C14 N2 112.2(10) . . ? N3 C14 H14 123.9 . . ? N2 C14 H14 123.9 . . ? C16 C15 N3 109.9(11) . . ? C16 C15 H15 125.1 . . ? N3 C15 H15 125.1 . . ? C15 C16 N2 107.1(11) . . ? C15 C16 H16 126.5 . . ? N2 C16 H16 126.5 . . ? C18 C17 C22 119.4(10) . . ? C18 C17 N1 121.2(10) . . ? C22 C17 N1 119.4(11) . . ? C17 C18 C19 121.3(11) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 119.5(11) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.6(10) . . ? C19 C20 N4 119.3(10) . . ? C21 C20 N4 120.0(9) . . ? C20 C21 C22 119.5(10) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C17 119.5(11) . . ? C21 C22 H22 120.2 . . ? C17 C22 H22 120.2 . . ? C24 C23 N4 107.3(9) . . ? C24 C23 H23 126.3 . . ? N4 C23 H23 126.3 . . ? C23 C24 N5 108.1(9) . . ? C23 C24 H24 126.0 . . ? N5 C24 H24 126.0 . . ? N5 C25 N4 110.8(9) . . ? N5 C25 H25 124.6 . . ? N4 C25 H25 124.6 . . ? C27 C26 C28 118.9(9) . . ? C27 C26 N1 120.5(9) . . ? C28 C26 N1 120.7(9) . . ? C26 C27 C31 120.1(10) . . ? C26 C27 H27 119.9 . . ? C31 C27 H27 119.9 . . ? C29 C28 C26 121.1(9) . . ? C29 C28 H28 119.5 . . ? C26 C28 H28 119.5 . . ? C28 C29 C30 119.2(10) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 119.3(10) . . ? C31 C30 N6 120.5(9) . . ? C29 C30 N6 120.1(9) . . ? C30 C31 C27 121.4(10) . . ? C30 C31 H31 119.3 . . ? C27 C31 H31 119.3 . . ? C34 C32 N6 106.1(10) . . ? C34 C32 H32 127.0 . . ? N6 C32 H32 127.0 . . ? N7 C33 N6 112.4(9) . . ? N7 C33 H33 123.8 . . ? N6 C33 H33 123.8 . . ? N7 C34 C32 110.1(9) . . ? N7 C34 H34 124.9 . . ? C32 C34 H34 124.9 . . ? C9 C35 C13 117.2(10) . . ? C9 C35 N1 123.7(10) . . ? C13 C35 N1 119.0(10) . . ? C35 N1 C26 118.7(8) . . ? C35 N1 C17 118.8(9) . . ? C26 N1 C17 117.7(9) . . ? C14 N2 C16 105.8(9) . . ? C14 N2 C11 126.8(9) . . ? C16 N2 C11 127.4(9) . . ? C14 N3 C15 105.1(9) . . ? C14 N3 Cd1 131.2(8) . . ? C15 N3 Cd1 123.7(8) . . ? C25 N4 C23 106.7(8) . . ? C25 N4 C20 127.4(9) . . ? C23 N4 C20 126.0(8) . . ? C25 N5 C24 107.2(8) . . ? C25 N5 Cd1 135.7(6) . 2_656 ? C24 N5 Cd1 117.1(6) . 2_656 ? C33 N6 C32 106.2(9) . . ? C33 N6 C30 126.8(8) . . ? C32 N6 C30 127.0(9) . . ? C33 N7 C34 105.2(8) . . ? C33 N7 Cd1 129.1(6) . 1_565 ? C34 N7 Cd1 125.1(7) . 1_565 ? C5 O1 H1 117(10) . . ? C7 O3 Cd1 100.3(6) . 1_455 ? C8 O5 Cd1 102.9(5) . . ? H1WB O1W H1WC 105(3) . . ? H2WA O2W H2WB 105(3) . . ? 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 C6 C1 C2 C3 1.1(14) . . . . ? C8 C1 C2 C3 -177.8(9) . . . . ? C1 C2 C3 C4 -0.9(15) . . . . ? C1 C2 C3 C7 179.9(9) . . . . ? C2 C3 C4 C5 -0.6(16) . . . . ? C7 C3 C4 C5 178.5(10) . . . . ? C3 C4 C5 C6 2.0(16) . . . . ? C3 C4 C5 O1 -177.0(10) . . . . ? O1 C5 C6 C1 177.2(10) . . . . ? C4 C5 C6 C1 -1.8(16) . . . . ? C2 C1 C6 C5 0.2(15) . . . . ? C8 C1 C6 C5 179.1(9) . . . . ? C4 C3 C7 O2 20.1(16) . . . . ? C2 C3 C7 O2 -160.8(10) . . . . ? C4 C3 C7 O3 -156.2(11) . . . . ? C2 C3 C7 O3 23.0(15) . . . . ? C2 C1 C8 O4 -22.5(14) . . . . ? C6 C1 C8 O4 158.6(9) . . . . ? C2 C1 C8 O5 156.3(9) . . . . ? C6 C1 C8 O5 -22.6(13) . . . . ? C35 C9 C10 C11 2(2) . . . . ? C9 C10 C11 C12 1(2) . . . . ? C9 C10 C11 N2 -178.6(12) . . . . ? C10 C11 C12 C13 -2(2) . . . . ? N2 C11 C12 C13 177.7(12) . . . . ? C11 C12 C13 C35 0(2) . . . . ? N3 C15 C16 N2 0.9(19) . . . . ? C22 C17 C18 C19 -4(2) . . . . ? N1 C17 C18 C19 176.3(12) . . . . ? C17 C18 C19 C20 1(2) . . . . ? C18 C19 C20 C21 3(2) . . . . ? C18 C19 C20 N4 -175.1(12) . . . . ? C19 C20 C21 C22 -3.3(19) . . . . ? N4 C20 C21 C22 174.5(11) . . . . ? C20 C21 C22 C17 0.3(19) . . . . ? C18 C17 C22 C21 3.3(19) . . . . ? N1 C17 C22 C21 -177.0(11) . . . . ? N4 C23 C24 N5 0.9(14) . . . . ? C28 C26 C27 C31 0.8(19) . . . . ? N1 C26 C27 C31 179.7(12) . . . . ? C27 C26 C28 C29 -0.1(17) . . . . ? N1 