# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email wxt@fjirsm.ac.cn _publ_contact_author_name 'Xin-Tao Wu' _publ_author_name 'Xin-Tao Wu' data_a _database_code_depnum_ccdc_archive 'CCDC 852450' #TrackingRef '852450.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H82 N20 O26 Zn3' _chemical_formula_weight 1551.45 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7652(12) _cell_length_b 26.451(2) _cell_length_c 14.9620(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.861(9) _cell_angle_gamma 90.00 _cell_volume 3406.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9010 _cell_measurement_theta_min 3.0805 _cell_measurement_theta_max 27.4972 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.140 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7222 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23282 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7680 _reflns_number_gt 6575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The free nitrate ion N10(O21O22O23) is abnormal, so the distance/angle and least-squares are restrained. The restraints used in the refinement are listed as follows: flat n10 o21 o22 o23 dfix 1.23 0.01 n10 o21 n10 o22 n10 o23 dfix 2.15 0.01 o21 o22 o21 o23 o22 o23 ; _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^)+(0.1588P)^2^+3.8923P] 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 7680 _refine_ls_number_parameters 419 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.2252 _refine_ls_wR_factor_gt 0.2114 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.011 _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 Zn1 Zn 0.49736(4) 0.331110(15) 0.59063(3) 0.03474(17) Uani 1 1 d . . . Zn2 Zn 0.0000 0.5000 1.0000 0.03894(19) Uani 1 2 d S . . C1 C 0.1964(6) 0.3802(2) 0.5189(4) 0.0711(15) Uani 1 1 d . . . H1A H 0.2365 0.4117 0.4992 0.085 Uiso 1 1 calc R . . H1B H 0.0873 0.3779 0.4911 0.085 Uiso 1 1 calc R . . C2 C 0.2125(6) 0.3805(2) 0.6188(4) 0.0659(13) Uani 1 1 d . . . H2A H 0.1593 0.3513 0.6375 0.079 Uiso 1 1 calc R . . H2B H 0.1633 0.4106 0.6372 0.079 Uiso 1 1 calc R . . C3 C 0.3926(7) 0.3668(2) 0.7619(3) 0.0722(16) Uani 1 1 d . . . H3A H 0.5006 0.3705 0.7912 0.087 Uiso 1 1 calc R . . H3B H 0.3643 0.3317 0.7670 0.087 Uiso 1 1 calc R . . C4 C 0.2932(6) 0.39915(19) 0.8132(3) 0.0595(12) Uani 1 1 d . . . C5 C 0.1708(8) 0.37840(17) 0.8450(4) 0.0713(15) Uani 1 1 d . . . H5A H 0.1465 0.3444 0.8347 0.086 Uiso 1 1 calc R . . C6 C 0.0822(7) 0.40817(17) 0.8930(3) 0.0624(12) Uani 1 1 d . . . H6A H -0.0029 0.3938 0.9124 0.075 Uiso 1 1 calc R . . C7 C 0.3257(5) 0.44965(19) 0.8294(3) 0.0539(10) Uani 1 1 d . . . H7A H 0.4062 0.4651 0.8070 0.065 Uiso 1 1 calc R . . C8 C 0.2361(5) 0.47714(15) 0.8797(3) 0.0459(8) Uani 1 1 d . . . H8A H 0.2600 0.5110 0.8915 0.055 Uiso 1 1 calc R . . C9 C 0.3276(5) 0.3486(2) 0.3995(3) 0.0621(12) Uani 1 1 d . . . H9A H 0.2458 0.3679 0.3618 0.074 Uiso 1 1 calc R . . H9B H 0.3403 0.3173 0.3680 0.074 Uiso 1 1 calc R . . C10 C 0.4755(5) 0.3779(2) 0.4126(3) 0.0569(11) Uani 1 1 d . . . H10A H 0.5092 0.3814 0.3547 0.068 Uiso 1 1 calc R . . H10B H 0.4583 0.4115 0.4347 0.068 Uiso 1 1 calc R . . C11 C 0.7440(5) 0.3799(2) 0.4973(3) 0.0622(13) Uani 1 1 d . . . H11A H 0.8215 0.3588 0.5346 0.075 Uiso 1 1 calc R . . H11B H 0.7307 0.4100 0.5321 0.075 Uiso 1 1 calc R . . C12 C 0.8042(5) 0.3956(2) 0.4113(3) 0.0530(10) Uani 1 1 d . . . C13 C 0.8457(7) 0.4450(2) 0.4001(3) 0.0652(12) Uani 1 1 d . . . H13A H 0.8346 0.4694 0.4432 0.078 Uiso 1 1 calc R . . C14 C 0.9046(8) 0.4576(2) 0.3229(4) 0.0745(15) Uani 1 1 d . . . H14A H 0.9333 0.4910 0.3165 0.089 Uiso 1 1 calc R . . C15 C 0.8231(6) 0.3611(2) 0.3447(3) 0.0644(12) Uani 1 1 d . . . H15A H 0.7979 0.3272 0.3501 0.077 Uiso 1 1 calc R . . C16 C 0.8804(6) 0.3781(2) 0.2699(3) 0.0610(11) Uani 1 1 d . . . H16A H 0.8899 0.3548 0.2247 0.073 Uiso 1 1 calc R . . C17 C 0.2021(5) 0.2880(2) 0.4872(3) 0.0617(12) Uani 1 1 d . . . H17A H 0.1379 0.2823 0.4277 0.074 Uiso 1 1 calc R . . H17B H 0.1350 0.2883 0.5318 0.074 Uiso 1 1 calc R . . C18 C 0.3190(5) 0.24579(18) 0.5086(3) 0.0544(10) Uani 1 1 d . . . H18A H 0.2651 0.2141 0.5127 0.065 Uiso 1 1 calc R . . H18B H 0.3775 0.2428 0.4600 0.065 Uiso 1 1 calc R . . C19 C 0.5567(5) 0.21934(16) 0.6163(3) 0.0506(9) Uani 1 1 d . . . H19A H 0.6134 0.2262 0.6772 0.061 Uiso 1 1 calc R . . H19B H 0.6271 0.2249 0.5743 0.061 Uiso 1 1 calc R . . C21 C 0.5070(5) 0.16474(15) 0.6107(3) 0.0460(9) Uani 1 1 d . . . C22 C 0.5597(5) 0.13149(17) 0.5513(3) 0.0528(9) Uani 1 1 d . . . H22A H 0.6277 0.1425 0.5146 0.063 Uiso 1 1 calc R . . C23 C 0.5099(6) 0.08187(18) 0.5474(3) 0.0584(11) Uani 1 1 d . . . H23A H 0.5451 0.0602 0.5068 0.070 Uiso 1 1 calc R . . C24 C 0.4079(6) 0.14605(18) 0.6637(3) 0.0558(10) Uani 1 1 d . . . H24A H 0.3693 0.1672 0.7039 0.067 Uiso 1 1 calc R . . C25 C 0.3659(6) 0.09568(18) 0.6569(4) 0.0615(11) Uani 1 1 d . . . H25A H 0.3008 0.0833 0.6942 0.074 Uiso 1 1 calc R . . N1 N 0.2818(4) 0.33706(15) 0.4880(2) 0.0475(8) Uani 1 1 d . . . N2 N 0.4257(4) 0.25551(13) 0.5947(2) 0.0467(7) Uani 1 1 d . . . H2C H 0.3696 0.2530 0.6399 0.056 Uiso 1 1 calc R . . N3 N 0.3782(4) 0.37940(15) 0.6653(2) 0.0513(8) Uani 1 1 d . . . H3C H 0.4172 0.4111 0.6619 0.062 Uiso 1 1 calc R . . N4 N 0.5968(4) 0.35237(16) 0.4780(2) 0.0495(8) Uani 1 1 d . . . H4A H 0.6172 0.3230 0.4508 0.059 Uiso 1 1 calc R . . N5 N 0.1165(4) 0.45702(12) 0.9122(2) 0.0423(7) Uani 1 1 d . . . N6 N 0.9227(6) 0.42565(18) 0.2586(3) 0.0668(11) Uani 1 1 d . . . N7 N 0.4158(5) 0.06370(14) 0.5979(3) 0.0603(10) Uani 1 1 d . . . N8 N 0.6944(6) 0.27249(19) 0.8864(3) 0.0681(11) Uani 1 1 d . . . N9 N 1.0363(5) 0.25669(15) 0.7152(3) 0.0544(8) Uani 1 1 d . . . N10 N 0.6452(14) 0.4822(5) 0.6720(8) 0.235(6) Uiso 1 1 d D . . O1 O 0.7044(3) 0.32825(11) 0.6833(2) 0.0482(7) Uani 1 1 d . . . O2 O 0.0098(4) 0.56506(11) 0.9153(2) 0.0537(8) Uani 1 1 d . . . O3 O 0.2212(4) 0.52047(11) 1.0797(2) 0.0507(7) Uani 1 1 d . . . O4 O 0.9795(8) 0.2545(3) 0.7831(5) 0.143(3) Uani 1 1 d . . . O5 O 0.9631(6) 0.2802(3) 0.6520(4) 0.140(3) Uani 1 1 d . . . O6 O 1.1659(6) 0.2400(2) 0.7133(4) 0.120(2) Uani 1 1 d . . . O7 O 0.5850(6) 0.25116(19) 0.8363(4) 0.0896(13) Uani 1 1 d . . . O8 O 0.7642(7) 0.2504(2) 0.9557(3) 0.0971(15) Uani 1 1 d . . . O9 O 0.7355(5) 0.31656(16) 0.8688(3) 0.0741(10) Uani 1 1 d . . . O11 O 0.0168(6) 0.66854(14) 0.9528(4) 0.0882(14) Uani 1 1 d . . . O21 O 0.6590(12) 0.4547(4) 0.7379(7) 0.206(4) Uiso 1 1 d D . . O22 O 0.5229(14) 0.4753(7) 0.6076(8) 0.291(7) Uiso 1 1 d D . . O23 O 0.7549(15) 0.5034(5) 0.6491(9) 0.272(7) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0328(2) 0.0451(3) 0.0284(3) -0.00057(14) 0.01125(17) 0.00475(14) Zn2 0.0531(4) 0.0347(3) 0.0350(3) -0.0037(2) 0.0237(3) 0.0031(2) C1 0.045(2) 0.105(4) 0.062(3) 0.004(3) 0.006(2) 0.033(2) C2 0.051(2) 0.091(4) 0.059(3) -0.004(2) 0.018(2) 0.027(2) C3 0.094(4) 0.083(3) 0.044(2) -0.003(2) 0.024(2) 0.046(3) C4 0.078(3) 0.067(3) 0.036(2) -0.0089(18) 0.017(2) 0.030(2) C5 0.121(5) 0.040(2) 0.065(3) -0.0088(19) 0.049(3) 0.008(2) C6 0.091(4) 0.046(2) 0.062(3) -0.0094(19) 0.044(3) -0.004(2) C7 0.049(2) 0.072(3) 0.046(2) -0.0082(19) 0.0216(18) 0.0102(19) C8 0.050(2) 0.049(2) 0.043(2) -0.0094(16) 0.0200(16) 0.0009(16) C9 0.044(2) 0.109(4) 0.033(2) 0.011(2) 0.0061(16) 0.002(2) C10 0.049(2) 0.085(3) 0.038(2) 0.0173(19) 0.0113(17) 0.006(2) C11 0.050(2) 0.103(4) 0.035(2) 0.008(2) 0.0132(17) -0.017(2) C12 0.041(2) 0.082(3) 0.037(2) 0.0111(19) 0.0124(16) 0.0007(18) C13 