# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'David Dolphin' _publ_contact_author_email DAVID.DOLPHIN@UBC.CA _publ_section_title ; A Triple-Stranded Helicate and Mesocate from the Same Metal and Ligand ; loop_ _publ_author_name 'David Dolphin' 'Zhan Zhang.' # Attachment 'FeHex.cif' data_FeHex _database_code_depnum_ccdc_archive 'CCDC 710490' _audit_update_record ; 2009-09-03 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H96.50 Cl6.50 Fe2 N12' _chemical_formula_weight 1616.36 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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3137(10) _cell_length_b 17.3134(14) _cell_length_c 18.8476(15) _cell_angle_alpha 88.243(4) _cell_angle_beta 72.590(4) _cell_angle_gamma 80.864(4) _cell_volume 4092.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 8674 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.94 _exptl_crystal_description column _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1694 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.884 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(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 81561 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.10 _reflns_number_total 19584 _reflns_number_gt 14380 _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. There appears to be two disordered ethyl substituents, in each case the disorder is modeled in two orientations. The material also crystallizes with methylene chloride in the lattice. There are three solvent molecules free in the asymmetric unit, including one that is disordered in two orientations. There is one final site that is partially occupied with solvent. In this case it occupies a site that is otherwise occupied by one disordered ethyl fragment. In total there are 3.13 solvent molecules in the asymmetric unit, or roughly 6.25 methylene chloride molecules in the unit cell. DFIX, SADI, EADP and EXYZ statements were used to maintain reasonable geometries for disordered fragments. ISOR, EADP and SIMU statements were used to maintain reasonable anisotropic displacement parameters. ; _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^)+(0.0671P)^2^+6.3652P] 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 19584 _refine_ls_number_parameters 1020 _refine_ls_number_restraints 1400 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1570 _refine_ls_wR_factor_gt 0.1338 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 1.920 _refine_ls_shift/su_mean 0.014 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 0.5917(3) 0.34443(16) 0.15770(16) 0.0325(6) Uani 1 1 d U A . H1 H 0.6602 0.3278 0.1238 0.039 Uiso 1 1 calc R . . C2 C 0.4974(3) 0.36129(17) 0.13633(17) 0.0373(7) Uani 1 1 d DU . . C3 C 0.4162(3) 0.38277(16) 0.20052(18) 0.0338(6) Uani 1 1 d U A . C4 C 0.4642(2) 0.37815(15) 0.25953(16) 0.0271(6) Uani 1 1 d U . . C5 C 0.4139(2) 0.39386(15) 0.33375(16) 0.0281(6) Uani 1 1 d U A . H5 H 0.3385 0.4071 0.3476 0.034 Uiso 1 1 calc R . . C6 C 0.4596(2) 0.39273(14) 0.39093(15) 0.0239(5) Uani 1 1 d U . . C7 C 0.4064(2) 0.40905(15) 0.46722(15) 0.0256(5) Uani 1 1 d U A . H7 H 0.3315 0.4216 0.4893 0.031 Uiso 1 1 calc R . . C8 C 0.4824(2) 0.40353(14) 0.50365(15) 0.0230(5) Uani 1 1 d U . . C9 C 0.5812(2) 0.38261(13) 0.44821(14) 0.0206(5) Uani 1 1 d U A . H9 H 0.6483 0.3744 0.4577 0.025 Uiso 1 1 calc R . . C10 C 0.4657(2) 0.42106(14) 0.58432(14) 0.0249(5) Uani 1 1 d U A . H10A H 0.4875 0.4724 0.5883 0.030 Uiso 1 1 calc R . . H10B H 0.3886 0.4257 0.6110 0.030 Uiso 1 1 calc R . . C11 C 0.52825(19) 0.27964(13) 0.61888(14) 0.0197(5) Uani 1 1 d U A . H11 H 0.4954 0.2548 0.5895 0.024 Uiso 1 1 calc R . . C12 C 0.5250(2) 0.36161(14) 0.62249(14) 0.0219(5) Uani 1 1 d U . . C13 C 0.5817(2) 0.37291(14) 0.66986(15) 0.0259(5) Uani 1 1 d U A . H13 H 0.5947 0.4219 0.6836 0.031 Uiso 1 1 calc R . . C14 C 0.6180(2) 0.29834(14) 0.69504(15) 0.0227(5) Uani 1 1 d U . . C15 C 0.6766(2) 0.28179(15) 0.74384(15) 0.0253(5) Uani 1 1 d U A . H15 H 0.6965 0.3254 0.7628 0.030 Uiso 1 1 calc R . . C16 C 0.71023(19) 0.20932(14) 0.76874(14) 0.0226(5) Uani 1 1 d U . . C17 C 0.7653(2) 0.19275(16) 0.82340(16) 0.0270(6) Uani 1 1 d U A . C18 C 0.7780(2) 0.11303(16) 0.83205(15) 0.0257(5) Uani 1 1 d U . . C19 C 0.7314(2) 0.08290(15) 0.78275(14) 0.0232(5) Uani 1 1 d U A . H19 H 0.7292 0.0289 0.7773 0.028 Uiso 1 1 calc R . . C20A C 0.4791(16) 0.3536(18) 0.0615(4) 0.047(3) Uani 0.513(11) 1 d PDU A 1 H20A H 0.4350 0.3121 0.0638 0.056 Uiso 0.513(11) 1 calc PR A 1 H20B H 0.4394 0.4034 0.0502 0.056 Uiso 0.513(11) 1 calc PR A 1 C21A C 0.5797(7) 0.3344(7) 0.0017(4) 0.072(4) Uani 0.513(11) 1 d PDU A 1 H21A H 0.5647 0.3315 -0.0459 0.109 Uiso 0.513(11) 1 calc PR A 1 H21B H 0.6176 0.2838 0.0114 0.109 Uiso 0.513(11) 1 calc PR A 1 H21C H 0.6240 0.3751 -0.0004 0.109 Uiso 0.513(11) 1 calc PR A 1 C20B C 0.5041(19) 0.3590(19) 0.0548(5) 0.057(5) Uani 0.487(11) 1 d PDU A 2 H20C H 0.5480 0.3089 0.0330 0.068 Uiso 0.487(11) 1 calc PR A 2 H20D H 0.4314 0.3585 0.0514 0.068 Uiso 0.487(11) 1 calc PR A 2 C21B C 0.5478(12) 0.4223(8) 0.0084(5) 0.102(5) Uani 0.487(11) 1 d PDU A 2 H21D H 0.5504 0.4130 -0.0432 0.153 Uiso 0.487(11) 1 calc PR A 2 H21E H 0.6199 0.4240 0.0109 0.153 Uiso 0.487(11) 1 calc PR A 2 H21F H 0.5022 0.4723 0.0266 0.153 Uiso 0.487(11) 1 calc PR A 2 C22 C 0.3008(3) 0.4088(2) 0.2087(2) 0.0489(9) Uani 1 1 d U . . H22A H 0.2579 0.3929 0.2579 0.059 Uiso 1 1 calc R A . H22B H 0.2814 0.3820 0.1702 0.059 Uiso 1 1 calc R . . C23 C 0.2728(4) 0.4963(3) 0.2016(3) 0.0863(16) Uani 1 1 d U A . H23A H 0.2871 0.5233 0.2417 0.130 Uiso 1 1 calc R . . H23B H 0.1971 0.5096 0.2051 0.130 Uiso 1 1 calc R . . H23C H 0.3160 0.5128 0.1534 0.130 Uiso 1 1 calc R . . C24 C 0.8065(3) 0.25165(18) 0.85960(19) 0.0395(7) Uani 1 1 d U . . H24A H 0.8092 0.2328 0.9092 0.047 Uiso 1 1 calc R A . H24B H 0.7564 0.3016 0.8669 0.047 Uiso 1 1 calc R . . C25 C 0.9163(3) 0.2665(3) 0.8144(3) 0.0721(13) Uani 1 1 d U A . H25A H 0.9657 0.2170 0.8053 0.108 Uiso 1 1 calc R . . H25B H 0.9412 0.3028 0.8418 0.108 Uiso 1 1 calc R . . H25C H 0.9130 0.2894 0.7668 0.108 Uiso 1 1 calc R . . C26 C 0.8230(2) 0.06507(18) 0.88648(17) 0.0348(7) Uani 1 1 d U A . H26A H 0.8620 0.0145 0.8626 0.042 Uiso 1 1 calc R . . H26B H 0.8746 0.0928 0.8997 0.042 Uiso 1 1 calc R . . C27 C 0.7385(4) 0.0499(3) 0.9559(3) 0.0791(15) Uani 1 1 d U . . H27A H 0.6984 0.0998 0.9792 0.119 Uiso 1 1 calc R A . H27B H 0.7717 0.0207 0.9906 0.119 Uiso 1 1 calc R . . H27C H 0.6899 0.0193 0.9436 0.119 Uiso 1 1 calc R . . C28 C 0.6572(2) 0.50115(15) 0.23180(15) 0.0270(5) Uani 1 1 d U . . H28 H 0.5987 0.4935 0.2152 0.032 Uiso 1 1 calc R . . C29 C 0.7028(2) 0.57094(15) 0.22097(16) 0.0284(6) Uani 1 1 d U . . C30 C 0.7831(2) 0.55903(15) 0.25327(17) 0.0306(6) Uani 1 1 d U . . C31 C 0.7853(2) 0.48202(14) 0.28327(16) 0.0263(5) Uani 1 1 d U . . C32 C 0.8526(2) 0.44432(15) 0.32029(16) 0.0284(6) Uani 1 1 d U . . H32 H 0.9036 0.4731 0.3281 0.034 Uiso 1 1 calc R . . C33 C 0.8550(2) 0.36856(15) 0.34781(15) 0.0249(5) Uani 1 1 d U . . C34 C 0.9230(2) 0.33010(15) 0.38761(16) 0.0275(6) Uani 1 1 d U . . H34 H 0.9764 0.3514 0.4011 0.033 Uiso 1 1 calc R . . C35 C 0.89730(19) 0.25640(15) 0.40309(15) 0.0240(5) Uani 1 1 d U . . C36 C 0.81392(19) 0.25157(14) 0.37255(15) 0.0233(5) Uani 1 1 d U . . H36 H 0.7806 0.2066 0.3750 0.028 Uiso 1 1 calc R . . C37 C 0.9495(2) 0.19093(16) 0.44078(16) 0.0275(6) Uani 1 1 d U . . H37A H 0.9993 0.1544 0.4020 0.033 Uiso 1 1 calc R . . H37B H 0.9924 0.2133 0.4673 0.033 Uiso 1 1 calc R . . C38 C 0.78507(18) 0.17481(14) 0.55369(14) 0.0206(5) Uani 1 1 d U . . H38 H 0.7592 0.2290 0.5635 0.025 Uiso 1 1 calc R . . C39 C 0.87528(18) 0.14513(14) 0.49494(14) 0.0205(5) Uani 1 1 d U . . C40 C 0.88478(19) 0.06499(14) 0.50017(14) 0.0217(5) Uani 1 1 d U . . H40 H 0.9376 0.0281 0.4676 0.026 Uiso 1 1 calc R . . C41 C 0.80229(18) 0.04743(14) 0.56237(14) 0.0187(5) Uani 1 1 d U . . C42 C 0.78530(19) -0.02590(14) 0.59162(14) 0.0204(5) Uani 1 1 d U . . H42 H 0.8351 -0.0693 0.5666 0.024 Uiso 1 1 calc R . . C43 C 0.70505(18) -0.04280(13) 0.65240(14) 0.0182(5) Uani 1 1 d U . . C44 C 0.68835(19) -0.11758(14) 0.68473(14) 0.0209(5) Uani 1 1 d U . . C45 C 0.59608(19) -0.10504(14) 0.74286(14) 0.0208(5) Uani 1 1 d U . . C46 C 0.55853(19) -0.02322(14) 0.74463(14) 0.0201(5) Uani 1 1 d U . . H46 H 0.4948 0.0016 0.7794 0.024 Uiso 1 1 calc R . . C47 C 0.6657(3) 0.64229(16) 0.18239(19) 0.0379(7) Uani 1 1 d U . . H47A H 0.6147 0.6792 0.2203 0.045 Uiso 1 1 calc R . . H47B H 0.7278 0.6685 0.1578 0.045 Uiso 1 1 calc R . . C48 C 0.6136(5) 0.6259(2) 0.1258(3) 0.0746(14) Uani 1 1 d U . . H48A H 0.6657 0.5940 0.0851 0.112 Uiso 1 1 calc R . . H48B H 0.5867 0.6754 0.1062 0.112 Uiso 1 1 calc R . . H48C H 0.5542 0.5975 0.1489 0.112 Uiso 1 1 calc R . . C49 C 0.8530(3) 0.61686(18) 0.2604(2) 0.0447(8) Uani 1 1 d U . . H49A H 0.8670 0.6496 0.2156 0.054 Uiso 1 1 calc R . . H49B H 0.9222 0.5881 0.2630 0.054 Uiso 1 1 calc R . . C50 C 0.8029(4) 0.6693(2) 0.3287(3) 0.0732(14) Uani 1 1 d U . . H50A H 0.7335 0.6970 0.3270 0.110 Uiso 1 1 calc R . . H50B H 0.8495 0.7074 0.3299 0.110 Uiso 1 1 calc R . . H50C H 0.7932 0.6375 0.3735 0.110 Uiso 1 1 calc R . . C51 C 0.7577(2) -0.19482(14) 0.65854(16) 0.0282(6) Uani 1 1 d U . . H51A H 0.7457 -0.2318 0.7003 0.034 Uiso 1 1 calc R . . H51B H 0.8333 -0.1874 0.6447 0.034 Uiso 1 1 calc R . . C52 C 0.7377(3) -0.23108(19) 0.5926(2) 0.0476(8) Uani 1 1 d U . . H52A H 0.6637 -0.2405 0.6063 0.071 Uiso 1 1 calc R . . H52B H 0.7860 -0.2808 0.5784 0.071 Uiso 1 1 calc R . . H52C H 0.7507 -0.1954 0.5507 0.071 Uiso 1 1 calc R . . C53 C 0.5424(2) -0.16413(15) 0.79427(16) 0.0282(6) Uani 1 1 d U . . H53A H 0.5968 -0.1992 0.8111 0.034 Uiso 1 1 calc R . . H53B H 0.5120 -0.1966 0.7661 0.034 Uiso 1 1 calc R . . C54 C 0.4542(3) -0.12899(18) 0.86228(17) 0.0366(7) Uani 1 1 d U . . H54A H 0.4838 -0.0980 0.8915 0.055 Uiso 1 1 calc R . . H54B H 0.4232 -0.1711 0.8928 0.055 Uiso 1 1 calc R . . H54C H 0.3988 -0.0952 0.8464 0.055 Uiso 1 1 calc R . . C55 C 0.8493(3) 0.35035(17) 0.14351(17) 0.0370(7) Uani 1 1 d U A . H55 H 0.8504 0.4041 0.1514 0.044 Uiso 1 1 calc R . . C56 C 0.9090(3) 0.30768(19) 0.07738(18) 0.0424(8) Uani 1 1 d U . . C57 C 0.8857(2) 0.23265(17) 0.08747(16) 0.0319(6) Uani 1 1 d U B . C58 C 0.8133(2) 0.23135(15) 0.16053(15) 0.0257(5) Uani 1 1 d U . . C59 C 0.7690(2) 0.16802(15) 0.19538(15) 0.0269(5) Uani 1 1 d U B . H59 H 0.7929 0.1195 0.1689 0.032 Uiso 1 1 calc R . . C60 C 0.69434(19) 0.16691(13) 0.26387(14) 0.0213(5) Uani 1 1 d U . . C61 C 0.6498(2) 0.10159(14) 0.29976(15) 0.0243(5) Uani 1 1 d U B . H61 H 0.6694 0.0489 0.2820 0.029 Uiso 1 1 calc R . . C62 C 0.57399(19) 0.12791(13) 0.36440(14) 0.0189(5) Uani 1 1 d U . . C63 C 0.57426(19) 0.20955(13) 0.36757(14) 0.0196(5) Uani 1 1 d U A . H63 H 0.5291 0.2433 0.4070 0.024 Uiso 1 1 calc R . . C64 C 0.5000(2) 0.08240(14) 0.41867(14) 0.0205(5) Uani 1 1 d U B . H64A H 0.5275 0.0259 0.4090 0.025 Uiso 1 1 calc R . . H64B H 0.4296 0.0928 0.4096 0.025 Uiso 1 1 calc R . . C65 C 0.56648(19) 0.10167(13) 0.53250(13) 0.0185(5) Uani 1 1 d U A . H65 H 0.6403 0.0946 0.5059 0.022 Uiso 1 1 calc R . . C66 C 0.48478(19) 0.10023(13) 0.49884(14) 0.0186(5) Uani 1 1 d U . . C67 C 0.39091(19) 0.11307(14) 0.55577(14) 0.0218(5) Uani 1 1 d U B . H67 H 0.3212 0.1159 0.5513 0.026 Uiso 1 1 calc R . . C68 C 0.41711(19) 0.12138(14) 0.62267(14) 0.0194(5) Uani 1 1 d U . . C69 C 0.34771(19) 0.13306(14) 0.69348(14) 0.0209(5) Uani 1 1 d U B . H69 H 0.2743 0.1350 0.6981 0.025 Uiso 1 1 calc R . . C70 C 0.37201(18) 0.14226(14) 0.75847(14) 0.0200(5) Uani 1 1 d U . . C71 C 0.3003(2) 0.15108(14) 0.83191(14) 0.0230(5) Uani 1 1 d U B . C72 C 0.3602(2) 0.15854(15) 0.87886(14) 0.0247(5) Uani 1 1 d U . . C73 C 0.4668(2) 0.15417(14) 0.83282(14) 0.0229(5) Uani 1 1 d U A . H73 H 0.5253 0.1581 0.8508 0.027 Uiso 1 1 calc R . . C74A C 0.9817(9) 0.3406(6) 0.0099(8) 0.074(2) Uani 0.859(4) 1 d PDU B 1 H74A H 1.0133 0.2989 -0.0287 0.089 Uiso 0.859(4) 1 calc PR B 1 H74B H 1.0405 0.3585 0.0237 0.089 Uiso 0.859(4) 1 calc PR B 1 C75A C 0.9217(8) 0.4096(4) -0.0222(4) 0.142(4) Uani 0.859(4) 1 d PDU B 1 H75A H 0.8607 0.3929 -0.0329 0.213 Uiso 0.859(4) 1 calc PR B 1 H75B H 0.9698 0.4266 -0.0682 0.213 Uiso 0.859(4) 1 calc PR B 1 H75C H 0.8964 0.4530 0.0141 0.213 Uiso 0.859(4) 1 calc PR B 1 C74B C 0.978(7) 0.345(5) 0.006(6) 0.074(2) Uani 0.141(4) 1 d PDU B 2 H74C H 0.9312 0.3797 -0.0176 0.089 Uiso 0.141(4) 1 calc PR B 2 H74D H 1.0212 0.3034 -0.0302 0.089 Uiso 0.141(4) 1 calc PR B 2 C75B C 1.051(5) 0.392(3) 0.031(2) 0.142(4) Uani 0.141(4) 1 d PDU B 2 H75D H 1.0935 0.4180 -0.0120 0.213 Uiso 0.141(4) 1 calc PR B 2 H75E H 1.0988 0.3569 0.0527 0.213 Uiso 0.141(4) 1 calc PR B 2 H75F H 1.0074 0.4319 0.0683 0.213 Uiso 0.141(4) 1 calc PR B 2 C76 C 0.9284(2) 0.16299(19) 0.03545(16) 0.0359(7) Uani 1 1 d U . . H76A H 0.9570 0.1815 -0.0158 0.043 Uiso 1 1 calc R B . H76B H 0.8691 0.1346 0.0363 0.043 Uiso 1 1 calc R . . C77 C 1.0153(3) 0.1069(2) 0.05523(19) 0.0435(8) Uani 1 1 d U B . H77A H 1.0757 0.1340 0.0523 0.065 Uiso 1 1 calc R . . H77B H 1.0388 0.0622 0.0203 0.065 Uiso 1 1 calc R . . H77C H 0.9875 0.0883 0.1059 0.065 Uiso 1 1 calc R . . C78 C 0.1827(2) 0.15007(17) 0.85245(16) 0.0312(6) Uani 1 1 d U . . H78A H 0.1537 0.1802 0.8156 0.037 Uiso 1 1 calc R B . H78B H 0.1477 0.1761 0.9016 0.037 Uiso 1 1 calc R . . C79 C 0.1562(2) 0.0676(2) 0.85547(19) 0.0420(8) Uani 1 1 d U B . H79A H 0.1843 0.0434 0.8057 0.063 Uiso 1 1 calc R . . H79B H 0.0787 0.0696 0.8731 0.063 Uiso 1 1 calc R . . H79C H 0.1886 0.0365 0.8896 0.063 Uiso 1 1 calc R . . C80 C 0.3222(3) 0.1696(2) 0.96168(16) 0.0390(7) Uani 1 1 d U B . H80A H 0.2903 0.2251 0.9734 0.047 Uiso 1 1 calc R . . H80B H 0.2652 0.1375 0.9824 0.047 Uiso 1 1 calc R . . C81 C 0.4053(3) 0.1487(4) 0.9995(2) 0.0771(15) Uani 1 1 d U . . H81A H 0.4421 0.0954 0.9848 0.116 Uiso 1 1 calc R B . H81B H 0.3720 0.1517 1.0535 0.116 Uiso 1 1 calc R . . H81C H 0.4567 0.1854 0.9853 0.116 Uiso 1 1 calc R . . N1 N 0.57394(18) 0.35442(12) 0.23026(12) 0.0247(5) Uani 1 1 d U A . N2 N 0.56892(16) 0.37574(11) 0.38077(12) 0.0200(4) Uani 1 1 d U A . N3 N 0.58280(15) 0.24142(11) 0.66152(11) 0.0188(4) Uani 1 1 d U A . N4 N 0.69067(15) 0.13947(12) 0.74474(12) 0.0198(4) Uani 1 1 d U A . N5 N 0.70570(17) 0.44767(12) 0.26788(12) 0.0240(4) Uani 1 1 d U A . N6 N 0.78733(16) 0.31830(12) 0.33964(12) 0.0213(4) Uani 1 1 d U A . N7 N 0.73977(15) 0.11724(11) 0.59432(11) 0.0176(4) Uani 1 1 d U A . N8 N 0.62220(15) 0.01449(11) 0.69238(11) 0.0180(4) Uani 1 1 d U A . N9 N 0.79114(18) 0.30563(12) 0.19356(12) 0.0260(5) Uani 1 1 d U A . N10 N 0.64588(16) 0.23323(11) 0.30822(11) 0.0193(4) Uani 1 1 d U A . N11 N 0.52774(15) 0.11413(11) 0.60582(11) 0.0169(4) Uani 1 1 d U A . N12 N 0.47544(16) 0.14383(11) 0.76121(11) 0.0188(4) Uani 1 1 d U A . Fe1 Fe 0.67894(3) 0.339696(19) 0.28716(2) 0.01983(9) Uani 1 1 d U . . Fe2 Fe 0.60695(3) 0.128191(18) 0.676513(19) 0.01540(8) Uani 1 1 d U . . C82A C 0.0519(3) 0.2292(3) 0.2115(3) 0.0677(12) Uani 0.746(12) 1 d PU C 1 H82A H -0.0085 0.2402 0.1904 0.081 Uiso 0.746(12) 1 calc PR C 1 H82B H 0.0358 0.2640 0.2555 0.081 Uiso 0.746(12) 1 calc PR C 1 Cl1 Cl 0.1661(3) 0.2484(4) 0.1465(2) 0.138(2) Uani 0.746(12) 1 d PU C 1 Cl2 Cl 0.0657(5) 0.13033(15) 0.23926(18) 0.0983(14) Uani 0.746(12) 1 d PU C 1 C82B C 0.0519(3) 0.2292(3) 0.2115(3) 0.0677(12) Uani 0.254(12) 1 d PU C 2 H82C H 0.0190 0.2442 0.2647 0.081 Uiso 0.254(12) 1 