C26 C28 C29 -179.0(10) . . . . ? C26 C28 C29 C30 -0.5(17) . . . . ? C28 C29 C30 C31 0.4(17) . . . . ? C28 C29 C30 N6 -177.0(10) . . . . ? C29 C30 C31 C27 0(2) . . . . ? N6 C30 C31 C27 177.7(12) . . . . ? C26 C27 C31 C30 -1(2) . . . . ? N6 C32 C34 N7 -2.7(15) . . . . ? C10 C9 C35 C13 -5(2) . . . . ? C10 C9 C35 N1 178.8(13) . . . . ? C12 C13 C35 C9 4(2) . . . . ? C12 C13 C35 N1 -179.6(12) . . . . ? C9 C35 N1 C26 -137.5(12) . . . . ? C13 C35 N1 C26 46.0(17) . . . . ? C9 C35 N1 C17 17.1(19) . . . . ? C13 C35 N1 C17 -159.3(12) . . . . ? C27 C26 N1 C35 36.1(17) . . . . ? C28 C26 N1 C35 -145.0(11) . . . . ? C27 C26 N1 C17 -118.8(13) . . . . ? C28 C26 N1 C17 60.1(16) . . . . ? C18 C17 N1 C35 -117.2(14) . . . . ? C22 C17 N1 C35 63.0(16) . . . . ? C18 C17 N1 C26 37.7(18) . . . . ? C22 C17 N1 C26 -142.1(11) . . . . ? N3 C14 N2 C16 0.8(15) . . . . ? N3 C14 N2 C11 -178.4(11) . . . . ? C15 C16 N2 C14 -1.0(17) . . . . ? C15 C16 N2 C11 178.2(12) . . . . ? C12 C11 N2 C14 141.4(13) . . . . ? C10 C11 N2 C14 -38.7(19) . . . . ? C12 C11 N2 C16 -38(2) . . . . ? C10 C11 N2 C16 142.3(15) . . . . ? N2 C14 N3 C15 -0.2(14) . . . . ? N2 C14 N3 Cd1 176.7(7) . . . . ? C16 C15 N3 C14 -0.4(16) . . . . ? C16 C15 N3 Cd1 -177.6(10) . . . . ? O5 Cd1 N3 C14 140.2(11) . . . . ? N5 Cd1 N3 C14 -4.2(11) 2_646 . . . ? O3 Cd1 N3 C14 -90.7(11) 1_655 . . . ? N7 Cd1 N3 C14 -164(2) 1_545 . . . ? O5 Cd1 N3 C15 -43.4(10) . . . . ? N5 Cd1 N3 C15 172.2(10) 2_646 . . . ? O3 Cd1 N3 C15 85.6(10) 1_655 . . . ? N7 Cd1 N3 C15 12(3) 1_545 . . . ? N5 C25 N4 C23 0.2(13) . . . . ? N5 C25 N4 C20 180.0(10) . . . . ? C24 C23 N4 C25 -0.7(13) . . . . ? C24 C23 N4 C20 179.6(11) . . . . ? C19 C20 N4 C25 -130.5(12) . . . . ? C21 C20 N4 C25 51.7(17) . . . . ? C19 C20 N4 C23 49.2(17) . . . . ? C21 C20 N4 C23 -128.6(13) . . . . ? N4 C25 N5 C24 0.3(13) . . . . ? N4 C25 N5 Cd1 -179.3(7) . . . 2_656 ? C23 C24 N5 C25 -0.8(14) . . . . ? C23 C24 N5 Cd1 179.0(8) . . . 2_656 ? N7 C33 N6 C32 -1.3(12) . . . . ? N7 C33 N6 C30 179.3(9) . . . . ? C34 C32 N6 C33 2.3(14) . . . . ? C34 C32 N6 C30 -178.2(10) . . . . ? C31 C30 N6 C33 131.6(12) . . . . ? C29 C30 N6 C33 -51.1(15) . . . . ? C31 C30 N6 C32 -47.7(18) . . . . ? C29 C30 N6 C32 129.6(13) . . . . ? N6 C33 N7 C34 -0.3(11) . . . . ? N6 C33 N7 Cd1 -171.8(6) . . . 1_565 ? C32 C34 N7 C33 1.9(13) . . . . ? C32 C34 N7 Cd1 173.8(8) . . . 1_565 ? O2 C7 O3 Cd1 -8.3(14) . . . 1_455 ? C3 C7 O3 Cd1 167.8(8) . . . 1_455 ? O4 C8 O5 Cd1 -11.9(11) . . . . ? C1 C8 O5 Cd1 169.4(7) . . . . ? N5 Cd1 O5 C8 -0.2(9) 2_646 . . . ? O3 Cd1 O5 C8 -171.8(6) 1_655 . . . ? N7 Cd1 O5 C8 95.6(6) 1_545 . . . ? N3 Cd1 O5 C8 -89.2(6) . . . . ? 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 O2W 0.85(2) 1.99(6) 2.815(12) 163(19) . O1W H1WB O2 0.85(2) 2.23(17) 2.817(11) 126(17) 1_655 O1W H1WC O5 0.85(2) 1.92(6) 2.742(11) 164(17) . O2W H2WA O1W 0.85(2) 2.02(6) 2.843(18) 161(17) . _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.014 _refine_diff_density_min -0.928 _refine_diff_density_rms 0.115 data_compound-2 _database_code_depnum_ccdc_archive 'CCDC 810539' #TrackingRef '- CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C70 H50 Cd3 Cl2 N14 O8, 4(H2 O)' _chemical_formula_sum 'C70 H58 Cd3 Cl2 N14 O12' _chemical_formula_weight 1695.40 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' Cd Cd -0.8075 1.2024 '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 Triclinic _symmetry_space_group_name_H-M 'p -1' _symmetry_space_group_name_hall '-p 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1750(3) _cell_length_b 13.2890(4) _cell_length_c 15.7120(7) _cell_angle_alpha 109.992(3) _cell_angle_beta 94.333(3) _cell_angle_gamma 90.490(2) _cell_volume 