# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_paper _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #TrackingRef '- CC_COM_07_2012_035543.cif' _publ_contact_author ; Prof St\'ephane Baudron Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; _publ_contact_author_email hosseini@unistra.fr _publ_contact_author_fax '33 3 68 85 13 23' _publ_contact_author_phone '33 3 68 85 13 25' _publ_requested_category FM loop_ _publ_author_name _publ_author_address A.Beziau ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; S.A.Baudron ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; D.Pogozhev ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; A.Fluck ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; M.W.Hosseini ; Laboratoire de Chimie de Coordination Organique, UMR CNRS 7140, Universit\'e de Strasbourg, CS 90032 F-67081 Strasbourg Cedex, France ; _publ_section_title ; Stepwise construction of grid-type Cu(II)/Cd(II) heterometallic MOFs based on an imidazole-appended dipyrrin ligand ; _publ_contact_author_name 'Prof Stephane Baudron' ###Material relevant to compound 2 at 173K ######## data_compound2 _database_code_depnum_ccdc_archive 'CCDC 894060' #TrackingRef '- CC_COM_07_2012_035543.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H26 Cu N8), 3(C H Cl3)' _chemical_formula_sum 'C75 H55 Cl9 Cu2 N16' _chemical_formula_weight 1626.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.4262(12) _cell_length_b 8.9610(3) _cell_length_c 28.2529(16) _cell_angle_alpha 90.00 _cell_angle_beta 130.2960(10) _cell_angle_gamma 90.00 _cell_volume 7227.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4897 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 26.84 _exptl_crystal_description plate _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3311 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8916 _exptl_absorpt_correction_T_max 0.9619 _exptl_absorpt_process_details sadabs _exptl_special_details ; One chloroform molecule shows disorder. This has been modeled over tow position. The other chloroform molecule lies on a mirror. Its hydrogen atom has not been introduced but has been taken into account in the formula sum. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21262 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8279 _reflns_number_gt 6291 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0664P)^2^+35.2259P] 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 8279 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1668 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.11996(14) 0.9681(4) 0.22293(18) 0.0317(8) Uani 1 1 d . . . H1 H 0.0961 1.0349 0.1950 0.038 Uiso 1 1 calc R . . C2 C 0.13570(14) 0.9394(5) 0.28271(19) 0.0356(9) Uani 1 1 d . . . H2 H 0.1245 0.9820 0.3010 0.043 Uiso 1 1 calc R . . C3 C 0.17094(13) 0.8357(4) 0.30869(17) 0.0306(8) Uani 1 1 d . . . H3 H 0.1886 0.7956 0.3484 0.037 Uiso 1 1 calc R . . C4 C 0.17532(11) 0.8014(4) 0.26354(15) 0.0230(7) Uani 1 1 d . . . C5 C 0.20679(11) 0.7004(4) 0.26969(16) 0.0235(7) Uani 1 1 d . . . C6 C 0.21058(11) 0.6713(4) 0.22465(15) 0.0222(7) Uani 1 1 d . . . C7 C 0.24195(12) 0.5716(4) 0.22888(17) 0.0268(7) Uani 1 1 d . . . H7 H 0.2633 0.5086 0.2620 0.032 Uiso 1 1 calc R . . C8 C 0.23515(13) 0.5850(4) 0.17512(18) 0.0331(8) Uani 1 1 d . . . H8 H 0.2512 0.5348 0.1650 0.040 Uiso 1 1 calc R . . C9 C 0.19891(12) 0.6903(4) 0.13839(17) 0.0272(7) Uani 1 1 d . . . H9 H 0.1870 0.7198 0.0990 0.033 Uiso 1 1 calc R . . C10 C 0.23781(12) 0.6178(4) 0.32969(16) 0.0239(7) Uani 1 1 d . . . C11 C 0.21876(13) 0.5068(5) 0.34176(18) 0.0379(10) Uani 1 1 d . . . H11 H 0.1876 0.4796 0.3112 0.045 Uiso 1 1 calc R . . C12 C 0.24586(13) 0.4364(5) 0.39895(19) 0.0381(10) Uani 1 1 d . . . H12 H 0.2331 0.3613 0.4067 0.046 Uiso 1 1 calc R . . C13 C 0.29207(12) 0.4786(4) 0.44442(16) 0.0256(7) Uani 1 1 d . . . C14 C 0.31189(12) 0.5853(4) 0.43276(16) 0.0290(8) Uani 1 1 d . . . H14 H 0.3433 0.6109 0.4633 0.035 Uiso 1 1 calc R . . C15 C 0.28481(12) 0.6549(4) 0.37515(16) 0.0271(7) Uani 1 1 d . . . H15 H 0.2982 0.7265 0.3670 0.033 Uiso 1 1 calc R . . C16 C 0.30199(16) 0.3763(5) 0.5343(2) 0.0440(11) Uani 1 1 d . . . H16 H 0.2713 0.3907 0.5182 0.053 Uiso 1 1 calc R . . C17 C 0.37609(19) 0.3169(6) 0.5955(2) 0.0551(8) Uani 1 1 d . . . H17 H 0.4055 0.2826 0.6297 0.066 Uiso 1 1 calc R . . C18 C 0.36509(14) 0.3725(5) 0.54415(18) 0.0393(10) Uani 1 1 d . . . H18 H 0.3855 0.3833 0.5362 0.047 Uiso 1 1 calc R . . C19 C 0.08576(12) 0.7016(4) 0.02373(16) 0.0252(7) Uani 1 1 d . . . H19 H 0.1045 0.6194 0.0466 0.030 Uiso 1 1 calc R . . C20 C 0.04549(13) 0.6959(4) -0.03930(17) 0.0300(8) Uani 1 1 d . . . H20 H 0.0331 0.6121 -0.0648 0.036 Uiso 1 1 calc R . . C21 C 0.02792(12) 0.8392(4) -0.05584(16) 0.0273(7) Uani 1 1 d . . . H21 H 0.0012 0.8706 -0.0947 0.033 Uiso 1 1 calc R . . C22 C 0.05827(11) 0.9294(4) -0.00251(15) 0.0201(6) Uani 1 1 d . . . C23 C 0.05556(11) 1.0845(4) 0.00273(15) 0.0211(7) Uani 1 1 d . . . C24 C 0.08443(11) 1.1651(4) 0.05781(15) 0.0211(7) Uani 1 1 d . . . C25 C 0.08961(12) 1.3233(4) 0.06491(17) 0.0268(7) Uani 1 1 d . . . H25 H 0.0725 1.3938 0.0334 0.032 Uiso 1 1 calc R . . C26 C 0.12464(13) 1.3519(4) 0.12714(17) 0.0285(8) Uani 1 1 d . . . H26 H 0.1361 1.4451 0.1457 0.034 Uiso 1 1 calc R . . C27 C 0.13961(12) 1.2133(4) 0.15698(17) 0.0255(7) Uani 1 1 d . . . H27 H 0.1628 1.2007 0.1996 0.031 Uiso 1 1 calc R . . C28 C 0.02092(11) 1.1703(4) -0.05502(15) 0.0211(7) Uani 1 1 d . . . C29 C -0.01131(12) 1.2648(4) -0.06043(17) 0.0258(7) Uani 1 1 d . . . H29 H -0.0124 1.2687 -0.0285 0.031 Uiso 1 1 calc R . . C30 C -0.04149(12) 1.3526(4) -0.11252(17) 0.0286(8) Uani 1 1 d . . . H30 H -0.0630 1.4138 -0.1157 0.034 Uiso 1 1 calc R . . C31 C -0.03969(11) 1.3496(4) -0.15971(16) 0.0257(7) Uani 1 1 d . . . C32 C -0.00819(13) 1.2558(4) -0.15550(17) 0.0306(8) Uani 1 1 d . . . H32 H -0.0069 1.2537 -0.1873 0.037 Uiso 1 1 calc R . . C33 C 0.02134(13) 1.1655(4) -0.10393(17) 0.0292(8) Uani 1 1 d . . . H33 H 0.0417 1.1008 -0.1019 0.035 Uiso 1 1 calc R . . C34 C -0.08721(14) 1.4184(5) -0.27106(19) 0.0399(10) Uani 1 1 d . . . H34 H -0.0830 1.3297 -0.2840 0.048 Uiso 1 1 calc R . . C35 C -0.10859(15) 1.6374(5) -0.2706(2) 0.0498(13) Uani 1 1 d . . . H35 H -0.1224 1.7313 -0.2841 0.060 Uiso 1 1 calc R . . C36 C -0.08275(14) 1.5881(5) -0.2114(2) 0.0420(10) Uani 1 1 d . . . H36 H -0.0759 1.6390 -0.1777 0.050 Uiso 1 1 calc R . . N1 N 0.18376(10) 0.7428(3) 0.16699(13) 0.0234(6) Uani 1 1 d . . . N2 N 0.14358(10) 0.8871(3) 0.21123(13) 0.0242(6) Uani 1 1 d . . . N3 N 0.31867(11) 0.4115(4) 0.50459(14) 0.0297(7) Uani 1 1 d . . . N4 N 0.33651(15) 0.3182(5) 0.59000(18) 0.0551(8) Uani 1 1 d . . . N5 N 0.09396(9) 0.8398(3) 0.04681(13) 0.0208(6) Uani 1 1 d . . . N6 N 0.11623(10) 1.1007(3) 0.11635(13) 0.0218(6) Uani 1 1 d . . . N7 N -0.06873(10) 1.4454(4) -0.21189(15) 