# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Zhan Zhang' ;Department of Chemistry, University of British Columbia, 2036 Main Mall, Vancouver BC V6T1Z1 Canada ; 'Yakun Chen' ;Department of Chemistry, University of British Columbia, 2036 Main Mall, Vancouver BC V6T1Z1 Canada ; _publ_contact_author_address ;Department of Chemistry, University of British Columbia, 2036 Main Mall, Vancouver BC V6T1Z1 Canada ; _publ_contact_author_email david.dolphin@ubc.ca _publ_contact_author_fax 1-604-822-9678 _publ_contact_author_phone 1-604-822-4571 #TrackingRef '- CIFs.txt' _publ_contact_author_name 'David Dolphin' data_Fe-helicate _database_code_depnum_ccdc_archive 'CCDC 815374' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C99 H78 Fe2 N12, 2(C H Cl3)' _chemical_formula_sum 'C101 H80 Cl6 Fe2 N12' _chemical_formula_weight 1786.17 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' Fe Fe 0.3463 0.8444 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.2832(19) _cell_length_b 12.7319(8) _cell_length_c 24.0914(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.252(3) _cell_angle_gamma 90.00 _cell_volume 8638.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9958 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.02 _exptl_crystal_description hexagon _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3696 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.861 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7772 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.18 _reflns_number_total 7772 _reflns_number_gt 6148 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+10.3755P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7772 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.20337(9) 0.0585(2) 0.66848(10) 0.0361(6) Uani 1 1 d . . . H1 H 0.2096 0.1249 0.6528 0.043 Uiso 1 1 calc R . . C2 C 0.22528(10) -0.0358(2) 0.65470(11) 0.0385(6) Uani 1 1 d . . . H2 H 0.2485 -0.0439 0.6289 0.046 Uiso 1 1 calc R . . C3 C 0.20719(9) -0.1129(2) 0.68509(10) 0.0320(6) Uani 1 1 d . . . H3 H 0.2152 -0.1853 0.6846 0.038 Uiso 1 1 calc R . . C4 C 0.17374(8) -0.06490(18) 0.71809(9) 0.0259(5) Uani 1 1 d . . . C5 C 0.14624(8) -0.11449(19) 0.75523(10) 0.0284(5) Uani 1 1 d . . . C6 C 0.11386(8) -0.06404(18) 0.78728(9) 0.0258(5) Uani 1 1 d . . . C7 C 0.08137(9) -0.1131(2) 0.82060(10) 0.0307(5) Uani 1 1 d . . . H7 H 0.0790 -0.1864 0.8272 0.037 Uiso 1 1 calc R . . C8 C 0.05397(9) -0.03651(19) 0.84152(9) 0.0292(5) Uani 1 1 d . . . C9 C 0.07012(9) 0.05898(19) 0.81991(9) 0.0298(5) Uani 1 1 d . . . H9 H 0.0572 0.1259 0.8273 0.036 Uiso 1 1 calc R . . C10 C 0.01476(9) -0.0497(2) 0.88050(10) 0.0369(6) Uani 1 1 d . . . C11 C -0.05079(9) 0.04510(19) 0.81848(10) 0.0306(5) Uani 1 1 d . . . H11 H -0.0471 0.0028 0.7867 0.037 Uiso 1 1 calc R . . C12 C -0.02242(9) 0.03540(19) 0.86934(9) 0.0311(6) Uani 1 1 d . . . C13 C -0.03857(9) 0.1104(2) 0.90381(9) 0.0317(6) Uani 1 1 d . . . H13 H -0.0265 0.1241 0.9412 0.038 Uiso 1 1 calc R . . C14 C -0.07703(9) 0.16443(18) 0.87322(9) 0.0277(5) Uani 1 1 d . . . C15 C -0.10540(9) 0.24387(18) 0.89180(9) 0.0291(5) Uani 1 1 d . . . C16 C -0.14503(9) 0.28699(18) 0.86059(10) 0.0287(5) Uani 1 1 d . . . C17 C -0.17691(10) 0.36486(19) 0.87779(11) 0.0372(6) Uani 1 1 d . . . H17 H -0.1746 0.4002 0.9127 0.045 Uiso 1 1 calc R . . C18 C -0.21136(10) 0.3793(2) 0.83477(11) 0.0385(6) Uani 1 1 d . . . H18 H -0.2378 0.4255 0.8343 0.046 Uiso 1 1 calc R . . C19 C -0.20017(9) 0.31290(19) 0.79167(11) 0.0332(6) Uani 1 1 d . . . H19 H -0.2181 0.3082 0.7564 0.040 Uiso 1 1 calc R . . C20 C -0.01007(11) -0.1578(2) 0.87007(14) 0.0531(8) Uani 1 1 d . . . H20A H -0.0366 -0.1637 0.8933 0.080 Uiso 1 1 calc R . . H20B H 0.0128 -0.2143 0.8796 0.080 Uiso 1 1 calc R . . H20C H -0.0220 -0.1636 0.8307 0.080 Uiso 1 1 calc R . . C21 C 0.03694(12) -0.0445(3) 0.94062(11) 0.0632(11) Uani 1 1 d . . . H21A H 0.0524 0.0238 0.9473 0.095 Uiso 1 1 calc R . . H21B H 0.0605 -0.1006 0.9471 0.095 Uiso 1 1 calc R . . H21C H 0.0121 -0.0533 0.9661 0.095 Uiso 1 1 calc R . . C22 C 0.15062(9) -0.2309(2) 0.76050(11) 0.0357(6) Uani 1 1 d . . . C23 C 0.13846(10) -0.2964(2) 0.71491(14) 0.0454(7) Uani 1 1 d . . . H23 H 0.1274 -0.2672 0.6798 0.055 Uiso 1 1 calc R . . C24 C 0.14266(11) -0.4050(3) 0.72136(19) 0.0657(11) Uani 1 1 d . . . H24 H 0.1347 -0.4496 0.6903 0.079 Uiso 1 1 calc R . . C25 C 0.15800(14) -0.4480(3) 0.7717(2) 0.0761(13) Uani 1 1 d . . . H25 H 0.1604 -0.5221 0.7755 0.091 Uiso 1 1 calc R . . C26 C 0.16985(14) -0.3849(3) 0.81622(18) 0.0743(12) Uani 1 1 d . . . H26 H 0.1803 -0.4154 0.8512 0.089 Uiso 1 1 calc R . . C27 C 0.16686(11) -0.2748(2) 0.81132(13) 0.0518(8) Uani 1 1 d . . . H27 H 0.1759 -0.2312 0.8425 0.062 Uiso 1 1 calc R . . C28 C -0.09337(10) 0.2857(2) 0.94927(10) 0.0374(6) Uani 1 1 d . . . C29 C -0.05146(13) 0.3375(2) 0.96311(13) 0.0547(8) Uani 1 1 d . . . H29 H -0.0291 0.3461 0.9364 0.066 Uiso 1 1 calc R . . C30 C -0.04182(17) 0.3784(3) 1.01798(17) 0.0776(12) Uani 1 1 d . . . H30 H -0.0129 0.4144 1.0282 0.093 Uiso 1 1 calc R . . C31 C -0.07470(19) 0.3651(3) 1.05589(14) 0.0755(13) Uani 1 1 d . . . H31 H -0.0685 0.3935 1.0923 0.091 Uiso 1 1 calc R . . C32 C -0.11553(17) 0.3128(3) 1.04273(13) 0.0729(12) Uani 1 1 d . . . H32 H -0.1374 0.3029 1.0700 0.087 Uiso 1 1 calc R . . C33 C -0.12551(13) 0.2739(2) 0.98972(11) 0.0514(8) Uani 1 1 d . . . H33 H -0.1547 0.2384 0.9804 0.062 Uiso 1 1 calc R . . C34 C 0.22582(9) 0.12563(19) 0.80929(10) 0.0302(5) Uani 1 1 d . . . H34 H 0.2393 0.0868 0.7810 0.036 Uiso 1 1 calc R . . C35 C 0.24839(9) 0.14264(19) 0.86303(10) 0.0324(6) Uani 1 1 d . . . H35 H 0.2791 0.1190 0.8770 0.039 Uiso 1 1 calc R . . C36 C 0.21736(9) 0.19999(19) 0.89127(10) 0.0319(5) Uani 1 1 d . . . H36 H 0.2224 0.2231 0.9288 0.038 Uiso 1 1 calc R . . C37 C 0.17619(8) 0.21863(18) 0.85392(9) 0.0270(5) Uani 1 1 d . . . C38 C 0.13649(8) 0.27975(18) 0.86356(10) 0.0281(5) Uani 1 1 d . . . C39 C 0.10030(9) 0.30654(18) 0.82269(9) 0.0279(5) Uani 1 1 d . . . C40 C 0.06465(9) 0.38481(19) 0.82461(10) 0.0308(5) Uani 1 1 d . . . H40 H 0.0585 0.4251 0.8564 0.037 Uiso 1 1 calc R . . C41 C 0.04053(8) 0.39215(18) 0.77240(10) 0.0285(5) Uani 1 1 d . . . C42 C 0.06126(8) 0.31507(18) 0.74004(10) 0.0286(5) Uani 1 1 d . . . H42 H 0.0512 0.3015 0.7020 0.034 Uiso 1 1 calc R . . C43 C 0.0000 0.4638(3) 0.7500 0.0324(8) Uani 1 2 d S . . C44 C -0.01591(10) 0.5336(2) 0.79673(13) 0.0451(7) Uani 1 1 d . . . H44A H -0.0419 0.5793 0.7817 0.068 Uiso 1 1 calc R . . H44B H 0.0109 0.5767 0.8121 0.068 Uiso 1 1 calc R . . H44C H -0.0269 0.4893 0.8263 0.068 Uiso 1 1 calc R . . C45 C 0.13163(9) 0.3180(2) 0.92150(10) 0.0324(6) Uani 1 1 d . . . C46 C 0.09378(13) 0.2838(3) 0.94842(14) 0.0642(9) Uani 1 1 d . . . H46 H 0.0706 0.2393 0.9296 0.077 Uiso 1 1 calc R . . C47 C 0.08940(16) 0.3143(4) 1.00354(16) 0.0857(13) Uani 1 1 d . . . H47 H 0.0636 0.2888 1.0224 0.103 Uiso 1 1 calc R . . C48 C 0.12199(13) 0.3806(3) 1.03050(13) 0.0659(10) Uani 1 1 d . . . H48 H 0.1205 0.3972 1.0687 0.079 Uiso 1 1 calc R . . C49 C 0.15638(14) 0.4221(3) 1.00168(13) 0.0648(10) Uani 1 1 d . . . H49 H 0.1771 0.4737 1.0188 0.078 Uiso 1 1 calc R . . C50 C 0.16188(12) 0.3905(3) 0.94748(12) 0.0527(8) Uani 1 1 d . . . H50 H 0.1868 0.4192 0.9283 0.063 Uiso 1 1 calc R . . N1 N 0.17247(7) 0.04272(15) 0.70665(8) 0.0279(4) Uani 1 1 d . . . N2 N 0.10603(7) 0.04397(15) 0.78755(7) 0.0260(4) Uani 1 1 d . . . N3 N -0.08344(7) 0.12005(15) 0.81992(8) 0.0264(4) Uani 1 1 d . . . N4 N -0.16101(7) 0.25681(15) 0.80629(8) 0.0274(4) Uani 1 1 d . . . N5 N 0.18298(7) 0.17102(15) 0.80300(8) 0.0286(4) Uani 1 1 d . . . N6 N 0.09652(7) 0.26350(15) 0.76897(8) 0.0260(4) Uani 1 1 d . . . Fe1 Fe 0.133844(11) 0.15022(2) 0.740079(13) 0.02422(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0408(15) 0.0327(14) 0.0374(14) 0.0044(11) 0.0170(12) 0.0028(12) C2 0.0402(15) 0.0397(15) 0.0388(14) 0.0013(12) 0.0206(12) 0.0054(12) C3 0.0307(13) 0.0282(13) 0.0379(13) -0.0058(11) 0.0069(11) 0.0042(10) C4 0.0267(12) 0.0248(12) 0.0265(11) -0.0030(10) 0.0044(9) 0.0021(10) C5 0.0297(13) 0.0241(12) 0.0314(12) -0.0005(10) 0.0032(10) 0.0004(10) C6 0.0306(13) 0.0234(12) 0.0240(11) 0.0025(9) 0.0061(9) 0.0026(10) C7 0.0366(14) 0.0261(12) 0.0307(12) 0.0068(10) 0.0093(10) 0.0043(11) C8 0.0321(13) 0.0332(13) 0.0230(11) 0.0066(10) 0.0071(10) 0.0079(10) C9 0.0377(14) 0.0276(13) 0.0252(12) -0.0003(10) 0.0084(10) 0.0079(10) C10 0.0435(15) 0.0405(15) 0.0292(12) 0.0143(11) 0.0171(11) 0.0161(12) C11 0.0355(14) 0.0299(13) 0.0283(12) 0.0029(10) 0.0126(10) 0.0048(11) C12 0.0343(14) 0.0352(14) 0.0257(12) 0.0090(10) 0.0129(10) 0.0071(11) C13 0.0372(14) 0.0378(14) 0.0210(11) 0.0068(10) 0.0072(10) 0.0064(11) C14 0.0340(13) 0.0277(13) 0.0225(11) 0.0046(10) 0.0079(10) 0.0013(10) C15 0.0398(14) 0.0245(12) 0.0240(11) 0.0032(10) 0.0087(10) -0.0003(10) C16 0.0374(14) 0.0202(12) 0.0292(12) 0.0006(10) 0.0063(10) 0.0002(10) C17 0.0517(17) 0.0255(13) 0.0349(13) -0.0044(11) 0.0072(12) 0.0074(12) C18 0.0410(15) 0.0292(14) 0.0452(15) -0.0034(12) 0.0028(12) 0.0128(11) C19 0.0327(14) 0.0286(13) 0.0377(13) -0.0023(11) -0.0002(11) 0.0035(11) C20 0.0510(18) 0.0391(16) 0.074(2) 0.0240(15) 0.0320(16) 0.0115(14) C21 0.070(2) 0.096(3) 0.0267(14) 0.0188(15) 0.0171(14) 0.051(2) C22 0.0302(13) 0.0262(13) 0.0539(16) 0.0057(12) 0.0207(12) 0.0043(10) C23 0.0369(15) 0.0289(15) 0.072(2) -0.0105(14) 0.0141(14) -0.0028(12) C24 0.0428(19) 0.0318(17) 0.127(3) -0.020(2) 0.034(2) -0.0070(14) C25 0.075(3) 0.0265(17) 0.137(4) 0.012(2) 0.066(3) 0.0089(16) C26 0.088(3) 0.050(2) 0.094(3) 0.037(2) 0.056(2) 0.035(2) C27 0.062(2) 0.0388(16) 0.0591(19) 0.0134(14) 0.0302(16) 0.0188(14) C28 0.0555(17) 0.0272(13) 0.0283(13) 0.0022(10) -0.0032(12) 0.0138(12) C29 0.068(2) 0.0488(18) 0.0430(16) 0.0030(14) -0.0149(15) -0.0006(16) C30 0.101(3) 0.051(2) 0.071(3) -0.0058(19) -0.042(2) 0.005(2) C31 0.130(4) 0.061(2) 0.0330(17) -0.0108(16) -0.008(2) 0.035(2) C32 0.110(3) 0.077(3) 0.0322(17) -0.0007(17) 0.0077(19) 0.033(3) C33 0.077(2) 0.0477(17) 0.0308(14) 0.0046(13) 0.0144(14) 0.0194(16) C34 0.0312(13) 0.0251(12) 0.0352(13) 0.0020(10) 0.0087(10) 0.0038(10) C35 0.0289(13) 0.0303(13) 0.0373(13) 0.0035(11) 0.0001(10) 0.0041(10) C36 0.0360(14) 0.0287(13) 0.0303(12) 0.0011(10) -0.0006(10) 0.0003(11) C37 0.0335(13) 0.0224(12) 0.0254(11) 0.0005(9) 0.0048(10) -0.0009(10) C38 0.0317(13) 0.0234(12) 0.0294(12) -0.0001(10) 0.0042(10) -0.0004(10) C39 0.0352(13) 0.0212(12) 0.0279(12) -0.0024(10) 0.0065(10) 0.0000(10) C40 0.0345(14) 0.0221(12) 0.0361(13) -0.0052(10) 0.0045(11) 0.0018(10) C41 0.0281(13) 0.0200(11) 0.0374(13) 0.0001(10) 0.0030(10) -0.0019(10) C42 0.0315(13) 0.0251(12) 0.0293(12) -0.0003(10) 0.0024(10) -0.0009(10) C43 0.0251(18) 0.0227(17) 0.048(2) 0.000 -0.0019(15) 0.000 C44 0.0365(15) 0.0296(14) 0.0666(19) -0.0167(13) -0.0094(13) 0.0070(12) C45 0.0357(14) 0.0324(13) 0.0293(12) -0.0033(11) 0.0040(11) 0.0052(11) C46 0.069(2) 0.076(2) 0.0510(19) -0.0129(17) 0.0195(16) -0.0169(19) C47 0.096(3) 0.108(3) 0.059(2) -0.008(2) 0.042(2) -0.014(3) C48 0.069(2) 0.093(3) 0.0364(16) -0.0258(18) 0.0111(16) 0.003(2) C49 0.089(3) 0.064(2) 0.0410(17) -0.0218(16) 0.0040(17) -0.0083(19) C50 0.071(2) 0.0508(18) 0.0370(15) -0.0109(14) 0.0118(14) -0.0159(16) N1 0.0323(11) 0.0243(10) 0.0281(10) -0.0013(8) 0.0081(8) 0.0002(8) N2 0.0315(11) 0.0253(10) 0.0219(9) -0.0010(8) 0.0067(8) 0.0037(8) N3 0.0298(11) 0.0268(10) 0.0234(9) 0.0027(8) 0.0072(8) 0.0023(8) N4 0.0309(11) 0.0224(10) 0.0296(10) -0.0003(8) 0.0067(8) -0.0004(8) N5 0.0326(11) 0.0252(10) 0.0287(10) 0.0007(8) 0.0062(8) 0.0028(9) N6 0.0287(10) 0.0203(10) 0.0294(10) 0.0003(8) 0.0046(8) 0.0014(8) Fe1 0.0284(2) 0.02101(19) 0.02392(18) -0.00064(13) 0.00640(13) 0.00126(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.340(3) . ? C1 C2 1.405(4) . ? C1 H1 0.9500 . ? C2 C3 1.353(4) . ? C2 H2 0.9500 . ? C3 C4 1.428(3) . ? C3 H3 0.9500 . ? C4 C5 1.390(3) . ? C4 N1 1.397(3) . ? C5 C6 1.406(3) . ? C5 C22 1.492(3) . ? C6 N2 1.393(3) . ? C6 C7 1.419(3) . ? C7 C8 1.371(3) . ? C7 H7 0.9500 . ? C8 C9 1.415(3) . ? C8 C10 1.526(3) . ? C9 N2 1.349(3) . ? C9 H9 0.9500 . ? C10 C12 1.516(3) . ? C10 C21 1.526(4) . ? C10 C20 1.556(4) . ? C11 N3 1.331(3) . ? C11 C12 1.407(3) . ? C11 H11 0.9500 . ? C12 C13 1.371(3) . ? C13 C14 1.432(3) . ? C13 H13 0.9500 . ? C14 C15 1.390(3) . ? C14 N3 1.399(3) . ? C15 C16 1.403(3) . ? C15 C28 1.493(3) . ? C16 N4 1.398(3) . ? C16 C17 1.427(3) . ? C17 C18 1.368(4) . ? C17 H17 0.9500 . ? C18 C19 1.397(4) . ? C18 H18 0.9500 . ? C19 N4 1.337(3) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.386(4) . ? C22 C23 1.397(4) . ? C23 C24 1.395(4) . ? C23 H23 0.9500 . ? C24 C25 1.364(6) . ? C24 H24 0.9500 . ? C25 C26 1.358(6) . ? C25 H25 0.9500 . ? C26 C27 1.408(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.371(4) . ? C28 C33 1.400(4) . ? C29 C30 1.423(5) . ? C29 H29 0.9500 . ? C30 C31 1.372(6) . ? C30 H30 0.9500 . ? C31 C32 1.345(6) . ? C31 H31 0.9500 . ? C32 C33 1.375(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N5 1.338(3) . ? C34 C35 1.407(3) . ? C34 H34 0.9500 . ? C35 C36 1.370(3) . ? C35 H35 0.9500 . ? C36 C37 