# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_author_name G.Brewer _publ_contact_author_name 'Greg Brewer' _publ_contact_author_email brewer@cua.edu data_1349 _database_code_depnum_ccdc_archive 'CCDC 609761' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Manganese perchlorate complex ; _chemical_name_common 'Manganese perchlorate complex' _chemical_formula_moiety '2(C21 H30 Mn N10), 4(Cl O4), 3.4(H2 O)' _chemical_formula_sum 'C42 H66.82 Cl4 Mn2 N20 O19.41' _chemical_formula_weight 1414.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P 21 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 18.3957(4) _cell_length_b 18.3957(4) _cell_length_c 18.3957(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6225.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 7615 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 22.4 _exptl_crystal_description plate _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method not-measured _exptl_crystal_F_000 2928 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.717 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'three-circle diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 41661 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.04 _reflns_number_total 3661 _reflns_number_gt 3082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker, 1999)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.012P)^2^+6.04P], P=(max(Fo^2^,0)+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_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 3661 # 2008 w/o Fiedel pairs _refine_ls_number_parameters 339 _refine_ls_number_restraints 149 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.36159(3) 0.13841(3) 0.86159(3) 0.0606(3) Uani 1 3 d S . . N11 N 0.26837(15) 0.23163(15) 0.76837(15) 0.0641(14) Uani 1 3 d S . . N12 N 0.39643(16) 0.25623(18) 0.84895(17) 0.0620(8) Uani 1 1 d . . . N13 N 0.42108(19) 0.1729(2) 0.96729(18) 0.0681(9) Uani 1 1 d . . . N14 N 0.44036(18) 0.1483(2) 1.03373(19) 0.0750(10) Uani 1 1 d . . . H14 H 0.4341 0.1037 1.0480 0.090 Uiso 1 1 calc R . . C11 C 0.2988(2) 0.3046(2) 0.7745(2) 0.0719(11) Uani 1 1 d . . . H11A H 0.2763 0.3299 0.8156 0.086 Uiso 1 1 calc R . . H11B H 0.2880 0.3322 0.7302 0.086 Uiso 1 1 calc R . . C12 C 0.3805(2) 0.3012(2) 0.7856(2) 0.0739(12) Uani 1 1 d . . . H12A H 0.4038 0.2805 0.7424 0.089 Uiso 1 1 calc R . . H12B H 0.3998 0.3503 0.7930 0.089 Uiso 1 1 calc R . . C13 C 0.4249(2) 0.2868(2) 0.9048(2) 0.0652(10) Uani 1 1 d . . . H13 H 0.4358 0.3368 0.9043 0.078 Uiso 1 1 calc R . . C14 C 0.4398(2) 0.2433(2) 0.9684(2) 0.0622(9) Uani 1 1 d . . . C15 C 0.4714(2) 0.2618(3) 1.0349(2) 0.0715(11) Uani 1 1 d . . . H15 H 0.4897 0.3075 1.0486 0.086 Uiso 1 1 calc R . . C16 C 0.4703(2) 0.2005(3) 1.0756(2) 0.0705(11) Uani 1 1 d . . . C17 C 0.4958(3) 0.1843(3) 1.1513(3) 0.0985(16) Uani 1 1 d . . . H17A H 0.4973 0.2290 1.1792 0.148 Uiso 1 1 calc R . . H17B H 0.5441 0.1631 1.1494 0.148 Uiso 1 1 calc R . . H17C H 0.4626 0.1504 1.1741 0.148 Uiso 1 1 calc R . . Mn2 Mn 0.24228(3) 0.74228(3) 0.75772(3) 0.0654(3) Uani 1 3 d S . . N21 N 0.33043(18) 0.83043(18) 0.66957(18) 0.0707(16) Uani 1 3 d S . . N22 N 0.23922(19) 0.86061(19) 0.78747(17) 0.0677(8) Uani 1 1 d . . . N23 N 0.12763(18) 0.76850(19) 0.8033(2) 0.0772(10) Uani 1 1 d . . . N24 N 0.0646(2) 0.7363(2) 0.8207(2) 0.0856(11) Uani 1 1 d . . . H24 H 0.0555 0.6907 0.8125 0.103 Uiso 1 1 calc R . . C21 C 0.3155(3) 0.9051(2) 0.6909(3) 0.0810(13) Uani 1 1 d . . . H21A H 0.2738 0.9234 0.6631 0.097 Uiso 1 1 calc R . . H21B H 0.3576 0.9356 0.6793 0.097 Uiso 1 1 calc R . . C22 C 0.2991(3) 0.9105(2) 0.7710(3) 0.0812(13) Uani 1 1 d . . . H22A H 0.3423 0.8973 0.7993 0.097 Uiso 1 1 calc R . . H22B H 0.2854 0.9604 0.7835 0.097 Uiso 1 1 calc R . . C23 C 0.1801(2) 0.8864(2) 0.8117(2) 0.0679(11) Uani 1 1 d . . . H23 H 0.1754 0.9364 0.8213 0.081 Uiso 1 1 calc R . . C24 C 0.1195(2) 0.8370(2) 0.8246(2) 0.0618(10) Uani 1 1 d . . . C25 C 0.0513(2) 0.8476(2) 0.8551(2) 0.0682(10) Uani 1 1 d . . . H25 H 0.0326 0.8913 0.8739 0.082 Uiso 1 1 calc R . . C26 C 0.0168(2) 0.7820(2) 0.8523(2) 0.0725(11) Uani 1 1 d . . . C27 C -0.0567(2) 0.7573(3) 0.8760(3) 0.0968(15) Uani 1 1 d . . . H27A H -0.0936 0.7864 0.8521 0.145 Uiso 1 1 calc R . . H27B H -0.0611 0.7628 0.9282 0.145 Uiso 1 1 calc R . . H27C H -0.0632 0.7066 0.8631 0.145 Uiso 1 1 calc R . . Cl1 Cl 0.51400(8) 0.84483(8) 0.90515(8) 0.0783(4) Uani 0.803(2) 1 d PDU A 1 O11 O 0.5858(2) 0.8433(3) 0.8863(3) 0.1279(18) Uani 0.803(2) 1 d PDU A 1 O12 O 0.4998(3) 0.9071(3) 0.9477(3) 0.150(2) Uani 0.803(2) 1 d PDU A 1 O13 O 0.4700(4) 0.8577(5) 0.8451(4) 0.211(3) Uani 0.803(2) 1 d PDU A 1 O14 O 0.4910(4) 0.7817(3) 0.9375(5) 0.205(3) Uani 0.803(2) 1 d PDU A 1 Cl1A Cl 0.5706(3) 0.7467(5) 0.9482(4) 0.103(2) Uani 0.197(2) 1 d PDU A 2 O11A O 0.6308(11) 0.7030(15) 0.9521(16) 0.123(8) Uani 0.197(2) 1 d PDU A 2 O12A O 0.5722(12) 0.8026(10) 0.9990(10) 0.143(7) Uani 0.197(2) 1 d PDU A 2 O13A O 0.5106(10) 0.7018(12) 0.9634(11) 0.156(8) Uani 0.197(2) 1 d PDU A 2 O14A O 0.5546(14) 0.7772(12) 0.8815(8) 0.148(8) Uani 0.197(2) 1 d PDU A 2 Cl2 Cl 0.51377(7) 0.48623(7) -0.01377(7) 0.1033(7) Uani 0.617(15) 3 d SPDU B 1 O21 O 0.5561(3) 0.4439(3) -0.0561(3) 0.162(7) Uani 0.617(15) 3 d SPDU B 1 O22 O 0.5282(7) 0.4736(7) 0.0607(4) 0.201(6) Uani 0.617(15) 1 d PDU B 1 Cl2A Cl 0.51377(7) 0.48623(7) -0.01377(7) 0.1033(7) Uani 0.383(15) 3 d SPDU B 2 O21A O 0.4711(3) 0.5289(3) 0.0289(3) 0.118(8) Uani 0.383(15) 3 d SPDU B 2 O22A O 0.5319(12) 0.4215(9) 0.0197(12) 0.234(11) Uani 0.383(15) 1 d PDU B 2 O1W O 0.0926(3) 0.5926(3) 0.9074(3) 0.185(4) Uani 1 3 d SU . . O2W O 0.6300(4) 0.7134(6) 0.9917(6) 0.099(4) Uani 0.509(15) 1 d PU C 3 O3W O 0.6018(16) 0.6621(13) 0.9424(15) 0.174(11) Uani 0.295(15) 1 d PU C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0606(3) 0.0606(3) 0.0606(3) 0.0038(3) -0.0038(3) 0.0038(3) N11 0.0641(14) 0.0641(14) 0.0641(14) 0.0089(15) -0.0089(15) 0.0089(15) N12 0.0577(17) 0.0645(19) 0.0639(19) 0.0085(17) -0.0041(15) 0.0015(16) N13 0.067(2) 0.081(2) 0.0560(19) 0.0071(17) -0.0048(16) 0.0052(18) N14 0.071(2) 0.086(2) 0.068(2) 0.014(2) -0.0084(18) 0.008(2) C11 0.082(3) 0.061(2) 0.073(3) 0.015(2) -0.015(2) 0.010(2) C12 0.086(3) 0.069(3) 0.067(3) 0.018(2) -0.009(2) -0.011(2) C13 0.057(2) 0.067(2) 0.072(3) 0.002(2) 0.000(2) -0.0012(19) C14 0.059(2) 0.066(2) 0.061(2) -0.001(2) -0.0020(17) -0.002(2) C15 0.055(2) 0.086(3) 0.074(3) -0.008(2) -0.004(2) 0.001(2) C16 0.054(2) 0.095(3) 0.062(2) -0.006(2) -0.006(2) 0.003(2) C17 0.085(3) 0.137(5) 0.074(3) 0.006(3) -0.026(3) 0.006(3) Mn2 0.0654(3) 0.0654(3) 0.0654(3) 0.0025(3) 0.0025(3) -0.0025(3) N21 0.0707(16) 0.0707(16) 0.0707(16) 0.0063(16) 0.0063(16) -0.0063(16) N22 0.071(2) 0.067(2) 0.0655(19) 0.0021(16) 0.0029(17) -0.0101(19) N23 0.060(2) 0.071(2) 0.101(3) -0.002(2) 0.0133(19) -0.0052(18) N24 0.073(2) 0.067(2) 0.116(3) -0.001(2) 0.019(2) -0.006(2) C21 0.081(3) 0.070(3) 0.092(3) 0.009(2) 0.006(3) -0.018(2) C22 0.076(3) 0.071(3) 0.096(4) -0.003(2) -0.005(3) -0.016(2) C23 0.081(3) 0.062(2) 0.061(2) -0.0063(19) -0.014(2) -0.005(2) C24 0.066(2) 0.068(3) 0.051(2) -0.0008(18) -0.0056(18) 0.000(2) C25 0.067(2) 0.078(3) 0.060(2) -0.011(2) -0.006(2) 0.011(2) C26 0.069(3) 0.086(3) 0.063(2) 0.002(2) 0.004(2) 0.007(2) C27 0.072(3) 0.118(4) 0.100(4) 0.006(3) 0.018(3) -0.002(3) Cl1 0.0722(9) 0.0773(9) 0.0855(10) -0.0034(7) 0.0037(7) -0.0012(7) O11 0.082(3) 0.165(5) 0.136(4) -0.023(4) 0.020(3) -0.006(3) O12 0.118(4) 0.156(4) 0.176(5) -0.076(4) -0.011(3) 0.034(4) O13 0.174(5) 0.307(9) 0.151(5) -0.021(5) -0.085(5) 0.032(6) O14 0.152(5) 0.130(4) 0.333(10) 0.077(5) 0.053(6) -0.012(4) Cl1A 0.072(4) 0.149(7) 0.086(4) -0.032(4) 0.013(3) -0.011(4) O11A 0.115(10) 0.147(16) 0.107(15) 0.008(13) 0.034(13) 0.016(10) O12A 0.148(14) 0.152(13) 0.128(10) -0.057(10) 0.084(11) -0.040(10) O13A 0.118(10) 0.223(16) 0.128(14) -0.032(11) 0.011(11) -0.072(11) O14A 0.184(17) 0.139(16) 0.121(8) -0.001(9) -0.002(11) 0.028(13) Cl2 0.1033(7) 0.1033(7) 0.1033(7) -0.0192(7) 0.0192(7) 0.0192(7) O21 0.162(7) 0.162(7) 0.162(7) -0.052(4) 0.052(4) 0.052(4) O22 0.247(12) 0.260(14) 0.095(4) -0.010(6) 0.017(6) -0.007(10) Cl2A 0.1033(7) 0.1033(7) 0.1033(7) -0.0192(7) 0.0192(7) 0.0192(7) O21A 0.118(8) 0.118(8) 0.118(8) -0.024(4) 0.024(4) 0.024(4) O22A 0.207(15) 0.163(11) 0.33(2) 0.051(11) -0.026(14) 0.097(11) O1W 0.185(4) 0.185(4) 0.185(4) 0.044(3) 0.044(3) -0.044(3) O2W 0.073(5) 0.134(8) 0.092(7) 0.035(5) -0.010(4) -0.007(4) O3W 0.202(18) 0.121(14) 0.199(17) -0.003(12) 0.057(14) 0.046(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 N12 2.272(3) 12_565 ? Mn1 N12 2.272(3) 6_456 ? Mn1 N12 2.272(3) . ? Mn1 N13 2.320(4) 12_565 ? Mn1 N13 2.320(4) 6_456 ? Mn1 N13 2.320(4) . ? N11 C11 1.459(4) 12_565 ? N11 C11 1.459(4) . ? N11 C11 1.459(4) 6_456 ? N12 C13 1.283(5) . ? N12 C12 1.459(5) . ? N13 C14 1.341(5) . ? N13 N14 1.350(4) . ? N14 C16 1.348(5) . ? N14 H14 0.8700 . ? C11 C12 1.519(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 C14 1.444(5) . ? C13 H13 0.9400 . ? C14 C15 1.397(5) . ? C15 C16 1.353(6) . ? C15 H15 0.9400 . ? C16 C17 1.499(6) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? Mn2 N22 2.245(4) 8_656 ? Mn2 N22 2.245(4) . ? Mn2 N22 2.245(4) 11_466 ? Mn2 N23 2.321(3) . ? Mn2 N23 2.321(3) 8_656 ? Mn2 N23 2.321(3) 11_466 ? N21 C21 1.455(5) . ? N21 C21 1.455(5) 8_656 ? N21 C21 1.455(5) 11_466 ? N22 C23 1.268(5) . ? N22 C22 1.466(5) . ? N23 C24 1.328(5) . ? N23 N24 1.341(5) . ? N24 C26 1.347(5) . ? N24 H24 0.8700 . ? C21 C22 1.507(6) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.457(6) . ? C23 H23 0.9400 . ? C24 C25 1.389(6) . ? C25 C26 1.364(6) . ? C25 H25 0.9400 . ? C26 C27 1.491(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? Cl1 O11 1.366(4) . ? Cl1 O14 1.371(6) . ? Cl1 O13 1.390(5) . ? Cl1 O12 1.412(5) . ? Cl2 O21 1.347(8) . ? Cl2 O22 1.414(7) . ? Cl2 O22 1.414(7) 10_655 ? Cl2 O22 1.414(7) 7_564 ? 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 N12 Mn1 N12 101.56(10) 12_565 6_456 ? N12 Mn1 N12 101.56(10) 12_565 . ? N12 Mn1 N12 101.56(10) 6_456 . ? N12 Mn1 N13 72.05(12) 12_565 12_565 ? N12 Mn1 N13 100.70(11) 6_456 12_565 ? N12 Mn1 N13 157.67(12) . 12_565 ? N12 Mn1 N13 157.67(12) 12_565 6_456 ? N12 Mn1 N13 72.05(12) 6_456 6_456 ? N12 Mn1 N13 100.70(11) . 6_456 ? N13 Mn1 N13 87.86(13) 12_565 6_456 ? N12 Mn1 N13 100.70(11) 12_565 . ? N12 Mn1 N13 157.67(12) 6_456 . ? N12 Mn1 N13 72.05(12) . . ? N13 Mn1 N13 87.87(13) 12_565 . ? N13 Mn1 N13 87.87(13) 6_456 . ? C11 N11 C11 113.2(2) 12_565 . ? C11 N11 C11 113.2(2) 12_565 6_456 ? C11 N11 C11 113.2(2) . 6_456 ? C13 N12 C12 118.2(4) . . ? C13 N12 Mn1 116.9(3) . . ? C12 N12 Mn1 124.5(3) . . ? C14 N13 N14 104.0(3) . . ? C14 N13 Mn1 113.4(3) . . ? N14 N13 Mn1 142.3(3) . . ? C16 N14 N13 112.7(4) . . ? C16 N14 H14 123.6 . . ? N13 N14 H14 123.6 . . ? N11 C11 C12 110.6(3) . . ? N11 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? N11 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N12 C12 C11 109.2(3) . . ? N12 C12 H12A 109.8 . . ? C11 C12 H12A 109.8 . . ? N12 C12 H12B 109.8 . . ? C11 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? N12 C13 C14 118.9(4) . . ? N12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? N13 C14 C15 110.8(4) . . ? N13 C14 C13 118.4(4) . . ? C15 C14 C13 130.9(4) . . ? C16 C15 C14 106.0(4) . . ? C16 C15 H15 127.0 . . ? C14 C15 H15 127.0 . . ? N14 C16 C15 106.5(4) . . ? N14 C16 C17 121.1(4) . . ? C15 C16 C17 132.4(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N22 Mn2 N22 104.75(10) 8_656 . ? N22 Mn2 N22 104.74(10) 8_656 11_466 ? N22 Mn2 N22 104.74(10) . 11_466 ? N22 Mn2 N23 97.71(13) 8_656 . ? N22 Mn2 N23 71.80(13) . . ? N22 Mn2 N23 157.34(13) 11_466 . ? N22 Mn2 N23 71.80(13) 8_656 8_656 ? N22 Mn2 N23 157.34(13) . 8_656 ? N22 Mn2 N23 97.71(13) 11_466 8_656 ? N23 Mn2 N23 86.30(13) . 8_656 ? N22 Mn2 N23 157.33(13) 8_656 11_466 ? N22 Mn2 N23 97.71(13) . 11_466 ? N22 Mn2 N23 71.80(13) 11_466 11_466 ? N23 Mn2 N23 86.30(13) . 11_466 ? N23 Mn2 N23 86.29(13) 8_656 11_466 ? C21 N21 C21 112.5(3) . 8_656 ? C21 N21 C21 112.5(3) . 11_466 ? C21 N21 C21 112.5(3) 8_656 11_466 ? C23 N22 C22 119.0(4) . . ? C23 N22 Mn2 118.0(3) . . ? C22 N22 Mn2 122.5(3) . . ? C24 N23 N24 104.5(3) . . ? C24 N23 Mn2 113.9(3) . . ? N24 N23 Mn2 141.3(3) . . ? N23 N24 C26 113.1(4) . . ? N23 N24 H24 123.5 . . ? C26 N24 H24 123.5 . . ? N21 C21 C22 111.3(4) . . ? N21 C21 H21A 109.4 . . ? C22 C21 H21A 109.4 . . ? N21 C21 H21B 109.4 . . ? C22 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? N22 C22 C21 108.1(4) . . ? N22 C22 H22A 110.1 . . ? C21 C22 H22A 110.1 . . ? N22 C22 H22B 110.1 . . ? C21 C22 H22B 110.1 . . ? H22A C22 H22B 108.4 . . ? N22 C23 C24 118.7(4) . . ? N22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? N23 C24 C25 110.7(4) . . ? N23 C24 C23 117.2(4) . . ? C25 C24 C23 132.0(4) . . ? C26 C25 C24 106.3(4) . . ? C26 C25 H25 126.9 . . ? C24 C25 H25 126.9 . . ? N24 C26 C25 105.4(4) . . ? N24 C26 C27 121.8(4) . . ? C25 C26 C27 132.8(4) . . ? 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 . . ? O11 Cl1 O14 113.0(4) . . ? O11 Cl1 O13 111.4(4) . . ? O14 Cl1 O13 108.0(5) . . ? O11 Cl1 O12 109.7(4) . . ? O14 Cl1 O12 112.9(5) . . ? O13 Cl1 O12 101.2(4) . . ? O21 Cl2 O22 110.8(5) . . ? O21 Cl2 O22 110.8(5) . 10_655 ? O22 Cl2 O22 108.1(5) . 10_655 ? O21 Cl2 O22 110.8(5) . 7_564 ? O22 Cl2 O22 108.1(5) . 7_564 ? O22 Cl2 O22 108.1(5) 10_655 7_564 ? 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 N12 Mn1 N12 C13 91.8(3) 12_565 . . . ? N12 Mn1 N12 C13 -163.7(3) 6_456 . . . ? N13 Mn1 N12 C13 21.1(5) 12_565 . . . ? N13 Mn1 N12 C13 -90.0(3) 6_456 . . . ? N13 Mn1 N12 C13 -5.8(3) . . . . ? N12 Mn1 N12 C12 -80.2(3) 12_565 . . . ? N12 Mn1 N12 C12 24.3(3) 6_456 . . . ? N13 Mn1 N12 C12 -151.0(4) 12_565 . . . ? N13 Mn1 N12 C12 97.9(3) 6_456 . . . ? N13 Mn1 N12 C12 -177.9(3) . . . . ? N12 Mn1 N13 C14 -94.4(3) 12_565 . . . ? N12 Mn1 N13 C14 80.9(4) 6_456 . . . ? N12 Mn1 N13 C14 4.4(3) . . . . ? N13 Mn1 N13 C14 -165.7(3) 12_565 . . . ? N13 Mn1 N13 C14 106.4(3) 6_456 . . . ? N12 Mn1 N13 N14 78.8(4) 12_565 . . . ? N12 Mn1 N13 N14 -106.0(5) 6_456 . . . ? N12 Mn1 N13 N14 177.6(4) . . . . ? N13 Mn1 N13 N14 7.5(4) 12_565 . . . ? N13 Mn1 N13 N14 -80.5(4) 6_456 . . . ? C14 N13 N14 C16 -0.1(5) . . . . ? Mn1 N13 N14 C16 -173.6(3) . . . . ? C11 N11 C11 C12 146.5(4) 12_565 . . . ? C11 N11 C11 C12 -82.8(5) 6_456 . . . ? C13 N12 C12 C11 -114.0(4) . . . . ? Mn1 N12 C12 C11 58.0(4) . . . . ? N11 C11 C12 N12 -55.6(5) . . . . ? C12 N12 C13 C14 179.0(3) . . . . ? Mn1 N12 C13 C14 6.4(5) . . . . ? N14 N13 C14 C15 0.8(4) . . . . ? Mn1 N13 C14 C15 176.4(3) . . . . ? N14 N13 C14 C13 -178.7(3) . . . . ? Mn1 N13 C14 C13 -3.0(5) . . . . ? N12 C13 C14 N13 -2.2(6) . . . . ? N12 C13 C14 C15 178.5(4) . . . . ? N13 C14 C15 C16 -1.1(5) . . . . ? C13 C14 C15 C16 178.3(4) . . . . ? N13 N14 C16 C15 -0.6(5) . . . . ? N13 N14 C16 C17 -179.7(4) . . . . ? C14 C15 C16 N14 1.0(5) . . . . ? C14 C15 C16 C17 179.9(5) . . . . ? N22 Mn2 N22 C23 91.5(4) 8_656 . . . ? N22 Mn2 N22 C23 -158.5(3) 11_466 . . . ? N23 Mn2 N22 C23 -1.9(3) . . . . ? N23 Mn2 N22 C23 13.5(5) 8_656 . . . ? N23 Mn2 N22 C23 -85.4(3) 11_466 . . . ? N22 Mn2 N22 C22 -80.2(3) 8_656 . . . ? N22 Mn2 N22 C22 29.7(3) 11_466 . . . ? N23 Mn2 N22 C22 -173.6(3) . . . . ? N23 Mn2 N22 C22 -158.2(3) 8_656 . . . ? N23 Mn2 N22 C22 102.9(3) 11_466 . . . ? N22 Mn2 N23 C24 -104.5(3) 8_656 . . . ? N22 Mn2 N23 C24 -1.5(3) . . . . ? N22 Mn2 N23 C24 83.2(4) 11_466 . . . ? N23 Mn2 N23 C24 -175.6(3) 8_656 . . . ? N23 Mn2 N23 C24 97.9(4) 11_466 . . . ? N22 Mn2 N23 N24 81.2(5) 8_656 . . . ? N22 Mn2 N23 N24 -175.8(5) . . . . ? N22 Mn2 N23 N24 -91.1(6) 11_466 . . . ? N23 Mn2 N23 N24 10.1(5) 8_656 . . . ? N23 Mn2 N23 N24 -76.4(4) 11_466 . . . ? C24 N23 N24 C26 0.0(5) . . . . ? Mn2 N23 N24 C26 174.6(3) . . . . ? C21 N21 C21 C22 149.7(5) 8_656 . . . ? C21 N21 C21 C22 -82.1(6) 11_466 . . . ? C23 N22 C22 C21 -117.9(4) . . . . ? Mn2 N22 C22 C21 53.7(5) . . . . ? N21 C21 C22 N22 -55.2(5) . . . . ? C22 N22 C23 C24 177.0(4) . . . . ? Mn2 N22 C23 C24 4.9(5) . . . . ? N24 N23 C24 C25 -0.2(5) . . . . ? Mn2 N23 C24 C25 -176.5(3) . . . . ? N24 N23 C24 C23 -179.3(4) . . . . ? Mn2 N23 C24 C23 4.4(5) . . . . ? N22 C23 C24 N23 -6.4(6) . . . . ? N22 C23 C24 C25 174.7(4) . . . . ? N23 C24 C25 C26 0.3(5) . . . . ? C23 C24 C25 C26 179.3(4) . . . . ? N23 N24 C26 C25 0.2(5) . . . . ? N23 N24 C26 C27 -180.0(4) . . . . ? C24 C25 C26 N24 -0.3(5) . . . . ? C24 C25 C26 C27 179.9(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N14 H14 O12 0.87 2.09 2.937(7) 164.5 6_457 N24 H24 O12A 0.87 2.42 3.27(2) 164.8 5_455 N24 H24 O2W 0.87 2.44 3.086(12) 131.7 5_455 N24 H24 O1W 0.87 2.60 3.130(7) 120.2 . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.229 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.039 _exptl_crystal_id Brewer _diffrn_measurement_details 606,606,606 _diffrn_measurement_total_frames-CCD 1818 _diffrn_measurement_frame_width-CCD 0.3 _diffrn_detector_distance-CCD 4.939 _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_measurement_frame_time-CCD 33 _diffrn_measurement_total_time-CCD 20.28 _diffrn_measurement_frame_size-CCD 512 _chemical_absolute_configuration ad _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 0.0287317 _diffrn_orient_matrix_UB_12 0.0381476 _diffrn_orient_matrix_UB_13 -0.0259475 _diffrn_orient_matrix_UB_21 0.0368278 _diffrn_orient_matrix_UB_22 -0.0005254 _diffrn_orient_matrix_UB_23 0.0399772 _diffrn_orient_matrix_UB_31 0.0278297 _diffrn_orient_matrix_UB_32 -0.0387182 _diffrn_orient_matrix_UB_33 -0.0261116 _symmetry_space_group_name_Hall 'P 2ac 2ab 3' _diffrn_measurement_specimen_support 'cactus needle' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart1000' _reflns_Friedel_coverage 0.823 #_______________________________________________________________________________ # _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Flack, H.D. (1983), Acta Cryst. A39, 876-881. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Spek, A. L. (1990). Acta Cryst., A46, C-34. ; data_crys1t5 _database_code_depnum_ccdc_archive 'CCDC 661178' #TrackingRef 'newpyrazole.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H61 F12 Fe2 N20 O P2' _chemical_formula_weight 1275.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0249(6) _cell_length_b 12.2729(6) _cell_length_c 18.5072(11) _cell_angle_alpha 103.106(1) _cell_angle_beta 95.299(1) _cell_angle_gamma 95.477(1) _cell_volume 2629.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2541 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 30.06 _exptl_crystal_description 'thick plate' _exptl_crystal_colour green _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1314 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.586 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex 2 CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% >2% _diffrn_reflns_number 16378 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 30.96 _reflns_number_total 16383 _reflns_number_gt 12282 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex 2' _computing_cell_refinement 'Bruker Apex 2' _computing_data_reduction 'Bruker Apex 2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^] 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 16383 _refine_ls_number_parameters 741 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0858 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.86242(2) 0.85478(2) 0.260659(17) 0.01247(7) Uani 1 1 d . . . Fe2 Fe 0.55355(2) 0.46040(2) 0.263688(17) 0.01282(7) Uani 1 1 d . . . P1 P 0.23694(5) 0.72883(6) 0.43885(3) 0.01932(12) Uani 1 1 d . . . P2 P 0.76335(5) 1.10533(5) -0.03195(4) 0.02336(14) Uani 1 1 d . . . F11 F 0.24918(18) 0.76243(17) 0.52738(8) 0.0634(5) Uani 1 1 d . . . F12 F 0.30376(13) 0.84637(13) 0.43821(11) 0.0495(5) Uani 1 1 d . . . F13 F 0.17091(13) 0.61040(13) 0.43856(10) 0.0466(4) Uani 1 1 d . . . F14 F 0.22537(15) 0.69485(15) 0.35016(8) 0.0453(4) Uani 1 1 d . . . F15 F 0.35145(11) 0.67372(13) 0.44170(9) 0.0384(4) Uani 1 1 d . . . F16 F 0.12324(11) 0.78404(13) 0.43643(9) 0.0403(4) Uani 1 1 d . . . F21 F 0.86755(15) 1.19359(15) -0.02854(13) 0.0792(7) Uani 1 1 d . . . F22 F 0.65830(16) 1.01596(15) -0.03507(11) 0.0715(6) Uani 1 1 d . . . F23 F 0.74915(17) 1.08094(16) -0.11985(9) 0.0624(5) Uani 1 1 d . . . F24 F 0.84100(16) 1.00864(15) -0.03647(10) 0.0610(5) Uani 1 1 d . . . F25 F 0.68397(14) 1.20160(14) -0.02621(10) 0.0536(5) Uani 1 1 d . . . F26 F 0.77766(16) 1.12938(14) 0.05683(9) 0.0548(5) Uani 1 1 d . . . N1 N 1.04334(15) 1.08946(16) 0.25926(11) 0.0213(4) Uani 1 1 d . . . N2 N 0.37077(15) 0.23743(15) 0.26635(11) 0.0209(4) Uani 1 1 d . . . N1A N 1.02733(14) 0.85534(14) 0.27233(10) 0.0146(4) Uani 1 1 d . . . N2A N 0.87569(14) 0.70918(15) 0.19416(10) 0.0157(4) Uani 1 1 d . . . N3A N 0.80763(16) 0.62943(16) 0.14318(11) 0.0196(4) Uani 1 1 d . . . H3A H 0.732(2) 0.620(2) 0.1418(15) 0.049(9) Uiso 1 1 d . . . N1B N 0.85931(14) 0.92161(15) 0.17296(10) 0.0159(4) Uani 1 1 d . . . N2B N 0.70033(14) 0.85241(14) 0.23719(10) 0.0143(4) Uani 1 1 d . . . N3B N 0.60827(15) 0.83362(16) 0.27058(11) 0.0177(4) Uani 1 1 d . . . H3B H 0.605(2) 0.791(2) 0.3010(15) 0.041(9) Uiso 1 1 d . . . N1C N 0.86288(14) 0.99948(14) 0.33465(10) 0.0156(4) Uani 1 1 d . . . N2C N 0.85529(14) 0.80086(14) 0.35200(10) 0.0138(4) Uani 1 1 d . . . N3C N 0.86435(14) 0.70351(15) 0.37242(10) 0.0160(4) Uani 1 1 d . . . H3C H 0.842(3) 0.612(3) 0.329(2) 0.115(14) Uiso 1 1 d . . . N1D N 0.57671(14) 0.37388(14) 0.34064(10) 0.0165(4) Uani 1 1 d . . . N2D N 0.59008(14) 0.58427(14) 0.35167(10) 0.0140(4) Uani 1 1 d . . . N3D N 0.58563(14) 0.69573(14) 0.36685(10) 0.0158(4) Uani 1 1 d . . . N1E N 0.52724(14) 0.32660(14) 0.17823(10) 0.0145(4) Uani 1 1 d . . . N2E N 0.70762(14) 0.44432(14) 0.24516(10) 0.0150(4) Uani 1 1 d . . . N3E N 0.80918(14) 0.49114(15) 0.28057(11) 0.0183(4) Uani 1 1 d . . . N1F N 0.39311(14) 0.47594(14) 0.27390(10) 0.0144(4) Uani 1 1 d . . . N2F N 0.52344(14) 0.55062(14) 0.19271(10) 0.0147(4) Uani 1 1 d . . . N3F N 0.57917(15) 0.58382(16) 0.13989(10) 0.0186(4) Uani 1 1 d . . . C1A C 1.13732(18) 1.03917(18) 0.28533(14) 0.0219(5) Uani 1 1 d . . . H1AA H 1.1886 1.0986 0.3217 0.026 Uiso 1 1 calc R . . H1AB H 1.1788 1.0112 0.2424 0.026 Uiso 1 1 calc R . . C2A C 1.10890(17) 0.94231(17) 0.32210(13) 0.0187(5) Uani 1 1 d . . . H2AA H 1.1783 0.9094 0.3341 0.022 Uiso 1 1 calc R . . H2AB H 1.0774 0.9711 0.3694 0.022 Uiso 1 1 calc R . . C3A C 1.06436(18) 0.76996(18) 0.23186(13) 0.0183(5) Uani 1 1 d . . . H3AA H 1.1423 0.7617 0.2339 0.022 Uiso 1 1 calc R . . C4A C 0.98108(17) 0.68824(18) 0.18354(13) 0.0175(5) Uani 1 1 d . . . C5A C 0.98031(19) 0.59340(19) 0.12484(13) 0.0233(5) Uani 1 1 d . . . H5AA H 1.0432 0.5606 0.1056 0.028 Uiso 1 1 calc R . . C6A C 0.8682(2) 0.55840(19) 0.10118(13) 0.0232(5) Uani 1 1 d . . . C7A C 0.8111(2) 0.4650(2) 0.03881(14) 0.0342(6) Uani 1 1 d . . . H7AA H 0.7373 0.4390 0.0513 0.051 Uiso 1 1 calc R . . H7AB H 0.8570 0.4024 0.0311 0.051 Uiso 1 1 calc R . . H7AC H 0.8014 0.4921 -0.0070 0.051 Uiso 1 1 calc R . . C1B C 1.01172(19) 1.07529(19) 0.18063(13) 0.0213(5) Uani 1 1 d . . . H1BA H 1.0798 1.0942 0.1575 0.026 Uiso 1 1 calc R . . H1BB H 0.9587 1.1302 0.1739 0.026 Uiso 1 1 calc R . . C2B C 0.95725(17) 0.95798(18) 0.13856(13) 0.0184(5) Uani 1 1 d . . . H2BA H 0.9333 0.9585 0.0860 0.022 Uiso 1 1 calc R . . H2BB H 1.0131 0.9037 0.1386 0.022 Uiso 1 1 calc R . . C3B C 0.76098(17) 0.93325(18) 0.14388(12) 0.0174(4) Uani 1 1 d . . . H3BA H 0.7500 0.9612 0.1002 0.021 Uiso 1 1 calc R . . C4B C 0.66879(17) 0.90105(18) 0.18201(12) 0.0155(4) Uani 1 1 d . . . C5B C 0.55436(17) 0.91359(18) 0.17958(13) 0.0193(5) Uani 1 1 d . . . H5BA H 0.5107 0.9452 0.1459 0.023 Uiso 1 1 calc R . . C6B C 0.51917(17) 0.86981(18) 0.23701(13) 0.0177(5) Uani 1 1 d . . . C7B C 0.40700(18) 0.8592(2) 0.26486(15) 0.0267(6) Uani 1 1 d . . . H7BA H 0.3969 0.7898 0.2825 0.040 Uiso 1 1 calc R . . H7BB H 0.3477 0.8566 0.2243 0.040 Uiso 1 1 calc R . . H7BC H 0.4027 0.9241 0.3061 0.040 Uiso 1 1 calc R . . C1C C 0.98395(19) 1.15942(18) 0.31188(13) 0.0213(5) Uani 1 1 d . . . H1CA H 0.9804 1.2323 0.2978 0.026 Uiso 1 1 calc R . . H1CB H 1.0279 1.1752 0.3618 0.026 Uiso 1 1 calc R . . C2C C 0.86385(18) 1.11009(18) 0.31787(13) 0.0209(5) Uani 1 1 d . . . H2CA H 0.8319 1.1617 0.3578 0.025 Uiso 1 1 calc R . . H2CB H 0.8161 1.1034 0.2702 0.025 Uiso 1 1 calc R . . C3C C 0.86142(17) 0.99283(17) 0.40251(13) 0.0166(5) Uani 1 1 d . . . H3CA H 0.8590 1.0571 0.4419 0.020 Uiso 1 1 calc R . . C4C C 0.86373(17) 0.88215(17) 0.41532(12) 0.0155(4) Uani 1 1 d . . . C5C C 0.87820(17) 0.83566(18) 0.47698(13) 0.0183(5) Uani 1 1 d . . . H5CA H 0.8860 0.8741 0.5282 0.022 Uiso 1 1 calc R . . C6C C 0.87886(17) 0.72159(18) 0.44777(13) 0.0177(5) Uani 1 1 d . . . C7C C 0.89622(19) 0.62833(19) 0.48475(14) 0.0239(5) Uani 1 1 d . . . H7CA H 0.8597 0.5571 0.4521 0.036 Uiso 1 1 calc R . . H7CB H 0.8634 0.6422 0.5321 0.036 Uiso 1 1 calc R . . H7CC H 0.9770 0.6240 0.4945 0.036 Uiso 1 1 calc R . . C1D C 0.44305(19) 0.20186(18) 0.32018(13) 0.0227(5) Uani 1 1 d . . . H1DA H 0.4384 0.1186 0.3062 0.027 Uiso 1 1 calc R . . H1DB H 0.4152 0.2236 0.3695 0.027 Uiso 1 1 calc R . . C2D C 0.56683(19) 0.25119(17) 0.32754(13) 0.0206(5) Uani 1 1 d . . . H2DA H 0.6095 0.2300 0.3696 0.025 Uiso 1 1 calc R . . H2DB H 0.5995 0.2195 0.2813 0.025 Uiso 1 1 calc R . . C3D C 0.60382(17) 0.43359(18) 0.40795(13) 0.0172(5) Uani 1 1 d . . . H3DA H 0.6206 0.4009 