# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_address ? _publ_contact_author_email beauvais@sciences.sdsu.edu _publ_contact_author_phone ? _publ_contact_author_name 'Laurance Beauvais' loop_ _publ_author_name 'Laurance Beauvais' 'Nathan Smythe' 'Derek Butler' 'Curtis Moore' 'William McGowan' 'Arnold Rheingold' # Attachment '- Structure_1 new.cif' data_structure_1new _database_code_depnum_ccdc_archive 'CCDC 865035' #TrackingRef '- Structure_1 new.cif' _audit_creation_date 2012-02-21 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H26.41 Cd1.07 N4 O9,3(C5 H11 N1 O1), (H2 O1), (C5, H11, N1)' _chemical_formula_sum 'C57 H53.32 Cd1.08 N6 O12' _chemical_formula_weight 1135.33 _chemical_melting_point ? 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' Cd Cd -0.8075 1.2024 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x, -y-1/2, z-1/2' _cell_length_a 18.170(3) _cell_length_b 9.3856(17) _cell_length_c 36.028(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.797(10) _cell_angle_gamma 90.00 _cell_volume 5781.0(17) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9889 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.54 _cell_measurement_theta_min 2.38 _exptl_absorpt_coefficient_mu 0.468 _exptl_absorpt_correction_T_max 0.9121 _exptl_absorpt_correction_T_min 0.8458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular blocks' _exptl_crystal_F_000 2340 _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_number 110880 _diffrn_reflns_theta_full 28.28 _diffrn_reflns_theta_max 28.28 _diffrn_reflns_theta_min 1.19 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'MO K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _reflns_number_gt 10447 _reflns_number_total 14359 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 13.974 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.262 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.465 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 570 _refine_ls_number_reflns 14359 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1609 _refine_ls_R_factor_gt 0.1434 _refine_ls_restrained_S_all 1.481 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3502 _refine_ls_wR_factor_ref 0.3645 _refine_special_details ; 'CHEMW03_2_A Alert-added in atoms found using SQUEEZE' 'DIFMX01_ALERT_2_A-electron density is due to disorder near Cd structural site, caused by crystal packing' 'PLAT043_ALERT_1_A-added atoms found using SQUEEZE' 'PLAT_094__ALERT_2_A-ratio residual density casued by disorder of crystal packing' 'PLAT097_97_ALERT_A_2-Positive residual density located near Cd structral site casued by crystal packing disorder' 'PLAT602_ALERT-A_2-Large void typical of MOFs, treated with SQUEEZE' 'PLAT939_ALERT_3_A-Large weight associated with large void space' 'the following constraints were used to better model disorder, DFIX AFIX 66, ISOR, and HFIX to determine Hydrogen atoms' Refinement of F^2^ against ALL reflections. The weighted R- 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 0.519 -0.047 0.009 2467 824 '12[HCON(C2H5)2]4(C2H5)2NH 4H2' _platon_squeeze_details 'SQUEEZE was performed using PLATON to account for disordered solvent molecules and counter cations. The electron density found in each cavity correlates to a final count of 3 molecules of HCON(C2H5)2, 2 H2Os, and 1 (C2H5)2NH+' 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.56449(3) 1.34695(4) 0.219673(13) 0.03426(19) Uani 1 1 d . . . Cd2 Cd 0.0329(5) 0.7756(12) -0.0210(3) 0.066(4) Uani 0.070(3) 1 d PU A 1 O9 O 0.5234(3) 1.5492(6) 0.23822(17) 0.0637(14) Uani 1 1 d U . . O101 O 0.6875(3) 1.3677(5) 0.27536(15) 0.0436(11) Uani 1 1 d . . . O102 O 0.6033(2) 1.2055(6) 0.27591(14) 0.0501(12) Uani 1 1 d . . . O201 O -0.3421(4) 0.8117(8) 0.1229(2) 0.0762(17) Uani 1 1 d U . . O202 O -0.2377(5) 0.8032(9) 0.1752(2) 0.096(3) Uani 1 1 d . . . O301 O 0.4535(3) 1.3715(5) 0.15627(13) 0.0424(10) Uani 1 1 d . . . O302 O 0.4529(3) 1.2105(6) 0.19934(12) 0.0488(12) Uani 1 1 d . . . O401 O 0.6360(3) 1.4461(5) 0.18276(13) 0.0392(9) Uani 1 1 d . . . O402 O 0.6302(3) 1.2149(5) 0.18621(14) 0.0451(11) Uani 1 1 d . . . N1 N -0.0666(3) 0.6601(5) -0.02038(14) 0.0319(10) Uani 1 1 d . . . H1 H -0.0269 0.7113 -0.0216 0.038 Uiso 0.64(8) 1 calc PR A 2 N2 N 0.0457(3) 0.8499(5) 0.03446(15) 0.0339(11) Uani 1 1 d . . . H2 H 0.0474 0.7946 0.0150 0.041 Uiso 0.64(8) 1 calc PR A 2 N3 N 0.1459(3) 0.8342(5) -0.01367(16) 0.0366(11) Uani 1 1 d . . . H3 H 0.0963 0.8139 -0.0182 0.044 Uiso 0.50 1 calc PR A 2 N4 N 0.0320(3) 0.6526(5) -0.07003(16) 0.0350(11) Uani 1 1 d . . . H4 H 0.0398 0.6798 -0.0456 0.042 Uiso 0.64(8) 1 calc PR A 2 C1 C -0.0953(3) 0.5355(7) -0.08402(17) 0.0357(12) Uani 1 1 d . . . C2 C -0.1068(3) 0.5620(7) -0.04770(17) 0.0348(12) Uani 1 1 d . A . C3 C -0.1640(3) 0.4961(7) -0.03459(19) 0.0415(15) Uani 1 1 d . . . H3A H -0.1989 0.4220 -0.0475 0.050 Uiso 1 1 calc R A . C4 C -0.1591(3) 0.5617(8) 0.00102(17) 0.0422(15) Uani 1 1 d . A . H4A H -0.1903 0.5415 0.0169 0.051 Uiso 1 1 calc R . . C5 C -0.0974(4) 0.6662(6) 0.00908(18) 0.0366(13) Uani 1 1 d . A . C6 C -0.0776(3) 0.7645(6) 0.04051(15) 0.0301(11) Uani 1 1 d . . . C7 C -0.0130(3) 0.8527(7) 0.05029(19) 0.0388(14) Uani 1 1 d . A . C8 C 0.0056(3) 0.9684(8) 0.07959(17) 0.0411(14) Uani 1 1 d . . . H8 H -0.0264 0.9998 0.0940 0.049 Uiso 1 1 calc R A . C9 C 0.0765(4) 1.0223(7) 0.08238(17) 0.0374(13) Uani 1 1 d . A . H9 H 0.1043 1.0953 0.0998 0.045 Uiso 1 1 calc R . . C10 C 0.1013(3) 0.9476(6) 0.05395(16) 0.0334(12) Uani 1 1 d . A . C11 C 0.1734(3) 0.9651(6) 0.04810(16) 0.0299(11) Uani 1 1 d . . . C12 C 0.1943(3) 0.9052(6) 0.01812(18) 0.0346(12) Uani 1 1 d . A . C13 C 0.2727(4) 0.9100(8) 0.0150(2) 0.0491(16) Uani 1 1 d . . . H13 H 0.3180 0.9521 0.0333 0.059 Uiso 1 1 calc R A . C14 C 0.2682(4) 0.8440(7) -0.0185(3) 0.0519(19) Uani 1 1 d . A . H14 H 0.3100 0.8287 -0.0283 0.062 Uiso 1 1 calc R . . C15 C 0.1881(4) 0.8004(8) -0.0371(2) 0.0459(15) Uani 1 1 d . A . C16 C 0.1580(4) 0.7227(7) -0.0741(2) 0.0417(15) Uani 1 1 d . . . C17 C 0.0823(4) 0.6708(8) -0.0898(2) 0.0469(16) Uani 1 1 d . A . C18 C 0.0463(5) 0.6208(9) -0.1294(2) 0.058(2) Uani 1 1 d . . . H18 H 0.0683 0.6237 -0.1498 0.070 Uiso 1 1 calc R A . C19 C -0.0247(4) 0.5686(8) -0.13226(19) 0.0465(16) Uani 1 1 d . A . H19 H -0.0622 0.5287 -0.1551 0.056 Uiso 1 1 calc R . . C20 C -0.0329(3) 0.5849(6) -0.09423(17) 0.0346(12) Uani 1 1 d . A . C100 C -0.1568(3) 0.4505(7) -0.11447(16) 0.0348(12) Uani 1 1 d . A . C101 C -0.1384(3) 0.3288(6) -0.1302(2) 0.0358(13) Uani 1 1 d . . . H101 H -0.0872 0.2903 -0.1195 0.043 Uiso 1 1 calc R A . C102 C -0.1939(3) 0.2597(6) -0.16202(17) 0.0307(11) Uani 1 1 d . A . H102 H -0.1797 0.1783 -0.1737 0.037 Uiso 1 1 calc R . . C103 C -0.2706(3) 0.3120(7) -0.17635(17) 0.0337(12) Uani 1 1 d . . . C104 C -0.2902(4) 0.4299(8) -0.15888(19) 0.0453(15) Uani 1 1 d . A . H104 H -0.3425 0.4642 -0.1679 0.054 Uiso 1 1 calc R . . C105 C -0.2339(4) 0.4989(8) -0.1281(2) 0.0504(18) Uani 1 1 d . . . H105 H -0.2480 0.5799 -0.1162 0.061 Uiso 1 1 calc R A . C106 C 0.6702(3) 1.2580(6) 0.28928(17) 0.0332(12) Uani 1 1 d . . . C200 C -0.1283(3) 0.7718(7) 0.06561(17) 0.0353(12) Uani 1 1 d D A . C201 C -0.2086(4) 0.7938(9) 0.04965(19) 0.0498(17) Uani 1 1 d . . . H201 H -0.2323 0.8050 0.0219 0.060 Uiso 1 1 calc R A . C202 C -0.2545(4) 0.7996(10) 0.0733(2) 0.058(2) Uani 1 1 d . A . H202 H -0.3096 0.8087 0.0613 0.070 Uiso 1 1 calc R . . C203 C -0.2237(5) 0.7928(7) 0.1122(2) 0.0511(19) Uani 1 1 d D . . C204 C -0.1422(4) 0.7707(9) 0.1294(2) 0.0545(19) Uani 1 1 d . A . H204 H -0.1191 0.7641 0.1573 0.065 Uiso 1 1 calc R . . C205 C -0.0962(4) 0.7589(9) 0.10632(19) 0.055(2) Uani 1 1 d D . . H205 H -0.0417 0.7416 0.1183 0.066 Uiso 1 1 calc R A . C206 C -0.2724(6) 0.8016(8) 0.1391(3) 0.062(2) Uani 1 1 d D A . C300 C 0.2347(3) 1.0501(6) 0.07889(16) 0.0337(12) Uani 1 1 d D A . C301 C 0.2614(4) 1.0099(8) 0.11797(19) 0.0512(18) Uani 1 1 d . . . H301 H 0.2363 0.9326 0.1259 0.061 Uiso 1 1 calc R A . C302 C 0.3227(4) 1.0769(8) 0.14598(18) 0.0481(17) Uani 1 1 d . A . H302 H 0.3404 1.0438 0.1725 0.058 Uiso 1 1 calc R . . C303 C 0.3583(3) 1.1914(6) 0.13560(15) 0.0300(11) Uani 1 1 d . . . C304 C 0.3284(4) 1.2377(6) 0.09710(16) 0.0335(12) Uani 1 1 d . A . H304 H 0.3499 1.3209 0.0898 0.040 Uiso 1 1 calc R . . C305 C 0.2692(4) 1.1687(6) 0.06916(16) 0.0349(13) Uani 1 1 d D . . H305 H 0.2515 1.2026 0.0427 0.042 Uiso 1 1 calc R A . C306 C 0.4244(3) 1.2624(6) 0.16558(16) 0.0335(12) Uani 1 1 d . A . C400 C 0.2092(4) 0.7111(6) -0.0985(2) 0.0397(14) Uani 1 1 d . A . C401 C 0.2346(5) 0.8325(6) -0.1138(2) 0.0477(18) Uani 1 1 d . . . H401 H 0.2195 0.9240 -0.1076 0.057 Uiso 1 1 calc R A . C402 C 0.2797(4) 0.8231(6) -0.1369(2) 0.0470(17) Uani 1 1 d . A . H402 H 0.2974 0.9068 -0.1462 0.056 Uiso 1 1 calc R . . C403 C 0.2997(4) 0.6899(6) -0.14692(19) 0.0375(13) Uani 1 1 d . . . C404 C 0.2725(5) 0.5678(7) -0.1340(3) 0.063(2) Uani 1 1 d . A . H404 H 0.2844 0.4765 -0.1419 0.076 Uiso 1 1 calc R . . C405 C 0.2273(5) 0.5796(7) -0.1094(3) 0.057(2) Uani 1 1 d . . . H405 H 0.2093 0.4962 -0.1003 0.068 Uiso 1 1 calc R A . C406 C 0.6526(3) 1.3237(6) 0.17366(17) 0.0313(12) 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 0.0378(3) 0.0321(3) 0.0367(3) -0.00079(16) 0.0176(2) -0.00099(16) Cd2 0.056(5) 0.093(5) 0.060(5) -0.022(3) 0.035(3) -0.020(3) O9 0.060(2) 0.067(2) 0.060(2) -0.0163(16) 0.0143(16) 0.0139(16) O101 0.030(2) 0.043(2) 0.046(3) -0.0029(19) -0.0027(19) 0.0015(18) O102 0.023(2) 0.083(3) 0.038(2) 0.000(2) 0.0011(18) -0.017(2) O201 0.072(2) 0.078(2) 0.087(2) 0.0034(18) 0.0385(18) 0.0043(17) O202 0.152(8) 0.090(5) 0.087(5) -0.001(4) 0.094(6) 0.013(5) O301 0.045(3) 0.041(2) 0.035(2) -0.0009(18) 0.0043(19) -0.0035(19) O302 0.044(3) 0.068(3) 0.025(2) 0.016(2) -0.0013(18) -0.010(2) O401 0.046(2) 0.037(2) 0.042(2) 0.0007(18) 0.0238(19) 0.0002(19) O402 0.054(3) 0.040(2) 0.053(3) -0.006(2) 0.033(2) -0.009(2) N1 0.030(2) 0.037(3) 0.025(2) 0.0058(18) 0.0046(19) 0.0025(19) N2 0.023(2) 0.049(3) 0.026(2) 0.001(2) 0.0033(18) 0.0001(19) N3 0.032(3) 0.041(3) 0.038(3) -0.005(2) 0.014(2) -0.004(2) N4 0.031(3) 0.041(3) 0.033(3) -0.004(2) 0.012(2) -0.005(2) C1 0.028(3) 0.043(3) 0.029(3) 0.007(2) 0.001(2) 0.002(2) C2 0.023(2) 0.047(3) 0.033(3) 0.010(2) 0.007(2) 0.005(2) C3 0.022(3) 0.056(4) 0.040(3) 0.018(3) 0.002(2) -0.009(3) C4 0.027(3) 0.068(4) 0.029(3) 0.014(3) 0.006(2) 0.001(3) C5 0.027(3) 0.046(3) 0.032(3) 0.012(2) 0.003(2) 0.008(2) C6 0.025(2) 0.046(3) 0.022(2) 0.002(2) 0.013(2) 0.003(2) C7 0.023(3) 0.055(4) 0.033(3) 0.010(3) 0.002(2) 0.012(2) C8 0.032(3) 0.063(4) 0.028(3) -0.002(3) 0.010(2) 0.016(3) C9 0.036(3) 0.045(3) 0.028(3) -0.002(2) 0.006(2) 0.012(3) C10 0.029(3) 0.039(3) 0.030(3) 0.005(2) 0.007(2) 0.009(2) C11 0.027(3) 0.033(3) 0.029(3) 0.009(2) 0.008(2) 0.006(2) C12 0.029(3) 0.036(3) 0.040(3) 0.001(2) 0.014(2) 0.000(2) C13 0.032(3) 0.061(4) 0.054(4) -0.012(3) 0.015(3) -0.011(3) C14 0.041(4) 0.052(4) 0.072(5) -0.022(3) 0.032(4) -0.009(3) C15 0.041(4) 0.050(4) 0.050(4) -0.011(3) 0.020(3) -0.010(3) C16 0.049(4) 0.030(3) 0.058(4) -0.011(3) 0.034(3) -0.006(3) C17 0.044(4) 0.055(4) 0.051(4) -0.009(3) 0.028(3) -0.009(3) C18 0.076(5) 0.061(4) 0.053(4) -0.016(4) 0.042(4) -0.017(4) C19 0.048(4) 0.059(4) 0.037(3) -0.012(3) 0.020(3) -0.015(3) C20 0.034(3) 0.034(3) 0.037(3) -0.006(2) 0.013(2) 0.000(2) C100 0.024(3) 0.047(3) 0.029(3) 0.012(2) 0.003(2) 0.004(2) C101 0.012(2) 0.038(3) 0.049(3) 0.010(2) 0.000(2) 0.006(2) C102 0.020(2) 0.031(3) 0.038(3) 0.012(2) 0.006(2) 0.004(2) C103 0.022(2) 0.046(3) 0.031(3) 0.011(2) 0.006(2) 0.009(2) C104 0.026(3) 0.063(4) 0.039(3) -0.001(3) 0.001(2) 0.015(3) C105 0.037(3) 0.062(4) 0.040(3) -0.009(3) -0.004(3) 0.022(3) C106 0.026(3) 0.041(3) 0.030(3) -0.003(2) 0.007(2) -0.003(2) C200 0.034(3) 0.045(3) 0.030(3) 0.004(2) 0.015(2) 0.002(3) C201 0.034(3) 0.086(5) 0.029(3) 0.011(3) 0.010(3) 0.015(3) C202 0.041(4) 0.093(6) 0.048(4) 0.014(4) 0.026(3) 0.024(4) C203 0.072(5) 0.029(3) 0.077(5) -0.016(3) 0.058(4) -0.016(3) C204 0.051(4) 0.083(6) 0.032(3) -0.001(3) 0.018(3) -0.001(4) C205 0.034(3) 0.099(6) 0.029(3) -0.007(3) 0.007(3) -0.008(4) C206 0.096(7) 0.027(3) 0.090(6) -0.009(4) 0.066(6) -0.008(4) C300 0.029(3) 0.041(3) 0.027(3) 0.007(2) 0.004(2) 0.009(2) C301 0.043(4) 0.071(5) 0.035(3) 0.024(3) 0.009(3) -0.010(3) C302 0.037(3) 0.070(5) 0.031(3) 0.023(3) 0.002(2) -0.009(3) C303 0.032(3) 0.036(3) 0.019(2) 0.007(2) 0.004(2) 0.003(2) C304 0.050(3) 0.025(3) 0.025(3) 0.005(2) 0.010(2) 0.002(2) C305 0.048(3) 0.034(3) 0.015(2) 0.006(2) 0.001(2) 0.005(2) C306 0.038(3) 0.039(3) 0.026(3) 0.003(2) 0.013(2) 0.007(2) C400 0.057(4) 0.016(2) 0.060(4) 0.003(3) 0.038(3) 0.001(3) C401 0.064(5) 0.018(3) 0.080(5) -0.005(3) 0.049(4) 0.000(3) C402 0.059(4) 0.017(3) 0.078(5) 0.009(3) 0.040(4) 0.000(2) C403 0.046(4) 0.027(3) 0.043(3) -0.005(2) 0.019(3) 0.003(2) C404 0.097(6) 0.020(3) 0.105(6) 0.006(3) 0.077(6) 0.006(3) C405 0.087(6) 0.024(3) 0.088(6) -0.005(3) 0.067(5) -0.006(3) C406 0.031(3) 0.035(3) 0.030(3) 0.001(2) 0.013(2) 0.004(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 Cd1 O9 2.224(5) . ? Cd1 O101 2.454(4) . ? Cd1 O102 2.323(5) . ? Cd1 O301 2.493(4) . ? Cd1 O302 2.299(5) . ? Cd1 O401 2.344(4) . ? Cd1 O402 2.321(5) . ? Cd2 N1 2.115(10) . ? Cd2 N2 2.055(10) . ? Cd2 N3 2.054(10) . ? Cd2 N4 2.104(10) . ? O101 C106 1.232(7) . ? O102 C106 1.247(7) . ? O201 C206 1.206(11) . ? O202 C206 1.237(12) . ? O301 C306 1.250(7) . ? O302 C306 1.248(7) . ? O401 C406 1.258(7) . ? O402 C406 1.239(7) . ? N1 H1 0.8800 . ? N1 C2 1.365(8) . ? N1 C5 1.359(8) . ? N2 H2 0.8800 . ? N2 C7 1.369(8) . ? N2 C10 1.369(8) . ? N3 H3 0.8800 . ? N3 C12 1.359(8) . ? N3 C15 1.357(8) . ? N4 H4 0.8800 . ? N4 C17 1.348(8) . ? N4 C20 1.363(8) . ? C1 C2 1.415(8) . ? C1 C20 1.385(8) . ? C1 C100 1.502(8) . ? C2 C3 1.422(8) . ? C3 H3A 0.9500 . ? C3 C4 1.398(9) . ? C4 H4A 0.9500 . ? C4 C5 1.442(9) . ? C5 C6 1.410(8) . ? C6 C7 1.382(9) . ? C6 C200 1.494(8) . ? C7 C8 1.472(9) . ? C8 H8 0.9500 . ? C8 C9 1.355(9) . ? C9 H9 0.9500 . ? C9 C10 1.434(8) . ? C10 C11 1.406(8) . ? C11 C12 1.380(8) . ? C11 C300 1.507(8) . ? C12 C13 1.467(8) . ? C13 H13 0.9500 . ? C13 C14 1.335(10) . ? C14 H14 0.9500 . ? C14 C15 1.440(10) . ? C15 C16 1.453(9) . ? C16 C17 1.387(10) . ? C16 C400 1.487(8) . ? C17 C18 1.429(11) . ? C18 H18 0.9500 . ? C18 C19 1.351(10) . ? C19 H19 0.9500 . ? C19 C20 1.436(8) . ? C100 C101 1.367(9) . ? C100 C105 1.395(8) . ? C101 H101 0.9500 . ? C101 C102 1.402(8) . ? C102 H102 0.9500 . ? C102 C103 1.401(7) . ? C103 C104 1.378(9) . ? C103 C106 1.490(8) 4_475 ? C104 H104 0.9500 . ? C104 C105 1.388(9) . ? C105 H105 0.9500 . ? C106 C103 1.490(8) 4_676 ? C200 C201 1.391(9) . ? C200 C205 1.388(8) . ? C201 H201 0.9500 . ? C201 C202 1.381(9) . ? C202 H202 0.9500 . ? C202 C203 1.324(11) . ? C203 C204 1.413(11) . ? C203 C206 1.520(9) . ? C204 H204 0.9500 . ? C204 C205 1.370(10) . ? C205 H205 0.9500 . ? C300 C301 1.377(8) . ? C300 C305 1.380(8) . ? C301 H301 0.9500 . ? C301 C302 1.377(10) . ? C302 H302 0.9500 . ? C302 C303 1.370(9) . ? C303 C304 1.377(7) . ? C303 C306 1.474(8) . ? C304 H304 0.9500 . ? C304 C305 1.362(8) . ? C305 H305 0.9500 . ? C400 C401 1.408(8) . ? C400 C405 1.368(8) . ? C401 H401 0.9500 . ? C401 C402 1.357(10) . ? C402 H402 0.9500 . ? C402 C403 1.383(8) . ? C403 C404 1.389(9) . ? C403 C406 1.504(8) 3_675 ? C404 H404 0.9500 . ? C404 C405 1.401(9) . ? C405 H405 0.9500 . ? C406 C403 1.504(8) 3_675 ? 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 O9 Cd1 O101 89.56(18) . . ? O9 Cd1 O102 105.0(2) . . ? O9 Cd1 O301 86.95(18) . . ? O9 Cd1 O302 102.8(2) . . ? O9 Cd1 O401 98.0(2) . . ? O9 Cd1 O402 153.6(2) . . ? O101 Cd1 O301 166.35(17) . . ? O102 Cd1 O101 53.77(16) . . ? O102 Cd1 O301 139.83(15) . . ? O102 Cd1 O401 131.20(16) . . ? O302 Cd1 O101 139.97(16) . . ? O302 Cd1 O102 86.20(15) . . ? O302 Cd1 O301 53.64(15) . . ? O302 Cd1 O401 129.74(16) . . ? O302 Cd1 O402 95.19(19) . . ? O401 Cd1 O101 84.59(17) . . ? O401 Cd1 O301 82.84(16) . . ? O402 Cd1 O101 88.89(18) . . ? O402 Cd1 O102 95.18(19) . . ? O402 Cd1 O301 88.40(17) . . ? O402 Cd1 O401 55.64(16) . . ? N2 Cd2 N1 88.8(4) . . ? N2 Cd2 N4 165.5(7) . . ? N3 Cd2 N1 163.0(7) . . ? N3 Cd2 N2 90.3(4) . . ? N3 Cd2 N4 88.8(4) . . ? N4 Cd2 N1 88.0(4) . . ? C106 O101 Cd1 88.8(3) . . ? C106 O102 Cd1 94.5(4) . . ? C306 O301 Cd1 87.9(3) . . ? C306 O302 Cd1 97.1(4) . . ? C406 O401 Cd1 90.7(3) . . ? C406 O402 Cd1 92.3(4) . . ? Cd2 N1 H1 3.2 . . ? C2 N1 Cd2 126.0(5) . . ? C2 N1 H1 125.4 . . ? C5 N1 Cd2 124.6(5) . . ? C5 N1 H1 125.4 . . ? C5 N1 C2 109.3(5) . . ? Cd2 N2 H2 18.1 . . ? C7 N2 Cd2 124.4(5) . . ? C7 N2 H2 125.8 . . ? C10 N2 Cd2 123.2(5) . . ? C10 N2 H2 125.8 . . ? C10 N2 C7 108.4(5) . . ? Cd2 N3 H3 4.3 . . ? C12 N3 Cd2 125.0(5) . . ? C12 N3 H3 126.3 . . ? C15 N3 Cd2 127.5(5) . . ? C15 N3 H3 126.3 . . ? C15 N3 C12 107.3(5) . . ? Cd2 N4 H4 18.1 . . ? C17 N4 Cd2 124.1(5) . . ? C17 N4 H4 125.8 . . ? C17 N4 C20 108.4(5) . . ? C20 N4 Cd2 123.5(5) . . ? C20 N4 H4 125.8 . . ? C2 C1 C100 117.6(5) . . ? C20 C1 C2 125.2(5) . . ? C20 C1 C100 117.2(5) . . ? N1 C2 C1 125.1(5) . . ? N1 C2 C3 109.1(5) . . ? C1 C2 C3 125.7(6) . . ? C2 C3 H3A 126.7 . . ? C4 C3 C2 106.6(6) . . ? C4 C3 H3A 126.7 . . ? C3 C4 H4A 126.6 . . ? C3 C4 C5 106.8(5) . . ? C5 C4 H4A 126.6 . . ? N1 C5 C4 108.2(5) . . ? N1 C5 C6 126.5(6) . . ? C6 C5 C4 125.1(6) . . ? C5 C6 C200 118.3(5) . . ? C7 C6 C5 124.1(5) . . ? C7 C6 C200 117.6(5) . . ? N2 C7 C6 126.7(6) . . ? N2 C7 C8 106.9(5) . . ? C6 C7 C8 126.4(6) . . ? C7 C8 H8 126.0 . . ? C9 C8 C7 108.1(5) . . ? C9 C8 H8 126.0 . . ? C8 C9 H9 126.7 . . ? C8 C9 C10 106.5(5) . . ? C10 C9 H9 126.7 . . ? N2 C10 C9 109.8(5) . . ? N2 C10 C11 124.4(5) . . ? C11 C10 C9 125.7(6) . . ? C10 C11 C300 116.5(5) . . ? C12 C11 C10 126.0(5) . . ? C12 C11 C300 117.4(5) . . ? N3 C12 C11 126.0(5) . . ? N3 C12 C13 108.5(5) . . ? C11 C12 C13 125.4(6) . . ? C12 C13 H13 126.5 . . ? C14 C13 C12 107.0(6) . . ? C14 C13 H13 126.5 . . ? C13 C14 H14 126.5 . . ? C13 C14 C15 107.1(6) . . ? C15 C14 H14 126.5 . . ? N3 C15 C14 109.9(6) . . ? N3 C15 C16 124.8(6) . . ? C14 C15 C16 125.1(6) . . ? C15 C16 C400 117.6(6) . . ? C17 C16 C15 124.4(6) . . ? C17 C16 C400 117.7(6) . . ? N4 C17 C16 125.7(7) . . ? N4 C17 C18 108.8(6) . . ? C16 C17 C18 125.4(7) . . ? C17 C18 H18 126.3 . . ? C19 C18 C17 107.4(6) . . ? C19 C18 H18 126.3 . . ? C18 C19 H19 126.5 . . ? C18 C19 C20 107.0(6) . . ? C20 C19 H19 126.5 . . ? N4 C20 C1 126.5(5) . . ? N4 C20 C19 108.2(5) . . ? C1 C20 C19 125.2(5) . . ? C101 C100 C1 121.5(5) . . ? C101 C100 C105 118.9(6) . . ? C105 C100 C1 119.6(6) . . ? C100 C101 H101 119.4 . . ? C100 C101 C102 121.1(5) . . ? C102 C101 H101 119.4 . . ? C101 C102 H102 120.3 . . ? C103 C102 C101 119.3(6) . . ? C103 C102 H102 120.3 . . ? C102 C103 C106 120.0(6) . 4_475 ? C104 C103 C102 119.4(6) . . ? C104 C103 C106 120.6(5) . 4_475 ? C103 C104 H104 119.8 . . ? C103 C104 C105 120.3(5) . . ? C105 C104 H104 119.8 . . ? C100 C105 H105 119.6 . . ? C104 C105 C100 120.7(6) . . ? C104 C105 H105 119.6 . . ? O101 C106 O102 121.6(6) . . ? O101 C106 C103 119.6(5) . 4_676 ? O102 C106 C103 118.8(5) . 4_676 ? C201 C200 C6 122.1(5) . . ? C205 C200 C6 120.7(6) . . ? C205 C200 C201 117.2(6) . . ? C200 C201 H201 119.3 . . ? C202 C201 C200 121.3(6) . . ? C202 C201 H201 119.3 . . ? C201 C202 H202 119.2 . . ? C203 C202 C201 121.6(7) . . ? C203 C202 H202 119.2 . . ? C202 C203 C204 118.4(6) . . ? C202 C203 C206 123.0(8) . . ? C204 C203 C206 118.6(8) . . ? C203 C204 H204 119.6 . . ? C205 C204 C203 120.7(7) . . ? C205 C204 H204 119.6 . . ? C200 C205 H205 119.7 . . ? C204 C205 C200 120.7(7) . . ? C204 C205 H205 119.7 . . ? O201 C206 O202 125.8(8) . . ? O201 C206 C203 116.0(9) . . ? O202 C206 C203 118.1(9) . . ? C301 C300 C11 121.6(5) . . ? C301 C300 C305 116.6(5) . . ? C305 C300 C11 121.7(5) . . ? C300 C301 H301 118.6 . . ? C302 C301 C300 122.7(6) . . ? C302 C301 H301 118.6 . . ? C301 C302 H302 120.1 . . ? C303 C302 C301 119.9(5) . . ? C303 C302 H302 120.1 . . ? C302 C303 C304 117.5(5) . . ? C302 C303 C306 119.8(5) . . ? C304 C303 C306 122.7(5) . . ? C303 C304 H304 118.7 . . ? C305 C304 C303 122.5(5) . . ? C305 C304 H304 118.7 . . ? C300 C305 H305 119.7 . . ? C304 C305 C300 120.5(5) . . ? C304 C305 H305 119.7 . . ? O301 C306 C303 119.2(5) . . ? O302 C306 O301 120.5(6) . . ? O302 C306 C303 120.2(5) . . ? C401 C400 C16 121.7(5) . . ? C405 C400 C16 119.6(5) . . ? C405 C400 C401 118.5(6) . . ? C400 C401 H401 118.9 . . ? C402 C401 C400 122.2(5) . . ? C402 C401 H401 118.9 . . ? C401 C402 H402 120.5 . . ? C401 C402 C403 119.0(6) . . ? C403 C402 H402 120.5 . . ? C402 C403 C404 120.3(6) . . ? C402 C403 C406 120.1(6) . 3_675 ? C404 C403 C406 119.5(5) . 3_675 ? C403 C404 H404 120.1 . . ? C403 C404 C405 119.8(6) . . ? C405 C404 H404 120.1 . . ? C400 C405 C404 120.1(6) . . ? C400 C405 H405 120.0 . . ? C404 C405 H405 120.0 . . ? O401 C406 C403 119.0(5) . 3_675 ? O402 C406 O401 121.3(5) . . ? O402 C406 C403 119.7(5) . 3_675 ? 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 Cd1 O101 C106 O102 -11.5(6) . . . . ? Cd1 O101 C106 C103 170.2(5) . . . 4_676 ? Cd1 O102 C106 O101 12.2(7) . . . . ? Cd1 O102 C106 C103 -169.5(5) . . . 4_676 ? Cd1 O301 C306 O302 9.2(6) . . . . ? Cd1 O301 C306 C303 -167.7(5) . . . . ? Cd1 O302 C306 O301 -10.0(6) . . . . ? Cd1 O302 C306 C303 166.9(5) . . . . ? Cd1 O401 C406 O402 -1.5(6) . . . . ? Cd1 O401 C406 C403 178.4(5) . . . 3_675 ? Cd1 O402 C406 O401 1.5(6) . . . . ? Cd1 O402 C406 C403 -178.4(5) . . . 3_675 ? Cd2 N1 C2 C1 -9.4(9) . . . . ? Cd2 N1 C2 C3 173.3(5) . . . . ? Cd2 N1 C5 C4 -173.9(5) . . . . ? Cd2 N1 C5 C6 10.9(9) . . . . ? Cd2 N2 C7 C6 26.2(9) . . . . ? Cd2 N2 C7 C8 -153.5(6) . . . . ? Cd2 N2 C10 C9 155.4(5) . . . . ? Cd2 N2 C10 C11 -27.8(8) . . . . ? Cd2 N3 C12 C11 -8.7(10) . . . . ? Cd2 N3 C12 C13 172.4(6) . . . . ? Cd2 N3 C15 C14 -171.4(6) . . . . ? Cd2 N3 C15 C16 4.6(12) . . . . ? Cd2 N4 C17 C16 28.8(11) . . . . ? Cd2 N4 C17 C18 -154.2(6) . . . . ? Cd2 N4 C20 C1 -27.9(9) . . . . ? Cd2 N4 C20 C19 154.1(6) . . . . ? O9 Cd1 O101 C106 115.6(4) . . . . ? O9 Cd1 O102 C106 -84.5(4) . . . . ? O9 Cd1 O301 C306 -113.7(4) . . . . ? O9 Cd1 O302 C306 81.8(4) . . . . ? O9 Cd1 O401 C406 -178.0(4) . . . . ? O9 Cd1 O402 C406 1.7(7) . . . . ? O101 Cd1 O102 C106 -6.5(4) . . . . ? O101 Cd1 O301 C306 170.9(6) . . . . ? O101 Cd1 O302 C306 -173.3(3) . . . . ? O101 Cd1 O401 C406 93.2(4) . . . . ? O101 Cd1 O402 C406 -85.0(4) . . . . ? O102 Cd1 O101 C106 6.5(4) . . . . ? O102 Cd1 O301 C306 -3.8(5) . . . . ? O102 Cd1 O302 C306 -173.7(4) . . . . ? O102 Cd1 O401 C406 63.8(4) . . . . ? O102 Cd1 O402 C406 -138.5(4) . . . . ? O301 Cd1 O101 C106 -169.3(6) . . . . ? O301 Cd1 O102 C106 172.0(3) . . . . ? O301 Cd1 O302 C306 5.4(3) . . . . ? O301 Cd1 O401 C406 -92.2(4) . . . . ? O301 Cd1 O402 C406 81.6(4) . . . . ? O302 Cd1 O101 C106 6.0(5) . . . . ? O302 Cd1 O102 C106 173.2(4) . . . . ? O302 Cd1 O301 C306 -5.3(3) . . . . ? O302 Cd1 O401 C406 -64.0(4) . . . . ? O302 Cd1 O402 C406 134.9(4) . . . . ? O401 Cd1 O101 C106 -146.3(4) . . . . ? O401 Cd1 O102 C106 30.7(5) . . . . ? O401 Cd1 O301 C306 147.9(4) . . . . ? O401 Cd1 O302 C306 -30.2(5) . . . . ? O401 Cd1 O402 C406 -0.8(4) . . . . ? O402 Cd1 O101 C106 -90.7(4) . . . . ? O402 Cd1 O102 C106 78.4(4) . . . . ? O402 Cd1 O301 C306 92.3(4) . . . . ? O402 Cd1 O302 C306 -78.8(4) . . . . ? O402 Cd1 O401 C406 0.8(3) . . . . ? N1 Cd2 N2 C7 -20.8(7) . . . . ? N1 Cd2 N2 C10 -175.6(5) . . . . ? N1 Cd2 N3 C12 -91.1(18) . . . . ? N1 Cd2 N3 C15 82.9(19) . . . . ? N1 Cd2 N4 C17 177.3(6) . . . . ? N1 Cd2 N4 C20 22.6(7) . . . . ? N1 C2 C3 C4 2.2(7) . . . . ? N1 C5 C6 C7 -13.1(9) . . . . ? N1 C5 C6 C200 168.6(5) . . . . ? N2 Cd2 N1 C2 -171.6(5) . . . . ? N2 Cd2 N1 C5 4.0(7) . . . . ? N2 Cd2 N3 C12 -4.6(8) . . . . ? N2 Cd2 N3 C15 169.4(6) . . . . ? N2 Cd2 N4 C17 -106(2) . . . . ? N2 Cd2 N4 C20 100(2) . . . . ? N2 C7 C8 C9 -4.6(7) . . . . ? N2 C10 C11 C12 11.2(9) . . . . ? N2 C10 C11 C300 -165.0(5) . . . . ? N3 Cd2 N1 C2 -84.8(18) . . . . ? N3 Cd2 N1 C5 90.8(18) . . . . ? N3 Cd2 N2 C7 176.2(5) . . . . ? N3 Cd2 N2 C10 21.4(7) . . . . ? N3 Cd2 N4 C17 -19.3(8) . . . . ? N3 Cd2 N4 C20 -174.0(5) . . . . ? N3 C12 C13 C14 0.8(8) . . . . ? N3 C15 C16 C17 -1.2(12) . . . . ? N3 C15 C16 C400 172.2(7) . . . . ? N4 Cd2 N1 C2 -5.7(7) . . . . ? N4 Cd2 N1 C5 169.9(5) . . . . ? N4 Cd2 N2 C7 -98(2) . . . . ? N4 Cd2 N2 C10 108(2) . . . . ? N4 Cd2 N3 C12 -170.1(5) . . . . ? N4 Cd2 N3 C15 3.9(8) . . . . ? N4 C17 C18 C19 -2.0(9) . . . . ? C1 C2 C3 C4 -175.1(6) . . . . ? C1 C100 C101 C102 -172.0(5) . . . . ? C1 C100 C105 C104 173.8(6) . . . . ? C2 N1 C5 C4 2.4(6) . . . . ? C2 N1 C5 C6 -172.8(5) . . . . ? C2 C1 C20 N4 8.0(10) . . . . ? C2 C1 C20 C19 -174.3(6) . . . . ? C2 C1 C100 C101 -124.0(6) . . . . ? C2 C1 C100 C105 58.3(8) . . . . ? C2 C3 C4 C5 -0.7(7) . . . . ? C3 C4 C5 N1 -1.0(7) . . . . ? C3 C4 C5 C6 174.3(6) . . . . ? C4 C5 C6 C7 172.5(6) . . . . ? C4 C5 C6 C200 -5.9(9) . . . . ? C5 N1 C2 C1 174.4(5) . . . . ? C5 N1 C2 C3 -2.9(6) . . . . ? C5 C6 C7 N2 -7.2(9) . . . . ? C5 C6 C7 C8 172.4(6) . . . . ? C5 C6 C200 C201 -54.4(9) . . . . ? C5 C6 C200 C205 126.5(7) . . . . ? C6 C7 C8 C9 175.8(6) . . . . ? C6 C200 C201 C202 179.7(8) . . . . ? C6 C200 C205 C204 177.6(7) . . . . ? C7 N2 C10 C9 -2.8(6) . . . . ? C7 N2 C10 C11 173.9(5) . . . . ? C7 C6 C200 C201 127.1(7) . . . . ? C7 C6 C200 C205 -51.9(9) . . . . ? C7 C8 C9 C10 2.8(7) . . . . ? C8 C9 C10 N2 -0.1(7) . . . . ? C8 C9 C10 C11 -176.8(6) . . . . ? C9 C10 C11 C12 -172.6(6) . . . . ? C9 C10 C11 C300 11.3(8) . . . . ? C10 N2 C7 C6 -175.9(6) . . . . ? C10 N2 C7 C8 4.4(6) . . . . ? C10 C11 C12 N3 9.0(10) . . . . ? C10 C11 C12 C13 -172.2(6) . . . . ? C10 C11 C300 C301 58.7(8) . . . . ? C10 C11 C300 C305 -123.9(6) . . . . ? C11 C12 C13 C14 -178.2(6) . . . . ? C11 C300 C301 C302 173.3(7) . . . . ? C11 C300 C305 C304 -175.3(5) . . . . ? C12 N3 C15 C14 3.5(8) . . . . ? C12 N3 C15 C16 179.5(7) . . . . ? C12 C11 C300 C301 -117.8(7) . . . . ? C12 C11 C300 C305 59.7(7) . . . . ? C12 C13 C14 C15 1.3(9) . . . . ? C13 C14 C15 N3 -3.0(9) . . . . ? C13 C14 C15 C16 -179.0(7) . . . . ? C14 C15 C16 C17 174.2(8) . . . . ? C14 C15 C16 C400 -12.4(11) . . . . ? C15 N3 C12 C11 176.3(6) . . . . ? C15 N3 C12 C13 -2.6(7) . . . . ? C15 C16 C17 N4 -17.2(12) . . . . ? C15 C16 C17 C18 166.3(8) . . . . ? C15 C16 C400 C401 -61.2(10) . . . . ? C15 C16 C400 C405 124.3(8) . . . . ? C16 C17 C18 C19 175.0(7) . . . . ? C16 C400 C401 C402 -178.4(8) . . . . ? C16 C400 C405 C404 177.0(8) . . . . ? C17 N4 C20 C1 174.0(6) . . . . ? C17 N4 C20 C19 -4.0(7) . . . . ? C17 C16 C400 C401 112.7(8) . . . . ? C17 C16 C400 C405 -61.9(10) . . . . ? C17 C18 C19 C20 -0.5(9) . . . . ? C18 C19 C20 N4 2.8(8) . . . . ? C18 C19 C20 C1 -175.3(7) . . . . ? C20 N4 C17 C16 -173.2(7) . . . . ? C20 N4 C17 C18 3.7(8) . . . . ? C20 C1 C2 N1 12.6(10) . . . . ? C20 C1 C2 C3 -170.6(6) . . . . ? C20 C1 C100 C101 57.6(8) . . . . ? C20 C1 C100 C105 -120.0(7) . . . . ? C100 C1 C2 N1 -165.6(5) . . . . ? C100 C1 C2 C3 11.2(9) . . . . ? C100 C1 C20 N4 -173.8(5) . . . . ? C100 C1 C20 C19 3.9(9) . . . . ? C100 C101 C102 C103 -3.6(9) . . . . ? C101 C100 C105 C104 -4.0(10) . . . . ? C101 C102 C103 C104 -0.3(9) . . . . ? C101 C102 C103 C106 178.5(5) . . . 