1.425(3) . ? C36 H36 0.9500 . ? C37 N5 1.397(3) . ? C37 C38 1.403(3) . ? C38 C39 1.396(3) . ? C38 C45 1.497(3) . ? C39 N6 1.401(3) . ? C39 C40 1.421(3) . ? C40 C41 1.378(3) . ? C40 H40 0.9500 . ? C41 C42 1.414(3) . ? C41 C43 1.525(3) . ? C42 N6 1.336(3) . ? C42 H42 0.9500 . ? C43 C41 1.525(3) 2_556 ? C43 C44 1.533(3) 2_556 ? C43 C44 1.533(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.370(4) . ? C45 C46 1.373(4) . ? C46 C47 1.400(5) . ? C46 H46 0.9500 . ? C47 C48 1.369(6) . ? C47 H47 0.9500 . ? C48 C49 1.353(5) . ? C48 H48 0.9500 . ? C49 C50 1.389(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? N1 Fe1 1.9688(19) . ? N2 Fe1 1.9802(19) . ? N3 Fe1 1.9728(19) 2_556 ? N4 Fe1 1.9589(19) 2_556 ? N5 Fe1 1.978(2) . ? N6 Fe1 1.9528(19) . ? Fe1 N4 1.9589(19) 2_556 ? Fe1 N3 1.9728(19) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.3(2) . . ? N1 C1 H1 124.3 . . ? C2 C1 H1 124.3 . . ? C3 C2 C1 107.2(2) . . ? C3 C2 H2 126.4 . . ? C1 C2 H2 126.4 . . ? C2 C3 C4 107.1(2) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C5 C4 N1 124.5(2) . . ? C5 C4 C3 127.0(2) . . ? N1 C4 C3 108.4(2) . . ? C4 C5 C6 125.2(2) . . ? C4 C5 C22 117.3(2) . . ? C6 C5 C22 117.4(2) . . ? N2 C6 C5 124.4(2) . . ? N2 C6 C7 108.71(19) . . ? C5 C6 C7 126.7(2) . . ? C8 C7 C6 108.2(2) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? C7 C8 C9 105.3(2) . . ? C7 C8 C10 128.0(2) . . ? C9 C8 C10 126.7(2) . . ? N2 C9 C8 112.1(2) . . ? N2 C9 H9 123.9 . . ? C8 C9 H9 123.9 . . ? C12 C10 C21 110.8(2) . . ? C12 C10 C8 110.10(19) . . ? C21 C10 C8 108.7(2) . . ? C12 C10 C20 108.0(2) . . ? C21 C10 C20 109.4(2) . . ? C8 C10 C20 109.9(2) . . ? N3 C11 C12 112.5(2) . . ? N3 C11 H11 123.8 . . ? C12 C11 H11 123.8 . . ? C13 C12 C11 105.7(2) . . ? C13 C12 C10 130.9(2) . . ? C11 C12 C10 123.2(2) . . ? C12 C13 C14 107.6(2) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? C15 C14 N3 124.0(2) . . ? C15 C14 C13 128.1(2) . . ? N3 C14 C13 107.9(2) . . ? C14 C15 C16 124.6(2) . . ? C14 C15 C28 118.0(2) . . ? C16 C15 C28 117.4(2) . . ? N4 C16 C15 124.6(2) . . ? N4 C16 C17 107.7(2) . . ? C15 C16 C17 127.7(2) . . ? C18 C17 C16 107.4(2) . . ? C18 C17 H17 126.3 . . ? C16 C17 H17 126.3 . . ? C17 C18 C19 106.7(2) . . ? C17 C18 H18 126.6 . . ? C19 C18 H18 126.6 . . ? N4 C19 C18 111.5(2) . . ? N4 C19 H19 124.3 . . ? C18 C19 H19 124.3 . . ? C10 C20 H20A 109.5 . . ? C10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C10 C21 H21A 109.5 . . ? C10 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C10 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 119.4(3) . . ? C27 C22 C5 119.6(3) . . ? C23 C22 C5 120.9(2) . . ? C24 C23 C22 119.5(3) . . ? C24 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C25 C24 C23 120.9(4) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C24 120.0(3) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.9(4) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C22 C27 C26 119.2(3) . . ? C22 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C29 C28 C33 119.0(3) . . ? C29 C28 C15 121.0(3) . . ? C33 C28 C15 120.0(3) . . ? C28 C29 C30 119.3(3) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C31 C30 C29 119.3(4) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C32 C31 C30 121.6(3) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C33 119.7(4) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C28 121.1(4) . . ? C32 C33 H33 119.5 . . ? C28 C33 H33 119.5 . . ? N5 C34 C35 111.6(2) . . ? N5 C34 H34 124.2 . . ? C35 C34 H34 124.2 . . ? C36 C35 C34 106.4(2) . . ? C36 C35 H35 126.8 . . ? C34 C35 H35 126.8 . . ? C35 C36 C37 107.4(2) . . ? C35 C36 H36 126.3 . . ? C37 C36 H36 126.3 . . ? N5 C37 C38 124.2(2) . . ? N5 C37 C36 108.2(2) . . ? C38 C37 C36 127.5(2) . . ? C39 C38 C37 124.4(2) . . ? C39 C38 C45 117.0(2) . . ? C37 C38 C45 118.6(2) . . ? C38 C39 N6 123.0(2) . . ? C38 C39 C40 128.7(2) . . ? N6 C39 C40 108.1(2) . . ? C41 C40 C39 108.1(2) . . ? C41 C40 H40 125.9 . . ? C39 C40 H40 125.9 . . ? C40 C41 C42 105.1(2) . . ? C40 C41 C43 131.1(2) . . ? C42 C41 C43 123.8(2) . . ? N6 C42 C41 112.4(2) . . ? N6 C42 H42 123.8 . . ? C41 C42 H42 123.8 . . ? C41 C43 C41 106.5(3) . 2_556 ? C41 C43 C44 110.17(14) . 2_556 ? C41 C43 C44 110.39(14) 2_556 2_556 ? C41 C43 C44 110.39(14) . . ? C41 C43 C44 110.17(14) 2_556 . ? C44 C43 C44 109.2(3) 2_556 . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 118.7(3) . . ? C50 C45 C38 122.6(2) . . ? C46 C45 C38 118.6(2) . . ? C45 C46 C47 120.0(3) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 120.5(4) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C49 C48 C47 118.8(3) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C48 C49 C50 121.1(3) . . ? C48 C49 H49 119.4 . . ? C50 C49 H49 119.4 . . ? C45 C50 C49 120.4(3) . . ? C45 C50 H50 119.8 . . ? C49 C50 H50 119.8 . . ? C1 N1 C4 105.98(19) . . ? C1 N1 Fe1 126.70(17) . . ? C4 N1 Fe1 127.32(15) . . ? C9 N2 C6 105.72(19) . . ? C9 N2 Fe1 126.64(16) . . ? C6 N2 Fe1 126.87(15) . . ? C11 N3 C14 106.4(2) . . ? C11 N3 Fe1 125.26(16) . 2_556 ? C14 N3 Fe1 128.16(16) . 2_556 ? C19 N4 C16 106.77(19) . . ? C19 N4 Fe1 125.33(16) . 2_556 ? C16 N4 Fe1 127.87(16) . 2_556 ? C34 N5 C37 106.5(2) . . ? C34 N5 Fe1 126.44(16) . . ? C37 N5 Fe1 125.97(16) . . ? C42 N6 C39 106.27(19) . . ? C42 N6 Fe1 125.39(16) . . ? C39 N6 Fe1 128.34(15) . . ? N6 Fe1 N4 86.83(8) . 2_556 ? N6 Fe1 N1 175.95(8) . . ? N4 Fe1 N1 89.26(8) 2_556 . ? N6 Fe1 N3 91.55(8) . 2_556 ? N4 Fe1 N3 90.68(8) 2_556 2_556 ? N1 Fe1 N3 87.46(8) . 2_556 ? N6 Fe1 N5 89.59(8) . . ? N4 Fe1 N5 93.41(8) 2_556 . ? N1 Fe1 N5 91.68(8) . . ? N3 Fe1 N5 175.80(8) 2_556 . ? N6 Fe1 N2 92.43(8) . . ? N4 Fe1 N2 179.24(8) 2_556 . ? N1 Fe1 N2 91.49(8) . . ? N3 Fe1 N2 89.51(8) 2_556 . ? N5 Fe1 N2 86.40(8) . . ? 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 N1 C1 C2 C3 0.4(3) . . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? C2 C3 C4 C5 179.3(2) . . . . ? C2 C3 C4 N1 -0.1(3) . . . . ? N1 C4 C5 C6 -1.1(4) . . . . ? C3 C4 C5 C6 179.6(2) . . . . ? N1 C4 C5 C22 177.4(2) . . . . ? C3 C4 C5 C22 -1.9(4) . . . . ? C4 C5 C6 N2 -2.2(4) . . . . ? C22 C5 C6 N2 179.3(2) . . . . ? C4 C5 C6 C7 172.2(2) . . . . ? C22 C5 C6 C7 -6.3(4) . . . . ? N2 C6 C7 C8 -0.4(3) . . . . ? C5 C6 C7 C8 -175.5(2) . . . . ? C6 C7 C8 C9 0.6(3) . . . . ? C6 C7 C8 C10 -178.7(2) . . . . ? C7 C8 C9 N2 -0.6(3) . . . . ? C10 C8 C9 N2 178.7(2) . . . . ? C7 C8 C10 C12 -149.5(3) . . . . ? C9 C8 C10 C12 31.4(4) . . . . ? C7 C8 C10 C21 88.9(3) . . . . ? C9 C8 C10 C21 -90.2(3) . . . . ? C7 C8 C10 C20 -30.8(4) . . . . ? C9 C8 C10 C20 150.2(3) . . . . ? N3 C11 C12 C13 -0.8(3) . . . . ? N3 C11 C12 C10 174.9(2) . . . . ? C21 C10 C12 C13 -1.3(4) . . . . ? C8 C10 C12 C13 -121.6(3) . . . . ? C20 C10 C12 C13 118.4(3) . . . . ? C21 C10 C12 C11 -175.8(3) . . . . ? C8 C10 C12 C11 63.9(3) . . . . ? C20 C10 C12 C11 -56.0(3) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? C10 C12 C13 C14 -174.8(2) . . . . ? C12 C13 C14 C15 177.4(2) . . . . ? C12 C13 C14 N3 0.0(3) . . . . ? N3 C14 C15 C16 2.6(4) . . . . ? C13 C14 C15 C16 -174.4(2) . . . . ? N3 C14 C15 C28 -178.2(2) . . . . ? C13 C14 C15 C28 4.8(4) . . . . ? C14 C15 C16 N4 -0.8(4) . . . . ? C28 C15 C16 N4 179.9(2) . . . . ? C14 C15 C16 C17 176.9(2) . . . . ? C28 C15 C16 C17 -2.3(4) . . . . ? N4 C16 C17 C18 0.8(3) . . . . ? C15 C16 C17 C18 -177.3(2) . . . . ? C16 C17 C18 C19 -1.1(3) . . . . ? C17 C18 C19 N4 1.1(3) . . . . ? C4 C5 C22 C27 118.2(3) . . . . ? C6 C5 C22 C27 -63.2(3) . . . . ? C4 C5 C22 C23 -61.9(3) . . . . ? C6 C5 C22 C23 116.7(3) . . . . ? C27 C22 C23 C24 0.3(4) . . . . ? C5 C22 C23 C24 -179.6(2) . . . . ? C22 C23 C24 C25 0.7(4) . . . . ? C23 C24 C25 C26 -0.6(5) . . . . ? C24 C25 C26 C27 -0.4(5) . . . . ? C23 C22 C27 C26 -1.3(4) . . . . ? C5 C22 C27 C26 178.6(3) . . . . ? C25 C26 C27 C22 1.4(5) . . . . ? C14 C15 C28 C29 64.6(3) . . . . ? C16 C15 C28 C29 -116.2(3) . . . . ? C14 C15 C28 C33 -116.6(3) . . . . ? C16 C15 C28 C33 62.7(3) . . . . ? C33 C28 C29 C30 -0.4(4) . . . . ? C15 C28 C29 C30 178.5(3) . . . . ? C28 C29 C30 C31 -0.1(5) . . . . ? C29 C30 C31 C32 1.2(6) . . . . ? C30 C31 C32 C33 -1.8(6) . . . . ? C31 C32 C33 C28 1.4(5) . . . . ? C29 C28 C33 C32 -0.3(4) . . . . ? C15 C28 C33 C32 -179.2(3) . . . . ? N5 C34 C35 C36 1.0(3) . . . . ? C34 C35 C36 C37 -0.8(3) . . . . ? C35 C36 C37 N5 0.3(3) . . . . ? C35 C36 C37 C38 -175.5(2) . . . . ? N5 C37 C38 C39 -4.4(4) . . . . ? C36 C37 C38 C39 170.8(2) . . . . ? N5 C37 C38 C45 174.5(2) . . . . ? C36 C37 C38 C45 -10.2(4) . . . . ? C37 C38 C39 N6 8.8(4) . . . . ? C45 C38 C39 N6 -170.2(2) . . . . ? C37 C38 C39 C40 -165.0(2) . . . . ? C45 C38 C39 C40 16.0(4) . . . . ? C38 C39 C40 C41 172.5(2) . . . . ? N6 C39 C40 C41 -2.0(3) . . . . ? C39 C40 C41 C42 1.8(3) . . . . ? C39 C40 C41 C43 -178.4(2) . . . . ? C40 C41 C42 N6 -1.0(3) . . . . ? C43 C41 C42 N6 179.2(2) . . . . ? C40 C41 C43 C41 -122.6(3) . . . 2_556 ? C42 C41 C43 C41 57.14(19) . . . 2_556 ? C40 C41 C43 C44 117.7(3) . . . 2_556 ? C42 C41 C43 C44 -62.6(3) . . . 2_556 ? C40 C41 C43 C44 -3.0(4) . . . . ? C42 C41 C43 C44 176.7(2) . . . . ? C39 C38 C45 C50 -113.6(3) . . . . ? C37 C38 C45 C50 67.4(3) . . . . ? C39 C38 C45 C46 62.6(3) . . . . ? C37 C38 C45 C46 -116.4(3) . . . . ? C50 C45 C46 C47 -6.6(5) . . . . ? C38 C45 C46 C47 177.1(3) . . . . ? C45 C46 C47 C48 1.8(7) . . . . ? C46 C47 C48 C49 4.8(7) . . . . ? C47 C48 C49 C50 -6.5(6) . . . . ? C46 C45 C50 C49 5.0(5) . . . . ? C38 C45 C50 C49 -178.8(3) . . . . ? C48 C49 C50 C45 1.6(6) . . . . ? C2 C1 N1 C4 -0.4(3) . . . . ? C2 C1 N1 Fe1 178.98(18) . . . . ? C5 C4 N1 C1 -179.1(2) . . . . ? C3 C4 N1 C1 0.3(3) . . . . ? C5 C4 N1 Fe1 1.5(3) . . . . ? C3 C4 N1 Fe1 -179.07(16) . . . . ? C8 C9 N2 C6 0.3(3) . . . . ? C8 C9 N2 Fe1 170.74(16) . . . . ? C5 C6 N2 C9 175.3(2) . . . . ? C7 C6 N2 C9 0.0(3) . . . . ? C5 C6 N2 Fe1 4.9(3) . . . . ? C7 C6 N2 Fe1 -170.35(15) . . . . ? C12 C11 N3 C14 0.8(3) . . . . ? C12 C11 N3 Fe1 -174.15(16) . . . 2_556 ? C15 C14 N3 C11 -178.0(2) . . . . ? C13 C14 N3 C11 -0.5(3) . . . . ? C15 C14 N3 Fe1 -3.3(3) . . . 2_556 ? C13 C14 N3 Fe1 174.25(16) . . . 2_556 ? C18 C19 N4 C16 -0.6(3) . . . . ? C18 C19 N4 Fe1 177.53(17) . . . 2_556 ? C15 C16 N4 C19 178.0(2) . . . . ? C17 C16 N4 C19 -0.1(3) . . . . ? C15 C16 N4 Fe1 -0.1(3) . . . 2_556 ? C17 C16 N4 Fe1 -178.20(16) . . . 2_556 ? C35 C34 N5 C37 -0.8(3) . . . . ? C35 C34 N5 Fe1 -169.33(16) . . . . ? C38 C37 N5 C34 176.3(2) . . . . ? C36 C37 N5 C34 0.3(3) . . . . ? C38 C37 N5 Fe1 -15.1(3) . . . . ? C36 C37 N5 Fe1 168.89(16) . . . . ? C41 C42 N6 C39 -0.2(3) . . . . ? C41 C42 N6 Fe1 179.29(15) . . . . ? C38 C39 N6 C42 -173.5(2) . . . . ? C40 C39 N6 C42 1.4(3) . . . . ? C38 C39 N6 Fe1 7.0(3) . . . . ? C40 C39 N6 Fe1 -178.12(16) . . . . ? C42 N6 Fe1 N4 68.90(19) . . . 2_556 ? C39 N6 Fe1 N4 -111.7(2) . . . 2_556 ? C42 N6 Fe1 N1 54.0(12) . . . . ? C39 N6 Fe1 N1 -126.5(11) . . . . ? C42 N6 Fe1 N3 -21.70(19) . . . 2_556 ? C39 N6 Fe1 N3 157.72(19) . . . 2_556 ? C42 N6 Fe1 N5 162.34(19) . . . . ? C39 N6 Fe1 N5 -18.2(2) . . . . ? C42 N6 Fe1 N2 -111.28(19) . . . . ? C39 N6 Fe1 N2 68.1(2) . . . . ? C1 N1 Fe1 N6 16.0(13) . . . . ? C4 N1 Fe1 N6 -164.7(11) . . . . ? C1 N1 Fe1 N4 1.1(2) . . . 2_556 ? C4 N1 Fe1 N4 -179.6(2) . . . 2_556 ? C1 N1 Fe1 N3 91.8(2) . . . 2_556 ? C4 N1 Fe1 N3 -88.9(2) . . . 2_556 ? C1 N1 Fe1 N5 -92.3(2) . . . . ? C4 N1 Fe1 N5 87.0(2) . . . . ? C1 N1 Fe1 N2 -178.7(2) . . . . ? C4 N1 Fe1 N2 0.6(2) . . . . ? C34 N5 Fe1 N6 -171.8(2) . . . . ? C37 N5 Fe1 N6 21.81(19) . . . . ? C34 N5 Fe1 N4 -85.0(2) . . . 2_556 ? C37 N5 Fe1 N4 108.61(19) . . . 2_556 ? C34 N5 Fe1 N1 4.4(2) . . . . ? C37 N5 Fe1 N1 -162.04(19) . . . . ? C34 N5 Fe1 N3 82.5(11) . . . 2_556 ? C37 N5 Fe1 N3 -83.9(11) . . . 2_556 ? C34 N5 Fe1 N2 95.7(2) . . . . ? C37 N5 Fe1 N2 -70.65(19) . . . . ? C9 N2 Fe1 N6 6.9(2) . . . . ? C6 N2 Fe1 N6 175.37(19) . . . . ? C9 N2 Fe1 N4 20(7) . . . 2_556 ? C6 N2 Fe1 N4 -171(100) . . . 2_556 ? C9 N2 Fe1 N1 -172.0(2) . . . . ? C6 N2 Fe1 N1 -3.6(2) . . . . ? C9 N2 Fe1 N3 -84.6(2) . . . 2_556 ? C6 N2 Fe1 N3 83.84(19) . . . 2_556 ? C9 N2 Fe1 N5 96.4(2) . . . . ? C6 N2 Fe1 N5 -95.20(19) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.18 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.866 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.055 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 -0.250 0.000 343 119 ' ' 2 0.250 0.250 0.500 343 119 ' ' 3 0.750 -0.250 0.500 343 119 ' ' 4 0.750 0.250 1.000 343 119 ' ' _platon_squeeze_details ; ; #===END data_Co-helicate _database_code_depnum_ccdc_archive 'CCDC 815375' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H82 Cl4 Co2 N12' _chemical_formula_weight 1723.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.2196(9) _cell_length_b 12.5132(4) _cell_length_c 23.8825(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.244(2) _cell_angle_gamma 90.00 _cell_volume 8383.