Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Vernon Gibson' _publ_contact_author_address ; Department of Chemistry Imperial College London Exhibition Road London SW72AZ UNITED KINGDOM ; _publ_contact_author_email V.GIBSON@IMPERIAL.AC.UK _publ_section_title ; Synthesis and Stuctures of Bimetallic and Polymeric Zinc Coordination Compounds Supported by Salicylaldiminato and Anilido-aldimine Ligands ; loop_ _publ_author_name 'Vernon Gibson' 'David J. Doyle' 'Andrew J. P. White' # Attachment 'Dalton_09-06_2.cif' data_Compound_2b _database_code_depnum_ccdc_archive 'CCDC 621015' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H60 N2 O2 Zn2' _chemical_formula_weight 707.62 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 Orthorhombic _symmetry_space_group_name_H-M Aba2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 18.1320(8) _cell_length_b 18.8215(7) _cell_length_c 23.1100(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7886.8(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.8450 _cell_measurement_theta_max 32.5695 _exptl_crystal_description plates _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3024 _exptl_absorpt_coefficient_mu 1.248 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.67462 _exptl_absorpt_correction_T_max 0.95857 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35788 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 4.05 _diffrn_reflns_theta_max 32.61 _reflns_number_total 12497 _reflns_number_gt 11979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. ; #Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0646 _refine_ls_wR_factor_obs+ 0.1524 _refine_ls_abs_structure_Flack+ 0.260(12) _refine_ls_R_factor_obs- 0.0726 _refine_ls_wR_factor_obs- 0.1715 _refine_ls_abs_structure_Flack- 0.740(12) _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^)+(0.0692P)^2^+11.1334P] 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 SHELXL _refine_ls_extinction_coef 0.00067(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.260(12) _refine_ls_number_reflns 12497 _refine_ls_number_parameters 404 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.172 _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 0.626192(18) 0.339164(18) 0.529199(19) 0.02837(9) Uani 1 1 d . . . Zn2 Zn 0.61837(2) 0.193449(19) 0.474042(18) 0.03070(10) Uani 1 1 d D A . O1 O 0.62613(11) 0.23757(12) 0.55810(11) 0.0260(4) Uani 1 1 d . . . C1 C 0.67022(16) 0.21874(14) 0.60181(13) 0.0237(5) Uani 1 1 d . . . C2 C 0.64641(17) 0.16930(17) 0.64456(15) 0.0279(6) Uani 1 1 d . . . C3 C 0.69617(18) 0.14809(17) 0.68712(15) 0.0291(6) Uani 1 1 d . . . H3A H 0.6796 0.1151 0.7154 0.035 Uiso 1 1 calc R . . C4 C 0.76907(18) 0.17222(16) 0.69096(15) 0.0290(6) Uani 1 1 d . . . C5 C 0.79118(17) 0.22123(16) 0.64973(15) 0.0286(6) Uani 1 1 d . . . H5A H 0.8405 0.2383 0.6505 0.034 Uiso 1 1 calc R . . C6 C 0.74282(16) 0.24643(15) 0.60670(14) 0.0247(5) Uani 1 1 d . . . C7 C 0.77314(18) 0.30357(16) 0.57133(15) 0.0285(6) Uani 1 1 d . . . H7A H 0.8253 0.3084 0.5717 0.034 Uiso 1 1 calc R . . N7 N 0.73797(14) 0.34792(13) 0.53985(13) 0.0278(5) Uani 1 1 d . . . C8 C 0.77935(19) 0.40458(16) 0.51029(16) 0.0313(6) Uani 1 1 d . . . H8A H 0.7751 0.3983 0.4679 0.038 Uiso 1 1 calc R . . H8B H 0.8322 0.4012 0.5208 0.038 Uiso 1 1 calc R . . C9 C 0.74995(19) 0.47734(15) 0.52718(17) 0.0315(6) Uani 1 1 d . . . H9A H 0.7628 0.4870 0.5681 0.038 Uiso 1 1 calc R . . H9B H 0.6955 0.4772 0.5240 0.038 Uiso 1 1 calc R . . C10 C 0.71886(19) 0.03658(16) 0.48908(15) 0.0312(6) Uani 1 1 d . . . H10A H 0.6650 0.0407 0.4953 0.037 Uiso 1 1 calc R . . H10B H 0.7275 0.0252 0.4478 0.037 Uiso 1 1 calc R . . C11 C 0.7565(2) 0.10683(16) 0.50443(18) 0.0358(7) Uani 1 1 d . . . H11A H 0.7498 0.1165 0.5462 0.043 Uiso 1 1 calc R . . H11B H 0.8101 0.1027 0.4969 0.043 Uiso 1 1 calc R . . N12 N 0.72656(17) 0.16666(13) 0.47082(14) 0.0307(5) Uani 1 1 d . . . C12 C 0.7714(2) 0.20356(17) 0.43999(16) 0.0314(6) Uani 1 1 d . . . H12A H 0.8216 0.1890 0.4412 0.038 Uiso 1 1 calc R . . C13 C 0.75569(18) 0.26457(16) 0.40359(14) 0.0280(6) Uani 1 1 d . . . C14 C 0.81213(18) 0.28136(17) 0.36418(16) 0.0312(6) Uani 1 1 d . . . H14A H 0.8557 0.2533 0.3642 0.037 Uiso 1 1 calc R . . C15 C 0.80678(18) 0.33668(17) 0.32558(15) 0.0291(6) Uani 1 1 d . . . C16 C 0.74111(18) 0.37598(17) 0.32692(14) 0.0287(6) Uani 1 1 d . . . H16A H 0.7364 0.4147 0.3008 0.034 Uiso 1 1 calc R . . C17 C 0.68217(16) 0.36183(15) 0.36414(14) 0.0252(5) Uani 1 1 d . . . C18 C 0.69010(17) 0.30653(15) 0.40576(13) 0.0245(5) Uani 1 1 d . . . O18 O 0.63759(13) 0.29389(11) 0.44554(11) 0.0263(4) Uani 1 1 d . . . C19 C 0.56760(17) 0.13812(18) 0.64393(16) 0.0304(6) Uani 1 1 d . . . C20 C 0.50870(19) 0.1971(2) 0.6391(2) 0.0399(8) Uani 1 1 d . . . H20A H 0.4595 0.1757 0.6389 0.060 Uiso 1 1 calc R . . H20B H 0.5162 0.2238 0.6031 0.060 Uiso 1 1 calc R . . H20C H 0.5131 0.2294 0.6722 0.060 Uiso 1 1 calc R . . C21 C 0.5594(2) 0.0863(2) 0.59316(19) 0.0398(8) Uani 1 1 d . . . H21A H 0.5093 0.0667 0.5929 0.060 Uiso 1 1 calc R . . H21B H 0.5951 0.0475 0.5974 0.060 Uiso 1 