0.081(3) 0.070(3) 0.050(3) 0.009(2) 0.027(2) 0.011(2) C14 0.107(4) 0.063(3) 0.062(3) 0.018(2) 0.037(3) 0.004(3) C15 0.065(3) 0.083(3) 0.050(3) 0.007(2) 0.023(2) -0.020(2) C16 0.069(3) 0.073(3) 0.047(2) 0.002(2) 0.027(2) -0.011(2) C17 0.039(2) 0.093(4) 0.053(2) -0.001(2) 0.0074(18) -0.008(2) C18 0.048(2) 0.069(3) 0.047(2) -0.0090(19) 0.0100(18) -0.0120(19) C19 0.049(2) 0.048(2) 0.055(2) -0.0068(17) 0.0124(18) -0.0039(16) C21 0.050(2) 0.046(2) 0.043(2) -0.0013(15) 0.0081(16) -0.0037(15) C22 0.056(2) 0.053(2) 0.054(2) -0.0006(18) 0.0204(19) 0.0030(18) C23 0.069(3) 0.054(2) 0.052(2) -0.0065(19) 0.011(2) 0.012(2) C24 0.064(3) 0.059(2) 0.049(2) -0.0046(19) 0.023(2) -0.003(2) C25 0.069(3) 0.058(3) 0.061(3) 0.005(2) 0.021(2) -0.012(2) N1 0.0346(15) 0.077(2) 0.0322(16) 0.0030(14) 0.0085(12) 0.0067(14) N2 0.0457(17) 0.0532(18) 0.0434(18) -0.0024(14) 0.0138(14) -0.0051(14) N3 0.0524(19) 0.062(2) 0.0425(18) -0.0053(15) 0.0162(15) 0.0183(15) N4 0.0403(16) 0.077(2) 0.0340(16) 0.0080(15) 0.0127(13) -0.0037(15) N5 0.0544(18) 0.0414(15) 0.0366(15) -0.0030(12) 0.0230(13) 0.0056(13) N6 0.083(3) 0.075(3) 0.050(2) 0.0182(19) 0.031(2) 0.003(2) N7 0.071(2) 0.0475(19) 0.058(2) 0.0004(16) 0.0021(19) -0.0092(17) N8 0.086(3) 0.077(3) 0.050(2) 0.006(2) 0.035(2) 0.013(2) N9 0.054(2) 0.059(2) 0.054(2) -0.0003(16) 0.0204(17) 0.0014(16) O1 0.0388(14) 0.0641(18) 0.0394(15) 0.0016(11) 0.0014(11) 0.0036(11) O2 0.084(2) 0.0395(14) 0.0463(16) 0.0075(11) 0.0343(15) 0.0052(13) O3 0.0577(17) 0.0460(15) 0.0494(16) -0.0070(12) 0.0127(13) -0.0013(12) O4 0.139(5) 0.184(7) 0.126(5) 0.078(5) 0.080(4) 0.070(5) O5 0.078(3) 0.269(8) 0.084(3) 0.064(4) 0.044(3) 0.067(4) O6 0.086(3) 0.157(5) 0.134(5) 0.060(4) 0.062(3) 0.059(3) O7 0.087(3) 0.094(3) 0.091(3) -0.005(2) 0.026(3) -0.011(2) O8 0.135(4) 0.107(3) 0.056(2) 0.023(2) 0.035(2) 0.019(3) O9 0.093(3) 0.078(2) 0.0510(19) 0.0010(18) 0.0128(18) -0.001(2) O11 0.115(4) 0.051(2) 0.103(4) 0.0023(19) 0.031(3) -0.0016(19) _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 Zn1 O1 2.067(3) . ? Zn1 N3 2.100(3) . ? Zn1 N2 2.101(3) . ? Zn1 N4 2.114(3) . ? Zn1 N1 2.205(3) . ? Zn2 N5 2.137(3) 3_567 ? Zn2 N5 2.137(3) . ? Zn2 O3 2.146(3) . ? Zn2 O3 2.146(3) 3_567 ? Zn2 O2 2.148(3) . ? Zn2 O2 2.148(3) 3_567 ? C1 C2 1.475(7) . ? C1 N1 1.486(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N3 1.488(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N3 1.465(6) . ? C3 C4 1.526(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.369(8) . ? C4 C7 1.378(7) . ? C5 C6 1.396(6) . ? C5 H5A 0.9300 . ? C6 N5 1.345(5) . ? C6 H6A 0.9300 . ? C7 C8 1.392(5) . ? C7 H7A 0.9300 . ? C8 N5 1.345(5) . ? C8 H8A 0.9300 . ? C9 N1 1.487(5) . ? C9 C10 1.491(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N4 1.467(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N4 1.462(5) . ? C11 C12 1.536(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.375(7) . ? C12 C15 1.383(7) . ? C13 C14 1.392(7) . ? C13 H13A 0.9300 . ? C14 N6 1.312(8) . ? C14 H14A 0.9300 . ? C15 C16 1.386(6) . ? C15 H15A 0.9300 . ? C16 N6 1.331(7) . ? C16 H16A 0.9300 . ? C17 N1 1.474(6) . ? C17 C18 1.508(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N2 1.465(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N2 1.483(6) . ? C19 C21 1.506(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C21 C24 1.373(6) . ? C21 C22 1.390(6) . ? C22 C23 1.381(7) . ? C22 H22A 0.9300 . ? C23 N7 1.310(7) . ? C23 H23A 0.9300 . ? C24 C25 1.381(7) . ? C24 H24A 0.9300 . ? C25 N7 1.353(7) . ? C25 H25A 0.9300 . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? N4 H4A 0.9100 . ? N8 O7 1.236(7) . ? N8 O8 1.245(6) . ? N8 O9 1.262(6) . ? N9 O5 1.210(6) . ? N9 O4 1.214(7) . ? N9 O6 1.224(6) . ? N10 O21 1.212(8) . ? N10 O23 1.217(8) . ? N10 O22 1.312(8) . ? 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 O1 Zn1 N3 97.31(13) . . ? O1 Zn1 N2 100.10(13) . . ? N3 Zn1 N2 112.45(15) . . ? O1 Zn1 N4 95.88(13) . . ? N3 Zn1 N4 125.70(16) . . ? N2 Zn1 N4 116.55(15) . . ? O1 Zn1 N1 177.12(13) . . ? N3 Zn1 N1 83.12(14) . . ? N2 Zn1 N1 82.32(14) . . ? N4 Zn1 N1 81.60(13) . . ? N5 Zn2 N5 180 3_567 . ? N5 Zn2 O3 90.60(12) 3_567 . ? N5 Zn2 O3 89.40(12) . . ? N5 Zn2 O3 89.40(12) 3_567 3_567 ? N5 Zn2 O3 90.60(12) . 3_567 ? O3 Zn2 O3 180 . 3_567 ? N5 Zn2 O2 90.75(11) 3_567 . ? N5 Zn2 O2 89.25(11) . . ? O3 Zn2 O2 89.62(13) . . ? O3 Zn2 O2 90.38(12) 3_567 . ? N5 Zn2 O2 89.25(11) 3_567 3_567 ? N5 Zn2 O2 90.75(11) . 3_567 ? O3 Zn2 O2 90.38(12) . 3_567 ? O3 Zn2 O2 89.62(13) 3_567 3_567 ? O2 Zn2 O2 180 . 3_567 ? C2 C1 N1 111.2(4) . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? N1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 N3 111.9(4) . . ? C1 C2 H2A 109.2 . . ? N3 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? N3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N3 C3 C4 114.7(4) . . ? N3 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? N3 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C7 118.5(4) . . ? C5 C4 C3 120.7(5) . . ? C7 C4 C3 120.8(5) . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? N5 C6 C5 121.9(5) . . ? N5 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C4 C7 C8 118.9(4) . . ? C4 C7 H7A 120.6 . . ? C8 C7 H7A 120.6 . . ? N5 C8 C7 123.1(4) . . ? N5 C8 H8A 118.4 . . ? C7 C8 H8A 118.4 . . ? N1 C9 C10 111.3(4) . . ? N1 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N1 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? N4 C10 C9 110.6(4) . . ? N4 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N4 C11 C12 113.5(4) . . ? N4 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? N4 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C15 117.9(4) . . ? C13 C12 C11 119.9(5) . . ? C15 C12 C11 122.2(5) . . ? C12 C13 C14 118.5(5) . . ? C12 C13 H13A 120.8 . . ? C14 C13 H13A 120.8 . . ? N6 C14 C13 124.7(5) . . ? N6 C14 H14A 117.6 . . ? C13 C14 H14A 117.6 . . ? C12 C15 C16 118.7(5) . . ? C12 C15 H15A 120.6 . . ? C16 C15 H15A 120.6 . . ? N6 C16 C15 124.0(5) . . ? N6 C16 H16A 118.0 . . ? C15 C16 H16A 118.0 . . ? N1 C17 C18 110.4(3) . . ? N1 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? N1 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N2 C18 C17 110.7(4) . . ? N2 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? N2 C19 C21 113.7(3) . . ? N2 C19 H19A 108.8 . . ? C21 C19 H19A 108.8 . . ? N2 C19 H19B 108.8 . . ? C21 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C24 C21 C22 117.6(4) . . ? C24 C21 C19 121.4(4) . . ? C22 C21 C19 120.9(4) . . ? C23 C22 C21 119.2(4) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? N7 C23 C22 123.6(4) . . ? N7 C23 H23A 118.2 . . ? C22 C23 H23A 118.2 . . ? C21 C24 C25 119.6(4) . . ? C21 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? N7 C25 C24 122.4(5) . . ? N7 C25 H25A 118.8 . . ? C24 C25 H25A 118.8 . . ? C17 N1 C1 114.5(4) . . ? C17 N1 C9 112.4(4) . . ? C1 N1 C9 110.8(4) . . ? C17 N1 Zn1 106.6(3) . . ? C1 N1 Zn1 104.7(3) . . ? C9 N1 Zn1 107.2(2) . . ? C18 N2 C19 114.7(3) . . ? C18 N2 Zn1 106.6(3) . . ? C19 N2 Zn1 113.4(2) . . ? C18 N2 H2C 107.2 . . ? C19 N2 H2C 107.2 . . ? Zn1 N2 H2C 107.2 . . ? C3 N3 C2 111.2(4) . . ? C3 N3 Zn1 115.3(3) . . ? C2 N3 Zn1 107.6(3) . . ? C3 N3 H3C 107.5 . . ? C2 N3 H3C 107.5 . . ? Zn1 N3 H3C 107.5 . . ? C11 N4 C10 113.8(4) . . ? C11 N4 Zn1 117.1(3) . . ? C10 N4 Zn1 107.4(3) . . ? C11 N4 H4A 105.9 . . ? C10 N4 H4A 105.9 . . ? Zn1 N4 H4A 105.9 . . ? C8 N5 C6 117.5(3) . . ? C8 N5 Zn2 120.4(3) . . ? C6 N5 Zn2 121.9(3) . . ? C14 N6 C16 116.2(4) . . ? C23 N7 C25 117.6(4) . . ? O7 N8 O8 119.6(6) . . ? O7 N8 O9 121.0(5) . . ? O8 N8 O9 119.4(6) . . ? O5 N9 O4 116.0(5) . . ? O5 N9 O6 121.6(5) . . ? O4 N9 O6 122.1(5) . . ? O21 N10 O23 122.8(10) . . ? O21 N10 O22 117.2(10) . . ? O23 N10 O22 115.9(9) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.753 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.111 # Attachment '852451.CIF' data_a2 _database_code_depnum_ccdc_archive 'CCDC 852451' #TrackingRef '852451.