0.0312(7) Uani 1 1 d . . . N8 N -0.11175(12) 1.5318(5) -0.30806(18) 0.0487(10) Uani 1 1 d . . . Cu1 Cu 0.134569(14) 0.89112(4) 0.135153(18) 0.02054(12) Uani 1 1 d . . . C37 C 0.1554(2) 0.4266(7) 0.9451(3) 0.0621(14) Uani 1 1 d . . . H37 H 0.1501 0.4988 0.9150 0.075 Uiso 1 1 calc R A 1 Cl1A Cl 0.19576(12) 0.5072(3) 1.02158(10) 0.0937(11) Uani 0.720(5) 1 d P B 1 Cl2A Cl 0.17871(19) 0.2726(4) 0.94165(18) 0.142(2) Uani 0.720(5) 1 d P B 1 Cl3A Cl 0.10421(10) 0.3980(5) 0.9297(2) 0.1240(15) Uani 0.720(5) 1 d P B 1 Cl3B Cl 0.1226(3) 0.2319(7) 0.9025(3) 0.088(2) Uani 0.280(5) 1 d P B 2 Cl1B Cl 0.1366(6) 0.4518(11) 0.9821(6) 0.180(8) Uani 0.280(5) 1 d P B 2 Cl2B Cl 0.2090(3) 0.3701(18) 0.9849(8) 0.221(11) Uani 0.280(5) 1 d P B 2 C38 C -0.0205(3) 0.7923(12) 0.7285(4) 0.054(3) Uani 0.50 1 d P . . Cl4 Cl 0.0000 0.6281(3) 0.7500 0.204(3) Uani 1 2 d S . . Cl5 Cl -0.01770(9) 0.9027(3) 0.78058(12) 0.1203(9) 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 C1 0.037(2) 0.030(2) 0.036(2) 0.0064(16) 0.0267(18) 0.0076(16) C2 0.046(2) 0.037(2) 0.037(2) 0.0021(18) 0.033(2) 0.0045(18) C3 0.038(2) 0.0316(19) 0.0232(18) 0.0054(15) 0.0204(17) 0.0004(16) C4 0.0247(16) 0.0218(16) 0.0175(15) 0.0024(13) 0.0114(14) -0.0017(13) C5 0.0201(15) 0.0217(17) 0.0211(16) 0.0035(13) 0.0099(14) -0.0024(13) C6 0.0212(15) 0.0191(15) 0.0193(16) 0.0037(13) 0.0100(13) 0.0006(13) C7 0.0236(16) 0.0225(17) 0.0249(17) 0.0061(14) 0.0114(15) 0.0076(13) C8 0.0345(19) 0.035(2) 0.032(2) 0.0048(17) 0.0221(17) 0.0107(16) C9 0.0311(18) 0.0271(18) 0.0234(17) 0.0046(15) 0.0176(15) 0.0070(15) C10 0.0236(16) 0.0243(17) 0.0194(16) 0.0045(14) 0.0118(14) 0.0025(13) C11 0.0236(18) 0.040(2) 0.029(2) 0.0136(17) 0.0074(16) -0.0042(16) C12 0.0312(19) 0.039(2) 0.033(2) 0.0156(18) 0.0157(18) -0.0022(17) C13 0.0265(17) 0.0277(18) 0.0188(16) 0.0067(14) 0.0130(14) 0.0079(14) C14 0.0202(16) 0.041(2) 0.0201(17) 0.0033(15) 0.0107(14) 0.0007(15) C15 0.0245(16) 0.0308(19) 0.0217(17) 0.0041(15) 0.0130(15) -0.0028(14) C16 0.043(2) 0.054(3) 0.036(2) 0.021(2) 0.026(2) 0.012(2) C17 0.0587(19) 0.059(2) 0.0334(15) 0.0185(15) 0.0234(15) 0.0156(17) C18 0.0300(19) 0.048(3) 0.028(2) 0.0114(18) 0.0134(17) 0.0102(18) C19 0.0298(17) 0.0155(15) 0.0259(17) 0.0023(13) 0.0160(15) 0.0018(13) C20 0.0349(19) 0.0208(17) 0.0247(18) -0.0042(14) 0.0150(16) -0.0046(15) C21 0.0265(17) 0.0253(18) 0.0183(16) 0.0010(14) 0.0092(14) -0.0018(14) C22 0.0232(15) 0.0183(15) 0.0163(15) 0.0034(12) 0.0117(13) 0.0015(12) C23 0.0213(15) 0.0207(16) 0.0214(16) 0.0062(13) 0.0138(14) 0.0031(12) C24 0.0225(15) 0.0171(15) 0.0231(16) 0.0060(13) 0.0145(14) 0.0042(12) C25 0.0311(18) 0.0143(15) 0.0281(18) 0.0032(14) 0.0160(16) 0.0017(14) C26 0.0333(19) 0.0165(16) 0.0312(19) -0.0029(14) 0.0189(17) -0.0022(14) C27 0.0264(16) 0.0206(17) 0.0232(17) -0.0016(14) 0.0133(14) 0.0009(13) C28 0.0198(15) 0.0162(15) 0.0214(16) 0.0058(13) 0.0107(13) 0.0027(12) C29 0.0263(17) 0.0258(18) 0.0250(17) 0.0048(14) 0.0164(15) 0.0042(14) C30 0.0230(16) 0.0286(19) 0.0301(19) 0.0071(15) 0.0153(15) 0.0071(14) C31 0.0208(16) 0.0209(16) 0.0227(17) 0.0072(14) 0.0084(14) 0.0013(13) C32 0.038(2) 0.033(2) 0.0248(18) 0.0086(15) 0.0219(17) 0.0060(16) C33 0.0322(18) 0.0258(18) 0.0307(19) 0.0086(15) 0.0208(17) 0.0095(15) C34 0.036(2) 0.041(2) 0.029(2) 0.0129(18) 0.0148(18) 0.0003(18) C35 0.030(2) 0.035(2) 0.062(3) 0.029(2) 0.020(2) 0.0068(18) C36 0.031(2) 0.031(2) 0.050(3) 0.0167(19) 0.020(2) 0.0084(17) N1 0.0236(14) 0.0225(14) 0.0202(14) 0.0049(11) 0.0125(12) 0.0048(11) N2 0.0273(14) 0.0229(14) 0.0219(14) 0.0044(12) 0.0157(13) 0.0054(12) N3 0.0313(16) 0.0324(17) 0.0207(15) 0.0101(13) 0.0146(13) 0.0093(13) N4 0.0587(19) 0.059(2) 0.0334(15) 0.0185(15) 0.0234(15) 0.0156(17) N5 0.0239(13) 0.0147(13) 0.0212(14) 0.0026(11) 0.0134(12) 0.0017(11) N6 0.0244(13) 0.0182(14) 0.0188(13) 0.0016(11) 0.0123(12) 0.0023(11) N7 0.0280(15) 0.0264(16) 0.0282(16) 0.0122(13) 0.0132(14) 0.0032(13) N8 0.0303(17) 0.052(2) 0.041(2) 0.0302(19) 0.0128(16) 0.0039(16) Cu1 0.0230(2) 0.0168(2) 0.0170(2) 0.00382(16) 0.01084(17) 0.00431(16) C37 0.073(4) 0.071(4) 0.056(3) 0.005(3) 0.048(3) 0.001(3) Cl1A 0.120(2) 0.0903(18) 0.0454(12) -0.0138(11) 0.0422(13) -0.0385(16) Cl2A 0.289(6) 0.103(2) 0.130(3) 0.057(2) 0.178(4) 0.107(3) Cl3A 0.0759(17) 0.166(3) 0.140(3) 0.033(3) 0.074(2) -0.0185(19) Cl3B 0.118(6) 0.078(4) 0.085(4) 0.013(3) 0.074(4) -0.006(4) Cl1B 0.37(2) 0.115(7) 0.182(12) 0.054(8) 0.236(16) 0.120(11) Cl2B 0.065(5) 0.247(17) 0.262(17) 0.144(15) 0.065(7) -0.015(7) C38 0.036(4) 0.074(7) 0.040(5) 0.007(5) 0.019(4) 0.018(5) Cl4 0.098(2) 0.0573(16) 0.455(8) 0.000 0.178(4) 0.000 Cl5 0.1350(18) 0.152(2) 0.1332(18) -0.0809(16) 0.1133(17) -0.0654(15) _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 N2 1.340(5) . ? C1 C2 1.406(5) . ? C1 H1 0.9300 . ? C2 C3 1.374(6) . ? C2 H2 0.9300 . ? C3 C4 1.421(5) . ? C3 H3 0.9300 . ? C4 N2 1.384(4) . ? C4 C5 1.404(5) . ? C5 C6 1.393(5) . ? C5 C10 1.491(5) . ? C6 N1 1.399(4) . ? C6 C7 1.417(5) . ? C7 C8 1.374(5) . ? C7 H7 0.9300 . ? C8 C9 1.410(5) . ? C8 H8 0.9300 . ? C9 N1 1.337(4) . ? C9 H9 0.9300 . ? C10 C11 1.388(5) . ? C10 C15 1.390(5) . ? C11 C12 1.385(5) . ? C11 H11 0.9300 . ? C12 C13 1.382(5) . ? C12 H12 0.9300 . ? C13 C14 1.375(5) . ? C13 N3 1.433(4) . ? C14 C15 1.390(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N4 1.337(5) . ? C16 N3 1.368(5) . ? C16 H16 0.9300 . ? C17 C18 1.323(6) . ? C17 N4 1.386(7) . ? C17 H17 0.9300 . ? C18 N3 1.370(5) . ? C18 H18 0.9300 . ? C19 N5 1.340(4) . ? C19 C20 1.405(5) . ? C19 H19 0.9300 . ? C20 C21 1.380(5) . ? C20 H20 0.9300 . ? C21 C22 1.414(5) . ? C21 H21 0.9300 . ? C22 N5 1.401(4) . ? C22 C23 1.408(5) . ? C23 C24 1.391(5) . ? C23 C28 1.482(4) . ? C24 N6 1.392(4) . ? C24 C25 1.427(5) . ? C25 C26 1.376(5) . ? C25 H25 0.9300 . ? C26 C27 1.399(5) . ? C26 H26 0.9300 . ? C27 N6 1.342(4) . ? C27 H27 0.9300 . ? C28 C33 1.393(5) . ? C28 C29 1.400(5) . ? C29 C30 1.382(5) . ? C29 H29 0.9300 . ? C30 C31 1.378(5) . ? C30 H30 0.9300 . ? C31 C32 1.389(5) . ? C31 N7 1.421(4) . ? C32 C33 1.385(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 N8 1.314(5) . ? C34 N7 1.355(5) . ? C34 H34 0.9300 . ? C35 C36 1.355(6) . ? C35 N8 1.366(7) . ? C35 H35 0.9300 . ? C36 N7 1.386(5) . ? C36 H36 0.9300 . ? N1 Cu1 1.955(3) . ? N2 Cu1 1.949(3) . ? N5 Cu1 1.961(3) . ? N6 Cu1 1.952(3) . ? C37 Cl1B 1.611(10) . ? C37 Cl2B 1.621(12) . ? C37 Cl2A 1.668(6) . ? C37 Cl3A 1.689(6) . ? C37 Cl1A 1.804(6) . ? C37 Cl3B 2.021(9) . ? C37 H37 0.9800 . ? C38 C38 1.189(18) 2_556 ? C38 Cl4 1.587(11) . ? C38 Cl5 1.720(11) . ? C38 Cl5 1.886(11) 2_556 ? Cl4 C38 1.587(11) 2_556 ? Cl5 C38 1.886(11) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C2 111.5(3) . . ? N2 C1 H1 124.3 . . ? C2 C1 H1 124.3 . . ? C3 C2 C1 106.1(3) . . ? C3 C2 H2 127.0 . . ? C1 C2 H2 127.0 . . ? C2 C3 C4 107.1(3) . . ? C2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? N2 C4 C5 124.2(3) . . ? N2 C4 C3 108.7(3) . . ? C5 C4 C3 127.1(3) . . ? C6 C5 C4 125.5(3) . . ? C6 C5 C10 118.8(3) . . ? C4 C5 C10 115.8(3) . . ? C5 C6 N1 123.9(3) . . ? C5 C6 C7 127.5(3) . . ? N1 C6 C7 108.6(3) . . ? C8 C7 C6 107.5(3) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 105.9(3) . . ? C7 C8 H8 127.0 . . ? C9 C8 H8 127.0 . . ? N1 C9 C8 111.9(3) . . ? N1 C9 H9 124.1 . . ? C8 C9 H9 124.1 . . ? C11 C10 C15 119.2(3) . . ? C11 C10 C5 119.2(3) . . ? C15 C10 C5 121.4(3) . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 119.4(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 120.8(3) . . ? C14 C13 N3 120.5(3) . . ? C12 C13 N3 118.6(3) . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C10 120.2(3) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? N4 C16 N3 109.6(4) . . ? N4 C16 H16 125.2 . . ? N3 C16 H16 125.2 . . ? C18 C17 N4 108.8(4) . . ? C18 C17 H17 125.6 . . ? N4 C17 H17 125.6 . . ? C17 C18 N3 108.8(4) . . ? C17 C18 H18 125.6 . . ? N3 C18 H18 125.6 . . ? N5 C19 C20 111.8(3) . . ? N5 C19 H19 124.1 . . ? C20 C19 H19 124.1 . . ? C21 C20 C19 106.3(3) . . ? C21 C20 H20 126.8 . . ? C19 C20 H20 126.8 . . ? C20 C21 C22 107.0(3) . . ? C20 C21 H21 126.5 . . ? C22 C21 H21 126.5 . . ? N5 C22 C23 123.3(3) . . ? N5 C22 C21 108.9(3) . . ? C23 C22 C21 127.8(3) . . ? C24 C23 C22 124.9(3) . . ? C24 C23 C28 117.2(3) . . ? C22 C23 C28 117.8(3) . . ? C23 C24 N6 124.3(3) . . ? C23 C24 C25 127.5(3) . . ? N6 C24 C25 108.1(3) . . ? C26 C25 C24 107.2(3) . . ? C26 C25 H25 126.4 . . ? C24 C25 H25 126.4 . . ? C25 C26 C27 106.5(3) . . ? C25 C26 H26 126.8 . . ? C27 C26 H26 126.8 . . ? N6 C27 C26 111.5(3) . . ? N6 C27 H27 124.3 . . ? C26 C27 H27 124.3 . . ? C33 C28 C29 118.2(3) . . ? C33 C28 C23 120.9(3) . . ? C29 C28 C23 120.8(3) . . ? C30 C29 C28 120.9(3) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C29 120.1(3) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 119.9(3) . . ? C30 C31 N7 120.6(3) . . ? C32 C31 N7 119.5(3) . . ? C33 C32 C31 120.0(3) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C28 120.8(3) . . ? C32 C33 H33 119.6 . . ? C28 C33 H33 119.6 . . ? N8 C34 N7 112.3(4) . . ? N8 C34 H34 123.8 . . ? N7 C34 H34 123.8 . . ? C36 C35 N8 111.4(4) . . ? C36 C35 H35 124.3 . . ? N8 C35 H35 124.3 . . ? C35 C36 N7 105.2(4) . . ? C35 C36 H36 127.4 . . ? N7 C36 H36 127.4 . . ? C9 N1 C6 106.1(3) . . ? C9 N1 Cu1 127.0(2) . . ? C6 N1 Cu1 126.9(2) . . ? C1 N2 C4 106.6(3) . . ? C1 N2 Cu1 126.2(2) . . ? C4 N2 Cu1 127.2(2) . . ? C16 N3 C18 106.4(3) . . ? C16 N3 C13 125.6(3) . . ? C18 N3 C13 128.0(3) . . ? C16 N4 C17 106.5(4) . . ? C19 N5 C22 106.0(3) . . ? C19 N5 Cu1 125.6(2) . . ? C22 N5 Cu1 125.9(2) . . ? C27 N6 C24 106.8(3) . . ? C27 N6 Cu1 124.8(2) . . ? C24 N6 Cu1 127.0(2) . . ? C34 N7 C36 106.4(3) . . ? C34 N7 C31 127.6(3) . . ? C36 N7 C31 126.0(4) . . ? C34 N8 C35 104.7(4) . . ? N2 Cu1 N6 95.59(12) . . ? N2 Cu1 N1 92.32(12) . . ? N6 Cu1 N1 147.15(12) . . ? N2 Cu1 N5 146.97(12) . . ? N6 Cu1 N5 91.87(11) . . ? N1 Cu1 N5 98.64(12) . . ? Cl1B C37 Cl2B 117.2(9) . . ? Cl1B C37 Cl2A 128.2(5) . . ? Cl2B C37 Cl2A 47.5(7) . . ? Cl1B C37 Cl3A 44.6(6) . . ? Cl2B C37 Cl3A 145.1(5) . . ? Cl2A C37 Cl3A 114.1(4) . . ? Cl1B C37 Cl1A 62.9(7) . . ? Cl2B C37 Cl1A 65.9(8) . . ? Cl2A C37 Cl1A 109.7(4) . . ? Cl3A C37 Cl1A 107.5(3) . . ? Cl1B C37 Cl3B 99.0(7) . . ? Cl2B C37 Cl3B 98.4(8) . . ? Cl2A C37 Cl3B 52.4(3) . . ? Cl3A C37 Cl3B 64.2(3) . . ? Cl1A C37 Cl3B 140.7(4) . . ? Cl1B C37 H37 122.7 . . ? Cl2B C37 H37 105.9 . . ? Cl2A C37 H37 108.5 . . ? Cl3A C37 H37 108.5 . . ? Cl1A C37 H37 108.5 . . ? Cl3B C37 H37 110.5 . . ? C38 C38 Cl4 68.0(4) 2_556 . ? C38 C38 Cl5 78.5(8) 2_556 . ? Cl4 C38 Cl5 117.3(6) . . ? C38 C38 Cl5 63.3(7) 2_556 2_556 ? Cl4 C38 Cl5 108.5(5) . 2_556 ? Cl5 C38 Cl5 100.5(6) . 2_556 ? C38 Cl4 C38 44.0(7) 2_556 . ? C38 Cl5 C38 38.2(5) . 2_556 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.477 _refine_diff_density_min -1.485 _refine_diff_density_rms 0.094 #===END ###Material relevant to compound 3 at 173K ## data_compound3 _database_code_depnum_ccdc_archive 'CCDC 894061' #TrackingRef '- CC_COM_07_2012_035543.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H59 Cd Cl2 Cu2 N17 O' _chemical_formula_weight 1524.77 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' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 14.5401(4) _cell_length_b 30.0895(11) _cell_length_c 19.4195(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.7360(10) _cell_angle_gamma 90.00 _cell_volume 8418.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9975 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 28.10 _exptl_crystal_description prism _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8464 _exptl_absorpt_correction_T_max 0.8464 _exptl_absorpt_process_details sadabs _exptl_special_details ; One of the phenyl groups of the ligand is disordered over two positions. This has been modeled accordingly. One DMF molecule close an inversion center could be identified. However, a mixture of disordered DMF and water molecules was present. The Squeeze command was applied to account for this. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 121879 _diffrn_reflns_av_R_equivalents 0.0393 _diffrn_reflns_av_sigmaI/netI 0.0228 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9818 _reflns_number_gt 8480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0647P)^2^+26.7062P] 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 9818 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9276(2) 0.22940(12) -0.16171(18) 0.0362(7) Uani 1 1 d . . . H1 H 0.9670 0.2421 -0.1902 0.043 Uiso 1 1 calc R . . C2 C 0.9546(3) 0.21719(13) -0.09272(19) 0.0435(9) Uani 1 1 d . . . H2 H 1.0131 0.2206 -0.0673 0.052 Uiso 1 1 calc R . . C3 C 0.8770(3) 0.19907(12) -0.06959(18) 0.0389(8) Uani 1 1 d . . . H3 H 0.8737 0.1875 -0.0256 0.047 Uiso 1 1 calc R . . C4 C 0.8039(2) 0.20141(10) -0.12489(16) 0.0293(7) Uani 1 1 d . . . C5 C 0.7121(2) 0.18589(9) -0.12596(16) 0.0297(7) Uani 1 1 d . . . C6 C 0.6433(2) 0.18841(10) -0.18203(16) 0.0290(7) Uani 1 1 d . . . C7 C 0.5535(2) 0.16815(11) -0.19095(19) 0.0346(7) Uani 1 1 d . . . H7 H 0.5280 0.1515 -0.1579 0.042 Uiso 1 1 calc R . . C8 C 0.5121(2) 0.17758(12) -0.2563(2) 0.0378(8) Uani 1 1 d . . . H8 H 0.4541 0.1680 -0.2770 0.045 Uiso 1 1 calc R . . C9 C 0.5751(2) 0.20482(11) -0.28653(18) 0.0337(7) Uani 1 1 d . . . H9 H 0.5635 0.2169 -0.3310 0.040 Uiso 1 1 calc R . . C10 C 0.6886(2) 0.16434(10) -0.06099(17) 0.0316(7) Uani 1 1 d . . . C11 C 0.6750(3) 0.11921(11) -0.05774(18) 0.0440(9) Uani 1 1 d . . . H11 H 0.6775 0.1020 -0.0972 0.053 Uiso 1 1 calc R . . C12 C 0.6576(3) 0.09895(11) 0.00343(18) 0.0425(9) Uani 1 1 d . . . H12 H 0.6509 0.0683 0.0055 0.051 Uiso 1 1 calc R . . C13 C 0.6505(2) 0.12466(10) 0.06097(16) 0.0302(7) Uani 1 1 d . . . C14 C 0.6593(3) 0.17033(11) 0.05775(17) 0.0377(8) Uani 1 1 d . . . H14 H 0.6519 0.1878 0.0961 0.045 Uiso 1 1 calc R . . C15 C 0.6794(3) 0.18985(10) -0.00308(18) 0.0394(8) Uani 1 1 d . . . H15 H 0.6868 0.2205 -0.0050 0.047 Uiso 1 1 calc R . . C16 C 0.5780(2) 0.06885(10) 0.13065(16) 0.0278(6) Uani 1 1 d . . . H16 H 0.5416 0.0552 0.0936 0.033 Uiso 1 1 calc R . . C17 C 0.6423(3) 0.08484(11) 0.23335(17) 0.0353(7) Uani 1 1 d . . . H17 H 0.6588 0.0838 0.2813 0.042 Uiso 1 1 calc R . . C18 C 0.6749(3) 0.11474(11) 0.18990(17) 0.0352(7) Uani 1 1 d . . . H18 H 0.7164 0.1378 0.2022 0.042 Uiso 1 1 calc R . . C19 C 0.1389(2) -0.18169(11) 0.71952(18) 0.0350(7) Uani 1 1 d . . . H19 H 0.1084 -0.1913 0.7560 0.042 Uiso 1 1 calc R . . C20 C 0.1212(3) -0.14109(12) 0.6846(2) 0.0412(8) Uani 1 1 d . . . H20 H 0.0791 -0.1194 0.6939 0.049 Uiso 1 1 calc R . . C21 C 0.1789(3) -0.14001(12) 0.63403(19) 0.0393(8) Uani 1 1 d . . . H21 H 0.1825 -0.1174 0.6019 0.047 Uiso 1 1 calc R . . C22 C 0.2320(2) -0.17987(11) 0.63975(16) 0.0309(7) Uani 1 1 d . . . C23 C 0.2997(2) -0.19370(11) 0.59969(16) 0.0302(7) Uani 1 1 d . A . C24 C 0.3549(2) -0.23158(11) 0.61160(16) 0.0311(7) Uani 1 1 d . . . C25 C 0.4201(2) -0.24858(14) 0.57014(18) 0.0429(9) Uani 1 1 d . . . H25 H 0.4345 -0.2363 0.5290 0.052 Uiso 1 1 calc R . . C26 C 0.4576(3) -0.28599(15) 0.60135(19) 0.0455(9) Uani 1 1 d . . . H26 H 0.5022 -0.3042 0.5858 0.055 Uiso 1 1 calc R . . C27 C 0.4151(2) -0.29176(12) 0.66241(18) 0.0362(7) Uani 1 1 d . . . H27 H 0.4283 -0.3149 0.6939 0.043 Uiso 1 1 calc R . . C28 C 0.3111(2) -0.16676(11) 0.53690(17) 0.0336(7) Uani 1 1 d . . . C29 C 0.3415(4) -0.12044(19) 0.5434(3) 0.0360(15) Uani 0.594(6) 1 d P A 1 H29 H 0.3534 -0.1072 0.5870 0.043 Uiso 0.594(6) 1 calc PR A 1 C30 C 0.3526(4) -0.09599(18) 0.4833(3) 0.0357(14) Uani 0.594(6) 1 d P A 1 H30 H 0.3709 -0.0664 0.4854 0.043 Uiso 0.594(6) 1 calc PR A 1 C32 C 0.2971(5) -0.1593(2) 0.4140(3) 0.0374(15) Uani 0.594(6) 1 d P A 1 H32 H 0.2778 -0.1719 0.3707 0.045 Uiso 0.594(6) 1 calc PR A 1 C33 C 0.2859(5) -0.1833(2) 0.4735(3) 0.0343(15) Uani 0.594(6) 1 d P A 1 H33 H 0.2601 -0.2116 0.4689 0.041 Uiso 0.594(6) 1 calc PR A 1 C29B C 0.4017(6) -0.1539(3) 0.5238(5) 0.041(2) Uani 0.406(6) 1 d P A 2 H29B H 0.4532 -0.1601 0.5562 0.049 Uiso 0.406(6) 1 calc PR A 2 C30B C 0.4122(6) -0.1318(3) 0.4617(5) 0.045(3) Uani 0.406(6) 1 d P A 2 H30B H 0.4710 -0.1252 0.4507 0.054 Uiso 0.406(6) 1 calc PR A 2 C33B C 0.2406(6) -0.1636(3) 0.4837(4) 0.031(2) Uani 0.406(6) 1 d P A 2 H33B H 0.1842 -0.1772 0.4883 0.038 Uiso 0.406(6) 1 calc PR A 2 C32B C 0.2494(7) -0.1414(3) 0.4237(5) 0.0317(19) Uani 0.406(6) 1 d P A 2 H32B H 0.2002 -0.1403 0.3878 0.038 Uiso 0.406(6) 1 calc PR A 2 C31 C 0.3334(2) -0.12018(13) 0.41687(18) 0.0383(8) Uani 1 1 d . . . C34 C 0.4140(3) -0.06830(12) 0.34541(18) 0.0370(8) Uani 1 1 d . . . H34 H 0.4630 -0.0610 0.3794 0.044 Uiso 1 1 calc R A . C35 C 0.3223(3) -0.07126(13) 0.24890(18) 0.0437(9) Uani 1 1 d . . . H35 H 0.2969 -0.0658 0.2031 0.052 Uiso 1 1 calc R A . C36 C 0.2855(3) -0.09856(14) 0.2928(2) 0.0489(10) Uani 1 1 d . A . H36 H 0.2316 -0.1154 0.2833 0.059 Uiso 1 1 calc R . . N1 N 0.83771(19) 0.22052(9) -0.18167(14) 0.0309(6) Uani 1 1 d . . . N2 N 0.65309(18) 0.21105(9) -0.24314(14) 0.0295(6) Uani 1 1 d . . . N3 N 0.63418(19) 0.10397(8) 0.12450(13) 0.0282(6) Uani 1 1 d . . . N4 N 0.58145(19) 0.05648(8) 0.19557(13) 0.0275(5) Uani 1 1 d . A . N5 N 0.20500(19) -0.20491(9) 0.69394(14) 0.0310(6) Uani 1 1 d . . . N6 N 0.35412(19) -0.25965(9) 0.66868(13) 0.0288(6) Uani 1 1 d . . . N7 N 0.3441(2) -0.09650(11) 0.35450(15) 0.0393(7) Uani 1 1 d . A . N8 N 0.4024(2) -0.05268(9) 0.28142(14) 0.0353(6) Uani 1 1 d . A . Cl1 Cl 0.60992(10) 0.0000 0.35650(6) 0.0464(3) Uani 1 2 d S A . Cl2 Cl 0.38841(9) 0.0000 0.11266(6) 0.0377(3) Uani 1 2 d S A . Cu1 Cu 0.76357(3) 0.241428(12) -0.265756(19) 0.02737(11) Uani 1 1 d . . . Cd1 Cd 0.49534(2) 0.0000 0.237711(15) 0.02578(10) Uani 1 2 d S . . C39 C 0.9344(5) 0.8928(2) 0.8332(4) 0.0401(16) Uani 0.50 1 d P B -1 H39 H 0.8745 0.8974 0.8435 0.048 Uiso 0.50 1 calc PR B -1 C40 C 1.1002(7) 0.8933(4) 0.8757(6) 0.075(3) Uani 0.50 1 d P B -1 H40A H 1.1238 0.8664 0.8981 0.112 Uiso 0.50 1 calc PR B -1 H40B H 1.1340 0.9182 0.8971 0.112 Uiso 0.50 1 calc PR B -1 H40C H 1.1075 0.8921 0.8273 0.112 Uiso 0.50 1 calc PR B -1 C41 C 0.9846(9) 0.9062(4) 0.9547(6) 0.080(3) Uani 0.50 1 d P B -1 H41A H 0.9242 0.9190 0.9549 0.120 Uiso 0.50 1 calc PR B -1 H41B H 1.0310 0.9262 0.9764 0.120 Uiso 0.50 1 calc PR B -1 H41C H 0.9881 0.8786 0.9797 0.120 Uiso 0.50 1 calc PR B -1 N9 N 1.0004(6) 0.8980(3) 0.8829(4) 0.062(2) Uani 0.50 1 d P B -1 O1 O 0.9421(3) 0.88228(17) 0.7729(3) 0.0431(12) Uani 0.50 1 d P B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0340(18) 0.0450(18) 0.0285(17) 0.0057(14) 0.0001(16) -0.0074(14) C2 0.039(2) 0.058(2) 0.0303(19) 0.0072(16) -0.0078(17) -0.0091(17) C3 0.047(2) 0.0436(18) 0.0245(17) 0.0064(13) 0.0002(17) -0.0074(15) C4 0.0384(18) 0.0284(14) 0.0208(15) 0.0042(11) 0.0024(15) -0.0041(12) C5 0.0419(18) 0.0232(13) 0.0256(16) 0.0008(11) 0.0105(15) -0.0057(12) C6 0.0336(17) 0.0263(14) 0.0282(17) 0.0029(11) 0.0083(15) -0.0027(12) C7 0.0317(17) 0.0308(15) 0.043(2) 0.0050(13) 0.0114(16) -0.0049(12) C8 0.0269(16) 0.0371(17) 0.049(2) 0.0050(15) 0.0036(17) -0.0056(13) C9 0.0287(17) 0.0387(17) 0.0326(18) 0.0092(13) 0.0001(16) -0.0022(13) C10 0.0434(19) 0.0278(14) 0.0255(16) 0.0025(11) 0.0115(15) -0.0049(13) C11 0.077(3) 0.0302(16) 0.0289(17) -0.0041(13) 0.0205(19) -0.0092(16) C12 0.075(3) 0.0216(14) 0.0352(18) -0.0006(12) 0.0219(19) -0.0096(15) C13 0.0398(18) 0.0288(14) 0.0235(15) 0.0033(11) 0.0095(14) -0.0068(12) C14 0.060(2) 0.0275(15) 0.0284(17) -0.0038(12) 0.0171(17) -0.0069(14) C15 0.064(2) 0.0229(14) 0.0344(18) -0.0003(12) 0.0171(18) -0.0079(14) C16 0.0352(17) 0.0256(13) 0.0231(15) 0.0025(11) 0.0056(14) -0.0044(12) C17 0.043(2) 0.0391(17) 0.0236(16) -0.0003(13) 0.0017(16) -0.0071(14) C18 0.0406(19) 0.0348(16) 0.0297(17) -0.0004(13) 0.0028(16) -0.0117(14) C19 0.0324(17) 0.0429(18) 0.0297(17) 0.0043(13) 0.0036(15) -0.0061(14) C20 0.047(2) 0.0357(17) 0.041(2) 0.0009(14) 0.0039(18) -0.0010(15) C21 0.046(2) 0.0363(17) 0.0332(18) 0.0069(14) -0.0016(17) -0.0104(15) C22 0.0313(16) 0.0353(15) 0.0244(15) 0.0075(12) -0.0020(14) -0.0108(13) C23 0.0292(16) 0.0374(16) 0.0227(15) 0.0067(12) -0.0018(14) -0.0140(13) C24 0.0285(16) 0.0430(17) 0.0216(15) 0.0027(12) 0.0027(14) -0.0135(13) C25 0.0301(18) 0.074(3) 0.0247(17) 0.0085(16) 0.0056(16) -0.0028(17) C26 0.0338(19) 0.071(3) 0.0326(19) 0.0008(17) 0.0065(17) 0.0036(17) C27 0.0301(17) 0.0483(19) 0.0294(17) 0.0001(14) 0.0012(15) -0.0034(14) C28 0.0317(18) 0.0434(18) 0.0249(17) 0.0103(13) 0.0007(16) -0.0167(14) C29 0.046(3) 0.041(3) 0.023(3) -0.004(2) 0.008(3) -0.019(3) C30 0.049(4) 0.030(3) 0.029(3) 0.000(2) 0.008(3) -0.019(2) C32 