0.4489 0.021 Uiso 1 1 calc R . . C4D C 0.60675(17) 0.55260(17) 0.41647(12) 0.0152(4) Uani 1 1 d . . . C5D C 0.61464(18) 0.64700(18) 0.47570(13) 0.0188(5) Uani 1 1 d . . . H5DA H 0.6270 0.6502 0.5276 0.023 Uiso 1 1 calc R . . C6D C 0.60043(17) 0.73499(18) 0.44203(13) 0.0176(5) Uani 1 1 d . . . C7D C 0.5947(2) 0.85708(18) 0.47588(13) 0.0240(5) Uani 1 1 d . . . H7DA H 0.6162 0.9019 0.4407 0.036 Uiso 1 1 calc R . . H7DB H 0.6463 0.8813 0.5222 0.036 Uiso 1 1 calc R . . H7DC H 0.5178 0.8679 0.4869 0.036 Uiso 1 1 calc R . . C1E C 0.37102(19) 0.18687(18) 0.18828(13) 0.0212(5) Uani 1 1 d . . . H1EA H 0.2930 0.1560 0.1664 0.025 Uiso 1 1 calc R . . H1EB H 0.4164 0.1230 0.1833 0.025 Uiso 1 1 calc R . . C2E C 0.41742(17) 0.26728(18) 0.14342(12) 0.0182(5) Uani 1 1 d . . . H2EA H 0.4245 0.2242 0.0922 0.022 Uiso 1 1 calc R . . H2EB H 0.3641 0.3229 0.1395 0.022 Uiso 1 1 calc R . . C3E C 0.61683(17) 0.29328(18) 0.15219(12) 0.0174(5) Uani 1 1 d . . . H3EA H 0.6141 0.2321 0.1099 0.021 Uiso 1 1 calc R . . C4E C 0.72097(17) 0.35380(18) 0.19070(12) 0.0174(5) Uani 1 1 d . . . C5E C 0.83480(18) 0.34348(18) 0.19044(13) 0.0214(5) Uani 1 1 d . . . H5EA H 0.8690 0.2882 0.1581 0.026 Uiso 1 1 calc R . . C6E C 0.88727(18) 0.43092(19) 0.24740(13) 0.0204(5) Uani 1 1 d . . . C7E C 1.00955(18) 0.46385(19) 0.27462(15) 0.0271(6) Uani 1 1 d . . . H7EA H 1.0269 0.5459 0.2842 0.041 Uiso 1 1 calc R . . H7EB H 1.0546 0.4276 0.2366 0.041 Uiso 1 1 calc R . . H7EC H 1.0273 0.4397 0.3209 0.041 Uiso 1 1 calc R . . C1F C 0.28451(18) 0.30599(18) 0.29006(14) 0.0220(5) Uani 1 1 d . . . H1FA H 0.2459 0.2748 0.3272 0.026 Uiso 1 1 calc R . . H1FB H 0.2283 0.3008 0.2465 0.026 Uiso 1 1 calc R . . C2F C 0.32623(18) 0.42992(17) 0.32428(13) 0.0181(5) Uani 1 1 d . . . H2FA H 0.2612 0.4727 0.3337 0.022 Uiso 1 1 calc R . . H2FB H 0.3725 0.4375 0.3727 0.022 Uiso 1 1 calc R . . C3F C 0.34627(17) 0.53291(17) 0.23248(12) 0.0171(5) Uani 1 1 d . . . H3FA H 0.2706 0.5483 0.2347 0.021 Uiso 1 1 calc R . . C4F C 0.41579(17) 0.57220(17) 0.18227(12) 0.0161(4) Uani 1 1 d . . . C5F C 0.40166(18) 0.62145(18) 0.12239(12) 0.0187(5) Uani 1 1 d . . . H5FA H 0.3351 0.6460 0.1030 0.022 Uiso 1 1 calc R . . C6F C 0.50645(18) 0.62704(18) 0.09699(12) 0.0200(5) Uani 1 1 d . . . C7F C 0.5439(2) 0.6693(2) 0.03254(13) 0.0277(6) Uani 1 1 d . . . H7FA H 0.6249 0.6942 0.0421 0.042 Uiso 1 1 calc R . . H7FB H 0.5033 0.7327 0.0263 0.042 Uiso 1 1 calc R . . H7FC H 0.5280 0.6086 -0.0130 0.042 Uiso 1 1 calc R . . O1S O 0.9247(4) 0.6781(3) -0.0823(2) 0.1553(17) Uani 1 1 d . . . H1S H 0.9913 0.7071 -0.0678 0.186 Uiso 1 1 d R . . C1S C 0.8595(3) 0.7257(3) -0.0366(2) 0.0690(11) Uani 1 1 d . . . H1S3 H 0.7885 0.6765 -0.0422 0.103 Uiso 1 1 calc R . . H1S2 H 0.8444 0.7977 -0.0475 0.103 Uiso 1 1 calc R . . H1S1 H 0.8959 0.7389 0.0148 0.103 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01306(14) 0.01129(14) 0.01357(16) 0.00393(12) 0.00217(12) 0.00105(11) Fe2 0.01404(14) 0.01198(14) 0.01260(16) 0.00335(12) 0.00212(12) 0.00084(11) P1 0.0186(2) 0.0211(3) 0.0196(3) 0.0054(3) 0.0027(3) 0.0069(2) P2 0.0315(3) 0.0204(3) 0.0191(3) 0.0041(3) 0.0042(3) 0.0079(3) F11 0.1035(14) 0.0709(12) 0.0193(8) 0.0032(9) 0.0047(10) 0.0480(11) F12 0.0385(9) 0.0292(9) 0.0779(14) 0.0165(9) -0.0055(9) -0.0071(7) F13 0.0425(9) 0.0333(9) 0.0695(13) 0.0228(9) 0.0153(9) -0.0019(8) F14 0.0634(10) 0.0501(10) 0.0244(8) 0.0072(9) 0.0059(9) 0.0200(8) F15 0.0237(7) 0.0447(9) 0.0536(11) 0.0208(8) 0.0051(7) 0.0153(7) F16 0.0246(7) 0.0488(10) 0.0561(11) 0.0217(8) 0.0110(7) 0.0192(7) F21 0.0600(12) 0.0485(12) 0.1190(19) -0.0046(12) 0.0423(12) -0.0151(10) F22 0.0694(12) 0.0539(12) 0.0763(14) -0.0060(10) 0.0236(11) -0.0301(10) F23 0.1038(15) 0.0648(12) 0.0242(9) 0.0121(9) 0.0108(10) 0.0306(11) F24 0.0894(14) 0.0514(11) 0.0476(11) 0.0059(9) 0.0103(10) 0.0480(10) F25 0.0620(11) 0.0571(12) 0.0504(11) 0.0156(9) 0.0120(9) 0.0383(9) F26 0.0921(13) 0.0455(10) 0.0254(9) 0.0008(8) -0.0017(9) 0.0273(10) N1 0.0228(10) 0.0207(10) 0.0216(11) 0.0077(9) 0.0020(8) 0.0036(8) N2 0.0250(10) 0.0161(9) 0.0216(11) 0.0025(8) 0.0076(8) 0.0022(8) N1A 0.0161(9) 0.0134(9) 0.0156(10) 0.0067(7) 0.0023(7) -0.0004(7) N2A 0.0160(9) 0.0147(9) 0.0148(9) 0.0024(7) 0.0011(7) -0.0032(7) N3A 0.0182(9) 0.0208(10) 0.0167(10) 0.0014(8) 0.0018(8) -0.0051(8) N1B 0.0169(9) 0.0153(9) 0.0170(10) 0.0061(7) 0.0056(7) 0.0013(7) N2B 0.0144(8) 0.0141(9) 0.0157(10) 0.0059(7) 0.0036(7) 0.0000(7) N3B 0.0179(9) 0.0180(10) 0.0203(11) 0.0092(8) 0.0062(8) 0.0032(7) N1C 0.0165(9) 0.0115(9) 0.0205(10) 0.0062(7) 0.0032(8) 0.0025(7) N2C 0.0139(8) 0.0122(9) 0.0149(9) 0.0033(7) -0.0004(7) 0.0010(7) N3C 0.0152(9) 0.0127(9) 0.0212(10) 0.0064(8) 0.0012(8) 0.0023(7) N1D 0.0181(9) 0.0127(9) 0.0196(10) 0.0051(8) 0.0032(8) 0.0022(7) N2D 0.0153(8) 0.0116(9) 0.0163(10) 0.0051(7) 0.0030(7) 0.0015(7) N3D 0.0158(9) 0.0126(9) 0.0211(10) 0.0066(8) 0.0053(8) 0.0035(7) N1E 0.0160(8) 0.0129(9) 0.0146(9) 0.0045(7) 0.0022(7) -0.0009(7) N2E 0.0164(8) 0.0145(9) 0.0139(9) 0.0032(7) 0.0011(7) 0.0021(7) N3E 0.0135(8) 0.0159(9) 0.0248(11) 0.0048(8) -0.0010(8) 0.0016(7) N1F 0.0169(9) 0.0097(8) 0.0169(10) 0.0023(7) 0.0058(7) 0.0007(7) N2F 0.0156(8) 0.0150(9) 0.0134(9) 0.0045(7) 0.0020(7) -0.0019(7) N3F 0.0208(9) 0.0207(10) 0.0135(9) 0.0051(8) 0.0026(8) -0.0047(8) C1A 0.0192(11) 0.0146(11) 0.0313(14) 0.0076(10) -0.0004(10) -0.0035(9) C2A 0.0157(10) 0.0145(11) 0.0234(13) 0.0032(9) -0.0031(9) -0.0026(8) C3A 0.0158(10) 0.0162(11) 0.0238(12) 0.0065(9) 0.0026(9) 0.0025(9) C4A 0.0157(10) 0.0161(11) 0.0210(12) 0.0047(9) 0.0032(9) 0.0019(9) C5A 0.0230(11) 0.0194(12) 0.0258(13) 0.0007(10) 0.0062(10) 0.0029(9) C6A 0.0310(13) 0.0191(12) 0.0179(12) 0.0018(9) 0.0057(10) -0.0024(10) C7A 0.0386(15) 0.0306(14) 0.0248(14) -0.0064(11) 0.0014(11) -0.0053(12) C1B 0.0215(11) 0.0208(12) 0.0250(13) 0.0127(10) 0.0055(10) -0.0006(9) C2B 0.0171(10) 0.0216(12) 0.0190(12) 0.0092(9) 0.0062(9) 0.0008(9) C3B 0.0200(11) 0.0173(11) 0.0173(11) 0.0092(9) 0.0018(9) 0.0031(9) C4B 0.0175(10) 0.0154(10) 0.0150(11) 0.0067(9) 0.0009(8) 0.0020(8) C5B 0.0172(10) 0.0182(11) 0.0239(12) 0.0079(9) 0.0013(9) 0.0031(9) C6B 0.0164(10) 0.0151(11) 0.0237(12) 0.0066(9) 0.0053(9) 0.0043(8) C7B 0.0188(11) 0.0260(13) 0.0389(15) 0.0116(12) 0.0098(11) 0.0054(10) C1C 0.0293(12) 0.0106(10) 0.0250(13) 0.0075(9) 0.0026(10) -0.0004(9) C2C 0.0272(12) 0.0132(11) 0.0237(13) 0.0050(9) 0.0058(10) 0.0060(9) C3C 0.0190(11) 0.0119(10) 0.0180(12) 0.0014(9) 0.0040(9) 0.0020(8) C4C 0.0146(10) 0.0142(10) 0.0166(11) 0.0022(9) 0.0021(8) 0.0001(8) C5C 0.0205(11) 0.0201(11) 0.0143(11) 0.0045(9) 0.0029(9) 0.0006(9) C6C 0.0136(10) 0.0208(11) 0.0185(12) 0.0068(9) -0.0005(9) -0.0005(9) C7C 0.0247(12) 0.0204(12) 0.0283(14) 0.0106(10) 0.0004(10) 0.0022(10) C1D 0.0347(13) 0.0116(10) 0.0234(13) 0.0060(9) 0.0085(10) 0.0019(10) C2D 0.0329(13) 0.0118(10) 0.0184(12) 0.0057(9) 0.0020(10) 0.0055(9) C3D 0.0189(11) 0.0183(11) 0.0165(12) 0.0086(9) 0.0020(9) 0.0020(9) C4D 0.0164(10) 0.0154(11) 0.0147(11) 0.0063(9) 0.0015(8) 0.0004(8) C5D 0.0210(11) 0.0208(12) 0.0137(11) 0.0033(9) 0.0024(9) 0.0000(9) C6D 0.0151(10) 0.0167(11) 0.0212(12) 0.0045(9) 0.0050(9) 0.0001(8) C7D 0.0297(13) 0.0177(12) 0.0241(13) 0.0013(10) 0.0093(10) 0.0027(10) C1E 0.0225(11) 0.0150(11) 0.0245(13) 0.0023(9) 0.0049(10) -0.0032(9) C2E 0.0157(10) 0.0177(11) 0.0182(11) 0.0001(9) 0.0009(9) -0.0021(9) C3E 0.0212(11) 0.0142(10) 0.0162(11) 0.0022(9) 0.0033(9) 0.0020(9) C4E 0.0185(11) 0.0143(11) 0.0187(12) 0.0027(9) 0.0025(9) 0.0014(9) C5E 0.0191(11) 0.0161(11) 0.0281(13) 0.0024(10) 0.0050(10) 0.0036(9) C6E 0.0185(11) 0.0169(11) 0.0275(13) 0.0090(10) 0.0014(10) 0.0036(9) C7E 0.0185(11) 0.0193(12) 0.0430(16) 0.0077(11) 0.0001(11) 0.0022(9) C1F 0.0225(11) 0.0162(11) 0.0286(14) 0.0055(10) 0.0123(10) -0.0011(9) C2F 0.0215(11) 0.0151(11) 0.0204(12) 0.0073(9) 0.0094(9) 0.0009(9) C3F 0.0165(10) 0.0127(10) 0.0212(12) 0.0023(9) 0.0035(9) -0.0003(8) C4F 0.0177(10) 0.0115(10) 0.0185(12) 0.0035(8) 0.0006(9) 0.0010(8) C5F 0.0202(11) 0.0181(11) 0.0187(12) 0.0074(9) -0.0010(9) 0.0021(9) C6F 0.0247(11) 0.0190(11) 0.0138(11) 0.0022(9) 0.0008(9) -0.0035(9) C7F 0.0306(13) 0.0355(14) 0.0181(12) 0.0112(11) 0.0024(10) -0.0019(11) O1S 0.182(4) 0.151(4) 0.138(3) 0.004(3) 0.097(3) 0.044(3) C1S 0.074(3) 0.072(3) 0.060(3) 0.012(2) -0.001(2) 0.019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2B 1.9533(17) . ? Fe1 N2C 1.9560(18) . ? Fe1 N2A 1.9562(17) . ? Fe1 N1A 1.9741(17) . ? Fe1 N1B 1.9766(19) . ? Fe1 N1C 1.9807(17) . ? Fe2 N2F 1.9315(19) . ? Fe2 N2E 1.9353(17) . ? Fe2 N2D 1.9425(17) . ? Fe2 N1D 1.9755(19) . ? Fe2 N1F 1.9787(17) . ? Fe2 N1E 1.9821(17) . ? P1 F16 1.5842(14) . ? P1 F11 1.5853(15) . ? P1 F12 1.5859(17) . ? P1 F13 1.5869(16) . ? P1 F14 1.5886(14) . ? P1 F15 1.5927(14) . ? P2 F21 1.5629(18) . ? P2 F24 1.5710(16) . ? P2 F23 1.5758(17) . ? P2 F25 1.5797(16) . ? P2 F22 1.5797(18) . ? P2 F26 1.5921(17) . ? N1 C1A 1.435(3) . ? N1 C1C 1.436(3) . ? N1 C1B 1.436(3) . ? N2 C1D 1.431(3) . ? N2 C1F 1.435(3) . ? N2 C1E 1.438(3) . ? N1A C3A 1.285(3) . ? N1A C2A 1.462(2) . ? N2A C4A 1.340(3) . ? N2A N3A 1.343(2) . ? N3A C6A 1.346(3) . ? N3A H3A 0.90(3) . ? N1B C3B 1.288(3) . ? N1B C2B 1.469(3) . ? N2B C4B 1.338(3) . ? N2B N3B 1.343(2) . ? N3B C6B 1.351(3) . ? N3B H3B 0.85(3) . ? N1C C3C 1.278(3) . ? N1C C2C 1.459(3) . ? N2C N3C 1.343(2) . ? N2C C4C 1.344(3) . ? N3C C6C 1.353(3) . ? N3C H3C 1.22(4) . ? N1D C3D 1.289(3) . ? N1D C2D 1.461(3) . ? N2D N3D 1.340(2) . ? N2D C4D 1.346(3) . ? N3D C6D 1.354(3) . ? N1E C3E 1.285(3) . ? N1E C2E 1.461(2) . ? N2E N3E 1.341(2) . ? N2E C4E 1.354(3) . ? N3E C6E 1.356(3) . ? N1F C3F 1.278(3) . ? N1F C2F 1.458(3) . ? N2F N3F 1.349(2) . ? N2F C4F 1.351(3) . ? N3F C6F 1.352(3) . ? C1A C2A 1.525(3) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.430(3) . ? C3A H3AA 0.9500 . ? C4A C5A 1.399(3) . ? C5A C6A 1.374(3) . ? C5A H5AA 0.9500 . ? C6A C7A 1.491(3) . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C1B C2B 1.525(3) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C4B 1.439(3) . ? C3B H3BA 0.9500 . ? C4B C5B 1.397(3) . ? C5B C6B 1.377(3) . ? C5B H5BA 0.9500 . ? C6B C7B 1.492(3) . ? C7B H7BA 0.9800 . ? C7B H7BB 0.9800 . ? C7B H7BC 0.9800 . ? C1C C2C 1.535(3) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C3C C4C 1.433(3) . ? C3C H3CA 0.9500 . ? C4C C5C 1.391(3) . ? C5C C6C 1.383(3) . ? C5C H5CA 0.9500 . ? C6C C7C 1.482(3) . ? C7C H7CA 0.9800 . ? C7C H7CB 0.9800 . ? C7C H7CC 0.9800 . ? C1D C2D 1.534(3) . ? C1D H1DA 0.9900 . ? C1D H1DB 0.9900 . ? C2D H2DA 0.9900 . ? C2D H2DB 0.9900 . ? C3D C4D 1.430(3) . ? C3D H3DA 0.9500 . ? C4D C5D 1.392(3) . ? C5D C6D 1.380(3) . ? C5D H5DA 0.9500 . ? C6D C7D 1.498(3) . ? C7D H7DA 0.9800 . ? C7D H7DB 0.9800 . ? C7D H7DC 0.9800 . ? C1E C2E 1.525(3) . ? C1E H1EA 0.9900 . ? C1E H1EB 0.9900 . ? C2E H2EA 0.9900 . ? C2E H2EB 0.9900 . ? C3E C4E 1.430(3) . ? C3E H3EA 0.9500 . ? C4E C5E 1.387(3) . ? C5E C6E 1.377(3) . ? C5E H5EA 0.9500 . ? C6E C7E 1.496(3) . ? C7E H7EA 0.9800 . ? C7E H7EB 0.9800 . ? C7E H7EC 0.9800 . ? C1F C2F 1.525(3) . ? C1F H1FA 0.9900 . ? C1F H1FB 0.9900 . ? C2F H2FA 0.9900 . ? C2F H2FB 0.9900 . ? C3F C4F 1.437(3) . ? C3F H3FA 0.9500 . ? C4F C5F 1.382(3) . ? C5F C6F 1.386(3) . ? C5F H5FA 0.9500 . ? C6F C7F 1.493(3) . ? C7F H7FA 0.9800 . ? C7F H7FB 0.9800 . ? C7F H7FC 0.9800 . ? O1S C1S 1.287(4) . ? O1S H1S 0.8383 . ? C1S H1S3 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S1 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 N2B Fe1 N2C 96.38(7) . . ? N2B Fe1 N2A 96.85(7) . . ? N2C Fe1 N2A 96.76(7) . . ? N2B Fe1 N1A 173.59(8) . . ? N2C Fe1 N1A 89.44(7) . . ? N2A Fe1 N1A 79.73(7) . . ? N2B Fe1 N1B 79.81(7) . . ? N2C Fe1 N1B 173.83(7) . . ? N2A Fe1 N1B 88.55(8) . . ? N1A Fe1 N1B 94.62(7) . . ? N2B Fe1 N1C 88.46(7) . . ? N2C Fe1 N1C 79.76(7) . . ? N2A Fe1 N1C 173.97(8) . . ? N1A Fe1 N1C 95.24(7) . . ? N1B Fe1 N1C 95.22(8) . . ? N2F Fe2 N2E 96.15(7) . . ? N2F Fe2 N2D 97.00(7) . . ? N2E Fe2 N2D 95.78(7) . . ? N2F Fe2 N1D 175.91(7) . . ? N2E Fe2 N1D 87.35(7) . . ? N2D Fe2 N1D 80.51(7) . . ? N2F Fe2 N1F 80.15(7) . . ? N2E Fe2 N1F 175.37(8) . . ? N2D Fe2 N1F 87.48(7) . . ? N1D Fe2 N1F 96.44(7) . . ? N2F Fe2 N1E 87.50(7) . . ? N2E Fe2 N1E 80.59(7) . . ? N2D Fe2 N1E 174.54(7) . . ? N1D Fe2 N1E 95.18(7) . . ? N1F Fe2 N1E 96.38(7) . . ? F16 P1 F11 89.80(10) . . ? F16 P1 F12 89.22(9) . . ? F11 P1 F12 90.33(11) . . ? F16 P1 F13 91.26(9) . . ? F11 P1 F13 90.29(11) . . ? F12 P1 F13 179.22(10) . . ? F16 P1 F14 90.54(9) . . ? F11 P1 F14 179.66(11) . . ? F12 P1 F14 89.66(11) . . ? F13 P1 F14 89.72(10) . . ? F16 P1 F15 179.71(10) . . ? F11 P1 F15 89.94(10) . . ? F12 P1 F15 90.66(9) . . ? F13 P1 F15 88.86(9) . . ? F14 P1 F15 89.72(9) . . ? F21 P2 F24 90.78(11) . . ? F21 P2 F23 89.86(12) . . ? F24 P2 F23 89.20(10) . . ? F21 P2 F25 90.04(11) . . ? F24 P2 F25 178.84(11) . . ? F23 P2 F25 91.62(10) . . ? F21 P2 F22 179.73(15) . . ? F24 P2 F22 89.06(12) . . ? F23 P2 F22 90.36(11) . . ? F25 P2 F22 90.11(11) . . ? F21 P2 F26 90.30(12) . . ? F24 P2 F26 90.61(10) . . ? F23 P2 F26 179.74(10) . . ? F25 P2 F26 88.58(9) . . ? F22 P2 F26 89.48(11) . . ? C1A N1 C1C 120.0(2) . . ? C1A N1 C1B 120.44(19) . . ? C1C N1 C1B 119.50(19) . . ? C1D N2 C1F 120.14(19) . . ? C1D N2 C1E 119.12(18) . . ? C1F N2 C1E 119.69(19) . . ? C3A N1A C2A 118.23(17) . . ? C3A N1A Fe1 115.51(15) . . ? C2A N1A Fe1 126.26(13) . . ? C4A N2A N3A 106.30(17) . . ? C4A N2A Fe1 115.27(14) . . ? N3A N2A Fe1 136.96(14) . . ? N2A N3A C6A 110.60(18) . . ? N2A N3A H3A 123.8(18) . . ? C6A N3A H3A 125.2(18) . . ? C3B N1B C2B 117.99(19) . . ? C3B N1B Fe1 115.65(15) . . ? C2B N1B Fe1 126.36(14) . . ? C4B N2B N3B 106.62(17) . . ? C4B N2B Fe1 115.57(14) . . ? N3B N2B Fe1 136.37(15) . . ? N2B N3B C6B 110.2(2) . . ? N2B N3B H3B 122.6(18) . . ? C6B N3B H3B 125.7(18) . . ? C3C N1C C2C 118.61(18) . . ? C3C N1C Fe1 115.72(15) . . ? C2C N1C Fe1 125.67(15) . . ? N3C N2C C4C 106.74(17) . . ? N3C N2C Fe1 136.88(14) . . ? C4C N2C Fe1 115.06(14) . . ? N2C N3C C6C 110.51(17) . . ? N2C N3C H3C 122.6(19) . . ? C6C N3C H3C 125.6(19) . . ? C3D N1D C2D 118.6(2) . . ? C3D N1D Fe2 115.32(15) . . ? C2D N1D Fe2 126.04(15) . . ? N3D N2D C4D 108.77(17) . . ? N3D N2D Fe2 135.57(15) . . ? C4D N2D Fe2 114.60(14) . . ? N2D N3D C6D 107.96(18) . . ? C3E N1E C2E 119.52(17) . . ? C3E N1E Fe2 114.77(14) . . ? C2E N1E Fe2 125.71(14) . . ? N3E N2E C4E 108.69(17) . . ? N3E N2E Fe2 135.35(14) . . ? C4E N2E Fe2 115.02(14) . . ? N2E N3E C6E 107.82(17) . . ? C3F N1F C2F 118.47(18) . . ? C3F N1F Fe2 115.56(15) . . ? C2F N1F Fe2 125.97(14) . . ? N3F N2F C4F 108.08(18) . . ? N3F N2F Fe2 135.27(14) . . ? C4F N2F Fe2 115.55(14) . . ? N2F N3F C6F 108.12(17) . . ? N1 C1A C2A 115.84(18) . . ? N1 C1A H1AA 108.3 . . ? C2A C1A H1AA 108.3 . . ? N1 C1A H1AB 108.3 . . ? C2A C1A H1AB 108.3 . . ? H1AA C1A H1AB 107.4 . . ? N1A C2A C1A 110.48(18) . . ? N1A C2A H2AA 109.6 . . ? C1A C2A H2AA 109.6 . . ? N1A C2A H2AB 109.6 . . ? C1A C2A H2AB 109.6 . . ? H2AA C2A H2AB 108.1 . . ? N1A C3A C4A 115.87(19) . . ? N1A C3A H3AA 122.1 . . ? C4A C3A H3AA 122.1 . . ? N2A C4A C5A 110.39(19) . . ? N2A C4A C3A 113.02(18) . . ? C5A C4A C3A 136.5(2) . . ? C6A C5A C4A 104.5(2) . . ? C6A C5A H5AA 127.8 . . ? C4A C5A H5AA 127.8 . . ? N3A C6A C5A 108.23(19) . . ? N3A C6A C7A 120.4(2) . . ? C5A C6A C7A 131.2(2) . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? N1 C1B C2B 115.65(19) . . ? N1 C1B H1BA 108.4 . . ? C2B C1B H1BA 108.4 . . ? N1 C1B H1BB 108.4 . . ? C2B C1B H1BB 108.4 . . ? H1BA C1B H1BB 107.4 . . ? N1B C2B C1B 111.23(17) . . ? N1B C2B H2BA 109.4 . . ? C1B C2B H2BA 109.4 . . ? N1B C2B H2BB 109.4 . . ? C1B C2B H2BB 109.4 . . ? H2BA C2B H2BB 108.0 . . ? N1B C3B C4B 115.4(2) . . ? N1B C3B H3BA 122.3 . . ? C4B C3B H3BA 122.3 . . ? N2B C4B C5B 110.48(19) . . ? N2B C4B C3B 113.06(19) . . ? C5B C4B C3B 136.3(2) . . ? C6B C5B C4B 104.4(2) . . ? C6B C5B H5BA 127.8 . . ? C4B C5B H5BA 127.8 . . ? N3B C6B C5B 108.32(19) . . ? N3B C6B C7B 120.2(2) . . ? C5B C6B C7B 131.5(2) . . ? C6B C7B H7BA 109.5 . . ? C6B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C6B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N1 C1C C2C 115.40(18) . . ? N1 C1C H1CA 108.4 . . ? C2C C1C H1CA 108.4 . . ? N1 C1C H1CB 108.4 . . ? C2C C1C H1CB 108.4 . . ? H1CA C1C H1CB 107.5 . . ? N1C C2C C1C 111.03(18) . . ? N1C C2C H2CA 109.4 . . ? C1C C2C H2CA 109.4 . . ? N1C C2C H2CB 109.4 . . ? C1C C2C H2CB 109.4 . . ? H2CA C2C H2CB 108.0 . . ? N1C C3C C4C 115.70(19) . . ? N1C C3C H3CA 122.2 . . ? C4C C3C H3CA 122.2 . . ? N2C C4C C5C 109.96(19) . . ? N2C C4C C3C 113.3(2) . . ? C5C C4C C3C 136.7(2) . . ? C6C C5C C4C 105.3(2) . . ? C6C C5C H5CA 127.4 . . ? C4C C5C H5CA 127.4 . . ? N3C C6C C5C 107.5(2) . . ? N3C C6C C7C 121.3(2) . . ? C5C C6C C7C 131.2(2) . . ? C6C C7C H7CA 109.5 . . ? C6C C7C H7CB 109.5 . . ? H7CA C7C H7CB 109.5 . . ? C6C C7C H7CC 109.5 . . ? H7CA C7C H7CC 109.5 . . ? H7CB C7C H7CC 109.5 . . ? N2 C1D C2D 114.37(19) . . ? N2 C1D H1DA 108.7 . . ? C2D C1D H1DA 108.7 . . ? N2 C1D H1DB 108.7 . . ? C2D C1D H1DB 108.7 . . ? H1DA C1D H1DB 107.6 . . ? N1D C2D C1D 110.53(18) . . ? N1D C2D H2DA 109.5 . . ? C1D C2D H2DA 109.5 . . ? N1D C2D H2DB 109.5 . . ? C1D C2D H2DB 109.5 . . ? H2DA C2D H2DB 108.1 . . ? N1D C3D C4D 115.1(2) . . ? N1D C3D H3DA 122.4 . . ? C4D C3D H3DA 122.4 . . ? N2D C4D C5D 109.18(19) . . ? N2D C4D C3D 114.19(19) . . ? C5D C4D C3D 136.4(2) . . ? C6D C5D C4D 104.4(2) . . ? C6D C5D H5DA 127.8 . . ? C4D C5D H5DA 127.8 . . ? N3D C6D C5D 109.64(19) . . ? N3D C6D C7D 120.1(2) . . ? C5D C6D C7D 130.2(2) . . ? C6D C7D H7DA 109.5 . . ? C6D C7D H7DB 109.5 . . ? H7DA C7D H7DB 109.5 . . ? C6D C7D H7DC 109.5 . . ? H7DA C7D H7DC 109.5 . . ? H7DB C7D H7DC 109.5 . . ? N2 C1E C2E 114.31(18) . . ? N2 C1E H1EA 108.7 . . ? C2E C1E H1EA 108.7 . . ? N2 C1E H1EB 108.7 . . ? C2E C1E H1EB 108.7 . . ? H1EA C1E H1EB 107.6 . . ? N1E C2E C1E 111.53(18) . . ? N1E C2E H2EA 109.3 . . ? C1E C2E H2EA 109.3 . . ? N1E C2E H2EB 109.3 . . ? C1E C2E H2EB 109.3 . . ? H2EA C2E H2EB 108.0 . . ? N1E C3E C4E 116.03(19) . . ? N1E C3E H3EA 122.0 . . ? C4E C3E H3EA 122.0 . . ? N2E C4E C5E 108.95(19) . . ? N2E C4E C3E 113.30(18) . . ? C5E C4E C3E 137.7(2) . . ? C6E C5E C4E 104.82(19) . . ? C6E C5E H5EA 127.6 . . ? C4E C5E H5EA 127.6 . . ? N3E C6E C5E 109.70(18) . . ? N3E C6E C7E 120.2(2) . . ? C5E C6E C7E 130.1(2) . . ? C6E C7E H7EA 109.5 . . ? C6E C7E H7EB 109.5 . . ? H7EA C7E H7EB 109.5 . . ? C6E C7E H7EC 109.5 . . ? H7EA C7E H7EC 109.5 . . ? H7EB C7E H7EC 109.5 . . ? N2 C1F C2F 114.74(17) . . ? N2 C1F H1FA 108.6 . . ? C2F C1F H1FA 108.6 . . ? N2 C1F H1FB 108.6 . . ? C2F C1F H1FB 108.6 . . ? H1FA C1F H1FB 107.6 . . ? N1F C2F C1F 110.12(17) . . ? N1F C2F H2FA 109.6 . . ? C1F C2F H2FA 109.6 . . ? N1F C2F H2FB 109.6 . . ? C1F C2F H2FB 109.6 . . ? H2FA C2F H2FB 108.1 . . ? N1F C3F C4F 115.51(19) . . ? N1F C3F H3FA 122.2 . . ? C4F C3F H3FA 122.2 . . ? N2F C4F C5F 109.73(19) . . ? N2F C4F C3F 112.9(2) . . ? C5F C4F C3F 137.2(2) . . ? C4F C5F C6F 104.5(2) . . ? C4F C5F H5FA 127.7 . . ? C6F C5F H5FA 127.7 . . ? N3F C6F C5F 109.6(2) . . ? N3F C6F C7F 120.4(2) . . ? C5F C6F C7F 130.0(2) . . ? C6F C7F H7FA 109.5 . . ? C6F C7F H7FB 109.5 . . ? H7FA C7F H7FB 109.5 . . ? C6F C7F H7FC 109.5 . . ? H7FA C7F H7FC 109.5 . . ? H7FB C7F H7FC 109.5 . . ? C1S O1S H1S 109.5 . . ? O1S C1S H1S3 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S3 C1S H1S2 109.5 . . ? O1S C1S H1S1 109.5 . . ? H1S3 C1S H1S1 109.5 . . ? H1S2 C1S H1S1 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 N2B Fe1 N1A C3A -55.4(7) . . . . ? N2C Fe1 N1A C3A 99.86(17) . . . . ? N2A Fe1 N1A C3A 2.88(16) . . . . ? N1B Fe1 N1A C3A -84.80(17) . . . . ? N1C Fe1 N1A C3A 179.52(17) . . . . ? N2B Fe1 N1A C2A 124.9(6) . . . . ? N2C Fe1 N1A C2A -79.91(17) . . . . ? N2A Fe1 N1A C2A -176.88(18) . . . . ? N1B Fe1 N1A C2A 95.44(17) . . . . ? N1C Fe1 N1A C2A -0.24(18) . . . . ? N2B Fe1 N2A C4A 168.05(16) . . . . ? N2C Fe1 N2A C4A -94.66(16) . . . . ? N1A Fe1 N2A C4A -6.47(16) . . . . ? N1B Fe1 N2A C4A 88.49(17) . . . . ? N1C Fe1 N2A C4A -40.2(8) . . . . ? N2B Fe1 N2A N3A 4.3(2) . . . . ? N2C Fe1 N2A N3A 101.6(2) . . . . ? N1A Fe1 N2A N3A -170.2(2) . . . . ? N1B Fe1 N2A N3A -75.3(2) . . . . ? N1C Fe1 N2A N3A 156.0(6) . . . . ? C4A N2A N3A C6A 0.5(2) . . . . ? Fe1 N2A N3A C6A 165.21(18) . . . . ? N2B Fe1 N1B C3B 0.82(15) . . . . ? N2C Fe1 N1B C3B -51.5(7) . . . . ? N2A Fe1 N1B C3B 98.05(16) . . . . ? N1A Fe1 N1B C3B 177.63(16) . . . . ? N1C Fe1 N1B C3B -86.67(16) . . . . ? N2B Fe1 N1B C2B -178.91(17) . . . . ? N2C Fe1 N1B C2B 128.8(6) . . . . ? N2A Fe1 N1B C2B -81.68(17) . . . . ? N1A Fe1 N1B C2B -2.11(17) . . . . ? N1C Fe1 N1B C2B 93.60(17) . . . . ? N2C Fe1 N2B C4B 170.30(15) . . . . ? N2A Fe1 N2B C4B -92.07(15) . . . . ? N1A Fe1 N2B C4B -34.6(7) . . . . ? N1B Fe1 N2B C4B -4.79(14) . . . . ? N1C Fe1 N2B C4B 90.79(15) . . . . ? N2C Fe1 N2B N3B 6.3(2) . . . . ? N2A Fe1 N2B N3B 103.9(2) . . . . ? N1A Fe1 N2B N3B 161.3(6) . . . . ? N1B Fe1 N2B N3B -168.8(2) . . . . ? N1C Fe1 N2B N3B -73.2(2) . . . . ? C4B N2B N3B C6B 0.0(2) . . . . ? Fe1 N2B N3B C6B 165.02(16) . . . . ? N2B Fe1 N1C C3C 98.38(16) . . . . ? N2C Fe1 N1C C3C 1.61(15) . . . . ? N2A Fe1 N1C C3C -53.5(8) . . . . ? N1A Fe1 N1C C3C -86.86(16) . . . . ? N1B Fe1 N1C C3C 178.00(16) . . . . ? N2B Fe1 N1C C2C -81.13(17) . . . . ? N2C Fe1 N1C C2C -177.89(17) . . . . ? N2A Fe1 N1C C2C 127.0(7) . . . . ? N1A Fe1 N1C C2C 93.63(17) . . . . ? N1B Fe1 N1C C2C -1.50(17) . . . . ? N2B Fe1 N2C N3C 102.76(19) . . . . ? N2A Fe1 N2C N3C 5.1(2) . . . . ? N1A Fe1 N2C N3C -74.5(2) . . . . ? N1B Fe1 N2C N3C 154.3(6) . . . . ? N1C Fe1 N2C N3C -170.0(2) . . . . ? N2B Fe1 N2C C4C -92.55(15) . . . . ? N2A Fe1 N2C C4C 169.74(14) . . . . ? N1A Fe1 N2C C4C 90.14(15) . . . . ? N1B Fe1 N2C C4C -41.0(7) . . . . ? N1C Fe1 N2C C4C -5.29(14) . . . . ? C4C N2C N3C C6C -0.2(2) . . . . ? Fe1 N2C N3C C6C 165.30(16) . . . . ? N2F Fe2 N1D C3D -53.2(11) . . . . ? N2E Fe2 N1D C3D 95.88(16) . . . . ? N2D Fe2 N1D C3D -0.43(15) . . . . ? N1F Fe2 N1D C3D -86.78(16) . . . . ? N1E Fe2 N1D C3D 176.18(16) . . . . ? N2F Fe2 N1D C2D 127.4(10) . . . . ? N2E Fe2 N1D C2D -83.54(17) . . . . ? N2D Fe2 N1D C2D -179.85(18) . . . . ? N1F Fe2 N1D C2D 93.80(17) . . . . ? N1E Fe2 N1D C2D -3.24(17) . . . . ? N2F Fe2 N2D N3D 7.6(2) . . . . ? N2E Fe2 N2D N3D 104.51(19) . . . . ? N1D Fe2 N2D N3D -169.2(2) . . . . ? N1F Fe2 N2D N3D -72.19(19) . . . . ? N1E Fe2 N2D N3D 152.7(7) . . . . ? N2F Fe2 N2D C4D 174.10(14) . . . . ? N2E Fe2 N2D C4D -88.95(15) . . . . ? N1D Fe2 N2D C4D -2.62(14) . . . . ? N1F Fe2 N2D C4D 94.34(15) . . . . ? N1E Fe2 N2D C4D -40.8(8) . . . . ? C4D N2D N3D C6D 0.4(2) . . . . ? Fe2 N2D N3D C6D 167.51(15) . . . . ? N2F Fe2 N1E C3E 96.87(16) . . . . ? N2E Fe2 N1E C3E 0.21(16) . . . . ? N2D Fe2 N1E C3E -48.5(8) . . . . ? N1D Fe2 N1E C3E -86.24(17) . . . . ? N1F Fe2 N1E C3E 176.67(16) . . . . ? N2F Fe2 N1E C2E -81.87(18) . . . . ? N2E Fe2 N1E C2E -178.53(18) . . . . ? N2D Fe2 N1E C2E 132.7(7) . . . . ? N1D Fe2 N1E C2E 95.02(18) . . . . ? N1F Fe2 N1E C2E -2.07(18) . . . . ? N2F Fe2 N2E N3E 102.8(2) . . . . ? N2D Fe2 N2E N3E 5.1(2) . . . . ? N1D Fe2 N2E N3E -75.0(2) . . . . ? N1F Fe2 N2E N3E 139.8(8) . . . . ? N1E Fe2 N2E N3E -170.7(2) . . . . ? N2F Fe2 N2E C4E -89.83(16) . . . . ? N2D Fe2 N2E C4E 172.46(16) . . . . ? N1D Fe2 N2E C4E 92.28(16) . . . . ? N1F Fe2 N2E C4E -52.9(9) . . . . ? N1E Fe2 N2E C4E -3.41(16) . . . . ? C4E N2E N3E C6E 1.0(2) . . . . ? Fe2 N2E N3E C6E 168.94(17) . . . . ? N2F Fe2 N1F C3F 0.30(15) . . . . ? N2E Fe2 N1F C3F -37.0(9) . . . . ? N2D Fe2 N1F C3F 97.85(15) . . . . ? N1D Fe2 N1F C3F 178.00(15) . . . . ? N1E Fe2 N1F C3F -86.03(15) . . . . ? N2F Fe2 N1F C2F -178.91(17) . . . . ? N2E Fe2 N1F C2F 143.7(8) . . . . ? N2D Fe2 N1F C2F -81.37(16) . . . . ? N1D Fe2 N1F C2F -1.21(17) . . . . ? N1E Fe2 N1F C2F 94.76(16) . . . . ? N2E Fe2 N2F N3F 7.29(19) . . . . ? N2D Fe2 N2F N3F 103.91(19) . . . . ? N1D Fe2 N2F N3F 156.2(9) . . . . ? N1F Fe2 N2F N3F -169.9(2) . . . . ? N1E Fe2 N2F N3F -72.97(19) . . . . ? N2E Fe2 N2F C4F 173.50(15) . . . . ? N2D Fe2 N2F C4F -89.87(15) . . . . ? N1D Fe2 N2F C4F -37.6(11) . . . . ? N1F Fe2 N2F C4F -3.67(14) . . . . ? N1E Fe2 N2F C4F 93.25(15) . . . . ? C4F N2F N3F C6F 0.6(2) . . . . ? Fe2 N2F N3F C6F 167.50(15) . . . . ? C1C N1 C1A C2A 72.4(3) . . . . ? C1B N1 C1A C2A -110.9(2) . . . . ? C3A N1A C2A C1A 96.5(2) . . . . ? Fe1 N1A C2A C1A -83.7(2) . . . . ? N1 C1A C2A N1A 54.4(3) . . . . ? C2A N1A C3A C4A -179.23(18) . . . . ? Fe1 N1A C3A C4A 1.0(3) . . . . ? N3A N2A C4A C5A -0.1(3) . . . . ? Fe1 N2A C4A C5A -168.62(16) . . . . ? N3A N2A C4A C3A 177.23(19) . . . . ? Fe1 N2A C4A C3A 8.7(2) . . . . ? N1A C3A C4A N2A -6.3(3) . . . . ? N1A C3A C4A C5A 170.0(3) . . . . ? N2A C4A C5A C6A -0.3(3) . . . . ? C3A C4A C5A C6A -176.7(3) . . . . ? N2A N3A C6A C5A -0.7(3) . . . . ? N2A N3A C6A C7A -177.8(2) . . . . ? C4A C5A C6A N3A 0.6(3) . . . . ? C4A C5A C6A C7A 177.3(3) . . . . ? C1A N1 C1B C2B 71.9(3) . . . . ? C1C N1 C1B C2B -111.4(2) . . . . ? C3B N1B C2B C1B 98.3(2) . . . . ? Fe1 N1B C2B C1B -82.0(2) . . . . ? N1 C1B C2B N1B 54.7(3) . . . . ? C2B N1B C3B C4B -177.24(18) . . . . ? Fe1 N1B C3B C4B 3.0(2) . . . . ? N3B N2B C4B C5B -0.2(2) . . . . ? Fe1 N2B C4B C5B -168.74(14) . . . . ? N3B N2B C4B C3B 176.14(17) . . . . ? Fe1 N2B C4B C3B 7.6(2) . . . . ? N1B C3B C4B N2B -6.9(3) . . . . ? N1B C3B C4B C5B 168.1(2) . . . . ? N2B C4B C5B C6B 0.2(2) . . . . ? C3B C4B C5B C6B -174.9(2) . . . . ? N2B N3B C6B C5B 0.1(2) . . . . ? N2B N3B C6B C7B -179.31(18) . . . . ? C4B C5B C6B N3B -0.2(2) . . . . ? C4B C5B C6B C7B 179.1(2) . . . . ? C1A N1 C1C C2C -111.0(2) . . . . ? C1B N1 C1C C2C 72.3(3) . . . . ? C3C N1C C2C C1C 97.4(2) . . . . ? Fe1 N1C C2C C1C -83.1(2) . . . . ? N1 C1C C2C N1C 55.2(3) . . . . ? C2C N1C C3C C4C -178.32(18) . . . . ? Fe1 N1C C3C C4C 2.1(2) . . . . ? N3C N2C C4C C5C -0.1(2) . . . . ? Fe1 N2C C4C C5C -169.23(14) . . . . ? N3C N2C C4C C3C 176.93(16) . . . . ? Fe1 N2C C4C C3C 7.8(2) . . . . ? N1C C3C C4C N2C -6.5(3) . . . . ? N1C C3C C4C C5C 169.4(2) . . . . ? N2C C4C C5C C6C 0.4(2) . . . . ? C3C C4C C5C C6C -175.7(2) . . . . ? N2C N3C C6C C5C 0.5(2) . . . . ? N2C N3C C6C C7C -177.24(18) . . . . ? C4C C5C C6C N3C -0.5(2) . . . . ? C4C C5C C6C C7C 176.9(2) . . . . ? C1F N2 C1D C2D -114.2(2) . . . . ? C1E N2 C1D C2D 77.5(2) . . . . ? C3D N1D C2D C1D 99.7(2) . . . . ? Fe2 N1D C2D C1D -80.9(2) . . . . ? N2 C1D C2D N1D 52.7(3) . . . . ? C2D N1D C3D C4D -177.30(17) . . . . ? Fe2 N1D C3D C4D 3.2(2) . . . . ? N3D N2D C4D C5D -0.7(2) . . . . ? Fe2 N2D C4D C5D -170.78(14) . . . . ? N3D N2D C4D C3D 175.10(16) . . . . ? Fe2 N2D C4D C3D 5.0(2) . . . . ? N1D C3D C4D N2D -5.4(3) . . . . ? N1D C3D C4D C5D 168.8(2) . . . . ? N2D C4D C5D C6D 0.7(2) . . . . ? C3D C4D C5D C6D -173.8(2) . . . . ? N2D N3D C6D C5D 0.0(2) . . . . ? N2D N3D C6D C7D -177.43(18) . . . . ? C4D C5D C6D N3D -0.4(2) . . . . ? C4D C5D C6D C7D 176.7(2) . . . . ? C1D N2 C1E C2E -113.2(2) . . . . ? C1F N2 C1E C2E 78.5(2) . . . . ? C3E N1E C2E C1E 101.0(2) . . . . ? Fe2 N1E C2E C1E -80.3(2) . . . . ? N2 C1E C2E N1E 51.3(2) . . . . ? C2E N1E C3E C4E -178.29(19) . . . . ? Fe2 N1E C3E C4E 2.9(3) . . . . ? N3E N2E C4E C5E -1.0(3) . . . . ? Fe2 N2E C4E C5E -171.66(15) . . . . ? N3E N2E C4E C3E 176.42(18) . . . . ? Fe2 N2E C4E C3E 5.8(3) . . . . ? N1E C3E C4E N2E -5.7(3) . . . . ? N1E C3E C4E C5E 170.7(3) . . . . ? N2E C4E C5E C6E 0.6(3) . . . . ? C3E C4E C5E C6E -175.9(3) . . . . ? N2E N3E C6E C5E -0.7(3) . . . . ? N2E N3E C6E C7E 179.5(2) . . . . ? C4E C5E C6E N3E 0.1(3) . . . . ? C4E C5E C6E C7E 179.8(2) . . . . ? C1D N2 C1F C2F 77.2(3) . . . . ? C1E N2 C1F C2F -114.6(2) . . . . ? C3F N1F C2F C1F 99.2(2) . . . . ? Fe2 N1F C2F C1F -81.6(2) . . . . ? N2 C1F C2F N1F 52.8(3) . . . . ? C2F N1F C3F C4F -177.80(17) . . . . ? Fe2 N1F C3F C4F 2.9(2) . . . . ? N3F N2F C4F C5F -0.8(2) . . . . ? Fe2 N2F C4F C5F -170.61(14) . . . . ? N3F N2F C4F C3F 175.95(16) . . . . ? Fe2 N2F C4F C3F 6.1(2) . . . . ? N1F C3F C4F N2F -5.9(3) . . . . ? N1F C3F C4F C5F 169.6(2) . . . . ? N2F C4F C5F C6F 0.7(2) . . . . ? C3F C4F C5F C6F -174.9(2) . . . . ? N2F N3F C6F C5F -0.2(2) . . . . ? N2F N3F C6F C7F -178.95(19) . . . . ? C4F C5F C6F N3F -0.3(2) . . . . ? C4F C5F C6F C7F 178.3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1S H1S F21 0.84 2.37 3.125(5) 150.5 2_775 N3A H3A N3F 0.90(3) 1.85(3) 2.743(2) 173(3) . N3B H3B N3D 0.85(3) 1.89(3) 2.735(3) 175(3) . N3C H3C N3E 1.22(4) 1.54(4) 2.752(2) 174(3) . N3C H3C N2E 1.22(4) 2.59(4) 3.722(2) 155(2) . _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.636 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.072 data_ams-4a _database_code_depnum_ccdc_archive 'CCDC 766394' #TrackingRef 'AMS-4ART.