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 _journal_year 2006 _journal_page_first 2350 _publ_contact_author_name 'Gregory Solan' _publ_contact_author_address ; Department of Chemistry University of Leicester University Road Leicester Leicestershire LE1 7RH UNITED KINGDOM ; _publ_contact_author_email GAS8@LEICESTER.AC.UK _publ_section_title ; Mono- versus Bi-metallic Assembly on a Bulky Bis(imino)terpyridine Framework: A Combined Experimental and Theoretical Study ; loop_ _publ_author_name 'Yohan D. M. Champouret' 'Jean-Didier Marechal' 'Ishaq Dadhiwala' 'John Fawcett' D.Palmer 'Kuldip Singh' G.A.Solan # Attachment '05008.cif' data_05008 _database_code_depnum_ccdc_archive 'CCDC 289324' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C43 H49 N5) (C H2 Cl2)' _chemical_formula_sum 'C44 H51 Cl2 N5' _chemical_formula_weight 720.80 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 20.807(3) _cell_length_b 11.0120(14) _cell_length_c 17.781(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.489(2) _cell_angle_gamma 90.00 _cell_volume 4061.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 966 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 25.75 _exptl_crystal_description colourless _exptl_crystal_colour plate _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.616 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details ; absorption correction based on 5629 reflections (SADABS); Rint 0.043 before correction and 0.031 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14234 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6954 _reflns_number_gt 4673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 ; Data appeared centrosymmetric but could not be solved in C2/c and was refined as a racemic twin in Cc. 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^)+(0.1231P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.54(17) _refine_ls_number_reflns 6954 _refine_ls_number_parameters 470 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.2148 _refine_ls_wR_factor_gt 0.1853 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 N1 N 0.38555(18) 0.9443(4) 0.1261(2) 0.0259(10) Uani 1 1 d . . . N2 N 0.2573(2) 0.9830(4) 0.2436(2) 0.0207(9) Uani 1 1 d . . . N3 N 0.1292(2) 0.9301(2) 0.3632(3) 0.0237(6) Uani 1 1 d . . . N4 N -0.0021(2) 0.9814(4) 0.4783(2) 0.0254(10) Uani 1 1 d . . . N5 N -0.12961(19) 0.9415(4) 0.5958(2) 0.0244(10) Uani 1 1 d . . . C1 C 0.5551(3) 1.0724(7) 0.2604(4) 0.0630(19) Uani 1 1 d . . . H1A H 0.5578 1.0473 0.3134 0.094 Uiso 1 1 calc R . . H1B H 0.5457 1.1595 0.2569 0.094 Uiso 1 1 calc R . . H1C H 0.5963 1.0559 0.2391 0.094 Uiso 1 1 calc R . . C2 C 0.5095(3) 0.8668(7) 0.2289(4) 0.0583(18) Uani 1 1 d . . . H2A H 0.5490 0.8386 0.2078 0.087 Uiso 1 1 calc R . . H2B H 0.4722 0.8257 0.2034 0.087 Uiso 1 1 calc R . . H2C H 0.5118 0.8483 0.2830 0.087 Uiso 1 1 calc R . . C3 C 0.5028(2) 1.0031(5) 0.2175(3) 0.0370(14) Uani 1 1 d . . . H3 H 0.4619 1.0266 0.2397 0.044 Uiso 1 1 calc R . . C4 C 0.4930(2) 1.0334(4) 0.1345(3) 0.0286(12) Uani 1 1 d . . . C5 C 0.5405(2) 1.0863(5) 0.0958(3) 0.0383(14) Uani 1 1 d . . . H5 H 0.5806 1.1046 0.1228 0.046 Uiso 1 1 calc R . . C6 C 0.5333(2) 1.1134(5) 0.0221(4) 0.0432(16) Uani 1 1 d . . . H6 H 0.5670 1.1519 -0.0019 0.052 Uiso 1 1 calc R . . C7 C 0.4756(3) 1.0844(6) -0.0185(3) 0.0409(15) Uani 1 1 d . . . H7 H 0.4708 1.1030 -0.0709 0.049 Uiso 1 1 calc R . . C8 C 0.4259(3) 1.0303(5) 0.0136(3) 0.0291(12) Uani 1 1 d . . . C9 C 0.3636(3) 0.9982(6) -0.0321(3) 0.0445(15) Uani 1 1 d . . . H9 H 0.3401 0.9381 -0.0022 0.053 Uiso 1 1 calc R . . C10 C 0.3765(4) 0.9383(9) -0.1062(3) 0.076(2) Uani 1 1 d . . . H10A H 0.3988 0.9957 -0.1373 0.115 Uiso 1 1 calc R . . H10B H 0.3355 0.9142 -0.1330 0.115 Uiso 1 1 calc R . . H10C H 0.4035 0.8663 -0.0963 0.115 Uiso 1 1 calc R . . C11 C 0.3203(4) 1.1104(8) -0.0440(5) 0.092(3) Uani 1 1 d . . . H11A H 0.3216 1.1577 0.0028 0.138 Uiso 1 1 calc R . . H11B H 0.2759 1.0846 -0.0581 0.138 Uiso 1 1 calc R . . H11C H 0.3357 1.1606 -0.0844 0.138 Uiso 1 1 calc R . . C12 C 0.4336(2) 1.0059(4) 0.0919(3) 0.0243(12) Uani 1 1 d . . . C13 C 0.3445(2) 0.9970(5) 0.1653(3) 0.0213(11) Uani 1 1 d . . . C13' C 0.3435(3) 1.1315(4) 0.1789(3) 0.0299(13) Uani 1 1 d . . . H13A H 0.3783 1.1700 0.1535 0.045 Uiso 1 1 calc R . . H13B H 0.3496 1.1475 0.2332 0.045 Uiso 1 1 calc R . . H13C H 0.3019 1.1647 0.1588 0.045 Uiso 1 1 calc R . . C14 C 0.2970(3) 0.9231(5) 0.2025(3) 0.0272(12) Uani 1 1 d . . . C15 C 0.2911(3) 0.7993(5) 0.1912(3) 0.0367(14) Uani 1 1 d . . . H15 H 0.3195 0.7581 0.1605 0.044 Uiso 1 1 calc R . . C16 C 0.2434(3) 0.7350(5) 0.2250(3) 0.0353(14) Uani 1 1 d . . . H16 H 0.2383 0.6502 0.2169 0.042 Uiso 1 1 calc R . . C17 C 0.2049(3) 0.7952(5) 0.2693(3) 0.0355(14) Uani 1 1 d . . . H17 H 0.1730 0.7533 0.2945 0.043 Uiso 1 1 calc R . . C18 C 0.2125(2) 0.9201(5) 0.2777(3) 0.0223(11) Uani 1 1 d . . . C19 C 0.1679(3) 0.9907(4) 0.3242(3) 0.0201(10) Uani 1 1 d . . . C20 C 0.1720(3) 1.1212(5) 0.3217(3) 0.0300(12) Uani 1 1 d . . . H20 H 0.2031 1.1630 0.2950 0.036 Uiso 1 1 calc R . . C21 C 0.1261(3) 1.1814(3) 0.3621(4) 0.0304(7) Uani 1 1 d . . . H21 H 0.1252 1.2676 0.3634 0.036 Uiso 1 1 calc R . . C22 C 0.0835(3) 1.1168(4) 0.3990(3) 0.0271(11) Uani 1 1 d . . . H22 H 0.0516 1.1588 0.4243 0.032 Uiso 1 1 calc R . . C23 C 0.0845(3) 0.9941(5) 0.4013(3) 0.0260(11) Uani 1 1 d . . . C24 C 0.0427(2) 0.9207(4) 0.4452(3) 0.0241(12) Uani 1 1 d . . . C25 C 0.0508(2) 0.7954(5) 0.4549(3) 0.0275(13) Uani 1 1 d . . . H25 H 0.0830 0.7528 0.4306 0.033 Uiso 1 1 calc R . . C26 C 0.0099(2) 0.7344(5) 0.5017(3) 0.0377(15) Uani 1 1 d . . . H26 H 0.0151 0.6496 0.5099 0.045 Uiso 1 1 calc R . . C27 C -0.0376(2) 0.7959(4) 0.5357(3) 0.0250(12) Uani 1 1 d . . . H27 H -0.0666 0.7556 0.5659 0.030 Uiso 1 1 calc R . . C28 C -0.0407(2) 0.9211(4) 0.5232(3) 0.0203(11) Uani 1 1 d . . . C29 C -0.0913(2) 0.9972(5) 0.5570(3) 0.0236(12) Uani 1 1 d . . . C29' C -0.0877(3) 1.1316(5) 0.5439(3) 0.0348(14) Uani 1 1 d . . . H29A H -0.1242 1.1715 0.5655 0.052 Uiso 1 1 calc R . . H29B H -0.0895 1.1477 0.4896 0.052 Uiso 1 1 calc R . . H29C H -0.0472 1.1632 0.5681 0.052 Uiso 1 1 calc R . . C30 C -0.1794(2) 1.0084(5) 0.6317(3) 0.0285(13) Uani 1 1 d . . . C31 C -0.2372(3) 1.0352(5) 0.5893(3) 0.0338(13) Uani 1 1 d . . . C32 C -0.2442(3) 0.9976(6) 0.5058(3) 0.0478(16) Uani 1 1 d . . . H32 H -0.2024 1.0127 0.4832 0.057 Uiso 1 1 calc R . . C33 C -0.2991(3) 1.0720(8) 0.4600(4) 0.065(2) Uani 1 1 d . . . H33A H -0.3411 1.0482 0.4765 0.097 Uiso 1 1 calc R . . H33B H -0.2979 1.0549 0.4060 0.097 Uiso 1 1 calc R . . H33C H -0.2922 1.1590 0.4690 0.097 Uiso 1 1 calc R . . C34 C -0.2605(3) 0.8629(7) 0.4988(4) 0.0588(18) Uani 1 1 d . . . H34A H -0.2244 0.8148 0.5215 0.088 Uiso 1 1 calc R . . H34B H -0.2683 0.8414 0.4453 0.088 Uiso 1 1 calc R . . H34C H -0.2992 0.8458 0.5249 0.088 Uiso 1 1 calc R . . C35 C -0.2867(3) 1.0868(5) 0.6274(4) 0.0448(15) Uani 1 1 d . . . H35 H -0.3269 1.1050 0.6006 0.054 Uiso 1 1 calc R . . C36 C -0.2776(3) 1.1120(5) 0.7047(4) 0.0476(18) Uani 1 1 d . . . H36 H -0.3118 1.1464 0.7300 0.057 Uiso 1 1 calc R . . C37 C -0.2197(3) 1.0875(5) 0.7443(3) 0.0392(15) Uani 1 1 d . . . H37 H -0.2136 1.1076 0.7963 0.047 Uiso 1 1 calc R . . C38 C -0.1700(3) 1.0337(5) 0.7086(3) 0.0320(13) Uani 1 1 d . . . C39 C -0.1065(3) 0.9991(5) 0.7519(3) 0.0413(14) Uani 1 1 d . . . H39 H -0.0850 0.9388 0.7202 0.050 Uiso 1 1 calc R . . C40 C -0.0611(3) 1.1044(6) 0.7635(3) 0.0558(18) Uani 1 1 d . . . H40A H -0.0806 1.1665 0.7941 0.084 Uiso 1 1 calc R . . H40B H -0.0527 1.1390 0.7145 0.084 Uiso 1 1 calc R . . H40C H -0.0205 1.0767 0.7895 0.084 Uiso 1 1 calc R . . C41 C -0.1143(4) 0.9375(9) 0.8282(4) 0.087(3) Uani 1 1 d . . . H41A H -0.0737 0.8979 0.8460 0.130 Uiso 1 1 calc R . . H41B H -0.1486 0.8767 0.8223 0.130 Uiso 1 1 calc R . . H41C H -0.1254 0.9987 0.8650 0.130 Uiso 1 1 calc R . . C42 C 0.1170(5) 0.9259(8) 0.1075(4) 0.135(5) Uani 1 1 d . . . H42A H 0.0903 0.8914 0.0641 0.163 Uiso 1 1 calc R . . H42B H 0.1419 0.8593 0.1334 0.163 Uiso 1 1 calc R . . Cl1 Cl 0.17768(19) 1.0562(5) 0.0719(3) 0.253(3) Uani 1 1 d . . . Cl2 Cl 0.07383(18) 0.9893(5) 0.16254(17) 0.215(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 N1 0.018(2) 0.040(3) 0.020(2) 0.000(2) 0.0030(17) 0.0066(19) N2 0.021(2) 0.022(2) 0.0188(19) -0.0003(18) 0.0028(17) 0.0072(18) N3 0.0234(14) 0.0235(13) 0.0248(13) 0.000(2) 0.0053(11) 0.017(2) N4 0.021(2) 0.027(3) 0.029(2) -0.003(2) 0.0069(19) 0.0082(19) N5 0.030(2) 0.017(2) 0.028(2) 0.0002(19) 0.0093(19) 0.0060(18) C1 0.049(4) 0.063(5) 0.074(4) -0.015(4) -0.017(3) -0.012(3) C2 0.051(4) 0.059(5) 0.062(4) 0.025(4) -0.008(3) 0.008(3) C3 0.019(3) 0.042(3) 0.051(3) 0.003(3) 0.011(3) 0.005(2) C4 0.020(3) 0.021(3) 0.044(3) 0.006(2) -0.004(2) 0.002(2) C5 0.015(3) 0.039(3) 0.062(4) -0.001(3) 0.012(3) -0.001(2) C6 0.013(3) 0.046(4) 0.074(5) 0.020(3) 0.024(3) -0.002(2) C7 0.046(4) 0.045(4) 0.034(3) 0.008(3) 0.017(3) 0.003(3) C8 0.035(3) 0.024(3) 0.028(3) 0.002(2) 0.006(2) 0.002(2) C9 0.052(4) 0.055(4) 0.028(3) 0.006(3) 0.011(3) 0.003(3) C10 0.096(6) 0.102(6) 0.029(3) -0.011(3) -0.007(3) 0.012(5) C11 0.066(5) 0.076(6) 0.123(7) -0.034(5) -0.060(4) 0.024(4) C12 0.036(3) 0.011(3) 0.028(3) 0.000(2) 0.011(2) -0.006(2) C13 0.020(3) 0.027(3) 0.017(2) 0.002(2) 0.003(2) -0.003(2) C13' 0.042(3) 0.012(3) 0.037(3) 0.009(2) 0.014(3) 0.006(2) C14 0.030(3) 0.034(3) 0.018(2) -0.002(2) -0.002(2) -0.003(2) C15 0.041(3) 0.031(3) 0.039(3) -0.013(3) 0.010(3) -0.001(3) C16 0.050(3) 0.022(3) 0.038(3) -0.003(2) 0.029(3) -0.003(3) C17 0.047(3) 0.024(3) 0.039(3) 0.005(2) 0.022(3) -0.010(2) C18 0.017(2) 0.031(3) 0.020(2) -0.007(2) 0.008(2) 0.005(2) C19 0.026(3) 0.015(2) 0.021(2) 0.001(2) 0.012(2) 0.002(2) C20 0.033(3) 0.027(3) 0.032(3) 0.000(2) 0.020(2) -0.001(2) C21 0.0311(18) 0.0223(15) 0.0387(18) -0.007(3) 0.0086(14) 0.011(3) C22 0.030(3) 0.019(3) 0.032(3) -0.003(2) 0.002(2) 0.006(2) C23 0.014(2) 0.036(3) 0.028(3) 0.000(2) -0.0017(19) 0.004(2) C24 0.028(3) 0.018(3) 0.025(3) -0.010(2) -0.003(2) -0.001(2) C25 0.016(2) 0.025(3) 0.042(3) 0.000(2) 0.007(2) -0.004(2) C26 0.025(3) 0.018(3) 0.071(4) 0.002(3) 0.009(3) 0.003(2) C27 0.018(2) 0.022(3) 0.037(3) -0.007(2) 0.016(2) -0.007(2) C28 0.017(2) 0.019(3) 0.026(2) -0.003(2) 0.009(2) -0.006(2) C29 0.020(3) 0.026(3) 0.024(2) 0.003(2) 0.003(2) -0.006(2) C29' 0.026(3) 0.038(3) 0.043(3) 0.011(3) 0.020(3) 0.007(2) C30 0.019(3) 0.032(3) 0.037(3) 0.003(2) 0.014(2) -0.008(2) C31 0.028(3) 0.033(3) 0.043(3) 0.005(3) 0.019(2) -0.003(2) C32 0.035(3) 0.067(5) 0.038(3) 0.001(3) -0.015(3) 0.010(3) C33 0.036(4) 0.100(6) 0.057(4) 0.014(4) -0.005(3) -0.008(4) C34 0.068(5) 0.064(5) 0.042(3) -0.012(3) -0.007(3) -0.006(4) C35 0.045(4) 0.026(3) 0.064(4) -0.009(3) 0.007(3) -0.006(3) C36 0.070(5) 0.018(3) 0.059(4) -0.008(3) 0.039(4) -0.010(3) C37 0.054(4) 0.019(3) 0.047(3) -0.006(3) 0.022(3) -0.013(3) C38 0.038(3) 0.033(3) 0.028(3) 0.000(2) 0.017(2) -0.013(2) C39 0.051(4) 0.042(3) 0.029(3) 0.007(2) -0.008(3) 0.011(3) C40 0.047(4) 0.069(5) 0.053(4) 0.024(3) 0.014(3) -0.003(3) C41 0.074(5) 0.097(6) 0.085(5) 0.053(5) -0.029(4) -0.043(5) C42 0.180(9) 0.141(7) 0.068(5) -0.042(5) -0.099(5) 0.124(7) Cl1 0.172(3) 0.311(6) 0.247(4) 0.188(4) -0.161(3) -0.137(4) Cl2 0.123(2) 0.421(6) 0.0912(17) -0.073(3) -0.0604(16) 0.110(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 N1 C13 1.284(6) . ? N1 C12 1.387(6) . ? N2 C14 1.321(6) . ? N2 C18 1.344(6) . ? N3 C19 1.289(6) . ? N3 C23 1.386(6) . ? N4 C24 1.322(6) . ? N4 C28 1.350(6) . ? N5 C29 1.255(6) . ? N5 C30 1.458(6) . ? C1 C3 1.489(8) . ? C2 C3 1.520(8) . ? C3 C4 1.510(8) . ? C4 C5 1.379(7) . ? C4 C12 1.430(7) . ? C5 C6 1.341(8) . ? C6 C7 1.389(8) . ? C7 C8 1.358(7) . ? C8 C12 1.415(7) . ? C8 C9 1.516(8) . ? C9 C10 1.517(9) . ? C9 C11 1.534(10) . ? C13 C14 1.476(7) . ? C13 C13' 1.500(7) . ? C14 C15 1.382(7) . ? C15 C16 1.394(7) . ? C16 C17 1.341(7) . ? C17 C18 1.391(7) . ? C18 C19 1.506(6) . ? C19 C20 1.441(7) . ? C20 C21 1.405(7) . ? C21 C22 1.348(8) . ? C22 C23 1.352(7) . ? C23 C24 1.458(7) . ? C24 C25 1.398(7) . ? C25 C26 1.407(7) . ? C26 C27 1.376(7) . ? C27 C28 1.397(7) . ? C28 C29 1.507(7) . ? C29 C29' 1.500(7) . ? C30 C38 1.395(7) . ? C30 C31 1.400(8) . ? C31 C35 1.398(7) . ? C31 C32 1.537(8) . ? C32 C34 1.525(9) . ? C32 C33 1.579(9) . ? C35 C36 1.401(8) . ? C36 C37 1.374(9) . ? C37 C38 1.388(7) . ? C38 C39 1.524(8) . ? C39 C40 1.498(9) . ? C39 C41 1.536(8) . ? C42 Cl2 1.546(9) . ? C42 Cl1 2.045(13) . ? 