1989.44(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7230 _cell_measurement_theta_min 4.3 _cell_measurement_theta_max 25.4 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17654 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0927 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.28 _diffrn_reflns_theta_max 25.35 _reflns_number_total 7230 _reflns_number_gt 4435 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. In order to give a reasonable O...O distance, the distance of O4...O2W was restrained to 3.15+-0.02 \%A. ; _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^)+(0.0519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7230 _refine_ls_number_parameters 457 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0958 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.929 _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 Cd1 Cd 0.5000 -0.5000 0.0000 0.03594(16) Uani 1 2 d S . . Cd2 Cd -0.20219(4) 0.58437(3) -0.16781(2) 0.03836(14) Uani 1 1 d . . . C1 C 0.2253(5) 0.0224(4) -0.3443(3) 0.0421(13) Uani 1 1 d . . . C2 C 0.2624(6) 0.0838(5) -0.2558(4) 0.0613(18) Uani 1 1 d . . . H2 H 0.3370 0.0665 -0.2263 0.074 Uiso 1 1 calc R . . C3 C 0.1912(6) 0.1710(5) -0.2095(4) 0.0607(17) Uani 1 1 d . . . H3 H 0.2170 0.2110 -0.1492 0.073 Uiso 1 1 calc R . . C4 C 0.0826(5) 0.1980(4) -0.2528(4) 0.0441(13) Uani 1 1 d . . . C5 C 0.0460(6) 0.1397(4) -0.3422(4) 0.0577(17) Uani 1 1 d . . . H5 H -0.0266 0.1591 -0.3720 0.069 Uiso 1 1 calc R . . C6 C 0.1169(6) 0.0518(4) -0.3879(4) 0.0636(18) Uani 1 1 d . . . H6 H 0.0915 0.0124 -0.4484 0.076 Uiso 1 1 calc R . . C7 C -0.0233(6) 0.3099(4) -0.1156(4) 0.0531(15) Uani 1 1 d . . . H7 H -0.0012 0.2721 -0.0768 0.064 Uiso 1 1 calc R . . C8 C -0.0918(5) 0.4006(4) -0.0965(4) 0.0488(14) Uani 1 1 d . . . H8 H -0.1241 0.4366 -0.0407 0.059 Uiso 1 1 calc R . . C9 C -0.0460(5) 0.3617(4) -0.2334(4) 0.0422(13) Uani 1 1 d . . . H9 H -0.0399 0.3642 -0.2915 0.051 Uiso 1 1 calc R . . C10 C 0.3137(5) -0.1091(4) -0.4792(3) 0.0411(13) Uani 1 1 d . . . C11 C 0.3364(6) -0.0396(4) -0.5248(4) 0.0519(15) Uani 1 1 d . . . H11 H 0.3361 0.0339 -0.4943 0.062 Uiso 1 1 calc R . . C12 C 0.3597(5) -0.0783(4) -0.6160(4) 0.0492(14) Uani 1 1 d . . . H12 H 0.3746 -0.0301 -0.6458 0.059 Uiso 1 1 calc R . . C13 C 0.3612(5) -0.1855(4) -0.6629(3) 0.0399(12) Uani 1 1 d . . . C14 C 0.3369(7) -0.2547(4) -0.6181(4) 0.0613(17) Uani 1 1 d . . . H14 H 0.3363 -0.3281 -0.6495 0.074 Uiso 1 1 calc R . . C15 C 0.3135(7) -0.2189(4) -0.5286(4) 0.0609(17) Uani 1 1 d . . . H15 H 0.2972 -0.2680 -0.5001 0.073 Uiso 1 1 calc R . . C16 C 0.3677(6) -0.1761(4) -0.8192(4) 0.0604(17) Uani 1 1 d . . . H16 H 0.3380 -0.1072 -0.8081 0.072 Uiso 1 1 calc R . . C17 C 0.4007(7) -0.2447(5) -0.8994(4) 0.0693(19) Uani 1 1 d . . . H17 H 0.3981 -0.2305 -0.9535 0.083 Uiso 1 1 calc R . . C18 C 0.4286(5) -0.3241(4) -0.8032(4) 0.0437(13) Uani 1 1 d . . . H18 H 0.4486 -0.3754 -0.7766 0.052 Uiso 1 1 calc R . . C19 C 0.2975(6) -0.1466(4) -0.3376(3) 0.0460(14) Uani 1 1 d . . . C20 C 0.4185(6) -0.1809(4) -0.3117(4) 0.0554(15) Uani 1 1 d . . . H23 H 0.4968 -0.1554 -0.3251 0.066 Uiso 1 1 calc R . . C21 C 0.4206(6) -0.2527(4) -0.2664(4) 0.0530(15) Uani 1 1 d . . . H22 H 0.5010 -0.2763 -0.2498 0.064 Uiso 1 1 calc R . . C22 C 0.3054(5) -0.2902(4) -0.2450(4) 0.0422(13) Uani 1 1 d . . . C23 C 0.1866(6) -0.2559(5) -0.2689(5) 0.0689(19) Uani 1 1 d . . . H20 H 0.1089 -0.2804 -0.2538 0.083 Uiso 1 1 calc R . . C24 C 0.1828(6) -0.1841(5) -0.3161(5) 0.0722(19) Uani 1 1 d . . . H19 H 0.1021 -0.1613 -0.3331 0.087 Uiso 1 1 calc R . . C25 C 0.2168(6) -0.4479(6) -0.2105(5) 0.076(2) Uani 1 1 d . . . H24 H 0.1405 -0.4641 -0.2499 0.092 Uiso 1 1 calc R . . C26 C 0.2585(6) -0.4996(5) -0.1548(4) 