# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #============================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Ulrich Siemeling' _publ_contact_author_address ; Institute for Chemistry University of Kassel D-34109 Kassel Germany ; _publ_contact_author_phone '+0049 561 804 4576' _publ_contact_author_fax '+0049 561 804 4777' _publ_contact_author_email siemeling@uni-kassel.de _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; The CIF has passed the Chester CHECKCIF routines. ; #===================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #===================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The coordination behaviour of ferrocene-based pyridylphosphine ligands towards Zn^II^, Cd^II^ and Hg^II^ ; loop_ _publ_author_name _publ_author_footnote _publ_author_address U.Siemeling ? ; Institute of Chemistry University of Kassel D-34109 Kassel Germany ; T.Klemann ? ; Institute of Chemistry University of Kassel D-34109 Kassel Germany ; C.Bruhn ? ; Institute of Chemistry University of Kassel D-34109 Kassel Germany ; J.Schulz ? ; Department of Inorganic Chemistry Faculty of Science Charles University in Prague Hlavova 2030 12840 Prague Czech Republic ; P.Stepnicka ? ; Department of Inorganic Chemistry Faculty of Science Charles University in Prague Hlavova 2030 12840 Prague Czech Republic ; #====================================================================== data_i0540a _database_code_depnum_ccdc_archive 'CCDC 805316' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H22 Fe N P' _chemical_formula_weight 447.28 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' 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 10.1437(9) _cell_length_b 11.0401(9) _cell_length_c 10.9432(9) _cell_angle_alpha 72.013(6) _cell_angle_beta 85.964(7) _cell_angle_gamma 66.324(6) _cell_volume 1065.47(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14638 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 25.66 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7162 _exptl_absorpt_correction_T_max 0.8225 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 420 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 9178 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.22 _reflns_number_total 3636 _reflns_number_gt 3430 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.2552P] 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 3636 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.06783(17) 0.23204(16) 0.96753(14) 0.0315(3) Uani 1 1 d . . . C2 C 0.16911(18) 0.24069(18) 1.04667(15) 0.0375(4) Uani 1 1 d . . . H2A H 0.1507 0.3101 1.0845 0.045 Uiso 1 1 calc R . . C3 C 0.30269(19) 0.12424(19) 1.05696(16) 0.0440(4) Uani 1 1 d . . . H3A H 0.3862 0.1043 1.1033 0.053 Uiso 1 1 calc R . . C4 C 0.28632(19) 0.04406(17) 0.98439(17) 0.0430(4) Uani 1 1 d . . . H4A H 0.3573 -0.0373 0.9747 0.052 Uiso 1 1 calc R . . C5 C 0.14210(18) 0.10972(16) 0.92877(16) 0.0359(4) Uani 1 1 d . . . H5A H 0.1030 0.0787 0.8765 0.043 Uiso 1 1 calc R . . C6 C 0.25829(17) 0.28926(16) 0.67131(14) 0.0320(3) Uani 1 1 d . . . C7 C 0.16725(19) 0.41059(16) 0.70565(15) 0.0362(4) Uani 1 1 d . . . H7A H 0.0706 0.4643 0.6790 0.043 Uiso 1 1 calc R . . C8 C 0.2508(2) 0.43437(19) 0.78765(17) 0.0451(4) Uani 1 1 d . . . H8A H 0.2184 0.5068 0.8234 0.054 Uiso 1 1 calc R . . C9 C 0.3920(2) 0.3284(2) 0.80548(17) 0.0455(4) Uani 1 1 d . . . H9A H 0.4681 0.3194 0.8550 0.055 Uiso 1 1 calc R . . C10 C 0.39738(18) 0.23832(18) 0.73492(16) 0.0374(4) Uani 1 1 d . . . H10A H 0.4773 0.1599 0.7307 0.045 Uiso 1 1 calc R . . C11 C 0.22229(17) 0.23342(15) 0.57863(14) 0.0304(3) Uani 1 1 d . . . C12 C 0.07950(18) 0.27194(17) 0.53750(15) 0.0363(4) Uani 1 1 d . . . H12A H 0.0035 0.3287 0.5736 0.044 Uiso 1 1 calc R . . C13 C 0.05271(19) 0.22487(18) 0.44309(16) 0.0398(4) Uani 1 1 d . . . H13A H -0.0414 0.2499 0.4141 0.048 Uiso 1 1 calc R . . C14 C 0.1685(2) 0.13942(18) 0.39180(16) 0.0416(4) Uani 1 1 d . . . H14A H 0.1535 0.1075 0.3269 0.050 Uiso 1 1 calc R . . C15 C 0.30642(19) 0.10279(18) 0.43924(16) 0.0411(4) Uani 1 1 d . . . H15A H 0.3834 0.0433 0.4064 0.049 Uiso 1 1 calc R . . C16 C -0.20918(17) 0.28098(15) 1.06382(14) 0.0303(3) Uani 1 1 d . . . C17 C -0.13996(19) 0.17905(17) 1.17764(16) 0.0387(4) Uani 1 1 d . . . H17A H -0.0398 0.1411 1.1873 0.046 Uiso 1 1 calc R . . C18 C -0.2182(2) 0.1330(2) 1.27727(17) 0.0480(4) Uani 1 1 d . . . H18A H -0.1699 0.0648 1.3527 0.058 Uiso 1 1 calc R . . C19 C -0.3676(2) 0.1879(2) 1.26499(19) 0.0492(4) Uani 1 1 d . . . H19A H -0.4198 0.1582 1.3322 0.059 Uiso 1 1 calc R . . C20 C -0.4383(2) 0.2880(2) 1.15085(19) 0.0470(4) Uani 1 1 d . . . H20A H -0.5384 0.3241 1.1408 0.056 Uiso 1 1 calc R . . C21 C -0.36022(18) 0.33439(17) 1.05178(16) 0.0374(4) Uani 1 1 d . . . H21A H -0.4088 0.4020 0.9762 0.045 Uiso 1 1 calc R . . C22 C -0.18698(16) 0.34521(16) 0.79471(14) 0.0315(3) Uani 1 1 d . . . C23 C -0.25036(17) 0.46516(18) 0.69028(16) 0.0381(4) Uani 1 1 d . . . H23A H -0.2513 0.5491 0.6924 0.046 Uiso 1 1 calc R . . C24 C -0.31200(18) 0.4600(2) 0.58334(17) 0.0477(5) Uani 1 1 d . . . H24A H -0.3553 0.5407 0.5151 0.057 Uiso 1 1 calc R . . C25 C -0.30903(19) 0.3359(2) 0.57829(18) 0.0512(5) Uani 1 1 d . . . H25A H -0.3483 0.3323 0.5059 0.061 Uiso 1 1 calc R . . C26 C -0.2471(2) 0.2159(2) 0.68171(19) 0.0467(4) Uani 1 1 d . . . H26A H -0.2453 0.1322 0.6783 0.056 Uiso 1 1 calc R . . C27 C -0.18804(17) 0.22044(17) 0.78998(16) 0.0366(4) Uani 1 1 d . . . H27A H -0.1490 0.1403 0.8596 0.044 Uiso 1 1 calc R . . N N 0.33518(15) 0.14861(14) 0.53046(13) 0.0372(3) Uani 1 1 d . . . P P -0.11612(4) 0.36315(4) 0.93517(4) 0.03074(11) Uani 1 1 d . . . Fe Fe 0.24277(2) 0.24364(2) 0.868141(19) 0.03011(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0322(8) 0.0318(7) 0.0294(7) -0.0081(6) 0.0049(6) -0.0133(6) C2 0.0370(8) 0.0475(9) 0.0280(8) -0.0102(7) 0.0032(7) -0.0182(7) C3 0.0336(9) 0.0536(10) 0.0320(8) -0.0012(7) -0.0016(7) -0.0130(8) C4 0.0339(9) 0.0329(8) 0.0467(10) 0.0006(7) 0.0070(8) -0.0083(7) C5 0.0354(8) 0.0295(8) 0.0409(8) -0.0083(6) 0.0064(7) -0.0135(7) C6 0.0335(8) 0.0324(8) 0.0287(7) -0.0070(6) 0.0059(6) -0.0142(6) C7 0.0448(9) 0.0288(7) 0.0312(8) -0.0055(6) 0.0048(7) -0.0140(7) C8 0.0658(12) 0.0411(9) 0.0393(9) -0.0145(7) 0.0110(9) -0.0319(9) C9 0.0494(10) 0.0599(11) 0.0400(9) -0.0152(8) 0.0057(8) -0.0352(9) C10 0.0323(8) 0.0463(9) 0.0344(8) -0.0101(7) 0.0054(7) -0.0188(7) C11 0.0311(7) 0.0284(7) 0.0262(7) -0.0044(6) 0.0031(6) -0.0097(6) C12 0.0322(8) 0.0357(8) 0.0344(8) -0.0105(6) 0.0016(7) -0.0071(7) C13 0.0356(8) 0.0410(9) 0.0364(8) -0.0096(7) -0.0053(7) -0.0095(7) C14 0.0488(10) 0.0416(9) 0.0323(8) -0.0136(7) -0.0007(8) -0.0139(8) C15 0.0396(9) 0.0416(9) 0.0380(9) -0.0167(7) 0.0066(7) -0.0094(7) C16 0.0342(8) 0.0277(7) 0.0311(7) -0.0127(6) 0.0049(6) -0.0123(6) C17 0.0372(8) 0.0401(9) 0.0367(8) -0.0091(7) 0.0010(7) -0.0151(7) C18 0.0557(11) 0.0458(10) 0.0365(9) -0.0028(7) 0.0038(8) -0.0218(9) C19 0.0533(11) 0.0489(10) 