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 103.0(1) _cell_measurement_reflns_used 9924 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.02 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3576 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59992 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0447 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 28.10 _reflns_number_total 10170 _reflns_number_gt 7448 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+18.2876P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10170 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.20077(8) 0.30639(17) 0.21356(9) 0.0181(4) Uani 1 1 d . . . H1 H 0.2192 0.2998 0.2491 0.022 Uiso 1 1 calc R . . C2 C 0.21223(8) 0.37432(17) 0.17030(10) 0.0206(5) Uani 1 1 d . . . H2 H 0.2393 0.4197 0.1711 0.025 Uiso 1 1 calc R . . C3 C 0.17683(8) 0.36251(17) 0.12663(9) 0.0180(4) Uani 1 1 d . . . H3 H 0.1744 0.3992 0.0916 0.022 Uiso 1 1 calc R . . C4 C 0.14449(8) 0.28473(16) 0.14377(9) 0.0149(4) Uani 1 1 d . . . C5 C 0.10496(8) 0.24072(16) 0.11098(9) 0.0147(4) Uani 1 1 d . . . C6 C 0.07653(8) 0.15965(16) 0.12872(9) 0.0151(4) Uani 1 1 d . . . C7 C 0.03822(8) 0.10477(17) 0.09708(9) 0.0172(4) Uani 1 1 d . . . H7 H 0.0261 0.1192 0.0592 0.021 Uiso 1 1 calc R . . C8 C 0.02204(8) 0.02773(17) 0.13093(9) 0.0164(4) Uani 1 1 d . . . C9 C 0.05038(7) 0.03752(16) 0.18347(9) 0.0157(4) Uani 1 1 d . . . H9 H 0.0466 -0.0057 0.2154 0.019 Uiso 1 1 calc R . . C10 C -0.01505(8) -0.05891(17) 0.11886(9) 0.0188(5) Uani 1 1 d . . . C11 C -0.06992(8) 0.05307(17) 0.17903(9) 0.0158(4) Uani 1 1 d . . . H11 H -0.0560 0.1207 0.1731 0.019 Uiso 1 1 calc R . . C12 C -0.05500(8) -0.04376(16) 0.15594(9) 0.0153(4) Uani 1 1 d . . . C13 C -0.08452(8) -0.12141(17) 0.17407(9) 0.0169(4) Uani 1 1 d . . . H13 H -0.0838 -0.1954 0.1654 0.020 Uiso 1 1 calc R . . C14 C -0.11618(8) -0.07049(16) 0.20810(9) 0.0154(4) Uani 1 1 d . . . C15 C -0.14766(8) -0.12204(16) 0.24081(9) 0.0156(4) Uani 1 1 d . . . C16 C -0.17222(7) -0.07283(16) 0.28095(9) 0.0147(4) Uani 1 1 d . . . C17 C -0.20181(8) -0.12284(17) 0.31790(9) 0.0182(4) Uani 1 1 d . . . H17 H -0.2098 -0.1965 0.3187 0.022 Uiso 1 1 calc R . . C18 C -0.21643(8) -0.04491(19) 0.35191(10) 0.0218(5) Uani 1 1 d . . . H18 H -0.2362 -0.0539 0.3813 0.026 Uiso 1 1 calc R . . C19 C -0.19650(8) 0.05192(18) 0.33508(10) 0.0210(5) Uani 1 1 d . . . H19 H -0.2013 0.1194 0.3518 0.025 Uiso 1 1 calc R . . C20 C -0.03502(9) -0.0566(2) 0.05688(10) 0.0291(6) Uani 1 1 d . . . H20A H -0.0516 0.0112 0.0485 0.044 Uiso 1 1 calc R . . H20B H -0.0574 -0.1160 0.0491 0.044 Uiso 1 1 calc R . . H20C H -0.0088 -0.0636 0.0333 0.044 Uiso 1 1 calc R . . C21 C 0.00949(9) -0.16820(18) 0.13144(11) 0.0267(5) Uani 1 1 d . . . H21A H 0.0365 -0.1754 0.1091 0.040 Uiso 1 1 calc R . . H21B H -0.0134 -0.2258 0.1215 0.040 Uiso 1 1 calc R . . H21C H 0.0210 -0.1726 0.1716 0.040 Uiso 1 1 calc R . . C22 C 0.09417(8) 0.28330(17) 0.05261(9) 0.0177(4) Uani 1 1 d . . . C23 C 0.12764(9) 0.27217(18) 0.01395(9) 0.0229(5) Uani 1 1 d . . . H23 H 0.1565 0.2347 0.0245 0.028 Uiso 1 1 calc R . . C24 C 0.11893(10) 0.3154(2) -0.03959(10) 0.0298(6) Uani 1 1 d . . . H24 H 0.1419 0.3076 -0.0656 0.036 Uiso 1 1 calc R . . C25 C 0.07734(11) 0.3693(2) -0.05523(10) 0.0343(7) Uani 1 1 d . . . H25 H 0.0717 0.3994 -0.0919 0.041 Uiso 1 1 calc R . . C26 C 0.04350(10) 0.3801(2) -0.01791(11) 0.0335(6) Uani 1 1 d . . . H26 H 0.0146 0.4170 -0.0290 0.040 Uiso 1 1 calc R . . C27 C 0.05183(9) 0.33676(19) 0.03617(10) 0.0250(5) Uani 1 1 d . . . H27 H 0.0285 0.3439 0.0617 0.030 Uiso 1 1 calc R . . C28 C -0.15375(8) -0.23998(17) 0.23274(10) 0.0203(5) Uani 1 1 d . . . C29 C -0.17375(9) -0.27930(19) 0.18121(11) 0.0279(6) Uani 1 1 d . . . H29 H -0.1838 -0.2312 0.1515 0.033 Uiso 1 1 calc R . . C30 C -0.17912(11) -0.3887(2) 0.17290(13) 0.0393(7) Uani 1 1 d . . . H30 H -0.1927 -0.4151 0.1374 0.047 Uiso 1 1 calc R . . C31 C -0.16489(11) -0.4591(2) 0.21577(15) 0.0425(8) Uani 1 1 d . . . H31 H -0.1687 -0.5338 0.2099 0.051 Uiso 1 1 calc R . . C32 C -0.14519(10) -0.4211(2) 0.26720(14) 0.0386(7) Uani 1 1 d . . . H32 H -0.1354 -0.4699 0.2967 0.046 Uiso 1 1 calc R . . C33 C -0.13949(9) -0.31173(19) 0.27629(12) 0.0275(5) Uani 1 1 d . . . H33 H -0.1260 -0.2859 0.3119 0.033 Uiso 1 1 calc R . . C34 C 0.22552(8) 0.11714(17) 0.31002(9) 0.0177(4) Uani 1 1 d . . . H34 H 0.2385 0.0789 0.2809 0.021 Uiso 1 1 calc R . . C35 C 0.24890(8) 0.13248(17) 0.36455(9) 0.0193(5) Uani 1 1 d . . . H35 H 0.2797 0.1075 0.3784 0.023 Uiso 1 1 calc R . . C36 C 0.21849(8) 0.19064(17) 0.39395(9) 0.0178(4) Uani 1 1 d . . . H36 H 0.2242 0.2126 0.4322 0.021 Uiso 1 1 calc R . . C37 C 0.17696(8) 0.21169(16) 0.35645(9) 0.0152(4) Uani 1 1 d . . . C38 C 0.13752(8) 0.27502(16) 0.36585(9) 0.0153(4) Uani 1 1 d . . . C39 C 0.10086(8) 0.30152(16) 0.32450(9) 0.0151(4) Uani 1 1 d . . . C40 C 0.06529(8) 0.38272(16) 0.32620(9) 0.0160(4) Uani 1 1 d . . . H40 H 0.0598 0.4246 0.3580 0.019 Uiso 1 1 calc R . . C41 C 0.04065(7) 0.38905(16) 0.27350(9) 0.0145(4) Uani 1 1 d . . . C42 C 0.06062(7) 0.30874(16) 0.24108(9) 0.0154(4) Uani 1 1 d . . . H42 H 0.0498 0.2938 0.2028 0.018 Uiso 1 1 calc R . . C43 C 0.0000 0.4611(2) 0.2500 0.0167(6) Uani 1 2 d S . . C44 C -0.01590(8) 0.53242(18) 0.29675(11) 0.0248(5) Uani 1 1 d . . . H44A H -0.0267 0.4876 0.3265 0.037 Uiso 1 1 calc R . . H44B H -0.0421 0.5786 0.2811 0.037 Uiso 1 1 calc R . . H44C H 0.0110 0.5767 0.3125 0.037 Uiso 1 1 calc R . . C45 C 0.13451(8) 0.31812(17) 0.42383(9) 0.0164(4) Uani 1 1 d . . . C46 C 0.09603(8) 0.28973(19) 0.45233(10) 0.0228(5) Uani 1 1 d . . . H46 H 0.0716 0.2452 0.4345 0.027 Uiso 1 1 calc R . . C47 C 0.09307(9) 0.3261(2) 0.50684(11) 0.0296(6) Uani 1 1 d . . . H47 H 0.0670 0.3054 0.5264 0.036 Uiso 1 1 calc R . . C48 C 0.12827(10) 0.3925(2) 0.53270(10) 0.0299(6) Uani 1 1 d . . . H48 H 0.1262 0.4177 0.5699 0.036 Uiso 1 1 calc R . . C49 C 0.16614(9) 0.4220(2) 0.50457(10) 0.0266(5) Uani 1 1 d . . . H49 H 0.1901 0.4678 0.5223 0.032 Uiso 1 1 calc R . . C50 C 0.16951(8) 0.38505(18) 0.45035(10) 0.0206(5) Uani 1 1 d . . . H50 H 0.1959 0.4055 0.4312 0.025 Uiso 1 1 calc R . . N1 N 0.16061(6) 0.25212(13) 0.19828(7) 0.0143(4) Uani 1 1 d . . . N2 N 0.08292(6) 0.11454(13) 0.18275(7) 0.0138(4) Uani 1 1 d . . . N3 N -0.10609(6) 0.03822(13) 0.21039(7) 0.0139(4) Uani 1 1 d . . . N4 N -0.17008(6) 0.03672(14) 0.29275(7) 0.0155(4) Uani 1 1 d . . . N5 N 0.18246(6) 0.16376(13) 0.30461(7) 0.0152(4) Uani 1 1 d . . . N6 N 0.09619(6) 0.25690(13) 0.27058(7) 0.0143(4) Uani 1 1 d . . . Cl1 Cl 0.27786(3) 0.38085(7) 0.04426(4) 0.0552(2) Uani 1 1 d . . . Cl2 Cl 0.33791(4) 0.53517(8) -0.00466(4) 0.0636(3) Uani 1 1 d . . . Co1 Co 0.133219(10) 0.14418(2) 0.242432(12) 0.01271(8) Uani 1 1 d . . . C51 C 0.32914(12) 0.4613(2) 0.05538(12) 0.0429(7) Uani 1 1 d . . . H51A H 0.3259 0.5108 0.0871 0.051 Uiso 1 1 calc R . . H51B H 0.3573 0.4155 0.0658 0.051 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 C1 0.0177(11) 0.0171(10) 0.0189(11) 0.0001(8) -0.0016(9) -0.0015(8) C2 0.0198(11) 0.0177(11) 0.0242(12) 0.0001(9) 0.0027(9) -0.0054(9) C3 0.0212(11) 0.0147(10) 0.0181(11) 0.0015(8) 0.0026(9) -0.0034(8) C4 0.0179(10) 0.0126(9) 0.0143(10) 0.0006(8) 0.0029(8) -0.0005(8) C5 0.0177(10) 0.0136(9) 0.0135(10) -0.0016(8) 0.0042(8) -0.0005(8) C6 0.0175(10) 0.0166(10) 0.0113(10) -0.0022(8) 0.0027(8) -0.0003(8) C7 0.0179(11) 0.0210(10) 0.0130(10) -0.0041(8) 0.0036(8) -0.0038(8) C8 0.0166(10) 0.0192(10) 0.0144(10) -0.0051(8) 0.0063(8) -0.0036(8) C9 0.0176(11) 0.0148(10) 0.0157(10) -0.0016(8) 0.0057(9) -0.0019(8) C10 0.0214(11) 0.0200(11) 0.0157(11) -0.0047(8) 0.0053(9) -0.0077(9) C11 0.0199(11) 0.0162(10) 0.0115(10) 0.0008(8) 0.0032(8) -0.0041(8) C12 0.0178(10) 0.0166(10) 0.0113(10) -0.0021(8) 0.0010(8) -0.0032(8) C13 0.0195(11) 0.0147(10) 0.0170(11) -0.0036(8) 0.0039(9) -0.0032(8) C14 0.0178(11) 0.0140(10) 0.0146(10) -0.0012(8) 0.0020(8) -0.0017(8) C15 0.0162(10) 0.0135(10) 0.0168(10) 0.0012(8) 0.0005(8) -0.0014(8) C16 0.0153(10) 0.0133(9) 0.0154(10) 0.0018(8) 0.0007(8) -0.0008(8) C17 0.0159(10) 0.0192(11) 0.0197(11) 0.0031(8) 0.0026(9) -0.0021(8) C18 0.0211(12) 0.0257(12) 0.0201(12) 0.0009(9) 0.0087(9) -0.0032(9) C19 0.0222(12) 0.0214(11) 0.0201(11) -0.0028(9) 0.0055(9) -0.0015(9) C20 0.0316(14) 0.0401(14) 0.0158(12) -0.0075(10) 0.0042(10) -0.0184(11) C21 0.0254(13) 0.0209(11) 0.0360(14) -0.0102(10) 0.0128(11) -0.0050(9) C22 0.0230(11) 0.0156(10) 0.0137(10) -0.0005(8) -0.0022(9) -0.0075(8) C23 0.0307(13) 0.0202(11) 0.0183(11) -0.0025(9) 0.0042(10) -0.0086(9) C24 0.0462(16) 0.0269(12) 0.0169(12) -0.0017(10) 0.0062(11) -0.0164(12) C25 0.0603(19) 0.0257(13) 0.0144(12) 0.0033(10) -0.0072(12) -0.0160(12) C26 0.0418(16) 0.0218(12) 0.0325(14) 0.0024(10) -0.0159(12) -0.0016(11) C27 0.0295(13) 0.0240(12) 0.0205(12) -0.0005(9) -0.0021(10) -0.0037(10) C28 0.0183(11) 0.0143(10) 0.0302(13) -0.0005(9) 0.0111(10) -0.0015(8) C29 0.0333(14) 0.0212(12) 0.0316(14) -0.0047(10) 0.0150(11) -0.0081(10) C30 0.0495(18) 0.0278(14) 0.0458(17) -0.0159(12) 0.0290(15) -0.0162(12) C31 0.0438(17) 0.0155(12) 0.075(2) -0.0109(13) 0.0353(17) -0.0062(11) C32 0.0285(14) 0.0204(12) 0.069(2) 0.0146(13) 0.0173(14) 0.0038(11) C33 0.0199(12) 0.0213(12) 0.0423(15) 0.0062(11) 0.0073(11) 0.0001(9) C34 0.0179(11) 0.0150(10) 0.0206(11) 0.0016(8) 0.0038(9) 0.0013(8) C35 0.0181(11) 0.0181(10) 0.0208(11) 0.0031(9) -0.0020(9) 0.0008(8) C36 0.0208(11) 0.0157(10) 0.0160(11) 0.0019(8) -0.0018(9) 0.0007(8) C37 0.0182(10) 0.0137(9) 0.0135(10) 0.0019(8) 0.0004(8) -0.0007(8) C38 0.0193(11) 0.0122(9) 0.0141(10) 0.0005(8) 0.0010(8) -0.0006(8) C39 0.0174(10) 0.0130(10) 0.0149(10) 0.0000(8) 0.0013(8) -0.0005(8) C40 0.0170(10) 0.0140(10) 0.0169(11) -0.0032(8) 0.0006(8) 0.0014(8) C41 0.0146(10) 0.0114(9) 0.0171(10) 0.0006(8) -0.0010(8) -0.0015(8) C42 0.0165(10) 0.0150(10) 0.0143(10) 0.0006(8) -0.0004(8) -0.0008(8) C43 0.0158(15) 0.0123(13) 0.0210(16) 0.000 -0.0029(12) 0.000 C44 0.0198(12) 0.0184(11) 0.0345(14) -0.0085(10) -0.0051(10) 0.0054(9) C45 0.0206(11) 0.0150(9) 0.0130(10) 0.0008(8) -0.0015(8) 0.0046(8) C46 0.0210(12) 0.0269(12) 0.0200(12) -0.0020(9) 0.0000(9) -0.0003(9) C47 0.0299(14) 0.0384(14) 0.0220(12) -0.0004(10) 0.0092(11) 0.0033(11) C48 0.0368(15) 0.0382(14) 0.0139(11) -0.0072(10) 0.0003(11) 0.0089(12) C49 0.0288(13) 0.0271(12) 0.0220(12) -0.0072(10) -0.0052(10) 0.0028(10) C50 0.0216(12) 0.0208(11) 0.0193(11) -0.0008(9) 0.0009(9) 0.0004(9) N1 0.0155(9) 0.0122(8) 0.0151(9) -0.0001(7) 0.0019(7) -0.0001(7) N2 0.0155(9) 0.0139(8) 0.0123(9) -0.0017(6) 0.0029(7) -0.0002(7) N3 0.0167(9) 0.0115(8) 0.0137(9) 0.0009(6) 0.0020(7) -0.0012(7) N4 0.0172(9) 0.0143(8) 0.0151(9) 0.0004(7) 0.0027(7) -0.0007(7) N5 0.0172(9) 0.0142(8) 0.0143(9) 0.0009(7) 0.0017(7) 0.0009(7) N6 0.0171(9) 0.0111(8) 0.0148(9) -0.0004(7) 0.0022(7) 0.0004(7) Cl1 0.0388(4) 0.0624(5) 0.0672(6) 0.0093(4) 0.0188(4) 0.0112(4) Cl2 0.0790(7) 0.0598(5) 0.0506(5) 0.0146(4) 0.0008(5) -0.0083(5) Co1 0.01520(14) 0.01127(13) 0.01170(14) -0.00009(11) 0.00173(10) 0.00052(11) C51 0.055(2) 0.0395(16) 0.0336(16) -0.0027(13) 0.0020(14) 0.0109(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.337(3) . ? C1 C2 1.402(3) . ? C1 H1 0.9500 . ? C2 C3 1.371(3) . ? C2 H2 0.9500 . ? C3 C4 1.425(3) . ? C3 H3 0.9500 . ? C4 N1 1.393(3) . ? C4 C5 1.404(3) . ? C5 C6 1.388(3) . ? C5 C22 1.492(3) . ? C6 N2 1.402(3) . ? C6 C7 1.426(3) . ? C7 C8 1.368(3) . ? C7 H7 0.9500 . ? C8 C9 1.418(3) . ? C8 C10 1.513(3) . ? C9 N2 1.333(3) . ? C9 H9 0.9500 . ? C10 C12 1.519(3) . ? C10 C20 1.526(3) . ? C10 C21 1.548(3) . ? C11 N3 1.343(3) . ? C11 C12 1.414(3) . ? C11 H11 0.9500 . ? C12 C13 1.380(3) . ? C13 C14 1.422(3) . ? C13 H13 0.9500 . ? C14 N3 1.390(3) . ? C14 C15 1.402(3) . ? C15 C16 1.387(3) . ? C15 C28 1.496(3) . ? C16 N4 1.399(3) . ? C16 C17 1.424(3) . ? C17 C18 1.362(3) . ? C17 H17 0.9500 . ? C18 C19 1.412(3) . ? C18 H18 0.9500 . ? C19 N4 1.334(3) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.388(3) . ? C22 C23 1.398(3) . ? C23 C24 1.386(3) . ? C23 H23 0.9500 . ? C24 C25 1.370(4) . ? C24 H24 0.9500 . ? C25 C26 1.382(4) . ? C25 H25 0.9500 . ? C26 C27 1.397(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.387(3) . ? C28 C33 1.399(3) . ? C29 C30 1.389(3) . ? C29 H29 0.9500 . ? C30 C31 1.377(4) . ? C30 H30 0.9500 . ? C31 C32 1.376(4) . ? C31 H31 0.9500 . ? C32 C33 1.392(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N5 1.342(3) . ? C34 C35 1.408(3) . ? C34 H34 0.9500 . ? C35 C36 1.375(3) . ? C35 H35 0.9500 . ? C36 C37 1.420(3) . ? C36 H36 0.9500 . ? C37 N5 1.399(3) . ? C37 C38 1.404(3) . ? C38 C39 1.390(3) . ? C38 C45 1.497(3) . ? C39 N6 1.396(3) . ? C39 C40 1.432(3) . ? C40 C41 1.372(3) . ? C40 H40 0.9500 . ? C41 C42 1.422(3) . ? C41 C43 1.518(3) . ? C42 N6 1.331(3) . ? C42 H42 0.9500 . ? C43 C41 1.518(3) 2 ? C43 C44 1.534(3) . ? C43 C44 1.534(3) 2 ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.389(3) . ? C45 C50 1.394(3) . ? C46 C47 1.390(3) . ? C46 H46 0.9500 . ? C47 C48 1.388(4) . ? C47 H47 0.9500 . ? C48 C49 1.373(4) . ? C48 H48 0.9500 . ? C49 C50 1.388(3) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? N1 Co1 1.9263(17) . ? N2 Co1 1.9350(18) . ? N3 Co1 1.9497(17) 2 ? N4 Co1 1.9458(17) 2 ? N5 Co1 1.9356(18) . ? N6 Co1 1.9201(17) . ? Cl1 C51 1.760(3) . ? Cl2 C51 1.746(3) . ? Co1 N4 1.9458(17) 2 ? Co1 N3 