4_475 ? C102 C103 C104 C105 1.9(10) . . . . ? C103 C104 C105 C100 0.2(11) . . . . ? C105 C100 C101 C102 5.7(9) . . . . ? C106 C103 C104 C105 -176.9(6) 4_475 . . . ? C200 C6 C7 N2 171.1(5) . . . . ? C200 C6 C7 C8 -9.3(9) . . . . ? C200 C201 C202 C203 4.0(15) . . . . ? C201 C200 C205 C204 -1.5(12) . . . . ? C201 C202 C203 C204 -3.7(14) . . . . ? C201 C202 C203 C206 178.9(8) . . . . ? C202 C203 C204 C205 1.0(13) . . . . ? C202 C203 C206 O201 1.8(12) . . . . ? C202 C203 C206 O202 -175.6(9) . . . . ? C203 C204 C205 C200 1.6(13) . . . . ? C204 C203 C206 O201 -175.6(7) . . . . ? C204 C203 C206 O202 7.0(11) . . . . ? C205 C200 C201 C202 -1.2(13) . . . . ? C206 C203 C204 C205 178.5(7) . . . . ? C300 C11 C12 N3 -174.9(5) . . . . ? C300 C11 C12 C13 3.9(9) . . . . ? C300 C301 C302 C303 2.1(12) . . . . ? C301 C300 C305 C304 2.2(9) . . . . ? C301 C302 C303 C304 2.2(10) . . . . ? C301 C302 C303 C306 -179.6(6) . . . . ? C302 C303 C304 C305 -4.3(9) . . . . ? C302 C303 C306 O301 -176.1(6) . . . . ? C302 C303 C306 O302 7.0(9) . . . . ? C303 C304 C305 C300 2.0(10) . . . . ? C304 C303 C306 O301 2.0(9) . . . . ? C304 C303 C306 O302 -174.9(6) . . . . ? C305 C300 C301 C302 -4.3(11) . . . . ? C306 C303 C304 C305 177.6(6) . . . . ? C400 C16 C17 N4 169.4(6) . . . . ? C400 C16 C17 C18 -7.1(11) . . . . ? C400 C401 C402 C403 2.0(13) . . . . ? C401 C400 C405 C404 2.2(13) . . . . ? C401 C402 C403 C404 1.3(12) . . . . ? C401 C402 C403 C406 178.0(7) . . . 3_675 ? C402 C403 C404 C405 -2.7(13) . . . . ? C403 C404 C405 C400 0.9(14) . . . . ? C405 C400 C401 C402 -3.8(13) . . . . ? C406 C403 C404 C405 -179.4(8) 3_675 . . . ? # Attachment '- Structure1_Cu New.cif' data_structure1_cunew _database_code_depnum_ccdc_archive 'CCDC 865036' #TrackingRef '- Structure1_Cu New.cif' _audit_creation_date 2012-02-21 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H24 Cd Cu N4 O7, 3(C5 H11 N1 O1), (H2 O1), (C5, H11, N1)' _chemical_formula_sum 'C57 H52 Cd Cu N6 O12' _chemical_formula_weight 1188.99 _chemical_melting_point ? 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' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 'x+1/2, -y+1/2, -z' 4 '-x, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x-1/2, y, -z-1/2' 7 '-x-1/2, y-1/2, z' 8 'x, -y-1/2, z-1/2' _cell_length_a 9.3440(6) _cell_length_b 41.835(3) _cell_length_c 30.0493(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11746.6(13) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9949 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 58.93 _cell_measurement_theta_min 2.57 _exptl_absorpt_coefficient_mu 3.869 _exptl_absorpt_correction_T_max 0.6153 _exptl_absorpt_correction_T_min 0.5131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour purple-red _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular blocks' _exptl_crystal_F_000 4872 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_unetI/netI 0.0523 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 36393 _diffrn_reflns_theta_full 59.02 _diffrn_reflns_theta_max 59.02 _diffrn_reflns_theta_min 2.11 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.884 _diffrn_measured_fraction_theta_max 0.884 _diffrn_measurement_device_type 'Bruker Smart 6K CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'CU K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 20.0 _diffrn_source_power 0.9 _diffrn_source_voltage 45.0 _reflns_number_gt 6147 _reflns_number_total 7487 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker Apex2' _computing_data_collection 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 4.267 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.159 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 538 _refine_ls_number_reflns 7487 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0991 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1748P)^2^+35.1926P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2592 _refine_ls_wR_factor_ref 0.2683 _refine_special_details ; 'CHEMW03_2_A Alert-added in atoms found using SQUEEZE' 'PALT029_ALERT_3_A-Crystal chosen had some suspect frames which were removed' 'PLAT043_ALERT_1_A-added atoms found using SQUEEZE' 'PLAT_094__ALERT_2_A-ratio residual density casued by disorder of crystal packing' 'PLAT602_ALERT-A_2-Large void typical of MOFs, treated with SQUEEZE' 'PLAT971_ALERT_3_A-Large positive residual near Cd caused by crystal disorder' 'PLAT973_ALERT_2_A-Large positve residual near Cu caused by crystal disorder' 'Oxygen atoms attached to C48 were greatly disordered so removed from refinment causing an incorrect bond distance for C36 to C48' 'the following constraints were used to better model disorder, DFIX, SIMU, and HFIX to determine Hydrogen atoms' 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 -0.015 0.000 -0.005 2815 894 '12[HCON(C2H5)2]4(C2H5)2NH 4H2' 2 0.536 0.500 0.120 2815 889 '12[HCON(C2H5)2]4(C2H5)2NH 4H2' _platon_squeeze_details 'SQUEEZE was performed using PLATON to account for disordered solvent molecules and counter cations. The electron density found in each cavity correlates to a final count of 3 molecules of HCON(C2H5)2, 2 H2Os, and 1 (C2H5)2NH+' 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 C32 C 0.4951(13) 0.74841(18) 0.2310(4) 0.077(3) Uani 1 1 d . . . H32 H 0.4072 0.7508 0.2466 0.092 Uiso 1 1 calc R . . C27 C 0.5557(9) 0.77437(16) 0.2102(3) 0.0459(19) Uani 1 1 d . . . C28 C 0.6880(10) 0.77003(19) 0.1888(3) 0.055(2) Uani 1 1 d . . . H28 H 0.7343 0.7876 0.1748 0.066 Uiso 1 1 calc R . . C31 C 0.5620(12) 0.71858(17) 0.2294(4) 0.072(3) Uani 1 1 d . . . H31 H 0.5175 0.7008 0.2434 0.087 Uiso 1 1 calc R . . C29 C 0.7491(10) 0.74076(17) 0.1881(4) 0.058(3) Uani 1 1 d . . . H29 H 0.8375 0.7383 0.1728 0.070 Uiso 1 1 calc R . . C30 C 0.6902(9) 0.71434(17) 0.2083(3) 0.0451(18) Uani 1 1 d . . . Cd1 Cd -0.34105(6) 1.120535(11) 0.18625(2) 0.0473(3) Uani 1 1 d . . . Cu1 Cu 0.27173(12) 0.87304(2) 0.20972(4) 0.0446(4) Uani 1 1 d . . . O1 O -0.5442(10) 1.12040(12) 0.2267(4) 0.104(3) Uani 1 1 d . . . O2 O -0.1924(8) 1.08364(13) 0.2204(2) 0.072(2) Uani 1 1 d . . . O3 O -0.1911(8) 1.15843(12) 0.2214(2) 0.0663(18) Uani 1 1 d . . . O4 O -0.3703(7) 1.17826(14) 0.1813(3) 0.071(2) Uani 1 1 d . . . O5 O -0.3581(6) 1.06158(13) 0.1793(2) 0.0565(16) Uani 1 1 d . . . O7 O -0.4481(7) 1.11990(11) 0.1144(2) 0.0553(15) Uani 1 1 d . . . O8 O -0.2133(7) 1.12244(14) 0.1193(2) 0.0631(17) Uani 1 1 d . . . C46 C -0.2589(11) 1.18150(17) 0.2036(3) 0.050(2) Uani 1 1 d . . . N3 N 0.3647(7) 0.84593(13) 0.2566(2) 0.0440(16) Uani 1 1 d . . . C45 C -0.2470(11) 1.05933(17) 0.2002(3) 0.052(2) Uani 1 1 d . . . C11 C 0.2727(9) 0.87262(16) 0.3240(3) 0.049(2) Uani 1 1 d . . . C43 C -0.2263(10) 1.00137(18) 0.1857(3) 0.056(2) Uani 1 1 d . . . H43 H -0.3161 1.0023 0.1710 0.067 Uiso 1 1 calc R . . C42 C -0.1699(9) 1.02864(17) 0.2042(3) 0.050(2) Uani 1 1 d . . . N1 N 0.1941(7) 0.90175(14) 0.1637(2) 0.0466(16) Uani 1 1 d . . . N2 N 0.3587(7) 0.84526(15) 0.1627(2) 0.0498(17) Uani 1 1 d . . . N4 N 0.1765(7) 0.89879(14) 0.2566(3) 0.0502(18) Uani 1 1 d . . . C47 C -0.3250(9) 1.12114(18) 0.0967(4) 0.055(2) Uani 1 1 d . . . C12 C 0.1754(9) 0.89273(18) 0.3017(3) 0.048(2) Uani 1 1 d . . . C20 C 0.2236(9) 0.90057(19) 0.1169(3) 0.057(2) Uani 1 1 d . . . C1 C 0.2857(10) 0.87560(19) 0.0955(4) 0.057(2) Uani 1 1 d . . . C41 C -0.0399(14) 1.02511(19) 0.2277(4) 0.083(4) Uani 1 1 d . . . H41 H 0.0004 1.0431 0.2424 0.100 Uiso 1 1 calc R . . C6 C 0.4799(9) 0.80529(17) 0.2091(3) 0.051(2) Uani 1 1 d . . . C19 C 0.1723(10) 0.9298(2) 0.0962(4) 0.065(2) Uani 1 1 d . . . H19 H 0.1800 0.9355 0.0657 0.077 Uiso 1 1 calc R . . C8 C 0.5302(9) 0.81338(17) 0.2909(3) 0.051(2) Uani 1 1 d . . . H8 H 0.6020 0.7975 0.2948 0.061 Uiso 1 1 calc R . . C7 C 0.4588(8) 0.82167(15) 0.2498(3) 0.0441(19) Uani 1 1 d . . . C15 C 0.0789(8) 0.92314(16) 0.2508(3) 0.048(2) Uani 1 1 d . . . C36 C 0.2967(12) 0.8710(3) 0.4661(3) 0.077(3) Uani 1 1 d DU . . C3 C 0.3923(10) 0.8195(2) 0.0952(4) 0.063(2) Uani 1 1 d . . . H3 H 0.3897 0.8153 0.0641 0.076 Uiso 1 1 calc R . . C16 C 0.0589(9) 0.93993(17) 0.2110(3) 0.0472(19) Uani 1 1 d . . . C2 C 0.3415(9) 0.8483(2) 0.1178(3) 0.053(2) Uani 1 1 d . . . C44 C -0.1534(9) 0.97230(19) 0.1883(4) 0.062(3) Uani 1 1 d . . . H44 H -0.1943 0.9538 0.1750 0.074 Uiso 1 1 calc R . . C10 C 0.3692(9) 0.85239(17) 0.3004(3) 0.049(2) Uani 1 1 d . . . C4 C 0.4429(10) 0.8002(2) 0.1268(4) 0.063(2) Uani 1 1 d . . . H4 H 0.4837 0.7797 0.1226 0.076 Uiso 1 1 calc R . . C5 C 0.4240(9) 0.81653(17) 0.1684(3) 0.052(2) Uani 1 1 d . . . C9 C 0.4746(9) 0.83267(17) 0.3228(3) 0.051(2) Uani 1 1 d . . . H9 H 0.4994 0.8332 0.3535 0.061 Uiso 1 1 calc R . . C34 C 0.2548(11) 0.8445(2) 0.3993(4) 0.072(3) Uani 1 1 d . . . H34 H 0.2354 0.8253 0.3837 0.086 Uiso 1 1 calc R . . C40 C 0.0270(13) 0.99704(19) 0.2295(5) 0.089(4) Uani 1 1 d . . . H40 H 0.1147 0.9958 0.2454 0.106 Uiso 1 1 calc R . . C18 C 0.1122(9) 0.94718(18) 0.1286(3) 0.057(2) Uani 1 1 d . . . H18 H 0.0706 0.9677 0.1247 0.069 Uiso 1 1 calc R . . C33 C 0.2769(9) 0.87277(18) 0.3744(3) 0.051(2) Uani 1 1 d . . . C17 C 0.1198(10) 0.93015(19) 0.1704(4) 0.061(3) Uani 1 1 d . . . C26 C 0.4300(5) 0.88094(18) 0.0253(2) 0.092(4) Uani 1 1 d G . . H26 H 0.5140 0.8833 0.0429 0.111 Uiso 1 1 calc R . . C25 C 0.4395(5) 0.88112(18) -0.0208(2) 0.089(4) Uani 1 1 d G . . H25 H 0.5299 0.8836 -0.0348 0.106 Uiso 1 1 calc R . . C24 C 0.3166(6) 0.87769(14) -0.04645(15) 0.056(2) Uani 1 1 d G . . C23 C 0.1843(5) 0.87408(16) -0.02593(19) 0.078(3) Uani 1 1 d G . . H23 H 0.1003 0.8717 -0.0434 0.094 Uiso 1 1 calc R . . C22 C 0.1748(5) 0.87389(16) 0.02024(19) 0.071(3) Uani 1 1 d G . . H22 H 0.0844 0.8714 0.0343 0.085 Uiso 1 1 calc R . . C21 C 0.2977(6) 0.87733(14) 0.04587(15) 0.059(2) Uani 1 1 d G . . C39 C -0.0249(10) 0.96978(17) 0.2095(3) 0.054(2) Uani 1 1 d . . . C38 C 0.3107(12) 0.8993(2) 0.3978(4) 0.070(3) Uani 1 1 d . . . H38 H 0.3304 0.9186 0.3825 0.084 Uiso 1 1 calc R . . C35 C 0.2598(14) 0.8434(3) 0.4434(4) 0.083(3) Uani 1 1 d . . . H35 H 0.2386 0.8243 0.4590 0.100 Uiso 1 1 calc R . . C37 C 0.3171(12) 0.8986(3) 0.4437(4) 0.081(3) Uani 1 1 d . . . H37 H 0.3360 0.9178 0.4597 0.098 Uiso 1 1 calc R . . C14 C 0.0111(9) 0.93086(17) 0.2921(3) 0.051(2) Uani 1 1 d . . . H14 H -0.0628 0.9462 0.2963 0.061 Uiso 1 1 calc R . . C13 C 0.0718(9) 0.91220(17) 0.3245(3) 0.055(2) Uani 1 1 d . . . H13 H 0.0502 0.9121 0.3554 0.065 Uiso 1 1 calc R . . C48 C 0.308(2) 0.8719(5) 0.5122(5) 0.170(8) Uani 1 1 d DU . . 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 C32 0.104(8) 0.043(4) 0.084(8) 0.008(4) 0.037(7) -0.005(5) C27 0.061(5) 0.036(4) 0.041(5) 0.002(3) -0.005(4) -0.011(3) C28 0.052(5) 0.042(4) 0.072(7) 0.016(4) -0.010(4) -0.008(4) C31 0.090(7) 0.030(4) 0.096(8) 0.010(4) 0.038(6) 0.001(4) C29 0.050(5) 0.035(4) 0.089(8) -0.001(4) -0.006(4) -0.008(4) C30 0.059(5) 0.044(4) 0.032(5) -0.001(3) 0.006(4) -0.010(3) Cd1 0.0512(4) 0.0433(4) 0.0473(5) 0.0027(2) 0.0014(3) 0.0012(2) Cu1 0.0447(6) 0.0453(6) 0.0437(8) 0.0025(4) -0.0026(5) -0.0019(5) O1 0.114(7) 0.046(3) 0.153(8) 0.003(4) 0.080(7) 0.003(3) O2 0.106(5) 0.038(3) 0.073(5) -0.003(3) -0.035(4) 0.000(3) O3 0.100(5) 0.035(3) 0.064(4) 0.012(3) -0.026(4) 0.011(3) O4 0.052(4) 0.042(3) 0.118(7) 0.016(3) 0.001(4) -0.002(3) O5 0.056(4) 0.044(3) 0.070(5) -0.012(3) 0.007(3) -0.006(2) O7 0.054(4) 0.067(3) 0.045(4) 0.009(2) 0.007(3) 0.009(2) O8 0.054(4) 0.094(5) 0.041(4) 0.017(3) 0.005(3) 0.009(3) C46 0.071(6) 0.034(4) 0.045(6) 0.009(3) 0.007(5) 0.009(4) N3 0.052(4) 0.037(3) 0.043(5) 0.000(3) -0.001(3) -0.009(3) C45 0.069(6) 0.037(4) 0.050(6) -0.003(3) 0.000(5) -0.012(4) C11 0.055(5) 0.037(4) 0.055(6) 0.000(3) -0.003(4) -0.015(4) C43 0.048(5) 0.048(4) 0.072(7) -0.016(4) -0.002(4) -0.005(4) C42 0.059(5) 0.034(4) 0.058(6) -0.003(4) -0.004(4) -0.007(3) N1 0.043(3) 0.048(3) 0.048(5) -0.005(3) -0.001(3) 0.004(3) N2 0.050(4) 0.055(4) 0.045(5) 0.011(3) -0.012(3) -0.002(3) N4 0.048(4) 0.039(3) 0.063(5) 0.008(3) -0.005(3) -0.013(3) C47 0.044(5) 0.061(5) 0.060(7) 0.016(4) 0.007(5) 0.008(3) C12 0.062(5) 0.041(4) 0.042(5) 0.005(3) 0.007(4) -0.007(3) C20 0.049(5) 0.056(5) 0.066(7) 0.002(4) -0.004(4) 0.003(4) C1 0.043(4) 0.067(5) 0.062(7) 0.001(4) 0.003(4) 0.003(4) C41 0.124(9) 0.042(5) 0.085(8) -0.010(4) -0.053(7) -0.014(5) C6 0.059(5) 0.040(4) 0.055(6) -0.002(4) 0.002(4) -0.016(3) C19 0.073(6) 0.074(6) 0.046(6) 0.012(4) -0.005(5) 0.010(4) C8 0.059(5) 0.040(4) 0.053(6) 0.011(3) -0.006(4) -0.003(3) C7 0.044(4) 0.035(3) 0.054(6) 0.009(3) -0.010(4) -0.011(3) C15 0.043(4) 0.040(4) 0.060(6) -0.003(3) -0.001(4) -0.004(3) C36 0.058(6) 0.148(10) 0.027(5) -0.002(6) -0.001(4) -0.013(6) C3 0.058(5) 0.078(6) 0.053(6) -0.014(5) -0.002(5) 0.003(4) C16 0.050(4) 0.042(4) 0.050(6) -0.004(3) -0.003(4) -0.005(3) C2 0.048(5) 0.061(5) 0.050(6) 0.000(4) 0.001(4) 0.008(3) C44 0.049(5) 0.035(4) 0.102(9) -0.023(4) -0.006(5) -0.003(3) C10 0.051(5) 0.041(4) 0.055(6) 0.006(4) -0.007(4) -0.012(3) C4 0.062(5) 0.055(5) 0.073(7) -0.006(4) -0.009(5) 0.000(4) C5 0.046(4) 0.046(4) 0.064(6) -0.004(4) -0.002(4) 0.005(3) C9 0.054(5) 0.047(4) 0.052(6) 0.000(4) -0.008(4) -0.011(3) C34 0.072(6) 0.076(6) 0.068(8) 0.007(5) 0.002(5) 0.003(5) C40 0.100(8) 0.049(5) 0.117(10) -0.008(5) -0.069(8) 0.000(5) C18 0.055(5) 0.049(4) 0.068(7) 0.012(4) -0.002(5) -0.002(4) C33 0.045(4) 0.061(5) 0.048(6) -0.001(4) 0.006(4) -0.007(4) C17 0.059(5) 0.048(4) 0.076(8) 0.008(4) -0.023(5) -0.008(4) C26 0.036(5) 0.202(14) 0.038(6) -0.008(6) -0.004(4) -0.007(6) C25 0.046(5) 0.165(12) 0.056(8) 0.006(6) 0.006(5) -0.002(6) C24 0.046(5) 0.073(6) 0.048(6) 0.009(4) 0.001(4) 0.016(4) C23 0.051(5) 0.141(10) 0.043(7) 0.005(6) -0.007(5) 0.009(5) C22 0.038(4) 0.130(8) 0.045(6) 0.015(5) -0.013(4) -0.007(5) C21 0.035(4) 0.075(6) 0.067(7) 0.006(4) -0.003(4) 0.004(3) C39 0.068(5) 0.039(4) 0.055(6) -0.004(3) 0.001(5) -0.011(4) C38 0.078(7) 0.079(6) 0.052(7) -0.001(5) 0.012(5) -0.009(5) C35 0.091(8) 0.115(9) 0.043(7) 0.022(6) 0.010(6) 0.000(7) C37 0.070(7) 0.112(9) 0.062(8) -0.017(6) -0.012(6) -0.004(6) C14 0.048(4) 0.037(4) 0.067(7) -0.002(4) 0.008(4) -0.007(3) C13 0.060(5) 0.038(4) 0.066(6) -0.002(4) 0.012(5) -0.016(4) C48 0.110(12) 0.35(3) 0.052(9) -0.002(12) -0.003(9) -0.008(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C32 H32 0.9500 . ? C32 C27 1.376(11) . ? C32 C31 1.397(12) . ? C27 C28 1.405(13) . ? C27 C6 1.475(11) . ? C28 H28 0.9500 . ? C28 C29 1.351(12) . ? C31 H31 0.9500 . ? C31 C30 1.367(12) . ? C29 H29 0.9500 . ? C29 C30 1.376(11) . ? C30 C46 1.523(12) 7_655 ? Cd1 O1 2.254(8) . ? Cd1 O2 2.316(6) . ? Cd1 O3 2.364(6) . ? Cd1 O4 2.435(6) . ? Cd1 O5 2.480(5) . ? Cd1 O7 2.379(6) . ? Cd1 O8 2.342(7) . ? Cd1 C46 2.714(8) . ? Cd1 C45 2.740(8) . ? Cd1 C47 2.696(11) . ? Cu1 N3 2.007(7) . ? Cu1 N1 1.969(7) . ? Cu1 N2 2.003(8) . ? Cu1 N4 1.985(7) . ? O2 C45 1.289(10) . ? O3 C46 1.273(10) . ? O4 C46 1.244(12) . ? O5 C45 1.219(11) . ? O7 C47 1.270(11) . ? O8 C47 1.246(12) . ? C46 C30 1.523(12) 7_665 ? N3 C7 1.358(10) . ? N3 C10 1.344(11) . ? C45 C42 1.477(12) . ? C11 C12 1.410(12) . ? C11 C10 1.426(12) . ? C11 C33 1.514(14) . ? C43 H43 0.9500 . ? C43 C42 1.374(11) . ? C43 C44 1.396(12) . ? C42 C41 1.412(13) . ? N1 C20 1.435(12) . ? N1 C17 1.391(11) . ? N2 C2 1.363(12) . ? N2 C5 1.359(10) . ? N4 C12 1.377(11) . ? N4 C15 1.378(10) . ? C47 C24 1.51(4) 5_575 ? C12 C13 1.439(12) . ? C20 C1 1.357(12) . ? C20 C19 1.454(12) . ? C1 C2 1.424(12) . ? C1 C21 1.497(12) . ? C41 H41 0.9500 . ? C41 C40 1.331(13) . ? C6 C7 1.416(12) . ? C6 C5 1.412(13) . ? C19 H19 0.9500 . ? C19 C18 1.337(14) . ? C8 H8 0.9500 . ? C8 C7 1.444(12) . ? C8 C9 1.358(12) . ? C15 C16 1.399(12) . ? C15 C14 1.432(12) . ? C36 C35 1.381(16) . ? C36 C37 1.352(17) . ? C36 C48 1.390(15) . ? C3 H3 0.9500 . ? C3 C2 1.462(12) . ? C3 C4 1.331(14) . ? C16 C17 1.406(14) . ? C16 C39 1.475(12) . ? C44 H44 0.9500 . ? C44 C39 1.363(13) . ? C10 C9 1.450(12) . ? C4 H4 0.9500 . ? C4 C5 1.435(13) . ? C9 H9 0.9500 . ? C34 H34 0.9500 . ? C34 C33 1.415(13) . ? C34 C35 1.327(15) . ? C40 H40 0.9500 . ? C40 C39 1.378(12) . ? C18 H18 0.9500 . ? C18 C17 1.447(14) . ? C33 C38 1.351(13) . ? C26 H26 0.9500 . ? C26 C25 1.3900 . ? C26 C21 1.3900 . ? C25 H25 0.9500 . ? C25 C24 1.3900 . ? C24 C47 1.512(12) 5_575 ? C24 C23 1.3900 . ? C23 H23 0.9500 . ? C23 C22 1.3900 . ? C22 H22 0.9500 . ? C22 C21 1.3900 . ? C38 H38 0.9500 . ? C38 C37 1.379(16) . ? C35 H35 0.9500 . ? C37 H37 0.9500 . ? C14 H14 0.9500 . ? C14 C13 1.371(13) . ? C13 H13 0.9500 . ? 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 C27 C32 H32 119.9 . . ? C27 C32 C31 120.3(10) . . ? C31 C32 H32 119.9 . . ? C32 C27 C28 118.0(8) . . ? C32 C27 C6 120.2(9) . . ? C28 C27 C6 121.7(7) . . ? C27 C28 H28 120.2 . . ? C29 C28 C27 119.7(8) . . ? C29 C28 H28 120.2 . . ? C32 C31 H31 119.2 . . ? C30 C31 C32 121.6(8) . . ? C30 C31 H31 119.2 . . ? C28 C29 H29 118.2 . . ? C28 C29 C30 123.5(9) . . ? C30 C29 H29 118.2 . . ? C31 C30 C29 116.8(8) . . ? C31 C30 C46 122.0(7) . 7_655 ? C29 C30 C46 121.0(8) . 7_655 ? O1 Cd1 O2 105.3(3) . . ? O1 Cd1 O3 105.1(3) . . ? O1 Cd1 O4 86.6(2) . . ? O1 Cd1 O5 89.38(19) . . ? O1 Cd1 O7 97.8(4) . . ? O1 Cd1 O8 153.2(4) . . ? O1 Cd1 C46 97.9(3) . . ? O1 Cd1 C45 100.7(3) . . ? O1 Cd1 C47 125.8(4) . . ? O2 Cd1 O3 83.9(2) . . ? O2 Cd1 O4 139.1(2) . . ? O2 Cd1 O5 54.1(2) . . ? O2 Cd1 O7 130.3(2) . . ? O2 Cd1 O8 95.6(3) . . ? O2 Cd1 C46 111.8(2) . . ? O2 Cd1 C45 28.0(3) . . ? O2 Cd1 C47 114.5(3) . . ? O3 Cd1 O4 55.2(2) . . ? O3 Cd1 O5 138.0(2) . . ? O3 Cd1 O7 131.44(19) . . ? O3 Cd1 C46 28.0(2) . . ? O3 Cd1 C45 111.6(2) . . ? O3 Cd1 C47 114.0(3) . . ? O4 Cd1 O5 166.9(3) . . ? O4 Cd1 C46 27.3(2) . . ? O4 Cd1 C45 166.5(3) . . ? O4 Cd1 C47 86.4(2) . . ? O5 Cd1 C46 165.7(3) . . ? O5 Cd1 C45 26.4(2) . . ? O5 Cd1 C47 85.9(2) . . ? O7 Cd1 O4 84.8(2) . . ? O7 Cd1 O5 83.4(2) . . ? O7 Cd1 C46 107.6(2) . . ? O7 Cd1 C45 105.3(2) . . ? O7 Cd1 C47 28.1(2) . . ? O8 Cd1 O3 93.4(2) . . ? O8 Cd1 O4 88.4(2) . . ? O8 Cd1 O5 89.6(2) . . ? O8 Cd1 O7 55.6(2) . . ? O8 Cd1 C46 89.3(2) . . ? O8 Cd1 C45 90.0(2) . . ? O8 Cd1 C47 27.5(3) . . ? C46 Cd1 C45 139.3(3) . . ? C46 Cd1 C47 99.6(3) . . ? C47 Cd1 C45 98.3(2) . . ? N1 Cu1 N3 175.5(3) . . ? N1 Cu1 N2 90.4(3) . . ? N1 Cu1 N4 90.1(3) . . ? N2 Cu1 N3 89.6(3) . . ? N4 Cu1 N3 90.1(3) . . ? N4 Cu1 N2 176.7(3) . . ? C45 O2 Cd1 94.6(6) . . ? C46 O3 Cd1 91.5(6) . . ? C46 O4 Cd1 89.0(4) . . ? C45 O5 Cd1 88.7(4) . . ? C47 O7 Cd1 90.0(6) . . ? C47 O8 Cd1 92.3(6) . . ? C30 C46 Cd1 170.0(6) 7_665 . ? O3 C46 C30 115.8(9) . 7_665 ? O3 C46 Cd1 60.6(4) . . ? O4 C46 C30 120.1(7) . 7_665 ? O4 C46 Cd1 63.8(4) . . ? O4 C46 O3 124.0(8) . . ? C7 N3 Cu1 126.7(6) . . ? C10 N3 Cu1 126.0(5) . . ? C10 N3 C7 106.0(7) . . ? O2 C45 Cd1 57.4(4) . . ? O2 C45 C42 117.1(9) . . ? O5 C45 Cd1 64.9(4) . . ? O5 C45 O2 121.3(8) . . ? O5 C45 C42 121.6(7) . . ? C42 C45 Cd1 168.9(7) . . ? C12 C11 C10 121.7(9) . . ? C12 C11 C33 119.4(8) . . ? C10 C11 C33 118.9(8) . . ? C42 C43 H43 119.6 . . ? C42 C43 C44 120.9(9) . . ? C44 C43 H43 119.6 . . ? C43 C42 C45 120.1(8) . . ? C43 C42 C41 116.4(8) . . ? C41 C42 C45 123.4(7) . . ? C20 N1 Cu1 126.6(5) . . ? C17 N1 Cu1 127.1(6) . . ? C17 N1 C20 105.5(7) . . ? C2 N2 Cu1 126.6(5) . . ? C5 N2 Cu1 127.3(6) . . ? C5 N2 C2 105.1(7) . . ? C12 N4 Cu1 127.0(5) . . ? C12 N4 C15 104.9(7) . . ? C15 N4 Cu1 127.4(6) . . ? O7 C47 Cd1 61.9(5) . . ? O7 C47 C24 118(2) . 5_575 ? O8 C47 Cd1 60.2(5) . . ? O8 C47 O7 122.1(10) . . ? O8 C47 C24 120(2) . 5_575 ? C24 C47 Cd1 178.7(8) 5_575 . ? C11 C12 C13 123.0(8) . . ? N4 C12 C11 125.0(8) . . ? N4 C12 C13 111.7(8) . . ? N1 C20 C19 109.1(7) . . ? C1 C20 N1 125.0(8) . . ? C1 C20 C19 125.9(10) . . ? C20 C1 C2 123.5(10) . . ? C20 C1 C21 117.8(8) . . ? C2 C1 C21 118.7(7) . . ? C42 C41 H41 119.4 . . ? C40 C41 C42 121.1(8) . . ? C40 C41 H41 119.4 . . ? C7 C6 C27 118.2(7) . . ? C5 C6 C27 119.2(7) . . ? C5 C6 C7 122.5(7) . . ? C20 C19 H19 126.7 . . ? C18 C19 C20 106.6(9) . . ? C18 C19 H19 126.7 . . ? C7 C8 H8 126.8 . . ? C9 C8 H8 126.8 . . ? C9 C8 C7 106.5(7) . . ? N3 C7 C6 125.5(7) . . ? N3 C7 C8 110.5(7) . . ? C6 C7 C8 123.8(7) . . ? N4 C15 C16 124.7(8) . . ? N4 C15 C14 110.4(7) . . ? C16 C15 C14 124.7(7) . . ? C37 C36 C35 120.2(10) . . ? C48 C36 C35 122.1(14) . . ? C48 C36 C37 117.5(14) . . ? C2 C3 H3 126.8 . . ? C4 C3 H3 126.8 . . ? C4 C3 C2 106.4(9) . . ? C15 C16 C17 122.7(7) . . ? C15 C16 C39 121.5(8) . . ? C17 C16 C39 115.8(8) . . ? N2 C2 C1 125.7(8) . . ? N2 C2 C3 110.2(8) . . ? C1 C2 C3 124.1(9) . . ? C43 C44 H44 119.2 . . ? C39 C44 C43 121.6(7) . . ? C39 C44 H44 119.2 . . ? N3 C10 C11 125.9(8) . . ? N3 C10 C9 111.2(8) . . ? C11 C10 C9 122.4(9) . . ? C3 C4 H4 126.6 . . ? C3 C4 C5 106.9(8) . . ? C5 C4 H4 126.6 . . ? N2 C5 C6 124.8(8) . . ? N2 C5 C4 111.4(8) . . ? C6 C5 C4 123.5(7) . . ? C8 C9 C10 105.6(8) . . ? C8 C9 H9 127.2 . . ? C10 C9 H9 127.2 . . ? C33 C34 H34 118.3 . . ? C35 C34 H34 118.3 . . ? C35 C34 C33 123.5(11) . . ? C41 C40 H40 118.4 . . ? C41 C40 C39 123.1(10) . . ? C39 C40 H40 118.4 . . ? C19 C18 H18 124.9 . . ? C19 C18 C17 110.1(8) . . ? C17 C18 H18 124.9 . . ? C34 C33 C11 121.5(8) . . ? C38 C33 C11 122.0(8) . . ? C38 C33 C34 116.3(10) . . ? N1 C17 C16 125.2(8) . . ? N1 C17 C18 108.6(9) . . ? C16 C17 C18 126.2(8) . . ? C25 C26 H26 120.0 . . ? C25 C26 C21 120.0 . . ? C21 C26 H26 120.0 . . ? C26 C25 H25 120.0 . . ? C26 C25 C24 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C24 C47 120.5(5) . 5_575 ? C23 C24 C47 119.5(5) . 5_575 ? C23 C24 C25 120.0 . . ? C24 C23 H23 120.0 . . ? C24 C23 C22 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 H22 120.0 . . ? C26 C21 C1 120.9(5) . . ? C22 C21 C1 119.0(5) . . ? C22 C21 C26 120.0 . . ? C44 C39 C16 123.2(7) . . ? C44 C39 C40 116.7(8) . . ? C40 C39 C16 120.1(9) . . ? C33 C38 H38 119.5 . . ? C33 C38 C37 121.0(10) . . ? C37 C38 H38 119.5 . . ? C36 C35 H35 120.9 . . ? C34 C35 C36 118.2(10) . . ? C34 C35 H35 120.9 . . ? C36 C37 C38 120.5(11) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C15 C14 H14 126.1 . . ? C13 C14 C15 107.7(7) . . ? C13 C14 H14 126.1 . . ? C12 C13 H13 127.4 . . ? C14 C13 C12 105.2(8) . . ? C14 C13 H13 127.4 . . ? # Attachment '- Structure1_Co New.cif' data_structure1_conew _database_code_depnum_ccdc_archive 'CCDC 865037' #TrackingRef '- Structure1_Co New.cif' _audit_creation_date 2012-02-21 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H26 Cd Co N4 O9, 3(C5 H11 N1 O1), 1(H2 O1), 1(C5, H11, N1)' _chemical_formula_sum 'C57 H52 Cd Co N6 O12' _chemical_formula_weight 1184.38 _chemical_melting_point ? 