1 calc R . . H21C H 0.5685 0.1114 0.5567 0.060 Uiso 1 1 calc R . . C22 C 0.5505(2) 0.0960(3) 0.6992(2) 0.0472(10) Uani 1 1 d . . . H22A H 0.5001 0.0772 0.6971 0.071 Uiso 1 1 calc R . . H22B H 0.5550 0.1273 0.7329 0.071 Uiso 1 1 calc R . . H22C H 0.5854 0.0565 0.7028 0.071 Uiso 1 1 calc R . . C23 C 0.82243(19) 0.14636(18) 0.73784(17) 0.0338(7) Uani 1 1 d . . . C24 C 0.8828(2) 0.1006(3) 0.7095(2) 0.0480(10) Uani 1 1 d . . . H24A H 0.8601 0.0595 0.6906 0.072 Uiso 1 1 calc R . . H24B H 0.9174 0.0843 0.7393 0.072 Uiso 1 1 calc R . . H24C H 0.9093 0.1290 0.6807 0.072 Uiso 1 1 calc R . . C25 C 0.7844(2) 0.1025(2) 0.7849(2) 0.0460(9) Uani 1 1 d . . . H25A H 0.7607 0.0610 0.7673 0.069 Uiso 1 1 calc R . . H25B H 0.7471 0.1317 0.8043 0.069 Uiso 1 1 calc R . . H25C H 0.8211 0.0867 0.8133 0.069 Uiso 1 1 calc R . . C26 C 0.8584(3) 0.2110(2) 0.76762(19) 0.0441(9) Uani 1 1 d . . . H26A H 0.8201 0.2401 0.7858 0.066 Uiso 1 1 calc R . . H26B H 0.8849 0.2394 0.7387 0.066 Uiso 1 1 calc R . . H26C H 0.8932 0.1945 0.7972 0.066 Uiso 1 1 calc R . . C27 C 0.86832(19) 0.3569(2) 0.28326(18) 0.0354(7) Uani 1 1 d . . . C28 C 0.9291(3) 0.3001(2) 0.2813(3) 0.0518(11) Uani 1 1 d . . . H28A H 0.9079 0.2549 0.2683 0.078 Uiso 1 1 calc R . . H28B H 0.9502 0.2941 0.3200 0.078 Uiso 1 1 calc R . . H28C H 0.9678 0.3150 0.2543 0.078 Uiso 1 1 calc R . . C29 C 0.8371(3) 0.3665(4) 0.2228(2) 0.0619(14) Uani 1 1 d . . . H29A H 0.7982 0.4026 0.2236 0.093 Uiso 1 1 calc R . . H29B H 0.8165 0.3213 0.2092 0.093 Uiso 1 1 calc R . . H29C H 0.8765 0.3817 0.1965 0.093 Uiso 1 1 calc R . . C30 C 0.9031(3) 0.4266(2) 0.3036(3) 0.0505(10) Uani 1 1 d . . . H30A H 0.8652 0.4637 0.3051 0.076 Uiso 1 1 calc R . . H30B H 0.9419 0.4408 0.2765 0.076 Uiso 1 1 calc R . . H30C H 0.9243 0.4200 0.3422 0.076 Uiso 1 1 calc R . . C31 C 0.61132(17) 0.40695(17) 0.35987(16) 0.0292(6) Uani 1 1 d . . . C32 C 0.6100(2) 0.4520(2) 0.3041(2) 0.0451(10) Uani 1 1 d . . . H32A H 0.6530 0.4836 0.3035 0.068 Uiso 1 1 calc R . . H32B H 0.5648 0.4805 0.3031 0.068 Uiso 1 1 calc R . . H32C H 0.6114 0.4206 0.2703 0.068 Uiso 1 1 calc R . . C33 C 0.6061(2) 0.4580(2) 0.4116(2) 0.0430(9) Uani 1 1 d . . . H33A H 0.6500 0.4883 0.4127 0.064 Uiso 1 1 calc R . . H33B H 0.6029 0.4305 0.4475 0.064 Uiso 1 1 calc R . . H33C H 0.5620 0.4877 0.4076 0.064 Uiso 1 1 calc R . . C34 C 0.54220(19) 0.3584(2) 0.3576(2) 0.0396(8) Uani 1 1 d . . . H34A H 0.4977 0.3878 0.3550 0.059 Uiso 1 1 calc R . . H34B H 0.5400 0.3294 0.3928 0.059 Uiso 1 1 calc R . . H34C H 0.5452 0.3273 0.3237 0.059 Uiso 1 1 calc R . . C35 C 0.5436(2) 0.3995(2) 0.5559(2) 0.0451(9) Uani 1 1 d . . . H35A H 0.5423 0.3976 0.5987 0.054 Uiso 1 1 calc R . . H35B H 0.5546 0.4492 0.5448 0.054 Uiso 1 1 calc R . . C36 C 0.4682(2) 0.3812(3) 0.5337(3) 0.0623(13) Uani 1 1 d . . . H36A H 0.4320 0.4144 0.5499 0.094 Uiso 1 1 calc R . . H36B H 0.4555 0.3327 0.5453 0.094 Uiso 1 1 calc R . . H36D H 0.4677 0.3847 0.4914 0.094 Uiso 1 1 calc R . . C37 C 0.5297(3) 0.1471(3) 0.4439(2) 0.0581(14) Uani 1 1 d D . . H37A H 0.5319 0.1479 0.4011 0.070 Uiso 0.751(18) 1 calc PR A 1 H37B H 0.5302 0.0968 0.4563 0.070 Uiso 0.751(18) 1 calc PR A 1 H37C H 0.5282 0.1574 0.4033 0.070 Uiso 0.249(18) 1 d PR A 2 H37D H 0.4887 0.1716 0.4609 0.070 Uiso 0.249(18) 1 d PR A 2 C38 C 0.4593(3) 0.1792(5) 0.4624(4) 0.070(3) Uani 0.751(18) 1 d PD A 1 H38A H 0.4182 0.1527 0.4454 0.105 Uiso 0.751(18) 1 calc PR A 1 H38B H 0.4573 0.2287 0.4494 0.105 Uiso 0.751(18) 1 calc PR A 1 H38C H 0.4557 0.1776 0.5047 0.105 Uiso 0.751(18) 1 calc PR A 1 C38' C 0.5117(12) 0.0715(6) 0.4502(12) 0.068(7) Uiso 0.249(18) 1 d PD A 2 H38D H 0.4642 0.0618 0.4317 0.101 Uiso 0.249(18) 1 calc PR A 2 H38E H 0.5089 0.0594 0.4914 0.101 Uiso 0.249(18) 1 calc PR A 2 H38F H 0.5502 0.0428 0.4317 0.101 Uiso 0.249(18) 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 Zn1 0.02778(15) 0.01977(15) 0.03755(19) 0.00565(14) 0.00156(15) 0.00193(11) Zn2 0.03504(18) 0.02063(15) 0.0364(2) 0.00608(14) -0.00844(17) -0.00320(12) O1 0.0272(10) 0.0202(9) 0.0305(11) 0.0103(8) -0.0037(7) -0.0027(7) C1 0.0245(12) 0.0180(11) 0.0285(14) 0.0019(9) 0.0012(10) -0.0041(9) C2 0.0245(12) 0.0260(13) 0.0333(15) 0.0041(11) 0.0011(11) -0.0025(10) C3 0.0291(14) 0.0278(14) 0.0303(15) 0.0066(11) -0.0011(11) 0.0005(11) C4 0.0300(14) 0.0208(12) 0.0362(16) 0.0031(11) -0.0021(12) 0.0018(10) C5 0.0264(12) 0.0238(12) 0.0356(16) 0.0052(11) 0.0006(11) -0.0033(10) C6 0.0239(12) 0.0203(11) 0.0299(14) 0.0048(10) 0.0008(10) -0.0002(9) C7 0.0291(13) 0.0214(12) 0.0349(16) 0.0038(11) 0.0000(11) -0.0029(10) N7 0.0289(11) 0.0182(10) 0.0364(15) 0.0057(9) 0.0011(10) -0.0040(8) C8 0.0362(15) 0.0201(12) 0.0375(16) 0.0078(11) 0.0009(12) -0.0064(11) C9 0.0418(15) 0.0179(11) 0.0350(15) 0.0065(11) 0.0022(14) -0.0068(10) C10 0.0374(15) 0.0199(12) 0.0362(17) 0.0052(10) -0.0004(12) 0.0071(11) C11 0.0468(19) 0.0192(12) 0.0413(18) 0.0054(12) -0.0109(15) 0.0060(12) N12 0.0399(14) 0.0173(10) 0.0349(14) 0.0043(10) -0.0043(12) 0.0046(9) C12 0.0388(16) 0.0239(13) 0.0316(16) 0.0003(11) -0.0070(13) 0.0076(12) C13 0.0308(14) 0.0213(12) 0.0319(15) 