0.047(4) 0.047(3) 0.020(3) -0.001(2) 0.007(3) -0.021(3) C33 0.044(4) 0.034(3) 0.025(3) 0.001(2) 0.006(3) -0.022(3) C29B 0.022(4) 0.053(5) 0.045(5) 0.025(4) -0.004(4) -0.012(3) C30B 0.025(4) 0.062(6) 0.047(6) 0.028(4) 0.003(4) -0.008(4) C33B 0.028(4) 0.038(4) 0.028(4) 0.008(3) 0.004(4) -0.010(4) C32B 0.031(5) 0.035(4) 0.026(4) 0.008(3) -0.006(4) -0.007(4) C31 0.0341(18) 0.053(2) 0.0278(17) 0.0142(14) 0.0042(16) -0.0143(15) C34 0.0367(18) 0.0429(18) 0.0327(18) 0.0122(14) 0.0091(16) -0.0084(14) C35 0.052(2) 0.055(2) 0.0242(17) 0.0071(15) 0.0077(17) -0.0109(18) C36 0.049(2) 0.064(2) 0.034(2) 0.0099(17) 0.0072(19) -0.0193(19) N1 0.0315(14) 0.0350(13) 0.0261(14) 0.0062(10) 0.0040(12) -0.0064(11) N2 0.0283(14) 0.0322(13) 0.0285(14) 0.0051(10) 0.0057(13) -0.0059(10) N3 0.0369(14) 0.0277(12) 0.0212(13) 0.0007(9) 0.0079(12) -0.0066(10) N4 0.0380(15) 0.0234(11) 0.0222(12) 0.0008(9) 0.0078(12) -0.0029(10) N5 0.0307(14) 0.0354(13) 0.0266(14) 0.0057(10) 0.0031(12) -0.0058(11) N6 0.0287(14) 0.0361(14) 0.0211(13) 0.0029(10) 0.0014(12) -0.0080(10) N7 0.0378(16) 0.0531(18) 0.0268(15) 0.0142(12) 0.0041(14) -0.0129(13) N8 0.0417(16) 0.0383(14) 0.0281(14) 0.0083(11) 0.0129(13) -0.0034(12) Cl1 0.0491(8) 0.0645(8) 0.0253(6) 0.000 0.0034(6) 0.000 Cl2 0.0492(7) 0.0314(5) 0.0302(6) 0.000 -0.0030(6) 0.000 Cu1 0.0271(2) 0.0344(2) 0.02052(19) 0.00610(14) 0.00271(17) -0.00707(14) Cd1 0.03822(19) 0.02173(14) 0.02019(16) 0.000 0.01413(14) 0.000 C39 0.036(4) 0.044(4) 0.037(4) 0.000(3) -0.007(4) -0.008(3) C40 0.049(5) 0.117(9) 0.057(6) -0.009(6) -0.001(5) 0.018(6) C41 0.097(9) 0.074(7) 0.067(7) -0.001(5) 0.005(7) 0.005(6) N9 0.068(5) 0.061(5) 0.063(5) -0.007(4) 0.030(5) 0.010(4) O1 0.033(3) 0.045(3) 0.051(3) -0.011(2) 0.005(3) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.340(4) . ? C1 C2 1.393(5) . ? C1 H1 0.9300 . ? C2 C3 1.381(5) . ? C2 H2 0.9300 . ? C3 C4 1.408(5) . ? C3 H3 0.9300 . ? C4 N1 1.391(4) . ? C4 C5 1.412(5) . ? C5 C6 1.378(5) . ? C5 C10 1.498(4) . ? C6 N2 1.392(4) . ? C6 C7 1.431(4) . ? C7 C8 1.360(5) . ? C7 H7 0.9300 . ? C8 C9 1.413(4) . ? C8 H8 0.9300 . ? C9 N2 1.332(4) . ? C9 H9 0.9300 . ? C10 C11 1.375(4) . ? C10 C15 1.383(4) . ? C11 C12 1.388(4) . ? C11 H11 0.9300 . ? C12 C13 1.374(4) . ? C12 H12 0.9300 . ? C13 C14 1.382(4) . ? C13 N3 1.430(4) . ? C14 C15 1.385(4) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N4 1.309(4) . ? C16 N3 1.351(4) . ? C16 H16 0.9300 . ? C17 C18 1.361(4) . ? C17 N4 1.369(4) . ? C17 H17 0.9300 . ? C18 N3 1.366(4) . ? C18 H18 0.9300 . ? C19 N5 1.336(4) . ? C19 C20 1.404(5) . ? C19 H19 0.9300 . ? C20 C21 1.375(5) . ? C20 H20 0.9300 . ? C21 C22 1.423(5) . ? C21 H21 0.9300 . ? C22 N5 1.393(4) . ? C22 C23 1.397(5) . ? C23 C24 1.395(5) . ? C23 C28 1.492(4) . ? C24 N6 1.395(4) . ? C24 C25 1.419(5) . ? C25 C26 1.358(6) . ? C25 H25 0.9300 . ? C26 C27 1.419(5) . ? C26 H26 0.9300 . ? C27 N6 1.328(4) . ? C27 H27 0.9300 . ? C28 C33 1.333(6) . ? C28 C33B 1.358(10) . ? C28 C29B 1.428(8) . ? C28 C29 1.462(6) . ? C29 C30 1.406(7) . ? C29 H29 0.9300 . ? C30 C31 1.475(7) . ? C30 H30 0.9300 . ? C32 C31 1.287(7) . ? C32 C33 1.390(7) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C29B C30B 1.403(11) . ? C29B H29B 0.9300 . ? C30B C31 1.388(10) . ? C30B H30B 0.9300 . ? C33B C32B 1.365(11) . ? C33B H33B 0.9300 . ? C32B C31 1.399(9) . ? C32B H32B 0.9300 . ? C31 N7 1.432(4) . ? C34 N8 1.318(4) . ? C34 N7 1.354(4) . ? C34 H34 0.9300 . ? C35 C36 1.345(5) . ? C35 N8 1.368(5) . ? C35 H35 0.9300 . ? C36 N7 1.376(5) . ? C36 H36 0.9300 . ? N1 Cu1 1.937(3) . ? N2 Cu1 1.949(2) . ? N4 Cd1 2.324(2) . ? N5 Cu1 1.940(3) 3_446 ? N6 Cu1 1.951(3) 3_446 ? N8 Cd1 2.317(3) . ? Cl1 Cd1 2.6575(14) . ? Cl2 Cd1 2.7015(13) . ? Cu1 N5 1.940(3) 3_554 ? Cu1 N6 1.951(3) 3_554 ? Cd1 N8 2.317(3) 6 ? Cd1 N4 2.324(2) 6 ? C39 O1 1.234(9) . ? C39 N9 1.275(11) . ? C39 H39 0.9300 . ? C40 N9 1.484(12) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 N9 1.463(12) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.3(3) . . ? N1 C1 H1 124.4 . . ? C2 C1 H1 124.4 . . ? C3 C2 C1 106.3(3) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.3(3) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? N1 C4 C3 108.3(3) . . ? N1 C4 C5 124.0(3) . . ? C3 C4 C5 127.6(3) . . ? C6 C5 C4 125.3(3) . . ? C6 C5 C10 117.8(3) . . ? C4 C5 C10 116.9(3) . . ? C5 C6 N2 123.7(3) . . ? C5 C6 C7 128.7(3) . . ? N2 C6 C7 107.5(3) . . ? C8 C7 C6 107.8(3) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? C7 C8 C9 106.2(3) . . ? C7 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? N2 C9 C8 111.3(3) . . ? N2 C9 H9 124.4 . . ? C8 C9 H9 124.4 . . ? C11 C10 C15 118.7(3) . . ? C11 C10 C5 121.1(3) . . ? C15 C10 C5 120.2(3) . . ? C10 C11 C12 121.1(3) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 119.4(3) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 120.3(3) . . ? C12 C13 N3 119.7(3) . . ? C14 C13 N3 119.9(3) . . ? C13 C14 C15 119.4(3) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C10 C15 C14 120.9(3) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? N4 C16 N3 111.3(3) . . ? N4 C16 H16 124.4 . . ? N3 C16 H16 124.4 . . ? C18 C17 N4 109.5(3) . . ? C18 C17 H17 125.3 . . ? N4 C17 H17 125.3 . . ? C17 C18 N3 106.0(3) . . ? C17 C18 H18 127.0 . . ? N3 C18 H18 127.0 . . ? N5 C19 C20 111.7(3) . . ? N5 C19 H19 124.1 . . ? C20 C19 H19 124.1 . . ? C21 C20 C19 106.0(3) . . ? C21 C20 H20 127.0 . . ? C19 C20 H20 127.0 . . ? C20 C21 C22 107.5(3) . . ? C20 C21 H21 126.3 . . ? C22 C21 H21 126.3 . . ? N5 C22 C23 123.4(3) . . ? N5 C22 C21 108.1(3) . . ? C23 C22 C21 128.5(3) . . ? C24 C23 C22 125.7(3) . . ? C24 C23 C28 117.0(3) . . ? C22 C23 C28 117.2(3) . . ? N6 C24 C23 124.1(3) . . ? N6 C24 C25 108.1(3) . . ? C23 C24 C25 127.9(3) . . ? C26 C25 C24 107.8(3) . . ? C26 C25 H25 126.1 . . ? C24 C25 H25 126.1 . . ? C25 C26 C27 106.3(3) . . ? C25 C26 H26 126.9 . . ? C27 C26 H26 126.9 . . ? N6 C27 C26 111.0(3) . . ? N6 C27 H27 124.5 . . ? C26 C27 H27 124.5 . . ? C33 C28 C33B 40.2(4) . . ? C33 C28 C29B 94.7(5) . . ? C33B C28 C29B 117.8(5) . . ? C33 C28 C29 118.5(4) . . ? C33B C28 C29 100.8(5) . . ? C29B C28 C29 58.8(5) . . ? C33 C28 C23 120.4(3) . . ? C33B C28 C23 120.2(4) . . ? C29B C28 C23 120.0(5) . . ? C29 C28 C23 120.9(3) . . ? C30 C29 C28 119.6(5) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 116.0(4) . . ? C29 C30 H30 122.0 . . ? C31 C30 H30 122.0 . . ? C31 C32 C33 122.1(5) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C28 C33 C32 121.8(5) . . ? C28 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C30B C29B C28 119.5(7) . . ? C30B C29B H29B 120.3 . . ? C28 C29B H29B 120.3 . . ? C31 C30B C29B 118.8(7) . . ? C31 C30B H30B 120.6 . . ? C29B C30B H30B 120.6 . . ? C28 C33B C32B 122.4(7) . . ? C28 C33B H33B 118.8 . . ? C32B C33B H33B 118.8 . . ? C33B C32B C31 119.2(8) . . ? C33B C32B H32B 120.4 . . ? C31 C32B H32B 120.4 . . ? C32 C31 C30B 95.5(6) . . ? C32 C31 C32B 39.7(4) . . ? C30B C31 C32B 118.9(5) . . ? C32 C31 N7 120.6(4) . . ? C30B C31 N7 118.8(4) . . ? C32B C31 N7 120.2(5) . . ? C32 C31 C30 121.2(4) . . ? C30B C31 C30 62.2(5) . . ? C32B C31 C30 102.0(5) . . ? N7 C31 C30 117.7(3) . . ? N8 C34 N7 110.1(3) . . ? N8 C34 H34 125.0 . . ? N7 C34 H34 125.0 . . ? C36 C35 N8 110.1(3) . . ? C36 C35 H35 124.9 . . ? N8 C35 H35 124.9 . . ? C35 C36 N7 105.8(3) . . ? C35 C36 H36 127.1 . . ? N7 C36 H36 127.1 . . ? C1 N1 C4 106.8(3) . . ? C1 N1 Cu1 126.2(2) . . ? C4 N1 Cu1 125.9(2) . . ? C9 N2 C6 107.1(3) . . ? C9 N2 Cu1 125.5(2) . . ? C6 N2 Cu1 127.1(2) . . ? C16 N3 C18 107.1(2) . . ? C16 N3 C13 126.1(3) . . ? C18 N3 C13 126.7(3) . . ? C16 N4 C17 106.1(3) . . ? C16 N4 Cd1 126.5(2) . . ? C17 N4 Cd1 127.4(2) . . ? C19 N5 C22 106.7(3) . . ? C19 N5 Cu1 125.7(2) . 