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' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 'x+1/2, -y+1/2, -z' 4 '-x, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x-1/2, y, -z-1/2' 7 '-x-1/2, y-1/2, z' 8 'x, -y-1/2, z-1/2' _cell_length_a 30.1991(9) _cell_length_b 9.2075(3) _cell_length_c 41.8863(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11646.8(6) _cell_formula_units_Z 8 _cell_measurement_reflns_used 28016 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 118.06 _cell_measurement_theta_min 4.22 _exptl_absorpt_coefficient_mu 5.684 _exptl_absorpt_correction_T_max 0.3548 _exptl_absorpt_correction_T_min 0.1430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour purple0orange _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular blocks' _exptl_crystal_F_000 4856 _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.23 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetI/netI 0.0380 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 28096 _diffrn_reflns_theta_full 59.03 _diffrn_reflns_theta_max 59.03 _diffrn_reflns_theta_min 2.11 _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.959 _diffrn_measured_fraction_theta_max 0.959 _diffrn_measurement_device_type 'Bruker Smart 6K CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'CU K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 20.0 _diffrn_source_power 0.9 _diffrn_source_voltage 45.0 _reflns_number_gt 6384 _reflns_number_total 8051 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker APEX2' _computing_data_collection 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 3.403 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.181 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 557 _refine_ls_number_reflns 8051 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0830 _refine_ls_restrained_S_all 4.604 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1374P)^2^+44.2145P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2265 _refine_ls_wR_factor_ref 0.2380 _refine_special_details ; 'CHEMW03_ALERT_2_A-added in atoms found using SQUEEZE' 'PLAT043_ALERT_1_A-added atoms found using SQUEEZE' 'PLAT602_ALERT-A_2-Large void typical of MOFs, treated with SQUEEZE' 'PLAT029_ALERT_3_B-Low theta full due to crystal not diffractng that far' 'the following constraints were used to better model disorder, DFIX AFIX 66, ISOR, and HFIX to determine Hydrogen atoms' 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 -0.005 -0.005 2530 831 '12[HCON(C2H5)2]4(C2H5)2NH 4H2' 2 0.500 0.849 0.117 2530 828 '12[HCON(C2H5)2]4(C2H5)2NH 4H2' _platon_squeeze_details 'SQUEEZE was performed using PLATON to account for disordered solvent molecules and counter cations. The electron density found in each cavity correlates to a final count of 3 molecules of HCON(C2H5)2, 2 H2Os, and 1 (C2H5)2NH+' 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.2534(11) 0.576(3) 0.4229(6) 0.039(7) Uani 1 1 d . . . C2 C 0.2122(10) 0.505(3) 0.4296(7) 0.039(7) Uani 1 1 d . . . H2 H 0.2082 0.4305 0.4443 0.046 Uiso 1 1 calc R . . C3 C 0.1806(9) 0.563(3) 0.4113(7) 0.038(7) Uani 1 1 d . . . H3 H 0.1509 0.5364 0.4106 0.045 Uiso 1 1 calc R . . C4 C 0.2017(10) 0.675(3) 0.3928(6) 0.036(7) Uani 1 1 d . . . C5 C 0.1795(11) 0.777(4) 0.3737(7) 0.040(8) Uani 1 1 d . . . C6 C 0.2022(9) 0.878(3) 0.3548(6) 0.032(6) Uani 1 1 d . . . C7 C 0.1812(10) 0.989(3) 0.3358(7) 0.039(7) Uani 1 1 d . . . H7 H 0.1516 1.0170 0.3365 0.047 Uiso 1 1 calc R . . C8 C 0.2129(9) 1.045(3) 0.3169(7) 0.036(6) Uani 1 1 d . . . H8 H 0.2093 1.1183 0.3018 0.043 Uiso 1 1 calc R . . C9 C 0.2540(10) 0.970(3) 0.3244(6) 0.033(6) Uani 1 1 d . . . C10 C 0.2929(10) 0.987(3) 0.3070(6) 0.036(7) Uani 1 1 d . . . C11 C 0.3325(10) 0.927(3) 0.3175(6) 0.037(7) Uani 1 1 d . . . C12 C 0.3746(10) 0.941(4) 0.3009(7) 0.044(7) Uani 1 1 d . . . H12 H 0.3787 0.9780 0.2804 0.053 Uiso 1 1 calc R . . C13 C 0.4062(11) 0.892(4) 0.3203(7) 0.048(8) Uani 1 1 d . . . H13 H 0.4364 0.8900 0.3163 0.057 Uiso 1 1 calc R . . C14 C 0.3840(10) 0.842(3) 0.3490(7) 0.040(7) Uani 1 1 d . . . C15 C 0.4058(11) 0.788(3) 0.3759(6) 0.039(7) Uani 1 1 d . . . C16 C 0.3834(10) 0.728(3) 0.4016(7) 0.040(7) Uani 1 1 d . . . C17 C 0.4045(11) 0.678(4) 0.4308(8) 0.048(8) Uani 1 1 d . . . H17 H 0.4343 0.6867 0.4361 0.057 Uiso 1 1 calc R . . C18 C 0.3729(10) 0.617(4) 0.4487(7) 0.045(8) Uani 1 1 d . . . H18 H 0.3765 0.5770 0.4689 0.054 Uiso 1 1 calc R . . C19 C 0.3320(10) 0.626(3) 0.4306(7) 0.041(7) Uani 1 1 d . . . C20 C 0.2924(9) 0.560(3) 0.4399(6) 0.035(7) Uani 1 1 d . . . C21 C 0.2940(11) 0.479(4) 0.4698(7) 0.045(8) Uani 1 1 d D . . C22 C 0.2769(17) 0.539(5) 0.4981(8) 0.093(18) Uani 1 1 d . . . H22 H 0.2653 0.6325 0.4977 0.111 Uiso 1 1 calc R . . C23 C 0.2768(16) 0.463(5) 0.5261(8) 0.083(14) Uani 1 1 d U . . H23 H 0.2635 0.5049 0.5439 0.099 Uiso 1 1 calc R . . C24 C 0.2952(10) 0.329(3) 0.5290(7) 0.041(7) Uani 1 1 d . . . C25 C 0.3115(12) 0.266(4) 0.5015(7) 0.051(9) Uani 1 1 d . . . H25 H 0.3243 0.1745 0.5025 0.061 Uiso 1 1 calc R . . C26 C 0.3093(14) 0.337(3) 0.4727(8) 0.060(11) Uani 1 1 d . . . H26 H 0.3184 0.2876 0.4545 0.072 Uiso 1 1 calc R . . C27 C 0.1297(11) 0.779(4) 0.3736(7) 0.041(7) Uani 1 1 d . . . C28 C 0.1055(12) 0.813(4) 0.4006(10) 0.063(10) Uani 1 1 d . . . H28 H 0.1201 0.8303 0.4197 0.076 Uiso 1 1 calc R . . C29 C 0.0597(14) 0.820(4) 0.3994(13) 0.077(13) Uani 1 1 d . . . H29 H 0.0441 0.8400 0.4180 0.093 Uiso 1 1 calc R . . C30 C 0.0364(14) 0.798(5) 0.3711(13) 0.082(15) Uani 1 1 d D . . C31 C 0.0603(12) 0.766(5) 0.3449(11) 0.067(10) Uani 1 1 d . . . H31 H 0.0459 0.7494 0.3256 0.080 Uiso 1 1 calc R . . C32 C 0.1065(11) 0.756(4) 0.3462(9) 0.057(9) Uani 1 1 d . . . H32 H 0.1219 0.7327 0.3277 0.069 Uiso 1 1 calc R . . C33 C -0.0123(17) 0.811(5) 0.370(2) 0.11(2) Uani 1 1 d D . . C34 C 0.4554(5) 0.797(2) 0.3768(5) 0.045(8) Uani 1 1 d GD . . C35 C 0.4755(7) 0.9309(19) 0.3821(7) 0.078(14) Uani 1 1 d G . . H35 H 0.4582 1.0134 0.3851 0.094 Uiso 1 1 calc R . . C36 C 0.5214(7) 0.9413(18) 0.3830(7) 0.072(12) Uani 1 1 d GD . . H36 H 0.5348 1.0308 0.3865 0.087 Uiso 1 1 calc R . . C37 C 0.5472(5) 0.818(2) 0.3785(5) 0.045(8) Uani 1 1 d G . . C38 C 0.5271(7) 0.6844(19) 0.3732(6) 0.069(12) Uani 1 1 d G . . H38 H 0.5444 0.6019 0.3702 0.082 Uiso 1 1 calc R . . C39 C 0.4812(7) 0.6739(18) 0.3724(6) 0.074(13) Uani 1 1 d GD . . H39 H 0.4678 0.5845 0.3688 0.089 Uiso 1 1 calc R . . C40 C 0.2922(10) 1.066(3) 0.2760(7) 0.040(7) Uani 1 1 d . . . C41 C 0.2725(15) 0.999(4) 0.2498(8) 0.073(13) Uani 1 1 d . . . H41 H 0.2589 0.9094 0.2523 0.087 Uiso 1 1 calc R . . C42 C 0.2727(15) 1.064(5) 0.2203(7) 0.072(13) Uani 1 1 d . . . H42 H 0.2583 1.0188 0.2033 0.086 Uiso 1 1 calc R . . C43 C 0.2940(9) 1.195(3) 0.2152(7) 0.036(7) Uani 1 1 d . . . C44 C 0.3126(11) 1.261(4) 0.2414(7) 0.044(8) Uani 1 1 d . . . H44 H 0.3265 1.3505 0.2389 0.053 Uiso 1 1 calc R . . C45 C 0.3112(11) 1.199(4) 0.2713(8) 0.049(9) Uani 1 1 d . . . H45 H 0.3233 1.2480 0.2886 0.059 Uiso 1 1 calc R . . C46 C 0.2971(10) 1.261(4) 0.1830(7) 0.038(7) Uani 1 1 d . . . C47 C 0.2990(10) 1.248(4) 0.0602(7) 0.038(7) Uani 1 1 d . . . C48 C 0.4027(12) 1.327(3) 0.1215(7) 0.041(8) Uani 1 1 d . . . Cd1 Cd 0.31379(7) 1.3436(2) 0.12134(4) 0.0343(10) Uani 1 1 d . . . Co2 Co 0.29330(19) 0.7764(6) 0.37429(11) 0.0454(16) Uani 1 1 d . . . N1 N 0.2468(8) 0.874(2) 0.3487(5) 0.034(5) Uani 1 1 d . . . N2 N 0.3395(8) 0.859(3) 0.3463(5) 0.037(6) Uani 1 1 d . . . N3 N 0.3389(8) 0.699(3) 0.4026(5) 0.038(6) Uani 1 1 d . . . N4 N 0.2468(8) 0.678(2) 0.3987(5) 0.036(6) Uani 1 1 d . . . O1 O -0.0335(12) 0.820(3) 0.3957(14) 0.14(2) Uani 1 1 d . . . O2 O -0.0306(13) 0.811(5) 0.3432(16) 0.16(2) Uani 1 1 d . . . O3 O 0.2799(8) 1.196(3) 0.1599(5) 0.059(6) Uani 1 1 d . . . O4 O 0.3180(8) 1.377(3) 0.1791(5) 0.053(6) Uani 1 1 d . . . O5 O 0.2814(8) 1.193(3) 0.0842(5) 0.065(7) Uani 1 1 d . . . O6 O 0.3188(8) 1.366(2) 0.0619(5) 0.050(6) Uani 1 1 d . . . O7 O 0.3846(7) 1.450(3) 0.1199(5) 0.050(6) Uani 1 1 d . . . O8 O 0.3805(8) 1.214(3) 0.1232(5) 0.048(6) Uani 1 1 d . . . O9 O 0.2747(12) 1.546(4) 0.1209(6) 0.081(8) Uani 1 1 d U . . H9A H 0.2461 1.5265 0.1215 0.121 Uiso 1 1 d R . . H9B H 0.2809 1.6015 0.1376 0.121 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.060(19) 0.035(15) 0.021(13) -0.001(12) 0.000(13) 0.003(14) C2 0.054(19) 0.033(15) 0.029(15) -0.002(12) 0.000(14) -0.009(14) C3 0.037(16) 0.043(17) 0.032(15) -0.009(13) 0.003(13) -0.009(13) C4 0.047(18) 0.039(16) 0.022(14) -0.008(12) 0.001(13) -0.004(14) C5 0.036(18) 0.042(18) 0.043(18) -0.010(14) -0.001(12) 0.006(14) C6 0.032(15) 0.036(15) 0.028(14) -0.005(12) 0.001(12) 0.005(12) C7 0.037(16) 0.045(17) 0.034(16) -0.005(14) -0.002(13) 0.009(14) C8 0.040(16) 0.036(15) 0.031(14) -0.004(13) 0.004(13) 0.003(13) C9 0.046(17) 0.036(15) 0.017(12) -0.001(12) -0.006(12) 0.003(13) C10 0.043(17) 0.039(16) 0.025(14) -0.003(12) 0.001(12) 0.000(13) C11 0.038(16) 0.047(17) 0.027(14) 0.001(13) 0.000(12) -0.003(14) C12 0.045(18) 0.053(19) 0.033(15) 0.005(14) 0.005(14) 0.006(16) C13 0.042(18) 0.056(19) 0.045(18) 0.003(16) 0.007(15) 0.005(16) C14 0.037(17) 0.044(17) 0.039(17) 0.000(13) 0.003(13) 0.004(14) C15 0.039(17) 0.034(15) 0.046(18) 0.004(13) -0.001(13) 0.004(14) C16 0.038(17) 0.042(17) 0.040(17) 0.004(14) -0.011(13) 0.002(14) C17 0.043(18) 0.054(19) 0.046(18) 0.002(15) -0.011(15) 0.006(16) C18 0.048(19) 0.053(18) 0.033(16) 0.008(15) -0.012(14) 0.006(16) C19 0.041(17) 0.050(18) 0.032(15) 0.000(14) -0.003(13) 0.006(15) C20 0.042(17) 0.040(16) 0.024(14) -0.002(12) -0.001(12) 0.006(13) C21 0.054(19) 0.052(19) 0.028(15) -0.005(14) -0.002(13) 0.009(16) C22 0.15(4) 0.09(3) 0.04(2) 0.02(2) 0.03(2) 0.08(3) C23 0.12(3) 0.10(3) 0.025(17) 0.002(19) 0.017(19) 0.05(3) C24 0.039(17) 0.047(18) 0.036(17) -0.003(14) 0.001(13) 0.001(14) C25 0.08(2) 0.042(18) 0.034(17) 0.001(15) 0.010(15) 0.004(17) C26 0.11(3) 0.036(18) 0.035(19) -0.004(14) 0.022(18) -0.002(18) C27 0.036(18) 0.041(17) 0.046(18) -0.003(14) 0.003(13) -0.002(14) C28 0.05(2) 0.06(2) 0.07(3) -0.01(2) 0.019(19) -0.004(19) C29 0.05(2) 0.06(2) 0.12(4) -0.02(3) 0.03(3) 0.00(2) C30 0.05(2) 0.04(2) 0.16(5) 0.00(3) 0.00(3) 0.001(19) C31 0.04(2) 0.07(2) 0.09(3) 0.00(2) -0.01(2) -0.002(19) C32 0.04(2) 0.06(2) 0.07(2) -0.003(19) -0.007(17) 0.000(17) C33 0.05(3) 0.05(3) 0.22(8) -0.01(4) 0.02(4) 0.00(3) C34 0.043(19) 0.044(18) 0.048(19) 0.001(14) -0.002(14) 0.002(16) C35 0.04(2) 0.035(19) 0.16(4) 0.00(2) 0.00(2) 0.004(16) C36 0.05(2) 0.037(19) 0.13(4) 0.00(2) 0.00(2) -0.003(17) C37 0.036(18) 0.044(18) 0.05(2) 0.009(14) 0.000(14) -0.004(15) C38 0.04(2) 0.04(2) 0.12(4) -0.01(2) -0.01(2) 0.008(17) C39 0.05(2) 0.038(19) 0.13(4) -0.02(2) -0.01(2) 0.001(17) C40 0.039(17) 0.049(19) 0.032(15) -0.004(13) 0.000(12) -0.001(14) C41 0.11(3) 0.08(3) 0.033(18) 0.011(18) -0.017(19) -0.05(2) C42 0.10(3) 0.09(3) 0.025(17) 0.005(17) -0.012(18) -0.05(3) C43 0.036(16) 0.043(16) 0.030(15) -0.003(13) -0.004(12) 0.004(13) C44 0.06(2) 0.038(16) 0.035(17) 0.001(14) -0.011(14) -0.002(14) C45 0.07(2) 0.045(19) 0.032(17) -0.008(15) -0.015(15) -0.003(16) C46 0.043(17) 0.047(18) 0.024(15) -0.005(14) 0.004(13) -0.002(15) C47 0.036(16) 0.048(19) 0.030(16) 0.000(14) -0.003(13) -0.002(14) C48 0.045(19) 0.036(18) 0.041(18) -0.006(13) -0.005(13) -0.005(16) Cd1 0.0346(15) 0.0416(15) 0.0268(14) -0.0008(8) -0.0014(8) 0.0016(9) Co2 0.044(3) 0.049(3) 0.043(3) 0.002(2) -0.001(2) 0.002(2) N1 0.045(14) 0.035(12) 0.023(11) -0.006(10) 0.004(10) 0.000(11) N2 0.040(14) 0.040(14) 0.032(13) -0.005(10) -0.003(11) 0.007(11) N3 0.044(15) 0.040(13) 0.029(12) 0.001(11) -0.002(11) 0.000(11) N4 0.046(15) 0.036(13) 0.026(12) -0.006(10) -0.003(11) -0.002(11) O1 0.06(2) 0.053(18) 0.31(7) -0.01(3) 0.06(3) -0.001(15) O2 0.05(2) 0.13(4) 0.30(7) -0.02(4) -0.06(3) 0.01(2) O3 0.070(16) 0.079(16) 0.027(11) 0.007(11) -0.009(11) -0.024(14) O4 0.069(16) 0.054(14) 0.035(12) 0.008(11) -0.003(10) -0.007(12) O5 0.068(16) 0.10(2) 0.025(11) -0.009(12) 0.012(11) -0.038(15) O6 0.077(17) 0.043(13) 0.031(12) -0.005(10) -0.004(10) 0.001(12) O7 0.039(12) 0.046(13) 0.063(14) 0.000(10) -0.005(10) 0.001(11) O8 0.035(12) 0.042(13) 0.067(15) -0.007(10) -0.002(9) 0.001(11) O9 0.084(11) 0.085(11) 0.074(11) -0.001(8) 0.001(8) 0.014(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.43(4) . ? C1 C20 1.38(4) . ? C1 N4 1.39(4) . ? C2 C3 1.34(4) . ? C3 C4 1.44(4) . ? C4 C5 1.40(4) . ? C4 N4 1.39(4) . ? C5 C6 1.40(5) . ? C5 C27 1.50(5) . ? C6 C7 1.44(4) . ? C6 N1 1.37(4) . ? C7 C8 1.34(4) . ? C8 C9 1.45(4) . ? C9 C10 1.39(4) . ? C9 N1 1.37(3) . ? C10 C11 1.39(4) . ? C10 C40 1.49(4) . ? C11 C12 1.46(4) . ? C11 N2 1.37(4) . ? C12 C13 1.33(4) . ? C13 C14 1.45(4) . ? C14 C15 1.39(4) . ? C14 N2 1.36(4) . ? C15 C16 1.39(4) . ? C15 C34 1.50(4) . ? C16 C17 1.45(4) . ? C16 N3 1.37(4) . ? C17 C18 1.33(5) . ? C18 C19 1.45(4) . ? C19 C20 1.40(4) . ? C19 N3 1.37(4) . ? C20 C21 1.46(4) . ? C21 C22 1.40(5) . ? C21 C26 1.40(5) . ? C22 C23 1.37(5) . ? C23 C24 1.36(5) . ? C24 C25 1.38(4) . ? C24 C47 1.49(4) 8_576 ? C25 C26 1.37(5) . ? C27 C28 1.38(5) . ? C27 C32 1.36(5) . ? C28 C29 1.38(6) . ? C29 C30 1.39(7) . ? C30 C31 1.35(6) . ? C30 C33 1.48(6) . ? C31 C32 1.40(5) . ? C33 O1 1.25(8) . ? C33 O2 1.26(9) . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C37 C48 1.52(4) 4_645 ? C38 C39 1.3900 . ? C40 C41 1.39(4) . ? C40 C45 1.37(5) . ? C41 C42 1.37(5) . ? C42 C43 1.38(5) . ? C43 C44 1.37(4) . ? C43 C46 1.48(4) . ? C44 C45 1.38(5) . ? C46 Cd1 2.74(3) . ? C46 O3 1.25(4) . ? C46 O4 1.25(4) . ? C47 C24 1.49(4) 8_575 ? C47 Cd1 2.74(3) . ? C47 O5 1.25(4) . ? C47 O6 1.24(4) . ? C48 C37 1.52(15) 4_655 ? C48 Cd1 2.69(4) . ? C48 O7 1.26(4) . ? C48 O8 1.24(4) . ? Cd1 O3 2.35(2) . ? Cd1 O4 2.44(2) . ? Cd1 O5 2.30(2) . ? Cd1 O6 2.50(2) . ? Cd1 O7 2.35(2) . ? Cd1 O8 2.34(2) . ? Cd1 O9 2.21(3) . ? Co2 N1 1.98(2) . ? Co2 N2 1.97(3) . ? Co2 N3 1.95(2) . ? Co2 N4 1.96(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 C20 C1 C2 126(3) . . ? C20 C1 N4 125(3) . . ? N4 C1 C2 109(3) . . ? C3 C2 C1 109(3) . . ? C2 C3 C4 106(3) . . ? C5 C4 C3 125(3) . . ? N4 C4 C3 111(3) . . ? N4 C4 C5 124(3) . . ? C4 C5 C6 122(3) . . ? C4 C5 C27 119(3) . . ? C6 C5 C27 118(3) . . ? C5 C6 C7 125(3) . . ? N1 C6 C5 124(3) . . ? N1 C6 C7 111(2) . . ? C8 C7 C6 106(3) . . ? C7 C8 C9 107(3) . . ? C10 C9 C8 124(2) . . ? N1 C9 C8 109(2) . . ? N1 C9 C10 127(3) . . ? C9 C10 C40 120(3) . . ? C11 C10 C9 121(3) . . ? C11 C10 C40 119(3) . . ? C10 C11 C12 124(3) . . ? N2 C11 C10 126(3) . . ? N2 C11 C12 109(3) . . ? C13 C12 C11 108(3) . . ? C12 C13 C14 106(3) . . ? C15 C14 C13 124(3) . . ? N2 C14 C13 111(3) . . ? N2 C14 C15 125(3) . . ? C14 C15 C34 118(3) . . ? C16 C15 C14 123(3) . . ? C16 C15 C34 119(2) . . ? C15 C16 C17 125(3) . . ? N3 C16 C15 125(3) . . ? N3 C16 C17 110(3) . . ? C18 C17 C16 107(3) . . ? C17 C18 C19 107(3) . . ? C20 C19 C18 124(3) . . ? N3 C19 C18 110(3) . . ? N3 C19 C20 126(3) . . ? C1 C20 C19 122(3) . . ? C1 C20 C21 122(3) . . ? C19 C20 C21 116(3) . . ? C22 C21 C20 121(3) . . ? C26 C21 C20 124(3) . . ? C26 C21 C22 115(3) . . ? C23 C22 C21 122(4) . . ? C24 C23 C22 123(3) . . ? C23 C24 C25 117(3) . . ? C23 C24 C47 123(3) . 8_576 ? C25 C24 C47 121(3) . 8_576 ? C26 C25 C24 121(3) . . ? C25 C26 C21 123(3) . . ? C28 C27 C5 122(3) . . ? C32 C27 C5 121(3) . . ? C32 C27 C28 117(4) . . ? C27 C28 C29 121(4) . . ? C28 C29 C30 122(4) . . ? C29 C30 C33 121(5) . . ? C31 C30 C29 117(4) . . ? C31 C30 C33 122(5) . . ? C30 C31 C32 121(4) . . ? C27 C32 C31 122(4) . . ? O1 C33 C30 120(7) . . ? O1 C33 O2 123(5) . . ? O2 C33 C30 117(7) . . ? C35 C34 C15 119.2(18) . . ? C35 C34 C39 120.0 . . ? C39 C34 C15 120.8(18) . . ? C34 C35 C36 120.0 . . ? C35 C36 C37 120.0 . . ? C36 C37 C48 121.0(18) . 4_645 ? C38 C37 C36 120.0 . . ? C38 C37 C48 118.9(18) . 4_645 ? C37 C38 C39 120.0 . . ? C38 C39 C34 120.0 . . ? C41 C40 C10 119(3) . . ? C45 C40 C10 124(3) . . ? C45 C40 C41 117(3) . . ? C42 C41 C40 121(3) . . ? C41 C42 C43 121(3) . . ? C42 C43 C46 122(3) . . ? C44 C43 C42 117(3) . . ? C44 C43 C46 121(3) . . ? C43 C44 C45 122(3) . . ? C40 C45 C44 121(3) . . ? C43 C46 Cd1 170(2) . . ? O3 C46 C43 119(3) . . ? O3 C46 Cd1 58.7(15) . . ? O3 C46 O4 121(3) . . ? O4 C46 C43 120(3) . . ? O4 C46 Cd1 63.1(15) . . ? C24 C47 Cd1 169(2) 8_575 . ? O5 C47 C24 119(3) . 8_575 ? O5 C47 Cd1 56.4(15) . . ? O6 C47 C24 120(3) . 8_575 ? O6 C47 Cd1 65.7(16) . . ? O6 C47 O5 121(3) . . ? C37 C48 Cd1 180(10) 4_655 . ? O7 C48 C37 119(8) . 4_655 ? O7 C48 Cd1 61.1(17) . . ? O8 C48 C37 120(8) . 4_655 ? O8 C48 Cd1 60.5(18) . . ? O8 C48 O7 122(3) . . ? C46 Cd1 C47 139.5(10) . . ? C48 Cd1 C46 99.5(9) . . ? C48 Cd1 C47 98.4(9) . . ? O3 Cd1 C46 27.1(9) . . ? O3 Cd1 C47 112.6(8) . . ? O3 Cd1 C48 113.6(9) . . ? O3 Cd1 O4 54.1(8) . . ? O3 Cd1 O6 139.3(8) . . ? O3 Cd1 O7 131.0(8) . . ? O4 Cd1 C46 27.2(9) . . ? O4 Cd1 C47 166.7(9) . . ? O4 Cd1 C48 87.3(8) . . ? O4 Cd1 O6 166.5(8) . . ? O5 Cd1 C46 113.0(8) . . ? O5 Cd1 C47 26.8(9) . . ? O5 Cd1 C48 113.1(9) . . ? O5 Cd1 O3 85.9(9) . . ? O5 Cd1 O4 140.0(8) . . ? O5 Cd1 O6 53.3(8) . . ? O5 Cd1 O7 128.4(8) . . ? O5 Cd1 O8 94.6(9) . . ? O6 Cd1 C46 166.3(8) . . ? O6 Cd1 C47 26.8(8) . . ? O6 Cd1 C48 86.9(8) . . ? O7 Cd1 C46 107.9(8) . . ? O7 Cd1 C47 104.9(8) . . ? O7 Cd1 C48 28.0(9) . . ? O7 Cd1 O4 85.8(8) . . ? O7 Cd1 O6 83.4(8) . . ? O8 Cd1 C46 89.1(8) . . ? O8 Cd1 C47 90.4(8) . . ? O8 Cd1 C48 27.5(9) . . ? O8 Cd1 O3 93.2(9) . . ? O8 Cd1 O4 89.2(8) . . ? O8 Cd1 O6 91.3(7) . . ? O8 Cd1 O7 55.5(8) . . ? O9 Cd1 C46 98.4(9) . . ? O9 Cd1 C47 100.1(10) . . ? O9 Cd1 C48 125.5(12) . . ? O9 Cd1 O3 105.3(10) . . ? O9 Cd1 O4 86.0(9) . . ? O9 Cd1 O5 106.1(11) . . ? O9 Cd1 O6 87.5(8) . . ? O9 Cd1 O7 97.5(11) . . ? O9 Cd1 O8 153.0(11) . . ? N2 Co2 N1 90.3(10) . . ? N3 Co2 N1 173.6(10) . . ? N3 Co2 N2 90.1(11) . . ? N3 Co2 N4 91.2(10) . . ? N4 Co2 N1 89.1(11) . . ? N4 Co2 N2 173.9(10) . . ? C6 N1 Co2 127.5(19) . . ? C9 N1 C6 106(2) . . ? C9 N1 Co2 126(2) . . ? C11 N2 Co2 126(2) . . ? C14 N2 C11 106(2) . . ? C14 N2 Co2 127(2) . . ? C16 N3 C19 106(2) . . ? C16 N3 Co2 127(2) . . ? C19 N3 Co2 126(2) . . ? C1 N4 Co2 126(2) . . ? C4 N4 C1 105(2) . . ? C4 N4 Co2 128.4(19) . . ? C46 O3 Cd1 94.3(19) . . ? C46 O4 Cd1 89.7(17) . . ? C47 O5 Cd1 96.8(19) . . ? C47 O6 Cd1 87.5(18) . . ? C48 O7 Cd1 90.9(19) . . ? C48 O8 Cd1 92(2) . . ? # Attachment '- Structure1_Fe New.cif' data_Structure1_Fe_New _database_code_depnum_ccdc_archive 'CCDC 865038' #TrackingRef '- Structure1_Fe New.cif' _audit_creation_date 2012-02-19 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H24 Cd Fe N4 O9' _chemical_formula_sum 'C55.75 H49.25 Cd Fe N5.75 O11.75' _chemical_formula_weight 1156.01 _chemical_melting_point ? 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' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 '-x, y+1/2, -z+1/2' 4 'x+1/2, -y+1/2, -z' 5 '-x, -y, -z' 6 'x-1/2, y, -z-1/2' 7 'x, -y-1/2, z-1/2' 8 '-x-1/2, y-1/2, z' _cell_length_a 30.1121(14) _cell_length_b 9.2525(4) _cell_length_c 41.8531(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11660.8(9) _cell_formula_units_Z 8 _cell_measurement_reflns_used 8053 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 115.8 _cell_measurement_theta_min 4.22 _exptl_absorpt_coefficient_mu 5.427 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour purple-brown _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular blocks' _exptl_crystal_F_000 4736 _exptl_crystal_size_max .48 _exptl_crystal_size_mid .38 _exptl_crystal_size_min .29 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_unetI/netI 0.0795 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_number 40806 _diffrn_reflns_theta_full 57.90 _diffrn_reflns_theta_max 57.90 _diffrn_reflns_theta_min 2.11 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker Smart 6K CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'CU K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 20.0 _diffrn_source_power 0.9 _diffrn_source_voltage 45.0 _reflns_number_gt 5404 _reflns_number_total 8053 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker Apex2' _computing_data_collection 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 10.201 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.310 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 532 _refine_ls_number_reflns 8053 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1661 _refine_ls_R_factor_gt 0.1441 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+135.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3300 _refine_ls_wR_factor_ref 0.3531 _refine_special_details ; 'SQUEEZE was performed using PLATON to account for disordered solvent molecules and counter cations. The electron density found in each cavity correlates to a final count of 3 molecules of HCON(C2H5)2, 2 H2Os, and 1 (C2H5)2NH+' 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 -0.028 0.007 2552 725 '10[HCON(C2H5)2]4(C2H5)2NH 4H2' 2 0.500 0.343 0.368 2552 727 '10[HCON(C2H5)2]4(C2H5)2NH 4H2' 'the following constraints were used to better model disorder, ISOR, AFIX 66, and HFIX to determine Hydrogen atoms' 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 C28 C 0.7719(5) 0.0033(17) 0.7495(3) 0.072(4) Uani 1 1 d . . . H28 H 0.7580 0.0948 0.7518 0.086 Uiso 1 1 calc R . . C29 C 0.7725(5) -0.0633(17) 0.7197(3) 0.072(5) Uani 1 1 d . . . H29 H 0.7577 -0.0177 0.7024 0.086 Uiso 1 1 calc R . . C27 C 0.7912(4) -0.0614(13) 0.7755(2) 0.042(3) Uani 1 1 d . . . C16 C 0.7922(4) 0.0190(13) 0.8064(3) 0.044(3) Uani 1 1 d . . . C32 C 0.8116(4) -0.1942(14) 0.7710(3) 0.051(3) Uani 1 1 d . . . H32 H 0.8244 -0.2428 0.7888 0.061 Uiso 1 1 calc R . . C31 C 0.8135(4) -0.2562(13) 0.7413(3) 0.050(3) Uani 1 1 d . . . H31 H 0.8288 -0.3453 0.7389 0.060 Uiso 1 1 calc R . . C30 C 0.7939(4) -0.1938(12) 0.7144(3) 0.044(3) Uani 1 1 d . . . C39 C 0.4828(8) 0.191(2) 0.8717(5) 0.096(6) Uani 1 1 d U . . O1 O 0.4668(5) 0.1902(17) 0.8450(5) 0.146(7) Uani 1 1 d . . . O2 O 0.4661(5) 0.1830(15) 0.8966(4) 0.110(4) Uani 1 1 d U . . C33 C 0.6285(2) 0.2286(11) 0.87367(18) 0.047(3) Uani 1 1 d G . . C38 C 0.6056(3) 0.1992(12) 0.90177(16) 0.073(4) Uani 1 1 d G . . H38 H 0.6214 0.1866 0.9212 0.087 Uiso 1 1 calc R . . C37 C 0.5595(3) 0.1884(13) 0.9014(2) 0.100(7) Uani 1 1 d G . . H37 H 0.5439 0.1683 0.9206 0.121 Uiso 1 1 calc R . . C36 C 0.5364(2) 0.2069(13) 0.8730(3) 0.088(6) Uani 1 1 d G . . C35 C 0.5593(3) 0.2362(12) 0.8449(2) 0.085(5) Uani 1 1 d GU . . H35 H 0.5435 0.2489 0.8254 0.102 Uiso 1 1 calc R . . C34 C 0.6053(3) 0.2471(12) 0.84522(15) 0.071(4) Uani 1 1 d G . . H34 H 0.6210 0.2672 0.8260 0.085 Uiso 1 1 calc R . . Cd1 Cd 0.81350(3) 0.84535(9) 1.121325(17) 0.0404(4) Uani 1 1 d . . . Fe2 Fe 0.79230(6) 0.2305(2) 0.87398(4) 0.0407(5) Uani 1 1 d . . . O4 O 0.8186(3) 0.8659(9) 1.06196(19) 0.053(2) Uani 1 1 d . . . O7 O 0.8180(3) 0.8759(10) 1.1787(2) 0.063(2) Uani 1 1 d . . . O9 O 0.7811(3) 0.6966(10) 1.15938(18) 0.058(2) Uani 1 1 d . . . N3 N 0.7457(3) 0.1327(9) 0.8475(2) 0.037(2) Uani 1 1 d . . . N4 N 0.8386(3) 0.1482(11) 0.8452(2) 0.046(2) Uani 1 1 d . . . O3 O 0.7805(3) 0.6966(11) 1.08432(19) 0.062(3) Uani 1 1 d . . . N2 N 0.7461(3) 0.3258(10) 0.8984(2) 0.042(2) Uani 1 1 d . . . N1 N 0.8379(3) 0.3099(9) 0.9020(2) 0.039(2) Uani 1 1 d . . . C6 C 0.7908(4) 0.4447(12) 0.9397(2) 0.038(3) Uani 1 1 d . . . C12 C 0.7015(4) 0.1284(11) 0.8542(2) 0.035(2) Uani 1 1 d . . . C14 C 0.7116(4) -0.0387(12) 0.8162(2) 0.038(3) Uani 1 1 d . . . H14 H 0.7078 -0.1143 0.8011 0.045 Uiso 1 1 calc R . . C11 C 0.6782(4) 0.2302(13) 0.8735(2) 0.041(3) Uani 1 1 d . . . C10 C 0.7010(4) 0.3314(13) 0.8921(3) 0.043(3) Uani 1 1 d . . . C48 C 0.7968(4) 0.7581(12) 1.1830(3) 0.041(3) Uani 1 1 d . . . C20 C 0.8840(4) 0.1643(16) 0.8478(3) 0.058(4) Uani 1 1 d . . . C21 C 0.9554(2) 0.2039(9) 0.8763(2) 0.059(4) Uani 1 1 d G . . C26 C 0.9811(3) 0.3278(7) 0.8732(2) 0.069(4) Uani 1 1 d G . . H26 H 0.9672 0.4192 0.8706 0.083 Uiso 1 1 calc R . . C25 C 1.0272(3) 0.3178(7) 0.8739(2) 0.080(5) Uani 1 1 d G . . H25 H 1.0448 0.4025 0.8718 0.096 Uiso 1 1 calc R . . C24 C 1.0475(2) 0.1840(9) 0.8777(2) 0.049(3) Uani 1 1 d G . . C23 C 1.0217(3) 0.0601(7) 0.8809(2) 0.076(5) Uani 1 1 d G . . H23 H 1.0356 -0.0313 0.8835 0.091 Uiso 1 1 calc R . . C22 C 0.9757(3) 0.0701(7) 0.8802(2) 0.070(4) Uani 1 1 d GU . . H22 H 0.9581 -0.0146 0.8823 0.084 Uiso 1 1 calc R . . C1 C 0.9062(4) 0.2179(14) 0.8757(3) 0.047(3) Uani 1 1 d . . . C40 C 0.7914(3) 0.5333(8) 0.96998(13) 0.045(3) Uani 1 1 d G . . C41 C 0.7734(4) 0.4685(8) 0.99703(17) 0.097(6) Uani 1 1 d G . . H41 H 0.7601 0.3757 0.9955 0.116 Uiso 1 1 calc R . . C42 C 0.7750(4) 0.5396(9) 1.02628(14) 0.081(5) Uani 1 1 d G . . H42 H 0.7628 0.4953 1.0448 0.098 Uiso 1 1 calc R . . C43 C 0.7946(3) 0.6753(8) 1.02847(13) 0.045(3) Uani 1 1 d G . . C44 C 0.8125(3) 0.7401(7) 1.00142(17) 0.060(4) Uani 1 1 d G . . H44 H 0.8258 0.8329 1.0029 0.072 Uiso 1 1 calc R . . C45 C 0.8109(3) 0.6691(8) 0.97217(14) 0.056(4) Uani 1 1 d G . . H45 H 0.8231 0.7133 0.9537 0.067 Uiso 1 1 calc R . . C46 C 0.7976(4) 0.7513(15) 1.0600(3) 0.046(3) Uani 1 1 d . . . C5 C 0.8321(4) 0.3839(15) 0.9296(3) 0.052(3) Uani 1 1 d . . . C13 C 