1.9497(17) 2 ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.3(2) . . ? N1 C1 H1 124.4 . . ? C2 C1 H1 124.4 . . ? C3 C2 C1 106.73(19) . . ? C3 C2 H2 126.6 . . ? C1 C2 H2 126.6 . . ? C2 C3 C4 106.94(19) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? N1 C4 C5 124.44(19) . . ? N1 C4 C3 108.33(18) . . ? C5 C4 C3 127.1(2) . . ? C6 C5 C4 124.55(19) . . ? C6 C5 C22 118.69(19) . . ? C4 C5 C22 116.74(18) . . ? C5 C6 N2 123.67(19) . . ? C5 C6 C7 128.3(2) . . ? N2 C6 C7 107.94(18) . . ? C8 C7 C6 107.98(19) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? C7 C8 C9 105.64(18) . . ? C7 C8 C10 131.4(2) . . ? C9 C8 C10 122.86(19) . . ? N2 C9 C8 111.97(19) . . ? N2 C9 H9 124.0 . . ? C8 C9 H9 124.0 . . ? C8 C10 C12 109.96(17) . . ? C8 C10 C20 110.27(18) . . ? C12 C10 C20 110.12(19) . . ? C8 C10 C21 108.10(19) . . ? C12 C10 C21 109.99(18) . . ? C20 C10 C21 108.37(19) . . ? N3 C11 C12 112.05(18) . . ? N3 C11 H11 124.0 . . ? C12 C11 H11 124.0 . . ? C13 C12 C11 105.40(18) . . ? C13 C12 C10 127.35(19) . . ? C11 C12 C10 127.26(19) . . ? C12 C13 C14 107.58(18) . . ? C12 C13 H13 126.2 . . ? C14 C13 H13 126.2 . . ? N3 C14 C15 124.60(19) . . ? N3 C14 C13 108.80(18) . . ? C15 C14 C13 125.99(19) . . ? C16 C15 C14 125.12(19) . . ? C16 C15 C28 117.91(19) . . ? C14 C15 C28 116.94(19) . . ? C15 C16 N4 124.08(19) . . ? C15 C16 C17 127.16(19) . . ? N4 C16 C17 108.72(18) . . ? C18 C17 C16 106.93(19) . . ? C18 C17 H17 126.5 . . ? C16 C17 H17 126.5 . . ? C17 C18 C19 106.8(2) . . ? C17 C18 H18 126.6 . . ? C19 C18 H18 126.6 . . ? N4 C19 C18 111.5(2) . . ? N4 C19 H19 124.3 . . ? C18 C19 H19 124.3 . . ? C10 C20 H20A 109.5 . . ? C10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C10 C21 H21A 109.5 . . ? C10 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C10 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 118.9(2) . . ? C27 C22 C5 121.2(2) . . ? C23 C22 C5 119.8(2) . . ? C24 C23 C22 120.4(2) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.3(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.3(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C27 120.0(3) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C22 C27 C26 120.1(2) . . ? C22 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C33 119.2(2) . . ? C29 C28 C15 119.6(2) . . ? C33 C28 C15 121.2(2) . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 120.4(3) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 C30 120.0(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.4(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C28 119.7(3) . . ? C32 C33 H33 120.1 . . ? C28 C33 H33 120.1 . . ? N5 C34 C35 110.99(19) . . ? N5 C34 H34 124.5 . . ? C35 C34 H34 124.5 . . ? C36 C35 C34 106.80(19) . . ? C36 C35 H35 126.6 . . ? C34 C35 H35 126.6 . . ? C35 C36 C37 107.11(19) . . ? C35 C36 H36 126.4 . . ? C37 C36 H36 126.4 . . ? N5 C37 C38 123.33(19) . . ? N5 C37 C36 108.37(18) . . ? C38 C37 C36 128.2(2) . . ? C39 C38 C37 124.22(19) . . ? C39 C38 C45 117.28(19) . . ? C37 C38 C45 118.50(19) . . ? C38 C39 N6 123.23(19) . . ? C38 C39 C40 128.22(19) . . ? N6 C39 C40 108.28(18) . . ? C41 C40 C39 107.55(18) . . ? C41 C40 H40 126.2 . . ? C39 C40 H40 126.2 . . ? C40 C41 C42 105.52(18) . . ? C40 C41 C43 131.35(18) . . ? C42 C41 C43 123.13(17) . . ? N6 C42 C41 112.13(19) . . ? N6 C42 H42 123.9 . . ? C41 C42 H42 123.9 . . ? C41 C43 C41 107.1(2) 2 . ? C41 C43 C44 110.22(12) 2 . ? C41 C43 C44 110.21(12) . . ? C41 C43 C44 110.21(12) 2 2 ? C41 C43 C44 110.22(12) . 2 ? C44 C43 C44 108.8(3) . 2 ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 C50 119.0(2) . . ? C46 C45 C38 119.2(2) . . ? C50 C45 C38 121.9(2) . . ? C45 C46 C47 120.3(2) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C48 C47 C46 120.0(2) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C49 C48 C47 120.0(2) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 120.2(2) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C45 120.5(2) . . ? C49 C50 H50 119.8 . . ? C45 C50 H50 119.8 . . ? C1 N1 C4 106.69(17) . . ? C1 N1 Co1 125.82(15) . . ? C4 N1 Co1 127.40(14) . . ? C9 N2 C6 106.46(17) . . ? C9 N2 Co1 125.47(15) . . ? C6 N2 Co1 127.70(14) . . ? C11 N3 C14 106.17(17) . . ? C11 N3 Co1 126.74(14) . 2 ? C14 N3 Co1 126.64(14) . 2 ? C19 N4 C16 106.08(17) . . ? C19 N4 Co1 126.73(15) . 2 ? C16 N4 Co1 127.11(14) . 2 ? C34 N5 C37 106.71(18) . . ? C34 N5 Co1 125.87(15) . . ? C37 N5 Co1 126.41(14) . . ? C42 N6 C39 106.48(17) . . ? C42 N6 Co1 125.48(15) . . ? C39 N6 Co1 128.03(14) . . ? N6 Co1 N1 86.71(7) . . ? N6 Co1 N2 90.87(7) . . ? N1 Co1 N2 92.12(7) . . ? N6 Co1 N5 90.63(7) . . ? N1 Co1 N5 91.94(7) . . ? N2 Co1 N5 175.74(7) . . ? N6 Co1 N4 174.72(7) . 2 ? N1 Co1 N4 89.03(7) . 2 ? N2 Co1 N4 86.16(7) . 2 ? N5 Co1 N4 92.63(7) . 2 ? N6 Co1 N3 91.97(7) . 2 ? N1 Co1 N3 177.86(7) . 2 ? N2 Co1 N3 89.58(7) . 2 ? N5 Co1 N3 86.39(7) . 2 ? N4 Co1 N3 92.38(7) 2 2 ? Cl2 C51 Cl1 111.51(17) . . ? Cl2 C51 H51A 109.3 . . ? Cl1 C51 H51A 109.3 . . ? Cl2 C51 H51B 109.3 . . ? Cl1 C51 H51B 109.3 . . ? H51A C51 H51B 108.0 . . ? 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 N1 C1 C2 C3 1.1(3) . . . . ? C1 C2 C3 C4 -1.3(2) . . . . ? C2 C3 C4 N1 1.0(2) . . . . ? C2 C3 C4 C5 -174.4(2) . . . . ? N1 C4 C5 C6 0.6(3) . . . . ? C3 C4 C5 C6 175.3(2) . . . . ? N1 C4 C5 C22 -177.77(19) . . . . ? C3 C4 C5 C22 -3.0(3) . . . . ? C4 C5 C6 N2 2.5(3) . . . . ? C22 C5 C6 N2 -179.15(19) . . . . ? C4 C5 C6 C7 -174.7(2) . . . . ? C22 C5 C6 C7 3.6(3) . . . . ? C5 C6 C7 C8 177.1(2) . . . . ? N2 C6 C7 C8 -0.5(2) . . . . ? C6 C7 C8 C9 0.8(2) . . . . ? C6 C7 C8 C10 -174.9(2) . . . . ? C7 C8 C9 N2 -0.9(2) . . . . ? C10 C8 C9 N2 175.23(19) . . . . ? C7 C8 C10 C12 -119.5(3) . . . . ? C9 C8 C10 C12 65.4(3) . . . . ? C7 C8 C10 C20 2.1(3) . . . . ? C9 C8 C10 C20 -173.0(2) . . . . ? C7 C8 C10 C21 120.4(3) . . . . ? C9 C8 C10 C21 -54.7(3) . . . . ? N3 C11 C12 C13 0.8(2) . . . . ? N3 C11 C12 C10 -179.4(2) . . . . ? C8 C10 C12 C13 -153.1(2) . . . . ? C20 C10 C12 C13 85.2(3) . . . . ? C21 C10 C12 C13 -34.2(3) . . . . ? C8 C10 C12 C11 27.1(3) . . . . ? C20 C10 C12 C11 -94.6(3) . . . . ? C21 C10 C12 C11 146.0(2) . . . . ? C11 C12 C13 C14 -0.6(2) . . . . ? C10 C12 C13 C14 179.6(2) . . . . ? C12 C13 C14 N3 0.3(2) . . . . ? C12 C13 C14 C15 -171.0(2) . . . . ? N3 C14 C15 C16 -1.7(4) . . . . ? C13 C14 C15 C16 168.3(2) . . . . ? N3 C14 C15 C28 -179.6(2) . . . . ? C13 C14 C15 C28 -9.6(3) . . . . ? C14 C15 C16 N4 2.4(3) . . . . ? C28 C15 C16 N4 -179.7(2) . . . . ? C14 C15 C16 C17 -175.2(2) . . . . ? C28 C15 C16 C17 2.7(3) . . . . ? C15 C16 C17 C18 176.8(2) . . . . ? N4 C16 C17 C18 -1.1(2) . . . . ? C16 C17 C18 C19 0.9(3) . . . . ? C17 C18 C19 N4 -0.5(3) . . . . ? C6 C5 C22 C27 64.9(3) . . . . ? C4 C5 C22 C27 -116.7(2) . . . . ? C6 C5 C22 C23 -116.9(2) . . . . ? C4 C5 C22 C23 61.5(3) . . . . ? C27 C22 C23 C24 1.0(3) . . . . ? C5 C22 C23 C24 -177.2(2) . . . . ? C22 C23 C24 C25 -0.2(4) . . . . ? C23 C24 C25 C26 -0.6(4) . . . . ? C24 C25 C26 C27 0.6(4) . . . . ? C23 C22 C27 C26 -1.1(3) . . . . ? C5 C22 C27 C26 177.1(2) . . . . ? C25 C26 C27 C22 0.3(4) . . . . ? C16 C15 C28 C29 117.4(2) . . . . ? C14 C15 C28 C29 -64.5(3) . . . . ? C16 C15 C28 C33 -62.7(3) . . . . ? C14 C15 C28 C33 115.3(2) . . . . ? C33 C28 C29 C30 -0.6(4) . . . . ? C15 C28 C29 C30 179.3(2) . . . . ? C28 C29 C30 C31 0.3(4) . . . . ? C29 C30 C31 C32 0.0(4) . . . . ? C30 C31 C32 C33 0.0(4) . . . . ? C31 C32 C33 C28 -0.2(4) . . . . ? C29 C28 C33 C32 0.5(4) . . . . ? C15 C28 C33 C32 -179.3(2) . . . . ? N5 C34 C35 C36 0.4(2) . . . . ? C34 C35 C36 C37 -0.9(2) . . . . ? C35 C36 C37 N5 1.1(2) . . . . ? C35 C36 C37 C38 -174.8(2) . . . . ? N5 C37 C38 C39 -3.2(3) . . . . ? C36 C37 C38 C39 172.1(2) . . . . ? N5 C37 C38 C45 177.32(19) . . . . ? C36 C37 C38 C45 -7.4(3) . . . . ? C37 C38 C39 N6 8.4(3) . . . . ? C45 C38 C39 N6 -172.19(19) . . . . ? C37 C38 C39 C40 -165.0(2) . . . . ? C45 C38 C39 C40 14.5(3) . . . . ? C38 C39 C40 C41 172.2(2) . . . . ? N6 C39 C40 C41 -1.9(2) . . . . ? C39 C40 C41 C42 2.0(2) . . . . ? C39 C40 C41 C43 -178.8(2) . . . . ? C40 C41 C42 N6 -1.5(2) . . . . ? C43 C41 C42 N6 179.22(18) . . . . ? C40 C41 C43 C41 -123.6(3) . . . 2 ? C42 C41 C43 C41 55.45(17) . . . 2 ? C40 C41 C43 C44 -3.7(3) . . . . ? C42 C41 C43 C44 175.4(2) . . . . ? C40 C41 C43 C44 116.4(2) . . . 2 ? C42 C41 C43 C44 -64.5(3) . . . 2 ? C39 C38 C45 C46 61.1(3) . . . . ? C37 C38 C45 C46 -119.4(2) . . . . ? C39 C38 C45 C50 -119.6(2) . . . . ? C37 C38 C45 C50 59.8(3) . . . . ? C50 C45 C46 C47 -1.2(3) . . . . ? C38 C45 C46 C47 178.1(2) . . . . ? C45 C46 C47 C48 1.1(4) . . . . ? C46 C47 C48 C49 -0.3(4) . . . . ? C47 C48 C49 C50 -0.3(4) . . . . ? C48 C49 C50 C45 0.2(4) . . . . ? C46 C45 C50 C49 0.5(3) . . . . ? C38 C45 C50 C49 -178.7(2) . . . . ? C2 C1 N1 C4 -0.4(2) . . . . ? C2 C1 N1 Co1 176.36(14) . . . . ? C5 C4 N1 C1 175.2(2) . . . . ? C3 C4 N1 C1 -0.4(2) . . . . ? C5 C4 N1 Co1 -1.5(3) . . . . ? C3 C4 N1 Co1 -177.10(14) . . . . ? C8 C9 N2 C6 0.7(2) . . . . ? C8 C9 N2 Co1 -172.80(14) . . . . ? C5 C6 N2 C9 -177.8(2) . . . . ? C7 C6 N2 C9 -0.1(2) . . . . ? C5 C6 N2 Co1 -4.6(3) . . . . ? C7 C6 N2 Co1 173.14(14) . . . . ? C12 C11 N3 C14 -0.5(2) . . . . ? C12 C11 N3 Co1 172.11(14) . . . 2 ? C15 C14 N3 C11 171.6(2) . . . . ? C13 C14 N3 C11 0.1(2) . . . . ? C15 C14 N3 Co1 -1.0(3) . . . 2 ? C13 C14 N3 Co1 -172.54(14) . . . 2 ? C18 C19 N4 C16 -0.1(3) . . . . ? C18 C19 N4 Co1 -177.02(15) . . . 2 ? C15 C16 N4 C19 -177.3(2) . . . . ? C17 C16 N4 C19 0.7(2) . . . . ? C15 C16 N4 Co1 -0.4(3) . . . 2 ? C17 C16 N4 Co1 177.60(14) . . . 2 ? C35 C34 N5 C37 0.3(2) . . . . ? C35 C34 N5 Co1 -168.82(14) . . . . ? C38 C37 N5 C34 175.27(19) . . . . ? C36 C37 N5 C34 -0.8(2) . . . . ? C38 C37 N5 Co1 -15.7(3) . . . . ? C36 C37 N5 Co1 168.17(14) . . . . ? C41 C42 N6 C39 0.3(2) . . . . ? C41 C42 N6 Co1 -179.15(14) . . . . ? C38 C39 N6 C42 -173.5(2) . . . . ? C40 C39 N6 C42 1.0(2) . . . . ? C38 C39 N6 Co1 5.9(3) . . . . ? C40 C39 N6 Co1 -179.60(14) . . . . ? C42 N6 Co1 N1 70.31(18) . . . . ? C39 N6 Co1 N1 -109.03(18) . . . . ? C42 N6 Co1 N2 -21.77(18) . . . . ? C39 N6 Co1 N2 158.90(18) . . . . ? C42 N6 Co1 N5 162.21(17) . . . . ? C39 N6 Co1 N5 -17.12(18) . . . . ? C42 N6 Co1 N4 34.0(9) . . . 2 ? C39 N6 Co1 N4 -145.3(8) . . . 2 ? C42 N6 Co1 N3 -111.38(17) . . . 2 ? C39 N6 Co1 N3 69.29(18) . . . 2 ? C1 N1 Co1 N6 93.00(18) . . . . ? C4 N1 Co1 N6 -90.87(17) . . . . ? C1 N1 Co1 N2 -176.25(18) . . . . ? C4 N1 Co1 N2 -0.11(18) . . . . ? C1 N1 Co1 N5 2.48(18) . . . . ? C4 N1 Co1 N5 178.61(17) . . . . ? C1 N1 Co1 N4 -90.12(18) . . . 2 ? C4 N1 Co1 N4 86.01(17) . . . 2 ? C1 N1 Co1 N3 41(2) . . . 2 ? C4 N1 Co1 N3 -142.9(19) . . . 2 ? C9 N2 Co1 N6 -98.18(17) . . . . ? C6 N2 Co1 N6 89.76(17) . . . . ? C9 N2 Co1 N1 175.08(17) . . . . ? C6 N2 Co1 N1 3.02(17) . . . . ? C9 N2 Co1 N5 12.5(11) . . . . ? C6 N2 Co1 N5 -159.6(9) . . . . ? C9 N2 Co1 N4 86.19(17) . . . 2 ? C6 N2 Co1 N4 -85.87(17) . . . 2 ? C9 N2 Co1 N3 -6.22(17) . . . 2 ? C6 N2 Co1 N3 -178.28(17) . . . 2 ? C34 N5 Co1 N6 -171.39(18) . . . . ? C37 N5 Co1 N6 21.63(17) . . . . ? C34 N5 Co1 N1 -84.65(18) . . . . ? C37 N5 Co1 N1 108.36(17) . . . . ? C34 N5 Co1 N2 78.0(10) . . . . ? C37 N5 Co1 N2 -89.0(10) . . . . ? C34 N5 Co1 N4 4.46(18) . . . 2 ? C37 N5 Co1 N4 -162.52(17) . . . 2 ? C34 N5 Co1 N3 96.68(18) . . . 2 ? C37 N5 Co1 N3 -70.30(17) . . . 