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H57 Fe2 N20, 2(B F4)' _chemical_formula_sum 'C42 H57 B2 F8 Fe2 N20' _chemical_formula_weight 1127.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.3419(3) _cell_length_b 12.5140(2) _cell_length_c 19.6566(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.0491(13) _cell_angle_gamma 90.00 _cell_volume 5242.33(14) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6073 _cell_measurement_theta_min 4.5013 _cell_measurement_theta_max 77.3582 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2332 _exptl_absorpt_coefficient_mu 5.138 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.44340 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12868 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 4.51 _diffrn_reflns_theta_max 77.48 _reflns_number_total 5494 _reflns_number_gt 4193 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Shelxtl (Bruker, 1998)' _computing_publication_material Shelxtl _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1164P)^2^] 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 5494 _refine_ls_number_parameters 378 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1632 _refine_ls_wR_factor_gt 0.1536 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.370774(19) 0.63338(3) 0.69282(2) 0.04202(16) Uani 1 1 d . . . N N 0.22510(15) 0.6477(3) 0.62780(18) 0.0682(8) Uani 1 1 d . . . N1A N 0.33855(11) 0.5233(2) 0.62353(13) 0.0509(6) Uani 1 1 d . . . N2A N 0.40521(12) 0.4986(2) 0.73458(12) 0.0491(5) Uani 1 1 d . . . N3A N 0.43341(14) 0.4689(3) 0.79392(14) 0.0658(8) Uani 1 1 d . . . H3AB H 0.4481 0.5118 0.8250 0.079 Uiso 0.66(3) 1 calc PR . . N1B N 0.29708(14) 0.6217(2) 0.75382(15) 0.0574(6) Uani 1 1 d . . . N2B N 0.39833(13) 0.7311(2) 0.76885(17) 0.0631(7) Uani 1 1 d . . . N3B N 0.44319(17) 0.8055(3) 0.7795(3) 0.0960(14) Uani 1 1 d . . . H3BB H 0.4752 0.8143 0.7554 0.115 Uiso 0.26(6) 1 calc PR . . N1C N 0.34066(12) 0.7631(2) 0.63843(14) 0.0541(6) Uani 1 1 d . . . N2C N 0.44307(12) 0.6574(2) 0.63467(13) 0.0532(6) Uani 1 1 d . . . N3C N 0.49479(14) 0.6026(3) 0.61938(14) 0.0671(8) Uani 1 1 d . . . H3CB H 0.5099 0.5484 0.6415 0.080 Uiso 0.58(6) 1 calc PR . . C1A C 0.23251(17) 0.5668(4) 0.5769(2) 0.0739(10) Uani 1 1 d . . . H1AA H 0.2091 0.5881 0.5354 0.089 Uiso 1 1 calc R . . H1AB H 0.2144 0.5007 0.5924 0.089 Uiso 1 1 calc R . . C2A C 0.30032(16) 0.5462(3) 0.56047(17) 0.0649(9) Uani 1 1 d . . . H2AA H 0.3022 0.4859 0.5296 0.078 Uiso 1 1 calc R . . H2AB H 0.3170 0.6083 0.5381 0.078 Uiso 1 1 calc R . . C3A C 0.35348(14) 0.4263(3) 0.63706(16) 0.0525(7) Uani 1 1 d . . . H3AA H 0.3423 0.3707 0.6075 0.063 Uiso 1 1 calc R . . C4A C 0.38871(14) 0.4081(3) 0.70069(16) 0.0504(6) Uani 1 1 d . . . C5A C 0.40715(16) 0.3195(3) 0.73877(19) 0.0607(8) Uani 1 1 d . . . H5AA H 0.4018 0.2479 0.7272 0.073 Uiso 1 1 calc R . . C6A C 0.43519(18) 0.3609(3) 0.7974(2) 0.0684(10) Uani 1 1 d . . . C7A C 0.4620(2) 0.3060(5) 0.8598(2) 0.0974(16) Uani 1 1 d . . . H7AA H 0.4885 0.2483 0.8468 0.146 Uiso 1 1 calc R . . H7AB H 0.4285 0.2783 0.8854 0.146 Uiso 1 1 calc R . . H7AC H 0.4862 0.3560 0.8873 0.146 Uiso 1 1 calc R . . C1B C 0.19631(17) 0.6186(4) 0.6889(2) 0.0759(11) Uani 1 1 d . . . H1BA H 0.1602 0.5737 0.6774 0.091 Uiso 1 1 calc R . . H1BB H 0.1813 0.6828 0.7104 0.091 Uiso 1 1 calc R . . C2B C 0.24022(17) 0.5593(3) 0.7399(2) 0.0703(9) Uani 1 1 d . . . H2BA H 0.2193 0.5476 0.7819 0.084 Uiso 1 1 calc R . . H2BB H 0.2510 0.4901 0.7215 0.084 Uiso 1 1 calc R . . C3B C 0.30224(18) 0.6769(3) 0.80911(19) 0.0657(9) Uani 1 1 d . . . H3BA H 0.2722 0.6736 0.8416 0.079 Uiso 1 1 calc R . . C4B C 0.35622(18) 0.7433(3) 0.81794(18) 0.0658(9) Uani 1 1 d . . . C5B C 0.3756(3) 0.8271(4) 0.8604(3) 0.0932(16) Uani 1 1 d . . . H5BA H 0.3561 0.8527 0.8983 0.112 Uiso 1 1 calc R . . C6B C 0.4298(3) 0.8636(4) 0.8341(4) 0.111(2) Uani 1 1 d . . . C7B C 0.4715(3) 0.9552(4) 0.8584(5) 0.169(4) Uani 1 1 d . . . H7BA H 0.4989 0.9744 0.8232 0.254 Uiso 1 1 calc R . . H7BB H 0.4960 0.9337 0.8985 0.254 Uiso 1 1 calc R . . H7BC H 0.4460 1.0155 0.8690 0.254 Uiso 1 1 calc R . . C1C C 0.22791(17) 0.7583(3) 0.6091(2) 0.0759(11) Uani 1 1 d . . . H1CA H 0.1886 0.7924 0.6190 0.091 Uiso 1 1 calc R . . H1CB H 0.2326 0.7634 0.5604 0.091 Uiso 1 1 calc R . . C2C C 0.28148(18) 0.8183(3) 0.6460(2) 0.0701(9) Uani 1 1 d . . . H2CA H 0.2840 0.8900 0.6276 0.084 Uiso 1 1 calc R . . H2CB H 0.2735 0.8242 0.6940 0.084 Uiso 1 1 calc R . . C3C C 0.37865(16) 0.7975(3) 0.59469(17) 0.0585(8) Uani 1 1 d . . . H3CA H 0.3702 0.8586 0.5689 0.070 Uiso 1 1 calc R . . C4C C 0.43512(15) 0.7357(3) 0.58800(15) 0.0545(7) Uani 1 1 d . . . C5C C 0.48277(17) 0.7305(4) 0.54220(16) 0.0663(9) Uani 1 1 d . . . H5CA H 0.4885 0.7746 0.5050 0.080 Uiso 1 1 calc R . . C6C C 0.51908(18) 0.6461(4) 0.56410(18) 0.0707(10) Uani 1 1 d . . . C7C C 0.5772(2) 0.5996(5) 0.5351(2) 0.0942(15) Uani 1 1 d . . . H7CA H 0.5990 0.5564 0.5691 0.141 Uiso 1 1 calc R . . H7CB H 0.6040 0.6565 0.5217 0.141 Uiso 1 1 calc R . . H7CC H 0.5654 0.5563 0.4962 0.141 Uiso 1 1 calc R . . B B 0.3597(2) 0.1100(3) 0.57813(19) 0.104(2) Uani 1 1 d D . . F1 F 0.3996(4) 0.0682(8) 0.5367(5) 0.188(5) Uani 0.486(7) 1 d PDU A 1 F2 F 0.3839(4) 0.1067(9) 0.6412(3) 0.222(5) Uani 0.486(7) 1 d PDU A 1 F3 F 0.3070(3) 0.0546(7) 0.5740(4) 0.159(4) Uani 0.486(7) 1 d PDU A 1 F4 F 0.3479(5) 0.2099(4) 0.5606(6) 0.244(6) Uani 0.486(7) 1 d PDU A 1 F1A F 0.4041(4) 0.1832(6) 0.5753(4) 0.178(4) Uani 0.514(7) 1 d PDU A 2 F2A F 0.3636(5) 0.0639(7) 0.6385(3) 0.193(5) Uani 0.514(7) 1 d PDU A 2 F3A F 0.3674(5) 0.0377(5) 0.5305(4) 0.145(4) Uani 0.514(7) 1 d PDU A 2 F4A F 0.3044(4) 0.1555(8) 0.5683(6) 0.277(6) Uani 0.514(7) 1 d PDU 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 Fe 0.0449(2) 0.0383(2) 0.0433(2) 0.00098(17) 0.00625(15) 0.00061(17) N 0.0608(17) 0.068(2) 0.0759(19) -0.0032(15) 0.0022(14) -0.0010(14) N1A 0.0467(13) 0.0567(16) 0.0494(13) -0.0044(11) 0.0038(10) -0.0024(11) N2A 0.0558(13) 0.0481(14) 0.0437(12) 0.0028(10) 0.0062(10) -0.0056(11) N3A 0.0705(17) 0.080(2) 0.0470(14) 0.0123(14) 0.0008(12) -0.0246(15) N1B 0.0579(15) 0.0555(16) 0.0592(15) 0.0039(12) 0.0071(12) 0.0024(12) N2B 0.0556(15) 0.0436(14) 0.090(2) -0.0031(14) -0.0028(13) 0.0037(12) N3B 0.0597(18) 0.0400(16) 0.186(4) -0.009(2) -0.019(2) 0.0053(13) N1C 0.0528(13) 0.0480(14) 0.0609(15) 0.0012(12) -0.0019(11) 0.0017(11) N2C 0.0533(14) 0.0629(17) 0.0438(12) 0.0090(11) 0.0051(10) 0.0075(11) N3C 0.0640(17) 0.094(2) 0.0434(13) -0.0017(14) 0.0056(11) 0.0250(16) C1A 0.0546(18) 0.082(3) 0.083(2) -0.017(2) -0.0122(17) -0.0044(17) C2A 0.0624(19) 0.080(2) 0.0507(16) -0.0055(17) -0.0073(14) 0.0048(17) C3A 0.0525(15) 0.0500(18) 0.0556(16) -0.0095(13) 0.0083(12) -0.0060(13) C4A 0.0517(15) 0.0466(15) 0.0539(16) -0.0009(13) 0.0126(12) -0.0042(12) C5A 0.0592(18) 0.0501(18) 0.073(2) 0.0106(16) 0.0099(15) -0.0079(14) C6A 0.0623(19) 0.078(3) 0.064(2) 0.0228(18) 0.0041(15) -0.0186(17) C7A 0.086(3) 0.116(4) 0.089(3) 0.050(3) -0.008(2) -0.020(3) C1B 0.0445(17) 0.086(3) 0.098(3) -0.006(2) 0.0110(17) 0.0006(16) C2B 0.064(2) 0.068(2) 0.080(2) 0.0033(19) 0.0164(17) -0.0117(17) C3B 0.070(2) 0.067(2) 0.0605(19) 0.0004(17) 0.0095(15) 0.0149(17) C4B 0.072(2) 0.063(2) 0.0612(19) -0.0091(16) -0.0074(16) 0.0201(17) C5B 0.097(3) 0.075(3) 0.104(3) -0.028(3) -0.032(3) 0.032(3) C6B 0.087(3) 0.053(2) 0.187(6) -0.020(3) -0.057(4) 0.018(2) C7B 0.114(4) 0.056(3) 0.326(11) -0.058(5) -0.088(6) 0.015(3) C1C 0.0547(19) 0.075(3) 0.096(3) 0.013(2) -0.0077(18) 0.0114(17) C2C 0.066(2) 0.0485(19) 0.095(3) -0.0004(18) 0.0010(18) 0.0119(16) C3C 0.0676(19) 0.0482(17) 0.0582(17) 0.0098(14) -0.0099(14) -0.0046(14) C4C 0.0569(16) 0.0593(19) 0.0470(15) 0.0096(13) -0.0014(12) -0.0072(14) C5C 0.070(2) 0.085(3) 0.0447(15) 0.0082(16) 0.0061(14) -0.0127(18) C6C 0.064(2) 0.102(3) 0.0467(17) -0.0062(18) 0.0073(14) 0.0028(19) C7C 0.081(3) 0.138(5) 0.066(2) -0.009(3) 0.022(2) 0.020(3) B 0.137(6) 0.070(4) 0.109(5) -0.009(3) 0.042(4) -0.011(4) F1 0.198(10) 0.195(11) 0.178(9) -0.033(8) 0.067(8) -0.014(8) F2 0.245(11) 0.289(12) 0.132(8) -0.049(8) 0.008(7) -0.137(9) F3 0.241(9) 0.100(5) 0.140(6) -0.017(5) 0.029(6) -0.056(6) F4 0.271(14) 0.053(4) 0.407(13) -0.014(7) 0.006(12) -0.013(7) F1A 0.208(9) 0.136(7) 0.193(8) -0.024(6) 0.034(7) -0.092(6) F2A 0.198(9) 0.275(12) 0.108(6) 0.025(7) 0.023(5) -0.132(8) F3A 0.232(10) 0.083(4) 0.119(5) -0.038(4) -0.009(6) -0.035(5) F4A 0.191(10) 0.217(12) 0.426(14) 0.029(12) 0.042(11) 0.057(9) _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 Fe N2C 1.991(3) . ? Fe N2B 1.995(3) . ? Fe N2A 1.998(3) . ? Fe N1C 2.029(3) . ? Fe N1A 2.031(3) . ? Fe N1B 2.033(3) . ? N C1B 1.426(6) . ? N C1C 1.435(5) . ? N C1A 1.438(5) . ? N1A C3A 1.279(4) . ? N1A C2A 1.475(4) . ? N2A N3A 1.336(4) . ? N2A C4A 1.351(4) . ? N3A C6A 1.354(5) . ? N3A H3AB 0.8600 . ? N1B C3B 1.288(5) . ? N1B C2B 1.457(5) . ? N2B N3B 1.344(4) . ? N2B C4B 1.362(5) . ? N3B C6B 1.340(8) . ? N3B H3BB 0.8600 . ? N1C C3C 1.287(4) . ? N1C C2C 1.454(4) . ? N2C N3C 1.347(4) . ? N2C C4C 1.347(4) . ? N3C C6C 1.344(5) . ? N3C H3CB 0.8600 . ? C1A C2A 1.522(5) . ? C1A H1AA 0.9700 . ? C1A H1AB 0.9700 . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A C4A 1.443(4) . ? C3A H3AA 0.9300 . ? C4A C5A 1.384(5) . ? C5A C6A 1.371(5) . ? C5A H5AA 0.9300 . ? C6A C7A 1.494(5) . ? C7A H7AA 0.9600 . ? C7A H7AB 0.9600 . ? C7A H7AC 0.9600 . ? C1B C2B 1.528(6) . ? C1B H1BA 0.9700 . ? C1B H1BB 0.9700 . ? C2B H2BA 0.9700 . ? C2B H2BB 0.9700 . ? C3B C4B 1.424(6) . ? C3B H3BA 0.9300 . ? C4B C5B 1.388(6) . ? C5B C6B 1.370(9) . ? C5B H5BA 0.9300 . ? C6B C7B 1.512(7) . ? C7B H7BA 0.9600 . ? C7B H7BB 0.9600 . ? C7B H7BC 0.9600 . ? C1C C2C 1.520(5) . ? C1C H1CA 0.9700 . ? C1C H1CB 0.9700 . ? C2C H2CA 0.9700 . ? C2C H2CB 0.9700 . ? C3C C4C 1.444(5) . ? C3C H3CA 0.9300 . ? C4C C5C 1.395(5) . ? C5C C6C 1.366(6) . ? C5C H5CA 0.9300 . ? C6C C7C 1.508(5) . ? C7C H7CA 0.9600 . ? C7C H7CB 0.9600 . ? C7C H7CC 0.9600 . ? B F4A 1.317(3) . ? B F2 1.317(3) . ? B F4 1.317(3) . ? B F1 1.318(3) . ? B F3A 1.318(3) . ? B F2A 1.319(3) . ? B F1A 1.321(3) . ? B F3 1.321(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2C Fe N2B 97.54(12) . . ? N2C Fe N2A 94.80(10) . . ? N2B Fe N2A 97.01(11) . . ? N2C Fe N1C 79.07(11) . . ? N2B Fe N1C 88.67(12) . . ? N2A Fe N1C 172.17(11) . . ? N2C Fe N1A 87.84(11) . . ? N2B Fe N1A 173.54(12) . . ? N2A Fe N1A 78.89(11) . . ? N1C Fe N1A 95.90(11) . . ? N2C Fe N1B 175.39(12) . . ? N2B Fe N1B 78.97(13) . . ? N2A Fe N1B 88.64(11) . . ? N1C Fe N1B 97.75(11) . . ? N1A Fe N1B 95.84(11) . . ? C1B N C1C 119.2(4) . . ? C1B N C1A 118.4(4) . . ? C1C N C1A 119.5(4) . . ? C3A N1A C2A 118.6(3) . . ? C3A N1A Fe 115.6(2) . . ? C2A N1A Fe 125.8(2) . . ? N3A N2A C4A 106.9(3) . . ? N3A N2A Fe 137.0(2) . . ? C4A N2A Fe 115.1(2) . . ? N2A N3A C6A 109.3(3) . . ? N2A N3A H3AB 125.3 . . ? C6A N3A H3AB 125.3 . . ? C3B N1B C2B 118.6(3) . . ? C3B N1B Fe 115.2(3) . . ? C2B N1B Fe 126.2(2) . . ? N3B N2B C4B 107.6(4) . . ? N3B N2B Fe 136.1(3) . . ? C4B N2B Fe 114.9(2) . . ? C6B N3B N2B 108.7(5) . . ? C6B N3B H3BB 125.6 . . ? N2B N3B H3BB 125.6 . . ? C3C N1C C2C 119.4(3) . . ? C3C N1C Fe 115.2(2) . . ? C2C N1C Fe 125.3(2) . . ? N3C N2C C4C 107.1(3) . . ? N3C N2C Fe 136.1(2) . . ? C4C N2C Fe 115.3(2) . . ? C6C N3C N2C 109.3(3) . . ? C6C N3C H3CB 125.3 . . ? N2C N3C H3CB 125.3 . . ? N C1A C2A 114.1(3) . . ? N C1A H1AA 108.7 . . ? C2A C1A H1AA 108.7 . . ? N C1A H1AB 108.7 . . ? C2A C1A H1AB 108.7 . . ? H1AA C1A H1AB 107.6 . . ? N1A C2A C1A 110.2(3) . . ? N1A C2A H2AA 109.6 . . ? C1A C2A H2AA 109.6 . . ? N1A C2A H2AB 109.6 . . ? C1A C2A H2AB 109.6 . . ? H2AA C2A H2AB 108.1 . . ? N1A C3A C4A 116.3(3) . . ? N1A C3A H3AA 121.9 . . ? C4A C3A H3AA 121.9 . . ? N2A C4A C5A 110.3(3) . . ? N2A C4A C3A 113.9(3) . . ? C5A C4A C3A 135.7(3) . . ? C6A C5A C4A 104.5(3) . . ? C6A C5A H5AA 127.8 . . ? C4A C5A H5AA 127.8 . . ? N3A C6A C5A 109.0(3) . . ? N3A C6A C7A 120.6(4) . . ? C5A C6A C7A 130.3(4) . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? N C1B C2B 113.6(3) . . ? N C1B H1BA 108.8 . . ? C2B C1B H1BA 108.8 . . ? N C1B H1BB 108.8 . . ? C2B C1B H1BB 108.8 . . ? H1BA C1B H1BB 107.7 . . ? N1B C2B C1B 109.7(3) . . ? N1B C2B H2BA 109.7 . . ? C1B C2B H2BA 109.7 . . ? N1B C2B H2BB 109.7 . . ? C1B C2B H2BB 109.7 . . ? H2BA C2B H2BB 108.2 . . ? N1B C3B C4B 116.7(3) . . ? N1B C3B H3BA 121.7 . . ? C4B C3B H3BA 121.7 . . ? N2B C4B C5B 108.9(4) . . ? N2B C4B C3B 114.1(3) . . ? C5B C4B C3B 136.6(4) . . ? C6B C5B C4B 104.9(5) . . ? C6B C5B H5BA 127.6 . . ? C4B C5B H5BA 127.6 . . ? N3B C6B C5B 109.9(4) . . ? N3B C6B C7B 121.1(7) . . ? C5B C6B C7B 128.9(7) . . ? C6B C7B H7BA 109.5 . . ? C6B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C6B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N C1C C2C 113.3(3) . . ? N C1C H1CA 108.9 . . ? C2C C1C H1CA 108.9 . . ? N C1C H1CB 108.9 . . ? C2C C1C H1CB 108.9 . . ? H1CA C1C H1CB 107.7 . . ? N1C C2C C1C 110.6(3) . . ? N1C C2C H2CA 109.5 . . ? C1C C2C H2CA 109.5 . . ? N1C C2C H2CB 109.5 . . ? C1C C2C H2CB 109.5 . . ? H2CA C2C H2CB 108.1 . . ? N1C C3C C4C 116.1(3) . . ? N1C C3C H3CA 121.9 . . ? C4C C3C H3CA 121.9 . . ? N2C C4C C5C 109.6(3) . . ? N2C C4C C3C 113.8(3) . . ? C5C C4C C3C 136.4(3) . . ? C6C C5C C4C 104.7(3) . . ? C6C C5C H5CA 127.7 . . ? C4C C5C H5CA 127.7 . . ? N3C C6C C5C 109.3(3) . . ? N3C C6C C7C 120.6(4) . . ? C5C C6C C7C 130.0(4) . . ? C6C C7C H7CA 109.5 . . ? C6C C7C H7CB 109.5 . . ? H7CA C7C H7CB 109.5 . . ? C6C C7C H7CC 109.5 . . ? H7CA C7C H7CC 109.5 . . ? H7CB C7C H7CC 109.5 . . ? F4A B F2 117.1(7) . . ? F4A B F4 52.6(4) . . ? F2 B F4 109.63(10) . . ? F4A B F1 133.2(7) . . ? F2 B F1 109.64(10) . . ? F4 B F1 109.62(10) . . ? F4A B F3A 109.69(10) . . ? F2 B F3A 126.1(8) . . ? F4 B F3A 119.6(8) . . ? F1 B F3A 34.9(4) . . ? F4A B F2A 109.60(10) . . ? F2 B F2A 30.3(4) . . ? F4 B F2A 130.8(8) . . ? F1 B F2A 111.8(8) . . ? F3A B F2A 109.52(10) . . ? F4A B F1A 109.43(10) . . ? F2 B F1A 79.4(4) . . ? F4 B F1A 57.2(4) . . ? F1 B F1A 76.2(4) . . ? F3A B F1A 109.30(10) . . ? F2A B F1A 109.29(10) . . ? F4A B F3 57.5(4) . . ? F2 B F3 109.33(10) . . ? F4 B F3 109.30(10) . . ? F1 B F3 109.31(10) . . ? F3A B F3 74.6(4) . . ? F2A B F3 80.7(4) . . ? F1A B F3 166.4(4) . . ? 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 N2C Fe N1A C3A 95.5(2) . . . . ? N2B Fe N1A C3A -50.9(10) . . . . ? N2A Fe N1A C3A 0.2(2) . . . . ? N1C Fe N1A C3A 174.3(2) . . . . ? N1B Fe N1A C3A -87.3(2) . . . . ? N2C Fe N1A C2A -84.4(3) . . . . ? N2B Fe N1A C2A 129.2(9) . . . . ? N2A Fe N1A C2A -179.8(3) . . . . ? N1C Fe N1A C2A -5.7(3) . . . . ? N1B Fe N1A C2A 92.8(3) . . . . ? N2C Fe N2A N3A 103.2(3) . . . . ? N2B Fe N2A N3A 5.0(3) . . . . ? N1C Fe N2A N3A 141.3(7) . . . . ? N1A Fe N2A N3A -170.0(3) . . . . ? N1B Fe N2A N3A -73.7(3) . . . . ? N2C Fe N2A C4A -89.8(2) . . . . ? N2B Fe N2A C4A 171.9(2) . . . . ? N1C Fe N2A C4A -51.7(8) . . . . ? N1A Fe N2A C4A -3.0(2) . . . . ? N1B Fe N2A C4A 93.2(2) . . . . ? C4A N2A N3A C6A 0.5(4) . . . . ? Fe N2A N3A C6A 168.2(3) . . . . ? N2C Fe N1B C3B -41.8(14) . . . . ? N2B Fe N1B C3B -0.9(3) . . . . ? N2A Fe N1B C3B 96.6(3) . . . . ? N1C Fe N1B C3B -88.0(3) . . . . ? N1A Fe N1B C3B 175.2(3) . . . . ? N2C Fe N1B C2B 137.1(13) . . . . ? N2B Fe N1B C2B 178.1(3) . . . . ? N2A Fe N1B C2B -84.5(3) . . . . ? N1C Fe N1B C2B 91.0(3) . . . . ? N1A Fe N1B C2B -5.8(3) . . . . ? N2C Fe N2B N3B 10.1(3) . . . . ? N2A Fe N2B N3B 105.9(3) . . . . ? N1C Fe N2B N3B -68.7(3) . . . . ? N1A Fe N2B N3B 156.2(8) . . . . ? N1B Fe N2B N3B -166.8(4) . . . . ? N2C Fe N2B C4B 174.5(2) . . . . ? N2A Fe N2B C4B -89.7(3) . . . . ? N1C Fe N2B C4B 95.7(3) . . . . ? N1A Fe N2B C4B -39.4(11) . . . . ? N1B Fe N2B C4B -2.4(2) . . . . ? C4B N2B N3B C6B -0.1(5) . . . . ? Fe N2B N3B C6B 165.1(3) . . . . ? N2C Fe N1C C3C 0.6(2) . . . . ? N2B Fe N1C C3C 98.6(3) . . . . ? N2A Fe N1C C3C -38.2(9) . . . . ? N1A Fe N1C C3C -86.0(3) . . . . ? N1B Fe N1C C3C 177.2(2) . . . . ? N2C Fe N1C C2C -178.6(3) . . . . ? N2B Fe N1C C2C -80.7(3) . . . . ? N2A Fe N1C C2C 142.5(7) . . . . ? N1A Fe N1C C2C 94.7(3) . . . . ? N1B Fe N1C C2C -2.0(3) . . . . ? N2B Fe N2C N3C 104.5(3) . . . . ? N2A Fe N2C N3C 6.7(3) . . . . ? N1C Fe N2C N3C -168.3(3) . . . . ? N1A Fe N2C N3C -71.9(3) . . . . ? N1B Fe N2C N3C 144.9(13) . . . . ? N2B Fe N2C C4C -91.9(3) . . . . ? N2A Fe N2C C4C 170.4(2) . . . . ? N1C Fe N2C C4C -4.7(2) . . . . ? N1A Fe N2C C4C 91.7(2) . . . . ? N1B Fe N2C C4C -51.4(14) . . . . ? C4C N2C N3C C6C 0.2(4) . . . . ? Fe N2C N3C C6C 164.7(3) . . . . ? C1B N C1A C2A -119.7(4) . . . . ? C1C N C1A C2A 79.5(4) . . . . ? C3A N1A C2A C1A 102.7(4) . . . . ? Fe N1A C2A C1A -77.3(4) . . . . ? N C1A C2A N1A 53.2(5) . . . . ? C2A N1A C3A C4A -177.6(3) . . . . ? Fe N1A C3A C4A 2.5(4) . . . . ? N3A N2A C4A C5A -0.5(3) . . . . ? Fe N2A C4A C5A -171.3(2) . . . . ? N3A N2A C4A C3A 175.8(3) . . . . ? Fe N2A C4A C3A 5.1(3) . . . . ? N1A C3A C4A N2A -5.0(4) . . . . ? N1A C3A C4A C5A 170.1(3) . . . . ? N2A C4A C5A C6A 0.4(4) . . . . ? C3A C4A C5A C6A -174.9(4) . . . . ? N2A N3A C6A C5A -0.3(4) . . . . ? N2A N3A C6A C7A -177.5(3) . . . . ? C4A C5A C6A N3A -0.1(4) . . . . ? C4A C5A C6A C7A 176.8(4) . . . . ? C1C N C1B C2B -120.8(4) . . . . ? C1A N C1B C2B 78.4(4) . . . . ? C3B N1B C2B C1B 100.7(4) . . . . ? Fe N1B C2B C1B -78.2(4) . . . . ? N C1B C2B N1B 54.1(5) . . . . ? C2B N1B C3B C4B -175.1(3) . . . . ? Fe N1B C3B C4B 3.9(4) . . . . ? N3B N2B C4B C5B -0.3(4) . . . . ? Fe N2B C4B C5B -169.0(3) . . . . ? N3B N2B C4B C3B 173.8(3) . . . . ? Fe N2B C4B C3B 5.1(4) . . . . ? N1B C3B C4B N2B -6.0(5) . . . . ? N1B C3B C4B C5B 165.9(5) . . . . ? N2B C4B C5B C6B 0.5(5) . . . . ? C3B C4B C5B C6B -171.7(5) . . . . ? N2B N3B C6B C5B 0.4(5) . . . . ? N2B N3B C6B C7B -179.2(4) . . . . ? C4B C5B C6B N3B -0.6(5) . . . . ? C4B C5B C6B C7B 178.9(5) . . . . ? C1B N C1C C2C 81.2(5) . . . . ? C1A N C1C C2C -118.2(4) . . . . ? C3C N1C C2C C1C 101.2(4) . . . . ? Fe N1C C2C C1C -79.6(4) . . . . ? N C1C C2C N1C 52.5(5) . . . . ? C2C N1C C3C C4C -177.4(3) . . . . ? Fe N1C C3C C4C 3.3(4) . . . . ? N3C N2C C4C C5C 0.0(4) . . . . ? Fe N2C C4C C5C -168.2(2) . . . . ? N3C N2C C4C C3C 175.9(3) . . . . ? Fe N2C C4C C3C 7.7(4) . . . . ? N1C C3C C4C N2C -7.3(4) . . . . ? N1C C3C C4C C5C 167.1(4) . . . . ? N2C C4C C5C C6C -0.2(4) . . . . ? C3C C4C C5C C6C -174.8(4) . . . . ? N2C N3C C6C C5C -0.3(5) . . . . ? N2C N3C C6C C7C -179.3(4) . . . . ? C4C C5C C6C N3C 0.3(4) . . . . ? C4C C5C C6C C7C 179.2(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3AB N3C 0.86 1.96 2.788(4) 162.2 2_656 N3B H3BB N3B 0.86 1.91 2.744(9) 163.4 2_656 N3C H3CB N3A 0.86 1.97 2.788(4) 157.4 2_656 C3A H3AA F4 0.93 2.22 3.097(9) 157.0 . C5A H5AA F2 0.93 2.46 3.304(11) 150.7 . C2B H2BA F2A 0.97 2.43 3.345(9) 156.7 4_556 C2C H2CA F3 0.97 2.38 3.336(9) 169.8 1_565 C3C H3CA F3A 0.93 2.36 3.264(9) 162.6 1_565 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.821 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.064 # Attachment 'CTBH12RT.CIF' data_ctbh12 _database_code_depnum_ccdc_archive 'CCDC 766395' #TrackingRef 'CTBH12RT.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C42 H59 Co Fe N20, 2(BF4) ; _chemical_formula_sum 'C42 H59 B2 Co F8 Fe N20' _chemical_formula_weight 1132.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.4341(14) _cell_length_b 12.4832(6) _cell_length_c 19.5995(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.713(5) _cell_angle_gamma 90.00 _cell_volume 5238.