0.6803(4) 0.0202(14) 0.8351(3) 0.048(3) Uani 1 1 d . . . H13 H 0.6498 -0.0054 0.8357 0.058 Uiso 1 1 calc R . . C2 C 0.8839(4) 0.2811(16) 0.9008(3) 0.055(3) Uani 1 1 d . . . C15 C 0.7520(4) 0.0370(13) 0.8238(2) 0.040(3) Uani 1 1 d . . . C17 C 0.8322(4) 0.0784(14) 0.8170(3) 0.045(3) Uani 1 1 d . . . C9 C 0.6793(4) 0.4403(13) 0.9113(3) 0.047(3) Uani 1 1 d . . . H9 H 0.6487 0.4655 0.9110 0.057 Uiso 1 1 calc R . . C8 C 0.7115(4) 0.4993(13) 0.9300(3) 0.047(3) Uani 1 1 d . . . H8 H 0.7073 0.5731 0.9455 0.056 Uiso 1 1 calc R . . C18 C 0.8741(4) 0.0611(16) 0.8006(3) 0.060(4) Uani 1 1 d . . . H18 H 0.8786 0.0205 0.7800 0.072 Uiso 1 1 calc R . . C19 C 0.9047(4) 0.1126(16) 0.8197(3) 0.059(3) Uani 1 1 d . . . H19 H 0.9357 0.1148 0.8154 0.070 Uiso 1 1 calc R . . C7 C 0.7520(4) 0.4327(12) 0.9225(3) 0.043(3) Uani 1 1 d . . . C3 C 0.9035(5) 0.3311(15) 0.9303(3) 0.062(4) Uani 1 1 d . . . H3 H 0.9338 0.3207 0.9362 0.075 Uiso 1 1 calc R . . C4 C 0.8733(4) 0.3919(15) 0.9473(3) 0.055(3) Uani 1 1 d . . . H4 H 0.8772 0.4344 0.9678 0.066 Uiso 1 1 calc R . . O6 O 0.8803(3) 0.7162(10) 1.12311(18) 0.051(2) Uani 1 1 d . . . O5 O 0.8850(3) 0.9483(10) 1.12044(17) 0.050(2) Uani 1 1 d . . . C47 C 0.9023(5) 0.8266(12) 1.1217(3) 0.044(3) Uani 1 1 d . . . O8 O 0.7732(5) 1.0463(17) 1.1213(2) 0.115(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 C28 0.086(11) 0.082(10) 0.047(8) -0.013(7) -0.005(7) 0.044(9) C29 0.094(11) 0.092(11) 0.030(7) 0.005(7) -0.006(7) 0.044(9) C27 0.036(6) 0.061(8) 0.030(6) -0.003(5) -0.003(5) -0.001(6) C16 0.030(6) 0.050(7) 0.052(7) 0.005(6) -0.006(5) -0.008(5) C32 0.067(9) 0.055(8) 0.032(6) 0.011(5) -0.007(6) -0.006(6) C31 0.060(9) 0.032(6) 0.057(8) -0.003(6) -0.006(6) 0.003(5) C30 0.045(7) 0.046(7) 0.040(7) 0.011(5) -0.003(5) -0.008(5) C39 0.096(6) 0.095(6) 0.096(6) 0.0000(10) -0.0001(10) 0.0002(10) O1 0.070(9) 0.118(12) 0.25(2) 0.004(12) -0.047(11) -0.005(8) O2 0.109(5) 0.109(5) 0.113(4) 0.000(2) 0.002(2) 0.000(2) C33 0.026(6) 0.049(7) 0.066(8) 0.001(6) 0.002(5) 0.010(5) C38 0.053(9) 0.092(11) 0.073(10) 0.024(8) 0.016(8) 0.014(8) C37 0.041(10) 0.119(15) 0.142(17) 0.043(13) 0.030(10) 0.016(9) C36 0.028(8) 0.051(8) 0.18(2) 0.003(10) 0.015(10) 0.001(7) C35 0.042(8) 0.096(11) 0.116(12) -0.012(9) -0.026(8) -0.005(7) C34 0.040(9) 0.095(12) 0.077(10) -0.011(9) -0.001(7) -0.007(7) Cd1 0.0355(6) 0.0526(6) 0.0330(5) -0.0006(3) -0.0011(3) 0.0009(4) Fe2 0.0267(10) 0.0523(11) 0.0430(10) -0.0058(8) 0.0001(7) -0.0023(8) O4 0.070(6) 0.052(5) 0.037(5) -0.002(4) -0.001(4) 0.004(4) O7 0.075(7) 0.064(6) 0.049(5) -0.001(4) 0.001(4) -0.001(5) O9 0.069(6) 0.075(6) 0.029(4) 0.000(4) -0.013(4) -0.014(5) N3 0.034(5) 0.046(5) 0.033(5) 0.003(4) 0.005(4) 0.009(4) N4 0.037(6) 0.063(6) 0.037(5) -0.001(5) 0.003(4) -0.006(5) O3 0.065(6) 0.087(7) 0.035(5) 0.000(4) 0.003(4) -0.025(5) N2 0.043(6) 0.044(6) 0.039(5) 0.007(4) -0.007(4) -0.003(4) N1 0.038(6) 0.044(5) 0.035(5) -0.014(4) 0.005(4) -0.006(4) C6 0.040(7) 0.049(7) 0.024(5) 0.003(5) -0.001(5) -0.006(5) C12 0.032(6) 0.039(6) 0.035(6) 0.004(5) 0.000(5) -0.003(5) C14 0.047(7) 0.044(6) 0.022(5) 0.001(5) -0.007(5) 0.005(5) C11 0.032(6) 0.055(7) 0.036(6) 0.014(6) -0.003(4) -0.001(5) C10 0.045(7) 0.054(7) 0.031(6) 0.010(5) -0.007(5) -0.002(6) C48 0.037(7) 0.042(7) 0.043(7) -0.007(5) 0.008(5) -0.005(5) C20 0.028(7) 0.089(10) 0.058(8) 0.007(7) -0.009(6) -0.009(6) C21 0.049(9) 0.071(9) 0.057(8) -0.015(6) 0.006(6) -0.010(7) C26 0.065(10) 0.030(7) 0.113(13) 0.010(7) -0.008(8) 0.002(6) C25 0.060(10) 0.039(8) 0.140(16) 0.001(8) -0.024(9) -0.018(7) C24 0.041(7) 0.055(8) 0.051(7) -0.015(5) 0.005(5) 0.004(6) C23 0.041(8) 0.056(9) 0.130(15) 0.005(8) 0.002(8) 0.003(7) C22 0.045(8) 0.040(7) 0.125(12) -0.005(7) -0.002(7) -0.019(6) C1 0.024(6) 0.057(7) 0.060(8) -0.026(6) 0.002(5) -0.008(5) C40 0.050(7) 0.059(8) 0.028(6) -0.007(5) 0.001(5) 0.001(6) C41 0.145(17) 0.107(14) 0.038(8) -0.014(8) 0.019(9) -0.059(12) C42 0.110(13) 0.084(11) 0.049(8) -0.003(8) 0.010(8) -0.041(10) C43 0.059(8) 0.044(7) 0.033(6) -0.002(5) -0.001(5) -0.001(6) C44 0.080(10) 0.061(8) 0.039(7) -0.009(6) 0.020(6) -0.006(7) C45 0.092(11) 0.030(6) 0.046(7) 0.000(5) 0.019(7) 0.006(6) C46 0.031(7) 0.070(9) 0.037(7) -0.003(6) -0.001(5) -0.001(6) C5 0.037(7) 0.079(9) 0.040(7) -0.011(6) -0.006(5) -0.011(6) C13 0.046(7) 0.064(8) 0.035(6) 0.005(6) 0.004(5) -0.017(6) C2 0.030(7) 0.075(9) 0.062(8) -0.005(7) -0.002(6) -0.012(6) C15 0.042(7) 0.052(7) 0.025(5) 0.007(5) -0.004(5) -0.008(5) C17 0.037(7) 0.061(8) 0.037(6) 0.001(5) 0.003(5) 0.004(6) C9 0.045(7) 0.057(8) 0.040(6) 0.014(6) 0.000(5) 0.005(6) C8 0.058(8) 0.050(7) 0.032(6) 0.008(5) 0.002(6) 0.008(6) C18 0.057(9) 0.075(9) 0.046(7) -0.008(7) 0.003(6) -0.017(7) C19 0.042(7) 0.085(10) 0.049(7) -0.012(7) 0.016(6) -0.011(7) C7 0.051(7) 0.041(7) 0.038(6) 0.004(5) -0.002(5) 0.003(5) C3 0.050(8) 0.080(10) 0.057(8) -0.020(7) -0.014(7) -0.002(7) C4 0.048(8) 0.071(9) 0.048(7) -0.010(6) -0.007(6) -0.003(7) O6 0.017(4) 0.063(6) 0.072(6) -0.003(4) 0.004(3) -0.010(4) O5 0.040(5) 0.055(6) 0.054(5) -0.005(4) -0.001(4) 0.000(4) C47 0.053(8) 0.026(6) 0.054(8) -0.004(5) -0.006(5) -0.004(6) O8 0.148(12) 0.160(13) 0.038(5) 0.008(6) 0.003(6) 0.111(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C28 H28 0.9500 . ? C28 C29 1.389(18) . ? C28 C27 1.371(17) . ? C29 H29 0.9500 . ? C29 C30 1.386(18) . ? C27 C16 1.493(16) . ? C27 C32 1.386(17) . ? C16 C15 1.424(16) . ? C16 C17 1.394(16) . ? C32 H32 0.9500 . ? C32 C31 1.373(17) . ? C31 H31 0.9500 . ? C31 C30 1.396(16) . ? C30 C48 1.446(17) 7_565 ? C39 O1 1.22(2) . ? C39 O2 1.16(2) . ? C39 C36 1.62(3) . ? C33 C38 1.3900 . ? C33 C34 1.3900 . ? C33 C11 1.498(14) . ? C38 H38 0.9500 . ? C38 C37 1.3900 . ? C37 H37 0.9500 . ? C37 C36 1.3900 . ? C36 C35 1.3900 . ? C35 H35 0.9500 . ? C35 C34 1.3900 . ? C34 H34 0.9500 . ? Cd1 O4 2.497(8) . ? Cd1 O7 2.423(9) . ? Cd1 O9 2.320(9) . ? Cd1 O3 2.297(9) . ? Cd1 C48 2.749(11) . ? Cd1 C46 2.753(11) . ? Cd1 O6 2.341(9) . ? Cd1 O5 2.354(8) . ? Cd1 C47 2.680(14) . ? Cd1 O8 2.221(11) . ? Fe2 N3 2.005(9) . ? Fe2 N4 1.993(10) . ? Fe2 N2 1.937(10) . ? Fe2 N1 1.950(9) . ? O4 C46 1.237(15) . ? O7 C48 1.275(15) . ? O9 C48 1.233(14) . ? N3 C12 1.362(14) . ? N3 C15 1.343(14) . ? N4 C20 1.381(15) . ? N4 C17 1.360(15) . ? O3 C46 1.248(15) . ? N2 C10 1.385(15) . ? N2 C7 1.425(14) . ? N1 C5 1.354(15) . ? N1 C2 1.411(15) . ? C6 C40 1.511(12) . ? C6 C5 1.428(17) . ? C6 C7 1.376(16) . ? C12 C11 1.425(16) . ? C12 C13 1.431(16) . ? C14 H14 0.9500 . ? C14 C13 1.345(16) . ? C14 C15 1.438(16) . ? C11 C10 1.396(17) . ? C10 C9 1.447(18) . ? C48 C30 1.446(17) 7_566 ? C20 C1 1.432(17) . ? C20 C19 1.414(18) . ? C21 C26 1.3900 . ? C21 C22 1.3900 . ? C21 C1 1.486(14) . ? C26 H26 0.9500 . ? C26 C25 1.3900 . ? C25 H25 0.9500 . ? C25 C24 1.3900 . ? C24 C23 1.3900 . ? C24 C47 1.516(15) 5_767 ? C23 H23 0.9500 . ? C23 C22 1.3900 . ? C22 H22 0.9500 . ? C1 C2 1.376(17) . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 H41 0.9500 . ? C41 C42 1.3900 . ? C42 H42 0.9500 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C43 C46 1.497(13) . ? C44 H44 0.9500 . ? C44 C45 1.3900 . ? C45 H45 0.9500 . ? C5 C4 1.449(17) . ? C13 H13 0.9500 . ? C2 C3 1.448(18) . ? C17 C18 1.447(17) . ? C9 H9 0.9500 . ? C9 C8 1.361(17) . ? C8 H8 0.9500 . ? C8 C7 1.400(16) . ? C18 H18 0.9500 . ? C18 C19 1.309(18) . ? C19 H19 0.9500 . ? C3 H3 0.9500 . ? C3 C4 1.285(19) . ? C4 H4 0.9500 . ? O6 C47 1.218(15) . ? O5 C47 1.243(14) . ? C47 C24 1.52(6) 5_767 ? 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 C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C27 C28 C29 120.8(12) . . ? C28 C29 H29 118.7 . . ? C30 C29 C28 122.5(12) . . ? C30 C29 H29 118.7 . . ? C28 C27 C16 118.6(11) . . ? C28 C27 C32 117.9(11) . . ? C32 C27 C16 123.3(10) . . ? C15 C16 C27 118.8(9) . . ? C17 C16 C27 119.4(10) . . ? C17 C16 C15 121.7(11) . . ? C27 C32 H32 119.6 . . ? C31 C32 C27 120.7(11) . . ? C31 C32 H32 119.6 . . ? C32 C31 H31 118.6 . . ? C32 C31 C30 122.8(12) . . ? C30 C31 H31 118.6 . . ? C29 C30 C31 115.2(11) . . ? C29 C30 C48 122.3(11) . 7_565 ? C31 C30 C48 122.5(11) . 7_565 ? O1 C39 C36 115.1(18) . . ? O2 C39 O1 131(3) . . ? O2 C39 C36 114.2(19) . . ? C38 C33 C34 120.0 . . ? C38 C33 C11 120.1(6) . . ? C34 C33 C11 119.8(6) . . ? C33 C38 H38 120.0 . . ? C33 C38 C37 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 C38 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C36 C39 121.0(10) . . ? C35 C36 C39 119.0(10) . . ? C35 C36 C37 120.0 . . ? C36 C35 H35 120.0 . . ? C36 C35 C34 120.0 . . ? C34 C35 H35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? O4 Cd1 C48 165.3(3) . . ? O4 Cd1 C46 26.7(3) . . ? O4 Cd1 C47 87.1(3) . . ? O7 Cd1 O4 167.0(3) . . ? O7 Cd1 C48 27.6(3) . . ? O7 Cd1 C46 166.3(4) . . ? O7 Cd1 C47 86.9(3) . . ? O9 Cd1 O4 139.0(3) . . ? O9 Cd1 O7 54.0(3) . . ? O9 Cd1 C48 26.5(3) . . ? O9 Cd1 C46 112.3(4) . . ? O9 Cd1 O6 92.1(3) . . ? O9 Cd1 O5 129.5(3) . . ? O9 Cd1 C47 112.1(3) . . ? O3 Cd1 O4 53.2(3) . . ? O3 Cd1 O7 139.7(3) . . ? O3 Cd1 O9 85.7(3) . . ? O3 Cd1 C48 112.2(3) . . ? O3 Cd1 C46 26.7(3) . . ? O3 Cd1 O6 95.0(3) . . ? O3 Cd1 O5 128.8(3) . . ? O3 Cd1 C47 113.4(3) . . ? C48 Cd1 C46 138.6(4) . . ? O6 Cd1 O4 91.0(3) . . ? O6 Cd1 O7 88.9(3) . . ? O6 Cd1 C48 88.7(3) . . ? O6 Cd1 C46 91.0(3) . . ? O6 Cd1 O5 54.6(3) . . ? O6 Cd1 C47 27.0(3) . . ? O5 Cd1 O4 84.1(3) . . ? O5 Cd1 O7 85.3(3) . . ? O5 Cd1 C48 107.5(3) . . ? O5 Cd1 C46 105.8(3) . . ? O5 Cd1 C47 27.6(3) . . ? C47 Cd1 C48 99.1(3) . . ? C47 Cd1 C46 99.1(3) . . ? O8 Cd1 O4 88.3(3) . . ? O8 Cd1 O7 86.1(3) . . ? O8 Cd1 O9 105.5(5) . . ? O8 Cd1 O3 105.4(5) . . ? O8 Cd1 C48 98.4(4) . . ? O8 Cd1 C46 99.8(4) . . ? O8 Cd1 O6 153.8(6) . . ? O8 Cd1 O5 99.2(6) . . ? O8 Cd1 C47 126.8(6) . . ? N4 Fe2 N3 89.0(4) . . ? N2 Fe2 N3 89.7(4) . . ? N2 Fe2 N4 173.8(4) . . ? N2 Fe2 N1 91.0(4) . . ? N1 Fe2 N3 174.9(4) . . ? N1 Fe2 N4 90.8(4) . . ? C46 O4 Cd1 88.3(7) . . ? C48 O7 Cd1 90.6(7) . . ? C48 O9 Cd1 96.6(7) . . ? C12 N3 Fe2 125.7(7) . . ? C15 N3 Fe2 127.4(7) . . ? C15 N3 C12 105.7(9) . . ? C20 N4 Fe2 127.2(9) . . ? C17 N4 Fe2 127.3(8) . . ? C17 N4 C20 105.1(10) . . ? C46 O3 Cd1 97.4(8) . . ? C10 N2 Fe2 128.3(8) . . ? C10 N2 C7 103.3(9) . . ? C7 N2 Fe2 127.0(8) . . ? C5 N1 Fe2 127.6(8) . . ? C5 N1 C2 104.8(9) . . ? C2 N1 Fe2 126.8(8) . . ? C5 C6 C40 116.9(9) . . ? C7 C6 C40 119.4(10) . . ? C7 C6 C5 123.6(10) . . ? N3 C12 C11 125.3(10) . . ? N3 C12 C13 109.9(10) . . ? C11 C12 C13 124.1(10) . . ? C13 C14 H14 127.3 . . ? C13 C14 C15 105.4(10) . . ? C15 C14 H14 127.3 . . ? C12 C11 C33 119.1(10) . . ? C10 C11 C33 119.7(10) . . ? C10 C11 C12 121.1(11) . . ? N2 C10 C11 124.3(11) . . ? N2 C10 C9 111.3(10) . . ? C11 C10 C9 123.7(11) . . ? C30 C48 Cd1 170.1(8) 7_566 . ? O7 C48 C30 120.6(10) . 7_566 ? O7 C48 Cd1 61.8(6) . . ? O9 C48 C30 120.9(11) . 7_566 ? O9 C48 Cd1 57.0(6) . . ? O9 C48 O7 118.4(11) . . ? N4 C20 C1 124.3(12) . . ? N4 C20 C19 109.5(11) . . ? C19 C20 C1 126.1(11) . . ? C26 C21 C22 120.0 . . ? C26 C21 C1 118.8(8) . . ? C22 C21 C1 121.2(8) . . ? C21 C26 H26 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C25 H25 120.0 . . ? C26 C25 C24 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C24 C47 119.9(7) . 5_767 ? C23 C24 C25 120.0 . . ? C23 C24 C47 120.1(7) . 5_767 ? C24 C23 H23 120.0 . . ? C24 C23 C22 120.0 . . ? C22 C23 H23 120.0 . . ? C21 C22 H22 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C20 C1 C21 116.7(10) . . ? C2 C1 C20 122.7(12) . . ? C2 C1 C21 120.6(10) . . ? C41 C40 C6 116.5(6) . . ? C41 C40 C45 120.0 . . ? C45 C40 C6 123.4(6) . . ? C40 C41 H41 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C41 C42 H42 120.0 . . ? C41 C42 C43 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 C46 120.6(7) . . ? C44 C43 C46 119.4(7) . . ? C43 C44 H44 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C40 C45 H45 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? O4 C46 Cd1 65.0(6) . . ? O4 C46 O3 120.2(11) . . ? O4 C46 C43 119.5(10) . . ? O3 C46 Cd1 55.9(6) . . ? O3 C46 C43 120.2(11) . . ? C43 C46 Cd1 168.8(8) . . ? N1 C5 C6 124.4(10) . . ? N1 C5 C4 110.6(11) . . ? C6 C5 C4 125.0(11) . . ? C12 C13 H13 126.3 . . ? C14 C13 C12 107.5(10) . . ? C14 C13 H13 126.3 . . ? N1 C2 C3 108.0(11) . . ? C1 C2 N1 125.9(11) . . ? C1 C2 C3 126.1(12) . . ? C16 C15 C14 123.4(10) . . ? N3 C15 C16 125.0(10) . . ? N3 C15 C14 111.4(10) . . ? C16 C17 C18 124.0(11) . . ? N4 C17 C16 125.9(11) . . ? N4 C17 C18 109.9(10) . . ? C10 C9 H9 127.0 . . ? C8 C9 C10 106.1(11) . . ? C8 C9 H9 127.0 . . ? C9 C8 H8 125.8 . . ? C9 C8 C7 108.4(11) . . ? C7 C8 H8 125.8 . . ? C17 C18 H18 126.7 . . ? C19 C18 C17 106.5(11) . . ? C19 C18 H18 126.7 . . ? C20 C19 H19 125.6 . . ? C18 C19 C20 108.7(12) . . ? C18 C19 H19 125.6 . . ? C6 C7 N2 122.0(10) . . ? C6 C7 C8 126.0(11) . . ? C8 C7 N2 110.9(10) . . ? C2 C3 H3 125.5 . . ? C4 C3 C2 109.0(12) . . ? C4 C3 H3 125.5 . . ? C5 C4 H4 126.3 . . ? C3 C4 C5 107.5(11) . . ? C3 C4 H4 126.3 . . ? C47 O6 Cd1 92.2(8) . . ? C47 O5 Cd1 91.0(8) . . ? C24 C47 Cd1 179.6(19) 5_767 . ? O6 C47 Cd1 60.8(7) . . ? O6 C47 C24 119(3) . 5_767 ? O6 C47 O5 122.2(13) . . ? O5 C47 Cd1 61.4(7) . . ? O5 C47 C24 119(3) . 5_767 ? # Attachment '- Structure1_Ni new.cif' data_dbsdsuni-sr _database_code_depnum_ccdc_archive 'CCDC 865039' #TrackingRef '- Structure1_Ni new.cif' _audit_creation_date 2012-02-16 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C96 H52 Cd2 N8 Ni1.12 O18, 3(C5 H11 N1 O1), (H2 O1), (C5, H11, N1)' _chemical_formula_sum 'C105.50 H76 Cd2 N10 Ni2 O20.50' _chemical_formula_weight 2153.98 _chemical_melting_point ? 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' Cd Cd 0.1185 4.6533 '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' Ni Ni -3.0029 0.5091 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 '-x, y+1/2, -z+1/2' 4 'x+1/2, -y+1/2, -z' 5 '-x, -y, -z' 6 'x-1/2, y, -z-1/2' 7 'x, -y-1/2, z-1/2' 8 '-x-1/2, y-1/2, z' _cell_length_a 59.431(2) _cell_length_b 9.3517(4) _cell_length_c 41.7871(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 23224.5(16) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9816 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 122.32 _cell_measurement_theta_min 2.98 _exptl_absorpt_coefficient_mu 3.790 _exptl_absorpt_correction_T_max 0.5753 _exptl_absorpt_correction_T_min 0.4461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour purple-red _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular blocks' _exptl_crystal_F_000 8760 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0740 _diffrn_reflns_av_unetI/netI 0.0560 _diffrn_reflns_limit_h_max 67 _diffrn_reflns_limit_h_min -66 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_number 95677 _diffrn_reflns_theta_full 61.16 _diffrn_reflns_theta_max 61.16 _diffrn_reflns_theta_min 1.49 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.960 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_device_type 'Bruker Smart 6K CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'CU K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 20.0 _diffrn_source_power 0.9 _diffrn_source_voltage 45.0 _reflns_number_gt 12550 _reflns_number_total 17152 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker APEX2' _computing_data_collection 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 2.718 _refine_diff_density_min -1.463 _refine_diff_density_rms 0.197 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.524 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1103 _refine_ls_number_reflns 17152 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1582 _refine_ls_R_factor_gt 0.1341 _refine_ls_restrained_S_all 1.530 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+109.1495P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3052 _refine_ls_wR_factor_ref 0.3175 _refine_special_details ; 'CHEMW03_ALERT_2_A-added in atoms found using SQUEEZE' 'PLAT043_ALERT_1_A-added atoms found using SQUEEZE' 'PLAT602_ALERT-A_2-Large void typical of MOFs, treated with SQUEEZE' 'the following constraints were used to better model disorder, AFIX 66, ISOR, and HFIX to determine Hydrogen atoms' 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 0.125 0.438 0.001 2484 896 '12[HCON(C2H5)2]4(C2H5)2NH 4H2' 2 0.375 0.073 0.002 2484 897 '12[HCON(C2H5)2]4(C2H5)2NH 4H2O' 3 0.625 1.028 -0.005 2484 898 '12[HCON(C2H5)2]4(C2H5)2NH 4H2O' 4 0.875 0.398 -0.005 2484 892 '12[HCON(C2H5)2]4(C2H5)2NH 4H2O' _platon_squeeze_details 'SQUEEZE was performed using PLATON to account for disordered solvent molecules and counter cations. The electron density found in each cavity correlates to a final count of 3 molecules of HCON(C2H5)2, 2 H2Os, and 1 (C2H5)2NH+' 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.01799(18) 1.4600(11) 0.4356(2) 0.048(3) Uani 1 1 d . . . C2 C 0.03874(17) 1.4086(10) 0.4455(2) 0.042(2) Uani 1 1 d . . . C3 C 0.06052(18) 1.4250(11) 0.4293(2) 0.051(3) Uani 1 1 d . . . H3 H 0.0628 1.4647 0.4087 0.061 Uiso 1 1 calc R . . C4 C 0.07673(19) 1.3736(12) 0.4490(3) 0.063(3) Uani 1 1 d . . . H4 H 0.0924 1.3697 0.4448 0.075 Uiso 1 1 calc R . . C5 C 0.06530(18) 1.3254(10) 0.4779(3) 0.049(2) Uani 1 1 d . . . C6 C 0.0776(2) 1.2763(12) 0.5042(2) 0.060(3) Uani 1 1 d . . . C7 C 0.06493(19) 1.2087(11) 0.5303(3) 0.053(3) Uani 1 1 d . . . C8 C 0.07656(18) 1.1673(11) 0.5607(3) 0.055(3) Uani 1 1 d . . . H8 H 0.0918 1.1849 0.5664 0.066 Uiso 1 1 calc R . . C9 C 0.06089(18) 1.1004(11) 0.5779(2) 0.052(3) Uani 1 1 d . . . H9 H 0.0632 1.0593 0.5984 0.062 Uiso 1 1 calc R . . C10 C 0.03946(17) 1.0999(10) 0.5601(2) 0.044(2) Uani 1 1 d . . . C11 C 0.01957(17) 1.0345(11) 0.5690(2) 0.045(2) Uani 1 1 d . . . C12 C -0.00119(17) 1.0519(10) 0.55279(19) 0.042(2) Uani 1 1 d . . . C13 C -0.02148(17) 0.9799(10) 0.5595(2) 0.044(2) Uani 1 1 d . . . H13 H -0.0231 0.9056 0.5748 0.053 Uiso 1 1 calc R . . C14 C -0.03798(17) 1.0310(10) 0.5413(2) 0.044(2) Uani 1 1 d . . . H14 H -0.0533 1.0030 0.5411 0.053 Uiso 1 1 calc R . . C15 C -0.02719(16) 1.1389(11) 0.5220(2) 0.046(2) Uani 1 1 d . . . C16 C -0.0398(2) 1.2302(11) 0.50145(19) 0.051(3) Uani 1 1 d . . . C17 C -0.02825(17) 1.3304(11) 0.4813(2) 0.047(2) Uani 1 1 d . . . C18 C -0.03958(17) 1.4356(11) 0.4606(2) 0.046(2) Uani 1 1 d . . . H18 H -0.0552 1.4580 0.4601 0.055 Uiso 1 1 calc R . . C19 C -0.02327(17) 1.4932(9) 0.44248(19) 0.039(2) Uani 1 1 d . . . H19 H -0.0256 1.5650 0.4267 0.046 Uiso 1 1 calc R . . C20 C -0.00262(17) 1.4330(9) 0.44999(18) 0.038(2) Uani 1 1 d . . . C25 C 0.13891(11) 1.1782(6) 0.5049(2) 0.083(4) Uani 1 1 d G . . H25 H 0.1482 1.0956 0.5044 0.099 Uiso 1 1 calc R . . C24 C 0.14858(9) 1.3135(8) 0.5057(2) 0.059(3) Uani 1 1 d G . . C23 C 0.13497(12) 1.4344(6) 0.5064(2) 0.081(4) Uani 1 1 d GU . . H23 H 0.1416 1.5268 0.5070 0.097 Uiso 1 1 calc R . . C22 C 0.11169(11) 1.4199(6) 0.5064(2) 0.092(5) Uani 1 1 d G . . H22 H 0.1024 1.5025 0.5069 0.110 Uiso 1 1 calc R . . C21 C 0.10202(9) 1.2846(7) 0.5056(2) 0.051(3) Uani 1 1 d G . . C26 C 0.11563(12) 1.1638(5) 0.5048(2) 0.076(4) Uani 1 1 d G . . H26 H 0.1090 1.0713 0.5043 0.092 Uiso 1 1 calc R . . C27 C 0.17389(18) 1.3262(11) 0.5054(3) 0.052(3) Uani 1 1 d . . . C28 C 0.01977(16) 0.9504(10) 0.5996(2) 0.040(2) Uani 1 1 d . . . C29 C 0.03366(17) 0.8330(10) 0.60381(19) 0.043(2) Uani 1 1 d . . . H29 H 0.0425 0.8003 0.5864 0.051 Uiso 1 1 calc R . . C30 C 0.03487(17) 0.7630(9) 0.6326(2) 0.041(2) Uani 1 1 d . . . H30 H 0.0444 0.6818 0.6348 0.049 Uiso 1 1 calc R . . C31 C 0.02244(15) 0.8093(10) 0.6585(2) 0.036(2) Uani 1 1 d . . . C32 C 0.00880(19) 0.9228(12) 0.6541(2) 0.057(3) Uani 1 1 d . . . H32 H 0.0001 0.9549 0.6718 0.068 Uiso 1 1 calc R . . C33 C 0.00670(19) 0.9945(12) 0.6258(2) 0.056(3) Uani 1 1 d . . . H33 H -0.0034 1.0727 0.6239 0.067 Uiso 1 1 calc R . . C34 C 0.02464(16) 0.7345(10) 0.6904(2) 0.038(2) Uani 1 1 d . . . C36 C -0.07693(11) 1.2481(8) 0.52890(11) 0.054(3) Uani 1 1 d G . . H36 H -0.0693 1.2671 0.5484 0.065 Uiso 1 1 calc R . . C37 C -0.10029(11) 1.2406(8) 0.52839(14) 0.069(3) Uani 1 1 d G . . H37 H -0.1086 1.2545 0.5475 0.082 Uiso 1 1 calc R . . C38 C -0.11146(8) 1.2127(8) 0.49984(17) 0.053(3) Uani 1 1 d G . . C39 C -0.09929(11) 1.1922(8) 0.47181(13) 0.063(3) Uani 1 1 d G . . H39 H -0.1069 1.1732 0.4523 0.076 Uiso 1 1 calc R . . C40 C -0.07593(10) 1.1997(8) 0.47233(11) 0.049(2) Uani 1 1 d G . . H40 H -0.0676 1.1858 0.4532 0.059 Uiso 1 1 calc R . . C35 C -0.06475(8) 1.2276(7) 0.50087(14) 0.040(2) Uani 1 1 d G . . C41 C -0.1361(3) 1.2014(13) 0.4993(4) 0.083(4) Uani 1 1 d . . . C42 C 0.23181(17) 0.9524(10) 0.6868(2) 0.044(2) Uani 1 1 d . . . C43 C 0.21065(17) 0.8905(10) 0.6964(3) 0.049(3) Uani 1 1 d . . . C44 C 0.19020(19) 0.8968(11) 0.6774(3) 0.055(3) Uani 1 1 d . . . H44 H 0.1885 0.9343 0.6564 0.066 Uiso 1 1 calc R . . C45 C 0.1740(2) 0.8370(11) 0.6963(3) 0.066(3) Uani 1 1 d . . . H45 H 0.1585 0.8276 0.6910 0.079 Uiso 1 1 calc R . . C46 C 0.18453(19) 0.7905(11) 0.7257(3) 0.055(3) Uani 1 1 d . . . C47 C 0.17392(19) 0.7275(9) 0.7520(3) 0.049(3) Uani 1 1 d . . . C48 C 0.1845(2) 0.6724(10) 0.7787(3) 0.059(3) Uani 1 1 d . . . C49 C 0.1730(2) 0.6234(12) 0.8075(3) 0.063(3) Uani 1 1 d . . . H49 H 0.1573 0.6267 0.8115 0.075 Uiso 1 1 calc R . . C50 C 0.18942(18) 0.5711(12) 0.8277(3) 0.060(3) Uani 1 1 d . . . H50 H 0.1874 0.5340 0.8487 0.072 Uiso 1 1 calc R . . C51 C 0.21039(18) 0.5845(11) 0.8103(2) 0.050(2) Uani 1 1 d . . . C52 C 0.23083(16) 0.5265(9) 0.8210(2) 0.042(2) Uani 1 1 d . . . C53 C 0.25146(18) 0.5461(11) 0.8055(2) 0.050(3) Uani 1 1 d . . . C54 C 0.27216(18) 0.4745(11) 0.8142(2) 0.051(3) Uani 1 1 d . . . H54 H 0.2742 0.4032 0.8301 0.062 Uiso 1 1 calc R . . C55 C 0.28827(19) 0.5321(11) 0.7944(3) 0.057(3) Uani 1 1 d . . . H55 H 0.3037 0.5053 0.7939 0.069 Uiso 1 1 calc R . . C56 C 0.27783(17) 0.6411(11) 0.7742(2) 0.049(3) Uani 1 1 d . . . C57 C 0.28937(19) 0.7353(10) 0.7542(2) 0.043(2) Uani 1 1 d . . . C58 C 0.27824(18) 0.8313(11) 0.7339(2) 0.051(3) Uani 1 1 d . . . C59 C 0.28942(19) 0.9355(11) 0.7142(2) 0.050(3) Uani 1 1 d . . . H59 H 0.3050 0.9575 0.7144 0.061 Uiso 1 1 calc R . . C60 C 0.27318(19) 0.9983(11) 0.6947(3) 0.057(3) Uani 1 1 d . . . H60 H 0.2754 1.0715 0.6793 0.068 Uiso 1 1 calc R . . C61 C 0.2519(2) 0.9278(11) 0.7030(2) 0.055(3) Uani 1 1 d . . . C62 C 0.23123(17) 1.0359(10) 0.6571(2) 0.047(2) Uani 1 1 d . . . C63 C 0.21781(18) 1.1575(10) 0.6534(2) 0.049(3) Uani 1 1 d . . . H63 H 0.2094 1.1918 0.6711 0.059 Uiso 1 1 calc R . . C64 C 0.21659(16) 1.2274(11) 0.6250(2) 0.044(2) Uani 1 1 d . . . H64 H 0.2072 1.3093 0.6235 0.053 Uiso 1 1 calc R . . C65 C 0.22840(19) 1.1848(12) 0.5981(2) 0.054(3) Uani 1 1 d . . . C66 C 0.2425(2) 1.0655(14) 0.6018(3) 0.070(4) Uani 1 1 d . . . H66 H 0.2511 1.0326 0.5841 0.084 Uiso 1 1 calc R . . C67 C 0.2442(2) 0.9952(13) 0.6307(3) 0.066(3) Uani 1 1 d . . . H67 H 0.2544 0.9174 0.6328 0.079 Uiso 1 1 calc R . . C68 C 0.22655(19) 1.2577(12) 0.5673(2) 0.051(3) Uani 1 1 d . . . C69 C 0.14832(8) 0.7143(7) 0.75078(18) 0.053(3) Uani 1 1 d G . . C70 C 0.13509(11) 0.8369(5) 0.75101(19) 0.058(3) Uani 1 1 d G . . H70 H 0.1420 0.9286 0.7511 0.070 Uiso 1 1 calc R . . C71 C 0.11178(10) 0.8254(5) 0.75107(19) 0.064(3) Uani 1 1 d G . . H71 H 0.1027 0.9092 0.7512 0.076 Uiso 1 1 calc R . . C72 C 0.10169(8) 0.6913(6) 0.75091(17) 0.044(2) Uani 1 1 d G . . C73 C 0.11492(11) 0.5687(5) 0.7507(2) 0.079(4) Uani 1 1 d G . . H73 H 0.1080 0.4771 0.7506 0.095 Uiso 1 1 calc R . . C74 C 0.13823(11) 0.5802(5) 0.7506(2) 0.083(5) Uani 1 1 d G . . H74 H 0.1473 0.4965 0.7505 0.100 Uiso 1 1 calc R . . C75 C 0.0767(2) 0.6804(11) 0.7521(2) 0.052(3) Uani 1 1 d . . . C76 C 0.23145(18) 0.4454(11) 0.8512(2) 0.051(3) Uani 1 1 d . . . C77 C 0.21837(18) 0.3203(9) 0.8558(3) 0.052(3) Uani 1 1 d . . . H77 H 0.2103 0.2812 0.8382 0.063 Uiso 1 1 calc R . . C78 C 0.21703(19) 0.2534(11) 0.8854(2) 0.052(3) Uani 1 1 d . . . H78 H 0.2078 0.1712 0.8876 0.062 Uiso 1 1 calc R . . C79 C 0.22880(17) 0.3032(10) 0.9118(2) 0.045(2) Uani 1 1 d . . . C80 C 0.2415(2) 0.4207(14) 0.9075(3) 0.068(3) Uani 1 1 d . . . H80 H 0.2493 0.4586 0.9254 0.081 Uiso 1 1 calc R . . C81 C 0.2437(2) 0.4907(13) 0.8778(2) 0.061(3) Uani 1 1 d . . . H81 H 0.2536 0.5697 0.8759 0.073 Uiso 1 1 calc R . . C82 C 0.3141(2) 0.7291(11) 0.7539(2) 0.048(3) Uani 1 1 d . . . C83 C 0.3267(2) 0.7495(12) 0.7826(2) 0.057(3) Uani 1 1 d . . . H83 H 0.3190 0.7715 0.8020 0.069 Uiso 1 1 calc R . . C84 C 0.3500(2) 0.7377(13) 0.7828(3) 0.063(3) Uani 1 1 d . . . H84 H 0.3579 0.7492 0.8024 0.076 Uiso 1 1 calc R . . C85 C 0.3621(2) 0.7089(11) 0.7544(3) 0.052(3) Uani 1 1 d . . . C86 C 0.3498(2) 0.6963(12) 0.7257(3) 0.064(3) Uani 1 1 d . . . H86 H 0.3576 0.6808 0.7062 0.077 Uiso 1 1 calc R . . C87 C 0.3263(2) 0.7058(13) 0.7253(3) 0.064(3) Uani 1 1 d . . . H87 H 0.3185 0.6966 0.7056 0.077 Uiso 1 1 calc R . . C88 C 0.3868(3) 0.7014(14) 0.7534(3) 0.067(3) Uani 1 1 d U . . C89 C 0.2270(2) 1.2680(16) 0.4428(2) 0.063(4) Uani 1 1 d . . . C90 C 0.02333(17) 0.7453(10) 0.8129(2) 0.040(2) Uani 1 1 d . . . C91 C 0.01777(17) 1.5443(10) 0.40466(19) 