0.0031(10) -0.0012(11) 0.0028(10) C14 0.0300(14) 0.0254(13) 0.0382(17) -0.0005(12) -0.0026(12) 0.0039(11) C15 0.0300(14) 0.0254(13) 0.0319(15) -0.0004(11) 0.0004(11) -0.0006(11) C16 0.0326(14) 0.0240(13) 0.0293(14) 0.0062(10) -0.0026(11) 0.0002(11) C17 0.0261(12) 0.0184(11) 0.0312(14) 0.0046(10) -0.0044(11) 0.0018(9) C18 0.0280(13) 0.0206(12) 0.0250(13) 0.0023(9) -0.0021(10) -0.0007(10) O18 0.0306(10) 0.0178(9) 0.0303(11) 0.0067(8) -0.0015(9) 0.0006(8) C19 0.0275(13) 0.0300(14) 0.0339(15) 0.0091(12) -0.0006(11) -0.0075(11) C20 0.0270(15) 0.0420(19) 0.051(2) 0.0033(15) 0.0024(14) 0.0007(13) C21 0.0447(19) 0.0307(16) 0.044(2) 0.0027(14) 0.0010(15) -0.0142(14) C22 0.0384(18) 0.057(2) 0.046(2) 0.0206(19) 0.0049(15) -0.0143(17) C23 0.0317(15) 0.0293(15) 0.0403(18) 0.0067(13) -0.0063(13) 0.0036(12) C24 0.044(2) 0.044(2) 0.055(3) 0.0036(19) -0.0062(18) 0.0163(17) C25 0.0413(19) 0.052(2) 0.045(2) 0.0202(18) -0.0062(16) -0.0015(16) C26 0.046(2) 0.045(2) 0.041(2) -0.0003(16) -0.0162(16) 0.0022(17) C27 0.0320(15) 0.0347(16) 0.0394(19) 0.0047(13) 0.0065(13) 0.0004(12) C28 0.043(2) 0.044(2) 0.069(3) -0.0014(19) 0.021(2) 0.0050(17) C29 0.047(2) 0.099(4) 0.039(2) 0.006(2) 0.0068(18) -0.008(3) C30 0.041(2) 0.0362(19) 0.074(3) 0.0032(19) 0.006(2) -0.0069(16) C31 0.0279(13) 0.0240(13) 0.0358(16) 0.0101(11) -0.0025(11) 0.0016(10) C32 0.0330(16) 0.047(2) 0.055(2) 0.0250(19) -0.0027(16) 0.0073(15) C33 0.0448(19) 0.0289(16) 0.055(2) 0.0007(15) -0.0067(17) 0.0122(15) C34 0.0281(15) 0.0359(17) 0.055(2) 0.0155(16) -0.0079(14) -0.0001(13) C35 0.0392(19) 0.0386(19) 0.058(3) -0.0080(17) 0.0080(17) 0.0104(15) C36 0.0345(18) 0.065(3) 0.088(4) -0.008(3) 0.001(2) 0.0104(18) C37 0.064(3) 0.050(2) 0.060(3) 0.015(2) -0.032(2) -0.025(2) C38 0.033(3) 0.112(7) 0.065(5) 0.010(4) -0.010(3) -0.012(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 Zn1 C35 1.978(4) . ? Zn1 O1 2.025(2) . ? Zn1 N7 2.048(3) . ? Zn1 O18 2.123(3) . ? Zn1 Zn2 3.0276(5) . ? Zn2 C37 1.956(4) . ? Zn2 N12 2.027(3) . ? Zn2 O18 2.032(2) . ? Zn2 O1 2.117(3) . ? O1 C1 1.336(4) . ? C1 C6 1.420(4) . ? C1 C2 1.424(4) . ? C2 C3 1.393(5) . ? C2 C19 1.545(4) . ? C3 C4 1.400(5) . ? C4 C5 1.386(4) . ? C4 C23 1.532(5) . ? C5 C6 1.408(4) . ? C6 C7 1.459(4) . ? C7 N7 1.278(4) . ? N7 C8 1.472(4) . ? C8 C9 1.521(5) . ? C9 C10 1.529(4) 4_655 ? C10 C9 1.529(4) 4_645 ? C10 C11 1.530(5) . ? C11 N12 1.472(4) . ? N12 C12 1.285(5) . ? C12 C13 1.452(4) . ? C13 C14 1.406(5) . ? C13 C18 1.429(4) . ? C14 C15 1.375(5) . ? C15 C16 1.402(5) . ? C15 C27 1.532(5) . ? C16 C17 1.398(4) . ? C17 C18 1.424(4) . ? C17 C31 1.543(4) . ? C18 O18 1.345(4) . ? C19 C21 1.533(5) . ? C19 C22 1.535(5) . ? C19 C20 1.545(5) . ? C23 C25 1.530(6) . ? C23 C24 1.538(6) . ? C23 C26 1.543(6) . ? C27 C29 1.518(7) . ? C27 C30 1.529(6) . ? C27 C28 1.536(6) . ? C31 C33 1.536(6) . ? C31 C32 1.542(5) . ? C31 C34 1.552(5) . ? C35 C36 1.501(6) . ? C37 C38' 1.467(9) . ? C37 C38 1.476(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C35 Zn1 O1 116.02(15) . . ? C35 Zn1 N7 131.70(15) . . ? O1 Zn1 N7 92.11(9) . . ? C35 Zn1 O18 126.05(16) . . ? O1 Zn1 O18 85.49(9) . . ? N7 Zn1 O18 92.60(11) . . ? C35 Zn1 Zn2 128.03(13) . . ? O1 Zn1 Zn2 44.24(7) . . ? N7 Zn1 Zn2 99.78(7) . . ? O18 Zn1 Zn2 42.06(6) . . ? C37 Zn2 N12 132.15(19) . . ? C37 Zn2 O18 116.12(16) . . ? N12 Zn2 O18 93.07(10) . . ? C37 Zn2 O1 123.76(19) . . ? N12 Zn2 O1 93.84(11) . . ? O18 Zn2 O1 85.48(9) . . ? C37 Zn2 Zn1 126.29(17) . . ? N12 Zn2 Zn1 101.28(8) . . ? O18 Zn2 Zn1 44.42(7) . . ? O1 Zn2 Zn1 41.87(6) . . ? C1 O1 Zn1 119.96(18) . . ? C1 O1 Zn2 129.01(19) . . ? Zn1 O1 Zn2 93.89(9) . . ? O1 C1 C6 121.2(3) . . ? O1 C1 C2 121.1(3) . . ? C6 C1 C2 117.7(3) . . ? C3 C2 C1 118.7(3) . . ? C3 C2 C19 119.8(3) . . ? C1 C2 C19 121.5(3) . . ? C2 C3 C4 124.3(3) . . ? C5 C4 C3 116.5(3) . . ? C5 C4 C23 121.0(3) . . ? C3 C4 C23 122.5(3) . . ? C4 C5 C6 122.0(3) . . ? C5 C6 C1 120.7(3) . . ? C5 C6 C7 114.2(3) . . ? C1 C6 C7 125.1(3) . . ? N7 C7 C6 127.8(3) . . ? C7 N7 C8 118.9(3) . . ? C7 N7 Zn1 120.6(2) . . ? C8 N7 Zn1 120.5(2) . . ? N7 C8 C9 110.8(3) . . ? C8 C9 C10 112.3(3) . 4_655 ? C9 C10 C11 109.4(3) 4_645 . ? N12 C11 C10 112.0(3) . . ? C12 N12 C11 118.2(3) . . ? C12 N12 Zn2 119.9(2) . . ? C11 N12 Zn2 121.9(2) . . ? N12 C12 C13 128.6(3) . . ? C14 C13 C18 120.3(3) . . ? C14 C13 C12 114.2(3) . . ? C18 C13 C12 125.5(3) . . ? C15 C14 C13 122.6(3) . . ? C14 C15 C16 116.4(3) . . ? C14 C15 C27 123.5(3) . . ? C16 C15 C27 120.1(3) . . ? C17 C16 C15 124.2(3) . . ? C16 C17 C18 118.5(3) . . ? C16 C17 C31 119.5(3) . . ? C18 C17 C31 122.0(3) . . ? O18 C18 C17 121.3(3) . . ? O18 C18 C13 121.0(3) . . ? C17 C18 C13 117.7(3) . . ? C18 O18 Zn2 120.51(19) . . ? C18 O18 Zn1 128.35(19) . . ? Zn2 O18 Zn1 93.53(10) . . ? C21 C19 C22 106.7(3) . . ? C21 C19 C2 109.8(3) . . ? C22 C19 C2 112.1(3) . . ? C21 C19 C20 109.6(3) . . ? C22 C19 C20 107.0(3) . . ? C2 C19 C20 111.5(3) . . ? C25 C23 C4 112.9(3) . . ? C25 C23 C24 108.7(3) . . ? C4 C23 C24 109.1(3) . . ? C25 C23 C26 107.4(4) . . ? C4 C23 C26 109.4(3) . . ? C24 C23 C26 109.3(3) . . ? C29 C27 C30 109.6(4) . . ? C29 C27 C15 110.2(3) . . ? C30 C27 C15 108.5(3) . . ? C29 C27 C28 108.8(4) . . ? C30 C27 C28 108.1(3) . . ? C15 C27 C28 111.6(3) . . ? C33 C31 C32 107.8(3) . . ? C33 C31 C17 110.2(3) . . ? C32 C31 C17 111.7(3) . . ? C33 C31 C34 110.2(3) . . ? C32 C31 C34 106.5(3) . . ? C17 C31 C34 110.5(3) . . ? C36 C35 Zn1 116.8(3) . . ? C38' C37 C38 100.2(11) . . ? C38' C37 Zn2 125.4(9) . . ? C38 C37 Zn2 115.2(4) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 32.61 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.854 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.097 #===END data_Compound_4c _database_code_depnum_ccdc_archive 'CCDC 621016' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H60 N4 Zn2' _chemical_formula_weight 787.