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 C13 N1 C12 123.4(5) . . ? C14 N2 C18 118.6(4) . . ? C19 N3 C23 118.1(3) . . ? C24 N4 C28 119.1(4) . . ? C29 N5 C30 119.8(4) . . ? C1 C3 C4 115.2(5) . . ? C1 C3 C2 112.4(5) . . ? C4 C3 C2 110.6(5) . . ? C5 C4 C12 116.7(5) . . ? C5 C4 C3 122.2(5) . . ? C12 C4 C3 121.1(4) . . ? C6 C5 C4 123.5(5) . . ? C5 C6 C7 119.0(5) . . ? C8 C7 C6 122.5(5) . . ? C7 C8 C12 117.8(5) . . ? C7 C8 C9 121.6(5) . . ? C12 C8 C9 120.6(5) . . ? C8 C9 C10 111.4(5) . . ? C8 C9 C11 110.8(5) . . ? C10 C9 C11 111.8(6) . . ? N1 C12 C8 119.6(5) . . ? N1 C12 C4 119.6(4) . . ? C8 C12 C4 120.5(4) . . ? N1 C13 C14 119.4(5) . . ? N1 C13 C13' 123.5(5) . . ? C14 C13 C13' 117.0(4) . . ? N2 C14 C15 121.4(5) . . ? N2 C14 C13 116.2(5) . . ? C15 C14 C13 122.3(5) . . ? C14 C15 C16 119.7(5) . . ? C17 C16 C15 118.7(5) . . ? C16 C17 C18 118.9(5) . . ? N2 C18 C17 122.5(4) . . ? N2 C18 C19 117.4(4) . . ? C17 C18 C19 120.0(4) . . ? N3 C19 C20 125.1(4) . . ? N3 C19 C18 117.7(4) . . ? C20 C19 C18 117.2(4) . . ? C21 C20 C19 114.2(5) . . ? C22 C21 C20 120.0(3) . . ? C21 C22 C23 122.2(5) . . ? C22 C23 N3 120.2(5) . . ? C22 C23 C24 124.2(5) . . ? N3 C23 C24 115.6(4) . . ? N4 C24 C25 121.8(5) . . ? N4 C24 C23 115.4(4) . . ? C25 C24 C23 122.8(4) . . ? C24 C25 C26 118.1(4) . . ? C27 C26 C25 120.8(5) . . ? C26 C27 C28 116.2(4) . . ? N4 C28 C27 123.9(4) . . ? N4 C28 C29 115.4(4) . . ? C27 C28 C29 120.7(4) . . ? N5 C29 C29' 127.5(5) . . ? N5 C29 C28 116.2(5) . . ? C29' C29 C28 116.2(4) . . ? C38 C30 C31 122.3(5) . . ? C38 C30 N5 118.7(5) . . ? C31 C30 N5 118.7(4) . . ? C35 C31 C30 117.4(5) . . ? C35 C31 C32 124.0(5) . . ? C30 C31 C32 118.4(5) . . ? C34 C32 C31 110.2(5) . . ? C34 C32 C33 108.4(6) . . ? C31 C32 C33 111.6(5) . . ? C31 C35 C36 120.5(6) . . ? C37 C36 C35 120.7(5) . . ? C36 C37 C38 120.4(5) . . ? C37 C38 C30 118.7(5) . . ? C37 C38 C39 121.6(5) . . ? C30 C38 C39 119.7(5) . . ? C40 C39 C38 112.8(5) . . ? C40 C39 C41 109.2(5) . . ? C38 C39 C41 114.1(5) . . ? Cl2 C42 Cl1 106.4(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.750 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.064 # Attachment '1076.cif' data_1076 _database_code_depnum_ccdc_archive 'CCDC 289325' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H45 Cl2 Fe N5, 3(O H2)' _chemical_formula_sum 'C41 H51 Cl2 Fe N5 O3' _chemical_formula_weight 788.62 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 15.1102(9) _cell_length_b 15.1102(9) _cell_length_c 18.4635(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4215.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 5412 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 27.06 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32793 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4162 _reflns_number_gt 2711 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.1577P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(6) _refine_ls_number_reflns 4162 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.2358 _refine_ls_wR_factor_gt 0.2266 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 Fe1 Fe 0.5000 0.0000 1.10553(5) 0.0420(3) Uani 1 2 d S . . Cl1 Cl 0.62009(11) 0.04942(12) 1.04171(9) 0.0544(5) Uani 1 1 d . . . N1 N 0.4029(3) 0.2427(3) 0.9694(2) 0.0451(13) Uani 1 1 d . . . N2 N 0.4566(3) 0.1364(3) 1.1360(3) 0.0437(12) Uani 1 1 d . . . N3 N 0.5000 0.0000 1.2178(3) 0.0434(15) Uani 1 2 d S . . C1 C 0.6541(10) 0.2521(13) 0.8713(10) 0.257(13) Uani 1 1 d . . . H1A H 0.6457 0.2098 0.8317 0.385 Uiso 1 1 calc R . . H1B H 0.6837 0.2226 0.9119 0.385 Uiso 1 1 calc R . . H1C H 0.6906 0.3016 0.8545 0.385 Uiso 1 1 calc R . . C2 C 0.5553(12) 0.3841(7) 0.8996(9) 0.186(8) Uani 1 1 d . . . H2A H 0.5790 0.4105 0.8552 0.279 Uiso 1 1 calc R . . H2B H 0.5881 0.4067 0.9415 0.279 Uiso 1 1 calc R . . H2C H 0.4926 0.3996 0.9045 0.279 Uiso 1 1 calc R . . C3 C 0.5645(5) 0.2868(5) 0.8961(4) 0.0631(19) Uani 1 1 d . . . H3 H 0.5583 0.2662 0.9473 0.076 Uiso 1 1 calc R . . C4 C 0.4853(5) 0.2475(4) 0.8566(3) 0.0542(17) Uani 1 1 d . . . C5 C 0.4841(6) 0.2327(5) 0.7816(4) 0.066(2) Uani 1 1 d . . . H5 H 0.5365 0.2437 0.7547 0.079 Uiso 1 1 calc R . . C6 C 0.4107(5) 0.2033(5) 0.7456(4) 0.061(2) Uani 1 1 d . . . H6 H 0.4130 0.1927 0.6949 0.074 Uiso 1 1 calc R . . C7 C 0.3338(5) 0.1892(5) 0.7831(3) 0.0592(19) Uani 1 1 d . . . H7 H 0.2819 0.1721 0.7577 0.071 Uiso 1 1 calc R . . C8 C 0.3306(5) 0.1997(4) 0.8583(3) 0.0487(17) Uani 1 1 d . . . C9 C 0.4074(5) 0.2260(4) 0.8940(3) 0.0495(16) Uani 1 1 d . . . C10 C 0.1615(5) 0.2111(5) 0.8558(4) 0.0631(19) Uani 1 1 d . . . H10A H 0.1498 0.1636 0.8209 0.095 Uiso 1 1 calc R . . H10B H 0.1712 0.2668 0.8299 0.095 Uiso 1 1 calc R . . H10C H 0.1106 0.2174 0.8883 0.095 Uiso 1 1 calc R . . C11 C 0.2363(5) 0.0957(5) 0.9334(4) 0.0610(18) Uani 1 1 d . . . H11A H 0.2323 0.0520 0.8943 0.091 Uiso 1 1 calc R . . H11B H 0.1825 0.0931 0.9630 0.091 Uiso 1 1 calc R . . H11C H 0.2879 0.0826 0.9637 0.091 Uiso 1 1 calc R . . C12 C 0.2457(4) 0.1877(4) 0.9011(3) 0.0516(16) Uani 1 1 d . . . H12 H 0.2480 0.2303 0.9425 0.062 Uiso 1 1 calc R . . C13 C 0.4321(4) 0.1846(4) 1.0141(3) 0.0448(15) Uani 1 1 d . . . H13 H 0.4520 0.1288 0.9968 0.054 Uiso 1 1 calc R . . C14 C 0.4347(4) 0.2040(4) 1.0914(3) 0.0411(14) Uani 1 1 d . . . C15 C 0.4154(4) 0.2876(5) 1.1172(3) 0.0486(16) Uani 1 1 d . . . H15 H 0.4021 0.3346 1.0848 0.058 Uiso 1 1 calc R . . C16 C 0.4160(5) 0.3013(5) 1.1915(4) 0.061(2) Uani 1 1 d . . . H16 H 0.4013 0.3578 1.2106 0.073 Uiso 1 1 calc R . . C17 C 0.4380(4) 0.2333(5) 1.2372(3) 0.0536(17) Uani 1 1 d . . . H17 H 0.4401 0.2425 1.2881 0.064 Uiso 1 1 calc R . . C18 C 0.4569(4) 0.1511(4) 1.2080(3) 0.0437(15) Uani 1 1 d . . . C19 C 0.4795(4) 0.0742(5) 1.2547(3) 0.0457(15) Uani 1 1 d . . . C20 C 0.4787(4) 0.0742(5) 1.3302(3) 0.0543(17) Uani 1 1 d . . . H20 H 0.4631 0.1264 1.3560 0.065 Uiso 1 1 calc R . . C21 C 0.5000 0.0000 1.3664(4) 0.055(2) Uani 1 2 d S . . H21 H 0.5000 0.0000 1.4178 0.066 Uiso 1 2 calc SR . . O1 O 0.5000 0.5000 0.2973(4) 0.100(3) Uani 1 2 d S . . O2 O 0.3763(7) 0.3715(5) 0.5902(5) 0.169(5) 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 Fe1 0.0481(7) 0.0581(8) 0.0198(5) 0.000 0.000 0.0033(6) Cl1 0.0509(9) 0.0737(11) 0.0386(8) -0.0047(8) 0.0089(7) -0.0041(8) N1 0.055(3) 0.052(3) 0.028(3) 0.000(2) 0.002(2) 0.001(2) N2 0.040(3) 0.063(3) 0.029(2) -0.006(2) 0.006(2) -0.001(2) N3 0.038(4) 0.064(5) 0.029(3) 0.000 0.000 -0.001(4) C1 0.140(12) 0.30(2) 0.33(2) -0.22(2) 0.165(15) -0.108(14) C2 0.243(18) 0.068(7) 0.246(17) -0.029(9) -0.146(15) -0.009(9) C3 0.075(5) 0.064(4) 0.051(4) 0.003(4) 0.019(4) -0.012(4) C4 0.070(5) 0.044(3) 0.049(4) 0.008(3) 0.011(4) 0.008(3) C5 0.098(7) 0.054(4) 0.045(4) 0.011(3) 0.030(4) 0.022(4) C6 0.097(6) 0.057(4) 0.030(3) -0.001(3) 0.009(4) 0.016(4) C7 0.089(6) 0.054(4) 0.035(3) -0.001(3) -0.005(4) 0.013(4) C8 0.076(4) 0.045(3) 0.025(3) 0.001(3) -0.001(3) 0.012(3) C9 0.080(5) 0.036(3) 0.032(3) 0.000(3) 0.008(3) 0.010(3) C10 0.076(5) 0.061(4) 0.052(4) 0.005(4) -0.018(4) 0.003(4) C11 0.071(5) 0.066(5) 0.046(4) 0.008(3) -0.005(4) 0.008(4) C12 0.065(4) 0.055(4) 0.035(3) -0.004(3) -0.009(3) 0.001(3) C13 0.056(4) 0.043(3) 0.035(3) -0.007(3) 0.010(3) -0.004(3) C14 0.041(3) 0.053(4) 0.029(3) -0.002(3) 0.006(2) -0.001(3) C15 0.048(4) 0.060(4) 0.038(3) -0.002(3) -0.005(3) 0.000(3) C16 0.061(4) 0.071(5) 0.050(4) -0.034(4) 0.000(3) 0.002(4) C17 0.048(4) 0.078(5) 0.035(3) -0.010(3) -0.006(3) 0.002(3) C18 0.041(3) 0.063(4) 0.027(3) -0.007(3) -0.002(2) 0.004(3) C19 0.044(3) 0.068(4) 0.025(3) -0.009(3) -0.002(2) -0.005(3) C20 0.056(4) 0.080(5) 0.027(3) -0.005(3) 0.004(3) -0.002(3) C21 0.057(6) 0.089(8) 0.020(3) 0.000 0.000 -0.012(5) O1 0.139(8) 0.090(6) 0.072(5) 0.000 0.000 -0.013(6) O2 0.252(10) 0.088(5) 0.166(7) 0.051(5) 0.103(7) 0.117(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 2.073(6) . ? Fe1 N2 2.234(5) 2_655 ? Fe1 N2 2.234(5) . ? Fe1 Cl1 2.2889(17) . ? Fe1 Cl1 2.2889(17) 2_655 ? N1 C13 1.283(8) . ? N1 C9 1.418(7) . ? N2 C18 1.348(7) . ? N2 C14 1.353(8) . ? N3 C19 1.348(7) 2_655 ? N3 C19 1.348(7) . ? C1 C3 1.523(16) . ? C2 C3 1.479(13) . ? C3 C4 1.521(11) . ? C4 C5 1.402(9) . ? C4 C9 1.403(9) . ? C5 C6 1.368(11) . ? C6 C7 1.369(11) . ? C7 C8 1.398(8) . ? C8 C9 1.392(10) . ? C8 C12 1.517(9) . ? C10 C12 1.563(9) . ? C11 C12 1.519(10) . ? C13 C14 1.458(7) . ? C14 C15 1.381(9) . ? C15 C16 1.386(9) . ? C16 C17 1.370(10) . ? C17 C18 1.384(9) . ? C18 C19 1.487(9) . ? C19 C20 1.394(8) . ? C20 C21 1.344(8) . ? C21 C20 1.344(8) 2_655 ? 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 N3 Fe1 N2 75.42(13) . 2_655 ? N3 Fe1 N2 75.42(13) . . ? N2 Fe1 N2 150.8(3) 2_655 . ? N3 Fe1 Cl1 120.99(5) . . ? N2 Fe1 Cl1 101.42(14) 2_655 . ? N2 Fe1 Cl1 93.50(13) . . ? N3 Fe1 Cl1 120.99(5) . 2_655 ? N2 Fe1 Cl1 93.50(13) 2_655 2_655 ? N2 Fe1 Cl1 101.42(14) . 2_655 ? Cl1 Fe1 Cl1 118.03(9) . 2_655 ? C13 N1 C9 119.5(5) . . ? C18 N2 C14 118.4(5) . . ? C18 N2 Fe1 113.6(4) . . ? C14 N2 Fe1 128.0(4) . . ? C19 N3 C19 119.3(7) 2_655 . ? C19 N3 Fe1 120.4(3) 2_655 . ? C19 N3 Fe1 120.4(3) . . ? C2 C3 C4 109.6(8) . . ? C2 C3 C1 116.0(12) . . ? C4 C3 C1 114.9(8) . . ? C5 C4 C9 116.0(7) . . ? C5 C4 C3 123.1(7) . . ? C9 C4 C3 120.9(6) . . ? C6 C5 C4 122.8(7) . . ? C5 C6 C7 119.5(6) . . ? C6 C7 C8 120.9(8) . . ? C9 C8 C7 118.2(7) . . ? C9 C8 C12 119.5(5) . . ? C7 C8 C12 122.1(6) . . ? C8 C9 C4 122.2(6) . . ? C8 C9 N1 118.4(6) . . ? C4 C9 N1 118.8(6) . . ? C8 C12 C11 113.2(6) . . ? C8 C12 C10 112.5(5) . . ? C11 C12 C10 109.9(6) . . ? N1 C13 C14 120.1(5) . . ? N2 C14 C15 122.2(5) . . ? N2 C14 C13 116.7(5) . . ? C15 C14 C13 121.1(6) . . ? C14 C15 C16 118.4(7) . . ? C17 C16 C15 119.9(7) . . ? C16 C17 C18 118.9(6) . . ? N2 C18 C17 122.1(6) . . ? N2 C18 C19 116.3(5) . . ? C17 C18 C19 121.5(5) . . ? N3 C19 C20 120.5(6) . . ? N3 C19 C18 114.2(5) . . ? C20 C19 C18 125.3(6) . . ? C21 C20 C19 119.6(7) . . ? C20 C21 C20 120.5(8) . 2_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.178 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.141 # Attachment '04124.cif' # Attachment '04124.cif' data_04124 _database_code_depnum_ccdc_archive 'CCDC 289326' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C41 H45 Br2 N5 Ni) (C2 H3 N)' _chemical_formula_sum 'C43 H48 Br2 N6 Ni' _chemical_formula_weight 867.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 14.9110(15) _cell_length_b 14.9110(15) _cell_length_c 19.143(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4256.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 982 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 21.50 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 2.369 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.347 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 5717 reflections (SADABS); Rint 0.065 before correction and 0.039 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30818 _diffrn_reflns_av_R_equivalents 0.0946 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3754 _reflns_number_gt 1963 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 ; Disordered MeCN was omitted using the SQUEEZE option of PLATON. The solvent accessible voids give an estimated 104e/cell to be added. Four solvent MeCN molecules/unit cell accounting for 88e were included in the formula, FWt, (000) and density calculations. PLATON Reference : Spek, A.L. (1990), Acta Cryst. A46, C-34 The Ni atom is located on a two-fold symmetry axis, primed atoms generated by 2x, 1-y, z. 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^)+(0.0590P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(19) _refine_ls_number_reflns 3754 _refine_ls_number_parameters 232 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1095 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1204 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 0.848 _refine_ls_restrained_S_all 0.848 _refine_ls_shift/su_max 0.005 _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 Ni1 Ni 1.0000 0.5000 -0.10713(5) 0.0630(4) Uani 1 2 d S . . Br1 Br 0.94752(6) 0.63526(6) -0.05381(4) 0.0851(3) Uani 1 1 d . . . N1 N 0.7599(4) 0.4069(4) 0.0323(3) 0.0665(18) Uani 1 1 d . . . N2 N 0.8670(4) 0.4583(4) -0.1292(2) 0.0645(16) Uani 1 1 d . . . N3 N 1.0000 0.5000 -0.2107(3) 0.063(2) Uani 1 2 d S . . C1 C 0.7784(4) 0.4077(6) 0.1066(3) 0.063(2) Uani 1 1 d . . . C2 C 0.8025(5) 0.3307(6) 0.1385(3) 0.066(2) Uani 1 1 d . . . C3 C 0.8119(5) 0.3347(7) 0.2118(3) 0.089(3) Uani 1 1 d . . . H3 H 0.8303 0.2828 0.2367 0.107 Uiso 1 1 calc R . . C4 C 0.7950(6) 0.4112(9) 0.2472(5) 0.104(4) Uani 1 1 d . . . H4 H 0.8030 0.4123 0.2964 0.124 Uiso 1 1 calc R . . C5 C 0.7683(6) 0.4828(9) 0.2154(5) 0.109(4) Uani 1 1 d . . . H5 H 0.7550 0.5345 0.2426 0.131 Uiso 1 1 calc R . . C6 C 0.7580(5) 0.4877(7) 0.1425(4) 0.079(3) Uani 1 1 d . B . C7 C 0.8136(5) 0.2456(6) 0.0982(3) 0.072(2) Uani 1 1 d . . . H7 H 0.7740 0.2497 0.0562 0.087 Uiso 1 1 calc R . . C8 C 0.9082(5) 0.2357(5) 0.0726(3) 0.083(2) Uani 1 1 d . . . H8A H 0.9240 0.2879 0.0440 0.125 Uiso 1 1 d R . . H8B H 0.9130 0.1811 0.0443 0.125 Uiso 1 1 d R . . H8C H 0.9492 0.2317 0.1124 0.125 Uiso 1 1 d R . . C9 C 0.7877(5) 0.1612(6) 0.1372(4) 0.094(3) Uani 1 1 d . . . H9A H 0.8329 0.1483 0.1730 0.141 Uiso 1 1 d R . . H9B H 0.7844 0.1108 0.1044 0.141 Uiso 1 1 d R . . H9C H 0.7292 0.1697 0.1594 0.141 Uiso 1 1 d R . . C10 C 0.7219(6) 0.5703(7) 0.1052(5) 0.108(3) Uani 1 1 d . . . H10 H 0.7564 0.5880 0.0626 0.129 Uiso 1 1 calc R A 1 C11 C 0.6207(6) 0.5561(8) 0.0927(5) 0.161(5) Uani 1 1 d . B . H11A H 0.5869 0.5801 0.1324 0.241 Uiso 1 1 d R . . H11B H 0.6083 0.4918 0.0879 0.241 Uiso 1 1 d R . . H11C H 0.6025 0.5873 0.0499 0.241 Uiso 1 1 d R . . C12 C 0.712(2) 0.6419(17) 0.1567(11) 0.118(10) Uani 0.50 1 d P B 1 H12A H 0.7689 0.6737 0.1605 0.177 Uiso 0.50 1 d PR B 1 H12B H 0.6954 0.6169 0.2024 0.177 Uiso 0.50 1 d PR B 1 H12C H 0.6648 0.6837 0.1414 0.177 Uiso 0.50 1 d PR B 1 C12' C 0.761(2) 0.6732(18) 0.1170(14) 0.171(14) Uani 0.50 1 d P B 2 H12D H 0.7280 0.7145 0.0865 0.257 Uiso 0.50 1 d PR B 2 H12E H 0.8249 0.6750 0.1053 0.257 Uiso 0.50 1 d PR B 2 H12F H 0.7527 0.6913 0.1658 0.257 Uiso 0.50 1 d PR B 2 C13 C 0.8193(5) 0.4341(5) -0.0091(3) 0.060(2) Uani 1 1 d . . . H13 H 0.8762 0.4522 0.0083 0.071 Uiso 1 1 calc R . . C14 C 0.8003(6) 0.4377(5) -0.0861(3) 0.058(2) Uani 1 1 d . . . C15 C 0.7138(6) 0.4183(5) -0.1083(4) 0.074(2) Uani 1 1 d . . . H15 H 0.6692 0.4027 -0.0750 0.088 Uiso 1 1 calc R . . C16 C 0.6918(6) 0.4213(6) -0.1794(4) 0.084(3) Uani 1 1 d . . . H16 H 0.6331 0.4098 -0.1964 0.101 Uiso 1 1 calc R . . C17 C 0.7620(7) 0.4423(5) -0.2222(4) 0.079(3) Uani 1 1 d . . . H17 H 0.7510 0.4446 -0.2710 0.095 Uiso 1 1 calc R . . C18 C 0.8489(6) 0.4607(5) -0.1991(3) 0.070(2) Uani 1 1 d . . . C19 C 0.9282(6) 0.4828(5) -0.2435(3) 0.075(2) Uani 1 1 d . . . C20 C 0.9252(7) 0.4802(5) -0.3166(3) 0.091(3) Uani 1 1 d . . . H20 H 0.8714 0.4647 -0.3403 0.109 Uiso 1 1 calc R . . C21 C 1.0000 0.5000 -0.3523(5) 0.105(5) Uani 1 2 d S . . H21 H 1.0000 0.5000 -0.4020 0.126 Uiso 1 2 calc SR . . 