0.042(2) Uani 1 1 d . . . C92 C 0.00606(19) 1.4912(12) 0.3778(2) 0.058(3) Uani 1 1 d . . . H92 H -0.0030 1.4078 0.3796 0.070 Uiso 1 1 calc R . . C93 C 0.00782(18) 1.5608(12) 0.3492(2) 0.054(3) Uani 1 1 d . . . H93 H -0.0001 1.5243 0.3313 0.065 Uiso 1 1 calc R . . C94 C 0.02039(17) 1.6792(10) 0.34555(19) 0.044(2) Uani 1 1 d . . . C95 C 0.03223(17) 1.7361(9) 0.3726(2) 0.041(2) Uani 1 1 d . . . H95 H 0.0412 1.8197 0.3708 0.049 Uiso 1 1 calc R . . C96 C 0.03011(16) 1.6659(9) 0.40121(18) 0.040(2) Uani 1 1 d . . . H96 H 0.0376 1.7037 0.4194 0.048 Uiso 1 1 calc R . . Cd1 Cd 0.218770(14) 1.34783(8) 0.50515(2) 0.0573(3) Uani 1 1 d . . . Cd2 Cd 0.031272(13) 0.65387(7) 0.752591(15) 0.0453(2) Uani 1 1 d . . . N1 N -0.00473(13) 1.1490(8) 0.52868(15) 0.0376(18) Uani 1 1 d . . . N2 N 0.04307(14) 1.1721(8) 0.53127(17) 0.0414(18) Uani 1 1 d . . . N3 N 0.04271(14) 1.3405(8) 0.47464(17) 0.0415(18) Uani 1 1 d . . . N4 N -0.00549(13) 1.3364(8) 0.47434(16) 0.0409(19) Uani 1 1 d . . . N5 N 0.20741(15) 0.8220(8) 0.7245(2) 0.049(2) Uani 1 1 d . . . N6 N 0.20716(13) 0.6503(8) 0.7819(2) 0.046(2) Uani 1 1 d . . . N7 N 0.25486(14) 0.6447(8) 0.7806(2) 0.049(2) Uani 1 1 d . . . N8 N 0.25519(15) 0.8317(9) 0.7277(2) 0.054(2) Uani 1 1 d . . . Ni1 Ni 0.01913(7) 1.2473(4) 0.50223(9) 0.0778(19) Uani 0.571(9) 1 d P . . Ni2 Ni 0.23106(8) 0.7407(5) 0.75373(10) 0.082(2) Uani 0.550(9) 1 d P . . O1 O 0.01359(13) 0.7857(8) 0.71402(15) 0.0561(19) Uani 1 1 d . . . O2 O 0.03616(12) 0.6265(7) 0.69306(14) 0.0483(17) Uani 1 1 d . . . O3 O 0.18534(14) 1.2133(8) 0.5044(2) 0.064(2) Uani 1 1 d . . . O4 O 0.18250(12) 1.4506(7) 0.50591(19) 0.059(2) Uani 1 1 d . . . O5 O -0.14648(14) 1.1950(10) 0.4722(3) 0.090(3) Uani 1 1 d . . . O6 O -0.14671(14) 1.2047(11) 0.5249(3) 0.092(3) Uani 1 1 d . . . O7 O 0.06750(12) 0.5542(6) 0.75206(14) 0.0432(16) Uani 1 1 d . . . O8 O 0.06449(12) 0.7891(7) 0.75247(16) 0.0459(16) Uani 1 1 d . . . O9 O 0.21432(14) 1.3659(7) 0.56436(17) 0.060(2) Uani 1 1 d . . . O10 O 0.23727(13) 1.2083(9) 0.54269(17) 0.066(2) Uani 1 1 d . . . O11 O 0.39681(15) 0.6933(9) 0.7281(3) 0.088(3) Uani 1 1 d . . . O12 O 0.39651(17) 0.6965(11) 0.7794(3) 0.102(3) Uani 1 1 d . . . O13 O 0.23631(15) 1.2065(10) 0.46649(17) 0.076(3) Uani 1 1 d . . . O14 O 0.21487(15) 1.3782(8) 0.44649(19) 0.066(2) Uani 1 1 d . . . O15 O 0.23814(16) 1.5510(10) 0.5046(2) 0.083(3) Uani 1 1 d U . . H15A H 0.2346 1.6094 0.4875 0.124 Uiso 1 1 d R . . H15B H 0.2358 1.6045 0.5227 0.124 Uiso 1 1 d R . . O16 O 0.03371(12) 0.6333(7) 0.81115(13) 0.0484(17) Uani 1 1 d . . . O17 O 0.01272(13) 0.7995(9) 0.78937(15) 0.060(2) Uani 1 1 d . . . O18 O 0.01222(16) 0.4472(9) 0.75036(16) 0.068(2) Uani 1 1 d U . . H18A H 0.0181 0.3846 0.7636 0.101 Uiso 1 1 d R . . H18B H -0.0018 0.4629 0.7559 0.101 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(7) 0.055(6) 0.036(5) -0.021(4) -0.006(5) 0.005(5) C2 0.044(6) 0.044(5) 0.036(5) -0.007(4) -0.001(4) 0.002(5) C3 0.056(7) 0.063(6) 0.034(5) 0.002(4) -0.006(4) -0.007(5) C4 0.037(7) 0.069(7) 0.081(8) 0.014(6) -0.006(6) 0.017(6) C5 0.040(6) 0.043(5) 0.063(6) 0.016(5) 0.001(5) -0.002(5) C6 0.084(10) 0.044(6) 0.053(6) 0.010(5) -0.012(6) -0.017(6) C7 0.055(8) 0.037(5) 0.068(7) 0.011(5) -0.002(5) -0.003(5) C8 0.042(7) 0.054(6) 0.070(7) 0.020(5) -0.028(5) -0.018(5) C9 0.052(7) 0.056(6) 0.046(5) 0.000(5) -0.018(5) -0.010(5) C10 0.047(7) 0.050(5) 0.034(5) 0.002(4) -0.010(4) 0.003(5) C11 0.039(6) 0.055(6) 0.041(5) -0.014(4) -0.001(4) -0.003(5) C12 0.057(7) 0.046(5) 0.023(4) -0.012(4) -0.002(4) 0.001(5) C13 0.052(7) 0.049(5) 0.030(4) -0.005(4) -0.006(4) 0.004(5) C14 0.042(6) 0.044(5) 0.046(5) -0.009(4) -0.009(4) -0.009(5) C15 0.035(6) 0.058(6) 0.044(5) -0.016(4) -0.010(4) -0.002(5) C16 0.077(9) 0.056(6) 0.021(4) -0.020(4) 0.001(4) -0.002(6) C17 0.041(6) 0.062(6) 0.037(5) -0.022(4) 0.003(4) 0.001(5) C18 0.045(6) 0.061(6) 0.032(5) -0.020(4) -0.008(4) 0.007(5) C19 0.053(7) 0.033(4) 0.030(4) 0.001(3) 0.005(4) -0.004(4) C20 0.052(7) 0.042(5) 0.020(4) -0.008(3) -0.006(4) 0.010(5) C25 0.057(9) 0.043(7) 0.148(14) 0.007(7) -0.002(8) 0.004(6) C24 0.063(8) 0.041(6) 0.073(7) 0.013(5) -0.006(6) 0.001(5) C23 0.077(5) 0.075(5) 0.091(5) 0.000(4) 0.000(4) -0.003(4) C22 0.039(8) 0.036(6) 0.200(17) -0.001(8) -0.022(9) -0.006(6) C21 0.029(6) 0.039(5) 0.086(8) 0.017(5) -0.017(5) -0.004(5) C26 0.037(7) 0.044(6) 0.149(13) 0.009(7) -0.013(7) -0.013(6) C27 0.028(6) 0.043(6) 0.086(8) 0.002(5) -0.005(5) -0.002(5) C28 0.043(6) 0.043(5) 0.033(4) -0.005(4) 0.002(4) 0.000(4) C29 0.053(6) 0.047(5) 0.028(4) -0.006(4) 0.022(4) 0.005(5) C30 0.043(6) 0.034(5) 0.044(5) -0.013(4) 0.012(4) 0.002(4) C31 0.027(5) 0.047(5) 0.035(4) -0.020(4) 0.000(4) 0.003(4) C32 0.068(8) 0.073(7) 0.030(5) -0.014(5) 0.005(5) 0.021(6) C33 0.068(8) 0.069(7) 0.030(5) -0.008(4) -0.010(5) 0.036(6) C34 0.030(6) 0.048(5) 0.036(5) -0.013(4) -0.001(4) -0.006(4) C36 0.056(8) 0.063(7) 0.044(5) -0.020(5) -0.003(5) 0.006(5) C37 0.077(10) 0.067(8) 0.063(7) -0.011(6) 0.011(6) 0.008(7) C38 0.037(7) 0.050(6) 0.073(7) 0.004(5) -0.001(5) -0.010(5) C39 0.069(9) 0.060(7) 0.061(7) 0.010(5) -0.026(6) -0.008(6) C40 0.045(7) 0.058(6) 0.044(5) 0.005(4) -0.003(5) -0.001(5) C35 0.010(5) 0.052(5) 0.058(6) -0.018(4) -0.002(4) -0.003(4) C41 0.070(11) 0.036(6) 0.143(14) 0.014(7) 0.013(10) 0.014(7) C42 0.048(7) 0.036(5) 0.047(5) -0.012(4) -0.004(4) 0.012(5) C43 0.036(6) 0.041(5) 0.070(7) -0.019(5) -0.011(5) 0.012(5) C44 0.048(7) 0.043(5) 0.074(7) -0.002(5) -0.005(5) 0.005(5) C45 0.061(8) 0.046(6) 0.092(9) 0.006(6) -0.023(7) 0.003(6) C46 0.044(7) 0.044(5) 0.076(7) -0.009(5) -0.019(6) 0.013(5) C47 0.040(7) 0.022(4) 0.084(7) 0.021(4) 0.001(5) 0.010(4) C48 0.050(7) 0.032(5) 0.094(8) 0.003(5) 0.006(6) 0.009(5) C49 0.037(7) 0.056(6) 0.094(9) 0.009(6) 0.007(6) 0.000(5) C50 0.034(7) 0.052(6) 0.094(9) 0.003(6) -0.004(6) -0.001(5) C51 0.042(6) 0.050(6) 0.057(6) -0.006(5) -0.006(5) -0.005(5) C52 0.038(6) 0.035(5) 0.053(5) -0.017(4) -0.003(4) 0.005(4) C53 0.049(7) 0.046(5) 0.053(6) -0.027(5) -0.005(5) 0.003(5) C54 0.047(7) 0.054(6) 0.053(6) -0.012(5) -0.006(5) 0.007(5) C55 0.049(7) 0.051(6) 0.071(7) -0.026(5) -0.004(6) 0.006(5) C56 0.041(6) 0.052(6) 0.055(6) -0.024(5) -0.009(5) 0.005(5) C57 0.047(7) 0.044(5) 0.037(5) -0.006(4) -0.002(4) -0.002(5) C58 0.051(7) 0.049(6) 0.054(6) -0.022(5) -0.007(5) -0.003(5) C59 0.050(7) 0.054(6) 0.047(5) -0.016(5) 0.006(5) -0.012(5) C60 0.061(8) 0.045(6) 0.064(7) -0.020(5) 0.016(6) -0.021(5) C61 0.061(8) 0.051(6) 0.055(6) -0.030(5) 0.002(5) 0.007(6) C62 0.046(7) 0.043(5) 0.051(6) -0.018(4) -0.002(5) -0.009(5) C63 0.050(7) 0.036(5) 0.062(6) -0.018(4) 0.021(5) -0.009(5) C64 0.024(6) 0.044(5) 0.064(6) 0.002(5) 0.009(4) 0.000(4) C65 0.048(7) 0.068(7) 0.046(6) -0.020(5) 0.001(5) -0.006(6) C66 0.071(9) 0.092(9) 0.046(6) -0.025(6) 0.005(5) 0.033(7) C67 0.077(9) 0.069(7) 0.051(6) -0.015(5) 0.002(6) 0.023(6) C68 0.047(7) 0.061(7) 0.045(5) -0.034(5) 0.013(5) -0.022(5) C69 0.054(8) 0.035(5) 0.071(7) 0.016(4) -0.008(5) 0.000(5) C70 0.041(7) 0.033(5) 0.101(9) 0.002(5) -0.006(6) -0.003(5) C71 0.058(8) 0.027(5) 0.106(10) 0.008(5) -0.011(6) 0.010(5) C72 0.045(7) 0.030(5) 0.056(6) 0.012(4) -0.005(4) -0.007(4) C73 0.045(8) 0.028(5) 0.164(15) 0.004(6) 0.000(7) -0.004(5) C74 0.038(7) 0.042(6) 0.170(16) 0.000(7) -0.008(7) 0.006(6) C75 0.060(8) 0.042(6) 0.055(6) 0.009(4) -0.013(5) -0.014(6) C76 0.043(7) 0.061(6) 0.049(6) -0.018(5) -0.007(5) 0.021(5) C77 0.054(7) 0.030(5) 0.073(7) -0.021(5) -0.021(5) 0.009(5) C78 0.057(8) 0.051(6) 0.048(6) -0.005(5) -0.018(5) 0.013(5) C79 0.040(6) 0.046(5) 0.050(5) -0.016(4) -0.006(4) 0.006(5) C80 0.062(8) 0.084(9) 0.057(7) -0.023(6) -0.008(6) -0.014(7) C81 0.071(8) 0.075(7) 0.038(5) -0.020(5) 0.002(5) -0.030(6) C82 0.051(7) 0.057(6) 0.036(5) -0.004(4) 0.000(4) 0.004(5) C83 0.059(8) 0.078(8) 0.035(5) 0.001(5) 0.003(5) -0.015(6) C84 0.058(8) 0.081(8) 0.051(6) 0.015(6) -0.014(5) -0.016(6) C85 0.051(7) 0.034(5) 0.073(7) 0.015(5) 0.007(5) 0.000(5) C86 0.063(9) 0.062(7) 0.067(7) -0.021(6) 0.010(6) 0.016(6) C87 0.058(8) 0.083(8) 0.051(6) -0.026(6) -0.002(5) -0.002(7) C88 0.065(4) 0.063(4) 0.073(4) 0.002(3) 0.000(3) 0.002(3) C89 0.043(7) 0.111(10) 0.036(5) 0.013(6) -0.009(5) -0.036(7) C90 0.040(6) 0.043(6) 0.038(5) 0.013(4) 0.003(4) -0.005(4) C91 0.046(6) 0.053(6) 0.026(4) -0.009(4) -0.010(4) 0.010(5) C92 0.068(8) 0.078(7) 0.030(5) -0.019(5) 0.003(5) -0.033(6) C93 0.052(7) 0.082(8) 0.027(5) -0.020(5) -0.016(4) -0.010(6) C94 0.052(7) 0.057(6) 0.022(4) -0.015(4) -0.011(4) 0.009(5) C95 0.049(7) 0.034(5) 0.039(5) -0.014(4) -0.007(4) 0.021(4) C96 0.051(6) 0.045(5) 0.022(4) -0.007(3) -0.021(4) 0.012(5) Cd1 0.0454(5) 0.0454(4) 0.0812(6) 0.0046(4) -0.0006(4) 0.0016(4) Cd2 0.0468(5) 0.0427(4) 0.0466(4) 0.0025(3) -0.0039(3) 0.0017(3) N1 0.041(5) 0.054(4) 0.018(3) -0.010(3) -0.007(3) 0.001(4) N2 0.038(5) 0.048(4) 0.038(4) 0.003(3) -0.012(3) -0.009(4) N3 0.041(5) 0.051(4) 0.033(4) 0.002(3) -0.003(3) 0.003(4) N4 0.046(5) 0.053(4) 0.024(3) -0.010(3) 0.002(3) 0.000(4) N5 0.053(6) 0.037(4) 0.057(5) 0.001(4) -0.009(4) 0.003(4) N6 0.029(5) 0.033(4) 0.075(6) -0.007(4) -0.006(4) 0.001(3) N7 0.038(5) 0.045(4) 0.063(5) -0.014(4) 0.005(4) -0.002(4) N8 0.054(6) 0.045(5) 0.064(5) -0.021(4) -0.014(4) 0.012(4) Ni1 0.056(3) 0.094(3) 0.083(3) 0.017(2) -0.0032(19) 0.003(2) Ni2 0.070(4) 0.094(4) 0.082(3) 0.017(2) -0.001(2) 0.003(2) O1 0.065(5) 0.068(4) 0.036(3) -0.011(3) -0.005(3) 0.014(4) O2 0.063(5) 0.042(4) 0.040(3) 0.002(3) 0.008(3) 0.006(3) O3 0.053(5) 0.043(4) 0.097(6) 0.013(4) 0.006(4) 0.015(4) O4 0.039(4) 0.039(4) 0.098(6) -0.001(3) -0.009(4) 0.000(3) O5 0.038(5) 0.076(6) 0.156(10) 0.008(6) -0.016(6) -0.004(5) O6 0.030(5) 0.095(7) 0.150(10) -0.009(7) 0.013(6) -0.025(5) O7 0.047(4) 0.037(3) 0.046(4) 0.006(3) -0.004(3) -0.012(3) O8 0.032(4) 0.033(3) 0.073(5) 0.006(3) 0.001(3) 0.004(3) O9 0.079(6) 0.041(4) 0.059(4) -0.012(3) 0.013(4) -0.006(4) O10 0.061(5) 0.084(5) 0.052(4) 0.001(4) 0.004(4) 0.020(5) O11 0.069(6) 0.057(5) 0.139(9) -0.024(5) 0.030(6) -0.020(5) O12 0.078(7) 0.075(6) 0.151(10) 0.015(6) -0.036(7) -0.012(5) O13 0.081(6) 0.109(6) 0.037(4) 0.022(4) -0.015(4) 0.024(5) O14 0.074(6) 0.055(5) 0.070(5) 0.010(4) -0.012(4) 0.011(4) O15 0.091(4) 0.083(4) 0.073(4) 0.003(3) 0.005(3) -0.026(3) O16 0.067(5) 0.050(4) 0.028(3) 0.007(3) -0.016(3) -0.012(4) O17 0.062(5) 0.085(5) 0.033(3) 0.010(3) -0.008(3) 0.005(4) O18 0.077(4) 0.078(4) 0.048(3) 0.001(3) -0.003(3) -0.025(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.386(14) . ? C1 C20 1.387(14) . ? C1 C91 1.515(14) . ? C2 C3 1.469(14) . ? C2 N3 1.394(12) . ? C3 H3 0.9500 . ? C3 C4 1.355(14) . ? C4 H4 0.9500 . ? C4 C5 1.459(15) . ? C5 C6 1.395(15) . ? C5 N3 1.357(12) . ? C6 C7 1.465(15) . ? C6 C21 1.457(15) . ? C7 C8 1.498(14) . ? C7 N2 1.344(13) . ? C8 H8 0.9500 . ? C8 C9 1.333(15) . ? C9 H9 0.9500 . ? C9 C10 1.475(13) . ? C10 C11 1.383(14) . ? C10 N2 1.396(12) . ? C11 C12 1.417(14) . ? C11 C28 1.500(13) . ? C12 C13 1.409(14) . ? C12 N1 1.372(12) . ? C13 H13 0.9500 . ? C13 C14 1.330(13) . ? C14 H14 0.9500 . ? C14 C15 1.443(14) . ? C15 C16 1.422(15) . ? C15 N1 1.368(12) . ? C16 C17 1.434(15) . ? C16 C35 1.485(13) . ? C17 C18 1.473(14) . ? C17 N4 1.384(12) . ? C18 H18 0.9500 . ? C18 C19 1.342(13) . ? C19 H19 0.9500 . ? C19 C20 1.386(13) . ? C20 N4 1.371(12) . ? C25 H25 0.9500 . ? C25 C24 1.3900 . ? C25 C26 1.3900 . ? C24 C23 1.3900 . ? C24 C27 1.509(12) . ? C23 H23 0.9500 . ? C23 C22 1.3900 . ? C22 H22 0.9500 . ? C22 C21 1.3900 . ? C21 C26 1.3900 . ? C26 H26 0.9500 . ? C27 Cd1 2.675(11) . ? C27 O3 1.256(13) . ? C27 O4 1.271(12) . ? C28 C29 1.385(13) . ? C28 C33 1.406(13) . ? C29 H29 0.9500 . ? C29 C30 1.373(13) . ? C30 H30 0.9500 . ? C30 C31 1.379(12) . ? C31 C32 1.349(14) . ? C31 C34 1.509(13) . ? C32 H32 0.9500 . ? C32 C33 1.364(14) . ? C33 H33 0.9500 . ? C34 Cd2 2.735(9) . ? C34 O1 1.280(11) . ? C34 O2 1.225(11) . ? C36 H36 0.9500 . ? C36 C37 1.3900 . ? C36 C35 1.3900 . ? C37 H37 0.9500 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C38 C41 1.471(17) . ? C39 H39 0.9500 . ? C39 C40 1.3900 . ? C40 H40 0.9500 . ? C40 C35 1.3900 . ? C41 O5 1.289(19) . ? C41 O6 1.240(18) . ? C42 C43 1.441(15) . ? C42 C61 1.394(15) . ? C42 C62 1.468(14) . ? C43 C44 1.453(14) . ? C43 N5 1.353(14) . ? C44 H44 0.9500 . ? C44 C45 1.365(17) . ? C45 H45 0.9500 . ? C45 C46 1.447(16) . ? C46 C47 1.399(16) . ? C46 N5 1.392(14) . ? C47 C48 1.379(15) . ? C47 C69 1.527(12) . ? C48 C49 1.459(16) . ? C48 N6 1.367(13) . ? C49 H49 0.9500 . ? C49 C50 1.380(16) . ? C50 H50 0.9500 . ? C50 C51 1.450(15) . ? C51 C52 1.405(14) . ? C51 N6 1.349(13) . ? C52 C53 1.400(14) . ? C52 C76 1.470(15) . ? C53 C54 1.447(15) . ? C53 N7 1.404(14) . ? C54 H54 0.9500 . ? C54 C55 1.375(16) . ? C55 H55 0.9500 . ? C55 C56 1.461(15) . ? C56 C57 1.394(15) . ? C56 N7 1.391(13) . ? C57 C58 1.401(15) . ? C57 C82 1.469(16) . ? C58 C59 1.440(15) . ? C58 N8 1.394(13) . ? C59 H59 0.9500 . ? C59 C60 1.393(16) . ? C60 H60 0.9500 . ? C60 C61 1.466(15) . ? C61 N8 1.382(14) . ? C62 C63 1.398(14) . ? C62 C67 1.399(14) . ? C63 H63 0.9500 . ? C63 C64 1.356(14) . ? C64 H64 0.9500 . ? C64 C65 1.384(14) . ? C65 C66 1.406(16) . ? C65 C68 1.461(16) . ? C66 H66 0.9500 . ? C66 C67 1.379(16) . ? C67 H67 0.9500 . ? C68 O9 1.252(13) . ? C68 O10 1.293(12) . ? C69 C70 1.3900 . ? C69 C74 1.3900 . ? C70 H70 0.9500 . ? C70 C71 1.3900 . ? C71 H71 0.9500 . ? C71 C72 1.3900 . ? C72 C73 1.3900 . ? C72 C75 1.487(13) . ? C73 H73 0.9500 . ? C73 C74 1.3900 . ? C74 H74 0.9500 . ? C75 Cd2 2.713(12) . ? C75 O7 1.301(12) . ? C75 O8 1.251(13) . ? C76 C77 1.419(15) . ? C76 C81 1.397(14) . ? C77 H77 0.9500 . ? C77 C78 1.387(15) . ? C78 H78 0.9500 . ? C78 C79 1.388(13) . ? C79 C80 1.344(16) . ? C79 C89 1.461(16) 7_576 ? C80 H80 0.9500 . ? C80 C81 1.409(16) . ? C81 H81 0.9500 . ? C82 C83 1.428(14) . ? C82 C87 1.418(14) . ? C83 H83 0.9500 . ? C83 C84 1.390(16) . ? C84 H84 0.9500 . ? C84 C85 1.415(16) . ? C85 C86 1.409(16) . ? C85 C88 1.470(18) . ? C86 H86 0.9500 . ? C86 C87 1.396(16) . ? C87 H87 0.9500 . ? C88 O11 1.213(15) . ? C88 O12 1.231(16) . ? C89 C79 1.461(16) 7_575 ? C89 Cd1 2.753(11) . ? C89 O13 1.271(13) . ? C89 O14 1.267(16) . ? C90 C94 1.544(13) 7_586 ? C90 Cd2 2.705(9) . ? C90 O16 1.218(11) . ? C90 O17 1.274(11) . ? C91 C92 1.411(12) . ? C91 C96 1.361(14) . ? C92 H92 0.9500 . ? C92 C93 1.364(15) . ? C93 H93 0.9500 . ? C93 C94 1.344(15) . ? C94 C90 1.544(13) 7_585 ? C94 C95 1.435(12) . ? C95 H95 0.9500 . ? C95 C96 1.369(13) . ? C96 H96 0.9500 . ? Cd1 O3 2.351(9) . ? Cd1 O4 2.360(7) . ? Cd1 O9 2.494(7) . ? Cd1 O10 2.318(8) . ? Cd1 O13 2.333(9) . ? Cd1 O14 2.478(8) . ? Cd1 O15 2.222(9) . ? Cd2 O1 2.285(7) . ? Cd2 O2 2.517(6) . ? Cd2 O7 2.346(7) . ? Cd2 O8 2.345(7) . ? Cd2 O16 2.459(6) . ? Cd2 O17 2.331(8) . ? Cd2 O18 2.242(8) . ? N1 Ni1 2.019(9) . ? N2 Ni1 1.998(8) . ? N3 Ni1 2.013(9) . ? N4 Ni1 2.048(9) . ? N5 Ni2 2.010(9) . ? N6 Ni2 2.030(10) . ? N7 Ni2 2.017(10) . ? N8 Ni2 1.990(11) . ? O15 H15A 0.9236 . ? O15 H15B 0.9195 . ? O18 H18A 0.8790 . ? O18 H18B 0.8788 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C20 126.4(10) . . ? C2 C1 C91 116.2(9) . . ? C20 C1 C91 117.2(9) . . ? C1 C2 C3 127.7(9) . . ? C1 C2 N3 124.7(9) . . ? N3 C2 C3 107.5(8) . . ? C2 C3 H3 126.0 . . ? C4 C3 C2 108.1(9) . . ? C4 C3 H3 126.0 . . ? C3 C4 H4 126.8 . . ? C3 C4 C5 106.4(10) . . ? C5 C4 H4 126.8 . . ? C6 C5 C4 120.8(10) . . ? N3 C5 C4 110.1(9) . . ? N3 C5 C6 129.1(10) . . ? C5 C6 C7 117.3(11) . . ? C5 C6 C21 122.3(10) . . ? C21 C6 C7 120.3(9) . . ? C6 C7 C8 120.4(10) . . ? N2 C7 C6 128.9(10) . . ? N2 C7 C8 110.7(9) . . ? C7 C8 H8 127.6 . . ? C9 C8 C7 104.9(9) . . ? C9 C8 H8 127.6 . . ? C8 C9 H9 125.3 . . ? C8 C9 C10 109.4(9) . . ? C10 C9 H9 125.3 . . ? C11 C10 C9 127.0(9) . . ? C11 C10 N2 125.4(9) . . ? N2 C10 C9 107.5(9) . . ? C10 C11 C12 124.3(9) . . ? C10 C11 C28 117.1(8) . . ? C12 C11 C28 118.4(9) . . ? C13 C12 C11 126.5(9) . . ? N1 C12 C11 124.1(9) . . ? N1 C12 C13 109.3(8) . . ? C12 C13 H13 124.9 . . ? C14 C13 C12 110.2(9) . . ? C14 C13 H13 124.9 . . ? C13 C14 H14 128.0 . . ? C13 C14 C15 104.1(9) . . ? C15 C14 H14 128.0 . . ? C16 C15 C14 121.6(9) . . ? N1 C15 C14 111.6(8) . . ? N1 C15 C16 126.5(10) . . ? C15 C16 C17 119.7(11) . . ? C15 C16 C35 121.7(9) . . ? C17 C16 C35 118.6(9) . . ? C16 C17 C18 124.3(10) . . ? N4 C17 C16 128.0(10) . . ? N4 C17 C18 107.2(9) . . ? C17 C18 H18 127.2 . . ? C19 C18 C17 105.6(9) . . ? C19 C18 H18 127.2 . . ? C18 C19 H19 124.8 . . ? C18 C19 C20 110.4(8) . . ? C20 C19 H19 124.8 . . ? C19 C20 C1 127.6(9) . . ? N4 C20 C1 123.4(9) . . ? N4 C20 C19 109.0(8) . . ? C24 C25 H25 120.0 . . ? C24 C25 C26 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 C27 118.9(6) . . ? C23 C24 C27 121.1(6) . . ? C24 C23 H23 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C22 H22 120.0 . . ? C23 C22 C21 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C21 C6 117.6(6) . . ? C26 C21 C6 122.4(6) . . ? C26 C21 C22 120.0 . . ? C25 C26 H26 120.0 . . ? C21 C26 C25 120.0 . . ? C21 C26 H26 120.0 . . ? C24 C27 Cd1 179.7(8) . . ? O3 C27 C24 118.3(9) . . ? O3 C27 Cd1 61.5(6) . . ? O3 C27 O4 123.4(10) . . ? O4 C27 C24 118.2(9) . . ? O4 C27 Cd1 61.9(5) . . ? C29 C28 C11 122.0(8) . . ? C29 C28 C33 117.5(8) . . ? C33 C28 C11 120.4(9) . . ? C28 C29 H29 119.3 . . ? C30 C29 C28 121.4(8) . . ? C30 C29 H29 119.3 . . ? C29 C30 H30 119.7 . . ? C29 C30 C31 120.7(9) . . ? C31 C30 H30 119.7 . . ? C30 C31 C34 120.0(8) . . ? C32 C31 C30 117.5(9) . . ? C32 C31 C34 122.5(8) . . ? C31 C32 H32 118.0 . . ? C31 C32 C33 124.0(9) . . ? C33 C32 H32 118.0 . . ? C28 C33 H33 120.6 . . ? C32 C33 C28 118.8(9) . . ? C32 C33 H33 120.6 . . ? C31 C34 Cd2 168.0(6) . . ? O1 C34 C31 117.6(8) . . ? O1 C34 Cd2 56.2(5) . . ? O2 C34 C31 120.8(8) . . ? O2 C34 Cd2 66.7(5) . . ? O2 C34 O1 121.7(9) . . ? C37 C36 H36 120.0 . . ? C37 C36 C35 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 H37 120.0 . . ? C36 C37 C38 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C41 120.2(9) . . ? C39 C38 C37 120.0 . . ? C39 C38 C41 119.8(9) . . ? C38 C39 H39 120.0 . . ? C40 C39 C38 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 H40 120.0 . . ? C39 C40 C35 120.0 . . ? C35 C40 H40 120.0 . . ? C36 C35 C16 120.3(5) . . ? C40 C35 C16 119.7(5) . . ? C40 C35 C36 120.0 . . ? O5 C41 C38 119.4(14) . . ? O6 C41 C38 119.4(15) . . ? O6 C41 O5 121.1(16) . . ? C43 C42 C62 115.3(9) . . ? C61 C42 C43 123.2(10) . . ? C61 C42 C62 121.3(10) . . ? C42 C43 C44 124.2(10) . . ? N5 C43 C42 123.7(9) . . ? N5 C43 C44 112.0(10) . . ? C43 C44 H44 127.5 . . ? C45 C44 C43 105.0(11) . . ? C45 C44 H44 127.5 . . ? C44 C45 H45 126.1 . . ? C44 C45 C46 107.9(11) . . ? C46 C45 H45 126.1 . . ? C47 C46 C45 126.9(11) . . ? N5 C46 C45 109.3(11) . . ? N5 C46 C47 123.8(9) . . ? C46 C47 C69 117.1(9) . . ? C48 C47 C46 125.9(11) . . ? C48 C47 C69 116.9(9) . . ? C47 C48 C49 124.7(11) . . ? N6 C48 C47 125.9(11) . . ? N6 C48 C49 109.4(10) . . ? C48 C49 H49 126.7 . . ? C50 C49 C48 106.6(10) . . ? C50 C49 H49 126.7 . . ? C49 C50 H50 127.2 . . ? C49 C50 C51 105.5(11) . . ? C51 C50 H50 127.2 . . ? C52 C51 C50 123.3(10) . . ? N6 C51 C50 111.1(9) . . ? N6 C51 C52 125.5(10) . . ? C51 C52 C76 119.7(9) . . ? C53 C52 C51 124.0(10) . . ? C53 C52 C76 116.3(9) . . ? C52 C53 C54 124.6(10) . . ? C52 C53 N7 123.8(10) . . ? N7 C53 C54 111.6(10) . . ? C53 C54 H54 127.5 . . ? C55 C54 C53 105.1(10) . . ? C55 C54 H54 127.5 . . ? C54 C55 H55 125.5 . . ? C54 C55 C56 108.9(10) . . ? C56 C55 H55 125.5 . . ? C57 C56 C55 125.3(10) . . ? N7 C56 C55 108.8(10) . . ? N7 C56 C57 125.6(10) . . ? C56 C57 C58 122.4(10) . . ? C56 C57 C82 118.2(9) . . ? C58 C57 C82 119.4(9) . . ? C57 C58 C59 124.3(10) . . ? N8 C58 C57 125.3(10) . . ? N8 C58 C59 110.2(10) . . ? C58 C59 H59 126.3 . . ? C60 C59 C58 107.5(10) . . ? C60 C59 H59 126.3 . . ? C59 C60 H60 127.2 . . ? C59 C60 C61 105.5(10) . . ? C61 C60 H60 127.2 . . ? C42 C61 C60 123.3(11) . . ? N8 C61 C42 126.2(11) . . ? N8 C61 C60 110.5(10) . . ? C63 C62 C42 122.7(9) . . ? C63 C62 C67 116.6(10) . . ? C67 C62 C42 120.6(10) . . ? C62 C63 H63 119.3 . . ? C64 C63 C62 121.4(9) . . ? C64 C63 H63 119.3 . . ? C63 C64 H64 118.5 . . ? C63 C64 C65 123.0(10) . . ? C65 C64 H64 118.5 . . ? C64 C65 C66 116.2(10) . . ? C64 C65 C68 123.0(10) . . ? C66 C65 C68 120.9(9) . . ? C65 C66 H66 119.4 . . ? C67 C66 C65 121.2(10) . . ? C67 C66 H66 119.4 . . ? C62 C67 H67 119.3 . . ? C66 C67 C62 121.4(11) . . ? C66 C67 H67 119.3 . . ? O9 C68 C65 120.4(9) . . ? O9 C68 O10 119.9(10) . . ? O10 C68 C65 119.7(11) . . ? C70 C69 C47 119.8(5) . . ? C70 C69 C74 120.0 . . ? C74 C69 C47 120.2(5) . . ? C69 C70 H70 120.0 . . ? C69 C70 C71 120.0 . . ? C71 C70 H70 120.0 . . ? C70 C71 H71 120.0 . . ? C72 C71 C70 120.0 . . ? C72 C71 H71 120.0 . . ? C71 C72 C73 120.0 . . ? C71 C72 C75 119.5(6) . . ? C73 C72 C75 120.5(6) . . ? C72 C73 H73 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73 120.0 . . ? C69 C74 H74 120.0 . . ? C73 C74 C69 120.0 . . ? C73 C74 H74 120.0 . . ? C72 C75 Cd2 178.0(7) . . ? O7 C75 C72 118.9(9) . . ? O7 C75 Cd2 59.8(6) . . ? O8 C75 C72 121.6(8) . . ? O8 C75 Cd2 59.7(6) . . ? O8 C75 O7 119.5(10) . . ? C77 C76 C52 121.9(9) . . ? C81 C76 C52 122.7(10) . . ? C81 C76 C77 115.2(10) . . ? C76 C77 H77 119.2 . . ? C78 C77 C76 121.7(9) . . ? C78 C77 H77 119.2 . . ? C77 C78 H78 119.0 . . ? C77 C78 C79 121.9(11) . . ? C79 C78 H78 119.0 . . ? C78 C79 C89 121.1(11) . 7_576 ? C80 C79 C78 116.8(10) . . ? C80 C79 C89 122.1(10) . 7_576 ? C79 C80 H80 118.4 . . ? C79 C80 C81 123.3(10) . . ? C81 C80 H80 118.4 . . ? C76 C81 C80 120.9(11) . . ? C76 C81 H81 119.5 . . ? C80 C81 H81 119.5 . . ? C83 C82 C57 120.9(9) . . ? C87 C82 C57 121.8(9) . . ? C87 C82 C83 117.3(11) . . ? C82 C83 H83 119.4 . . ? C84 C83 C82 121.2(10) . . ? C84 C83 H83 119.4 . . ? C83 C84 H84 119.4 . . ? C83 C84 C85 121.2(10) . . ? C85 C84 H84 119.4 . . ? C84 C85 C88 122.7(11) . . ? C86 C85 C84 117.6(11) . . ? C86 C85 C88 119.5(11) . . ? C85 C86 H86 119.1 . . ? C87 C86 C85 121.8(10) . . ? C87 C86 H86 119.1 . . ? C82 C87 H87 119.6 . . ? C86 C87 C82 120.8(10) . . ? C86 C87 H87 119.6 . . ? O11 C88 C85 121.0(13) . . ? O11 C88 O12 122.6(15) . . ? O12 C88 C85 116.4(12) . . ? C79 C89 Cd1 167.4(8) 7_575 . ? O13 C89 C79 116.9(13) . 7_575 ? O13 C89 Cd1 57.6(6) . . ? O14 C89 C79 121.3(10) . 7_575 ? O14 C89 Cd1 64.2(6) . . ? O14 C89 O13 121.5(11) . . ? C94 C90 Cd2 170.8(6) 7_586 . ? O16 C90 C94 120.3(8) . 7_586 ? O16 C90 Cd2 65.3(5) . . ? O16 C90 O17 123.0(9) . . ? O17 C90 C94 116.4(9) . 7_586 ? O17 C90 Cd2 59.4(5) . . ? C92 C91 C1 120.0(9) . . ? C96 C91 C1 121.4(8) . . ? C96 C91 C92 118.4(9) . . ? C91 C92 H92 120.3 . . ? C93 C92 C91 119.4(10) . . ? C93 C92 H92 120.3 . . ? C92 C93 H93 118.8 . . ? C94 C93 C92 122.4(8) . . ? C94 C93 H93 118.8 . . ? C93 C94 C90 122.7(8) . 7_585 ? C93 C94 C95 119.2(9) . . ? C95 C94 C90 118.1(9) . 7_585 ? C94 C95 H95 121.2 . . ? C96 C95 C94 117.7(9) . . ? C96 C95 H95 121.2 . . ? C91 C96 C95 122.9(8) . . ? C91 C96 H96 118.6 . . ? C95 C96 H96 118.6 . . ? C27 Cd1 C89 99.2(3) . . ? O3 Cd1 C27 28.0(3) . . ? O3 Cd1 C89 89.6(3) . . ? O3 Cd1 O4 56.4(2) . . ? O3 Cd1 O9 87.7(3) . . ? O3 Cd1 O14 88.2(3) . . ? O4 Cd1 C27 28.4(3) . . ? O4 Cd1 C89 106.6(3) . . ? O4 Cd1 O9 82.1(3) . . ? O4 Cd1 O14 83.2(3) . . ? O9 Cd1 C27 84.0(3) . . ? O9 Cd1 C89 167.3(4) . . ? O10 Cd1 C27 115.3(3) . . ? O10 Cd1 C89 113.8(3) . . ? O10 Cd1 O3 96.2(3) . . ? O10 Cd1 O4 130.8(3) . . ? O10 Cd1 O9 54.3(3) . . ? O10 Cd1 O13 86.4(3) . . ? O10 Cd1 O14 141.1(3) . . ? O13 Cd1 C27 113.9(3) . . ? O13 Cd1 C89 27.4(3) . . ? O13 Cd1 O3 93.7(3) . . ? O13 Cd1 O4 130.4(3) . . ? O13 Cd1 O9 140.6(3) . . ? O13 Cd1 O14 54.7(3) . . ? O14 Cd1 C27 85.4(3) . . ? O14 Cd1 C89 27.4(3) . . ? O14 Cd1 O9 164.5(3) . . ? O15 Cd1 C27 125.6(3) . . ? O15 Cd1 C89 97.5(3) . . ? O15 Cd1 O3 153.5(3) . . ? O15 Cd1 O4 97.2(3) . . ? O15 Cd1 O9 90.4(3) . . ? O15 Cd1 O10 104.1(3) . . ? O15 Cd1 O13 104.2(3) . . ? O15 Cd1 O14 86.6(3) . . ? C75 Cd2 C34 96.4(3) . . ? C90 Cd2 C34 140.7(3) . . ? C90 Cd2 C75 98.7(3) . . ? O1 Cd2 C34 27.7(3) . . ? O1 Cd2 C75 113.8(3) . . ? O1 Cd2 C90 114.0(3) . . ? O1 Cd2 O2 53.9(2) . . ? O1 Cd2 O7 129.0(2) . . ? O1 Cd2 O8 95.4(3) . . ? O1 Cd2 O16 140.5(2) . . ? O1 Cd2 O17 86.1(2) . . ? O2 Cd2 C34 26.6(2) . . ? O2 Cd2 C75 83.5(3) . . ? O2 Cd2 C90 166.8(2) . . ? O7 Cd2 C34 103.5(2) . . ? O7 Cd2 C75 28.6(3) . . ? O7 Cd2 C90 107.1(3) . . ? O7 Cd2 O2 81.0(2) . . ? O7 Cd2 O16 85.7(2) . . ? O8 Cd2 C34 88.3(3) . . ? O8 Cd2 C75 27.4(3) . . ? O8 Cd2 C90 88.8(3) . . ? O8 Cd2 O2 87.5(2) . . ? O8 Cd2 O7 56.0(2) . . ? O8 Cd2 O16 89.7(2) . . ? O16 Cd2 C34 167.4(3) . . ? O16 Cd2 C75 87.5(3) . . ? O16 Cd2 C90 26.8(2) . . ? O16 Cd2 O2 165.6(2) . . ? O17 Cd2 C34 113.4(3) . . ? O17 Cd2 C75 115.0(3) . . ? O17 Cd2 C90 28.1(3) . . ? O17 Cd2 O2 140.0(2) . . ? O17 Cd2 O7 132.3(2) . . ? O17 Cd2 O8 94.8(3) . . ? O17 Cd2 O16 54.4(2) . . ? O18 Cd2 C34 97.2(3) . . ? O18 Cd2 C75 125.5(3) . . ? O18 Cd2 C90 102.9(3) . . ? O18 Cd2 O1 101.7(3) . . ? O18 Cd2 O2 86.0(2) . . ? O18 Cd2 O7 96.9(3) . . ? O18 Cd2 O8 152.9(3) . . ? O18 Cd2 O16 90.2(2) . . ? O18 Cd2 O17 107.0(3) . . ? C12 N1 Ni1 126.6(7) . . ? C15 N1 C12 104.7(8) . . ? C15 N1 Ni1 127.2(6) . . ? C7 N2 C10 107.4(8) . . ? C7 N2 Ni1 125.4(7) . . ? C10 N2 Ni1 125.7(7) . . ? C2 N3 Ni1 125.4(7) . . ? C5 N3 C2 107.7(8) . . ? C5 N3 Ni1 125.8(6) . . ? C17 N4 Ni1 124.2(6) . . ? C20 N4 C17 107.7(8) . . ? C20 N4 Ni1 127.0(7) . . ? C43 N5 C46 105.6(9) . . ? C43 N5 Ni2 127.4(8) . . ? C46 N5 Ni2 125.6(7) . . ? C48 N6 Ni2 124.6(7) . . ? C51 N6 C48 107.2(9) . . ? C51 N6 Ni2 126.9(7) . . ? C53 N7 Ni2 127.1(7) . . ? C56 N7 C53 105.5(9) . . ? C56 N7 Ni2 126.3(7) . . ? C58 N8 Ni2 127.3(8) . . ? C61 N8 C58 106.2(10) . . ? C61 N8 Ni2 125.8(8) . . ? N1 Ni1 N4 89.7(4) . . ? N2 Ni1 N1 90.4(3) . . ? N2 Ni1 N3 90.2(4) . . ? N2 Ni1 N4 176.2(4) . . ? N3 Ni1 N1 178.0(4) . . ? N3 Ni1 N4 89.7(3) . . ? N5 Ni2 N6 91.2(4) . . ? N5 Ni2 N7 175.2(4) . . ? N7 Ni2 N6 89.0(4) . . ? N8 Ni2 N5 90.6(4) . . ? N8 Ni2 N6 177.6(4) . . ? N8 Ni2 N7 89.3(4) . . ? C34 O1 Cd2 96.1(6) . . ? C34 O2 Cd2 86.7(5) . . ? C27 O3 Cd1 90.5(7) . . ? C27 O4 Cd1 89.7(6) . . ? C75 O7 Cd2 91.6(6) . . ? C75 O8 Cd2 92.9(6) . . ? C68 O9 Cd1 88.8(6) . . ? C68 O10 Cd1 95.9(7) . . ? C89 O13 Cd1 95.0(8) . . ? C89 O14 Cd1 88.4(6) . . ? Cd1 O15 H15A 113.3 . . ? Cd1 O15 H15B 112.2 . . ? H15A O15 H15B 106.4 . . ? C90 O16 Cd2 87.9(5) . . ? C90 O17 Cd2 92.5(6) . . ? Cd2 O18 H18A 110.3 . . ? Cd2 O18 H18B 108.9 . . ? H18A O18 H18B 109.0 . . ? # Attachment '- Structure1_Pd New.cif' data_structure1_pdnew _database_code_depnum_ccdc_archive 'CCDC 865040' #TrackingRef '- Structure1_Pd New.