0.0471(10) -0.0122(8) 0.0199(9) -0.0268(9) C20 0.0375(9) 0.0478(10) 0.0550(11) -0.0183(8) 0.0111(8) -0.0159(8) C21 0.0337(8) 0.0357(8) 0.0382(8) -0.0107(7) 0.0046(7) -0.0101(7) C22 0.0265(7) 0.0349(8) 0.0299(7) -0.0080(6) 0.0040(6) -0.0107(6) C23 0.0295(8) 0.0385(9) 0.0364(8) -0.0025(7) 0.0055(7) -0.0111(7) C24 0.0296(8) 0.0649(12) 0.0326(8) 0.0016(8) -0.0001(7) -0.0148(8) C25 0.0336(9) 0.0868(15) 0.0372(9) -0.0216(9) 0.0028(8) -0.0262(10) C26 0.0375(9) 0.0602(11) 0.0532(11) -0.0278(9) 0.0057(8) -0.0229(9) C27 0.0317(8) 0.0377(8) 0.0392(9) -0.0106(7) 0.0020(7) -0.0136(7) N 0.0327(7) 0.0386(7) 0.0364(7) -0.0139(6) 0.0046(6) -0.0090(6) P 0.0313(2) 0.0273(2) 0.0321(2) -0.00890(15) 0.00305(16) -0.01050(16) Fe 0.02995(14) 0.03169(14) 0.02818(14) -0.00806(9) 0.00257(9) -0.01281(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.436(2) . ? C1 C2 1.439(2) . ? C1 P 1.8192(16) . ? C1 Fe 2.0428(16) . ? C2 C3 1.426(2) . ? C2 Fe 2.0374(17) . ? C2 H2A 0.9300 . ? C3 C4 1.419(3) . ? C3 Fe 2.0561(16) . ? C3 H3A 0.9300 . ? C4 C5 1.427(2) . ? C4 Fe 2.0579(16) . ? C4 H4A 0.9300 . ? C5 Fe 2.0446(16) . ? C5 H5A 0.9300 . ? C6 C10 1.432(2) . ? C6 C7 1.434(2) . ? C6 C11 1.470(2) . ? C6 Fe 2.0649(15) . ? C7 C8 1.422(2) . ? C7 Fe 2.0444(15) . ? C7 H7A 0.9300 . ? C8 C9 1.418(3) . ? C8 Fe 2.0489(17) . ? C8 H8A 0.9300 . ? C9 C10 1.418(3) . ? C9 Fe 2.0568(18) . ? C9 H9A 0.9300 . ? C10 Fe 2.0605(17) . ? C10 H10A 0.9300 . ? C11 N 1.351(2) . ? C11 C12 1.400(2) . ? C12 C13 1.377(2) . ? C12 H12A 0.9300 . ? C13 C14 1.389(3) . ? C13 H13A 0.9300 . ? C14 C15 1.382(2) . ? C14 H14A 0.9300 . ? C15 N 1.345(2) . ? C15 H15A 0.9300 . ? C16 C17 1.391(2) . ? C16 C21 1.403(2) . ? C16 P 1.8461(16) . ? C17 C18 1.392(3) . ? C17 H17A 0.9300 . ? C18 C19 1.387(3) . ? C18 H18A 0.9300 . ? C19 C20 1.390(3) . ? C19 H19A 0.9300 . ? C20 C21 1.388(3) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.399(2) . ? C22 C23 1.399(2) . ? C22 P 1.8376(16) . ? C23 C24 1.392(3) . ? C23 H23A 0.9300 . ? C24 C25 1.376(3) . ? C24 H24A 0.9300 . ? C25 C26 1.392(3) . ? C25 H25A 0.9300 . ? C26 C27 1.388(2) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? 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 C5 C1 C2 107.14(14) . . ? C5 C1 P 132.51(12) . . ? C2 C1 P 120.35(12) . . ? C5 C1 Fe 69.49(9) . . ? C2 C1 Fe 69.15(9) . . ? P C1 Fe 126.42(8) . . ? C3 C2 C1 108.13(15) . . ? C3 C2 Fe 70.31(10) . . ? C1 C2 Fe 69.56(9) . . ? C3 C2 H2A 125.9 . . ? C1 C2 H2A 125.9 . . ? Fe C2 H2A 125.8 . . ? C4 C3 C2 108.29(15) . . ? C4 C3 Fe 69.89(9) . . ? C2 C3 Fe 68.90(9) . . ? C4 C3 H3A 125.9 . . ? C2 C3 H3A 125.9 . . ? Fe C3 H3A 126.9 . . ? C3 C4 C5 108.24(15) . . ? C3 C4 Fe 69.76(10) . . ? C5 C4 Fe 69.14(9) . . ? C3 C4 H4A 125.9 . . ? C5 C4 H4A 125.9 . . ? Fe C4 H4A 126.8 . . ? C4 C5 C1 108.19(15) . . ? C4 C5 Fe 70.14(10) . . ? C1 C5 Fe 69.36(9) . . ? C4 C5 H5A 125.9 . . ? C1 C5 H5A 125.9 . . ? Fe C5 H5A 126.2 . . ? C10 C6 C7 107.35(14) . . ? C10 C6 C11 125.29(15) . . ? C7 C6 C11 127.12(14) . . ? C10 C6 Fe 69.52(9) . . ? C7 C6 Fe 68.81(9) . . ? C11 C6 Fe 131.22(11) . . ? C8 C7 C6 108.00(15) . . ? C8 C7 Fe 69.84(9) . . ? C6 C7 Fe 70.34(8) . . ? C8 C7 H7A 126.0 . . ? C6 C7 H7A 126.0 . . ? Fe C7 H7A 125.4 . . ? C9 C8 C7 108.14(16) . . ? C9 C8 Fe 70.09(10) . . ? C7 C8 Fe 69.49(9) . . ? C9 C8 H8A 125.9 . . ? C7 C8 H8A 125.9 . . ? Fe C8 H8A 126.1 . . ? C8 C9 C10 108.43(16) . . ? C8 C9 Fe 69.50(11) . . ? C10 C9 Fe 69.99(10) . . ? C8 C9 H9A 125.8 . . ? C10 C9 H9A 125.8 . . ? Fe C9 H9A 126.3 . . ? C9 C10 C6 108.08(16) . . ? C9 C10 Fe 69.71(11) . . ? C6 C10 Fe 69.86(10) . . ? C9 C10 H10A 126.0 . . ? C6 C10 H10A 126.0 . . ? Fe C10 H10A 126.0 . . ? N C11 C12 121.96(15) . . ? N C11 C6 116.08(14) . . ? C12 C11 C6 121.88(15) . . ? C13 C12 C11 119.32(16) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C14 118.94(16) . . ? C12 C13 H13A 120.5 . . ? C14 C13 H13A 120.5 . . ? C15 C14 C13 118.62(16) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? N C15 C14 123.44(16) . . ? N C15 H15A 118.3 . . ? C14 C15 H15A 118.3 . . ? C17 C16 C21 117.91(15) . . ? C17 C16 P 123.88(13) . . ? C21 C16 P 117.88(12) . . ? C16 C17 C18 121.06(16) . . ? C16 C17 H17A 119.5 . . ? C18 C17 H17A 119.5 . . ? C19 C18 C17 120.53(17) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 119.11(18) . . ? C18 C19 H19A 120.4 . . ? C20 C19 H19A 120.4 . . ? C21 C20 C19 120.30(17) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C16 121.07(15) . . ? C20 C21 H21A 119.5 . . ? C16 C21 H21A 119.5 . . ? C27 C22 C23 118.71(15) . . ? C27 C22 P 123.53(11) . . ? C23 C22 P 117.67(13) . . ? C24 C23 C22 120.59(17) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C25 C24 C23 120.18(16) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 119.87(17) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C27 C26 C25 120.42(19) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C26 C27 C22 120.19(16) . . ? C26 C27 H27A 119.9 . . ? C22 C27 H27A 119.9 . . ? C15 N C11 117.69(14) . . ? C1 P C22 105.33(7) . . ? C1 P C16 101.12(7) . . ? C22 P C16 100.07(7) . . ? C2 Fe C1 41.29(6) . . ? C2 Fe C7 124.96(7) . . ? C1 Fe C7 107.16(7) . . ? C2 Fe C5 69.04(7) . . ? C1 Fe C5 41.14(6) . . ? C7 Fe C5 120.83(7) . . ? C2 Fe C8 105.94(7) . . ? C1 Fe C8 118.83(7) . . ? C7 Fe C8 40.67(7) . . ? C5 Fe C8 154.84(8) . . ? C2 Fe C3 40.78(7) . . ? C1 Fe C3 68.93(7) . . ? C7 Fe C3 162.17(8) . . ? C5 Fe C3 68.43(7) . . ? C8 Fe C3 124.71(8) . . ? C2 Fe C9 118.29(7) . . ? C1 Fe C9 153.28(7) . . ? C7 Fe C9 68.22(7) . . ? C5 Fe C9 163.92(8) . . ? C8 Fe C9 40.41(8) . . ? C3 Fe C9 106.99(7) . . ? C2 Fe C4 68.54(7) . . ? C1 Fe C4 68.89(7) . . ? C7 Fe C4 156.12(8) . . ? C5 Fe C4 40.72(7) . . ? C8 Fe C4 162.27(8) . . ? C3 Fe C4 40.34(8) . . ? C9 Fe C4 126.03(7) . . ? C2 Fe C10 153.28(7) . . ? C1 Fe C10 164.69(7) . . ? C7 Fe C10 68.46(7) . . ? C5 Fe C10 127.37(7) . . ? C8 Fe C10 68.10(8) . . ? C3 Fe C10 119.79(7) . . ? C9 Fe C10 40.31(7) . . ? C4 Fe C10 108.80(7) . . ? C2 Fe C6 163.55(7) . . ? C1 Fe C6 126.65(6) . . ? C7 Fe C6 40.85(6) . . ? C5 Fe C6 109.16(7) . . ? C8 Fe C6 68.36(7) . . ? C3 Fe C6 155.08(7) . . ? C9 Fe C6 68.08(7) . . ? C4 Fe C6 121.49(7) . . ? C10 Fe C6 40.62(6) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.22 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.311 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.038 #====================================================================== data_i0697a _database_code_depnum_ccdc_archive 'CCDC 805317' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Fe N P' _chemical_formula_sum 'C28 H24 Fe N P' _chemical_formula_weight 461.30 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' 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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4956(11) _cell_length_b 10.9419(13) _cell_length_c 13.4071(15) _cell_angle_alpha 67.813(9) _cell_angle_beta 75.752(9) _cell_angle_gamma 84.294(10) _cell_volume 1118.