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H37 Cd2 Cl4 N7 O2' _chemical_formula_weight 822.21 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1042(16) _cell_length_b 9.2778(6) _cell_length_c 21.079(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.627(6) _cell_angle_gamma 90.00 _cell_volume 3084.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6624 _cell_measurement_theta_min 3.3772 _cell_measurement_theta_max 27.5011 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.1500 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 1.760 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9082 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23321 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6951 _reflns_number_gt 5549 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6951 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1505 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.87137(2) 1.33887(3) 1.315492(17) 0.03832(13) Uani 1 1 d . . . Cd2 Cd 0.69871(2) 0.55252(3) 1.001846(17) 0.03633(13) Uani 1 1 d . . . Cl1 Cl 0.61504(10) 0.3852(2) 1.05521(9) 0.0733(5) Uani 1 1 d . . . Cl2 Cl 0.77511(9) 1.33268(14) 1.39507(7) 0.0523(3) Uani 1 1 d . . . Cl3 Cl 0.79945(9) 1.50511(13) 1.22825(7) 0.0514(3) Uani 1 1 d . . . Cl4 Cl 1.00174(9) 1.19058(14) 1.35865(7) 0.0558(4) Uani 1 1 d . . . C1 C 0.7476(3) 1.1591(5) 1.1954(3) 0.0429(12) Uani 1 1 d . . . H1A H 0.7229 1.2501 1.1896 0.051 Uiso 1 1 calc R . . C2 C 0.7137(4) 1.0501(5) 1.1541(3) 0.0493(13) Uani 1 1 d . . . H2A H 0.6681 1.0695 1.1205 0.059 Uiso 1 1 calc R . . C3 C 0.8169(4) 0.8938(5) 1.2102(3) 0.0556(15) Uani 1 1 d . . . H3A H 0.8436 0.8046 1.2161 0.067 Uiso 1 1 calc R . . C4 C 0.8484(4) 1.0078(6) 1.2503(3) 0.0528(14) Uani 1 1 d . . . H4A H 0.8953 0.9915 1.2833 0.063 Uiso 1 1 calc R . . C5 C 0.7463(3) 0.9119(5) 1.1618(2) 0.0429(11) Uani 1 1 d . . . C6 C 1.0241(3) 0.1492(6) 1.1818(3) 0.0465(12) Uani 1 1 d . . . H6A H 1.0566 0.1544 1.2236 0.056 Uiso 1 1 calc R . . C7 C 0.9633(3) 0.2544(5) 1.1623(2) 0.0437(11) Uani 1 1 d . . . H7A H 0.9552 0.3275 1.1906 0.052 Uiso 1 1 calc R . . C8 C 0.9142(3) 0.2499(5) 1.0998(2) 0.0415(11) Uani 1 1 d . . . C9 C 0.9308(3) 0.1412(5) 1.0596(3) 0.0430(12) Uani 1 1 d . . . H9A H 0.9010 0.1360 1.0170 0.052 Uiso 1 1 calc R . . C10 C 0.9928(3) 0.0390(5) 1.0836(3) 0.0442(12) Uani 1 1 d . . . H10A H 1.0029 -0.0346 1.0561 0.053 Uiso 1 1 calc R . . C11 C 0.7085(3) 0.7886(5) 1.1184(3) 0.0470(12) Uani 1 1 d . . . H11A H 0.6994 0.7079 1.1454 0.056 Uiso 1 1 calc R . . H11B H 0.6536 0.8185 1.0940 0.056 Uiso 1 1 calc R . . C12 C 0.5762(4) 0.4159(7) 0.8748(3) 0.0601(15) Uani 1 1 d . . . H12A H 0.5368 0.4003 0.9035 0.072 Uiso 1 1 calc R . . H12B H 0.6164 0.3368 0.8813 0.072 Uiso 1 1 calc R . . C13 C 0.8423(4) 0.3559(6) 1.0823(3) 0.0523(14) Uani 1 1 d . . . H13A H 0.7922 0.3132 1.0935 0.063 Uiso 1 1 calc R . . H13B H 0.8563 0.4409 1.1092 0.063 Uiso 1 1 calc R . . C14 C 0.7760(3) 0.8534(5) 1.0267(3) 0.0438(12) Uani 1 1 d . . . H14A H 0.8042 0.9346 1.0510 0.053 Uiso 1 1 calc R . . H14B H 0.7223 0.8870 1.0016 0.053 Uiso 1 1 calc R . . C15 C 0.8305(3) 0.7974(5) 0.9811(3) 0.0424(11) Uani 1 1 d . . . H15A H 0.8390 0.8741 0.9518 0.051 Uiso 1 1 calc R . . H15B H 0.8856 0.7704 1.0062 0.051 Uiso 1 1 calc R . . C16 C 0.7384(4) 0.7159(6) 0.8804(3) 0.0491(12) Uani 1 1 d . . . H16A H 0.7743 0.7428 0.8505 0.059 Uiso 1 1 calc R . . H16B H 0.7056 0.8000 0.8874 0.059 Uiso 1 1 calc R . . C17 C 0.6782(4) 0.5970(6) 0.8501(3) 0.0536(14) Uani 1 1 d . . . H17A H 0.6437 0.6314 0.8099 0.064 Uiso 1 1 calc R . . H17B H 0.7108 0.5151 0.8402 0.064 Uiso 1 1 calc R . . C18 C 0.8578(3) 0.5666(5) 0.9329(2) 0.0413(11) Uani 1 1 d . . . H18A H 0.9049 0.6174 0.9209 0.050 Uiso 1 1 calc R . . H18B H 0.8337 0.5026 0.8976 0.050 Uiso 1 1 calc R . . C19 C 0.8901(3) 0.4781(5) 0.9933(2) 0.0403(11) Uani 1 1 d . . . H19A H 0.9311 0.4082 0.9843 0.048 Uiso 1 1 calc R . . H19B H 0.9185 0.5409 1.0276 0.048 Uiso 1 1 calc R . . C20 C 0.5622(5) 0.3530(10) 0.7575(4) 0.091(3) Uani 1 1 d . . . H20A H 0.6153 0.3096 0.7672 0.109 Uiso 1 1 calc R . . C21 C 0.5183(6) 0.3588(13) 0.6944(4) 0.113(4) Uani 1 1 d . . . H21A H 0.5426 0.3153 0.6628 0.135 Uiso 1 1 calc R . . C22 C 0.4066(5) 0.4701(12) 0.7239(4) 0.101(3) Uani 1 1 d . . . H22A H 0.3515 0.5055 0.7136 0.121 Uiso 1 1 calc R . . C23 C 0.4463(4) 0.4683(9) 0.7869(4) 0.076(2) Uani 1 1 d . . . H23A H 0.4189 0.5058 0.8181 0.092 Uiso 1 1 calc R . . C24 C 0.5275(4) 0.4114(7) 0.8059(3) 0.0606(16) Uani 1 1 d . . . N1 N 0.8150(3) 1.1395(4) 1.2440(2) 0.0403(9) Uani 1 1 d . . . N2 N 1.0383(3) 0.0416(4) 1.1440(2) 0.0411(9) Uani 1 1 d . . . N3 N 0.4427(5) 0.4232(11) 0.6755(3) 0.118(3) Uani 1 1 d . . . N4 N 0.7602(3) 0.7392(4) 1.07267(19) 0.0398(9) Uani 1 1 d . . . H4B H 0.8110 0.7079 1.0956 0.048 Uiso 1 1 calc R . . N5 N 0.6228(3) 0.5510(5) 0.8940(2) 0.0487(11) Uani 1 1 d . . . H5A H 0.5826 0.6209 0.8916 0.058 Uiso 1 1 calc R . . N6 N 0.8205(2) 0.4025(4) 1.0146(2) 0.0374(9) Uani 1 1 d . . . H6B H 0.8070 0.3231 0.9893 0.045 Uiso 1 1 calc R . . N7 N 0.7927(3) 0.6722(4) 0.9429(2) 0.0398(9) Uani 1 1 d . . . O1 O 0.5827(6) 1.0368(11) 0.9553(4) 0.171(4) Uani 1 1 d . . . O2 O 0.5685(3) 0.7475(7) 0.9880(3) 0.103(2) 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 0.0421(2) 0.03311(19) 0.0364(2) -0.00147(13) -0.00017(16) -0.00106(13) Cd2 0.0356(2) 0.03474(19) 0.0365(2) -0.00184(13) 0.00230(15) -0.00303(13) Cl1 0.0465(8) 0.0960(12) 0.0742(11) 0.0316(9) 0.0045(7) -0.0180(8) Cl2 0.0554(8) 0.0547(7) 0.0473(7) 0.0077(6) 0.0117(6) 0.0004(6) Cl3 0.0608(8) 0.0380(6) 0.0476(7) 0.0038(5) -0.0076(6) -0.0025(6) Cl4 0.0549(8) 0.0466(6) 0.0581(8) -0.0024(6) -0.0075(6) 0.0086(6) C1 0.044(3) 0.032(2) 0.054(3) -0.006(2) 0.011(2) 0.0020(19) C2 0.057(3) 0.036(2) 0.050(3) -0.004(2) -0.001(3) 0.008(2) C3 0.066(4) 0.032(2) 0.060(4) -0.003(2) -0.009(3) 0.007(2) C4 0.066(4) 0.039(2) 0.046(3) -0.003(2) -0.006(3) 0.004(2) C5 0.052(3) 0.035(2) 0.039(3) -0.002(2) 0.005(2) -0.004(2) C6 0.038(3) 0.051(3) 0.046(3) -0.003(2) -0.001(2) 0.009(2) C7 0.041(3) 0.044(2) 0.044(3) -0.003(2) 0.005(2) 0.010(2) C8 0.034(2) 0.044(2) 0.047(3) 0.009(2) 0.008(2) 0.004(2) C9 0.043(3) 0.044(2) 0.037(3) 0.002(2) -0.003(2) 0.003(2) C10 0.047(3) 0.037(2) 0.045(3) -0.001(2) 0.001(2) 0.003(2) C11 0.048(3) 0.036(2) 0.058(3) -0.007(2) 0.012(2) -0.009(2) C12 0.053(3) 0.064(3) 0.058(4) -0.004(3) 0.000(3) -0.009(3) C13 0.051(3) 0.064(3) 0.041(3) 0.017(3) 0.008(2) 0.023(3) C14 0.047(3) 0.028(2) 0.055(3) -0.002(2) 0.008(2) -0.006(2) C15 0.039(3) 0.036(2) 0.050(3) -0.001(2) 0.005(2) -0.011(2) C16 0.051(3) 0.050(3) 0.044(3) 0.006(2) 0.005(2) 0.000(2) C17 0.056(3) 0.061(3) 0.041(3) 0.003(3) 0.001(3) 0.001(3) C18 0.040(3) 0.045(2) 0.040(3) 0.000(2) 0.010(2) 0.004(2) C19 0.031(2) 0.043(2) 0.048(3) 0.006(2) 0.010(2) 0.0055(19) C20 0.055(4) 0.136(7) 0.079(5) -0.045(5) 0.011(4) -0.006(4) C21 0.070(5) 0.194(11) 0.075(5) -0.057(6) 0.019(4) -0.046(6) C22 0.049(4) 0.170(9) 0.074(5) -0.008(6) -0.013(4) 0.004(5) C23 