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H52 Cd2 N8 Ni1.12 O18, 3(C5 H11 N1 O1), (H2 O1), (C5, H11, N1)' _chemical_formula_sum 'C114 H106.50 Cd2 N12 O26 Pd2' _chemical_formula_weight 2498.21 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' Cd Cd -0.8075 1.2024 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.329(7) _cell_length_b 9.543(4) _cell_length_c 35.954(12) _cell_angle_alpha 90.00 _cell_angle_beta 109.701(18) _cell_angle_gamma 90.00 _cell_volume 5921(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9850 _cell_measurement_theta_min 50.7 _cell_measurement_theta_max 2.36 _exptl_crystal_description 'irregular blocks' _exptl_crystal_colour purple-red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2541 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8741 _exptl_absorpt_correction_T_max 0.9508 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 85816 _diffrn_reflns_av_R_equivalents 0.0668 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.35 _reflns_number_total 10830 _reflns_number_gt 8156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _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 ? _computing_publication_material ? _refine_special_details ; 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 0.527 -0.004 0.013 2575 818 '10[HCON(C2H5)2]4(C2H5)2NH 4H2 ' _platon_squeeze_details 'SQUEEZE was performed using PLATON to account for disordered solvent molecules and counter cations. The electron density found in each cavity correlates to a final count of 3 molecules of HCON(C2H5)2, 2 H2Os, and 1 (C2H5)2NH+' 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^)+(0.1492P)^2^+10.5986P] 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 10830 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2300 _refine_ls_wR_factor_gt 0.2202 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _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 0.8243(3) 0.5445(6) 0.95019(16) 0.0422(12) Uani 1 1 d . . . C2 C 0.8049(3) 0.6048(7) 0.98075(17) 0.0447(13) Uani 1 1 d . . . C3 C 0.7276(3) 0.5999(7) 0.9841(2) 0.0553(16) Uani 1 1 d . . . H3 H 0.6823 0.5603 0.9657 0.066 Uiso 1 1 calc R . . C4 C 0.7335(4) 0.6623(8) 1.0182(2) 0.0646(19) Uani 1 1 d . . . H4 H 0.6927 0.6740 1.0287 0.078 Uiso 1 1 calc R . . C5 C 0.8121(4) 0.7087(8) 1.0363(2) 0.0571(17) Uani 1 1 d . . . C6 C 0.8428(4) 0.7750(7) 1.0741(2) 0.0572(17) Uani 1 1 d . . . C7 C 0.9176(4) 0.8245(7) 1.0899(2) 0.0629(19) Uani 1 1 d . . . C8 C 0.9521(5) 0.8754(9) 1.1279(2) 0.072(2) Uani 1 1 d . . . H8 H 0.9291 0.8762 1.1480 0.087 Uiso 1 1 calc R . . C9 C 1.0234(4) 0.9236(8) 1.1320(2) 0.0613(18) Uani 1 1 d . . . H9 H 1.0603 0.9614 1.1551 0.074 Uiso 1 1 calc R . . C10 C 1.0321(4) 0.9060(7) 1.09368(19) 0.0503(14) Uani 1 1 d . . . C11 C 1.0961(3) 0.9545(7) 1.08403(17) 0.0459(13) Uani 1 1 d . . . C12 C 1.1065(3) 0.9260(6) 1.04818(16) 0.0432(13) Uani 1 1 d . . . C13 C 1.1649(3) 0.9894(7) 1.03498(19) 0.0547(16) Uani 1 1 d . . . H13 H 1.2008 1.0598 1.0483 0.066 Uiso 1 1 calc R . . C14 C 1.1588(3) 0.9291(8) 0.99985(17) 0.0520(15) Uani 1 1 d . . . H14 H 1.1905 0.9495 0.9843 0.062 Uiso 1 1 calc R . . C15 C 1.0957(3) 0.8283(7) 0.99002(19) 0.0474(15) Uani 1 1 d . . . C16 C 1.0754(3) 0.7336(6) 0.95874(16) 0.0429(13) Uani 1 1 d . . . C17 C 1.0097(3) 0.6483(7) 0.94895(16) 0.0466(14) Uani 1 1 d . . . C18 C 0.9916(4) 0.5406(8) 0.91873(17) 0.0549(16) Uani 1 1 d . . . H18 H 1.0230 0.5119 0.9038 0.066 Uiso 1 1 calc R . . C19 C 0.9213(3) 0.4891(7) 0.91603(17) 0.0503(15) Uani 1 1 d . . . H19 H 0.8935 0.4182 0.8984 0.060 Uiso 1 1 calc R . . C20 C 0.8961(3) 0.5616(7) 0.94488(16) 0.0456(13) Uani 1 1 d . . . C100 C 0.7633(3) 0.4631(6) 0.92005(15) 0.0413(12) Uani 1 1 d . . . C101 C 0.7327(4) 0.5100(8) 0.8812(2) 0.072(2) Uani 1 1 d . . . H101 H 0.7543 0.5911 0.8736 0.087 Uiso 1 1 calc R . . C102 C 0.6728(4) 0.4431(8) 0.85364(17) 0.0619(19) Uani 1 1 d . . . H102 H 0.6530 0.4786 0.8275 0.074 Uiso 1 1 calc R . . C103 C 0.6405(3) 0.3229(6) 0.86372(15) 0.0396(12) Uani 1 1 d . . . C104 C 0.6714(4) 0.2742(6) 0.90152(17) 0.0449(13) Uani 1 1 d . . . H104 H 0.6503 0.1922 0.9090 0.054 Uiso 1 1 calc R . . C105 C 0.7324(4) 0.3415(6) 0.92911(17) 0.0470(14) Uani 1 1 d . . . H105 H 0.7536 0.3032 0.9549 0.056 Uiso 1 1 calc R . . C106 C 0.5730(3) 0.2518(6) 0.83435(16) 0.0426(13) Uani 1 1 d . . . C205 C 0.7669(3) 0.9176(3) 1.10687(16) 0.071(2) Uani 1 1 d G . . H205 H 0.7816 0.9999 1.0963 0.085 Uiso 1 1 calc R . . C204 C 0.7219(3) 0.9282(3) 1.13111(16) 0.082(3) Uani 1 1 d G . . H204 H 0.7060 1.0176 1.1371 0.098 Uiso 1 1 calc R . . C203 C 0.7004(3) 0.8079(4) 1.14661(15) 0.0547(16) Uani 1 1 d G . . C202 C 0.7238(3) 0.6771(3) 1.13785(16) 0.075(2) Uani 1 1 d G . . H202 H 0.7090 0.5949 1.1484 0.090 Uiso 1 1 calc R . . C201 C 0.7687(3) 0.6665(3) 1.11360(17) 0.074(2) Uani 1 1 d G . . H201 H 0.7847 0.5771 1.1076 0.088 Uiso 1 1 calc R . . C200 C 0.7902(3) 0.7868(4) 1.09811(15) 0.0568(16) Uani 1 1 d G . . C206 C 0.3480(4) 0.1837(7) 0.8270(2) 0.0543(16) Uani 1 1 d . . . C300 C 1.1569(3) 1.0344(6) 1.11475(16) 0.0434(13) Uani 1 1 d . . . C301 C 1.1401(3) 1.1579(6) 1.13023(19) 0.0469(14) Uani 1 1 d . . . H301 H 1.0896 1.1969 1.1198 0.056 Uiso 1 1 calc R . . C302 C 1.1961(3) 1.2249(6) 1.16067(18) 0.0444(13) Uani 1 1 d . . . H302 H 1.1836 1.3099 1.1709 0.053 Uiso 1 1 calc R . . C303 C 1.2702(3) 1.1708(6) 1.17657(16) 0.0422(13) Uani 1 1 d . . . C304 C 1.2879(3) 1.0476(8) 1.15985(19) 0.0583(17) Uani 1 1 d . . . H304 H 1.3389 1.0105 1.1691 0.070 Uiso 1 1 calc R . . C305 C 1.2314(4) 0.9822(8) 1.1304(2) 0.0637(19) Uani 1 1 d . . . H305 H 1.2436 0.8969 1.1202 0.076 Uiso 1 1 calc R . . C306 C 0.3289(3) 0.2583(6) 0.71036(17) 0.0447(13) Uani 1 1 d . . . C400 C 1.1262(2) 0.7282(5) 0.93349(11) 0.0525(15) Uani 1 1 d G . . C405 C 1.0945(2) 0.7554(6) 0.89324(12) 0.070(2) Uani 1 1 d G . . H405 H 1.0412 0.7790 0.8819 0.084 Uiso 1 1 calc R . . C404 C 1.1408(3) 0.7481(6) 0.86960(10) 0.087(3) Uani 1 1 d G . . H404 H 1.1191 0.7667 0.8421 0.104 Uiso 1 1 calc R . . C403 C 1.2187(3) 0.7137(6) 0.88620(14) 0.077(3) Uani 1 1 d G . . C402 C 1.2505(2) 0.6865(6) 0.92644(15) 0.077(2) Uani 1 1 d G . . H402 H 1.3038 0.6629 0.9378 0.093 Uiso 1 1 calc R . . C401 C 1.2042(2) 0.6937(6) 0.95009(11) 0.076(2) Uani 1 1 d G . . H401 H 1.2259 0.6751 0.9776 0.091 Uiso 1 1 calc R . . C406 C 1.2746(10) 0.7080(9) 0.8627(4) 0.107(5) Uani 1 1 d . . . Cd1 Cd 0.43500(2) 0.17006(5) 0.780231(12) 0.04293(18) Uani 1 1 d . . . N1 N 0.8544(3) 0.6745(5) 1.01261(15) 0.0472(12) Uani 1 1 d . . . N2 N 0.9685(3) 0.8425(5) 1.06932(17) 0.0505(13) Uani 1 1 d . . . N3 N 0.9527(3) 0.6526(5) 0.96530(14) 0.0436(11) Uani 1 1 d . . . N4 N 1.0632(3) 0.8356(5) 1.02026(14) 0.0448(11) Uani 1 1 d . . . O1 O 0.4165(4) 0.3312(7) 0.7712(2) 0.0354(16) Uani 0.50 1 d P A 1 O3 O 0.4795(3) -0.0236(7) 0.76003(16) 0.093(2) Uani 1 1 d . A . O101 O 0.5473(3) 0.1442(5) 0.84264(14) 0.0631(12) Uani 1 1 d . A . O102 O 0.5446(2) 0.3075(5) 0.80072(13) 0.0615(12) Uani 1 1 d . A . O201 O 0.3644(3) 0.0623(5) 0.81713(13) 0.0557(11) Uani 1 1 d . A . O202 O 0.3686(3) 0.2927(5) 0.81513(15) 0.0647(13) Uani 1 1 d . A . O301 O 0.3141(3) 0.1522(5) 0.72450(14) 0.0602(12) Uani 1 1 d . A . O302 O 0.3947(3) 0.3136(6) 0.72434(14) 0.0645(13) Uani 1 1 d . A . O401 O 1.3403(5) 0.7026(9) 0.8761(3) 0.142(4) Uani 1 1 d . . . O402 O 1.2388(6) 0.7143(10) 0.8254(3) 0.140(3) Uani 1 1 d . . . Pd2 Pd 0.95923(4) 0.75049(7) 1.01609(2) 0.0398(3) Uani 0.600(2) 1 d P . . 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 0.040(3) 0.043(3) 0.040(3) 0.007(2) 0.010(2) 0.006(2) C2 0.031(3) 0.056(4) 0.044(3) 0.005(3) 0.009(2) -0.004(3) C3 0.037(3) 0.066(4) 0.061(4) -0.009(3) 0.014(3) -0.004(3) C4 0.045(4) 0.082(5) 0.077(5) -0.014(4) 0.034(3) -0.010(3) C5 0.053(4) 0.072(4) 0.050(4) -0.019(3) 0.021(3) -0.021(3) C6 0.061(4) 0.053(4) 0.077(5) -0.013(3) 0.048(4) -0.016(3) C7 0.072(5) 0.064(4) 0.070(5) -0.029(4) 0.047(4) -0.026(4) C8 0.076(5) 0.094(6) 0.061(4) -0.021(4) 0.041(4) -0.030(4) C9 0.060(4) 0.070(4) 0.059(4) -0.016(3) 0.027(3) -0.023(4) C10 0.050(3) 0.046(3) 0.061(4) -0.008(3) 0.027(3) -0.005(3) C11 0.028(3) 0.054(3) 0.049(3) 0.006(3) 0.003(2) 0.004(2) C12 0.042(3) 0.047(3) 0.039(3) 0.004(3) 0.011(2) 0.003(3) C13 0.036(3) 0.067(4) 0.056(4) 0.013(3) 0.010(3) -0.006(3) C14 0.032(3) 0.080(5) 0.043(3) 0.011(3) 0.012(2) -0.003(3) C15 0.029(3) 0.063(4) 0.054(4) 0.021(3) 0.020(3) 0.012(3) C16 0.039(3) 0.057(4) 0.037(3) 0.003(3) 0.019(2) 0.008(3) C17 0.030(3) 0.071(4) 0.034(3) -0.001(3) 0.005(2) 0.010(3) C18 0.052(4) 0.076(4) 0.039(3) -0.004(3) 0.017(3) 0.008(3) C19 0.043(3) 0.066(4) 0.040(3) -0.012(3) 0.011(3) 0.003(3) C20 0.041(3) 0.057(4) 0.036(3) -0.006(3) 0.011(2) -0.004(3) C100 0.035(3) 0.053(3) 0.031(3) 0.004(2) 0.005(2) 0.005(2) C101 0.064(4) 0.080(5) 0.063(4) 0.027(4) 0.008(4) -0.025(4) C102 0.053(4) 0.087(5) 0.032(3) 0.024(3) -0.006(3) -0.020(4) C103 0.031(3) 0.051(3) 0.033(3) 0.000(2) 0.006(2) 0.003(2) C104 0.059(4) 0.037(3) 0.039(3) 0.002(2) 0.017(3) 0.000(3) C105 0.056(4) 0.046(3) 0.034(3) 0.003(2) 0.007(3) 0.006(3) C106 0.040(3) 0.053(4) 0.035(3) -0.002(3) 0.012(2) -0.001(3) C205 0.106(6) 0.046(4) 0.091(5) 0.000(4) 0.073(5) 0.001(4) C204 0.112(6) 0.048(4) 0.123(7) -0.004(4) 0.090(6) -0.008(4) C203 0.066(4) 0.046(3) 0.065(4) -0.008(3) 0.038(4) -0.002(3) C202 0.101(6) 0.048(4) 0.104(6) -0.010(4) 0.069(6) -0.018(4) C201 0.090(6) 0.046(4) 0.118(7) -0.015(4) 0.079(6) -0.015(4) C200 0.056(4) 0.052(4) 0.070(4) -0.007(3) 0.032(3) -0.008(3) C206 0.060(4) 0.056(4) 0.054(4) -0.011(3) 0.028(3) -0.009(3) C300 0.037(3) 0.049(3) 0.043(3) 0.005(3) 0.011(2) 0.004(3) C301 0.033(3) 0.045(3) 0.058(4) 0.003(3) 0.009(3) 0.005(2) C302 0.035(3) 0.041(3) 0.056(4) 0.008(3) 0.013(3) 0.003(2) C303 0.040(3) 0.053(3) 0.032(3) 0.004(2) 0.010(2) 0.001(3) C304 0.035(3) 0.074(4) 0.056(4) -0.006(3) 0.002(3) 0.013(3) C305 0.044(3) 0.065(4) 0.064(4) -0.021(3) -0.005(3) 0.022(3) C306 0.044(3) 0.050(4) 0.041(3) -0.002(3) 0.014(3) 0.001(3) C400 0.045(3) 0.066(4) 0.056(4) -0.008(3) 0.030(3) -0.007(3) C405 0.054(4) 0.112(7) 0.050(4) 0.002(4) 0.026(3) -0.008(4) C404 0.090(6) 0.130(8) 0.049(4) 0.018(5) 0.035(4) 0.006(6) C403 0.102(6) 0.053(4) 0.115(7) -0.022(4) 0.086(6) -0.015(4) C402 0.061(5) 0.099(6) 0.082(6) 0.001(5) 0.037(4) 0.021(4) C401 0.065(5) 0.114(7) 0.061(4) 0.009(4) 0.036(4) 0.017(4) C406 0.187(13) 0.043(4) 0.151(11) -0.023(6) 0.137(11) -0.019(6) Cd1 0.0393(3) 0.0481(3) 0.0437(3) -0.00084(18) 0.01700(19) -0.00084(18) N1 0.039(3) 0.056(3) 0.049(3) -0.004(2) 0.018(2) 0.000(2) N2 0.053(3) 0.044(3) 0.068(3) -0.004(2) 0.040(3) -0.004(2) N3 0.037(2) 0.054(3) 0.038(2) 0.003(2) 0.011(2) 0.008(2) N4 0.045(3) 0.049(3) 0.044(3) 0.013(2) 0.019(2) 0.016(2) O1 0.034(4) 0.043(4) 0.025(3) 0.002(3) 0.004(3) -0.001(3) O3 0.066(3) 0.110(5) 0.071(3) -0.049(3) -0.019(2) 0.044(3) O101 0.062(3) 0.062(3) 0.059(3) 0.002(2) 0.011(2) -0.006(2) O102 0.042(2) 0.085(3) 0.043(2) 0.018(2) -0.0037(19) -0.012(2) O201 0.062(3) 0.057(3) 0.058(3) -0.002(2) 0.033(2) 0.007(2) O202 0.083(3) 0.061(3) 0.070(3) -0.002(2) 0.052(3) -0.009(3) O301 0.043(2) 0.064(3) 0.058(3) 0.001(2) -0.003(2) 0.001(2) O302 0.043(3) 0.087(4) 0.057(3) 0.010(2) 0.007(2) -0.006(2) O401 0.128(7) 0.126(6) 0.241(12) 0.045(6) 0.152(8) 0.025(5) O402 0.183(9) 0.156(7) 0.136(7) -0.021(6) 0.125(7) -0.012(6) Pd2 0.0399(4) 0.0419(5) 0.0427(5) -0.0018(3) 0.0205(3) -0.0016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.389(8) . ? C1 C20 1.400(8) . ? C1 C100 1.487(8) . ? C2 N1 1.370(8) . ? C2 C3 1.463(8) . ? C3 C4 1.334(10) . ? C3 H3 0.9500 . ? C4 C5 1.437(9) . ? C4 H4 0.9500 . ? C5 N1 1.371(8) . ? C5 C6 1.431(10) . ? C6 C7 1.379(10) . ? C6 C200 1.499(6) . ? C7 N2 1.382(8) . ? C7 C8 1.387(10) . ? C8 C9 1.345(10) . ? C8 H8 0.9500 . ? C9 C10 1.449(9) . ? C9 H9 0.9500 . ? C10 N2 1.344(8) . ? C10 C11 1.408(8) . ? C11 C12 1.392(8) . ? C11 C300 1.489(8) . ? C12 N4 1.358(8) . ? C12 C13 1.442(8) . ? C13 C14 1.358(9) . ? C13 H13 0.9500 . ? C14 C15 1.454(9) . ? C14 H14 0.9500 . ? C15 C16 1.392(9) . ? C15 N4 1.407(7) . ? C16 C17 1.396(9) . ? C16 C400 1.506(6) . ? C17 N3 1.361(7) . ? C17 C18 1.450(9) . ? C18 C19 1.353(9) . ? C18 H18 0.9500 . ? C19 C20 1.446(8) . ? C19 H19 0.9500 . ? C20 N3 1.362(8) . ? C100 C105 1.378(8) . ? C100 C101 1.392(8) . ? C101 C102 1.364(9) . ? C101 H101 0.9500 . ? C102 C103 1.393(9) . ? C102 H102 0.9500 . ? C103 C104 1.366(8) . ? C103 C106 1.492(8) . ? C104 C105 1.378(9) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C106 O101 1.208(7) . ? C106 O102 1.261(7) . ? C205 C204 1.3900 . ? C205 C200 1.3900 . ? C205 H205 0.9500 . ? C204 C203 1.3900 . ? C204 H204 0.9500 . ? C203 C202 1.3900 . ? C203 C206 1.505(7) 3_667 ? C202 C201 1.3900 . ? C202 H202 0.9500 . ? C201 C200 1.3900 . ? C201 H201 0.9500 . ? C206 O202 1.231(8) . ? C206 O201 1.276(8) . ? C206 C203 1.51(4) 3_667 ? C300 C301 1.381(8) . ? C300 C305 1.382(8) . ? C301 C302 1.379(9) . ? C301 H301 0.9500 . ? C302 C303 1.384(8) . ? C302 H302 0.9500 . ? C303 C304 1.406(9) . ? C303 C306 1.486(8) 4_676 ? C304 C305 1.357(9) . ? C304 H304 0.9500 . ? C305 H305 0.9500 . ? C306 O301 1.205(7) . ? C306 O302 1.255(7) . ? C306 C303 1.486(8) 4_475 ? C400 C405 1.3900 . ? C400 C401 1.3900 . ? C405 C404 1.3900 . ? C405 H405 0.9500 . ? C404 C403 1.3900 . ? C404 H404 0.9500 . ? C403 C402 1.3900 . ? C403 C406 1.533(10) . ? C402 C401 1.3900 . ? C402 H402 0.9500 . ? C401 H401 0.9500 . ? C406 O401 1.137(17) . ? C406 O402 1.278(17) . ? Cd1 O1 1.584(7) . ? Cd1 O3 2.238(5) . ? Cd1 O102 2.302(5) . ? Cd1 O202 2.336(5) . ? Cd1 O302 2.336(5) . ? Cd1 O201 2.377(4) . ? Cd1 O301 2.442(4) . ? Cd1 O101 2.493(5) . ? N1 Pd2 2.018(5) . ? N2 Pd2 2.060(5) . ? N3 Pd2 2.019(5) . ? N4 Pd2 2.030(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C20 124.2(5) . . ? C2 C1 C100 117.6(5) . . ? C20 C1 C100 118.1(5) . . ? N1 C2 C1 126.1(5) . . ? N1 C2 C3 109.5(5) . . ? C1 C2 C3 124.4(5) . . ? C4 C3 C2 106.3(6) . . ? C4 C3 H3 126.8 . . ? C2 C3 H3 126.8 . . ? C3 C4 C5 108.2(6) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? N1 C5 C6 124.9(6) . . ? N1 C5 C4 109.6(6) . . ? C6 C5 C4 125.5(6) . . ? C7 C6 C5 124.1(6) . . ? C7 C6 C200 118.7(6) . . ? C5 C6 C200 117.2(6) . . ? C6 C7 N2 125.4(7) . . ? C6 C7 C8 125.9(6) . . ? N2 C7 C8 108.6(6) . . ? C9 C8 C7 109.3(6) . . ? C9 C8 H8 125.4 . . ? C7 C8 H8 125.4 . . ? C8 C9 C10 105.8(6) . . ? C8 C9 H9 127.1 . . ? C10 C9 H9 127.1 . . ? N2 C10 C11 126.9(6) . . ? N2 C10 C9 108.7(5) . . ? C11 C10 C9 124.4(6) . . ? C12 C11 C10 123.3(6) . . ? C12 C11 C300 119.0(5) . . ? C10 C11 C300 117.6(5) . . ? N4 C12 C11 125.5(5) . . ? N4 C12 C13 109.7(5) . . ? C11 C12 C13 124.9(6) . . ? C14 C13 C12 107.0(6) . . ? C14 C13 H13 126.5 . . ? C12 C13 H13 126.5 . . ? C13 C14 C15 108.4(5) . . ? C13 C14 H14 125.8 . . ? C15 C14 H14 125.8 . . ? C16 C15 N4 126.0(5) . . ? C16 C15 C14 126.9(5) . . ? N4 C15 C14 106.8(6) . . ? C15 C16 C17 123.8(5) . . ? C15 C16 C400 117.2(5) . . ? C17 C16 C400 119.0(5) . . ? N3 C17 C16 126.6(5) . . ? N3 C17 C18 109.3(5) . . ? C16 C17 C18 124.2(5) . . ? C19 C18 C17 106.4(5) . . ? C19 C18 H18 126.8 . . ? C17 C18 H18 126.8 . . ? C18 C19 C20 107.6(5) . . ? C18 C19 H19 126.2 . . ? C20 C19 H19 126.2 . . ? N3 C20 C1 125.5(5) . . ? N3 C20 C19 108.7(5) . . ? C1 C20 C19 125.7(5) . . ? C105 C100 C101 116.7(5) . . ? C105 C100 C1 122.4(5) . . ? C101 C100 C1 120.9(6) . . ? C102 C101 C100 122.1(6) . . ? C102 C101 H101 118.9 . . ? C100 C101 H101 118.9 . . ? C101 C102 C103 120.3(5) . . ? C101 C102 H102 119.8 . . ? C103 C102 H102 119.8 . . ? C104 C103 C102 118.0(5) . . ? C104 C103 C106 121.1(5) . . ? C102 C103 C106 120.9(5) . . ? C103 C104 C105 121.4(6) . . ? C103 C104 H104 119.3 . . ? C105 C104 H104 119.3 . . ? C100 C105 C104 121.4(5) . . ? C100 C105 H105 119.3 . . ? C104 C105 H105 119.3 . . ? O101 C106 O102 121.7(6) . . ? O101 C106 C103 120.8(5) . . ? O102 C106 C103 117.6(5) . . ? C204 C205 C200 120.0 . . ? C204 C205 H205 120.0 . . ? C200 C205 H205 120.0 . . ? C203 C204 C205 120.0 . . ? C203 C204 H204 120.0 . . ? C205 C204 H204 120.0 . . ? C204 C203 C202 120.0 . . ? C204 C203 C206 121.1(4) . 3_667 ? C202 C203 C206 118.9(4) . 3_667 ? C201 C202 C203 120.0 . . ? C201 C202 H202 120.0 . . ? C203 C202 H202 120.0 . . ? C202 C201 C200 120.0 . . ? C202 C201 H201 120.0 . . ? C200 C201 H201 120.0 . . ? C201 C200 C205 120.0 . . ? C201 C200 C6 119.5(4) . . ? C205 C200 C6 120.3(4) . . ? O202 C206 O201 123.0(6) . . ? O202 C206 C203 119.2(16) . 3_667 ? O201 C206 C203 117.9(16) . 3_667 ? C301 C300 C305 117.9(6) . . ? C301 C300 C11 121.5(5) . . ? C305 C300 C11 120.5(5) . . ? C302 C301 C300 120.5(5) . . ? C302 C301 H301 119.7 . . ? C300 C301 H301 119.7 . . ? C301 C302 C303 121.2(6) . . ? C301 C302 H302 119.4 . . ? C303 C302 H302 119.4 . . ? C302 C303 C304 118.0(5) . . ? C302 C303 C306 120.4(5) . 4_676 ? C304 C303 C306 121.5(5) . 4_676 ? C305 C304 C303 119.6(6) . . ? C305 C304 H304 120.2 . . ? C303 C304 H304 120.2 . . ? C304 C305 C300 122.7(6) . . ? C304 C305 H305 118.6 . . ? C300 C305 H305 118.6 . . ? O301 C306 O302 120.5(6) . . ? O301 C306 C303 121.6(5) . 4_475 ? O302 C306 C303 118.0(6) . 4_475 ? C405 C400 C401 120.0 . . ? C405 C400 C16 119.6(3) . . ? C401 C400 C16 120.4(3) . . ? C404 C405 C400 120.0 . . ? C404 C405 H405 120.0 . . ? C400 C405 H405 120.0 . . ? C405 C404 C403 120.0 . . ? C405 C404 H404 120.0 . . ? C403 C404 H404 120.0 . . ? C404 C403 C402 120.0 . . ? C404 C403 C406 123.5(7) . . ? C402 C403 C406 116.4(7) . . ? C401 C402 C403 120.0 . . ? C401 C402 H402 120.0 . . ? C403 C402 H402 120.0 . . ? C402 C401 C400 120.0 . . ? C402 C401 H401 120.0 . . ? C400 C401 H401 120.0 . . ? O401 C406 O402 122.9(10) . . ? O401 C406 C403 125.1(13) . . ? O402 C406 C403 111.9(13) . . ? O1 Cd1 O3 144.2(3) . . ? O1 Cd1 O102 67.4(3) . . ? O3 Cd1 O102 101.5(2) . . ? O1 Cd1 O202 60.6(3) . . ? O3 Cd1 O202 154.3(2) . . ? O102 Cd1 O202 95.68(19) . . ? O1 Cd1 O302 43.2(3) . . ? O3 Cd1 O302 104.4(2) . . ? O102 Cd1 O302 86.00(16) . . ? O202 Cd1 O302 95.58(19) . . ? O1 Cd1 O201 114.5(3) . . ? O3 Cd1 O201 98.7(2) . . ? O102 Cd1 O201 130.41(16) . . ? O202 Cd1 O201 55.71(16) . . ? O302 Cd1 O201 131.29(16) . . ? O1 Cd1 O301 80.1(3) . . ? O3 Cd1 O301 90.31(17) . . ? O102 Cd1 O301 139.03(16) . . ? O202 Cd1 O301 89.02(18) . . ? O302 Cd1 O301 53.04(17) . . ? O201 Cd1 O301 85.04(17) . . ? O1 Cd1 O101 109.6(3) . . ? O3 Cd1 O101 85.96(17) . . ? O102 Cd1 O101 53.28(16) . . ? O202 Cd1 O101 89.29(19) . . ? O302 Cd1 O101 139.27(17) . . ? O201 Cd1 O101 83.93(16) . . ? O301 Cd1 O101 167.69(17) . . ? C2 N1 C5 106.4(5) . . ? C2 N1 Pd2 125.1(4) . . ? C5 N1 Pd2 127.0(4) . . ? C10 N2 C7 107.5(5) . . ? C10 N2 Pd2 125.3(4) . . ? C7 N2 Pd2 125.8(4) . . ? C17 N3 C20 107.8(5) . . ? C17 N3 Pd2 125.8(4) . . ? C20 N3 Pd2 125.7(4) . . ? C12 N4 C15 108.0(5) . . ? C12 N4 Pd2 127.5(4) . . ? C15 N4 Pd2 123.7(4) . . ? C106 O101 Cd1 88.1(4) . . ? C106 O102 Cd1 95.8(4) . . ? C206 O201 Cd1 89.1(4) . . ? C206 O202 Cd1 92.2(4) . . ? C306 O301 Cd1 90.9(4) . . ? C306 O302 Cd1 94.6(4) . . ? N1 Pd2 N3 90.7(2) . . ? N1 Pd2 N4 177.4(2) . . ? N3 Pd2 N4 91.1(2) . . ? N1 Pd2 N2 89.4(2) . . ? N3 Pd2 N2 177.4(2) . . ? N4 Pd2 N2 88.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 C1 C2 N1 -8.5(10) . . . . ? C100 C1 C2 N1 175.0(5) . . . . ? C20 C1 C2 C3 173.1(6) . . . . ? C100 C1 C2 C3 -3.4(9) . . . . ? N1 C2 C3 C4 -2.0(8) . . . . ? C1 C2 C3 C4 176.7(6) . . . . ? C2 C3 C4 C5 0.9(9) . . . . ? C3 C4 C5 N1 0.4(9) . . . . ? C3 C4 C5 C6 -177.1(8) . . . . ? N1 C5 C6 C7 6.2(13) . . . . ? C4 C5 C6 C7 -176.7(8) . . . . ? N1 C5 C6 C200 -172.1(6) . . . . ? C4 C5 C6 C200 5.1(12) . . . . ? C5 C6 C7 N2 13.2(13) . . . . ? C200 C6 C7 N2 -168.6(6) . . . . ? C5 C6 C7 C8 -172.6(8) . . . . ? C200 C6 C7 C8 5.6(12) . . . . ? C6 C7 C8 C9 -175.6(8) . . . . ? N2 C7 C8 C9 -0.6(10) . . . . ? C7 C8 C9 C10 2.2(10) . . . . ? C8 C9 C10 N2 -3.1(9) . . . . ? C8 C9 C10 C11 174.3(7) . . . . ? N2 C10 C11 C12 -8.8(10) . . . . ? C9 C10 C11 C12 174.3(6) . . . . ? N2 C10 C11 C300 174.1(6) . . . . ? C9 C10 C11 C300 -2.7(10) . . . . ? C10 C11 C12 N4 -8.7(9) . . . . ? C300 C11 C12 N4 168.4(5) . . . . ? C10 C11 C12 C13 170.9(6) . . . . ? C300 C11 C12 C13 -12.1(9) . . . . ? N4 C12 C13 C14 -3.6(7) . . . . ? C11 C12 C13 C14 176.8(6) . . . . ? C12 C13 C14 C15 0.8(7) . . . . ? C13 C14 C15 C16 -172.7(6) . . . . ? C13 C14 C15 N4 2.1(7) . . . . ? N4 C15 C16 C17 12.2(9) . . . . ? C14 C15 C16 C17 -174.0(6) . . . . ? N4 C15 C16 C400 -170.1(5) . . . . ? C14 C15 C16 C400 3.7(9) . . . . ? C15 C16 C17 N3 6.5(10) . . . . ? C400 C16 C17 N3 -171.2(5) . . . . ? C15 C16 C17 C18 -174.2(6) . . . . ? C400 C16 C17 C18 8.1(9) . . . . ? N3 C17 C18 C19 3.9(7) . . . . ? C16 C17 C18 C19 -175.5(6) . . . . ? C17 C18 C19 C20 -1.2(7) . . . . ? C2 C1 C20 N3 -9.0(10) . . . . ? C100 C1 C20 N3 167.5(5) . . . . ? C2 C1 C20 C19 173.1(6) . . . . ? C100 C1 C20 C19 -10.4(9) . . . . ? C18 C19 C20 N3 -1.8(7) . . . . ? C18 C19 C20 C1 176.4(6) . . . . ? C2 C1 C100 C105 -64.6(8) . . . . ? C20 C1 C100 C105 118.7(6) . . . . ? C2 C1 C100 C101 113.2(7) . . . . ? C20 C1 C100 C101 -63.5(8) . . . . ? C105 C100 C101 C102 2.8(11) . . . . ? C1 C100 C101 C102 -175.1(7) . . . . ? C100 C101 C102 C103 -0.7(12) . . . . ? C101 C102 C103 C104 -0.9(10) . . . . ? C101 C102 C103 C106 177.6(7) . . . . ? C102 C103 C104 C105 0.2(9) . . . . ? C106 C103 C104 C105 -178.2(5) . . . . ? C101 C100 C105 C104 -3.5(9) . . . . ? C1 C100 C105 C104 174.4(5) . . . . ? C103 C104 C105 C100 2.0(9) . . . . ? C104 C103 C106 O101 -4.9(9) . . . . ? C102 C103 C106 O101 176.7(6) . . . . ? C104 C103 C106 O102 175.8(6) . . . . ? C102 C103 C106 O102 -2.6(9) . . . . ? C200 C205 C204 C203 0.0 . . . . ? C205 C204 C203 C202 0.0 . . . . ? C205 C204 C203 C206 179.8(6) . . . 3_667 ? C204 C203 C202 C201 0.0 . . . . ? C206 C203 C202 C201 -179.8(6) 3_667 . . . ? C203 C202 C201 C200 0.0 . . . . ? C202 C201 C200 C205 0.0 . . . . ? C202 C201 C200 C6 176.1(6) . . . . ? C204 C205 C200 C201 0.0 . . . . ? C204 C205 C200 C6 -176.1(6) . . . . ? C7 C6 C200 C201 -109.8(7) . . . . ? C5 C6 C200 C201 68.5(8) . . . . ? C7 C6 C200 C205 66.3(8) . . . . ? C5 C6 C200 C205 -115.4(6) . . . . ? C12 C11 C300 C301 122.9(6) . . . . ? C10 C11 C300 C301 -59.9(8) . . . . ? C12 C11 C300 C305 -61.2(8) . . . . ? C10 C11 C300 C305 116.1(7) . . . . ? C305 C300 C301 C302 -0.8(9) . . . . ? C11 C300 C301 C302 175.3(6) . . . . ? C300 C301 C302 C303 -0.1(9) . . . . ? C301 C302 C303 C304 2.2(9) . . . . ? C301 C302 C303 C306 -177.7(5) . . . 