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 Ni1 0.1003(10) 0.0690(9) 0.0195(4) 0.000 0.000 0.0202(8) Br1 0.1116(7) 0.0876(6) 0.0560(4) -0.0167(5) -0.0054(5) 0.0193(5) N1 0.078(4) 0.089(5) 0.033(3) -0.021(3) -0.011(3) 0.005(4) N2 0.102(5) 0.067(4) 0.024(2) -0.005(3) 0.002(3) 0.020(3) N3 0.096(7) 0.073(6) 0.019(3) 0.000 0.000 0.021(6) C1 0.046(5) 0.115(7) 0.029(3) -0.022(5) -0.001(3) -0.004(5) C2 0.055(5) 0.116(7) 0.028(3) -0.002(5) -0.003(3) 0.002(5) C3 0.059(5) 0.177(10) 0.031(3) -0.017(5) 0.000(4) -0.019(5) C4 0.052(7) 0.214(14) 0.045(5) -0.039(7) -0.001(4) -0.011(7) C5 0.061(6) 0.191(12) 0.076(7) -0.075(7) 0.004(5) 0.000(8) C6 0.055(5) 0.124(8) 0.057(4) -0.044(5) -0.009(4) 0.006(5) C7 0.074(6) 0.111(7) 0.032(4) 0.008(4) 0.000(4) -0.008(5) C8 0.097(7) 0.101(6) 0.052(5) -0.006(4) 0.021(4) -0.009(5) C9 0.089(7) 0.137(8) 0.056(5) 0.010(5) -0.005(4) -0.004(6) C10 0.075(7) 0.147(10) 0.101(6) -0.075(7) 0.000(6) 0.014(6) C11 0.096(9) 0.272(16) 0.115(8) 0.014(9) -0.014(6) 0.030(9) C12 0.18(3) 0.083(17) 0.088(15) -0.035(13) 0.028(15) 0.007(16) C12' 0.22(4) 0.11(3) 0.18(3) -0.07(2) -0.09(3) 0.06(2) C13 0.080(5) 0.061(5) 0.038(4) -0.003(4) -0.017(4) 0.011(4) C14 0.084(6) 0.057(5) 0.034(3) -0.015(3) -0.026(4) 0.012(4) C15 0.106(7) 0.065(5) 0.050(4) -0.002(4) -0.011(5) 0.008(5) C16 0.105(7) 0.087(6) 0.060(5) 0.000(5) -0.038(5) 0.003(6) C17 0.148(9) 0.048(5) 0.041(4) 0.000(4) -0.022(5) 0.009(5) C18 0.114(7) 0.056(5) 0.039(4) -0.012(3) -0.039(4) 0.022(5) C19 0.119(7) 0.079(6) 0.026(3) -0.004(4) -0.013(4) 0.033(5) C20 0.157(9) 0.079(6) 0.037(4) -0.017(4) -0.019(5) 0.060(6) C21 0.162(14) 0.119(11) 0.033(5) 0.000 0.000 0.070(10) _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 Ni1 N3 1.983(6) . ? Ni1 N2 2.121(6) . ? Ni1 N2 2.121(6) 2_765 ? Ni1 Br1 2.3921(9) . ? Ni1 Br1 2.3921(9) 2_765 ? N1 C13 1.256(8) . ? N1 C1 1.447(8) . ? N2 C14 1.328(8) . ? N2 C18 1.365(7) . ? N3 C19 1.268(8) . ? N3 C19 1.268(8) 2_765 ? C1 C2 1.350(10) . ? C1 C6 1.409(10) . ? C2 C3 1.412(8) . ? C2 C7 1.494(10) . ? C3 C4 1.349(12) . ? C4 C5 1.292(13) . ? C5 C6 1.407(11) . ? C6 C10 1.523(12) . ? C7 C8 1.501(9) . ? C7 C9 1.513(10) . ? C10 C12 1.46(2) . ? C10 C11 1.542(11) . ? C10 C12' 1.66(3) . ? C13 C14 1.502(8) . ? C14 C15 1.389(10) . ? C15 C16 1.400(10) . ? C16 C17 1.365(11) . ? C17 C18 1.396(10) . ? C18 C19 1.492(11) . ? C19 C20 1.400(8) . ? C20 C21 1.342(9) . ? C21 C20 1.342(9) 2_765 ? 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 N3 Ni1 N2 78.48(13) . . ? N3 Ni1 N2 78.48(13) . 2_765 ? N2 Ni1 N2 157.0(3) . 2_765 ? N3 Ni1 Br1 115.26(3) . . ? N2 Ni1 Br1 91.53(14) . . ? N2 Ni1 Br1 98.26(15) 2_765 . ? N3 Ni1 Br1 115.26(3) . 2_765 ? N2 Ni1 Br1 98.26(15) . 2_765 ? N2 Ni1 Br1 91.53(14) 2_765 2_765 ? Br1 Ni1 Br1 129.48(5) . 2_765 ? C13 N1 C1 118.9(6) . . ? C14 N2 C18 117.9(6) . . ? C14 N2 Ni1 130.0(4) . . ? C18 N2 Ni1 111.9(5) . . ? C19 N3 C19 120.6(8) . 2_765 ? C19 N3 Ni1 119.7(4) . . ? C19 N3 Ni1 119.7(4) 2_765 . ? C2 C1 C6 123.8(7) . . ? C2 C1 N1 119.2(7) . . ? C6 C1 N1 116.4(7) . . ? C1 C2 C3 116.1(8) . . ? C1 C2 C7 121.2(6) . . ? C3 C2 C7 122.6(8) . . ? C4 C3 C2 121.1(9) . . ? C5 C4 C3 121.3(9) . . ? C4 C5 C6 122.9(10) . . ? C5 C6 C1 114.7(9) . . ? C5 C6 C10 123.0(9) . . ? C1 C6 C10 122.2(6) . . ? C2 C7 C8 110.9(6) . . ? C2 C7 C9 115.1(6) . . ? C8 C7 C9 108.6(7) . . ? C12 C10 C6 108.2(13) . . ? C12 C10 C11 95.9(13) . . ? C6 C10 C11 107.9(9) . . ? C12 C10 C12' 43.0(11) . . ? C6 C10 C12' 124.1(12) . . ? C11 C10 C12' 119.5(13) . . ? N1 C13 C14 119.9(7) . . ? N2 C14 C15 123.6(6) . . ? N2 C14 C13 118.5(7) . . ? C15 C14 C13 117.9(7) . . ? C14 C15 C16 120.5(8) . . ? C17 C16 C15 114.3(8) . . ? C16 C17 C18 124.6(7) . . ? N2 C18 C17 119.2(8) . . ? N2 C18 C19 114.0(7) . . ? C17 C18 C19 126.8(6) . . ? N3 C19 C20 121.8(9) . . ? N3 C19 C18 115.6(5) . . ? C20 C19 C18 122.5(8) . . ? C21 C20 C19 118.5(9) . . ? C20 C21 C20 118.7(10) 2_765 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.547 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.074 # Attachment '05124.cif' data_05124 _database_code_depnum_ccdc_archive 'CCDC 289327' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H45 Cl2 N5 Zn' _chemical_formula_sum 'C41 H45 Cl2 N5 Zn' _chemical_formula_weight 744.09 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' Cl Cl 0.1484 0.1585 '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 Tetragonal _symmetry_space_group_name_H-M P4(2)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' _cell_length_a 15.044(7) _cell_length_b 15.044(7) _cell_length_c 18.659(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4223(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 819 _cell_measurement_theta_min 2.183 _cell_measurement_theta_max 24.311 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.325 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 6317 reflections(SADABS);Rint 0.114 before correction and 0.101 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16378 _diffrn_reflns_av_R_equivalents 0.1391 _diffrn_reflns_av_sigmaI/netI 0.0678 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2092 _reflns_number_gt 1667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 ; Data was poor.Gemini was used to find the cell.The isopropyl on C2 is disordered, C21 and C9 was refined as isotropic. 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^)+(0.1764P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_number_reflns 2092 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2221 _refine_ls_wR_factor_gt 0.2079 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.006 _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 0.0000 0.5000 0.39675(6) 0.0336(4) Uani 1 2 d S . . N1 N 0.2436(5) 0.5975(5) 0.5326(3) 0.0408(17) Uani 1 1 d . . . N2 N 0.1379(5) 0.5438(4) 0.3680(3) 0.0370(17) Uani 1 1 d . . . N3 N 0.0000 0.5000 0.2876(4) 0.040(2) Uani 1 2 d S . . Cl1 Cl -0.04719(17) 0.61978(16) 0.45777(12) 0.0459(6) Uani 1 1 d . . . C1 C 0.2242(6) 0.5941(6) 0.6069(4) 0.038(2) Uani 1 1 d . . . C2 C 0.2462(6) 0.5147(8) 0.6442(5) 0.056(3) Uani 1 1 d . . . C3 C 0.2305(7) 0.5192(10) 0.7198(5) 0.060(4) Uani 1 1 d . . . H3 H 0.2400 0.4671 0.7475 0.072 Uiso 1 1 calc R . . C4 C 0.2033(7) 0.5922(8) 0.7530(6) 0.060(3) Uani 1 1 d . . . H4 H 0.1950 0.5913 0.8035 0.072 Uiso 1 1 calc R . . C5 C 0.1870(9) 0.6701(10) 0.7152(4) 0.066(4) Uani 1 1 d . . . H5 H 0.1671 0.7222 0.7390 0.079 Uiso 1 1 calc R . . C6 C 0.2007(6) 0.6695(7) 0.6404(4) 0.043(2) Uani 1 1 d . . . C7 C 0.2852(7) 0.4343(8) 0.6055(6) 0.062(3) Uani 1 1 d . . . H7 H 0.2635 0.4360 0.5549 0.074 Uiso 1 1 calc R . . C8 C 0.3836(11) 0.4454(14) 0.6037(11) 0.142(9) Uani 1 1 d . . . H8A H 0.4079 0.4364 0.6519 0.213 Uiso 1 1 calc R . . H8B H 0.3982 0.5055 0.5872 0.213 Uiso 1 1 calc R . . H8C H 0.4095 0.4017 0.5708 0.213 Uiso 1 1 calc R . . C9 C 0.267(3) 0.359(2) 0.6303(14) 0.215(15) Uiso 1 1 d . . . H9A H 0.2337 0.3248 0.5944 0.322 Uiso 1 1 calc R . . H9B H 0.2301 0.3658 0.6735 0.322 Uiso 1 1 calc R . . H9C H 0.3217 0.3276 0.6426 0.322 Uiso 1 1 calc R . . C10 C 0.1855(7) 0.7580(7) 0.5976(4) 0.049(2) Uani 1 1 d . . . H10 H 0.2253 0.7557 0.5547 0.059 Uiso 1 1 calc R . . C11 C 0.0936(8) 0.7637(10) 0.5706(6) 0.060(3) Uani 1 1 d . . . H11A H 0.0525 0.7691 0.6111 0.090 Uiso 1 1 calc R . . H11B H 0.0795 0.7099 0.5433 0.090 Uiso 1 1 calc R . . H11C H 0.0877 0.8158 0.5395 0.090 Uiso 1 1 calc R . . C12 C 0.2119(8) 0.8393(8) 0.6400(5) 0.059(3) Uani 1 1 d . . . H12A H 0.2253 0.8882 0.6071 0.089 Uiso 1 1 calc R . . H12B H 0.2647 0.8258 0.6689 0.089 Uiso 1 1 calc R . . H12C H 0.1629 0.8566 0.6717 0.089 Uiso 1 1 calc R . . C13 C 0.1849(6) 0.5677(6) 0.4893(5) 0.043(2) Uani 1 1 d . . . H13 H 0.1292 0.5475 0.5068 0.052 Uiso 1 1 calc R . . C14 C 0.2044(6) 0.5648(5) 0.4121(4) 0.0302(16) Uani 1 1 d . . . C15 C 0.2890(7) 0.5851(7) 0.3867(5) 0.045(2) Uani 1 1 d . . . H15 H 0.3346 0.6026 0.4190 0.054 Uiso 1 1 calc R . . C16 C 0.3061(8) 0.5795(7) 0.3127(5) 0.057(3) Uani 1 1 d . . . H16 H 0.3641 0.5889 0.2942 0.068 Uiso 1 1 calc R . . C17 C 0.2355(8) 0.5600(7) 0.2680(5) 0.053(3) Uani 1 1 d . . . H17 H 0.2444 0.5592 0.2175 0.063 Uiso 1 1 calc R . . C18 C 0.1515(7) 0.5414(6) 0.2957(5) 0.041(2) Uani 1 1 d . . . C19 C 0.0748(7) 0.5198(6) 0.2520(11) 0.048(3) Uani 1 1 d . . . C20 C 0.0766(7) 0.5215(6) 0.1767(4) 0.045(2) Uani 1 1 d . . . H20 H 0.1290 0.5370 0.1511 0.053 Uiso 1 1 calc R . . C21 C 0.0000 0.5000 0.1421(12) 0.073(5) Uiso 1 2 d S . . H21 H 0.0000 0.5000 0.0912 0.088 Uiso 1 2 calc SR . . 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 0.0463(8) 0.0335(7) 0.0210(7) 0.000 0.000 -0.0023(6) N1 0.047(4) 0.044(4) 0.031(3) 0.009(3) -0.003(3) -0.010(3) N2 0.052(4) 0.030(3) 0.029(3) 0.008(3) 0.015(3) 0.001(3) N3 0.079(8) 0.018(4) 0.023(4) 0.000 0.000 0.005(5) Cl1 0.0539(13) 0.0455(13) 0.0382(10) -0.0141(10) -0.0027(10) 0.0026(11) C1 0.034(4) 0.052(5) 0.029(4) 0.010(4) -0.007(4) -0.021(4) C2 0.033(4) 0.081(8) 0.052(5) 0.024(5) -0.016(4) -0.024(5) C3 0.048(6) 0.092(10) 0.041(4) 0.040(6) 0.000(4) -0.018(5) C4 0.053(5) 0.101(9) 0.026(4) 0.008(6) -0.004(5) -0.029(6) C5 0.068(8) 0.103(10) 0.025(4) -0.004(5) -0.006(5) -0.046(7) C6 0.037(4) 0.075(6) 0.017(3) 0.009(4) -0.002(3) -0.019(4) C7 0.056(6) 0.058(6) 0.072(7) 0.040(6) -0.002(6) 0.004(5) C8 0.063(9) 0.150(17) 0.21(2) -0.096(16) 0.055(11) -0.005(10) C10 0.057(6) 0.059(6) 0.031(4) -0.003(4) 0.000(4) -0.024(5) C11 0.065(8) 0.075(9) 0.040(6) -0.004(6) -0.009(6) -0.001(6) C12 0.069(7) 0.062(6) 0.047(5) 0.000(5) 0.007(5) -0.006(5) C13 0.045(5) 0.048(5) 0.037(5) 0.016(4) 0.004(4) 0.001(4) C14 0.034(4) 0.029(4) 0.028(4) 0.002(3) 0.003(4) -0.005(3) C15 0.053(6) 0.050(5) 0.032(5) -0.004(4) 0.008(4) -0.011(4) C16 0.063(6) 0.054(6) 0.055(6) -0.012(5) 0.032(5) -0.019(5) C17 0.073(7) 0.057(6) 0.029(5) 0.001(4) 0.022(5) 0.011(5) C18 0.066(6) 0.026(4) 0.030(4) 0.000(3) 0.010(4) 0.000(4) C19 0.070(5) 0.050(9) 0.025(4) -0.004(8) 0.024(6) 0.000(4) C20 0.073(6) 0.041(5) 0.020(4) 0.002(3) 0.011(4) 0.009(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 Zn1 N3 2.036(8) . ? Zn1 Cl1 2.247(2) . ? Zn1 Cl1 2.247(2) 2_565 ? Zn1 N2 2.242(7) . ? Zn1 N2 2.242(7) 2_565 ? N1 C13 1.278(12) . ? N1 C1 1.418(10) . ? N2 C14 1.332(11) . ? N2 C18 1.364(10) . ? N3 C19 1.340(12) . ? N3 C19 1.340(12) 2_565 ? C1 C6 1.344(14) . ? C1 C2 1.422(14) . ? C2 C3 1.432(14) . ? C2 C7 1.525(18) . ? C3 C4 1.327(17) . ? C3 H3 0.9500 . ? C4 C5 1.389(19) . ? C4 H4 0.9500 . ? C5 C6 1.411(11) . ? C5 H5 0.9500 . ? C6 C10 1.569(14) . ? C7 C9 1.25(3) . ? C7 C8 1.491(19) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.474(15) . ? C10 C12 1.510(14) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.471(11) . ? C13 H13 0.9500 . ? C14 C15 1.392(13) . ? C15 C16 1.407(14) . ? C15 H15 0.9500 . ? C16 C17 1.382(15) . ? C16 H16 0.9500 . ? C17 C18 1.395(14) . ? C17 H17 0.9500 . ? C18 C19 1.451(19) . ? C19 C20 1.41(2) . ? C20 C21 1.360(14) . ? C20 H20 0.9500 . ? C21 C20 1.360(14) 2_565 ? C21 H21 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Zn1 Cl1 120.45(7) . . ? N3 Zn1 Cl1 120.45(7) . 2_565 ? Cl1 Zn1 Cl1 119.10(14) . 2_565 ? N3 Zn1 N2 76.16(18) . . ? Cl1 Zn1 N2 100.24(19) . . ? Cl1 Zn1 N2 93.71(18) 2_565 . ? N3 Zn1 N2 76.16(18) . 2_565 ? Cl1 Zn1 N2 93.71(18) . 2_565 ? Cl1 Zn1 N2 100.24(19) 2_565 2_565 ? N2 Zn1 N2 152.3(4) . 