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9147(5) _cell_length_b 14.7627(9) _cell_length_c 16.4967(9) _cell_angle_alpha 88.863(6) _cell_angle_beta 86.406(4) _cell_angle_gamma 72.948(5) _cell_volume 2071.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.6816 _cell_measurement_theta_max 70.8476 _exptl_crystal_description blocks _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 1.676 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.73481 _exptl_absorpt_correction_T_max 0.86540 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54248 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18858 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 71.05 _reflns_number_total 7684 _reflns_number_gt 6428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. ; _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^)+(0.0734P)^2^+0.6712P] 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 7684 _refine_ls_number_parameters 469 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 0.66697(4) 0.84748(2) 0.85374(2) 0.04077(12) Uani 1 1 d . . . Zn2 Zn 0.34298(4) 0.52513(2) 0.789522(19) 0.03594(11) Uani 1 1 d . . . N1 N 0.6007(2) 0.97713(13) 0.81434(12) 0.0315(4) Uani 1 1 d . . . C1 C 0.4797(3) 1.04839(16) 0.84690(14) 0.0292(5) Uani 1 1 d . . . C2 C 0.4455(3) 1.14308(17) 0.81726(15) 0.0359(5) Uani 1 1 d . . . H2A H 0.5075 1.1561 0.7721 0.043 Uiso 1 1 calc R . . C3 C 0.3270(3) 1.21606(18) 0.85106(16) 0.0404(6) Uani 1 1 d . . . H3A H 0.3086 1.2780 0.8289 0.048 Uiso 1 1 calc R . . C4 C 0.2327(3) 1.20080(18) 0.91768(17) 0.0423(6) Uani 1 1 d . . . H4A H 0.1527 1.2520 0.9421 0.051 Uiso 1 1 calc R . . C5 C 0.2578(3) 1.11071(18) 0.94701(15) 0.0379(6) Uani 1 1 d . . . H5A H 0.1925 1.1000 0.9917 0.045 Uiso 1 1 calc R . . C6 C 0.3780(3) 1.03245(16) 0.91312(14) 0.0312(5) Uani 1 1 d . . . C7 C 0.3791(3) 0.94147(17) 0.94524(14) 0.0333(5) Uani 1 1 d . . . H7A H 0.2994 0.9411 0.9862 0.040 Uiso 1 1 calc R . . N7 N 0.4749(2) 0.85979(14) 0.92543(12) 0.0343(4) Uani 1 1 d . . . C8 C 0.4413(4) 0.77575(18) 0.96300(16) 0.0429(6) Uani 1 1 d . . . H8A H 0.3809 0.7938 1.0156 0.051 Uiso 1 1 calc R . . H8B H 0.5415 0.7273 0.9738 0.051 Uiso 1 1 calc R . . C9 C 0.3465(3) 0.73343(18) 0.90717(16) 0.0410(6) Uani 1 1 d . . . H9A H 0.3247 0.6778 0.9342 0.049 Uiso 1 1 calc R . . H9B H 0.2445 0.7811 0.8984 0.049 Uiso 1 1 calc R . . C10 C 0.4335(4) 0.7035(2) 0.82583(17) 0.0451(6) Uani 1 1 d . . . H10A H 0.4519 0.7596 0.7979 0.054 Uiso 1 1 calc R . . H10B H 0.5372 0.6576 0.8346 0.054 Uiso 1 1 calc R . . N11 N 0.3444(3) 0.65955(15) 0.77319(13) 0.0383(5) Uani 1 1 d . . . C11 C 0.2687(3) 0.71084(17) 0.71587(16) 0.0394(6) Uani 1 1 d . . . H11A H 0.2704 0.7749 0.7143 0.047 Uiso 1 1 calc R . . C12 C 0.1830(3) 0.68447(16) 0.65464(14) 0.0332(5) Uani 1 1 d . . . C13 C 0.1108(3) 0.75789(17) 0.60029(17) 0.0425(6) Uani 1 1 d . . . H13A H 0.1190 0.8197 0.6087 0.051 Uiso 1 1 calc R . . C14 C 0.0302(4) 0.74357(19) 0.53667(18) 0.0487(7) Uani 1 1 d . . . H14A H -0.0177 0.7943 0.5017 0.058 Uiso 1 1 calc R . . C15 C 0.0196(3) 0.65210(19) 0.52401(17) 0.0449(6) Uani 1 1 d . . . H15A H -0.0345 0.6405 0.4794 0.054 Uiso 1 1 calc R . . C16 C 0.0863(3) 0.57916(17) 0.57514(15) 0.0366(5) Uani 1 1 d . . . H16A H 0.0775 0.5180 0.5646 0.044 Uiso 1 1 calc R . . C17 C 0.1680(3) 0.59130(15) 0.64323(13) 0.0290(5) Uani 1 1 d . . . N17 N 0.2293(2) 0.51886(13) 0.69498(11) 0.0293(4) Uani 1 1 d . . . C18 C 0.6893(3) 0.99639(16) 0.74392(15) 0.0343(5) Uani 1 1 d . . . C19 C 0.8101(3) 1.03865(18) 0.75219(16) 0.0384(6) Uani 1 1 d . . . C20 C 0.8956(3) 1.0551(2) 0.68260(18) 0.0480(7) Uani 1 1 d . . . H20A H 0.9772 1.0837 0.6875 0.058 Uiso 1 1 calc R . . C21 C 0.8636(4) 1.0307(2) 0.60731(19) 0.0545(8) Uani 1 1 d . . . H21A H 0.9212 1.0438 0.5604 0.065 Uiso 1 1 calc R . . C22 C 0.7473(4) 0.9868(2) 0.59939(17) 0.0514(7) Uani 1 1 d . . . H22A H 0.7277 0.9690 0.5470 0.062 Uiso 1 1 calc R . . C23 C 0.6586(3) 0.96832(18) 0.66726(16) 0.0402(6) Uani 1 1 d . A . C24 C 0.8508(3) 1.0614(2) 0.83568(17) 0.0454(6) Uani 1 1 d . . . H24A H 0.7596 1.0618 0.8743 0.055 Uiso 1 1 calc R . . C25 C 0.9939(4) 0.9831(3) 0.8636(2) 0.0644(9) Uani 1 1 d . . . H25A H 0.9740 0.9215 0.8602 0.097 Uiso 1 1 calc R . . H25B H 1.0120 0.9950 0.9199 0.097 Uiso 1 1 calc R . . H25C H 1.0869 0.9831 0.8286 0.097 Uiso 1 1 calc R . . C26 C 