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14403 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 25.79 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7248 _exptl_absorpt_correction_T_max 0.8761 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 218 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 8622 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3867 _reflns_number_gt 3663 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.3257P] 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 3867 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.056 _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 C1 C 0.1481(2) 0.29025(17) 0.26020(14) 0.0249(3) Uani 1 1 d . . . C2 C 0.3077(2) 0.30982(17) 0.18792(13) 0.0258(4) Uani 1 1 d . . . H2A H 0.3643 0.2500 0.1552 0.031 Uiso 1 1 calc R . . C3 C 0.3663(2) 0.43498(17) 0.17389(14) 0.0293(4) Uani 1 1 d . . . H3A H 0.4687 0.4722 0.1307 0.035 Uiso 1 1 calc R . . C4 C 0.2440(2) 0.49412(17) 0.23624(15) 0.0304(4) Uani 1 1 d . . . H4A H 0.2506 0.5777 0.2413 0.036 Uiso 1 1 calc R . . C5 C 0.1098(2) 0.40523(17) 0.28974(15) 0.0281(4) Uani 1 1 d . . . H5A H 0.0122 0.4196 0.3368 0.034 Uiso 1 1 calc R . . C6 C 0.2781(2) 0.28880(17) 0.50288(14) 0.0263(4) Uani 1 1 d . . . C7 C 0.2839(2) 0.16353(17) 0.49023(14) 0.0289(4) Uani 1 1 d . . . H7A H 0.1996 0.1000 0.5222 0.035 Uiso 1 1 calc R . . C8 C 0.4371(2) 0.15039(18) 0.42169(14) 0.0312(4) Uani 1 1 d . . . H8A H 0.4722 0.0776 0.3993 0.037 Uiso 1 1 calc R . . C9 C 0.5284(2) 0.26709(19) 0.39271(15) 0.0303(4) Uani 1 1 d . . . H9A H 0.6353 0.2849 0.3479 0.036 Uiso 1 1 calc R . . C10 C 0.4313(2) 0.35202(18) 0.44268(14) 0.0276(4) Uani 1 1 d . . . H10A H 0.4625 0.4358 0.4371 0.033 Uiso 1 1 calc R . . C11 C 0.1378(2) 0.34492(19) 0.56665(15) 0.0309(4) Uani 1 1 d . . . H11A H 0.0370 0.2989 0.5770 0.037 Uiso 1 1 calc R . . H11B H 0.1241 0.4395 0.5228 0.037 Uiso 1 1 calc R . . C12 C 0.1611(2) 0.33153(17) 0.67921(14) 0.0263(4) Uani 1 1 d . . . C13 C 0.0761(2) 0.23826(18) 0.77676(15) 0.0313(4) Uani 1 1 d . . . H13A H 0.0035 0.1795 0.7741 0.038 Uiso 1 1 calc R . . C14 C 0.0985(2) 0.23208(19) 0.87784(16) 0.0354(4) Uani 1 1 d . . . H14A H 0.0414 0.1694 0.9451 0.042 Uiso 1 1 calc R . . C15 C 0.2062(2) 0.31970(19) 0.87864(15) 0.0331(4) Uani 1 1 d . . . H15A H 0.2244 0.3183 0.9462 0.040 Uiso 1 1 calc R . . C16 C 0.2863(2) 0.40927(18) 0.77749(15) 0.0309(4) Uani 1 1 d . . . H16A H 0.3595 0.4691 0.7780 0.037 Uiso 1 1 calc R . . C17 C 0.1576(2) 0.02439(16) 0.27637(14) 0.0252(3) Uani 1 1 d . . . C18 C 0.2144(2) -0.07547(18) 0.36175(16) 0.0325(4) Uani 1 1 d . . . H18A H 0.1759 -0.0799 0.4358 0.039 Uiso 1 1 calc R . . C19 C 0.3275(3) -0.1689(2) 0.33870(18) 0.0403(5) Uani 1 1 d . . . H19A H 0.3663 -0.2360 0.3969 0.048 Uiso 1 1 calc R . . C20 C 0.3829(2) -0.1633(2) 0.23052(19) 0.0394(5) Uani 1 1 d . . . H20A H 0.4598 -0.2266 0.2149 0.047 Uiso 1 1 calc R . . C22 C 0.2140(2) 0.02827(17) 0.16768(15) 0.0276(4) Uani 1 1 d . . . H22A H 0.1756 0.0951 0.1091 0.033 Uiso 1 1 calc R . . C23 C -0.1019(2) 0.19347(17) 0.20393(14) 0.0244(3) Uani 1 1 d . . . C24 C -0.2040(2) 0.09742(18) 0.20706(15) 0.0291(4) Uani 1 1 d . . . H24A H -0.2068 0.0113 0.2620 0.035 Uiso 1 1 calc R . . C25 C -0.3010(2) 0.12721(19) 0.13050(16) 0.0319(4) Uani 1 1 d . . . H25A H -0.3682 0.0612 0.1331 0.038 Uiso 1 1 calc R . . C26 C -0.2992(2) 0.25393(19) 0.05013(15) 0.0316(4) Uani 1 1 d . . . H26A H -0.3641 0.2741 -0.0026 0.038 Uiso 1 1 calc R . . C27 C -0.2016(2) 0.35050(18) 0.04781(15) 0.0304(4) Uani 1 1 d . . . H27A H -0.2017 0.4372 -0.0060 0.036 Uiso 1 1 calc R . . C28 C -0.1038(2) 0.32097(17) 0.12385(14) 0.0269(4) Uani 1 1 d . . . H28A H -0.0379 0.3878 0.1214 0.032 Uiso 1 1 calc R . . N1 N 0.26636(18) 0.41627(15) 0.67916(12) 0.0293(3) Uani 1 1 d . . . P1 P 0.01500(5) 0.14829(4) 0.31230(3) 0.02386(13) Uani 1 1 d . . . Fe1 Fe 0.31494(3) 0.31497(2) 0.338882(18) 0.02337(11) Uani 1 1 d . . . C21 C 0.3262(2) -0.06557(19) 0.14499(16) 0.0331(4) Uani 1 1 d . . . H21A H 0.3637 -0.0626 0.0713 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0274(8) 0.0261(8) 0.0246(8) -0.0098(7) -0.0116(7) 0.0007(7) C2 0.0291(9) 0.0274(8) 0.0238(8) -0.0098(7) -0.0095(7) -0.0017(7) C3 0.0354(10) 0.0276(9) 0.0249(8) -0.0042(7) -0.0134(7) -0.0055(7) C4 0.0401(10) 0.0232(8) 0.0326(9) -0.0083(7) -0.0200(8) 0.0011(7) C5 0.0302(9) 0.0279(9) 0.0321(9) -0.0129(7) -0.0165(7) 0.0050(7) C6 0.0292(9) 0.0299(9) 0.0228(8) -0.0098(7) -0.0112(7) 0.0007(7) C7 0.0364(10) 0.0263(8) 0.0242(8) -0.0056(7) -0.0124(7) -0.0016(7) C8 0.0416(10) 0.0282(9) 0.0261(9) -0.0097(7) -0.0156(8) 0.0085(8) C9 0.0261(9) 0.0404(10) 0.0261(8) -0.0118(8) -0.0116(7) 0.0049(7) C10 0.0298(9) 0.0305(9) 0.0257(8) -0.0103(7) -0.0119(7) -0.0012(7) C11 0.0274(9) 0.0384(10) 0.0317(9) -0.0167(8) -0.0094(7) 0.0013(7) C12 0.0237(8) 0.0282(8) 0.0302(9) -0.0144(7) -0.0070(7) 0.0030(7) C13 0.0297(9) 0.0292(9) 0.0363(10) -0.0146(8) -0.0047(8) -0.0031(7) C14 0.0368(10) 0.0353(10) 0.0291(9) -0.0090(8) -0.0022(8) -0.0024(8) C15 0.0368(10) 0.0382(10) 0.0287(9) -0.0164(8) -0.0099(8) 0.0033(8) C16 0.0315(9) 0.0315(9) 0.0347(9) -0.0159(8) -0.0104(8) -0.0006(7) C17 0.0258(8) 0.0234(8) 0.0297(9) -0.0109(7) -0.0094(7) -0.0021(6) C18 0.0386(10) 0.0293(9) 0.0334(9) -0.0119(8) -0.0147(8) 0.0005(8) C19 0.0460(12) 0.0312(10) 0.0506(12) -0.0153(9) -0.0266(10) 0.0099(9) C20 0.0312(10) 0.0339(10) 0.0615(13) -0.0262(10) -0.0136(9) 0.0048(8) C22 0.0286(9) 0.0275(8) 0.0292(9) -0.0115(7) -0.0084(7) -0.0025(7) C23 0.0230(8) 0.0276(8) 0.0246(8) -0.0122(7) -0.0049(6) 0.0011(7) C24 0.0289(9) 0.0285(9) 0.0306(9) -0.0103(7) -0.0081(7) -0.0011(7) C25 0.0282(9) 0.0357(10) 0.0367(10) -0.0152(8) -0.0112(8) -0.0045(7) C26 0.0284(9) 0.0396(10) 0.0312(9) -0.0146(8) -0.0130(7) 0.0024(7) C27 0.0323(9) 0.0303(9) 0.0283(9) -0.0092(7) -0.0094(7) 0.0009(7) C28 0.0252(8) 0.0285(9) 0.0285(8) -0.0116(7) -0.0067(7) -0.0008(7) N1 0.0294(8) 0.0297(8) 0.0300(8) -0.0110(6) -0.0080(6) -0.0025(6) P1 0.0254(2) 0.0250(2) 0.0229(2) -0.00968(18) -0.00694(17) -0.00038(17) Fe1 0.02678(16) 0.02252(16) 0.02311(16) -0.00842(11) -0.00989(11) 0.00049(10) C21 0.0304(9) 0.0354(10) 0.0388(10) -0.0215(8) -0.0028(8) -0.0046(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.441(2) . ? C1 C2 1.441(2) . ? C1 P1 1.8220(18) . ? C1 Fe1 2.0551(17) . ? C2 C3 1.433(2) . ? C2 Fe1 2.0620(17) . ? C2 H2A 0.9500 . ? C3 C4 1.430(3) . ? C3 Fe1 2.0622(17) . ? C3 H3A 0.9500 . ? C4 C5 1.432(3) . ? C4 Fe1 2.0580(17) . ? C4 H4A 0.9500 . ? C5 Fe1 2.0437(18) . ? C5 H5A 0.9500 . ? C6 C10 1.436(3) . ? C6 C7 1.438(2) . ? C6 C11 1.510(2) . ? C6 Fe1 2.0538(17) . ? C7 C8 1.426(3) . ? C7 Fe1 2.0535(17) . ? C7 H7A 0.9500 . ? C8 C9 1.434(3) . ? C8 Fe1 2.0585(18) . ? C8 H8A 0.9500 . ? C9 C10 1.428(3) . ? C9 Fe1 2.0622(18) . ? C9 H9A 0.9500 . ? C10 Fe1 2.0642(17) . ? C10 H10A 0.9500 . ? C11 C12 1.521(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N1 1.350(2) . ? C12 C13 1.396(3) . ? C13 C14 1.390(3) . ? C13 H13A 0.9500 . ? C14 C15 1.394(3) . ? C14 H14A 0.9500 . ? C15 C16 1.392(3) . ? C15 H15A 0.9500 . ? C16 N1 1.343(2) . ? C16 