3_446 ? C22 N5 Cu1 127.0(2) . 3_446 ? C27 N6 C24 106.9(3) . . ? C27 N6 Cu1 126.1(2) . 3_446 ? C24 N6 Cu1 125.9(2) . 3_446 ? C34 N7 C36 107.6(3) . . ? C34 N7 C31 126.3(3) . . ? C36 N7 C31 126.1(3) . . ? C34 N8 C35 106.4(3) . . ? C34 N8 Cd1 125.6(2) . . ? C35 N8 Cd1 127.8(2) . . ? N1 Cu1 N5 140.77(12) . 3_554 ? N1 Cu1 N2 92.28(11) . . ? N5 Cu1 N2 98.67(11) 3_554 . ? N1 Cu1 N6 101.36(11) . 3_554 ? N5 Cu1 N6 92.79(11) 3_554 3_554 ? N2 Cu1 N6 142.02(11) . 3_554 ? N8 Cd1 N8 86.34(14) . 6 ? N8 Cd1 N4 176.13(9) . . ? N8 Cd1 N4 89.83(9) 6 . ? N8 Cd1 N4 89.83(9) . 6 ? N8 Cd1 N4 176.13(9) 6 6 ? N4 Cd1 N4 93.98(12) . 6 ? N8 Cd1 Cl1 90.59(8) . . ? N8 Cd1 Cl1 90.59(8) 6 . ? N4 Cd1 Cl1 90.07(7) . . ? N4 Cd1 Cl1 90.07(7) 6 . ? N8 Cd1 Cl2 92.05(8) . . ? N8 Cd1 Cl2 92.05(8) 6 . ? N4 Cd1 Cl2 87.45(7) . . ? N4 Cd1 Cl2 87.45(7) 6 . ? Cl1 Cd1 Cl2 176.37(4) . . ? O1 C39 N9 126.4(8) . . ? O1 C39 H39 116.8 . . ? N9 C39 H39 116.8 . . ? C39 N9 C41 122.8(9) . . ? C39 N9 C40 124.3(8) . . ? C41 N9 C40 112.8(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.175 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.085 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 0.155 799 144 ' ' 2 0.000 0.500 0.500 20 10 ' ' 3 0.163 0.216 0.883 10 1 ' ' 4 0.163 0.784 0.883 10 1 ' ' 5 0.500 0.500 0.571 799 144 ' ' 6 0.337 0.284 0.117 10 1 ' ' 7 0.336 0.716 0.117 10 1 ' ' 8 0.500 0.000 0.500 19 10 ' ' 9 0.663 0.284 0.883 10 1 ' ' 10 0.663 0.716 0.883 10 1 ' ' 11 0.836 0.216 0.117 10 1 ' ' 12 0.837 0.784 0.117 10 1 ' ' _platon_squeeze_details ; The disordered solvent molecules are a mixture of DMF, MeOH and H2O. ; #===END ###Material relevant to compound 4 at 173K ## data_compound4 _database_code_depnum_ccdc_archive 'CCDC 894062' #TrackingRef '- CC_COM_07_2012_035543.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H52 Cd Cu2 N18 S2' _chemical_formula_weight 1496.94 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' S S 0.1246 0.1234 '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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.1765(8) _cell_length_b 29.6240(9) _cell_length_c 14.4219(4) _cell_angle_alpha 90.00 _cell_angle_beta 121.9580(10) _cell_angle_gamma 90.00 _cell_volume 8401.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9933 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 29.80 _exptl_crystal_description prism _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8157 _exptl_absorpt_correction_T_max 0.9352 _exptl_absorpt_process_details sadabs _exptl_special_details ; The Squeeze command has been applied. One phenyl group as well as the thiocyanate anion are disordered over two positions. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88657 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 30.07 _reflns_number_total 12288 _reflns_number_gt 9823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics '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^)+(0.0664P)^2^+0.0092P] 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 12288 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.65991(10) 0.02325(7) 0.83590(16) 0.0356(4) Uani 1 1 d . . . H1 H 0.6880 0.0105 0.9046 0.043 Uiso 1 1 calc R . . C2 C 0.59219(11) 0.03696(8) 0.79421(18) 0.0459(5) Uani 1 1 d . . . H2 H 0.5680 0.0346 0.8289 0.055 Uiso 1 1 calc R . . C3 C 0.56892(10) 0.05459(7) 0.69181(17) 0.0396(5) Uani 1 1 d . . . H3 H 0.5261 0.0668 0.6444 0.048 Uiso 1 1 calc R . . C4 C 0.62248(8) 0.05069(6) 0.67267(14) 0.0276(4) Uani 1 1 d . . . C5 C 0.62270(9) 0.06525(5) 0.57965(14) 0.0268(3) Uani 1 1 d . . . C6 C 0.67758(9) 0.06212(5) 0.56526(13) 0.0265(3) Uani 1 1 d . . . C7 C 0.68505(10) 0.08192(6) 0.48278(15) 0.0336(4) Uani 1 1 d . . . H7 H 0.6525 0.0988 0.4237 0.040 Uiso 1 1 calc R . . C8 C 0.74889(10) 0.07167(7) 0.50599(15) 0.0358(4) Uani 1 1 d . . . H8 H 0.7684 0.0807 0.4669 0.043 Uiso 1 1 calc R . . C9 C 0.77923(9) 0.04468(6) 0.60087(15) 0.0305(4) Uani 1 1 d . . . H9 H 0.8227 0.0325 0.6339 0.037 Uiso 1 1 calc R . . C10 C 0.55930(9) 0.08700(6) 0.49155(14) 0.0287(4) Uani 1 1 d . . . C11 C 0.55546(9) 0.13322(6) 0.47461(16) 0.0373(4) Uani 1 1 d . . . H11 H 0.5941 0.1509 0.5155 0.045 Uiso 1 1 calc R . . C12 C 0.49420(9) 0.15353(6) 0.39684(16) 0.0349(4) Uani 1 1 d . . . H12 H 0.4919 0.1846 0.3865 0.042 Uiso 1 1 calc R . . C13 C 0.43744(9) 0.12741(6) 0.33585(14) 0.0269(3) Uani 1 1 d . . . C14 C 0.44038(10) 0.08097(6) 0.34799(16) 0.0398(5) Uani 1 1 d . . . H14 H 0.4022 0.0633 0.3042 0.048 Uiso 1 1 calc R . . C15 C 0.50122(10) 0.06115(6) 0.42649(17) 0.0410(5) Uani 1 1 d . . . H15 H 0.5033 0.0300 0.4359 0.049 Uiso 1 1 calc R . . C16 C 0.36370(9) 0.18297(6) 0.19137(14) 0.0268(3) Uani 1 1 d . . . H16 H 0.3978 0.1966 0.1856 0.032 Uiso 1 1 calc R . . C17 C 0.26615(9) 0.16685(6) 0.16719(16) 0.0330(4) Uani 1 1 d . . . H17 H 0.2198 0.1676 0.1405 0.040 Uiso 1 1 calc R . . C18 C 0.31146(9) 0.13777(6) 0.24468(16) 0.0338(4) Uani 1 1 d . . . H18 H 0.3022 0.1154 0.2803 0.041 Uiso 1 1 calc R . . C19 C 0.77444(9) -0.06955(6) 0.66473(15) 0.0305(4) Uani 1 1 d . . . H19 H 0.7375 -0.0607 0.5974 0.037 Uiso 1 1 calc R . . C20 C 0.81019(10) -0.11061(6) 0.68349(18) 0.0373(4) Uani 1 1 d . . . H20 H 0.8008 -0.1333 0.6328 0.045 Uiso 1 1 calc R . . C21 C 0.86140(10) -0.11025(6) 0.79139(17) 0.0348(4) Uani 1 1 d . . . H21 H 0.8940 -0.1326 0.8277 0.042 Uiso 1 1 calc R . . C22 C 0.85551(9) -0.06930(6) 0.83774(14) 0.0269(3) Uani 1 1 d . . . C23 C 0.89589(8) -0.05376(6) 0.94616(15) 0.0274(4) Uani 1 1 d . A . C24 C 0.88298(8) -0.01534(6) 0.98868(14) 0.0265(3) Uani 1 1 d . . . C25 C 0.92367(10) 0.00271(8) 1.09521(15) 0.0394(5) Uani 1 1 d . . . H25 H 0.9647 -0.0089 1.1514 0.047 Uiso 1 1 calc R . . C26 C 0.89127(10) 0.04071(8) 1.10023(16) 0.0410(5) Uani 1 1 d . . . H26 H 0.9062 0.0597 1.1601 0.049 Uiso 1 1 calc R . . C27 C 0.83108(9) 0.04517(6) 0.99694(15) 0.0304(4) Uani 1 1 d . . . H27 H 0.7995 0.0683 0.9776 0.036 Uiso 1 1 calc R . . C28 C 0.95930(9) -0.07945(6) 1.02103(15) 0.0300(4) Uani 1 1 d . . . C31 C 