calc PR C 2 H82D H -0.0055 0.2248 0.1891 0.081 Uiso 0.254(12) 1 calc PR C 2 Cl1B Cl 0.1290(16) 0.2985(16) 0.1649(13) 0.200(9) Uani 0.254(12) 1 d PU C 2 Cl2B Cl 0.1328(17) 0.1464(10) 0.2030(14) 0.159(8) Uani 0.254(12) 1 d PU C 2 C83 C 0.0205(3) 0.8892(2) 0.3446(2) 0.0528(9) Uani 1 1 d DU . . H83A H 0.0574 0.9104 0.3762 0.063 Uiso 1 1 calc R . . H83B H 0.0747 0.8555 0.3054 0.063 Uiso 1 1 calc R . . Cl3 Cl -0.04106(15) 0.96562(12) 0.30362(9) 0.1190(6) Uani 1 1 d DU . . Cl4 Cl -0.07071(10) 0.83314(9) 0.39846(8) 0.0869(4) Uani 1 1 d DU . . C84 C 0.8473(6) 0.4378(4) 0.5648(4) 0.124(3) Uani 1 1 d U . . H84A H 0.8570 0.4305 0.5112 0.149 Uiso 1 1 calc R . . H84B H 0.7710 0.4378 0.5916 0.149 Uiso 1 1 calc R . . Cl5 Cl 0.87848(17) 0.52425(14) 0.5780(2) 0.2140(17) Uani 1 1 d U . . Cl6 Cl 0.9227(3) 0.35865(16) 0.59466(16) 0.1775(11) Uani 1 1 d U . . Cl7 Cl 0.9558(8) 0.5085(7) -0.1223(5) 0.097(4) Uani 0.141(4) 1 d PDU B 2 Cl8 Cl 0.7735(12) 0.4566(9) -0.0186(10) 0.165(8) Uani 0.141(4) 1 d PDU B 2 C85 C 0.8420(18) 0.5341(12) -0.0487(15) 0.075(10) Uani 0.141(4) 1 d PDU B 2 H85A H 0.7945 0.5769 -0.0641 0.090 Uiso 0.141(4) 1 calc PR B 2 H85B H 0.8619 0.5539 -0.0069 0.090 Uiso 0.141(4) 1 calc PR B 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 0.0461(17) 0.0270(13) 0.0253(14) 0.0017(11) -0.0132(13) -0.0037(12) C2 0.057(2) 0.0286(14) 0.0325(16) 0.0023(12) -0.0235(15) -0.0054(13) C3 0.0446(17) 0.0244(13) 0.0407(17) 0.0039(12) -0.0252(14) -0.0062(12) C4 0.0320(14) 0.0219(12) 0.0316(15) 0.0015(10) -0.0154(12) -0.0051(10) C5 0.0245(13) 0.0261(13) 0.0344(15) 0.0019(11) -0.0106(11) -0.0031(10) C6 0.0214(12) 0.0209(11) 0.0289(14) 0.0011(10) -0.0072(10) -0.0026(9) C7 0.0222(12) 0.0240(12) 0.0274(14) 0.0009(10) -0.0043(11) -0.0004(10) C8 0.0253(13) 0.0151(10) 0.0264(13) 0.0026(9) -0.0057(10) -0.0014(9) C9 0.0232(12) 0.0143(10) 0.0242(13) 0.0013(9) -0.0082(10) -0.0006(9) C10 0.0303(14) 0.0172(11) 0.0235(13) -0.0006(9) -0.0063(11) 0.0036(10) C11 0.0200(11) 0.0172(11) 0.0216(12) -0.0012(9) -0.0068(10) -0.0010(9) C12 0.0224(12) 0.0175(11) 0.0217(13) -0.0004(9) -0.0023(10) 0.0005(9) C13 0.0313(14) 0.0159(11) 0.0314(15) -0.0011(10) -0.0108(11) -0.0031(10) C14 0.0226(12) 0.0186(11) 0.0274(13) -0.0023(10) -0.0075(10) -0.0039(9) C15 0.0264(13) 0.0227(12) 0.0304(14) -0.0033(10) -0.0121(11) -0.0067(10) C16 0.0194(12) 0.0245(12) 0.0247(13) -0.0042(10) -0.0078(10) -0.0029(9) C17 0.0225(13) 0.0323(14) 0.0296(14) -0.0048(11) -0.0134(11) -0.0021(10) C18 0.0218(12) 0.0311(13) 0.0266(14) -0.0012(11) -0.0121(11) -0.0013(10) C19 0.0219(12) 0.0243(12) 0.0244(13) 0.0014(10) -0.0099(10) -0.0013(9) C20A 0.050(7) 0.063(8) 0.030(5) 0.001(4) -0.018(4) -0.003(4) C21A 0.056(5) 0.129(10) 0.029(4) -0.002(5) -0.012(4) -0.002(5) C20B 0.079(13) 0.062(8) 0.042(7) -0.002(6) -0.040(7) -0.006(8) C21B 0.168(13) 0.120(11) 0.045(6) 0.035(6) -0.052(7) -0.068(9) C22 0.049(2) 0.053(2) 0.057(2) -0.0017(17) -0.0350(18) -0.0066(16) C23 0.073(3) 0.062(3) 0.124(5) 0.006(3) -0.046(3) 0.020(2) C24 0.0465(18) 0.0379(16) 0.0457(19) -0.0056(14) -0.0308(16) -0.0060(13) C25 0.060(3) 0.090(3) 0.084(3) -0.008(3) -0.033(2) -0.040(2) C26 0.0362(16) 0.0385(16) 0.0345(16) -0.0020(12) -0.0218(13) 0.0024(12) C27 0.057(3) 0.120(4) 0.062(3) 0.049(3) -0.025(2) -0.013(3) C28 0.0312(14) 0.0203(12) 0.0283(14) 0.0031(10) -0.0081(11) -0.0029(10) C29 0.0324(14) 0.0178(11) 0.0301(15) 0.0042(10) -0.0025(12) -0.0033(10) C30 0.0304(14) 0.0206(12) 0.0380(16) 0.0054(11) -0.0052(12) -0.0064(10) C31 0.0258(13) 0.0185(11) 0.0324(15) 0.0031(10) -0.0045(11) -0.0059(10) C32 0.0261(13) 0.0229(12) 0.0372(16) 0.0025(11) -0.0081(12) -0.0094(10) C33 0.0226(12) 0.0232(12) 0.0284(14) 0.0031(10) -0.0052(11) -0.0066(10) C34 0.0207(12) 0.0276(13) 0.0354(15) 0.0049(11) -0.0090(11) -0.0070(10) C35 0.0163(11) 0.0268(12) 0.0251(13) 0.0043(10) -0.0012(10) -0.0031(9) C36 0.0192(12) 0.0200(11) 0.0275(14) 0.0036(10) -0.0028(10) -0.0027(9) C37 0.0162(12) 0.0308(13) 0.0334(15) 0.0105(11) -0.0049(11) -0.0040(10) C38 0.0147(11) 0.0195(11) 0.0281(13) 0.0043(9) -0.0073(10) -0.0033(9) C39 0.0115(10) 0.0242(12) 0.0258(13) 0.0046(10) -0.0063(9) -0.0017(9) C40 0.0137(11) 0.0254(12) 0.0231(13) 0.0015(10) -0.0037(9) 0.0013(9) C41 0.0141(11) 0.0209(11) 0.0212(12) -0.0009(9) -0.0067(9) 0.0000(8) C42 0.0159(11) 0.0187(11) 0.0270(13) -0.0010(9) -0.0085(10) 0.0005(9) C43 0.0167(11) 0.0159(10) 0.0243(12) 0.0000(9) -0.0099(9) -0.0019(8) C44 0.0201(12) 0.0189(11) 0.0256(13) 0.0018(9) -0.0099(10) -0.0028(9) C45 0.0212(12) 0.0206(11) 0.0233(13) 0.0035(9) -0.0104(10) -0.0043(9) C46 0.0194(11) 0.0199(11) 0.0216(12) 0.0032(9) -0.0062(10) -0.0049(9) C47 0.0468(18) 0.0208(13) 0.0454(19) 0.0095(12) -0.0147(15) -0.0035(12) C48 0.132(4) 0.037(2) 0.074(3) 0.0154(19) -0.063(3) -0.007(2) C49 0.0422(18) 0.0259(14) 0.071(2) 0.0158(15) -0.0218(17) -0.0143(13) C50 0.070(3) 0.044(2) 0.114(4) -0.021(2) -0.033(3) -0.020(2) C51 0.0225(13) 0.0191(12) 0.0397(16) 0.0041(11) -0.0063(11) 0.0000(9) C52 0.049(2) 0.0298(15) 0.062(2) -0.0157(15) -0.0166(17) 0.0043(14) C53 0.0301(14) 0.0246(12) 0.0307(15) 0.0072(11) -0.0094(12) -0.0071(10) C54 0.0404(17) 0.0379(16) 0.0296(16) 0.0085(12) -0.0051(13) -0.0125(13) C55 0.0433(17) 0.0272(14) 0.0322(16) 0.0031(12) 0.0035(13) -0.0105(12) C56 0.0468(19) 0.0393(17) 0.0298(16) 0.0020(13) 0.0076(14) -0.0110(14) C57 0.0300(14) 0.0364(15) 0.0256(14) 0.0005(11) -0.0028(12) -0.0047(12) C58 0.0258(13) 0.0239(12) 0.0241(13) -0.0031(10) -0.0031(11) -0.0019(10) C59 0.0268(13) 0.0240(12) 0.0267(14) -0.0023(10) -0.0035(11) -0.0027(10) C60 0.0215(12) 0.0169(11) 0.0248(13) -0.0019(9) -0.0062(10) -0.0023(9) C61 0.0267(13) 0.0189(11) 0.0260(13) -0.0020(10) -0.0051(11) -0.0049(9) C62 0.0207(11) 0.0176(11) 0.0211(12) 0.0016(9) -0.0095(10) -0.0046(9) C63 0.0213(12) 0.0176(11) 0.0195(12) 0.0014(9) -0.0047(9) -0.0045(9) C64 0.0241(12) 0.0193(11) 0.0213(12) 0.0019(9) -0.0092(10) -0.0086(9) C65 0.0186(11) 0.0161(10) 0.0210(12) 0.0004(9) -0.0061(9) -0.0035(8) C66 0.0208(11) 0.0144(10) 0.0227(12) 0.0027(9) -0.0091(10) -0.0049(8) C67 0.0174(11) 0.0249(12) 0.0255(13) 0.0032(10) -0.0096(10) -0.0047(9) C68 0.0174(11) 0.0198(11) 0.0223(12) 0.0015(9) -0.0079(9) -0.0031(9) C69 0.0140(11) 0.0229(11) 0.0253(13) 0.0002(9) -0.0061(10) -0.0006(9) C70 0.0159(11) 0.0195(11) 0.0226(12) 0.0011(9) -0.0042(9) 0.0005(8) C71 0.0202(12) 0.0213(11) 0.0238(13) -0.0001(10) -0.0023(10) -0.0003(9) C72 0.0244(13) 0.0256(12) 0.0211(13) 0.0000(10) -0.0031(10) -0.0023(10) C73 0.0235(12) 0.0254(12) 0.0202(13) -0.0003(10) -0.0076(10) -0.0025(10) C74A 0.097(5) 0.056(3) 0.047(4) 0.006(3) 0.022(4) -0.031(3) C75A 0.200(9) 0.084(5) 0.084(5) 0.041(4) 0.034(5) -0.008(5) C74B 0.097(5) 0.056(3) 0.047(4) 0.006(3) 0.022(4) -0.031(3) C75B 0.200(9) 0.084(5) 0.084(5) 0.041(4) 0.034(5) -0.008(5) C76 0.0336(15) 0.0456(17) 0.0239(15) -0.0042(12) -0.0013(12) -0.0061(13) C77 0.0395(18) 0.0495(19) 0.0346(17) -0.0092(14) -0.0033(14) -0.0003(14) C78 0.0190(13) 0.0419(16) 0.0270(15) -0.0030(12) -0.0006(11) -0.0002(11) C79 0.0294(15) 0.055(2) 0.0402(18) -0.0039(15) -0.0012(13) -0.0182(14) C80 0.0347(16) 0.0553(19) 0.0226(15) -0.0044(13) -0.0024(12) -0.0055(14) C81 0.051(2) 0.150(5) 0.029(2) -0.005(2) -0.0124(18) -0.009(3) N1 0.0335(12) 0.0190(10) 0.0233(11) 0.0030(8) -0.0101(9) -0.0067(9) N2 0.0215(10) 0.0154(9) 0.0224(11) 0.0009(8) -0.0066(8) -0.0008(7) N3 0.0166(9) 0.0188(9) 0.0201(10) -0.0009(8) -0.0044(8) -0.0018(7) N4 0.0152(9) 0.0228(10) 0.0223(11) -0.0003(8) -0.0071(8) -0.0029(8) N5 0.0282(11) 0.0175(9) 0.0244(11) 0.0014(8) -0.0054(9) -0.0033(8) N6 0.0181(10) 0.0197(10) 0.0233(11) 0.0022(8) -0.0020(8) -0.0034(8) N7 0.0146(9) 0.0175(9) 0.0213(10) 0.0010(8) -0.0066(8) -0.0017(7) N8 0.0159(9) 0.0175(9) 0.0218(10) 0.0002(8) -0.0079(8) -0.0018(7) N9 0.0270(11) 0.0230(10) 0.0237(11) 0.0027(9) -0.0010(9) -0.0043(9) N10 0.0203(10) 0.0169(9) 0.0200(10) -0.0003(8) -0.0051(8) -0.0025(7) N11 0.0152(9) 0.0162(9) 0.0203(10) 0.0017(7) -0.0067(8) -0.0033(7) N12 0.0183(10) 0.0187(9) 0.0194(10) 0.0008(8) -0.0062(8) -0.0016(7) Fe1 0.02209(18) 0.01541(16) 0.02044(19) 0.00173(13) -0.00415(14) -0.00296(13) Fe2 0.01337(16) 0.01553(15) 0.01780(17) 0.00020(12) -0.00573(13) -0.00165(11) C82A 0.044(2) 0.091(3) 0.062(3) -0.027(2) -0.0067(19) -0.004(2) Cl1 0.0724(16) 0.247(5) 0.0855(17) -0.070(2) 0.0212(12) -0.076(2) Cl2 0.146(3) 0.0753(13) 0.0822(17) -0.0319(11) -0.0692(19) 0.0310(16) C82B 0.044(2) 0.091(3) 0.062(3) -0.027(2) -0.0067(19) -0.004(2) Cl1B 0.152(12) 0.27(2) 0.207(16) 0.051(13) -0.032(11) -0.172(14) Cl2B 0.143(11) 0.177(10) 0.180(14) -0.109(10) -0.129(11) 0.088(9) C83 0.0379(18) 0.075(3) 0.047(2) -0.0145(19) -0.0136(16) -0.0084(17) Cl3 0.1205(13) 0.1449(15) 0.0781(10) 0.0143(9) -0.0380(9) 0.0326(11) Cl4 0.0604(7) 0.1097(10) 0.0937(10) -0.0042(8) -0.0138(6) -0.0396(7) C84 0.130(6) 0.126(6) 0.095(5) -0.048(4) 0.004(4) -0.019(5) Cl5 0.0882(13) 0.1191(17) 0.368(5) -0.041(2) 0.033(2) -0.0099(12) Cl6 0.222(3) 0.136(2) 0.168(2) 0.0262(17) -0.057(2) -0.0156(19) Cl7 0.076(6) 0.136(10) 0.074(6) -0.020(6) -0.005(5) -0.036(6) Cl8 0.125(12) 0.138(13) 0.196(17) -0.043(11) 0.034(11) -0.059(10) C85 0.060(19) 0.07(2) 0.09(2) 0.011(18) -0.009(17) -0.018(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.328(4) . ? C1 C2 1.415(4) . ? C1 H1 0.9500 . ? C2 C3 1.374(5) . ? C2 C20A 1.514(7) . ? C2 C20B 1.515(7) . ? C3 C4 1.433(4) . ? C3 C22 1.494(4) . ? C4 C5 1.373(4) . ? C4 N1 1.396(4) . ? C5 C6 1.386(4) . ? C5 H5 0.9500 . ? C6 N2 1.394(3) . ? C6 C7 1.415(4) . ? C7 C8 1.373(4) . ? C7 H7 0.9500 . ? C8 C9 1.416(3) . ? C8 C10 1.503(4) . ? C9 N2 1.340(3) . ? C9 H9 0.9500 . ? C10 C12 1.496(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N3 1.332(3) . ? C11 C12 1.416(3) . ? C11 H11 0.9500 . ? C12 C13 1.366(4) . ? C13 C14 1.424(3) . ? C13 H13 0.9500 . ? C14 C15 1.371(4) . ? C14 N3 1.397(3) . ? C15 C16 1.381(4) . ? C15 H15 0.9500 . ? C16 N4 1.392(3) . ? C16 C17 1.431(4) . ? C17 C18 1.374(4) . ? C17 C24 1.501(4) . ? C18 C19 1.414(4) . ? C18 C26 1.503(4) . ? C19 N4 1.337(3) . ? C19 H19 0.9500 . ? C20A C21A 1.467(18) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C20B C21B 1.464(18) . ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22 C23 1.513(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.513(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.497(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N5 1.331(3) . ? C28 C29 1.419(4) . ? C28 H28 0.9500 . ? C29 C30 1.366(4) . ? C29 C47 1.505(4) . ? C30 C31 1.432(3) . ? C30 C49 1.505(4) . ? C31 C32 1.370(4) . ? C31 N5 1.398(3) . ? C32 C33 1.395(4) . ? C32 H32 0.9500 . ? C33 N6 1.390(3) . ? C33 C34 1.417(4) . ? C34 C35 1.373(4) . ? C34 H34 0.9500 . ? C35 C36 1.409(4) . ? C35 C37 1.506(3) . ? C36 N6 1.343(3) . ? C36 H36 0.9500 . ? C37 C39 1.498(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 N7 1.346(3) . ? C38 C39 1.406(3) . ? C38 H38 0.9500 . ? C39 C40 1.376(3) . ? C40 C41 1.410(3) . ? C40 H40 0.9500 . ? C41 C42 1.393(3) . ? C41 N7 1.393(3) . ? C42 C43 1.373(3) . ? C42 H42 0.9500 . ? C43 N8 1.403(3) . ? C43 C44 1.435(3) . ? C44 C45 1.372(4) . ? C44 C51 1.503(3) . ? C45 C46 1.423(3) . ? C45 C53 1.501(3) . ? C46 N8 1.323(3) . ? C46 H46 0.9500 . ? C47 C48 1.491(5) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.514(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.519(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.521(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N9 1.341(3) . ? C55 C56 1.417(4) . ? C55 H55 0.9500 . ? C56 C57 1.378(4) . ? C56 C74B 1.57(9) . ? C56 C74A 1.507(13) . ? C57 C58 1.427(4) . ? C57 C76 1.503(4) . ? C58 C59 1.382(4) . ? C58 N9 1.395(3) . ? C59 C60 1.375(4) . ? C59 H59 0.9500 . ? C60 N10 1.391(3) . ? C60 C61 1.419(3) . ? C61 C62 1.365(4) . ? C61 H61 0.9500 . ? C62 C63 1.417(3) . ? C62 C64 1.494(3) . ? C63 N10 1.337(3) . ? C63 H63 0.9500 . ? C64 C66 1.498(3) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 N11 1.334(3) . ? C65 C66 1.417(3) . ? C65 H65 0.9500 . ? C66 C67 1.374(3) . ? C67 C68 1.422(3) . ? C67 H67 0.9500 . ? C68 C69 1.377(3) . ? C68 N11 1.396(3) . ? C69 C70 1.377(4) . ? C69 H69 0.9500 . ? C70 N12 1.398(3) . ? C70 C71 1.423(3) . ? C71 C72 1.377(4) . ? C71 C78 1.499(4) . ? C72 C73 1.416(4) . ? C72 C80 1.498(4) . ? C73 N12 1.335(3) . ? C73 H73 0.9500 . ? C74A C75A 1.540(5) . ? C74A H74A 0.9900 . ? C74A H74B 0.9900 . ? C75A H75A 0.9800 . ? C75A H75B 0.9800 . ? C75A H75C 0.9800 . ? C74B C75B 1.548(18) . ? C74B H74C 0.9900 . ? C74B H74D 0.9900 . ? C75B H75D 0.9800 . ? C75B H75E 0.9800 . ? C75B H75F 0.9800 . ? C76 C77 1.517(5) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.520(4) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.480(5) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? N1 Fe1 1.984(2) . ? N2 Fe1 1.969(2) . ? N3 Fe2 1.961(2) . ? N4 Fe2 1.969(2) . ? N5 Fe1 1.961(2) . ? N6 Fe1 1.965(2) . ? N7 Fe2 1.958(2) . ? N8 Fe2 1.9695(19) . ? N9 Fe1 1.974(2) . ? N10 Fe1 1.964(2) . ? N11 Fe2 1.972(2) . ? N12 Fe2 1.972(2) . ? C82A Cl1 1.716(5) . ? C82A Cl2 1.772(6) . ? C82A H82A 0.9900 . ? C82A H82B 0.9900 . ? C83 Cl3 1.729(4) . ? C83 Cl4 1.738(4) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 Cl5 1.660(7) . ? C84 Cl6 1.748(8) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? Cl7 C85 1.727(10) . ? Cl8 C85 1.728(10) . ? C85 H85A 0.9900 . ? C85 H85B 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 112.7(3) . . ? N1 C1 H1 123.7 . . ? C2 C1 H1 123.7 . . ? C3 C2 C1 106.0(3) . . ? C3 C2 C20A 123.1(9) . . ? C1 C2 C20A 130.7(9) . . ? C3 C2 C20B 134.1(11) . . ? C1 C2 C20B 119.7(10) . . ? C20A C2 C20B 13.1(9) . . ? C2 C3 C4 106.5(3) . . ? C2 C3 C22 127.8(3) . . ? C4 C3 C22 125.7(3) . . ? C5 C4 N1 123.4(2) . . ? C5 C4 C3 127.3(3) . . ? N1 C4 C3 109.3(2) . . ? C4 C5 C6 127.9(3) . . ? C4 C5 H5 116.0 . . ? C6 C5 H5 116.0 . . ? C5 C6 N2 123.9(2) . . ? C5 C6 C7 127.1(2) . . ? N2 C6 C7 108.9(2) . . ? C8 C7 C6 107.7(2) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 105.5(2) . . ? C7 C8 C10 127.6(2) . . ? C9 C8 C10 126.7(2) . . ? N2 C9 C8 111.9(2) . . ? N2 C9 H9 124.0 . . ? C8 C9 H9 124.0 . . ? C12 C10 C8 115.0(2) . . ? C12 C10 H10A 108.5 . . ? C8 C10 H10A 108.5 . . ? C12 C10 H10B 108.5 . . ? C8 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? N3 C11 C12 112.1(2) . . ? N3 C11 H11 124.0 . . ? C12 C11 H11 124.0 . . ? C13 C12 C11 105.5(2) . . ? C13 C12 C10 129.1(2) . . ? C11 C12 C10 125.3(2) . . ? C12 C13 C14 108.0(2) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? C15 C14 N3 123.8(2) . . ? C15 C14 C13 128.1(2) . . ? N3 C14 C13 108.1(2) . . ? C14 C15 C16 127.7(2) . . ? C14 C15 H15 116.2 . . ? C16 C15 H15 116.2 . . ? C15 C16 N4 123.4(2) . . ? C15 C16 C17 127.5(2) . . ? N4 C16 C17 109.1(2) . . ? C18 C17 C16 106.6(2) . . ? C18 C17 C24 127.6(2) . . ? C16 C17 C24 125.6(3) . . ? C17 C18 C19 106.3(2) . . ? C17 C18 C26 128.8(2) . . ? C19 C18 C26 124.7(2) . . ? N4 C19 C18 112.0(2) . . ? N4 C19 H19 124.0 . . ? C18 C19 H19 124.0 . . ? C21A C20A C2 111.9(12) . . ? C21A C20A H20A 109.2 . . ? C2 C20A H20A 109.2 . . ? C21A C20A H20B 109.2 . . ? C2 C20A H20B 109.2 . . ? H20A C20A H20B 107.9 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C21B C20B C2 117.4(13) . . ? C21B C20B H20C 108.0 . . ? C2 C20B H20C 107.9 . . ? C21B C20B H20D 107.9 . . ? C2 C20B H20D 107.9 . . ? H20C C20B H20D 107.2 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C3 C22 C23 113.2(3) . . ? C3 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? C3 