0.049(4) 0.111(6) 0.065(4) -0.022(4) 0.002(3) -0.003(4) C24 0.039(3) 0.080(4) 0.060(4) -0.016(3) 0.004(3) -0.014(3) N1 0.047(2) 0.0331(18) 0.039(2) -0.0062(17) 0.0044(18) -0.0024(17) N2 0.043(2) 0.0345(19) 0.042(2) 0.0033(17) 0.0013(18) 0.0016(17) N3 0.082(5) 0.210(10) 0.056(4) -0.020(5) -0.003(4) -0.057(6) N4 0.044(2) 0.0359(19) 0.039(2) -0.0043(17) 0.0077(18) -0.0008(17) N5 0.041(2) 0.060(3) 0.041(2) -0.002(2) -0.0005(19) -0.001(2) N6 0.038(2) 0.0340(18) 0.040(2) 0.0025(17) 0.0070(17) 0.0045(16) N7 0.043(2) 0.0373(19) 0.037(2) -0.0004(17) 0.0033(18) 0.0006(17) O1 0.169(9) 0.205(10) 0.138(7) 0.022(7) 0.025(6) 0.057(7) O2 0.056(3) 0.145(5) 0.108(4) -0.056(4) 0.012(3) -0.011(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 Cd1 N2 2.425(4) 2_767 ? Cd1 N1 2.442(4) . ? Cd1 Cl3 2.4988(13) . ? Cd1 Cl2 2.5037(15) . ? Cd1 Cl4 2.5216(14) . ? Cd2 N5 2.354(4) . ? Cd2 N4 2.369(4) . ? Cd2 N6 2.375(4) . ? Cd2 N7 2.413(4) . ? Cd2 Cl1 2.4702(16) . ? C1 N1 1.347(6) . ? C1 C2 1.374(7) . ? C1 H1A 0.9300 . ? C2 C5 1.383(6) . ? C2 H2A 0.9300 . ? C3 C5 1.376(7) . ? C3 C4 1.384(7) . ? C3 H3A 0.9300 . ? C4 N1 1.332(6) . ? C4 H4A 0.9300 . ? C5 C11 1.514(7) . ? C6 N2 1.327(6) . ? C6 C7 1.385(7) . ? C6 H6A 0.9300 . ? C7 C8 1.393(7) . ? C7 H7A 0.9300 . ? C8 C9 1.378(7) . ? C8 C13 1.508(7) . ? C9 C10 1.396(7) . ? C9 H9A 0.9300 . ? C10 N2 1.335(6) . ? C10 H10A 0.9300 . ? C11 N4 1.467(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 N5 1.475(7) . ? C12 C24 1.506(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N6 1.465(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N4 1.493(6) . ? C14 C15 1.518(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 N7 1.474(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N7 1.484(6) . ? C16 C17 1.521(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N5 1.472(8) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N7 1.480(6) . ? C18 C19 1.515(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N6 1.468(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C24 1.371(10) . ? C20 C21 1.374(11) . ? C20 H20A 0.9300 . ? C21 N3 1.343(13) . ? C21 H21A 0.9300 . ? C22 N3 1.345(11) . ? C22 C23 1.354(10) . ? C22 H22A 0.9300 . ? C23 C24 1.392(9) . ? C23 H23A 0.9300 . ? N2 Cd1 2.425(4) 2_737 ? N4 H4B 0.9100 . ? N5 H5A 0.9100 . ? N6 H6B 0.9100 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cd1 N1 157.93(15) 2_767 . ? N2 Cd1 Cl3 86.38(10) 2_767 . ? N1 Cd1 Cl3 87.36(10) . . ? N2 Cd1 Cl2 100.95(11) 2_767 . ? N1 Cd1 Cl2 101.10(11) . . ? Cl3 Cd1 Cl2 104.45(5) . . ? N2 Cd1 Cl4 84.22(10) 2_767 . ? N1 Cd1 Cl4 89.33(10) . . ? Cl3 Cd1 Cl4 146.20(6) . . ? Cl2 Cd1 Cl4 109.19(5) . . ? N5 Cd2 N4 133.04(15) . . ? N5 Cd2 N6 111.24(15) . . ? N4 Cd2 N6 97.27(14) . . ? N5 Cd2 N7 76.30(15) . . ? N4 Cd2 N7 76.26(14) . . ? N6 Cd2 N7 74.87(14) . . ? N5 Cd2 Cl1 102.19(12) . . ? N4 Cd2 Cl1 111.68(11) . . ? N6 Cd2 Cl1 95.38(11) . . ? N7 Cd2 Cl1 168.45(11) . . ? N1 C1 C2 122.6(4) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C5 121.0(5) . . ? C1 C2 H2A 119.5 . . ? C5 C2 H2A 119.5 . . ? C5 C3 C4 120.4(5) . . ? C5 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? N1 C4 C3 123.3(5) . . ? N1 C4 H4A 118.4 . . ? C3 C4 H4A 118.4 . . ? C3 C5 C2 115.9(5) . . ? C3 C5 C11 121.9(5) . . ? C2 C5 C11 122.1(5) . . ? N2 C6 C7 123.2(5) . . ? N2 C6 H6A 118.4 . . ? C7 C6 H6A 118.4 . . ? C6 C7 C8 119.5(5) . . ? C6 C7 H7A 120.2 . . ? C8 C7 H7A 120.2 . . ? C9 C8 C7 117.4(4) . . ? C9 C8 C13 124.2(5) . . ? C7 C8 C13 118.2(5) . . ? C8 C9 C10 119.2(5) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? N2 C10 C9 123.3(5) . . ? N2 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? N4 C11 C5 114.9(4) . . ? N4 C11 H11A 108.5 . . ? C5 C11 H11A 108.5 . . ? N4 C11 H11B 108.5 . . ? C5 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N5 C12 C24 115.1(5) . . ? N5 C12 H12A 108.5 . . ? C24 C12 H12A 108.5 . . ? N5 C12 H12B 108.5 . . ? C24 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? N6 C13 C8 116.9(5) . . ? N6 C13 H13A 108.1 . . ? C8 C13 H13A 108.1 . . ? N6 C13 H13B 108.1 . . ? C8 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? N4 C14 C15 111.4(4) . . ? N4 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N4 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N7 C15 C14 112.8(4) . . ? N7 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? N7 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N7 C16 C17 112.7(4) . . ? N7 C16 H16A 109.1 . . ? C17 C16 H16A 109.1 . . ? N7 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? N5 C17 C16 111.2(5) . . ? N5 C17 H17A 109.4 . . ? C16 C17 H17A 109.4 . . ? N5 C17 H17B 109.4 . . ? C16 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N7 C18 C19 111.9(4) . . ? N7 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N7 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N6 C19 C18 111.2(4) . . ? N6 C19 H19A 109.4 . . ? C18 C19 H19A 109.4 . . ? N6 C19 H19B 109.4 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? C24 C20 C21 119.8(8) . . ? C24 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? N3 C21 C20 124.3(8) . . ? N3 C21 H21A 117.8 . . ? C20 C21 H21A 117.8 . . ? N3 C22 C23 123.3(8) . . ? N3 C22 H22A 118.3 . . ? C23 C22 H22A 118.3 . . ? C22 C23 C24 121.2(7) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C20 C24 C23 115.9(6) . . ? C20 C24 C12 121.2(6) . . ? C23 C24 C12 122.9(6) . . ? C4 N1 C1 116.6(4) . . ? C4 N1 Cd1 122.8(3) . . ? C1 N1 Cd1 120.7(3) . . ? C6 N2 C10 117.3(4) . . ? C6 N2 Cd1 122.4(3) . 2_737 ? C10 N2 Cd1 119.8(3) . 2_737 ? C21 N3 C22 115.0(7) . . ? C11 N4 C14 113.5(4) . . ? C11 N4 Cd2 115.0(3) . . ? C14 N4 Cd2 102.4(3) . . ? C11 N4 H4B 108.6 . . ? C14 N4 H4B 108.6 . . ? Cd2 N4 H4B 108.6 . . ? C17 N5 C12 114.4(5) . . ? C17 N5 Cd2 110.0(3) . . ? C12 N5 Cd2 113.9(3) . . ? C17 N5 H5A 105.9 . . ? C12 N5 H5A 105.9 . . ? Cd2 N5 H5A 105.9 . . ? C13 N6 C19 113.1(4) . . ? C13 N6 Cd2 108.3(3) . . ? C19 N6 Cd2 110.5(3) . . ? C13 N6 H6B 108.3 . . ? C19 N6 H6B 108.3 . . ? Cd2 N6 H6B 108.3 . . ? C15 N7 C18 111.9(4) . . ? C15 N7 C16 112.0(4) . . ? C18 N7 C16 111.2(4) . . ? C15 N7 Cd2 108.3(3) . . ? C18 N7 Cd2 107.7(3) . . ? C16 N7 Cd2 105.4(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.488 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.100 # Attachment '852452.CIF' data_a3 _database_code_depnum_ccdc_archive 'CCDC 852452' #TrackingRef '852452.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H39 Cd1.50 N10 O12' _chemical_formula_weight 828.