H16A 0.9500 . ? C17 C18 1.400(3) . ? C17 C22 1.403(2) . ? C17 P1 1.8487(18) . ? C18 C19 1.400(3) . ? C18 H18A 0.9500 . ? C19 C20 1.390(3) . ? C19 H19A 0.9500 . ? C20 C21 1.390(3) . ? C20 H20A 0.9500 . ? C22 C21 1.398(3) . ? C22 H22A 0.9500 . ? C23 C28 1.404(2) . ? C23 C24 1.410(2) . ? C23 P1 1.8471(18) . ? C24 C25 1.396(3) . ? C24 H24A 0.9500 . ? C25 C26 1.397(3) . ? C25 H25A 0.9500 . ? C26 C27 1.393(3) . ? C26 H26A 0.9500 . ? C27 C28 1.396(3) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C21 H21A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 107.10(15) . . ? C5 C1 P1 123.99(14) . . ? C2 C1 P1 128.87(13) . . ? C5 C1 Fe1 68.99(9) . . ? C2 C1 Fe1 69.76(9) . . ? P1 C1 Fe1 124.72(9) . . ? C3 C2 C1 108.28(15) . . ? C3 C2 Fe1 69.67(9) . . ? C1 C2 Fe1 69.25(9) . . ? C3 C2 H2A 125.9 . . ? C1 C2 H2A 125.9 . . ? Fe1 C2 H2A 126.8 . . ? C4 C3 C2 108.17(16) . . ? C4 C3 Fe1 69.54(10) . . ? C2 C3 Fe1 69.65(10) . . ? C4 C3 H3A 125.9 . . ? C2 C3 H3A 125.9 . . ? Fe1 C3 H3A 126.5 . . ? C3 C4 C5 107.98(15) . . ? C3 C4 Fe1 69.86(10) . . ? C5 C4 Fe1 69.03(10) . . ? C3 C4 H4A 126.0 . . ? C5 C4 H4A 126.0 . . ? Fe1 C4 H4A 126.7 . . ? C4 C5 C1 108.47(16) . . ? C4 C5 Fe1 70.10(10) . . ? C1 C5 Fe1 69.84(10) . . ? C4 C5 H5A 125.8 . . ? C1 C5 H5A 125.8 . . ? Fe1 C5 H5A 125.9 . . ? C10 C6 C7 107.24(16) . . ? C10 C6 C11 125.93(16) . . ? C7 C6 C11 126.83(16) . . ? C10 C6 Fe1 69.98(10) . . ? C7 C6 Fe1 69.49(10) . . ? C11 C6 Fe1 125.44(12) . . ? C8 C7 C6 108.72(16) . . ? C8 C7 Fe1 69.91(10) . . ? C6 C7 Fe1 69.52(10) . . ? C8 C7 H7A 125.6 . . ? C6 C7 H7A 125.6 . . ? Fe1 C7 H7A 126.5 . . ? C7 C8 C9 107.50(16) . . ? C7 C8 Fe1 69.53(10) . . ? C9 C8 Fe1 69.77(10) . . ? C7 C8 H8A 126.2 . . ? C9 C8 H8A 126.2 . . ? Fe1 C8 H8A 126.0 . . ? C10 C9 C8 108.42(16) . . ? C10 C9 Fe1 69.83(10) . . ? C8 C9 Fe1 69.49(10) . . ? C10 C9 H9A 125.8 . . ? C8 C9 H9A 125.8 . . ? Fe1 C9 H9A 126.5 . . ? C9 C10 C6 108.10(16) . . ? C9 C10 Fe1 69.68(10) . . ? C6 C10 Fe1 69.20(10) . . ? C9 C10 H10A 126.0 . . ? C6 C10 H10A 126.0 . . ? Fe1 C10 H10A 126.7 . . ? C6 C11 C12 112.93(15) . . ? C6 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? C6 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? N1 C12 C13 122.22(16) . . ? N1 C12 C11 116.19(16) . . ? C13 C12 C11 121.58(16) . . ? C14 C13 C12 119.46(17) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C13 C14 C15 118.74(17) . . ? C13 C14 H14A 120.6 . . ? C15 C14 H14A 120.6 . . ? C16 C15 C14 118.00(17) . . ? C16 C15 H15A 121.0 . . ? C14 C15 H15A 121.0 . . ? N1 C16 C15 123.99(17) . . ? N1 C16 H16A 118.0 . . ? C15 C16 H16A 118.0 . . ? C18 C17 C22 119.00(16) . . ? C18 C17 P1 117.99(13) . . ? C22 C17 P1 122.99(13) . . ? C17 C18 C19 120.43(18) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C20 C19 C18 119.90(18) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 120.32(17) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C21 C22 C17 120.44(17) . . ? C21 C22 H22A 119.8 . . ? C17 C22 H22A 119.8 . . ? C28 C23 C24 118.30(16) . . ? C28 C23 P1 123.44(13) . . ? C24 C23 P1 118.08(13) . . ? C25 C24 C23 120.87(17) . . ? C25 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C24 C25 C26 120.07(17) . . ? C24 C25 H25A 120.0 . . ? C26 C25 H25A 120.0 . . ? C27 C26 C25 119.58(17) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 120.55(17) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C27 C28 C23 120.61(16) . . ? C27 C28 H28A 119.7 . . ? C23 C28 H28A 119.7 . . ? C16 N1 C12 117.60(16) . . ? C1 P1 C23 101.20(8) . . ? C1 P1 C17 100.81(8) . . ? C23 P1 C17 100.83(8) . . ? C5 Fe1 C7 117.09(8) . . ? C5 Fe1 C6 106.17(7) . . ? C7 Fe1 C6 40.99(7) . . ? C5 Fe1 C1 41.17(7) . . ? C7 Fe1 C1 107.43(7) . . ? C6 Fe1 C1 127.11(7) . . ? C5 Fe1 C4 40.87(7) . . ? C7 Fe1 C4 150.61(8) . . ? C6 Fe1 C4 116.51(7) . . ? C1 Fe1 C4 69.05(7) . . ? C5 Fe1 C8 151.18(8) . . ? C7 Fe1 C8 40.57(8) . . ? C6 Fe1 C8 68.94(7) . . ? C1 Fe1 C8 117.93(7) . . ? C4 Fe1 C8 167.21(8) . . ? C5 Fe1 C2 68.77(7) . . ? C7 Fe1 C2 128.94(7) . . ? C6 Fe1 C2 166.44(7) . . ? C1 Fe1 C2 40.99(7) . . ? C4 Fe1 C2 68.50(7) . . ? C8 Fe1 C2 109.04(7) . . ? C5 Fe1 C9 165.89(7) . . ? C7 Fe1 C9 68.16(7) . . ? C6 Fe1 C9 68.57(7) . . ? C1 Fe1 C9 152.30(7) . . ? C4 Fe1 C9 128.51(8) . . ? C8 Fe1 C9 40.74(8) . . ? C2 Fe1 C9 119.27(7) . . ? C5 Fe1 C3 68.63(8) . . ? C7 Fe1 C3 167.47(7) . . ? C6 Fe1 C3 150.70(7) . . ? C1 Fe1 C3 68.92(7) . . ? C4 Fe1 C3 40.61(8) . . ? C8 Fe1 C3 129.52(8) . . ? C2 Fe1 C3 40.67(7) . . ? C9 Fe1 C3 109.13(7) . . ? C5 Fe1 C10 127.20(7) . . ? C7 Fe1 C10 68.39(7) . . ? C6 Fe1 C10 40.83(7) . . ? C1 Fe1 C10 165.58(7) . . ? C4 Fe1 C10 107.39(7) . . ? C8 Fe1 C10 68.55(7) . . ? C2 Fe1 C10 152.10(7) . . ? C9 Fe1 C10 40.49(7) . . ? C3 Fe1 C10 118.10(7) . . ? C20 C21 C22 119.91(18) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.383 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.055 #====================================================================== data_i0653 _database_code_depnum_ccdc_archive 'CCDC 805318' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H22 Fe N P' _chemical_formula_sum 'C27 H22 Fe N P' _chemical_formula_weight 447.28 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' 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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1847(12) _cell_length_b 11.0585(12) _cell_length_c 10.9491(13) _cell_angle_alpha 72.890(9) _cell_angle_beta 85.100(10) _cell_angle_gamma 65.974(8) _cell_volume 1075.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6168 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 25.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.789 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5543 _exptl_absorpt_correction_T_max 0.9589 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 7001 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3555 _reflns_number_gt 2598 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3555 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1119 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0575(3) 0.2322(4) 0.9654(3) 0.0363(8) Uani 1 1 d . . . C2 C 0.1594(4) 0.2409(4) 1.0432(3) 0.0415(9) Uani 1 1 d . . . H2A H 0.1416 0.3126 1.0815 0.050 Uiso 1 1 calc R . . C3 C 0.2920(4) 0.1225(5) 1.0523(4) 0.0488(11) Uani 1 1 d . . . H3A H 0.3769 0.1012 1.0990 0.059 Uiso 1 1 calc R . . C4 C 0.2746(4) 0.0425(4) 0.9796(4) 0.0463(10) Uani 1 1 d . . . H4A H 0.3459 -0.0414 0.9690 0.056 Uiso 1 1 calc R . . C5 C 0.1305(4) 0.1101(4) 0.9247(3) 0.0395(9) Uani 1 1 d . . . H5A H 0.0906 0.0792 0.8708 0.047 Uiso 1 1 calc R . . C6 C 0.2552(4) 0.2800(4) 0.6681(3) 0.0391(9) Uani 1 1 d . . . C7 C 0.1668(4) 0.4040(4) 0.7026(3) 0.0423(9) Uani 1 1 d . . . H7A H 0.0695 0.4615 0.6752 0.051 Uiso 1 1 calc R . . C8 C 0.2515(5) 0.4251(5) 0.7854(4) 0.0530(11) Uani 1 1 d . . . H8A H 0.2199 0.4995 0.8223 0.064 Uiso 1 1 calc R . . C9 C 0.3903(4) 0.3164(5) 0.8032(4) 0.0534(11) Uani 1 1 d . . . H9A H 0.4676 0.3056 0.8539 0.064 Uiso 1 1 calc R . . C10 C 0.3941(4) 0.2262(5) 