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.8 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C24 C25 112.8(3) . . ? C17 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? C17 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C18 112.4(3) . . ? C27 C26 H26A 109.1 . . ? C18 C26 H26A 109.1 . . ? C27 C26 H26B 109.1 . . ? C18 C26 H26B 109.1 . . ? H26A C26 H26B 107.8 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C28 C29 112.3(2) . . ? N5 C28 H28 123.9 . . ? C29 C28 H28 123.9 . . ? C30 C29 C28 105.9(2) . . ? C30 C29 C47 129.0(3) . . ? C28 C29 C47 125.1(3) . . ? C29 C30 C31 107.2(2) . . ? C29 C30 C49 127.1(2) . . ? C31 C30 C49 125.6(3) . . ? C32 C31 N5 123.1(2) . . ? C32 C31 C30 128.3(3) . . ? N5 C31 C30 108.7(2) . . ? C31 C32 C33 127.5(2) . . ? C31 C32 H32 116.2 . . ? C33 C32 H32 116.2 . . ? N6 C33 C32 123.4(2) . . ? N6 C33 C34 109.0(2) . . ? C32 C33 C34 127.6(2) . . ? C35 C34 C33 107.3(2) . . ? C35 C34 H34 126.4 . . ? C33 C34 H34 126.4 . . ? C34 C35 C36 105.9(2) . . ? C34 C35 C37 128.5(2) . . ? C36 C35 C37 125.5(2) . . ? N6 C36 C35 111.8(2) . . ? N6 C36 H36 124.1 . . ? C35 C36 H36 124.1 . . ? C39 C37 C35 115.7(2) . . ? C39 C37 H37A 108.4 . . ? C35 C37 H37A 108.4 . . ? C39 C37 H37B 108.4 . . ? C35 C37 H37B 108.4 . . ? H37A C37 H37B 107.4 . . ? N7 C38 C39 111.9(2) . . ? N7 C38 H38 124.1 . . ? C39 C38 H38 124.1 . . ? C40 C39 C38 105.6(2) . . ? C40 C39 C37 127.0(2) . . ? C38 C39 C37 127.3(2) . . ? C39 C40 C41 107.9(2) . . ? C39 C40 H40 126.1 . . ? C41 C40 H40 126.1 . . ? C42 C41 N7 123.5(2) . . ? C42 C41 C40 127.7(2) . . ? N7 C41 C40 108.7(2) . . ? C43 C42 C41 127.6(2) . . ? C43 C42 H42 116.2 . . ? C41 C42 H42 116.2 . . ? C42 C43 N8 122.8(2) . . ? C42 C43 C44 128.3(2) . . ? N8 C43 C44 108.9(2) . . ? C45 C44 C43 106.8(2) . . ? C45 C44 C51 126.9(2) . . ? C43 C44 C51 126.3(2) . . ? C44 C45 C46 105.9(2) . . ? C44 C45 C53 128.2(2) . . ? C46 C45 C53 125.8(2) . . ? N8 C46 C45 112.5(2) . . ? N8 C46 H46 123.7 . . ? C45 C46 H46 123.7 . . ? C48 C47 C29 114.4(3) . . ? C48 C47 H47A 108.6 . . ? C29 C47 H47A 108.7 . . ? C48 C47 H47B 108.7 . . ? C29 C47 H47B 108.6 . . ? H47A C47 H47B 107.6 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C30 C49 C50 112.3(3) . . ? C30 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? C30 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C44 C51 C52 114.0(2) . . ? C44 C51 H51A 108.8 . . ? C52 C51 H51A 108.8 . . ? C44 C51 H51B 108.8 . . ? C52 C51 H51B 108.8 . . ? H51A C51 H51B 107.7 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C45 C53 C54 114.4(2) . . ? C45 C53 H53A 108.7 . . ? C54 C53 H53A 108.7 . . ? C45 C53 H53B 108.7 . . ? C54 C53 H53B 108.7 . . ? H53A C53 H53B 107.6 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N9 C55 C56 111.8(3) . . ? N9 C55 H55 124.1 . . ? C56 C55 H55 124.1 . . ? C57 C56 C55 106.5(3) . . ? C57 C56 C74B 129(3) . . ? C55 C56 C74B 124(3) . . ? C57 C56 C74A 128.2(5) . . ? C55 C56 C74A 125.3(5) . . ? C74B C56 C74A 4(3) . . ? C56 C57 C58 106.3(3) . . ? C56 C57 C76 128.9(3) . . ? C58 C57 C76 124.7(3) . . ? C59 C58 N9 123.3(2) . . ? C59 C58 C57 127.0(2) . . ? N9 C58 C57 109.6(2) . . ? C60 C59 C58 127.7(2) . . ? C60 C59 H59 116.1 . . ? C58 C59 H59 116.1 . . ? C59 C60 N10 123.9(2) . . ? C59 C60 C61 127.5(2) . . ? N10 C60 C61 108.5(2) . . ? C62 C61 C60 107.8(2) . . ? C62 C61 H61 126.1 . . ? C60 C61 H61 126.1 . . ? C61 C62 C63 105.7(2) . . ? C61 C62 C64 127.9(2) . . ? C63 C62 C64 126.2(2) . . ? N10 C63 C62 111.6(2) . . ? N10 C63 H63 124.2 . . ? C62 C63 H63 124.2 . . ? C62 C64 C66 114.94(19) . . ? C62 C64 H64A 108.5 . . ? C66 C64 H64A 108.5 . . ? C62 C64 H64B 108.5 . . ? C66 C64 H64B 108.5 . . ? H64A C64 H64B 107.5 . . ? N11 C65 C66 112.2(2) . . ? N11 C65 H65 123.9 . . ? C66 C65 H65 123.9 . . ? C67 C66 C65 105.6(2) . . ? C67 C66 C64 127.9(2) . . ? C65 C66 C64 126.4(2) . . ? C66 C67 C68 107.5(2) . . ? C66 C67 H67 126.3 . . ? C68 C67 H67 126.3 . . ? C69 C68 N11 124.0(2) . . ? C69 C68 C67 127.2(2) . . ? N11 C68 C67 108.7(2) . . ? C68 C69 C70 127.7(2) . . ? C68 C69 H69 116.1 . . ? C70 C69 H69 116.1 . . ? C69 C70 N12 123.4(2) . . ? C69 C70 C71 127.4(2) . . ? N12 C70 C71 109.1(2) . . ? C72 C71 C70 106.9(2) . . ? C72 C71 C78 127.7(2) . . ? C70 C71 C78 125.3(2) . . ? C71 C72 C73 106.0(2) . . ? C71 C72 C80 127.9(2) . . ? C73 C72 C80 126.2(2) . . ? N12 C73 C72 112.1(2) . . ? N12 C73 H73 123.9 . . ? C72 C73 H73 123.9 . . ? C56 C74A C75A 111.8(7) . . ? C56 C74A H74A 108.9 . . ? C75A C74A H74A 108.7 . . ? C56 C74A H74B 109.8 . . ? C75A C74A H74B 109.5 . . ? H74A C74A H74B 108.1 . . ? C56 C74B C75B 107(6) . . ? C56 C74B H74C 106.2 . . ? C75B C74B H74C 108.2 . . ? C56 C74B H74D 112.7 . . ? C75B C74B H74D 114.4 . . ? H74C C74B H74D 107.5 . . ? C74B C75B H75D 103.8 . . ? C74B C75B H75E 109.2 . . ? H75D C75B H75E 109.5 . . ? C74B C75B H75F 115.2 . . ? H75D C75B H75F 109.5 . . ? H75E C75B H75F 109.5 . . ? C57 C76 C77 113.0(3) . . ? C57 C76 H76A 109.0 . . ? C77 C76 H76A 109.0 . . ? C57 C76 H76B 109.0 . . ? C77 C76 H76B 109.0 . . ? H76A C76 H76B 107.8 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C71 C78 C79 112.5(2) . . ? C71 C78 H78A 109.1 . . ? C79 C78 H78A 109.1 . . ? C71 C78 H78B 109.1 . . ? C79 C78 H78B 109.1 . . ? H78A C78 H78B 107.8 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C81 C80 C72 115.2(3) . . ? C81 C80 H80A 108.5 . . ? C72 C80 H80A 108.5 . . ? C81 C80 H80B 108.5 . . ? C72 C80 H80B 108.5 . . ? H80A C80 H80B 107.5 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C1 N1 C4 105.6(2) . . ? C1 N1 Fe1 128.2(2) . . ? C4 N1 Fe1 126.17(18) . . ? C9 N2 C6 105.9(2) . . ? C9 N2 Fe1 128.01(17) . . ? C6 N2 Fe1 125.87(17) . . ? C11 N3 C14 106.3(2) . . ? C11 N3 Fe2 127.28(17) . . ? C14 N3 Fe2 126.42(17) . . ? C19 N4 C16 106.0(2) . . ? C19 N4 Fe2 127.18(17) . . ? C16 N4 Fe2 126.52(17) . . ? C28 N5 C31 106.0(2) . . ? C28 N5 Fe1 126.63(19) . . ? C31 N5 Fe1 127.20(17) . . ? C36 N6 C33 105.9(2) . . ? C36 N6 Fe1 127.27(17) . . ? C33 N6 Fe1 126.75(17) . . ? C38 N7 C41 105.9(2) . . ? C38 N7 Fe2 127.32(16) . . ? C41 N7 Fe2 126.58(16) . . ? C46 N8 C43 105.90(19) . . ? C46 N8 Fe2 127.05(17) . . ? C43 N8 Fe2 127.01(16) . . ? C55 N9 C58 105.7(2) . . ? C55 N9 Fe1 127.75(19) . . ? C58 N9 Fe1 125.79(17) . . ? C63 N10 C60 106.3(2) . . ? C63 N10 Fe1 127.52(17) . . ? C60 N10 Fe1 126.17(16) . . ? C65 N11 C68 106.03(19) . . ? C65 N11 Fe2 127.90(16) . . ? C68 N11 Fe2 125.91(16) . . ? C73 N12 C70 105.9(2) . . ? C73 N12 Fe2 127.65(17) . . ? C70 N12 Fe2 126.42(16) . . ? N5 Fe1 N10 177.64(9) . . ? N5 Fe1 N6 91.80(9) . . ? N10 Fe1 N6 89.64(8) . . ? N5 Fe1 N2 89.32(9) . . ? N10 Fe1 N2 88.79(8) . . ? N6 Fe1 N2 90.64(9) . . ? N5 Fe1 N9 89.48(9) . . ? N10 Fe1 N9 92.43(9) . . ? N6 Fe1 N9 88.69(9) . . ? N2 Fe1 N9 178.60(9) . . ? N5 Fe1 N1 90.87(9) . . ? N10 Fe1 N1 87.79(8) . . ? N6 Fe1 N1 176.04(9) . . ? N2 Fe1 N1 92.31(9) . . ? N9 Fe1 N1 88.41(10) . . ? N7 Fe2 N3 90.51(8) . . ? N7 Fe2 N4 88.36(8) . . ? N3 Fe2 N4 92.14(8) . . ? N7 Fe2 N8 91.99(8) . . ? N3 Fe2 N8 176.62(8) . . ? N4 Fe2 N8 90.20(8) . . ? N7 Fe2 N11 89.82(8) . . ? N3 Fe2 N11 89.08(8) . . ? N4 Fe2 N11 177.82(8) . . ? N8 Fe2 N11 88.65(8) . . ? N7 Fe2 N12 177.07(8) . . ? N3 Fe2 N12 87.45(8) . . ? N4 Fe2 N12 89.61(8) . . ? N8 Fe2 N12 90.13(8) . . ? N11 Fe2 N12 92.25(8) . . ? Cl1 C82A Cl2 111.1(3) . . ? Cl1 C82A H82A 109.4 . . ? Cl2 C82A H82A 109.4 . . ? Cl1 C82A H82B 109.4 . . ? Cl2 C82A H82B 109.4 . . ? H82A C82A H82B 108.0 . . ? Cl3 C83 Cl4 111.6(2) . . ? Cl3 C83 H83A 109.3 . . ? Cl4 C83 H83A 109.3 . . ? Cl3 C83 H83B 109.3 . . ? Cl4 C83 H83B 109.3 . . ? H83A C83 H83B 108.0 . . ? Cl5 C84 Cl6 114.1(5) . . ? Cl5 C84 H84A 108.7 . . ? Cl6 C84 H84A 108.7 . . ? Cl5 C84 H84B 108.7 . . ? Cl6 C84 H84B 108.7 . . ? H84A C84 H84B 107.6 . . ? Cl7 C85 Cl8 112.7(10) . . ? Cl7 C85 H85A 109.1 . . ? Cl8 C85 H85A 109.1 . . ? Cl7 C85 H85B 109.1 . . ? Cl8 C85 H85B 109.1 . . ? H85A C85 H85B 107.8 . . ? 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 -0.3(3) . . . . ? N1 C1 C2 C20A -176.0(13) . . . . ? N1 C1 C2 C20B 175.3(12) . . . . ? C1 C2 C3 C4 -0.1(3) . . . . ? C20A C2 C3 C4 176.1(13) . . . . ? C20B C2 C3 C4 -174.8(14) . . . . ? C1 C2 C3 C22 177.9(3) . . . . ? C20A C2 C3 C22 -5.9(13) . . . . ? C20B C2 C3 C22 3.2(14) . . . . ? C2 C3 C4 C5 -179.6(3) . . . . ? C22 C3 C4 C5 2.4(5) . . . . ? C2 C3 C4 N1 0.4(3) . . . . ? C22 C3 C4 N1 -177.7(3) . . . . ? N1 C4 C5 C6 2.9(4) . . . . ? C3 C4 C5 C6 -177.1(3) . . . . ? C4 C5 C6 N2 1.0(4) . . . . ? C4 C5 C6 C7 -179.9(3) . . . . ? C5 C6 C7 C8 -178.1(2) . . . . ? N2 C6 C7 C8 1.0(3) . . . . ? C6 C7 C8 C9 -0.8(3) . . . . ? C6 C7 C8 C10 175.5(2) . . . . ? C7 C8 C9 N2 0.4(3) . . . . ? C10 C8 C9 N2 -176.0(2) . . . . ? C7 C8 C10 C12 134.9(3) . . . . ? C9 C8 C10 C12 -49.6(3) . . . . ? N3 C11 C12 C13 0.4(3) . . . . ? N3 C11 C12 C10 -176.7(2) . . . . ? C8 C10 C12 C13 135.7(3) . . . . ? C8 C10 C12 C11 -47.9(4) . . . . ? C11 C12 C13 C14 -0.5(3) . . . . ? C10 C12 C13 C14 176.5(2) . . . . ? C12 C13 C14 C15 -179.1(3) . . . . ? C12 C13 C14 N3 0.4(3) . . . . ? N3 C14 C15 C16 -0.5(4) . . . . ? C13 C14 C15 C16 179.0(3) . . . . ? C14 C15 C16 N4 2.0(4) . . . . ? C14 C15 C16 C17 -175.5(3) . . . . ? C15 C16 C17 C18 177.5(3) . . . . ? N4 C16 C17 C18 -0.2(3) . . . . ? C15 C16 C17 C24 -6.1(5) . . . . ? N4 C16 C17 C24 176.1(3) . . . . ? C16 C17 C18 C19 0.3(3) . . . . ? C24 C17 C18 C19 -176.0(3) . . . . ? C16 C17 C18 C26 -174.9(3) . . . . ? C24 C17 C18 C26 8.9(5) . . . . ? C17 C18 C19 N4 -0.2(3) . . . . ? C26 C18 C19 N4 175.2(2) . . . . ? C3 C2 C20A C21A 176.7(11) . . . . ? C1 C2 C20A C21A -8(3) . . . . ? C20B C2 C20A C21A 27(9) . . . . ? C3 C2 C20B C21B 101.8(17) . . . . ? C1 C2 C20B C21B -72(3) . . . . ? C20A C2 C20B C21B 138(13) . . . . ? C2 C3 C22 C23 -89.4(4) . . . . ? C4 C3 C22 C23 88.2(4) . . . . ? C18 C17 C24 C25 90.1(4) . . . . ? C16 C17 C24 C25 -85.5(4) . . . . ? C17 C18 C26 C27 93.4(4) . . . . ? C19 C18 C26 C27 -80.9(4) . . . . ? N5 C28 C29 C30 -0.7(3) . . . . ? N5 C28 C29 C47 -179.7(3) . . . . ? C28 C29 C30 C31 0.1(3) . . . . ? C47 C29 C30 C31 179.1(3) . . . . ? C28 C29 C30 C49 -176.8(3) . . . . ? C47 C29 C30 C49 2.2(5) . . . . ? C29 C30 C31 C32 179.6(3) . . . . ? C49 C30 C31 C32 -3.5(5) . . . . ? C29 C30 C31 N5 0.5(3) . . . . ? C49 C30 C31 N5 177.4(3) . . . . ? N5 C31 C32 C33 0.4(5) . . . . ? C30 C31 C32 C33 -178.5(3) . . . . ? C31 C32 C33 N6 1.3(5) . . . . ? C31 C32 C33 C34 -178.4(3) . . . . ? N6 C33 C34 C35 0.5(3) . . . . ? C32 C33 C34 C35 -179.7(3) . . . . ? C33 C34 C35 C36 -0.2(3) . . . . ? C33 C34 C35 C37 176.6(3) . . . . ? C34 C35 C36 N6 -0.2(3) . . . . ? C37 C35 C36 N6 -177.1(2) . . . . ? C34 C35 C37 C39 139.2(3) . . . . ? C36 C35 C37 C39 -44.6(4) . . . . ? N7 C38 C39 C40 0.3(3) . . . . ? N7 C38 C39 C37 -176.4(2) . . . . ? C35 C37 C39 C40 133.6(3) . . . . ? C35 C37 C39 C38 -50.5(4) . . . . ? C38 C39 C40 C41 -1.2(3) . . . . ? C37 C39 C40 C41 175.4(2) . . . . ? C39 C40 C41 C42 -175.4(2) . . . . ? C39 C40 C41 N7 1.7(3) . . . . ? N7 C41 C42 C43 3.1(4) . . . . ? C40 C41 C42 C43 179.8(2) . . . . ? C41 C42 C43 N8 3.8(4) . . . . ? C41 C42 C43 C44 -177.7(2) . . . . ? C42 C43 C44 C45 -178.1(2) . . . . ? N8 C43 C44 C45 0.5(3) . . . . ? C42 C43 C44 C51 0.7(4) . . . . ? N8 C43 C44 C51 179.3(2) . . . . ? C43 C44 C45 C46 0.1(3) . . . . ? C51 C44 C45 C46 -178.7(2) . . . . ? C43 C44 C45 C53 179.1(2) . . . . ? C51 C44 C45 C53 0.3(4) . . . . ? C44 C45 C46 N8 -0.8(3) . . . . ? C53 C45 C46 N8 -179.8(2) . . . . ? C30 C29 C47 C48 153.8(4) . . . . ? C28 C29 C47 C48 -27.4(5) . . . . ? C29 C30 C49 C50 85.7(4) . . . . ? C31 C30 C49 C50 -90.6(4) . . . . ? C45 C44 C51 C52 97.9(3) . . . . ? C43 C44 C51 C52 -80.6(3) . . . . ? C44 C45 C53 C54 168.0(3) . . . . ? C46 C45 C53 C54 -13.2(4) . . . . ? N9 C55 C56 C57 0.2(4) . . . . ? N9 C55 C56 C74B 175(3) . . . . ? N9 C55 C56 C74A 179.3(5) . . . . ? C55 C56 C57 C58 -1.0(4) . . . . ? C74B C56 C57 C58 -175(3) . . . . ? C74A C56 C57 C58 179.9(6) . . . . ? C55 C56 C57 C76 -178.9(3) . . . . ? C74B C56 C57 C76 7(3) . . . . ? C74A C56 C57 C76 2.1(7) . . . . ? C56 C57 C58 C59 -179.1(3) . . . . ? C76 C57 C58 C59 -1.1(5) . . . . ? C56 C57 C58 N9 1.4(3) . . . . ? C76 C57 C58 N9 179.4(3) . . . . ? N9 C58 C59 C60 3.6(5) . . . . ? C57 C58 C59 C60 -175.8(3) . . . . ? C58 C59 C60 N10 4.0(4) . . . . ? C58 C59 C60 C61 -179.3(3) . . . . ? C59 C60 C61 C62 -176.0(3) . . . . ? N10 C60 C61 C62 1.1(3) . . . . ? C60 C61 C62 C63 -0.8(3) . . . . ? C60 C61 C62 C64 175.3(2) . . . . ? C61 C62 C63 N10 0.2(3) . . . . ? C64 C62 C63 N10 -176.0(2) . . . . ? C61 C62 C64 C66 138.4(3) . . . . ? C63 C62 C64 C66 -46.3(3) . . . . ? N11 C65 C66 C67 0.3(3) . . . . ? N11 C65 C66 C64 -175.6(2) . . . . ? C62 C64 C66 C67 134.3(2) . . . . ? C62 C64 C66 C65 -50.6(3) . . . . ? C65 C66 C67 C68 -0.5(3) . . . . ? C64 C66 C67 C68 175.4(2) . . . . ? C66 C67 C68 C69 -178.3(2) . . . . ? C66 C67 C68 N11 0.5(3) . . . . ? N11 C68 C69 C70 2.4(4) . . . . ? C67 C68 C69 C70 -179.0(2) . . . . ? C68 C69 C70 N12 2.5(4) . . . . ? C68 C69 C70 C71 -177.2(2) . . . . ? C69 C70 C71 C72 -179.9(2) . . . . ? N12 C70 C71 C72 0.4(3) . . . . ? C69 C70 C71 C78 1.5(4) . . . . ? N12 C70 C71 C78 -178.1(2) . . . . ? C70 C71 C72 C73 0.1(3) . . . . ? C78 C71 C72 C73 178.6(3) . . . . ? C70 C71 C72 C80 179.7(3) . . . . ? C78 C71 C72 C80 -1.8(5) . . . . ? C71 C72 C73 N12 -0.6(3) . . . . ? C80 C72 C73 N12 179.8(3) . . . . ? C57 C56 C74A C75A 120.4(8) . . . . ? C55 C56 C74A C75A -58.5(10) . . . . ? C74B C56 C74A C75A 14(55) . . . . ? C57 C56 C74B C75B -135(4) . . . . ? C55 C56 C74B C75B 51(6) . . . . ? C74A C56 C74B C75B -59(52) . . . . ? C56 C57 C76 C77 100.7(4) . . . . ? C58 C57 C76 C77 -76.8(4) . . . . ? C72 C71 C78 C79 -98.7(3) . . . . ? C70 C71 C78 C79 79.6(3) . . . . ? C71 C72 C80 C81 159.8(4) . . . . ? C73 C72 C80 C81 -20.7(5) . . . . ? C2 C1 N1 C4 0.5(3) . . . . ? C2 C1 N1 Fe1 -179.30(18) . . . . ? C5 C4 N1 C1 179.4(3) . . . . ? C3 C4 N1 C1 -0.6(3) . . . . ? C5 C4 N1 Fe1 -0.8(4) . . . . ? C3 C4 N1 Fe1 179.28(17) . . . . ? C8 C9 N2 C6 0.3(3) . . . . ? C8 C9 N2 Fe1 -174.51(16) . . . . ? C5 C6 N2 C9 178.4(2) . . . . ? C7 C6 N2 C9 -0.8(3) . . . . ? C5 C6 N2 Fe1 -6.7(3) . . . . ? C7 C6 N2 Fe1 174.13(16) . . . . ? C12 C11 N3 C14 -0.1(3) . . . . ? C12 C11 N3 Fe2 178.68(16) . . . . ? C15 C14 N3 C11 179.4(2) . . . . ? C13 C14 N3 C11 -0.2(3) . . . . ? C15 C14 N3 Fe2 0.6(4) . . . . ? C13 C14 N3 Fe2 -179.01(17) . . . . ? C18 C19 N4 C16 0.1(3) . . . . ? C18 C19 N4 Fe2 -174.16(17) . . . . ? C15 C16 N4 C19 -177.8(2) . . . . ? C17 C16 N4 C19 0.1(3) . . . . ? C15 C16 N4 Fe2 -3.5(4) . . . . ? C17 C16 N4 Fe2 174.37(17) . . . . ? C29 C28 N5 C31 1.0(3) . . . . ? C29 C28 N5 Fe1 -173.99(18) . . . . ? C32 C31 N5 C28 180.0(3) . . . . ? C30 C31 N5 C28 -0.9(3) . . . . ? C32 C31 N5 Fe1 -5.1(4) . . . . ? C30 C31 N5 Fe1 174.02(18) . . . . ? C35 C36 N6 C33 0.5(3) . . . . ? C35 C36 N6 Fe1 178.35(17) . . . . ? C32 C33 N6 C36 179.6(3) . . . . ? C34 C33 N6 C36 -0.6(3) . . . . ? C32 C33 N6 Fe1 1.7(4) . . . . ? C34 C33 N6 Fe1 -178.45(18) . . . . ? C39 C38 N7 C41 0.8(3) . . . . ? C39 C38 N7 Fe2 -174.76(16) . . . . ? C42 C41 N7 C38 175.7(2) . . . . ? C40 C41 N7 C38 -1.5(3) . . . . ? C42 C41 N7 Fe2 -8.7(3) . . . . ? C40 C41 N7 Fe2 174.06(16) . . . . ? C45 C46 N8 C43 1.1(3) . . . . ? C45 C46 N8 Fe2 -176.67(16) . . . . ? C42 C43 N8 C46 177.7(2) . . . . ? C44 C43 N8 C46 -1.0(3) . . . . ? C42 C43 N8 Fe2 -4.5(3) . . . . ? C44 C43 N8 Fe2 176.77(16) . . . . ? C56 C55 N9 C58 0.6(4) . . . . ? C56 