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.184(15) _cell_length_b 17.768(11) _cell_length_c 16.452(8) _cell_angle_alpha 90.00 _cell_angle_beta 114.83(3) _cell_angle_gamma 90.00 _cell_volume 6681(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.6591 _cell_measurement_theta_max 27.4856 _exptl_crystal_description Prism _exptl_crystal_colour White _exptl_crystal_size_max 0.1000 _exptl_crystal_size_mid 0.0800 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_absorpt_coefficient_mu 1.036 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9005 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25014 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7652 _reflns_number_gt 5331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The nitrate ion N9(O5O6O7) is abnormal, so the following least-squares restraint is used in the refinement, flat n9 o5 o6 o7. The N4-C7 group is disorder, so the following process is used in the refinement. PART 1 N4 3 0.11867 0.57454 0.33963 10.50000 0.04848 0.02296 = 0.04977 0.02139 0.00952 -0.00575 C7 1 0.15372 0.63521 0.32377 10.50000 0.04399 0.04126 = 0.05254 0.01502 0.01181 -0.00160 PART 2 N4' 3 0.13997 0.59706 0.36184 10.50000 0.08173 0.04776 = 0.08227 0.02487 0.05383 0.02490 C7' 1 0.13928 0.61634 0.27923 10.50000 0.10094 0.06847 = 0.08144 0.03673 0.05883 0.04284 PART 0 ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7652 _refine_ls_number_parameters 448 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1933 _refine_ls_wR_factor_gt 0.1648 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.170536(19) 0.47293(3) 0.41585(3) 0.03599(16) Uani 1 1 d . . . Cd2 Cd 0.5000 0.5000 1.0000 0.03586(18) Uani 1 2 d S . . C1 C 0.1822(3) 0.5347(4) 0.6051(5) 0.0549(19) Uani 1 1 d . . . H1A H 0.1880 0.4877 0.6378 0.066 Uiso 1 1 calc R A . H1B H 0.1728 0.5731 0.6389 0.066 Uiso 1 1 calc R . . C2 C 0.2382(3) 0.5558(4) 0.5989(5) 0.0515(17) Uani 1 1 d . A . H2A H 0.2334 0.6046 0.5704 0.062 Uiso 1 1 calc R . . H2B H 0.2692 0.5599 0.6588 0.062 Uiso 1 1 calc R . . C3 C 0.0884(4) 0.4734(4) 0.5204(6) 0.059(2) Uani 1 1 d . . . H3A H 0.0513 0.4833 0.4699 0.071 Uiso 1 1 calc R A . H3B H 0.0831 0.4818 0.5748 0.071 Uiso 1 1 calc R . . C4 C 0.1054(3) 0.3914(4) 0.5173(5) 0.0578(19) Uani 1 1 d . A . H4A H 0.1414 0.3806 0.5694 0.069 Uiso 1 1 calc R . . H4B H 0.0751 0.3588 0.5191 0.069 Uiso 1 1 calc R . . C5 C 0.1072(3) 0.5990(4) 0.4801(5) 0.0556(18) Uani 1 1 d . . . H5A H 0.1364 0.6379 0.5078 0.067 Uiso 1 1 d R A . H5B H 0.0747 0.6091 0.4954 0.067 Uiso 1 1 d R . . C6 C 0.0874(5) 0.6049(6) 0.3830(7) 0.100(4) Uani 0.50 1 d P A 1 H6A H 0.0486 0.5829 0.3559 0.120 Uiso 0.50 1 calc PR A 1 H6B H 0.0828 0.6581 0.3685 0.120 Uiso 0.50 1 calc PR A 1 C6' C 0.0874(5) 0.6049(6) 0.3830(7) 0.100(4) Uani 0.50 1 d P A 2 H6C H 0.0687 0.6532 0.3621 0.120 Uiso 0.50 1 calc PR A 2 H6D H 0.0592 0.5655 0.3532 0.120 Uiso 0.50 1 calc PR A 2 C8 C 0.1130(4) 0.6959(5) 0.2569(6) 0.067(2) Uani 1 1 d . . . C9 C 0.0614(4) 0.6887(5) 0.1833(7) 0.076(3) Uani 1 1 d . . . H9A H 0.0481 0.6414 0.1591 0.091 Uiso 1 1 calc R . . C10 C 0.0285(4) 0.7529(6) 0.1443(6) 0.076(3) Uani 1 1 d . . . H10A H -0.0073 0.7468 0.0952 0.091 Uiso 1 1 calc R A . C11 C 0.1321(5) 0.7655(6) 0.2846(8) 0.102(4) Uani 1 1 d . . . H11A H 0.1689 0.7726 0.3312 0.123 Uiso 1 1 calc R . . C12 C 0.0976(5) 0.8268(5) 0.2447(8) 0.112(4) Uani 1 1 d . . . H12A H 0.1108 0.8743 0.2682 0.134 Uiso 1 1 calc R A . C13 C 0.2824(3) 0.4306(4) 0.5989(4) 0.0487(16) Uani 1 1 d . . . H13A H 0.2523 0.4018 0.6071 0.058 Uiso 1 1 calc R A . H13B H 0.2966 0.4004 0.5630 0.058 Uiso 1 1 calc R . . C14 C 0.3318(3) 0.4435(4) 0.6885(4) 0.0424(14) Uani 1 1 d . . . C15 C 0.3863(3) 0.4663(4) 0.6989(5) 0.0519(18) Uani 1 1 d . . . H15A H 0.3937 0.4722 0.6484 0.062 Uiso 1 1 calc R A . C16 C 0.4301(3) 0.4807(4) 0.7812(4) 0.0461(16) Uani 1 1 d . . . H16A H 0.4665 0.4957 0.7851 0.055 Uiso 1 1 calc R . . C17 C 0.3246(3) 0.4370(4) 0.7662(4) 0.0473(16) Uani 1 1 d . . . H17A H 0.2884 0.4226 0.7635 0.057 Uiso 1 1 calc R A . C18 C 0.3705(3) 0.4515(4) 0.8493(4) 0.0447(15) Uani 1 1 d . . . H18A H 0.3642 0.4451 0.9007 0.054 Uiso 1 1 calc R . . C19 C 0.1382(3) 0.3008(4) 0.4342(6) 0.0559(19) Uani 1 1 d . . . H19A H 0.1782 0.2990 0.4794 0.067 Uiso 1 1 calc R A . H19B H 0.1390 0.2937 0.3763 0.067 Uiso 1 1 calc R . . C20 C 0.1038(3) 0.2362(4) 0.4506(5) 0.0484(16) Uani 1 1 d . . . C21 C 0.1328(3) 0.1824(4) 0.5117(5) 0.0563(19) Uani 1 1 d . . . H21A H 0.1729 0.1864 0.5460 0.068 Uiso 1 1 calc R A . C22 C 0.1022(3) 0.1212(4) 0.5227(5) 0.061(2) Uani 1 1 d . . . H22A H 0.1231 0.0863 0.5666 0.073 Uiso 1 1 calc R . . C23 C 0.0448(4) 0.2268(5) 0.4017(7) 0.086(3) Uani 1 1 d . . . H23A H 0.0232 0.2618 0.3584 0.103 Uiso 1 1 calc R A . C24 C 0.0172(3) 0.1631(5) 0.4179(6) 0.074(3) Uani 1 1 d . . . H24A H -0.0232 0.1585 0.3866 0.089 Uiso 1 1 calc R . . N1 N 0.1328(2) 0.5262(3) 0.5178(4) 0.0442(13) Uani 1 1 d . A . N2 N 0.2553(2) 0.5007(3) 0.5479(4) 0.0460(13) Uani 1 1 d . A . H2C H 0.2819 0.5229 0.5315 0.055 Uiso 1 1 calc R . . N3 N 0.1137(2) 0.3759(3) 0.4363(4) 0.0416(12) Uani 1 1 d . A . H3C H 0.0778 0.3781 0.3893 0.050 Uiso 1 1 calc R . . N5 N 0.0455(3) 0.8214(4) 0.1735(5) 0.0718(19) Uani 1 1 d . . . N6 N 0.4224(2) 0.4738(3) 0.8576(3) 0.0367(11) Uani 1 1 d . . . N7 N 0.0464(2) 0.1087(3) 0.4765(4) 0.0435(13) Uani 1 1 d . . . N8 N 0.2451(2) 0.4175(3) 0.3408(4) 0.0439(13) Uani 1 1 d . . . N9 N 0.0571(4) 0.4192(6) 0.1999(6) 0.098(3) Uani 1 1 d D . . N10 N 0.6695(5) 0.6673(7) 1.0134(8) 0.110(3) Uani 1 1 d . . . O1 O 0.2310(3) 0.4841(3) 0.3319(4) 0.0670(15) Uani 1 1 d . . . O2 O 0.2279(2) 0.3770(3) 0.3871(3) 0.0522(12) Uani 1 1 d . . . O3 O 0.2743(2) 0.3907(3) 0.3033(3) 0.0632(14) Uani 1 1 d . . . O4 O 0.5378(2) 0.5716(3) 0.9190(3) 0.0550(12) Uani 1 1 d . . . O5 O 0.1049(3) 0.4166(5) 0.2542(5) 0.112(3) Uani 1 1 d D . . O6 O 0.0368(5) 0.4873(7) 0.1877(8) 0.170(5) Uani 1 1 d D . . O7 O 0.0317(4) 0.3856(6) 0.1331(7) 0.158(4) Uani 1 1 d D . . O12 O 0.6283(7) 0.7497(7) 1.1927(9) 0.224(6) Uani 1 1 d . . . O11 O 0.2530(5) 0.2179(6) 0.2967(10) 0.202(5) Uani 1 1 d . . . O8 O 0.6562(3) 0.6047(5) 0.9746(5) 0.095(2) Uani 1 1 d . . . O9 O 0.6251(5) 0.7043(5) 1.0116(8) 0.145(4) Uani 1 1 d . . . O10 O 0.7167(5) 0.6909(10) 1.0422(11) 0.266(9) Uani 1 1 d . . . N4 N 0.1187(8) 0.5745(10) 0.3396(14) 0.044(4) Uani 0.50 1 d P A 1 H4D H 0.0924 0.5581 0.2851 0.053 Uiso 0.50 1 calc PR A 1 C7 C 0.1537(9) 0.6352(12) 0.3238(13) 0.049(5) Uani 0.50 1 d P A 1 H7B H 0.1793 0.6136 0.2994 0.059 Uiso 0.50 1 calc PR A 1 H7C H 0.1780 0.6592 0.3802 0.059 Uiso 0.50 1 calc PR A 1 N4' N 0.1400(9) 0.5971(12) 0.3618(16) 0.064(5) Uani 0.50 1 d P A 2 H4'A H 0.1676 0.6276 0.4020 0.077 Uiso 0.50 1 calc PR A 2 C7' C 0.1393(12) 0.6163(15) 0.2792(15) 0.077(7) Uani 0.50 1 d P A 2 H7'A H 0.1156 0.5809 0.2335 0.092 Uiso 0.50 1 calc PR A 2 H7'B H 0.1787 0.6158 0.2826 0.092 Uiso 0.50 1 calc PR A 2 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 0.0382(3) 0.0315(3) 0.0341(3) 0.00343(18) 0.01104(19) -0.00034(18) Cd2 0.0332(3) 0.0315(4) 0.0345(3) -0.0017(3) 0.0061(3) 0.0065(3) C1 0.068(5) 0.055(5) 0.039(4) -0.006(3) 0.020(3) 0.003(4) C2 0.051(4) 0.044(4) 0.043(4) -0.010(3) 0.003(3) -0.004(3) C3 0.061(5) 0.053(5) 0.072(5) 0.004(4) 0.036(4) 0.001(4) C4 0.063(4) 0.057(5) 0.061(4) 0.007(4) 0.033(4) -0.014(4) C5 0.057(4) 0.049(4) 0.055(4) 0.007(4) 0.018(3) 0.013(4) C6 0.133(9) 0.103(8) 0.093(7) 0.053(6) 0.076(7) 0.076(7) C6' 0.133(9) 0.103(8) 0.093(7) 0.053(6) 0.076(7) 0.076(7) C8 0.079(6) 0.049(5) 0.086(6) 0.030(5) 0.047(5) 0.014(4) C9 0.099(7) 0.045(5) 0.090(7) 0.010(5) 0.045(6) 0.002(5) C10 0.076(6) 0.071(6) 0.075(6) 0.022(5) 0.026(5) 0.001(5) C11 0.093(7) 0.063(7) 0.106(8) 0.030(6) -0.002(6) 0.012(6) C12 0.129(10) 0.037(5) 0.109(8) 0.017(5) -0.009(7) 0.003(6) C13 0.046(4) 0.047(4) 0.038(3) -0.006(3) 0.003(3) -0.002(3) C14 0.042(3) 0.035(3) 0.042(3) -0.004(3) 0.009(3) 0.002(3) C15 0.052(4) 0.063(5) 0.037(3) -0.002(3) 0.014(3) -0.004(3) C16 0.042(4) 0.057(4) 0.041(4) -0.007(3) 0.019(3) -0.007(3) C17 0.041(3) 0.055(4) 0.039(3) -0.005(3) 0.010(3) -0.005(3) C18 0.047(4) 0.041(4) 0.043(3) -0.005(3) 0.016(3) 0.000(3) C19 0.066(5) 0.031(4) 0.080(5) -0.002(4) 0.040(4) -0.006(3) C20 0.049(4) 0.036(4) 0.055(4) 0.000(3) 0.017(3) -0.012(3) C21 0.045(4) 0.040(4) 0.075(5) 0.015(4) 0.016(4) -0.006(3) C22 0.041(4) 0.051(5) 0.070(5) 0.032(4) 0.005(3) -0.006(3) C23 0.065(5) 0.047(5) 0.102(7) 0.032(5) -0.006(5) -0.017(4) C24 0.043(4) 0.057(5) 