1.08038(9) -0.12442(6) 1.16297(15) 0.0321(4) Uani 1 1 d . . . C29A C 0.97863(18) -0.09017(13) 1.1321(3) 0.0292(8) Uani 0.484(2) 1 d P A 3 H29A H 0.9501 -0.0819 1.1564 0.035 Uiso 0.484(2) 1 calc PR A 3 C30A C 1.03882(19) -0.11249(13) 1.2023(3) 0.0311(8) Uani 0.484(2) 1 d P A 3 H30A H 1.0512 -0.1194 1.2735 0.037 Uiso 0.484(2) 1 calc PR A 3 C32A C 1.07056(18) -0.10751(13) 1.0687(3) 0.0280(8) Uani 0.484(2) 1 d P A 3 H32A H 1.1034 -0.1110 1.0507 0.034 Uiso 0.484(2) 1 calc PR A 3 C33A C 1.01022(17) -0.08479(12) 0.9993(3) 0.0269(8) Uani 0.484(2) 1 d P A 3 H33A H 1.0038 -0.0726 0.9351 0.032 Uiso 0.484(2) 1 calc PR A 3 C30B C 1.01418(16) -0.15052(11) 1.1091(3) 0.0267(7) Uani 0.516(2) 1 d P A 4 H30B H 1.0138 -0.1811 1.1231 0.032 Uiso 0.516(2) 1 calc PR A 4 C32B C 1.07841(17) -0.08306(12) 1.1311(3) 0.0299(8) Uani 0.516(2) 1 d P A 4 H32B H 1.1193 -0.0678 1.1579 0.036 Uiso 0.516(2) 1 calc PR A 4 C29B C 0.95400(16) -0.12771(11) 1.0383(3) 0.0243(7) Uani 0.516(2) 1 d P A 4 H29B H 0.9122 -0.1424 1.0034 0.029 Uiso 0.516(2) 1 calc PR A 4 C33B C 1.01843(17) -0.06055(11) 1.0593(3) 0.0283(8) Uani 0.516(2) 1 d P A 4 H33B H 1.0205 -0.0313 1.0379 0.034 Uiso 0.516(2) 1 calc PR A 4 C34 C 1.14996(10) -0.17821(6) 1.31255(15) 0.0333(4) Uani 1 1 d . . . H34 H 1.1161 -0.1862 1.3257 0.040 Uiso 1 1 calc R A . C35 C 1.24529(9) -0.17430(6) 1.32218(15) 0.0333(4) Uani 1 1 d . . . H35 H 1.2904 -0.1796 1.3442 0.040 Uiso 1 1 calc R A . C36 C 1.20303(9) -0.14521(6) 1.24244(16) 0.0332(4) Uani 1 1 d . A . H36 H 1.2133 -0.1271 1.2004 0.040 Uiso 1 1 calc R . . N1 N 0.67839(7) 0.03099(5) 0.76403(12) 0.0279(3) Uani 1 1 d . . . N2 N 0.73735(7) 0.03882(5) 0.63711(12) 0.0264(3) Uani 1 1 d . . . N3 N 0.37395(7) 0.14829(5) 0.25971(11) 0.0261(3) Uani 1 1 d . . . N4 N 0.29926(7) 0.19494(5) 0.13423(12) 0.0278(3) Uani 1 1 d . . . N5 N 0.80069(7) -0.04505(5) 0.75637(12) 0.0263(3) Uani 1 1 d . . . N6 N 0.82543(7) 0.01160(5) 0.93016(12) 0.0253(3) Uani 1 1 d . . . N7 N 1.14170(8) -0.14792(5) 1.23623(12) 0.0307(3) Uani 1 1 d . A . N8 N 1.21182(7) -0.19490(5) 1.36574(12) 0.0299(3) Uani 1 1 d . . . N9 N 0.14587(9) 0.24446(6) -0.00599(17) 0.0415(4) Uani 1 1 d . . . S1 S 0.08981(9) 0.24392(4) 0.11854(14) 0.0663(5) Uani 0.542(2) 1 d P B 1 C37 C 0.12231(18) 0.24299(11) 0.0418(4) 0.0363(9) Uani 0.542(2) 1 d P B 1 S2 S 0.01068(6) 0.23126(5) -0.16673(16) 0.0752(7) Uani 0.458(2) 1 d P . 2 C38 C 0.0900(2) 0.23949(14) -0.0648(4) 0.0386(11) Uani 0.458(2) 1 d P B 2 Cd1 Cd 0.2500 0.2500 0.0000 0.02219(6) Uani 1 2 d S . . Cu1 Cu 0.760297(10) 0.009247(7) 0.773044(17) 0.02367(6) 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 C1 0.0278(9) 0.0455(10) 0.0338(10) 0.0130(9) 0.0164(8) 0.0089(8) C2 0.0317(10) 0.0662(14) 0.0475(12) 0.0189(11) 0.0262(10) 0.0151(10) C3 0.0224(8) 0.0496(12) 0.0437(11) 0.0131(9) 0.0154(8) 0.0105(8) C4 0.0204(7) 0.0277(8) 0.0285(9) 0.0071(7) 0.0087(7) 0.0067(6) C5 0.0251(8) 0.0204(7) 0.0250(8) 0.0030(6) 0.0066(7) 0.0045(6) C6 0.0271(8) 0.0233(7) 0.0217(8) 0.0029(6) 0.0078(7) 0.0042(6) C7 0.0430(10) 0.0292(9) 0.0244(8) 0.0065(7) 0.0150(8) 0.0079(7) C8 0.0474(12) 0.0357(10) 0.0323(10) 0.0050(8) 0.0266(9) 0.0032(8) C9 0.0308(9) 0.0327(9) 0.0300(9) 0.0039(7) 0.0173(8) 0.0048(7) C10 0.0252(8) 0.0263(8) 0.0253(8) 0.0046(7) 0.0070(7) 0.0061(6) C11 0.0231(8) 0.0286(9) 0.0390(10) 0.0044(8) 0.0020(8) 0.0011(7) C12 0.0271(9) 0.0212(8) 0.0397(10) 0.0060(7) 0.0062(8) 0.0022(6) C13 0.0235(8) 0.0247(8) 0.0223(8) 0.0063(6) 0.0051(6) 0.0048(6) C14 0.0298(9) 0.0259(9) 0.0365(10) 0.0030(8) -0.0011(8) -0.0013(7) C15 0.0340(10) 0.0211(8) 0.0402(11) 0.0044(8) 0.0009(8) 0.0027(7) C16 0.0228(8) 0.0240(8) 0.0242(8) 0.0050(6) 0.0060(6) 0.0016(6) C17 0.0228(8) 0.0325(9) 0.0344(10) 0.0060(7) 0.0088(7) -0.0012(7) C18 0.0264(9) 0.0339(9) 0.0352(10) 0.0093(8) 0.0123(8) -0.0012(7) C19 0.0287(9) 0.0303(8) 0.0325(9) 0.0007(7) 0.0163(8) -0.0019(7) C20 0.0363(10) 0.0299(9) 0.0504(12) -0.0057(8) 0.0261(10) -0.0032(7) C21 0.0328(9) 0.0257(8) 0.0509(12) 0.0061(8) 0.0254(9) 0.0048(7) C22 0.0256(8) 0.0260(8) 0.0321(9) 0.0102(7) 0.0174(7) 0.0063(6) C23 0.0231(8) 0.0312(8) 0.0312(9) 0.0143(7) 0.0166(7) 0.0077(6) C24 0.0208(7) 0.0341(9) 0.0251(8) 0.0094(7) 0.0124(7) 0.0069(6) C25 0.0268(9) 0.0657(13) 0.0220(9) 0.0066(9) 0.0104(7) 0.0142(9) C26 0.0318(10) 0.0631(13) 0.0261(9) -0.0062(9) 0.0138(8) 0.0066(9) C27 0.0270(8) 0.0374(9) 0.0276(9) 0.0020(7) 0.0150(7) 0.0048(7) C28 0.0268(8) 0.0345(9) 0.0319(9) 0.0157(7) 0.0178(7) 0.0125(7) C31 0.0285(9) 0.0385(10) 0.0328(9) 0.0170(8) 0.0186(8) 0.0160(7) C29A 0.0277(17) 0.040(2) 0.0237(17) 0.0114(15) 0.0160(15) 0.0108(15) C30A 0.0339(19) 0.039(2) 0.0229(17) 0.0141(15) 0.0168(16) 0.0128(15) C32A 0.0224(16) 0.0339(19) 0.0289(18) 0.0094(16) 0.0144(15) 0.0060(14) C33A 0.0243(17) 0.0321(18) 0.0223(17) 0.0110(15) 0.0109(14) 0.0063(14) C30B 0.0237(15) 0.0265(15) 0.0240(16) 0.0065(13) 0.0086(13) 0.0037(12) C32B 0.0210(15) 0.0327(17) 0.0334(19) 0.0052(15) 0.0127(14) -0.0011(13) C29B 0.0192(14) 0.0265(15) 0.0230(15) 0.0033(12) 0.0081(12) 0.0030(11) C33B 0.0268(16) 0.0261(16) 0.0320(19) 0.0082(14) 0.0156(14) 0.0017(12) C34 0.0301(9) 0.0359(9) 0.0301(9) 0.0108(8) 0.0135(8) 0.0103(7) C35 0.0216(8) 0.0341(9) 0.0337(9) 0.0039(8) 0.0075(7) 0.0028(7) C36 0.0264(8) 0.0372(9) 0.0348(10) 0.0086(8) 0.0153(8) 0.0052(7) N1 0.0216(7) 0.0330(8) 0.0260(7) 0.0067(6) 0.0104(6) 0.0076(6) N2 0.0251(7) 0.0274(7) 0.0237(7) 0.0047(6) 0.0109(6) 0.0062(5) N3 0.0219(7) 0.0241(7) 0.0218(7) 0.0057(5) 0.0043(6) 0.0025(5) N4 0.0209(7) 0.0258(7) 0.0256(7) 0.0040(6) 0.0047(6) 0.0013(5) N5 0.0270(7) 0.0250(7) 0.0281(7) 0.0057(6) 0.0154(6) 0.0043(5) N6 0.0213(6) 0.0277(7) 0.0237(7) 0.0051(5) 0.0098(6) 0.0053(5) N7 0.0275(7) 0.0334(8) 0.0294(8) 0.0123(6) 0.0137(6) 0.0110(6) N8 0.0252(7) 0.0273(7) 0.0253(7) 0.0030(6) 0.0053(6) 0.0050(6) N9 0.0263(8) 0.0482(10) 0.0452(10) 0.0033(8) 0.0157(8) -0.0029(7) S1 0.0820(10) 0.0573(8) 0.0914(11) -0.0044(7) 0.0675(10) -0.0071(6) C37 0.0249(16) 0.0234(15) 0.054(2) 0.0012(15) 0.0164(17) -0.0008(12) S2 0.0220(6) 0.0593(9) 0.1138(14) -0.0458(9) 0.0150(7) -0.0040(5) C38 0.029(2) 0.0267(18) 0.062(3) -0.0065(19) 0.025(2) 0.0000(15) Cd1 0.01569(8) 0.02081(8) 0.01730(8) 0.00135(6) 0.00005(6) -0.00067(5) Cu1 0.01907(10) 0.02632(11) 0.02214(11) 0.00616(7) 0.00855(8) 0.00644(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 N1 1.334(2) . ? C1 C2 1.411(3) . ? C1 H1 0.9300 . ? C2 C3 1.379(3) . ? C2 H2 0.9300 . ? C3 C4 1.412(3) . ? C3 H3 0.9300 . ? C4 N1 1.396(2) . ? C4 C5 1.412(3) . ? C5 C6 1.396(3) . ? C5 C10 1.487(2) . ? C6 N2 1.396(2) . ? C6 C7 1.417(2) . ? C7 C8 1.367(3) . ? C7 H7 0.9300 . ? C8 C9 1.410(3) . ? C8 H8 0.9300 . ? C9 N2 1.335(2) . ? C9 H9 0.9300 . ? C10 C11 1.386(2) . ? C10 C15 1.393(3) . ? C11 C12 1.396(2) . ? C11 H11 0.9300 . ? C12 C13 1.370(2) . ? C12 H12 0.9300 . ? C13 C14 1.384(2) . ? C13 N3 1.429(2) . ? C14 C15 