C55 N9 Fe1 -169.9(2) . . . . ? C59 C58 N9 C55 179.3(3) . . . . ? C57 C58 N9 C55 -1.2(3) . . . . ? C59 C58 N9 Fe1 -10.0(4) . . . . ? C57 C58 N9 Fe1 169.49(19) . . . . ? C62 C63 N10 C60 0.5(3) . . . . ? C62 C63 N10 Fe1 -178.82(16) . . . . ? C59 C60 N10 C63 176.3(2) . . . . ? C61 C60 N10 C63 -0.9(3) . . . . ? C59 C60 N10 Fe1 -4.4(4) . . . . ? C61 C60 N10 Fe1 178.36(17) . . . . ? C66 C65 N11 C68 0.0(3) . . . . ? C66 C65 N11 Fe2 -175.56(15) . . . . ? C69 C68 N11 C65 178.5(2) . . . . ? C67 C68 N11 C65 -0.3(2) . . . . ? C69 C68 N11 Fe2 -5.8(3) . . . . ? C67 C68 N11 Fe2 175.38(15) . . . . ? C72 C73 N12 C70 0.8(3) . . . . ? C72 C73 N12 Fe2 -176.19(16) . . . . ? C69 C70 N12 C73 179.5(2) . . . . ? C71 C70 N12 C73 -0.8(3) . . . . ? C69 C70 N12 Fe2 -3.4(3) . . . . ? C71 C70 N12 Fe2 176.30(16) . . . . ? C28 N5 Fe1 N10 -53(2) . . . . ? C31 N5 Fe1 N10 133(2) . . . . ? C28 N5 Fe1 N6 179.9(2) . . . . ? C31 N5 Fe1 N6 6.0(2) . . . . ? C28 N5 Fe1 N2 -89.5(2) . . . . ? C31 N5 Fe1 N2 96.6(2) . . . . ? C28 N5 Fe1 N9 91.3(2) . . . . ? C31 N5 Fe1 N9 -82.7(2) . . . . ? C28 N5 Fe1 N1 2.9(2) . . . . ? C31 N5 Fe1 N1 -171.1(2) . . . . ? C63 N10 Fe1 N5 -38(2) . . . . ? C60 N10 Fe1 N5 143(2) . . . . ? C63 N10 Fe1 N6 89.7(2) . . . . ? C60 N10 Fe1 N6 -89.4(2) . . . . ? C63 N10 Fe1 N2 -0.9(2) . . . . ? C60 N10 Fe1 N2 179.9(2) . . . . ? C63 N10 Fe1 N9 178.4(2) . . . . ? C60 N10 Fe1 N9 -0.7(2) . . . . ? C63 N10 Fe1 N1 -93.3(2) . . . . ? C60 N10 Fe1 N1 87.6(2) . . . . ? C36 N6 Fe1 N5 178.2(2) . . . . ? C33 N6 Fe1 N5 -4.4(2) . . . . ? C36 N6 Fe1 N10 0.1(2) . . . . ? C33 N6 Fe1 N10 177.5(2) . . . . ? C36 N6 Fe1 N2 88.9(2) . . . . ? C33 N6 Fe1 N2 -93.7(2) . . . . ? C36 N6 Fe1 N9 -92.3(2) . . . . ? C33 N6 Fe1 N9 85.1(2) . . . . ? C36 N6 Fe1 N1 -49.4(13) . . . . ? C33 N6 Fe1 N1 128.0(12) . . . . ? C9 N2 Fe1 N5 -88.8(2) . . . . ? C6 N2 Fe1 N5 97.4(2) . . . . ? C9 N2 Fe1 N10 92.6(2) . . . . ? C6 N2 Fe1 N10 -81.16(19) . . . . ? C9 N2 Fe1 N6 3.0(2) . . . . ? C6 N2 Fe1 N6 -170.78(19) . . . . ? C9 N2 Fe1 N9 -58(4) . . . . ? C6 N2 Fe1 N9 128(4) . . . . ? C9 N2 Fe1 N1 -179.6(2) . . . . ? C6 N2 Fe1 N1 6.58(19) . . . . ? C55 N9 Fe1 N5 -2.3(3) . . . . ? C58 N9 Fe1 N5 -171.0(2) . . . . ? C55 N9 Fe1 N10 176.3(3) . . . . ? C58 N9 Fe1 N10 7.6(2) . . . . ? C55 N9 Fe1 N6 -94.2(3) . . . . ? C58 N9 Fe1 N6 97.1(2) . . . . ? C55 N9 Fe1 N2 -33(4) . . . . ? C58 N9 Fe1 N2 159(4) . . . . ? C55 N9 Fe1 N1 88.5(3) . . . . ? C58 N9 Fe1 N1 -80.2(2) . . . . ? C1 N1 Fe1 N5 87.3(2) . . . . ? C4 N1 Fe1 N5 -92.4(2) . . . . ? C1 N1 Fe1 N10 -94.6(2) . . . . ? C4 N1 Fe1 N10 85.6(2) . . . . ? C1 N1 Fe1 N6 -45.0(14) . . . . ? C4 N1 Fe1 N6 135.2(12) . . . . ? C1 N1 Fe1 N2 176.7(2) . . . . ? C4 N1 Fe1 N2 -3.1(2) . . . . ? C1 N1 Fe1 N9 -2.1(2) . . . . ? C4 N1 Fe1 N9 178.1(2) . . . . ? C38 N7 Fe2 N3 3.3(2) . . . . ? C41 N7 Fe2 N3 -171.37(19) . . . . ? C38 N7 Fe2 N4 -88.8(2) . . . . ? C41 N7 Fe2 N4 96.50(19) . . . . ? C38 N7 Fe2 N8 -179.0(2) . . . . ? C41 N7 Fe2 N8 6.4(2) . . . . ? C38 N7 Fe2 N11 92.4(2) . . . . ? C41 N7 Fe2 N11 -82.29(19) . . . . ? C38 N7 Fe2 N12 -42.7(17) . . . . ? C41 N7 Fe2 N12 142.6(16) . . . . ? C11 N3 Fe2 N7 91.6(2) . . . . ? C14 N3 Fe2 N7 -89.8(2) . . . . ? C11 N3 Fe2 N4 180.0(2) . . . . ? C14 N3 Fe2 N4 -1.4(2) . . . . ? C11 N3 Fe2 N8 -46.2(16) . . . . ? C14 N3 Fe2 N8 132.4(14) . . . . ? C11 N3 Fe2 N11 1.8(2) . . . . ? C14 N3 Fe2 N11 -179.6(2) . . . . ? C11 N3 Fe2 N12 -90.5(2) . . . . ? C14 N3 Fe2 N12 88.1(2) . . . . ? C19 N4 Fe2 N7 -93.6(2) . . . . ? C16 N4 Fe2 N7 93.3(2) . . . . ? C19 N4 Fe2 N3 175.9(2) . . . . ? C16 N4 Fe2 N3 2.8(2) . . . . ? C19 N4 Fe2 N8 -1.7(2) . . . . ? C16 N4 Fe2 N8 -174.7(2) . . . . ? C19 N4 Fe2 N11 -60(2) . . . . ? C16 N4 Fe2 N11 127(2) . . . . ? C19 N4 Fe2 N12 88.5(2) . . . . ? C16 N4 Fe2 N12 -84.6(2) . . . . ? C46 N8 Fe2 N7 177.3(2) . . . . ? C43 N8 Fe2 N7 -0.1(2) . . . . ? C46 N8 Fe2 N3 -45.0(16) . . . . ? C43 N8 Fe2 N3 137.7(14) . . . . ? C46 N8 Fe2 N4 88.9(2) . . . . ? C43 N8 Fe2 N4 -88.42(19) . . . . ? C46 N8 Fe2 N11 -93.0(2) . . . . ? C43 N8 Fe2 N11 89.72(19) . . . . ? C46 N8 Fe2 N12 -0.7(2) . . . . ? C43 N8 Fe2 N12 -178.03(19) . . . . ? C65 N11 Fe2 N7 0.72(19) . . . . ? C68 N11 Fe2 N7 -174.01(19) . . . . ? C65 N11 Fe2 N3 91.23(19) . . . . ? C68 N11 Fe2 N3 -83.49(19) . . . . ? C65 N11 Fe2 N4 -33(2) . . . . ? C68 N11 Fe2 N4 152(2) . . . . ? C65 N11 Fe2 N8 -91.28(19) . . . . ? C68 N11 Fe2 N8 93.99(19) . . . . ? C65 N11 Fe2 N12 178.65(19) . . . . ? C68 N11 Fe2 N12 3.92(19) . . . . ? C73 N12 Fe2 N7 -48.1(17) . . . . ? C70 N12 Fe2 N7 135.5(16) . . . . ? C73 N12 Fe2 N3 -94.2(2) . . . . ? C70 N12 Fe2 N3 89.40(19) . . . . ? C73 N12 Fe2 N4 -2.0(2) . . . . ? C70 N12 Fe2 N4 -178.44(19) . . . . ? C73 N12 Fe2 N8 88.2(2) . . . . ? C70 N12 Fe2 N8 -88.24(19) . . . . ? C73 N12 Fe2 N11 176.9(2) . . . . ? C70 N12 Fe2 N11 0.42(19) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.10 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.978 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.079 # Attachment 'FeMeso.cif' data_FeMeso _database_code_depnum_ccdc_archive 'CCDC 710491' _audit_update_record ; 2009-07-23 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H90 Fe2 N12' _chemical_formula_weight 1343.35 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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' '-x+y, -x, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' '-x, -y, -z' 'x, y, -z-1/2' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, -x, -z-1/2' '-y, x-y, -z-1/2' _cell_length_a 15.0249(11) _cell_length_b 15.0249(11) _cell_length_c 24.422(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4774.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 7172 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.36 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.112 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 0.516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(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 3788 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.69 _reflns_number_total 3788 _reflns_number_gt 3024 _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. The material crystallizes with 1/6th of the molecule in the asymmetric unit. The remainder of the molecule is made up of fragments related by symmetry. Additionally, the crystal forms with solvent in the lattice. Unfortunately the solvent, CH2Cl2, is too disordered to be modeled properly. The PLATON/SQUEEZE (Sluis, 1990) program was used to correct the raw data for any residual electron density found in voids otherwise occupied by solvent atoms. The output from SQUEEZE suggested that there was roughly one half molecule of CH2Cl2 in each asymmetric unit. SADI, EADP and EXYZ statements were used to maintain reasonable geometries and anisotropic displacement parameters for disordered fragments. ; _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^)+(0.0633P)^2^+0.6733P] 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 3788 _refine_ls_number_parameters 157 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1066 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.172 _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 0.59467(12) 0.18376(11) 0.49122(5) 0.0285(3) Uani 1 1 d . A . H1 H 0.6626 0.2099 0.4779 0.034 Uiso 1 1 calc R . . C2 C 0.50589(13) 0.10399(12) 0.46528(6) 0.0322(3) Uani 1 1 d . . . C3 C 0.42394(13) 0.08750(12) 0.49726(6) 0.0326(3) Uani 1 1 d . A . C4 C 0.46493(11) 0.15922(11) 0.54191(5) 0.0265(3) Uani 1 1 d . . . C5 C 0.41144(12) 0.17327(11) 0.58350(5) 0.0280(3) Uani 1 1 d . A . H5 H 0.3394 0.1272 0.5840 0.034 Uiso 1 1 calc R . . C6 C 0.44996(11) 0.24650(11) 0.62482(5) 0.0247(3) Uani 1 1 d . . . C7 C 0.39458(11) 0.26036(12) 0.66768(5) 0.0279(3) Uani 1 1 d . A . H7 H 0.3226 0.2203 0.6739 0.033 Uiso 1 1 calc R . . C8 C 0.46373(11) 0.34234(11) 0.69878(5) 0.0244(3) Uani 1 1 d . . . C9 C 0.56070(11) 0.37694(11) 0.67401(5) 0.0232(3) Uani 1 1 d . A . H9 H 0.6231 0.4333 0.6869 0.028 Uiso 1 1 calc R . . C10 C 0.44503(17) 0.38635(17) 0.7500 0.0274(4) Uani 1 2 d S . . H10A H 0.3732 0.3721 0.7500 0.033 Uiso 1 2 calc SR . . H10B H 0.4909 0.4619 0.7500 0.033 Uiso 1 2 calc SR . . C16 C 0.25822(18) 0.04446(19) 0.44985(12) 0.0747(8) Uani 1 1 d . A . H16A H 0.2622 0.1074 0.4640 0.112 Uiso 1 1 calc R . . H16B H 0.1860 -0.0094 0.4467 0.112 Uiso 1 1 calc R . . H16C H 0.2909 0.0580 0.4137 0.112 Uiso 1 1 calc R . . C20A C 0.50568(17) 0.05320(15) 0.41227(6) 0.0430(4) Uani 0.70 1 d PD A 1 H20A H 0.4381 -0.0098 0.4073 0.052 Uiso 0.70 1 calc PR A 1 H20B H 0.5589 0.0328 0.4136 0.052 Uiso 0.70 1 calc PR A 1 C21A C 0.5266(3) 0.1248(3) 0.36417(11) 0.0717(11) Uani 0.70 1 d PD A 1 H21A H 0.5257 0.0897 0.3302 0.108 Uiso 0.70 1 calc PR A 1 H21B H 0.5942 0.1864 0.3687 0.108 Uiso 0.70 1 calc PR A 1 H21C H 0.4736 0.1444 0.3626 0.108 Uiso 0.70 1 calc PR A 1 C20B C 0.50568(17) 0.05320(15) 0.41227(6) 0.0430(4) Uani 0.30 1 d PD A 2 H20C H 0.4766 -0.0211 0.4196 0.052 Uiso 0.30 1 calc PR A 2 H20D H 0.4580 0.0600 0.3869 0.052 Uiso 0.30 1 calc PR A 2 C21B C 0.6030(6) 0.0895(6) 0.3837(3) 0.072(2) Uani 0.30 1 d PD A 2 H21D H 0.5912 0.0498 0.3499 0.108 Uiso 0.30 1 calc PR A 2 H21E H 0.6508 0.0808 0.4072 0.108 Uiso 0.30 1 calc PR A 2 H21F H 0.6323 0.1624 0.3746 0.108 Uiso 0.30 1 calc PR A 2 C22 C 0.31320(14) 0.00944(14) 0.48874(8) 0.0464(4) Uani 1 1 d . . . H22A H 0.2777 -0.0072 0.5246 0.056 Uiso 1 1 calc R A . H22B H 0.3084 -0.0543 0.4742 0.056 Uiso 1 1 calc R . . N1 N 0.57161(9) 0.21780(9) 0.53648(4) 0.0248(3) Uani 1 1 d . A . N2 N 0.55357(9) 0.32007(9) 0.62987(4) 0.0214(2) Uani 1 1 d . A . Fe1 Fe 0.6667 0.3333 0.583345(12) 0.02024(12) Uani 1 3 d S . . 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 0.0364(8) 0.0310(8) 0.0201(7) -0.0029(5) -0.0010(6) 0.0184(7) C2 0.0452(9) 0.0293(8) 0.0222(7) -0.0060(6) -0.0071(6) 0.0188(7) C3 0.0395(9) 0.0267(8) 0.0279(7) -0.0061(6) -0.0070(6) 0.0138(7) C4 0.0308(7) 0.0238(7) 0.0220(6) -0.0021(5) -0.0049(5) 0.0115(6) C5 0.0250(7) 0.0265(7) 0.0262(7) 0.0006(6) -0.0023(5) 0.0083(6) C6 0.0248(7) 0.0286(7) 0.0202(6) 0.0022(5) -0.0008(5) 0.0130(6) C7 0.0250(7) 0.0363(8) 0.0230(6) 0.0028(6) 0.0009(5) 0.0159(6) C8 0.0289(7) 0.0341(8) 0.0169(6) 0.0031(5) 0.0003(5) 0.0207(6) C9 0.0264(7) 0.0287(7) 0.0176(6) -0.0007(5) -0.0019(5) 0.0160(6) C10 0.0325(11) 0.0401(12) 0.0186(9) 0.000 0.000 0.0248(10) C16 0.0537(13) 0.0636(15) 0.108(2) -0.0316(14) -0.0371(14) 0.0300(12) C20A 0.0618(12) 0.0411(10) 0.0278(8) -0.0134(7) -0.0091(7) 0.0269(9) C21A 0.121(3) 0.0565(19) 0.0272(13) -0.0090(13) -0.0008(16) 0.037(2) C20B 0.0618(12) 0.0411(10) 0.0278(8) -0.0134(7) -0.0091(7) 0.0269(9) C21B 0.077(5) 0.073(5) 0.042(4) -0.024(4) 0.011(4) 0.019(4) C22 0.0412(10) 0.0393(10) 0.0453(10) -0.0169(8) -0.0092(8) 0.0101(8) N1 0.0303(6) 0.0266(6) 0.0180(5) -0.0014(4) -0.0025(4) 0.0146(5) N2 0.0248(6) 0.0237(6) 0.0168(5) 0.0000(4) -0.0011(4) 0.0129(5) Fe1 0.02375(15) 0.02375(15) 0.01324(17) 0.000 0.000 0.01187(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 1.3346(17) . ? C1 C2 1.421(2) . ? C1 H1 0.9500 . ? C2 C3 1.372(2) . ? C2 C20A 1.502(2) . ? C3 C4 1.4374(19) . ? C3 C22 1.495(2) . ? C4 C5 1.375(2) . ? C4 N1 1.3967(19) . ? C5 C6 1.3883(19) . ? C5 H5 0.9500 . ? C6 N2 1.3927(18) . ? C6 C7 1.4160(19) . ? C7 C8 1.376(2) . ? C7 H7 0.9500 . ? C8 C9 1.4149(19) . ? C8 C10 1.5055(17) . ? C9 N2 1.3462(17) . ? C9 H9 0.9500 . ? C10 C8 1.5055(17) 8_557 ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C16 C22 1.515(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C20A C21A 1.515(3) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N1 Fe1 1.9707(12) . ? N2 Fe1 1.9696(11) . ? Fe1 N2 1.9696(11) 3_655 ? Fe1 N2 1.9696(12) 4_665 ? Fe1 N1 1.9707(12) 3_655 ? Fe1 N1 1.9707(12) 4_665 ? 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 112.24(14) . . ? N1 C1 H1 123.9 . . ? C2 C1 H1 123.9 . . ? C3 C2 C1 106.14(13) . . ? C3 C2 C20A 128.70(15) . . ? C1 C2 C20A 125.13(16) . . ? C2 C3 C4 106.68(14) . . ? C2 C3 C22 127.50(14) . . ? C4 C3 C22 125.81(15) . . ? C5 C4 N1 123.22(13) . . ? C5 C4 C3 127.67(14) . . ? N1 C4 C3 109.09(13) . . ? C4 C5 C6 127.91(14) . . ? C4 C5 H5 116.0 . . ? C6 C5 H5 116.0 . . ? C5 C6 N2 123.43(13) . . ? C5 C6 C7 127.68(14) . . ? N2 C6 C7 108.89(12) . . ? C8 C7 C6 107.66(13) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 105.71(12) . . ? C7 C8 C10 128.94(15) . . ? C9 C8 C10 125.30(15) . . ? N2 C9 C8 111.63(13) . . ? N2 C9 H9 124.2 . . ? C8 C9 H9 124.2 . . ? C8 C10 C8 112.37(16) . 8_557 ? C8 C10 H10A 109.1 . . ? C8 C10 H10A 109.1 8_557 . ? C8 C10 H10B 109.1 . . ? C8 C10 H10B 109.1 8_557 . ? H10A C10 H10B 107.9 . . ? C22 C16 H16A 109.5 . . ? C22 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C22 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C20A C21A 111.15(17) . . ? C2 C20A H20A 109.4 . . ? C21A C20A H20A 109.4 . . ? C2 C20A H20B 109.4 . . ? C21A C20A H20B 109.4 . . ? H20A C20A H20B 108.0 . . ? C20A C21A H21A 109.5 . . ? C20A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C20A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? H21D C21B H21E 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C3 C22 C16 113.63(17) . . ? C3 C22 H22A 108.8 . . ? C16 C22 H22A 108.8 . . ? C3 C22 H22B 108.8 . . ? C16 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C1 N1 C4 105.85(12) . . ? C1 N1 Fe1 127.30(10) . . ? C4 N1 Fe1 126.72(9) . . ? C9 N2 C6 106.10(11) . . ? C9 N2 Fe1 127.36(10) . . ? C6 N2 Fe1 126.49(9) . . ? N2 Fe1 N2 90.05(5) 3_655 4_665 ? N2 Fe1 N2 90.05(5) 3_655 . ? N2 Fe1 N2 90.05(5) 4_665 . ? N2 Fe1 N1 92.14(5) 3_655 3_655 ? N2 Fe1 N1 88.22(5) 4_665 3_655 ? N2 Fe1 N1 177.21(5) . 3_655 ? N2 Fe1 N1 88.22(5) 3_655 . ? N2 Fe1 N1 177.21(5) 4_665 . ? N2 Fe1 N1 92.14(5) . . ? N1 Fe1 N1 89.66(5) 3_655 . ? N2 Fe1 N1 177.21(5) 3_655 4_665 ? N2 Fe1 N1 92.14(5) 4_665 4_665 ? N2 Fe1 N1 88.22(5) . 4_665 ? N1 Fe1 N1 89.66(5) 3_655 4_665 ? N1 Fe1 N1 89.66(5) . 4_665 ? 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 -0.96(18) . . . . ? N1 C1 C2 C20A 176.98(14) . . . . ? C1 C2 C3 C4 0.80(17) . . . . ? C20A C2 C3 C4 -177.04(15) . . . . ? C1 C2 C3 C22 -178.22(16) . . . . ? C20A C2 C3 C22 3.9(3) . . . . ? C2 C3 C4 C5 177.93(15) . . . . ? C22 C3 C4 C5 -3.0(3) . . . . ? C2 C3 C4 N1 -0.43(17) . . . . ? C22 C3 C4 N1 178.61(16) . . . . ? N1 C4 C5 C6 2.4(2) . . . . ? C3 C4 C5 C6 -175.74(15) . . . . ? C4 C5 C6 N2 0.4(2) . . . . ? C4 C5 C6 C7 -179.73(15) . . . . ? C5 C6 C7 C8 -179.63(14) . . . . ? N2 C6 C7 C8 0.26(16) . . . . ? C6 C7 C8 C9 -0.05(15) . . . . ? C6 C7 C8 C10 -177.77(14) . . . . ? C7 C8 C9 N2 -0.18(16) . . . . ? C10 C8 C9 N2 177.64(13) . . . . ? C7 C8 C10 C8 93.9(2) . . . 8_557 ? C9 C8 C10 C8 -83.4(2) . . . 8_557 ? C3 C2 C20A C21A 105.4(3) . . . . ? C1 C2 C20A C21A -72.1(3) . . . . ? C2 C3 C22 C16 -84.7(2) . . . . ? C4 C3 C22 C16 96.5(2) . . . . ? C2 C1 N1 C4 0.67(16) . . . . ? C2 C1 N1 Fe1 -175.39(10) . . . . ? C5 C4 N1 C1 -178.60(14) . . . . ? C3 C4 N1 C1 -0.15(15) . . . . ? C5 C4 N1 Fe1 -2.5(2) . . . . ? C3 C4 N1 Fe1 175.95(10) . . . . ? C8 C9 N2 C6 0.33(15) . . . . ? C8 C9 N2 Fe1 -177.24(9) . . . . ? C5 C6 N2 C9 179.53(13) . . . . ? C7 C6 N2 C9 -0.36(15) . . . . ? C5 C6 N2 Fe1 -2.87(19) . . . . ? C7 C6 N2 Fe1 177.24(9) . . . . ? C9 N2 Fe1 N2 91.06(9) . . . 3_655 ? C6 N2 Fe1 N2 -86.04(13) . . . 3_655 ? C9 N2 Fe1 N2 1.00(11) . . . 4_665 ? C6 N2 Fe1 N2 -176.10(11) . . . 4_665 ? C9 N2 Fe1 N1 -50.6(10) . . . 