2_565 ? C13 N1 C1 117.6(7) . . ? C14 N2 C18 120.3(8) . . ? C14 N2 Zn1 128.1(5) . . ? C18 N2 Zn1 111.5(6) . . ? C19 N3 C19 120.5(19) . 2_565 ? C19 N3 Zn1 119.8(9) . . ? C19 N3 Zn1 119.8(9) 2_565 . ? C6 C1 C2 122.9(8) . . ? C6 C1 N1 118.7(7) . . ? C2 C1 N1 117.5(9) . . ? C1 C2 C3 113.8(11) . . ? C1 C2 C7 121.6(8) . . ? C3 C2 C7 124.5(10) . . ? C4 C3 C2 123.4(12) . . ? C4 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? C3 C4 C5 121.0(10) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 118.1(13) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C1 C6 C5 120.3(10) . . ? C1 C6 C10 121.2(7) . . ? C5 C6 C10 118.5(10) . . ? C9 C7 C8 109(2) . . ? C9 C7 C2 117.1(19) . . ? C8 C7 C2 107.7(11) . . ? C9 C7 H7 107.4 . . ? C8 C7 H7 107.5 . . ? C2 C7 H7 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C12 112.3(10) . . ? C11 C10 C6 111.1(9) . . ? C12 C10 C6 112.5(7) . . ? C11 C10 H10 106.9 . . ? C12 C10 H10 106.9 . . ? C6 C10 H10 106.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 119.4(8) . . ? N1 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? N2 C14 C15 121.9(8) . . ? N2 C14 C13 117.5(7) . . ? C15 C14 C13 120.5(9) . . ? C16 C15 C14 119.1(9) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 117.8(9) . . ? C17 C16 H16 121.1 . . ? C15 C16 H16 121.1 . . ? C18 C17 C16 120.9(8) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? N2 C18 C17 119.8(9) . . ? N2 C18 C19 116.3(10) . . ? C17 C18 C19 123.8(10) . . ? N3 C19 C20 121.1(13) . . ? N3 C19 C18 116.0(15) . . ? C20 C19 C18 122.9(10) . . ? C21 C20 C19 116.9(12) . . ? C21 C20 H20 121.5 . . ? C19 C20 H20 121.5 . . ? C20 C21 C20 123.3(18) . 2_565 ? C20 C21 H21 118.3 . . ? C20 C21 H21 118.3 2_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Zn1 N2 C14 -179.9(7) . . . . ? Cl1 Zn1 N2 C14 61.0(7) . . . . ? Cl1 Zn1 N2 C14 -59.4(7) 2_565 . . . ? N2 Zn1 N2 C14 -179.9(7) 2_565 . . . ? N3 Zn1 N2 C18 -4.3(6) . . . . ? Cl1 Zn1 N2 C18 -123.4(6) . . . . ? Cl1 Zn1 N2 C18 116.1(6) 2_565 . . . ? N2 Zn1 N2 C18 -4.3(6) 2_565 . . . ? Cl1 Zn1 N3 C19 96.7(5) . . . . ? Cl1 Zn1 N3 C19 -83.3(5) 2_565 . . . ? N2 Zn1 N3 C19 2.8(5) . . . . ? N2 Zn1 N3 C19 -177.2(5) 2_565 . . . ? Cl1 Zn1 N3 C19 -83.3(5) . . . 2_565 ? Cl1 Zn1 N3 C19 96.7(5) 2_565 . . 2_565 ? N2 Zn1 N3 C19 -177.2(5) . . . 2_565 ? N2 Zn1 N3 C19 2.8(5) 2_565 . . 2_565 ? C13 N1 C1 C6 -103.8(10) . . . . ? C13 N1 C1 C2 87.2(10) . . . . ? C6 C1 C2 C3 7.2(12) . . . . ? N1 C1 C2 C3 175.7(8) . . . . ? C6 C1 C2 C7 -171.2(9) . . . . ? N1 C1 C2 C7 -2.7(12) . . . . ? C1 C2 C3 C4 -4.1(14) . . . . ? C7 C2 C3 C4 174.3(10) . . . . ? C2 C3 C4 C5 1.0(16) . . . . ? C3 C4 C5 C6 -0.5(16) . . . . ? C2 C1 C6 C5 -7.2(14) . . . . ? N1 C1 C6 C5 -175.5(9) . . . . ? C2 C1 C6 C10 174.3(8) . . . . ? N1 C1 C6 C10 6.0(12) . . . . ? C4 C5 C6 C1 3.5(15) . . . . ? C4 C5 C6 C10 -177.9(9) . . . . ? C1 C2 C7 C9 -149(2) . . . . ? C3 C2 C7 C9 33(2) . . . . ? C1 C2 C7 C8 87.6(13) . . . . ? C3 C2 C7 C8 -90.7(14) . . . . ? C1 C6 C10 C11 86.5(11) . . . . ? C5 C6 C10 C11 -92.0(11) . . . . ? C1 C6 C10 C12 -146.7(9) . . . . ? C5 C6 C10 C12 34.8(12) . . . . ? C1 N1 C13 C14 -176.3(8) . . . . ? C18 N2 C14 C15 0.2(13) . . . . ? Zn1 N2 C14 C15 175.4(6) . . . . ? C18 N2 C14 C13 179.0(8) . . . . ? Zn1 N2 C14 C13 -5.8(11) . . . . ? N1 C13 C14 N2 -171.9(8) . . . . ? N1 C13 C14 C15 7.0(13) . . . . ? N2 C14 C15 C16 -2.9(14) . . . . ? C13 C14 C15 C16 178.3(9) . . . . ? C14 C15 C16 C17 4.5(15) . . . . ? C15 C16 C17 C18 -3.6(16) . . . . ? C14 N2 C18 C17 0.8(13) . . . . ? Zn1 N2 C18 C17 -175.2(7) . . . . ? C14 N2 C18 C19 -178.7(8) . . . . ? Zn1 N2 C18 C19 5.3(10) . . . . ? C16 C17 C18 N2 1.0(15) . . . . ? C16 C17 C18 C19 -179.5(10) . . . . ? C19 N3 C19 C20 0.8(6) 2_565 . . . ? Zn1 N3 C19 C20 -179.2(6) . . . . ? C19 N3 C19 C18 179.1(9) 2_565 . . . ? Zn1 N3 C19 C18 -0.9(9) . . . . ? N2 C18 C19 N3 -3.3(12) . . . . ? C17 C18 C19 N3 177.2(8) . . . . ? N2 C18 C19 C20 174.9(8) . . . . ? C17 C18 C19 C20 -4.5(14) . . . . ? N3 C19 C20 C21 -1.6(12) . . . . ? C18 C19 C20 C21 -179.8(8) . . . . ? C19 C20 C21 C20 0.8(6) . . . 2_565 ? _diffrn_measured_fraction_theta_max 0.525 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.525 _refine_diff_density_max 0.946 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.105 # Attachment '05002.cif' data_05002 _database_code_depnum_ccdc_archive 'CCDC 289328' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C43 H49 Br2 N5 Ni) 2(C2 H3 N) 2(C H Cl3)' _chemical_formula_sum 'C49 H57 Br2 Cl6 N7 Ni' _chemical_formula_weight 1175.25 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.257(2) _cell_length_b 12.916(2) _cell_length_c 19.574(4) _cell_angle_alpha 84.660(3) _cell_angle_beta 84.591(3) _cell_angle_gamma 67.688(3) _cell_volume 2615.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 910 _cell_measurement_theta_min 2.784 _cell_measurement_theta_max 26.265 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 2.246 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 9740 reflections(SADABS);Rint 0.0837 before correction and 0.0244 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20399 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10135 _reflns_number_gt 7042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 ; Disordered MeCN was omitted using the SQUEEZE option of PLATON. The solvent accessible voids are 290.6 \%A3 with an estimated 90e/cell to be added.Four solvent MeCN molecules/unit cell accounting for 88e were included in the formula, FWt, (000) and density calculations. PLATON Reference: Spek, A.L. (1990), Acta Cryst. A46, C-34. 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^)+(0.0464P)^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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10135 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _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 Ni1 Ni 0.76757(4) 0.28773(3) 0.374064(19) 0.02187(10) Uani 1 1 d . . . Br1 Br 0.98498(3) 0.28899(3) 0.384943(16) 0.02861(9) Uani 1 1 d . . . Br2 Br 0.54527(3) 0.30852(3) 0.354140(16) 0.02893(9) Uani 1 1 d . . . N1 N 0.8507(2) 0.1694(2) 0.27056(13) 0.0269(6) Uani 1 1 d . . . N2 N 0.8219(2) 0.1223(2) 0.40611(13) 0.0259(6) Uani 1 1 d . . . N3 N 0.7280(2) 0.3003(2) 0.47449(12) 0.0225(6) Uani 1 1 d . . . N4 N 0.6895(2) 0.47922(19) 0.38624(12) 0.0204(5) Uani 1 1 d . . . N5 N 0.6181(2) 0.6424(2) 0.22943(13) 0.0284(6) Uani 1 1 d . . . C1 C 1.1868(5) 0.0921(5) 0.1896(4) 0.156(4) Uani 1 1 d . . . H1A H 1.1524 0.0324 0.1960 0.234 Uiso 1 1 calc R . . H1B H 1.2591 0.0738 0.2187 0.234 Uiso 1 1 calc R . . H1C H 1.2164 0.0990 0.1413 0.234 Uiso 1 1 calc R . . C2 C 1.0816(4) 0.2029(3) 0.2094(2) 0.0510(11) Uani 1 1 d . . . H2 H 1.0560 0.1934 0.2592 0.061 Uiso 1 1 calc R . . C3 C 1.1303(4) 0.2983(5) 0.2018(2) 0.0813(16) Uani 1 1 d . . . H3A H 1.1680 0.3030 0.1550 0.122 Uiso 1 1 calc R . . H3B H 1.1958 0.2845 0.2348 0.122 Uiso 1 1 calc R . . H3C H 1.0585 0.3690 0.2108 0.122 Uiso 1 1 calc R . . C4 C 0.9632(3) 0.2267(3) 0.16975(17) 0.0352(8) Uani 1 1 d . . . C5 C 0.9604(4) 0.2720(3) 0.10281(18) 0.0424(9) Uani 1 1 d . . . H5 H 1.0322 0.2880 0.0827 0.051 Uiso 1 1 calc R . . C6 C 0.8559(4) 0.2944(3) 0.06471(19) 0.0469(10) Uani 1 1 d . . . H6 H 0.8544 0.3279 0.0193 0.056 Uiso 1 1 calc R . . C7 C 0.7539(4) 0.2678(3) 0.09273(18) 0.0399(9) Uani 1 1 d . . . H7 H 0.6826 0.2822 0.0659 0.048 Uiso 1 1 calc R . . C8 C 0.7520(3) 0.2209(3) 0.15883(17) 0.0323(8) Uani 1 1 d . . . C9 C 0.8575(3) 0.2024(3) 0.19785(16) 0.0290(8) Uani 1 1 d . . . C10 C 0.6371(4) 0.1908(3) 0.18535(18) 0.0442(10) Uani 1 1 d . . . H10 H 0.6462 0.1670 0.2353 0.053 Uiso 1 1 calc R . . C11 C 0.5102(4) 0.2888(4) 0.1785(2) 0.0715(14) Uani 1 1 d . . . H11A H 0.5073 0.3485 0.2068 0.107 Uiso 1 1 calc R . . H11B H 0.4393 0.2641 0.1939 0.107 Uiso 1 1 calc R . . H11C H 0.5017 0.3172 0.1303 0.107 Uiso 1 1 calc R . . C12 C 0.6387(6) 0.0909(4) 0.1479(2) 0.0945(19) Uani 1 1 d . . . H12A H 0.6365 0.1102 0.0983 0.142 Uiso 1 1 calc R . . H12B H 0.5633 0.0729 0.1642 0.142 Uiso 1 1 calc R . . H12C H 0.7172 0.0257 0.1573 0.142 Uiso 1 1 calc R . . C13 C 0.8848(4) 0.0664(3) 0.29015(18) 0.0418(9) Uani 1 1 d . . . C13A C 0.9344(6) -0.0295(3) 0.2439(2) 0.100(2) Uani 1 1 d . . . H13A H 0.9270 -0.0002 0.1958 0.150 Uiso 1 1 calc R . . H13B H 0.8837 -0.0769 0.2538 0.150 Uiso 1 1 calc R . . H13C H 1.0248 -0.0740 0.2519 0.150 Uiso 1 1 calc R . . C14 C 0.8750(4) 0.0359(3) 0.36522(17) 0.0381(9) Uani 1 1 d . . . C15 C 0.9155(4) -0.0731(3) 0.3929(2) 0.0534(11) Uani 1 1 d . . . H15 H 0.9535 -0.1338 0.3639 0.064 Uiso 1 1 calc R . . C16 C 0.9004(4) -0.0937(3) 0.46300(19) 0.0480(10) Uani 1 1 d . . . H16 H 0.9283 -0.1685 0.4825 0.058 Uiso 1 1 calc R . . C17 C 0.8451(3) -0.0059(3) 0.50430(18) 0.0382(9) Uani 1 1 d . . . H17 H 0.8340 -0.0186 0.5526 0.046 Uiso 1 1 calc R . . C18 C 0.8055(3) 0.1028(3) 0.47388(16) 0.0273(7) Uani 1 1 d . . . C19 C 0.7455(3) 0.2042(2) 0.51311(15) 0.0251(7) Uani 1 1 d . . . C20 C 0.7096(3) 0.2065(3) 0.58240(16) 0.0329(8) Uani 1 1 d . . . H20 H 0.7221 0.1388 0.6097 0.040 Uiso 1 1 calc R . . C21 C 0.6548(3) 0.3094(3) 0.61140(16) 0.0327(8) Uani 1 1 d . . . H21 H 0.6277 0.3128 0.6589 0.039 Uiso 1 1 calc R . . C22 C 0.6397(3) 0.4063(3) 0.57170(15) 0.0265(7) Uani 1 1 d . . . H22 H 0.6024 0.4771 0.5913 0.032 Uiso 1 1 calc R . . C23 C 0.6798(3) 0.3990(2) 0.50244(15) 0.0215(7) Uani 1 1 d . . . C24 C 0.6724(3) 0.4967(2) 0.45404(15) 0.0218(7) Uani 1 1 d . . . C25 C 0.6504(3) 0.6002(3) 0.47907(16) 0.0286(7) Uani 1 1 d . . . H25 H 0.6406 0.6093 0.5271 0.034 Uiso 1 1 calc R . . C26 C 0.6432(3) 0.6890(3) 0.43288(17) 0.0324(8) Uani 1 1 d . . . H26 H 0.6320 0.7596 0.4487 0.039 Uiso 1 1 calc R . . C27 C 0.6522(3) 0.6746(3) 0.36407(16) 0.0293(8) Uani 1 1 d . . . H27 H 0.6434 0.7360 0.3315 0.035 Uiso 1 1 calc R . . C28 C 0.6745(3) 0.5684(2) 0.34215(15) 0.0214(7) Uani 1 1 d . . . C29 C 0.6772(3) 0.5547(2) 0.26696(15) 0.0234(7) Uani 1 1 d . . . C29A C 0.7451(3) 0.4405(2) 0.24192(16) 0.0296(8) Uani 1 1 d . . . H29A H 0.6923 0.3955 0.2544 0.044 Uiso 1 1 calc R . . H29B H 0.8278 0.4048 0.2630 0.044 Uiso 1 1 calc R . . H29C H 0.7601 0.4459 0.1918 0.044 Uiso 1 1 calc R . . C30 C 0.6154(3) 0.6322(2) 0.15768(16) 0.0288(8) Uani 1 1 d . . . C31 C 0.7213(3) 0.6293(3) 0.11297(17) 0.0345(8) Uani 1 1 d . . . C32 C 0.7130(4) 0.6200(3) 0.04322(18) 0.0465(10) Uani 1 1 d . . . H32 H 0.7829 0.6189 0.0116 0.056 Uiso 1 1 calc R . . C33 C 0.6047(4) 0.6124(3) 0.01938(19) 0.0511(11) Uani 1 1 d . . . H33 H 0.6022 0.6033 -0.0280 0.061 Uiso 1 1 calc R . . C34 C 0.5007(4) 0.6180(3) 0.06393(19) 0.0470(10) Uani 1 1 d . . . H34 H 0.4264 0.6143 0.0467 0.056 Uiso 1 1 calc R . . C35 C 0.5022(3) 0.6290(3) 0.13370(17) 0.0350(8) Uani 1 1 d . . . C36 C 0.8376(3) 0.6400(3) 0.13890(18) 0.0379(9) Uani 1 1 d . . . H36 H 0.8558 0.5938 0.1834 0.045 Uiso 1 1 calc R . . C37 C 0.9589(4) 0.5964(4) 0.0915(2) 0.0659(13) Uani 1 1 d . . . H37A H 0.9752 0.5192 0.0812 0.099 Uiso 1 1 calc R . . H37B H 1.0321 0.5981 0.1141 0.099 Uiso 1 1 calc R . . H37C H 0.9474 0.6438 0.0486 0.099 Uiso 1 1 calc R . . C38 C 0.8073(5) 0.7615(3) 0.1548(2) 0.0650(13) Uani 1 1 d . . . H38A H 0.7827 0.8103 0.1129 0.098 Uiso 1 1 calc R . . H38B H 0.8836 0.7677 0.1715 0.098 Uiso 1 1 calc R . . H38C H 0.7362 0.7843 0.1901 0.098 Uiso 1 1 calc R . . C39 C 0.3870(3) 0.6412(3) 0.18252(19) 0.0419(9) Uani 1 1 d . . . H39 H 0.4187 0.5947 0.2256 0.050 Uiso 1 1 calc R . . C40 C 0.3202(4) 0.7636(3) 0.2014(2) 0.0577(12) Uani 1 1 d . . . H40A H 0.3821 0.7878 0.2205 0.087 Uiso 1 1 calc R . . H40B H 0.2488 0.7699 0.2357 0.087 Uiso 1 1 calc R . . H40C H 0.2870 0.8113 0.1602 0.087 Uiso 1 1 calc R . . C41 C 0.2895(4) 0.6009(4) 0.1554(2) 0.0625(12) Uani 1 1 d . . . H41A H 0.2496 0.6503 0.1160 0.094 Uiso 1 1 calc R . . H41B H 0.2229 0.6026 0.1919 0.094 Uiso 1 1 calc R . . H41C H 0.3337 0.5241 0.1412 0.094 Uiso 1 1 calc R . . C42 C 0.0466(3) 0.5414(3) 0.3647(2) 0.0424(9) Uani 1 1 d . . . H42 H -0.0013 0.4896 0.3714 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.03227(9) 0.60522(8) 0.44210(5) 0.0467(2) Uani 1 1 d . . . Cl2 Cl 0.20807(9) 0.46283(8) 0.34115(5) 0.0520(3) Uani 1 1 d . . . Cl3 Cl -0.02264(10) 0.64407(9) 0.29898(6) 0.0607(3) Uani 1 1 d . . . C43 C 0.4778(4) 0.0659(3) 0.3473(3) 0.0704(15) Uani 1 1 d . . . H43 H 0.5142 0.1202 0.3235 0.084 Uiso 1 1 calc R . . Cl4 Cl 0.49727(16) -0.03893(11) 0.29047(9) 0.1108(6) Uani 1 1 d . . . Cl5 Cl 0.5605(2) 0.00669(13) 0.41833(13) 0.1667(10) Uani 1 1 d . . . Cl6 Cl 0.31559(12) 0.13679(11) 0.36648(9) 0.1011(5) 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 Ni1 0.0239(2) 0.0212(2) 0.0188(2) 0.00137(16) -0.00347(16) -0.00654(17) Br1 0.02445(18) 0.03063(18) 0.02957(19) -0.00206(14) -0.00442(14) -0.00832(14) Br2 0.02551(18) 0.03181(18) 0.02920(19) -0.00630(14) -0.00211(14) -0.00935(14) N1 0.0296(15) 0.0239(14) 0.0230(15) -0.0041(12) -0.0048(12) -0.0041(12) N2 0.0312(15) 0.0186(13) 0.0241(15) 0.0000(11) -0.0079(12) -0.0039(11) N3 0.0234(14) 0.0229(14) 0.0188(14) 