2 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.570 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.072 #===END data_Mn-helicate _database_code_depnum_ccdc_archive 'CCDC 815376' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C99 H78 Mn2 N12, (CH2Cl2)' _chemical_formula_sum 'C100 H80 Cl2 Mn2 N12' _chemical_formula_weight 1630.54 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' Mn Mn 0.3368 0.7283 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.649(5) _cell_length_b 11.6904(18) _cell_length_c 25.147(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.172(5) _cell_angle_gamma 90.00 _cell_volume 8510(2) _cell_formula_units_Z 4 _cell_measurement_temperature 103.0(1) _cell_measurement_reflns_used 7162 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 24.03 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6927 _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_sigmaI/netI 0.0951 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 24.11 _reflns_number_total 6927 _reflns_number_gt 5125 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ISOR SIMU DFIX 1.780 0.020 C51A CL3 DFIX 1.780 0.020 C51A CL4 DFIX 1.780 0.020 CL2 C51B DFIX 1.780 0.020 C51B CL1 DFIX 2.900 0.020 CL2 CL1 EQIV $2 -x+1/2, -y+1/2, -z+1 EQIV $1 -x, y, -z+1/2 FREE C51B CL2_$2 FREE C51B C51B_$2 FREE Cl1 Cl2_$2 FREE Cl3 Cl4_$2 FREE Cl2 C51B_$2 FREE Cl2 Cl1_$2 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^)+(0.0446P)^2^+27.3441P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6927 _refine_ls_number_parameters 568 _refine_ls_number_restraints 785 _refine_ls_R_factor_all 0.1051 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1314 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.15023(18) 0.7645(4) 0.1494(2) 0.0247(13) Uani 1 1 d U . . H1 H 0.1789 0.7718 0.1790 0.030 Uiso 1 1 calc R . . C2 C 0.14285(18) 0.6939(5) 0.1023(2) 0.0282(14) Uani 1 1 d U . . H2 H 0.1650 0.6474 0.0937 0.034 Uiso 1 1 calc R . . C3 C 0.09686(18) 0.7056(5) 0.0711(2) 0.0259(13) Uani 1 1 d U . . H3 H 0.0813 0.6669 0.0369 0.031 Uiso 1 1 calc R . . C4 C 0.07687(17) 0.7850(4) 0.0985(2) 0.0196(12) Uani 1 1 d U . . C5 C 0.03074(18) 0.8257(4) 0.0786(2) 0.0210(12) Uani 1 1 d U . . C6 C 0.01258(16) 0.9160(4) 0.1008(2) 0.0195(12) Uani 1 1 d U . . C7 C -0.03275(17) 0.9639(4) 0.0802(2) 0.0192(12) Uani 1 1 d U . . H7 H -0.0574 0.9383 0.0485 0.023 Uiso 1 1 calc R . . C8 C -0.03403(16) 1.0530(4) 0.11438(19) 0.0173(11) Uani 1 1 d U . . C9 C 0.01056(16) 1.0551(4) 0.1568(2) 0.0195(11) Uani 1 1 d U . . H9 H 0.0191 1.1077 0.1872 0.023 Uiso 1 1 calc R . . C10 C -0.07303(17) 1.1371(4) 0.1100(2) 0.0212(12) Uani 1 1 d U . . C11 C -0.08242(17) 1.0325(4) 0.1982(2) 0.0202(12) Uani 1 1 d U . . H11 H -0.0670 0.9641 0.1943 0.024 Uiso 1 1 calc R . . C12 C -0.08738(16) 1.1288(4) 0.1626(2) 0.0175(11) Uani 1 1 d U . . C13 C -0.11085(17) 1.2075(5) 0.1827(2) 0.0234(13) Uani 1 1 d U . . H13 H -0.1198 1.2817 0.1675 0.028 Uiso 1 1 calc R . . C14 C -0.11975(16) 1.1601(4) 0.2301(2) 0.0193(12) Uani 1 1 d U . . C15 C -0.14284(16) 1.2111(4) 0.2624(2) 0.0216(12) Uani 1 1 d U . . C16 C -0.15163(16) 1.1624(4) 0.3093(2) 0.0188(11) Uani 1 1 d U . . C17 C -0.17575(17) 1.2132(5) 0.3427(2) 0.0243(13) Uani 1 1 d U . . H17 H -0.1900 1.2864 0.3374 0.029 Uiso 1 1 calc R . . C18 C -0.17444(17) 1.1358(5) 0.3841(2) 0.0252(13) Uani 1 1 d U . . H18 H -0.1875 1.1455 0.4132 0.030 Uiso 1 1 calc R . . C19 C -0.15032(16) 1.0398(5) 0.3757(2) 0.0220(12) Uani 1 1 d U . . H19 H -0.1444 0.9736 0.3989 0.026 Uiso 1 1 calc R . . C20 C -0.11524(18) 1.1103(5) 0.0583(2) 0.0261(13) Uani 1 1 d U . . H20A H -0.1067 1.1168 0.0241 0.039 Uiso 1 1 calc R . . H20B H -0.1401 1.1646 0.0564 0.039 Uiso 1 1 calc R . . H20C H -0.1259 1.0323 0.0614 0.039 Uiso 1 1 calc R . . C21 C -0.05607(19) 1.2589(4) 0.1042(2) 0.0267(13) Uani 1 1 d U . . H21A H -0.0300 1.2779 0.1379 0.040 Uiso 1 1 calc R . . H21B H -0.0812 1.3134 0.1001 0.040 Uiso 1 1 calc R . . H21C H -0.0461 1.2628 0.0710 0.040 Uiso 1 1 calc R . . C22 C -0.00208(17) 0.7644(4) 0.02927(19) 0.0174(12) Uani 1 1 d U . . C23 C -0.02357(18) 0.8156(5) -0.0222(2) 0.0269(13) Uani 1 1 d U . . H23 H -0.0167 0.8932 -0.0276 0.032 Uiso 1 1 calc R . . C24 C -0.05472(18) 0.7569(5) -0.0660(2) 0.0304(14) Uani 1 1 d U . . H24 H -0.0687 0.7935 -0.1012 0.037 Uiso 1 1 calc R . . C25 C -0.0655(2) 0.6443(5) -0.0583(2) 0.0350(15) Uani 1 1 d U . . H25 H -0.0873 0.6038 -0.0881 0.042 Uiso 1 1 calc R . . C26 C -0.0448(2) 0.5920(5) -0.0080(2) 0.0385(16) Uani 1 1 d U . . H26 H -0.0522 0.5147 -0.0030 0.046 Uiso 1 1 calc R . . C27 C -0.01289(19) 0.6500(5) 0.0361(2) 0.0301(14) Uani 1 1 d U . . H27 H 0.0015 0.6122 0.0709 0.036 Uiso 1 1 calc R . . C28 C -0.16020(19) 1.3308(5) 0.2474(2) 0.0282(14) Uani 1 1 d U . . C29 C -0.2002(2) 1.3501(5) 0.2029(3) 0.0429(17) Uani 1 1 d U . . H29 H -0.2173 1.2877 0.1819 0.051 Uiso 1 1 calc R . . C30 C -0.2153(3) 1.4622(7) 0.1890(4) 0.066(2) Uani 1 1 d U . . H30 H -0.2431 1.4761 0.1589 0.079 Uiso 1 1 calc R . . C31 C -0.1903(3) 1.5519(6) 0.2184(4) 0.064(2) Uani 1 1 d U . . H31 H -0.2010 1.6278 0.2087 0.077 Uiso 1 1 calc R . . C32 C -0.1501(3) 1.5334(5) 0.2616(3) 0.057(2) Uani 1 1 d U . . H32 H -0.1326 1.5962 0.2816 0.068 Uiso 1 1 calc R . . C33 C -0.1349(2) 1.4218(5) 0.2763(3) 0.0407(15) Uani 1 1 d U . . H33 H -0.1070 1.4086 0.3063 0.049 Uiso 1 1 calc R . . C34 C 0.21656(17) 0.9638(4) 0.2728(2) 0.0273(13) Uani 1 1 d U . . H34 H 0.2223 0.9994 0.2418 0.033 Uiso 1 1 calc R . . C35 C 0.24658(19) 0.9711(5) 0.3287(2) 0.0351(15) Uani 1 1 d U . . H35 H 0.2752 1.0110 0.3415 0.042 Uiso 1 1 calc R . . C36 C 0.22684(18) 0.9101(5) 0.3609(2) 0.0289(14) Uani 1 1 d U . . H36 H 0.2387 0.9003 0.4006 0.035 Uiso 1 1 calc R . . C37 C 0.18482(17) 0.8638(4) 0.3236(2) 0.0216(12) Uani 1 1 d U . . C38 C 0.15205(17) 0.7966(4) 0.3366(2) 0.0216(12) Uani 1 1 d U . . C39 C 0.10921(17) 0.7626(4) 0.2989(2) 0.0199(12) Uani 1 1 d U . . C40 C 0.08051(17) 0.6756(4) 0.3085(2) 0.0189(12) Uani 1 1 d U . . H40 H 0.0868 0.6312 0.3418 0.023 Uiso 1 1 calc R . . C41 C 0.04183(17) 0.6664(4) 0.2613(2) 0.0216(12) Uani 1 1 d U . . C42 C 0.04770(16) 0.7508(4) 0.2244(2) 0.0202(12) Uani 1 1 d U . . H42 H 0.0257 0.7663 0.1884 0.024 Uiso 1 1 calc R . . C43 C 0.0000 0.5890(6) 0.2500 0.0234(17) Uani 1 2 d SU . . C44 C -0.0047(2) 0.5126(4) 0.1989(2) 0.0338(15) Uani 1 1 d U . . H44A H -0.0316 0.4623 0.1924 0.051 Uiso 1 1 calc R . . H44B H 0.0232 0.4663 0.2060 0.051 Uiso 1 1 calc R . . H44C H -0.0089 0.5606 0.1656 0.051 Uiso 1 1 calc R . . C45 C 0.16340(18) 0.7536(5) 0.3958(2) 0.0255(13) Uani 1 1 d U . . C46 C 0.13262(18) 0.7757(5) 0.4249(2) 0.0268(14) Uani 1 1 d U . . H46 H 0.1058 0.8206 0.4079 0.032 Uiso 1 1 calc R . . C47 C 0.1410(2) 0.7325(5) 0.4784(2) 0.0355(15) Uani 1 1 d U . . H47 H 0.1205 0.7501 0.4985 0.043 Uiso 1 1 calc R . . C48 C 0.1787(2) 0.6643(6) 0.5026(2) 0.0433(17) Uani 1 1 d U . . H48 H 0.1834 0.6323 0.5388 0.052 Uiso 1 1 calc R . . C49 C 0.2099(2) 0.6417(6) 0.4745(3) 0.0477(18) Uani 1 1 d U . . H49 H 0.2364 0.5959 0.4916 0.057 Uiso 1 1 calc R . . C50 C 0.2020(2) 0.6868(5) 0.4210(2) 0.0353(16) Uani 1 1 d U . . H50 H 0.2232 0.6717 0.4016 0.042 Uiso 1 1 calc R . . C51A C 0.2122(14) 0.372(6) 0.5131(12) 0.25(2) Uani 0.25 1 d PDU A 1 H51A H 0.1849 0.3291 0.5154 0.300 Uiso 0.25 1 calc PR A 1 H51B H 0.2062 0.4547 0.5133 0.300 Uiso 0.25 1 calc PR A 1 C51B C 0.249(3) 0.252(3) 0.472(3) 0.150(17) Uani 0.25 1 d PDU B 2 H51C H 0.2230 0.2190 0.4410 0.180 Uiso 0.25 1 calc PR B 2 H51D H 0.2724 0.1912 0.4873 0.180 Uiso 0.25 1 calc PR B 2 N1 N 0.11162(13) 0.8201(4) 0.14720(16) 0.0189(10) Uani 1 1 d U . . N2 N 0.03846(13) 0.9763(3) 0.14884(16) 0.0176(10) Uani 1 1 d U . . N3 N -0.10183(13) 1.0486(3) 0.23788(16) 0.0176(10) Uani 1 1 d U . . N4 N -0.13669(13) 1.0534(4) 0.33070(16) 0.0197(10) Uani 1 1 d U . . N5 N 0.17906(13) 0.9009(4) 0.26837(16) 0.0203(10) Uani 1 1 d U . . N6 N 0.08767(13) 0.8068(4) 0.24558(16) 0.0192(10) Uani 1 1 d U . . Mn1 Mn 0.10903(3) 0.93283(7) 0.20596(3) 0.0181(2) Uani 1 1 d U . . Cl1 Cl 0.2741(4) 0.3689(13) 0.4465(4) 0.127(5) Uani 0.25 1 d PDU B 2 Cl2 Cl 0.2304(11) 0.312(2) 0.5241(14) 0.264(14) Uani 0.25 1 d PDU . 2 Cl3 Cl 0.2632(5) 0.3320(12) 0.5684(11) 0.180(9) Uani 0.25 1 d PDU A 1 Cl4 Cl 0.2262(7) 0.3316(15) 0.4543(10) 0.176(8) Uani 0.25 1 d PDU . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(3) 0.029(3) 0.020(3) 0.000(3) 0.008(2) 0.008(3) C2 0.028(3) 0.029(3) 0.027(3) 0.000(3) 0.008(3) 0.014(3) C3 0.033(3) 0.025(3) 0.017(3) -0.003(2) 0.004(2) 0.000(3) C4 0.025(3) 0.019(3) 0.017(3) 0.000(2) 0.010(2) 0.001(2) C5 0.026(3) 0.017(3) 0.019(3) 0.005(2) 0.007(2) -0.001(3) C6 0.022(3) 0.019(3) 0.021(3) 0.006(2) 0.012(2) 0.003(2) C7 0.019(3) 0.017(3) 0.022(3) 0.002(2) 0.007(2) -0.001(2) C8 0.018(3) 0.016(3) 0.020(3) 0.001(2) 0.011(2) 0.000(2) C9 0.025(3) 0.012(3) 0.021(3) -0.004(2) 0.007(2) 0.001(3) C10 0.025(3) 0.022(3) 0.017(3) 0.005(2) 0.007(2) 0.002(3) C11 0.022(3) 0.014(3) 0.022(3) 0.002(2) 0.004(2) 0.003(2) C12 0.015(3) 0.018(3) 0.017(3) 0.002(2) 0.001(2) 0.000(2) C13 0.029(3) 0.021(3) 0.022(3) 0.011(3) 0.010(2) 0.008(3) C14 0.021(3) 0.016(3) 0.022(3) 0.002(2) 0.007(2) 0.003(2) C15 0.015(3) 0.027(3) 0.023(3) 0.001(3) 0.006(2) 0.001(2) C16 0.021(3) 0.021(3) 0.015(3) -0.002(2) 0.006(2) -0.001(2) C17 0.025(3) 0.025(3) 0.024(3) -0.003(3) 0.009(2) 0.000(3) C18 0.017(3) 0.040(4) 0.020(3) -0.004(3) 0.006(2) 0.004(3) C19 0.021(3) 0.026(3) 0.021(3) 0.004(2) 0.009(2) -0.002(2) C20 0.027(3) 0.024(3) 0.026(3) 0.007(2) 0.008(2) 0.013(3) C21 0.036(3) 0.023(3) 0.027(3) 0.002(3) 0.019(3) 0.008(3) C22 0.022(3) 0.016(3) 0.015(3) -0.006(2) 0.008(2) 0.004(2) C23 0.025(3) 0.027(3) 0.032(3) -0.002(3) 0.013(3) 0.003(3) C24 0.030(3) 0.042(4) 0.016(3) -0.007(3) 0.002(2) -0.001(3) C25 0.031(3) 0.033(4) 0.033(3) -0.012(3) 0.001(3) -0.004(3) C26 0.038(4) 0.024(4) 0.048(4) -0.018(3) 0.007(3) -0.006(3) C27 0.036(3) 0.022(3) 0.028(3) 0.001(3) 0.006(3) 0.001(3) C28 0.031(3) 0.028(3) 0.034(3) 0.005(3) 0.022(3) 0.006(3) C29 0.035(4) 0.040(4) 0.061(4) 0.021(3) 0.025(3) 0.015(3) C30 0.064(5) 0.060(6) 0.096(6) 0.044(5) 0.055(5) 0.039(4) C31 0.098(6) 0.025(4) 0.100(7) 0.035(5) 0.075(6) 0.029(5) C32 0.111(6) 0.023(4) 0.067(5) 0.005(4) 0.071(5) -0.004(4) C33 0.055(4) 0.027(4) 0.050(4) 0.005(3) 0.030(3) 0.000(3) C34 0.025(3) 0.026(3) 0.030(3) -0.001(3) 0.008(2) 0.001(3) C35 0.025(3) 0.039(4) 0.035(4) -0.006(3) 0.002(3) -0.003(3) C36 0.033(3) 0.033(4) 0.018(3) 0.001(3) 0.004(2) 0.008(3) C37 0.019(3) 0.024(3) 0.019(3) -0.004(2) 0.002(2) 0.011(2) C38 0.022(3) 0.021(3) 0.020(3) -0.006(2) 0.003(2) 0.007(2) C39 0.021(3) 0.022(3) 0.014(3) -0.001(2) 0.002(2) 0.008(2) C40 0.024(3) 0.020(3) 0.015(3) 0.002(2) 0.009(2) 0.007(2) C41 0.026(3) 0.014(3) 0.025(3) 0.001(2) 0.009(2) 0.008(2) C42 0.019(3) 0.022(3) 0.017(3) -0.005(2) 0.003(2) 0.008(2) C43 0.032(4) 0.012(4) 0.023(4) 0.000 0.005(3) 0.000 C44 0.034(3) 0.020(3) 0.049(4) -0.016(3) 0.014(3) -0.005(3) C45 0.023(3) 0.030(3) 0.020(3) -0.004(3) 0.002(2) 0.006(3) C46 0.021(3) 0.033(3) 0.022(3) -0.003(3) 0.001(2) 0.000(3) C47 0.033(4) 0.050(4) 0.021(3) -0.001(3) 0.005(3) 0.000(3) C48 0.045(4) 0.066(5) 0.017(3) 0.009(3) 0.006(3) 0.007(4) C49 0.039(4) 0.065(5) 0.034(4) 0.010(4) 0.004(3) 0.017(4) C50 0.034(4) 0.051(4) 0.020(3) 0.005(3) 0.007(3) 0.011(3) C51A 0.30(4) 0.14(4) 0.39(4) -0.05(4) 0.23(4) -0.13(3) C51B 0.17(3) 0.16(4) 0.18(3) -0.07(3) 0.15(3) 0.00(3) N1 0.020(2) 0.020(2) 0.016(2) -0.0007(19) 0.0060(18) 0.002(2) N2 0.020(2) 0.015(2) 0.015(2) -0.0003(18) 0.0018(18) 0.002(2) N3 0.017(2) 0.017(2) 0.017(2) 0.000(2) 0.0032(18) 0.003(2) N4 0.021(2) 0.020(2) 0.017(2) 0.005(2) 0.0050(18) 0.001(2) N5 0.018(2) 0.026(3) 0.017(2) -0.006(2) 0.0060(18) -0.001(2) N6 0.015(2) 0.020(2) 0.022(2) -0.002(2) 0.0052(19) 0.002(2) Mn1 0.0188(4) 0.0184(4) 0.0160(4) -0.0015(4) 0.0044(3) -0.0001(4) Cl1 0.080(7) 0.207(14) 0.085(7) 0.022(8) 0.014(6) 0.027(9) Cl2 0.27(3) 0.21(3) 0.41(3) -0.15(2) 0.24(2) -0.07(2) Cl3 0.105(10) 0.084(8) 0.41(3) -0.072(14) 0.162(15) -0.031(8) Cl4 0.212(19) 0.116(13) 0.240(19) -0.028(13) 0.128(16) -0.061(13) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.335(6) . ? C1 C2 1.400(7) . ? C1 H1 0.9500 . ? C2 C3 1.377(7) . ? C2 H2 0.9500 . ? C3 C4 1.411(7) . ? C3 H3 0.9500 . ? C4 N1 1.395(6) . ? C4 C5 1.418(7) . ? C5 C6 1.393(7) . ? C5 C22 1.498(7) . ? C6 N2 1.398(6) . ? C6 C7 1.428(6) . ? C7 C8 1.359(6) . ? C7 H7 0.9500 . ? C8 C9 1.431(6) . ? C8 C10 1.524(7) . ? C9 N2 1.316(6) . ? C9 H9 0.9500 . ? C10 C12 1.529(7) . ? C10 C20 1.536(7) . ? C10 C21 1.538(7) . ? C11 N3 1.332(6) . ? C11 C12 1.415(6) . ? C11 H11 0.9500 . ? C12 C13 1.363(7) . ? C13 C14 1.419(7) . ? C13 H13 0.9500 . ? C14 C15 1.377(7) . ? C14 N3 1.404(6) . ? C15 C16 1.413(7) . ? C15 C28 1.501(7) . ? C16 N4 1.400(6) . ? C16 C17 1.419(7) . ? C17 C18 1.370(7) . ? C17 H17 0.9500 . ? C18 C19 1.397(7) . ? C18 H18 0.9500 . ? C19 N4 1.338(6) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.381(7) . ? C22 C27 1.402(7) . ? C23 C24 1.380(7) . ? C23 H23 0.9500 . ? C24 C25 1.386(8) . ? C24 H24 0.9500 . ? C25 C26 1.359(8) . ? C25 H25 0.9500 . ? C26 C27 1.391(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.375(8) . ? C28 C29 1.380(8) . ? C29 C30 1.396(9) . ? C29 H29 0.9500 . ? C30 C31 1.363(10) . ? C30 H30 0.9500 . ? C31 C32 1.368(10) . ? C31 H31 0.9500 . ? C32 C33 1.393(8) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N5 1.338(6) . ? C34 C35 1.408(7) . ? C34 H34 0.9500 . ? C35 C36 1.361(7) . ? C35 H35 0.9500 . ? C36 C37 1.428(7) . ? C36 H36 0.9500 . ? C37 C38 1.397(7) . ? C37 N5 1.409(6) . ? C38 C39 1.401(7) . ? C38 C45 1.498(7) . ? C39 N6 1.386(6) . ? C39 C40 1.416(7) . ? C40 C41 1.380(7) . ? C40 H40 0.9500 . ? C41 C42 1.407(7) . ? C41 C43 1.518(6) . ? C42 N6 1.336(6) . ? C42 H42 0.9500 . ? C43 C41 1.518(6) 2 ? C43 C44 1.532(6) . ? C43 C44 1.532(6) 2 ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.385(7) . ? C45 C46 1.395(7) . ? C46 C47 1.379(7) . ? C46 H46 0.9500 . ? C47 C48 1.370(8) . ? C47 H47 0.9500 . ? C48 C49 1.391(8) . ? C48 H48 0.9500 . ? C49 C50 1.389(8) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51A Cl4 1.733(19) . ? C51A Cl3 1.78(2) . ? C51A H51A 0.9900 . ? C51A H51B 0.9900 . ? C51B Cl2 1.751(18) . ? C51B Cl1 1.780(19) . ? C51B H51C 0.9900 . ? C51B H51D 0.9900 . ? N1 Mn1 2.001(4) . ? N2 Mn1 2.227(4) . ? N3 Mn1 2.019(4) 2 ? N4 Mn1 2.017(4) 2 ? N5 Mn1 2.235(4) . ? N6 Mn1 2.005(4) . ? Mn1 N4 2.017(4) 2 ? Mn1 N3 2.019(4) 2 ? Cl2 Cl2 2.44(4) 7_556 ? Cl4 Cl3 2.05(2) 7_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.9(5) . . ? N1 C1 H1 124.5 . . ? C2 C1 H1 124.5 . . ? C3 C2 C1 106.0(5) . . ? C3 C2 H2 127.0 . . ? C1 C2 H2 127.0 . . ? C2 C3 C4 108.3(5) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? N1 C4 C3 107.1(4) . . ? N1 C4 C5 126.6(4) . . ? C3 C4 C5 126.2(5) . . ? C6 C5 C4 126.6(5) . . ? C6 C5 C22 116.5(4) . . ? C4 C5 C22 116.9(4) . . ? C5 C6 N2 122.7(4) . . ? C5 