0.7321(4) 0.0464(10) Uani 1 1 d . . . H10A H 0.4743 0.1446 0.7275 0.056 Uiso 1 1 calc R . . C11 C 0.2173(3) 0.2255(4) 0.5746(3) 0.0341(8) Uani 1 1 d . . . C12 C 0.0749(4) 0.2636(4) 0.5355(3) 0.0424(9) Uani 1 1 d . . . H12A H -0.0027 0.3218 0.5737 0.051 Uiso 1 1 calc R . . C13 C 0.0484(4) 0.2161(5) 0.4410(4) 0.0485(10) Uani 1 1 d . . . H13A H -0.0475 0.2420 0.4129 0.058 Uiso 1 1 calc R . . C14 C 0.1636(4) 0.1301(5) 0.3878(4) 0.0503(11) Uani 1 1 d . . . H14A H 0.1434 0.0985 0.3226 0.060 Uiso 1 1 calc R . . C15 C 0.3251(4) 0.1380(4) 0.5143(3) 0.0440(10) Uani 1 1 d . . . H15A H 0.4222 0.1111 0.5398 0.053 Uiso 1 1 calc R . . C16 C -0.1940(3) 0.3496(4) 0.7915(3) 0.0361(8) Uani 1 1 d . . . C17 C -0.2520(3) 0.4690(4) 0.6892(3) 0.0409(9) Uani 1 1 d . . . H17A H -0.2506 0.5530 0.6935 0.049 Uiso 1 1 calc R . . C18 C -0.3123(4) 0.4660(5) 0.5799(3) 0.0509(12) Uani 1 1 d . . . H18A H -0.3518 0.5478 0.5110 0.061 Uiso 1 1 calc R . . C19 C -0.3143(4) 0.3445(6) 0.5724(4) 0.0522(12) Uani 1 1 d . . . H19A H -0.3544 0.3428 0.4981 0.063 Uiso 1 1 calc R . . C20 C -0.2576(4) 0.2238(5) 0.6737(4) 0.0492(10) Uani 1 1 d . . . H20A H -0.2584 0.1400 0.6682 0.059 Uiso 1 1 calc R . . C21 C -0.1994(4) 0.2276(4) 0.7840(3) 0.0404(9) Uani 1 1 d . . . H21A H -0.1634 0.1465 0.8540 0.049 Uiso 1 1 calc R . . C22 C -0.2223(3) 0.2850(4) 1.0602(3) 0.0348(8) Uani 1 1 d . . . C23 C -0.1563(4) 0.1886(4) 1.1755(3) 0.0436(9) Uani 1 1 d . . . H23A H -0.0549 0.1542 1.1880 0.052 Uiso 1 1 calc R . . C24 C -0.2371(5) 0.1422(5) 1.2723(4) 0.0525(11) Uani 1 1 d . . . H24A H -0.1907 0.0766 1.3502 0.063 Uiso 1 1 calc R . . C25 C -0.3859(5) 0.1919(5) 1.2553(4) 0.0542(11) Uani 1 1 d . . . H25A H -0.4410 0.1604 1.3216 0.065 Uiso 1 1 calc R . . C26 C -0.4532(4) 0.2870(5) 1.1419(4) 0.0500(10) Uani 1 1 d . . . H26A H -0.5545 0.3209 1.1297 0.060 Uiso 1 1 calc R . . C27 C -0.3716(4) 0.3331(4) 1.0451(4) 0.0417(9) Uani 1 1 d . . . H27A H -0.4186 0.3986 0.9673 0.050 Uiso 1 1 calc R . . N1 N 0.3017(3) 0.0886(4) 0.4225(3) 0.0525(9) Uani 1 1 d . . . P1 P -0.12538(9) 0.36537(10) 0.93450(8) 0.0363(2) Uani 1 1 d . . . Fe1 Fe 0.23546(5) 0.23945(6) 0.86477(5) 0.03580(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0344(17) 0.046(2) 0.0316(18) -0.0120(16) 0.0041(13) -0.0190(16) C2 0.0438(19) 0.048(3) 0.0345(19) -0.0075(17) -0.0016(15) -0.0221(18) C3 0.040(2) 0.062(3) 0.040(2) -0.0024(19) -0.0042(15) -0.0227(19) C4 0.0402(19) 0.041(2) 0.046(2) -0.0030(18) 0.0042(16) -0.0120(17) C5 0.0374(18) 0.038(2) 0.042(2) -0.0101(16) 0.0062(14) -0.0154(16) C6 0.0389(18) 0.044(2) 0.0343(19) -0.0062(16) 0.0053(14) -0.0205(17) C7 0.050(2) 0.040(2) 0.0363(19) -0.0066(16) 0.0071(15) -0.0213(18) C8 0.076(3) 0.056(3) 0.045(2) -0.021(2) 0.014(2) -0.042(2) C9 0.055(2) 0.075(3) 0.048(2) -0.015(2) 0.0060(18) -0.047(2) C10 0.0379(19) 0.062(3) 0.045(2) -0.015(2) 0.0067(16) -0.0269(19) C11 0.0321(16) 0.034(2) 0.0288(17) -0.0042(14) 0.0028(13) -0.0089(15) C12 0.0366(18) 0.049(3) 0.0367(19) -0.0151(17) 0.0030(15) -0.0104(17) C13 0.043(2) 0.054(3) 0.040(2) -0.0098(19) -0.0099(16) -0.0112(18) C14 0.052(2) 0.055(3) 0.034(2) -0.0167(18) -0.0040(16) -0.009(2) C15 0.0327(17) 0.052(3) 0.038(2) -0.0124(18) 0.0010(14) -0.0077(17) C16 0.0307(16) 0.041(2) 0.0313(18) -0.0078(15) 0.0053(13) -0.0115(15) C17 0.0328(17) 0.043(2) 0.0388(19) -0.0060(17) 0.0038(14) -0.0111(16) C18 0.0336(18) 0.071(3) 0.0315(19) 0.0020(19) 0.0001(14) -0.0155(19) C19 0.0360(19) 0.082(4) 0.040(2) -0.016(2) -0.0007(16) -0.025(2) C20 0.0394(19) 0.064(3) 0.056(2) -0.028(2) 0.0043(17) -0.0249(19) C21 0.0366(18) 0.047(3) 0.0363(19) -0.0108(17) 0.0005(14) -0.0161(16) C22 0.0383(18) 0.035(2) 0.0331(18) -0.0157(15) 0.0029(14) -0.0127(16) C23 0.045(2) 0.047(2) 0.0376(19) -0.0100(17) -0.0011(15) -0.0176(18) C24 0.065(3) 0.055(3) 0.034(2) -0.0044(18) 0.0055(17) -0.026(2) C25 0.062(3) 0.057(3) 0.048(2) -0.017(2) 0.0232(19) -0.030(2) C26 0.041(2) 0.054(3) 0.054(2) -0.020(2) 0.0140(17) -0.0181(19) C27 0.0398(19) 0.040(2) 0.042(2) -0.0126(17) 0.0068(15) -0.0141(17) N1 0.0442(17) 0.064(3) 0.0404(18) -0.0237(17) 0.0014(14) -0.0069(16) P1 0.0367(5) 0.0363(6) 0.0351(5) -0.0104(4) 0.0032(4) -0.0141(4) Fe1 0.0353(3) 0.0420(4) 0.0319(3) -0.0088(2) 0.00156(19) -0.0186(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 C1 C5 1.434(5) . ? C1 C2 1.447(5) . ? C1 P1 1.826(4) . ? C1 Fe1 2.057(3) . ? C2 C3 1.433(6) . ? C2 Fe1 2.041(4) . ? C3 C4 1.420(6) . ? C3 Fe1 2.063(4) . ? C4 C5 1.437(5) . ? C4 Fe1 2.062(4) . ? C5 Fe1 2.047(4) . ? C6 C7 1.440(6) . ? C6 C10 1.444(5) . ? C6 C11 1.476(5) . ? C6 Fe1 2.077(4) . ? C7 C8 1.428(6) . ? C7 Fe1 2.056(4) . ? C8 C9 1.417(6) . ? C8 Fe1 2.048(5) . ? C9 C10 1.422(6) . ? C9 Fe1 2.059(4) . ? C10 Fe1 2.068(4) . ? C11 C15 1.402(5) . ? C11 C12 1.402(5) . ? C12 C13 1.379(6) . ? C13 C14 1.387(5) . ? C14 N1 1.341(5) . ? C15 N1 1.355(5) . ? C16 C17 1.398(5) . ? C16 C21 1.399(6) . ? C16 P1 1.849(4) . ? C17 C18 1.406(6) . ? C18 C19 1.378(7) . ? C19 C20 1.398(7) . ? C20 C21 1.408(5) . ? C22 C23 1.397(5) . ? C22 C27 1.398(5) . ? C22 P1 1.850(4) . ? C23 C24 1.393(6) . ? C24 C25 1.394(6) . ? C25 C26 1.382(6) . ? C26 C27 1.396(6) . ? 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 C5 C1 C2 107.3(3) . . ? C5 C1 P1 132.3(3) . . ? C2 C1 P1 120.4(3) . . ? C5 C1 Fe1 69.2(2) . . ? C2 C1 Fe1 68.74(19) . . ? P1 C1 Fe1 126.3(2) . . ? C3 C2 C1 108.0(4) . . ? C3 C2 Fe1 70.4(2) . . ? C1 C2 Fe1 69.92(19) . . ? C4 C3 C2 108.2(3) . . ? C4 C3 Fe1 69.8(2) . . ? C2 C3 Fe1 68.8(2) . . ? C3 C4 C5 108.4(4) . . ? C3 C4 Fe1 69.9(2) . . ? C5 C4 Fe1 69.0(2) . . ? C1 C5 C4 108.1(3) . . ? C1 C5 Fe1 69.9(2) . . ? C4 C5 Fe1 70.1(2) . . ? C7 C6 C10 107.0(4) . . ? C7 C6 C11 126.8(3) . . ? C10 C6 C11 125.9(3) . . ? C7 C6 Fe1 68.8(2) . . ? C10 C6 Fe1 69.3(2) . . ? C11 C6 Fe1 131.6(3) . . ? C8 C7 C6 107.9(4) . . ? C8 C7 Fe1 69.3(2) . . ? C6 C7 Fe1 70.4(2) . . ? C9 C8 C7 108.6(4) . . ? C9 C8 Fe1 70.2(3) . . ? C7 C8 Fe1 69.9(2) . . ? C8 C9 C10 108.3(4) . . ? C8 C9 Fe1 69.4(2) . . ? C10 C9 Fe1 70.2(2) . . ? C9 C10 C6 108.2(4) . . ? C9 C10 Fe1 69.5(2) . . ? C6 C10 Fe1 69.94(19) . . ? C15 C11 C12 116.4(3) . . ? C15 C11 C6 120.6(3) . . ? C12 C11 C6 122.9(3) . . ? C13 C12 C11 119.6(3) . . ? C12 C13 C14 119.1(3) . . ? N1 C14 C13 124.0(4) . . ? N1 C15 C11 125.1(3) . . ? C17 C16 C21 118.7(3) . . ? C17 C16 P1 117.6(3) . . ? C21 C16 P1 123.5(3) . . ? C16 C17 C18 120.6(4) . . ? C19 C18 C17 120.1(4) . . ? C18 C19 C20 120.3(4) . . ? C19 C20 C21 119.5(4) . . ? C16 C21 C20 120.7(4) . . ? C23 C22 C27 118.0(3) . . ? C23 C22 P1 123.2(3) . . ? C27 C22 P1 118.4(3) . . ? C24 C23 C22 120.8(3) . . ? C23 C24 C25 120.2(4) . . ? C26 C25 C24 119.8(4) . . ? C25 C26 C27 119.7(4) . . ? C26 C27 C22 121.4(4) . . ? C14 N1 C15 115.8(3) . . ? C1 P1 C16 105.40(16) . . ? C1 P1 C22 100.94(16) . . ? C16 P1 C22 100.07(16) . . ? C2 Fe1 C5 69.12(16) . . ? C2 Fe1 C8 106.36(17) . . ? C5 Fe1 C8 155.60(16) . . ? C2 Fe1 C7 125.52(16) . . ? C5 Fe1 C7 121.25(16) . . ? C8 Fe1 C7 40.73(16) . . ? C2 Fe1 C1 41.34(14) . . ? C5 Fe1 C1 40.88(15) . . ? C8 