0.8788(4) 1.1586(2) 0.8405(2) 0.0607(8) Uani 1 1 d . . . H26A H 0.7863 1.2076 0.8229 0.091 Uiso 1 1 calc R . . H26B H 0.9709 1.1594 0.8051 0.091 Uiso 1 1 calc R . . H26C H 0.8972 1.1709 0.8967 0.091 Uiso 1 1 calc R . . C27 C 0.5328(3) 0.9188(2) 0.65887(18) 0.0478(7) Uani 1 1 d D . . H27A H 0.5269 0.8817 0.7098 0.057 Uiso 0.752(9) 1 calc PR A 1 H27B H 0.4850 0.9157 0.7122 0.057 Uiso 0.248(9) 1 d PR A 2 C28 C 0.3721(5) 0.9917(3) 0.6508(3) 0.0583(14) Uani 0.752(9) 1 d PD A 1 H28A H 0.2923 0.9588 0.6458 0.088 Uiso 0.752(9) 1 calc PR A 1 H28B H 0.3759 1.0306 0.6024 0.088 Uiso 0.752(9) 1 calc PR A 1 H28C H 0.3453 1.0322 0.6990 0.088 Uiso 0.752(9) 1 calc PR A 1 C29 C 0.5682(7) 0.8503(4) 0.5882(4) 0.080(2) Uani 0.752(9) 1 d PD A 1 H29A H 0.4839 0.8203 0.5863 0.119 Uiso 0.752(9) 1 calc PR A 1 H29B H 0.6682 0.8015 0.5952 0.119 Uiso 0.752(9) 1 calc PR A 1 H29C H 0.5752 0.8848 0.5374 0.119 Uiso 0.752(9) 1 calc PR A 1 C28' C 0.4085(19) 0.9633(13) 0.5994(12) 0.084(6) Uiso 0.248(9) 1 d PD A 2 H28D H 0.3343 0.9259 0.5981 0.127 Uiso 0.248(9) 1 calc PR A 2 H28E H 0.4590 0.9647 0.5451 0.127 Uiso 0.248(9) 1 calc PR A 2 H28F H 0.3521 1.0281 0.6167 0.127 Uiso 0.248(9) 1 calc PR A 2 C29' C 0.6087(16) 0.8137(8) 0.6373(10) 0.056(4) Uiso 0.248(9) 1 d PD A 2 H29D H 0.6920 0.7856 0.6742 0.084 Uiso 0.248(9) 1 calc PR A 2 H29E H 0.6538 0.8086 0.5812 0.084 Uiso 0.248(9) 1 calc PR A 2 H29F H 0.5288 0.7801 0.6426 0.084 Uiso 0.248(9) 1 calc PR A 2 C30 C 0.2066(3) 0.42821(15) 0.67932(13) 0.0275(4) Uani 1 1 d . . . C31 C 0.3285(3) 0.35724(16) 0.63939(14) 0.0296(5) Uani 1 1 d . . . C32 C 0.3064(3) 0.26825(16) 0.62918(15) 0.0344(5) Uani 1 1 d . . . H32A H 0.3878 0.2195 0.6027 0.041 Uiso 1 1 calc R . . C33 C 0.1690(3) 0.24981(16) 0.65667(15) 0.0359(5) Uani 1 1 d . . . H33A H 0.1567 0.1888 0.6494 0.043 Uiso 1 1 calc R . . C34 C 0.0495(3) 0.32021(17) 0.69475(16) 0.0352(5) Uani 1 1 d . . . H34A H -0.0452 0.3072 0.7130 0.042 Uiso 1 1 calc R . . C35 C 0.0649(3) 0.41009(16) 0.70702(14) 0.0307(5) Uani 1 1 d . . . C36 C 0.4799(3) 0.37494(17) 0.60607(16) 0.0368(5) Uani 1 1 d . . . H36A H 0.4801 0.4385 0.6258 0.044 Uiso 1 1 calc R . . C37 C 0.6247(4) 0.3016(2) 0.6369(3) 0.0655(9) Uani 1 1 d . . . H37A H 0.7199 0.3153 0.6140 0.098 Uiso 1 1 calc R . . H37B H 0.6255 0.2382 0.6202 0.098 Uiso 1 1 calc R . . H37C H 0.6216 0.3045 0.6963 0.098 Uiso 1 1 calc R . . C38 C 0.4874(4) 0.3780(3) 0.51338(19) 0.0656(9) Uani 1 1 d . . . H38A H 0.3940 0.4257 0.4950 0.098 Uiso 1 1 calc R . . H38B H 0.4914 0.3157 0.4922 0.098 Uiso 1 1 calc R . . H38C H 0.5819 0.3946 0.4934 0.098 Uiso 1 1 calc R . . C39 C -0.0702(3) 0.48512(18) 0.74955(17) 0.0406(6) Uani 1 1 d . . . H39A H -0.0383 0.5445 0.7521 0.049 Uiso 1 1 calc R . . C40 C -0.2191(4) 0.5075(3) 0.7025(2) 0.0648(9) Uani 1 1 d . . . H40A H -0.1962 0.5266 0.6470 0.097 Uiso 1 1 calc R . . H40B H -0.3012 0.5591 0.7295 0.097 Uiso 1 1 calc R . . H40C H -0.2554 0.4510 0.7008 0.097 Uiso 1 1 calc R . . C41 C -0.1009(5) 0.4549(3) 0.8365(2) 0.0671(9) Uani 1 1 d . . . H41A H -0.0039 0.4411 0.8653 0.101 Uiso 1 1 calc R . . H41B H -0.1364 0.3981 0.8357 0.101 Uiso 1 1 calc R . . H41C H -0.1823 0.5062 0.8643 0.101 Uiso 1 1 calc R . . C42 C 0.8509(4) 0.7404(2) 0.8215(2) 0.0591(8) Uani 1 1 d . . . H42A H 0.8134 0.6954 0.7905 0.071 Uiso 1 1 calc R . . H42B H 0.9204 0.7651 0.7837 0.071 Uiso 1 1 calc R . . C43 C 0.9496(4) 0.6852(2) 0.8868(2) 0.0657(9) Uani 1 1 d . . . H43A H 1.0366 0.6346 0.8619 0.099 Uiso 1 1 calc R . . H43B H 0.8848 0.6574 0.9238 0.099 Uiso 1 1 calc R . . H43C H 0.9918 0.7277 0.9172 0.099 Uiso 1 1 calc R . . C44 C 0.4315(4) 0.4492(2) 0.88326(18) 0.0499(7) Uani 1 1 d . . . H44A H 0.4662 0.3815 0.8676 0.060 Uiso 1 1 calc R . . H44B H 0.5255 0.4666 0.8978 0.060 Uiso 1 1 calc R . . C45 C 0.3187(5) 0.4614(2) 0.95721(19) 0.0615(8) Uani 1 1 d . . . H45A H 0.3708 0.4213 1.0014 0.092 Uiso 1 1 calc R . . H45B H 0.2262 0.4429 0.9439 0.092 Uiso 1 1 calc R . . H45C H 0.2860 0.5279 0.9743 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0412(2) 0.03141(19) 0.0501(2) -0.00400(14) -0.00113(15) -0.01145(14) Zn2 0.0439(2) 0.03618(19) 0.03318(19) -0.00114(13) -0.00723(14) -0.01918(15) N1 0.0336(10) 0.0297(10) 0.0336(10) -0.0025(8) 0.0006(8) -0.0135(8) C1 0.0292(11) 0.0317(11) 0.0309(11) -0.0044(9) -0.0078(9) -0.0142(9) C2 0.0387(13) 0.0324(12) 0.0389(13) -0.0009(10) -0.0056(10) -0.0132(10) C3 0.0433(14) 0.0319(12) 0.0473(15) -0.0028(11) -0.0113(11) -0.0112(10) C4 0.0360(13) 0.0383(14) 0.0515(16) -0.0144(11) -0.0052(11) -0.0075(11) C5 0.0331(13) 0.0459(14) 0.0376(13) -0.0107(11) -0.0012(10) -0.0156(11) C6 0.0306(12) 0.0353(12) 0.0322(12) -0.0052(9) -0.0081(9) -0.0149(9) C7 0.0370(13) 0.0434(14) 0.0261(11) -0.0045(9) -0.0064(9) -0.0208(11) N7 0.0411(11) 0.0351(11) 0.0338(10) -0.0022(8) -0.0102(9) -0.0204(9) C8 0.0606(17) 0.0387(14) 0.0374(14) 0.0032(11) -0.0103(12) -0.0256(12) C9 0.0512(15) 0.0372(13) 0.0413(14) -0.0006(11) -0.0047(12) -0.0229(12) C10 0.0531(16) 0.0433(14) 0.0481(16) -0.0094(12) -0.0025(12) -0.0277(12) N11 0.0482(12) 0.0368(11) 0.0369(11) -0.0059(9) -0.0012(9) -0.0233(9) C11 