C6 C7 128.4(5) . . ? N2 C6 C7 108.9(4) . . ? C8 C7 C6 107.4(4) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? C7 C8 C9 105.4(4) . . ? C7 C8 C10 129.3(4) . . ? C9 C8 C10 125.2(4) . . ? N2 C9 C8 112.6(4) . . ? N2 C9 H9 123.7 . . ? C8 C9 H9 123.7 . . ? C8 C10 C12 109.8(4) . . ? C8 C10 C20 110.6(4) . . ? C12 C10 C20 108.6(4) . . ? C8 C10 C21 108.8(4) . . ? C12 C10 C21 110.1(4) . . ? C20 C10 C21 109.0(4) . . ? N3 C11 C12 112.3(4) . . ? N3 C11 H11 123.8 . . ? C12 C11 H11 123.8 . . ? C13 C12 C11 105.3(4) . . ? C13 C12 C10 127.9(4) . . ? C11 C12 C10 126.6(4) . . ? C12 C13 C14 108.5(4) . . ? C12 C13 H13 125.8 . . ? C14 C13 H13 125.8 . . ? C15 C14 N3 124.9(4) . . ? C15 C14 C13 127.2(5) . . ? N3 C14 C13 107.8(4) . . ? C14 C15 C16 126.5(5) . . ? C14 C15 C28 117.6(4) . . ? C16 C15 C28 115.9(4) . . ? N4 C16 C15 124.0(4) . . ? N4 C16 C17 108.8(4) . . ? C15 C16 C17 127.2(5) . . ? C18 C17 C16 106.4(5) . . ? C18 C17 H17 126.8 . . ? C16 C17 H17 126.8 . . ? C17 C18 C19 107.5(5) . . ? C17 C18 H18 126.3 . . ? C19 C18 H18 126.3 . . ? N4 C19 C18 111.1(5) . . ? N4 C19 H19 124.4 . . ? C18 C19 H19 124.4 . . ? C10 C20 H20A 109.5 . . ? C10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C10 C21 H21A 109.5 . . ? C10 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C10 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 118.0(5) . . ? C23 C22 C5 123.5(5) . . ? C27 C22 C5 118.4(5) . . ? C24 C23 C22 121.6(5) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 119.7(5) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 119.8(5) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.9(5) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C26 C27 C22 120.0(5) . . ? C26 C27 H27 120.0 . . ? C22 C27 H27 120.0 . . ? C33 C28 C29 119.9(6) . . ? C33 C28 C15 119.8(5) . . ? C29 C28 C15 120.2(5) . . ? C28 C29 C30 119.3(7) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C31 C30 C29 120.3(7) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.6(7) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C31 C32 C33 119.6(7) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C28 C33 C32 120.2(6) . . ? C28 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? N5 C34 C35 112.2(5) . . ? N5 C34 H34 123.9 . . ? C35 C34 H34 123.9 . . ? C36 C35 C34 106.9(5) . . ? C36 C35 H35 126.6 . . ? C34 C35 H35 126.6 . . ? C35 C36 C37 106.7(5) . . ? C35 C36 H36 126.6 . . ? C37 C36 H36 126.6 . . ? C38 C37 N5 122.5(4) . . ? C38 C37 C36 128.4(5) . . ? N5 C37 C36 109.0(5) . . ? C37 C38 C39 125.9(5) . . ? C37 C38 C45 118.1(4) . . ? C39 C38 C45 115.9(5) . . ? N6 C39 C38 126.3(5) . . ? N6 C39 C40 107.9(4) . . ? C38 C39 C40 125.8(5) . . ? C41 C40 C39 108.4(4) . . ? C41 C40 H40 125.8 . . ? C39 C40 H40 125.8 . . ? C40 C41 C42 104.7(4) . . ? C40 C41 C43 129.9(4) . . ? C42 C41 C43 125.3(4) . . ? N6 C42 C41 112.3(4) . . ? N6 C42 H42 123.9 . . ? C41 C42 H42 123.9 . . ? C41 C43 C41 106.8(5) . 2 ? C41 C43 C44 110.2(3) . . ? C41 C43 C44 110.4(3) 2 . ? C41 C43 C44 110.4(3) . 2 ? C41 C43 C44 110.2(3) 2 2 ? C44 C43 C44 108.7(6) . 2 ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 119.1(5) . . ? C50 C45 C38 121.9(5) . . ? C46 C45 C38 118.9(5) . . ? C47 C46 C45 120.2(5) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C48 C47 C46 120.5(6) . . ? C48 C47 H47 119.8 . . ? C46 C47 H47 119.8 . . ? C47 C48 C49 120.3(6) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C48 119.3(6) . . ? C50 C49 H49 120.3 . . ? C48 C49 H49 120.3 . . ? C45 C50 C49 120.6(6) . . ? C45 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? Cl4 C51A Cl3 101(2) . . ? Cl4 C51A H51A 111.5 . . ? Cl3 C51A H51A 111.5 . . ? Cl4 C51A H51B 111.5 . . ? Cl3 C51A H51B 111.5 . . ? H51A C51A H51B 109.3 . . ? Cl2 C51B Cl1 104.3(14) . . ? Cl2 C51B H51C 110.9 . . ? Cl1 C51B H51C 110.9 . . ? Cl2 C51B H51D 110.9 . . ? Cl1 C51B H51D 110.9 . . ? H51C C51B H51D 108.9 . . ? C1 N1 C4 107.7(4) . . ? C1 N1 Mn1 122.6(3) . . ? C4 N1 Mn1 129.6(3) . . ? C9 N2 C6 105.7(4) . . ? C9 N2 Mn1 127.1(3) . . ? C6 N2 Mn1 126.7(3) . . ? C11 N3 C14 106.1(4) . . ? C11 N3 Mn1 127.4(3) . 2 ? C14 N3 Mn1 126.4(3) . 2 ? C19 N4 C16 106.2(4) . . ? C19 N4 Mn1 126.8(4) . 2 ? C16 N4 Mn1 126.4(3) . 2 ? C34 N5 C37 105.1(4) . . ? C34 N5 Mn1 124.5(3) . . ? C37 N5 Mn1 121.6(3) . . ? C42 N6 C39 106.7(4) . . ? C42 N6 Mn1 124.6(3) . . ? C39 N6 Mn1 128.7(3) . . ? N1 Mn1 N6 88.96(16) . . ? N1 Mn1 N4 89.88(16) . 2 ? N6 Mn1 N4 174.49(16) . 2 ? N1 Mn1 N3 176.07(17) . 2 ? N6 Mn1 N3 90.93(16) . 2 ? N4 Mn1 N3 90.59(15) 2 2 ? N1 Mn1 N2 86.52(15) . . ? N6 Mn1 N2 94.69(15) . . ? N4 Mn1 N2 90.62(15) 2 . ? N3 Mn1 N2 89.57(15) 2 . ? N1 Mn1 N5 98.43(15) . . ? N6 Mn1 N5 85.59(15) . . ? N4 Mn1 N5 89.25(15) 2 . ? N3 Mn1 N5 85.48(15) 2 . ? N2 Mn1 N5 175.04(15) . . ? C51B Cl2 Cl2 18(3) . 7_556 ? C51A Cl4 Cl3 126(3) . 7_556 ? 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 N1 C1 C2 C3 -1.9(6) . . . . ? C1 C2 C3 C4 1.4(6) . . . . ? C2 C3 C4 N1 -0.6(6) . . . . ? C2 C3 C4 C5 176.4(5) . . . . ? N1 C4 C5 C6 6.7(8) . . . . ? C3 C4 C5 C6 -169.7(5) . . . . ? N1 C4 C5 C22 -172.3(5) . . . . ? C3 C4 C5 C22 11.3(8) . . . . ? C4 C5 C6 N2 -2.9(8) . . . . ? C22 C5 C6 N2 176.1(4) . . . . ? C4 C5 C6 C7 176.0(5) . . . . ? C22 C5 C6 C7 -5.0(8) . . . . ? C5 C6 C7 C8 -177.8(5) . . . . ? N2 C6 C7 C8 1.2(5) . . . . ? C6 C7 C8 C9 -2.0(5) . . . . ? C6 C7 C8 C10 176.7(5) . . . . ? C7 C8 C9 N2 2.2(6) . . . . ? C10 C8 C9 N2 -176.6(4) . . . . ? C7 C8 C10 C12 119.7(5) . . . . ? C9 C8 C10 C12 -61.8(6) . . . . ? C7 C8 C10 C20 -0.1(7) . . . . ? C9 C8 C10 C20 178.4(5) . . . . ? C7 C8 C10 C21 -119.8(5) . . . . ? C9 C8 C10 C21 58.7(6) . . . . ? N3 C11 C12 C13 0.6(6) . . . . ? N3 C11 C12 C10 -174.6(4) . . . . ? C8 C10 C12 C13 160.1(5) . . . . ? C20 C10 C12 C13 -78.9(6) . . . . ? C21 C10 C12 C13 40.4(7) . . . . ? C8 C10 C12 C11 -25.8(7) . . . . ? C20 C10 C12 C11 95.2(6) . . . . ? C21 C10 C12 C11 -145.6(5) . . . . ? C11 C12 C13 C14 0.4(6) . . . . ? C10 C12 C13 C14 175.5(4) . . . . ? C12 C13 C14 C15 -179.6(5) . . . . ? C12 C13 C14 N3 -1.2(6) . . . . ? N3 C14 C15 C16 1.5(8) . . . . ? C13 C14 C15 C16 179.6(5) . . . . ? N3 C14 C15 C28 -179.2(4) . . . . ? C13 C14 C15 C28 -1.1(8) . . . . ? C14 C15 C16 N4 1.6(8) . . . . ? C28 C15 C16 N4 -177.7(4) . . . . ? C14 C15 C16 C17 -179.3(5) . . . . ? C28 C15 C16 C17 1.4(7) . . . . ? N4 C16 C17 C18 1.0(5) . . . . ? C15 C16 C17 C18 -178.2(5) . . . . ? C16 C17 C18 C19 -0.4(6) . . . . ? C17 C18 C19 N4 -0.4(6) . . . . ? C6 C5 C22 C23 63.8(7) . . . . ? C4 C5 C22 C23 -117.2(6) . . . . ? C6 C5 C22 C27 -113.9(5) . . . . ? C4 C5 C22 C27 65.1(6) . . . . ? C27 C22 C23 C24 -0.2(8) . . . . ? C5 C22 C23 C24 -177.9(5) . . . . ? C22 C23 C24 C25 1.0(8) . . . . ? C23 C24 C25 C26 -1.0(9) . . . . ? C24 C25 C26 C27 0.2(9) . . . . ? C25 C26 C27 C22 0.6(9) . . . . ? C23 C22 C27 C26 -0.6(8) . . . . ? C5 C22 C27 C26 177.2(5) . . . . ? C14 C15 C28 C33 -98.0(6) . . . . ? C16 C15 C28 C33 81.4(6) . . . . ? C14 C15 C28 C29 78.7(6) . . . . ? C16 C15 C28 C29 -101.9(6) . . . . ? C33 C28 C29 C30 -2.2(9) . . . . ? C15 C28 C29 C30 -178.9(5) . . . . ? C28 C29 C30 C31 1.3(10) . . . . ? C29 C30 C31 C32 0.3(11) . . . . ? C30 C31 C32 C33 -1.0(10) . . . . ? C29 C28 C33 C32 1.6(8) . . . . ? C15 C28 C33 C32 178.3(5) . . . . ? C31 C32 C33 C28 0.0(9) . . . . ? N5 C34 C35 C36 -0.2(6) . . . . ? C34 C35 C36 C37 1.1(6) . . . . ? C35 C36 C37 C38 -178.9(5) . . . . ? C35 C36 C37 N5 -1.7(6) . . . . ? N5 C37 C38 C39 -3.6(8) . . . . ? C36 C37 C38 C39 173.4(5) . . . . ? N5 C37 C38 C45 174.9(4) . . . . ? C36 C37 C38 C45 -8.1(8) . . . . ? C37 C38 C39 N6 -13.7(8) . . . . ? C45 C38 C39 N6 167.8(5) . . . . ? C37 C38 C39 C40 165.4(5) . . . . ? C45 C38 C39 C40 -13.1(7) . . . . ? N6 C39 C40 C41 0.3(5) . . . . ? C38 C39 C40 C41 -179.0(5) . . . . ? C39 C40 C41 C42 -1.3(5) . . . . ? C39 C40 C41 C43 -178.4(5) . . . . ? C40 C41 C42 N6 2.0(6) . . . . ? C43 C41 C42 N6 179.3(4) . . . . ? C40 C41 C43 C41 119.6(6) . . . 2 ? C42 C41 C43 C41 -57.0(4) . . . 2 ? C40 C41 C43 C44 -120.4(5) . . . . ? C42 C41 C43 C44 63.0(6) . . . . ? C40 C41 C43 C44 -0.2(7) . . . 2 ? C42 C41 C43 C44 -176.8(5) . . . 2 ? C37 C38 C45 C50 -58.1(7) . . . . ? C39 C38 C45 C50 120.6(6) . . . . ? C37 C38 C45 C46 126.0(5) . . . . ? C39 C38 C45 C46 -55.3(7) . . . . ? C50 C45 C46 C47 0.8(8) . . . . ? C38 C45 C46 C47 176.8(5) . . . . ? C45 C46 C47 C48 -2.3(9) . . . . ? C46 C47 C48 C49 2.7(10) . . . . ? C47 C48 C49 C50 -1.5(10) . . . . ? C46 C45 C50 C49 0.4(9) . . . . ? C38 C45 C50 C49 -175.5(6) . . . . ? C48 C49 C50 C45 0.0(10) . . . . ? C2 C1 N1 C4 1.5(6) . . . . ? C2 C1 N1 Mn1 -178.1(3) . . . . ? C3 C4 N1 C1 -0.6(5) . . . . ? C5 C4 N1 C1 -177.6(5) . . . . ? C3 C4 N1 Mn1 179.0(3) . . . . ? C5 C4 N1 Mn1 2.0(8) . . . . ? C8 C9 N2 C6 -1.4(5) . . . . ? C8 C9 N2 Mn1 -174.2(3) . . . . ? C5 C6 N2 C9 179.2(4) . . . . ? C7 C6 N2 C9 0.1(5) . . . . ? C5 C6 N2 Mn1 -7.9(7) . . . . ? C7 C6 N2 Mn1 173.0(3) . . . . ? C12 C11 N3 C14 -1.3(5) . . . . ? C12 C11 N3 Mn1 174.1(3) . . . 2 ? C15 C14 N3 C11 179.9(5) . . . . ? C13 C14 N3 C11 1.5(5) . . . . ? C15 C14 N3 Mn1 4.4(7) . . . 2 ? C13 C14 N3 Mn1 -174.0(3) . . . 2 ? C18 C19 N4 C16 1.0(5) . . . . ? C18 C19 N4 Mn1 -170.5(3) . . . 2 ? C15 C16 N4 C19 178.0(5) . . . . ? C17 C16 N4 C19 -1.2(5) . . . . ? C15 C16 N4 Mn1 -10.4(7) . . . 2 ? C17 C16 N4 Mn1 170.4(3) . . . 2 ? C35 C34 N5 C37 -0.8(6) . . . . ? C35 C34 N5 Mn1 146.9(4) . . . . ? C38 C37 N5 C34 178.9(5) . . . . ? C36 C37 N5 C34 1.5(5) . . . . ? C38 C37 N5 Mn1 30.1(6) . . . . ? C36 C37 N5 Mn1 -147.4(3) . . . . ? C41 C42 N6 C39 -1.8(5) . . . . ? C41 C42 N6 Mn1 179.7(3) . . . . ? C38 C39 N6 C42 -179.8(5) . . . . ? C40 C39 N6 C42 1.0(5) . . . . ? C38 C39 N6 Mn1 -1.5(7) . . . . ? C40 C39 N6 Mn1 179.3(3) . . . . ? C1 N1 Mn1 N6 -94.1(4) . . . . ? C4 N1 Mn1 N6 86.4(4) . . . . ? C1 N1 Mn1 N4 80.5(4) . . . 2 ? C4 N1 Mn1 N4 -99.0(4) . . . 2 ? C1 N1 Mn1 N3 177(51) . . . 2 ? C4 N1 Mn1 N3 -2(3) . . . 2 ? C1 N1 Mn1 N2 171.2(4) . . . . ? C4 N1 Mn1 N2 -8.3(4) . . . . ? C1 N1 Mn1 N5 -8.7(4) . . . . ? C4 N1 Mn1 N5 171.8(4) . . . . ? C42 N6 Mn1 N1 -64.6(4) . . . . ? C39 N6 Mn1 N1 117.4(4) . . . . ? C42 N6 Mn1 N4 -142.4(16) . . . 2 ? C39 N6 Mn1 N4 39.5(19) . . . 2 ? C42 N6 Mn1 N3 111.5(4) . . . 2 ? C39 N6 Mn1 N3 -66.5(4) . . . 2 ? C42 N6 Mn1 N2 21.9(4) . . . . ? C39 N6 Mn1 N2 -156.2(4) . . . . ? C42 N6 Mn1 N5 -163.1(4) . . . . ? C39 N6 Mn1 N5 18.9(4) . . . . ? C9 N2 Mn1 N1 -177.3(4) . . . . ? C6 N2 Mn1 N1 11.3(4) . . . . ? C9 N2 Mn1 N6 94.0(4) . . . . ? C6 N2 Mn1 N6 -77.3(4) . . . . ? C9 N2 Mn1 N4 -87.5(4) . . . 2 ? C6 N2 Mn1 N4 101.2(4) . . . 2 ? C9 N2 Mn1 N3 3.1(4) . . . 2 ? C6 N2 Mn1 N3 -168.2(4) . . . 2 ? C9 N2 Mn1 N5 1(2) . . . . ? C6 N2 Mn1 N5 -170.4(17) . . . . ? C34 N5 Mn1 N1 97.0(4) . . . . ? C37 N5 Mn1 N1 -120.3(4) . . . . ? C34 N5 Mn1 N6 -174.7(4) . . . . ? C37 N5 Mn1 N6 -32.1(4) . . . . ? C34 N5 Mn1 N4 7.2(4) . . . 2 ? C37 N5 Mn1 N4 149.9(4) . . . 2 ? C34 N5 Mn1 N3 -83.5(4) . . . 2 ? C37 N5 Mn1 N3 59.2(4) . . . 2 ? C34 N5 Mn1 N2 -81.3(19) . . . . ? C37 N5 Mn1 N2 61(2) . . . . ? Cl1 C51B Cl2 Cl2 -125(10) . . . 7_556 ? Cl3 C51A Cl4 Cl3 66(4) . . . 7_556 ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 24.11 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.432 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.087 #===END data_Ga-helicate _database_code_depnum_ccdc_archive 'CCDC 815377' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H78 Ga2 N12' _chemical_formula_weight 1575.17 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.1300(7) _cell_length_b 12.8500(3) _cell_length_c 24.1340(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.9510(10) _cell_angle_gamma 90.00 _cell_volume 8691.