0.068(2) Uani 1 1 d . . . H25 H 0.2141 -0.5575 -0.1478 0.081 Uiso 1 1 calc R . . C27 C 0.4041(5) -0.3758(4) -0.1378(3) 0.0438(13) Uani 1 1 d . . . H26 H 0.4799 -0.3317 -0.1187 0.053 Uiso 1 1 calc R . . C28 C -0.1283(7) 0.9871(5) -0.0364(5) 0.087(2) Uani 1 1 d . . . H30 H -0.2153 0.9797 -0.0611 0.105 Uiso 1 1 calc R . . C29 C -0.0540(7) 0.8988(4) -0.0520(4) 0.0604(17) Uani 1 1 d . . . C30 C 0.0755(7) 0.9113(5) -0.0162(6) 0.088(3) Uani 1 1 d . . . H29 H 0.1278 0.8519 -0.0271 0.105 Uiso 1 1 calc R . . C31 C -0.1096(8) 0.7886(5) -0.1082(4) 0.0646(18) Uani 1 1 d . . . C32 C -0.5511(6) 0.4890(5) -0.4244(4) 0.0561(15) Uani 1 1 d . . . H34 H -0.5856 0.4808 -0.3739 0.067 Uiso 1 1 calc R . . C33 C -0.4193(6) 0.5153(4) -0.4214(3) 0.0452(14) Uani 1 1 d . . . C34 C -0.3684(6) 0.5252(5) -0.4976(4) 0.0585(16) Uani 1 1 d . . . H33 H -0.2790 0.5416 -0.4961 0.070 Uiso 1 1 calc R . . C35 C -0.3309(6) 0.5331(4) -0.3358(4) 0.0436(14) Uani 1 1 d . . . N1 N 0.2949(5) -0.0721(3) -0.3859(3) 0.0502(12) Uani 1 1 d . . . N2 N 0.0067(4) 0.2849(3) -0.2038(3) 0.0402(10) Uani 1 1 d . . . N3 N -0.1064(4) 0.4317(3) -0.1701(3) 0.0401(10) Uani 1 1 d . . . N4 N 0.3859(4) -0.2265(3) -0.7573(3) 0.0399(10) Uani 1 1 d . . . N5 N 0.4392(4) -0.3394(3) -0.8885(3) 0.0450(11) Uani 1 1 d . . . N6 N 0.3083(4) -0.3657(3) -0.1990(3) 0.0453(11) Uani 1 1 d . . . N7 N 0.3780(4) -0.4543(3) -0.1087(3) 0.0448(11) Uani 1 1 d . . . O1 O -0.0400(4) 0.7105(3) -0.1108(3) 0.0675(12) Uani 1 1 d . . . O2 O -0.2253(5) 0.7795(3) -0.1459(3) 0.0787(14) Uani 1 1 d . . . O1W O 0.7451(8) -0.1069(7) -0.2719(7) 0.197(4) Uani 1 1 d . . . O3 O -0.3846(4) 0.5343(3) -0.2660(3) 0.0491(9) Uani 1 1 d . . . O2W O -0.0008(9) 0.4341(11) -0.4320(8) 0.264(6) Uani 1 1 d D . . O4 O -0.2099(4) 0.5486(4) -0.3339(3) 0.0699(12) Uani 1 1 d D . . Cl1 Cl -0.30011(12) 0.62146(10) -0.01675(8) 0.0442(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0476(3) 0.0365(3) 0.0251(3) 0.0120(2) 0.0039(2) 0.0084(2) Cd2 0.0486(3) 0.0303(2) 0.0331(2) 0.00714(16) 0.00199(18) 0.00475(16) C1 0.059(3) 0.037(3) 0.033(3) 0.014(2) 0.007(3) 0.022(2) C2 0.067(4) 0.062(4) 0.042(4) 0.005(3) -0.011(3) 0.035(3) C3 0.072(4) 0.058(4) 0.036(3) -0.003(3) -0.006(3) 0.026(3) C4 0.050(3) 0.039(3) 0.041(3) 0.010(2) 0.006(3) 0.019(2) C5 0.071(4) 0.056(4) 0.036(3) 0.005(3) -0.008(3) 0.026(3) C6 0.085(4) 0.052(4) 0.037(3) -0.003(3) -0.008(3) 0.028(3) C7 0.072(4) 0.054(3) 0.039(3) 0.021(3) 0.015(3) 0.025(3) C8 0.063(4) 0.043(3) 0.036(3) 0.007(3) 0.012(3) 0.019(3) C9 0.049(3) 0.040(3) 0.038(3) 0.015(3) 0.004(3) 0.008(3) C10 0.057(3) 0.034(3) 0.032(3) 0.011(2) 0.005(2) 0.016(2) C11 0.090(4) 0.029(3) 0.035(3) 0.007(2) 0.008(3) 0.006(3) C12 0.075(4) 0.036(3) 0.042(3) 0.018(3) 0.017(3) 0.008(3) C13 0.051(3) 0.037(3) 0.030(3) 0.008(2) 0.007(2) 0.006(2) C14 0.118(5) 0.028(3) 0.036(3) 0.006(3) 0.023(3) 0.012(3) C15 0.113(5) 0.037(3) 0.039(3) 0.017(3) 0.025(3) 0.016(3) C16 0.101(5) 0.041(3) 0.044(4) 0.018(3) 0.019(3) 0.026(3) C17 0.123(6) 0.055(4) 0.038(4) 0.022(3) 0.022(4) 0.033(4) C18 0.059(3) 0.039(3) 0.034(3) 0.014(2) 0.007(3) 0.009(3) C19 0.070(4) 0.036(3) 0.033(3) 0.011(2) 0.014(3) 0.027(3) C20 0.055(4) 0.058(4) 0.067(4) 0.037(3) 0.017(3) 0.016(3) C21 0.053(4) 0.061(4) 0.057(4) 0.035(3) 0.006(3) 0.023(3) C22 0.051(3) 0.043(3) 0.039(3) 0.022(3) 0.006(3) 0.016(3) C23 0.059(4) 0.097(5) 0.079(5) 0.065(4) 0.013(3) 0.012(4) C24 0.058(4) 0.097(5) 0.086(5) 0.060(4) 0.016(4) 0.032(4) C25 0.063(4) 0.098(5) 0.088(5) 0.064(4) -0.025(4) -0.013(4) C26 0.063(4) 0.082(4) 0.077(5) 0.056(4) -0.019(4) -0.018(3) C27 0.051(3) 0.048(3) 0.034(3) 0.017(3) -0.002(3) 0.002(3) C28 0.078(5) 0.054(4) 0.106(6) 0.002(4) -0.015(4) -0.008(4) C29 0.088(5) 0.030(3) 0.055(4) 0.003(3) 