4_676 ? C302 C303 C304 C305 -3.4(10) . . . . ? C306 C303 C304 C305 176.5(6) 4_676 . . . ? C303 C304 C305 C300 2.6(12) . . . . ? C301 C300 C305 C304 -0.5(11) . . . . ? C11 C300 C305 C304 -176.6(7) . . . . ? C15 C16 C400 C405 -121.0(5) . . . . ? C17 C16 C400 C405 56.8(7) . . . . ? C15 C16 C400 C401 60.2(6) . . . . ? C17 C16 C400 C401 -122.0(5) . . . . ? C401 C400 C405 C404 0.0 . . . . ? C16 C400 C405 C404 -178.8(5) . . . . ? C400 C405 C404 C403 0.0 . . . . ? C405 C404 C403 C402 0.0 . . . . ? C405 C404 C403 C406 -177.9(6) . . . . ? C404 C403 C402 C401 0.0 . . . . ? C406 C403 C402 C401 178.0(6) . . . . ? C403 C402 C401 C400 0.0 . . . . ? C405 C400 C401 C402 0.0 . . . . ? C16 C400 C401 C402 178.8(5) . . . . ? C404 C403 C406 O401 166.7(9) . . . . ? C402 C403 C406 O401 -11.3(12) . . . . ? C404 C403 C406 O402 -11.4(10) . . . . ? C402 C403 C406 O402 170.6(7) . . . . ? C1 C2 N1 C5 -176.5(6) . . . . ? C3 C2 N1 C5 2.2(7) . . . . ? C1 C2 N1 Pd2 16.9(9) . . . . ? C3 C2 N1 Pd2 -164.5(4) . . . . ? C6 C5 N1 C2 175.9(7) . . . . ? C4 C5 N1 C2 -1.6(8) . . . . ? C6 C5 N1 Pd2 -17.8(11) . . . . ? C4 C5 N1 Pd2 164.7(5) . . . . ? C11 C10 N2 C7 -174.5(7) . . . . ? C9 C10 N2 C7 2.7(8) . . . . ? C11 C10 N2 Pd2 17.8(9) . . . . ? C9 C10 N2 Pd2 -164.9(5) . . . . ? C6 C7 N2 C10 173.7(7) . . . . ? C8 C7 N2 C10 -1.4(9) . . . . ? C6 C7 N2 Pd2 -18.8(11) . . . . ? C8 C7 N2 Pd2 166.2(5) . . . . ? C16 C17 N3 C20 174.3(6) . . . . ? C18 C17 N3 C20 -5.1(7) . . . . ? C16 C17 N3 Pd2 -15.1(9) . . . . ? C18 C17 N3 Pd2 165.5(4) . . . . ? C1 C20 N3 C17 -173.9(6) . . . . ? C19 C20 N3 C17 4.3(7) . . . . ? C1 C20 N3 Pd2 15.5(9) . . . . ? C19 C20 N3 Pd2 -166.3(4) . . . . ? C11 C12 N4 C15 -175.5(5) . . . . ? C13 C12 N4 C15 4.9(6) . . . . ? C11 C12 N4 Pd2 14.8(8) . . . . ? C13 C12 N4 Pd2 -164.9(4) . . . . ? C16 C15 N4 C12 170.6(6) . . . . ? C14 C15 N4 C12 -4.3(6) . . . . ? C16 C15 N4 Pd2 -19.2(8) . . . . ? C14 C15 N4 Pd2 166.0(4) . . . . ? O102 C106 O101 Cd1 -10.9(6) . . . . ? C103 C106 O101 Cd1 169.8(5) . . . . ? O1 Cd1 O101 C106 -33.0(5) . . . . ? O3 Cd1 O101 C106 113.9(4) . . . . ? O102 Cd1 O101 C106 6.3(4) . . . . ? O202 Cd1 O101 C106 -91.3(4) . . . . ? O302 Cd1 O101 C106 6.4(5) . . . . ? O201 Cd1 O101 C106 -146.9(4) . . . . ? O301 Cd1 O101 C106 -173.4(7) . . . . ? O101 C106 O102 Cd1 11.9(7) . . . . ? C103 C106 O102 Cd1 -168.8(4) . . . . ? O1 Cd1 O102 C106 133.6(5) . . . . ? O3 Cd1 O102 C106 -82.1(4) . . . . ? O202 Cd1 O102 C106 78.8(4) . . . . ? O302 Cd1 O102 C106 174.0(4) . . . . ? O201 Cd1 O102 C106 30.0(5) . . . . ? O301 Cd1 O102 C106 173.8(3) . . . . ? O101 Cd1 O102 C106 -6.1(3) . . . . ? O202 C206 O201 Cd1 2.0(7) . . . . ? C203 C206 O201 Cd1 -179.6(11) 3_667 . . . ? O1 Cd1 O201 C206 -16.5(5) . . . . ? O3 Cd1 O201 C206 177.2(4) . . . . ? O102 Cd1 O201 C206 63.9(5) . . . . ? O202 Cd1 O201 C206 -1.0(4) . . . . ? O302 Cd1 O201 C206 -64.8(5) . . . . ? O301 Cd1 O201 C206 -93.2(4) . . . . ? O101 Cd1 O201 C206 92.2(4) . . . . ? O201 C206 O202 Cd1 -2.0(8) . . . . ? C203 C206 O202 Cd1 179.6(11) 3_667 . . . ? O1 Cd1 O202 C206 164.9(6) . . . . ? O3 Cd1 O202 C206 -2.9(7) . . . . ? O102 Cd1 O202 C206 -135.0(4) . . . . ? O302 Cd1 O202 C206 138.5(4) . . . . ? O201 Cd1 O202 C206 1.1(4) . . . . ? O301 Cd1 O202 C206 85.8(5) . . . . ? O101 Cd1 O202 C206 -82.0(4) . . . . ? O302 C306 O301 Cd1 9.6(6) . . . . ? C303 C306 O301 Cd1 -169.3(5) 4_475 . . . ? O1 Cd1 O301 C306 31.8(4) . . . . ? O3 Cd1 O301 C306 -113.5(4) . . . . ? O102 Cd1 O301 C306 -5.4(5) . . . . ? O202 Cd1 O301 C306 92.2(4) . . . . ? O302 Cd1 O301 C306 -5.6(4) . . . . ? O201 Cd1 O301 C306 147.8(4) . . . . ? O101 Cd1 O301 C306 174.3(7) . . . . ? O301 C306 O302 Cd1 -10.1(6) . . . . ? C303 C306 O302 Cd1 168.9(4) 4_475 . . . ? O1 Cd1 O302 C306 -113.7(6) . . . . ? O3 Cd1 O302 C306 84.6(4) . . . . ? O102 Cd1 O302 C306 -174.5(4) . . . . ? O202 Cd1 O302 C306 -79.2(4) . . . . ? O201 Cd1 O302 C306 -31.1(5) . . . . ? O301 Cd1 O302 C306 5.4(3) . . . . ? O101 Cd1 O302 C306 -174.6(3) . . . . ? C2 N1 Pd2 N3 -8.6(5) . . . . ? C5 N1 Pd2 N3 -172.5(6) . . . . ? C2 N1 Pd2 N4 127(4) . . . . ? C5 N1 Pd2 N4 -37(5) . . . . ? C2 N1 Pd2 N2 174.0(5) . . . . ? C5 N1 Pd2 N2 10.1(6) . . . . ? C17 N3 Pd2 N1 -175.2(5) . . . . ? C20 N3 Pd2 N1 -6.3(5) . . . . ? C17 N3 Pd2 N4 6.6(5) . . . . ? C20 N3 Pd2 N4 175.5(5) . . . . ? C17 N3 Pd2 N2 -83(4) . . . . ? C20 N3 Pd2 N2 86(4) . . . . ? C12 N4 Pd2 N1 42(5) . . . . ? C15 N4 Pd2 N1 -127(4) . . . . ? C12 N4 Pd2 N3 177.2(5) . . . . ? C15 N4 Pd2 N3 8.9(4) . . . . ? C12 N4 Pd2 N2 -5.4(5) . . . . ? C15 N4 Pd2 N2 -173.7(4) . . . . ? C10 N2 Pd2 N1 172.3(5) . . . . ? C7 N2 Pd2 N1 6.9(6) . . . . ? C10 N2 Pd2 N3 80(4) . . . . ? C7 N2 Pd2 N3 -85(4) . . . . ? C10 N2 Pd2 N4 -9.6(5) . . . . ? C7 N2 Pd2 N4 -175.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.109 _refine_diff_density_min -1.242 _refine_diff_density_rms 0.147 # Attachment '- Structure 1-Zn.cif' data_Structure_1-Zn _database_code_depnum_ccdc_archive 'CCDC 865041' #TrackingRef '- Structure 1-Zn.cif' _audit_creation_date 2012-01-06 _audit_creation_method ; Olex2 1.1 (compiled Nov 1 2011 20:42:30, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H26 Cd N4 O9 Zn' _chemical_formula_sum 'C48 H26 Cd N4 O9 Zn' _chemical_formula_weight 980.50 _chemical_melting_point ? 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' Zn Zn 0.2839 1.4301 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, y+1/2, -z+1/2' 3 '-x, -y, -z' 4 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.255(4) _cell_length_b 9.3888(19) _cell_length_c 34.534(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.624(6) _cell_angle_gamma 90.00 _cell_volume 5836(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9855 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.315 _cell_measurement_theta_min 3.263 _exptl_absorpt_coefficient_mu 0.821 _exptl_absorpt_correction_T_max 0.9137 _exptl_absorpt_correction_T_min 0.8248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'irregular blocks' _exptl_crystal_F_000 1968 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0957 _diffrn_reflns_av_unetI/netI 0.0546 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_number 23675 _diffrn_reflns_theta_full 21.97 _diffrn_reflns_theta_max 21.97 _diffrn_reflns_theta_min 8.53 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.863 _diffrn_measured_fraction_theta_max 0.863 _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'MO K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _reflns_number_gt 5307 _reflns_number_total 6142 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 4.112 _refine_diff_density_min -1.363 _refine_diff_density_rms 0.141 _refine_ls_extinction_coef 0.0069(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 575 _refine_ls_number_reflns 6142 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.1249 _refine_ls_R_factor_gt 0.1157 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.368 _refine_ls_shift/su_mean 0.006 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+130.3883P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2696 _refine_ls_wR_factor_ref 0.2754 _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 C39 C 0.0923(9) 0.0678(14) 0.3674(5) 0.054(3) Uani 1 1 d U A 4 H39 H 0.0718 -0.0242 0.3614 0.065 Uiso 1 1 calc R A 4 C34 C 0.1607(9) 0.0800(13) 0.3902(5) 0.052(3) Uani 1 1 d U A 4 H34 H 0.1872 -0.0037 0.3995 0.062 Uiso 1 1 calc R A 4 C37 C 0.0826(9) 0.3124(13) 0.3621(4) 0.050(3) Uani 1 1 d U A 4 H37 H 0.0557 0.3956 0.3527 0.060 Uiso 1 1 calc R A 4 C35 C 0.1916(8) 0.2098(13) 0.3999(4) 0.044(3) Uani 1 1 d U A 4 C38 C 0.0531(9) 0.1850(13) 0.3531(4) 0.046(3) Uani 1 1 d U . 4 C36 C 0.1553(10) 0.3258(15) 0.3858(4) 0.056(4) Uani 1 1 d . A 4 H36 H 0.1769 0.4172 0.3913 0.068 Uiso 1 1 calc R A 4 C48 C 0.1208(8) 0.7585(14) 0.7888(3) 0.036(3) Uani 1 1 d . . 4 C24 C 0.5938(8) -0.1873(11) 0.3225(3) 0.033(3) Uani 1 1 d . . 4 O8 O 0.1711(6) 0.7019(10) 0.7752(2) 0.050(2) Uani 1 1 d D . 4 Cd1 Cd 0.15547(5) 0.84643(9) 0.71871(2) 0.0345(5) Uani 1 1 d D . 1 Zn2 Zn 0.44090(11) 0.2492(2) 0.48083(5) 0.0601(7) Uani 1 1 d . A . C17 C 0.5598(8) 0.3552(15) 0.5481(3) 0.043(3) Uani 1 1 d . . . C15 C 0.6038(8) 0.1608(14) 0.5077(3) 0.041(3) Uani 1 1 d . A . C1 C 0.3737(7) 0.4619(12) 0.5467(3) 0.026(3) Uani 1 1 d . . . C7 C 0.3259(9) 0.1695(15) 0.4088(4) 0.051(4) Uani 1 1 d . A . C11 C 0.5088(7) 0.0333(12) 0.4147(3) 0.033(3) Uani 1 1 d . . . C16 C 0.6149(7) 0.2554(13) 0.5390(3) 0.033(3) Uani 1 1 d . . . C13 C 0.6256(7) -0.0066(14) 0.4639(4) 0.040(3) Uani 1 1 d . . . H13 H 0.6473 -0.0812 0.4511 0.048 Uiso 1 1 calc R . . C10 C 0.4381(8) 0.0846(13) 0.4051(4) 0.039(3) Uani 1 1 d . A . C18 C 0.5715(9) 0.4641(15) 0.5783(4) 0.049(4) Uani 1 1 d . . . H18 H 0.6178 0.4904 0.5934 0.059 Uiso 1 1 calc R . . C14 C 0.6553(8) 0.0565(15) 0.4989(4) 0.045(4) Uani 1 1 d . . . H14 H 0.7019 0.0344 0.5145 0.054 Uiso 1 1 calc R . . C19 C 0.5052(7) 0.5210(14) 0.5811(3) 0.034(3) Uani 1 1 d . . . H19 H 0.4961 0.5954 0.5983 0.041 Uiso 1 1 calc R . . C4 C 0.2138(10) 0.3457(18) 0.4795(5) 0.063(4) Uani 1 1 d . . . H4 H 0.1623 0.3318 0.4701 0.075 Uiso 1 1 calc R . . C5 C 0.2730(10) 0.3003(15) 0.4605(4) 0.054(4) Uani 1 1 d . A . C20 C 0.4491(8) 0.4465(14) 0.5524(3) 0.038(3) Uani 1 1 d . . . C2 C 0.3204(7) 0.4054(14) 0.5166(4) 0.039(3) Uani 1 1 d . A . C6 C 0.2673(8) 0.2239(15) 0.4244(4) 0.046(3) Uani 1 1 d . . . C12 C 0.5580(8) 0.0594(12) 0.4509(3) 0.039(3) Uani 1 1 d . A . C9 C 0.3903(9) 0.0668(16) 0.3667(4) 0.054(4) Uani 1 1 d . A . H9 H 0.4051 0.0293 0.3437 0.065 Uiso 1 1 calc R . . C3 C 0.2431(9) 0.4126(17) 0.5136(4) 0.055(4) Uani 1 1 d . . . H3 H 0.2163 0.4559 0.5318 0.066 Uiso 1 1 calc R . . C8 C 0.3215(10) 0.113(2) 0.3701(5) 0.071(5) Uani 1 1 d . . . H8 H 0.2785 0.1091 0.3504 0.085 Uiso 1 1 calc R A . N2 N 0.4867(6) 0.3491(11) 0.5325(3) 0.038(3) Uani 1 1 d . . . N3 N 0.3398(6) 0.3301(11) 0.4849(3) 0.040(3) Uani 1 1 d . . . N4 N 0.3978(6) 0.1542(11) 0.4286(3) 0.039(3) Uani 1 1 d . . . N1 N 0.5427(6) 0.1580(10) 0.4789(3) 0.031(2) Uani 1 1 d . . . C21 C 0.5412(7) -0.0472(13) 0.3844(3) 0.032(3) Uani 1 1 d . . . C23 C 0.5353(7) -0.2429(12) 0.3377(3) 0.029(3) Uani 1 1 d . . . H23 H 0.5120 -0.3275 0.3267 0.035 Uiso 1 1 calc R . 4 C22 C 0.5090(8) -0.1772(12) 0.3694(4) 0.038(3) Uani 1 1 d . . . H22 H 0.4701 -0.2197 0.3805 0.046 Uiso 1 1 calc R . . C25 C 0.6274(9) -0.0655(16) 0.3398(4) 0.054(4) Uani 1 1 d . . . H25 H 0.6695 -0.0274 0.3306 0.064 Uiso 1 1 calc R . 4 C26 C 0.6010(10) 0.0006(15) 0.3696(4) 0.053(4) Uani 1 1 d . . . H26 H 0.6255 0.0840 0.3807 0.064 Uiso 1 1 calc R . . C28 C 0.3049(9) 0.6726(12) 0.5694(3) 0.040(3) Uani 1 1 d . . . H28 H 0.3009 0.7133 0.5440 0.048 Uiso 1 1 calc R . . C27 C 0.3429(7) 0.5462(14) 0.5779(3) 0.035(3) Uani 1 1 d . . . C30 C 0.2779(8) 0.6883(13) 0.6347(3) 0.036(3) Uani 1 1 d U . . C29 C 0.2721(7) 0.7411(11) 0.5984(3) 0.030(3) Uani 1 1 d . . . H29 H 0.2452 0.8269 0.5921 0.036 Uiso 1 1 calc R . . C31 C 0.3206(9) 0.5667(16) 0.6437(4) 0.052(3) Uani 1 1 d U . . H31 H 0.3289 0.5304 0.6697 0.063 Uiso 1 1 calc R . . C32 C 0.3503(10) 0.4998(17) 0.6152(4) 0.060(5) Uani 1 1 d . . . H32 H 0.3780 0.4152 0.6220 0.073 Uiso 1 1 calc R . . C33 C 0.2411(7) 0.7612(14) 0.6650(3) 0.031(3) Uani 1 1 d U . . O2 O 0.2041(6) 0.8691(10) 0.6563(2) 0.045(2) Uani 1 1 d . . . O1 O 0.2469(5) 0.7064(11) 0.6983(2) 0.046(2) Uani 1 1 d . . . C40 C 0.0226(8) 0.8264(12) 0.6726(4) 0.035(3) Uani 1 1 d . . . O3 O 0.0545(6) 0.7151(10) 0.6848(3) 0.047(2) Uani 1 1 d . . . O4 O 0.0479(5) 0.9488(8) 0.6820(2) 0.040(2) Uani 1 1 d . . . C42 C 0.6877(8) 0.2650(13) 0.5637(4) 0.038(3) Uani 1 1 d . . . C43 C 0.6982(10) 0.2501(19) 0.6051(4) 0.063(4) Uani 1 1 d . . . H43 H 0.6572 0.2247 0.6173 0.076 Uiso 1 1 calc R . . C41 C 0.7538(9) 0.2883(18) 0.5482(4) 0.056(4) Uani 1 1 d . . . H41 H 0.7509 0.2989 0.5206 0.067 Uiso 1 1 calc R . . C45 C 0.8300(11) 0.2966(16) 0.6124(6) 0.068(3) Uani 1 1 d U . . C44 C 0.8220(10) 0.296(2) 0.5718(6) 0.075(5) Uani 1 1 d . . . H44 H 0.8652 0.3011 0.5600 0.090 Uiso 1 1 calc R . . C46 C 0.7670(11) 0.2718(16) 0.6279(6) 0.068(3) Uani 1 1 d U . . H46 H 0.7707 0.2693 0.6557 0.082 Uiso 1 1 calc R . . C47 C 0.9072(12) 0.3058(16) 0.6359(7) 0.068(3) Uani 1 1 d U . . O6 O 0.9619(8) 0.3137(14) 0.6238(6) 0.117(6) Uani 1 1 d . . . O5 O 0.9092(10) 0.3069(15) 0.6717(6) 0.112(6) Uani 1 1 d . . . O7 O 0.0885(6) 0.8658(10) 0.7746(3) 0.047(2) Uani 1 1 d . . . O9 O 0.2153(8) 1.0469(14) 0.7385(3) 0.094(5) Uani 1 1 d D . . H9A H 0.241(14) 1.097(13) 0.725(4) 0.140 Uiso 1 1 d D B 1 H9B H 0.208(13) 1.098(13) 0.758(5) 0.140 Uiso 1 1 d D C 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 C39 0.047(8) 0.021(6) 0.090(8) -0.001(6) -0.004(6) 0.009(5) C34 0.049(7) 0.020(5) 0.081(7) -0.006(5) -0.006(5) 0.008(5) C37 0.062(8) 0.013(5) 0.075(8) 0.003(5) 0.010(6) 0.008(5) C35 0.039(7) 0.026(6) 0.067(7) 0.003(5) 0.007(6) 0.014(5) C38 0.059(8) 0.027(6) 0.052(7) 0.005(5) 0.013(6) 0.002(5) C36 0.070(12) 0.037(8) 0.057(9) -0.009(7) -0.007(7) -0.026(7) C48 0.037(9) 0.038(8) 0.033(7) -0.007(6) 0.002(6) 0.000(6) C24 0.056(9) 0.020(6) 0.028(6) 0.011(5) 0.023(6) 0.011(5) O8 0.056(7) 0.061(6) 0.039(5) 0.004(4) 0.025(5) 0.017(5) Cd1 0.0395(7) 0.0331(6) 0.0325(6) -0.0004(4) 0.0108(4) 0.0014(4) Zn2 0.0523(14) 0.0679(13) 0.0580(11) -0.0080(9) 0.0027(8) 0.0089(9) C17 0.049(10) 0.062(9) 0.020(6) 0.001(6) 0.013(6) -0.002(7) C15 0.052(10) 0.043(7) 0.032(7) 0.016(6) 0.015(6) 0.011(6) C1 0.025(8) 0.028(6) 0.026(6) 0.011(5) 0.008(5) 0.002(5) C7 0.047(11) 0.047(8) 0.053(8) -0.016(7) -0.007(7) 0.018(7) C11 0.036(9) 0.031(6) 0.034(6) 0.008(5) 0.015(5) 0.002(6) C16 0.033(8) 0.046(7) 0.020(6) 0.004(5) 0.004(5) 0.004(5) C13 0.038(9) 0.045(8) 0.042(8) 0.019(6) 0.022(6) 0.022(6) C10 0.048(10) 0.028(6) 0.044(7) 0.003(6) 0.016(6) 0.002(6) C18 0.063(12) 0.051(8) 0.035(7) -0.003(6) 0.013(6) -0.023(8) C14 0.038(9) 0.065(9) 0.038(7) 0.028(7) 0.024(6) 0.015(7) C19 0.036(9) 0.046(7) 0.023(6) 0.001(5) 0.013(5) -0.016(6) C4 0.048(11) 0.066(10) 0.076(11) -0.025(9) 0.018(8) -0.003(8) C5 0.065(12) 0.044(8) 0.052(8) -0.023(7) 0.009(8) 0.013(7) C20 0.042(10) 0.053(8) 0.023(6) -0.003(6) 0.012(5) 0.006(6) C2 0.024(8) 0.051(8) 0.041(7) 0.009(6) 0.008(5) 0.008(6) C6 0.032(9) 0.056(8) 0.049(8) -0.002(7) 0.009(6) 0.004(6) C12 0.061(10) 0.027(6) 0.034(7) 0.006(5) 0.029(6) 0.001(6) C9 0.061(12) 0.060(9) 0.035(7) -0.021(7) -0.009(6) 0.005(8) C3 0.047(11) 0.069(10) 0.053(9) -0.001(8) 0.020(7) 0.014(7) C8 0.046(12) 0.097(13) 0.059(9) -0.031(9) -0.019(7) 0.028(9) N2 0.040(8) 0.050(6) 0.028(5) 0.001(5) 0.017(5) -0.014(5) N3 0.034(7) 0.049(6) 0.036(6) -0.019(5) 0.003(5) 0.014(5) N4 0.047(8) 0.033(6) 0.038(5) -0.008(5) 0.014(5) -0.002(5) N1 0.039(7) 0.032(5) 0.025(5) 0.014(4) 0.013(4) 0.006(4) C21 0.031(8) 0.038(7) 0.031(6) 0.007(5) 0.014(5) 0.007(5) C23 0.026(7) 0.026(6) 0.038(6) 0.003(5) 0.013(5) 0.006(5) C22 0.039(8) 0.027(7) 0.053(8) 0.007(6) 0.024(6) 0.005(5) C25 0.049(10) 0.068(10) 0.050(8) -0.021(7) 0.027(7) -0.038(8) C26 0.082(12) 0.041(8) 0.044(8) -0.008(6) 0.034(8) -0.023(7) C28 0.087(11) 0.020(6) 0.016(5) 0.003(5) 0.016(6) 0.001(6) C27 0.032(8) 0.049(8) 0.025(6) 0.002(5) 0.008(5) -0.004(6) C30 0.042(6) 0.044(6) 0.026(5) 0.011(5) 0.017(4) 0.003(5) C29 0.036(8) 0.022(6) 0.030(6) 0.004(5) 0.003(5) 0.000(5) C31 0.057(8) 0.069(7) 0.033(6) 0.027(6) 0.015(5) 0.021(6) C32 0.086(13) 0.069(10) 0.037(8) 0.022(7) 0.041(8) 0.036(9) C33 0.031(6) 0.046(7) 0.022(5) 0.008(5) 0.022(5) -0.004(5) O2 0.053(6) 0.047(6) 0.040(5) 0.002(4) 0.020(4) 0.001(5) O1 0.024(6) 0.079(6) 0.041(5) 0.011(5) 0.025(4) 0.009(4) C40 0.052(9) 0.011(6) 0.045(7) -0.004(5) 0.018(6) -0.007(6) O3 0.045(6) 0.042(6) 0.048(5) -0.001(4) -0.011(4) 0.008(4) O4 0.045(6) 0.026(5) 0.049(5) 0.005(4) 0.007(4) -0.002(4) C42 0.032(9) 0.038(7) 0.043(7) -0.002(6) 0.002(6) 0.014(5) C43 0.054(12) 0.091(12) 0.039(8) -0.008(8) -0.004(7) 0.003(8) C41 0.039(10) 0.077(10) 0.049(8) 0.010(7) 0.003(7) -0.005(7) C45 0.062(7) 0.042(5) 0.088(7) -0.012(5) -0.024(5) 0.009(5) C44 0.041(12) 0.092(13) 0.088(13) 0.023(10) 0.005(9) -0.018(9) C46 0.062(7) 0.043(5) 0.088(7) -0.012(5) -0.024(5) 0.010(5) C47 0.062(7) 0.042(5) 0.088(7) -0.012(5) -0.025(5) 0.009(5) O6 0.038(9) 0.063(8) 0.25(2) 0.067(10) 0.013(10) 0.008(6) O5 0.108(14) 0.074(9) 0.130(14) -0.006(8) -0.053(10) 0.001(8) O7 0.061(7) 0.046(6) 0.042(5) 0.002(4) 0.030(4) 0.005(5) O9 0.130(12) 0.102(9) 0.072(7) -0.065(7) 0.083(8) -0.085(9) _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 C39 C34 1.36(2) . ? C39 C38 1.36(2) . ? C34 C35 1.36(2) . ? C37 C38 1.33(2) . ? C37 C36 1.44(2) . ? C35 C36 1.33(2) . ? C35 C6 1.50(2) . ? C38 C40 1.52(2) 3_566 ? C48 C24 1.497(18) 4_566 ? C48 O8 1.220(16) . ? C48 O7 1.227(16) . ? C24 C48 1.497(18) 4_665 ? C24 C23 1.370(17) . ? C24 C25 1.385(18) . ? Cd1 C33 2.738(11) . ? Cd1 O2 2.473(8) . ? Cd1 O1 2.325(8) . ? Cd1 C40 2.676(14) . ? Cd1 O3 2.359(9) . ? Cd1 O4 2.357(9) . ? Cd1 O7 2.459(8) . ? Cd1 O9 2.226(10) . ? Zn2 N2 2.066(10) . ? Zn2 N3 2.022(11) . ? Zn2 N4 2.048(10) . ? Zn2 N1 2.057(10) . ? C17 C16 1.45(2) . ? C17 C18 1.451(19) . ? C17 N2 1.354(18) . ? C15 C16 1.389(18) . ? C15 C14 1.42(2) . ? C15 N1 1.366(17) . ? C1 C20 1.366(18) . ? C1 C2 1.404(18) . ? C1 C27 1.517(17) . ? C7 C6 1.37(2) . ? C7 C8 1.43(2) . ? C7 N4 1.381(18) . ? C11 C10 1.365(19) . ? C11 C12 1.432(19) . ? C11 C21 1.491(17) . ? C16 C42 1.457(19) . ? C13 C14 1.37(2) . ? C13 C12 1.387(19) . ? C10 C9 1.47(2) . ? C10 N4 1.352(17) . ? C18 C19 1.34(2) . ? C19 C20 1.477(19) . ? C4 C5 1.42(2) . ? C4 C3 1.36(2) . ? C5 C6 1.43(2) . ? C5 N3 1.39(2) . ? C20 N2 1.390(17) . ? C2 C3 1.40(2) . ? C2 N3 1.400(16) . ? C12 N1 1.401(15) . ? C9 C8 1.35(2) . ? C21 C22 1.415(18) . ? C21 C26 1.355(19) . ? C23 C22 1.408(17) . ? C25 C26 1.36(2) . ? C28 C27 1.382(19) . ? C28 C29 1.406(17) . ? C27 C32 1.346(18) . ? C30 C29 1.334(16) . ? C30 C31 1.388(19) . ? C30 C33 1.500(18) . ? C31 C32 1.35(2) . ? C33 O2 1.227(15) . ? C33 O1 1.248(14) . ? C40 C38 1.52(2) 3_566 ? C40 O3 1.236(15) . ? C40 O4 1.260(14) . ? C42 C43 1.41(2) . ? C42 C41 1.42(2) . ? C43 C46 1.38(2) . ? C41 C44 1.37(2) . ? C45 C44 1.38(3) . ? C45 C46 1.37(3) . ? C45 C47 1.51(3) . ? C47 O6 1.15(3) . ? C47 O5 1.23(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C38 C39 C34 121.1(13) . . ? C35 C34 C39 121.3(12) . . ? C38 C37 C36 120.6(13) . . ? C34 C35 C6 121.6(12) . . ? C36 C35 C34 118.9(14) . . ? C36 C35 C6 119.5(13) . . ? C39 C38 C40 121.9(12) . 3_566 ? C37 C38 C39 118.4(15) . . ? C37 C38 C40 119.7(12) . 3_566 ? C35 C36 C37 119.6(12) . . ? O8 C48 C24 118.1(12) . 4_566 ? O8 C48 O7 123.2(12) . . ? O7 C48 C24 118.5(12) . 4_566 ? C23 C24 C48 120.5(11) . 4_665 ? C23 C24 C25 117.9(10) . . ? C25 C24 C48 121.6(12) . 4_665 ? O2 Cd1 C33 26.6(3) . . ? O2 Cd1 C40 84.8(3) . . ? O1 Cd1 C33 27.0(3) . . ? O1 Cd1 O2 53.4(3) . . ? O1 Cd1 C40 113.9(4) . . ? O1 Cd1 O3 95.4(3) . . ? O1 Cd1 O4 130.0(3) . . ? O1 Cd1 O7 139.1(3) . . ? C40 Cd1 C33 98.1(4) . . ? O3 Cd1 C33 89.9(4) . . ? O3 Cd1 O2 88.7(3) . . ? O3 Cd1 C40 27.5(3) . . ? O3 Cd1 O7 88.8(3) . . ? O4 Cd1 C33 105.9(3) . . ? O4 Cd1 O2 83.3(3) . . ? O4 Cd1 C40 28.1(3) . . ? O4 Cd1 O3 55.6(3) . . ? O4 Cd1 O7 85.0(3) . . ? O7 Cd1 C33 165.7(3) . . ? O7 Cd1 O2 167.4(3) . . ? O7 Cd1 C40 87.2(4) . . ? O9 Cd1 C33 98.5(4) . . ? O9 Cd1 O2 88.0(3) . . ? O9 Cd1 O1 103.3(4) . . ? O9 Cd1 C40 126.3(5) . . ? O9 Cd1 O3 153.8(5) . . ? O9 Cd1 O4 98.2(5) . . ? O9 Cd1 O7 88.9(3) . . ? N3 Zn2 N2 90.7(4) . . ? N3 Zn2 N4 90.2(4) . . ? N3 Zn2 N1 176.8(4) . . ? N4 Zn2 N2 178.1(4) . . ? N4 Zn2 N1 90.4(4) . . ? N1 Zn2 N2 88.9(4) . . ? C16 C17 C18 126.0(13) . . ? N2 C17 C16 124.2(12) . . ? N2 C17 C18 109.4(12) . . ? C16 C15 C14 126.2(13) . . ? N1 C15 C16 125.1(11) . . ? N1 C15 C14 108.7(12) . . ? C20 C1 C2 128.5(11) . . ? C20 C1 C27 116.0(10) . . ? C2 C1 C27 115.4(11) . . ? C6 C7 C8 125.3(13) . . ? C6 C7 N4 125.7(12) . . ? N4 C7 C8 108.9(12) . . ? C10 C11 C12 125.5(11) . . ? C10 C11 C21 118.5(11) . . ? C12 C11 C21 115.8(11) . . ? C17 C16 C42 115.6(11) . . ? C15 C16 C17 124.5(12) . . ? C15 C16 C42 119.7(11) . . ? C14 C13 C12 107.0(11) . . ? C11 C10 C9 125.0(12) . . ? N4 C10 C11 127.8(12) . . ? N4 C10 C9 107.2(13) . . ? C19 C18 C17 107.9(13) . . ? C13 C14 C15 107.8(12) . . ? C18 C19 C20 107.2(11) . . ? C3 C4 C5 108.5(15) . . ? C4 C5 C6 127.2(15) . . ? N3 C5 C4 108.6(12) . . ? N3 C5 C6 123.9(13) . . ? C1 C20 C19 127.9(11) . . ? C1 C20 N2 124.6(12) . . ? N2 C20 C19 107.4(12) . . ? C3 C2 C1 127.1(12) . . ? C3 C2 N3 110.4(12) . . ? N3 C2 C1 122.4(11) . . ? C7 C6 C35 116.9(12) . . ? C7 C6 C5 125.5(14) . . ? C5 C6 C35 117.5(12) . . ? C13 C12 C11 126.9(11) . . ? C13 C12 N1 109.9(11) . . ? N1 C12 C11 123.1(12) . . ? C8 C9 C10 107.8(12) . . ? C4 C3 C2 106.9(13) . . ? C9 C8 C7 107.0(12) . . ? C17 N2 Zn2 126.3(8) . . ? C17 N2 C20 108.1(10) . . ? C20 N2 Zn2 124.3(9) . . ? C5 N3 Zn2 127.0(8) . . ? C5 N3 C2 105.3(10) . . ? C2 N3 Zn2 126.7(8) . . ? C7 N4 Zn2 125.7(8) . . ? C10 N4 Zn2 124.8(10) . . ? C10 N4 C7 108.8(11) . . ? C15 N1 Zn2 127.0(8) . . ? C15 N1 C12 106.4(10) . . ? C12 N1 Zn2 125.7(9) . . ? C22 C21 C11 120.4(11) . . ? C26 C21 C11 122.3(11) . . ? C26 C21 C22 117.3(11) . . ? C24 C23 C22 121.3(11) . . ? C23 C22 C21 119.2(11) . . ? C26 C25 C24 121.1(12) . . ? C21 C26 C25 122.9(13) . . ? C27 C28 C29 120.0(10) . . ? C28 C27 C1 122.0(9) . . ? C32 C27 C1 121.4(12) . . ? C32 C27 C28 116.6(11) . . ? C29 C30 C31 118.0(11) . . ? C29 C30 C33 120.7(11) . . ? C31 C30 C33 121.3(10) . . ? C30 C29 C28 121.5(11) . . ? C32 C31 C30 119.8(11) . . ? C27 C32 C31 123.9(13) . . ? C30 C33 Cd1 168.3(9) . . ? O2 C33 Cd1 64.6(6) . . ? O2 C33 C30 119.9(10) . . ? O2 C33 O1 121.6(10) . . ? O1 C33 Cd1 57.7(6) . . ? O1 C33 C30 118.4(11) . . ? C33 O2 Cd1 88.8(6) . . ? C33 O1 Cd1 95.3(7) . . ? C38 C40 Cd1 179.5(9) 3_566 . ? O3 C40 C38 118.1(10) . 3_566 ? O3 C40 Cd1 61.8(7) . . ? O3 C40 O4 123.5(13) . . ? O4 C40 C38 118.3(11) . 3_566 ? O4 C40 Cd1 61.7(7) . . ? C40 O3 Cd1 90.7(8) . . ? C40 O4 Cd1 90.2(8) . . ? C43 C42 C16 122.8(13) . . ? C43 C42 C41 114.7(13) . . ? C41 C42 C16 122.6(11) . . ? C46 C43 C42 121.2(17) . . ? C44 C41 C42 121.8(14) . . ? C44 C45 C47 118.4(19) . . ? C46 C45 C44 116.2(16) . . ? C46 C45 C47 124.9(19) . . ? C41 C44 C45 122.4(17) . . ? C45 C46 C43 123.1(18) . . ? O6 C47 C45 127(2) . . ? O6 C47 O5 119(2) . . ? O5 C47 C45 114(2) . . ? C48 O7 Cd1 89.0(8) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.677 -0.743 0.177 2576.5 0.0 ? # Attachment '- Structure2.cif' data_ns47 _database_code_depnum_ccdc_archive 'CCDC 865042' #TrackingRef '- Structure2.cif' _audit_creation_date 2012-02-23 _audit_creation_method ; Olex2 1.1 (compiled 2011.11.01 svn.r2039, GUI svn.r3906) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '0.13(C768 H384 Cd16 Fe16 N64 O136), 4.75(C5 H11 N1 O1), .25(C5 H11 N1), /25(H2 O1)' _chemical_formula_sum 'C120.75 H104.75 Cd2 Fe2 N13 O23' _chemical_formula_weight 2442.43 _chemical_melting_point ? 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _space_group_crystal_system tetragonal _space_group_IT_number 88 _space_group_name_H-M_alt 'I 41/a' _space_group_name_Hall '-I 4ad' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x+1/2, -y, z+1/2' 3 '-y+3/4, x+1/4, z+1/4' 4 'y+3/4, -x+3/4, z+3/4' 5 'x+1/2, y+1/2, z+1/2' 6 '-x+1, -y+1/2, z+1' 7 '-y+5/4, x+3/4, z+3/4' 8 'y+5/4, -x+5/4, z+5/4' 9 '-x, -y, -z' 10 'x-1/2, y, -z-1/2' 11 'y-3/4, -x-1/4, -z-1/4' 12 '-y-3/4, x-3/4, -z-3/4' 13 '-x+1/2, -y+1/2, -z+1/2' 14 'x, y+1/2, -z' 15 'y-1/4, -x+1/4, -z+1/4' 16 '-y-1/4, x-1/4, -z-1/4' _cell_length_a 18.967(2) _cell_length_b 18.967(2) _cell_length_c 61.245(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22032(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 8863 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 17.474 _cell_measurement_theta_min 2.248 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.498659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2004/1 (Bruker,2004) was used for absorption correction. R(int) was 0.1032 before and 0.0648 after correction. The Ratio of minimum to maximum transmission is 0.4987. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description plates _exptl_crystal_F_000 10018 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.1135 _diffrn_reflns_av_unetI/netI 0.0352 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_number 105508 _diffrn_reflns_theta_full 18.85 _diffrn_reflns_theta_max 18.85 _diffrn_reflns_theta_min 1.12 _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX II CCd' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'MO K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3662 _reflns_number_total 4335 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SAINT' _computing_data_reduction 'SAINT v7.34A (Bruker, 200?)