3_655 ? C6 N2 Fe1 N1 132.3(9) . . . 3_655 ? C9 N2 Fe1 N1 179.27(11) . . . . ? C6 N2 Fe1 N1 2.17(11) . . . . ? C9 N2 Fe1 N1 -91.13(11) . . . 4_665 ? C6 N2 Fe1 N1 91.77(11) . . . 4_665 ? C1 N1 Fe1 N2 -94.35(12) . . . 3_655 ? C4 N1 Fe1 N2 90.37(11) . . . 3_655 ? C1 N1 Fe1 N2 -42.7(10) . . . 4_665 ? C4 N1 Fe1 N2 142.0(9) . . . 4_665 ? C1 N1 Fe1 N2 175.66(12) . . . . ? C4 N1 Fe1 N2 0.39(11) . . . . ? C1 N1 Fe1 N1 -2.20(12) . . . 3_655 ? C4 N1 Fe1 N1 -177.48(11) . . . 3_655 ? C1 N1 Fe1 N1 87.46(9) . . . 4_665 ? C4 N1 Fe1 N1 -87.82(14) . . . 4_665 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.318 _refine_diff_density_min -0.179 _refine_diff_density_rms 0.052 # 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 -0.006 -0.002 -0.001 1534 271 ' ' _platon_squeeze_details ; ; # Attachment 'CoHex.cif' data_CoHex _database_code_depnum_ccdc_archive 'CCDC 710492' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H96 Cl6 Co2 N12' _chemical_formula_weight 1604.29 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7050(9) _cell_length_b 17.5163(9) _cell_length_c 17.8828(11) _cell_angle_alpha 81.878(3) _cell_angle_beta 76.930(3) _cell_angle_gamma 83.402(3) _cell_volume 4124.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 23.72 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(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 12657 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.0584 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 23.85 _reflns_number_total 12657 _reflns_number_gt 8912 _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. Three molecules of CH2Cl2 were located and modeled, however there was residual electron density that could not be resolved. As a result the PLATON/SQUEEZE program was used to generate a data set free of any solvent in the region of the remaining electron density. The output from SQUEEZE generates a completely merged (i.e., only unique) dataset, and thus the Rint value will be zero. The post-SQUEEZE Rint(=0.00) has been exchanged for the original Rint (pre-SQUEEZE =0.048) to give the reader some feel for the quality of the data. By leaving the Rint=0.00, the reader has no idea whether the agreement for the original dataset was good (i.e. 3%) or bad (30%). The disordered ethyl groups and solvent methylene chloride molecules were modelled using DFIX and SADI commands in order to maintain similar bond lengths and angles. Unrestrained anisotropic refinements resulted in numerous NPD atoms, thus the ISOR command was used to ensure approximate isotropic behaviour of all atoms. The EADP and EXYZ commands were used when refining disordered solvent molecules where only the chloride atoms were in different orientations and the central carbon was common to both fragments. SQUEEZE was employed to resolve any unmodelled lattice solvent. The formula (and any values subsequently derived from it) no longer takes into account any unmodelled solvent ; _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^)+(0.1080P)^2^+4.9268P] 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 12657 _refine_ls_number_parameters 993 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1966 _refine_ls_wR_factor_gt 0.1821 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.082 _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 0.2988(4) 0.4904(3) 0.2419(3) 0.0323(12) Uani 1 1 d . A . H1 H 0.2873 0.4734 0.1967 0.039 Uiso 1 1 calc R . . C2 C 0.3189(4) 0.5666(3) 0.2460(3) 0.0336(13) Uani 1 1 d . . . C3 C 0.3291(4) 0.5680(3) 0.3203(3) 0.0323(12) Uani 1 1 d . A . C4 C 0.3167(3) 0.4920(3) 0.3592(3) 0.0254(11) Uani 1 1 d . . . C5 C 0.3270(4) 0.4636(3) 0.4329(3) 0.0319(12) Uani 1 1 d . A . H5 H 0.3400 0.5002 0.4631 0.038 Uiso 1 1 calc R . . C6 C 0.3208(3) 0.3885(3) 0.4687(3) 0.0251(11) Uani 1 1 d . . . C7 C 0.3367(4) 0.3582(3) 0.5415(3) 0.0310(12) Uani 1 1 d . A . H7 H 0.3510 0.3868 0.5784 0.037 Uiso 1 1 calc R . . C8 C 0.3281(3) 0.2792(3) 0.5510(3) 0.0275(11) Uani 1 1 d . . . C9 C 0.3040(3) 0.2646(3) 0.4826(3) 0.0243(11) Uani 1 1 d . A . H9 H 0.2921 0.2150 0.4729 0.029 Uiso 1 1 calc R . . C10 C 0.3413(4) 0.2205(3) 0.6185(3) 0.0343(12) Uani 1 1 d . A . H10A H 0.3474 0.2479 0.6618 0.041 Uiso 1 1 calc R . . H10B H 0.4049 0.1878 0.6037 0.041 Uiso 1 1 calc R . . C11 C 0.1531(3) 0.1941(3) 0.6582(2) 0.0237(11) Uani 1 1 d . A . H11 H 0.1276 0.2465 0.6481 0.028 Uiso 1 1 calc R . . C12 C 0.2558(4) 0.1688(3) 0.6461(3) 0.0261(11) Uani 1 1 d . . . C13 C 0.2604(4) 0.0905(3) 0.6671(3) 0.0311(12) Uani 1 1 d . A . H13 H 0.3197 0.0563 0.6651 0.037 Uiso 1 1 calc R . . C14 C 0.1607(3) 0.0700(3) 0.6923(3) 0.0240(11) Uani 1 1 d . . . C15 C 0.1291(4) -0.0035(3) 0.7208(3) 0.0247(11) Uani 1 1 d . A . H15 H 0.1809 -0.0444 0.7218 0.030 Uiso 1 1 calc R . . C16 C 0.0332(3) -0.0238(2) 0.7473(2) 0.0202(10) Uani 1 1 d . . . C17 C -0.0006(4) -0.0980(3) 0.7787(3) 0.0233(11) Uani 1 1 d . A . C18 C -0.1038(4) -0.0889(3) 0.7977(2) 0.0229(10) Uani 1 1 d . . . C19 C -0.1298(4) -0.0090(2) 0.7778(2) 0.0199(10) Uani 1 1 d . A . H19 H -0.1972 0.0134 0.7852 0.024 Uiso 1 1 calc R . . C20 C 0.335(2) 0.6283(19) 0.1753(17) 0.029(4) Uani 0.55(4) 1 d PD A 1 H20A H 0.2814 0.6711 0.1856 0.035 Uiso 0.55(4) 1 calc PR A 1 H20B H 0.3996 0.6496 0.1719 0.035 Uiso 0.55(4) 1 calc PR A 1 C21 C 0.335(2) 0.605(2) 0.0967(16) 0.074(6) Uani 0.55(4) 1 d PDU A 1 H21A H 0.3284 0.6521 0.0602 0.110 Uiso 0.55(4) 1 calc PR A 1 H21B H 0.2783 0.5744 0.1009 0.110 Uiso 0.55(4) 1 calc PR A 1 H21C H 0.3981 0.5749 0.0780 0.110 Uiso 0.55(4) 1 calc PR A 1 C22 C 0.3474(5) 0.6371(3) 0.3545(4) 0.0491(16) Uani 1 1 d . A 1 H22A H 0.3179 0.6311 0.4107 0.059 Uiso 1 1 calc R A 1 H22B H 0.3136 0.6842 0.3307 0.059 Uiso 1 1 calc R A 1 C23 C 0.4591(6) 0.6466(4) 0.3417(5) 0.076(2) Uani 1 1 d . . . H23A H 0.4928 0.6000 0.3653 0.114 Uiso 1 1 calc R A 1 H23B H 0.4685 0.6916 0.3654 0.114 Uiso 1 1 calc R A 1 H23C H 0.4881 0.6543 0.2861 0.114 Uiso 1 1 calc R A 1 C24 C 0.0649(4) -0.1723(3) 0.7871(3) 0.0328(12) Uani 1 1 d . . . H24A H 0.0313 -0.2062 0.8325 0.039 Uiso 1 1 calc R A . H24B H 0.1291 -0.1605 0.7977 0.039 Uiso 1 1 calc R . . C25 C 0.0878(5) -0.2160(3) 0.7170(4) 0.0575(18) Uani 1 1 d . A . H25A H 0.0246 -0.2258 0.7045 0.086 Uiso 1 1 calc R . . H25B H 0.1262 -0.2654 0.7283 0.086 Uiso 1 1 calc R . . H25C H 0.1273 -0.1851 0.6730 0.086 Uiso 1 1 calc R . . C26 C -0.1759(4) -0.1487(3) 0.8325(3) 0.0324(12) Uani 1 1 d . A . H26A H -0.1498 -0.1826 0.8741 0.039 Uiso 1 1 calc R . . H26B H -0.1791 -0.1814 0.7924 0.039 Uiso 1 1 calc R . . C27 C -0.2812(5) -0.1156(3) 0.8656(4) 0.0566(18) Uani 1 1 d . . . H27A H -0.2786 -0.0807 0.9033 0.085 Uiso 1 1 calc R A . H27B H -0.3225 -0.1578 0.8912 0.085 Uiso 1 1 calc R . . H27C H -0.3107 -0.0868 0.8239 0.085 Uiso 1 1 calc R . . C28 C 0.4856(4) 0.3510(3) 0.2660(3) 0.0307(12) Uani 1 1 d . . . H28 H 0.4782 0.4056 0.2663 0.037 Uiso 1 1 calc R . . C29 C 0.5763(4) 0.3087(3) 0.2358(3) 0.0323(12) Uani 1 1 d . . . C30 C 0.5552(4) 0.2329(3) 0.2460(3) 0.0349(12) Uani 1 1 d . . . C31 C 0.4527(4) 0.2310(3) 0.2829(3) 0.0270(11) Uani 1 1 d . . . C32 C 0.3973(4) 0.1669(3) 0.3037(3) 0.0311(12) Uani 1 1 d . . . H32 H 0.4335 0.1182 0.2950 0.037 Uiso 1 1 calc R . . C33 C 0.2968(4) 0.1654(2) 0.3351(3) 0.0253(11) Uani 1 1 d . . . C34 C 0.2388(4) 0.1003(3) 0.3559(3) 0.0266(11) Uani 1 1 d . . . H34 H 0.2634 0.0479 0.3510 0.032 Uiso 1 1 calc R . . C35 C 0.1420(3) 0.1265(2) 0.3841(2) 0.0202(10) Uani 1 1 d . . . C36 C 0.1419(4) 0.2077(2) 0.3800(2) 0.0214(10) Uani 1 1 d . . . H36 H 0.0836 0.2412 0.3962 0.026 Uiso 1 1 calc R . . C37 C 0.0519(3) 0.0815(2) 0.4109(2) 0.0208(10) Uani 1 1 d . . . H37A H 0.0110 0.0912 0.3709 0.025 Uiso 1 1 calc R . . H37B H 0.0747 0.0256 0.4158 0.025 Uiso 1 1 calc R . . C38 C 0.0195(3) 0.1069(2) 0.5534(2) 0.0181(10) Uani 1 1 d . . . H38 H 0.0883 0.1032 0.5563 0.022 Uiso 1 1 calc R . . C39 C -0.0132(3) 0.1001(2) 0.4860(2) 0.0174(10) Uani 1 1 d . . . C40 C -0.1160(3) 0.1086(2) 0.5062(3) 0.0217(10) Uani 1 1 d . . . H40 H -0.1609 0.1071 0.4730 0.026 Uiso 1 1 calc R . . C41 C -0.1438(3) 0.1202(2) 0.5858(3) 0.0199(10) Uani 1 1 d . . . C42 C -0.2388(3) 0.1309(2) 0.6307(3) 0.0240(11) Uani 1 1 d . . . H42 H -0.2928 0.1292 0.6059 0.029 Uiso 1 1 calc R . . C43 C -0.2654(3) 0.1438(2) 0.7069(3) 0.0218(10) Uani 1 1 d . . . C44 C -0.3629(4) 0.1488(3) 0.7555(3) 0.0269(11) Uani 1 1 d . . . C45 C -0.3511(4) 0.1614(3) 0.8265(3) 0.0267(11) Uani 1 1 d . . . C46 C -0.2473(3) 0.1637(2) 0.8200(3) 0.0243(11) Uani 1 1 d . . . H46 H -0.2182 0.1722 0.8612 0.029 Uiso 1 1 calc R . . C47 C 0.6720(4) 0.3437(3) 0.1967(4) 0.0478(15) Uani 1 1 d . . . H47A H 0.7217 0.3025 0.1751 0.057 Uiso 1 1 calc R . . H47B H 0.6991 0.3646 0.2357 0.057 Uiso 1 1 calc R . . C48 C 0.6600(6) 0.4070(4) 0.1331(5) 0.090(3) Uani 1 1 d . . . H48A H 0.6386 0.3858 0.0921 0.135 Uiso 1 1 calc R . . H48B H 0.7243 0.4293 0.1121 0.135 Uiso 1 1 calc R . . H48C H 0.6092 0.4473 0.1536 0.135 Uiso 1 1 calc R . . C49 C 0.6239(4) 0.1629(3) 0.2179(4) 0.0600(19) Uani 1 1 d . . . H49A H 0.6949 0.1742 0.2104 0.072 Uiso 1 1 calc R . . H49B H 0.6122 0.1179 0.2580 0.072 Uiso 1 1 calc R . . C50 C 0.6059(6) 0.1428(5) 0.1430(5) 0.090(3) Uani 1 1 d . . . H50A H 0.5357 0.1319 0.1500 0.135 Uiso 1 1 calc R . . H50B H 0.6501 0.0969 0.1278 0.135 Uiso 1 1 calc R . . H50C H 0.6204 0.1864 0.1025 0.135 Uiso 1 1 calc R . . C51 C -0.4578(4) 0.1379(3) 0.7322(3) 0.0356(13) Uani 1 1 d . . . H51A H -0.4523 0.1576 0.6769 0.043 Uiso 1 1 calc R . . H51B H -0.5144 0.1686 0.7625 0.043 Uiso 1 1 calc R . . C52 C -0.4804(5) 0.0537(4) 0.7449(4) 0.064(2) Uani 1 1 d . . . H52A H -0.4273 0.0237 0.7118 0.095 Uiso 1 1 calc R . . H52B H -0.5452 0.0496 0.7318 0.095 Uiso 1 1 calc R . . H52C H -0.4833 0.0332 0.7992 0.095 Uiso 1 1 calc R . . C53 C -0.4289(4) 0.1689(3) 0.8996(3) 0.0381(13) Uani 1 1 d . . . H53A H -0.4114 0.2092 0.9268 0.046 Uiso 1 1 calc R . . H53B H -0.4948 0.1862 0.8862 0.046 Uiso 1 1 calc R . . C54 C -0.4384(6) 0.0951(4) 0.9532(4) 0.068(2) Uani 1 1 d . . . H54A H -0.4548 0.0547 0.9266 0.102 Uiso 1 1 calc R . . H54B H -0.4919 0.1032 0.9988 0.102 Uiso 1 1 calc R . . H54C H -0.3746 0.0793 0.9694 0.102 Uiso 1 1 calc R . . C55 C 0.3170(4) 0.3211(3) 0.1648(3) 0.0333(12) Uani 1 1 d . A . H55 H 0.3837 0.2996 0.1655 0.040 Uiso 1 1 calc R . . C56 C 0.2778(5) 0.3382(3) 0.0969(3) 0.0419(14) Uani 1 1 d . . . C57 C 0.1812(5) 0.3674(3) 0.1196(3) 0.0383(14) Uani 1 1 d . B . C58 C 0.1622(4) 0.3669(3) 0.2019(3) 0.0300(12) Uani 1 1 d . . . C59 C 0.0754(4) 0.3889(3) 0.2513(3) 0.0341(13) Uani 1 1 d . B . H59 H 0.0194 0.4052 0.2281 0.041 Uiso 1 1 calc R . . C60 C 0.0577(4) 0.3910(3) 0.3290(3) 0.0277(11) Uani 1 1 d . . . C61 C -0.0337(4) 0.4090(3) 0.3815(3) 0.0337(12) Uani 1 1 d . B . H61 H -0.0971 0.4238 0.3682 0.040 Uiso 1 1 calc R . . C62 C -0.0155(4) 0.4017(2) 0.4539(3) 0.0267(11) Uani 1 1 d . . . C63 C 0.0880(3) 0.3792(2) 0.4453(3) 0.0242(11) Uani 1 1 d . A . H63 H 0.1220 0.3700 0.4869 0.029 Uiso 1 1 calc R . . C64 C -0.0883(4) 0.4179(3) 0.5278(3) 0.0309(12) Uani 1 1 d . B . H64A H -0.0837 0.4718 0.5367 0.037 Uiso 1 1 calc R . . H64B H -0.1574 0.4143 0.5211 0.037 Uiso 1 1 calc R . . C65 C -0.0681(3) 0.2832(3) 0.6059(3) 0.0248(11) Uani 1 1 d . A . H65 H -0.0723 0.2545 0.5656 0.030 Uiso 1 1 calc R . . C66 C -0.0725(4) 0.3653(3) 0.5980(3) 0.0280(11) Uani 1 1 d . . . C67 C -0.0635(4) 0.3828(3) 0.6677(3) 0.0341(13) Uani 1 1 d . B . H67 H -0.0634 0.4333 0.6813 0.041 Uiso 1 1 calc R . . C68 C -0.0544(4) 0.3124(3) 0.7165(3) 0.0269(11) Uani 1 1 d . . . C69 C -0.0413(4) 0.3020(3) 0.7912(3) 0.0327(12) Uani 1 1 d . B . H69 H -0.0373 0.3478 0.8128 0.039 Uiso 1 1 calc R . . C70 C -0.0333(4) 0.2332(3) 0.8390(3) 0.0279(11) Uani 1 1 d . . . C71 C -0.0253(4) 0.2224(3) 0.9176(3) 0.0323(12) Uani 1 1 d . B . C72 C -0.0249(4) 0.1448(3) 0.9415(3) 0.0300(12) Uani 1 1 d . . . C73 C -0.0306(4) 0.1090(3) 0.8764(3) 0.0267(11) Uani 1 1 d . A . H73 H -0.0306 0.0547 0.8765 0.032 Uiso 1 1 calc R . . C74 C 0.336(4) 0.3318(19) 0.018(3) 0.062(6) Uani 0.65(3) 1 d PDU B 1 H74A H 0.2884 0.3407 -0.0176 0.075 Uiso 0.65(3) 1 calc PR B 1 H74B H 0.3669 0.2780 0.0154 0.075 Uiso 0.65(3) 1 calc PR B 1 C75 C 0.4161(17) 0.3850(12) -0.0119(11) 0.107(6) Uani 0.65(3) 1 d PDU B 1 H75A H 0.4443 0.3803 -0.0667 0.160 Uiso 0.65(3) 1 calc PR B 1 H75B H 0.4693 0.3717 0.0175 0.160 Uiso 0.65(3) 1 calc PR B 1 H75C H 0.3879 0.4384 -0.0060 0.160 Uiso 0.65(3) 1 calc PR B 1 C76 C 0.1099(5) 0.4011(4) 0.0698(4) 0.0568(18) Uani 1 1 d . . . H76A H 0.0404 0.3919 0.0978 0.068 Uiso 1 1 calc R B . H76B H 0.1245 0.3750 0.0224 0.068 Uiso 1 1 calc R . . C77 C 0.1174(6) 0.4883(4) 0.0472(4) 0.074(2) Uani 1 1 d . B . H77A H 0.0945 0.5152 0.0934 0.111 Uiso 1 1 calc R . . H77B H 0.0751 0.5076 0.0099 0.111 Uiso 1 1 calc R . . H77C H 0.1874 0.4981 0.0238 0.111 Uiso 1 1 calc R . . C78 C -0.0200(5) 0.2854(3) 0.9662(3) 0.0466(15) Uani 1 1 d . . . H78A H 0.0331 0.2690 0.9959 0.056 Uiso 1 1 calc R B . H78B H -0.0008 0.3330 0.9314 0.056 Uiso 1 1 calc R . . C79 C -0.1182(5) 0.3038(3) 1.0217(3) 0.0511(16) Uani 1 1 d . B . H79A H -0.1704 0.3227 0.9926 0.077 Uiso 1 1 calc R . . H79B H -0.1097 0.3436 1.0526 0.077 Uiso 1 1 calc R . . H79C H -0.1380 0.2568 1.0561 0.077 Uiso 1 1 calc R . . C80 C -0.0236(4) 0.1021(3) 1.0203(3) 0.0367(13) Uani 1 1 d . B . H80A H -0.0015 0.1362 1.0519 0.044 Uiso 1 1 calc R . . H80B H 0.0256 0.0561 1.0153 0.044 Uiso 1 1 calc R . . C81 C -0.1264(4) 0.0764(4) 1.0615(3) 0.0462(15) Uani 1 1 d . . . H81A H -0.1743 0.1220 1.0697 0.069 Uiso 1 1 calc R B . H81B H -0.1217 0.0468 1.1115 0.069 Uiso 1 1 calc R . . H81C H -0.1494 0.0439 1.0297 0.069 Uiso 1 1 calc R . . C82 C 0.2344(6) 0.1558(5) 0.8516(5) 0.079(2) Uani 1 1 d . . . H82A H 0.1604 0.1573 0.8690 0.094 Uiso 1 1 calc R . . H82B H 0.2526 0.1364 0.8004 0.094 Uiso 1 1 calc R . . C84 C 0.1820(8) 0.4253(6) 0.7402(8) 0.138(4) Uani 0.610(9) 1 d P C 1 H84A H 0.1664 0.4594 0.6945 0.165 Uiso 0.610(9) 1 calc PR C 1 H84B H 0.1649 0.3723 0.7382 0.165 Uiso 0.610(9) 1 calc PR C 1 N1 N 0.2977(3) 0.4448(2) 0.3081(2) 0.0233(9) Uani 1 1 d . A . N2 N 0.2998(3) 0.3282(2) 0.4327(2) 0.0212(9) Uani 1 1 d . A . N3 N 0.0956(3) 0.1356(2) 0.6857(2) 0.0210(9) Uani 1 1 d . A . N4 N -0.0516(3) 0.0309(2) 0.74819(19) 0.0209(9) Uani 1 1 d . A . N5 N 0.4117(3) 0.3054(2) 0.2938(2) 0.0237(9) Uani 1 1 d . A . N6 N 0.2328(3) 0.2317(2) 0.3510(2) 0.0192(8) Uani 1 1 d . A . N7 N -0.0563(3) 0.11913(19) 0.6129(2) 0.0170(8) Uani 1 1 d . A . N8 N -0.1942(3) 0.1526(2) 0.7495(2) 0.0214(9) Uani 1 1 d . A . N9 N 0.2499(3) 0.3387(2) 0.2273(2) 0.0260(9) Uani 1 1 d . A . N10 N 0.1327(3) 0.37233(19) 0.3720(2) 0.0212(9) Uani 1 1 d . A . N11 N -0.0575(3) 0.2512(2) 0.6753(2) 0.0250(9) Uani 1 1 d . A . N12 N -0.0360(3) 0.1611(2) 0.8151(2) 0.0238(9) Uani 1 1 d . A . Co1 Co 0.27073(5) 0.33679(3) 0.33125(3) 0.02036(19) Uani 1 1 d . . . Co2 Co -0.04964(4) 0.14175(3) 0.71433(3) 0.01868(18) Uani 1 1 d . . . Cl1 Cl 0.2698(2) 0.24821(15) 0.84141(17) 0.1123(8) Uani 1 1 d . . . Cl2 Cl 0.2871(3) 0.0939(2) 0.9142(3) 0.201(2) Uani 1 1 d . . . C83 C 0.4137(8) 0.6789(6) 0.5657(5) 0.074(3) Uani 0.835(3) 1 d PU D 1 H83A H 0.4727 0.6852 0.5223 0.089 Uiso 0.835(3) 1 calc PR D 1 H83B H 0.4287 0.6979 0.6111 0.089 Uiso 0.835(3) 1 calc PR D 1 Cl3 Cl 0.3934(3) 0.5823(2) 0.5874(2) 0.1202(12) Uani 0.835(3) 1 d P D 1 Cl4 Cl 0.3100(3) 0.7334(3) 0.5404(3) 0.167(2) Uani 0.835(3) 1 d P D 1 Cl5 Cl 0.1161(3) 0.46124(18) 0.8274(2) 0.1435(12) Uani 0.610(9) 1 d P C 1 Cl6A Cl 0.3104(5) 