0.007(3) -0.016(3) C30 0.085(5) 0.041(4) 0.121(7) 0.010(4) -0.008(5) 0.000(3) C31 0.100(5) 0.045(4) 0.050(4) 0.015(3) 0.022(4) -0.018(4) C32 0.069(4) 0.069(4) 0.030(3) 0.015(3) 0.006(3) 0.000(3) C33 0.063(4) 0.044(3) 0.027(3) 0.011(2) 0.004(3) 0.007(3) C34 0.054(4) 0.081(4) 0.043(4) 0.025(3) 0.002(3) -0.003(3) C35 0.063(4) 0.029(3) 0.036(3) 0.008(2) 0.002(3) 0.009(3) N1 0.085(3) 0.039(2) 0.032(3) 0.017(2) 0.013(2) 0.029(2) N2 0.052(3) 0.029(2) 0.036(3) 0.0061(19) 0.003(2) 0.0100(19) N3 0.047(3) 0.035(2) 0.036(3) 0.009(2) 0.004(2) 0.0110(19) N4 0.058(3) 0.029(2) 0.030(2) 0.0059(19) 0.011(2) 0.0083(19) N5 0.060(3) 0.042(3) 0.033(3) 0.011(2) 0.010(2) 0.008(2) N6 0.056(3) 0.052(3) 0.035(3) 0.024(2) 0.004(2) 0.012(2) N7 0.057(3) 0.045(3) 0.038(3) 0.022(2) 0.002(2) 0.007(2) O1 0.081(3) 0.034(2) 0.077(3) 0.003(2) 0.021(2) -0.003(2) O2 0.105(4) 0.049(3) 0.075(3) 0.018(2) -0.020(3) -0.016(2) O1W 0.202(8) 0.204(8) 0.245(10) 0.180(8) -0.092(7) -0.043(6) O3 0.059(2) 0.053(2) 0.034(2) 0.0146(18) -0.0008(19) 0.0071(18) O2W 0.144(7) 0.439(18) 0.256(13) 0.172(13) 0.054(8) 0.068(9) O4 0.068(3) 0.098(3) 0.041(2) 0.023(2) -0.007(2) -0.004(2) Cl1 0.0524(8) 0.0436(7) 0.0335(7) 0.0088(6) 0.0072(6) 0.0003(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 Cd1 N7 2.286(4) 2_645 ? Cd1 N7 2.286(4) . ? Cd1 N5 2.374(4) 2_644 ? Cd1 N5 2.374(4) 1_556 ? Cd1 Cl1 2.6695(13) 1_645 ? Cd1 Cl1 2.6695(13) 2 ? Cd2 O1 2.245(4) . ? Cd2 N3 2.249(4) . ? Cd2 O3 2.261(3) . ? Cd2 O4 2.483(4) . ? Cd2 O2 2.512(4) . ? Cd2 Cl1 2.5367(14) . ? Cd2 C31 2.686(6) . ? Cd2 C35 2.716(5) . ? C1 C2 1.372(7) . ? C1 C6 1.385(7) . ? C1 N1 1.424(6) . ? C2 C3 1.383(7) . ? C2 H2 0.9300 . ? C3 C4 1.370(7) . ? C3 H3 0.9300 . ? C4 C5 1.372(7) . ? C4 N2 1.421(6) . ? C5 C6 1.385(7) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.352(7) . ? C7 N2 1.369(7) . ? C7 H7 0.9300 . ? C8 N3 1.354(7) . ? C8 H8 0.9300 . ? C9 N3 1.304(6) . ? C9 N2 1.358(6) . ? C9 H9 0.9300 . ? C10 C11 1.376(7) . ? C10 C15 1.399(7) . ? C10 N1 1.407(6) . ? C11 C12 1.387(7) . ? C11 H11 0.9300 . ? C12 C13 1.363(7) . ? C12 H12 0.9300 . ? C13 C14 1.366(7) . ? C13 N4 1.438(6) . ? C14 C15 1.362(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.348(8) . ? C16 N4 1.359(7) . ? C16 H16 0.9300 . ? C17 N5 1.383(7) . ? C17 H17 0.9300 . ? C18 N5 1.298(6) . ? C18 N4 1.345(6) . ? C18 H18 0.9300 . ? C19 C24 1.375(8) . ? C19 C20 1.396(7) . ? C19 N1 1.438(7) . ? C20 C21 1.371(7) . ? C20 H23 0.9300 . ? C21 C22 1.378(8) . ? C21 H22 0.9300 . ? C22 C23 1.366(7) . ? C22 N6 1.422(6) . ? C23 C24 1.394(8) . ? C23 H20 0.9300 . ? C24 H19 0.9300 . ? C25 C26 1.335(8) . ? C25 N6 1.384(7) . ? C25 H24 0.9300 . ? C26 N7 1.386(7) . ? C26 H25 0.9300 . ? C27 N7 1.308(6) . ? C27 N6 1.356(6) . ? C27 H26 0.9300 . ? C28 C29 1.363(9) . ? C28 C30 1.397(8) 2_575 ? C28 H30 0.9300 . ? C29 C30 1.378(9) . ? C29 C31 1.507(8) . ? C30 C28 1.397(8) 2_575 ? C30 H29 0.9300 . ? C31 O1 1.253(8) . ? C31 O2 1.262(8) . ? C32 C33 1.376(8) . ? C32 C34 1.377(7) 2_464 ? C32 H34 0.9300 . ? C33 C34 1.385(8) . ? C33 C35 1.507(7) . ? C34 C32 1.377(7) 2_464 ? C34 H33 0.9300 . ? C35 O4 1.243(7) . ? C35 O3 1.256(6) . ? N5 Cd1 2.374(4) 1_554 ? Cl1 Cd1 2.6695(13) 1_465 ? 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 Cd1 N7 180 2_645 . ? N7 Cd1 N5 89.29(15) 2_645 2_644 ? N7 Cd1 N5 90.71(15) . 2_644 ? N7 Cd1 N5 90.71(15) 2_645 1_556 ? N7 Cd1 N5 89.29(15) . 1_556 ? N5 Cd1 N5 180 2_644 1_556 ? N7 Cd1 Cl1 91.36(12) 2_645 1_645 ? N7 Cd1 Cl1 88.64(12) . 1_645 ? N5 Cd1 Cl1 95.80(11) 2_644 1_645 ? N5 Cd1 Cl1 84.20(11) 1_556 1_645 ? N7 Cd1 Cl1 88.64(12) 2_645 2 ? N7 Cd1 Cl1 91.36(12) . 