0.0004(11) -0.0020(11) -0.0062(11) N4 0.0215(14) 0.0214(13) 0.0166(14) -0.0004(11) -0.0017(10) -0.0062(11) N5 0.0324(16) 0.0277(15) 0.0220(15) 0.0009(12) -0.0070(12) -0.0072(12) C1 0.071(4) 0.157(6) 0.185(7) -0.116(6) -0.070(4) 0.058(4) C2 0.038(2) 0.065(3) 0.044(2) -0.022(2) -0.0026(18) -0.009(2) C3 0.063(3) 0.154(5) 0.052(3) -0.010(3) -0.002(2) -0.068(3) C4 0.037(2) 0.035(2) 0.029(2) -0.0130(16) 0.0046(16) -0.0069(16) C5 0.049(2) 0.054(2) 0.030(2) -0.0138(18) 0.0123(18) -0.026(2) C6 0.066(3) 0.048(2) 0.025(2) -0.0012(17) 0.0014(19) -0.021(2) C7 0.046(2) 0.042(2) 0.029(2) -0.0012(17) -0.0076(17) -0.0126(18) C8 0.037(2) 0.0290(18) 0.0284(19) -0.0073(15) -0.0010(15) -0.0080(15) C9 0.036(2) 0.0228(17) 0.0221(18) -0.0044(14) -0.0038(15) -0.0027(15) C10 0.056(3) 0.060(3) 0.026(2) -0.0035(18) -0.0014(18) -0.033(2) C11 0.040(3) 0.123(4) 0.038(3) 0.008(3) -0.014(2) -0.016(3) C12 0.142(5) 0.122(5) 0.070(4) -0.035(3) 0.027(3) -0.107(4) C13 0.062(3) 0.0243(19) 0.028(2) -0.0061(15) -0.0062(18) -0.0015(17) C13A 0.199(6) 0.027(2) 0.031(3) -0.0107(19) -0.004(3) 0.006(3) C14 0.054(2) 0.0243(18) 0.029(2) -0.0022(15) -0.0120(17) -0.0050(17) C15 0.085(3) 0.0232(19) 0.039(2) -0.0063(17) -0.015(2) -0.002(2) C16 0.072(3) 0.0208(18) 0.042(2) 0.0113(17) -0.022(2) -0.0067(18) C17 0.056(2) 0.0268(18) 0.028(2) 0.0069(15) -0.0117(17) -0.0108(17) C18 0.0299(18) 0.0262(17) 0.0249(19) 0.0048(14) -0.0088(14) -0.0093(15) C19 0.0280(18) 0.0254(17) 0.0214(18) 0.0026(13) -0.0048(14) -0.0097(14) C20 0.037(2) 0.0340(19) 0.0258(19) 0.0077(15) -0.0047(15) -0.0127(16) C21 0.036(2) 0.044(2) 0.0175(18) 0.0006(15) -0.0020(15) -0.0152(17) C22 0.0261(18) 0.0317(18) 0.0229(18) -0.0058(14) -0.0008(14) -0.0113(15) C23 0.0212(16) 0.0263(17) 0.0181(16) 0.0000(13) -0.0035(13) -0.0100(14) C24 0.0208(16) 0.0224(16) 0.0210(17) -0.0012(13) -0.0034(13) -0.0063(13) C25 0.0302(19) 0.0294(18) 0.0241(18) -0.0071(14) -0.0011(14) -0.0078(15) C26 0.044(2) 0.0221(17) 0.032(2) -0.0075(15) -0.0008(16) -0.0123(16) C27 0.040(2) 0.0211(17) 0.0248(18) -0.0004(14) -0.0025(15) -0.0099(15) C28 0.0187(16) 0.0225(16) 0.0211(17) -0.0009(13) -0.0017(13) -0.0055(13) C29 0.0241(17) 0.0251(17) 0.0221(17) -0.0001(13) -0.0032(13) -0.0104(14) C29A 0.038(2) 0.0244(17) 0.0234(18) -0.0002(14) -0.0006(15) -0.0084(15) C30 0.039(2) 0.0237(17) 0.0203(18) 0.0045(14) -0.0088(15) -0.0074(15) C31 0.043(2) 0.0288(18) 0.0275(19) 0.0055(15) -0.0057(16) -0.0099(16) C32 0.055(3) 0.057(3) 0.023(2) 0.0027(18) 0.0016(18) -0.019(2) C33 0.065(3) 0.063(3) 0.022(2) -0.0010(18) -0.013(2) -0.019(2) C34 0.050(3) 0.058(3) 0.032(2) 0.0021(19) -0.0179(19) -0.017(2) C35 0.037(2) 0.0331(19) 0.029(2) 0.0048(15) -0.0095(16) -0.0056(16) C36 0.048(2) 0.045(2) 0.027(2) 0.0059(16) -0.0054(17) -0.0256(18) C37 0.057(3) 0.109(4) 0.043(3) -0.002(3) 0.000(2) -0.046(3) C38 0.089(4) 0.046(3) 0.074(3) 0.009(2) -0.027(3) -0.038(2) C39 0.033(2) 0.051(2) 0.036(2) -0.0017(18) -0.0087(17) -0.0080(18) C40 0.048(3) 0.051(3) 0.051(3) 0.002(2) -0.007(2) 0.008(2) C41 0.042(3) 0.093(3) 0.056(3) -0.005(3) -0.012(2) -0.028(2) C42 0.037(2) 0.037(2) 0.060(3) -0.0033(19) -0.0083(18) -0.0204(17) Cl1 0.0442(6) 0.0444(5) 0.0481(6) -0.0023(5) -0.0029(4) -0.0129(4) Cl2 0.0392(6) 0.0490(6) 0.0660(7) -0.0187(5) -0.0103(5) -0.0093(5) Cl3 0.0536(7) 0.0649(7) 0.0561(7) 0.0037(5) -0.0205(5) -0.0118(5) C43 0.041(3) 0.037(2) 0.126(4) 0.024(3) -0.008(3) -0.013(2) Cl4 0.1236(13) 0.0521(8) 0.1189(13) 0.0106(8) 0.0099(10) 0.0018(8) Cl5 0.205(2) 0.0712(10) 0.251(2) 0.0677(13) -0.1557(19) -0.0672(12) Cl6 0.0585(8) 0.0676(8) 0.1738(16) -0.0139(9) 0.0376(9) -0.0287(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 1.982(2) . ? Ni1 N2 2.040(2) . ? Ni1 N4 2.316(2) . ? Ni1 Br2 2.4780(7) . ? Ni1 Br1 2.4827(7) . ? N1 C13 1.269(4) . ? N1 C9 1.451(4) . ? N2 C18 1.336(4) . ? N2 C14 1.347(4) . ? N3 C23 1.330(4) . ? N3 C19 1.348(3) . ? N4 C28 1.340(3) . ? N4 C24 1.350(4) . ? N5 C29 1.277(4) . ? N5 C30 1.427(4) . ? C1 C2 1.527(6) . ? C2 C3 1.518(6) . ? C2 C4 1.521(5) . ? C4 C5 1.382(5) . ? C4 C9 1.394(5) . ? C5 C6 1.375(5) . ? C6 C7 1.372(5) . ? C7 C8 1.379(5) . ? C8 C9 1.404(4) . ? C8 C10 1.520(5) . ? C10 C11 1.514(5) . ? C10 C12 1.537(5) . ? C13 C14 1.490(5) . ? C13 C13A 1.501(5) . ? C14 C15 1.379(4) . ? C15 C16 1.380(5) . ? C16 C17 1.366(5) . ? C17 C18 1.394(4) . ? C18 C19 1.476(4) . ? C19 C20 1.378(4) . ? C20 C21 1.386(4) . ? C21 C22 1.372(4) . ? C22 C23 1.388(4) . ? C23 C24 1.486(4) . ? C24 C25 1.391(4) . ? C25 C26 1.374(4) . ? C26 C27 1.366(4) . ? C27 C28 1.398(4) . ? C28 C29 1.495(4) . ? C29 C29A 1.486(4) . ? C30 C31 1.401(4) . ? C30 C35 1.415(5) . ? C31 C32 1.396(5) . ? C31 C36 1.506(5) . ? C32 C33 1.386(5) . ? C33 C34 1.375(5) . ? C34 C35 1.388(5) . ? C35 C39 1.503(5) . ? C36 C37 1.522(5) . ? C36 C38 1.530(5) . ? C39 C41 1.534(5) . ? C39 C40 1.535(5) . ? C42 Cl2 1.753(4) . ? C42 Cl1 1.758(4) . ? C42 Cl3 1.762(4) . ? C43 Cl5 1.700(5) . ? C43 Cl6 1.726(4) . ? C43 Cl4 1.768(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 N3 Ni1 N2 79.76(10) . . ? N3 Ni1 N4 76.51(9) . . ? N2 Ni1 N4 156.26(9) . . ? N3 Ni1 Br2 92.49(7) . . ? N2 Ni1 Br2 93.80(7) . . ? N4 Ni1 Br2 87.78(6) . . ? N3 Ni1 Br1 90.81(7) . . ? N2 Ni1 Br1 93.04(7) . . ? N4 Ni1 Br1 86.80(6) . . ? Br2 Ni1 Br1 172.838(19) . . ? C13 N1 C9 119.9(3) . . ? C18 N2 C14 120.0(3) . . ? C18 N2 Ni1 114.6(2) . . ? C14 N2 Ni1 125.3(2) . . ? C23 N3 C19 121.1(3) . . ? C23 N3 Ni1 121.9(2) . . ? C19 N3 Ni1 116.90(19) . . ? C28 N4 C24 117.4(2) . . ? C28 N4 Ni1 133.69(19) . . ? C24 N4 Ni1 108.32(18) . . ? C29 N5 C30 118.6(3) . . ? C3 C2 C4 113.2(4) . . ? C3 C2 C1 111.8(4) . . ? C4 C2 C1 110.2(3) . . ? C5 C4 C9 118.3(3) . . ? C5 C4 C2 119.2(3) . . ? C9 C4 C2 122.4(3) . . ? C6 C5 C4 121.4(3) . . ? C7 C6 C5 119.5(3) . . ? C6 C7 C8 121.8(3) . . ? C7 C8 C9 117.9(3) . . ? C7 C8 C10 118.5(3) . . ? C9 C8 C10 123.5(3) . . ? C4 C9 C8 121.0(3) . . ? C4 C9 N1 119.1(3) . . ? C8 C9 N1 119.5(3) . . ? C11 C10 C8 112.7(3) . . ? C11 C10 C12 110.7(4) . . ? C8 C10 C12 109.6(3) . . ? N1 C13 C14 118.3(3) . . ? N1 C13 C13A 125.6(3) . . ? C14 C13 C13A 116.1(3) . . ? N2 C14 C15 120.5(3) . . ? N2 C14 C13 115.9(3) . . ? C15 C14 C13 123.6(3) . . ? C14 C15 C16 119.7(3) . . ? C17 C16 C15 119.7(3) . . ? C16 C17 C18 118.5(3) . . ? N2 C18 C17 121.6(3) . . ? N2 C18 C19 114.9(3) . . ? C17 C18 C19 123.5(3) . . ? N3 C19 C20 120.6(3) . . ? N3 C19 C18 113.5(3) . . ? C20 C19 C18 126.0(3) . . ? C19 C20 C21 118.7(3) . . ? C22 C21 C20 120.2(3) . . ? C21 C22 C23 118.8(3) . . ? N3 C23 C22 120.7(3) . . ? N3 C23 C24 114.9(3) . . ? C22 C23 C24 124.5(3) . . ? N4 C24 C25 122.7(3) . . ? N4 C24 C23 117.1(2) . . ? C25 C24 C23 120.2(3) . . ? C26 C25 C24 118.7(3) . . ? C27 C26 C25 119.4(3) . . ? C26 C27 C28 119.2(3) . . ? N4 C28 C27 122.4(3) . . ? N4 C28 C29 118.7(2) . . ? C27 C28 C29 118.9(3) . . ? N5 C29 C29A 125.1(3) . . ? N5 C29 C28 116.9(3) . . ? C29A C29 C28 117.9(3) . . ? C31 C30 C35 122.0(3) . . ? C31 C30 N5 120.0(3) . . ? C35 C30 N5 118.0(3) . . ? C32 C31 C30 117.5(3) . . ? C32 C31 C36 121.3(3) . . ? C30 C31 C36 121.2(3) . . ? C33 C32 C31 121.1(4) . . ? C34 C33 C32 120.4(3) . . ? C33 C34 C35 121.2(4) . . ? C34 C35 C30 117.7(3) . . ? C34 C35 C39 121.9(3) . . ? C30 C35 C39 120.3(3) . . ? C31 C36 C37 114.3(3) . . ? C31 C36 C38 110.1(3) . . ? C37 C36 C38 111.0(3) . . ? C35 C39 C41 114.0(3) . . ? C35 C39 C40 110.0(3) . . ? C41 C39 C40 109.9(3) . . ? Cl2 C42 Cl1 111.08(19) . . ? Cl2 C42 Cl3 110.4(2) . . ? Cl1 C42 Cl3 109.98(19) . . ? Cl5 C43 Cl6 112.8(3) . . ? Cl5 C43 Cl4 109.7(2) . . ? Cl6 C43 Cl4 108.9(3) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.024 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.078 # Attachment '2156.cif' data_2156 _database_code_depnum_ccdc_archive 'CCDC 289329' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C43 H49 Cl4 Fe2 N5)(C2 H3 N)' _chemical_formula_sum 'C45 H52 Cl4 Fe2 N6' _chemical_formula_weight 930.43 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 17.050(6) _cell_length_b 18.307(7) _cell_length_c 15.606(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.109(6) _cell_angle_gamma 90.00 _cell_volume 4574(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2516 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.56 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max .33 _exptl_crystal_size_mid .23 _exptl_crystal_size_min .17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.32 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details ; absorption correction based on 5243 reflections (SADABS); Rint 0.99 before correction and 0.072 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31786 _diffrn_reflns_av_R_equivalents 0.1585 _diffrn_reflns_av_sigmaI/netI 0.1637 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8049 _reflns_number_gt 3984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0885P)^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 8049 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1592 _refine_ls_R_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.1984 _refine_ls_wR_factor_gt 0.1675 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 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 Fe1 Fe 0.41925(7) 0.31448(6) 0.85275(7) 0.0343(3) Uani 1 1 d . . . Fe2 Fe 0.11241(7) 0.36277(6) 0.86941(7) 0.0364(3) Uani 1 1 d . . . Cl1 Cl 0.44398(12) 0.19307(11) 0.84517(12) 0.0401(5) Uani 1 1 d . . . Cl2 Cl 0.32183(12) 0.38960(11) 0.75605(12) 0.0422(5) Uani 1 1 d . . . Cl3 Cl 0.19633(14) 0.43904(12) 0.97054(14) 0.0565(6) Uani 1 1 d . . . Cl4 Cl 0.02281(13) 0.29460(12) 0.91123(13) 0.0502(6) Uani 1 1 d . . . N1 N 0.5385(4) 0.3530(3) 0.8318(4) 0.0350(15) Uani 1 1 d . . . N2 N 0.4893(4) 0.3654(3) 0.9723(4) 0.0342(15) Uani 1 1 d . . . N3 N 0.3457(4) 0.2957(3) 0.9473(4) 0.0337(15) Uani 1 1 d . . . N4 N 0.1627(4) 0.2891(3) 0.7989(4) 0.0338(15) Uani 1 1 d . . . N5 N 0.0532(4) 0.3932(3) 0.7319(4) 0.0329(15) Uani 1 1 d . . . C1 C 0.5662(5) 0.3287(4) 0.7588(5) 0.0350(19) Uani 1 1 d . . . C2 C 0.5329(5) 0.3637(4) 0.6731(5) 0.042(2) Uani 1 1 d . . . C3 C 0.5544(5) 0.3342(4) 0.6014(5) 0.042(2) Uani 1 1 d . . . H3 H 0.5314 0.3548 0.5421 0.051 Uiso 1 1 calc R . . C4 C 0.6082(5) 0.2762(5) 0.6155(5) 0.051(2) Uani 1 1 d . . . H4 H 0.6233 0.2585 0.5660 0.061 Uiso 1 1 calc R . . C5 C 0.6411(5) 0.2427(4) 0.6997(6) 0.049(2) Uani 1 1 d . . . H5 H 0.6768 0.2016 0.7073 0.059 Uiso 1 1 calc R . . C6 C 0.6213(5) 0.2701(4) 0.7741(5) 0.0376(19) Uani 1 1 d . . . C7 C 0.5843(5) 0.3934(4) 0.8955(5) 0.0369(19) Uani 1 1 d . . . C8 C 0.6632(5) 0.4314(5) 0.8991(5) 0.056(2) Uani 1 1 d . . . H8A H 0.6757 0.4201 0.8438 0.083 Uiso 1 1 calc R . . H8B H 0.7093 0.4147 0.9528 0.083 Uiso 1 1 calc R . . H8C H 0.6562 0.4843 0.9032 0.083 Uiso 1 1 calc R . . C9 C 0.5562(5) 0.4064(4) 0.9764(5) 0.0338(18) Uani 1 1 d . . . C10 C 0.5976(5) 0.4496(4) 1.0502(5) 0.046(2) Uani 1 1 d . . . H10 H 0.6447 0.4780 1.0515 0.056 Uiso 1 1 calc R . . C11 C 0.5680(5) 0.4503(5) 1.1225(5) 0.047(2) Uani 1 1 d . . . H11 H 0.5939 0.4808 1.1737 0.056 Uiso 1 1 calc R . . C12 C 0.5009(5) 0.4067(5) 1.1208(5) 0.049(2) Uani 1 1 d . . . H12 H 0.4820 0.4060 1.1714 0.059 Uiso 1 1 calc R . . C13 C 0.4617(5) 0.3642(4) 1.0444(5) 0.039(2) Uani 1 1 d . . . C14 C 0.3895(5) 0.3162(4) 1.0339(5) 0.0363(19) Uani 1 1 d . . . C15 C 0.3689(5) 0.2914(4) 1.1066(5) 0.041(2) Uani 1 1 d . . . H15 H 0.4015 0.3052 1.1671 0.049 Uiso 1 1 calc R . . C16 C 0.3012(5) 0.2470(4) 1.0911(5) 0.046(2) Uani 1 1 d . . . H16 H 0.2874 0.2287 1.1411 0.055 Uiso 1 1 calc R . . C17 C 0.2526(5) 0.2285(4) 1.0029(5) 0.041(2) Uani 1 1 d . . . H17 H 0.2043 0.1988 0.9909 0.050 Uiso 1 1 calc R . . C18 C 0.2772(5) 0.2551(4) 0.9316(5) 0.0335(18) Uani 1 1 d . . . C19 C 0.2247(5) 0.2399(4) 0.8350(5) 0.0338(18) Uani 1 1 d . . . C20 C 0.2368(5) 0.1812(4) 0.7855(5) 0.0365(19) Uani 1 1 d . . . H20 H 0.2795 0.1464 0.8125 0.044 Uiso 1 1 calc R . . C21 C 0.1855(5) 0.1744(4) 0.6962(5) 0.0394(19) Uani 1 1 d . . . H21 H 0.1918 0.1339 0.6612 0.047 Uiso 1 1 calc R . . C22 C 0.1246(5) 0.2264(4) 0.6567(5) 0.0378(19) Uani 1 1 d . . . H22 H 0.0899 0.2223 0.5945 0.045 Uiso 1 1 calc R . . C23 C 0.1152(4) 0.2841(4) 0.7091(5) 0.0296(17) Uani 1 1 d . . . C24 C 0.0573(4) 0.3465(4) 0.6736(5) 0.0315(17) Uani 1 1 d . . . C25 C 0.0134(5) 0.3518(4) 0.5723(5) 0.050(2) Uani 1 1 d . . . H25A H -0.0168 0.3983 0.5577 0.075 Uiso 1 1 calc R . . H25B H -0.0262 0.3113 0.5518 0.075 Uiso 1 1 calc R . . H25C H 0.0545 0.3494 0.5414 0.075 Uiso 1 1 calc R . . C26 C 0.0083(5) 0.4618(4) 0.7040(4) 0.0345(19) Uani 1 1 d . . . C27 C -0.0761(5) 0.4677(4) 0.6948(5) 0.0332(18) Uani 1 1 d . . . C28 C -0.1138(5) 0.5365(4) 0.6716(5) 0.041(2) Uani 1 1 d . . . H28 H -0.1707 0.5427 0.6655 0.049 Uiso 1 1 calc R . . C29 C -0.0691(5) 0.5948(5) 0.6576(5) 0.043(2) Uani 1 1 d . . . H29 H -0.0959 0.6408 0.6415 0.052 Uiso 1 1 calc R . . C30 C 0.0133(5) 0.5882(4) 0.6662(5) 0.046(2) Uani 1 1 d . . . H30 H 0.0429 0.6296 0.6567 0.055 Uiso 1 1 calc R . . C31 C 0.0540(5) 