0.4255(4) 0.7440(4) 0.151(3) Uani 0.610(9) 1 d P C 1 C75B C 0.370(4) 0.384(2) -0.0395(19) 0.107(6) Uani 0.35(3) 1 d PDU B 2 H75D H 0.4145 0.3675 -0.0866 0.160 Uiso 0.35(3) 1 calc PR B 2 H75E H 0.4061 0.4166 -0.0161 0.160 Uiso 0.35(3) 1 calc PR B 2 H75F H 0.3103 0.4143 -0.0526 0.160 Uiso 0.35(3) 1 calc PR B 2 C74B C 0.340(7) 0.316(4) 0.016(5) 0.062(6) Uani 0.35(3) 1 d PDU B 2 H74C H 0.4011 0.2820 0.0237 0.075 Uiso 0.35(3) 1 calc PR B 2 H74D H 0.2989 0.2856 -0.0063 0.075 Uiso 0.35(3) 1 calc PR B 2 C84B C 0.1820(8) 0.4253(6) 0.7402(8) 0.138(4) Uani 0.390(9) 1 d P C 2 H84C H 0.1343 0.4190 0.7078 0.165 Uiso 0.390(9) 1 calc PR C 2 H84D H 0.2182 0.3743 0.7517 0.165 Uiso 0.390(9) 1 calc PR C 2 Cl5B Cl 0.1161(3) 0.46124(18) 0.8274(2) 0.1435(12) Uani 0.390(9) 1 d P C 2 Cl6B Cl 0.2687(6) 0.4933(6) 0.6907(7) 0.153(5) Uani 0.390(9) 1 d P C 2 Cl4B Cl 0.4029(14) 0.8337(9) 0.5376(10) 0.1202(12) Uani 0.165(3) 1 d PD D 2 Cl3B Cl 0.3244(17) 0.6863(9) 0.5728(14) 0.167(2) Uani 0.165(3) 1 d PD D 2 C83B C 0.429(2) 0.7360(13) 0.567(2) 0.076(12) Uani 0.165(3) 1 d PDU D 2 H83C H 0.4479 0.7296 0.6180 0.091 Uiso 0.165(3) 1 calc PR D 2 H83D H 0.4871 0.7145 0.5294 0.091 Uiso 0.165(3) 1 calc PR D 2 C20B C 0.313(3) 0.641(2) 0.194(2) 0.029(4) Uani 0.45(4) 1 d PD A 2 H20C H 0.3759 0.6664 0.1853 0.035 Uiso 0.45(4) 1 calc PR A 2 H20D H 0.2562 0.6763 0.2173 0.035 Uiso 0.45(4) 1 calc PR A 2 C21B C 0.297(2) 0.6195(16) 0.1187(17) 0.046(6) Uani 0.45(4) 1 d PDU A 2 H21D H 0.2955 0.6662 0.0815 0.070 Uiso 0.45(4) 1 calc PR A 2 H21E H 0.2327 0.5964 0.1281 0.070 Uiso 0.45(4) 1 calc PR A 2 H21F H 0.3518 0.5823 0.0979 0.070 Uiso 0.45(4) 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 0.033(3) 0.023(3) 0.039(3) 0.005(2) -0.006(2) -0.006(2) C2 0.026(3) 0.019(3) 0.050(4) 0.007(2) 0.000(3) -0.004(2) C3 0.022(3) 0.020(3) 0.050(4) -0.004(2) 0.004(2) -0.006(2) C4 0.022(3) 0.018(2) 0.034(3) -0.007(2) 0.003(2) -0.006(2) C5 0.033(3) 0.026(3) 0.038(3) -0.011(2) 0.000(2) -0.012(2) C6 0.023(3) 0.028(3) 0.024(3) -0.007(2) 0.001(2) -0.009(2) C7 0.031(3) 0.042(3) 0.023(3) -0.008(2) -0.006(2) -0.014(2) C8 0.017(2) 0.042(3) 0.023(3) 0.003(2) -0.005(2) -0.008(2) C9 0.023(3) 0.022(3) 0.025(3) 0.003(2) -0.004(2) -0.004(2) C10 0.028(3) 0.052(3) 0.026(3) 0.007(2) -0.011(2) -0.017(2) C11 0.029(3) 0.028(3) 0.016(2) -0.001(2) -0.007(2) -0.008(2) C12 0.027(3) 0.041(3) 0.013(2) 0.001(2) -0.007(2) -0.012(2) C13 0.028(3) 0.041(3) 0.025(3) 0.004(2) -0.010(2) -0.006(2) C14 0.022(3) 0.032(3) 0.019(2) -0.001(2) -0.008(2) -0.001(2) C15 0.028(3) 0.029(3) 0.018(2) -0.002(2) -0.012(2) 0.003(2) C16 0.026(3) 0.020(2) 0.017(2) -0.0025(19) -0.010(2) -0.002(2) C17 0.035(3) 0.022(2) 0.016(2) -0.002(2) -0.013(2) -0.001(2) C18 0.031(3) 0.025(3) 0.015(2) -0.002(2) -0.005(2) -0.008(2) C19 0.027(3) 0.019(2) 0.015(2) -0.0023(19) -0.006(2) -0.006(2) C20 0.024(11) 0.011(9) 0.042(12) 0.001(6) 0.006(9) 0.006(7) C21 0.086(17) 0.075(16) 0.062(14) 0.023(10) -0.026(12) -0.036(13) C22 0.062(4) 0.025(3) 0.064(4) -0.005(3) -0.015(3) -0.015(3) C23 0.082(6) 0.058(4) 0.101(6) 0.005(4) -0.040(5) -0.041(4) C24 0.036(3) 0.033(3) 0.030(3) 0.001(2) -0.012(2) -0.003(2) C25 0.083(5) 0.040(3) 0.053(4) -0.017(3) -0.033(4) 0.032(3) C26 0.043(3) 0.019(2) 0.034(3) 0.004(2) -0.009(3) -0.011(2) C27 0.049(4) 0.044(4) 0.066(4) -0.006(3) 0.017(3) -0.018(3) C28 0.035(3) 0.024(3) 0.032(3) -0.002(2) -0.001(2) -0.011(2) C29 0.025(3) 0.039(3) 0.031(3) 0.000(2) -0.001(2) -0.008(2) C30 0.027(3) 0.034(3) 0.041(3) -0.002(2) -0.003(2) -0.005(2) C31 0.028(3) 0.020(3) 0.031(3) -0.002(2) -0.001(2) -0.003(2) C32 0.032(3) 0.020(3) 0.039(3) -0.008(2) -0.002(2) 0.000(2) C33 0.033(3) 0.014(2) 0.027(3) -0.002(2) -0.002(2) -0.002(2) C34 0.031(3) 0.016(2) 0.030(3) -0.003(2) -0.002(2) -0.001(2) C35 0.033(3) 0.017(2) 0.012(2) -0.0003(18) -0.007(2) -0.006(2) C36 0.029(3) 0.017(2) 0.018(2) -0.0015(19) -0.002(2) -0.004(2) C37 0.031(3) 0.016(2) 0.017(2) -0.0021(19) -0.006(2) -0.007(2) C38 0.017(2) 0.016(2) 0.022(2) 0.0008(19) -0.004(2) -0.0040(18) C39 0.022(2) 0.012(2) 0.019(2) 0.0026(18) -0.0062(19) -0.0072(18) C40 0.030(3) 0.019(2) 0.018(2) 0.0013(19) -0.010(2) -0.007(2) C41 0.022(3) 0.016(2) 0.021(2) 0.0007(19) -0.006(2) -0.0027(19) C42 0.022(3) 0.021(2) 0.032(3) -0.001(2) -0.011(2) -0.004(2) C43 0.018(2) 0.019(2) 0.027(3) -0.004(2) -0.005(2) 0.0006(19) C44 0.027(3) 0.020(2) 0.032(3) -0.002(2) -0.001(2) -0.003(2) C45 0.026(3) 0.020(2) 0.030(3) -0.002(2) 0.003(2) -0.006(2) C46 0.028(3) 0.020(2) 0.024(3) -0.006(2) 0.001(2) -0.005(2) C47 0.033(3) 0.047(4) 0.059(4) -0.005(3) 0.006(3) -0.016(3) C48 0.061(5) 0.074(5) 0.106(7) 0.033(5) 0.026(5) -0.025(4) C49 0.026(3) 0.042(4) 0.101(6) -0.012(4) 0.010(3) -0.002(3) C50 0.061(5) 0.092(6) 0.117(7) -0.074(6) 0.016(5) -0.002(4) C51 0.024(3) 0.041(3) 0.039(3) -0.002(3) -0.004(2) 0.002(2) C52 0.042(4) 0.059(4) 0.101(6) -0.007(4) -0.034(4) -0.015(3) C53 0.030(3) 0.041(3) 0.038(3) -0.011(3) 0.007(2) -0.005(2) C54 0.078(5) 0.064(4) 0.046(4) 0.000(3) 0.021(4) -0.017(4) C55 0.051(3) 0.023(3) 0.024(3) 0.000(2) -0.003(3) -0.010(2) C56 0.068(4) 0.036(3) 0.024(3) 0.001(2) -0.008(3) -0.020(3) C57 0.058(4) 0.038(3) 0.025(3) 0.009(2) -0.016(3) -0.028(3) C58 0.039(3) 0.025(3) 0.028(3) 0.004(2) -0.010(2) -0.013(2) C59 0.038(3) 0.033(3) 0.036(3) 0.009(2) -0.018(3) -0.014(2) C60 0.030(3) 0.017(2) 0.034(3) 0.006(2) -0.009(2) -0.006(2) C61 0.021(3) 0.030(3) 0.048(3) 0.008(2) -0.010(2) -0.004(2) C62 0.025(3) 0.012(2) 0.038(3) 0.003(2) 0.003(2) -0.0046(19) C63 0.025(3) 0.014(2) 0.034(3) -0.004(2) -0.006(2) -0.006(2) C64 0.026(3) 0.017(2) 0.045(3) -0.002(2) 0.001(2) -0.002(2) C65 0.024(3) 0.027(3) 0.023(3) -0.005(2) -0.001(2) -0.004(2) C66 0.024(3) 0.021(3) 0.032(3) -0.004(2) 0.011(2) -0.004(2) C67 0.036(3) 0.023(3) 0.040(3) -0.011(2) 0.005(2) -0.009(2) C68 0.030(3) 0.021(3) 0.029(3) -0.012(2) 0.004(2) -0.010(2) C69 0.039(3) 0.027(3) 0.032(3) -0.016(2) 0.006(2) -0.016(2) C70 0.030(3) 0.032(3) 0.022(3) -0.013(2) 0.005(2) -0.012(2) C71 0.034(3) 0.041(3) 0.023(3) -0.015(2) 0.004(2) -0.016(2) C72 0.027(3) 0.047(3) 0.017(3) -0.008(2) -0.002(2) -0.009(2) C73 0.028(3) 0.032(3) 0.021(3) -0.005(2) -0.003(2) -0.007(2) C74 0.096(7) 0.062(15) 0.026(4) -0.008(10) -0.004(4) -0.011(10) C75 0.125(18) 0.146(10) 0.037(10) -0.011(9) 0.027(8) -0.052(13) C76 0.069(5) 0.074(5) 0.037(4) 0.008(3) -0.026(3) -0.035(4) C77 0.074(5) 0.072(5) 0.084(6) 0.033(4) -0.051(4) -0.022(4) C78 0.062(4) 0.055(4) 0.030(3) -0.020(3) -0.008(3) -0.019(3) C79 0.071(4) 0.048(4) 0.035(3) -0.023(3) -0.006(3) 0.002(3) C80 0.042(3) 0.054(3) 0.019(3) -0.013(2) -0.008(2) -0.008(3) C81 0.047(4) 0.067(4) 0.023(3) -0.008(3) -0.002(3) -0.007(3) C82 0.053(5) 0.118(7) 0.079(5) -0.043(5) -0.028(4) 0.004(4) C84 0.102(9) 0.102(8) 0.189(13) 0.018(8) -0.008(8) -0.013(7) N1 0.021(2) 0.025(2) 0.022(2) -0.0002(18) -0.0019(17) -0.0012(17) N2 0.019(2) 0.021(2) 0.022(2) -0.0047(17) 0.0021(16) -0.0042(16) N3 0.021(2) 0.027(2) 0.016(2) -0.0023(17) -0.0044(16) -0.0093(18) N4 0.025(2) 0.030(2) 0.0095(19) -0.0014(16) -0.0043(16) -0.0100(18) N5 0.025(2) 0.021(2) 0.024(2) 0.0002(17) -0.0012(17) -0.0065(17) N6 0.020(2) 0.022(2) 0.0139(19) 0.0013(16) -0.0038(16) 0.0002(17) N7 0.017(2) 0.0158(19) 0.019(2) -0.0019(15) -0.0054(16) -0.0034(15) N8 0.023(2) 0.0180(19) 0.022(2) -0.0049(16) 0.0003(17) -0.0034(16) N9 0.035(2) 0.020(2) 0.022(2) 0.0014(17) -0.0032(19) -0.0093(18) N10 0.025(2) 0.0132(19) 0.024(2) 0.0022(16) -0.0045(18) -0.0027(16) N11 0.025(2) 0.025(2) 0.025(2) -0.0077(18) 0.0023(18) -0.0089(17) N12 0.024(2) 0.028(2) 0.021(2) -0.0075(18) -0.0017(17) -0.0107(17) Co1 0.0242(4) 0.0156(3) 0.0204(4) -0.0003(3) -0.0028(3) -0.0044(3) Co2 0.0216(4) 0.0192(3) 0.0162(3) -0.0044(3) -0.0021(3) -0.0067(3) Cl1 0.118(2) 0.1036(18) 0.128(2) -0.0350(16) -0.0431(17) -0.0041(15) Cl2 0.175(4) 0.199(4) 0.246(5) 0.115(3) -0.124(3) -0.109(3) C83 0.069(6) 0.092(8) 0.057(6) -0.012(6) -0.020(5) 0.027(6) Cl3 0.140(3) 0.125(3) 0.115(2) -0.0135(19) -0.056(2) -0.035(2) Cl4 0.170(4) 0.182(4) 0.158(4) -0.068(3) -0.083(3) 0.105(3) Cl5 0.131(3) 0.121(2) 0.160(3) -0.010(2) -0.001(2) -0.0001(19) Cl6A 0.112(5) 0.172(6) 0.155(6) -0.057(5) 0.031(4) -0.020(4) C75B 0.125(18) 0.146(10) 0.037(10) -0.011(9) 0.027(8) -0.052(13) C74B 0.096(7) 0.062(15) 0.026(4) -0.008(10) -0.004(4) -0.011(10) C84B 0.102(9) 0.102(8) 0.189(13) 0.018(8) -0.008(8) -0.013(7) Cl5B 0.131(3) 0.121(2) 0.160(3) -0.010(2) -0.001(2) -0.0001(19) Cl6B 0.115(6) 0.169(10) 0.210(10) -0.113(8) -0.081(7) 0.049(6) Cl4B 0.140(3) 0.125(3) 0.115(2) -0.0135(19) -0.056(2) -0.035(2) Cl3B 0.170(4) 0.182(4) 0.158(4) -0.068(3) -0.083(3) 0.105(3) C83B 0.09(3) 0.10(3) 0.05(2) -0.04(2) -0.033(19) 0.00(2) C20B 0.024(11) 0.011(9) 0.042(12) 0.001(6) 0.006(9) 0.006(7) C21B 0.060(15) 0.028(10) 0.051(15) 0.034(9) -0.028(11) -0.017(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.330(6) . ? C1 C2 1.408(7) . ? C1 H1 0.9500 . ? C2 C3 1.372(7) . ? C2 C20B 1.49(4) . ? C2 C20 1.53(3) . ? C3 C4 1.422(7) . ? C3 C22 1.499(7) . ? C4 C5 1.374(7) . ? C4 N1 1.398(6) . ? C5 C6 1.382(7) . ? C5 H5 0.9500 . ? C6 C7 1.389(7) . ? C6 N2 1.398(6) . ? C7 C8 1.385(7) . ? C7 H7 0.9500 . ? C8 C9 1.400(6) . ? C8 C10 1.502(7) . ? C9 N2 1.329(6) . ? C9 H9 0.9500 . ? C10 C12 1.515(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N3 1.334(6) . ? C11 C12 1.404(7) . ? C11 H11 0.9500 . ? C12 C13 1.368(7) . ? C13 C14 1.409(7) . ? C13 H13 0.9500 . ? C14 N3 1.380(6) . ? C14 C15 1.394(6) . ? C15 C16 1.363(6) . ? C15 H15 0.9500 . ? C16 N4 1.418(6) . ? C16 C17 1.426(6) . ? C17 C18 1.373(7) . ? C17 C24 1.503(7) . ? C18 C19 1.418(6) . ? C18 C26 1.497(6) . ? C19 N4 1.315(6) . ? C19 H19 0.9500 . ? C20 C21 1.516(13) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.521(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.515(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.512(8) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N5 1.325(6) . ? C28 C29 1.408(7) . ? C28 H28 0.9500 . ? C29 C30 1.370(7) . ? C29 C47 1.494(7) . ? C30 C31 1.412(7) . ? C30 C49 1.528(8) . ? C31 N5 1.380(6) . ? C31 C32 1.388(7) . ? C32 C33 1.367(7) . ? C32 H32 0.9500 . ? C33 N6 1.394(6) . ? C33 C34 1.423(6) . ? C34 C35 1.359(7) . ? C34 H34 0.9500 . ? C35 C36 1.415(6) . ? C35 C37 1.491(6) . ? C36 N6 1.328(6) . ? C36 H36 0.9500 . ? C37 C39 1.491(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 N7 1.331(5) . ? C38 C39 1.401(6) . ? C38 H38 0.9500 . ? C39 C40 1.370(6) . ? C40 C41 1.426(6) . ? C40 H40 0.9500 . ? C41 C42 1.375(6) . ? C41 N7 1.388(5) . ? C42 C43 1.371(6) . ? C42 H42 0.9500 . ? C43 N8 1.400(6) . ? C43 C44 1.421(6) . ? C44 C45 1.366(7) . ? C44 C51 1.493(7) . ? C45 C46 1.405(7) . ? C45 C53 1.501(7) . ? C46 N8 1.333(6) . ? C46 H46 0.9500 . ? C47 C48 1.495(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.512(10) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.518(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.495(8) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 N9 1.325(6) . ? C55 C56 1.416(7) . ? C55 H55 0.9500 . ? C56 C57 1.356(8) . ? C56 C74 1.47(5) . ? C56 C74B 1.58(10) . ? C57 C58 1.435(7) . ? C57 C76 1.486(8) . ? C58 C59 1.363(7) . ? C58 N9 1.393(6) . ? C59 C60 1.361(7) . ? C59 H59 0.9500 . ? C60 N10 1.400(6) . ? C60 C61 1.418(7) . ? C61 C62 1.360(7) . ? C61 H61 0.9500 . ? C62 C63 1.407(6) . ? C62 C64 1.506(7) . ? C63 N10 1.332(6) . ? C63 H63 0.9500 . ? C64 C66 1.491(7) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 N11 1.320(6) . ? C65 C66 1.420(6) . ? C65 H65 0.9500 . ? C66 C67 1.360(7) . ? C67 C68 1.418(7) . ? C67 H67 0.9500 . ? C68 C69 1.371(7) . ? C68 N11 1.393(6) . ? C69 C70 1.384(7) . ? C69 H69 0.9500 . ? C70 N12 1.397(6) . ? C70 C71 1.420(7) . ? C71 C72 1.366(7) . ? C71 C78 1.515(7) . ? C72 C73 1.419(6) . ? C72 C80 1.503(7) . ? C73 N12 1.334(6) . ? C73 H73 0.9500 . ? C74 C75 1.48(2) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 C77 1.533(9) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.512(8) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 C81 1.520(7) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 Cl2 1.673(8) . ? C82 Cl1 1.716(8) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C84 Cl5 1.777(13) . ? C84 Cl6A 1.778(13) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? N1 Co1 1.939(4) . ? N2 Co1 1.927(4) . ? N3 Co2 1.934(4) . ? N4 Co2 1.951(4) . ? N5 Co1 1.939(4) . ? N6 Co1 1.934(4) . ? N7 Co2 1.935(3) . ? N8 Co2 1.934(4) . ? N9 Co1 1.939(4) . ? N10 Co1 1.932(4) . ? N11 Co2 1.945(4) . ? N12 Co2 1.932(4) . ? C83 Cl3 1.721(11) . ? C83 Cl4 1.730(9) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C75B C74B 1.48(3) . ? C75B H75D 0.9800 . ? C75B H75E 0.9800 . ? C75B H75F 0.9800 . ? C74B H74C 0.9900 . ? C74B H74D 0.9900 . ? Cl4B C83B 1.741(14) . ? Cl3B C83B 1.742(10) . ? C83B H83C 0.9900 . ? C83B H83D 0.9900 . ? C20B C21B 1.516(14) . ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? 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 112.7(5) . . ? N1 C1 H1 123.6 . . ? C2 C1 H1 123.6 . . ? C3 C2 C1 105.8(4) . . ? C3 C2 C20B 119.4(13) . . ? C1 C2 C20B 133.7(14) . . ? C3 C2 C20 131.0(11) . . ? C1 C2 C20 123.0(11) . . ? C20B C2 C20 17.3(12) . . ? C2 C3 C4 106.9(4) . . ? C2 C3 C22 126.4(5) . . ? C4 C3 C22 126.6(5) . . ? C5 C4 N1 122.2(4) . . ? C5 C4 C3 128.5(4) . . ? N1 C4 C3 109.1(4) . . ? C4 C5 C6 128.2(4) . . ? C4 C5 H5 115.9 . . ? C6 C5 H5 115.9 . . ? C5 C6 C7 128.7(4) . . ? C5 C6 N2 122.9(4) . . ? C7 C6 N2 108.3(4) . . ? C8 C7 C6 108.4(4) . . ? C8 C7 H7 125.8 . . ? C6 C7 H7 125.8 . . ? C7 C8 C9 104.7(4) . . ? C7 C8 C10 128.9(4) . . ? C9 C8 C10 126.4(4) . . ? N2 C9 C8 112.3(4) . . ? N2 C9 H9 123.8 . . ? C8 C9 H9 123.8 . . ? C8 C10 C12 113.5(4) . . ? C8 C10 H10A 108.9 . . ? C12 C10 H10A 108.9 . . ? C8 C10 H10B 108.9 . . ? C12 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N3 C11 C12 111.6(4) . . ? N3 C11 H11 124.2 . . ? C12 C11 H11 124.2 . . ? C13 C12 C11 105.9(4) . . ? C13 C12 C10 128.7(5) . . ? C11 C12 C10 125.3(5) . . ? C12 C13 C14 107.2(4) . . ? C12 C13 H13 126.4 . . ? C14 C13 H13 126.4 . . ? N3 C14 C15 123.6(4) . . ? N3 C14 C13 109.0(4) . . ? C15 C14 C13 127.4(4) . . ? C16 C15 C14 128.0(4) . . ? C16 C15 H15 116.0 . . ? C14 C15 H15 116.0 . . ? C15 C16 N4 122.2(4) . . ? C15 C16 C17 129.0(4) . . ? N4 C16 C17 108.8(4) . . ? C18 C17 C16 107.1(4) . . ? C18 C17 C24 126.8(4) . . ? C16 C17 C24 126.1(4) . . ? C17 C18 C19 105.4(4) . . ? C17 C18 C26 128.6(4) . . ? C19 C18 C26 126.0(4) . . ? N4 C19 C18 113.6(4) . . ? N4 C19 H19 123.2 . . ? C18 C19 H19 123.2 . . ? C21 C20 C2 119(2) . . ? C21 C20 H20A 107.6 . . ? C2 C20 H20A 107.6 . . ? C21 C20 H20B 107.6 . . ? C2 C20 H20B 107.6 . . ? H20A C20 H20B 107.