1.387(2) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 N4 1.316(2) . ? C16 N3 1.355(2) . ? C16 H16 0.9300 . ? C17 C18 1.361(2) . ? C17 N4 1.376(2) . ? C17 H17 0.9300 . ? C18 N3 1.382(2) . ? C18 H18 0.9300 . ? C19 N5 1.339(2) . ? C19 C20 1.415(3) . ? C19 H19 0.9300 . ? C20 C21 1.369(3) . ? C20 H20 0.9300 . ? C21 C22 1.426(2) . ? C21 H21 0.9300 . ? C22 N5 1.389(2) . ? C22 C23 1.408(3) . ? C23 C24 1.398(2) . ? C23 C28 1.492(2) . ? C24 N6 1.392(2) . ? C24 C25 1.415(3) . ? C25 C26 1.376(3) . ? C25 H25 0.9300 . ? C26 C27 1.408(3) . ? C26 H26 0.9300 . ? C27 N6 1.342(2) . ? C27 H27 0.9300 . ? C28 C33B 1.302(4) . ? C28 C33A 1.381(4) . ? C28 C29A 1.451(4) . ? C28 C29B 1.468(4) . ? C31 C32B 1.301(4) . ? C31 C32A 1.350(4) . ? C31 C30A 1.397(4) . ? C31 N7 1.425(2) . ? C31 C30B 1.514(4) . ? C29A C30A 1.383(5) . ? C29A H29A 0.9300 . ? C30A H30A 0.9300 . ? C32A C33A 1.389(4) . ? C32A H32A 0.9300 . ? C33A H33A 0.9300 . ? C30B C29B 1.392(4) . ? C30B H30B 0.9300 . ? C32B C33B 1.388(5) . ? C32B H32B 0.9300 . ? C29B H29B 0.9300 . ? C33B H33B 0.9300 . ? C34 N8 1.313(2) . ? C34 N7 1.353(2) . ? C34 H34 0.9300 . ? C35 C36 1.354(2) . ? C35 N8 1.373(2) . ? C35 H35 0.9300 . ? C36 N7 1.378(2) . ? C36 H36 0.9300 . ? N1 Cu1 1.9427(14) . ? N2 Cu1 1.9467(14) . ? N4 Cd1 2.3177(14) . ? N5 Cu1 1.9390(14) . ? N6 Cu1 1.9486(15) . ? N8 Cd1 2.3202(14) 4_646 ? N9 C37 1.084(5) . ? N9 C38 1.120(5) . ? N9 Cd1 2.3745(19) . ? S1 C37 1.635(5) . ? S2 C38 1.655(5) . ? S2 S2 2.181(4) 2_554 ? Cd1 N4 2.3177(14) 7 ? Cd1 N8 2.3202(14) 6_454 ? Cd1 N8 2.3202(14) 4_656 ? Cd1 N9 2.3745(19) 7 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.20(17) . . ? N1 C1 H1 124.4 . . ? C2 C1 H1 124.4 . . ? C3 C2 C1 106.36(17) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.00(16) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C3 108.83(15) . . ? N1 C4 C5 123.79(15) . . ? C3 C4 C5 127.34(16) . . ? C6 C5 C4 125.65(15) . . ? C6 C5 C10 117.88(15) . . ? C4 C5 C10 116.44(15) . . ? C5 C6 N2 123.14(15) . . ? C5 C6 C7 128.55(16) . . ? N2 C6 C7 108.28(16) . . ? C8 C7 C6 107.45(16) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 106.42(16) . . ? C7 C8 H8 126.8 . . ? C9 C8 H8 126.8 . . ? N2 C9 C8 111.18(16) . . ? N2 C9 H9 124.4 . . ? C8 C9 H9 124.4 . . ? C11 C10 C15 118.38(16) . . ? C11 C10 C5 121.39(16) . . ? C15 C10 C5 120.18(15) . . ? C10 C11 C12 120.69(17) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 119.66(16) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 120.92(16) . . ? C12 C13 N3 119.79(15) . . ? C14 C13 N3 119.28(15) . . ? C13 C14 C15 118.97(17) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C14 C15 C10 121.30(17) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? N4 C16 N3 111.32(15) . . ? N4 C16 H16 124.3 . . ? N3 C16 H16 124.3 . . ? C18 C17 N4 109.72(16) . . ? C18 C17 H17 125.1 . . ? N4 C17 H17 125.1 . . ? C17 C18 N3 105.97(16) . . ? C17 C18 H18 127.0 . . ? N3 C18 H18 127.0 . . ? N5 C19 C20 111.30(17) . . ? N5 C19 H19 124.4 . . ? C20 C19 H19 124.4 . . ? C21 C20 C19 106.16(17) . . ? C21 C20 H20 126.9 . . ? C19 C20 H20 126.9 . . ? C20 C21 C22 107.38(16) . . ? C20 C21 H21 126.3 . . ? C22 C21 H21 126.3 . . ? N5 C22 C23 122.83(15) . . ? N5 C22 C21 108.40(16) . . ? C23 C22 C21 128.77(16) . . ? C24 C23 C22 125.61(15) . . ? C24 C23 C28 117.08(16) . . ? C22 C23 C28 117.27(16) . . ? N6 C24 C23 124.04(16) . . ? N6 C24 C25 108.40(16) . . ? C23 C24 C25 127.55(16) . . ? C26 C25 C24 107.32(16) . . ? C26 C25 H25 126.3 . . ? C24 C25 H25 126.3 . . ? C25 C26 C27 106.47(17) . . ? C25 C26 H26 126.8 . . ? C27 C26 H26 126.8 . . ? N6 C27 C26 110.83(16) . . ? N6 C27 H27 124.6 . . ? C26 C27 H27 124.6 . . ? C33B C28 C33A 46.5(2) . . ? C33B C28 C29A 89.2(2) . . ? C33A C28 C29A 115.1(2) . . ? C33B C28 C29B 120.7(2) . . ? C33A C28 C29B 94.9(2) . . ? C29A C28 C29B 66.7(2) . . ? C33B C28 C23 120.0(2) . . ? C33A C28 C23 121.79(19) . . ? C29A C28 C23 121.39(19) . . ? C29B C28 C23 118.75(19) . . ? C32B C31 C32A 48.7(2) . . ? C32B C31 C30A 90.1(2) . . ? C32A C31 C30A 122.0(2) . . ? C32B C31 N7 123.8(2) . . ? C32A C31 N7 119.9(2) . . ? C30A C31 N7 117.0(2) . . ? C32B C31 C30B 117.6(2) . . ? C32A C31 C30B 95.0(2) . . ? C30A C31 C30B 66.9(2) . . ? N7 C31 C30B 118.21(19) . . ? C30A C29A C28 121.0(3) . . ? C30A C29A H29A 119.5 . . ? C28 C29A H29A 119.5 . . ? C29A C30A C31 117.9(3) . . ? C29A C30A H30A 121.0 . . ? C31 C30A H30A 121.0 . . ? C31 C32A C33A 118.3(3) . . ? C31 C32A H32A 120.8 . . ? C33A C32A H32A 120.8 . . ? C28 C33A C32A 123.2(3) . . ? C28 C33A H33A 118.4 . . ? C32A C33A H33A 118.4 . . ? C29B C30B C31 118.6(3) . . ? C29B C30B H30B 120.7 . . ? C31 C30B H30B 120.7 . . ? C31 C32B C33B 123.4(3) . . ? C31 C32B H32B 118.3 . . ? C33B C32B H32B 118.3 . . ? C30B C29B C28 117.1(3) . . ? C30B C29B H29B 121.4 . . ? C28 C29B H29B 121.4 . . ? C28 C33B C32B 121.6(3) . . ? C28 C33B H33B 119.2 . . ? C32B C33B H33B 119.2 . . ? N8 C34 N7 111.44(17) . . ? N8 C34 H34 124.3 . . ? N7 C34 H34 124.3 . . ? C36 C35 N8 109.98(16) . . ? C36 C35 H35 125.0 . . ? N8 C35 H35 125.0 . . ? C35 C36 N7 106.00(16) . . ? C35 C36 H36 127.0 . . ? N7 C36 H36 127.0 . . ? C1 N1 C4 106.59(14) . . ? C1 N1 Cu1 126.52(12) . . ? C4 N1 Cu1 126.01(12) . . ? C9 N2 C6 106.65(14) . . ? C9 N2 Cu1 125.81(12) . . ? C6 N2 Cu1 127.20(12) . . ? C16 N3 C18 106.94(14) . . ? C16 N3 C13 126.86(15) . . ? C18 N3 C13 126.17(15) . . ? C16 N4 C17 106.04(14) . . ? C16 N4 Cd1 127.34(12) . . ? C17 N4 Cd1 126.57(11) . . ? C19 N5 C22 106.74(14) . . ? C19 N5 Cu1 125.12(12) . . ? C22 N5 Cu1 127.59(12) . . ? C27 N6 C24 106.96(15) . . ? C27 N6 Cu1 125.63(12) . . ? C24 N6 Cu1 126.05(12) . . ? C34 N7 C36 106.79(15) . . ? C34 N7 C31 125.68(16) . . ? C36 N7 C31 127.52(15) . . ? C34 N8 C35 105.79(15) . . ? C34 N8 Cd1 124.65(13) . 4_646 ? C35 N8 Cd1 129.52(11) . 4_646 ? C37 N9 C38 72.9(3) . . ? C37 N9 Cd1 145.5(3) . . ? C38 N9 Cd1 141.4(3) . . ? N9 C37 S1 176.0(3) . . ? C38 S2 S2 118.4(2) . 2_554 ? N9 C38 S2 170.8(5) . . ? N4 Cd1 N4 180.00(5) . 7 ? N4 Cd1 N8 90.20(5) . 6_454 ? N4 Cd1 N8 89.80(5) 7 6_454 ? N4 Cd1 N8 89.80(5) . 4_656 ? N4 Cd1 N8 90.20(5) 7 4_656 ? N8 Cd1 N8 180.00(8) 6_454 4_656 ? N4 Cd1 N9 88.65(6) . 7 ? N4 Cd1 N9 91.35(6) 7 7 ? N8 Cd1 N9 90.59(6) 6_454 7 ? N8 Cd1 N9 89.41(6) 4_656 7 ? N4 Cd1 N9 91.35(6) . . ? N4 Cd1 N9 88.65(6) 7 . ? N8 Cd1 N9 89.41(6) 6_454 . ? N8 Cd1 N9 90.59(6) 4_656 . ? N9 Cd1 N9 180.00(10) 7 . ? N5 Cu1 N1 141.77(6) . . ? N5 Cu1 N2 98.10(6) . . ? N1 Cu1 N2 92.69(6) . . ? N5 Cu1 N6 92.65(6) . . ? N1 Cu1 N6 101.19(6) . . ? N2 Cu1 N6 141.76(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.365 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.085 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 0.577 0.250 -0.173 1090 238 ' ' 2 0.077 0.750 -0.173 1090 238 ' ' _platon_squeeze_details ; The disordered solvent molecules are a mixture of DMF, MeOH and H2O. ; #===END