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4492 _cell_measurement_theta_min 4.5138 _cell_measurement_theta_max 77.3609 _exptl_crystal_description needle _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 5.402 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.71804 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13247 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.52 _diffrn_reflns_theta_max 77.64 _reflns_number_total 5517 _reflns_number_gt 3735 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Shelxtl (Bruker, 1998)' _computing_publication_material Shelxtl _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^] 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 5517 _refine_ls_number_parameters 381 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1508 _refine_ls_wR_factor_gt 0.1405 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.009 _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 Co Co 0.37071(2) 0.63326(4) 0.69276(2) 0.04343(14) Uani 0.50 1 d P A 1 Fe Fe 0.37071(2) 0.63326(4) 0.69276(2) 0.04343(14) Uani 0.50 1 d P A 2 N N 0.22294(16) 0.6479(3) 0.62680(19) 0.0726(9) Uani 1 1 d . A . N1A N 0.33850(12) 0.5245(2) 0.62326(13) 0.0517(6) Uani 1 1 d . . . N2A N 0.40535(13) 0.4996(2) 0.73408(13) 0.0502(6) Uani 1 1 d . . . N3A N 0.43345(14) 0.4700(3) 0.79308(14) 0.0655(8) Uani 1 1 d . A . H3AB H 0.4484 0.5129 0.8240 0.079 Uiso 0.687(5) 1 calc PR . . N1B N 0.34042(13) 0.7618(2) 0.63886(15) 0.0560(7) Uani 1 1 d . . . N2B N 0.44301(13) 0.6578(2) 0.63528(13) 0.0543(7) Uani 1 1 d . . . N3B N 0.49434(15) 0.6028(3) 0.62017(15) 0.0681(9) Uani 1 1 d . A . H3BB H 0.5093 0.5484 0.6424 0.082 Uiso 0.41(2) 1 calc PR . . N1C N 0.29681(14) 0.6216(2) 0.75268(15) 0.0591(7) Uani 1 1 d . . . N2C N 0.39823(14) 0.7297(2) 0.76853(18) 0.0652(8) Uani 1 1 d . . . N3C N 0.44315(17) 0.8029(3) 0.7795(3) 0.0998(15) Uani 1 1 d . A . H3CB H 0.4753 0.8107 0.7554 0.120 Uiso 0.41(2) 1 calc PR . . C1A C 0.23237(18) 0.5678(4) 0.5758(2) 0.0742(11) Uani 1 1 d . . . H1AA H 0.2099 0.5890 0.5339 0.089 Uiso 1 1 calc R A . H1AB H 0.2143 0.5010 0.5907 0.089 Uiso 1 1 calc R . . C2A C 0.30094(17) 0.5479(4) 0.56053(19) 0.0669(10) Uani 1 1 d . A . H2AA H 0.3035 0.4881 0.5292 0.080 Uiso 1 1 calc R . . H2AB H 0.3176 0.6107 0.5387 0.080 Uiso 1 1 calc R . . C3A C 0.35345(16) 0.4274(3) 0.63707(17) 0.0557(8) Uani 1 1 d . A . H3AA H 0.3423 0.3715 0.6076 0.067 Uiso 1 1 calc R . . C4A C 0.38832(15) 0.4091(3) 0.70051(17) 0.0522(7) Uani 1 1 d . A . C5A C 0.40675(17) 0.3206(3) 0.7386(2) 0.0635(9) Uani 1 1 d . . . H5AA H 0.4013 0.2487 0.7272 0.076 Uiso 1 1 calc R A . C6A C 0.43469(18) 0.3623(4) 0.7966(2) 0.0712(11) Uani 1 1 d . A . C7A C 0.4624(2) 0.3078(5) 0.8594(3) 0.1009(17) Uani 1 1 d . . . H7AA H 0.4819 0.2420 0.8466 0.151 Uiso 1 1 calc R A . H7AB H 0.4301 0.2928 0.8902 0.151 Uiso 1 1 calc R . . H7AC H 0.4931 0.3539 0.8815 0.151 Uiso 1 1 calc R . . C1B C 0.22777(18) 0.7591(4) 0.6089(2) 0.0769(11) Uani 1 1 d . . . H1BA H 0.1888 0.7946 0.6182 0.092 Uiso 1 1 calc R A . H1BB H 0.2335 0.7646 0.5602 0.092 Uiso 1 1 calc R . . C2B C 0.28138(18) 0.8173(3) 0.6472(2) 0.0701(10) Uani 1 1 d . A . H2BA H 0.2843 0.8899 0.6301 0.084 Uiso 1 1 calc R . . H2BB H 0.2730 0.8211 0.6954 0.084 Uiso 1 1 calc R . . C3B C 0.37817(17) 0.7964(3) 0.59505(18) 0.0600(8) Uani 1 1 d . A . H3BA H 0.3697 0.8577 0.5693 0.072 Uiso 1 1 calc R . . C4B C 0.43425(16) 0.7355(3) 0.58777(16) 0.0554(8) Uani 1 1 d . A . C5B C 0.48247(18) 0.7308(4) 0.54237(18) 0.0689(10) Uani 1 1 d . . . H5BA H 0.4885 0.7755 0.5053 0.083 Uiso 1 1 calc R A . C6B C 0.51868(19) 0.6471(4) 0.56404(18) 0.0716(11) Uani 1 1 d . A . C7B C 0.5769(2) 0.6006(5) 0.5354(2) 0.0998(17) Uani 1 1 d . . . H7BA H 0.5985 0.5581 0.5698 0.150 Uiso 1 1 calc R A . H7BB H 0.6035 0.6576 0.5216 0.150 Uiso 1 1 calc R . . H7BC H 0.5656 0.5565 0.4967 0.150 Uiso 1 1 calc R . . C1C C 0.19606(17) 0.6178(4) 0.6892(2) 0.0772(12) Uani 1 1 d . . . H1CA H 0.1599 0.5729 0.6787 0.093 Uiso 1 1 calc R A . H1CB H 0.1815 0.6819 0.7116 0.093 Uiso 1 1 calc R . . C2C C 0.24066(18) 0.5578(3) 0.7390(2) 0.0718(10) Uani 1 1 d . A . H2CA H 0.2203 0.5442 0.7813 0.086 Uiso 1 1 calc R . . H2CB H 0.2518 0.4894 0.7195 0.086 Uiso 1 1 calc R . . C3C C 0.30184(19) 0.6766(3) 0.8080(2) 0.0676(9) Uani 1 1 d . A . H3CA H 0.2718 0.6732 0.8406 0.081 Uiso 1 1 calc R . . C4C C 0.3555(2) 0.7428(3) 0.8171(2) 0.0695(10) Uani 1 1 d . A . C5C C 0.3749(3) 0.8261(4) 0.8606(3) 0.1005(18) Uani 1 1 d . . . H5CA H 0.3439 0.8827 0.8604 0.121 Uiso 1 1 calc R A . H5CB H 0.3822 0.8004 0.9070 0.121 Uiso 1 1 calc R . . C6C C 0.4302(3) 0.8624(4) 0.8340(4) 0.115(2) Uani 1 1 d . A . C7C C 0.4718(3) 0.9531(4) 0.8572(5) 0.177(4) Uani 1 1 d . . . H7CA H 0.5147 0.9328 0.8531 0.265 Uiso 1 1 calc R A . H7CB H 0.4647 0.9697 0.9040 0.265 Uiso 1 1 calc R . . H7CC H 0.4628 1.0149 0.8294 0.265 Uiso 1 1 calc R . . B1A B 0.35533(12) 0.0977(2) 0.58245(14) 0.111(3) Uani 0.547(5) 1 d PD B 1 F1 F 0.38954(18) 0.0665(4) 0.53214(17) 0.201(4) Uani 0.547(5) 1 d PDU B 1 F2 F 0.38077(19) 0.0635(4) 0.64087(16) 0.163(3) Uani 0.547(5) 1 d PDU B 1 F3 F 0.3522(3) 0.2029(2) 0.5832(3) 0.236(5) Uani 0.547(5) 1 d PDU B 1 F4 F 0.29871(14) 0.0577(4) 0.5736(2) 0.166(3) Uani 0.547(5) 1 d PDU B 1 B1B B 0.36146(13) 0.1250(2) 0.57237(16) 0.111(3) Uani 0.453(5) 1 d PD B 2 F1A F 0.41434(16) 0.1787(3) 0.5744(3) 0.169(4) Uani 0.453(5) 1 d PDU B 2 F2A F 0.3683(3) 0.0351(3) 0.5386(3) 0.160(4) Uani 0.453(5) 1 d PDU B 2 F3A F 0.3174(2) 0.1830(4) 0.5415(4) 0.247(6) Uani 0.453(5) 1 d PDU B 2 F4A F 0.3458(3) 0.1034(5) 0.6350(2) 0.217(5) Uani 0.453(5) 1 d PDU 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 Co 0.0446(2) 0.0415(2) 0.0445(2) 0.0009(2) 0.00579(17) 0.0001(2) Fe 0.0446(2) 0.0415(2) 0.0445(2) 0.0009(2) 0.00579(17) 0.0001(2) N 0.0654(19) 0.069(2) 0.083(2) -0.0030(17) 0.0042(16) -0.0010(16) N1A 0.0472(14) 0.0589(16) 0.0491(13) -0.0049(12) 0.0044(11) 0.0003(12) N2A 0.0542(14) 0.0539(15) 0.0425(12) 0.0003(11) 0.0017(11) -0.0077(12) N3A 0.0616(17) 0.085(2) 0.0502(15) 0.0113(15) 0.0028(13) -0.0199(16) N1B 0.0533(15) 0.0507(15) 0.0634(16) 0.0003(13) -0.0030(13) 0.0032(12) N2B 0.0519(14) 0.0668(18) 0.0441(13) 0.0053(12) 0.0019(11) 0.0074(12) N3B 0.0605(17) 0.097(2) 0.0470(14) -0.0045(15) 0.0045(13) 0.0233(16) N1C 0.0585(16) 0.0576(17) 0.0617(16) 0.0028(13) 0.0072(13) 0.0025(13) N2C 0.0548(16) 0.0476(15) 0.092(2) -0.0016(15) -0.0054(15) 0.0044(13) N3C 0.061(2) 0.0445(18) 0.191(5) -0.001(2) -0.029(2) 0.0035(15) C1A 0.057(2) 0.085(3) 0.079(2) -0.015(2) -0.0114(18) -0.001(2) C2A 0.063(2) 0.083(3) 0.0537(18) -0.0043(18) -0.0086(16) 0.0030(19) C3A 0.0545(17) 0.058(2) 0.0554(17) -0.0108(15) 0.0101(14) -0.0060(15) C4A 0.0503(16) 0.0499(16) 0.0573(17) -0.0006(14) 0.0102(14) -0.0046(14) C5A 0.059(2) 0.0567(19) 0.076(2) 0.0106(18) 0.0099(17) -0.0061(16) C6A 0.061(2) 0.088(3) 0.065(2) 0.026(2) 0.0021(17) -0.019(2) C7A 0.087(3) 0.122(4) 0.093(3) 0.050(3) -0.007(3) -0.019(3) C1B 0.054(2) 0.077(3) 0.099(3) 0.010(2) -0.007(2) 0.0126(19) C2B 0.066(2) 0.0509(19) 0.094(3) -0.0004(19) 0.007(2) 0.0114(17) C3B 0.065(2) 0.0538(19) 0.0601(19) 0.0092(15) -0.0085(16) -0.0064(16) C4B 0.0553(18) 0.063(2) 0.0468(16) 0.0084(14) -0.0026(14) -0.0067(15) C5B 0.067(2) 0.091(3) 0.0492(17) 0.0036(18) 0.0073(16) -0.016(2) C6B 0.061(2) 0.106(3) 0.0483(17) -0.008(2) 0.0063(16) 0.007(2) C7B 0.080(3) 0.154(5) 0.067(2) -0.011(3) 0.024(2) 0.020(3) C1C 0.0449(18) 0.088(3) 0.099(3) -0.009(2) 0.0132(19) -0.0034(19) C2C 0.065(2) 0.069(2) 0.083(2) 0.006(2) 0.0156(19) -0.0101(19) C3C 0.068(2) 0.069(2) 0.067(2) -0.0006(19) 0.0099(18) 0.0128(19) C4C 0.075(2) 0.063(2) 0.069(2) -0.0083(18) -0.0125(19) 0.0179(19) C5C 0.115(4) 0.070(3) 0.111(4) -0.024(3) -0.051(3) 0.039(3) C6C 0.081(3) 0.054(2) 0.205(7) -0.023(4) -0.060(4) 0.017(2) C7C 0.125(5) 0.063(3) 0.332(12) -0.053(5) -0.101(7) 0.017(3) B1A 0.208(10) 0.027(4) 0.105(5) 0.018(4) 0.073(6) -0.030(5) F1 0.251(10) 0.200(10) 0.162(7) -0.011(7) 0.106(7) -0.021(8) F2 0.156(7) 0.218(9) 0.118(5) 0.032(6) 0.018(5) 0.047(6) F3 0.313(11) 0.074(4) 0.315(10) -0.056(6) -0.049(10) -0.007(6) F4 0.211(8) 0.140(6) 0.147(6) -0.022(5) 0.016(5) -0.058(6) B1B 0.208(10) 0.027(4) 0.105(5) 0.018(4) 0.073(6) -0.030(5) F1A 0.177(9) 0.140(7) 0.194(9) -0.024(7) 0.055(7) -0.094(7) F2A 0.270(10) 0.062(4) 0.145(7) -0.035(4) -0.016(7) -0.036(6) F3A 0.254(12) 0.159(9) 0.319(13) 0.003(10) -0.076(11) 0.026(9) F4A 0.233(10) 0.259(10) 0.168(8) -0.007(8) 0.099(7) -0.061(9) _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 Co N2C 1.980(3) . ? Co N2B 1.982(3) . ? Co N2A 1.984(3) . ? Co N1B 2.012(3) . ? Co N1C 2.021(3) . ? Co N1A 2.022(3) . ? N C1C 1.427(6) . ? N C1B 1.436(5) . ? N C1A 1.435(5) . ? N1A C3A 1.279(4) . ? N1A C2A 1.467(4) . ? N2A N3A 1.330(4) . ? N2A C4A 1.348(4) . ? N3A C6A 1.347(5) . ? N3A H3AB 0.8600 . ? N1B C3B 1.282(5) . ? N1B C2B 1.459(4) . ? N2B N3B 1.342(4) . ? N2B C4B 1.351(4) . ? N3B C6B 1.358(5) . ? N3B H3BB 0.8600 . ? N1C C3C 1.283(5) . ? N1C C2C 1.458(5) . ? N2C N3C 1.338(5) . ? N2C C4C 1.362(5) . ? N3C C6C 1.340(8) . ? N3C H3CB 0.8600 . ? C1A C2A 1.534(5) . ? C1A H1AA 0.9700 . ? C1A H1AB 0.9700 . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A C4A 1.438(5) . ? C3A H3AA 0.9300 . ? C4A C5A 1.381(5) . ? C5A C6A 1.363(6) . ? C5A H5AA 0.9300 . ? C6A C7A 1.504(6) . ? C7A H7AA 0.9600 . ? C7A H7AB 0.9600 . ? C7A H7AC 0.9600 . ? C1B C2B 1.528(6) . ? C1B H1BA 0.9700 . ? C1B H1BB 0.9700 . ? C2B H2BA 0.9700 . ? C2B H2BB 0.9700 . ? C3B C4B 1.435(5) . ? C3B H3BA 0.9300 . ? C4B C5B 1.397(5) . ? C5B C6B 1.357(6) . ? C5B H5BA 0.9300 . ? C6B C7B 1.508(5) . ? C7B H7BA 0.9600 . ? C7B H7BB 0.9600 . ? C7B H7BC 0.9600 . ? C1C C2C 1.529(6) . ? C1C H1CA 0.9700 . ? C1C H1CB 0.9700 . ? C2C H2CA 0.9700 . ? C2C H2CB 0.9700 . ? C3C C4C 1.420(6) . ? C3C H3CA 0.9300 . ? C4C C5C 1.396(6) . ? C5C C6C 1.392(9) . ? C5C H5CA 0.9700 . ? C5C H5CB 0.9700 . ? C6C C7C 1.500(7) . ? C7C H7CA 0.9600 . ? C7C H7CB 0.9600 . ? C7C H7CC 0.9600 . ? B1A F3 1.3150(12) . ? B1A F1 1.3155(12) . ? B1A F2 1.3157(12) . ? B1A F4 1.3159(12) . ? B1B F1A 1.3154(12) . ? B1B F3A 1.3154(12) . ? B1B F4A 1.3154(12) . ? B1B F2A 1.3155(12) . ? 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 N2C Co N2B 96.84(13) . . ? N2C Co N2A 96.49(12) . . ? N2B Co N2A 94.27(11) . . ? N2C Co N1B 89.19(13) . . ? N2B Co N1B 79.62(12) . . ? N2A Co N1B 172.14(11) . . ? N2C Co N1C 79.73(13) . . ? N2B Co N1C 175.20(13) . . ? N2A Co N1C 89.48(11) . . ? N1B Co N1C 96.90(12) . . ? N2C Co N1A 173.71(13) . . ? N2B Co N1A 88.39(11) . . ? N2A Co N1A 79.59(11) . . ? N1B Co N1A 95.20(12) . . ? N1C Co N1A 95.24(12) . . ? C1C N C1B 120.1(4) . . ? C1C N C1A 119.3(4) . . ? C1B N C1A 119.3(4) . . ? C3A N1A C2A 119.2(3) . . ? C3A N1A Co 114.8(2) . . ? C2A N1A Co 126.0(3) . . ? N3A N2A C4A 107.1(3) . . ? N3A N2A Co 137.2(2) . . ? C4A N2A Co 114.7(2) . . ? N2A N3A C6A 109.2(3) . . ? N2A N3A H3AB 125.4 . . ? C6A N3A H3AB 125.4 . . ? C3B N1B C2B 119.6(3) . . ? C3B N1B Co 114.9(2) . . ? C2B N1B Co 125.4(2) . . ? N3B N2B C4B 107.7(3) . . ? N3B N2B Co 135.9(2) . . ? C4B N2B Co 114.6(2) . . ? N2B N3B C6B 108.7(3) . . ? N2B N3B H3BB 125.6 . . ? C6B N3B H3BB 125.6 . . ? C3C N1C C2C 118.9(3) . . ? C3C N1C Co 114.6(3) . . ? C2C N1C Co 126.5(2) . . ? N3C N2C C4C 108.0(4) . . ? N3C N2C Co 136.3(3) . . ? C4C N2C Co 114.2(3) . . ? N2C N3C C6C 109.4(5) . . ? N2C N3C H3CB 125.3 . . ? C6C N3C H3CB 125.3 . . ? N C1A C2A 114.6(3) . . ? N C1A H1AA 108.6 . . ? C2A C1A H1AA 108.6 . . ? N C1A H1AB 108.6 . . ? C2A C1A H1AB 108.6 . . ? H1AA C1A H1AB 107.6 . . ? N1A C2A C1A 111.2(3) . . ? N1A C2A H2AA 109.4 . . ? C1A C2A H2AA 109.4 . . ? N1A C2A H2AB 109.4 . . ? C1A C2A H2AB 109.4 . . ? H2AA C2A H2AB 108.0 . . ? N1A C3A C4A 116.6(3) . . ? N1A C3A H3AA 121.7 . . ? C4A C3A H3AA 121.7 . . ? N2A C4A C5A 110.0(3) . . ? N2A C4A C3A 114.0(3) . . ? C5A C4A C3A 135.9(3) . . ? C6A C5A C4A 104.4(4) . . ? C6A C5A H5AA 127.8 . . ? C4A C5A H5AA 127.8 . . ? N3A C6A C5A 109.4(3) . . ? N3A C6A C7A 120.0(4) . . ? C5A C6A C7A 130.6(4) . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? N C1B C2B 113.6(3) . . ? N C1B H1BA 108.8 . . ? C2B C1B H1BA 108.8 . . ? N C1B H1BB 108.8 . . ? C2B C1B H1BB 108.8 . . ? H1BA C1B H1BB 107.7 . . ? N1B C2B C1B 110.8(3) . . ? N1B C2B H2BA 109.5 . . ? C1B C2B H2BA 109.5 . . ? N1B C2B H2BB 109.5 . . ? C1B C2B H2BB 109.5 . . ? H2BA C2B H2BB 108.1 . . ? N1B C3B C4B 116.5(3) . . ? N1B C3B H3BA 121.7 . . ? C4B C3B H3BA 121.7 . . ? N2B C4B C5B 109.0(3) . . ? N2B C4B C3B 113.7(3) . . ? C5B C4B C3B 137.2(3) . . ? C6B C5B C4B 105.2(3) . . ? C6B C5B H5BA 127.4 . . ? C4B C5B H5BA 127.4 . . ? C5B C6B N3B 109.4(3) . . ? C5B C6B C7B 130.6(4) . . ? N3B C6B C7B 120.0(4) . . ? C6B C7B H7BA 109.5 . . ? C6B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C6B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N C1C C2C 114.2(3) . . ? N C1C H1CA 108.7 . . ? C2C C1C H1CA 108.7 . . ? N C1C H1CB 108.7 . . ? C2C C1C H1CB 108.7 . . ? H1CA C1C H1CB 107.6 . . ? N1C C2C C1C 109.6(3) . . ? N1C C2C H2CA 109.8 . . ? C1C C2C H2CA 109.8 . . ? N1C C2C H2CB 109.8 . . ? C1C C2C H2CB 109.8 . . ? H2CA C2C H2CB 108.2 . . ? N1C C3C C4C 116.9(4) . . ? N1C C3C H3CA 121.6 . . ? C4C C3C H3CA 121.6 . . ? N2C C4C C5C 108.9(5) . . ? N2C C4C C3C 114.2(3) . . ? C5C C4C C3C 136.6(5) . . ? C6C C5C C4C 104.4(5) . . ? C6C C5C H5CA 110.9 . . ? C4C C5C H5CA 110.9 . . ? C6C C5C H5CB 110.9 . . ? C4C C5C H5CB 110.9 . . ? H5CA C5C H5CB 108.9 . . ? N3C C6C C5C 109.3(4) . . ? N3C C6C C7C 121.1(7) . . ? C5C C6C C7C 129.6(7) . . ? C6C C7C H7CA 109.5 . . ? C6C C7C H7CB 109.5 . . ? H7CA C7C H7CB 109.5 . . ? C6C C7C H7CC 109.5 . . ? H7CA C7C H7CC 109.5 . . ? H7CB C7C H7CC 109.5 . . ? F3 B1A F1 109.53(10) . . ? F3 B1A F2 109.48(10) . . ? F1 B1A F2 109.49(10) . . ? F3 B1A F4 109.45(10) . . ? F1 B1A F4 109.44(10) . . ? F2 B1A F4 109.44(10) . . ? F1A B1B F3A 109.47(10) . . ? F1A B1B F4A 109.43(10) . . ? F3A B1B F4A 109.48(10) . . ? F1A B1B F2A 109.47(10) . . ? F3A B1B F2A 109.45(10) . . ? F4A B1B F2A 109.53(10) . . ? 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 N2C Co N1A C3A -51.1(12) . . . . ? N2B Co N1A C3A 95.3(2) . . . . ? N2A Co N1A C3A 0.7(2) . . . . ? N1B Co N1A C3A 174.7(2) . . . . ? N1C Co N1A C3A -87.8(2) . . . . ? N2C Co N1A C2A 129.1(10) . . . . ? N2B Co N1A C2A -84.5(3) . . . . ? N2A Co N1A C2A -179.1(3) . . . . ? N1B Co N1A C2A -5.1(3) . . . . ? N1C Co N1A C2A 92.4(3) . . . . ? N2C Co N2A N3A 5.2(3) . . . . ? N2B Co N2A N3A 102.6(3) . . . . ? N1B Co N2A N3A 141.3(8) . . . . ? N1C Co N2A N3A -74.4(3) . . . . ? N1A Co N2A N3A -169.8(3) . . . . ? N2C Co N2A C4A 171.2(2) . . . . ? N2B Co N2A C4A -91.4(2) . . . . ? N1B Co N2A C4A -52.7(9) . . . . ? N1C Co N2A C4A 91.6(2) . . . . ? N1A Co N2A C4A -3.8(2) . . . . ? C4A N2A N3A C6A 0.5(4) . . . . ? Co N2A N3A C6A 167.2(3) . . . . ? N2C Co N1B C3B 98.2(3) . . . . ? N2B Co N1B C3B 1.0(3) . . . . ? N2A Co N1B C3B -38.3(10) . . . . ? N1C Co N1B C3B 177.7(3) . . . . ? N1A Co N1B C3B -86.4(3) . . . . ? N2C Co N1B C2B -80.4(3) . . . . ? N2B Co N1B C2B -177.5(3) . . . . ? N2A Co N1B C2B 143.2(8) . . . . ? N1C Co N1B C2B -0.9(3) . . . . ? N1A Co N1B C2B 95.1(3) . . . . ? N2C Co N2B N3B 104.5(3) . . . . ? N2A Co N2B N3B 7.4(3) . . . . ? N1B Co N2B N3B -167.6(3) . . . . ? N1C Co N2B N3B 148.7(13) . . . . ? N1A Co N2B N3B -72.0(3) . . . . ? N2C Co N2B C4B -93.7(3) . . . . ? N2A Co N2B C4B 169.3(2) . . . . ? N1B Co N2B C4B -5.7(2) . . . . ? N1C Co N2B C4B -49.5(15) . . . . ? N1A Co N2B C4B 89.9(3) . . . . ? C4B N2B N3B C6B 1.3(4) . . . . ? Co N2B N3B C6B 164.0(3) . . . . ? N2C Co N1C C3C -0.8(3) . . . . ? N2B Co N1C C3C -45.5(15) . . . . ? N2A Co N1C C3C 95.9(3) . . . . ? N1B Co N1C C3C -88.7(3) . . . . ? N1A Co N1C C3C 175.4(3) . . . . ? N2C Co N1C C2C 179.7(3) . . . . ? N2B Co N1C C2C 135.1(13) . . . . ? N2A Co N1C C2C -83.6(3) . . . . ? N1B Co N1C C2C 91.8(3) . . . . ? N1A Co N1C C2C -4.1(3) . . . . ? N2B Co N2C N3C 9.6(4) . . . . ? N2A Co N2C N3C 104.7(4) . . . . ? N1B Co N2C N3C -69.8(4) . . . . ? N1C Co N2C N3C -167.0(4) . . . . ? N1A Co N2C N3C 155.8(9) . . . . ? N2B Co N2C C4C 173.6(3) . . . . ? N2A Co N2C C4C -91.3(3) . . . . ? N1B Co N2C C4C 94.2(3) . . . . ? N1C Co N2C C4C -3.0(3) . . . . ? N1A Co N2C C4C -40.2(12) . . . . ? C4C N2C N3C C6C 0.1(5) . . . . ? Co N2C N3C C6C 164.7(4) . . . . ? C1C N C1A C2A -116.2(4) . . . . ? C1B N C1A C2A 77.2(5) . . . . ? C3A N1A C2A C1A 101.9(4) . . . . ? Co N1A C2A C1A -78.3(4) . . . . ? N C1A C2A N1A 53.4(5) . . . . ? C2A N1A C3A C4A -177.8(3) . . . . ? Co N1A C3A C4A 2.4(4) . . . . ? N3A N2A C4A C5A -0.8(4) . . . . ? Co N2A C4A C5A -170.9(2) . . . . ? N3A N2A C4A C3A 176.2(3) . . . . ? Co N2A C4A C3A 6.1(3) . . . . ? N1A C3A C4A N2A -5.7(4) . . . . ? N1A C3A C4A C5A 170.3(4) . . . . ? N2A C4A C5A C6A 0.8(4) . . . . ? C3A C4A C5A C6A -175.3(4) . . . . ? N2A N3A C6A C5A 0.0(4) . . . . ? N2A N3A C6A C7A -178.3(3) . . . . ? C4A C5A C6A N3A -0.5(4) . . . . ? C4A C5A C6A C7A 177.5(4) . . . . ? C1C N C1B C2B 77.4(5) . . . . ? C1A N C1B C2B -116.1(4) . . . . ? C3B N1B C2B C1B 99.8(4) . . . . ? Co N1B C2B C1B -81.7(4) . . . . ? N C1B C2B N1B 54.3(5) . . . . ? C2B N1B C3B C4B -177.7(3) . . . . ? Co N1B C3B C4B 3.6(4) . . . . ? N3B N2B C4B C5B -1.5(4) . . . . ? Co N2B C4B C5B -168.4(2) . . . . ? N3B N2B C4B C3B 176.0(3) . . . . ? Co N2B C4B C3B 9.1(4) . . . . ? N1B C3B C4B N2B -8.5(5) . . . . ? N1B C3B C4B C5B 168.0(4) . . . . ? N2B C4B C5B C6B 1.2(4) . . . . ? C3B C4B C5B C6B -175.5(4) . . . . ? C4B C5B C6B N3B -0.4(5) . . . . ? C4B C5B C6B C7B 178.7(5) . . . . ? N2B N3B C6B C5B -0.6(5) . . . . ? N2B N3B C6B C7B -179.8(4) . . . . ? C1B N C1C C2C -118.3(4) . . . . ? C1A N C1C C2C 75.2(5) . . . . ? C3C N1C C2C C1C 99.8(4) . . . . ? Co N1C C2C C1C -80.8(4) . . . . ? N C1C C2C N1C 55.5(5) . . . . ? C2C N1C C3C C4C -176.1(3) . . . . ? Co N1C C3C C4C 4.4(5) . . . . ? N3C N2C C4C C5C -0.9(5) . . . . ? Co N2C C4C C5C -169.3(3) . . . . ? N3C N2C C4C C3C 174.5(3) . . . . ? Co N2C C4C C3C 6.1(4) . . . . ? N1C C3C C4C N2C -6.9(5) . . . . ? N1C C3C C4C C5C 166.7(5) . . . . ? N2C C4C C5C C6C 1.4(5) . . . . ? C3C C4C C5C C6C -172.5(5) . . . . ? N2C N3C C6C C5C 0.8(6) . . . . ? N2C N3C C6C C7C -178.4(5) . . . . ? C4C C5C C6C N3C -1.3(6) . . . . ? C4C C5C C6C C7C 177.8(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3AB N3B 0.86 1.96 2.790(5) 162.6 2_656 N3B H3BB N3A 0.86 1.98 2.790(5) 156.8 2_656 N3C H3CB N3C 0.86 1.91 2.747(9) 164.4 2_656 C3A H3AA F3 0.93 2.17 2.995(5) 147.1 . C2B H2BA F4 0.97 2.40 3.358(7) 171.6 1_565 C3B H3BA F2A 0.93 2.29 3.182(6) 159.5 1_565 C2C H2CA F4A 0.97 2.34 3.209(5) 149.0 4_556 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.535 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.058 # Attachment 'CTBH12ALN.CIF' data_ctbh12a _database_code_depnum_ccdc_archive 'CCDC 766396' #TrackingRef 'CTBH12ALN.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H28.50 B Co0.50 F4 Fe0.50 N10' _chemical_formula_weight 565.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.2022(4) _cell_length_b 12.3477(2) _cell_length_c 19.3014(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.5681(19) _cell_angle_gamma 90.00 _cell_volume 5047.98(18) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5580 _cell_measurement_theta_min 4.5743 _cell_measurement_theta_max 74.1024 _exptl_crystal_description prism _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 5.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.54076 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 9678 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.59 _diffrn_reflns_theta_max 74.11 _reflns_number_total 4958 _reflns_number_gt 4122 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^2^] 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 4958 _refine_ls_number_parameters 375 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1431 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.370184(3) 0.630703(5) 0.692132(3) 0.01814(2) Uani 0.50 1 d P . . Fe Fe 0.370184(3) 0.630703(5) 0.692132(3) 0.01814(2) Uani 0.50 1 d P . . F1A F 0.37420(3) 0.03519(2) 0.525739(12) 0.0610(3) Uani 0.3803(5) 1 d PDU A 1 F2A F 0.37095(4) 0.05785(3) 0.643238(10) 0.0564(3) Uani 0.3803(5) 1 d PDU A 1 F3A F 0.409812(11) 0.18065(2) 0.57905(5) 0.0935(4) Uani 0.3803(5) 1 d PDU A 1 F4A F 0.313510(11) 0.17789(2) 0.57547(11) 0.1365(7) Uani 0.3803(5) 1 d PDU A 1 F1B F 0.393240(14) 0.04087(2) 0.53323(1) 0.05504(2) Uani 0.6197(5) 1 d PDU A 2 F2B F 0.37733(3) 0.07316(4) 0.645954(10) 0.1099(4) Uani 0.6197(5) 1 d PDU A 2 F3B F 0.299103(8) 0.08347(5) 0.56788(4) 0.0975(3) Uani 0.6197(5) 1 d PDU A 2 F4B F 0.38278(2) 0.208901(15) 0.56929(4) 0.1403(4) Uani 0.6197(5) 1 d PDU A 2 N N 0.21895(2) 0.64961(3) 0.62223(2) 0.03072(12) Uani 1 1 d . . . N1A N 0.338121(17) 0.52668(3) 0.620825(19) 0.02229(10) Uani 1 1 d . . . N2A N 0.403035(18) 0.49678(3) 0.732854(19) 0.02193(10) Uani 1 1 d . . . N3A N 0.431905(19) 0.46576(3) 0.79272(2) 0.02769(11) Uani 1 1 d . . . H3AB H 0.4472 0.5097 0.8252 0.033 Uiso 1 1 calc R . . N1B N 0.340480(18) 0.76054(3) 0.640501(19) 0.02275(10) Uani 1 1 d . . . N2B N 0.442388(18) 0.65475(3) 0.635626(19) 0.02352(10) Uani 1 1 d . . . N3B N 0.494410(19) 0.59829(4) 0.62103(2) 0.02809(11) Uani 1 1 d . . . N1C N 0.295933(19) 0.61724(3) 0.75033(2) 0.02459(10) Uani 1 1 d . . . N2C N 0.396945(19) 0.72614(3) 0.76849(2) 0.02683(11) Uani 1 1 d . . . N3C N 0.44242(2) 0.79975(3) 0.77976(3) 0.03552(13) Uani 1 1 d . . . H3CB H 0.4758 0.8079 0.7548 0.043 Uiso 0.50 1 calc PR . . C1A C 0.23223(2) 0.57250(4) 0.56922(3) 0.03000(13) Uani 1 1 d . . . H1AA H 0.2109 0.5967 0.5253 0.036 Uiso 1 1 calc R . . H1AB H 0.2134 0.5022 0.5817 0.036 Uiso 1 1 calc R . . C2A C 0.30202(2) 0.55402(4) 0.55625(2) 0.02612(12) Uani 1 1 d . . . H2AA H 0.3060 0.4944 0.5224 0.031 Uiso 1 1 calc R . . H2AB H 0.3199 0.6203 0.5360 0.031 Uiso 1 1 calc R . . C3A C 0.35195(2) 0.42694(4) 0.63274(2) 0.02330(11) Uani 1 1 d . . . H3AA H 0.3401 0.3707 0.6012 0.028 Uiso 1 1 calc R . . C4A C 0.38662(2) 0.40613(4) 0.69723(2) 0.02332(11) Uani 1 1 d . . . C5A C 0.40580(2) 0.31475(4) 0.73546(3) 0.02634(12) Uani 1 1 d . . . H5AA H 0.4006 0.2408 0.7229 0.032 Uiso 1 1 calc R . . C6A C 0.43381(3) 0.35611(4) 0.79538(3) 0.03066(13) Uani 1 1 d . . . C7A C 0.46125(3) 0.29955(5) 0.85810(3) 0.04187(16) Uani 1 1 d . . . H7AA H 0.4911 0.3479 0.8831 0.063 Uiso 1 1 calc R . . H7AB H 0.4834 0.2341 0.8439 0.063 Uiso 1 1 calc R . . H7AC H 0.4273 0.2796 0.8885 0.063 Uiso 1 1 calc R . . C1B C 0.22613(2) 0.76374(4) 0.60916(3) 0.03042(13) Uani 1 1 d . . . H1BA H 0.1865 0.8009 0.6203 0.037 Uiso 1 1 calc R . . H1BB H 0.2322 0.7741 0.5590 0.037 Uiso 1 1 calc R . . C2B C 0.28105(2) 0.81833(4) 0.65009(3) 0.02755(13) Uani 1 1 d . . . H2BA H 0.2852 0.8942 0.6343 0.033 Uiso 1 1 calc R . . H2BB H 0.2721 0.8195 0.7000 0.033 Uiso 1 1 calc R . . C3B C 0.37861(2) 0.79741(4) 0.59621(2) 0.02591(12) Uani 1 1 d . . . H3BA H 0.3701 0.8617 0.5705 0.031 Uiso 1 1 calc R . . C4B C 0.43495(2) 0.73507(4) 0.58824(2) 0.02322(11) Uani 1 1 d . . . C5B C 0.48425(2) 0.73065(4) 0.54226(2) 0.02962(13) Uani 1 1 d . . . H5BA H 0.4912 0.7772 0.5042 0.036 Uiso 1 1 calc R . . C6B C 0.52034(2) 0.64381(5) 0.56468(3) 0.03082(14) Uani 1 1 d . . . C7B C 0.57885(3) 0.59559(5) 0.53616(3) 0.04033(16) Uani 1 1 d . . . H7BA H 0.6055 0.5653 0.5742 0.060 Uiso 1 1 calc R . . H7BB H 0.6023 0.6520 0.5125 0.060 Uiso 1 1 calc R . . H7BC H 0.5670 0.5380 0.5032 0.060 Uiso 1 1 calc R . . C1C C 0.19306(2) 0.61360(4) 0.68564(3) 0.03161(14) Uani 1 1 d . . . H1CA H 0.1566 0.5659 0.6741 0.038 Uiso 1 1 calc R . . H1CB H 0.1771 0.6775 0.7104 0.038 Uiso 1 1 calc R . . C2C C 0.23941(2) 0.55219(4) 0.73494(3) 0.02974(13) Uani 1 1 d . . . H2CA H 0.2187 0.5353 0.7786 0.036 Uiso 1 1 calc R . . H2CB H 0.2515 0.4830 0.7133 0.036 Uiso 1 1 calc R . . C3C C 0.29980(2) 0.67186(4) 0.80743(3) 0.02874(13) Uani 1 1 d . . . H3CA H 0.2682 0.6675 0.8407 0.034 Uiso 1 1 calc R . . C4C C 0.35407(2) 0.73893(4) 0.81760(3) 0.02822(12) Uani 1 1 d . . . C5C C 0.37321(3) 0.82306(4) 0.86197(3) 0.03722(15) Uani 1 1 d . . . H5CA H 0.3526 0.8492 0.9013 0.045 Uiso 1 1 calc R . . C6C C 0.42884(3) 0.85989(4) 0.83587(4) 0.04265(17) Uani 1 1 d . . . C7C C 0.47059(3) 0.95194(5) 0.85931(4) 0.0601(2) Uani 1 1 d . . . H7CB H 0.5143 0.9357 0.8486 0.090 Uiso 1 1 calc R . . H7CC H 0.4678 0.9620 0.9094 0.090 Uiso 1 1 calc R . . H7CD H 0.4569 1.0183 0.8352 0.090 Uiso 1 1 calc R . . B B 0.362369(5) 0.104819(9) 0.579025(6) 0.0516(2) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.01800(3) 0.01761(3) 0.01912(3) 0.00087(3) 0.00423(2) 0.00016(3) Fe 0.01800(3) 0.01761(3) 0.01912(3) 0.00087(3) 0.00423(2) 0.00016(3) F1A 0.0941(6) 0.0291(4) 0.0562(5) -0.0059(4) -0.0361(4) -0.0236(4) F2A 0.0888(6) 0.0289(4) 0.0560(4) 0.0065(4) 0.0526(4) -0.0066(4) F3A 0.1858(10) 0.0492(5) 0.0478(5) -0.0126(4) 0.0315(6) -0.0705(5) F4A 0.0898(9) 0.0877(9) 0.2341(16) -0.0152(11) 0.0284(10) 0.0442(7) F1B 0.0708(4) 0.0473(3) 0.0477(3) -0.0113(3) 0.0099(3) -0.0141(3) F2B 0.1274(7) 0.1434(8) 0.0580(4) -0.0056(6) -0.0065(5) -0.0268(7) F3B 0.0612(4) 0.1389(6) 0.0915(5) -0.0557(4) -0.0060(4) 0.0287(4) F4B 0.2587(11) 0.0206(3) 0.1478(8) -0.0050(4) 0.0791(7) -0.0049(5) N 0.0302(2) 0.02667(19) 0.0356(2) -0.00102(17) 0.00510(18) -0.00073(17) N1A 0.01860(17) 0.02598(17) 0.02261(16) -0.00149(15) 0.00445(14) -0.00189(15) N2A 0.02254(18) 0.02501(17) 0.01850(15) 0.00213(14) 0.00375(14) -0.00231(15) N3A 0.02855(19) 0.0350(2) 0.01965(16) 0.00435(16) 0.00216(15) -0.00747(17) N1B 0.02386(18) 0.02225(17) 0.02185(16) -0.00075(15) -0.00226(14) 0.00012(15) N2B 0.02288(18) 0.02874(18) 0.01912(16) 0.00391(15) 0.00297(15) 0.00240(15) N3B 0.02312(19) 0.0408(2) 0.02057(17) -0.00317(17) 0.00321(15) 0.00704(17) N1C 0.02334(18) 0.02289(17) 0.02801(18) 0.00516(15) 0.00623(16) 0.00279(15) N2C 0.02480(19) 0.02226(17) 0.0335(2) -0.00091(16) 0.00209(16) 0.00119(16) N3C 0.0240(2) 0.02152(18) 0.0602(3) 0.00028(19) -0.00769(19) 0.00136(17) C1A 0.0224(2) 0.0318(2) 0.0355(2) -0.0046(2) -0.00237(19) -0.0013(2) C2A 0.0242(2) 0.0309(2) 0.0231(2) -0.00221(18) -0.00109(18) 0.00064(19) C3A 0.0212(2) 0.0241(2) 0.0251(2) -0.00314(17) 0.00707(17) -0.00116(17) C4A 0.02062(19) 0.0227(2) 0.0273(2) -0.00133(17) 0.00865(16) -0.00103(17) C5A 0.0251(2) 0.0224(2) 0.0320(2) 0.00365(18) 0.00705(18) -0.00169(18) C6A 0.0289(2) 0.0338(2) 0.0298(2) 0.0096(2) 0.00730(19) -0.0063(2) C7A 0.0385(3) 0.0470(3) 0.0399(3) 0.0218(2) -0.0009(2) -0.0069(2) C1B 0.0225(2) 0.0297(2) 0.0387(2) 0.0028(2) -0.0016(2) 0.00378(19) C2B 0.0245(2) 0.0224(2) 0.0356(2) 0.00119(19) -0.00049(19) 0.00575(18) C3B 0.0277(2) 0.0239(2) 0.0256(2) 0.00376(17) -0.00512(18) -0.00473(18) C4B 0.0219(2) 0.0277(2) 0.01976(18) 0.00314(17) -0.00176(16) -0.00569(18) C5B 0.0291(2) 0.0380(2) 0.0219(2) 0.00201(19) 0.00342(18) -0.0102(2) C6B 0.0237(2) 0.0450(3) 0.0240(2) -0.0064(2) 0.00469(18) -0.0014(2) C7B 0.0324(3) 0.0596(3) 0.0299(2) -0.0050(3) 0.0117(2) 0.0072(3) C1C 0.0199(2) 0.0312(2) 0.0444(3) 0.0010(2) 0.0090(2) -0.00018(19) C2C 0.0251(2) 0.0281(2) 0.0369(2) 0.0032(2) 0.01128(19) -0.00343(19) C3C 0.0310(2) 0.0295(2) 0.0263(2) 0.00285(19) 0.00801(19) 0.0092(2) C4C 0.0294(2) 0.0285(2) 0.0267(2) 0.00003(19) 0.00034(18) 0.00867(19) C5C 0.0395(3) 0.0315(2) 0.0397(3) -0.0085(2) -0.0085(2) 0.0121(2) C6C 0.0339(3) 0.0256(2) 0.0666(4) -0.0056(2) -0.0187(3) 0.0088(2) C7C 0.0440(3) 0.0289(3) 0.1046(5) -0.0155(3) -0.0253(3) 0.0084(3) B 0.0644(5) 0.0338(3) 0.0579(4) -0.0024(3) 0.0178(4) -0.0013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N2B 1.9419(4) . ? Co N2A 1.9464(4) . ? Co N2C 1.9513(4) . ? Co N1B 1.9758(4) . ? Co N1A 1.9805(4) . ? Co N1C 1.9815(4) . ? F1A B 1.3723(3) . ? F2A B 1.3731(3) . ? F3A B 1.3742(3) . ? F4A B 1.3731(3) . ? F1B B 1.3729(3) . ? F2B B 1.3731(3) . ? F3B B 1.3745(3) . ? F4B B 1.3717(3) . ? N C1C 1.4344(7) . ? N C1A 1.4347(7) . ? N C1B 1.4408(7) . ? N1A C3A 1.2843(6) . ? N1A C2A 1.4723(6) . ? N2A N3A 1.3390(5) . ? N2A C4A 1.3511(6) . ? N3A C6A 1.3554(7) . ? N3A H3AB 0.8800 . ? N1B C3B 1.2860(6) . ? N1B C2B 1.4671(6) . ? N2B N3B 1.3452(6) . ? N2B C4B 1.3536(6) . ? N3B C6B 1.3619(7) . ? N1C C3C 1.2915(6) . ? N1C C2C 1.4621(6) . ? N2C N3C 1.3358(6) . ? N2C C4C 1.3517(7) . ? N3C C6C 1.3546(8) . ? N3C H3CB 0.8800 . ? C1A C2A 1.5288(7) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.4400(6) . ? C3A H3AA 0.9500 . ? C4A C5A 1.3987(7) . ? C5A C6A 1.3747(7) . ? C5A H5AA 0.9500 . ? C6A C7A 1.4929(8) . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C1B C2B 1.5336(7) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C4B 1.4351(7) . ? C3B H3BA 0.9500 . ? C4B C5B 1.4022(7) . ? C5B C6B 1.3758(7) . ? C5B H5BA 0.9500 . ? C6B C7B 1.5026(8) . ? C7B H7BA 0.9800 . ? C7B H7BB 0.9800 . ? C7B H7BC 0.9800 . ? C1C C2C 1.5370(7) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C3C C4C 1.4241(7) . ? C3C H3CA 0.9500 . ? C4C C5C 1.3951(7) . ? C5C C6C 1.3802(8) . ? C5C H5CA 0.9500 . ? C6C C7C 1.4982(9) . ? C7C H7CB 0.9800 . ? C7C H7CC 0.9800 . ? C7C H7CD 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 N2B Co N2A 94.579(16) . . ? N2B Co N2C 97.008(17) . . ? N2A Co N2C 96.972(16) . . ? N2B Co N1B 80.454(16) . . ? N2A Co N1B 173.351(16) . . ? N2C Co N1B 88.067(16) . . ? N2B Co N1A 87.910(16) . . ? N2A Co N1A 80.508(16) . . ? N2C Co N1A 174.662(17) . . ? N1B Co N1A 94.819(16) . . ? N2B Co N1C 176.018(17) . . ? N2A Co N1C 88.786(16) . . ? N2C Co N1C 80.445(17) . . ? N1B Co N1C 96.351(16) . . ? N1A Co N1C 94.754(16) . . ? C1C N C1A 119.84(4) . . ? C1C N C1B 120.00(4) . . ? C1A N C1B 119.91(4) . . ? C3A N1A C2A 118.51(4) . . ? C3A N1A Co 115.40(3) . . ? C2A N1A Co 126.07(3) . . ? N3A N2A C4A 107.43(4) . . ? N3A N2A Co 137.13(3) . . ? C4A N2A Co 114.77(3) . . ? N2A N3A C6A 109.28(4) . . ? N2A N3A H3AB 125.4 . . ? C6A N3A H3AB 125.4 . . ? C3B N1B C2B 118.74(4) . . ? C3B N1B Co 115.27(3) . . ? C2B N1B Co 125.96(3) . . ? N3B N2B C4B 108.06(4) . . ? N3B N2B Co 135.46(3) . . ? C4B N2B Co 114.87(3) . . ? N2B N3B C6B 108.51(4) . . ? C3C N1C C2C 118.71(4) . . ? C3C N1C Co 114.73(3) . . ? C2C N1C Co 126.56(3) . . ? N3C N2C C4C 108.03(4) . . ? N3C N2C Co 135.83(4) . . ? C4C N2C Co 114.72(3) . . ? N2C N3C C6C 109.00(4) . . ? N2C N3C H3CB 125.5 . . ? C6C N3C H3CB 125.5 . . ? N C1A C2A 115.98(4) . . ? N C1A H1AA 108.3 . . ? C2A C1A H1AA 108.3 . . ? N C1A H1AB 108.3 . . ? C2A C1A H1AB 108.3 . . ? H1AA C1A H1AB 107.4 . . ? N1A C2A C1A 111.47(4) . . ? N1A C2A H2AA 109.3 . . ? C1A C2A H2AA 109.3 . . ? N1A C2A H2AB 109.3 . . ? C1A C2A H2AB 109.3 . . ? H2AA C2A H2AB 108.0 . . ? N1A C3A C4A 115.44(4) . . ? N1A C3A H3AA 122.3 . . ? C4A C3A H3AA 122.3 . . ? N2A C4A C5A 109.73(4) . . ? N2A C4A C3A 113.70(4) . . ? C5A C4A C3A 136.48(4) . . ? C6A C5A C4A 104.40(4) . . ? C6A C5A H5AA 127.8 . . ? C4A C5A H5AA 127.8 . . ? N3A C6A C5A 109.16(4) . . ? N3A C6A C7A 120.53(5) . . ? C5A C6A C7A 130.27(5) . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? N C1B C2B 115.05(4) . . ? N C1B H1BA 108.5 . . ? C2B C1B H1BA 108.5 . . ? N C1B H1BB 108.5 . . ? C2B C1B H1BB 108.5 . . ? H1BA C1B H1BB 107.5 . . ? N1B C2B C1B 110.96(4) . . ? N1B C2B H2BA 109.4 . . ? C1B C2B H2BA 109.4 . . ? N1B C2B H2BB 109.4 . . ? C1B C2B H2BB 109.4 . . ? H2BA C2B H2BB 108.0 . . ? N1B C3B C4B 115.63(4) . . ? N1B C3B H3BA 122.2 . . ? C4B C3B H3BA 122.2 . . ? N2B C4B C5B 109.36(4) . . ? N2B C4B C3B 113.14(4) . . ? C5B C4B C3B 137.42(4) . . ? C6B C5B C4B 104.54(4) . . ? C6B C5B H5BA 127.7 . . ? C4B C5B H5BA 127.7 . . ? N3B C6B C5B 109.52(5) . . ? N3B C6B C7B 119.90(5) . . ? C5B C6B C7B 130.56(5) . . ? C6B C7B H7BA 109.5 . . ? C6B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C6B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N C1C C2C 115.01(4) . . ? N C1C H1CA 108.5 . . ? C2C C1C H1CA 108.5 . . ? N C1C H1CB 108.5 . . ? C2C C1C H1CB 108.5 . . ? H1CA C1C H1CB 107.5 . . ? N1C C2C C1C 110.50(4) . . ? N1C C2C H2CA 109.5 . . ? C1C C2C H2CA 109.5 . . ? N1C C2C H2CB 109.5 . . ? C1C C2C H2CB 109.5 . . ? H2CA C2C H2CB 108.1 . . ? N1C C3C C4C 116.18(5) . . ? N1C C3C H3CA 121.9 . . ? C4C C3C H3CA 121.9 . . ? N2C C4C C5C 109.34(5) . . ? N2C C4C C3C 113.58(4) . . ? C5C C4C C3C 136.77(5) . . ? C6C C5C C4C 104.54(5) . . ? C6C C5C H5CA 127.7 . . ? C4C C5C H5CA 127.7 . . ? N3C C6C C5C 109.08(5) . . ? N3C C6C C7C 120.89(6) . . ? C5C C6C C7C 130.01(6) . . ? C6C C7C H7CB 109.5 . . ? C6C C7C H7CC 109.5 . . ? H7CB C7C H7CC 109.5 . . ? C6C C7C H7CD 109.5 . . ? H7CB C7C H7CD 109.5 . . ? H7CC C7C H7CD 109.5 . . ? F4B B F1A 114.52(4) . . ? F4B B F1B 106.75(3) . . ? F1A B F1B 17.96(3) . . ? F4B B F2A 119.31(4) . . ? F1A B F2A 112.99(2) . . ? F1B B F2A 106.88(3) . . ? F4B B F4A 67.63(3) . . ? F1A B F4A 122.48(9) . . ? F1B B F4A 136.56(9) . . ? F2A B F4A 113.07(9) . . ? F4B B F2B 109.55(4) . . ? F1A B F2B 118.98(3) . . ? F1B B F2B 110.19(3) . . ? F2A B F2B 9.89(4) . . ? F4A B F2B 112.09(9) . . ? F4B B F3A 29.11(3) . . ? F1A B F3A 105.59(4) . . ? F1B B F3A 91.26(3) . . ? F2A B F3A 102.71(5) . . ? F4A B F3A 95.907(17) . . ? F2B B F3A 93.18(5) . . ? F4B B F3B 118.03(4) . . ? F1A B F3B 88.42(4) . . ? F1B B F3B 106.20(3) . . ? F2A B F3B 98.58(5) . . ? F4A B F3B 52.37(3) . . ? F2B B F3B 105.97(4) . . ? F3A B F3B 147.14(3) . . ? 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 N2B Co N1A C3A 95.30(4) . . . . ? N2A Co N1A C3A 0.31(3) . . . . ? N2C Co N1A C3A -61.89(19) . . . . ? N1B Co N1A C3A 175.54(3) . . . . ? N1C Co N1A C3A -87.66(4) . . . . ? N2B Co N1A C2A -83.18(4) . . . . ? N2A Co N1A C2A -178.18(4) . . . . ? N2C Co N1A C2A 119.63(17) . . . . ? N1B Co N1A C2A -2.94(4) . . . . ? N1C Co N1A C2A 93.86(4) . . . . ? N2B Co N2A N3A 100.92(5) . . . . ? N2C Co N2A N3A 3.27(5) . . . . ? N1B Co N2A N3A 142.34(13) . . . . ? N1A Co N2A N3A -171.97(5) . . . . ? N1C Co N2A N3A -76.95(5) . . . . ? N2B Co N2A C4A -89.93(3) . . . . ? N2C Co N2A C4A 172.42(3) . . . . ? N1B Co N2A C4A -48.50(15) . . . . ? N1A Co N2A C4A -2.82(3) . . . . ? N1C Co N2A C4A 92.20(3) . . . . ? C4A N2A N3A C6A -0.12(5) . . . . ? Co N2A N3A C6A 169.56(4) . . . . ? N2B Co N1B C3B 0.99(3) . . . . ? N2A Co N1B C3B -40.98(15) . . . . ? N2C Co N1B C3B 98.43(4) . . . . ? N1A Co N1B C3B -86.07(3) . . . . ? N1C Co N1B C3B 178.59(3) . . . . ? N2B Co N1B C2B -176.98(4) . . . . ? N2A Co N1B C2B 141.05(13) . . . . ? N2C Co N1B C2B -79.54(4) . . . . ? N1A Co N1B C2B 95.96(4) . . . . ? N1C Co N1B C2B 0.62(4) . . . . ? N2A Co N2B N3B 6.58(4) . . . . ? N2C Co N2B N3B 104.19(4) . . . . ? N1B Co N2B N3B -168.97(4) . . . . ? N1A Co N2B N3B -73.72(4) . . . . ? N1C Co N2B N3B 154.2(2) . . . . ? N2A Co N2B C4B 169.99(3) . . . . ? N2C Co N2B C4B -92.40(3) . . . . ? N1B Co N2B C4B -5.56(3) . . . . ? N1A Co N2B C4B 89.69(3) . . . . ? N1C Co N2B C4B -42.4(2) . . . . ? C4B N2B N3B C6B 0.66(5) . . . . ? Co N2B N3B C6B 164.85(4) . . . . ? N2B Co N1C C3C -51.4(2) . . . . ? N2A Co N1C C3C 96.33(4) . . . . ? N2C Co N1C C3C -0.95(4) . . . . ? N1B Co N1C C3C -87.90(4) . . . . ? N1A Co N1C C3C 176.70(4) . . . . ? N2B Co N1C C2C 129.2(2) . . . . ? N2A Co N1C C2C -83.07(4) . . . . ? N2C Co N1C C2C 179.65(4) . . . . ? N1B Co N1C C2C 92.70(4) . . . . ? N1A Co N1C C2C -2.70(4) . . . . ? N2B Co N2C N3C 9.80(5) . . . . ? N2A Co N2C N3C 105.32(5) . . . . ? N1B Co N2C N3C -70.33(5) . . . . ? N1A Co N2C N3C 166.83(16) . . . . ? N1C Co N2C N3C -167.10(5) . . . . ? N2B Co N2C C4C 174.16(3) . . . . ? N2A Co N2C C4C -90.32(4) . . . . ? N1B Co N2C C4C 94.03(4) . . . . ? N1A Co N2C C4C -28.81(19) . . . . ? N1C Co N2C C4C -2.75(3) . . . . ? C4C N2C N3C C6C -0.10(6) . . . . ? Co N2C N3C C6C 164.98(4) . . . . ? C1C N C1A C2A -111.50(5) . . . . ? C1B N C1A C2A 74.23(6) . . . . ? C3A N1A C2A C1A 100.85(5) . . . . ? Co N1A C2A C1A -80.71(5) . . . . ? N C1A C2A N1A 53.25(6) . . . . ? C2A N1A C3A C4A -179.27(4) . . . . ? Co N1A C3A C4A 2.13(5) . . . . ? N3A N2A C4A C5A -0.19(5) . . . . ? Co N2A C4A C5A -172.48(3) . . . . ? N3A N2A C4A C3A 176.96(4) . . . . ? Co N2A C4A C3A 4.67(5) . . . . ? N1A C3A C4A N2A -4.47(6) . . . . ? N1A C3A C4A C5A 171.63(5) . . . . ? N2A C4A C5A C6A 0.41(5) . . . . ? C3A C4A C5A C6A -175.79(6) . . . . ? N2A N3A C6A C5A 0.39(6) . . . . ? N2A N3A C6A C7A -177.49(5) . . . . ? C4A C5A C6A N3A -0.48(6) . . . . ? C4A C5A C6A C7A 177.13(5) . . . . ? C1C N C1B C2B 74.91(6) . . . . ? C1A N C1B C2B -110.83(5) . . . . ? C3B N1B C2B C1B 98.89(5) . . . . ? Co N1B C2B C1B -83.20(5) . . . . ? N C1B C2B N1B 53.17(6) . . . . ? C2B N1B C3B C4B -178.35(4) . . . . ? Co N1B C3B C4B 3.53(5) . . . . ? N3B N2B C4B C5B -0.69(5) . . . . ? Co N2B C4B C5B -168.53(3) . . . . ? N3B N2B C4B C3B 176.66(4) . . . . ? Co N2B C4B C3B 8.82(5) . . . . ? N1B C3B C4B N2B -8.10(6) . . . . ? N1B C3B C4B C5B 168.21(5) . . . . ? N2B C4B C5B C6B 0.44(5) . . . . ? C3B C4B C5B C6B -175.95(6) . . . . ? N2B N3B C6B C5B -0.38(6) . . . . ? N2B N3B C6B C7B -179.05(4) . . . . ? C4B C5B C6B N3B -0.04(6) . . . . ? C4B C5B C6B C7B 178.44(5) . . . . ? C1A N C1C C2C 72.48(6) . . . . ? C1B N C1C C2C -113.26(5) . . . . ? C3C N1C C2C C1C 98.17(5) . . . . ? Co N1C C2C C1C -82.45(5) . . . . ? N C1C C2C N1C 55.03(6) . . . . ? C2C N1C C3C C4C -176.22(4) . . . . ? Co N1C C3C C4C 4.33(6) . . . . ? N3C N2C C4C C5C -0.49(6) . . . . ? Co N2C C4C C5C -169.09(3) . . . . ? N3C N2C C4C C3C 174.29(4) . . . . ? Co N2C C4C C3C 5.68(5) . . . . ? N1C C3C C4C N2C -6.62(7) . . . . ? N1C C3C C4C C5C 166.17(6) . . . . ? N2C C4C C5C C6C 0.85(6) . . . . ? C3C C4C C5C C6C -172.14(6) . . . . ? N2C N3C C6C C5C 0.65(6) . . . . ? N2C N3C C6C C7C -177.73(5) . . . . ? C4C C5C C6C N3C -0.91(6) . . . . ? C4C C5C C6C C7C 177.28(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3AB N3B 0.88 1.92 2.7672(6) 160.8 2_656 N3C H3CB N3C 0.88 1.89 2.7448(9) 164.1 2_656 _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.533 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.079 # Attachment 'GB-AMS4ALN.CIF' data_gb-ams4a _database_code_depnum_ccdc_archive 'CCDC 766397' #TrackingRef 'GB-AMS4ALN.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H29.50 B F4 Fe N10 O0.50' _chemical_formula_weight 572.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.1965(15) _cell_length_b 12.4243(8) _cell_length_c 19.3105(15) _cell_angle_alpha 90.00 _cell_angle_beta 92.783(7) _cell_angle_gamma 90.00 _cell_volume 5079.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 346 _cell_measurement_theta_min 4.1178 _cell_measurement_theta_max 74.1892 _exptl_crystal_description chunk _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2372 _exptl_absorpt_coefficient_mu 5.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.32947 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Goniometer Xcalibur, detector: Ruby (Gemini Cu) ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 10938 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.58 _diffrn_reflns_theta_max 74.30 _reflns_number_total 4974 _reflns_number_gt 3643 _reflns_threshold_expression I>2/s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^] 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 4974 _refine_ls_number_parameters 410 _refine_ls_number_restraints 128 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1282 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.370626(8) 0.367577(14) 0.192413(9) 0.01742(4) Uani 1 1 d . . . N N 0.22105(5) 0.34968(8) 0.12344(5) 0.0278(3) Uani 1 1 d . . . N1A N 0.33880(4) 0.47135(8) 0.12078(5) 0.0201(2) Uani 1 1 d . . . N2A N 0.40340(4) 0.50127(8) 0.23347(5) 0.0207(2) Uani 1 1 d . . . N3A N 0.43167(5) 0.53222(8) 0.29330(5) 0.0261(3) Uani 1 1 d . . . H3AB H 0.4467 0.4886 0.3260 0.031 Uiso 1 1 calc R . . N1B N 0.34114(4) 0.23745(8) 0.14091(5) 0.0215(2) Uani 1 1 d . . . N2B N 0.44258(4) 0.34371(8) 0.13538(5) 0.0215(3) Uani 1 1 d . . . N3B N 0.49471(5) 0.40005(9) 0.12045(5) 0.0263(3) Uani 1 1 d . . . N1C N 0.29672(4) 0.38088(8) 0.25121(5) 0.0221(3) Uani 1 1 d . . . N2C N 0.39705(5) 0.27193(8) 0.26893(5) 0.0223(3) Uani 1 1 d . . . N3C N 0.44243(5) 0.19745(8) 0.27966(6) 0.0300(3) Uani 1 1 d . . . H3CB H 0.4756 0.1890 0.2544 0.036 Uiso 0.50 1 calc PR . . C1A C 0.23287(6) 0.42681(10) 0.06963(6) 0.0274(3) Uani 1 1 d . . . H1AA H 0.2139 0.4966 0.0822 0.033 Uiso 1 1 calc R . . H1AB H 0.2112 0.4022 0.0259 0.033 Uiso 1 1 calc R . . C2A C 0.30267(5) 0.44485(10) 0.05661(6) 0.0239(3) Uani 1 1 d . . . H2AA H 0.3203 0.3789 0.0362 0.029 Uiso 1 1 calc R . . H2AB H 0.3066 0.5042 0.0229 0.029 Uiso 1 1 calc R . . C3A C 0.35294(5) 0.57050(9) 0.13292(6) 0.0213(3) Uani 1 1 d . . . H3AA H 0.3414 0.6262 0.1011 0.026 Uiso 1 1 calc R . . C4A C 0.38718(5) 0.59187(9) 0.19742(6) 0.0205(3) Uani 1 1 d . . . C5A C 0.40597(5) 0.68199(10) 0.23587(6) 0.0242(3) Uani 1 1 d . . . H5AA H 0.4007 0.7555 0.2233 0.029 Uiso 1 1 calc R . . C6A C 0.43379(6) 0.64117(10) 0.29615(6) 0.0279(3) Uani 1 1 d . . . C7A C 0.46171(7) 0.69709(11) 0.35911(7) 0.0358(4) Uani 1 1 d . . . H7AA H 0.4920 0.6492 0.3836 0.054 Uiso 1 1 calc R . . H7AB H 0.4280 0.7160 0.3899 0.054 Uiso 1 1 calc R . . H7AC H 0.4834 0.7627 0.3451 0.054 Uiso 1 1 calc R . . C1B C 0.22676(5) 0.23570(10) 0.10960(7) 0.0287(3) Uani 1 1 d . . . H1BA H 0.2323 0.2255 0.0594 0.034 Uiso 1 1 calc R . . H1BB H 0.1869 0.1997 0.1210 0.034 Uiso 1 1 calc R . . C2B C 0.28164(5) 0.18073(10) 0.15011(7) 0.0259(3) Uani 1 1 d . . . H2BA H 0.2728 0.1791 0.2000 0.031 Uiso 1 1 calc R . . H2BB H 0.2855 0.1055 0.1340 0.031 Uiso 1 1 calc R . . C3B C 0.37922(5) 0.20086(9) 0.09659(6) 0.0222(3) Uani 1 1 d . . . H3BA H 0.3706 0.1369 0.0708 0.027 Uiso 1 1 calc R . . C4B C 0.43565(5) 0.26308(9) 0.08862(6) 0.0218(3) Uani 1 1 d . . . C5B C 0.48437(6) 0.26712(11) 0.04275(6) 0.0268(3) Uani 1 1 d . . . H5BA H 0.4912 0.2203 0.0049 0.032 Uiso 1 1 calc R . . C6B C 0.52053(6) 0.35420(11) 0.06453(6) 0.0276(3) Uani 1 1 d . . . C7B C 0.57897(6) 0.40218(12) 0.03589(7) 0.0381(4) Uani 1 1 d . . . H7BA H 0.6065 0.4299 0.0741 0.057 Uiso 1 1 calc R . . H7BB H 0.5670 0.4612 0.0042 0.057 Uiso 1 1 calc R . . H7BC H 0.6015 0.3468 0.0107 0.057 Uiso 1 1 calc R . . C1C C 0.19401(6) 0.38524(10) 0.18623(7) 0.0295(3) Uani 1 1 d . . . H1CA H 0.1777 0.3217 0.2107 0.035 Uiso 1 1 calc R . . H1CB H 0.1576 0.4327 0.1740 0.035 Uiso 1 1 calc R . . C2C C 0.23988(5) 0.44589(10) 0.23583(6) 0.0257(3) Uani 1 1 d . . . H2CA H 0.2519 0.5150 0.2146 0.031 Uiso 1 1 calc R . . H2CB H 0.2190 0.4620 0.2794 0.031 Uiso 1 1 calc R . . C3C C 0.30002(6) 0.32606(10) 0.30812(6) 0.0254(3) Uani 1 1 d . . . H3CA H 0.2684 0.3300 0.3412 0.031 Uiso 1 1 calc R . . C4C C 0.35458(6) 0.25892(10) 0.31787(6) 0.0257(3) Uani 1 1 d . . . C5C C 0.37338(6) 0.17488(11) 0.36216(7) 0.0322(3) Uani 1 1 d . . . H5CA H 0.3527 0.1493 0.4015 0.039 Uiso 1 1 calc R . . C6C C 0.42890(6) 0.13716(10) 0.33587(8) 0.0352(4) Uani 1 1 d . . . C7C C 0.47088(7) 0.04521(12) 0.35864(9) 0.0503(5) Uani 1 1 d . . . H7CA H 0.5152 0.0659 0.3546 0.075 Uiso 1 1 calc R . . H7CB H 0.4614 -0.0175 0.3292 0.075 Uiso 1 1 calc R . . H7CC H 0.4635 0.0272 0.4070 0.075 Uiso 1 1 calc R . . B B 0.13415(7) 0.39626(11) 0.41874(8) 0.0468(5) Uani 1 1 d D . . F1 F 0.12379(5) 0.43706(8) 0.35316(5) 0.0736(4) Uani 1 1 d D A . F2 F 0.09929(10) 0.45715(17) 0.46562(10) 0.0595(7) Uani 0.3878(0) 1 d PDU A 1 F3 F 0.12978(15) 0.29287(14) 0.42921(16) 0.1009(11) Uani 0.3878(0) 1 d PDU A 1 F4 F 0.19946(9) 0.42968(19) 0.43590(13) 0.0818(8) Uani 0.3878(0) 1 d PDU A 1 F2A F 0.07669(10) 0.3277(2) 0.42207(15) 0.0653(10) Uani 0.3050(0) 1 d PDU A 2 F3A F 0.13697(14) 0.45848(18) 0.47042(11) 0.0658(9) Uani 0.3050(0) 1 d PDU A 2 F4A F 0.18107(11) 0.3161(2) 0.41201(16) 0.0677(8) Uani 0.3050(0) 1 d PDU A 2 F2B F 0.11016(10) 0.46524(16) 0.46884(10) 0.0276(3) Uani 0.3073(0) 1 d PDU A 3 F3B F 0.10659(11) 0.29818(15) 0.42482(12) 0.0371(6) Uani 0.3073(0) 1 d PDU A 3 F4B F 0.19979(9) 0.3920(2) 0.43230(16) 0.0737(10) Uani 0.3073(0) 1 d PDU A 3 O1W O 0.25100(16) 0.3014(3) 0.53539(18) 0.1255(16) Uani 0.50 1 d PD . . H1W1 H 0.2819(3) 0.2764(14) 0.5158(8) 0.188 Uiso 0.50 1 d PD . . H1W2 H 0.2240(4) 0.3114(19) 0.5026(6) 0.188 Uiso 0.50 1 d PD . . 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 Fe 0.01588(7) 0.01719(7) 0.01937(7) -0.00093(7) 0.00263(6) 0.00017(7) N 0.0236(5) 0.0261(5) 0.0337(5) 0.0004(4) 0.0026(4) 0.0017(4) N1A 0.0153(4) 0.0236(5) 0.0215(4) 0.0017(4) 0.0023(4) 0.0006(4) N2A 0.0219(4) 0.0212(5) 0.0191(4) -0.0021(4) 0.0025(4) -0.0003(4) N3A 0.0282(5) 0.0286(5) 0.0212(5) -0.0030(4) -0.0006(4) 0.0072(4) N1B 0.0193(4) 0.0188(4) 0.0263(5) 0.0001(4) -0.0013(4) 0.0002(4) N2B 0.0170(4) 0.0278(5) 0.0198(4) -0.0044(4) 0.0025(4) -0.0003(4) N3B 0.0204(4) 0.0369(6) 0.0217(5) 0.0003(4) 0.0029(4) -0.0063(4) N1C 0.0199(4) 0.0218(5) 0.0251(5) -0.0034(4) 0.0077(4) -0.0015(4) N2C 0.0230(4) 0.0177(5) 0.0261(5) 0.0025(4) 0.0001(4) -0.0010(4) N3C 0.0227(5) 0.0182(5) 0.0486(6) 0.0046(4) -0.0038(5) -0.0002(4) C1A 0.0190(5) 0.0300(6) 0.0329(6) 0.0032(5) -0.0029(5) 0.0008(5) C2A 0.0217(5) 0.0263(6) 0.0233(5) -0.0003(5) -0.0040(5) -0.0013(5) C3A 0.0197(5) 0.0206(6) 0.0241(5) 0.0036(4) 0.0048(4) -0.0002(5) C4A 0.0188(5) 0.0184(5) 0.0247(5) 0.0009(4) 0.0058(4) 0.0010(4) C5A 0.0220(5) 0.0220(6) 0.0291(6) -0.0014(5) 0.0059(5) 0.0020(5) C6A 0.0256(6) 0.0299(6) 0.0286(6) -0.0092(5) 0.0055(5) 0.0034(5) C7A 0.0382(7) 0.0367(7) 0.0322(6) -0.0170(5) -0.0032(6) 0.0035(6) C1B 0.0183(5) 0.0302(6) 0.0373(7) -0.0020(5) -0.0028(5) -0.0044(5) C2B 0.0225(5) 0.0200(6) 0.0351(6) -0.0016(5) 0.0005(5) -0.0030(5) C3B 0.0231(5) 0.0195(5) 0.0234(5) -0.0021(4) -0.0037(5) 0.0040(5) C4B 0.0211(5) 0.0237(6) 0.0204(5) -0.0009(4) -0.0019(4) 0.0038(5) C5B 0.0265(6) 0.0355(6) 0.0182(5) -0.0034(5) 0.0006(5) 0.0085(5) C6B 0.0198(5) 0.0425(7) 0.0206(5) 0.0036(5) 0.0027(4) 0.0006(5) C7B 0.0282(6) 0.0556(9) 0.0314(6) 0.0026(6) 0.0120(5) -0.0052(6) C1C 0.0163(5) 0.0322(7) 0.0406(7) 0.0028(5) 0.0062(5) -0.0006(5) C2C 0.0216(5) 0.0242(6) 0.0319(6) -0.0019(5) 0.0089(5) 0.0021(5) C3C 0.0263(6) 0.0273(6) 0.0232(5) -0.0020(5) 0.0058(5) -0.0080(5) C4C 0.0266(5) 0.0259(6) 0.0245(6) 0.0007(5) 0.0005(5) -0.0069(5) C5C 0.0324(6) 0.0305(6) 0.0328(6) 0.0100(5) -0.0062(5) -0.0117(5) C6C 0.0282(6) 0.0228(6) 0.0531(8) 0.0047(6) -0.0123(6) -0.0090(5) C7C 0.0386(7) 0.0281(7) 0.0821(11) 0.0140(7) -0.0179(8) -0.0045(6) B 0.0469(10) 0.0289(8) 0.0659(11) 0.0049(8) 0.0168(8) 0.0022(8) F1 0.0867(7) 0.0778(7) 0.0585(6) 0.0093(5) 0.0253(5) 0.0029(6) F2 0.0677(13) 0.0550(12) 0.0562(12) 0.0011(10) 0.0062(11) -0.0089(11) F3 0.134(2) 0.0256(13) 0.148(2) 0.0027(15) 0.0556(19) -0.0070(15) F4 0.0659(16) 0.0707(14) 0.1075(16) -0.0668(11) -0.0072(14) 0.0065(13) F2A 0.0481(15) 0.0728(19) 0.0770(19) -0.0021(16) 0.0248(14) -0.0313(15) F3A 0.0826(18) 0.0368(15) 0.0727(17) -0.0176(13) -0.0499(15) 0.0021(14) F4A 0.0639(15) 0.0525(14) 0.0881(15) -0.0093(13) 0.0165(13) 0.0141(12) F2B 0.0278(5) 0.0272(5) 0.0276(5) -0.0005(4) 0.0004(4) -0.0016(4) F3B 0.0378(11) 0.0283(11) 0.0463(12) -0.0103(9) 0.0139(10) 0.0015(10) F4B 0.0404(15) 0.0723(17) 0.108(2) -0.0645(14) 0.0018(15) 0.0173(14) O1W 0.112(3) 0.123(3) 0.137(3) -0.024(2) -0.046(2) 0.024(2) _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 Fe N2B 1.9468(10) . ? Fe N2A 1.9537(10) . ? Fe N2C 1.9567(10) . ? Fe N1B 1.9833(10) . ? Fe N1A 1.9850(9) . ? Fe N1C 1.9857(10) . ? N C1C 1.4357(17) . ? N C1A 1.4443(16) . ? N C1B 1.4474(16) . ? N1A C3A 1.2867(15) . ? N1A C2A 1.4622(14) . ? N2A N3A 1.3320(13) . ? N2A C4A 1.3590(15) . ? N3A C6A 1.3554(16) . ? N3A H3AB 0.8800 . ? N1B C3B 1.2876(15) . ? N1B C2B 1.4631(15) . ? N2B N3B 1.3510(14) . ? N2B C4B 1.3520(15) . ? N3B C6B 1.3592(16) . ? N1C C3C 1.2919(15) . ? N1C C2C 1.4688(15) . ? N2C N3C 1.3436(14) . ? N2C C4C 1.3463(16) . ? N3C C6C 1.3608(18) . ? N3C H3CB 0.8800 . ? C1A C2A 1.5293(16) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.4355(16) . ? C3A H3AA 0.9500 . ? C4A C5A 1.3910(17) . ? C5A C6A 1.3760(17) . ? C5A H5AA 0.9500 . ? C6A C7A 1.4971(18) . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C1B C2B 1.5307(17) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C4B 1.4386(16) . ? C3B H3BA 0.9500 . ? C4B C5B 1.3937(16) . ? C5B C6B 1.3797(18) . ? C5B H5BA 0.9500 . ? C6B C7B 1.5040(18) . ? C7B H7BA 0.9800 . ? C7B H7BB 0.9800 . ? C7B H7BC 0.9800 . ? C1C C2C 1.5298(17) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C3C C4C 1.4310(17) . ? C3C H3CA 0.9500 . ? C4C C5C 1.3955(18) . ? C5C C6C 1.3858(19) . ? C5C H5CA 0.9500 . ? C6C C7C 1.501(2) . ? C7C H7CA 0.9800 . ? C7C H7CB 0.9800 . ? C7C H7CC 0.9800 . ? B F3A 1.261(3) . ? B F3 1.304(2) . ? B F3B 1.359(2) . ? B F1 1.3718(18) . ? B F4B 1.404(2) . ? B F2B 1.406(2) . ? B F2 1.415(3) . ? B F4A 1.418(3) . ? B F4 1.468(2) . ? B F2A 1.490(3) . ? O1W H1W1 0.832(11) . ? O1W H1W2 0.842(10) . ? 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 N2B Fe N2A 94.95(4) . . ? N2B Fe N2C 97.54(4) . . ? N2A Fe N2C 97.29(4) . . ? N2B Fe N1B 80.13(4) . . ? N2A Fe N1B 173.62(4) . . ? N2C Fe N1B 87.44(4) . . ? N2B Fe N1A 87.35(4) . . ? N2A Fe N1A 80.37(4) . . ? N2C Fe N1A 174.76(4) . . ? N1B Fe N1A 95.27(4) . . ? N2B Fe N1C 176.01(4) . . ? N2A Fe N1C 88.39(4) . . ? N2C Fe N1C 79.84(4) . . ? N1B Fe N1C 96.69(4) . . ? N1A Fe N1C 95.37(4) . . ? C1C N C1A 119.59(10) . . ? C1C N C1B 119.83(10) . . ? C1A N C1B 119.83(10) . . ? C3A N1A C2A 118.54(10) . . ? C3A N1A Fe 115.25(7) . . ? C2A N1A Fe 126.20(8) . . ? N3A N2A C4A 107.29(9) . . ? N3A N2A Fe 137.18(8) . . ? C4A N2A Fe 114.85(7) . . ? N2A N3A C6A 109.64(9) . . ? N2A N3A H3AB 125.2 . . ? C6A N3A H3AB 125.2 . . ? C3B N1B C2B 118.86(10) . . ? C3B N1B Fe 115.38(8) . . ? C2B N1B Fe 125.75(8) . . ? N3B N2B C4B 107.75(9) . . ? N3B N2B Fe 135.49(8) . . ? C4B N2B Fe 115.34(8) . . ? N2B N3B C6B 108.51(10) . . ? C3C N1C C2C 118.15(10) . . ? C3C N1C Fe 115.52(8) . . ? C2C N1C Fe 126.32(7) . . ? N3C N2C C4C 107.89(10) . . ? N3C N2C Fe 135.34(8) . . ? C4C N2C Fe 115.24(8) . . ? N2C N3C C6C 108.97(10) . . ? N2C N3C H3CB 125.5 . . ? C6C N3C H3CB 125.5 . . ? N C1A C2A 114.74(10) . . ? N C1A H1AA 108.6 . . ? C2A C1A H1AA 108.6 . . ? N C1A H1AB 108.6 . . ? C2A C1A H1AB 108.6 . . ? H1AA C1A H1AB 107.6 . . ? N1A C2A C1A 111.40(9) . . ? N1A C2A H2AA 109.3 . . ? C1A C2A H2AA 109.3 . . ? N1A C2A H2AB 109.3 . . ? C1A C2A H2AB 109.3 . . ? H2AA C2A H2AB 108.0 . . ? N1A C3A C4A 116.02(10) . . ? N1A C3A H3AA 122.0 . . ? C4A C3A H3AA 122.0 . . ? N2A C4A C5A 109.54(10) . . ? N2A C4A C3A 113.32(10) . . ? C5A C4A C3A 137.02(11) . . ? C6A C5A C4A 104.76(11) . . ? C6A C5A H5AA 127.6 . . ? C4A C5A H5AA 127.6 . . ? N3A C6A C5A 108.77(11) . . ? N3A C6A C7A 120.50(11) . . ? C5A C6A C7A 130.71(12) . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? N C1B C2B 114.23(10) . . ? N C1B H1BA 108.7 . . ? C2B C1B H1BA 108.7 . . ? N C1B H1BB 108.7 . . ? C2B C1B H1BB 108.7 . . ? H1BA C1B H1BB 107.6 . . ? N1B C2B C1B 111.17(10) . . ? N1B C2B H2BA 109.4 . . ? C1B C2B H2BA 109.4 . . ? N1B C2B H2BB 109.4 . . ? C1B C2B H2BB 109.4 . . ? H2BA C2B H2BB 108.0 . . ? N1B C3B C4B 115.64(10) . . ? N1B C3B H3BA 122.2 . . ? C4B C3B H3BA 122.2 . . ? N2B C4B C5B 109.75(10) . . ? N2B C4B C3B 113.00(10) . . ? C5B C4B C3B 137.13(11) . . ? C6B C5B C4B 104.62(10) . . ? C6B C5B H5BA 127.7 . . ? C4B C5B H5BA 127.7 . . ? N3B C6B C5B 109.37(11) . . ? N3B C6B C7B 119.77(11) . . ? C5B C6B C7B 130.84(11) . . ? C6B C7B H7BA 109.5 . . ? C6B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C6B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N C1C C2C 114.37(10) . . ? N C1C H1CA 108.7 . . ? C2C C1C H1CA 108.7 . . ? N C1C H1CB 108.7 . . ? C2C C1C H1CB 108.7 . . ? H1CA C1C H1CB 107.6 . . ? N1C C2C C1C 110.24(10) . . ? N1C C2C H2CA 109.6 . . ? C1C C2C H2CA 109.6 . . ? N1C C2C H2CB 109.6 . . ? C1C C2C H2CB 109.6 . . ? H2CA C2C H2CB 108.1 . . ? N1C C3C C4C 115.42(11) . . ? N1C C3C H3CA 122.3 . . ? C4C C3C H3CA 122.3 . . ? N2C C4C C5C 109.83(11) . . ? N2C C4C C3C 113.66(10) . . ? C5C C4C C3C 136.20(12) . . ? C6C C5C C4C 104.52(12) . . ? C6C C5C H5CA 127.7 . . ? C4C C5C H5CA 127.7 . . ? N3C C6C C5C 108.77(11) . . ? N3C C6C C7C 120.52(13) . . ? C5C C6C C7C 130.69(13) . . ? C6C C7C H7CA 109.5 . . ? C6C C7C H7CB 109.5 . . ? H7CA C7C H7CB 109.5 . . ? C6C C7C H7CC 109.5 . . ? H7CA C7C H7CC 109.5 . . ? H7CB C7C H7CC 109.5 . . ? F3A B F3 118.8(2) . . ? F3A B F3B 119.03(19) . . ? F3 B F3B 21.48(17) . . ? F3A B F1 120.21(15) . . ? F3 B F1 119.84(18) . . ? F3B B F1 111.15(15) . . ? F3A B F4B 82.4(2) . . ? F3 B F4B 90.6(2) . . ? F3B B F4B 112.10(18) . . ? F1 B F4B 107.39(17) . . ? F3A B F2B 24.06(16) . . ? F3 B F2B 117.58(19) . . ? F3B B F2B 108.41(17) . . ? F1 B F2B 111.27(13) . . ? F4B B F2B 106.45(17) . . ? F3A B F2 34.15(16) . . ? F3 B F2 112.59(19) . . ? F3B B F2 100.61(16) . . ? F1 B F2 109.13(13) . . ? F4B B F2 116.38(18) . . ? F2B B F2 10.41(13) . . ? F3A B F4A 119.8(2) . . ? F3 B F4A 51.54(18) . . ? F3B B F4A 71.62(15) . . ? F1 B F4A 104.87(17) . . ? F4B B F4A 45.35(16) . . ? F2B B F4A 140.35(19) . . ? F2 B F4A 145.53(19) . . ? F3A B F4 68.91(18) . . ? F3 B F4 108.48(19) . . ? F3B B F4 129.72(17) . . ? F1 B F4 102.18(14) . . ? F4B B F4 18.82(15) . . ? F2B B F4 92.34(15) . . ? F2 B F4 102.73(16) . . ? F4A B F4 63.97(15) . . ? F3A B F2A 108.9(2) . . ? F3 B F2A 50.66(17) . . ? F3B B F2A 29.31(14) . . ? F1 B F2A 99.00(15) . . ? F4B B F2A 140.79(19) . . ? F2B B F2A 89.71(16) . . ? F2 B F2A 79.91(16) . . ? F4A B F2A 100.43(16) . . ? F4 B F2A 156.34(18) . . ? H1W1 O1W H1W2 103.5(13) . . ? 