Fe1 C1 119.94(17) . . ? C7 Fe1 C1 108.11(15) . . ? C2 Fe1 C9 118.26(16) . . ? C5 Fe1 C9 163.21(17) . . ? C8 Fe1 C9 40.36(18) . . ? C7 Fe1 C9 68.30(17) . . ? C1 Fe1 C9 153.95(17) . . ? C2 Fe1 C4 68.54(17) . . ? C5 Fe1 C4 40.94(14) . . ? C8 Fe1 C4 161.59(17) . . ? C7 Fe1 C4 156.36(17) . . ? C1 Fe1 C4 68.71(15) . . ? C9 Fe1 C4 125.09(17) . . ? C2 Fe1 C3 40.87(16) . . ? C5 Fe1 C3 68.61(16) . . ? C8 Fe1 C3 124.53(18) . . ? C7 Fe1 C3 162.40(18) . . ? C1 Fe1 C3 68.90(14) . . ? C9 Fe1 C3 106.34(16) . . ? C4 Fe1 C3 40.27(17) . . ? C2 Fe1 C10 153.00(15) . . ? C5 Fe1 C10 126.90(16) . . ? C8 Fe1 C10 68.00(18) . . ? C7 Fe1 C10 68.43(16) . . ? C1 Fe1 C10 164.54(15) . . ? C9 Fe1 C10 40.30(17) . . ? C4 Fe1 C10 108.03(17) . . ? C3 Fe1 C10 119.08(15) . . ? C2 Fe1 C6 163.94(14) . . ? C5 Fe1 C6 108.96(15) . . ? C8 Fe1 C6 68.42(16) . . ? C7 Fe1 C6 40.80(16) . . ? C1 Fe1 C6 126.88(13) . . ? C9 Fe1 C6 68.31(16) . . ? C4 Fe1 C6 121.17(17) . . ? C3 Fe1 C6 154.58(16) . . ? C10 Fe1 C6 40.79(14) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.550 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.078 #=================================================================== data_i0531a _database_code_depnum_ccdc_archive 'CCDC 805319' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H22 Cl2 Fe N P Zn' _chemical_formula_sum 'C27 H22 Cl2 Fe N P Zn' _chemical_formula_weight 583.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.2868(16) _cell_length_b 9.2179(5) _cell_length_c 28.835(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.856(7) _cell_angle_gamma 90.00 _cell_volume 5017.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 14670 _cell_measurement_theta_min 1.17 _cell_measurement_theta_max 25.31 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 1.827 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7455 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 31242 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.1040 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8832 _reflns_number_gt 5152 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8832 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.846 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2951(3) 0.4923(6) 0.67681(16) 0.0378(13) Uani 1 1 d . . . C2 C 0.2236(3) 0.5225(6) 0.68197(17) 0.0432(14) Uani 1 1 d . . . H2A H 0.1882 0.4532 0.6829 0.052 Uiso 1 1 calc R . . C3 C 0.2161(3) 0.6764(7) 0.68544(19) 0.0481(14) Uani 1 1 d . . . H3A H 0.1748 0.7261 0.6885 0.058 Uiso 1 1 calc R . . C4 C 0.2830(3) 0.7411(7) 0.6835(2) 0.0514(15) Uani 1 1 d . . . H4A H 0.2933 0.8408 0.6855 0.062 Uiso 1 1 calc R . . C5 C 0.3310(3) 0.6295(6) 0.67787(18) 0.0460(14) Uani 1 1 d . . . H5A H 0.3784 0.6428 0.6753 0.055 Uiso 1 1 calc R . . C6 C 0.2832(3) 0.6464(6) 0.56116(17) 0.0372(12) Uani 1 1 d . . . C7 C 0.2420(3) 0.5171(6) 0.55933(16) 0.0370(12) Uani 1 1 d . . . H7A H 0.2584 0.4230 0.5553 0.044 Uiso 1 1 calc R . . C8 C 0.1721(3) 0.5524(7) 0.56459(18) 0.0436(13) Uani 1 1 d . . . H8A H 0.1348 0.4870 0.5647 0.052 Uiso 1 1 calc R . . C9 C 0.1698(3) 0.7069(7) 0.5697(2) 0.0520(15) Uani 1 1 d . . . H9A H 0.1304 0.7612 0.5740 0.062 Uiso 1 1 calc R . . C10 C 0.2370(3) 0.7637(6) 0.56706(19) 0.0441(14) Uani 1 1 d . . . H10A H 0.2494 0.8625 0.5689 0.053 Uiso 1 1 calc R . . C11 C 0.3572(3) 0.6601(6) 0.55526(17) 0.0365(12) Uani 1 1 d . . . C12 C 0.3774(3) 0.7886(7) 0.5361(2) 0.0556(16) Uani 1 1 d . . . H12A H 0.3455 0.8666 0.5297 0.067 Uiso 1 1 calc R . . C13 C 0.4455(3) 0.8007(8) 0.5265(3) 0.070(2) Uani 1 1 d . . . H13A H 0.4596 0.8869 0.5137 0.084 Uiso 1 1 calc R . . C14 C 0.4910(3) 0.6866(8) 0.5358(2) 0.0638(18) Uani 1 1 d . . . H14A H 0.5364 0.6913 0.5286 0.077 Uiso 1 1 calc R . . C15 C 0.4689(3) 0.5628(7) 0.5563(2) 0.0521(15) Uani 1 1 d . . . H15A H 0.5008 0.4851 0.5634 0.062 Uiso 1 1 calc R . . C16 C 0.3826(3) 0.2508(7) 0.71710(19) 0.0426(14) Uani 1 1 d . . . C17 C 0.4024(3) 0.3366(8) 0.75727(19) 0.0561(16) Uani 1 1 d . . . H17A H 0.3886 0.4346 0.7563 0.067 Uiso 1 1 calc R . . C18 C 0.4428(4) 0.2787(9) 0.7992(2) 0.070(2) Uani 1 1 d . . . H18A H 0.4570 0.3384 0.8258 0.084 Uiso 1 1 calc R . . C19 C 0.4615(3) 0.1364(9) 0.8013(2) 0.068(2) Uani 1 1 d . . . H19A H 0.4870 0.0970 0.8298 0.082 Uiso 1 1 calc R . . C20 C 0.4433(3) 0.0500(8) 0.7620(3) 0.0662(19) Uani 1 1 d . . . H20A H 0.4570 -0.0481 0.7635 0.079 Uiso 1 1 calc R . . C21 C 0.4045(3) 0.1072(7) 0.7196(2) 0.0580(17) Uani 1 1 d . . . H21A H 0.3932 0.0479 0.6926 0.070 Uiso 1 1 calc R . . C22 C 0.2498(3) 0.2021(6) 0.65324(17) 0.0396(13) Uani 1 1 d . . . C23 C 0.2233(3) 0.1559(6) 0.69271(18) 0.0447(14) Uani 1 1 d . . . H23A H 0.2475 0.1806 0.7234 0.054 Uiso 1 1 calc R . . C24 C 0.1623(3) 0.0747(6) 0.6867(2) 0.0460(14) Uani 1 1 d . . . H24A H 0.1458 0.0421 0.7133 0.055 Uiso 1 1 calc R . . C25 C 0.1244(3) 0.0401(6) 0.6411(2) 0.0496(14) Uani 1 1 d . . . H25A H 0.0817 -0.0123 0.6368 0.059 Uiso 1 1 calc R . . C26 C 0.1518(3) 0.0856(6) 0.60220(19) 0.0456(14) Uani 1 1 d . . . H26A H 0.1274 0.0621 0.5714 0.055 Uiso 1 1 calc R . . C27 C 0.2140(3) 0.1643(6) 0.60809(18) 0.0410(13) Uani 1 1 d . . . H27A H 0.2320 0.1923 0.5815 0.049 Uiso 1 1 calc R . . C28 C 0.1928(3) 0.3817(6) 0.32607(16) 0.0351(12) Uani 1 1 d . . . C29 C 0.2616(3) 0.4114(6) 0.31565(17) 0.0404(13) Uani 1 1 d . . . H29A H 0.2989 0.3446 0.3175 0.049 Uiso 1 1 calc R . . C30 C 0.2628(3) 0.5593(7) 0.30206(18) 0.0481(15) Uani 1 1 d . . . H30A H 0.3010 0.6070 0.2929 0.058 Uiso 1 1 calc R . . C31 C 0.1968(3) 0.6229(7) 0.30462(18) 0.0502(15) Uani 1 1 d . . . H31A H 0.1840 0.7201 0.2976 0.060 Uiso 1 1 calc R . . C32 C 0.1534(3) 0.5165(6) 0.31952(16) 0.0396(13) Uani 1 1 d . . . H32A H 0.1071 0.5306 0.3243 0.048 Uiso 1 1 calc R . . C33 C 0.2174(3) 0.6124(5) 0.43129(16) 0.0315(11) Uani 1 1 d . . . C34 C 0.2549(3) 0.4789(6) 0.44012(16) 0.0341(12) Uani 1 1 d . . . H34A H 0.2376 0.3934 0.4515 0.041 Uiso 1 1 calc R . . C35 C 0.3229(3) 0.4963(6) 0.42883(18) 0.0400(13) Uani 1 1 d . . . H35A H 0.3580 0.4243 0.4312 0.048 Uiso 1 1 calc R . . C36 C 0.3286(3) 0.6422(6) 0.41321(19) 0.0444(14) Uani 1 1 d . . . H36A H 0.3679 0.6833 0.4035 0.053 Uiso 1 1 calc R . . C37 C 0.2639(3) 0.7139(6) 0.41506(18) 0.0380(12) Uani 1 1 d . . . H37A H 0.2533 0.8114 0.4070 0.046 Uiso 1 1 calc R . . C38 C 0.1452(3) 0.6447(5) 0.43932(16) 0.0310(11) Uani 1 1 d . . . C39 C 0.1279(3) 0.7855(6) 0.45063(18) 0.0393(13) Uani 1 1 d . . . H39A H 0.1612 0.8607 0.4520 0.047 Uiso 1 1 calc R . . C40 C 0.0617(3) 0.8144(7) 0.45981(19) 0.0487(14) Uani 1 1 d . . . H40A H 0.0489 0.9096 0.4662 0.058 Uiso 1 1 calc R . . C41 C 0.0148(3) 0.7021(7) 0.4594(2) 0.0551(16) Uani 1 1 d . . . H41A H -0.0297 0.7184 0.4671 0.066 Uiso 1 1 calc R . . C42 C 0.0340(3) 0.5640(7) 0.4476(2) 0.0476(14) Uani 1 1 d . . . H42A H 0.0016 0.4877 0.4471 0.057 Uiso 1 1 calc R . . C43 C 0.1107(3) 0.1076(6) 0.31194(17) 0.0372(12) Uani 1 1 d . . . C44 C 0.0779(3) -0.0104(6) 0.3287(2) 0.0476(14) Uani 1 1 d . . . H44A H 0.0822 -0.0221 0.3616 0.057 Uiso 1 1 calc R . . C45 