0.096(6) 0.023(5) 0.003(4) -0.011(4) N1 0.050(3) 0.037(3) 0.043(3) -0.002(2) 0.017(3) 0.004(2) N2 0.041(3) 0.049(3) 0.041(3) -0.003(3) 0.011(2) -0.001(3) N3 0.042(3) 0.035(3) 0.049(3) 0.007(2) 0.019(2) -0.004(2) N5 0.078(5) 0.051(4) 0.078(5) 0.018(4) 0.023(4) 0.010(4) N6 0.037(3) 0.034(3) 0.027(2) 0.000(2) 0.002(2) 0.010(2) N7 0.043(3) 0.032(3) 0.048(3) 0.005(2) 0.012(2) -0.006(2) N8 0.035(3) 0.047(4) 0.043(3) 0.010(3) 0.010(2) 0.005(3) N9 0.060(5) 0.106(7) 0.093(6) -0.022(6) -0.004(5) 0.026(5) N10 0.108(8) 0.099(8) 0.121(8) 0.007(7) 0.047(7) -0.031(7) O1 0.082(4) 0.058(4) 0.077(4) 0.009(3) 0.048(3) 0.006(3) O2 0.052(3) 0.055(3) 0.055(3) 0.011(2) 0.028(2) 0.003(2) O3 0.061(3) 0.078(4) 0.058(3) 0.011(3) 0.032(3) 0.018(3) O4 0.055(3) 0.052(3) 0.055(3) 0.010(2) 0.020(2) -0.003(2) O5 0.065(4) 0.159(8) 0.076(4) 0.000(5) -0.006(4) -0.004(5) O6 0.158(10) 0.185(11) 0.137(9) -0.022(8) 0.033(8) 0.055(9) O7 0.120(7) 0.157(9) 0.123(7) -0.017(7) -0.020(6) -0.022(7) O12 0.301(16) 0.131(10) 0.219(14) 0.021(10) 0.087(13) 0.085(11) O11 0.228(13) 0.086(7) 0.267(15) -0.006(8) 0.081(11) -0.050(8) O8 0.101(5) 0.099(6) 0.095(5) 0.007(5) 0.051(4) 0.009(5) O9 0.154(9) 0.083(6) 0.174(9) -0.013(6) 0.046(7) 0.024(6) O10 0.146(10) 0.36(2) 0.278(18) -0.107(17) 0.081(11) -0.166(13) N4 0.048(9) 0.023(8) 0.050(9) 0.021(6) 0.010(7) -0.006(6) C7 0.044(8) 0.041(10) 0.053(11) 0.015(9) 0.012(9) -0.002(7) N4' 0.082(16) 0.048(14) 0.082(16) 0.025(11) 0.054(14) 0.025(10) C7' 0.10(2) 0.068(17) 0.081(16) 0.037(14) 0.059(16) 0.043(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N4 2.27(2) . ? Cd1 N3 2.353(5) . ? Cd1 N2 2.372(6) . ? Cd1 N4' 2.38(2) . ? Cd1 O2 2.407(5) . ? Cd1 N1 2.440(6) . ? Cd1 O1 2.456(5) . ? Cd2 O4 2.317(5) . ? Cd2 O4 2.317(5) 5_667 ? Cd2 N7 2.372(5) 8_556 ? Cd2 N7 2.372(5) 4_556 ? Cd2 N6 2.383(5) . ? Cd2 N6 2.383(5) 5_667 ? C1 N1 1.461(9) . ? C1 C2 1.503(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N2 1.468(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.474(9) . ? C3 C4 1.526(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N3 1.460(9) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.463(12) . ? C5 N1 1.463(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N4 1.38(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 C11 1.336(14) . ? C8 C9 1.361(13) . ? C8 C7' 1.54(3) . ? C8 C7 1.57(2) . ? C9 C10 1.399(12) . ? C9 H9A 0.9300 . ? C10 N5 1.313(12) . ? C10 H10A 0.9300 . ? C11 C12 1.376(13) . ? C11 H11A 0.9300 . ? C12 N5 1.345(12) . ? C12 H12A 0.9300 . ? C13 C14 1.495(9) . ? C13 N2 1.495(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C17 1.369(9) . ? C14 C15 1.371(9) . ? C15 C16 1.364(9) . ? C15 H15A 0.9300 . ? C16 N6 1.355(8) . ? C16 H16A 0.9300 . ? C17 C18 1.394(9) . ? C17 H17A 0.9300 . ? C18 N6 1.319(8) . ? C18 H18A 0.9300 . ? C19 N3 1.475(8) . ? C19 C20 1.529(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.359(10) . ? C20 C23 1.371(10) . ? C21 C22 1.387(9) . ? C21 H21A 0.9300 . ? C22 N7 1.305(8) . ? C22 H22A 0.9300 . ? C23 C24 1.411(11) . ? C23 H23A 0.9300 . ? C24 N7 1.344(9) . ? C24 H24A 0.9300 . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? N7 Cd2 2.372(5) 4_546 ? N8 O1 1.226(8) . ? N8 O3 1.238(7) . ? N8 O2 1.250(7) . ? N9 O5 1.161(9) . ? N9 O7 1.175(12) . ? N9 O6 1.297(13) . ? N10 O10 1.158(12) . ? N10 O8 1.255(12) . ? N10 O9 1.288(13) . ? N4 C7 1.48(2) . ? N4 H4D 0.9100 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? N4' C7' 1.39(3) . ? N4' H4'A 0.9100 . ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? 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 N4 Cd1 N3 114.7(4) . . ? N4 Cd1 N2 115.4(4) . . ? N3 Cd1 N2 112.9(2) . . ? N4 Cd1 N4' 15.7(6) . . ? N3 Cd1 N4' 127.7(5) . . ? N2 Cd1 N4' 100.1(6) . . ? N4 Cd1 O2 135.1(6) . . ? N3 Cd1 O2 87.73(18) . . ? N2 Cd1 O2 86.74(19) . . ? N4' Cd1 O2 135.2(5) . . ? N4 Cd1 N1 76.8(6) . . ? N3 Cd1 N1 75.52(19) . . ? N2 Cd1 N1 75.6(2) . . ? N4' Cd1 N1 74.9(5) . . ? O2 Cd1 N1 148.13(17) . . ? N4 Cd1 O1 88.5(6) . . ? N3 Cd1 O1 134.21(19) . . ? N2 Cd1 O1 88.0(2) . . ? N4' Cd1 O1 84.0(5) . . ? O2 Cd1 O1 51.79(18) . . ? N1 Cd1 O1 150.2(2) . . ? O4 Cd2 O4 180 . 5_667 ? O4 Cd2 N7 90.25(19) . 8_556 ? O4 Cd2 N7 89.75(19) 5_667 8_556 ? O4 Cd2 N7 89.75(19) . 4_556 ? O4 Cd2 N7 90.25(19) 5_667 4_556 ? N7 Cd2 N7 180 8_556 4_556 ? O4 Cd2 N6 84.68(18) . . ? O4 Cd2 N6 95.32(18) 5_667 . ? N7 Cd2 N6 86.40(18) 8_556 . ? N7 Cd2 N6 93.60(18) 4_556 . ? O4 Cd2 N6 95.32(18) . 5_667 ? O4 Cd2 N6 84.68(18) 5_667 5_667 ? N7 Cd2 N6 93.60(18) 8_556 5_667 ? N7 Cd2 N6 86.40(18) 4_556 5_667 ? N6 Cd2 N6 180 . 5_667 ? N1 C1 C2 113.2(6) . . ? N1 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N1 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N2 C2 C1 112.5(6) . . ? N2 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N2 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? N1 C3 C4 112.2(6) . . ? N1 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N1 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N3 C4 C3 111.2(6) . . ? N3 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N3 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C6 C5 N1 114.5(7) . . ? C6 C5 H5A 107.8 . . ? N1 C5 H5A 108.6 . . ? C6 C5 H5B 109.4 . . ? N1 C5 H5B 108.8 . . ? H5A C5 H5B 107.6 . . ? N4 C6 C5 122.1(11) . . ? N4 C6 H6A 106.8 . . ? C5 C6 H6A 106.8 . . ? N4 C6 H6B 106.8 . . ? C5 C6 H6B 106.8 . . ? H6A C6 H6B 106.7 . . ? C11 C8 C9 117.6(8) . . ? C11 C8 C7' 135.5(14) . . ? C9 C8 C7' 106.3(13) . . ? C11 C8 C7 111.2(11) . . ? C9 C8 C7 131.0(10) . . ? C7' C8 C7 27.8(9) . . ? C8 C9 C10 119.5(9) . . ? C8 C9 H9A 120.2 . . ? C10 C9 H9A 120.2 . . ? N5 C10 C9 123.3(9) . . ? N5 C10 H10A 118.4 . . ? C9 C10 H10A 118.4 . . ? C8 C11 C12 120.4(10) . . ? C8 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? N5 C12 C11 123.3(10) . . ? N5 C12 H12A 118.3 . . ? C11 C12 H12A 118.3 . . ? C14 C13 N2 114.9(6) . . ? C14 C13 H13A 108.5 . . ? N2 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? N2 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C17 C14 C15 115.2(6) . . ? C17 C14 C13 121.8(6) . . ? C15 C14 C13 122.9(6) . . ? C16 C15 C14 121.9(7) . . ? C16 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? N6 C16 C15 122.2(6) . . ? N6 C16 H16A 118.9 . . ? C15 C16 H16A 118.9 . . ? C14 C17 C18 121.3(6) . . ? C14 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? N6 C18 C17 122.3(6) . . ? N6 C18 H18A 118.8 . . ? C17 C18 H18A 118.8 . . ? N3 C19 C20 113.7(6) . . ? N3 C19 H19A 108.8 . . ? C20 C19 H19A 108.8 . . ? N3 C19 H19B 108.8 . . ? C20 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C21 C20 C23 117.5(7) . . ? C21 C20 C19 119.4(6) . . ? C23 C20 C19 122.9(7) . . ? C20 C21 C22 119.5(7) . . ? C20 C21 H21A 120.2 . . ? C22 C21 H21A 120.2 . . ? N7 C22 C21 125.3(7) . . ? N7 C22 H22A 117.3 . . ? C21 C22 H22A 117.3 . . ? C20 C23 C24 119.0(7) . . ? C20 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? N7 C24 C23 123.2(7) . . ? N7 C24 H24A 118.4 . . ? C23 C24 H24A 118.4 . . ? C1 N1 C5 111.5(6) . . ? C1 N1 C3 112.4(6) . . ? C5 N1 C3 111.8(6) . . ? C1 N1 Cd1 107.4(4) . . ? C5 N1 Cd1 106.3(4) . . ? C3 N1 Cd1 107.0(4) . . ? C2 N2 C13 114.2(5) . . ? C2 N2 Cd1 107.1(4) . . ? C13 N2 Cd1 111.3(4) . . ? C2 N2 H2C 108.0 . . ? C13 N2 H2C 108.0 . . ? Cd1 N2 H2C 108.0 . . ? C4 N3 C19 114.4(6) . . ? C4 N3 Cd1 108.7(4) . . ? C19 N3 Cd1 112.0(4) . . ? C4 N3 H3C 107.1 . . ? C19 N3 H3C 107.1 . . ? Cd1 N3 H3C 107.1 . . ? C10 N5 C12 115.7(8) . . ? C18 N6 C16 116.9(5) . . ? C18 N6 Cd2 121.9(4) . . ? C16 N6 Cd2 121.1(4) . . ? C22 N7 C24 115.3(6) . . ? C22 N7 Cd2 121.8(4) . 