0.0535(15) 0.0306(12) 0.0391(14) -0.0048(10) 0.0037(11) -0.0212(11) C12 0.0391(13) 0.0283(11) 0.0339(12) -0.0034(9) 0.0043(10) -0.0133(10) C13 0.0528(16) 0.0268(12) 0.0490(15) 0.0009(10) -0.0026(12) -0.0137(11) C14 0.0558(17) 0.0347(14) 0.0537(17) 0.0116(12) -0.0126(13) -0.0093(12) C15 0.0525(16) 0.0405(14) 0.0434(15) 0.0052(11) -0.0150(12) -0.0140(12) C16 0.0424(14) 0.0296(12) 0.0402(13) -0.0015(10) -0.0055(11) -0.0134(10) C17 0.0279(11) 0.0296(11) 0.0301(11) -0.0040(9) 0.0026(9) -0.0101(9) N17 0.0332(10) 0.0254(9) 0.0320(10) -0.0018(7) -0.0025(8) -0.0127(8) C18 0.0348(12) 0.0304(12) 0.0373(13) -0.0005(9) -0.0001(10) -0.0089(10) C19 0.0340(13) 0.0366(13) 0.0452(14) 0.0013(11) 0.0008(11) -0.0123(10) C20 0.0432(15) 0.0482(15) 0.0545(17) 0.0013(13) 0.0079(13) -0.0186(12) C21 0.0631(19) 0.0495(16) 0.0481(17) -0.0035(13) 0.0183(14) -0.0163(14) C22 0.0652(19) 0.0493(16) 0.0366(15) -0.0092(12) 0.0041(13) -0.0130(14) C23 0.0447(14) 0.0334(13) 0.0410(14) -0.0061(10) 0.0009(11) -0.0095(11) C24 0.0435(15) 0.0559(16) 0.0461(15) 0.0039(12) -0.0067(12) -0.0282(13) C25 0.060(2) 0.070(2) 0.072(2) 0.0194(17) -0.0213(17) -0.0296(17) C26 0.069(2) 0.0609(19) 0.064(2) -0.0011(15) -0.0107(16) -0.0358(17) C27 0.0559(17) 0.0470(15) 0.0435(15) -0.0101(12) -0.0044(13) -0.0187(13) C28 0.053(3) 0.056(3) 0.069(3) -0.012(2) -0.016(2) -0.0172(19) C29 0.085(4) 0.070(4) 0.093(4) -0.046(3) 0.012(3) -0.036(3) C30 0.0339(12) 0.0263(11) 0.0254(11) 0.0017(8) -0.0056(9) -0.0132(9) C31 0.0318(12) 0.0287(11) 0.0304(11) -0.0003(9) -0.0053(9) -0.0113(9) C32 0.0368(13) 0.0280(11) 0.0388(13) -0.0021(9) -0.0080(10) -0.0088(9) C33 0.0417(14) 0.0263(11) 0.0437(14) 0.0020(10) -0.0098(11) -0.0152(10) C34 0.0336(12) 0.0330(12) 0.0447(14) 0.0071(10) -0.0066(10) -0.0180(10) C35 0.0323(12) 0.0317(12) 0.0302(12) 0.0005(9) -0.0046(9) -0.0124(9) C36 0.0348(13) 0.0343(12) 0.0432(14) -0.0072(10) 0.0030(10) -0.0134(10) C37 0.0344(15) 0.060(2) 0.102(3) 0.0059(18) -0.0069(16) -0.0133(14) C38 0.071(2) 0.087(2) 0.0484(18) -0.0109(16) 0.0185(16) -0.0419(19) C39 0.0337(13) 0.0386(13) 0.0512(15) -0.0086(11) 0.0046(11) -0.0142(11) C40 0.0361(16) 0.067(2) 0.084(2) -0.0168(18) -0.0080(15) -0.0017(14) C41 0.075(2) 0.071(2) 0.0542(19) -0.0110(16) 0.0243(17) -0.0259(18) C42 0.0565(19) 0.0449(16) 0.068(2) -0.0092(14) 0.0071(15) -0.0045(14) C43 0.0465(18) 0.062(2) 0.080(2) -0.0121(17) 0.0013(16) -0.0037(15) C44 0.0608(18) 0.0424(15) 0.0518(17) 0.0029(12) -0.0176(14) -0.0205(13) C45 0.087(2) 0.0496(17) 0.0474(17) 0.0104(13) -0.0092(16) -0.0180(16) _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 N1 1.942(2) . ? Zn1 C42 1.968(3) . ? Zn1 N7 1.984(2) . ? Zn2 N17 1.9307(19) . ? Zn2 C44 1.958(3) . ? Zn2 N11 2.001(2) . ? N1 C1 1.358(3) . ? N1 C18 1.434(3) . ? C1 C2 1.424(3) . ? C1 C6 1.436(3) . ? C2 C3 1.367(4) . ? C3 C4 1.397(4) . ? C4 C5 1.366(4) . ? C5 C6 1.421(3) . ? C6 C7 1.432(3) . ? C7 N7 1.291(3) . ? N7 C8 1.476(3) . ? C8 C9 1.544(3) . ? C9 C10 1.513(4) . ? C10 N11 1.490(3) . ? N11 C11 1.294(3) . ? C11 C12 1.429(4) . ? C12 C13 1.421(4) . ? C12 C17 1.437(3) . ? C13 C14 1.362(4) . ? C14 C15 1.401(4) . ? C15 C16 1.370(4) . ? C16 C17 1.418(3) . ? C17 N17 1.360(3) . ? N17 C30 1.441(3) . ? C18 C23 1.406(4) . ? C18 C19 1.408(4) . ? C19 C20 1.395(4) . ? C19 C24 1.515(4) . ? C20 C21 1.370(4) . ? C21 C22 1.387(5) . ? C22 C23 1.399(4) . ? C23 C27 1.522(4) . ? C24 C26 1.532(4) . ? C24 C25 1.536(4) . ? C27 C29 1.514(5) . ? C27 C28' 1.518(12) . ? C27 C28 1.530(5) . ? C27 C29' 1.538(10) . ? C30 C31 1.408(3) . ? C30 C35 1.413(3) . ? C31 C32 1.399(3) . ? C31 C36 1.516(3) . ? C32 C33 1.379(3) . ? C33 C34 1.379(4) . ? C34 C35 1.393(3) . ? C35 C39 1.521(3) . ? C36 C38 1.527(4) . ? C36 C37 1.529(4) . ? C39 C41 1.526(4) . ? C39 C40 1.528(4) . ? C42 C43 1.504(5) . ? C44 C45 1.510(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 N1 Zn1 C42 130.87(12) . . ? N1 Zn1 N7 94.97(8) . . ? C42 Zn1 N7 133.82(12) . . ? N17 Zn2 C44 141.04(10) . . ? N17 Zn2 N11 96.11(8) . . ? C44 Zn2 N11 122.76(11) . . ? C1 N1 C18 118.83(19) . . ? C1 N1 Zn1 125.87(16) . . ? C18 N1 Zn1 115.29(15) . . ? N1 C1 C2 122.1(2) . . ? N1 C1 C6 121.8(2) . . ? C2 C1 C6 116.0(2) . . ? C3 C2 C1 122.7(2) . . ? C2 C3 C4 120.9(2) . . ? C5 C4 C3 118.7(2) . . ? C4 C5 C6 122.4(2) . . ? C5 C6 C7 115.6(2) . . ? C5 C6 C1 119.2(2) . . ? C7 C6 C1 125.1(2) . . ? N7 C7 C6 128.0(2) . . ? C7 N7 C8 117.0(2) . . ? C7 N7 Zn1 121.78(17) . . ? C8 N7 Zn1 121.10(17) . . ? N7 C8 C9 111.1(2) . . ? C10 C9 C8 112.0(2) . . ? N11 C10 C9 111.9(2) . . ? C11 N11 C10 117.8(2) . . ? C11 N11 Zn2 120.88(17) . . ? C10 N11 Zn2 121.28(18) . . ? N11 C11 C12 129.0(2) . . ? C13 C12 C11 115.6(2) . . ? C13 C12 C17 118.8(2) . . ? C11 C12 C17 125.7(2) . . ? C14 C13 C12 122.9(2) . . ? C13 C14 C15 118.4(2) . . ? C16 C15 C14 120.9(3) . . ? C15 C16 C17 122.7(2) . . ? N17 C17 C16 122.0(2) . . ? N17 C17 C12 121.7(2) . . ? C16 C17 C12 116.4(2) . . ? C17 N17 C30 117.73(18) . . ? C17 N17 Zn2 126.41(15) . . ? C30 N17 Zn2 115.85(14) . . ? C23 C18 C19 120.7(2) . . ? C23 C18 N1 118.9(2) . . ? C19 C18 N1 120.3(2) . . ? C20 C19 C18 