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 103.0(1) _cell_measurement_reflns_used 9059 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 25.97 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.852 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8504 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.01 _reflns_number_total 8504 _reflns_number_gt 6463 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The material crystallizes with a mixture of disordered solvent occupying one site in the asymmetric unit. The mixture appears to contain both CH2Cl2 and CHCl3 however no reasonable model for each fragment was obtained. As a result the PLATON/SQUEEZE program was used to generate a 'solvent-free' data set. Additionally, one phenyl ring (C45 -- C50) is disordered in two orientations, using restraints on bond lengths and angles on the minor fragment. EADP C45 C45B EADP C48 C48B ISOR SIMU 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^)+(0.0550P)^2^+9.6878P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8504 _refine_ls_number_parameters 548 _refine_ls_number_restraints 894 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.011 _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 C1 C 0.20266(9) 0.31284(19) 0.20237(10) 0.0295(6) Uani 1 1 d U . . H1 H 0.2218 0.3086 0.2367 0.035 Uiso 1 1 calc R . . C2 C 0.21194(10) 0.3786(2) 0.15913(11) 0.0350(6) Uani 1 1 d U . . H2 H 0.2380 0.4254 0.1583 0.042 Uiso 1 1 calc R . . C3 C 0.17627(11) 0.36291(19) 0.11796(11) 0.0359(6) Uani 1 1 d U . . H3 H 0.1726 0.3981 0.0832 0.043 Uiso 1 1 calc R . . C4 C 0.14578(9) 0.28494(18) 0.13629(9) 0.0264(5) Uani 1 1 d U . . C5 C 0.10501(9) 0.24083(18) 0.10685(9) 0.0260(5) Uani 1 1 d U . . C6 C 0.07661(9) 0.16251(19) 0.12590(9) 0.0253(5) Uani 1 1 d U . . C7 C 0.03842(9) 0.1076(2) 0.09562(10) 0.0302(6) Uani 1 1 d U . . H7 H 0.0264 0.1208 0.0583 0.036 Uiso 1 1 calc R . . C8 C 0.02231(9) 0.0330(2) 0.12959(9) 0.0287(6) Uani 1 1 d U . . C9 C 0.05037(9) 0.0448(2) 0.18072(9) 0.0278(5) Uani 1 1 d U . . H9 H 0.0465 0.0036 0.2127 0.033 Uiso 1 1 calc R . . C10 C -0.01393(10) -0.0529(2) 0.11922(10) 0.0349(6) Uani 1 1 d U . . C11 C -0.07125(9) 0.05335(19) 0.17830(9) 0.0253(5) Uani 1 1 d U . . H11 H -0.0594 0.1201 0.1696 0.030 Uiso 1 1 calc R . . C12 C -0.05337(9) -0.04078(19) 0.15829(9) 0.0263(5) Uani 1 1 d U . . C13 C -0.08015(9) -0.1175(2) 0.18042(9) 0.0270(5) Uani 1 1 d U . . H13 H -0.0768 -0.1902 0.1749 0.032 Uiso 1 1 calc R . . C14 C -0.11353(8) -0.06906(18) 0.21280(9) 0.0230(5) Uani 1 1 d U . . C15 C -0.14626(8) -0.11903(18) 0.24501(9) 0.0242(5) Uani 1 1 d U . . C16 C -0.17569(8) -0.07075(18) 0.28077(9) 0.0223(5) Uani 1 1 d U . . C17 C -0.20941(8) -0.1199(2) 0.31310(10) 0.0273(5) Uani 1 1 d U . . H17 H -0.2162 -0.1922 0.3143 0.033 Uiso 1 1 calc R . . C18 C -0.22995(9) -0.0440(2) 0.34182(10) 0.0319(6) Uani 1 1 d U . . H18 H -0.2537 -0.0532 0.3671 0.038 Uiso 1 1 calc R . . C19 C -0.20954(9) 0.0507(2) 0.32717(10) 0.0287(5) Uani 1 1 d U . . H19 H -0.2178 0.1167 0.3413 0.034 Uiso 1 1 calc R . . C20 C -0.03606(12) -0.0490(3) 0.05911(11) 0.0586(10) Uani 1 1 d U . . H20A H -0.0526 0.0176 0.0524 0.088 Uiso 1 1 calc R . . H20B H -0.0589 -0.1062 0.0527 0.088 Uiso 1 1 calc R . . H20C H -0.0109 -0.0558 0.0337 0.088 Uiso 1 1 calc R . . C21 C 0.01131(11) -0.1587(2) 0.12972(14) 0.0499(8) Uani 1 1 d U . . H21A H 0.0386 -0.1633 0.1072 0.075 Uiso 1 1 calc R . . H21B H -0.0111 -0.2152 0.1194 0.075 Uiso 1 1 calc R . . H21C H 0.0225 -0.1647 0.1692 0.075 Uiso 1 1 calc R . . C22 C 0.09252(11) 0.2831(2) 0.04943(10) 0.0378(7) Uani 1 1 d U . . C23 C 0.12446(14) 0.2718(2) 0.00849(11) 0.0522(9) Uani 1 1 d U . . H23 H 0.1538 0.2363 0.0171 0.063 Uiso 1 1 calc R . . C24 C 0.11402(18) 0.3110(3) -0.04369(14) 0.0743(13) Uani 1 1 d U . . H24 H 0.1359 0.3015 -0.0712 0.089 Uiso 1 1 calc R . . C25 C 0.0742(2) 0.3616(3) -0.05623(16) 0.0754(13) Uani 1 1 d U . . H25 H 0.0681 0.3894 -0.0926 0.090 Uiso 1 1 calc R . . C26 C 0.04040(18) 0.3761(3) -0.01792(19) 0.0780(14) Uani 1 1 d U . . H26 H 0.0116 0.4127 -0.0279 0.094 Uiso 1 1 calc R . . C27 C 0.05028(14) 0.3344(2) 0.03674(14) 0.0578(10) Uani 1 1 d U . . H27 H 0.0280 0.3421 0.0638 0.069 Uiso 1 1 calc R . . C28 C -0.14927(9) -0.23461(19) 0.24047(11) 0.0287(5) Uani 1 1 d U . . C29 C -0.16363(10) -0.2812(2) 0.19036(12) 0.0397(7) Uani 1 1 d U . . H29 H -0.1716 -0.2396 0.1584 0.048 Uiso 1 1 calc R . . C30 C -0.16644(12) -0.3895(2) 0.18648(14) 0.0511(9) Uani 1 1 d U . . H30 H -0.1754 -0.4211 0.1516 0.061 Uiso 1 1 calc R . . C31 C -0.15639(11) -0.4505(2) 0.23232(16) 0.0510(9) Uani 1 1 d U . . H31 H -0.1591 -0.5240 0.2295 0.061 Uiso 1 1 calc R . . C32 C -0.14229(10) -0.4046(2) 0.28271(15) 0.0465(8) Uani 1 1 d U . . H32 H -0.1349 -0.4470 0.3145 0.056 Uiso 1 1 calc R . . C33 C -0.13882(9) -0.2978(2) 0.28746(12) 0.0343(6) Uani 1 1 d U . . H33 H -0.1294 -0.2670 0.3225 0.041 Uiso 1 1 calc R . . C34 C 0.22835(9) 0.13158(18) 0.31568(10) 0.0252(5) Uani 1 1 d U A . H34 H 0.2431 0.0927 0.2884 0.030 Uiso 1 1 calc R . . C35 C 0.24834(9) 0.14693(19) 0.37037(10) 0.0276(5) Uani 1 1 d U . . H35 H 0.2783 0.1218 0.3860 0.033 Uiso 1 1 calc R . . C36 C 0.21647(9) 0.20490(19) 0.39667(10) 0.0267(5) Uani 1 1 d U . . H36 H 0.2200 0.2274 0.4343 0.032 Uiso 1 1 calc R . . C37 C 0.17677(8) 0.22553(18) 0.35725(9) 0.0237(5) Uani 1 1 d U A . C38 C 0.13619(8) 0.28537(17) 0.36489(9) 0.0230(5) Uani 1 1 d U . . C39 C 0.10009(8) 0.31072(18) 0.32410(9) 0.0237(5) Uani 1 1 d U A . C40 C 0.06412(8) 0.38903(18) 0.32544(10) 0.0255(5) Uani 1 1 d U . . H40 H 0.0578 0.4299 0.3568 0.031 Uiso 1 1 calc R A . C41 C 0.04035(9) 0.39454(19) 0.27332(10) 0.0259(5) Uani 1 1 d U A . C42 C 0.06121(8) 0.31646(18) 0.24221(10) 0.0241(5) Uani 1 1 d U . . H42 H 0.0511 0.3010 0.2045 0.029 Uiso 1 1 calc R A . C43 C 0.0000 0.4644(3) 0.2500 0.0297(8) Uani 1 2 d SU . . C44 C -0.01686(10) 0.5338(2) 0.29616(13) 0.0430(7) Uani 1 1 d U A . H44A H -0.0432 0.5780 0.2808 0.065 Uiso 1 1 calc R . . H44B H 0.0096 0.5777 0.3113 0.065 Uiso 1 1 calc R . . H44C H -0.0278 0.4901 0.3258 0.065 Uiso 1 1 calc R . . C45 C 0.12994(17) 0.3263(3) 0.42164(14) 0.0250(7) Uani 0.805(6) 1 d PU A 1 C46 C 0.09182(14) 0.2901(3) 0.44929(14) 0.0432(11) Uani 0.805(6) 1 d PU A 1 H46 H 0.0690 0.2447 0.4309 0.052 Uiso 0.805(6) 1 calc PR A 1 C47 C 0.08716(17) 0.3203(4) 0.50360(17) 0.0589(14) Uani 0.805(6) 1 d PU A 1 H47 H 0.0615 0.2939 0.5225 0.071 Uiso 0.805(6) 1 calc PR A 1 C48 C 0.1192(2) 0.3879(4) 0.53049(16) 0.0509(11) Uani 0.805(6) 1 d PU A 1 H48 H 0.1156 0.4084 0.5677 0.061 Uiso 0.805(6) 1 calc PR A 1 C49 C 0.15578(17) 0.4250(4) 0.50360(18) 0.0406(11) Uani 0.805(6) 1 d PU A 1 H49 H 0.1778 0.4723 0.5220 0.049 Uiso 0.805(6) 1 calc PR A 1 C50 C 0.16162(16) 0.3948(3) 0.44917(16) 0.0311(9) Uani 0.805(6) 1 d PU A 1 H50 H 0.1876 0.4214 0.4309 0.037 Uiso 0.805(6) 1 calc PR A 1 N1 N 0.16321(7) 0.25579(15) 0.18967(8) 0.0243(4) Uani 1 1 d U . . N2 N 0.08275(7) 0.11957(16) 0.17915(8) 0.0244(4) Uani 1 1 d U . . N3 N -0.10693(7) 0.03810(15) 0.21091(7) 0.0232(4) Uani 1 1 d U . . N4 N -0.17700(7) 0.03610(15) 0.29087(8) 0.0233(4) Uani 1 1 d U . . N5 N 0.18592(7) 0.17865(15) 0.30683(8) 0.0246(4) Uani 1 1 d U . . N6 N 0.09656(7) 0.26685(15) 0.27119(8) 0.0226(4) Uani 1 1 d U A . Ga1 Ga 0.136260(9) 0.149341(19) 0.241129(10) 0.02128(9) Uani 1 1 d U . . C45B C 0.1333(6) 0.3094(9) 0.4267(4) 0.0250(7) Uani 0.195(6) 1 d PGU A 2 C46B C 0.1225(5) 0.2354(7) 0.4657(4) 0.035(4) Uani 0.195(6) 1 d PGU A 2 H46B H 0.1178 0.1648 0.4548 0.042 Uiso 0.195(6) 1 calc PR A 2 C47B C 0.1184(5) 0.2646(9) 0.5205(4) 0.050(5) Uani 0.195(6) 1 d PGU A 2 H47B H 0.1110 0.2140 0.5471 0.061 Uiso 0.195(6) 1 calc PR A 2 C48B C 0.1252(7) 0.3679(10) 0.5364(4) 0.0509(11) Uani 0.195(6) 1 d PGU A 2 H48B H 0.1225 0.3879 0.5739 0.061 Uiso 0.195(6) 1 calc PR A 2 C49B C 0.1361(7) 0.4419(7) 0.4974(6) 0.045(5) Uani 0.195(6) 1 d PGU A 2 H49B H 0.1407 0.5125 0.5083 0.054 Uiso 0.195(6) 1 calc PR A 2 C50B C 0.1401(6) 0.4127(8) 0.4426(5) 0.034(4) Uani 0.195(6) 1 d PGU A 2 H50B H 0.1475 0.4633 0.4159 0.041 Uiso 0.195(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0296(14) 0.0252(13) 0.0330(13) -0.0015(10) -0.0012(11) -0.0041(11) C2 0.0409(16) 0.0266(14) 0.0372(14) -0.0002(11) 0.0015(12) -0.0106(12) C3 0.0523(17) 0.0237(13) 0.0312(13) 0.0018(10) 0.0019(12) -0.0086(12) C4 0.0361(14) 0.0190(12) 0.0241(12) -0.0011(9) 0.0030(10) 0.0045(10) C5 0.0333(14) 0.0226(12) 0.0222(11) -0.0031(9) 0.0020(10) 0.0038(11) C6 0.0290(13) 0.0284(13) 0.0188(11) -0.0069(9) 0.0040(9) 0.0026(11) C7 0.0321(14) 0.0397(15) 0.0191(11) -0.0100(10) 0.0031(10) -0.0025(12) C8 0.0249(13) 0.0408(15) 0.0215(11) -0.0117(10) 0.0082(10) -0.0053(11) C9 0.0288(13) 0.0346(14) 0.0210(11) -0.0046(10) 0.0088(10) -0.0044(11) C10 0.0348(15) 0.0474(17) 0.0237(12) -0.0132(11) 0.0089(11) -0.0132(13) C11 0.0298(13) 0.0284(13) 0.0178(11) 0.0009(9) 0.0024(10) -0.0047(11) C12 0.0245(13) 0.0358(14) 0.0187(11) -0.0055(10) 0.0021(9) -0.0065(11) C13 0.0275(13) 0.0274(13) 0.0257(12) -0.0059(10) 0.0001(10) -0.0009(11) C14 0.0252(12) 0.0247(12) 0.0194(11) -0.0001(9) 0.0030(9) -0.0019(10) C15 0.0226(12) 0.0229(12) 0.0266(12) -0.0001(9) 0.0000(9) -0.0010(10) C16 0.0208(12) 0.0221(12) 0.0239(11) 0.0039(9) 0.0012(9) -0.0001(10) C17 0.0212(12) 0.0271(13) 0.0338(13) 0.0028(10) 0.0045(10) -0.0034(10) C18 0.0302(14) 0.0344(15) 0.0327(13) -0.0007(11) 0.0119(11) -0.0041(12) C19 0.0291(13) 0.0294(13) 0.0290(12) -0.0022(10) 0.0096(10) 0.0013(11) C20 0.057(2) 0.098(3) 0.0222(13) -0.0167(15) 0.0110(13) -0.048(2) C21 0.0448(18) 0.0451(18) 0.064(2) -0.0254(15) 0.0266(16) -0.0060(15) C22 0.0611(19) 0.0228(13) 0.0269(13) -0.0011(10) -0.0107(13) -0.0107(13) C23 0.084(2) 0.0462(18) 0.0272(14) -0.0033(13) 0.0090(15) -0.0246(17) C24 0.120(4) 0.067(3) 0.0343(18) 0.0047(17) -0.002(2) -0.033(3) C25 0.124(4) 0.051(2) 0.047(2) 0.0089(17) -0.017(2) -0.029(2) C26 0.100(3) 0.0371(19) 0.088(3) -0.0017(19) -0.047(3) 0.002(2) C27 0.079(3) 0.0416(18) 0.0471(18) -0.0082(14) -0.0270(17) 0.0079(17) C28 0.0222(12) 0.0235(13) 0.0416(14) -0.0033(11) 0.0094(11) -0.0009(10) C29 0.0387(16) 0.0368(16) 0.0459(16) -0.0076(12) 0.0170(13) -0.0095(13) C30 0.052(2) 0.0411(17) 0.065(2) -0.0256(16) 0.0320(17) -0.0205(15) C31 0.0399(18) 0.0244(15) 0.094(3) -0.0069(16) 0.0345(18) -0.0036(13) C32 0.0287(15) 0.0278(15) 0.085(2) 0.0101(15) 0.0176(15) 0.0082(12) C33 0.0244(14) 0.0288(14) 0.0500(16) 0.0054(12) 0.0058(12) 0.0022(11) C34 0.0242(12) 0.0234(13) 0.0280(12) -0.0002(9) 0.0026(10) 0.0017(10) C35 0.0242(12) 0.0259(13) 0.0320(12) 0.0011(10) -0.0025(10) 0.0016(11) C36 0.0296(13) 0.0256(13) 0.0244(12) 0.0025(10) -0.0008(10) -0.0019(11) C37 0.0275(13) 0.0196(12) 0.0239(11) 0.0008(9) 0.0011(10) 0.0000(10) C38 0.0235(12) 0.0205(12) 0.0252(11) -0.0033(9) 0.0030(9) -0.0024(10) C39 0.0266(13) 0.0211(12) 0.0235(11) -0.0031(9) 0.0019(10) -0.0031(10) C40 0.0230(13) 0.0198(12) 0.0336(13) -0.0060(10) 0.0015(10) 0.0015(10) C41 0.0221(12) 0.0233(12) 0.0318(12) -0.0020(10) -0.0014(10) -0.0020(10) C42 0.0210(12) 0.0253(12) 0.0256(12) 0.0009(9) -0.0007(9) -0.0002(10) C43 0.0198(17) 0.0246(18) 0.044(2) 0.000 -0.0031(15) 0.000 C44 0.0279(15) 0.0311(15) 0.068(2) -0.0164(13) -0.0086(13) 0.0058(12) C45 0.0278(15) 0.0232(17) 0.0236(13) -0.0006(11) 0.0009(11) 0.0066(13) C46 0.038(2) 0.057(3) 0.0356(19) -0.0086(17) 0.0125(16) -0.013(2) C47 0.057(3) 0.081(3) 0.043(2) -0.003(2) 0.025(2) -0.008(3) C48 0.061(3) 0.067(3) 0.0250(16) -0.0109(17) 0.0050(16) 0.015(2) C49 0.045(3) 0.044(2) 0.030(2) -0.0128(17) -0.0091(19) 0.009(2) C50 0.032(2) 0.032(2) 0.0284(18) -0.0056(15) -0.0020(17) 0.0017(18) N1 0.0259(11) 0.0204(10) 0.0266(10) 0.0013(8) 0.0029(8) 0.0030(9) N2 0.0241(11) 0.0282(11) 0.0214(9) -0.0039(8) 0.0047(8) 0.0008(9) N3 0.0283(11) 0.0244(10) 0.0170(9) 0.0014(8) 0.0026(8) -0.0028(9) N4 0.0245(11) 0.0233(10) 0.0224(10) 0.0000(8) 0.0038(8) 0.0018(8) N5 0.0259(11) 0.0263(11) 0.0213(10) -0.0009(8) 0.0008(8) 0.0017(9) N6 0.0231(10) 0.0213(10) 0.0236(10) -0.0022(8) 0.0023(8) 0.0007(8) Ga1 0.02239(14) 0.02125(14) 0.02021(13) -0.00158(10) 0.00189(9) 0.00069(11) C45B 0.0278(15) 0.0232(17) 0.0236(13) -0.0006(11) 0.0009(11) 0.0066(13) C46B 0.045(9) 0.033(7) 0.030(7) -0.001(6) 0.013(6) -0.010(7) C47B 0.063(10) 0.077(11) 0.014(6) -0.004(7) 0.017(7) -0.011(9) C48B 0.061(3) 0.067(3) 0.0250(16) -0.0109(17) 0.0050(16) 0.015(2) C49B 0.065(12) 0.034(8) 0.034(8) -0.005(6) -0.014(9) 0.027(9) C50B 0.047(10) 0.025(7) 0.028(7) 0.004(5) -0.015(7) 0.012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.343(3) . ? C1 C2 1.385(4) . ? C1 H1 0.9500 . ? C2 C3 1.365(4) . ? C2 H2 0.9500 . ? C3 C4 1.414(4) . ? C3 H3 0.9500 . ? C4 N1 1.390(3) . ? C4 C5 1.415(3) . ? C5 C6 1.388(3) . ? C5 C22 1.502(3) . ? C6 N2 1.396(3) . ? C6 C7 1.432(3) . ? C7 C8 1.364(4) . ? C7 H7 0.9500 . ? C8 C9 1.414(3) . ? C8 C10 1.509(4) . ? C9 N2 1.327(3) . ? C9 H9 0.9500 . ? C10 C12 1.525(3) . ? C10 C20 1.529(4) . ? C10 C21 1.545(4) . ? C11 N3 1.342(3) . ? C11 C12 1.411(3) . ? C11 H11 0.9500 . ? C12 C13 1.376(3) . ? C13 C14 1.416(3) . ? C13 H13 0.9500 . ? C14 N3 1.391(3) . ? C14 C15 1.410(3) . ? C15 C16 1.392(3) . ? C15 C28 1.491(3) . ? C16 N4 1.395(3) . ? C16 C17 1.427(3) . ? C17 C18 1.354(4) . ? C17 H17 0.9500 . ? C18 C19 1.405(4) . ? C18 H18 0.9500 . ? C19 N4 1.334(3) . ? C19 H19 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C27 1.370(4) . ? C22 C23 1.399(4) . ? C23 C24 1.365(5) . ? C23 H23 0.9500 . ? C24 C25 1.309(6) . ? C24 H24 0.9500 . ? C25 C26 1.394(6) . ? C25 H25 0.9500 . ? C26 C27 1.429(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.378(4) . ? C28 C33 1.405(4) . ? C29 C30 1.397(4) . ? C29 H29 0.9500 . ? C30 C31 1.365(5) . ? C30 H30 0.9500 . ? C31 C32 1.379(5) . ? C31 H31 0.9500 . ? C32 C33 1.380(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 N5 1.339(3) . ? C34 C35 1.403(3) . ? C34 H34 0.9500 . ? C35 C36 1.364(3) . ? C35 H35 0.9500 . ? C36 C37 1.428(3) . ? C36 H36 0.9500 . ? C37 C38 1.402(3) . ? C37 N5 1.401(3) . ? C38 C39 1.391(3) . ? C38 C45 1.492(4) . ? C38 C45B 1.532(9) . ? C39 N6 1.392(3) . ? C39 C40 1.429(3) . ? C40 C41 1.374(3) . ? C40 H40 0.9500 . ? C41 C42 1.411(3) . ? C41 C43 1.517(3) . ? C42 N6 1.328(3) . ? C42 H42 0.9500 . ? C43 C41 1.517(3) 2 ? C43 C44 1.534(3) 2 ? C43 C44 1.534(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.381(6) . ? C45 C46 1.391(5) . ? C46 C47 1.384(5) . ? C46 H46 0.9500 . ? C47 C48 1.373(7) . ? C47 H47 0.9500 . ? C48 C49 1.350(7) . ? C48 H48 0.9500 . ? C49 C50 1.393(5) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? N1 Ga1 2.0373(19) . ? N2 Ga1 2.0641(19) . ? N3 Ga1 