4_546 ? C24 N7 Cd2 122.9(4) . 4_546 ? O1 N8 O3 121.0(6) . . ? O1 N8 O2 118.2(6) . . ? O3 N8 O2 120.8(6) . . ? O5 N9 O7 132.8(11) . . ? O5 N9 O6 111.8(11) . . ? O7 N9 O6 107.8(10) . . ? O10 N10 O8 122.6(15) . . ? O10 N10 O9 123.8(15) . . ? O8 N10 O9 113.3(10) . . ? N8 O1 Cd1 94.1(4) . . ? N8 O2 Cd1 95.8(4) . . ? C6 N4 C7 108.6(17) . . ? C6 N4 Cd1 110.3(12) . . ? C7 N4 Cd1 115.3(13) . . ? C6 N4 H4D 107.4 . . ? C7 N4 H4D 107.4 . . ? Cd1 N4 H4D 107.4 . . ? N4 C7 C8 111.1(15) . . ? N4 C7 H7B 109.4 . . ? C8 C7 H7B 109.4 . . ? N4 C7 H7C 109.4 . . ? C8 C7 H7C 109.4 . . ? H7B C7 H7C 108.0 . . ? C7' N4' Cd1 117.4(16) . . ? C7' N4' H4'A 104.7 . . ? Cd1 N4' H4'A 104.7 . . ? N4' C7' C8 106.7(18) . . ? N4' C7' H7'A 110.4 . . ? C8 C7' H7'A 110.4 . . ? N4' C7' H7'B 110.4 . . ? C8 C7' H7'B 110.4 . . ? H7'A C7' H7'B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.457 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.122 # Attachment '852453.CIF' data_a4 _database_code_depnum_ccdc_archive 'CCDC 852453' #TrackingRef '852453.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H47 Cl3 Mn1.50 N7 O7' _chemical_formula_weight 734.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1896(8) _cell_length_b 14.2875(13) _cell_length_c 27.356(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.552(8) _cell_angle_gamma 90.00 _cell_volume 3584.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7088 _cell_measurement_theta_min 2.0613 _cell_measurement_theta_max 27.4856 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1538 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9552 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27664 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7940 _reflns_number_gt 5466 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1435P)^2^+1.9723P] 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 7940 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.2457 _refine_ls_wR_factor_gt 0.2156 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.5000 0.0000 0.0000 0.0352(2) Uani 1 2 d S . . Mn2 Mn -0.00271(7) -0.28136(5) 0.16562(2) 0.0397(2) Uani 1 1 d . . . Cl1 Cl 0.25955(15) -0.25005(11) 0.17287(6) 0.0658(4) Uani 1 1 d . . . Cl2 Cl 0.69652(13) -0.10998(9) 0.03109(5) 0.0528(3) Uani 1 1 d . . . Cl3 Cl -0.0447(2) -0.09810(13) 0.29937(6) 0.0856(5) Uani 1 1 d . . . C1 C -0.2288(5) -0.3413(4) 0.08747(17) 0.0486(11) Uani 1 1 d . . . H1A H -0.2027 -0.4043 0.0980 0.058 Uiso 1 1 calc R . . H1B H -0.2782 -0.3450 0.0552 0.058 Uiso 1 1 calc R . . C2 C -0.3296(5) -0.2975(4) 0.12326(17) 0.0478(11) Uani 1 1 d . . . H2A H -0.3642 -0.2376 0.1105 0.057 Uiso 1 1 calc R . . H2B H -0.4136 -0.3377 0.1263 0.057 Uiso 1 1 calc R . . C3 C -0.2805(6) -0.3640(4) 0.20456(19) 0.0557(13) Uani 1 1 d . . . H3A H -0.2634 -0.4217 0.1871 0.067 Uiso 1 1 calc R . . H3B H -0.3816 -0.3636 0.2128 0.067 Uiso 1 1 calc R . . C4 C -0.1835(6) -0.3618(5) 0.2511(2) 0.0675(17) Uani 1 1 d . . . H4A H -0.2313 -0.3250 0.2752 0.081 Uiso 1 1 calc R . . H4B H -0.1738 -0.4251 0.2637 0.081 Uiso 1 1 calc R . . C5 C -0.2211(6) -0.1123(3) 0.1714(2) 0.0526(12) Uani 1 1 d . . . H5A H -0.2515 -0.1073 0.1369 0.063 Uiso 1 1 calc R . . H5B H -0.2476 -0.0547 0.1874 0.063 Uiso 1 1 calc R . . C6 C -0.2984(6) -0.1936(4) 0.19356(19) 0.0522(12) Uani 1 1 d . . . H6A H -0.2758 -0.1945 0.2287 0.063 Uiso 1 1 calc R . . H6B H -0.4029 -0.1855 0.1879 0.063 Uiso 1 1 calc R . . C7 C -0.0025(6) -0.3192(4) 0.04695(19) 0.0550(12) Uani 1 1 d . . . H7A H -0.0634 -0.3325 0.0175 0.066 Uiso 1 1 calc R . . H7B H 0.0432 -0.3773 0.0580 0.066 Uiso 1 1 calc R . . C8 C 0.1146(6) -0.2494(4) 0.03501(16) 0.0464(11) Uani 1 1 d . . . C9 C 0.2574(6) -0.2729(4) 0.03601(19) 0.0562(13) Uani 1 1 d . . . H9A H 0.2862 -0.3335 0.0446 0.067 Uiso 1 1 calc R . . C10 C 0.3612(6) -0.2072(4) 0.0243(2) 0.0552(12) Uani 1 1 d . . . H10A H 0.4583 -0.2258 0.0250 0.066 Uiso 1 1 calc R . . C11 C 0.1878(6) -0.0965(4) 0.01122(18) 0.0533(12) Uani 1 1 d . . . H11A H 0.1611 -0.0355 0.0029 0.064 Uiso 1 1 calc R . . C12 C 0.0788(6) -0.1581(4) 0.0218(2) 0.0548(12) Uani 1 1 d . . . H12A H -0.0179 -0.1387 0.0202 0.066 Uiso 1 1 calc R . . C13 C 0.0173(7) -0.0608(4) 0.1448(2) 0.0593(13) Uani 1 1 d . . . H13A H -0.0108 -0.0759 0.1109 0.071 Uiso 1 1 calc R . . H13B H 0.1209 -0.0729 0.1500 0.071 Uiso 1 1 calc R . . C14 C -0.0087(6) 0.0419(3) 0.15251(19) 0.0538(12) Uani 1 1 d . . . C15 C 0.0460(6) 0.0880(4) 0.1930(2) 0.0603(13) Uani 1 1 d . . . H15A H 0.0977 0.0556 0.2180 0.072 Uiso 1 1 calc R . . C16 C 0.0244(7) 0.1838(4) 0.1971(3) 0.0730(17) Uani 1 1 d . . . H16A H 0.0640 0.2138 0.2250 0.088 Uiso 1 1 calc R . . C17 C -0.1148(12) 0.1880(6) 0.1251(4) 0.117(3) Uani 1 1 d . . . H17A H -0.1740 0.2210 0.1023 0.141 Uiso 1 1 calc R . . C18 C -0.0964(10) 0.0930(5) 0.1185(3) 0.097(3) Uani 1 1 d . . . H18A H -0.1424 0.0631 0.0916 0.116 Uiso 1 1 calc R . . C19 C 0.0807(7) -0.3663(6) 0.2716(2) 0.088(2) Uani 1 1 d . . . H19A H 0.1627 -0.3235 0.2718 0.106 Uiso 1 1 calc R . . H19B H 0.1067 -0.4212 0.2532 0.106 Uiso 1 1 calc R . . C20 C 0.0627(6) -0.3964(5) 0.32405(18) 0.0620(15) Uani 1 1 d . . . C21 C 0.0708(6) -0.4877(4) 0.33746(17) 0.0598(14) Uani 1 1 d . . . H21A H 0.0871 -0.5332 0.3141 0.072 Uiso 1 1 calc R . . C22 C 0.0551(6) -0.5140(4) 0.38539(16) 0.0522(12) Uani 1 1 d . . . H22A H 0.0596 -0.5774 0.3932 0.063 Uiso 1 1 calc R . . C23 C 0.0268(8) -0.3632(5) 0.4082(2) 0.080(2) Uani 1 1 d . . . H23A H 0.0120 -0.3188 0.4322 0.096 Uiso 1 1 calc R . . C24 C 0.0407(9) -0.3326(5) 0.3603(2) 0.088(2) Uani 1 1 d . . . H24A H 0.0350 -0.2691 0.3530 0.105 Uiso 1 1 calc R . . N1 N -0.2544(4) -0.2837(3) 0.17212(13) 0.0407(8) Uani 1 1 d . . . N2 N -0.0952(4) -0.2833(3) 0.08553(13) 0.0435(9) Uani 1 1 d . . . H2C H -0.1230 -0.2240 0.0772 0.052 Uiso 1 1 calc R . . N3 N -0.0618(4) -0.1248(3) 0.17687(14) 0.0456(9) Uani 1 1 d . . . H3C H -0.0334 -0.1100 0.2084 0.055 Uiso 1 1 calc R . . N4 N -0.0371(5) -0.3234(4) 0.24617(16) 0.0664(13) Uani 1 1 d . . . H4C H -0.0419 -0.2670 0.2614 0.080 Uiso 1 1 calc R . . N5 N 0.3288(4) -0.1185(3) 0.01213(13) 0.0401(8) Uani 1 1 d . . . N6 N -0.0492(8) 0.2349(4) 0.1636(3) 0.0957(19) Uani 1 1 d . . . N7 N 0.0337(4) -0.4528(3) 0.42112(13) 0.0485(9) Uani 1 1 d . . . O1 O 0.0380(5) -0.4337(3) 0.15291(15) 0.0691(11) Uani 1 1 d . . . O2 O -0.1170(10) 0.4203(4) 0.1835(5) 0.240(6) Uani 1 1 d . . . O3 O 0.2155(14) 0.4066(12) 0.2399(6) 0.285(8) Uani 1 1 d . . . O4 O 0.247(3) -0.5388(18) 0.0495(9) 0.444(13) Uiso 1 1 d . . . O5 O -0.404(2) -0.0717(16) 0.4419(7) 0.375(10) Uiso 1 1 d . . . O6 O -0.146(2) -0.1156(14) 0.4125(7) 0.352(10) Uani 1 1 d . . . O7 O 0.3312(7) -0.4605(6) 0.1384(3) 0.147(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0345(5) 0.0422(5) 0.0287(4) 0.0026(3) 0.0014(3) 0.0011(4) Mn2 0.0377(4) 0.0394(4) 0.0423(4) 0.0099(3) 0.0043(3) -0.0014(3) Cl1 0.0406(8) 0.0769(10) 0.0802(9) 0.0148(7) 0.0050(6) -0.0030(6) Cl2 0.0402(7) 0.0548(7) 0.0629(7) 0.0218(5) -0.0006(5) 0.0035(5) Cl3 0.1042(14) 0.0742(11) 0.0784(10) -0.0076(8) 0.0046(9) 0.0045(9) C1 0.043(3) 0.054(3) 0.049(2) 0.002(2) 0.005(2) -0.015(2) C2 0.037(3) 0.056(3) 0.050(2) 0.006(2) 0.001(2) -0.009(2) C3 0.049(3) 0.054(3) 0.064(3) 0.020(2) 0.012(2) -0.008(2) C4 0.048(3) 0.100(5) 0.055(3) 0.037(3) 0.010(2) -0.003(3) C5 0.046(3) 0.041(3) 0.070(3) -0.001(2) 0.002(2) 0.001(2) C6 0.045(3) 0.053(3) 0.059(3) -0.002(2) 0.011(2) 0.003(2) C7 