C 0.0390(3) -0.1114(7) 0.2981(2) 0.0547(16) Uani 1 1 d . . . H45A H 0.0175 -0.1904 0.3101 0.066 Uiso 1 1 calc R . . C46 C 0.0325(3) -0.0939(7) 0.2497(2) 0.0530(16) Uani 1 1 d . . . H46A H 0.0063 -0.1615 0.2287 0.064 Uiso 1 1 calc R . . C47 C 0.0645(3) 0.0237(7) 0.2321(2) 0.0519(16) Uani 1 1 d . . . H47A H 0.0599 0.0352 0.1992 0.062 Uiso 1 1 calc R . . C48 C 0.1034(3) 0.1242(6) 0.26300(18) 0.0422(13) Uani 1 1 d . . . H48A H 0.1247 0.2034 0.2509 0.051 Uiso 1 1 calc R . . C49 C 0.2487(3) 0.1190(6) 0.37092(18) 0.0384(12) Uani 1 1 d . . . C50 C 0.2734(3) 0.0421(6) 0.33588(18) 0.0431(13) Uani 1 1 d . . . H50A H 0.2458 0.0372 0.3050 0.052 Uiso 1 1 calc R . . C51 C 0.3390(3) -0.0276(6) 0.3465(2) 0.0486(15) Uani 1 1 d . . . H51A H 0.3553 -0.0806 0.3230 0.058 Uiso 1 1 calc R . . C52 C 0.3799(3) -0.0182(6) 0.3917(2) 0.0472(14) Uani 1 1 d . . . H52A H 0.4250 -0.0614 0.3987 0.057 Uiso 1 1 calc R . . C53 C 0.3546(3) 0.0546(6) 0.4266(2) 0.0463(14) Uani 1 1 d . . . H53A H 0.3824 0.0597 0.4574 0.056 Uiso 1 1 calc R . . C54 C 0.2888(3) 0.1200(5) 0.41689(18) 0.0372(12) Uani 1 1 d . . . H54A H 0.2711 0.1651 0.4413 0.045 Uiso 1 1 calc R . . N1 N 0.4037(2) 0.5484(5) 0.56638(14) 0.0373(10) Uani 1 1 d . . . N2 N 0.0980(2) 0.5344(4) 0.43673(14) 0.0340(10) Uani 1 1 d . . . Cl1 Cl 0.50702(7) 0.29465(17) 0.63826(5) 0.0519(4) Uani 1 1 d . . . Cl2 Cl 0.35812(9) 0.19385(18) 0.53807(5) 0.0580(4) Uani 1 1 d . . . Cl3 Cl 0.13591(8) 0.18564(16) 0.48192(5) 0.0488(3) Uani 1 1 d . . . Cl4 Cl -0.01186(7) 0.28638(18) 0.37546(5) 0.0544(4) Uani 1 1 d . . . Fe1 Fe 0.24638(4) 0.62238(8) 0.62290(3) 0.0379(2) Uani 1 1 d . . . Fe2 Fe 0.24422(4) 0.53987(8) 0.36990(2) 0.03346(18) Uani 1 1 d . . . Zn1 Zn 0.39526(3) 0.34260(7) 0.59923(2) 0.03675(16) Uani 1 1 d . . . Zn2 Zn 0.10144(3) 0.31330(7) 0.415192(19) 0.03447(15) Uani 1 1 d . . . P1 P 0.32849(7) 0.31930(17) 0.66229(4) 0.0379(3) Uani 1 1 d . . . P2 P 0.16613(7) 0.22457(15) 0.35557(5) 0.0341(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(3) 0.045(4) 0.024(3) 0.000(2) 0.007(2) 0.005(3) C2 0.048(3) 0.054(4) 0.030(3) -0.001(3) 0.012(2) 0.007(3) C3 0.055(4) 0.049(4) 0.045(3) -0.009(3) 0.020(3) 0.009(3) C4 0.067(4) 0.038(4) 0.049(4) -0.009(3) 0.010(3) 0.000(3) C5 0.046(3) 0.055(4) 0.035(3) -0.007(3) 0.004(2) -0.009(3) C6 0.044(3) 0.034(3) 0.033(3) 0.003(2) 0.006(2) 0.003(3) C7 0.034(3) 0.042(3) 0.034(3) 0.001(2) 0.006(2) 0.003(2) C8 0.038(3) 0.053(4) 0.038(3) 0.002(3) 0.003(2) -0.004(3) C9 0.045(3) 0.059(4) 0.050(3) 0.007(3) 0.006(3) 0.020(3) C10 0.039(3) 0.045(4) 0.047(3) 0.007(3) 0.006(3) 0.007(3) C11 0.045(3) 0.031(3) 0.035(3) 0.002(2) 0.011(2) -0.002(3) C12 0.046(4) 0.044(4) 0.076(4) 0.022(3) 0.012(3) 0.004(3) C13 0.051(4) 0.059(5) 0.098(5) 0.033(4) 0.012(4) -0.011(4) C14 0.042(3) 0.068(5) 0.085(5) 0.027(4) 0.019(3) -0.004(3) C15 0.039(3) 0.048(4) 0.072(4) 0.013(3) 0.016(3) 0.004(3) C16 0.036(3) 0.053(4) 0.041(3) 0.007(3) 0.012(2) 0.006(3) C17 0.057(4) 0.073(5) 0.037(3) 0.001(3) 0.007(3) 0.017(3) C18 0.063(4) 0.105(7) 0.038(3) -0.001(4) 0.000(3) 0.014(4) C19 0.056(4) 0.100(6) 0.049(4) 0.024(4) 0.013(3) 0.025(4) C20 0.059(4) 0.069(5) 0.071(5) 0.026(4) 0.014(4) 0.018(4) C21 0.051(4) 0.058(4) 0.063(4) 0.010(3) 0.007(3) 0.003(3) C22 0.047(3) 0.040(3) 0.033(3) 0.002(2) 0.009(2) 0.011(3) C23 0.056(3) 0.048(4) 0.031(3) 0.006(3) 0.011(2) -0.002(3) C24 0.058(4) 0.043(4) 0.043(3) 0.008(3) 0.022(3) 0.001(3) C25 0.047(3) 0.043(4) 0.061(4) 0.000(3) 0.018(3) -0.005(3) C26 0.057(4) 0.041(4) 0.037(3) 0.002(3) 0.006(3) -0.004(3) C27 0.048(3) 0.038(3) 0.040(3) 0.005(3) 0.015(2) -0.001(3) C28 0.040(3) 0.043(3) 0.023(2) -0.002(2) 0.006(2) 0.001(3) C29 0.047(3) 0.041(4) 0.035(3) -0.008(2) 0.014(2) -0.004(3) C30 0.059(4) 0.058(4) 0.033(3) 0.000(3) 0.022(3) -0.009(3) C31 0.071(4) 0.045(4) 0.036(3) 0.009(3) 0.015(3) 0.002(3) C32 0.043(3) 0.048(4) 0.026(3) -0.001(2) 0.003(2) 0.004(3) C33 0.035(3) 0.034(3) 0.026(2) -0.001(2) 0.005(2) -0.002(2) C34 0.037(3) 0.032(3) 0.032(3) -0.001(2) 0.003(2) 0.001(2) C35 0.037(3) 0.040(4) 0.041(3) -0.005(2) 0.001(2) 0.001(3) C36 0.039(3) 0.044(4) 0.052(3) -0.011(3) 0.014(3) -0.010(3) C37 0.037(3) 0.034(3) 0.042(3) -0.001(2) 0.007(2) 0.000(2) C38 0.041(3) 0.025(3) 0.026(2) 0.001(2) 0.005(2) 0.004(2) C39 0.046(3) 0.033(3) 0.041(3) 0.004(2) 0.016(3) 0.000(3) C40 0.057(4) 0.041(4) 0.051(3) -0.001(3) 0.018(3) 0.011(3) C41 0.046(3) 0.051(4) 0.074(4) 0.000(3) 0.024(3) 0.010(3) C42 0.044(3) 0.046(4) 0.057(4) -0.002(3) 0.019(3) 0.000(3) C43 0.037(3) 0.036(3) 0.039(3) -0.002(2) 0.009(2) 0.006(2) C44 0.056(4) 0.046(4) 0.040(3) 0.003(3) 0.008(3) -0.005(3) C45 0.050(4) 0.047(4) 0.066(4) -0.009(3) 0.011(3) -0.016(3) C46 0.044(3) 0.057(4) 0.058(4) -0.020(3) 0.009(3) -0.013(3) C47 0.048(3) 0.071(5) 0.035(3) -0.010(3) 0.005(3) 0.001(3) C48 0.040(3) 0.049(4) 0.040(3) 0.000(3) 0.013(2) -0.002(3) C49 0.044(3) 0.034(3) 0.041(3) -0.001(2) 0.015(2) -0.001(3) C50 0.049(3) 0.046(3) 0.036(3) -0.006(3) 0.011(3) 0.001(3) C51 0.062(4) 0.043(4) 0.048(3) -0.004(3) 0.027(3) 0.009(3) C52 0.042(3) 0.043(4) 0.057(4) 0.008(3) 0.012(3) 0.002(3) C53 0.045(3) 0.043(4) 0.049(3) -0.009(3) 0.004(3) 0.002(3) C54 0.046(3) 0.028(3) 0.037(3) -0.001(2) 0.007(2) 0.007(2) N1 0.041(3) 0.033(3) 0.041(2) 0.002(2) 0.015(2) 0.002(2) N2 0.035(2) 0.032(3) 0.038(2) 0.003(2) 0.0130(19) 0.001(2) Cl1 0.0393(8) 0.0600(10) 0.0577(9) 0.0050(7) 0.0131(6) 0.0107(7) Cl2 0.0746(10) 0.0542(10) 0.0464(8) -0.0152(7) 0.0150(7) -0.0053(8) Cl3 0.0626(9) 0.0469(9) 0.0389(7) 0.0083(7) 0.0154(6) 0.0051(7) Cl4 0.0353(7) 0.0689(11) 0.0571(9) -0.0144(8) 0.0053(6) -0.0045(7) Fe1 0.0357(4) 0.0406(5) 0.0386(4) -0.0020(3) 0.0103(3) 0.0029(4) Fe2 0.0347(4) 0.0335(4) 0.0339(4) -0.0015(3) 0.0111(3) -0.0002(3) Zn1 0.0403(3) 0.0333(4) 0.0383(3) -0.0002(3) 0.0120(3) 0.0017(3) Zn2 0.0363(3) 0.0340(4) 0.0339(3) -0.0007(3) 0.0091(2) -0.0006(3) P1 0.0380(7) 0.0443(9) 0.0322(7) 0.0031(7) 0.0089(6) 0.0042(7) P2 0.0376(7) 0.0348(8) 0.0304(7) -0.0009(6) 0.0081(6) -0.0024(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.438(8) . ? C1 C2 1.444(7) . ? C1 P1 1.801(5) . ? C1 Fe1 2.034(5) . ? C2 C3 1.431(8) . ? C2 Fe1 2.061(5) . ? C2 H2A 0.9400 . ? C3 C4 1.433(8) . ? C3 Fe1 2.067(5) . ? C3 H3A 0.9400 . ? C4 C5 1.415(8) . ? C4 Fe1 2.059(6) . ? C4 H4A 0.9400 . ? C5 Fe1 2.029(5) . ? C5 H5A 0.9400 . ? C6 C7 1.428(7) . ? C6 C10 1.434(7) . ? C6 C11 1.476(7) . ? C6 Fe1 2.060(5) . ? C7 C8 1.423(7) . ? C7 Fe1 2.060(5) . ? C7 H7A 0.9400 . ? C8 C9 1.434(8) . ? C8 Fe1 2.075(5) . ? C8 H8A 0.9400 . ? C9 C10 1.414(8) . ? C9 Fe1 2.052(6) . ? C9 H9A 0.9400 . ? C10 Fe1 2.050(5) . ? C10 H10A 0.9400 . ? C11 N1 1.360(6) . ? C11 C12 1.396(7) . ? C12 C13 1.400(8) . ? C12 H12A 0.9400 . ? C13 C14 1.362(9) . ? C13 H13A 0.9400 . ? C14 C15 1.391(8) . ? C14 H14A 0.9400 . ? C15 N1 1.354(6) . ? C15 H15A 0.9400 . ? C16 C21 1.387(8) . ? C16 C17 1.390(8) . ? C16 P1 1.818(6) . ? C17 C18 1.401(8) . ? C17 H17A 0.9400 . ? C18 C19 1.359(10) . ? C18 H18A 0.9400 . ? C19 C20 1.370(10) . ? C19 H19A 0.9400 . ? C20 C21 1.398(8) . ? C20 H20A 