118.8(2) . . ? C20 C19 C24 120.8(2) . . ? C18 C19 C24 120.3(2) . . ? C21 C20 C19 121.0(3) . . ? C20 C21 C22 120.2(3) . . ? C21 C22 C23 121.2(3) . . ? C22 C23 C18 118.1(2) . . ? C22 C23 C27 121.2(2) . . ? C18 C23 C27 120.7(2) . . ? C19 C24 C26 113.4(2) . . ? C19 C24 C25 110.3(3) . . ? C26 C24 C25 110.5(2) . . ? C29 C27 C28' 75.3(8) . . ? C29 C27 C23 113.3(3) . . ? C28' C27 C23 115.9(8) . . ? C29 C27 C28 109.7(3) . . ? C28' C27 C28 36.2(8) . . ? C23 C27 C28 110.4(3) . . ? C29 C27 C29' 37.9(5) . . ? C28' C27 C29' 109.5(9) . . ? C23 C27 C29' 110.5(6) . . ? C28 C27 C29' 136.3(6) . . ? C31 C30 C35 120.6(2) . . ? C31 C30 N17 119.57(19) . . ? C35 C30 N17 119.75(19) . . ? C32 C31 C30 118.2(2) . . ? C32 C31 C36 119.5(2) . . ? C30 C31 C36 122.2(2) . . ? C33 C32 C31 121.5(2) . . ? C32 C33 C34 119.8(2) . . ? C33 C34 C35 121.4(2) . . ? C34 C35 C30 118.5(2) . . ? C34 C35 C39 119.3(2) . . ? C30 C35 C39 122.2(2) . . ? C31 C36 C38 110.9(2) . . ? C31 C36 C37 111.9(2) . . ? C38 C36 C37 110.9(3) . . ? C35 C39 C41 110.6(2) . . ? C35 C39 C40 111.7(2) . . ? C41 C39 C40 111.1(3) . . ? C43 C42 Zn1 118.5(2) . . ? C45 C44 Zn2 114.1(2) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 71.05 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.461 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.060 #===END data_Compound_5c _database_code_depnum_ccdc_archive 'CCDC 621017' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H66 N4 Zn2' _chemical_formula_weight 829.79 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' 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)/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 11.5694(6) _cell_length_b 13.4841(8) _cell_length_c 14.3159(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.626(4) _cell_angle_gamma 90.00 _cell_volume 2208.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.8836 _cell_measurement_theta_max 32.6299 _exptl_crystal_description blocks _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 1.122 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.79982 _exptl_absorpt_correction_T_max 0.96455 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24370 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 32.70 _reflns_number_total 7658 _reflns_number_gt 3959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. ; _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^)+(0.0495P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7658 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 0.910 _refine_ls_restrained_S_all 0.910 _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 Zn Zn 0.62694(2) 0.378067(17) 0.341198(17) 0.03623(9) Uani 1 1 d . . . N1 N 0.57257(14) 0.29523(11) 0.43539(12) 0.0305(4) Uani 1 1 d . . . C1 C 0.55919(16) 0.32451(14) 0.52371(14) 0.0297(4) Uani 1 1 d . . . C2 C 0.49750(18) 0.26587(15) 0.58224(15) 0.0352(5) Uani 1 1 d . . . H2A H 0.4677 0.2033 0.5597 0.042 Uiso 1 1 calc R . . C3 C 0.47954(18) 0.29645(17) 0.67009(15) 0.0388(5) Uani 1 1 d . . . H3A H 0.4375 0.2548 0.7067 0.047 Uiso 1 1 calc R . . C4 C 0.52132(18) 0.38685(16) 0.70674(15) 0.0383(5) Uani 1 1 d . . . H4A H 0.5066 0.4084 0.7670 0.046 Uiso 1 1 calc R . . C5 C 0.58429(17) 0.44410(16) 0.65376(15) 0.0349(5) Uani 1 1 d . . . H5A H 0.6149 0.5054 0.6792 0.042 Uiso 1 1 calc R . . C6 C 0.60583(16) 0.41630(14) 0.56303(14) 0.0296(4) Uani 1 1 d . . . C7 C 0.67711(16) 0.48293(14) 0.51821(15) 0.0316(4) Uani 1 1 d . . . H7A H 0.7102 0.5371 0.5554 0.038 Uiso 1 1 calc R . . N7 N 0.70141(14) 0.47791(11) 0.43359(12) 0.0325(4) Uani 1 1 d . . . C8 C 0.53753(17) 0.19688(14) 0.40504(14) 0.0302(4) Uani 1 1 d . . . C9 C 0.42417(18) 0.17927(15) 0.35788(15) 0.0355(5) Uani 1 1 d . . . C10 C 0.3964(2) 0.08469(16) 0.32333(16) 0.0407(5) Uani 1 1 d . . . H10A H 0.3205 0.0722 0.2899 0.049 Uiso 1 1 calc R . . C11 C 0.4767(2) 0.00864(17) 0.33651(18) 0.0453(6) Uani 1 1 d . . . H11A H 0.4561 -0.0557 0.3127 0.054 Uiso 1 1 calc R . . C12 C 0.5868(2) 0.02648(15) 0.38436(16) 0.0418(5) Uani 1 1 d . . . H12A H 0.6413 -0.0266 0.3937 0.050 Uiso 1 1 calc R . . C13 C 0.62095(18) 0.11997(14) 0.41956(15) 0.0344(5) Uani 1 1 d . . . C14 C 0.33275(19) 0.26032(16) 0.34492(18) 0.0441(6) Uani 1 1 d . . . H14A H 0.3691 0.3214 0.3763 0.053 Uiso 1 1 calc R . . C15 C 0.2950(2) 0.2849(2) 0.2407(2) 0.0580(7) Uani 1 1 d . . . H15A H 0.3638 0.3023 0.2117 0.087 Uiso 1 1 calc R . . H15B H 0.2406 0.3411 0.2351 0.087 Uiso 1 1 calc R . . H15C H 0.2562 0.2272 0.2083 0.087 Uiso 1 1 calc R . . C16 C 0.2276(2) 0.23380(19) 0.39298(19) 0.0539(7) Uani 1 1 d . . . H16A H 0.2541 0.2186 0.4597 0.081 Uiso 1 1 calc R . . H16B H 0.1878 0.1758 0.3619 0.081 Uiso 1 1 calc R . . H16C H 0.1732 0.2900 0.3882 0.081 Uiso 1 1 calc R . . C17 C 0.74437(19) 0.13984(16) 0.46744(16) 0.0402(5) Uani 1 1 d . . . H17A H 0.7406 0.1955 0.5131 0.048 Uiso 1 1 calc R . . C18 C 0.8013(2) 0.05183(18) 0.52333(18) 0.0545(6) Uani 1 1 d . . . H18A H 0.7522 0.0307 0.5698 0.082 Uiso 1 1 calc R . . H18B H 0.8785 0.0713 0.5560 0.082 Uiso 1 1 calc R . . H18C H 0.8098 -0.0031 0.4801 0.082 Uiso 1 1 calc R . . C19 C 0.8212(2) 