0.059(3) 0.052(3) 0.055(3) -0.004(2) 0.014(2) -0.009(2) C8 0.050(3) 0.052(3) 0.037(2) 0.0006(18) 0.0068(19) -0.011(2) C9 0.060(4) 0.043(3) 0.066(3) 0.010(2) 0.010(3) 0.000(2) C10 0.046(3) 0.051(3) 0.068(3) 0.006(2) 0.002(2) 0.000(2) C11 0.052(3) 0.051(3) 0.058(3) 0.012(2) 0.012(2) 0.003(2) C12 0.040(3) 0.055(3) 0.071(3) 0.016(2) 0.013(2) 0.001(2) C13 0.075(4) 0.039(3) 0.065(3) 0.005(2) 0.014(3) -0.006(2) C14 0.064(3) 0.038(2) 0.061(3) 0.004(2) 0.014(2) -0.006(2) C15 0.061(3) 0.050(3) 0.070(3) -0.007(2) 0.006(3) -0.004(3) C16 0.063(4) 0.055(3) 0.102(5) -0.022(3) 0.013(3) -0.006(3) C17 0.153(9) 0.073(5) 0.125(7) 0.036(5) -0.008(6) 0.017(6) C18 0.153(8) 0.058(4) 0.077(4) 0.001(3) -0.018(5) 0.010(4) C19 0.061(4) 0.154(7) 0.051(3) 0.043(4) 0.006(3) 0.021(4) C20 0.047(3) 0.099(5) 0.040(2) 0.017(3) 0.004(2) 0.009(3) C21 0.059(3) 0.087(4) 0.034(2) 0.000(2) 0.006(2) -0.009(3) C22 0.057(3) 0.063(3) 0.036(2) -0.002(2) 0.003(2) -0.013(2) C23 0.121(6) 0.066(4) 0.055(3) 0.008(3) 0.023(3) 0.019(4) C24 0.126(6) 0.074(4) 0.065(4) 0.033(3) 0.028(4) 0.030(4) N1 0.036(2) 0.045(2) 0.0419(18) 0.0105(15) 0.0051(15) -0.0036(16) N2 0.044(2) 0.042(2) 0.0451(19) 0.0058(15) 0.0105(16) -0.0057(17) N3 0.047(2) 0.041(2) 0.049(2) 0.0071(16) 0.0028(17) -0.0053(17) N4 0.051(3) 0.097(4) 0.051(2) 0.029(2) 0.001(2) -0.010(3) N5 0.036(2) 0.044(2) 0.0399(18) 0.0047(14) 0.0032(15) -0.0008(16) N6 0.102(5) 0.049(3) 0.136(6) -0.005(3) 0.008(4) -0.001(3) N7 0.055(3) 0.055(2) 0.0361(18) 0.0037(16) 0.0057(17) 0.0000(19) O1 0.077(3) 0.049(2) 0.081(3) 0.0127(18) 0.006(2) 0.0084(19) O2 0.169(8) 0.045(3) 0.522(19) 0.018(6) 0.165(10) 0.001(4) O3 0.204(12) 0.34(2) 0.302(17) -0.098(14) -0.017(10) 0.023(12) O6 0.37(2) 0.35(3) 0.35(2) 0.041(17) 0.144(18) 0.013(17) O7 0.099(5) 0.132(6) 0.210(8) 0.017(6) 0.014(5) 0.028(4) _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 Mn1 N7 2.300(4) 4_655 ? Mn1 N7 2.300(4) 2 ? Mn1 N5 2.348(4) 3_655 ? Mn1 N5 2.348(4) . ? Mn1 Cl2 2.5027(11) . ? Mn1 Cl2 2.5027(11) 3_655 ? Mn2 O1 2.239(4) . ? Mn2 N2 2.301(4) . ? Mn2 N4 2.324(4) . ? Mn2 N3 2.327(4) . ? Mn2 N1 2.331(4) . ? Mn2 Cl1 2.4471(15) . ? C1 N2 1.485(6) . ? C1 C2 1.524(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N1 1.479(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.480(6) . ? C3 C4 1.509(7) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N4 1.467(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 N3 1.472(7) . ? C5 C6 1.508(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N1 1.482(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.488(6) . ? C7 C8 1.518(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.353(7) . ? C8 C12 1.387(7) . ? C9 C10 1.391(7) . ? C9 H9A 0.9300 . ? C10 N5 1.339(6) . ? C10 H10A 0.9300 . ? C11 N5 1.333(6) . ? C11 C12 1.378(7) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 N3 1.488(6) . ? C13 C14 1.504(7) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.359(7) . ? C14 C18 1.398(9) . ? C15 C16 1.388(8) . ? C15 H15A 0.9300 . ? C16 N6 1.324(9) . ? C16 H16A 0.9300 . ? C17 N6 1.359(11) . ? C17 C18 1.380(11) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 N4 1.392(7) . ? C19 C20 1.516(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.356(9) . ? C20 C24 1.372(9) . ? C21 C22 1.380(6) . ? C21 H21A 0.9300 . ? C22 N7 1.335(6) . ? C22 H22A 0.9300 . ? C23 N7 1.328(7) . ? C23 C24 1.394(8) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? N4 H4C 0.9100 . ? N7 Mn1 2.300(4) 2_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Mn1 N7 180 4_655 2 ? N7 Mn1 N5 87.04(14) 4_655 3_655 ? N7 Mn1 N5 92.96(14) 2 3_655 ? N7 Mn1 N5 92.96(14) 4_655 . ? N7 Mn1 N5 87.04(14) 2 . ? N5 Mn1 N5 180 3_655 . ? N7 Mn1 Cl2 89.92(11) 4_655 . ? N7 Mn1 Cl2 90.08(11) 2 . ? N5 Mn1 Cl2 91.43(9) 3_655 . ? N5 Mn1 Cl2 88.57(9) . . ? N7 Mn1 Cl2 90.08(11) 4_655 3_655 ? N7 Mn1 Cl2 89.92(11) 2 3_655 ? N5 Mn1 Cl2 88.57(9) 3_655 3_655 ? N5 Mn1 Cl2 91.43(9) . 3_655 ? Cl2 Mn1 Cl2 180 . 3_655 ? O1 Mn2 N2 84.03(14) . . ? O1 Mn2 N4 85.97(18) . . ? N2 Mn2 N4 146.71(15) . . ? O1 Mn2 N3 176.01(15) . . ? N2 Mn2 N3 93.55(14) . . ? N4 Mn2 N3 94.40(18) . . ? O1 Mn2 N1 100.03(14) . . ? N2 Mn2 N1 76.28(13) . . ? N4 Mn2 N1 74.34(14) . . ? N3 Mn2 N1 76.27(14) . . ? O1 Mn2 Cl1 90.97(12) . . ? N2 Mn2 Cl1 112.53(10) . . ? N4 Mn2 Cl1 99.29(12) . . ? N3 Mn2 Cl1 92.89(11) . . ? N1 Mn2 Cl1 166.74(11) . . ? N2 C1 C2 109.3(4) . . ? N2 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? N2 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N1 C2 C1 111.5(4) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N1 C3 C4 112.4(4) . . ? N1 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N1 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? N4 C4 C3 115.3(4) . . ? N4 C4 H4A 108.5 . . ? C3 C4 H4A 108.5 . . ? N4 C4 H4B 108.5 . . ? C3 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? N3 C5 C6 110.8(4) . . ? N3 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? N1 C6 C5 111.3(4) . . ? N1 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N1 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 111.8(4) . . ? N2 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C12 116.9(5) . . ? C9 C8 C7 122.2(5) . . ? C12 C8 C7 120.9(5) . . ? C8 C9 C10 120.4(5) . . ? C8 C9 H9A 119.8 . . ? C10 C9 H9A 119.8 . . ? N5 C10 C9 123.5(5) . . ? N5 C10 H10A 118.3 . . ? C9 C10 H10A 118.3 . . ? N5 C11 C12 124.3(5) . . ? N5 C11 H11A 117.8 . . ? C12 C11 H11A 117.8 . . ? C11 C12 C8 119.5(5) . . ? C11 C12 H12A 120.3 . . ? C8 C12 H12A 120.3 . . ? N3 C13 C14 115.4(4) . . ? N3 C13 H13A 108.4 . . ? C14 C13 H13A 108.4 . . ? N3 C13 H13B 108.4 . . ? C14 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C15 C14 C18 117.2(5) . . ? C15 C14 C13 122.3(5) . . ? C18 C14 C13 120.5(5) . . ? C14 C15 C16 119.7(6) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? N6 C16 C15 124.0(6) . . ? N6 C16 H16A 118.0 . . ? C15 C16 H16A 118.0 . . ? N6 C17 C18 122.2(7) . . ? N6 C17 H17A 118.9 . . ? C18 C17 H17A 118.9 . . ? C17 C18 C14 119.9(7) . . ? C17 C18 H18A 120.1 . . ? C14 C18 H18A 120.1 . . ? N4 C19 C20 118.1(5) . . ? N4 C19 H19A 107.8 . . ? C20 C19 H19A 107.8 . . ? N4 C19 H19B 107.8 . . ? C20 C19 H19B 107.8 . . ? H19A C19 H19B 107.1 . . ? C21 C20 C24 116.9(5) . . ? C21 C20 C19 121.5(6) . . ? C24 C20 C19 121.6(6) . . ? C20 C21 C22 120.8(5) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? N7 C22 C21 123.1(5) . . ? N7 C22 H22A 118.4 . . ? C21 C22 H22A 118.4 . . ? N7 C23 C24 123.1(6) . . ? N7 C23 H23A 118.4 . . ? C24 C23 H23A 118.4 . . ? C20 C24 C23 119.8(6) . . ? C20 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C3 N1 C2 110.8(4) . . ? C3 N1 C6 112.2(4) . . ? C2 N1 C6 110.4(4) . . ? C3 N1 Mn2 104.8(3) . . ? C2 N1 Mn2 110.1(3) . . ? C6 N1 Mn2 108.3(3) . . ? C1 N2 C7 110.1(4) . . ? C1 N2 Mn2 103.3(3) . . ? C7 N2 Mn2 119.1(3) . . ? C1 N2 H2C 108.0 . . ? C7 N2 H2C 108.0 . . ? Mn2 N2 H2C 108.0 . . ? C5 N3 C13 112.6(4) . . ? C5 N3 Mn2 110.0(3) . . ? C13 N3 Mn2 112.7(3) . . ? C5 N3 H3C 107.1 . . ? C13 N3 H3C 107.1 . . ? Mn2 N3 H3C 107.1 . . ? C19 N4 C4 118.6(5) . . ? C19 N4 Mn2 116.2(4) . . ? C4 N4 Mn2 111.3(3) . . ? C19 N4 H4C 102.6 . . ? C4 N4 H4C 102.6 . . ? Mn2 N4 H4C 102.6 . . ? C11 N5 C10 115.4(4) . . ? C11 N5 Mn1 119.1(3) . . ? C10 N5 Mn1 125.2(3) . . ? C16 N6 C17 116.6(6) . . ? C23 N7 C22 116.3(4) . . ? C23 N7 Mn1 121.7(4) . 2_545 ? C22 N7 Mn1 122.0(3) . 2_545 ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.734 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.099