0.5210(5) 0.6890(5) 0.041(2) Uani 1 1 d . . . C32 C 0.4822(5) 0.4326(5) 0.6596(5) 0.046(2) Uani 1 1 d . . . H32 H 0.4622 0.4379 0.7124 0.056 Uiso 1 1 calc R . . C33 C 0.4064(5) 0.4321(5) 0.5728(6) 0.063(3) Uani 1 1 d . . . H33A H 0.4245 0.4265 0.5200 0.095 Uiso 1 1 calc R . . H33B H 0.3759 0.4782 0.5676 0.095 Uiso 1 1 calc R . . H33C H 0.3698 0.3913 0.5747 0.095 Uiso 1 1 calc R . . C34 C 0.5373(6) 0.4979(5) 0.6596(7) 0.072(3) Uani 1 1 d . . . H34A H 0.5858 0.4981 0.7161 0.108 Uiso 1 1 calc R . . H34B H 0.5053 0.5430 0.6556 0.108 Uiso 1 1 calc R . . H34C H 0.5562 0.4947 0.6071 0.108 Uiso 1 1 calc R . . C35 C 0.6626(5) 0.2339(4) 0.8674(5) 0.047(2) Uani 1 1 d . . . H35 H 0.6352 0.2537 0.9098 0.057 Uiso 1 1 calc R . . C36 C 0.6509(5) 0.1518(4) 0.8634(6) 0.056(2) Uani 1 1 d . . . H36A H 0.5920 0.1402 0.8312 0.084 Uiso 1 1 calc R . . H36B H 0.6681 0.1321 0.9256 0.084 Uiso 1 1 calc R . . H36C H 0.6852 0.1300 0.8309 0.084 Uiso 1 1 calc R . . C37 C 0.7555(6) 0.2524(5) 0.9074(6) 0.068(3) Uani 1 1 d . . . H37A H 0.7849 0.2295 0.8704 0.102 Uiso 1 1 calc R . . H37B H 0.7784 0.2341 0.9701 0.102 Uiso 1 1 calc R . . H37C H 0.7627 0.3055 0.9073 0.102 Uiso 1 1 calc R . . C38 C -0.1251(5) 0.4031(5) 0.7106(6) 0.049(2) Uani 1 1 d . . . H38 H -0.0873 0.3597 0.7282 0.058 Uiso 1 1 calc R . . C39 C -0.1585(6) 0.4198(5) 0.7873(7) 0.085(4) Uani 1 1 d . . . H39A H -0.1118 0.4308 0.8433 0.128 Uiso 1 1 calc R . . H39B H -0.1891 0.3773 0.7976 0.128 Uiso 1 1 calc R . . H39C H -0.1961 0.4619 0.7704 0.128 Uiso 1 1 calc R . . C40 C -0.1977(6) 0.3856(6) 0.6214(7) 0.085(3) Uani 1 1 d . . . H40A H -0.2354 0.4277 0.6038 0.127 Uiso 1 1 calc R . . H40B H -0.2286 0.3430 0.6310 0.127 Uiso 1 1 calc R . . H40C H -0.1752 0.3749 0.5728 0.127 Uiso 1 1 calc R . . C41 C 0.1461(5) 0.5140(5) 0.6973(5) 0.046(2) Uani 1 1 d . . . H41 H 0.1655 0.4639 0.7203 0.055 Uiso 1 1 calc R . . C42 C 0.1999(5) 0.5693(5) 0.7660(5) 0.058(3) Uani 1 1 d . . . H42A H 0.2591 0.5585 0.7784 0.087 Uiso 1 1 calc R . . H42B H 0.1879 0.5661 0.8229 0.087 Uiso 1 1 calc R . . H42C H 0.1874 0.6187 0.7409 0.087 Uiso 1 1 calc R . . C43 C 0.1573(5) 0.5236(5) 0.6056(6) 0.061(3) Uani 1 1 d . . . H43A H 0.1180 0.4919 0.5604 0.092 Uiso 1 1 calc R . . H43B H 0.2146 0.5105 0.6112 0.092 Uiso 1 1 calc R . . H43C H 0.1466 0.5746 0.5861 0.092 Uiso 1 1 calc R . . N6 N 0.9079(8) 0.2103(7) 0.6284(9) 0.116(4) Uani 1 1 d . . . C44 C 0.9318(8) 0.1572(8) 0.6081(8) 0.082(4) Uani 1 1 d . . . C45 C 0.9611(7) 0.0898(6) 0.5856(7) 0.088(4) Uani 1 1 d . . . H45A H 1.0083 0.0725 0.6379 0.133 Uiso 1 1 calc R . . H45B H 0.9792 0.0967 0.5330 0.133 Uiso 1 1 calc R . . H45C H 0.9160 0.0536 0.5705 0.133 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 Fe1 0.0473(7) 0.0506(7) 0.0132(6) -0.0042(5) 0.0208(5) -0.0024(6) Fe2 0.0524(7) 0.0501(7) 0.0140(6) -0.0002(5) 0.0209(5) 0.0004(6) Cl1 0.0541(13) 0.0530(12) 0.0212(10) 0.0011(9) 0.0232(9) 0.0009(10) Cl2 0.0551(13) 0.0558(12) 0.0231(10) 0.0015(9) 0.0231(9) 0.0036(10) Cl3 0.0718(16) 0.0623(14) 0.0335(13) -0.0111(11) 0.0155(11) -0.0020(12) Cl4 0.0675(14) 0.0700(14) 0.0231(11) 0.0076(10) 0.0283(10) -0.0065(12) N1 0.052(4) 0.044(4) 0.018(3) -0.003(3) 0.024(3) 0.003(3) N2 0.041(4) 0.052(4) 0.016(3) 0.005(3) 0.017(3) 0.005(3) N3 0.044(4) 0.053(4) 0.015(3) 0.003(3) 0.025(3) 0.002(3) N4 0.046(4) 0.049(4) 0.017(3) 0.001(3) 0.025(3) 0.003(3) N5 0.044(4) 0.048(4) 0.014(3) 0.007(3) 0.020(3) 0.000(3) C1 0.045(5) 0.043(5) 0.031(5) -0.004(4) 0.032(4) -0.008(4) C2 0.066(6) 0.054(5) 0.016(4) -0.008(4) 0.027(4) -0.013(5) C3 0.056(5) 0.052(5) 0.024(4) 0.002(4) 0.021(4) -0.005(4) C4 0.075(6) 0.066(6) 0.035(5) -0.015(5) 0.048(5) -0.017(5) C5 0.074(6) 0.045(5) 0.044(5) -0.006(4) 0.042(5) -0.003(5) C6 0.054(5) 0.048(5) 0.022(4) -0.004(4) 0.027(4) -0.003(4) C7 0.052(5) 0.052(5) 0.017(4) -0.003(4) 0.025(4) -0.002(4) C8 0.051(6) 0.088(7) 0.035(5) -0.024(5) 0.025(4) -0.012(5) C9 0.037(5) 0.047(5) 0.018(4) -0.007(4) 0.012(4) 0.002(4) C10 0.058(6) 0.061(6) 0.022(5) -0.011(4) 0.017(4) 0.008(4) C11 0.052(6) 0.067(6) 0.022(4) -0.017(4) 0.014(4) 0.014(5) C12 0.051(6) 0.083(7) 0.019(4) -0.017(4) 0.019(4) 0.021(5) C13 0.050(5) 0.060(5) 0.016(4) -0.009(4) 0.021(4) 0.013(4) C14 0.049(5) 0.053(5) 0.011(4) 0.004(4) 0.016(3) 0.005(4) C15 0.054(5) 0.063(5) 0.012(4) 0.000(4) 0.020(4) 0.011(5) C16 0.055(6) 0.067(6) 0.028(5) 0.025(4) 0.031(4) 0.018(5) C17 0.056(5) 0.049(5) 0.029(5) 0.015(4) 0.028(4) 0.002(4) C18 0.048(5) 0.044(4) 0.017(4) 0.006(4) 0.023(4) 0.008(4) C19 0.039(5) 0.052(5) 0.020(4) 0.006(4) 0.022(4) -0.004(4) C20 0.048(5) 0.049(5) 0.022(4) -0.002(4) 0.025(4) 0.005(4) C21 0.050(5) 0.047(5) 0.029(5) 0.000(4) 0.023(4) 0.005(4) C22 0.047(5) 0.056(5) 0.017(4) -0.005(4) 0.019(4) -0.008(4) C23 0.035(4) 0.042(4) 0.022(4) -0.001(4) 0.023(4) -0.004(4) C24 0.039(5) 0.044(4) 0.015(4) 0.003(4) 0.014(3) -0.004(4) C25 0.064(6) 0.069(6) 0.015(4) -0.001(4) 0.012(4) 0.013(5) C26 0.047(5) 0.050(5) 0.010(4) 0.012(3) 0.015(3) 0.003(4) C27 0.039(5) 0.051(5) 0.018(4) -0.002(4) 0.021(4) -0.002(4) C28 0.047(5) 0.063(5) 0.025(4) -0.002(4) 0.027(4) 0.009(4) C29 0.056(6) 0.055(5) 0.027(5) 0.003(4) 0.024(4) 0.004(5) C30 0.055(6) 0.053(5) 0.034(5) 0.012(4) 0.020(4) 0.001(4) C31 0.047(5) 0.062(6) 0.019(4) 0.006(4) 0.017(4) 0.005(4) C32 0.060(6) 0.064(6) 0.026(5) 0.005(4) 0.028(4) 0.006(5) C33 0.069(6) 0.079(7) 0.042(6) 0.022(5) 0.018(5) -0.010(5) C34 0.097(8) 0.057(6) 0.073(7) -0.005(5) 0.043(6) -0.011(6) C35 0.070(6) 0.049(5) 0.034(5) 0.008(4) 0.033(5) 0.013(5) C36 0.063(6) 0.068(6) 0.045(6) 0.005(5) 0.029(5) 0.006(5) C37 0.077(7) 0.075(7) 0.045(6) 0.018(5) 0.012(5) -0.003(6) C38 0.055(6) 0.060(6) 0.045(6) 0.000(5) 0.035(5) -0.002(5) C39 0.121(9) 0.087(8) 0.093(8) 0.017(6) 0.095(8) 0.006(7) C40 0.074(7) 0.096(8) 0.085(9) 0.001(7) 0.029(7) -0.025(6) C41 0.047(5) 0.055(5) 0.040(5) 0.019(4) 0.021(4) 0.003(4) C42 0.053(6) 0.090(7) 0.038(5) 0.013(5) 0.025(5) -0.014(5) C43 0.055(6) 0.095(7) 0.044(6) -0.001(5) 0.030(5) -0.002(5) N6 0.116(9) 0.128(10) 0.108(10) 0.053(9) 0.042(7) 0.013(9) C44 0.085(10) 0.100(10) 0.054(8) 0.034(8) 0.018(7) -0.024(9) C45 0.116(10) 0.111(10) 0.044(7) -0.008(7) 0.036(7) -0.053(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.061(6) . ? Fe1 N3 2.267(5) . ? Fe1 Cl1 2.273(2) . ? Fe1 N1 2.278(6) . ? Fe1 Cl2 2.281(2) . ? Fe2 N4 2.102(6) . ? Fe2 N5 2.109(5) . ? Fe2 Cl3 2.221(2) . ? Fe2 Cl4 2.237(2) . ? N1 C7 1.269(9) . ? N1 C1 1.446(8) . ? N2 C9 1.349(9) . ? N2 C13 1.359(8) . ? N3 C18 1.333(9) . ? N3 C14 1.352(8) . ? N4 C19 1.354(9) . ? N4 C23 1.360(8) . ? N5 C24 1.268(8) . ? N5 C26 1.457(9) . ? C1 C6 1.392(10) . ? C1 C2 1.415(10) . ? C2 C3 1.400(10) . ? C2 C32 1.501(10) . ? C3 C4 1.371(10) . ? C4 C5 1.382(11) . ? C5 C6 1.407(9) . ? C6 C35 1.534(10) . ? C7 C8 1.498(10) . ? C7 C9 1.515(9) . ? C9 C10 1.375(10) . ? C10 C11 1.385(10) . ? C11 C12 1.388(11) . ? C12 C13 1.388(10) . ? C13 C14 1.477(10) . ? C14 C15 1.374(9) . ? C15 C16 1.364(10) . ? C16 C17 1.382(10) . ? C17 C18 1.405(9) . ? C18 C19 1.492(10) . ? C19 C20 1.379(10) . ? C20 C21 1.373(9) . ? C21 C22 1.387(10) . ? C22 C23 1.379(9) . ? C23 C24 1.486(9) . ? C24 C25 1.501(9) . ? C26 C27 1.399(9) . ? C26 C31 1.400(10) . ? C27 C28 1.404(10) . ? C27 C38 1.517(10) . ? C28 C29 1.373(10) . ? C29 C30 1.368(10) . ? C30 C31 1.397(10) . ? C31 C41 1.536(10) . ? C32 C33 1.517(10) . ? C32 C34 1.519(11) . ? C35 C36 1.514(10) . ? C35 C37 1.527(11) . ? C38 C39 1.523(10) . ? C38 C40 1.546(11) . ? C41 C43 1.518(10) . ? C41 C42 1.531(11) . ? N6 C44 1.139(15) . ? C44 C45 1.420(16) . ? 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 Fe1 N3 75.9(2) . . ? N2 Fe1 Cl1 115.44(17) . . ? N3 Fe1 Cl1 92.29(16) . . ? N2 Fe1 N1 73.9(2) . . ? N3 Fe1 N1 149.4(2) . . ? Cl1 Fe1 N1 95.98(16) . . ? N2 Fe1 Cl2 112.95(18) . . ? N3 Fe1 Cl2 94.71(16) . . ? Cl1 Fe1 Cl2 131.37(8) . . ? N1 Fe1 Cl2 101.62(16) . . ? N4 Fe2 N5 77.0(2) . . ? N4 Fe2 Cl3 119.75(18) . . ? N5 Fe2 Cl3 121.54(18) . . ? N4 Fe2 Cl4 103.73(17) . . ? N5 Fe2 Cl4 107.96(17) . . ? Cl3 Fe2 Cl4 118.76(9) . . ? C7 N1 C1 121.0(6) . . ? C7 N1 Fe1 114.0(4) . . ? C1 N1 Fe1 124.6(5) . . ? C9 N2 C13 119.9(6) . . ? C9 N2 Fe1 120.8(4) . . ? C13 N2 Fe1 118.9(5) . . ? C18 N3 C14 119.1(6) . . ? C18 N3 Fe1 127.5(4) . . ? C14 N3 Fe1 111.7(5) . . ? C19 N4 C23 119.2(6) . . ? C19 N4 Fe2 127.6(5) . . ? C23 N4 Fe2 112.1(5) . . ? C24 N5 C26 121.3(6) . . ? C24 N5 Fe2 115.3(5) . . ? C26 N5 Fe2 123.4(4) . . ? C6 C1 C2 122.7(7) . . ? C6 C1 N1 119.1(6) . . ? C2 C1 N1 118.2(7) . . ? C3 C2 C1 116.8(7) . . ? C3 C2 C32 120.5(7) . . ? C1 C2 C32 122.5(6) . . ? C4 C3 C2 121.1(7) . . ? C3 C4 C5 121.7(7) . . ? C4 C5 C6 119.5(8) . . ? C1 C6 C5 118.1(7) . . ? C1 C6 C35 123.9(6) . . ? C5 C6 C35 117.9(7) . . ? N1 C7 C8 127.1(6) . . ? N1 C7 C9 117.3(7) . . ? C8 C7 C9 115.6(6) . . ? N2 C9 C10 122.8(7) . . ? N2 C9 C7 112.2(6) . . ? C10 C9 C7 124.8(7) . . ? C9 C10 C11 117.5(8) . . ? C10 C11 C12 120.6(7) . . ? C11 C12 C13 119.2(7) . . ? N2 C13 C12 120.0(7) . . ? N2 C13 C14 115.5(6) . . ? C12 C13 C14 124.4(7) . . ? N3 C14 C15 121.6(7) . . ? N3 C14 C13 115.3(6) . . ? C15 C14 C13 123.0(7) . . ? C16 C15 C14 119.4(7) . . ? C15 C16 C17 120.2(7) . . ? C16 C17 C18 117.6(7) . . ? N3 C18 C17 121.9(7) . . ? N3 C18 C19 118.3(6) . . ? C17 C18 C19 119.8(7) . . ? N4 C19 C20 122.0(7) . . ? N4 C19 C18 114.1(6) . . ? C20 C19 C18 123.9(7) . . ? C21 C20 C19 118.2(7) . . ? C20 C21 C22 120.5(7) . . ? C23 C22 C21 119.0(7) . . ? N4 C23 C22 120.8(7) . . ? N4 C23 C24 114.7(6) . . ? C22 C23 C24 124.4(7) . . ? N5 C24 C23 116.4(6) . . ? N5 C24 C25 125.5(7) . . ? C23 C24 C25 118.0(6) . . ? C27 C26 C31 122.3(7) . . ? C27 C26 N5 120.8(7) . . ? C31 C26 N5 116.8(6) . . ? C26 C27 C28 117.3(7) . . ? C26 C27 C38 121.9(7) . . ? C28 C27 C38 120.8(7) . . ? C29 C28 C27 120.6(7) . . ? C30 C29 C28 121.5(8) . . ? C29 C30 C31 120.4(8) . . ? C30 C31 C26 117.9(7) . . ? C30 C31 C41 119.9(7) . . ? C26 C31 C41 122.2(7) . . ? C2 C32 C33 113.1(7) . . ? C2 C32 C34 109.6(7) . . ? C33 C32 C34 110.0(7) . . ? C36 C35 C37 109.9(7) . . ? C36 C35 C6 112.3(7) . . ? C37 C35 C6 111.4(7) . . ? C27 C38 C39 110.4(7) . . ? C27 C38 C40 109.3(7) . . ? C39 C38 C40 110.5(8) . . ? C43 C41 C42 110.2(7) . . ? C43 C41 C31 111.6(6) . . ? C42 C41 C31 110.7(7) . . ? N6 C44 C45 177.9(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.781 _refine_diff_density_min -1.242 _refine_diff_density_rms 0.106 # Attachment '05028bcn.cif' data_05028bcn _database_code_depnum_ccdc_archive 'CCDC 289330' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C43 H52 Br4 N5 Ni2 O) (C H Cl3) (H2 O)' _chemical_formula_sum 'C44 H55 Br4 Cl3 N5 Ni2 O2' _chemical_formula_weight 1229.34 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 21.921(6) _cell_length_b 16.246(5) _cell_length_c 28.685(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10216(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 984 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 21.77 _exptl_crystal_description lozenge _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4936 _exptl_absorpt_coefficient_mu 4.062 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.532 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details ; absorption correction based on 5577 reflections (SADABS); Rint 0.155 before correction and 0.058 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59878 _diffrn_reflns_av_R_equivalents 0.2637 _diffrn_reflns_av_sigmaI/netI 0.1979 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 23.32 _reflns_number_total 7368 _reflns_number_gt 3920 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1385P)^2^+187.8032P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7368 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2179 _refine_ls_R_factor_gt 0.1331 _refine_ls_wR_factor_ref 0.3433 _refine_ls_wR_factor_gt 0.3076 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.004 _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 Ni1 Ni 0.10815(12) 0.30843(19) 0.38505(9) 0.0266(8) Uani 1 1 d . . . Ni2 Ni -0.09132(12) 0.47432(18) 0.42155(9) 0.0240(7) Uani 1 1 d . . . Br1 Br 0.10834(11) 0.18277(16) 0.33967(8) 0.0376(7) Uani 1 1 d . . . Br2 Br 0.07648(10) 0.42214(15) 0.33781(8) 0.0323(6) Uani 1 1 d . . . Br3 Br -0.09689(11) 0.56251(18) 0.49145(8) 0.0421(8) Uani 1 1 d . . . Br4 Br -0.18670(12) 0.40258(17) 0.43547(9) 0.0444(8) Uani 1 1 d . . . N1 N 0.2040(8) 0.3383(10) 0.3818(5) 0.018(4) Uiso 1 1 d . . . N2 N 0.1385(8) 0.2603(11) 0.4421(6) 0.026(5) Uiso 1 1 d . . . N3 N 0.0240(8) 0.2727(10) 0.4211(5) 0.019(4) Uiso 1 1 d . . . N4 N -0.0747(8) 0.3967(10) 0.3653(6) 0.023(4) Uiso 1 1 d . . . O1 O 0.0010(8) 0.4911(10) 0.4233(5) 0.046(5) Uiso 1 1 d . . . H1 H 0.0184 0.4471 0.4311 0.070 Uiso 1 1 d R . . H1A H 0.0097 0.5308 0.4442 0.070 Uiso 1 1 d R . . C1 C 0.2605(11) 0.3574(15) 0.3078(8) 0.034(6) Uiso 1 1 d . . . C2 C 0.2869(11) 0.4178(15) 0.2778(8) 0.040(7) Uiso 1 1 d . . . H2 H 0.3053 0.3989 0.2498 0.048 Uiso 1 1 calc R . . C3 C 0.2878(11) 0.4993(16) 0.2860(8) 