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 4.718 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.171 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 2.504 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 528 _refine_ls_number_reflns 4335 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1328 _refine_ls_R_factor_gt 0.1182 _refine_ls_restrained_S_all 2.513 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+98.2410P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3031 _refine_ls_wR_factor_ref 0.3087 _refine_special_details ; 'CHEMW03_2_A Alert-added in atoms found using SQUEEZE' 'PLAT043_ALERT_1_A-added atoms found using SQUEEZE' 'PLAT241_ALERT_2_A-Oxygen atom is near heavy atom, Cd' 'PLAT602_ALERT-A_2-Large void typical of MOFs, treated with SQUEEZE' 'PLAT971_ALERT_3_A-Large positive residual near Cd caused by crystal disorder' 'the following constraints were used to better model disorder, EDAP, ISOR, and HFIX to determine Hydrogen atoms' 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 0.181 0.637 0.152 7457 2281 '38[HCON(C2H5)2],2(C2H5)2NH, 4H2O' ' 2 0.000 0.250 0.125 30 0 ' ' 3 0.000 0.750 0.875 30 0 ' ' 4 0.500 0.250 0.375 30 0 ' ' 5 0.500 0.750 0.625 30 0 ' ' _platon_squeeze_details 'SQUEEZE was performed using PLATON to account for disordered solvent molecules and counter cations. The electron density found in each cavity correlates to a final count of 38 molecules of HCON(C2H5)2, 7 H2Os, and 2 (C2H5)2NH+' 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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 -0.1145(17) 0.6654(13) 0.0383(4) 0.093(3) Uani 1 1 d . . . C2 C -0.0462(10) 0.6369(9) 0.0370(3) 0.040(5) Uani 1 1 d . . . C3 C -0.0030(12) 0.6217(11) 0.0554(3) 0.054(6) Uani 1 1 d . . . H3 H -0.0141 0.6293 0.0704 0.065 Uiso 1 1 calc R . . C4 C 0.0563(12) 0.5944(10) 0.0472(3) 0.049(5) Uani 1 1 d . . . H4 H 0.0956 0.5784 0.0555 0.059 Uiso 1 1 calc R . . C5 C 0.0503(11) 0.5937(9) 0.0240(3) 0.032(5) Uani 1 1 d . . . C6 C 0.1005(10) 0.5669(9) 0.0095(3) 0.041(5) Uani 1 1 d . . . C7 C 0.0929(11) 0.5632(9) -0.0134(3) 0.039(5) Uani 1 1 d . . . C8 C 0.1372(10) 0.5268(9) -0.0280(4) 0.044(5) Uani 1 1 d . . . H8 H 0.1766 0.4986 -0.0241 0.053 Uiso 1 1 calc R . . C9 C 0.1149(11) 0.5385(10) -0.0484(3) 0.046(6) Uani 1 1 d . . . H9 H 0.1353 0.5209 -0.0614 0.055 Uiso 1 1 calc R . . C10 C 0.0524(9) 0.5840(8) -0.0465(3) 0.032(5) Uani 1 1 d . . . C11 C 0.0154(10) 0.6084(9) -0.0646(3) 0.034(5) Uani 1 1 d D . . C12 C -0.0453(10) 0.6464(9) -0.0630(3) 0.030(4) Uani 1 1 d . . . C13 C -0.0868(12) 0.6731(10) -0.0808(3) 0.049(5) Uani 1 1 d . . . H13 H -0.0752 0.6692 -0.0958 0.058 Uiso 1 1 calc R . . C14 C -0.1439(10) 0.7041(10) -0.0728(3) 0.040(5) Uani 1 1 d . . . H14 H -0.1803 0.7260 -0.0810 0.048 Uiso 1 1 calc R . . C15 C -0.1403(10) 0.6984(9) -0.0492(3) 0.033(5) Uani 1 1 d . . . C16 C -0.1927(10) 0.7194(9) -0.0351(3) 0.038(5) Uani 1 1 d . . . C17 C -0.1946(10) 0.7093(10) -0.0128(4) 0.045(5) Uani 1 1 d . . . C18 C -0.2467(10) 0.7306(10) 0.0021(3) 0.048(5) Uani 1 1 d . . . H18 H -0.2903 0.7521 -0.0017 0.057 Uiso 1 1 calc R . . C19 C -0.2260(10) 0.7163(9) 0.0221(4) 0.046(5) Uani 1 1 d . . . H19 H -0.2515 0.7248 0.0352 0.056 Uiso 1 1 calc R . . C20 C -0.1583(10) 0.6856(10) 0.0202(3) 0.042(5) Uani 1 1 d . . . C21 C -0.1414(15) 0.6789(13) 0.0610(4) 0.093(3) Uani 1 1 d . . . C22 C -0.1785(14) 0.6285(13) 0.0715(3) 0.093(3) Uani 1 1 d . . . H22 H -0.1897 0.5863 0.0639 0.111 Uiso 1 1 calc R . . C23 C -0.2011(14) 0.6360(13) 0.0931(3) 0.093(3) Uani 1 1 d . . . H23 H -0.2271 0.6001 0.1003 0.111 Uiso 1 1 calc R . . C24 C -0.1834(15) 0.6988(13) 0.1035(4) 0.093(3) Uani 1 1 d . . . C25 C -0.1581(14) 0.7512(13) 0.0918(4) 0.093(3) Uani 1 1 d . . . H25 H -0.1565 0.7976 0.0976 0.111 Uiso 1 1 calc R . . C26 C -0.1345(14) 0.7380(13) 0.0713(3) 0.093(3) Uani 1 1 d . . . H26 H -0.1108 0.7752 0.0640 0.111 Uiso 1 1 calc R . . C27 C 0.4555(18) 0.4526(14) 0.1206(5) 0.090(9) Uani 1 1 d . . . C28 C 0.1692(11) 0.5420(10) 0.0187(3) 0.047(5) Uani 1 1 d . . . C29 C 0.1700(11) 0.4839(9) 0.0337(3) 0.044(5) Uani 1 1 d . . . H29 H 0.1280 0.4587 0.0369 0.052 Uiso 1 1 calc R . . C30 C 0.2320(12) 0.4657(10) 0.0432(3) 0.051(5) Uani 1 1 d . . . H30 H 0.2330 0.4278 0.0533 0.062 Uiso 1 1 calc R . . C31 C 0.2944(11) 0.5016(11) 0.0383(3) 0.054(6) Uani 1 1 d . . . C32 C 0.2931(12) 0.5541(12) 0.0231(3) 0.068(6) Uani 1 1 d U . . H32 H 0.3360 0.5765 0.0192 0.081 Uiso 1 1 calc R . . C33 C 0.2314(11) 0.5758(11) 0.0132(4) 0.065(6) Uani 1 1 d . . . H33 H 0.2316 0.6130 0.0028 0.078 Uiso 1 1 calc R . . C34 C 0.3602(12) 0.4828(13) 0.0513(4) 0.072(7) Uani 1 1 d . . . C35 C -0.2542(9) 0.7614(12) -0.0437(3) 0.040(5) Uani 1 1 d . . . C36 C -0.3195(12) 0.7270(11) -0.0473(3) 0.056(6) Uani 1 1 d . . . H36 H -0.3244 0.6777 -0.0452 0.067 Uiso 1 1 calc R . . C37 C -0.3761(10) 0.7678(12) -0.0542(3) 0.051(6) Uani 1 1 d . . . H37 H -0.4206 0.7464 -0.0568 0.061 Uiso 1 1 calc R . . C38 C -0.3679(12) 0.8385(11) -0.0572(3) 0.045(5) Uani 1 1 d . . . C39 C -0.3026(12) 0.8717(11) -0.0539(3) 0.051(5) Uani 1 1 d . . . H39 H -0.2971 0.9208 -0.0564 0.061 Uiso 1 1 calc R . . C40 C -0.2478(10) 0.8320(12) -0.0471(3) 0.047(5) Uani 1 1 d . . . H40 H -0.2035 0.8540 -0.0446 0.056 Uiso 1 1 calc R . . C41 C 0.5674(13) 0.3837(14) 0.0638(3) 0.057(6) Uani 1 1 d . . . C42 C 0.0475(12) 0.5907(10) -0.0867(3) 0.049(5) Uani 1 1 d D . . C43 C 0.1126(12) 0.6176(11) -0.0926(4) 0.060(6) Uani 1 1 d . . . H43 H 0.1346 0.6514 -0.0834 0.072 Uiso 1 1 calc R . . C44 C 0.1458(11) 0.5968(12) -0.1112(4) 0.061(6) Uani 1 1 d . . . H44 H 0.1892 0.6179 -0.1153 0.074 Uiso 1 1 calc R . . C45 C 0.1164(13) 0.5450(12) -0.1240(3) 0.058(6) Uani 1 1 d . . . C46 C 0.0496(14) 0.5215(11) -0.1193(3) 0.064(6) Uani 1 1 d . . . H46 H 0.0271 0.4898 -0.1291 0.076 Uiso 1 1 calc R . . C47 C 0.0136(11) 0.5430(11) -0.1003(4) 0.059(6) Uani 1 1 d . . . H47 H -0.0321 0.5255 -0.0970 0.071 Uiso 1 1 calc R . . C48 C 0.1573(16) 0.5164(14) -0.1434(3) 0.065(7) Uani 1 1 d . . . Cd1 Cd 0.47234(8) 0.47938(8) 0.07834(2) 0.0564(7) Uani 1 1 d . . . Fe1 Fe -0.03684(14) 0.66462(14) -0.01236(4) 0.0450(9) Uani 1 1 d . . . N1 N -0.1378(8) 0.6801(7) -0.0008(2) 0.039(4) Uani 1 1 d . . . N2 N -0.0133(8) 0.6212(7) 0.0180(2) 0.037(4) Uani 1 1 d . . . N3 N 0.0395(8) 0.5974(7) -0.0251(3) 0.033(4) Uani 1 1 d . . . N4 N -0.0802(8) 0.6639(7) -0.0437(2) 0.037(4) Uani 1 1 d . . . O1 O 0.4118(14) 0.4888(16) 0.1131(4) 0.159(9) Uani 1 1 d U . . O2 O 0.5117(15) 0.4470(13) 0.1138(3) 0.145(9) Uani 1 1 d U . . O3 O 0.3581(7) 0.4467(7) 0.0677(2) 0.055(4) Uani 1 1 d . . . O4 O 0.4159(9) 0.5095(11) 0.0443(3) 0.129(8) Uani 1 1 d . . . O5 O 0.5127(8) 0.3543(8) 0.0704(2) 0.060(4) Uani 1 1 d . . . O6 O 0.5745(7) 0.4490(10) 0.0625(2) 0.068(4) Uani 1 1 d . . . O7 O 0.0000 0.7500 -0.0109(2) 0.038(4) Uani 1 2 d S . . O8 O 0.1251(8) 0.4664(8) -0.1541(2) 0.066(4) Uani 1 1 d . . . O9 O 0.2140(10) 0.5377(9) -0.1479(3) 0.086(5) Uani 1 1 d U . . 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 0.146(9) 0.085(8) 0.047(6) -0.007(5) 0.043(6) -0.004(7) C2 0.033(12) 0.045(12) 0.042(15) -0.008(10) 0.006(13) -0.001(10) C3 0.073(16) 0.073(15) 0.016(12) -0.012(10) -0.001(13) 0.019(13) C4 0.062(16) 0.050(13) 0.035(16) 0.002(10) -0.007(12) -0.003(12) C5 0.040(14) 0.038(11) 0.018(14) 0.009(9) -0.001(11) -0.009(10) C6 0.035(13) 0.033(12) 0.054(17) 0.016(11) 0.000(13) 0.010(10) C7 0.059(14) 0.034(12) 0.026(14) 0.017(11) -0.006(13) -0.009(11) C8 0.041(12) 0.041(12) 0.051(16) 0.004(11) 0.017(13) 0.016(10) C9 0.069(16) 0.055(14) 0.013(13) -0.003(10) -0.002(11) -0.015(13) C10 0.036(13) 0.018(11) 0.042(17) 0.004(10) -0.010(11) 0.007(9) C11 0.042(13) 0.039(12) 0.020(13) -0.006(10) -0.002(12) 0.004(11) C12 0.036(13) 0.028(11) 0.024(13) 0.002(10) -0.002(12) -0.004(10) C13 0.064(16) 0.057(14) 0.024(13) -0.007(11) -0.002(13) 0.007(12) C14 0.031(12) 0.059(13) 0.029(15) 0.002(10) -0.003(10) 0.004(11) C15 0.036(14) 0.033(11) 0.031(15) -0.007(9) -0.006(12) 0.003(10) C16 0.049(15) 0.048(13) 0.018(14) 0.003(10) -0.007(12) -0.004(11) C17 0.027(13) 0.057(13) 0.051(18) -0.006(11) -0.016(13) 0.000(10) C18 0.039(13) 0.075(15) 0.029(14) 0.002(11) 0.014(12) 0.013(11) C19 0.041(15) 0.055(13) 0.043(16) 0.003(11) -0.001(11) 0.016(11) C20 0.054(15) 0.056(13) 0.017(14) 0.009(9) -0.002(11) 0.001(11) C21 0.146(9) 0.085(8) 0.047(6) -0.007(5) 0.043(6) -0.004(7) C22 0.146(9) 0.085(8) 0.047(6) -0.007(5) 0.043(6) -0.004(7) C23 0.146(9) 0.085(8) 0.047(6) -0.007(5) 0.043(6) -0.004(7) C24 0.146(9) 0.085(8) 0.047(6) -0.007(5) 0.043(6) -0.004(7) C25 0.146(9) 0.085(8) 0.047(6) -0.007(5) 0.043(6) -0.004(7) C26 0.146(9) 0.085(8) 0.047(6) -0.007(5) 0.043(6) -0.004(7) C27 0.10(2) 0.067(18) 0.11(2) 0.049(17) 0.02(2) -0.020(17) C28 0.065(17) 0.036(13) 0.041(13) 0.007(11) -0.014(12) 0.015(12) C29 0.051(15) 0.040(13) 0.040(12) 0.004(11) -0.002(11) -0.004(10) C30 0.059(16) 0.058(14) 0.038(13) 0.012(10) -0.008(12) 0.012(13) C31 0.040(15) 0.072(15) 0.051(14) 0.027(12) 0.007(12) 0.009(13) C32 0.063(14) 0.082(14) 0.059(12) 0.042(12) -0.002(11) -0.006(11) C33 0.038(14) 0.076(16) 0.082(17) 0.034(13) -0.004(13) -0.007(13) C34 0.029(15) 0.100(19) 0.09(2) 0.048(16) 0.023(15) 0.015(13) C35 0.020(13) 0.073(18) 0.026(11) -0.009(11) -0.009(9) 0.008(12) C36 0.052(16) 0.058(14) 0.058(14) 0.008(11) -0.010(12) 0.019(15) C37 0.027(13) 0.067(18) 0.060(14) 0.009(12) 0.000(10) -0.002(12) C38 0.068(19) 0.040(15) 0.026(11) 0.001(10) 0.006(10) 0.015(14) C39 0.041(14) 0.059(14) 0.052(14) 0.018(11) -0.009(11) -0.008(15) C40 0.040(15) 0.044(16) 0.056(14) 0.004(11) -0.006(11) -0.004(12) C41 0.06(2) 0.055(18) 0.054(15) -0.004(13) -0.008(13) 0.006(16) C42 0.066(16) 0.045(13) 0.035(14) 0.008(12) 0.001(13) 0.022(12) C43 0.068(17) 0.063(15) 0.049(16) -0.007(12) 0.020(13) -0.014(13) C44 0.071(16) 0.074(16) 0.039(14) -0.011(13) 0.019(14) -0.021(14) C45 0.062(17) 0.071(17) 0.042(15) 0.016(14) -0.004(14) 0.007(14) C46 0.09(2) 0.068(16) 0.032(15) -0.022(12) -0.004(13) -0.013(15) C47 0.070(15) 0.056(14) 0.052(15) -0.022(12) 0.010(13) -0.017(12) C48 0.09(2) 0.08(2) 0.025(15) 0.008(14) 0.017(15) 0.015(17) Cd1 0.0568(12) 0.0772(13) 0.0352(10) 0.0133(8) 0.0069(8) 0.0250(9) Fe1 0.0500(19) 0.0509(19) 0.0341(18) -0.0004(14) -0.0007(14) 0.0018(14) N1 0.043(11) 0.049(10) 0.025(11) 0.005(8) 0.015(9) -0.001(8) N2 0.037(11) 0.038(9) 0.037(11) -0.001(8) 0.003(9) 0.009(8) N3 0.053(11) 0.020(8) 0.025(11) 0.001(8) 0.008(9) -0.007(8) N4 0.040(11) 0.047(10) 0.024(10) 0.003(8) 0.000(9) 0.001(9) O1 0.148(16) 0.218(18) 0.111(14) 0.058(14) -0.010(12) -0.018(14) O2 0.189(17) 0.161(16) 0.087(13) 0.039(11) 0.028(13) 0.057(14) O3 0.059(10) 0.073(10) 0.031(8) 0.019(8) 0.002(7) 0.014(8) O4 0.045(11) 0.19(2) 0.156(18) 0.126(16) -0.008(11) 0.005(12) O5 0.041(9) 0.068(10) 0.072(10) -0.001(8) 0.003(8) 0.010(8) O6 0.054(10) 0.083(13) 0.067(11) 0.008(9) 0.018(7) 0.020(9) O7 0.042(10) 0.033(10) 0.038(10) 0.000 0.000 0.000(8) O8 0.091(12) 0.059(10) 0.048(9) -0.008(8) 0.016(8) 0.002(9) O9 0.088(12) 0.105(13) 0.067(11) -0.016(9) 0.041(10) -0.016(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.41(3) . ? C1 C20 1.44(3) . ? C1 C21 1.51(3) . ? C2 C3 1.42(2) . ? C2 N2 1.35(2) . ? C3 H3 0.9500 . ? C3 C4 1.34(2) . ? C4 H4 0.9500 . ? C4 C5 1.43(2) . ? C5 C6 1.40(2) . ? C5 N2 1.36(2) . ? C6 C7 1.41(2) . ? C6 C28 1.50(2) . ? C7 C8 1.41(2) . ? C7 N3 1.40(2) . ? C8 H8 0.9500 . ? C8 C9 1.33(2) . ? C9 H9 0.9500 . ? C9 C10 1.47(2) . ? C10 C11 1.39(2) . ? C10 N3 1.36(2) . ? C11 C12 1.36(2) . ? C11 C42 1.524(16) . ? C12 C13 1.44(2) . ? C12 N4 1.39(2) . ? C13 H13 0.9500 . ? C13 C14 1.33(2) . ? C14 H14 0.9500 . ? C14 C15 1.45(2) . ? C15 C16 1.38(2) . ? C15 N4 1.36(2) . ? C16 C17 1.38(3) . ? C16 C35 1.51(2) . ? C17 C18 1.40(3) . ? C17 N1 1.41(2) . ? C18 H18 0.9500 . ? C18 C19 1.31(2) . ? C19 H19 0.9500 . ? C19 C20 1.41(2) . ? C20 N1 1.35(2) . ? C21 C22 1.35(3) . ? C21 C26 1.29(3) . ? C22 H22 0.9500 . ? C22 C23 1.40(3) . ? C23 H23 0.9500 . ? C23 C24 1.39(3) . ? C24 C25 1.32(3) . ? C24 C27 1.63(4) 12_666 ? C25 H25 0.9500 . ? C25 C26 1.35(3) . ? C26 H26 0.9500 . ? C27 C24 1.63(4) 15 ? C27 Cd1 2.66(3) . ? C27 O1 1.17(3) . ? C27 O2 1.15(3) . ? C28 C29 1.44(2) . ? C28 C33 1.38(3) . ? C29 H29 0.9500 . ? C29 C30 1.35(2) . ? C30 H30 0.9500 . ? C30 C31 1.40(3) . ? C31 C32 1.36(3) . ? C31 C34 1.52(3) . ? C32 H32 0.9500 . ? C32 C33 1.38(3) . ? C33 H33 0.9500 . ? C34 O3 1.22(2) . ? C34 O4 1.25(2) . ? C35 C36 1.42(2) . ? C35 C40 1.36(2) . ? C36 H36 0.9500 . ? C36 C37 1.39(3) . ? C37 H37 0.9500 . ? C37 C38 1.36(2) . ? C38 C39 1.40(3) . ? C38 C41 1.55(3) 14_455 ? C39 H39 0.9500 . ? C39 C40 1.35(2) . ? C40 H40 0.9500 . ? C41 C38 1.55(3) 14_645 ? C41 O5 1.24(2) . ? C41 O6 1.25(2) . ? C42 C43 1.38(3) . ? C42 C47 1.39(3) . ? C43 H43 0.9500 . ? C43 C44 1.36(3) . ? C44 H44 0.9500 . ? C44 C45 1.38(3) . ? C45 C46 1.38(3) . ? C45 C48 1.52(3) . ? C46 H46 0.9500 . ? C46 C47 1.41(3) . ? C47 H47 0.9500 . ? C48 O8 1.31(3) . ? C48 O9 1.18(3) . ? Cd1 O1 2.42(2) . ? Cd1 O2 2.37(2) . ? Cd1 O3 2.346(13) . ? Cd1 O4 2.411(16) . ? Cd1 O5 2.540(13) . ? Cd1 O6 2.244(12) . ? Fe1 N1 2.063(14) . ? Fe1 N2 2.084(14) . ? Fe1 N3 2.082(14) . ? Fe1 N4 2.088(14) . ? Fe1 O7 1.766(3) . ? O7 Fe1 1.766(3) 6_464 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C20 126.3(19) . . ? C2 C1 C21 115(2) . . ? C20 C1 C21 118(3) . . ? C1 C2 C3 124(2) . . ? N2 C2 C1 124.0(19) . . ? N2 C2 C3 111.7(16) . . ? C2 C3 H3 127.3 . . ? C4 C3 C2 105.4(16) . . ? C4 C3 H3 127.3 . . ? C3 C4 H4 126.0 . . ? C3 C4 C5 108.1(18) . . ? C5 C4 H4 126.0 . . ? C6 C5 C4 126(2) . . ? N2 C5 C4 109.5(17) . . ? N2 C5 C6 124.9(16) . . ? C5 C6 C7 125.4(17) . . ? C5 C6 C28 118.0(18) . . ? C7 C6 C28 116.6(18) . . ? C6 C7 C8 126.6(19) . . ? N3 C7 C6 124.1(18) . . ? N3 C7 C8 109.2(16) . . ? C7 C8 H8 125.5 . . ? C9 C8 C7 109.0(17) . . ? C9 C8 H8 125.5 . . ? C8 C9 H9 126.9 . . ? C8 C9 C10 106.3(16) . . ? C10 C9 H9 126.9 . . ? C11 C10 C9 122.7(19) . . ? N3 C10 C9 109.3(15) . . ? N3 C10 C11 128.1(17) . . ? C10 C11 C42 115.8(17) . . ? C12 C11 C10 123.0(15) . . ? C12 C11 C42 121.2(16) . . ? C11 C12 C13 126.5(18) . . ? C11 C12 N4 126.1(16) . . ? N4 C12 C13 107.3(16) . . ? C12 C13 H13 125.5 . . ? C14 C13 C12 109.0(16) . . ? C14 C13 H13 125.5 . . ? C13 C14 H14 126.4 . . ? C13 C14 C15 107.2(16) . . ? C15 C14 H14 126.4 . . ? C16 C15 C14 124.8(18) . . ? N4 C15 C14 108.9(16) . . ? N4 C15 C16 126.1(17) . . ? C15 C16 C17 127.0(18) . . ? C15 C16 C35 119.5(17) . . ? C17 C16 C35 113.5(17) . . ? C16 C17 C18 128.5(19) . . ? C16 C17 N1 123.0(18) . . ? C18 C17 N1 108.2(17) . . ? C17 C18 H18 125.2 . . ? C19 C18 C17 109.6(18) . . ? C19 C18 H18 125.2 . . ? C18 C19 H19 126.7 . . ? C18 C19 C20 106.5(17) . . ? C20 C19 H19 126.7 . . ? C19 C20 C1 125(2) . . ? N1 C20 C1 123.3(19) . . ? N1 C20 C19 111.5(15) . . ? C22 C21 C1 120(2) . . ? C26 C21 C1 124(2) . . ? C26 C21 C22 116(2) . . ? C21 C22 H22 118.8 . . ? C21 C22 C23 122(2) . . ? C23 C22 H22 118.8 . . ? C22 C23 H23 121.7 . . ? C24 C23 C22 117(2) . . ? C24 C23 H23 121.7 . . ? C23 C24 C27 117(2) . 12_666 ? C25 C24 C23 119(2) . . ? C25 C24 C27 124(2) . 12_666 ? C24 C25 H25 120.5 . . ? C24 C25 C26 119(2) . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 125(2) . . ? C21 C26 H26 117.3 . . ? C25 C26 H26 117.3 . . ? C24 C27 Cd1 177(2) 15 . ? O1 C27 C24 117(3) . 15 ? O1 C27 Cd1 65.8(19) . . ? O2 C27 C24 114(3) . 15 ? O2 C27 Cd1 63.3(18) . . ? O2 C27 O1 124(3) . . ? C29 C28 C6 119.6(19) . . ? C33 C28 C6 120.3(17) . . ? C33 C28 C29 120.2(18) . . ? C28 C29 H29 120.7 . . ? C30 C29 C28 118.6(18) . . ? C30 C29 H29 120.7 . . ? C29 C30 H30 119.3 . . ? C29 C30 C31 121.3(18) . . ? C31 C30 H30 119.3 . . ? C30 C31 C34 118.1(19) . . ? C32 C31 C30 118.9(19) . . ? C32 C31 C34 123(2) . . ? C31 C32 H32 118.8 . . ? C31 C32 C33 122(2) . . ? C33 C32 H32 118.8 . . ? C28 C33 H33 120.8 . . ? C32 C33 C28 118.4(19) . . ? C32 C33 H33 120.8 . . ? O3 C34 C31 122(2) . . ? O3 C34 O4 123(2) . . ? O4 C34 C31 115(2) . . ? C36 C35 C16 119.3(19) . . ? C40 C35 C16 120.3(18) . . ? C40 C35 C36 120.4(17) . . ? C35 C36 H36 121.1 . . ? C37 C36 C35 117.8(19) . . ? C37 C36 H36 121.1 . . ? C36 C37 H37 119.9 . . ? C38 C37 C36 120.1(19) . . ? C38 C37 H37 119.9 . . ? C37 C38 C39 121.5(18) . . ? C37 C38 C41 119(2) . 14_455 ? C39 C38 C41 119(2) . 14_455 ? C38 C39 H39 120.8 . . ? C40 C39 C38 118.4(18) . . ? C40 C39 H39 120.8 . . ? C35 C40 H40 119.1 . . ? C39 C40 C35 121.8(18) . . ? C39 C40 H40 119.1 . . ? O5 C41 C38 120(2) . 14_645 ? O5 C41 O6 124(2) . . ? O6 C41 C38 116(2) . 14_645 ? C43 C42 C11 120.4(19) . . ? C43 C42 C47 119.8(17) . . ? C47 C42 C11 119.5(19) . . ? C42 C43 H43 119.2 . . ? C44 C43 C42 121.7(19) . . ? C44 C43 H43 119.2 . . ? C43 C44 H44 120.1 . . ? C43 C44 C45 120(2) . . ? C45 C44 H44 120.1 . . ? C44 C45 C48 120(2) . . ? C46 C45 C44 119(2) . . ? C46 C45 C48 121(2) . . ? C45 C46 H46 119.1 . . ? C45 C46 C47 121.8(19) . . ? C47 C46 H46 119.1 . . ? C42 C47 C46 117.4(18) . . ? C42 C47 H47 121.3 . . ? C46 C47 H47 121.3 . . ? O8 C48 C45 114(2) . . ? O9 C48 C45 122(3) . . ? O9 C48 O8 124(2) . . ? O1 Cd1 C27 26.1(7) . . ? O1 Cd1 O5 112.4(8) . . ? O2 Cd1 C27 25.6(7) . . ? O2 Cd1 O1 50.7(8) . . ? O2 Cd1 O4 172.0(8) . . ? O2 Cd1 O5 80.8(6) . . ? O3 Cd1 C27 96.2(8) . . ? O3 Cd1 O1 79.9(7) . . ? O3 Cd1 O2 118.3(8) . . ? O3 Cd1 O4 54.1(5) . . ? O3 Cd1 O5 88.8(5) . . ? O4 Cd1 C27 146.5(9) . . ? O4 Cd1 O1 122.1(8) . . ? O4 Cd1 O5 100.8(6) . . ? O5 Cd1 C27 92.6(8) . . ? O6 Cd1 C27 118.5(9) . . ? O6 Cd1 O1 143.9(7) . . ? O6 Cd1 O2 93.3(7) . . ? O6 Cd1 O3 127.6(5) . . ? O6 Cd1 O4 94.0(6) . . ? O6 Cd1 O5 54.3(5) . . ? N1 Fe1 N2 87.1(6) . . ? N1 Fe1 N3 149.5(5) . . ? N1 Fe1 N4 87.1(6) . . ? N2 Fe1 N4 154.5(5) . . ? N3 Fe1 N2 86.8(6) . . ? N3 Fe1 N4 85.7(7) . . ? O7 Fe1 N1 102.7(4) . . ? O7 Fe1 N2 103.5(6) . . ? O7 Fe1 N3 107.8(4) . . ? O7 Fe1 N4 102.0(6) . . ? C17 N1 Fe1 125.9(12) . . ? C20 N1 C17 104.2(15) . . ? C20 N1 Fe1 127.1(13) . . ? C2 N2 C5 105.3(14) . . ? C2 N2 Fe1 125.6(13) . . ? C5 N2 Fe1 125.4(12) . . ? C7 N3 Fe1 126.4(13) . . ? C10 N3 C7 106.2(14) . . ? C10 N3 Fe1 127.0(13) . . ? C12 N4 Fe1 126.3(12) . . ? C15 N4 C12 107.7(14) . . ? C15 N4 Fe1 123.8(12) . . ? C27 O1 Cd1 88(2) . . ? C27 O2 Cd1 91(2) . . ? C34 O3 Cd1 92.8(13) . . ? C34 O4 Cd1 89.0(14) . . ? C41 O5 Cd1 84.0(13) . . ? C41 O6 Cd1 97.6(13) . . ? Fe1 O7 Fe1 174.3(10) . 6_464 ? 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 C1 C2 C3 C4 178.8(19) . . . . ? C1 C2 N2 C5 -178.6(18) . . . . ? C1 C2 N2 Fe1 22(3) . . . . ? C1 C20 N1 C17 -176.7(19) . . . . ? C1 C20 N1 Fe1 -15(3) . . . . ? C1 C21 C22 C23 176(3) . . . . ? C1 C21 C26 C25 -180(3) . . . . ? C2 C1 C20 C19 -178(2) . . . . ? C2 C1 C20 N1 -1(3) . . . . ? C2 C1 C21 C22 -92(3) . . . . ? C2 C1 C21 C26 92(3) . . . . ? C2 C3 C4 C5 1(2) . . . . ? C3 C2 N2 C5 1.8(19) . . . . ? C3 C2 N2 Fe1 -157.1(13) . . . . ? C3 C4 C5 C6 -177.7(17) . . . . ? C3 C4 C5 N2 0(2) . . . . ? C4 C5 C6 C7 176.7(17) . . . . ? C4 C5 C6 C28 -5(3) . . . . ? C4 C5 N2 C2 -1.3(18) . . . . ? C4 C5 N2 Fe1 157.6(11) . . . . ? C5 C6 C7 C8 -169.3(17) . . . . ? C5 C6 C7 N3 12(3) . . . . ? C5 C6 C28 C29 63(2) . . . . ? C5 C6 C28 C33 -116(2) . . . . ? C6 C5 N2 C2 176.7(16) . . . . ? C6 C5 N2 Fe1 -24(2) . . . . ? C6 C7 C8 C9 -177.0(17) . . . . ? C6 C7 N3 C10 176.8(16) . . . . ? C6 C7 N3 Fe1 3(2) . . . . ? C6 C28 C29 C30 -174.8(17) . . . . ? C6 C28 C33 C32 175.8(19) . . . . ? C7 C6 C28 C29 -119.0(18) . . . . ? C7 C6 C28 C33 63(2) . . . . ? C7 C8 C9 C10 -0.8(19) . . . . ? C8 C7 N3 C10 -1.9(18) . . . . ? C8 C7 N3 Fe1 -175.4(11) . . . . ? C8 C9 C10 C11 178.8(16) . . . . ? C8 C9 C10 N3 -0.5(19) . . . . ? C9 C10 C11 C12 175.2(15) . . . . ? C9 C10 C11 C42 -6(2) . . . . ? C9 C10 N3 C7 1.5(17) . . . . ? C9 C10 N3 Fe1 174.9(10) . . . . ? C10 C11 C12 C13 -179.7(16) . . . . ? C10 C11 C12 N4 -3(3) . . . . ? C10 C11 C42 C43 -64(2) . . . . ? C10 C11 C42 C47 111(2) . . . . ? C11 C10 N3 C7 -177.8(16) . . . . ? C11 C10 N3 Fe1 -4(2) . . . . ? C11 C12 C13 C14 176.7(16) . . . . ? C11 C12 N4 C15 -176.6(16) . . . . ? C11 C12 N4 Fe1 20(2) . . . . ? C11 C42 C43 C44 172.8(18) . . . . ? C11 C42 C47 C46 -171.9(17) . . . . ? C12 C11 C42 C43 115(2) . . . . ? C12 C11 C42 C47 -70(2) . . . . ? C12 C13 C14 C15 0(2) . . . . ? C13 C12 N4 C15 0.9(17) . . . . ? C13 C12 N4 Fe1 -162.7(11) . . . . ? C13 C14 C15 C16 -174.7(17) . . . . ? C13 C14 C15 N4 0.2(19) . . . . ? C14 C15 C16 C17 173.6(17) . . . . ? C14 C15 C16 C35 -10(3) . . . . ? C14 C15 N4 C12 -0.7(17) . . . . ? C14 C15 N4 Fe1 163.4(11) . . . . ? C15 C16 C17 C18 179.3(18) . . . . ? C15 C16 C17 N1 6(3) . . . . ? C15 C16 C35 C36 102(2) . . . . ? C15 C16 C35 C40 -81(2) . . . . ? C16 C15 N4 C12 174.1(16) . . . . ? C16 C15 N4 Fe1 -22(2) . . . . ? C16 C17 C18 C19 -174.6(18) . . . . ? C16 C17 N1 C20 174.4(17) . . . . ? C16 C17 N1 Fe1 12(2) . . . . ? C16 C35 C36 C37 176.7(17) . . . . ? C16 C35 C40 C39 -177.2(17) . . . . ? C17 C16 C35 C36 -81(2) . . . . ? C17 C16 C35 C40 96(2) . . . . ? C17 C18 C19 C20 1(2) . . . . ? C18 C17 N1 C20 -0.3(18) . . . . ? C18 C17 N1 Fe1 -162.4(12) . . . . ? C18 C19 C20 C1 176(2) . . . . ? C18 C19 C20 N1 -1(2) . . . . ? C19 C20 N1 C17 0.7(19) . . . . ? C19 C20 N1 Fe1 162.6(12) . . . . ? C20 C1 C2 C3 176(2) . . . . ? C20 C1 C2 N2 -4(3) . . . . ? C20 C1 C21 C22 92(3) . . . . ? C20 C1 C21 C26 -85(4) . . . . ? C21 C1 C2 C3 -1(3) . . . . ? C21 C1 C2 N2 180.0(18) . . . . ? C21 C1 C20 C19 -1(3) . . . . ? C21 C1 C20 N1 175.7(19) . . . . ? C21 C22 C23 C24 0(4) . . . . ? C22 C21 C26 C25 3(5) . . . . ? C22 C23 C24 C25 12(4) . . . . ? C22 C23 C24 C27 -174(2) . . . 12_666 ? C23 C24 C25 C26 -16(4) . . . . ? C24 C25 C26 C21 8(5) . . . . ? C24 C27 O1 Cd1 -180(2) 15 . . . ? C24 C27 O2 Cd1 179(2) 15 . . . ? C26 C21 C22 C23 -7(4) . . . . ? C27 C24 C25 C26 171(3) 12_666 . . . ? C27 Cd1 O3 C34 156.7(14) . . . . ? C27 Cd1 O4 C34 -25(2) . . . . ? C27 Cd1 O5 C41 -120.5(13) . . . . ? C27 Cd1 O6 C41 67.7(14) . . . . ? C28 C6 C7 C8 13(3) . . . . ? C28 C6 C7 N3 -165.9(15) . . . . ? C28 C29 C30 C31 -1(3) . . . . ? C29 C28 C33 C32 -3(3) . . . . ? C29 C30 C31 C32 -3(3) . . . . ? C29 C30 C31 C34 174.1(18) . . . . ? C30 C31 C32 C33 4(3) . . . . ? C30 C31 C34 O3 -12(3) . . . . ? C30 C31 C34 O4 171(2) . . . . ? C31 C32 C33 C28 -1(3) . . . . ? C31 C34 O3 Cd1 -165(2) . . . . ? C31 C34 O4 Cd1 165.3(18) . . . . ? C32 C31 C34 O3 164(2) . . . . ? C32 C31 C34 O4 -13(3) . . . . ? C33 C28 C29 C30 4(3) . . . . ? C34 C31 C32 C33 -173(2) . . . . ? C35 C16 C17 C18 2(3) . . . . ? C35 C16 C17 N1 -171.0(16) . . . . ? C35 C36 C37 C38 0(3) . . . . ? C36 C35 C40 C39 0(3) . . . . ? C36 C37 C38 C39 1(3) . . . . ? C36 C37 C38 C41 -177.2(17) . . . 14_455 ? C37 C38 C39 C40 -2(3) . . . . ? C38 C39 C40 C35 1(3) . . . . ? C38 C41 O5 Cd1 173.2(17) 14_645 . . . ? C38 C41 O6 Cd1 -172.5(14) 14_645 . . . ? C40 C35 C36 C37 -1(3) . . . . ? C41 C38 C39 C40 176.7(17) 14_455 . . . ? C42 C11 C12 C13 1(3) . . . . ? C42 C11 C12 N4 178.1(16) . . . . ? C42 C43 C44 C45 -4(3) . . . . ? C43 C42 C47 C46 3(3) . . . . ? C43 C44 C45 C46 8(3) . . . . ? C43 C44 C45 C48 -173.4(19) . . . . ? C44 C45 C46 C47 -7(3) . . . . ? C44 C45 C48 O8 178.5(18) . . . . ? C44 C45 C48 O9 -1(3) . . . . ? C45 C46 C47 C42 2(3) . . . . ? C46 C45 C48 O8 -3(3) . . . . ? C46 C45 C48 O9 178(2) . . . . ? C47 C42 C43 C44 -2(3) . . . . ? C48 C45 C46 C47 174.3(19) . . . . ? N1 C17 C18 C19 0(2) . . . . ? N1 Fe1 N2 C2 -26.8(14) . . . . ? N1 Fe1 N2 C5 178.4(13) . . . . ? N1 Fe1 N3 C7 -97.1(17) . . . . ? N1 Fe1 N3 C10 90.8(17) . . . . ? N1 Fe1 N4 C12 -171.3(13) . . . . ? N1 Fe1 N4 C15 27.6(13) . . . . ? N2 C2 C3 C4 -2(2) . . . . ? N2 C5 C6 C7 -1(3) . . . . ? N2 C5 C6 C28 177.0(16) . . . . ? N2 Fe1 N1 C17 -178.6(14) . . . . ? N2 Fe1 N1 C20 23.4(14) . . . . ? N2 Fe1 N3 C7 -18.3(13) . . . . ? N2 Fe1 N3 C10 169.6(13) . . . . ? N2 Fe1 N4 C12 -94.3(18) . . . . ? N2 Fe1 N4 C15 104.7(18) . . . . ? N3 C7 C8 C9 2(2) . . . . ? N3 C10 C11 C12 -6(3) . . . . ? N3 C10 C11 C42 173.6(16) . . . . ? N3 Fe1 N1 C17 -99.8(17) . . . . ? N3 Fe1 N1 C20 102.1(18) . . . . ? N3 Fe1 N2 C2 -177.0(14) . . . . ? N3 Fe1 N2 C5 28.2(13) . . . . ? N3 Fe1 N4 C12 -21.0(13) . . . . ? N3 Fe1 N4 C15 178.0(13) . . . . ? N4 C12 C13 C14 -1(2) . . . . ? N4 C15 C16 C17 0(3) . . . . ? N4 C15 C16 C35 176.2(16) . . . . ? N4 Fe1 N1 C17 -23.4(13) . . . . ? N4 Fe1 N1 C20 178.5(15) . . . . ? N4 Fe1 N2 C2 -103.9(18) . . . . ? N4 Fe1 N2 C5 101.3(18) . . . . ? N4 Fe1 N3 C7 -173.9(13) . . . . ? N4 Fe1 N3 C10 14.0(13) . . . . ? O1 C27 Cd1 O2 157(3) . . . . ? O1 C27 Cd1 O3 -52(2) . . . . ? O1 C27 Cd1 O4 -26(3) . . . . ? O1 C27 Cd1 O5 -141(2) . . . . ? O1 C27 Cd1 O6 169.2(19) . . . . ? O1 C27 O2 Cd1 -25(4) . . . . ? O1 Cd1 O2 C27 12.8(19) . . . . ? O1 Cd1 O3 C34 136.2(15) . . . . ? O1 Cd1 O4 C34 -38.5(19) . . . . ? O1 Cd1 O5 C41 -138.1(13) . . . . ? O1 Cd1 O6 C41 75.8(19) . . . . ? O2 C27 Cd1 O1 -157(3) . . . . ? O2 C27 Cd1 O3 151(2) . . . . ? O2 C27 Cd1 O4 176.5(19) . . . . ? O2 C27 Cd1 O5 62(2) . . . . ? O2 C27 Cd1 O6 12(2) . . . . ? O2 C27 O1 Cd1 25(4) . . . . ? O2 Cd1 O1 C27 -12.5(19) . . . . ? O2 Cd1 O3 C34 170.3(14) . . . . ? O2 Cd1 O5 C41 -97.7(13) . . . . ? O2 Cd1 O6 C41 72.9(14) . . . . ? O3 C34 O4 Cd1 -12(3) . . . . ? O3 Cd1 O1 C27 128(2) . . . . ? O3 Cd1 O2 C27 -33(2) . . . . ? O3 Cd1 O4 C34 6.3(14) . . . . ? O3 Cd1 O5 C41 143.4(12) . . . . ? O3 Cd1 O6 C41 -57.3(14) . . . . ? O4 C34 O3 Cd1 12(3) . . . . ? O4 Cd1 O1 C27 163.2(18) . . . . ? O4 Cd1 O3 C34 -6.5(14) . . . . ? O4 Cd1 O5 C41 90.3(12) . . . . ? O4 Cd1 O6 C41 -103.7(13) . . . . ? O5 C41 O6 Cd1 6(2) . . . . ? O5 Cd1 O1 C27 43(2) . . . . ? O5 Cd1 O2 C27 -116(2) . . . . ? O5 Cd1 O3 C34 -110.9(13) . . . . ? O5 Cd1 O4 C34 86.8(16) . . . . ? O5 Cd1 O6 C41 -3.2(11) . . . . ? O6 C41 O5 Cd1 -6(2) . . . . ? O6 Cd1 O1 C27 -16(3) . . . . ? O6 Cd1 O2 C27 -169(2) . . . . ? O6 Cd1 O3 C34 -69.8(15) . . . . ? O6 Cd1 O4 C34 141.2(16) . . . . ? O6 Cd1 O5 C41 3.2(11) . . . . ? O7 Fe1 N1 C17 78.3(14) . . . . ? O7 Fe1 N1 C20 -79.8(15) . . . . ? O7 Fe1 N2 C2 75.5(14) . . . . ? O7 Fe1 N2 C5 -79.3(13) . . . . ? O7 Fe1 N3 C7 84.9(13) . . . . ? O7 Fe1 N3 C10 -87.3(14) . . . . ? O7 Fe1 N4 C12 86.3(13) . . . . ? O7 Fe1 N4 C15 -74.7(13) . . . . ?