0.1743(2) 0.39542(19) 0.0551(7) Uani 1 1 d . . . H19A H 0.7844 0.2312 0.3601 0.083 Uiso 1 1 calc R . . H19B H 0.8302 0.1201 0.3515 0.083 Uiso 1 1 calc R . . H19C H 0.8982 0.1938 0.4285 0.083 Uiso 1 1 calc R . . C20 C 0.78067(18) 0.55126(15) 0.40208(16) 0.0387(5) Uani 1 1 d . . . H20A H 0.8003 0.6021 0.4518 0.046 Uiso 1 1 calc R . . H20B H 0.7411 0.5849 0.3445 0.046 Uiso 1 1 calc R . . C21 C 0.89234(19) 0.50254(17) 0.38090(17) 0.0439(5) Uani 1 1 d . . . H21A H 0.8709 0.4480 0.3353 0.053 Uiso 1 1 calc R . . H21B H 0.9372 0.5520 0.3499 0.053 Uiso 1 1 calc R . . C22 C 0.97124(19) 0.46102(16) 0.46612(17) 0.0448(6) Uani 1 1 d . . . H22A H 0.9246 0.4164 0.5008 0.054 Uiso 1 1 calc R . . H22B H 1.0330 0.4206 0.4438 0.054 Uiso 1 1 calc R . . C23 C 0.6227(2) 0.38175(18) 0.20477(17) 0.0521(6) Uani 1 1 d . . . H23A H 0.5561 0.4242 0.1780 0.063 Uiso 1 1 calc R . . H23B H 0.6948 0.4151 0.1918 0.063 Uiso 1 1 calc R . . C24 C 0.6123(3) 0.2858(2) 0.1516(2) 0.0804(9) Uani 1 1 d . . . H24A H 0.6108 0.2989 0.0841 0.121 Uiso 1 1 calc R . . H24B H 0.5398 0.2522 0.1612 0.121 Uiso 1 1 calc R . . H24C H 0.6793 0.2434 0.1746 0.121 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn 0.04150(16) 0.03579(15) 0.03154(14) 0.00028(11) 0.00587(10) -0.00763(11) N1 0.0354(9) 0.0254(8) 0.0311(9) -0.0007(7) 0.0057(7) -0.0025(7) C1 0.0279(10) 0.0292(10) 0.0316(11) 0.0013(8) 0.0025(8) 0.0042(8) C2 0.0364(11) 0.0339(11) 0.0347(12) 0.0020(9) 0.0033(9) -0.0026(9) C3 0.0356(11) 0.0468(13) 0.0348(12) 0.0066(10) 0.0074(9) 0.0007(10) C4 0.0376(12) 0.0473(13) 0.0300(11) -0.0007(10) 0.0056(9) 0.0105(10) C5 0.0332(11) 0.0347(11) 0.0349(12) -0.0026(9) -0.0004(9) 0.0073(9) C6 0.0256(10) 0.0292(10) 0.0329(11) 0.0002(8) 0.0004(8) 0.0035(8) C7 0.0291(10) 0.0259(10) 0.0377(12) -0.0026(9) -0.0020(8) 0.0020(8) N7 0.0318(9) 0.0269(8) 0.0380(10) 0.0023(7) 0.0028(7) -0.0009(7) C8 0.0350(11) 0.0291(10) 0.0274(10) -0.0018(8) 0.0081(8) -0.0027(8) C9 0.0396(12) 0.0329(11) 0.0341(12) -0.0014(9) 0.0057(9) -0.0041(9) C10 0.0419(13) 0.0375(11) 0.0421(13) -0.0048(10) 0.0039(10) -0.0098(10) C11 0.0539(15) 0.0333(12) 0.0516(15) -0.0108(10) 0.0174(12) -0.0087(11) C12 0.0507(14) 0.0318(11) 0.0454(14) -0.0015(10) 0.0151(11) 0.0041(10) C13 0.0368(11) 0.0326(11) 0.0355(11) 0.0007(9) 0.0106(9) -0.0007(9) C14 0.0374(12) 0.0341(12) 0.0572(16) -0.0051(11) -0.0043(11) -0.0019(10) C15 0.0446(14) 0.0598(16) 0.0665(18) 0.0186(14) -0.0013(13) -0.0020(12) C16 0.0448(14) 0.0579(15) 0.0585(17) -0.0144(13) 0.0057(12) 0.0056(12) C17 0.0404(12) 0.0389(12) 0.0413(13) -0.0054(10) 0.0064(10) 0.0065(10) C18 0.0559(15) 0.0571(16) 0.0488(16) 0.0019(13) 0.0028(12) 0.0131(13) C19 0.0441(14) 0.0581(16) 0.0636(18) 0.0063(14) 0.0097(12) -0.0036(12) C20 0.0372(12) 0.0355(11) 0.0425(13) 0.0022(10) 0.0028(9) -0.0050(9) C21 0.0373(12) 0.0498(13) 0.0453(14) -0.0041(11) 0.0083(10) -0.0088(10) C22 0.0328(11) 0.0460(13) 0.0560(16) -0.0110(11) 0.0075(10) 0.0012(10) C23 0.0656(16) 0.0543(15) 0.0375(13) 0.0014(12) 0.0111(11) -0.0151(12) C24 0.100(2) 0.087(2) 0.0538(19) -0.0245(17) 0.0117(17) 0.0249(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 Zn N1 1.9277(16) . ? Zn C23 1.947(2) . ? Zn N7 1.9906(17) . ? N1 C1 1.355(2) . ? N1 C8 1.435(2) . ? C1 C2 1.420(3) . ? C1 C6 1.431(3) . ? C2 C3 1.369(3) . ? C3 C4 1.385(3) . ? C4 C5 1.367(3) . ? C5 C6 1.410(3) . ? C6 C7 1.434(3) . ? C7 N7 1.286(3) . ? N7 C20 1.465(2) . ? C8 C9 1.402(3) . ? C8 C13 1.411(3) . ? C9 C10 1.388(3) . ? C9 C14 1.513(3) . ? C10 C11 1.377(3) . ? C11 C12 1.374(3) . ? C12 C13 1.393(3) . ? C13 C17 1.512(3) . ? C14 C15 1.527(4) . ? C14 C16 1.528(3) . ? C17 C18 1.525(3) . ? C17 C19 1.531(3) . ? C20 C21 1.520(3) . ? C21 C22 1.517(3) . ? C22 C22 1.515(4) 3_766 ? C23 C24 1.497(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn C23 139.00(9) . . ? N1 Zn N7 94.65(7) . . ? C23 Zn N7 126.34(9) . . ? C1 N1 C8 119.02(16) . . ? C1 N1 Zn 125.36(13) . . ? C8 N1 Zn 115.51(12) . . ? N1 C1 C2 121.74(18) . . ? N1 C1 C6 121.98(17) . . ? C2 C1 C6 116.28(18) . . ? C3 C2 C1 122.24(19) . . ? C2 C3 C4 121.4(2) . . ? C5 C4 C3 118.1(2) . . ? C4 C5 C6 122.9(2) . . ? C5 C6 C1 118.94(18) . . ? C5 C6 C7 116.02(18) . . ? C1 C6 C7 125.02(18) . . ? N7 C7 C6 127.59(19) . . ? C7 N7 C20 119.34(17) . . ? C7 N7 Zn 121.84(13) . . ? C20 N7 Zn 118.71(14) . . ? C9 C8 C13 121.07(18) . . ? C9 C8 N1 120.24(18) . . ? C13 C8 N1 118.61(18) . . ? C10 C9 C8 118.47(19) . . ? C10 C9 C14 120.00(19) . . ? C8 C9 C14 121.52(18) . . ? C11 C10 C9 121.3(2) . . ? C12 C11 C10 119.6(2) . . ? C11 C12 C13 122.0(2) . . ? C12 C13 C8 117.5(2) . . ? C12 C13 C17 121.46(19) . . ? C8 C13 C17 121.00(18) . . ? C9 C14 C15 111.7(2) . . ? C9 C14 C16 111.42(19) . . ? C15 C14 C16 111.12(19) . . ? C13 C17 C18 113.84(19) . . ? C13 C17 C19 110.65(19) . . ? C18 C17 C19 109.94(19) . . ? N7 C20 C21 111.07(17) . . ? C22 C21 C20 115.2(2) . . ? C22 C22 C21 114.4(2) 3_766 . ? C24 C23 Zn 118.43(19) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 32.70 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.624 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.060 #===END