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 N2B Fe N1A C3A -95.50(9) . . . . ? N2A Fe N1A C3A -0.03(8) . . . . ? N2C Fe N1A C3A 63.7(5) . . . . ? N1B Fe N1A C3A -175.33(8) . . . . ? N1C Fe N1A C3A 87.42(8) . . . . ? N2B Fe N1A C2A 83.31(9) . . . . ? N2A Fe N1A C2A 178.79(9) . . . . ? N2C Fe N1A C2A -117.4(4) . . . . ? N1B Fe N1A C2A 3.48(9) . . . . ? N1C Fe N1A C2A -93.76(9) . . . . ? N2B Fe N2A N3A -101.89(11) . . . . ? N2C Fe N2A N3A -3.62(12) . . . . ? N1B Fe N2A N3A -141.2(3) . . . . ? N1A Fe N2A N3A 171.65(12) . . . . ? N1C Fe N2A N3A 75.93(11) . . . . ? N2B Fe N2A C4A 89.10(8) . . . . ? N2C Fe N2A C4A -172.63(8) . . . . ? N1B Fe N2A C4A 49.8(4) . . . . ? N1A Fe N2A C4A 2.63(8) . . . . ? N1C Fe N2A C4A -93.09(8) . . . . ? C4A N2A N3A C6A 0.03(13) . . . . ? Fe N2A N3A C6A -169.54(9) . . . . ? N2B Fe N1B C3B -0.87(8) . . . . ? N2A Fe N1B C3B 38.9(4) . . . . ? N2C Fe N1B C3B -98.98(9) . . . . ? N1A Fe N1B C3B 85.51(9) . . . . ? N1C Fe N1B C3B -178.44(8) . . . . ? N2B Fe N1B C2B 178.08(10) . . . . ? N2A Fe N1B C2B -142.1(3) . . . . ? N2C Fe N1B C2B 79.96(9) . . . . ? N1A Fe N1B C2B -95.54(9) . . . . ? N1C Fe N1B C2B 0.51(9) . . . . ? N2A Fe N2B N3B -6.56(11) . . . . ? N2C Fe N2B N3B -104.60(11) . . . . ? N1B Fe N2B N3B 169.35(11) . . . . ? N1A Fe N2B N3B 73.53(11) . . . . ? N1C Fe N2B N3B -153.4(5) . . . . ? N2A Fe N2B C4B -170.93(8) . . . . ? N2C Fe N2B C4B 91.03(8) . . . . ? N1B Fe N2B C4B 4.97(8) . . . . ? N1A Fe N2B C4B -90.84(8) . . . . ? N1C Fe N2B C4B 42.2(6) . . . . ? C4B N2B N3B C6B -0.32(12) . . . . ? Fe N2B N3B C6B -165.51(9) . . . . ? N2B Fe N1C C3C 49.8(6) . . . . ? N2A Fe N1C C3C -97.11(9) . . . . ? N2C Fe N1C C3C 0.59(9) . . . . ? N1B Fe N1C C3C 86.76(9) . . . . ? N1A Fe N1C C3C -177.28(9) . . . . ? N2B Fe N1C C2C -130.0(5) . . . . ? N2A Fe N1C C2C 83.09(9) . . . . ? N2C Fe N1C C2C -179.21(10) . . . . ? N1B Fe N1C C2C -93.04(9) . . . . ? N1A Fe N1C C2C 2.92(9) . . . . ? N2B Fe N2C N3C -10.23(11) . . . . ? N2A Fe N2C N3C -106.24(11) . . . . ? N1B Fe N2C N3C 69.46(11) . . . . ? N1A Fe N2C N3C -169.3(4) . . . . ? N1C Fe N2C N3C 166.72(11) . . . . ? N2B Fe N2C C4C -174.01(8) . . . . ? N2A Fe N2C C4C 89.98(9) . . . . ? N1B Fe N2C C4C -94.32(9) . . . . ? N1A Fe N2C C4C 26.9(5) . . . . ? N1C Fe N2C C4C 2.94(8) . . . . ? C4C N2C N3C C6C -0.28(13) . . . . ? Fe N2C N3C C6C -164.88(9) . . . . ? C1C N C1A C2A 113.61(12) . . . . ? C1B N C1A C2A -76.40(13) . . . . ? C3A N1A C2A C1A -100.91(12) . . . . ? Fe N1A C2A C1A 80.31(11) . . . . ? N C1A C2A N1A -52.82(14) . . . . ? C2A N1A C3A C4A 178.62(10) . . . . ? Fe N1A C3A C4A -2.46(13) . . . . ? N3A N2A C4A C5A 0.07(13) . . . . ? Fe N2A C4A C5A 172.28(8) . . . . ? N3A N2A C4A C3A -176.78(9) . . . . ? Fe N2A C4A C3A -4.58(12) . . . . ? N1A C3A C4A N2A 4.63(15) . . . . ? N1A C3A C4A C5A -171.02(13) . . . . ? N2A C4A C5A C6A -0.14(13) . . . . ? C3A C4A C5A C6A 175.62(14) . . . . ? N2A N3A C6A C5A -0.12(14) . . . . ? N2A N3A C6A C7A 178.29(11) . . . . ? C4A C5A C6A N3A 0.15(14) . . . . ? C4A C5A C6A C7A -178.04(13) . . . . ? C1C N C1B C2B -77.31(14) . . . . ? C1A N C1B C2B 112.72(12) . . . . ? C3B N1B C2B C1B -99.08(12) . . . . ? Fe N1B C2B C1B 82.01(12) . . . . ? N C1B C2B N1B -52.57(14) . . . . ? C2B N1B C3B C4B 177.83(10) . . . . ? Fe N1B C3B C4B -3.15(13) . . . . ? N3B N2B C4B C5B 0.24(13) . . . . ? Fe N2B C4B C5B 168.81(8) . . . . ? N3B N2B C4B C3B -176.45(9) . . . . ? Fe N2B C4B C3B -7.89(12) . . . . ? N1B C3B C4B N2B 7.21(15) . . . . ? N1B C3B C4B C5B -168.21(13) . . . . ? N2B C4B C5B C6B -0.07(13) . . . . ? C3B C4B C5B C6B 175.45(13) . . . . ? N2B N3B C6B C5B 0.28(13) . . . . ? N2B N3B C6B C7B 179.05(11) . . . . ? C4B C5B C6B N3B -0.12(14) . . . . ? C4B C5B C6B C7B -178.72(13) . . . . ? C1A N C1C C2C -74.84(14) . . . . ? C1B N C1C C2C 115.17(12) . . . . ? C3C N1C C2C C1C -98.08(12) . . . . ? Fe N1C C2C C1C 81.72(11) . . . . ? N C1C C2C N1C -54.32(14) . . . . ? C2C N1C C3C C4C 176.01(10) . . . . ? Fe N1C C3C C4C -3.80(14) . . . . ? N3C N2C C4C C5C 0.91(13) . . . . ? Fe N2C C4C C5C 169.01(8) . . . . ? N3C N2C C4C C3C -173.77(10) . . . . ? Fe N2C C4C C3C -5.68(13) . . . . ? N1C C3C C4C N2C 6.22(16) . . . . ? N1C C3C C4C C5C -166.55(14) . . . . ? N2C C4C C5C C6C -1.16(14) . . . . ? C3C C4C C5C C6C 171.80(14) . . . . ? N2C N3C C6C C5C -0.46(14) . . . . ? N2C N3C C6C C7C 178.16(11) . . . . ? C4C C5C C6C N3C 0.98(14) . . . . ? C4C C5C C6C C7C -177.46(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3AB N3B 0.88 1.92 2.7664(14) 160.0 2_655 N3C H3CB N3C 0.88 1.89 2.746(2) 163.2 2_655 O1W H1W2 F4B 0.842(10) 1.743(16) 2.490(5) 146.6(19) . O1W H1W2 F4 0.842(10) 2.005(18) 2.687(4) 138(2) . O1W H1W2 F4A 0.842(10) 1.933(11) 2.750(4) 163.4(13) . O1W H1W2 F3A 0.842(10) 2.649(17) 3.306(4) 135.9(18) . O1W H1W2 F3 0.842(10) 2.403(10) 3.210(5) 160.8(17) . _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.565 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.070 # Attachment 'GB-SL335.CIF' data_gb-sl335 _database_code_depnum_ccdc_archive 'CCDC 766398' #TrackingRef 'GB-SL335.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H30 Fe N10, 2(B F4)' _chemical_formula_sum 'C21 H30 B2 F8 Fe N10' _chemical_formula_weight 652.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.2482(9) _cell_length_b 12.2583(5) _cell_length_c 22.2844(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.653(4) _cell_angle_gamma 90.00 _cell_volume 5798.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6386 _cell_measurement_theta_min 3.9653 _cell_measurement_theta_max 73.4642 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.4182 _exptl_crystal_size_mid 0.3531 _exptl_crystal_size_min 0.0544 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 4.926 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.228 _exptl_absorpt_correction_T_max 0.767 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2% _diffrn_reflns_number 14661 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1155 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.97 _diffrn_reflns_theta_max 73.78 _reflns_number_total 14661 _reflns_number_gt 8843 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WinGX _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1310P)^2^] 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 14661 _refine_ls_number_parameters 423 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.2412 _refine_ls_wR_factor_gt 0.2221 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.66271(3) 0.17783(5) 0.71691(2) 0.04042(16) Uani 1 1 d . . . N N 0.66305(18) 0.1837(3) 0.84583(14) 0.0549(8) Uani 1 1 d . . . N1A N 0.75234(16) 0.1333(3) 0.76246(14) 0.0484(8) Uani 1 1 d . . . N2A N 0.73767(16) 0.2477(3) 0.66119(14) 0.0455(8) Uani 1 1 d . . . N3A N 0.74608(18) 0.2989(3) 0.60861(15) 0.0516(9) Uani 1 1 d . . . H3AB H 0.7156 0.3220 0.5852 0.062 Uiso 1 1 calc R . . N1B N 0.59587(15) 0.0674(3) 0.75654(13) 0.0449(8) Uani 1 1 d . . . N2B N 0.66236(15) 0.0270(2) 0.66082(13) 0.0417(7) Uani 1 1 d . . . N3B N 0.68432(16) -0.0127(3) 0.60938(13) 0.0443(7) Uani 1 1 d . . . H3BB H 0.7118 0.0203 0.5888 0.053 Uiso 1 1 calc R . . N1C N 0.63992(18) 0.3362(3) 0.75425(15) 0.0528(9) Uani 1 1 d . . . N2C N 0.59027(16) 0.2519(3) 0.65265(15) 0.0456(7) Uani 1 1 d . . . N3C N 0.56122(16) 0.2360(3) 0.59890(15) 0.0504(8) Uani 1 1 d . . . H3CB H 0.5636 0.1761 0.5790 0.060 Uiso 1 1 calc R . . C1A C 0.7272(2) 0.1557(4) 0.86598(18) 0.0659(14) Uani 1 1 d . . . H1AA H 0.7267 0.1196 0.9047 0.079 Uiso 1 1 calc R . . H1AB H 0.7520 0.2218 0.8708 0.079 Uiso 1 1 calc R . . C2A C 0.7567(2) 0.0819(4) 0.82152(19) 0.0619(12) Uani 1 1 d . . . H2AA H 0.8005 0.0690 0.8336 0.074 Uiso 1 1 calc R . . H2AB H 0.7350 0.0123 0.8201 0.074 Uiso 1 1 calc R . . C3A C 0.8017(2) 0.1656(4) 0.73871(18) 0.0528(10) Uani 1 1 d . . . H3AA H 0.8411 0.1520 0.7571 0.063 Uiso 1 1 calc R . . C4A C 0.7960(2) 0.2245(4) 0.68233(18) 0.0484(9) Uani 1 1 d . . . C5A C 0.8400(2) 0.2622(4) 0.6432(2) 0.0639(12) Uani 1 1 d . . . H5AA H 0.8836 0.2558 0.6481 0.077 Uiso 1 1 calc R . . C6A C 0.8075(2) 0.3102(4) 0.59648(19) 0.0596(11) Uani 1 1 d . . . C7A C 0.8284(3) 0.3602(5) 0.5392(2) 0.0822(17) Uani 1 1 d . . . H7AA H 0.8090 0.4304 0.5336 0.123 Uiso 1 1 calc R . . H7AB H 0.8162 0.3137 0.5060 0.123 Uiso 1 1 calc R . . H7AC H 0.8734 0.3684 0.5413 0.123 Uiso 1 1 calc R . . C1B C 0.6160(2) 0.1015(5) 0.86220(18) 0.0664(14) Uani 1 1 d . . . H1BA H 0.5970 0.1236 0.8990 0.080 Uiso 1 1 calc R . . H1BB H 0.6368 0.0320 0.8694 0.080 Uiso 1 1 calc R . . C2B C 0.5659(2) 0.0888(4) 0.81339(18) 0.0598(12) Uani 1 1 d . . . H2BA H 0.5383 0.0288 0.8227 0.072 Uiso 1 1 calc R . . H2BB H 0.5408 0.1548 0.8100 0.072 Uiso 1 1 calc R . . C3B C 0.5884(2) -0.0257(4) 0.73223(18) 0.0495(10) Uani 1 1 d . . . H3BA H 0.5625 -0.0778 0.7487 0.059 Uiso 1 1 calc R . . C4B C 0.62157(19) -0.0488(3) 0.67776(17) 0.0428(9) Uani 1 1 d . . . C5B C 0.6180(2) -0.1348(3) 0.63733(18) 0.0508(10) Uani 1 1 d . . . H5BA H 0.5930 -0.1969 0.6394 0.061 Uiso 1 1 calc R . . C6B C 0.6586(2) -0.1094(3) 0.59384(16) 0.0465(9) Uani 1 1 d . . . C7B C 0.6751(3) -0.1641(4) 0.53676(19) 0.0656(13) Uani 1 1 d . . . H7BA H 0.6445 -0.1451 0.5054 0.098 Uiso 1 1 calc R . . H7BB H 0.6752 -0.2417 0.5424 0.098 Uiso 1 1 calc R . . H7BC H 0.7161 -0.1406 0.5257 0.098 Uiso 1 1 calc R . . C1C C 0.6438(3) 0.2941(4) 0.8605(2) 0.0693(14) Uani 1 1 d . . . H1CA H 0.6621 0.3144 0.8996 0.083 Uiso 1 1 calc R . . H1CB H 0.5983 0.2969 0.8624 0.083 Uiso 1 1 calc R . . C2C C 0.6650(3) 0.3748(4) 0.8132(2) 0.0731(15) Uani 1 1 d . . . H2CA H 0.6491 0.4472 0.8214 0.088 Uiso 1 1 calc R . . H2CB H 0.7107 0.3781 0.8138 0.088 Uiso 1 1 calc R . . C3C C 0.6004(2) 0.3937(4) 0.7256(2) 0.0609(12) Uani 1 1 d . . . H3CA H 0.5881 0.4609 0.7405 0.073 Uiso 1 1 calc R . . C4C C 0.5737(2) 0.3532(3) 0.6681(2) 0.0512(10) Uani 1 1 d . . . C5C C 0.5353(2) 0.4001(4) 0.6232(2) 0.0676(13) Uani 1 1 d . . . H5CA H 0.5181 0.4699 0.6233 0.081 Uiso 1 1 calc R . . C6C C 0.5276(2) 0.3235(4) 0.5789(2) 0.0608(11) Uani 1 1 d . . . C7C C 0.4937(3) 0.3265(5) 0.5186(3) 0.0838(17) Uani 1 1 d . . . H7CA H 0.5178 0.2878 0.4900 0.126 Uiso 1 1 calc R . . H7CB H 0.4884 0.4009 0.5059 0.126 Uiso 1 1 calc R . . H7CC H 0.4531 0.2927 0.5211 0.126 Uiso 1 1 calc R . . B1 B 0.83638(11) 0.03383(19) 0.51703(10) 0.0701(16) Uani 1 1 d D . . F11 F 0.79010(14) 0.0571(3) 0.55325(15) 0.1255(15) Uani 1 1 d D . . F12 F 0.8237(2) -0.0598(3) 0.48873(18) 0.171(2) Uani 1 1 d D . . F13 F 0.89038(14) 0.0245(3) 0.54935(14) 0.1254(15) Uani 1 1 d D . . F14 F 0.84132(14) 0.1135(3) 0.47693(14) 0.1069(13) Uani 1 1 d D . . B2 B 0.5000 0.0000 0.5000 0.111(5) Uani 1 2 d SD . . F21 F 0.5526(2) 0.0369(5) 0.5278(3) 0.089(2) Uani 0.50 1 d PD . . F22 F 0.4892(3) -0.1017(3) 0.5177(4) 0.42(2) Uani 0.50 1 d PD . . F23 F 0.4519(2) 0.0633(6) 0.5137(4) 0.132(3) Uani 0.50 1 d PD . . F24 F 0.5065(3) 0.0017(8) 0.44092(9) 0.348(17) Uani 0.50 1 d PD . . B3 B 0.5000 0.6717(4) 0.7500 0.082(3) Uani 1 2 d SD . . F31 F 0.4719(4) 0.6000(6) 0.7127(4) 0.143(4) Uani 0.50 1 d PD . . F32 F 0.4996(4) 0.7696(4) 0.7242(3) 0.213(9) Uani 0.50 1 d PD . . F33 F 0.4689(5) 0.6764(8) 0.8004(3) 0.283(12) Uani 0.50 1 d PD . . F34 F 0.55905(16) 0.6405(8) 0.7625(5) 0.284(13) Uani 0.50 1 d PD . . 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 Fe 0.0404(3) 0.0377(3) 0.0434(3) -0.0014(3) 0.0052(2) -0.0012(3) N 0.057(2) 0.066(2) 0.0420(16) -0.0075(17) 0.0025(15) -0.008(2) N1A 0.0465(19) 0.053(2) 0.0453(17) -0.0005(15) 0.0007(14) 0.0037(16) N2A 0.0446(18) 0.0451(19) 0.0471(17) 0.0033(14) 0.0061(14) -0.0034(15) N3A 0.057(2) 0.050(2) 0.0480(17) 0.0039(15) 0.0059(15) -0.0047(16) N1B 0.0424(18) 0.057(2) 0.0356(15) -0.0028(14) 0.0054(13) -0.0068(16) N2B 0.0470(18) 0.0352(17) 0.0436(15) -0.0032(13) 0.0087(14) -0.0057(14) N3B 0.0464(19) 0.0468(19) 0.0402(15) 0.0002(14) 0.0061(13) 0.0049(15) N1C 0.064(2) 0.044(2) 0.0508(18) -0.0041(16) 0.0054(16) -0.0018(17) N2C 0.0439(19) 0.0408(18) 0.0524(17) -0.0014(15) 0.0048(15) 0.0023(14) N3C 0.047(2) 0.051(2) 0.0539(19) -0.0006(16) 0.0034(15) -0.0028(16) C1A 0.069(3) 0.089(4) 0.0384(19) 0.005(2) -0.005(2) -0.003(3) C2A 0.057(3) 0.074(3) 0.053(2) 0.008(2) -0.002(2) 0.002(2) C3A 0.046(2) 0.059(3) 0.053(2) 0.002(2) -0.0011(18) 0.007(2) C4A 0.044(2) 0.051(2) 0.050(2) -0.0058(18) 0.0057(17) -0.0092(18) C5A 0.054(3) 0.069(3) 0.071(3) -0.008(2) 0.020(2) -0.009(2) C6A 0.073(3) 0.053(3) 0.054(2) -0.006(2) 0.018(2) -0.018(2) C7A 0.104(5) 0.078(4) 0.068(3) 0.009(3) 0.031(3) -0.023(3) C1B 0.080(3) 0.086(4) 0.0341(19) -0.003(2) 0.014(2) -0.007(3) C2B 0.057(3) 0.075(3) 0.049(2) -0.003(2) 0.017(2) -0.008(2) C3B 0.047(2) 0.053(3) 0.049(2) 0.0058(19) 0.0093(18) -0.0143(19) C4B 0.047(2) 0.037(2) 0.0448(19) 0.0028(16) 0.0020(16) -0.0031(16) C5B 0.062(3) 0.038(2) 0.052(2) 0.0003(17) 0.0006(19) -0.0056(19) C6B 0.053(2) 0.045(2) 0.0409(18) -0.0030(16) -0.0041(17) 0.0072(18) C7B 0.080(3) 0.067(3) 0.049(2) -0.020(2) -0.004(2) 0.008(3) C1C 0.079(4) 0.077(4) 0.052(2) -0.021(2) 0.009(2) -0.002(3) C2C 0.092(4) 0.067(3) 0.060(3) -0.025(2) -0.002(3) -0.009(3) C3C 0.068(3) 0.039(2) 0.077(3) -0.009(2) 0.015(2) 0.005(2) C4C 0.046(2) 0.045(2) 0.063(2) 0.0035(19) 0.0089(19) 0.0050(18) C5C 0.057(3) 0.054(3) 0.091(3) 0.007(3) 0.002(3) 0.009(2) C6C 0.046(2) 0.068(3) 0.069(3) 0.019(3) 0.0059(19) 0.001(2) C7C 0.067(3) 0.097(4) 0.086(4) 0.028(3) -0.012(3) 0.001(3) B1 0.061(4) 0.075(4) 0.075(4) 0.006(3) 0.017(3) 0.002(3) F11 0.098(3) 0.149(4) 0.134(3) -0.006(3) 0.058(3) -0.028(3) F12 0.218(6) 0.092(3) 0.203(5) -0.063(3) 0.004(5) -0.016(4) F13 0.089(3) 0.158(4) 0.127(3) 0.036(3) -0.012(2) 0.002(3) F14 0.079(2) 0.115(3) 0.127(3) 0.064(2) 0.014(2) 0.013(2) B2 0.057(6) 0.095(9) 0.178(14) -0.074(9) -0.016(7) 0.004(6) F21 0.076(4) 0.087(5) 0.100(5) -0.004(4) -0.023(4) -0.009(4) F22 0.21(2) 0.145(14) 0.88(7) -0.11(2) -0.10(3) -0.083(14) F23 0.143(8) 0.116(7) 0.142(7) 0.008(6) 0.074(6) 0.047(6) F24 0.126(10) 0.78(5) 0.128(9) -0.211(18) -0.035(8) 0.155(17) B3 0.054(5) 0.052(5) 0.142(9) 0.000 0.025(5) 0.000 F31 0.104(7) 0.104(7) 0.217(10) 0.008(7) -0.036(7) -0.048(6) F32 0.246(12) 0.056(4) 0.36(2) -0.015(7) 0.241(15) -0.020(7) F33 0.29(2) 0.42(3) 0.144(10) 0.027(14) 0.080(12) 0.21(2) F34 0.026(4) 0.159(12) 0.67(4) -0.160(17) 0.036(10) 0.017(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 Fe N1C 2.175(4) . ? Fe N1B 2.178(3) . ? Fe N1A 2.186(3) . ? Fe N2B 2.232(3) . ? Fe N2A 2.235(3) . ? Fe N2C 2.245(3) . ? N C1A 1.455(6) . ? N C1C 1.456(6) . ? N C1B 1.476(6) . ? N1A C3A 1.260(5) . ? N1A C2A 1.458(5) . ? N2A C4A 1.337(5) . ? N2A N3A 1.348(4) . ? N3A C6A 1.353(6) . ? N3A H3AB 0.8600 . ? N1B C3B 1.271(5) . ? N1B C2B 1.468(5) . ? N2B C4B 1.336(5) . ? N2B N3B 1.349(4) . ? N3B C6B 1.343(5) . ? N3B H3BB 0.8600 . ? N1C C3C 1.249(6) . ? N1C C2C 1.473(5) . ? N2C N3C 1.336(5) . ? N2C C4C 1.340(5) . ? N3C C6C 1.352(6) . ? N3C H3CB 0.8600 . ? C1A C2A 1.500(7) . ? C1A H1AA 0.9700 . ? C1A H1AB 0.9700 . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C3A C4A 1.449(6) . ? C3A H3AA 0.9300 . ? C4A C5A 1.387(6) . ? C5A C6A 1.357(7) . ? C5A H5AA 0.9300 . ? C6A C7A 1.502(6) . ? C7A H7AA 0.9600 . ? C7A H7AB 0.9600 . ? C7A H7AC 0.9600 . ? C1B C2B 1.495(6) . ? C1B H1BA 0.9700 . ? C1B H1BB 0.9700 . ? C2B H2BA 0.9700 . ? C2B H2BB 0.9700 . ? C3B C4B 1.459(6) . ? C3B H3BA 0.9300 . ? C4B C5B 1.387(5) . ? C5B C6B 1.364(6) . ? C5B H5BA 0.9300 . ? C6B C7B 1.494(5) . ? C7B H7BA 0.9600 . ? C7B H7BB 0.9600 . ? C7B H7BC 0.9600 . ? C1C C2C 1.529(7) . ? C1C H1CA 0.9700 . ? C1C H1CB 0.9700 . ? C2C H2CA 0.9700 . ? C2C H2CB 0.9700 . ? C3C C4C 1.465(6) . ? C3C H3CA 0.9300 . ? C4C C5C 1.386(6) . ? C5C C6C 1.369(7) . ? C5C H5CA 0.9300 . ? C6C C7C 1.495(7) . ? C7C H7CA 0.9600 . ? C7C H7CB 0.9600 . ? C7C H7CC 0.9600 . ? B1 F12 1.3308(17) . ? B1 F14 1.3310(17) . ? B1 F13 1.3311(17) . ? B1 F11 1.3318(17) . ? B2 F24 1.3302(18) 5_656 ? B2 F24 1.3302(18) . ? B2 F22 1.3305(18) . ? B2 F22 1.3305(18) 5_656 ? B2 F23 1.3307(17) . ? B2 F23 1.3307(17) 5_656 ? B2 F21 1.3317(17) . ? B2 F21 1.3317(17) 5_656 ? B3 F34 1.3285(17) 2_656 ? B3 F34 1.3285(17) . ? B3 F33 1.3309(18) . ? B3 F33 1.3309(18) 2_656 ? B3 F32 1.3311(18) . ? B3 F32 1.3311(18) 2_656 ? B3 F31 1.3326(18) . ? B3 F31 1.3326(18) 2_656 ? 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 N1C Fe N1B 103.79(13) . . ? N1C Fe N1A 104.48(14) . . ? N1B Fe N1A 103.12(13) . . ? N1C Fe N2B 163.44(13) . . ? N1B Fe N2B 74.16(12) . . ? N1A Fe N2B 91.91(13) . . ? N1C Fe N2A 92.72(13) . . ? N1B Fe N2A 163.37(13) . . ? N1A Fe N2A 74.08(13) . . ? N2B Fe N2A 89.45(12) . . ? N1C Fe N2C 74.04(13) . . ? N1B Fe N2C 93.96(12) . . ? N1A Fe N2C 162.61(13) . . ? N2B Fe N2C 89.61(12) . . ? N2A Fe N2C 88.62(12) . . ? C1A N C1C 114.7(4) . . ? C1A N C1B 113.4(4) . . ? C1C N C1B 112.2(4) . . ? C3A N1A C2A 119.8(4) . . ? C3A N1A Fe 116.7(3) . . ? C2A N1A Fe 123.0(3) . . ? C4A N2A N3A 104.3(3) . . ? C4A N2A Fe 113.3(3) . . ? N3A N2A Fe 142.0(3) . . ? N2A N3A C6A 112.9(4) . . ? N2A N3A H3AB 123.5 . . ? C6A N3A H3AB 123.5 . . ? C3B N1B C2B 118.6(4) . . ? C3B N1B Fe 117.1(3) . . ? C2B N1B Fe 123.8(3) . . ? C4B N2B N3B 104.1(3) . . ? C4B N2B Fe 113.8(2) . . ? N3B N2B Fe 141.5(2) . . ? C6B N3B N2B 112.7(3) . . ? C6B N3B H3BB 123.7 . . ? N2B N3B H3BB 123.7 . . ? C3C N1C C2C 118.8(4) . . ? C3C N1C Fe 117.7(3) . . ? C2C N1C Fe 123.4(3) . . ? N3C N2C C4C 104.4(3) . . ? N3C N2C Fe 142.0(3) . . ? C4C N2C Fe 113.1(3) . . ? N2C N3C C6C 113.3(4) . . ? N2C N3C H3CB 123.4 . . ? C6C N3C H3CB 123.4 . . ? N C1A C2A 110.6(4) . . ? N C1A H1AA 109.5 . . ? C2A C1A H1AA 109.5 . . ? N C1A H1AB 109.5 . . ? C2A C1A H1AB 109.5 . . ? H1AA C1A H1AB 108.1 . . ? N1A C2A C1A 109.0(4) . . ? N1A C2A H2AA 109.9 . . ? C1A C2A H2AA 109.9 . . ? N1A C2A H2AB 109.9 . . ? C1A C2A H2AB 109.9 . . ? H2AA C2A H2AB 108.3 . . ? N1A C3A C4A 118.9(4) . . ? N1A C3A H3AA 120.5 . . ? C4A C3A H3AA 120.5 . . ? N2A C4A C5A 110.4(4) . . ? N2A C4A C3A 116.7(4) . . ? C5A C4A C3A 132.8(4) . . ? C6A C5A C4A 107.0(4) . . ? C6A C5A H5AA 126.5 . . ? C4A C5A H5AA 126.5 . . ? N3A C6A C5A 105.3(4) . . ? N3A C6A C7A 122.5(5) . . ? C5A C6A C7A 132.0(5) . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? N C1B C2B 111.0(4) . . ? N C1B H1BA 109.4 . . ? C2B C1B H1BA 109.4 . . ? N C1B H1BB 109.4 . . ? C2B C1B H1BB 109.4 . . ? H1BA C1B H1BB 108.0 . . ? N1B C2B C1B 108.9(4) . . ? N1B C2B H2BA 109.9 . . ? C1B C2B H2BA 109.9 . . ? N1B C2B H2BB 109.9 . . ? C1B C2B H2BB 109.9 . . ? H2BA C2B H2BB 108.3 . . ? N1B C3B C4B 118.2(4) . . ? N1B C3B H3BA 120.9 . . ? C4B C3B H3BA 120.9 . . ? N2B C4B C5B 111.2(3) . . ? N2B C4B C3B 116.4(3) . . ? C5B C4B C3B 132.3(4) . . ? C6B C5B C4B 105.7(4) . . ? C6B C5B H5BA 127.2 . . ? C4B C5B H5BA 127.2 . . ? N3B C6B C5B 106.3(3) . . ? N3B C6B C7B 120.5(4) . . ? C5B C6B C7B 133.1(4) . . ? C6B C7B H7BA 109.5 . . ? C6B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C6B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N C1C C2C 110.6(4) . . ? N C1C H1CA 109.5 . . ? C2C C1C H1CA 109.5 . . ? N C1C H1CB 109.5 . . ? C2C C1C H1CB 109.5 . . ? H1CA C1C H1CB 108.1 . . ? N1C C2C C1C 107.5(4) . . ? N1C C2C H2CA 110.2 . . ? C1C C2C H2CA 110.2 . . ? N1C C2C H2CB 110.2 . . ? C1C C2C H2CB 110.2 . . ? H2CA C2C H2CB 108.5 . . ? N1C C3C C4C 118.7(4) . . ? N1C C3C H3CA 120.7 . . ? C4C C3C H3CA 120.7 . . ? N2C C4C C5C 110.7(4) . . ? N2C C4C C3C 116.3(4) . . ? C5C C4C C3C 132.9(4) . . ? C6C C5C C4C 106.3(4) . . ? C6C C5C H5CA 126.8 . . ? C4C C5C H5CA 126.8 . . ? N3C C6C C5C 105.2(4) . . ? N3C C6C C7C 122.8(5) . . ? C5C C6C C7C 131.9(5) . . ? C6C C7C H7CA 109.5 . . ? C6C C7C H7CB 109.5 . . ? H7CA C7C H7CB 109.5 . . ? C6C C7C H7CC 109.5 . . ? H7CA C7C H7CC 109.5 . . ? H7CB C7C H7CC 109.5 . . ? F12 B1 F14 109.57(9) . . ? F12 B1 F13 109.46(9) . . ? F14 B1 F13 109.48(9) . . ? F12 B1 F11 109.44(9) . . ? F14 B1 F11 109.44(9) . . ? F13 B1 F11 109.43(9) . . ? F24 B2 F22 109.56(9) . . ? F24 B2 F22 109.56(9) 5_656 5_656 ? F24 B2 F23 109.53(9) . . ? F22 B2 F23 109.50(9) . . ? F24 B2 F23 109.53(9) 5_656 5_656 ? F22 B2 F23 109.50(9) 5_656 5_656 ? F24 B2 F21 109.40(9) . . ? F22 B2 F21 109.43(9) . . ? F23 B2 F21 109.41(9) . . ? F24 B2 F21 109.40(9) 5_656 5_656 ? F22 B2 F21 109.43(9) 5_656 5_656 ? F23 B2 F21 109.41(9) 5_656 5_656 ? F34 B3 F33 109.65(9) . . ? F34 B3 F33 109.65(9) 2_656 2_656 ? F34 B3 F32 109.65(9) . . ? F33 B3 F32 109.43(9) . . ? F34 B3 F32 109.65(9) 2_656 2_656 ? F33 B3 F32 109.43(9) 2_656 2_656 ? F34 B3 F31 109.47(9) . . ? F33 B3 F31 109.29(9) . . ? F32 B3 F31 109.33(9) . . ? F34 B3 F31 109.47(9) 2_656 2_656 ? F33 B3 F31 109.29(9) 2_656 2_656 ? F32 B3 F31 109.33(9) 2_656 2_656 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3A H3AB F14 0.86 1.96 2.812(4) 169.1 7_656 N3B H3BB F11 0.86 1.93 2.759(4) 161.6 . N3C H3CB F21 0.86 2.06 2.911(7) 169.8 . N3C H3CB F22 0.86 2.55 3.217(10) 134.9 5_656 C3A H3AA F34 0.93 2.19 2.977(6) 141.7 4_646 C3B H3BA F32 0.93 2.35 3.139(8) 142.7 1_545 C3B H3BA F32 0.93 2.38 3.303(7) 169.8 2_646 C3C H3CA F31 0.93 2.40 3.292(9) 161.6 2_656 C3C H3CA F34 0.93 2.34 3.266(9) 170.9 . _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.825 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.090 data_1955 _database_code_depnum_ccdc_archive 'CCDC 785614' #TrackingRef '1955.cif' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Cobalt Manganese complex ; _chemical_name_common 'Cobalt Manganese complex' _chemical_formula_moiety 'C21 H30 Mn N10, C21 H27 Co N10, 2(Cl O4), 0.66(H2 O)' _chemical_formula_sum 'C42 H58.30 Cl2 Co Mn N20 O8.65' _chemical_formula_weight 1166.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 21.327(4) _cell_length_b 12.677(2) _cell_length_c 20.069(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.904(3) _cell_angle_gamma 90.00 _cell_volume 5419.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10261 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 24.5 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.375 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2422 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.776 _exptl_absorpt_correction_T_max 0.912 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'three-circle diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 11.198 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28552 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9454 _reflns_number_gt 7067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker, 2004)' _computing_publication_material SHELXL-97 _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. Merohedral/racemic twin in a 0.55:0.45 ratio. Two independent perchlorate ions disordered near the same position and therefore theri geometry and adp's were restrained to be similar. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+19.P], P=(max(Fo^2^,0)+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_abs_structure_details '(Flack, 1983)' _refine_ls_abs_structure_Flack 0.43(3) _refine_ls_number_reflns 9454 # 4772 w/o Fiedel pairs _refine_ls_number_parameters 736 _refine_ls_number_restraints 317 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.1077 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.69204(4) 0.62728(7) 0.50481(4) 0.0525(2) Uani 1 1 d . . . N1A N 0.8409(4) 0.6402(6) 0.5631(4) 0.085(2) Uani 1 1 d . . . C11A C 0.8366(4) 0.7518(9) 0.5837(6) 0.096(3) Uani 1 1 d . . . H11A H 0.8745 0.7882 0.5720 0.115 Uiso 1 1 calc R . . H11B H 0.8343 0.7550 0.6318 0.115 Uiso 1 1 calc R . . C12A C 0.7814(5) 0.8074(7) 0.5522(6) 0.090(3) Uani 1 1 d . . . H12A H 0.7780 0.8766 0.5723 0.108 Uiso 1 1 calc R . . H12B H 0.7879 0.8173 0.5051 0.108 Uiso 1 1 calc R . . C13A C 0.6842(4) 0.7774(6) 0.6027(4) 0.065(2) Uani 1 1 d . . . H13A H 0.6925 0.8354 0.6301 0.078 Uiso 1 1 calc R . . C14A C 0.6289(4) 0.7190(7) 0.6084(4) 0.059(2) Uani 1 1 d . . . C15A C 0.5810(5) 0.7098(8) 0.6538(4) 0.079(3) Uani 1 1 d . . . H15A H 0.5749 0.7509 0.6913 0.095 Uiso 1 1 calc R . . C16A C 0.5451(5) 0.6262(7) 0.6301(4) 0.076(2) Uani 1 1 d . . . C17A C 0.4882(5) 0.5802(10) 0.6565(6) 0.110(4) Uani 1 1 d . . . H17A H 0.4669 0.6327 0.6813 0.165 Uiso 1 1 calc R . . H17B H 0.4995 0.5219 0.6852 0.165 Uiso 1 1 calc R . . H17C H 0.4609 0.5559 0.6201 0.165 Uiso 1 1 calc R . . N11A N 0.7230(3) 0.7501(5) 0.5595(4) 0.0610(18) Uani 1 1 d . . . N12A N 0.6208(4) 0.6431(5) 0.5623(4) 0.0640(19) Uani 1 1 d . . . N13A N 0.5721(3) 0.5829(5) 0.5739(3) 0.0654(17) Uani 1 1 d . . . C21A C 0.8345(4) 0.5595(10) 0.6131(6) 0.096(3) Uani 1 1 d . . . H21A H 0.8583 0.5804 0.6534 0.115 Uiso 1 1 calc R . . H21B H 0.8526 0.4945 0.5974 0.115 Uiso 1 1 calc R . . C22A C 0.7663(4) 0.5386(8) 0.6301(5) 0.078(2) Uani 1 1 d . . . H22A H 0.7646 0.4774 0.6591 0.093 Uiso 1 1 calc R . . H22B H 0.7502 0.5987 0.6537 0.093 Uiso 1 1 calc R . . C23A C 0.7127(4) 0.4261(8) 0.5554(4) 0.065(2) Uani 1 1 d . . . H23A H 0.7249 0.3704 0.5833 0.078 Uiso 1 1 calc R . . C24A C 0.6753(4) 0.4099(6) 0.4929(4) 0.061(2) Uani 1 1 d . . . C25A C 0.6581(4) 0.3272(7) 0.4531(5) 0.073(2) Uani 1 1 d . . . H25A H 0.6627 0.2555 0.4618 0.088 Uiso 1 1 calc R . . C26A C 0.6315(4) 0.3768(7) 0.3953(4) 0.070(2) Uani 1 1 d . . . C27A C 0.6048(5) 0.3269(8) 0.3319(6) 0.111(4) Uani 1 1 d . . . H27A H 0.5752 0.3742 0.3101 0.167 Uiso 1 1 calc R . . H27B H 0.5840 0.2622 0.3424 0.167 Uiso 1 1 calc R . . H27C H 0.6381 0.3123 0.3029 0.167 Uiso 1 1 calc R . . N21A N 0.7274(3) 0.5199(6) 0.5689(3) 0.0594(17) Uani 1 1 d . . . N22A N 0.6590(3) 0.4995(6) 0.4609(3) 0.0613(17) Uani 1 1 d . . . N23A N 0.6331(3) 0.4819(5) 0.4014(3) 0.0687(17) Uani 1 1 d . . . C3A C 0.8673(4) 0.6171(9) 0.5036(6) 0.082(3) Uani 1 1 d . . . H31A H 0.9040 0.5729 0.5122 0.099 Uiso 1 1 calc R . . H31B H 0.8810 0.6821 0.4833 0.099 Uiso 1 1 calc R . . C32A C 0.8213(5) 0.5607(8) 0.4553(5) 0.083(3) Uani 1 1 d . . . H32A H 0.8402 0.5507 0.4128 0.100 Uiso 1 1 calc R . . H32B H 0.8114 0.4917 0.4729 0.100 Uiso 1 1 calc R . . C33A C 0.7548(4) 0.6789(8) 0.3917(5) 0.076(3) Uani 1 1 d . . . H33A H 0.7826 0.6784 0.3575 0.091 Uiso 1 1 calc R . . C34A C 0.6998(4) 0.7404(7) 0.3895(4) 0.074(2) Uani 1 1 d U . . C35A C 0.6755(6) 0.8279(8) 0.3503(6) 0.106(3) Uani 1 1 d U . . H35A H 0.6912 0.8578 0.3123 0.127 Uiso 1 1 calc R . . C36A C 0.6221(4) 0.8565(7) 0.3843(5) 0.086(2) Uani 1 1 d U . . C37A C 0.5775(5) 0.9481(7) 0.3653(6) 0.147(5) Uani 1 1 d . . . H37A H 0.5927 1.0117 0.3866 0.221 Uiso 1 1 calc R . . H37B H 0.5363 0.9324 0.3796 0.221 Uiso 1 1 calc R . . H37C H 0.5758 0.9576 0.3178 0.221 Uiso 1 1 calc R . . N31A N 0.7633(3) 0.6233(5) 0.4455(4) 0.0637(19) Uani 1 1 d . . . N32A N 0.6619(3) 0.7249(5) 0.4380(4) 0.0710(19) Uani 1 1 d U . . N33A N 0.6145(3) 0.7964(5) 0.4383(3) 0.0780(17) Uani 1 1 d U . . Mn1 Mn 0.43096(4) 0.62798(8) 0.38915(4) 0.0518(3) Uani 1 1 d . . . N1B N 0.2932(4) 0.6358(7) 0.3228(4) 0.084(2) Uani 1 1 d . . . C11B C 0.2939(4) 0.5433(10) 0.2814(5) 0.097(3) Uani 1 1 d . . . H11C H 0.2671 0.5550 0.2417 0.116 Uiso 1 1 calc R . . H11D H 0.2769 0.4843 0.3054 0.116 Uiso 1 1 calc R . . C12B C 0.3594(4) 0.5151(10) 0.2610(5) 0.099(4) Uani 1 1 d . . . H12C H 0.3580 0.4511 0.2344 0.118 Uiso 1 1 calc R . . H12D H 0.3761 0.5715 0.2344 0.118 Uiso 1 1 calc R . . C13B C 0.4169(4) 0.4073(8) 0.3390(5) 0.071(2) Uani 1 1 d . . . H13B H 0.4061 0.3491 0.3126 0.086 Uiso 1 1 calc R . . C14B C 0.4536(4) 0.3932(7) 0.4001(5) 0.069(2) Uani 1 1 d . . . C15B C 0.4738(4) 0.3033(7) 0.4354(5) 0.076(2) Uani 1 1 d . . . H15B H 0.4672 0.2332 0.4232 0.091 Uiso 1 1 calc R . . C16B C 0.5050(4) 0.3398(7) 0.4905(5) 0.075(2) Uani 1 1 d . . . C17B C 0.5348(5) 0.2853(8) 0.5522(5) 0.106(3) Uani 1 1 d . . . H17D H 0.5062 0.2338 0.5682 0.159 Uiso 1 1 calc R . . H17E H 0.5439 0.3368 0.5864 0.159 Uiso 1 1 calc R . . H17F H 0.5729 0.2511 0.5408 0.159 Uiso 1 1 calc R . . N11B N 0.3989(3) 0.4996(6) 0.3206(3) 0.0657(19) Uani 1 1 d . . . N12B N 0.4724(4) 0.4836(6) 0.4312(4) 0.0692(19) Uani 1 1 d . . . N13B N 0.5047(3) 0.4451(6) 0.4879(3) 0.0708(19) Uani 1 1 d . . . H13C H 0.5227 0.4847 0.5180 0.10(3) Uiso 1 1 calc R . . C21B C 0.2926(5) 0.7349(9) 0.2922(6) 0.098(3) Uani 1 1 d . . . H21C H 0.2511 0.7653 0.2942 0.118 Uiso 1 1 calc R . . H21D H 0.3014 0.7264 0.2456 0.118 Uiso 1 1 calc R . . C22B C 0.3415(4) 0.8118(8) 0.3255(6) 0.098(3) Uani 1 1 d . . . H22C H 0.3420 0.8777 0.3009 0.118 Uiso 1 1 calc R . . H22D H 0.3309 0.8269 0.3710 0.118 Uiso 1 1 calc R . . C23B C 0.4408(4) 0.7915(7) 0.2818(5) 0.071(2) Uani 1 1 d . . . H23B H 0.4321 0.8490 0.2540 0.085 Uiso 1 1 calc R . . C24B C 0.4999(4) 0.7305(7) 0.2787(4) 0.068(2) Uani 1 1 d . . . C25B C 0.5488(4) 0.7330(8) 0.2362(4) 0.077(2) Uani 1 1 d . . . H25B H 0.5534 0.7782 0.2003 0.093 Uiso 1 1 calc R . . C26B C 0.5886(5) 0.6558(10) 0.2579(5) 0.092(3) Uani 1 1 d . . . C27B C 0.6487(6) 0.6125(12) 0.2320(6) 0.130(5) Uani 1 1 d . . . H27D H 0.6413 0.5900 0.1866 0.195 Uiso 1 1 calc R . . H27E H 0.6626 0.5536 0.2589 0.195 Uiso 1 1 calc R . . H27F H 0.6803 0.6665 0.2341 0.195 Uiso 1 1 calc R . . N21B N 0.4023(3) 0.7609(6) 0.3249(4) 0.0689(19) Uani 1 1 d . . . N22B N 0.5104(3) 0.6607(6) 0.3289(3) 0.0637(17) Uani 1 1 d . . . N23B N 0.5671(3) 0.6191(5) 0.3137(3) 0.0702(19) Uani 1 1 d . . . H23C H 0.5868 0.5731 0.3383 0.048(17) Uiso 1 1 calc R . . C31B C 0.2571(5) 0.6225(9) 0.3832(7) 0.101(4) Uani 1 1 d . . . H31C H 0.2189 0.5837 0.3713 0.121 Uiso 1 1 calc R . . H31D H 0.2450 0.6915 0.3989 0.121 Uiso 1 1 calc R . . C32B C 0.2927(5) 0.5650(10) 0.4395(5) 0.092(3) Uani 1 1 d . . . H32C H 0.2675 0.5623 0.4784 0.111 Uiso 1 1 calc R . . H32D H 0.3016 0.4933 0.4261 0.111 Uiso 1 1 calc R . . C33B C 0.3553(5) 0.6786(8) 0.5072(5) 0.083(3) Uani 1 1 d . . . H33B H 0.3227 0.6814 0.5362 0.100 Uiso 1 1 calc R . . C34B C 0.4110(4) 0.7399(8) 0.5212(5) 0.079(2) Uani 1 1 d . . . C35B C 0.4279(5) 0.8148(8) 0.5684(5) 0.096(3) Uani 1 1 d . . . H35B H 0.4049 0.8351 0.6044 0.115 Uiso 1 1 calc R . . C36B C 0.4839(5) 0.8532(6) 0.5527(5) 0.093(3) Uani 1 1 d . . . C37B C 0.5252(5) 0.9419(9) 0.5826(6) 0.142(5) Uani 1 1 d . . . H37D H 0.5385 0.9241 0.6276 0.213 Uiso 1 1 calc R . . H37E H 0.5016 1.0064 0.5825 0.213 Uiso 1 1 calc R . . H37F H 0.5613 0.9508 0.5565 0.213 Uiso 1 1 calc R . . N31B N 0.3501(4) 0.6202(6) 0.4554(4) 0.078(2) Uani 1 1 d . . . N32B N 0.4584(3) 0.7281(6) 0.4768(4) 0.081(2) Uani 1 1 d . . . N33B N 0.5018(3) 0.7977(5) 0.4991(4) 0.081(2) Uani 1 1 d . . . H33C H 0.5373 0.8063 0.4813 0.10(3) Uiso 1 1 calc R . . Cl1 Cl 0.92326(19) 0.6071(2) 0.27210(17) 0.1130(10) Uani 0.627(9) 1 d PDU A 1 O11 O 0.9401(8) 0.5989(14) 0.3399(5) 0.180(5) Uani 0.627(9) 1 d PDU A 1 O12 O 0.8584(5) 0.5806(13) 0.2652(8) 0.177(5) Uani 0.627(9) 1 d PDU A 1 O13 O 0.9519(7) 0.5296(8) 0.2342(7) 0.140(4) Uani 0.627(9) 1 d PDU A 1 O14 O 0.9377(8) 0.7037(7) 0.2454(8) 0.173(5) Uani 0.627(9) 1 d PDU A 1 Cl1A Cl 0.92326(19) 0.6071(2) 0.27210(17) 0.1130(10) Uani 0.373(9) 1 d PD A 2 O11A O 0.9091(16) 0.544(2) 0.2191(9) 0.180(5) Uani 0.373(9) 1 d PDU A 2 O12A O 0.9841(8) 0.654(2) 0.2747(15) 0.177(5) Uani 0.373(9) 1 d PDU A 2 O13A O 0.9265(12) 0.5379(14) 0.3287(8) 0.140(4) Uani 0.373(9) 1 d PDU A 2 O14A O 0.8793(10) 0.6784(14) 0.2965(14) 0.173(5) Uani 0.373(9) 1 d PDU A 2 Cl2 Cl 0.6940(7) 0.9001(12) 0.1149(7) 0.0966(17) Uani 0.455(7) 1 d PDU B 1 O21 O 0.7518(8) 0.847(2) 0.1295(10) 0.169(5) Uani 0.455(7) 1 d PDU B 1 O22 O 0.6797(12) 0.9602(19) 0.1708(11) 0.182(6) Uani 0.455(7) 1 d PDU B 1 O23 O 0.6501(9) 0.8166(11) 0.1172(8) 0.130(4) Uani 0.455(7) 1 d PDU B 1 O24 O 0.6795(10) 0.9475(15) 0.0555(9) 0.160(4) Uani 0.455(7) 1 d PDU B 1 Cl2A Cl 0.7027(6) 0.8906(10) 0.1266(6) 0.0966(17) Uani 0.545(7) 1 d PD B 2 O21A O 0.6501(7) 0.9134(16) 0.1608(9) 0.169(5) Uani 0.545(7) 1 d PDU B 2 O22A O 0.6982(9) 0.8318(14) 0.0694(8) 0.182(6) Uani 0.545(7) 1 d PDU B 2 O23A O 0.7485(7) 0.9664(8) 0.1208(7) 0.130(4) Uani 0.545(7) 1 d PDU B 2 O24A O 0.7393(7) 0.8158(11) 0.1692(8) 0.160(4) Uani 0.545(7) 1 d PDU B 2 O1W O 0.6254(16) 0.083(3) 0.2411(17) 0.140(18) Uani 0.206(18) 1 d PU . . O2W O 0.813(2) 0.699(3) 0.171(2) 0.21(3) Uani 0.26(3) 1 d PU C 1 O3W O 0.797(2) 0.759(4) 0.249(2) 0.17(3) Uani 0.19(3) 1 d PU D 3 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 Co1 0.0561(6) 0.0468(5) 0.0551(6) 0.0007(5) 0.0075(4) -0.0006(5) N1A 0.087(5) 0.080(5) 0.087(6) -0.002(4) 0.006(4) 0.013(4) C11A 0.056(5) 0.115(8) 0.116(8) -0.020(6) -0.008(5) -0.017(5) C12A 0.095(7) 0.058(5) 0.117(7) -0.005(5) 0.009(5) -0.004(5) C13A 0.101(6) 0.038(4) 0.055(4) -0.012(3) -0.010(4) 0.006(4) C14A 0.060(5) 0.069(5) 0.049(4) 0.001(4) 0.003(3) 0.002(4) C15A 0.111(7) 0.085(6) 0.042(4) 0.001(4) 0.015(4) 0.034(5) C16A 0.084(6) 0.093(6) 0.051(5) 0.004(4) 0.014(4) -0.016(5) C17A 0.093(7) 0.142(9) 0.097(7) 0.029(7) 0.031(6) -0.023(6) N11A 0.061(4) 0.046(4) 0.076(4) -0.003(3) 0.003(3) -0.002(3) N12A 0.084(5) 0.061(4) 0.046(4) -0.008(3) 0.003(3) -0.011(3) N13A 0.076(4) 0.079(4) 0.042(3) 0.002(3) 0.008(3) -0.015(3) C21A 0.072(6) 0.106(8) 0.110(8) 0.013(6) -0.003(6) -0.003(5) C22A 0.075(5) 0.091(6) 0.067(5) 0.008(4) -0.005(4) 0.000(5) C23A 0.061(5) 0.079(6) 0.054(5) 0.012(4) 0.002(4) 0.019(4) C24A 0.064(5) 0.056(4) 0.064(5) -0.005(4) 0.007(4) 0.010(4) C25A 0.072(5) 0.059(5) 0.089(6) -0.006(4) 0.015(4) 0.022(4) C26A 0.069(5) 0.086(6) 0.056(5) -0.017(4) 0.014(3) 0.006(4) C27A 0.087(6) 0.113(8) 0.131(9) -0.048(7) -0.014(6) 0.013(6) N21A 0.059(4) 0.065(4) 0.055(4) -0.004(3) 0.004(3) 0.003(3) N22A 0.068(4) 0.073(4) 0.044(4) 0.006(3) 0.010(3) 0.021(3) N23A 0.071(4) 0.078(4) 0.058(4) -0.008(3) 0.010(3) 0.010(3) C3A 0.052(5) 0.094(7) 0.101(8) 0.012(6) 0.014(5) -0.003(5) C32A 0.087(6) 0.072(6) 0.091(7) -0.005(5) 0.018(5) 0.000(5) C33A 0.074(6) 0.079(6) 0.075(6) -0.007(5) 0.006(4) -0.027(5) C34A 0.080(5) 0.058(5) 0.081(6) 0.013(4) -0.015(4) -0.014(4) C35A 0.129(8) 0.079(6) 0.109(7) 0.028(5) 0.001(5) -0.033(6) C36A 0.081(5) 0.071(5) 0.102(6) 0.020(5) -0.018(4) -0.011(4) C37A 0.143(9) 0.058(5) 0.233(13) 0.046(7) -0.065(9) 0.003(6) N31A 0.061(4) 0.048(4) 0.082(5) -0.003(3) -0.006(3) -0.003(3) N32A 0.060(4) 0.046(4) 0.106(5) 0.003(3) -0.001(3) -0.010(3) N33A 0.089(4) 0.047(3) 0.096(4) 0.012(3) -0.011(3) 0.003(3) Mn1 0.0601(7) 0.0443(6) 0.0518(7) -0.0014(5) 0.0115(5) 0.0005(6) N1B 0.081(5) 0.094(6) 0.079(5) -0.023(4) 0.025(4) -0.015(4) C11B 0.064(5) 0.136(9) 0.090(7) -0.046(6) -0.010(5) 0.001(6) C12B 0.070(6) 0.154(10) 0.070(6) -0.028(6) -0.019(5) 0.024(6) C13B 0.064(5) 0.070(5) 0.082(6) -0.022(4) 0.018(4) -0.009(4) C14B 0.076(6) 0.060(5) 0.074(6) -0.011(4) 0.022(5) -0.017(4) C15B 0.078(6) 0.065(5) 0.084(6) 0.015(5) 0.013(5) -0.012(4) C16B 0.083(6) 0.067(5) 0.078(6) 0.016(4) 0.017(4) -0.023(4) C17B 0.118(7) 0.116(8) 0.086(6) 0.046(6) 0.018(5) -0.014(6) N11B 0.053(4) 0.087(5) 0.057(4) -0.015(3) 0.003(3) 0.002(4) N12B 0.077(4) 0.074(5) 0.057(4) 0.007(3) 0.014(3) -0.016(4) N13B 0.078(4) 0.081(5) 0.053(4) 0.004(3) 0.005(3) -0.032(4) C21B 0.070(6) 0.107(8) 0.115(8) 0.022(6) -0.021(5) 0.010(5) C22B 0.067(6) 0.070(6) 0.158(10) 0.018(6) 0.016(6) 0.022(5) C23B 0.062(5) 0.069(5) 0.080(6) 0.018(4) -0.017(4) -0.005(4) C24B 0.084(6) 0.066(5) 0.054(5) 0.019(4) -0.006(4) -0.005(4) C25B 0.073(5) 0.100(6) 0.060(5) 0.016(4) 0.009(4) -0.006(5) C26B 0.089(7) 0.140(9) 0.047(5) 0.000(5) -0.001(4) 0.005(6) C27B 0.100(8) 0.210(13) 0.083(7) -0.005(8) 0.037(6) 0.029(8) N21B 0.068(4) 0.065(4) 0.073(5) 0.005(3) -0.001(4) 0.001(3) N22B 0.068(4) 0.073(4) 0.050(4) 0.002(3) 0.000(3) 0.015(3) N23B 0.072(4) 0.083(5) 0.056(4) 0.004(3) 0.003(3) 0.022(3) C31B 0.064(6) 0.105(9) 0.136(11) -0.023(7) 0.022(6) -0.008(6) C32B 0.076(6) 0.111(8) 0.091(7) -0.004(6) 0.027(5) -0.033(6) C33B 0.087(6) 0.080(6) 0.082(6) -0.013(5) 0.010(5) 0.002(5) C34B 0.078(5) 0.074(5) 0.084(6) -0.017(4) 0.007(4) 0.025(4) C35B 0.094(7) 0.085(6) 0.104(7) -0.037(5) -0.028(5) 0.030(5) C36B 0.098(7) 0.057(5) 0.123(8) -0.020(5) -0.012(6) 0.027(5) C37B 0.120(8) 0.101(7) 0.198(12) -0.049(8) -0.069(8) 0.025(6) N31B 0.079(5) 0.079(5) 0.077(5) -0.006(4) 0.018(4) 0.001(4) N32B 0.067(4) 0.056(4) 0.117(6) -0.008(4) -0.007(4) 0.001(4) N33B 0.066(4) 0.057(4) 0.117(6) -0.010(4) -0.011(4) 0.012(3) Cl1 0.168(3) 0.0651(16) 0.106(2) -0.0109(15) 0.005(2) -0.0135(19) O11 0.265(11) 0.190(10) 0.084(5) -0.033(6) -0.018(7) -0.042(10) O12 0.150(7) 0.186(11) 0.194(10) -0.046(9) -0.002(7) -0.033(7) O13 0.197(9) 0.084(5) 0.140(7) -0.014(6) 0.021(7) 0.000(6) O14 0.238(11) 0.075(5) 0.211(10) 0.008(6) 0.051(9) 0.003(7) Cl1A 0.168(3) 0.0651(16) 0.106(2) -0.0109(15) 0.005(2) -0.0135(19) O11A 0.265(11) 0.190(10) 0.084(5) -0.033(6) -0.018(7) -0.042(10) O12A 0.150(7) 0.186(11) 0.194(10) -0.046(9) -0.002(7) -0.033(7) O13A 0.197(9) 0.084(5) 0.140(7) -0.014(6) 0.021(7) 0.000(6) O14A 0.238(11) 0.075(5) 0.211(10) 0.008(6) 0.051(9) 0.003(7) Cl2 0.128(4) 0.066(2) 0.099(4) -0.008(2) 0.028(3) -0.016(2) O21 0.153(7) 0.226(12) 0.135(8) 0.029(8) 0.066(7) 0.043(7) O22 0.192(10) 0.181(10) 0.172(8) -0.119(8) -0.008(8) -0.001(8) O23 0.197(8) 0.072(5) 0.122(7) -0.005(5) 0.025(7) -0.068(6) O24 0.184(9) 0.139(8) 0.159(7) 0.076(6) 0.017(7) -0.015(7) Cl2A 0.128(4) 0.066(2) 0.099(4) -0.008(2) 0.028(3) -0.016(2) O21A 0.153(7) 0.226(12) 0.135(8) 0.029(8) 0.066(7) 0.043(7) O22A 0.192(10) 0.181(10) 0.172(8) -0.119(8) -0.008(8) -0.001(8) O23A 0.197(8) 0.072(5) 0.122(7) -0.005(5) 0.025(7) -0.068(6) O24A 0.184(9) 0.139(8) 0.159(7) 0.076(6) 0.017(7) -0.015(7) O1W 0.15(2) 0.14(2) 0.13(2) -0.004(16) -0.006(16) 0.005(16) O2W 0.21(3) 0.19(3) 0.23(3) -0.014(18) 0.002(19) 0.009(18) O3W 0.18(3) 0.19(3) 0.14(3) 0.030(18) 0.018(18) 0.000(18) _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 Co1 N32A 1.911(8) . ? Co1 N22A 1.958(8) . ? Co1 N12A 1.964(8) . ? Co1 N31A 1.978(8) . ? Co1 N21A 1.994(7) . ? Co1 N11A 1.997(7) . ? N1A C3A 1.379(13) . ? N1A C21A 1.443(13) . ? N1A C11A 1.478(13) . ? C11A C12A 1.485(14) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C12A N11A 1.456(11) . ? C12A H12A 0.9700 . ? C12A H12B 0.9700 . ? C13A N11A 1.277(10) . ? C13A C14A 1.402(11) . ? C13A H13A 0.9300 . ? C14A N12A 1.340(10) . ? C14A C15A 1.408(11) . ? C15A C16A 1.378(13) . ? C15A H15A 0.9300 . ? C16A N13A 1.405(10) . ? C16A C17A 1.469(13) . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? N12A N13A 1.319(9) . ? C21A C22A 1.533(13) . ? C21A H21A 0.9700 . ? C21A H21B 0.9700 . ? C22A N21A 1.467(11) . ? C22A H22A 0.9700 . ? C22A H22B 0.9700 . ? C23A N21A 1.256(11) . ? C23A C24A 1.467(12) . ? C23A H23A 0.9300 . ? C24A N22A 1.342(10) . ? C24A C25A 1.357(12) . ? C25A C26A 1.414(12) . ? C25A H25A 0.9300 . ? C26A N23A 1.338(10) . ? C26A C27A 1.506(12) . ? C27A H27A 0.9600 . ? C27A H27B 0.9600 . ? C27A H27C 0.9600 . ? N22A N23A 1.309(9) . ? C3A C32A 1.524(14) . ? C3A H31A 0.9700 . ? C3A H31B 0.9700 . ? C32A N31A 1.473(11) . ? C32A H32A 0.9700 . ? C32A H32B 0.9700 . ? C33A N31A 1.295(12) . ? C33A C34A 1.408(13) . ? C33A H33A 0.9300 . ? C34A N32A 1.310(11) . ? C34A C35A 1.441(13) . ? C35A C36A 1.404(14) . ? C35A H35A 0.9300 . ? C36A N33A 1.341(11) . ? C36A C37A 1.538(12) . ? C37A H37A 0.9600 . ? C37A H37B 0.9600 . ? C37A H37C 0.9600 . ? N32A N33A 1.359(9) . ? Mn1 N22B 2.171(7) . ? Mn1 N12B 2.184(8) . ? Mn1 N21B 2.189(7) . ? Mn1 N11B 2.216(7) . ? Mn1 N32B 2.223(8) . ? Mn1 N31B 2.232(8) . ? N1B C21B 1.397(12) . ? N1B C11B 1.438(12) . ? N1B C31B 1.478(14) . ? C11B C12B 1.519(13) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12B N11B 1.442(11) . ? C12B H12C 0.9700 . ? C12B H12D 0.9700 . ? C13B N11B 1.281(12) . ? C13B C14B 1.431(14) . ? C13B H13B 0.9300 . ? C14B N12B 1.357(11) . ? C14B C15B 1.399(13) . ? C15B C16B 1.345(13) . ? C15B H15B 0.9300 . ? C16B N13B 1.336(11) . ? C16B C17B 1.528(13) . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? N12B N13B 1.389(10) . ? N13B H13C 0.8600 . ? C21B C22B 1.553(14) . ? C21B H21C 0.9700 . ? C21B H21D 0.9700 . ? C22B N21B 1.451(11) . ? C22B H22C 0.9700 . ? C22B H22D 0.9700 . ? C23B N21B 1.283(10) . ? C23B C24B 1.484(12) . ? C23B H23B 0.9300 . ? C24B N22B 1.350(11) . ? C24B C25B 1.380(12) . ? C25B C26B 1.352(14) . ? C25B H25B 0.9300 . ? C26B N23B 1.317(11) . ? C26B C27B 1.509(14) . ? C27B H27D 0.9600 . ? C27B H27E 0.9600 . ? C27B H27F 0.9600 . ? N22B N23B 1.368(9) . ? N23B H23C 0.8600 . ? C31B C32B 1.516(16) . ? C31B H31C 0.9700 . ? C31B H31D 0.9700 . ? C32B N31B 1.432(12) . ? C32B H32C 0.9700 . ? C32B H32D 0.9700 . ? C33B N31B 1.278(12) . ? C33B C34B 1.435(13) . ? C33B H33B 0.9300 . ? C34B C35B 1.377(12) . ? C34B N32B 1.388(11) . ? C35B C36B 1.341(13) . ? C35B H35B 0.9300 . ? C36B N33B 1.356(11) . ? C36B C37B 1.533(13) . ? C37B H37D 0.9600 . ? C37B H37E 0.9600 . ? C37B H37F 0.9600 . ? N32B N33B 1.340(9) . ? N33B H33C 0.8600 . ? Cl1 O14 1.378(9) . ? Cl1 O11 1.393(9) . ? Cl1 O13 1.401(9) . ? Cl1 O12 1.422(10) . ? Cl2 O24 1.357(13) . ? Cl2 O22 1.402(13) . ? Cl2 O23 1.416(13) . ? Cl2 O21 1.423(13) . ? Cl2A O22A 1.370(12) . ? Cl2A O21A 1.374(11) . ? Cl2A O23A 1.379(11) . ? Cl2A O24A 1.474(12) . ? 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 N32A Co1 N22A 96.9(3) . . ? N32A Co1 N12A 95.9(3) . . ? N22A Co1 N12A 94.4(3) . . ? N32A Co1 N31A 80.6(3) . . ? N22A Co1 N31A 88.8(3) . . ? N12A Co1 N31A 175.5(3) . . ? N32A Co1 N21A 175.4(3) . . ? N22A Co1 N21A 80.9(3) . . ? N12A Co1 N21A 88.3(3) . . ? N31A Co1 N21A 95.3(3) . . ? N32A Co1 N11A 88.3(3) . . ? N22A Co1 N11A 173.4(3) . . ? N12A Co1 N11A 80.9(3) . . ? N31A Co1 N11A 96.2(3) . . ? N21A Co1 N11A 94.3(3) . . ? C3A N1A C21A 120.6(9) . . ? C3A N1A C11A 118.6(9) . . ? C21A N1A C11A 118.4(9) . . ? N1A C11A C12A 113.3(8) . . ? N1A C11A H11A 108.9 . . ? C12A C11A H11A 108.9 . . ? N1A C11A H11B 108.9 . . ? C12A C11A H11B 108.9 . . ? H11A C11A H11B 107.7 . . ? N11A C12A C11A 112.6(8) . . ? N11A C12A H12A 109.1 . . ? C11A C12A H12A 109.1 . . ? N11A C12A H12B 109.1 . . ? C11A C12A H12B 109.1 . . ? H12A C12A H12B 107.8 . . ? N11A C13A C14A 119.3(7) . . ? N11A C13A H13A 120.4 . . ? C14A C13A H13A 120.4 . . ? N12A C14A C13A 113.7(7) . . ? N12A C14A C15A 108.4(8) . . ? C13A C14A C15A 137.5(8) . . ? C16A C15A C14A 104.4(8) . . ? C16A C15A H15A 127.8 . . ? C14A C15A H15A 127.8 . . ? C15A C16A N13A 109.5(7) . . ? C15A C16A C17A 129.5(9) . . ? N13A C16A C17A 120.9(9) . . ? C16A C17A H17A 109.5 . . ? C16A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C13A N11A C12A 121.3(8) . . ? C13A N11A Co1 112.2(6) . . ? C12A N11A Co1 126.5(6) . . ? N13A N12A C14A 111.6(7) . . ? N13A N12A Co1 133.1(5) . . ? C14A N12A Co1 113.8(6) . . ? N12A N13A C16A 105.9(7) . . ? N1A C21A C22A 113.7(9) . . ? N1A C21A H21A 108.8 . . ? C22A C21A H21A 108.8 . . ? N1A C21A H21B 108.8 . . ? C22A C21A H21B 108.8 . . ? H21A C21A H21B 107.7 . . ? N21A C22A C21A 110.1(8) . . ? N21A C22A H22A 109.6 . . ? C21A C22A H22A 109.6 . . ? N21A C22A H22B 109.6 . . ? C21A C22A H22B 109.6 . . ? H22A C22A H22B 108.2 . . ? N21A C23A C24A 115.9(8) . . ? N21A C23A H23A 122.1 . . ? C24A C23A H23A 122.1 . . ? N22A C24A C25A 108.5(8) . . ? N22A C24A C23A 114.0(8) . . ? C25A C24A C23A 137.0(9) . . ? C24A C25A C26A 103.0(8) . . ? C24A C25A H25A 128.5 . . ? C26A C25A H25A 128.5 . . ? N23A C26A C25A 111.1(7) . . ? N23A C26A C27A 120.2(8) . . ? C25A C26A C27A 128.7(9) . . ? C26A C27A H27A 109.5 . . ? C26A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C26A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C23A N21A C22A 117.2(8) . . ? C23A N21A Co1 115.2(6) . . ? C22A N21A Co1 127.6(6) . . ? N23A N22A C24A 112.2(8) . . ? N23A N22A Co1 132.6(6) . . ? C24A N22A Co1 114.0(6) . . ? N22A N23A C26A 105.2(7) . . ? N1A C3A C32A 111.8(8) . . ? N1A C3A H31A 109.2 . . ? C32A C3A H31A 109.2 . . ? N1A C3A H31B 109.2 . . ? C32A C3A H31B 109.2 . . ? H31A C3A H31B 107.9 . . ? N31A C32A C3A 109.9(8) . . ? N31A C32A H32A 109.7 . . ? C3A C32A H32A 109.7 . . ? N31A C32A H32B 109.7 . . ? C3A C32A H32B 109.7 . . ? H32A C32A H32B 108.2 . . ? N31A C33A C34A 114.1(9) . . ? N31A C33A H33A 122.9 . . ? C34A C33A H33A 122.9 . . ? N32A C34A C33A 116.0(8) . . ? N32A C34A C35A 107.7(9) . . ? C33A C34A C35A 135.9(10) . . ? C36A C35A C34A 102.1(8) . . ? C36A C35A H35A 128.9 . . ? C34A C35A H35A 128.9 . . ? N33A C36A C35A 112.4(8) . . ? N33A C36A C37A 122.1(9) . . ? C35A C36A C37A 125.5(10) . . ? C36A C37A H37A 109.5 . . ? C36A C37A H37B 109.5 . . ? H37A C37A H37B 109.5 . . ? C36A C37A H37C 109.5 . . ? H37A C37A H37C 109.5 . . ? H37B C37A H37C 109.5 . . ? C33A N31A C32A 119.1(9) . . ? C33A N31A Co1 114.1(6) . . ? C32A N31A Co1 126.8(6) . . ? C34A N32A N33A 112.9(7) . . ? C34A N32A Co1 114.9(6) . . ? N33A N32A Co1 130.8(6) . . ? C36A N33A N32A 104.7(7) . . ? N22B Mn1 N12B 93.7(3) . . ? N22B Mn1 N21B 74.2(3) . . ? N12B Mn1 N21B 165.5(3) . . ? N22B Mn1 N11B 91.1(3) . . ? N12B Mn1 N11B 74.4(3) . . ? N21B Mn1 N11B 97.6(3) . . ? N22B Mn1 N32B 98.6(3) . . ? N12B Mn1 N32B 95.0(3) . . ? N21B Mn1 N32B 94.6(3) . . ? N11B Mn1 N32B 166.1(3) . . ? N22B Mn1 N31B 171.3(3) . . ? N12B Mn1 N31B 92.4(3) . . ? N21B Mn1 N31B 100.6(3) . . ? N11B Mn1 N31B 96.5(3) . . ? N32B Mn1 N31B 74.6(3) . . ? C21B N1B C11B 118.7(10) . . ? C21B N1B C31B 118.0(9) . . ? C11B N1B C31B 113.6(9) . . ? N1B C11B C12B 112.7(8) . . ? N1B C11B H11C 109.1 . . ? C12B C11B H11C 109.1 . . ? N1B C11B H11D 109.1 . . ? C12B C11B H11D 109.1 . . ? H11C C11B H11D 107.8 . . ? N11B C12B C11B 108.3(8) . . ? N11B C12B H12C 110.0 . . ? C11B C12B H12C 110.0 . . ? N11B C12B H12D 110.0 . . ? C11B C12B H12D 110.0 . . ? H12C C12B H12D 108.4 . . ? N11B C13B C14B 120.3(9) . . ? N11B C13B H13B 119.9 . . ? C14B C13B H13B 119.9 . . ? N12B C14B C15B 112.3(9) . . ? N12B C14B C13B 115.2(9) . . ? C15B C14B C13B 132.5(9) . . ? C16B C15B C14B 105.2(9) . . ? C16B C15B H15B 127.4 . . ? C14B C15B H15B 127.4 . . ? N13B C16B C15B 108.1(8) . . ? N13B C16B C17B 119.0(9) . . ? C15B C16B C17B 132.8(9) . . ? C16B C17B H17D 109.5 . . ? C16B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C16B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C13B N11B C12B 121.2(9) . . ? C13B N11B Mn1 114.4(6) . . ? C12B N11B Mn1 124.4(7) . . ? C14B N12B N13B 101.7(8) . . ? C14B N12B Mn1 115.2(6) . . ? N13B N12B Mn1 141.8(6) . . ? C16B N13B N12B 112.6(7) . . ? C16B N13B H13C 123.7 . . ? N12B N13B H13C 123.7 . . ? N1B C21B C22B 112.6(9) . . ? N1B C21B H21C 109.1 . . ? C22B C21B H21C 109.1 . . ? N1B C21B H21D 109.1 . . ? C22B C21B H21D 109.1 . . ? H21C C21B H21D 107.8 . . ? N21B C22B C21B 107.3(8) . . ? N21B C22B H22C 110.2 . . ? C21B C22B H22C 110.2 . . ? N21B C22B H22D 110.2 . . ? C21B C22B H22D 110.2 . . ? H22C C22B H22D 108.5 . . ? N21B C23B C24B 116.4(8) . . ? N21B C23B H23B 121.8 . . ? C24B C23B H23B 121.8 . . ? N22B C24B C25B 112.1(8) . . ? N22B C24B C23B 114.7(8) . . ? C25B C24B C23B 133.1(8) . . ? C26B C25B C24B 105.4(8) . . ? C26B C25B H25B 127.3 . . ? C24B C25B H25B 127.3 . . ? N23B C26B C25B 106.8(9) . . ? N23B C26B C27B 120.1(10) . . ? C25B C26B C27B 133.0(10) . . ? C26B C27B H27D 109.5 . . ? C26B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C26B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C23B N21B C22B 118.3(8) . . ? C23B N21B Mn1 117.5(6) . . ? C22B N21B Mn1 124.1(6) . . ? C24B N22B N23B 101.6(7) . . ? C24B N22B Mn1 115.9(6) . . ? N23B N22B Mn1 140.7(5) . . ? C26B N23B N22B 113.8(8) . . ? C26B N23B H23C 123.1 . . ? N22B N23B H23C 123.1 . . ? N1B C31B C32B 113.9(9) . . ? N1B C31B H31C 108.8 . . ? C32B C31B H31C 108.8 . . ? N1B C31B H31D 108.8 . . ? C32B C31B H31D 108.8 . . ? H31C C31B H31D 107.7 . . ? N31B C32B C31B 108.7(9) . . ? N31B C32B H32C 109.9 . . ? C31B C32B H32C 109.9 . . ? N31B C32B H32D 109.9 . . ? C31B C32B H32D 109.9 . . ? H32C C32B H32D 108.3 . . ? N31B C33B C34B 120.7(9) . . ? N31B C33B H33B 119.7 . . ? C34B C33B H33B 119.7 . . ? C35B C34B N32B 110.0(9) . . ? C35B C34B C33B 133.9(9) . . ? N32B C34B C33B 116.0(8) . . ? C36B C35B C34B 107.1(9) . . ? C36B C35B H35B 126.4 . . ? C34B C35B H35B 126.4 . . ? C35B C36B N33B 106.7(8) . . ? C35B C36B C37B 132.4(10) . . ? N33B C36B C37B 120.8(10) . . ? C36B C37B H37D 109.5 . . ? C36B C37B H37E 109.5 . . ? H37D C37B H37E 109.5 . . ? C36B C37B H37F 109.5 . . ? H37D C37B H37F 109.5 . . ? H37E C37B H37F 109.5 . . ? C33B N31B C32B 120.1(9) . . ? C33B N31B Mn1 114.9(7) . . ? C32B N31B Mn1 124.6(7) . . ? N33B N32B C34B 103.2(8) . . ? N33B N32B Mn1 142.2(6) . . ? C34B N32B Mn1 113.5(6) . . ? N32B N33B C36B 112.9(8) . . ? N32B N33B H33C 123.6 . . ? C36B N33B H33C 123.6 . . ? O14 Cl1 O11 113.3(9) . . ? O14 Cl1 O13 107.5(8) . . ? O11 Cl1 O13 112.3(9) . . ? O14 Cl1 O12 114.0(9) . . ? O11 Cl1 O12 106.2(9) . . ? O13 Cl1 O12 103.3(8) . . ? O24 Cl2 O22 114.4(17) . . ? O24 Cl2 O23 103.7(13) . . ? O22 Cl2 O23 102.0(14) . . ? O24 Cl2 O21 123.3(16) . . ? O22 Cl2 O21 108.4(15) . . ? O23 Cl2 O21 101.8(15) . . ? O22A Cl2A O21A 120.5(14) . . ? O22A Cl2A O23A 109.1(12) . . ? O21A Cl2A O23A 119.7(13) . . ? O22A Cl2A O24A 98.5(12) . . ? O21A Cl2A O24A 105.5(12) . . ? O23A Cl2A O24A 98.1(10) . . ? 