0.041(7) Uiso 1 1 d . . . H3 H 0.3051 0.5365 0.2641 0.049 Uiso 1 1 calc R . . C4 C 0.2625(10) 0.5276(14) 0.3279(7) 0.028(6) Uiso 1 1 d . . . H4 H 0.2657 0.5842 0.3359 0.033 Uiso 1 1 calc R . . C5 C 0.2331(11) 0.4742(14) 0.3574(8) 0.031(6) Uiso 1 1 d . . . C6 C 0.2332(11) 0.3931(14) 0.3488(8) 0.031(6) Uiso 1 1 d . . . C7 C 0.2624(11) 0.2686(14) 0.2990(8) 0.034(6) Uiso 1 1 d . . . H7 H 0.2410 0.2396 0.3251 0.040 Uiso 1 1 calc R . . C8 C 0.2318(13) 0.2443(17) 0.2527(9) 0.059(8) Uiso 1 1 d . . . H8A H 0.1928 0.2733 0.2497 0.089 Uiso 1 1 calc R . . H8B H 0.2246 0.1848 0.2522 0.089 Uiso 1 1 calc R . . H8C H 0.2585 0.2594 0.2267 0.089 Uiso 1 1 calc R . . C9 C 0.3281(13) 0.2368(17) 0.2962(9) 0.057(8) Uiso 1 1 d . . . H9A H 0.3488 0.2623 0.2696 0.086 Uiso 1 1 calc R . . H9B H 0.3278 0.1769 0.2923 0.086 Uiso 1 1 calc R . . H9C H 0.3498 0.2509 0.3250 0.086 Uiso 1 1 calc R . . C10 C 0.2063(11) 0.5082(15) 0.4042(8) 0.039(6) Uiso 1 1 d . . . H10 H 0.1773 0.4667 0.4174 0.047 Uiso 1 1 calc R . . C11 C 0.2574(12) 0.5230(17) 0.4395(9) 0.052(7) Uiso 1 1 d . . . H11A H 0.2861 0.5636 0.4270 0.079 Uiso 1 1 calc R . . H11B H 0.2789 0.4711 0.4455 0.079 Uiso 1 1 calc R . . H11C H 0.2400 0.5436 0.4687 0.079 Uiso 1 1 calc R . . C12 C 0.1720(12) 0.5890(16) 0.3964(9) 0.048(7) Uiso 1 1 d . . . H12A H 0.1635 0.6150 0.4266 0.073 Uiso 1 1 calc R . . H12B H 0.1334 0.5777 0.3804 0.073 Uiso 1 1 calc R . . H12C H 0.1969 0.6260 0.3774 0.073 Uiso 1 1 calc R . . C13 C 0.2344(10) 0.3057(14) 0.4141(7) 0.028(6) Uiso 1 1 d . . . C14 C 0.3036(11) 0.3163(15) 0.4198(8) 0.039(6) Uiso 1 1 d . . . H14A H 0.3211 0.3366 0.3906 0.059 Uiso 1 1 calc R . . H14B H 0.3220 0.2632 0.4278 0.059 Uiso 1 1 calc R . . H14C H 0.3118 0.3560 0.4448 0.059 Uiso 1 1 calc R . . C15 C 0.1993(10) 0.2596(13) 0.4496(7) 0.028(6) Uiso 1 1 d . . . C16 C 0.2239(11) 0.2206(14) 0.4872(7) 0.033(6) Uiso 1 1 d . . . H16 H 0.2669 0.2203 0.4915 0.040 Uiso 1 1 calc R . . C17 C 0.1849(11) 0.1797(14) 0.5204(8) 0.035(6) Uiso 1 1 d . . . H17 H 0.2008 0.1505 0.5464 0.042 Uiso 1 1 calc R . . C18 C 0.1242(11) 0.1856(14) 0.5122(8) 0.037(6) Uiso 1 1 d . . . H18 H 0.0970 0.1619 0.5343 0.044 Uiso 1 1 calc R . . C19 C 0.0993(10) 0.2241(14) 0.4735(7) 0.028(6) Uiso 1 1 d . . . C20 C 0.0364(11) 0.2332(14) 0.4610(8) 0.033(6) Uiso 1 1 d . . . C21 C -0.0077(11) 0.1985(14) 0.4886(8) 0.036(6) Uiso 1 1 d . . . H21 H 0.0028 0.1702 0.5164 0.043 Uiso 1 1 calc R . . C22 C -0.0681(12) 0.2056(16) 0.4748(9) 0.046(7) Uiso 1 1 d . . . H22 H -0.0993 0.1790 0.4921 0.055 Uiso 1 1 calc R . . C23 C -0.0826(13) 0.2510(16) 0.4364(9) 0.052(8) Uiso 1 1 d . . . H23 H -0.1238 0.2635 0.4291 0.063 Uiso 1 1 calc R . . C24 C -0.0349(10) 0.2785(14) 0.4082(7) 0.027(6) Uiso 1 1 d . . . C25 C -0.0532(9) 0.3221(13) 0.3638(7) 0.018(5) Uiso 1 1 d . . . C26 C -0.0475(10) 0.2756(14) 0.3236(7) 0.027(6) Uiso 1 1 d . . . H26 H -0.0287 0.2230 0.3252 0.032 Uiso 1 1 calc R . . C27 C -0.0680(10) 0.3036(13) 0.2822(7) 0.023(5) Uiso 1 1 d . . . H27 H -0.0672 0.2713 0.2546 0.027 Uiso 1 1 calc R . . C28 C -0.0912(9) 0.3871(13) 0.2834(7) 0.024(5) Uiso 1 1 d . . . H28 H -0.1032 0.4147 0.2557 0.029 Uiso 1 1 calc R . . C29 C -0.0951(11) 0.4226(14) 0.3235(8) 0.034(6) Uiso 1 1 d . . . C30 C -0.1165(10) 0.5146(13) 0.3267(7) 0.024(5) Uiso 1 1 d . . . C31 C -0.1383(11) 0.5496(14) 0.2827(8) 0.036(6) Uiso 1 1 d . . . H31A H -0.1816 0.5367 0.2786 0.054 Uiso 1 1 d R . . H31B H -0.1149 0.5264 0.2567 0.054 Uiso 1 1 d R . . H31C H -0.1329 0.6094 0.2834 0.054 Uiso 1 1 d R . . N5 N -0.1178(8) 0.5472(10) 0.3674(6) 0.023(4) Uiso 1 1 d . . . C33 C -0.1349(10) 0.6291(13) 0.3700(7) 0.026(6) Uiso 1 1 d . . . C34 C -0.1965(10) 0.6572(13) 0.3754(7) 0.024(5) Uiso 1 1 d . . . C35 C -0.2077(12) 0.7404(15) 0.3739(8) 0.043(7) Uiso 1 1 d . . . H35 H -0.2485 0.7584 0.3783 0.051 Uiso 1 1 calc R . . C36 C -0.1644(11) 0.7980(16) 0.3667(8) 0.039(7) Uiso 1 1 d . . . H36 H -0.1760 0.8542 0.3644 0.046 Uiso 1 1 calc R . . C37 C -0.1036(11) 0.7769(14) 0.3626(7) 0.031(6) Uiso 1 1 d . . . H37 H -0.0731 0.8178 0.3582 0.038 Uiso 1 1 calc R . . C38 C -0.0881(10) 0.6932(14) 0.3650(8) 0.030(6) Uiso 1 1 d . . . C39 C -0.2448(11) 0.5946(15) 0.3873(7) 0.032(6) Uiso 1 1 d . . . H39 H -0.2247 0.5394 0.3862 0.039 Uiso 1 1 calc R . . C40 C -0.2970(14) 0.5933(19) 0.3503(10) 0.069(9) Uiso 1 1 d . . . H40A H -0.3211 0.5429 0.3540 0.104 Uiso 1 1 calc R . . H40B H -0.2794 0.5948 0.3189 0.104 Uiso 1 1 calc R . . H40C H -0.3234 0.6413 0.3547 0.104 Uiso 1 1 calc R . . C41 C -0.2688(13) 0.6053(17) 0.4349(9) 0.055(8) Uiso 1 1 d . . . H41A H -0.2348 0.6070 0.4571 0.083 Uiso 1 1 calc R . . H41B H -0.2957 0.5590 0.4426 0.083 Uiso 1 1 calc R . . H41C H -0.2919 0.6569 0.4368 0.083 Uiso 1 1 calc R . . C42 C -0.0230(11) 0.6666(16) 0.3605(8) 0.039(7) Uiso 1 1 d . . . H42 H -0.0206 0.6056 0.3645 0.047 Uiso 1 1 calc R . . C43 C 0.0156(14) 0.7087(18) 0.3993(10) 0.066(9) Uiso 1 1 d . . . H43A H 0.0253 0.7652 0.3899 0.100 Uiso 1 1 calc R . . H43B H 0.0535 0.6778 0.4040 0.100 Uiso 1 1 calc R . . H43C H -0.0078 0.7096 0.4284 0.100 Uiso 1 1 calc R . . C44 C 0.0036(15) 0.6897(19) 0.3123(10) 0.076(10) Uiso 1 1 d . . . H44A H -0.0233 0.7300 0.2974 0.114 Uiso 1 1 d R . . H44B H 0.0065 0.6405 0.2926 0.114 Uiso 1 1 d R . . H44C H 0.0442 0.7136 0.3164 0.114 Uiso 1 1 d R . . C45 C 0.0471(13) 0.0150(17) 0.4026(9) 0.052(8) Uiso 1 1 d . . . H45 H 0.0621 0.0699 0.3918 0.063 Uiso 1 1 calc R . . Cl1 Cl 0.0717(4) -0.0629(6) 0.3648(3) 0.081(3) Uiso 1 1 d . . . Cl2 Cl 0.0712(4) -0.0046(5) 0.4590(3) 0.079(3) Uiso 1 1 d . . . Cl3 Cl -0.0348(5) 0.0121(7) 0.4024(4) 0.110(4) Uiso 1 1 d . . . O2 O 0.0405(14) 0.9215(19) 0.2414(10) 0.039(9) Uiso 0.50 1 d P . . O3 O 0.0428(17) 0.055(2) 0.2343(12) 0.055(10) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0082(15) 0.0459(19) 0.0257(16) 0.0004(15) -0.0006(12) 0.0047(14) Ni2 0.0136(16) 0.0338(17) 0.0245(15) 0.0015(14) 0.0030(12) -0.0003(14) Br1 0.0249(14) 0.0472(16) 0.0405(15) -0.0072(13) 0.0015(12) 0.0073(13) Br2 0.0175(12) 0.0480(16) 0.0313(13) 0.0064(12) 0.0007(10) -0.0031(12) Br3 0.0242(14) 0.0704(19) 0.0318(14) -0.0105(13) -0.0037(11) 0.0095(14) Br4 0.0272(15) 0.0464(16) 0.0597(18) 0.0048(14) 0.0178(13) -0.0070(13) _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 Ni1 N2 1.933(17) . ? Ni1 N1 2.157(17) . ? Ni1 N3 2.192(17) . ? Ni1 Br2 2.394(4) . ? Ni1 Br1 2.421(4) . ? Ni2 N5 2.036(17) . ? Ni2 O1 2.042(17) . ? Ni2 N4 2.079(17) . ? Ni2 Br4 2.427(4) . ? Ni2 Br3 2.468(4) . ? N1 C13 1.26(3) . ? N1 C6 1.45(3) . ? N2 C15 1.35(3) . ? N2 C19 1.38(3) . ? N3 C20 1.34(3) . ? N3 C24 1.35(3) . ? N4 C25 1.30(2) . ? N4 C29 1.35(3) . ? C1 C2 1.43(3) . ? C1 C6 1.44(3) . ? C1 C7 1.47(3) . ? C2 C3 1.34(3) . ? C3 C4 1.40(3) . ? C4 C5 1.37(3) . ? C5 C6 1.34(3) . ? C5 C10 1.57(3) . ? C7 C9 1.53(3) . ? C7 C8 1.54(3) . ? C10 C12 1.53(3) . ? C10 C11 1.53(3) . ? C13 C15 1.48(3) . ? C13 C14 1.54(3) . ? C15 C16 1.36(3) . ? C16 C17 1.44(3) . ? C17 C18 1.36(3) . ? C18 C19 1.39(3) . ? C19 C20 1.43(3) . ? C20 C21 1.37(3) . ? C21 C22 1.39(3) . ? C22 C23 1.36(3) . ? C23 C24 1.40(3) . ? C24 C25 1.51(3) . ? C25 C26 1.39(3) . ? C26 C27 1.35(3) . ? C27 C28 1.45(3) . ? C28 C29 1.29(3) . ? C29 C30 1.57(3) . ? C30 N5 1.28(2) . ? C30 C31 1.47(3) . ? N5 C33 1.39(3) . ? C33 C34 1.43(3) . ? C33 C38 1.47(3) . ? C34 C35 1.37(3) . ? C34 C39 1.51(3) . ? C35 C36 1.35(3) . ? C36 C37 1.38(3) . ? C37 C38 1.40(3) . ? C38 C42 1.50(3) . ? C39 C41 1.48(3) . ? C39 C40 1.56(3) . ? C42 C44 1.55(4) . ? C42 C43 1.56(4) . ? C45 Cl2 1.73(3) . ? C45 Cl1 1.75(3) . ? C45 Cl3 1.80(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 78.0(7) . . ? N2 Ni1 N3 77.5(7) . . ? N1 Ni1 N3 154.0(6) . . ? N2 Ni1 Br2 153.1(5) . . ? N1 Ni1 Br2 94.8(4) . . ? N3 Ni1 Br2 103.1(4) . . ? N2 Ni1 Br1 96.5(5) . . ? N1 Ni1 Br1 99.5(4) . . ? N3 Ni1 Br1 91.8(4) . . ? Br2 Ni1 Br1 110.29(13) . . ? N5 Ni2 O1 102.9(7) . . ? N5 Ni2 N4 79.1(7) . . ? O1 Ni2 N4 85.8(7) . . ? N5 Ni2 Br4 99.2(5) . . ? O1 Ni2 Br4 156.0(5) . . ? N4 Ni2 Br4 89.3(5) . . ? N5 Ni2 Br3 105.6(5) . . ? O1 Ni2 Br3 87.2(5) . . ? N4 Ni2 Br3 172.3(5) . . ? Br4 Ni2 Br3 95.88(13) . . ? C13 N1 C6 120.3(19) . . ? C13 N1 Ni1 112.9(14) . . ? C6 N1 Ni1 126.7(13) . . ? C15 N2 C19 120.6(19) . . ? C15 N2 Ni1 118.6(15) . . ? C19 N2 Ni1 120.7(15) . . ? C20 N3 C24 117.6(18) . . ? C20 N3 Ni1 111.0(14) . . ? C24 N3 Ni1 131.2(14) . . ? C25 N4 C29 112.4(18) . . ? C25 N4 Ni2 130.8(14) . . ? C29 N4 Ni2 116.3(14) . . ? C2 C1 C6 112(2) . . ? C2 C1 C7 124(2) . . ? C6 C1 C7 123(2) . . ? C3 C2 C1 125(2) . . ? C2 C3 C4 118(2) . . ? C5 C4 C3 121(2) . . ? C6 C5 C4 120(2) . . ? C6 C5 C10 120(2) . . ? C4 C5 C10 119(2) . . ? C5 C6 C1 123(2) . . ? C5 C6 N1 119(2) . . ? C1 C6 N1 118(2) . . ? C1 C7 C9 112(2) . . ? C1 C7 C8 113(2) . . ? C9 C7 C8 106(2) . . ? C12 C10 C11 109(2) . . ? C12 C10 C5 111(2) . . ? C11 C10 C5 110(2) . . ? N1 C13 C15 116(2) . . ? N1 C13 C14 124(2) . . ? C15 C13 C14 120(2) . . ? N2 C15 C16 121(2) . . ? N2 C15 C13 113.5(19) . . ? C16 C15 C13 125(2) . . ? C15 C16 C17 120(2) . . ? C18 C17 C16 116(2) . . ? C17 C18 C19 124(2) . . ? N2 C19 C18 118(2) . . ? N2 C19 C20 113.2(19) . . ? C18 C19 C20 129(2) . . ? N3 C20 C21 123(2) . . ? N3 C20 C19 117(2) . . ? C21 C20 C19 120(2) . . ? C20 C21 C22 118(2) . . ? C23 C22 C21 120(3) . . ? C22 C23 C24 118(3) . . ? N3 C24 C23 122(2) . . ? N3 C24 C25 121.3(19) . . ? C23 C24 C25 116(2) . . ? N4 C25 C26 124.6(19) . . ? N4 C25 C24 120.4(18) . . ? C26 C25 C24 114.9(19) . . ? C27 C26 C25 121(2) . . ? C26 C27 C28 114.3(19) . . ? C29 C28 C27 118(2) . . ? C28 C29 N4 129(2) . . ? C28 C29 C30 120(2) . . ? N4 C29 C30 110.2(18) . . ? N5 C30 C31 128(2) . . ? N5 C30 C29 116.9(18) . . ? C31 C30 C29 114.7(18) . . ? C30 N5 C33 116.8(18) . . ? C30 N5 Ni2 116.6(14) . . ? C33 N5 Ni2 126.5(14) . . ? N5 C33 C34 125(2) . . ? N5 C33 C38 119(2) . . ? C34 C33 C38 116.2(19) . . ? C35 C34 C33 119(2) . . ? C35 C34 C39 123(2) . . ? C33 C34 C39 118.1(19) . . ? C36 C35 C34 124(3) . . ? C35 C36 C37 121(2) . . ? C36 C37 C38 118(2) . . ? C37 C38 C33 122(2) . . ? C37 C38 C42 120(2) . . ? C33 C38 C42 118(2) . . ? C41 C39 C34 112(2) . . ? C41 C39 C40 112(2) . . ? C34 C39 C40 112(2) . . ? C38 C42 C44 112(2) . . ? C38 C42 C43 109(2) . . ? C44 C42 C43 109(2) . . ? Cl2 C45 Cl1 110.6(15) . . ? Cl2 C45 Cl3 107.7(15) . . ? Cl1 C45 Cl3 106.6(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.836 _refine_diff_density_min -1.288 _refine_diff_density_rms 0.226 data_04008 _database_code_depnum_ccdc_archive 'CCDC 289331' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C43 H49 Cl4 N5 Zn2) (C2 H3 N)' _chemical_formula_sum 'C45 H52 Cl4 N6 Zn2' _chemical_formula_weight 949.47 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' Cl Cl 0.1484 0.1585 '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 17.026(4) _cell_length_b 18.321(4) _cell_length_c 15.777(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.599(4) _cell_angle_gamma 90.00 _cell_volume 4575.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2828 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 20.29 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 1.320 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ; absorption correction based on 6674 reflections (SADABS); Rint 0.063 before correction and 0.045 after. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32683 _diffrn_reflns_av_R_equivalents 0.0866 _diffrn_reflns_av_sigmaI/netI 0.1095 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8048 _reflns_number_gt 5167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0207P)^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 8048 _refine_ls_number_parameters 525 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.846 _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 0.07776(3) 0.31617(3) 0.64697(3) 0.02417(14) Uani 1 1 d . . . Zn2 Zn 0.38568(3) 0.36421(3) 0.63309(3) 0.02757(14) Uani 1 1 d . . . Cl1 Cl 0.05481(7) 0.19718(5) 0.65438(7) 0.0283(3) Uani 1 1 d . . . Cl2 Cl 0.17996(7) 0.38164(6) 0.74923(7) 0.0288(3) Uani 1 1 d . . . Cl3 Cl 0.30440(8) 0.44287(6) 0.53613(8) 0.0458(4) Uani 1 1 d . . . Cl4 Cl 0.47035(8) 0.29728(7) 0.58572(8) 0.0431(3) Uani 1 1 d . . . N1 N -0.0381(2) 0.35602(17) 0.6718(2) 0.0241(9) Uani 1 1 d . . . N2 N 0.0053(2) 0.37002(18) 0.5292(2) 0.0242(9) Uani 1 1 d . . . N3 N 0.1486(2) 0.30030(17) 0.5503(2) 0.0227(8) Uani 1 1 d . . . N4 N 0.3341(2) 0.29098(17) 0.6967(2) 0.0240(9) Uani 1 1 d . . . N5 N 0.4484(2) 0.39317(18) 0.7682(2) 0.0250(9) Uani 1 1 d . . . N6 N 0.5884(5) 0.2058(4) 0.8795(6) 0.126(3) Uani 1 1 d . . . C1 C -0.0625(3) 0.3331(2) 0.7460(3) 0.0257(11) Uani 1 1 d . . . C2 C -0.0262(3) 0.3682(2) 0.8308(3) 0.0282(11) Uani 1 1 d . . . C3 C -0.0455(3) 0.3405(2) 0.9030(3) 0.0350(12) Uani 1 1 d . . . H3 H -0.0215 0.3629 0.9611 0.042 Uiso 1 1 calc R . . C4 C -0.0978(3) 0.2819(3) 0.8927(3) 0.0401(13) Uani 1 1 d . . . H4 H -0.1094 0.2637 0.9433 0.048 Uiso 1 1 calc R . . C5 C -0.1336(3) 0.2494(2) 0.8083(3) 0.0365(12) Uani 1 1 d . . . H5 H -0.1709 0.2093 0.8012 0.044 Uiso 1 1 calc R . . C6 C -0.1166(3) 0.2737(2) 0.7334(3) 0.0302(11) Uani 1 1 d . . . C7 C -0.0861(3) 0.3984(2) 0.6088(3) 0.0279(11) Uani 1 1 d . . . C8 C -0.1640(3) 0.4358(3) 0.6085(3) 0.0472(14) Uani 1 1 d . . . H8A H -0.1745 0.4223 0.6635 0.071 Uiso 1 1 calc R . . H8B H -0.2121 0.4208 0.5544 0.071 Uiso 1 1 calc R . . H8C H -0.1565 0.4887 0.6073 0.071 Uiso 1 1 calc R . . C9 C -0.0608(3) 0.4093(2) 0.5287(3) 0.0259(11) Uani 1 1 d . . . C10 C -0.1047(3) 0.4540(2) 0.4555(3) 0.0339(12) Uani 1 1 d . . . H10 H -0.1517 0.4820 0.4554 0.041 Uiso 1 1 calc R . . C11 C -0.0778(3) 0.4565(2) 0.3822(3) 0.0344(12) Uani 1 1 d . . . H11 H -0.1056 0.4878 0.3321 0.041 Uiso 1 1 calc R . . C12 C -0.0117(3) 0.4142(2) 0.3816(3) 0.0319(12) Uani 1 1 d . . . H12 H 0.0055 0.4145 0.3308 0.038 Uiso 1 1 calc R . . C13 C 0.0298(3) 0.3705(2) 0.4578(3) 0.0256(11) Uani 1 1 d . . . C14 C 0.1017(3) 0.3226(2) 0.4647(3) 0.0248(10) Uani 1 1 d . . . C15 C 0.1201(3) 0.3020(2) 0.3903(3) 0.0314(12) Uani 1 1 d . . . H15 H 0.0859 0.3185 0.3311 0.038 Uiso 1 1 calc R . . C16 C 0.1873(3) 0.2580(2) 0.4017(3) 0.0349(12) Uani 1 1 d . . . H16 H 0.1988 0.2414 0.3504 0.042 Uiso 1 1 calc R . . C17 C 0.2393(3) 0.2375(2) 0.4894(3) 0.0321(12) Uani 1 1 d . . . H17 H 0.2888 0.2093 0.4997 0.038 Uiso 1 1 calc R . . C18 C 0.2164(3) 0.2596(2) 0.5611(3) 0.0260(11) Uani 1 1 d . . . C19 C 0.2721(3) 0.2431(2) 0.6582(3) 0.0240(10) Uani 1 1 d . . . C20 C 0.2591(3) 0.1834(2) 0.7056(3) 0.0293(11) Uani 1 1 d . . . H20 H 0.2157 0.1491 0.6767 0.035 Uiso 1 1 calc R . . C21 C 0.3116(3) 0.1751(2) 0.7969(3) 0.0307(11) Uani 1 1 d . . . H21 H 0.3058 0.1337 0.8303 0.037 Uiso 1 1 calc R . . C22 C 0.3714(3) 0.2272(2) 0.8381(3) 0.0307(12) Uani 1 1 d . . . H22 H 0.4055 0.2235 0.9010 0.037 Uiso 1 1 calc R . . C23 C 0.3815(3) 0.2853(2) 0.7864(3) 0.0250(11) Uani 1 1 d . . . C24 C 0.4413(3) 0.3473(2) 0.8256(3) 0.0258(11) Uani 1 1 d . . . C25 C 0.4842(3) 0.3519(2) 0.9267(3) 0.0413(13) Uani 1 1 d . . . H25A H 0.5178 0.3967 0.9428 0.062 Uiso 1 1 calc R . . H25B H 0.5212 0.3095 0.9489 0.062 Uiso 1 1 calc R . . H25C H 0.4416 0.3525 0.9549 0.062 Uiso 1 1 calc R . . C26 C 0.4949(3) 0.4610(2) 0.7984(3) 0.0258(11) Uani 1 1 d . . . C27 C 0.4498(3) 0.5210(2) 0.8115(3) 0.0293(11) Uani 1 1 d . . . C28 C 0.4938(3) 0.5871(2) 0.8376(3) 0.0378(13) Uani 1 1 d . . . H28 H 0.4652 0.6292 0.8467 0.045 Uiso 1 1 calc R . . C29 C 0.5770(3) 0.5916(3) 0.8500(3) 0.0385(13) Uani 1 1 d . . . H29 H 0.6060 0.6366 0.8685 0.046 Uiso 1 1 calc R . . C30 C 0.6197(3) 0.5322(3) 0.8362(3) 0.0391(13) Uani 1 1 d . . . H30 H 0.6777 0.5369 0.8448 0.047 Uiso 1 1 calc R . . C31 C 0.5794(3) 0.4647(2) 0.8097(3) 0.0306(11) Uani 1 1 d . . . C32 C 0.0262(3) 0.4373(2) 0.8438(3) 0.0378(13) Uani 1 1 d . . . H32 H 0.0430 0.4431 0.7897 0.045 Uiso 1 1 calc R . . C33 C 0.1065(3) 0.4362(3) 0.9293(3) 0.0534(15) Uani 1 1 d . . . H33A H 0.0913 0.4335 0.9834 0.080 Uiso 1 1 calc R . . H33B H 0.1390 0.4808 0.9318 0.080 Uiso 1 1 calc R . . H33C H 0.1406 0.3935 0.9276 0.080 Uiso 1 1 calc R . . C34 C -0.0288(3) 0.5028(2) 0.8466(4) 0.0546(16) Uani 1 1 d . . . H34A H -0.0779 0.5053 0.7895 0.082 Uiso 1 1 calc R . . H34B H 0.0043 0.5478 0.8544 0.082 Uiso 1 1 calc R . . H34C H -0.0478 0.4972 0.8978 0.082 Uiso 1 1 calc R . . C35 C -0.1605(3) 0.2368(2) 0.6404(3) 0.0378(13) Uani 1 1 d . . . H35 H -0.1342 0.2559 0.5976 0.045 Uiso 1 1 calc R . . C36 C -0.1502(3) 0.1543(2) 0.6455(3) 0.0428(13) Uani 1 1 d . . . H36A H -0.0899 0.1420 0.6696 0.064 Uiso 1 1 calc R . . H36B H -0.1770 0.1334 0.5844 0.064 Uiso 1 1 calc R . . H36C H -0.1770 0.1343 0.6859 0.064 Uiso 1 1 calc R . . C37 C -0.2541(3) 0.2553(3) 0.6013(3) 0.0666(18) Uani 1 1 d . . . H37A H -0.2815 0.2355 0.6411 0.100 Uiso 1 1 calc R . . H37B H -0.2799 0.2339 0.5404 0.100 Uiso 1 1 calc R . . H37C H -0.2612 0.3084 0.5972 0.100 Uiso 1 1 calc R . . C38 C 0.3574(3) 0.5174(2) 0.7979(3) 0.0376(13) Uani 1 1 d . . . H38 H 0.3357 0.4687 0.7710 0.045 Uiso 1 1 calc R . . C39 C 0.3055(3) 0.5756(3) 0.7319(3) 0.0591(17) Uani 1 1 d . . . H39A H 0.3242 0.6241 0.7575 0.089 Uiso 1 1 calc R . . H39B H 0.2456 0.5692 0.7221 0.089 Uiso 1 1 calc R . . H39C H 0.3133 0.5707 0.6736 0.089 Uiso 1 1 calc R . . C40 C 0.3453(3) 0.5233(3) 0.8891(3) 0.0610(17) Uani 1 1 d . . . H40A H 0.3815 0.4875 0.9319 0.092 Uiso 1 1 calc R . . H40B H 0.2860 0.5135 0.8797 0.092 Uiso 1 1 calc R . . H40C H 0.3605 0.5725 0.9140 0.092 Uiso 1 1 calc R . . C41 C 0.6279(3) 0.4001(3) 0.7952(3) 0.0449(14) Uani 1 1 d . . . H41 H 0.5880 0.3580 0.7742 0.054 Uiso 1 1 calc R . . C42 C 0.6647(4) 0.4153(3) 0.7235(4) 0.085(2) Uani 1 1 d . . . H42A H 0.6190 0.4255 0.6652 0.128 Uiso 1 1 calc R . . H42B H 0.6968 0.3727 0.7169 0.128 Uiso 1 1 calc R . . H42C H 0.7024 0.4577 0.7417 0.128 Uiso 1 1 calc R . . C43 C 0.6984(3) 0.3784(3) 0.8853(4) 0.085(2) Uani 1 1 d . . . H43A H 0.7414 0.4169 0.9038 0.127 Uiso 1 1 calc R . . H43B H 0.7243 0.3326 0.8769 0.127 Uiso 1 1 calc R . . H43C H 0.6745 0.3720 0.9326 0.127 Uiso 1 1 calc R . . C44 C 0.5639(5) 0.1526(5) 0.8957(6) 0.092(3) Uani 1 1 d . . . C45 C 0.5299(4) 0.0855(4) 0.9151(4) 0.099(3) Uani 1 1 d . . . H45A H 0.5071 0.0939 0.9629 0.149 Uiso 1 1 calc R . . H45B H 0.5747 0.0487 0.9358 0.149 Uiso 1 1 calc R . . H45C H 0.4847 0.0681 0.8598 0.149 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 0.0313(3) 0.0230(3) 0.0163(3) 0.0024(2) 0.0065(2) 0.0007(2) Zn2 0.0356(3) 0.0252(3) 0.0202(3) 0.0011(2) 0.0083(2) -0.0002(3) Cl1 0.0371(7) 0.0239(6) 0.0230(6) 0.0003(5) 0.0099(5) -0.0025(5) Cl2 0.0333(7) 0.0280(6) 0.0240(6) -0.0021(5) 0.0091(5) -0.0038(5) Cl3 0.0483(9) 0.0367(7) 0.0391(8) 0.0129(6) 0.0003(6) 0.0028(6) Cl4 0.0499(9) 0.0520(8) 0.0306(7) -0.0065(6) 0.0186(6) 0.0077(7) N1 0.030(2) 0.022(2) 0.017(2) -0.0009(16) 0.0049(17) -0.0023(17) N2 0.028(2) 0.024(2) 0.020(2) 0.0029(17) 0.0076(18) 0.0017(18) N3 0.025(2) 0.020(2) 0.022(2) 0.0017(16) 0.0079(18) -0.0061(17) N4 0.031(2) 0.022(2) 0.017(2) -0.0030(16) 0.0066(18) 0.0021(17) N5 0.026(2) 0.027(2) 0.023(2) 0.0006(17) 0.0092(18) 0.0019(17) N6 0.100(6) 0.124(7) 0.137(6) -0.070(6) 0.026(5) -0.012(5) C1 0.027(3) 0.024(3) 0.026(3) 0.007(2) 0.010(2) 0.011(2) C2 0.033(3) 0.029(3) 0.023(3) 0.003(2) 0.010(2) 0.010(2) C3 0.045(3) 0.034(3) 0.030(3) 0.005(2) 0.017(3) 0.012(2) C4 0.058(4) 0.040(3) 0.032(3) 0.016(3) 0.029(3) 0.018(3) C5 0.040(3) 0.030(3) 0.046(3) 0.009(3) 0.025(3) 0.006(2) C6 0.035(3) 0.024(3) 0.033(3) 0.001(2) 0.014(2) 0.002(2) C7 0.030(3) 0.028(3) 0.026(3) 0.003(2) 0.010(2) 0.006(2) C8 0.042(3) 0.058(4) 0.046(3) 0.026(3) 0.022(3) 0.025(3) C9 0.031(3) 0.024(3) 0.018(2) 0.004(2) 0.003(2) -0.003(2) C10 0.036(3) 0.033(3) 0.029(3) 0.003(2) 0.008(2) -0.004(2) C11 0.035(3) 0.034(3) 0.023(3) 0.011(2) -0.003(2) -0.008(2) C12 0.037(3) 0.036(3) 0.017(3) 0.004(2) 0.003(2) -0.012(2) C13 0.032(3) 0.024(3) 0.017(2) 0.003(2) 0.005(2) -0.009(2) C14 0.030(3) 0.023(3) 0.021(3) -0.003(2) 0.009(2) -0.011(2) C15 0.039(3) 0.035(3) 0.019(3) 0.001(2) 0.010(2) -0.010(2) C16 0.045(3) 0.046(3) 0.021(3) -0.016(2) 0.021(3) -0.015(3) C17 0.036(3) 0.031(3) 0.034(3) -0.008(2) 0.019(3) -0.002(2) C18 0.032(3) 0.027(3) 0.019(2) -0.005(2) 0.009(2) -0.004(2) C19 0.025(3) 0.022(3) 0.029(3) -0.005(2) 0.015(2) 0.004(2) C20 0.031(3) 0.024(3) 0.034(3) -0.004(2) 0.013(2) 0.001(2) C21 0.038(3) 0.023(3) 0.036(3) 0.008(2) 0.019(2) 0.004(2) C22 0.036(3) 0.033(3) 0.023(3) 0.006(2) 0.010(2) 0.004(2) C23 0.025(3) 0.025(3) 0.026(3) -0.001(2) 0.011(2) 0.004(2) C24 0.029(3) 0.027(3) 0.021(3) -0.003(2) 0.009(2) 0.000(2) C25 0.057(4) 0.040(3) 0.021(3) -0.001(2) 0.008(3) -0.006(3) C26 0.026(3) 0.032(3) 0.018(2) -0.004(2) 0.007(2) -0.006(2) C27 0.028(3) 0.032(3) 0.028(3) -0.007(2) 0.010(2) -0.003(2) C28 0.039(3) 0.031(3) 0.043(3) -0.006(2) 0.014(3) 0.000(2) C29 0.038(3) 0.035(3) 0.043(3) -0.006(2) 0.015(3) -0.009(3) C30 0.028(3) 0.051(3) 0.040(3) 0.004(3) 0.015(3) -0.005(3) C31 0.033(3) 0.031(3) 0.029(3) -0.002(2) 0.013(2) 0.001(2) C32 0.051(4) 0.034(3) 0.032(3) -0.007(2) 0.019(3) 0.001(3) C33 0.052(4) 0.062(4) 0.043(3) -0.018(3) 0.013(3) 0.000(3) C34 0.070(4) 0.025(3) 0.073(4) 0.000(3) 0.030(3) 0.003(3) C35 0.042(3) 0.034(3) 0.035(3) -0.002(2) 0.012(3) -0.002(3) C36 0.044(3) 0.039(3) 0.045(3) 0.000(3) 0.016(3) 0.000(3) C37 0.062(4) 0.057(4) 0.059(4) -0.018(3) -0.003(3) 0.009(3) C38 0.030(3) 0.035(3) 0.050(3) -0.017(3) 0.016(3) -0.005(2) C39 0.039(4) 0.076(4) 0.053(4) -0.015(3) 0.006(3) 0.016(3) C40 0.049(4) 0.069(4) 0.074(4) 0.006(3) 0.033(3) 0.006(3) C41 0.027(3) 0.048(3) 0.063(4) -0.004(3) 0.020(3) 0.007(3) C42 0.105(6) 0.071(4) 0.120(6) -0.020(4) 0.090(5) 0.004(4) C43 0.059(4) 0.081(5) 0.103(5) 0.011(4) 0.016(4) 0.036(4) C44 0.064(6) 0.098(7) 0.090(6) -0.061(7) 0.001(5) 0.022(6) C45 0.114(7) 0.104(6) 0.065(5) -0.018(5) 0.015(4) 0.060(5) _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 N2 2.064(3) . ? Zn1 Cl1 2.2254(12) . ? Zn1 Cl2 2.2367(12) . ? Zn1 N1 2.270(3) . ? Zn1 N3 2.285(3) . ? Zn2 N4 2.056(3) . ? Zn2 N5 2.071(3) . ? Zn2 Cl3 2.1848(13) . ? Zn2 Cl4 2.2212(13) . ? N1 C7 1.289(5) . ? N1 C1 1.441(5) . ? N2 C9 1.333(5) . ? N2 C13 1.337(5) . ? N3 C18 1.331(5) . ? N3 C14 1.354(5) . ? N4 C19 1.335(5) . ? N4 C23 1.350(5) . ? N5 C24 1.274(5) . ? N5 C26 1.456(5) . ? N6 C44 1.125(10) . ? C1 C6 1.391(5) . ? C1 C2 1.406(5) . ? C2 C3 1.392(5) . ? C2 C32 1.519(6) . ? C3 C4 1.366(6) . ? C4 C5 1.379(6) . ? C5 C6 1.390(5) . ? C6 C35 1.536(6) . ? C7 C8 1.490(5) . ? C7 C9 1.493(5) . ? C9 C10 1.389(5) . ? C10 C11 1.393(6) . ? C11 C12 1.369(6) . ? C12 C13 1.401(5) . ? C13 C14 1.477(6) . ? C14 C15 1.375(5) . ? C15 C16 1.357(6) . ? C16 C17 1.392(6) . ? C17 C18 1.386(5) . ? C18 C19 1.506(5) . ? C19 C20 1.387(5) . ? C20 C21 1.396(5) . ? C21 C22 1.372(5) . ? C22 C23 1.390(5) . ? C23 C24 1.499(5) . ? C24 C25 1.493(5) . ? C26 C31 1.384(5) . ? C26 C27 1.399(5) . ? C27 C28 1.404(5) . ? C27 C38 1.509(6) . ? C28 C29 1.359(6) . ? C29 C30 1.370(6) . ? C30 C31 1.402(6) . ? C31 C41 1.509(6) . ? C32 C33 1.527(6) . ? C32 C34 1.532(5) . ? C35 C37 1.521(6) . ? C35 C36 1.521(5) . ? C38 C39 1.524(6) . ? C38 C40 1.531(6) . ? C41 C42 1.507(6) . ? C41 C43 1.537(6) . ? C44 C45 1.440(9) . ? 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 Zn1 Cl1 117.20(10) . . ? N2 Zn1 Cl2 116.21(10) . . ? Cl1 Zn1 Cl2 126.33(4) . . ? N2 Zn1 N1 74.47(13) . . ? Cl1 Zn1 N1 97.20(9) . . ? Cl2 Zn1 N1 101.41(9) . . ? N2 Zn1 N3 75.36(13) . . ? Cl1 Zn1 N3 93.24(8) . . ? Cl2 Zn1 N3 95.06(9) . . ? N1 Zn1 N3 149.61(12) . . ? N4 Zn2 N5 79.40(13) . . ? N4 Zn2 Cl3 119.86(10) . . ? N5 Zn2 Cl3 120.36(10) . . ? N4 Zn2 Cl4 104.53(10) . . ? N5 Zn2 Cl4 109.56(10) . . ? Cl3 Zn2 Cl4 116.80(5) . . ? C7 N1 C1 120.8(4) . . ? C7 N1 Zn1 113.9(3) . . ? C1 N1 Zn1 125.1(3) . . ? C9 N2 C13 121.1(4) . . ? C9 N2 Zn1 119.1(3) . . ? C13 N2 Zn1 119.5(3) . . ? C18 N3 C14 117.6(4) . . ? C18 N3 Zn1 129.1(3) . . ? C14 N3 Zn1 111.4(3) . . ? C19 N4 C23 119.6(4) . . ? C19 N4 Zn2 128.0(3) . . ? C23 N4 Zn2 111.3(3) . . ? C24 N5 C26 120.8(3) . . ? C24 N5 Zn2 114.5(3) . . ? C26 N5 Zn2 124.6(3) . . ? C6 C1 C2 122.0(4) . . ? C6 C1 N1 119.1(4) . . ? C2 C1 N1 118.8(4) . . ? C3 C2 C1 117.3(4) . . ? C3 C2 C32 119.8(4) . . ? C1 C2 C32 122.7(4) . . ? C4 C3 C2 122.0(5) . . ? C3 C4 C5 119.4(4) . . ? C4 C5 C6 121.7(5) . . ? C5 C6 C1 117.6(4) . . ? C5 C6 C35 119.4(4) . . ? C1 C6 C35 122.9(4) . . ? N1 C7 C8 126.2(4) . . ? N1 C7 C9 115.8(4) . . ? C8 C7 C9 118.0(4) . . ? N2 C9 C10 121.2(4) . . ? N2 C9 C7 115.4(4) . . ? C10 C9 C7 123.2(4) . . ? C9 C10 C11 117.9(4) . . ? C12 C11 C10 120.7(4) . . ? C11 C12 C13 118.3(4) . . ? N2 C13 C12 120.8(4) . . ? N2 C13 C14 116.2(4) . . ? C12 C13 C14 123.0(4) . . ? N3 C14 C15 122.1(4) . . ? N3 C14 C13 114.9(4) . . ? C15 C14 C13 122.9(4) . . ? C16 C15 C14 119.8(4) . . ? C15 C16 C17 119.3(4) . . ? C18 C17 C16 117.8(4) . . ? N3 C18 C17 123.3(4) . . ? N3 C18 C19 115.8(4) . . ? C17 C18 C19 120.7(4) . . ? N4 C19 C20 121.9(4) . . ? N4 C19 C18 115.3(4) . . ? C20 C19 C18 122.7(4) . . ? C19 C20 C21 118.3(4) . . ? C22 C21 C20 119.6(4) . . ? C21 C22 C23 119.0(4) . . ? N4 C23 C22 121.2(4) . . ? N4 C23 C24 115.3(4) . . ? C22 C23 C24 123.4(4) . . ? N5 C24 C25 125.9(4) . . ? N5 C24 C23 115.7(4) . . ? C25 C24 C23 118.3(4) . . ? C31 C26 C27 122.8(4) . . ? C31 C26 N5 119.9(4) . . ? C27 C26 N5 117.2(4) . . ? C26 C27 C28 117.4(4) . . ? C26 C27 C38 123.0(4) . . ? C28 C27 C38 119.6(4) . . ? C29 C28 C27 120.6(4) . . ? C28 C29 C30 121.0(5) . . ? C29 C30 C31 121.2(4) . . ? C26 C31 C30 117.0(4) . . ? C26 C31 C41 122.9(4) . . ? C30 C31 C41 120.1(4) . . ? C2 C32 C33 113.5(4) . . ? C2 C32 C34 108.8(4) . . ? C33 C32 C34 110.0(4) . . ? C37 C35 C36 109.0(4) . . ? C37 C35 C6 111.0(4) . . ? C36 C35 C6 112.4(4) . . ? C27 C38 C39 112.3(4) . . ? C27 C38 C40 111.0(4) . . ? C39 C38 C40 110.4(4) . . ? C42 C41 C31 111.8(4) . . ? C42 C41 C43 110.1(4) . . ? C31 C41 C43 110.4(4) . . ? N6 C44 C45 178.2(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.624 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.075