2.0564(19) 2 ? N4 Ga1 2.0445(19) 2 ? N5 Ga1 2.0554(19) . ? N6 Ga1 2.0478(19) . ? Ga1 N4 2.0445(19) 2 ? Ga1 N3 2.0564(19) 2 ? C45B C46B 1.3900 . ? C45B C50B 1.3900 . ? C46B C47B 1.3900 . ? C46B H46B 0.9500 . ? C47B C48B 1.3900 . ? C47B H47B 0.9500 . ? C48B C49B 1.3900 . ? C48B H48B 0.9500 . ? C49B C50B 1.3900 . ? C49B H49B 0.9500 . ? C50B H50B 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 N1 C1 C2 111.5(2) . . ? N1 C1 H1 124.2 . . ? C2 C1 H1 124.2 . . ? C3 C2 C1 106.5(2) . . ? C3 C2 H2 126.8 . . ? C1 C2 H2 126.8 . . ? C2 C3 C4 107.7(2) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? N1 C4 C3 107.8(2) . . ? N1 C4 C5 124.3(2) . . ? C3 C4 C5 127.9(2) . . ? C6 C5 C4 126.1(2) . . ? C6 C5 C22 118.2(2) . . ? C4 C5 C22 115.7(2) . . ? C5 C6 N2 124.2(2) . . ? C5 C6 C7 128.1(2) . . ? N2 C6 C7 107.6(2) . . ? C8 C7 C6 108.3(2) . . ? C8 C7 H7 125.9 . . ? C6 C7 H7 125.9 . . ? C7 C8 C9 105.1(2) . . ? C7 C8 C10 132.0(2) . . ? C9 C8 C10 122.7(2) . . ? N2 C9 C8 112.6(2) . . ? N2 C9 H9 123.7 . . ? C8 C9 H9 123.7 . . ? C8 C10 C12 109.9(2) . . ? C8 C10 C20 110.3(2) . . ? C12 C10 C20 109.0(2) . . ? C8 C10 C21 108.8(2) . . ? C12 C10 C21 109.7(2) . . ? C20 C10 C21 109.2(3) . . ? N3 C11 C12 112.5(2) . . ? N3 C11 H11 123.8 . . ? C12 C11 H11 123.8 . . ? C13 C12 C11 104.9(2) . . ? C13 C12 C10 128.2(2) . . ? C11 C12 C10 126.8(2) . . ? C12 C13 C14 108.1(2) . . ? C12 C13 H13 125.9 . . ? C14 C13 H13 125.9 . . ? N3 C14 C15 124.4(2) . . ? N3 C14 C13 108.7(2) . . ? C15 C14 C13 126.9(2) . . ? C16 C15 C14 126.2(2) . . ? C16 C15 C28 117.2(2) . . ? C14 C15 C28 116.7(2) . . ? C15 C16 N4 124.9(2) . . ? C15 C16 C17 126.9(2) . . ? N4 C16 C17 108.1(2) . . ? C18 C17 C16 107.1(2) . . ? C18 C17 H17 126.4 . . ? C16 C17 H17 126.4 . . ? C17 C18 C19 107.1(2) . . ? C17 C18 H18 126.5 . . ? C19 C18 H18 126.5 . . ? N4 C19 C18 111.2(2) . . ? N4 C19 H19 124.4 . . ? C18 C19 H19 124.4 . . ? C10 C20 H20A 109.5 . . ? C10 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C10 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C10 C21 H21A 109.5 . . ? C10 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C10 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 119.3(3) . . ? C27 C22 C5 120.7(3) . . ? C23 C22 C5 120.0(3) . . ? C24 C23 C22 120.9(4) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 120.6(4) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 122.2(4) . . ? C24 C25 H25 118.9 . . ? C26 C25 H25 118.9 . . ? C25 C26 C27 118.2(4) . . ? C25 C26 H26 120.9 . . ? C27 C26 H26 120.9 . . ? C22 C27 C26 118.9(4) . . ? C22 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C29 C28 C33 118.8(2) . . ? C29 C28 C15 120.5(2) . . ? C33 C28 C15 120.6(2) . . ? C28 C29 C30 120.2(3) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 120.7(3) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 119.5(3) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C31 C32 C33 120.8(3) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C28 120.0(3) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? N5 C34 C35 111.5(2) . . ? N5 C34 H34 124.3 . . ? C35 C34 H34 124.3 . . ? C36 C35 C34 106.8(2) . . ? C36 C35 H35 126.6 . . ? C34 C35 H35 126.6 . . ? C35 C36 C37 107.4(2) . . ? C35 C36 H36 126.3 . . ? C37 C36 H36 126.3 . . ? C38 C37 N5 124.2(2) . . ? C38 C37 C36 127.8(2) . . ? N5 C37 C36 107.9(2) . . ? C39 C38 C37 126.1(2) . . ? C39 C38 C45 115.5(3) . . ? C37 C38 C45 118.4(3) . . ? C39 C38 C45B 123.0(7) . . ? C37 C38 C45B 110.5(7) . . ? C45 C38 C45B 9.9(6) . . ? C38 C39 N6 123.0(2) . . ? C38 C39 C40 128.6(2) . . ? N6 C39 C40 108.1(2) . . ? C41 C40 C39 107.7(2) . . ? C41 C40 H40 126.1 . . ? C39 C40 H40 126.1 . . ? C40 C41 C42 105.0(2) . . ? C40 C41 C43 131.2(2) . . ? C42 C41 C43 123.8(2) . . ? N6 C42 C41 112.8(2) . . ? N6 C42 H42 123.6 . . ? C41 C42 H42 123.6 . . ? C41 C43 C41 107.4(3) 2 . ? C41 C43 C44 110.07(14) 2 2 ? C41 C43 C44 110.20(14) . 2 ? C41 C43 C44 110.20(14) 2 . ? C41 C43 C44 110.07(14) . . ? C44 C43 C44 108.9(3) 2 . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 118.3(3) . . ? C50 C45 C38 123.0(4) . . ? C46 C45 C38 118.6(3) . . ? C47 C46 C45 120.0(4) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.9(4) . . ? C46 C47 H47 119.6 . . ? C48 C47 H47 119.6 . . ? C49 C48 C47 119.5(3) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 120.8(4) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C45 C50 C49 120.5(4) . . ? C45 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C1 N1 C4 106.4(2) . . ? C1 N1 Ga1 124.81(16) . . ? C4 N1 Ga1 128.77(16) . . ? C9 N2 C6 106.38(19) . . ? C9 N2 Ga1 124.95(16) . . ? C6 N2 Ga1 128.21(16) . . ? C11 N3 C14 105.81(19) . . ? C11 N3 Ga1 125.82(16) . 2 ? C14 N3 Ga1 127.49(15) . 2 ? C19 N4 C16 106.5(2) . . ? C19 N4 Ga1 125.91(16) . 2 ? C16 N4 Ga1 127.60(15) . 2 ? C34 N5 C37 106.48(19) . . ? C34 N5 Ga1 125.28(16) . . ? C37 N5 Ga1 125.81(16) . . ? C42 N6 C39 106.24(19) . . ? C42 N6 Ga1 125.01(16) . . ? C39 N6 Ga1 128.74(16) . . ? N1 Ga1 N4 89.85(8) . 2 ? N1 Ga1 N6 87.93(8) . . ? N4 Ga1 N6 177.78(8) 2 . ? N1 Ga1 N5 94.79(8) . . ? N4 Ga1 N5 93.21(8) 2 . ? N6 Ga1 N5 86.95(8) . . ? N1 Ga1 N3 176.68(8) . 2 ? N4 Ga1 N3 89.03(8) 2 2 ? N6 Ga1 N3 93.19(8) . 2 ? N5 Ga1 N3 88.40(8) . 2 ? N1 Ga1 N2 88.23(8) . . ? N4 Ga1 N2 89.53(8) 2 . ? N6 Ga1 N2 90.43(7) . . ? N5 Ga1 N2 175.92(8) . . ? N3 Ga1 N2 88.63(8) 2 . ? C46B C45B C50B 120.0 . . ? C46B C45B C38 123.6(7) . . ? C50B C45B C38 116.3(7) . . ? C47B C46B C45B 120.0 . . ? C47B C46B H46B 120.0 . . ? C45B C46B H46B 120.0 . . ? C46B C47B C48B 120.0 . . ? C46B C47B H47B 120.0 . . ? C48B C47B H47B 120.0 . . ? C49B C48B C47B 120.0 . . ? C49B C48B H48B 120.0 . . ? C47B C48B H48B 120.0 . . ? C48B C49B C50B 120.0 . . ? C48B C49B H49B 120.0 . . ? C50B C49B H49B 120.0 . . ? C49B C50B C45B 120.0 . . ? C49B C50B H50B 120.0 . . ? C45B C50B H50B 120.0 . . ? 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 N1 C1 C2 C3 0.9(3) . . . . ? C1 C2 C3 C4 -1.3(3) . . . . ? C2 C3 C4 N1 1.3(3) . . . . ? C2 C3 C4 C5 -177.7(2) . . . . ? N1 C4 C5 C6 -0.5(4) . . . . ? C3 C4 C5 C6 178.4(2) . . . . ? N1 C4 C5 C22 -179.6(2) . . . . ? C3 C4 C5 C22 -0.7(4) . . . . ? C4 C5 C6 N2 4.0(4) . . . . ? C22 C5 C6 N2 -176.9(2) . . . . ? C4 C5 C6 C7 -172.4(2) . . . . ? C22 C5 C6 C7 6.7(4) . . . . ? C5 C6 C7 C8 176.4(2) . . . . ? N2 C6 C7 C8 -0.5(3) . . . . ? C6 C7 C8 C9 1.1(3) . . . . ? C6 C7 C8 C10 -174.2(3) . . . . ? C7 C8 C9 N2 -1.4(3) . . . . ? C10 C8 C9 N2 174.4(2) . . . . ? C7 C8 C10 C12 -121.9(3) . . . . ? C9 C8 C10 C12 63.5(3) . . . . ? C7 C8 C10 C20 -1.8(4) . . . . ? C9 C8 C10 C20 -176.4(3) . . . . ? C7 C8 C10 C21 117.9(3) . . . . ? C9 C8 C10 C21 -56.7(3) . . . . ? N3 C11 C12 C13 0.0(3) . . . . ? N3 C11 C12 C10 178.3(2) . . . . ? C8 C10 C12 C13 -149.1(2) . . . . ? C20 C10 C12 C13 89.9(3) . . . . ? C21 C10 C12 C13 -29.5(3) . . . . ? C8 C10 C12 C11 32.9(3) . . . . ? C20 C10 C12 C11 -88.0(3) . . . . ? C21 C10 C12 C11 152.5(2) . . . . ? C11 C12 C13 C14 0.3(2) . . . . ? C10 C12 C13 C14 -178.0(2) . . . . ? C12 C13 C14 N3 -0.5(3) . . . . ? C12 C13 C14 C15 -176.6(2) . . . . ? N3 C14 C15 C16 -2.1(4) . . . . ? C13 C14 C15 C16 173.5(2) . . . . ? N3 C14 C15 C28 178.4(2) . . . . ? C13 C14 C15 C28 -6.1(4) . . . . ? C14 C15 C16 N4 -0.7(4) . . . . ? C28 C15 C16 N4 178.8(2) . . . . ? C14 C15 C16 C17 179.1(2) . . . . ? C28 C15 C16 C17 -1.3(4) . . . . ? C15 C16 C17 C18 179.8(2) . . . . ? N4 C16 C17 C18 -0.3(3) . . . . ? C16 C17 C18 C19 0.5(3) . . . . ? C17 C18 C19 N4 -0.5(3) . . . . ? C6 C5 C22 C27 64.1(3) . . . . ? C4 C5 C22 C27 -116.7(3) . . . . ? C6 C5 C22 C23 -116.9(3) . . . . ? C4 C5 C22 C23 62.3(3) . . . . ? C27 C22 C23 C24 0.0(4) . . . . ? C5 C22 C23 C24 -179.0(3) . . . . ? C22 C23 C24 C25 1.1(5) . . . . ? C23 C24 C25 C26 -1.3(6) . . . . ? C24 C25 C26 C27 0.4(6) . . . . ? C23 C22 C27 C26 -0.8(4) . . . . ? C5 C22 C27 C26 178.2(3) . . . . ? C25 C26 C27 C22 0.7(5) . . . . ? C16 C15 C28 C29 118.1(3) . . . . ? C14 C15 C28 C29 -62.3(3) . . . . ? C16 C15 C28 C33 -60.1(3) . . . . ? C14 C15 C28 C33 119.5(3) . . . . ? C33 C28 C29 C30 -1.6(4) . . . . ? C15 C28 C29 C30 -179.9(2) . . . . ? C28 C29 C30 C31 1.9(4) . . . . ? C29 C30 C31 C32 -1.5(5) . . . . ? C30 C31 C32 C33 0.9(4) . . . . ? C31 C32 C33 C28 -0.6(4) . . . . ? C29 C28 C33 C32 1.0(4) . . . . ? C15 C28 C33 C32 179.3(2) . . . . ? N5 C34 C35 C36 0.9(3) . . . . ? C34 C35 C36 C37 -0.4(3) . . . . ? C35 C36 C37 C38 -177.5(2) . . . . ? C35 C36 C37 N5 -0.2(3) . . . . ? N5 C37 C38 C39 -2.6(4) . . . . ? C36 C37 C38 C39 174.3(2) . . . . ? N5 C37 C38 C45 177.1(2) . . . . ? C36 C37 C38 C45 -6.0(4) . . . . ? N5 C37 C38 C45B 170.6(5) . . . . ? C36 C37 C38 C45B -12.5(6) . . . . ? C37 C38 C39 N6 9.3(4) . . . . ? C45 C38 C39 N6 -170.3(2) . . . . ? C45B C38 C39 N6 -163.0(6) . . . . ? C37 C38 C39 C40 -164.3(2) . . . . ? C45 C38 C39 C40 16.1(4) . . . . ? C45B C38 C39 C40 23.4(6) . . . . ? C38 C39 C40 C41 172.3(2) . . . . ? N6 C39 C40 C41 -2.0(3) . . . . ? C39 C40 C41 C42 2.3(3) . . . . ? C39 C40 C41 C43 -178.4(2) . . . . ? C40 C41 C42 N6 -1.9(3) . . . . ? C43 C41 C42 N6 178.7(2) . . . . ? C40 C41 C43 C41 -124.0(3) . . . 2 ? C42 C41 C43 C41 55.23(19) . . . 2 ? C40 C41 C43 C44 116.1(3) . . . 2 ? C42 C41 C43 C44 -64.7(3) . . . 2 ? C40 C41 C43 C44 -4.0(4) . . . . ? C42 C41 C43 C44 175.2(2) . . . . ? C39 C38 C45 C50 -118.3(5) . . . . ? C37 C38 C45 C50 62.1(5) . . . . ? C45B C38 C45 C50 100(5) . . . . ? C39 C38 C45 C46 65.0(4) . . . . ? C37 C38 C45 C46 -114.6(4) . . . . ? C45B C38 C45 C46 -76(4) . . . . ? C50 C45 C46 C47 -1.9(7) . . . . ? C38 C45 C46 C47 174.9(4) . . . . ? C45 C46 C47 C48 1.5(8) . . . . ? C46 C47 C48 C49 -0.2(8) . . . . ? C47 C48 C49 C50 -0.6(8) . . . . ? C46 C45 C50 C49 1.1(7) . . . . ? C38 C45 C50 C49 -175.6(3) . . . . ? C48 C49 C50 C45 0.2(7) . . . . ? C2 C1 N1 C4 -0.1(3) . . . . ? C2 C1 N1 Ga1 -179.82(17) . . . . ? C3 C4 N1 C1 -0.7(3) . . . . ? C5 C4 N1 C1 178.3(2) . . . . ? C3 C4 N1 Ga1 178.96(17) . . . . ? C5 C4 N1 Ga1 -2.0(3) . . . . ? C8 C9 N2 C6 1.1(3) . . . . ? C8 C9 N2 Ga1 -171.72(16) . . . . ? C5 C6 N2 C9 -177.4(2) . . . . ? C7 C6 N2 C9 -0.3(3) . . . . ? C5 C6 N2 Ga1 -4.9(3) . . . . ? C7 C6 N2 Ga1 172.15(16) . . . . ? C12 C11 N3 C14 -0.3(3) . . . . ? C12 C11 N3 Ga1 169.60(15) . . . 2 ? C15 C14 N3 C11 176.7(2) . . . . ? C13 C14 N3 C11 0.5(2) . . . . ? C15 C14 N3 Ga1 7.0(3) . . . 2 ? C13 C14 N3 Ga1 -169.19(15) . . . 2 ? C18 C19 N4 C16 0.3(3) . . . . ? C18 C19 N4 Ga1 -178.16(16) . . . 2 ? C15 C16 N4 C19 179.9(2) . . . . ? C17 C16 N4 C19 0.0(3) . . . . ? C15 C16 N4 Ga1 -1.7(3) . . . 2 ? C17 C16 N4 Ga1 178.41(15) . . . 2 ? C35 C34 N5 C37 -1.0(3) . . . . ? C35 C34 N5 Ga1 -164.04(16) . . . . ? C38 C37 N5 C34 178.1(2) . . . . ? C36 C37 N5 C34 0.7(3) . . . . ? C38 C37 N5 Ga1 -18.9(3) . . . . ? C36 C37 N5 Ga1 163.66(16) . . . . ? C41 C42 N6 C39 0.7(3) . . . . ? C41 C42 N6 Ga1 -179.54(16) . . . . ? C38 C39 N6 C42 -173.9(2) . . . . ? C40 C39 N6 C42 0.8(3) . . . . ? C38 C39 N6 Ga1 6.4(3) . . . . ? C40 C39 N6 Ga1 -178.96(16) . . . . ? C1 N1 Ga1 N4 -89.8(2) . . . 2 ? C4 N1 Ga1 N4 90.6(2) . . . 2 ? C1 N1 Ga1 N6 90.2(2) . . . . ? C4 N1 Ga1 N6 -89.5(2) . . . . ? C1 N1 Ga1 N5 3.4(2) . . . . ? C4 N1 Ga1 N5 -176.23(19) . . . . ? C1 N1 Ga1 N3 -160.1(13) . . . 2 ? C4 N1 Ga1 N3 20.2(14) . . . 2 ? C1 N1 Ga1 N2 -179.3(2) . . . . ? C4 N1 Ga1 N2 1.0(2) . . . . ? C42 N6 Ga1 N1 66.87(19) . . . . ? C39 N6 Ga1 N1 -113.4(2) . . . . ? C42 N6 Ga1 N4 68(2) . . . 2 ? C39 N6 Ga1 N4 -113(2) . . . 2 ? C42 N6 Ga1 N5 161.78(19) . . . . ? C39 N6 Ga1 N5 -18.5(2) . . . . ? C42 N6 Ga1 N3 -109.99(19) . . . 2 ? C39 N6 Ga1 N3 69.8(2) . . . 2 ? C42 N6 Ga1 N2 -21.34(19) . . . . ? C39 N6 Ga1 N2 158.4(2) . . . . ? C34 N5 Ga1 N1 -88.5(2) . . . . ? C37 N5 Ga1 N1 111.62(19) . . . . ? C34 N5 Ga1 N4 1.6(2) . . . 2 ? C37 N5 Ga1 N4 -158.26(19) . . . 2 ? C34 N5 Ga1 N6 -176.2(2) . . . . ? C37 N5 Ga1 N6 23.96(19) . . . . ? C34 N5 Ga1 N3 90.6(2) . . . 2 ? C37 N5 Ga1 N3 -69.32(19) . . . 2 ? C34 N5 Ga1 N2 133.9(10) . . . . ? C37 N5 Ga1 N2 -26.0(12) . . . . ? C9 N2 Ga1 N1 173.45(19) . . . . ? C6 N2 Ga1 N1 2.25(19) . . . . ? C9 N2 Ga1 N4 83.58(19) . . . 2 ? C6 N2 Ga1 N4 -87.62(19) . . . 2 ? C9 N2 Ga1 N6 -98.64(19) . . . . ? C6 N2 Ga1 N6 90.16(19) . . . . ? C9 N2 Ga1 N5 -48.8(12) . . . . ? C6 N2 Ga1 N5 140.0(10) . . . . ? C9 N2 Ga1 N3 -5.46(19) . . . 2 ? C6 N2 Ga1 N3 -176.7(2) . . . 2 ? C39 C38 C45B C46B 102.2(10) . . . . ? C37 C38 C45B C46B -71.1(11) . . . . ? C45 C38 C45B C46B 144(5) . . . . ? C39 C38 C45B C50B -74.9(9) . . . . ? C37 C38 C45B C50B 111.7(8) . . . . ? C45 C38 C45B C50B -33(4) . . . . ? C50B C45B C46B C47B 0.0 . . . . ? C38 C45B C46B C47B -177.1(15) . . . . ? C45B C46B C47B C48B 0.0 . . . . ? C46B C47B C48B C49B 0.0 . . . . ? C47B C48B C49B C50B 0.0 . . . . ? C48B C49B C50B C45B 0.0 . . . . ? C46B C45B C50B C49B 0.0 . . . . ? C38 C45B C50B C49B 177.3(14) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.716 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.064 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.250 0.000 293 114 ' ' 2 0.250 -0.250 0.500 293 113 ' ' 3 0.750 0.250 0.500 293 113 ' ' 4 0.750 -0.250 1.000 293 114 ' ' _platon_squeeze_details ; ; #===END