2 ? N5 Cd1 Cl1 84.20(11) 2_644 2 ? N5 Cd1 Cl1 95.80(11) 1_556 2 ? Cl1 Cd1 Cl1 180 1_645 2 ? O1 Cd2 N3 104.11(16) . . ? O1 Cd2 O3 144.24(16) . . ? N3 Cd2 O3 105.97(13) . . ? O1 Cd2 O4 103.33(16) . . ? N3 Cd2 O4 96.58(15) . . ? O3 Cd2 O4 54.48(14) . . ? O1 Cd2 O2 55.23(15) . . ? N3 Cd2 O2 159.29(15) . . ? O3 Cd2 O2 93.16(14) . . ? O4 Cd2 O2 88.03(15) . . ? O1 Cd2 Cl1 94.26(12) . . ? N3 Cd2 Cl1 96.07(12) . . ? O3 Cd2 Cl1 101.29(11) . . ? O4 Cd2 Cl1 155.07(11) . . ? O2 Cd2 Cl1 87.67(12) . . ? O1 Cd2 C31 27.62(19) . . ? N3 Cd2 C31 131.6(2) . . ? O3 Cd2 C31 120.3(2) . . ? O4 Cd2 C31 98.92(18) . . ? O2 Cd2 C31 27.85(18) . . ? Cl1 Cd2 C31 88.48(14) . . ? O1 Cd2 C35 125.06(18) . . ? N3 Cd2 C35 103.85(14) . . ? O3 Cd2 C35 27.33(15) . . ? O4 Cd2 C35 27.20(15) . . ? O2 Cd2 C35 89.45(14) . . ? Cl1 Cd2 C35 128.20(15) . . ? C31 Cd2 C35 110.64(19) . . ? C2 C1 C6 118.4(5) . . ? C2 C1 N1 118.9(4) . . ? C6 C1 N1 122.6(4) . . ? C1 C2 C3 121.3(5) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 119.7(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 N2 119.4(5) . . ? C5 C4 N2 120.6(4) . . ? C4 C5 C6 120.1(5) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 120.5(5) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 N2 105.9(5) . . ? C8 C7 H7 127.0 . . ? N2 C7 H7 127.0 . . ? C7 C8 N3 110.3(5) . . ? C7 C8 H8 124.8 . . ? N3 C8 H8 124.8 . . ? N3 C9 N2 111.3(5) . . ? N3 C9 H9 124.3 . . ? N2 C9 H9 124.3 . . ? C11 C10 C15 117.5(5) . . ? C11 C10 N1 121.8(4) . . ? C15 C10 N1 120.8(5) . . ? C10 C11 C12 120.6(5) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 121.3(5) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 118.3(5) . . ? C12 C13 N4 121.8(5) . . ? C14 C13 N4 120.0(4) . . ? C15 C14 C13 121.7(5) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C10 120.8(5) . . ? C14 C15 H15 119.6 . . ? C10 C15 H15 119.6 . . ? C17 C16 N4 107.2(5) . . ? C17 C16 H16 126.4 . . ? N4 C16 H16 126.4 . . ? C16 C17 N5 109.2(5) . . ? C16 C17 H17 125.4 . . ? N5 C17 H17 125.4 . . ? N5 C18 N4 113.1(5) . . ? N5 C18 H18 123.5 . . ? N4 C18 H18 123.5 . . ? C24 C19 C20 119.5(5) . . ? C24 C19 N1 121.0(5) . . ? C20 C19 N1 119.5(6) . . ? C21 C20 C19 119.3(6) . . ? C21 C20 H23 120.3 . . ? C19 C20 H23 120.3 . . ? C20 C21 C22 121.1(5) . . ? C20 C21 H22 119.5 . . ? C22 C21 H22 119.5 . . ? C23 C22 C21 120.0(5) . . ? C23 C22 N6 119.3(5) . . ? C21 C22 N6 120.7(4) . . ? C22 C23 C24 119.6(6) . . ? C22 C23 H20 120.2 . . ? C24 C23 H20 120.2 . . ? C19 C24 C23 120.5(5) . . ? C19 C24 H19 119.7 . . ? C23 C24 H19 119.7 . . ? C26 C25 N6 107.3(5) . . ? C26 C25 H24 126.4 . . ? N6 C25 H24 126.4 . . ? C25 C26 N7 109.8(5) . . ? C25 C26 H25 125.1 . . ? N7 C26 H25 125.1 . . ? N7 C27 N6 112.5(5) . . ? N7 C27 H26 123.8 . . ? N6 C27 H26 123.8 . . ? C29 C28 C30 120.9(6) . 2_575 ? C29 C28 H30 119.6 . . ? C30 C28 H30 119.6 2_575 . ? C28 C29 C30 118.9(5) . . ? C28 C29 C31 121.5(6) . . ? C30 C29 C31 119.6(6) . . ? C29 C30 C28 120.2(6) . 2_575 ? C29 C30 H29 119.9 . . ? C28 C30 H29 119.9 2_575 . ? O1 C31 O2 123.7(5) . . ? O1 C31 C29 117.4(7) . . ? O2 C31 C29 118.7(7) . . ? O1 C31 Cd2 56.2(3) . . ? O2 C31 Cd2 68.4(3) . . ? C29 C31 Cd2 165.4(5) . . ? C33 C32 C34 119.7(6) . 2_464 ? C33 C32 H34 120.1 . . ? C34 C32 H34 120.1 2_464 . ? C32 C33 C34 119.6(5) . . ? C32 C33 C35 120.1(5) . . ? C34 C33 C35 120.3(5) . . ? C32 C34 C33 120.6(5) 2_464 . ? C32 C34 H33 119.7 2_464 . ? C33 C34 H33 119.7 . . ? O4 C35 O3 121.5(5) . . ? O4 C35 C33 121.0(6) . . ? O3 C35 C33 117.5(5) . . ? O4 C35 Cd2 65.9(3) . . ? O3 C35 Cd2 55.7(2) . . ? C33 C35 Cd2 171.0(4) . . ? C10 N1 C1 122.1(4) . . ? C10 N1 C19 119.4(4) . . ? C1 N1 C19 114.2(4) . . ? C9 N2 C7 106.4(4) . . ? C9 N2 C4 127.1(5) . . ? C7 N2 C4 126.5(4) . . ? C9 N3 C8 106.0(4) . . ? C9 N3 Cd2 130.7(4) . . ? C8 N3 Cd2 123.0(3) . . ? C18 N4 C16 105.8(4) . . ? C18 N4 C13 126.9(4) . . ? C16 N4 C13 127.3(4) . . ? C18 N5 C17 104.8(4) . . ? C18 N5 Cd1 126.4(3) . 