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 C3A N1A C11A C12A 82.4(12) . . . . ? C21A N1A C11A C12A -115.2(11) . . . . ? N1A C11A C12A N11A 50.8(12) . . . . ? N11A C13A C14A N12A -5.1(12) . . . . ? N11A C13A C14A C15A 166.8(10) . . . . ? N12A C14A C15A C16A -0.9(10) . . . . ? C13A C14A C15A C16A -173.1(10) . . . . ? C14A C15A C16A N13A 2.6(10) . . . . ? C14A C15A C16A C17A -179.4(10) . . . . ? C14A C13A N11A C12A -179.2(8) . . . . ? C14A C13A N11A Co1 2.5(10) . . . . ? C11A C12A N11A C13A 102.2(11) . . . . ? C11A C12A N11A Co1 -79.7(11) . . . . ? N32A Co1 N11A C13A 96.6(6) . . . . ? N12A Co1 N11A C13A 0.3(6) . . . . ? N31A Co1 N11A C13A 176.9(6) . . . . ? N21A Co1 N11A C13A -87.3(6) . . . . ? N32A Co1 N11A C12A -81.7(8) . . . . ? N12A Co1 N11A C12A -177.9(8) . . . . ? N31A Co1 N11A C12A -1.3(8) . . . . ? N21A Co1 N11A C12A 94.5(8) . . . . ? C13A C14A N12A N13A 173.1(7) . . . . ? C15A C14A N12A N13A -1.2(10) . . . . ? C13A C14A N12A Co1 5.1(9) . . . . ? C15A C14A N12A Co1 -169.2(6) . . . . ? N32A Co1 N12A N13A 105.1(8) . . . . ? N22A Co1 N12A N13A 7.7(8) . . . . ? N21A Co1 N12A N13A -73.0(8) . . . . ? N11A Co1 N12A N13A -167.6(9) . . . . ? N32A Co1 N12A C14A -90.4(6) . . . . ? N22A Co1 N12A C14A 172.2(6) . . . . ? N21A Co1 N12A C14A 91.5(6) . . . . ? N11A Co1 N12A C14A -3.1(6) . . . . ? C14A N12A N13A C16A 2.8(10) . . . . ? Co1 N12A N13A C16A 167.6(7) . . . . ? C15A C16A N13A N12A -3.4(10) . . . . ? C17A C16A N13A N12A 178.4(9) . . . . ? C3A N1A C21A C22A -119.4(11) . . . . ? C11A N1A C21A C22A 78.6(12) . . . . ? N1A C21A C22A N21A 51.4(12) . . . . ? N21A C23A C24A N22A -3.7(11) . . . . ? N21A C23A C24A C25A 166.3(10) . . . . ? N22A C24A C25A C26A 1.0(9) . . . . ? C23A C24A C25A C26A -169.4(10) . . . . ? C24A C25A C26A N23A -0.2(10) . . . . ? C24A C25A C26A C27A 178.7(9) . . . . ? C24A C23A N21A C22A -178.4(7) . . . . ? C24A C23A N21A Co1 3.5(9) . . . . ? C21A C22A N21A C23A 103.0(10) . . . . ? C21A C22A N21A Co1 -79.2(9) . . . . ? N22A Co1 N21A C23A -1.9(6) . . . . ? N12A Co1 N21A C23A 92.8(6) . . . . ? N31A Co1 N21A C23A -89.8(6) . . . . ? N11A Co1 N21A C23A 173.6(6) . . . . ? N22A Co1 N21A C22A -179.8(7) . . . . ? N12A Co1 N21A C22A -85.0(7) . . . . ? N31A Co1 N21A C22A 92.3(7) . . . . ? N11A Co1 N21A C22A -4.3(7) . . . . ? C25A C24A N22A N23A -1.5(9) . . . . ? C23A C24A N22A N23A 171.4(7) . . . . ? C25A C24A N22A Co1 -170.8(5) . . . . ? C23A C24A N22A Co1 2.1(9) . . . . ? N32A Co1 N22A N23A 9.2(8) . . . . ? N12A Co1 N22A N23A 105.7(7) . . . . ? N31A Co1 N22A N23A -71.1(7) . . . . ? N21A Co1 N22A N23A -166.8(7) . . . . ? N32A Co1 N22A C24A 175.7(6) . . . . ? N12A Co1 N22A C24A -87.8(6) . . . . ? N31A Co1 N22A C24A 95.4(6) . . . . ? N21A Co1 N22A C24A -0.2(6) . . . . ? C24A N22A N23A C26A 1.3(9) . . . . ? Co1 N22A N23A C26A 168.0(6) . . . . ? C25A C26A N23A N22A -0.6(9) . . . . ? C27A C26A N23A N22A -179.6(7) . . . . ? C21A N1A C3A C32A 78.4(12) . . . . ? C11A N1A C3A C32A -119.6(10) . . . . ? N1A C3A C32A N31A 54.8(12) . . . . ? N31A C33A C34A N32A -6.8(12) . . . . ? N31A C33A C34A C35A 164.8(10) . . . . ? N32A C34A C35A C36A 0.9(10) . . . . ? C33A C34A C35A C36A -171.2(10) . . . . ? C34A C35A C36A N33A 1.0(11) . . . . ? C34A C35A C36A C37A 178.9(9) . . . . ? C34A C33A N31A C32A -176.4(8) . . . . ? C34A C33A N31A Co1 6.7(10) . . . . ? C3A C32A N31A C33A 101.8(9) . . . . ? C3A C32A N31A Co1 -81.7(9) . . . . ? N32A Co1 N31A C33A -3.9(6) . . . . ? N22A Co1 N31A C33A 93.3(6) . . . . ? N21A Co1 N31A C33A 174.0(6) . . . . ? N11A Co1 N31A C33A -91.1(6) . . . . ? N32A Co1 N31A C32A 179.4(8) . . . . ? N22A Co1 N31A C32A -83.4(7) . . . . ? N21A Co1 N31A C32A -2.7(8) . . . . ? N11A Co1 N31A C32A 92.2(7) . . . . ? C33A C34A N32A N33A 171.3(7) . . . . ? C35A C34A N32A N33A -2.6(10) . . . . ? C33A C34A N32A Co1 3.5(10) . . . . ? C35A C34A N32A Co1 -170.4(6) . . . . ? N22A Co1 N32A C34A -87.5(7) . . . . ? N12A Co1 N32A C34A 177.3(6) . . . . ? N31A Co1 N32A C34A 0.1(6) . . . . ? N11A Co1 N32A C34A 96.6(6) . . . . ? N22A Co1 N32A N33A 107.3(7) . . . . ? N12A Co1 N32A N33A 12.2(7) . . . . ? N31A Co1 N32A N33A -165.1(7) . . . . ? N11A Co1 N32A N33A -68.5(7) . . . . ? C35A C36A N33A N32A -2.5(10) . . . . ? C37A C36A N33A N32A 179.6(8) . . . . ? C34A N32A N33A C36A 3.1(9) . . . . ? Co1 N32A N33A C36A 168.5(6) . . . . ? C21B N1B C11B C12B 82.6(12) . . . . ? C31B N1B C11B C12B -131.9(11) . . . . ? N1B C11B C12B N11B 57.8(13) . . . . ? N11B C13B C14B N12B -6.7(12) . . . . ? N11B C13B C14B C15B 172.4(9) . . . . ? N12B C14B C15B C16B 1.2(10) . . . . ? C13B C14B C15B C16B -177.9(10) . . . . ? C14B C15B C16B N13B -1.3(10) . . . . ? C14B C15B C16B C17B 174.9(9) . . . . ? C14B C13B N11B C12B -177.0(8) . . . . ? C14B C13B N11B Mn1 1.2(10) . . . . ? C11B C12B N11B C13B 107.3(10) . . . . ? C11B C12B N11B Mn1 -70.8(11) . . . . ? N22B Mn1 N11B C13B 96.1(6) . . . . ? N12B Mn1 N11B C13B 2.6(6) . . . . ? N21B Mn1 N11B C13B 170.2(6) . . . . ? N32B Mn1 N11B C13B -38.8(14) . . . . ? N31B Mn1 N11B C13B -88.1(6) . . . . ? N22B Mn1 N11B C12B -85.8(7) . . . . ? N12B Mn1 N11B C12B -179.2(7) . . . . ? N21B Mn1 N11B C12B -11.6(7) . . . . ? N32B Mn1 N11B C12B 139.4(11) . . . . ? N31B Mn1 N11B C12B 90.1(7) . . . . ? C15B C14B N12B N13B -0.6(9) . . . . ? C13B C14B N12B N13B 178.7(7) . . . . ? C15B C14B N12B Mn1 -170.6(6) . . . . ? C13B C14B N12B Mn1 8.7(10) . . . . ? N22B Mn1 N12B C14B -96.3(6) . . . . ? N21B Mn1 N12B C14B -63.9(14) . . . . ? N11B Mn1 N12B C14B -6.1(6) . . . . ? N32B Mn1 N12B C14B 164.7(6) . . . . ? N31B Mn1 N12B C14B 90.0(6) . . . . ? N22B Mn1 N12B N13B 99.7(8) . . . . ? N21B Mn1 N12B N13B 132.1(11) . . . . ? N11B Mn1 N12B N13B -170.1(9) . . . . ? N32B Mn1 N12B N13B 0.7(8) . . . . ? N31B Mn1 N12B N13B -74.0(8) . . . . ? C15B C16B N13B N12B 1.0(10) . . . . ? C17B C16B N13B N12B -175.8(7) . . . . ? C14B N12B N13B C16B -0.3(9) . . . . ? Mn1 N12B N13B C16B 165.0(7) . . . . ? C11B N1B C21B C22B -132.8(9) . . . . ? C31B N1B C21B C22B 83.3(12) . . . . ? N1B C21B C22B N21B 55.5(12) . . . . ? N21B C23B C24B N22B -10.2(12) . . . . ? N21B C23B C24B C25B 173.2(10) . . . . ? N22B C24B C25B C26B 5.0(11) . . . . ? C23B C24B C25B C26B -178.3(10) . . . . ? C24B C25B C26B N23B -6.3(11) . . . . ? C24B C25B C26B C27B 176.1(12) . . . . ? C24B C23B N21B C22B -174.3(8) . . . . ? C24B C23B N21B Mn1 2.1(11) . . . . ? C21B C22B N21B C23B 103.5(10) . . . . ? C21B C22B N21B Mn1 -72.6(10) . . . . ? N22B Mn1 N21B C23B 3.5(7) . . . . ? N12B Mn1 N21B C23B -30.2(16) . . . . ? N11B Mn1 N21B C23B -85.5(7) . . . . ? N32B Mn1 N21B C23B 101.2(7) . . . . ? N31B Mn1 N21B C23B 176.4(7) . . . . ? N22B Mn1 N21B C22B 179.7(8) . . . . ? N12B Mn1 N21B C22B 146.0(11) . . . . ? N11B Mn1 N21B C22B 90.7(8) . . . . ? N32B Mn1 N21B C22B -82.6(8) . . . . ? N31B Mn1 N21B C22B -7.4(8) . . . . ? C25B C24B N22B N23B -1.6(10) . . . . ? C23B C24B N22B N23B -179.0(7) . . . . ? C25B C24B N22B Mn1 -169.5(6) . . . . ? C23B C24B N22B Mn1 13.2(10) . . . . ? N12B Mn1 N22B C24B 162.8(7) . . . . ? N21B Mn1 N22B C24B -9.2(6) . . . . ? N11B Mn1 N22B C24B 88.4(7) . . . . ? N32B Mn1 N22B C24B -101.5(7) . . . . ? N12B Mn1 N22B N23B 1.8(9) . . . . ? N21B Mn1 N22B N23B -170.2(9) . . . . ? N11B Mn1 N22B N23B -72.6(9) . . . . ? N32B Mn1 N22B N23B 97.5(9) . . . . ? C25B C26B N23B N22B 5.8(12) . . . . ? C27B C26B N23B N22B -176.2(9) . . . . ? C24B N22B N23B C26B -2.6(10) . . . . ? Mn1 N22B N23B C26B 160.1(8) . . . . ? C21B N1B C31B C32B -134.1(10) . . . . ? C11B N1B C31B C32B 80.2(12) . . . . ? N1B C31B C32B N31B 56.4(13) . . . . ? N31B C33B C34B C35B 173.5(11) . . . . ? N31B C33B C34B N32B -2.3(15) . . . . ? N32B C34B C35B C36B 2.4(12) . . . . ? C33B C34B C35B C36B -173.5(11) . . . . ? C34B C35B C36B N33B -3.3(11) . . . . ? C34B C35B C36B C37B 175.6(10) . . . . ? C34B C33B N31B C32B -175.7(10) . . . . ? C34B C33B N31B Mn1 -2.4(13) . . . . ? C31B C32B N31B C33B 103.3(11) . . . . ? C31B C32B N31B Mn1 -69.3(12) . . . . ? N12B Mn1 N31B C33B 98.6(8) . . . . ? N21B Mn1 N31B C33B -87.8(8) . . . . ? N11B Mn1 N31B C33B 173.2(8) . . . . ? N32B Mn1 N31B C33B 4.1(7) . . . . ? N12B Mn1 N31B C32B -88.4(9) . . . . ? N21B Mn1 N31B C32B 85.1(9) . . . . ? N11B Mn1 N31B C32B -13.9(9) . . . . ? N32B Mn1 N31B C32B 177.0(9) . . . . ? C35B C34B N32B N33B -0.5(10) . . . . ? C33B C34B N32B N33B 176.3(8) . . . . ? C35B C34B N32B Mn1 -171.0(6) . . . . ? C33B C34B N32B Mn1 5.8(11) . . . . ? N22B Mn1 N32B N33B 4.4(9) . . . . ? N12B Mn1 N32B N33B 98.9(9) . . . . ? N21B Mn1 N32B N33B -70.3(9) . . . . ? N11B Mn1 N32B N33B 138.6(10) . . . . ? N31B Mn1 N32B N33B -170.0(10) . . . . ? N22B Mn1 N32B C34B 169.2(6) . . . . ? N12B Mn1 N32B C34B -96.3(7) . . . . ? N21B Mn1 N32B C34B 94.6(7) . . . . ? N11B Mn1 N32B C34B -56.6(14) . . . . ? N31B Mn1 N32B C34B -5.1(6) . . . . ? C34B N32B N33B C36B -1.7(10) . . . . ? Mn1 N32B N33B C36B 164.1(7) . . . . ? C35B C36B N33B N32B 3.2(11) . . . . ? C37B C36B N33B N32B -175.8(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13B H13C N13A 0.86 1.95 2.800(10) 170 . N23B H23C N23A 0.86 1.95 2.804(10) 173 . N33B H33C N33A 0.86 1.90 2.750(10) 169 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.321 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.048 _chemical_absolute_configuration ad _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 -0.0112538 _diffrn_orient_matrix_UB_12 0.0738948 _diffrn_orient_matrix_UB_13 -0.0133185 _diffrn_orient_matrix_UB_21 0.0455413 _diffrn_orient_matrix_UB_22 0.0190190 _diffrn_orient_matrix_UB_23 0.0012731 _diffrn_orient_matrix_UB_31 0.0018558 _diffrn_orient_matrix_UB_32 -0.0199894 _diffrn_orient_matrix_UB_33 -0.0480653 _symmetry_space_group_name_Hall 'C -2yc' _exptl_crystal_id 'CUA/Brewer CTBH25A at RT' _diffrn_measurement_frame_width-CCD -0.30 _diffrn_measurement_details 510,610,610,1200 _diffrn_measurement_total_frames-CCD 2930 _diffrn_measurement_frame_time-CCD 40 _diffrn_measurement_total_time-CCD 37.4 _diffrn_source_voltage 50.00 _diffrn_source_current 30.00 _diffrn_detector_distance-CCD 5.0000 _diffrn_measurement_frame_size-CCD 512 _diffrn_measurement_specimen_support 'MiTeGen loop' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart Apex II' _reflns_Friedel_coverage 0.981 #_______________________________________________________________________________ # _publ_section_references ; Bruker (2005). Apex2. Bruker AXS Inc., Madison, Wisconsin, USA. Flack, H.D. (1983), Acta Cryst. A39, 876-881. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Spek, A. L. (1990). Acta Cryst., A46, C-34. ; # Attachment 'CTBH23CU.CIF' data_ctbh23cu _database_code_depnum_ccdc_archive 'CCDC 785615' #TrackingRef 'CTBH23CU.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H57 Co Mn N20, 2(Cl O4)' _chemical_formula_sum 'C42 H57 Cl2 Co Mn N20 O8' _chemical_formula_weight 1154.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 12.4408(2) _cell_length_b 21.6681(5) _cell_length_c 21.9574(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5919.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4624 _cell_measurement_theta_min 4.5112 _cell_measurement_theta_max 77.4858 _exptl_crystal_description needle _exptl_crystal_colour 'pale orange' _exptl_crystal_size_max 0.3776 _exptl_crystal_size_mid 0.1714 _exptl_crystal_size_min 0.1524 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2396 _exptl_absorpt_coefficient_mu 5.284 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.308 _exptl_absorpt_correction_T_max 0.557 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.5081 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18951 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.57 _diffrn_reflns_theta_max 77.70 _reflns_number_total 6225 _reflns_number_gt 3308 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1468P)^2^] 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 6225 _refine_ls_number_parameters 338 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2581 _refine_ls_wR_factor_gt 0.2294 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.64129(5) 0.58054(3) 0.63428(4) 0.0625(3) Uani 0.50 1 d P . . Mn Mn 0.64129(5) 0.58054(3) 0.63428(4) 0.0625(3) Uani 0.50 1 d P . . Cl Cl 1.01794(14) 0.75575(9) 0.59673(10) 0.1221(8) Uani 1 1 d D . . O1 O 0.9677(5) 0.8091(2) 0.5822(3) 0.309(7) Uani 1 1 d D . . O2 O 1.1250(3) 0.7660(3) 0.6005(2) 0.171(3) Uani 1 1 d D . . O3 O 0.9985(5) 0.7133(2) 0.5531(2) 0.251(5) Uani 1 1 d D . . O4 O 0.9811(4) 0.7351(3) 0.65083(19) 0.216(4) Uani 1 1 d D . . N N 0.7973(4) 0.5769(2) 0.5109(3) 0.0928(15) Uani 1 1 d . . . N1A N 0.6311(3) 0.5068(3) 0.5731(3) 0.0923(16) Uani 1 1 d . . . N2A N 0.6264(4) 0.5057(2) 0.6904(3) 0.0974(17) Uani 1 1 d . . . N3A N 0.6356(5) 0.4945(4) 0.7519(4) 0.131(3) Uani 1 1 d . . . N1B N 0.8105(4) 0.58102(19) 0.6421(2) 0.0753(12) Uani 1 1 d . . . N2B N 0.6679(3) 0.64267(16) 0.7038(2) 0.0749(13) Uani 1 1 d . . . N3B N 0.6109(4) 0.68172(19) 0.7392(3) 0.105(2) Uani 1 1 d . . . H3BB H 0.5404 0.6813 0.7427 0.126 Uiso 0.50 1 calc PR . . N1C N 0.6327(3) 0.65129(19) 0.5692(2) 0.0779(13) Uani 1 1 d . . . N2C N 0.4763(4) 0.6004(3) 0.6294(3) 0.0927(16) Uani 1 1 d . . . N3C N 0.3827(6) 0.5771(4) 0.6517(3) 0.133(3) Uani 1 1 d . . . H3CB H 0.3768 0.5486 0.6800 0.159 Uiso 1 1 calc R . . C1A C 0.7516(5) 0.5230(3) 0.4847(3) 0.099(2) Uani 1 1 d . . . H1AA H 0.7971 0.4870 0.4952 0.119 Uiso 1 1 calc R . . H1AB H 0.7515 0.5273 0.4398 0.119 Uiso 1 1 calc R . . C2A C 0.6365(5) 0.5107(4) 0.5065(4) 0.116(3) Uani 1 1 d . . . H2AA H 0.5890 0.5444 0.4922 0.139 Uiso 1 1 calc R . . H2AB H 0.6104 0.4716 0.4886 0.139 Uiso 1 1 calc R . . C3A C 0.6224(4) 0.4525(3) 0.5973(5) 0.103(2) Uani 1 1 d . . . H3AA H 0.6146 0.4165 0.5731 0.123 Uiso 1 1 calc R . . C4A C 0.6251(4) 0.4498(3) 0.6630(4) 0.097(2) Uani 1 1 d . . . C5A C 0.6329(5) 0.4036(3) 0.7072(5) 0.108(3) Uani 1 1 d . . . H5AA H 0.6327 0.3602 0.7010 0.130 Uiso 1 1 calc R . . C6A C 0.6412(6) 0.4353(5) 0.7624(5) 0.126(3) Uani 1 1 d . . . C7A C 0.6524(6) 0.4093(5) 0.8236(4) 0.137(3) Uani 1 1 d . . . H7AA H 0.6455 0.3643 0.8216 0.205 Uiso 1 1 calc R . . H7AB H 0.5961 0.4261 0.8500 0.205 Uiso 1 1 calc R . . H7AC H 0.7231 0.4201 0.8401 0.205 Uiso 1 1 calc R . . C1B C 0.8983(4) 0.5718(3) 0.5442(3) 0.093(2) Uani 1 1 d . . . H1BA H 0.9306 0.6133 0.5483 0.111 Uiso 1 1 calc R . . H1BB H 0.9488 0.5459 0.5204 0.111 Uiso 1 1 calc R . . C2B C 0.8850(5) 0.5439(3) 0.6070(3) 0.094(2) Uani 1 1 d . . . H2BA H 0.8573 0.5012 0.6035 0.113 Uiso 1 1 calc R . . H2BB H 0.9554 0.5424 0.6279 0.113 Uiso 1 1 calc R . . C3B C 0.8475(4) 0.6207(2) 0.6798(3) 0.0761(16) Uani 1 1 d . . . H3BA H 0.9228 0.6256 0.6854 0.091 Uiso 1 1 calc R . . C4B C 0.7731(4) 0.6574(2) 0.7128(3) 0.0657(13) Uani 1 1 d . . . C5B C 0.7809(5) 0.7071(2) 0.7539(3) 0.0852(17) Uani 1 1 d . . . H5BA H 0.8439 0.7269 0.7686 0.102 Uiso 1 1 calc R . . C6B C 0.6745(6) 0.7203(3) 0.7677(3) 0.099(2) Uani 1 1 d . . . C7B C 0.6316(7) 0.7696(3) 0.8123(4) 0.134(3) Uani 1 1 d . . . H7BA H 0.6815 0.7739 0.8465 0.200 Uiso 1 1 calc R . . H7BB H 0.5609 0.7570 0.8275 0.200 Uiso 1 1 calc R . . H7BC H 0.6252 0.8092 0.7911 0.200 Uiso 1 1 calc R . . C1C C 0.7662(5) 0.6363(3) 0.4884(3) 0.0963(19) Uani 1 1 d . . . H1CA H 0.7092 0.6310 0.4573 0.116 Uiso 1 1 calc R . . H1CB H 0.8287 0.6558 0.4682 0.116 Uiso 1 1 calc R . . C2C C 0.7252(5) 0.6791(2) 0.5380(4) 0.097(2) Uani 1 1 d . . . H2CA H 0.7833 0.6870 0.5679 0.117 Uiso 1 1 calc R . . H2CB H 0.7038 0.7191 0.5199 0.117 Uiso 1 1 calc R . . C3C C 0.5377(4) 0.6717(2) 0.5569(3) 0.0799(16) Uani 1 1 d . . . H3CA H 0.5268 0.7044 0.5288 0.096 Uiso 1 1 calc R . . C4C C 0.4496(4) 0.6431(3) 0.5877(3) 0.0795(16) Uani 1 1 d . . . C5C C 0.3373(5) 0.6470(4) 0.5828(4) 0.101(2) Uani 1 1 d . . . H5CA H 0.2972 0.6736 0.5569 0.121 Uiso 1 1 calc R . . C6C C 0.2987(7) 0.6058(4) 0.6222(4) 0.119(3) Uani 1 1 d . . . C7C C 0.1901(7) 0.5855(5) 0.6426(4) 0.168(5) Uani 1 1 d . . . H7CA H 0.1966 0.5472 0.6661 0.252 Uiso 1 1 calc R . . H7CB H 0.1443 0.5783 0.6070 0.252 Uiso 1 1 calc R . . H7CC H 0.1580 0.6176 0.6683 0.252 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0290(3) 0.0407(3) 0.1178(7) -0.0070(4) 0.0066(4) -0.0022(2) Mn 0.0290(3) 0.0407(3) 0.1178(7) -0.0070(4) 0.0066(4) -0.0022(2) Cl 0.0897(11) 0.1007(12) 0.176(2) 0.0383(13) -0.0192(12) -0.0454(10) O1 0.463(17) 0.283(11) 0.180(7) 0.037(7) 0.021(9) 0.283(12) O2 0.100(4) 0.212(8) 0.203(6) 0.010(6) 0.011(4) -0.056(4) O3 0.302(11) 0.116(5) 0.334(11) -0.056(6) 0.071(9) -0.115(6) O4 0.127(6) 0.238(9) 0.284(9) 0.114(8) 0.066(6) -0.022(5) N 0.076(3) 0.067(3) 0.135(4) -0.025(3) -0.018(3) -0.001(2) N1A 0.042(2) 0.105(4) 0.130(5) -0.010(4) 0.024(2) 0.000(2) N2A 0.069(3) 0.077(3) 0.146(5) -0.009(3) 0.026(3) 0.030(2) N3A 0.091(4) 0.147(6) 0.154(6) 0.006(5) 0.018(4) 0.082(4) N1B 0.052(2) 0.056(2) 0.118(4) 0.001(3) 0.013(2) 0.0092(18) N2B 0.0445(18) 0.0381(17) 0.142(4) 0.011(2) 0.025(2) 0.0017(14) N3B 0.079(3) 0.039(2) 0.198(6) 0.011(3) 0.064(4) 0.006(2) N1C 0.052(2) 0.059(2) 0.123(4) -0.024(3) 0.016(2) -0.0107(18) N2C 0.064(3) 0.100(4) 0.114(4) -0.010(3) -0.001(3) -0.046(3) N3C 0.127(6) 0.153(6) 0.119(5) -0.035(4) 0.017(4) -0.099(5) C1A 0.063(3) 0.082(4) 0.151(6) -0.034(4) 0.028(4) -0.010(3) C2A 0.060(3) 0.123(6) 0.165(8) -0.028(6) 0.014(4) -0.023(4) C3A 0.052(3) 0.071(4) 0.184(8) -0.017(5) 0.034(4) -0.008(3) C4A 0.054(3) 0.077(4) 0.161(7) -0.014(5) 0.031(4) 0.004(3) C5A 0.065(4) 0.080(4) 0.180(8) 0.017(5) 0.031(5) 0.009(3) C6A 0.064(4) 0.160(8) 0.155(8) 0.002(7) 0.027(4) 0.047(5) C7A 0.088(5) 0.176(9) 0.145(7) 0.022(7) 0.013(5) 0.055(5) C1B 0.041(2) 0.083(4) 0.155(6) -0.011(4) 0.024(3) 0.000(2) C2B 0.064(3) 0.084(4) 0.133(5) -0.003(4) 0.013(4) 0.032(3) C3B 0.041(2) 0.064(3) 0.124(5) 0.011(3) 0.004(3) 0.007(2) C4B 0.048(2) 0.048(2) 0.101(4) 0.015(2) 0.003(2) 0.0003(19) C5B 0.075(3) 0.056(3) 0.124(5) 0.009(3) 0.007(3) -0.002(3) C6B 0.105(5) 0.051(3) 0.140(6) 0.023(3) 0.053(4) 0.014(3) C7B 0.165(8) 0.055(3) 0.181(8) 0.011(4) 0.078(7) 0.021(4) C1C 0.084(4) 0.088(4) 0.117(5) 0.002(4) 0.028(4) 0.018(3) C2C 0.075(3) 0.056(3) 0.161(6) -0.001(3) 0.041(4) -0.005(3) C3C 0.060(3) 0.056(3) 0.123(5) -0.019(3) 0.005(3) -0.003(2) C4C 0.060(3) 0.077(3) 0.101(4) -0.019(3) -0.001(3) -0.007(3) C5C 0.055(3) 0.110(5) 0.138(6) -0.044(5) 0.009(3) -0.018(3) C6C 0.087(5) 0.140(7) 0.129(6) -0.049(5) 0.009(5) -0.057(5) C7C 0.106(6) 0.212(11) 0.186(9) -0.103(8) 0.047(6) -0.098(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 Co N2A 2.045(6) . ? Co N2B 2.063(5) . ? Co N1A 2.091(6) . ? Co N1C 2.099(5) . ? Co N2C 2.100(6) . ? Co N1B 2.113(5) . ? Cl O4 1.349(3) . ? Cl O3 1.350(3) . ? Cl O1 1.353(3) . ? Cl O2 1.353(3) . ? N C1A 1.420(7) . ? N C1C 1.433(7) . ? N C1B 1.459(8) . ? N1A C3A 1.296(9) . ? N1A C2A 1.467(10) . ? N2A C4A 1.353(8) . ? N2A N3A 1.378(9) . ? N3A C6A 1.305(12) . ? N1B C3B 1.279(7) . ? N1B C2B 1.448(7) . ? N2B N3B 1.350(6) . ? N2B C4B 1.362(6) . ? N3B C6B 1.311(9) . ? N3B H3BB 0.8800 . ? N1C C3C 1.291(7) . ? N1C C2C 1.467(6) . ? N2C C4C 1.344(8) . ? N2C N3C 1.360(7) . ? N3C C6C 1.377(13) . ? N3C H3CB 0.8800 . ? C1A C2A 1.532(8) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.446(12) . ? C3A H3AA 0.9500 . ? C4A C5A 1.397(11) . ? C5A C6A 1.396(13) . ? C5A H5AA 0.9500 . ? C6A C7A 1.464(12) . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C1B C2B 1.515(9) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C4B 1.420(7) . ? C3B H3BA 0.9500 . ? C4B C5B 1.407(8) . ? C5B C6B 1.389(8) . ? C5B H5BA 0.9500 . ? C6B C7B 1.542(9) . ? C7B H7BA 0.9800 . ? C7B H7BB 0.9800 . ? C7B H7BC 0.9800 . ? C1C C2C 1.519(8) . ? C1C H1CA 0.9900 . ? C1C H1CB 0.9900 . ? C2C H2CA 0.9900 . ? C2C H2CB 0.9900 . ? C3C C4C 1.430(8) . ? C3C H3CA 0.9500 . ? C4C C5C 1.403(7) . ? C5C C6C 1.334(11) . ? C5C H5CA 0.9500 . ? C6C C7C 1.489(10) . ? C7C H7CA 0.9800 . ? C7C H7CB 0.9800 . ? C7C H7CC 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 N2A Co N2B 94.9(2) . . ? N2A Co N1A 77.1(3) . . ? N2B Co N1A 169.8(2) . . ? N2A Co N1C 170.1(2) . . ? N2B Co N1C 92.04(17) . . ? N1A Co N1C 96.7(2) . . ? N2A Co N2C 96.0(2) . . ? N2B Co N2C 93.52(18) . . ? N1A Co N2C 93.68(18) . . ? N1C Co N2C 76.5(2) . . ? N2A Co N1B 92.57(18) . . ? N2B Co N1B 77.08(17) . . ? N1A Co N1B 96.68(17) . . ? N1C Co N1B 95.88(16) . . ? N2C Co N1B 167.80(19) . . ? O4 Cl O3 109.78(9) . . ? O4 Cl O1 109.49(9) . . ? O3 Cl O1 109.44(9) . . ? O4 Cl O2 109.51(9) . . ? O3 Cl O2 109.38(9) . . ? O1 Cl O2 109.22(9) . . ? C1A N C1C 119.4(6) . . ? C1A N C1B 119.0(5) . . ? C1C N C1B 118.3(5) . . ? C3A N1A C2A 117.7(7) . . ? C3A N1A Co 115.8(6) . . ? C2A N1A Co 126.5(5) . . ? C4A N2A N3A 106.2(7) . . ? C4A N2A Co 116.3(6) . . ? N3A N2A Co 136.4(6) . . ? C6A N3A N2A 110.5(8) . . ? C3B N1B C2B 119.2(5) . . ? C3B N1B Co 114.5(3) . . ? C2B N1B Co 126.2(4) . . ? N3B N2B C4B 105.9(5) . . ? N3B N2B Co 138.7(4) . . ? C4B N2B Co 114.5(3) . . ? C6B N3B N2B 111.0(5) . . ? C6B N3B H3BB 124.5 . . ? N2B N3B H3BB 124.5 . . ? C3C N1C C2C 118.7(6) . . ? C3C N1C Co 116.0(4) . . ? C2C N1C Co 125.3(4) . . ? C4C N2C N3C 106.8(7) . . ? C4C N2C Co 114.7(4) . . ? N3C N2C Co 137.9(6) . . ? N2C N3C C6C 108.2(7) . . ? N2C N3C H3CB 125.9 . . ? C6C N3C H3CB 125.9 . . ? N C1A C2A 113.0(5) . . ? N C1A H1AA 109.0 . . ? C2A C1A H1AA 109.0 . . ? N C1A H1AB 109.0 . . ? C2A C1A H1AB 109.0 . . ? H1AA C1A H1AB 107.8 . . ? N1A C2A C1A 111.3(6) . . ? N1A C2A H2AA 109.4 . . ? C1A C2A H2AA 109.4 . . ? N1A C2A H2AB 109.4 . . ? C1A C2A H2AB 109.4 . . ? H2AA C2A H2AB 108.0 . . ? N1A C3A C4A 116.4(7) . . ? N1A C3A H3AA 121.8 . . ? C4A C3A H3AA 121.8 . . ? N2A C4A C5A 109.4(8) . . ? N2A C4A C3A 114.1(7) . . ? C5A C4A C3A 136.4(7) . . ? C6A C5A C4A 104.8(8) . . ? C6A C5A H5AA 127.6 . . ? C4A C5A H5AA 127.6 . . ? N3A C6A C5A 109.1(9) . . ? N3A C6A C7A 123.0(10) . . ? C5A C6A C7A 127.9(10) . . ? C6A C7A H7AA 109.5 . . ? C6A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C6A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? N C1B C2B 113.1(5) . . ? N C1B H1BA 109.0 . . ? C2B C1B H1BA 109.0 . . ? N C1B H1BB 109.0 . . ? C2B C1B H1BB 109.0 . . ? H1BA C1B H1BB 107.8 . . ? N1B C2B C1B 109.5(5) . . ? N1B C2B H2BA 109.8 . . ? C1B C2B H2BA 109.8 . . ? N1B C2B H2BB 109.8 . . ? C1B C2B H2BB 109.8 . . ? H2BA C2B H2BB 108.2 . . ? N1B C3B C4B 118.2(5) . . ? N1B C3B H3BA 120.9 . . ? C4B C3B H3BA 120.9 . . ? N2B C4B C5B 109.8(4) . . ? N2B C4B C3B 114.9(5) . . ? C5B C4B C3B 135.3(5) . . ? C6B C5B C4B 103.4(6) . . ? C6B C5B H5BA 128.3 . . ? C4B C5B H5BA 128.3 . . ? N3B C6B C5B 109.8(6) . . ? N3B C6B C7B 122.4(6) . . ? C5B C6B C7B 127.7(8) . . ? C6B C7B H7BA 109.5 . . ? C6B C7B H7BB 109.5 . . ? H7BA C7B H7BB 109.5 . . ? C6B C7B H7BC 109.5 . . ? H7BA C7B H7BC 109.5 . . ? H7BB C7B H7BC 109.5 . . ? N C1C C2C 113.0(6) . . ? N C1C H1CA 109.0 . . ? C2C C1C H1CA 109.0 . . ? N C1C H1CB 109.0 . . ? C2C C1C H1CB 109.0 . . ? H1CA C1C H1CB 107.8 . . ? N1C C2C C1C 110.3(5) . . ? N1C C2C H2CA 109.6 . . ? C1C C2C H2CA 109.6 . . ? N1C C2C H2CB 109.6 . . ? C1C C2C H2CB 109.6 . . ? H2CA C2C H2CB 108.1 . . ? N1C C3C C4C 117.1(6) . . ? N1C C3C H3CA 121.5 . . ? C4C C3C H3CA 121.5 . . ? N2C C4C C5C 109.9(6) . . ? N2C C4C C3C 115.6(5) . . ? C5C C4C C3C 134.5(7) . . ? C6C C5C C4C 105.5(8) . . ? C6C C5C H5CA 127.2 . . ? C4C C5C H5CA 127.2 . . ? C5C C6C N3C 109.5(7) . . ? C5C C6C C7C 136.0(11) . . ? N3C C6C C7C 114.4(9) . . ? C6C C7C H7CA 109.5 . . ? C6C C7C H7CB 109.5 . . ? H7CA C7C H7CB 109.5 . . ? C6C C7C H7CC 109.5 . . ? H7CA C7C H7CC 109.5 . . ? H7CB C7C H7CC 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 N2A Co N1A C3A -0.9(4) . . . . ? N2B Co N1A C3A 38.4(11) . . . . ? N1C Co N1A C3A -173.0(4) . . . . ? N2C Co N1A C3A -96.2(4) . . . . ? N1B Co N1A C3A 90.3(4) . . . . ? N2A Co N1A C2A -178.7(5) . . . . ? N2B Co N1A C2A -139.4(9) . . . . ? N1C Co N1A C2A 9.2(5) . . . . ? N2C Co N1A C2A 86.0(5) . . . . ? N1B Co N1A C2A -87.6(5) . . . . ? N2B Co N2A C4A -169.3(4) . . . . ? N1A Co N2A C4A 4.2(4) . . . . ? N1C Co N2A C4A 56.3(12) . . . . ? N2C Co N2A C4A 96.6(4) . . . . ? N1B Co N2A C4A -92.1(4) . . . . ? N2B Co N2A N3A -3.6(5) . . . . ? N1A Co N2A N3A 169.9(6) . . . . ? N1C Co N2A N3A -137.9(10) . . . . ? N2C Co N2A N3A -97.7(5) . . . . ? N1B Co N2A N3A 73.7(5) . . . . ? C4A N2A N3A C6A 0.8(7) . . . . ? Co N2A N3A C6A -165.9(5) . . . . ? N2A Co N1B C3B -100.0(4) . . . . ? N2B Co N1B C3B -5.5(4) . . . . ? N1A Co N1B C3B -177.3(4) . . . . ? N1C Co N1B C3B 85.2(4) . . . . ? N2C Co N1B C3B 34.7(12) . . . . ? N2A Co N1B C2B 83.7(5) . . . . ? N2B Co N1B C2B 178.2(5) . . . . ? N1A Co N1B C2B 6.4(5) . . . . ? N1C Co N1B C2B -91.1(5) . . . . ? N2C Co N1B C2B -141.6(10) . . . . ? N2A Co N2B N3B -93.3(5) . . . . ? N1A Co N2B N3B -131.5(9) . . . . ? N1C Co N2B N3B 79.6(5) . . . . ? N2C Co N2B N3B 3.0(5) . . . . ? N1B Co N2B N3B 175.2(5) . . . . ? N2A Co N2B C4B 99.5(4) . . . . ? N1A Co N2B C4B 61.3(10) . . . . ? N1C Co N2B C4B -87.6(4) . . . . ? N2C Co N2B C4B -164.1(4) . . . . ? N1B Co N2B C4B 8.0(3) . . . . ? C4B N2B N3B C6B 1.8(7) . . . . ? Co N2B N3B C6B -166.0(4) . . . . ? N2A Co N1C C3C 40.6(12) . . . . ? N2B Co N1C C3C -93.9(4) . . . . ? N1A Co N1C C3C 91.4(4) . . . . ? N2C Co N1C C3C -0.8(4) . . . . ? N1B Co N1C C3C -171.1(4) . . . . ? N2A Co N1C C2C -140.3(10) . . . . ? N2B Co N1C C2C 85.1(4) . . . . ? N1A Co N1C C2C -89.6(5) . . . . ? N2C Co N1C C2C 178.3(5) . . . . ? N1B Co N1C C2C 7.9(5) . . . . ? N2A Co N2C C4C -170.3(4) . . . . ? N2B Co N2C C4C 94.4(4) . . . . ? N1A Co N2C C4C -92.9(5) . . . . ? N1C Co N2C C4C 3.1(4) . . . . ? N1B Co N2C C4C 55.2(12) . . . . ? N2A Co N2C N3C -0.5(7) . . . . ? N2B Co N2C N3C -95.8(6) . . . . ? N1A Co N2C N3C 76.9(7) . . . . ? N1C Co N2C N3C 172.9(7) . . . . ? N1B Co N2C N3C -134.9(10) . . . . ? C4C N2C N3C C6C 0.8(8) . . . . ? Co N2C N3C C6C -169.6(5) . . . . ? C1C N C1A C2A -77.0(9) . . . . ? C1B N C1A C2A 123.7(7) . . . . ? C3A N1A C2A C1A -103.6(7) . . . . ? Co N1A C2A C1A 74.2(7) . . . . ? N C1A C2A N1A -56.0(9) . . . . ? C2A N1A C3A C4A 175.6(5) . . . . ? Co N1A C3A C4A -2.4(6) . . . . ? N3A N2A C4A C5A 0.3(6) . . . . ? Co N2A C4A C5A 170.1(4) . . . . ? N3A N2A C4A C3A -176.4(5) . . . . ? Co N2A C4A C3A -6.6(6) . . . . ? N1A C3A C4A N2A 5.9(8) . . . . ? N1A C3A C4A C5A -169.6(6) . . . . ? N2A C4A C5A C6A -1.2(7) . . . . ? C3A C4A C5A C6A 174.5(7) . . . . ? N2A N3A C6A C5A -1.6(8) . . . . ? N2A N3A C6A C7A 179.4(6) . . . . ? C4A C5A C6A N3A 1.7(8) . . . . ? C4A C5A C6A C7A -179.3(7) . . . . ? C1A N C1B C2B -76.1(7) . . . . ? C1C N C1B C2B 124.3(6) . . . . ? C3B N1B C2B C1B -98.3(6) . . . . ? Co N1B C2B C1B 77.8(6) . . . . ? N C1B C2B N1B -58.2(7) . . . . ? C2B N1B C3B C4B 178.8(5) . . . . ? Co N1B C3B C4B 2.3(6) . . . . ? N3B N2B C4B C5B -0.9(6) . . . . ? Co N2B C4B C5B 170.4(3) . . . . ? N3B N2B C4B C3B 179.3(5) . . . . ? Co N2B C4B C3B -9.4(6) . . . . ? N1B C3B C4B N2B 4.8(7) . . . . ? N1B C3B C4B C5B -175.0(6) . . . . ? N2B C4B C5B C6B -0.3(6) . . . . ? C3B C4B C5B C6B 179.4(6) . . . . ? N2B N3B C6B C5B -2.1(8) . . . . ? N2B N3B C6B C7B -178.9(5) . . . . ? C4B C5B C6B N3B 1.4(7) . . . . ? C4B C5B C6B C7B 178.0(6) . . . . ? C1A N C1C C2C 125.5(7) . . . . ? C1B N C1C C2C -75.0(8) . . . . ? C3C N1C C2C C1C -104.1(6) . . . . ? Co N1C C2C C1C 76.9(7) . . . . ? N C1C C2C N1C -58.3(8) . . . . ? C2C N1C C3C C4C 179.3(5) . . . . ? Co N1C C3C C4C -1.6(7) . . . . ? N3C N2C C4C C5C -0.3(7) . . . . ? Co N2C C4C C5C 172.6(4) . . . . ? N3C N2C C4C C3C -177.8(5) . . . . ? Co N2C C4C C3C -4.9(7) . . . . ? N1C C3C C4C N2C 4.4(8) . . . . ? N1C C3C C4C C5C -172.3(6) . . . . ? N2C C4C C5C C6C -0.3(8) . . . . ? C3C C4C C5C C6C 176.5(7) . . . . ? C4C C5C C6C N3C 0.8(8) . . . . ? C4C C5C C6C C7C 178.3(8) . . . . ? N2C N3C C6C C5C -1.0(9) . . . . ? N2C N3C C6C C7C -179.1(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3B H3BB N3B 0.88 1.92 2.800(10) 173.0 4_656 N3C H3CB N3A 0.88 1.90 2.780(11) 173.4 4_656 C3A H3AA O1 0.95 2.55 3.320(8) 138.4 7_755 C1B H1BA O3 0.99 2.33 3.316(7) 176.3 . C3B H3BA O4 0.95 2.60 3.051(7) 109.7 . C3C H3CA O1 0.95 2.56 3.205(9) 125.1 3_466 C3C H3CA O3 0.95 2.56 3.504(9) 175.9 3_466 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.530 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.066 # 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 0.000 0.384 0.750 293 60 ' ' 2 0.000 0.616 0.250 293 60 ' ' 3 0.500 0.116 0.250 293 60 ' ' 4 0.500 0.884 0.750 293 60 ' ' _platon_squeeze_details ; ;