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C3 C22 C23 111.6(5) . . ? C3 C22 H22A 109.3 . . ? C23 C22 H22A 109.3 . . ? C3 C22 H22B 109.3 . . ? C23 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C17 C24 C25 114.2(4) . . ? C17 C24 H24A 108.7 . . ? C25 C24 H24A 108.7 . . ? C17 C24 H24B 108.7 . . ? C25 C24 H24B 108.7 . . ? H24A C24 H24B 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C18 C26 C27 114.0(4) . . ? C18 C26 H26A 108.7 . . ? C27 C26 H26A 108.7 . . ? C18 C26 H26B 108.7 . . ? C27 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C28 C29 111.7(4) . . ? N5 C28 H28 124.1 . . ? C29 C28 H28 124.1 . . ? C30 C29 C28 105.9(4) . . ? C30 C29 C47 129.2(5) . . ? C28 C29 C47 124.8(5) . . ? C29 C30 C31 106.8(4) . . ? C29 C30 C49 128.2(5) . . ? C31 C30 C49 124.7(5) . . ? N5 C31 C32 123.2(4) . . ? N5 C31 C30 109.2(4) . . ? C32 C31 C30 127.6(4) . . ? C33 C32 C31 127.7(4) . . ? C33 C32 H32 116.1 . . ? C31 C32 H32 116.1 . . ? C32 C33 N6 123.4(4) . . ? C32 C33 C34 128.3(4) . . ? N6 C33 C34 108.3(4) . . ? C35 C34 C33 107.8(4) . . ? C35 C34 H34 126.1 . . ? C33 C34 H34 126.1 . . ? C34 C35 C36 105.7(4) . . ? C34 C35 C37 128.6(4) . . ? C36 C35 C37 125.7(4) . . ? N6 C36 C35 112.1(4) . . ? N6 C36 H36 123.9 . . ? C35 C36 H36 123.9 . . ? C39 C37 C35 114.5(3) . . ? C39 C37 H37A 108.6 . . ? C35 C37 H37A 108.6 . . ? C39 C37 H37B 108.6 . . ? C35 C37 H37B 108.6 . . ? H37A C37 H37B 107.6 . . ? N7 C38 C39 112.6(4) . . ? N7 C38 H38 123.7 . . ? C39 C38 H38 123.7 . . ? C40 C39 C38 105.3(4) . . ? C40 C39 C37 128.3(4) . . ? C38 C39 C37 126.2(4) . . ? C39 C40 C41 107.8(4) . . ? C39 C40 H40 126.1 . . ? C41 C40 H40 126.1 . . ? C42 C41 N7 123.8(4) . . ? C42 C41 C40 128.2(4) . . ? N7 C41 C40 108.0(4) . . ? C43 C42 C41 128.1(4) . . ? C43 C42 H42 115.9 . . ? C41 C42 H42 115.9 . . ? C42 C43 N8 122.3(4) . . ? C42 C43 C44 128.6(4) . . ? N8 C43 C44 109.1(4) . . ? C45 C44 C43 107.0(4) . . ? C45 C44 C51 128.0(5) . . ? C43 C44 C51 125.0(4) . . ? C44 C45 C46 106.2(4) . . ? C44 C45 C53 129.3(5) . . ? C46 C45 C53 124.5(5) . . ? N8 C46 C45 112.5(4) . . ? N8 C46 H46 123.8 . . ? C45 C46 H46 123.8 . . ? C29 C47 C48 113.6(5) . . ? C29 C47 H47A 108.8 . . ? C48 C47 H47A 108.8 . . ? C29 C47 H47B 108.8 . . ? C48 C47 H47B 108.8 . . ? H47A C47 H47B 107.7 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 C30 112.1(6) . . ? C50 C49 H49A 109.2 . . ? C30 C49 H49A 109.2 . . ? C50 C49 H49B 109.2 . . ? C30 C49 H49B 109.2 . . ? H49A C49 H49B 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C44 C51 C52 112.3(4) . . ? C44 C51 H51A 109.1 . . ? C52 C51 H51A 109.1 . . ? C44 C51 H51B 109.1 . . ? C52 C51 H51B 109.1 . . ? H51A C51 H51B 107.9 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 C45 113.3(4) . . ? C54 C53 H53A 108.9 . . ? C45 C53 H53A 108.9 . . ? C54 C53 H53B 108.9 . . ? C45 C53 H53B 108.9 . . ? H53A C53 H53B 107.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N9 C55 C56 112.3(5) . . ? N9 C55 H55 123.9 . . ? C56 C55 H55 123.9 . . ? C57 C56 C55 106.3(5) . . ? C57 C56 C74 128(2) . . ? C55 C56 C74 125(2) . . ? C57 C56 C74B 131(4) . . ? C55 C56 C74B 122(4) . . ? C74 C56 C74B 10(3) . . ? C56 C57 C58 106.8(5) . . ? C56 C57 C76 127.8(5) . . ? C58 C57 C76 125.1(6) . . ? C59 C58 N9 122.4(4) . . ? C59 C58 C57 128.8(5) . . ? N9 C58 C57 108.8(5) . . ? C60 C59 C58 129.1(5) . . ? C60 C59 H59 115.4 . . ? C58 C59 H59 115.4 . . ? C59 C60 N10 123.1(5) . . ? C59 C60 C61 129.4(5) . . ? N10 C60 C61 107.4(4) . . ? C62 C61 C60 108.6(4) . . ? C62 C61 H61 125.7 . . ? C60 C61 H61 125.7 . . ? C61 C62 C63 105.5(4) . . ? C61 C62 C64 127.9(5) . . ? C63 C62 C64 126.5(5) . . ? N10 C63 C62 112.1(4) . . ? N10 C63 H63 124.0 . . ? C62 C63 H63 124.0 . . ? C66 C64 C62 115.1(4) . . ? C66 C64 H64A 108.5 . . ? C62 C64 H64A 108.5 . . ? C66 C64 H64B 108.5 . . ? C62 C64 H64B 108.5 . . ? H64A C64 H64B 107.5 . . ? N11 C65 C66 112.6(4) . . ? N11 C65 H65 123.7 . . ? C66 C65 H65 123.7 . . ? C67 C66 C65 105.1(4) . . ? C67 C66 C64 129.5(4) . . ? C65 C66 C64 125.4(4) . . ? C66 C67 C68 107.9(4) . . ? C66 C67 H67 126.1 . . ? C68 C67 H67 126.1 . . ? C69 C68 N11 123.1(4) . . ? C69 C68 C67 128.2(4) . . ? N11 C68 C67 108.6(4) . . ? C68 C69 C70 128.1(4) . . ? C68 C69 H69 116.0 . . ? C70 C69 H69 116.0 . . ? C69 C70 N12 122.7(4) . . ? C69 C70 C71 128.3(4) . . ? N12 C70 C71 108.9(4) . . ? C72 C71 C70 107.1(4) . . ? C72 C71 C78 126.6(5) . . ? C70 C71 C78 126.3(5) . . ? C71 C72 C73 106.3(4) . . ? C71 C72 C80 129.3(4) . . ? C73 C72 C80 124.3(5) . . ? N12 C73 C72 111.5(4) . . ? N12 C73 H73 124.3 . . ? C72 C73 H73 124.3 . . ? C56 C74 C75 116(3) . . ? C56 C74 H74A 108.2 . . ? C75 C74 H74A 108.2 . . ? C56 C74 H74B 108.2 . . ? C75 C74 H74B 108.2 . . ? H74A C74 H74B 107.4 . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C57 C76 C77 111.6(5) . . ? C57 C76 H76A 109.3 . . ? C77 C76 H76A 109.3 . . ? C57 C76 H76B 109.3 . . ? C77 C76 H76B 109.3 . . ? H76A C76 H76B 108.0 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C79 C78 C71 113.1(5) . . ? C79 C78 H78A 109.0 . . ? C71 C78 H78A 109.0 . . ? C79 C78 H78B 109.0 . . ? C71 C78 H78B 109.0 . . ? H78A C78 H78B 107.8 . . ? C78 C79 H79A 109.5 . . ? C78 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C78 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? C72 C80 C81 112.0(4) . . ? C72 C80 H80A 109.2 . . ? C81 C80 H80A 109.2 . . ? C72 C80 H80B 109.2 . . ? C81 C80 H80B 109.2 . . ? H80A C80 H80B 107.9 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? Cl2 C82 Cl1 113.8(4) . . ? Cl2 C82 H82A 108.8 . . ? Cl1 C82 H82A 108.8 . . ? Cl2 C82 H82B 108.8 . . ? Cl1 C82 H82B 108.8 . . ? H82A C82 H82B 107.7 . . ? Cl5 C84 Cl6A 103.5(7) . . ? Cl5 C84 H84A 111.1 . . ? Cl6A C84 H84A 111.1 . . ? Cl5 C84 H84B 111.1 . . ? Cl6A C84 H84B 111.1 . . ? H84A C84 H84B 109.0 . . ? C1 N1 C4 105.4(4) . . ? C1 N1 Co1 127.8(3) . . ? C4 N1 Co1 126.8(3) . . ? C9 N2 C6 106.2(4) . . ? C9 N2 Co1 127.4(3) . . ? C6 N2 Co1 126.4(3) . . ? C11 N3 C14 106.2(4) . . ? C11 N3 Co2 127.0(3) . . ? C14 N3 Co2 126.7(3) . . ? C19 N4 C16 105.1(4) . . ? C19 N4 Co2 128.4(3) . . ? C16 N4 Co2 126.5(3) . . ? C28 N5 C31 106.3(4) . . ? C28 N5 Co1 127.2(3) . . ? C31 N5 Co1 126.1(3) . . ? C36 N6 C33 106.1(4) . . ? C36 N6 Co1 127.9(3) . . ? C33 N6 Co1 126.0(3) . . ? C38 N7 C41 106.2(4) . . ? C38 N7 Co2 128.0(3) . . ? C41 N7 Co2 125.5(3) . . ? C46 N8 C43 105.3(4) . . ? C46 N8 Co2 128.1(3) . . ? C43 N8 Co2 126.4(3) . . ? C55 N9 C58 105.8(4) . . ? C55 N9 Co1 127.9(4) . . ? C58 N9 Co1 125.9(3) . . ? C63 N10 C60 106.4(4) . . ? C63 N10 Co1 128.1(3) . . ? C60 N10 Co1 125.4(3) . . ? C65 N11 C68 105.8(4) . . ? C65 N11 Co2 127.9(3) . . ? C68 N11 Co2 126.3(3) . . ? C73 N12 C70 106.1(4) . . ? C73 N12 Co2 127.2(3) . . ? C70 N12 Co2 126.6(3) . . ? N2 Co1 N10 90.47(15) . . ? N2 Co1 N6 90.38(15) . . ? N10 Co1 N6 89.04(15) . . ? N2 Co1 N9 175.36(16) . . ? N10 Co1 N9 93.56(16) . . ? N6 Co1 N9 87.40(15) . . ? N2 Co1 N1 93.05(15) . . ? N10 Co1 N1 87.12(15) . . ? N6 Co1 N1 174.87(15) . . ? N9 Co1 N1 89.45(15) . . ? N2 Co1 N5 87.15(15) . . ? N10 Co1 N5 176.58(15) . . ? N6 Co1 N5 93.43(15) . . ? N9 Co1 N5 88.91(16) . . ? N1 Co1 N5 90.55(15) . . ? N12 Co2 N8 89.22(15) . . ? N12 Co2 N3 86.53(15) . . ? N8 Co2 N3 175.42(15) . . ? N12 Co2 N7 176.90(16) . . ? N8 Co2 N7 93.52(15) . . ? N3 Co2 N7 90.77(15) . . ? N12 Co2 N11 93.17(16) . . ? N8 Co2 N11 87.72(15) . . ? N3 Co2 N11 90.80(15) . . ? N7 Co2 N11 88.39(15) . . ? N12 Co2 N4 90.98(15) . . ? N8 Co2 N4 88.88(15) . . ? N3 Co2 N4 92.91(15) . . ? N7 Co2 N4 87.63(14) . . ? N11 Co2 N4 174.59(15) . . ? Cl3 C83 Cl4 111.3(7) . . ? Cl3 C83 H83A 109.4 . . ? Cl4 C83 H83A 109.4 . . ? Cl3 C83 H83B 109.4 . . ? Cl4 C83 H83B 109.4 . . ? H83A C83 H83B 108.0 . . ? C74B C75B H75D 109.5 . . ? C74B C75B H75E 109.5 . . ? H75D C75B H75E 109.5 . . ? C74B C75B H75F 109.5 . . ? H75D C75B H75F 109.5 . . ? H75E C75B H75F 109.5 . . ? C75B C74B C56 112(5) . . ? C75B C74B H74C 109.1 . . ? C56 C74B H74C 109.1 . . ? C75B C74B H74D 109.1 . . ? C56 C74B H74D 109.1 . . ? H74C C74B H74D 107.9 . . ? Cl4B C83B Cl3B 109.6(11) . . ? Cl4B C83B H83C 109.8 . . ? Cl3B C83B H83C 109.8 . . ? Cl4B C83B H83D 109.8 . . ? Cl3B C83B H83D 109.7 . . ? H83C C83B H83D 108.2 . . ? C2 C20B C21B 106(3) . . ? C2 C20B H20C 110.5 . . ? C21B C20B H20C 110.5 . . ? C2 C20B H20D 110.5 . . ? C21B C20B H20D 110.5 . . ? H20C C20B H20D 108.7 . . ? C20B C21B H21D 109.5 . . ? C20B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C20B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? 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(6) . . . . ? N1 C1 C2 C20B -168.9(19) . . . . ? N1 C1 C2 C20 173.7(14) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C20B C2 C3 C4 170.9(16) . . . . ? C20 C2 C3 C4 -173.2(16) . . . . ? C1 C2 C3 C22 -177.7(5) . . . . ? C20B C2 C3 C22 -7.7(17) . . . . ? C20 C2 C3 C22 8.1(17) . . . . ? C2 C3 C4 C5 175.3(5) . . . . ? C22 C3 C4 C5 -6.1(8) . . . . ? C2 C3 C4 N1 -0.7(5) . . . . ? C22 C3 C4 N1 178.0(5) . . . . ? N1 C4 C5 C6 -0.2(8) . . . . ? C3 C4 C5 C6 -175.7(5) . . . . ? C4 C5 C6 C7 175.9(5) . . . . ? C4 C5 C6 N2 -1.5(8) . . . . ? C5 C6 C7 C8 -176.4(5) . . . . ? N2 C6 C7 C8 1.3(5) . . . . ? C6 C7 C8 C9 -1.5(5) . . . . ? C6 C7 C8 C10 178.3(5) . . . . ? C7 C8 C9 N2 1.3(5) . . . . ? C10 C8 C9 N2 -178.5(4) . . . . ? C7 C8 C10 C12 130.4(5) . . . . ? C9 C8 C10 C12 -49.8(7) . . . . ? N3 C11 C12 C13 0.4(5) . . . . ? N3 C11 C12 C10 -177.4(4) . . . . ? C8 C10 C12 C13 136.8(5) . . . . ? C8 C10 C12 C11 -46.0(7) . . . . ? C11 C12 C13 C14 -0.7(5) . . . . ? C10 C12 C13 C14 177.0(4) . . . . ? C12 C13 C14 N3 0.8(5) . . . . ? C12 C13 C14 C15 -178.4(4) . . . . ? N3 C14 C15 C16 -1.0(7) . . . . ? C13 C14 C15 C16 178.1(5) . . . . ? C14 C15 C16 N4 0.9(7) . . . . ? C14 C15 C16 C17 -177.9(4) . . . . ? C15 C16 C17 C18 179.4(4) . . . . ? N4 C16 C17 C18 0.5(5) . . . . ? C15 C16 C17 C24 -2.1(7) . . . . ? N4 C16 C17 C24 179.0(4) . . . . ? C16 C17 C18 C19 -0.4(5) . . . . ? C24 C17 C18 C19 -178.9(4) . . . . ? C16 C17 C18 C26 179.9(4) . . . . ? C24 C17 C18 C26 1.4(8) . . . . ? C17 C18 C19 N4 0.2(5) . . . . ? C26 C18 C19 N4 179.9(4) . . . . ? C3 C2 C20 C21 169.6(12) . . . . ? C1 C2 C20 C21 -4(2) . . . . ? C20B C2 C20 C21 -137(9) . . . . ? C2 C3 C22 C23 -88.1(7) . . . . ? C4 C3 C22 C23 93.5(7) . . . . ? C18 C17 C24 C25 89.7(6) . . . . ? C16 C17 C24 C25 -88.5(6) . . . . ? C17 C18 C26 C27 164.2(5) . . . . ? C19 C18 C26 C27 -15.4(7) . . . . ? N5 C28 C29 C30 0.3(6) . . . . ? N5 C28 C29 C47 176.7(5) . . . . ? C28 C29 C30 C31 -0.8(6) . . . . ? C47 C29 C30 C31 -177.0(5) . . . . ? C28 C29 C30 C49 174.6(6) . . . . ? C47 C29 C30 C49 -1.6(10) . . . . ? C29 C30 C31 N5 1.1(6) . . . . ? C49 C30 C31 N5 -174.5(5) . . . . ? C29 C30 C31 C32 178.8(5) . . . . ? C49 C30 C31 C32 3.2(9) . . . . ? N5 C31 C32 C33 1.8(8) . . . . ? C30 C31 C32 C33 -175.6(5) . . . . ? C31 C32 C33 N6 0.4(8) . . . . ? C31 C32 C33 C34 179.3(5) . . . . ? C32 C33 C34 C35 -179.2(5) . . . . ? N6 C33 C34 C35 -0.2(5) . . . . ? C33 C34 C35 C36 0.1(5) . . . . ? C33 C34 C35 C37 177.6(4) . . . . ? C34 C35 C36 N6 0.1(5) . . . . ? C37 C35 C36 N6 -177.5(4) . . . . ? C34 C35 C37 C39 133.6(5) . . . . ? C36 C35 C37 C39 -49.3(6) . . . . ? N7 C38 C39 C40 -0.1(5) . . . . ? N7 C38 C39 C37 -175.9(4) . . . . ? C35 C37 C39 C40 138.5(4) . . . . ? C35 C37 C39 C38 -46.6(6) . . . . ? C38 C39 C40 C41 -0.2(4) . . . . ? C37 C39 C40 C41 175.5(4) . . . . ? C39 C40 C41 C42 -179.6(4) . . . . ? C39 C40 C41 N7 0.5(5) . . . . ? N7 C41 C42 C43 1.5(7) . . . . ? C40 C41 C42 C43 -178.3(4) . . . . ? C41 C42 C43 N8 4.1(7) . . . . ? C41 C42 C43 C44 -174.4(4) . . . . ? C42 C43 C44 C45 179.3(4) . . . . ? N8 C43 C44 C45 0.7(5) . . . . ? C42 C43 C44 C51 2.1(7) . . . . ? N8 C43 C44 C51 -176.5(4) . . . . ? C43 C44 C45 C46 -0.1(5) . . . . ? C51 C44 C45 C46 177.0(5) . . . . ? C43 C44 C45 C53 -178.1(5) . . . . ? C51 C44 C45 C53 -1.0(8) . . . . ? C44 C45 C46 N8 -0.5(5) . . . . ? C53 C45 C46 N8 177.5(4) . . . . ? C30 C29 C47 C48 124.0(7) . . . . ? C28 C29 C47 C48 -51.5(8) . . . . ? C29 C30 C49 C50 -97.1(7) . . . . ? C31 C30 C49 C50 77.6(8) . . . . ? C45 C44 C51 C52 -89.1(6) . . . . ? C43 C44 C51 C52 87.5(6) . . . . ? C44 C45 C53 C54 96.6(7) . . . . ? C46 C45 C53 C54 -81.0(6) . . . . ? N9 C55 C56 C57 -0.3(6) . . . . ? N9 C55 C56 C74 174.4(14) . . . . ? N9 C55 C56 C74B -174(2) . . . . ? C55 C56 C57 C58 -0.7(5) . . . . ? C74 C56 C57 C58 -175.2(16) . . . . ? C74B C56 C57 C58 173(2) . . . . ? C55 C56 C57 C76 173.8(5) . . . . ? C74 C56 C57 C76 -0.7(17) . . . . ? C74B C56 C57 C76 -13(3) . . . . ? C56 C57 C58 C59 -178.3(5) . . . . ? C76 C57 C58 C59 7.0(8) . . . . ? C56 C57 C58 N9 1.4(5) . . . . ? C76 C57 C58 N9 -173.2(5) . . . . ? N9 C58 C59 C60 2.6(8) . . . . ? C57 C58 C59 C60 -177.6(5) . . . . ? C58 C59 C60 N10 2.9(8) . . . . ? C58 C59 C60 C61 -175.5(5) . . . . ? C59 C60 C61 C62 178.5(5) . . . . ? N10 C60 C61 C62 0.0(5) . . . . ? C60 C61 C62 C63 0.1(5) . . . . ? C60 C61 C62 C64 177.4(4) . . . . ? C61 C62 C63 N10 -0.2(5) . . . . ? C64 C62 C63 N10 -177.5(4) . . . . ? C61 C62 C64 C66 144.7(5) . . . . ? C63 C62 C64 C66 -38.6(6) . . . . ? N11 C65 C66 C67 0.2(5) . . . . ? N11 C65 C66 C64 -177.4(4) . . . . ? C62 C64 C66 C67 128.4(5) . . . . ? C62 C64 C66 C65 -54.6(6) . . . . ? C65 C66 C67 C68 -0.3(5) . . . . ? C64 C66 C67 C68 177.1(5) . . . . ? C66 C67 C68 C69 178.3(5) . . . . ? C66 C67 C68 N11 0.3(5) . . . . ? N11 C68 C69 C70 -2.9(8) . . . . ? C67 C68 C69 C70 179.4(5) . . . . ? C68 C69 C70 N12 1.2(8) . . . . ? C68 C69 C70 C71 -176.1(5) . . . . ? C69 C70 C71 C72 176.6(5) . . . . ? N12 C70 C71 C72 -0.9(5) . . . . ? C69 C70 C71 C78 -2.4(9) . . . . ? N12 C70 C71 C78 180.0(5) . . . . ? C70 C71 C72 C73 1.1(5) . . . . ? C78 C71 C72 C73 -179.8(5) . . . . ? C70 C71 C72 C80 -176.2(5) . . . . ? C78 C71 C72 C80 2.9(9) . . . . ? C71 C72 C73 N12 -0.9(6) . . . . ? C80 C72 C73 N12 176.6(4) . . . . ? C57 C56 C74 C75 108(4) . . . . ? C55 C56 C74 C75 -65(4) . . . . ? C74B C56 C74 C75 -138(38) . . . . ? C56 C57 C76 C77 -89.0(8) . . . . ? C58 C57 C76 C77 84.5(7) . . . . ? C72 C71 C78 C79 -75.9(7) . . . . ? C70 C71 C78 C79 103.0(6) . . . . ? C71 C72 C80 C81 103.2(6) . . . . ? C73 C72 C80 C81 -73.7(6) . . . . ? C2 C1 N1 C4 0.6(5) . . . . ? C2 C1 N1 Co1 178.5(3) . . . . ? C5 C4 N1 C1 -176.2(4) . . . . ? C3 C4 N1 C1 0.0(5) . . . . ? C5 C4 N1 Co1 5.9(6) . . . . ? C3 C4 N1 Co1 -177.9(3) . . . . ? C8 C9 N2 C6 -0.6(5) . . . . ? C8 C9 N2 Co1 179.5(3) . . . . ? C5 C6 N2 C9 177.4(4) . . . . ? C7 C6 N2 C9 -0.4(5) . . . . ? C5 C6 N2 Co1 -2.6(6) . . . . ? C7 C6 N2 Co1 179.5(3) . . . . ? C12 C11 N3 C14 0.1(5) . . . . ? C12 C11 N3 Co2 178.0(3) . . . . ? C15 C14 N3 C11 178.7(4) . . . . ? C13 C14 N3 C11 -0.6(5) . . . . ? C15 C14 N3 Co2 0.8(6) . . . . ? C13 C14 N3 Co2 -178.4(3) . . . . ? C18 C19 N4 C16 0.1(5) . . . . ? C18 C19 N4 Co2 -178.7(3) . . . . ? C15 C16 N4 C19 -179.4(4) . . . . ? C17 C16 N4 C19 -0.4(4) . . . . ? C15 C16 N4 Co2 -0.5(6) . . . . ? C17 C16 N4 Co2 178.5(3) . . . . ? C29 C28 N5 C31 0.3(6) . . . . ? C29 C28 N5 Co1 -173.0(3) . . . . ? C32 C31 N5 C28 -178.7(5) . . . . ? C30 C31 N5 C28 -0.9(5) . . . . ? C32 C31 N5 Co1 -5.2(7) . . . . ? C30 C31 N5 Co1 172.6(3) . . . . ? C35 C36 N6 C33 -0.3(5) . . . . ? C35 C36 N6 Co1 178.1(3) . . . . ? C32 C33 N6 C36 179.3(5) . . . . ? C34 C33 N6 C36 0.3(5) . . . . ? C32 C33 N6 Co1 1.0(7) . . . . ? C34 C33 N6 Co1 -178.1(3) . . . . ? C39 C38 N7 C41 0.5(5) . . . . ? C39 C38 N7 Co2 -173.7(3) . . . . ? C42 C41 N7 C38 179.5(4) . . . . ? C40 C41 N7 C38 -0.6(4) . . . . ? C42 C41 N7 Co2 -6.1(6) . . . . ? C40 C41 N7 Co2 173.8(3) . . . . ? C45 C46 N8 C43 1.0(5) . . . . ? C45 C46 N8 Co2 -174.2(3) . . . . ? C42 C43 N8 C46 -179.7(4) . . . . ? C44 C43 N8 C46 -1.0(5) . . . . ? C42 C43 N8 Co2 -4.5(6) . . . . ? C44 C43 N8 Co2 174.2(3) . . . . ? C56 C55 N9 C58 1.2(5) . . . . ? C56 C55 N9 Co1 -172.7(3) . . . . ? C59 C58 N9 C55 178.2(4) . . . . ? C57 C58 N9 C55 -1.6(5) . . . . ? C59 C58 N9 Co1 -7.7(6) . . . . ? C57 C58 N9 Co1 172.5(3) . . . . ? C62 C63 N10 C60 0.3(5) . . . . ? C62 C63 N10 Co1 -175.7(3) . . . . ? C59 C60 N10 C63 -178.8(4) . . . . ? C61 C60 N10 C63 -0.2(5) . . . . ? C59 C60 N10 Co1 -2.7(6) . . . . ? C61 C60 N10 Co1 175.9(3) . . . . ? C66 C65 N11 C68 0.0(5) . . . . ? C66 C65 N11 Co2 179.1(3) . . . . ? C69 C68 N11 C65 -178.2(5) . . . . ? C67 C68 N11 C65 -0.1(5) . . . . ? C69 C68 N11 Co2 2.6(7) . . . . ? C67 C68 N11 Co2 -179.3(3) . . . . ? C72 C73 N12 C70 0.3(5) . . . . ? C72 C73 N12 Co2 -177.7(3) . . . . ? C69 C70 N12 C73 -177.4(4) . . . . ? C71 C70 N12 C73 0.4(5) . . . . ? C69 C70 N12 Co2 0.6(7) . . . . ? C71 C70 N12 Co2 178.4(3) . . . . ? C9 N2 Co1 N10 98.5(4) . . . . ? C6 N2 Co1 N10 -81.4(4) . . . . ? C9 N2 Co1 N6 9.5(4) . . . . ? C6 N2 Co1 N6 -170.5(4) . . . . ? C9 N2 Co1 N9 -52(2) . . . . ? C6 N2 Co1 N9 128.1(18) . . . . ? C9 N2 Co1 N1 -174.3(4) . . . . ? C6 N2 Co1 N1 5.7(4) . . . . ? C9 N2 Co1 N5 -83.9(4) . . . . ? C6 N2 Co1 N5 96.1(4) . . . . ? C63 N10 Co1 N2 -3.7(4) . . . . ? C60 N10 Co1 N2 -178.9(3) . . . . ? C63 N10 Co1 N6 86.7(4) . . . . ? C60 N10 Co1 N6 -88.5(3) . . . . ? C63 N10 Co1 N9 174.0(4) . . . . ? C60 N10 Co1 N9 -1.2(3) . . . . ? C63 N10 Co1 N1 -96.7(4) . . . . ? C60 N10 Co1 N1 88.1(3) . . . . ? C63 N10 Co1 N5 -50(3) . . . . ? C60 N10 Co1 N5 135(3) . . . . ? C36 N6 Co1 N2 91.8(4) . . . . ? C33 N6 Co1 N2 -90.2(4) . . . . ? C36 N6 Co1 N10 1.3(4) . . . . ? C33 N6 Co1 N10 179.3(4) . . . . ? C36 N6 Co1 N9 -92.3(4) . . . . ? C33 N6 Co1 N9 85.7(4) . . . . ? C36 N6 Co1 N1 -40.2(19) . . . . ? C33 N6 Co1 N1 137.8(16) . . . . ? C36 N6 Co1 N5 178.9(4) . . . . ? C33 N6 Co1 N5 -3.0(4) . . . . ? C55 N9 Co1 N2 -31(2) . . . . ? C58 N9 Co1 N2 156.6(18) . . . . ? C55 N9 Co1 N10 179.0(4) . . . . ? C58 N9 Co1 N10 6.2(4) . . . . ? C55 N9 Co1 N6 -92.2(4) . . . . ? C58 N9 Co1 N6 95.1(4) . . . . ? C55 N9 Co1 N1 91.9(4) . . . . ? C58 N9 Co1 N1 -80.9(4) . . . . ? C55 N9 Co1 N5 1.3(4) . . . . ? C58 N9 Co1 N5 -171.4(4) . . . . ? C1 N1 Co1 N2 175.2(4) . . . . ? C4 N1 Co1 N2 -7.3(4) . . . . ? C1 N1 Co1 N10 -94.5(4) . . . . ? C4 N1 Co1 N10 83.0(4) . . . . ? C1 N1 Co1 N6 -52.9(19) . . . . ? C4 N1 Co1 N6 124.6(16) . . . . ? C1 N1 Co1 N9 -0.9(4) . . . . ? C4 N1 Co1 N9 176.6(4) . . . . ? C1 N1 Co1 N5 88.0(4) . . . . ? C4 N1 Co1 N5 -94.5(4) . . . . ? C28 N5 Co1 N2 -92.6(4) . . . . ? C31 N5 Co1 N2 95.3(4) . . . . ? C28 N5 Co1 N10 -47(3) . . . . ? C31 N5 Co1 N10 141(2) . . . . ? C28 N5 Co1 N6 177.2(4) . . . . ? C31 N5 Co1 N6 5.1(4) . . . . ? C28 N5 Co1 N9 89.9(4) . . . . ? C31 N5 Co1 N9 -82.2(4) . . . . ? C28 N5 Co1 N1 0.4(4) . . . . ? C31 N5 Co1 N1 -171.7(4) . . . . ? C73 N12 Co2 N8 89.3(4) . . . . ? C70 N12 Co2 N8 -88.3(4) . . . . ? C73 N12 Co2 N3 -92.4(4) . . . . ? C70 N12 Co2 N3 90.0(4) . . . . ? C73 N12 Co2 N7 -63(3) . . . . ? C70 N12 Co2 N7 119(3) . . . . ? C73 N12 Co2 N11 177.0(4) . . . . ? C70 N12 Co2 N11 -0.6(4) . . . . ? C73 N12 Co2 N4 0.4(4) . . . . ? C70 N12 Co2 N4 -177.2(4) . . . . ? C46 N8 Co2 N12 -3.8(4) . . . . ? C43 N8 Co2 N12 -178.0(4) . . . . ? C46 N8 Co2 N3 -26(2) . . . . ? C43 N8 Co2 N3 160.1(18) . . . . ? C46 N8 Co2 N7 174.7(4) . . . . ? C43 N8 Co2 N7 0.6(4) . . . . ? C46 N8 Co2 N11 -97.0(4) . . . . ? C43 N8 Co2 N11 88.8(4) . . . . ? C46 N8 Co2 N4 87.2(4) . . . . ? C43 N8 Co2 N4 -87.0(3) . . . . ? C11 N3 Co2 N12 -87.1(4) . . . . ? C14 N3 Co2 N12 90.4(4) . . . . ? C11 N3 Co2 N8 -65(2) . . . . ? C14 N3 Co2 N8 112.4(19) . . . . ? C11 N3 Co2 N7 94.5(4) . . . . ? C14 N3 Co2 N7 -88.1(4) . . . . ? C11 N3 Co2 N11 6.1(4) . . . . ? C14 N3 Co2 N11 -176.5(4) . . . . ? C11 N3 Co2 N4 -177.9(4) . . . . ? C14 N3 Co2 N4 -0.4(4) . . . . ? C38 N7 Co2 N12 -30(3) . . . . ? C41 N7 Co2 N12 157(3) . . . . ? C38 N7 Co2 N8 177.6(3) . . . . ? C41 N7 Co2 N8 4.4(3) . . . . ? C38 N7 Co2 N3 -0.8(4) . . . . ? C41 N7 Co2 N3 -174.0(3) . . . . ? C38 N7 Co2 N11 90.0(4) . . . . ? C41 N7 Co2 N11 -83.2(3) . . . . ? C38 N7 Co2 N4 -93.7(4) . . . . ? C41 N7 Co2 N4 93.2(3) . . . . ? C65 N11 Co2 N12 -179.9(4) . . . . ? C68 N11 Co2 N12 -0.9(4) . . . . ? C65 N11 Co2 N8 -90.8(4) . . . . ? C68 N11 Co2 N8 88.2(4) . . . . ? C65 N11 Co2 N3 93.6(4) . . . . ? C68 N11 Co2 N3 -87.5(4) . . . . ? C65 N11 Co2 N7 2.8(4) . . . . ? C68 N11 Co2 N7 -178.2(4) . . . . ? C65 N11 Co2 N4 -39.7(18) . . . . ? C68 N11 Co2 N4 139.2(15) . . . . ? C19 N4 Co2 N12 92.3(4) . . . . ? C16 N4 Co2 N12 -86.3(3) . . . . ? C19 N4 Co2 N8 3.1(4) . . . . ? C16 N4 Co2 N8 -175.5(3) . . . . ? C19 N4 Co2 N3 178.9(4) . . . . ? C16 N4 Co2 N3 0.3(3) . . . . ? C19 N4 Co2 N7 -90.5(4) . . . . ? C16 N4 Co2 N7 90.9(3) . . . . ? C19 N4 Co2 N11 -47.9(18) . . . . ? C16 N4 Co2 N11 133.5(16) . . . . ? C57 C56 C74B C75B 76(7) . . . . ? C55 C56 C74B C75B -112(6) . . . . ? C74 C56 C74B C75B 1(29) . . . . ? C3 C2 C20B C21B -177.2(13) . . . . ? C1 C2 C20B C21B -11(3) . . . . ? C20 C2 C20B C21B 47(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.85 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.520 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.090 # 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 0.500 0.000 0.500 121 33 ' ' _platon_squeeze_details ; ; # Attachment 'CoMeso.cif' data_CoMeso _database_code_depnum_ccdc_archive 'CCDC 710493' _audit_update_record ; 2009-07-23 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C81 H90 Co2 N12' _chemical_formula_weight 1349.51 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' '-x+y, -x, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' '-x, -y, -z' 'x, y, -z-1/2' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, -x, -z-1/2' '-y, x-y, -z-1/2' _cell_length_a 15.0431(8) _cell_length_b 15.0431(8) _cell_length_c 24.400(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4781.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 9930 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 27.64 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details 'SADABS (Bruker, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(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 45184 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.80 _reflns_number_total 3875 _reflns_number_gt 3252 _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. The material crystallizes with the unique one-6th of the molecule residing on a 63 screw-axis. Additionally, one ethyl substituent is disordered and was modeled in two orientations. Finally, disordered solvent was present in the lattice, however the degree of disorder made it impossible to be reasonably modeled. As a result the PLATON/SQUEEZE (Sluis, 1990) program was used to generate a 'solvent-free' data set. EADP and EXYZ statements were used to maintain reasonable geometries and anisotropic displacement parameters for disordered fragments. ; _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^)+(0.0499P)^2^+0.7354P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3875 _refine_ls_number_parameters 158 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.094 _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 0.58775(9) 0.40236(10) 0.49123(5) 0.0262(3) Uani 1 1 d . A . H1 H 0.5459 0.3344 0.4780 0.031 Uiso 1 1 calc R . . C2 C 0.59677(10) 0.49116(11) 0.46510(5) 0.0294(3) Uani 1 1 d . . . C3 C 0.66232(10) 0.57351(10) 0.49692(5) 0.0294(3) Uani 1 1 d . A . C4 C 0.69346(10) 0.53282(9) 0.54187(5) 0.0244(3) Uani 1 1 d . . . C5 C 0.76186(10) 0.58685(10) 0.58319(5) 0.0257(3) Uani 1 1 d . A . H5 H 0.7883 0.6589 0.5836 0.031 Uiso 1 1 calc R . . C6 C 0.79652(9) 0.54779(9) 0.62440(5) 0.0225(2) Uani 1 1 d . . . C7 C 0.86626(9) 0.60295(9) 0.66740(5) 0.0257(3) Uani 1 1 d . A . H7 H 0.8987 0.6748 0.6736 0.031 Uiso 1 1 calc R . . C8 C 0.87826(9) 0.53328(9) 0.69850(4) 0.0225(2) Uani 1 1 d . . . C9 C 0.81507(9) 0.43646(9) 0.67369(4) 0.0212(2) Uani 1 1 d . A . H9 H 0.8083 0.3738 0.6867 0.025 Uiso 1 1 calc R . . C10 C 0.94084(13) 0.55157(14) 0.7500 0.0251(4) Uani 1 2 d S . . H10A H 0.9987 0.6232 0.7500 0.030 Uiso 1 2 calc SR . . H10B H 0.9700 0.5054 0.7500 0.030 Uiso 1 2 calc SR . . C11A C 0.54598(12) 0.49052(14) 0.41182(5) 0.0400(4) Uani 0.746(5) 1 d PD A 1 H11A H 0.5503 0.5578 0.4066 0.048 Uiso 0.746(5) 1 calc PR A 1 H11B H 0.4725 0.4372 0.4133 0.048 Uiso 0.746(5) 1 calc PR A 1 C12A C 0.5961(2) 0.4694(3) 0.36369(8) 0.0654(10) Uani 0.746(5) 1 d PD A 1 H12A H 0.6672 0.5253 0.3601 0.098 Uiso 0.746(5) 1 calc PR A 1 H12B H 0.5582 0.4646 0.3301 0.098 Uiso 0.746(5) 1 calc PR A 1 H12C H 0.5952 0.4045 0.3697 0.098 Uiso 0.746(5) 1 calc PR A 1 C13 C 0.69515(13) 0.68454(12) 0.48829(6) 0.0423(4) Uani 1 1 d . . . H13A H 0.7136 0.7201 0.5242 0.051 Uiso 1 1 calc R A . H13B H 0.6365 0.6894 0.4734 0.051 Uiso 1 1 calc R . . C14 C 0.78574(15) 0.73922(15) 0.44957(10) 0.0693(6) Uani 1 1 d . A . H14A H 0.8442 0.7348 0.4640 0.104 Uiso 1 1 calc R . . H14B H 0.8045 0.8115 0.4464 0.104 Uiso 1 1 calc R . . H14C H 0.7670 0.7067 0.4134 0.104 Uiso 1 1 calc R . . N1 N 0.64521(7) 0.42604(8) 0.53658(4) 0.0223(2) Uani 1 1 d . A . N2 N 0.76580(7) 0.44413(7) 0.62951(4) 0.0193(2) Uani 1 1 d . A . Co1 Co 0.6667 0.3333 0.583235(10) 0.01788(9) Uani 1 3 d S . . C11B C 0.54598(12) 0.49052(14) 0.41182(5) 0.0400(4) Uani 0.254(5) 1 d PD A 2 H11C H 0.5000 0.5186 0.4191 0.048 Uiso 0.254(5) 1 calc PR A 2 H11D H 0.6002 0.5389 0.3866 0.048 Uiso 0.254(5) 1 calc PR A 2 C12B C 0.4857(7) 0.3924(4) 0.3824(3) 0.070(3) Uani 0.254(5) 1 d PD A 2 H12D H 0.5301 0.3643 0.3730 0.104 Uiso 0.254(5) 1 calc PR A 2 H12E H 0.4574 0.4041 0.3488 0.104 Uiso 0.254(5) 1 calc PR A 2 H12F H 0.4294 0.3437 0.4059 0.104 Uiso 0.254(5) 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 0.0275(6) 0.0334(7) 0.0188(6) 0.0017(5) -0.0011(5) 0.0161(5) C2 0.0335(7) 0.0423(7) 0.0206(6) 0.0069(5) 0.0013(5) 0.0251(6) C3 0.0348(7) 0.0351(7) 0.0249(6) 0.0067(5) 0.0019(5) 0.0224(6) C4 0.0292(6) 0.0273(6) 0.0209(6) 0.0049(5) 0.0037(5) 0.0174(5) C5 0.0311(7) 0.0228(6) 0.0242(6) 0.0024(5) 0.0038(5) 0.0143(5) C6 0.0249(6) 0.0221(6) 0.0186(5) 0.0009(4) 0.0037(5) 0.0103(5) C7 0.0276(6) 0.0218(6) 0.0212(6) -0.0010(5) 0.0017(5) 0.0075(5) C8 0.0193(6) 0.0275(6) 0.0150(5) 0.0001(4) 0.0028(4) 0.0075(5) C9 0.0212(6) 0.0237(6) 0.0165(5) 0.0017(4) 0.0013(4) 0.0094(5) C10 0.0197(8) 0.0288(9) 0.0176(8) 0.000 0.000 0.0052(7) C11A 0.0439(8) 0.0580(10) 0.0258(7) 0.0087(6) -0.0041(6) 0.0313(8) C12A 0.096(2) 0.109(2) 0.0235(10) 0.0017(12) -0.0069(12) 0.075(2) C13 0.0554(9) 0.0379(8) 0.0410(8) 0.0091(6) -0.0058(7) 0.0289(7) C14 0.0522(11) 0.0489(11) 0.1012(16) 0.0338(11) 0.0063(11) 0.0211(9) N1 0.0248(5) 0.0269(5) 0.0166(4) 0.0025(4) 0.0012(4) 0.0140(4) N2 0.0209(5) 0.0215(5) 0.0147(4) 0.0010(4) 0.0018(4) 0.0100(4) Co1 0.02096(11) 0.02096(11) 0.01172(14) 0.000 0.000 0.01048(6) C11B 0.0439(8) 0.0580(10) 0.0258(7) 0.0087(6) -0.0041(6) 0.0313(8) C12B 0.104(7) 0.066(5) 0.044(4) -0.007(4) -0.034(4) 0.046(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.3380(15) . ? C1 C2 1.4242(17) . ? C1 H1 0.9500 . ? C2 C3 1.3742(19) . ? C2 C11A 1.5054(17) . ? C3 C4 1.4433(16) . ? C3 C13 1.5010(19) . ? C4 C5 1.3783(17) . ? C4 N1 1.3992(16) . ? C5 C6 1.3909(16) . ? C5 H5 0.9500 . ? C6 N2 1.3928(15) . ? C6 C7 1.4211(16) . ? C7 C8 1.3770(17) . ? C7 H7 0.9500 . ? C8 C9 1.4166(16) . ? C8 C10 1.5106(14) . ? C9 N2 1.3454(14) . ? C9 H9 0.9500 . ? C10 C8 1.5106(14) 8_557 ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11A C12A 1.512(3) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C13 C14 1.518(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? N1 Co1 1.9481(10) . ? N2 Co1 1.9471(9) . ? Co1 N2 1.9471(9) 4_665 ? Co1 N2 1.9471(9) 3_655 ? Co1 N1 1.9481(10) 3_655 ? Co1 N1 1.9481(10) 4_665 ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? 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 112.00(11) . . ? N1 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? C3 C2 C1 106.35(11) . . ? C3 C2 C11A 128.81(13) . . ? C1 C2 C11A 124.80(13) . . ? C2 C3 C4 106.60(11) . . ? C2 C3 C13 127.76(12) . . ? C4 C3 C13 125.63(12) . . ? C5 C4 N1 123.38(11) . . ? C5 C4 C3 127.63(12) . . ? N1 C4 C3 108.95(11) . . ? C4 C5 C6 127.35(12) . . ? C4 C5 H5 116.3 . . ? C6 C5 H5 116.3 . . ? C5 C6 N2 123.58(11) . . ? C5 C6 C7 127.61(11) . . ? N2 C6 C7 108.81(10) . . ? C8 C7 C6 107.57(11) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 105.73(10) . . ? C7 C8 C10 128.80(12) . . ? C9 C8 C10 125.42(12) . . ? N2 C9 C8 111.68(10) . . ? N2 C9 H9 124.2 . . ? C8 C9 H9 124.2 . . ? C8 C10 C8 112.58(13) . 8_557 ? C8 C10 H10A 109.1 . . ? C8 C10 H10A 109.1 8_557 . ? C8 C10 H10B 109.1 . . ? C8 C10 H10B 109.1 8_557 . ? H10A C10 H10B 107.8 . . ? C2 C11A C12A 111.55(14) . . ? C2 C11A H11A 109.3 . . ? C12A C11A H11A 109.3 . . ? C2 C11A H11B 109.3 . . ? C12A C11A H11B 109.3 . . ? H11A C11A H11B 108.0 . . ? C3 C13 C14 113.39(14) . . ? C3 C13 H13A 108.9 . . ? C14 C13 H13A 108.9 . . ? C3 C13 H13B 108.9 . . ? C14 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1 N1 C4 106.09(10) . . ? C1 N1 Co1 127.50(9) . . ? C4 N1 Co1 126.26(8) . . ? C9 N2 C6 106.21(9) . . ? C9 N2 Co1 127.60(8) . . ? C6 N2 Co1 126.14(8) . . ? N2 Co1 N2 89.75(4) 4_665 . ? N2 Co1 N2 89.75(4) 4_665 3_655 ? N2 Co1 N2 89.75(4) . 3_655 ? N2 Co1 N1 87.85(4) 4_665 3_655 ? N2 Co1 N1 176.17(4) . 3_655 ? N2 Co1 N1 93.22(4) 3_655 3_655 ? N2 Co1 N1 93.22(4) 4_665 4_665 ? N2 Co1 N1 87.85(4) . 4_665 ? N2 Co1 N1 176.17(4) 3_655 4_665 ? N1 Co1 N1 89.30(4) 3_655 4_665 ? N2 Co1 N1 176.17(4) 4_665 . ? N2 Co1 N1 93.22(4) . . ? N2 Co1 N1 87.85(4) 3_655 . ? N1 Co1 N1 89.30(4) 3_655 . ? N1 Co1 N1 89.30(4) 4_665 . ? H12D C12B H12E 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? 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 -0.99(15) . . . . ? N1 C1 C2 C11A 176.78(12) . . . . ? C1 C2 C3 C4 0.87(14) . . . . ? C11A C2 C3 C4 -176.78(13) . . . . ? C1 C2 C3 C13 -178.19(13) . . . . ? C11A C2 C3 C13 4.2(2) . . . . ? C2 C3 C4 C5 177.37(12) . . . . ? C13 C3 C4 C5 -3.6(2) . . . . ? C2 C3 C4 N1 -0.51(14) . . . . ? C13 C3 C4 N1 178.57(13) . . . . ? N1 C4 C5 C6 2.0(2) . . . . ? C3 C4 C5 C6 -175.56(12) . . . . ? C4 C5 C6 N2 0.4(2) . . . . ? C4 C5 C6 C7 -179.36(12) . . . . ? C5 C6 C7 C8 179.95(12) . . . . ? N2 C6 C7 C8 0.17(13) . . . . ? C6 C7 C8 C9 -0.07(13) . . . . ? C6 C7 C8 C10 -177.54(12) . . . . ? C7 C8 C9 N2 -0.06(13) . . . . ? C10 C8 C9 N2 177.52(11) . . . . ? C7 C8 C10 C8 93.96(17) . . . 8_557 ? C9 C8 C10 C8 -83.05(18) . . . 8_557 ? C3 C2 C11A C12A 105.2(2) . . . . ? C1 C2 C11A C12A -72.1(2) . . . . ? C2 C3 C13 C14 -85.16(19) . . . . ? C4 C3 C13 C14 95.96(17) . . . . ? C2 C1 N1 C4 0.65(13) . . . . ? C2 C1 N1 Co1 -175.10(8) . . . . ? C5 C4 N1 C1 -178.08(11) . . . . ? C3 C4 N1 C1 -0.09(13) . . . . ? C5 C4 N1 Co1 -2.25(17) . . . . ? C3 C4 N1 Co1 175.74(8) . . . . ? C8 C9 N2 C6 0.16(12) . . . . ? C8 C9 N2 Co1 -177.40(8) . . . . ? C5 C6 N2 C9 -179.99(11) . . . . ? C7 C6 N2 C9 -0.20(12) . . . . ? C5 C6 N2 Co1 -2.38(16) . . . . ? C7 C6 N2 Co1 177.41(8) . . . . ? C9 N2 Co1 N2 1.24(9) . . . 4_665 ? C6 N2 Co1 N2 -175.86(9) . . . 4_665 ? C9 N2 Co1 N2 90.99(7) . . . 3_655 ? C6 N2 Co1 N2 -86.11(11) . . . 3_655 ? C9 N2 Co1 N1 -50.0(6) . . . 3_655 ? C6 N2 Co1 N1 132.9(6) . . . 3_655 ? C9 N2 Co1 N1 -91.99(9) . . . 4_665 ? C6 N2 Co1 N1 90.91(9) . . . 4_665 ? C9 N2 Co1 N1 178.83(9) . . . . ? C6 N2 Co1 N1 1.73(9) . . . . ? C1 N1 Co1 N2 -43.7(6) . . . 4_665 ? C4 N1 Co1 N2 141.4(6) . . . 4_665 ? C1 N1 Co1 N2 175.42(10) . . . . ? C4 N1 Co1 N2 0.48(10) . . . . ? C1 N1 Co1 N2 -94.95(10) . . . 3_655 ? C4 N1 Co1 N2 90.11(10) . . . 3_655 ? C1 N1 Co1 N1 -1.70(10) . . . 3_655 ? C4 N1 Co1 N1 -176.64(9) . . . 3_655 ? C1 N1 Co1 N1 87.61(8) . . . 4_665 ? C4 N1 Co1 N1 -87.33(11) . . . 4_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.80 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.319 _refine_diff_density_min -0.234 _refine_diff_density_rms 0.042