1_554 ? C17 N5 Cd1 128.8(4) . 1_554 ? C27 N6 C25 105.3(4) . . ? C27 N6 C22 127.5(5) . . ? C25 N6 C22 127.1(4) . . ? C27 N7 C26 105.1(4) . . ? C27 N7 Cd1 126.8(3) . . ? C26 N7 Cd1 128.1(3) . . ? C31 O1 Cd2 96.2(4) . . ? C31 O2 Cd2 83.8(4) . . ? C35 O3 Cd2 97.0(3) . . ? C35 O4 Cd2 86.9(3) . . ? Cd2 Cl1 Cd1 121.13(4) . 1_465 ? 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 C6 C1 C2 C3 2.4(10) . . . . ? N1 C1 C2 C3 -174.2(6) . . . . ? C1 C2 C3 C4 -1.1(11) . . . . ? C2 C3 C4 C5 -0.9(10) . . . . ? C2 C3 C4 N2 177.4(6) . . . . ? C3 C4 C5 C6 1.5(10) . . . . ? N2 C4 C5 C6 -176.7(6) . . . . ? C2 C1 C6 C5 -1.7(10) . . . . ? N1 C1 C6 C5 174.7(6) . . . . ? C4 C5 C6 C1 -0.2(10) . . . . ? N2 C7 C8 N3 0.8(6) . . . . ? C15 C10 C11 C12 -0.8(8) . . . . ? N1 C10 C11 C12 177.5(5) . . . . ? C10 C11 C12 C13 -0.2(9) . . . . ? C11 C12 C13 C14 1.0(8) . . . . ? C11 C12 C13 N4 -179.6(5) . . . . ? C12 C13 C14 C15 -0.9(9) . . . . ? N4 C13 C14 C15 179.8(5) . . . . ? C13 C14 C15 C10 -0.1(10) . . . . ? C11 C10 C15 C14 0.9(9) . . . . ? N1 C10 C15 C14 -177.4(6) . . . . ? N4 C16 C17 N5 0.4(8) . . . . ? C24 C19 C20 C21 1.0(9) . . . . ? N1 C19 C20 C21 -179.5(5) . . . . ? C19 C20 C21 C22 -0.8(9) . . . . ? C20 C21 C22 C23 -0.1(9) . . . . ? C20 C21 C22 N6 179.2(5) . . . . ? C21 C22 C23 C24 0.9(10) . . . . ? N6 C22 C23 C24 -178.4(6) . . . . ? C20 C19 C24 C23 -0.1(10) . . . . ? N1 C19 C24 C23 -179.7(6) . . . . ? C22 C23 C24 C19 -0.8(11) . . . . ? N6 C25 C26 N7 -1.7(8) . . . . ? C30 C28 C29 C30 -1.0(13) 2_575 . . . ? C30 C28 C29 C31 179.8(7) 2_575 . . . ? C28 C29 C30 C28 1.0(13) . . . 2_575 ? C31 C29 C30 C28 -179.8(7) . . . 2_575 ? C28 C29 C31 O1 -172.1(7) . . . . ? C30 C29 C31 O1 8.7(9) . . . . ? C28 C29 C31 O2 4.2(10) . . . . ? C30 C29 C31 O2 -175.0(7) . . . . ? C28 C29 C31 Cd2 -112(2) . . . . ? C30 C29 C31 Cd2 69(2) . . . . ? N3 Cd2 C31 O1 5.4(5) . . . . ? O3 Cd2 C31 O1 -155.6(3) . . . . ? O4 Cd2 C31 O1 -101.7(4) . . . . ? O2 Cd2 C31 O1 -169.9(6) . . . . ? Cl1 Cd2 C31 O1 102.2(4) . . . . ? C35 Cd2 C31 O1 -127.2(4) . . . . ? O1 Cd2 C31 O2 169.9(6) . . . . ? N3 Cd2 C31 O2 175.3(3) . . . . ? O3 Cd2 C31 O2 14.3(5) . . . . ? O4 Cd2 C31 O2 68.2(4) . . . . ? Cl1 Cd2 C31 O2 -87.9(4) . . . . ? C35 Cd2 C31 O2 42.7(4) . . . . ? O1 Cd2 C31 C29 -68(2) . . . . ? N3 Cd2 C31 C29 -63(2) . . . . ? O3 Cd2 C31 C29 136(2) . . . . ? O4 Cd2 C31 C29 -170(2) . . . . ? O2 Cd2 C31 C29 122(2) . . . . ? Cl1 Cd2 C31 C29 34(2) . . . . ? C35 Cd2 C31 C29 165(2) . . . . ? C34 C32 C33 C34 -1.3(10) 2_464 . . . ? C34 C32 C33 C35 178.9(5) 2_464 . . . ? C32 C33 C34 C32 1.3(10) . . . 2_464 ? C35 C33 C34 C32 -178.9(5) . . . 2_464 ? C32 C33 C35 O4 174.3(5) . . . . ? C34 C33 C35 O4 -5.5(8) . . . . ? C32 C33 C35 O3 -7.5(7) . . . . ? C34 C33 C35 O3 172.6(5) . . . . ? C32 C33 C35 Cd2 -47(3) . . . . ? C34 C33 C35 Cd2 133(2) . . . . ? O1 Cd2 C35 O4 41.5(4) . . . . ? N3 Cd2 C35 O4 -77.2(3) . . . . ? O3 Cd2 C35 O4 -175.3(5) . . . . ? O2 Cd2 C35 O4 86.8(3) . . . . ? Cl1 Cd2 C35 O4 173.4(3) . . . . ? C31 Cd2 C35 O4 68.3(4) . . . . ? O1 Cd2 C35 O3 -143.3(3) . . . . ? N3 Cd2 C35 O3 98.1(3) . . . . ? O4 Cd2 C35 O3 175.3(5) . . . . ? O2 Cd2 C35 O3 -98.0(3) . . . . ? Cl1 Cd2 C35 O3 -11.4(3) . . . . ? C31 Cd2 C35 O3 -116.4(3) . . . . ? O1 Cd2 C35 C33 -100(3) . . . . ? N3 Cd2 C35 C33 141(3) . . . . ? O3 Cd2 C35 C33 43(2) . . . . ? O4 Cd2 C35 C33 -142(3) . . . . ? O2 Cd2 C35 C33 -55(3) . . . . ? Cl1 Cd2 C35 C33 32(3) . . . . ? C31 Cd2 C35 C33 -73(3) . . . . ? C11 C10 N1 C1 36.8(8) . . . . ? C15 C10 N1 C1 -144.9(5) . . . . ? C11 C10 N1 C19 -167.8(5) . . . . ? C15 C10 N1 C19 10.5(8) . . . . ? C2 C1 N1 C10 -147.5(6) . . . . ? C6 C1 N1 C10 36.1(8) . . . . ? C2 C1 N1 C19 55.9(7) . . . . ? C6 C1 N1 C19 -120.5(6) . . . . ? C24 C19 N1 C10 -102.7(7) . . . . ? C20 C19 N1 C10 77.8(7) . . . . ? C24 C19 N1 C1 54.6(7) . . . . ? C20 C19 N1 C1 -125.0(5) . . . . ? N3 C9 N2 C7 -0.2(6) . . . . ? N3 C9 N2 C4 -177.9(4) . . . . ? C8 C7 N2 C9 -0.4(6) . . . . ? C8 C7 N2 C4 177.4(5) . . . . ? C3 C4 N2 C9 138.4(6) . . . . ? C5 C4 N2 C9 -43.3(8) . . . . ? C3 C4 N2 C7 -38.9(8) . . . . ? C5 C4 N2 C7 139.4(6) . . . . ? N2 C9 N3 C8 0.7(6) . . . . ? N2 C9 N3 Cd2 175.1(3) . . . . ? C7 C8 N3 C9 -0.9(6) . . . . ? C7 C8 N3 Cd2 -175.8(4) . . . . ? O1 Cd2 N3 C9 -90.7(4) . . . . ? O3 Cd2 N3 C9 69.7(5) . . . . ? O4 Cd2 N3 C9 14.8(4) . . . . ? O2 Cd2 N3 C9 -87.2(6) . . . . ? Cl1 Cd2 N3 C9 173.3(4) . . . . ? C31 Cd2 N3 C9 -93.3(5) . . . . ? C35 Cd2 N3 C9 41.5(5) . . . . ? O1 Cd2 N3 C8 82.8(4) . . . . ? O3 Cd2 N3 C8 -116.7(4) . . . . ? O4 Cd2 N3 C8 -171.6(4) . . . . ? O2 Cd2 N3 C8 86.4(6) . . . . ? Cl1 Cd2 N3 C8 -13.1(4) . . . . ? C31 Cd2 N3 C8 80.2(5) . . . . ? C35 Cd2 N3 C8 -144.9(4) . . . . ? N5 C18 N4 C16 0.1(6) . . . . ? N5 C18 N4 C13 178.5(4) . . . . ? C17 C16 N4 C18 -0.3(7) . . . . ? C17 C16 N4 C13 -178.7(5) . . . . ? C12 C13 N4 C18 158.4(5) . . . . ? C14 C13 N4 C18 -22.3(8) . . . . ? C12 C13 N4 C16 -23.5(8) . . . . ? C14 C13 N4 C16 155.8(6) . . . . ? N4 C18 N5 C17 0.1(6) . . . . ? N4 C18 N5 Cd1 -176.8(3) . . . 1_554 ? C16 C17 N5 C18 -0.3(7) . . . . ? C16 C17 N5 Cd1 176.5(4) . . . 1_554 ? N7 C27 N6 C25 -2.0(7) . . . . ? N7 C27 N6 C22 -179.2(5) . . . . ? C26 C25 N6 C27 2.2(8) . . . . ? C26 C25 N6 C22 179.4(6) . . . . ? C23 C22 N6 C27 -149.5(6) . . . . ? C21 C22 N6 C27 31.3(8) . . . . ? C23 C22 N6 C25 33.9(9) . . . . ? C21 C22 N6 C25 -145.3(6) . . . . ? N6 C27 N7 C26 1.0(7) . . . . ? N6 C27 N7 Cd1 -176.4(3) . . . . ? C25 C26 N7 C27 0.5(8) . . . . ? C25 C26 N7 Cd1 177.8(5) . . . . ? N7 Cd1 N7 C27 156(87) 2_645 . . . ? N5 Cd1 N7 C27 -111.0(5) 2_644 . . . ? N5 Cd1 N7 C27 69.0(5) 1_556 . . . ? Cl1 Cd1 N7 C27 -15.2(5) 1_645 . . . ? Cl1 Cd1 N7 C27 164.8(5) 2 . . . ? N7 Cd1 N7 C26 -21(87) 2_645 . . . ? N5 Cd1 N7 C26 72.2(5) 2_644 . . . ? N5 Cd1 N7 C26 -107.8(5) 1_556 . . . ? Cl1 Cd1 N7 C26 168.0(5) 1_645 . . . ? Cl1 Cd1 N7 C26 -12.0(5) 2 . . . ? O2 C31 O1 Cd2 -11.3(7) . . . . ? C29 C31 O1 Cd2 164.8(5) . . . . ? N3 Cd2 O1 C31 -175.8(4) . . . . ? O3 Cd2 O1 C31 37.6(5) . . . . ? O4 Cd2 O1 C31 83.7(4) . . . . ? O2 Cd2 O1 C31 5.7(4) . . . . ? Cl1 Cd2 O1 C31 -78.5(4) . . . . ? C35 Cd2 O1 C31 65.6(4) . . . . ? O1 C31 O2 Cd2 10.1(6) . . . . ? C29 C31 O2 Cd2 -165.9(5) . . . . ? O1 Cd2 O2 C31 -5.7(4) . . . . ? N3 Cd2 O2 C31 -9.9(7) . . . . ? O3 Cd2 O2 C31 -167.7(4) . . . . ? O4 Cd2 O2 C31 -113.4(4) . . . . ? Cl1 Cd2 O2 C31 91.2(4) . . . . ? C35 Cd2 O2 C31 -140.6(4) . . . . ? O4 C35 O3 Cd2 5.1(5) . . . . ? C33 C35 O3 Cd2 -173.1(4) . . . . ? O1 Cd2 O3 C35 56.9(4) . . . . ? N3 Cd2 O3 C35 -89.3(3) . . . . ? O4 Cd2 O3 C35 -2.6(3) . . . . ? O2 Cd2 O3 C35 82.7(3) . . . . ? Cl1 Cd2 O3 C35 170.9(3) . . . . ? C31 Cd2 O3 C35 76.0(3) . . . . ? O3 C35 O4 Cd2 -4.6(5) . . . . ? C33 C35 O4 Cd2 173.5(4) . . . . ? O1 Cd2 O4 C35 -146.2(3) . . . . ? N3 Cd2 O4 C35 107.6(3) . . . . ? O3 Cd2 O4 C35 2.7(3) . . . . ? O2 Cd2 O4 C35 -92.6(3) . . . . ? Cl1 Cd2 O4 C35 -12.5(5) . . . . ? C31 Cd2 O4 C35 -118.4(3) . . . . ? O1 Cd2 Cl1 Cd1 -174.93(13) . . . 1_465 ? N3 Cd2 Cl1 Cd1 -70.23(11) . . . 1_465 ? O3 Cd2 Cl1 Cd1 37.43(11) . . . 1_465 ? O4 Cd2 Cl1 Cd1 49.9(3) . . . 1_465 ? O2 Cd2 Cl1 Cd1 130.20(12) . . . 1_465 ? C31 Cd2 Cl1 Cd1 158.05(19) . . . 1_465 ? C35 Cd2 Cl1 Cd1 42.73(14) . . . 1_465 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.936 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.086