0.9400 . ? C21 H21A 0.9400 . ? C22 C27 1.387(7) . ? C22 C23 1.406(7) . ? C22 P1 1.837(6) . ? C23 C24 1.376(8) . ? C23 H23A 0.9400 . ? C24 C25 1.403(8) . ? C24 H24A 0.9400 . ? C25 C26 1.398(7) . ? C25 H25A 0.9400 . ? C26 C27 1.383(7) . ? C26 H26A 0.9400 . ? C27 H27A 0.9400 . ? C28 C29 1.445(7) . ? C28 C32 1.449(7) . ? C28 P2 1.807(5) . ? C28 Fe2 2.047(5) . ? C29 C30 1.420(8) . ? C29 Fe2 2.044(5) . ? C29 H29A 0.9400 . ? C30 C31 1.418(8) . ? C30 Fe2 2.068(5) . ? C30 H30A 0.9400 . ? C31 C32 1.413(8) . ? C31 Fe2 2.064(5) . ? C31 H31A 0.9400 . ? C32 Fe2 2.045(5) . ? C32 H32A 0.9400 . ? C33 C34 1.424(7) . ? C33 C37 1.440(7) . ? C33 C38 1.488(7) . ? C33 Fe2 2.055(5) . ? C34 C35 1.424(7) . ? C34 Fe2 2.070(5) . ? C34 H34A 0.9400 . ? C35 C36 1.430(8) . ? C35 Fe2 2.072(5) . ? C35 H35A 0.9400 . ? C36 C37 1.421(7) . ? C36 Fe2 2.064(5) . ? C36 H36A 0.9400 . ? C37 Fe2 2.052(5) . ? C37 H37A 0.9400 . ? C38 N2 1.356(6) . ? C38 C39 1.396(7) . ? C39 C40 1.382(7) . ? C39 H39A 0.9400 . ? C40 C41 1.374(8) . ? C40 H40A 0.9400 . ? C41 C42 1.388(8) . ? C41 H41A 0.9400 . ? C42 N2 1.362(6) . ? C42 H42A 0.9400 . ? C43 C44 1.394(7) . ? C43 C48 1.397(7) . ? C43 P2 1.827(5) . ? C44 C45 1.392(8) . ? C44 H44A 0.9400 . ? C45 C46 1.383(8) . ? C45 H45A 0.9400 . ? C46 C47 1.395(8) . ? C46 H46A 0.9400 . ? C47 C48 1.392(8) . ? C47 H47A 0.9400 . ? C48 H48A 0.9400 . ? C49 C54 1.391(7) . ? C49 C50 1.396(7) . ? C49 P2 1.841(5) . ? C50 C51 1.396(7) . ? C50 H50A 0.9400 . ? C51 C52 1.381(8) . ? C51 H51A 0.9400 . ? C52 C53 1.379(7) . ? C52 H52A 0.9400 . ? C53 C54 1.380(7) . ? C53 H53A 0.9400 . ? C54 H54A 0.9400 . ? N1 Zn1 2.142(4) . ? N2 Zn2 2.135(4) . ? Cl1 Zn1 2.2609(15) . ? Cl2 Zn1 2.2324(16) . ? Cl3 Zn2 2.2369(14) . ? Cl4 Zn2 2.2627(15) . ? Zn1 P1 2.4442(14) . ? Zn2 P2 2.4623(14) . ? 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 C5 C1 C2 107.1(5) . . ? C5 C1 P1 126.2(4) . . ? C2 C1 P1 126.1(4) . . ? C5 C1 Fe1 69.1(3) . . ? C2 C1 Fe1 70.4(3) . . ? P1 C1 Fe1 118.4(2) . . ? C3 C2 C1 108.1(5) . . ? C3 C2 Fe1 69.9(3) . . ? C1 C2 Fe1 68.4(3) . . ? C3 C2 H2A 125.9 . . ? C1 C2 H2A 125.9 . . ? Fe1 C2 H2A 127.3 . . ? C2 C3 C4 107.7(5) . . ? C2 C3 Fe1 69.5(3) . . ? C4 C3 Fe1 69.4(3) . . ? C2 C3 H3A 126.1 . . ? C4 C3 H3A 126.1 . . ? Fe1 C3 H3A 126.6 . . ? C5 C4 C3 108.5(5) . . ? C5 C4 Fe1 68.6(3) . . ? C3 C4 Fe1 70.0(3) . . ? C5 C4 H4A 125.8 . . ? C3 C4 H4A 125.8 . . ? Fe1 C4 H4A 127.2 . . ? C4 C5 C1 108.6(5) . . ? C4 C5 Fe1 70.9(3) . . ? C1 C5 Fe1 69.4(3) . . ? C4 C5 H5A 125.7 . . ? C1 C5 H5A 125.7 . . ? Fe1 C5 H5A 125.5 . . ? C7 C6 C10 106.2(5) . . ? C7 C6 C11 127.7(5) . . ? C10 C6 C11 126.0(5) . . ? C7 C6 Fe1 69.7(3) . . ? C10 C6 Fe1 69.2(3) . . ? C11 C6 Fe1 128.5(4) . . ? C8 C7 C6 109.8(5) . . ? C8 C7 Fe1 70.4(3) . . ? C6 C7 Fe1 69.7(3) . . ? C8 C7 H7A 125.1 . . ? C6 C7 H7A 125.1 . . ? Fe1 C7 H7A 126.3 . . ? C7 C8 C9 106.7(5) . . ? C7 C8 Fe1 69.3(3) . . ? C9 C8 Fe1 68.8(3) . . ? C7 C8 H8A 126.6 . . ? C9 C8 H8A 126.6 . . ? Fe1 C8 H8A 126.8 . . ? C10 C9 C8 108.3(5) . . ? C10 C9 Fe1 69.8(3) . . ? C8 C9 Fe1 70.5(3) . . ? C10 C9 H9A 125.8 . . ? C8 C9 H9A 125.8 . . ? Fe1 C9 H9A 125.4 . . ? C9 C10 C6 109.0(5) . . ? C9 C10 Fe1 69.9(3) . . ? C6 C10 Fe1 69.9(3) . . ? C9 C10 H10A 125.5 . . ? C6 C10 H10A 125.5 . . ? Fe1 C10 H10A 126.2 . . ? N1 C11 C12 120.7(5) . . ? N1 C11 C6 120.9(4) . . ? C12 C11 C6 118.3(5) . . ? C11 C12 C13 119.7(6) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C14 C13 C12 119.5(6) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 118.3(6) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? N1 C15 C14 123.5(5) . . ? N1 C15 H15A 118.3 . . ? C14 C15 H15A 118.3 . . ? C21 C16 C17 118.1(6) . . ? C21 C16 P1 119.4(5) . . ? C17 C16 P1 122.5(5) . . ? C16 C17 C18 120.7(6) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C19 C18 C17 120.1(7) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C18 C19 C20 120.3(6) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C21 120.2(7) . . ? C19 C20 H20A 119.9 . . ? C21 C20 H20A 119.9 . . ? C16 C21 C20 120.6(7) . . ? C16 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C27 C22 C23 119.3(5) . . ? C27 C22 P1 121.3(4) . . ? C23 C22 P1 119.3(4) . . ? C24 C23 C22 120.4(5) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 120.7(5) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C26 C25 C24 118.2(5) . . ? C26 C25 H25A 120.9 . . ? C24 C25 H25A 120.9 . . ? C27 C26 C25 121.3(5) . . ? C27 C26 H26A 119.3 . . ? C25 C26 H26A 119.3 . . ? C26 C27 C22 120.0(5) . . ? C26 C27 H27A 120.0 . . ? C22 C27 H27A 120.0 . . ? C29 C28 C32 106.9(5) . . ? C29 C28 P2 127.8(4) . . ? C32 C28 P2 123.8(4) . . ? C29 C28 Fe2 69.2(3) . . ? C32 C28 Fe2 69.2(3) . . ? P2 C28 Fe2 115.4(2) . . ? C30 C29 C28 107.9(5) . . ? C30 C29 Fe2 70.7(3) . . ? C28 C29 Fe2 69.4(3) . . ? C30 C29 H29A 126.0 . . ? C28 C29 H29A 126.0 . . ? Fe2 C29 H29A 125.4 . . ? C31 C30 C29 108.5(5) . . ? C31 C30 Fe2 69.8(3) . . ? C29 C30 Fe2 68.9(3) . . ? C31 C30 H30A 125.8 . . ? C29 C30 H30A 125.8 . . ? Fe2 C30 H30A 127.1 . . ? C32 C31 C30 108.9(5) . . ? C32 C31 Fe2 69.2(3) . . ? C30 C31 Fe2 70.1(3) . . ? C32 C31 H31A 125.6 . . ? C30 C31 H31A 125.6 . . ? Fe2 C31 H31A 126.8 . . ? C31 C32 C28 107.8(5) . . ? C31 C32 Fe2 70.6(3) . . ? C28 C32 Fe2 69.3(3) . . ? C31 C32 H32A 126.1 . . ? C28 C32 H32A 126.1 . . ? Fe2 C32 H32A 125.6 . . ? C34 C33 C37 107.0(4) . . ? C34 C33 C38 127.0(4) . . ? C37 C33 C38 125.9(5) . . ? C34 C33 Fe2 70.4(3) . . ? C37 C33 Fe2 69.3(3) . . ? C38 C33 Fe2 127.5(3) . . ? C33 C34 C35 108.6(5) . . ? C33 C34 Fe2 69.2(3) . . ? C35 C34 Fe2 69.9(3) . . ? C33 C34 H34A 125.7 . . ? C35 C34 H34A 125.7 . . ? Fe2 C34 H34A 126.7 . . ? C34 C35 C36 108.2(5) . . ? C34 C35 Fe2 69.9(3) . . ? C36 C35 Fe2 69.5(3) . . ? C34 C35 H35A 125.9 . . ? C36 C35 H35A 125.9 . . ? Fe2 C35 H35A 126.3 . . ? C37 C36 C35 107.5(5) . . ? C37 C36 Fe2 69.3(3) . . ? C35 C36 Fe2 70.0(3) . . ? C37 C36 H36A 126.2 . . ? C35 C36 H36A 126.2 . . ? Fe2 C36 H36A 126.0 . . ? C36 C37 C33 108.7(5) . . ? C36 C37 Fe2 70.3(3) . . ? C33 C37 Fe2 69.6(3) . . ? C36 C37 H37A 125.7 . . ? C33 C37 H37A 125.7 . . ? Fe2 C37 H37A 126.0 . . ? N2 C38 C39 121.4(4) . . ? N2 C38 C33 118.7(4) . . ? C39 C38 C33 119.9(4) . . ? C40 C39 C38 119.9(5) . . ? C40 C39 H39A 120.1 . . ? C38 C39 H39A 120.1 . . ? C41 C40 C39 119.1(5) . . ? C41 C40 H40A 120.4 . . ? C39 C40 H40A 120.4 . . ? C40 C41 C42 118.9(5) . . ? C40 C41 H41A 120.5 . . ? C42 C41 H41A 120.5 . . ? N2 C42 C41 122.8(5) . . ? N2 C42 H42A 118.6 . . ? C41 C42 H42A 118.6 . . ? C44 C43 C48 118.5(5) . . ? C44 C43 P2 117.7(4) . . ? C48 C43 P2 123.7(4) . . ? C45 C44 C43 121.6(5) . . ? C45 C44 H44A 119.2 . . ? C43 C44 H44A 119.2 . . ? C46 C45 C44 119.2(6) . . ? C46 C45 H45A 120.4 . . ? C44 C45 H45A 120.4 . . ? C45 C46 C47 120.2(5) . . ? C45 C46 H46A 119.9 . . ? C47 C46 H46A 119.9 . . ? C48 C47 C46 120.2(5) . . ? C48 C47 H47A 119.9 . . ? C46 C47 H47A 119.9 . . ? C47 C48 C43 120.2(5) . . ? C47 C48 H48A 119.9 . . ? C43 C48 H48A 119.9 . . ? C54 C49 C50 119.2(5) . . ? C54 C49 P2 120.7(4) . . ? C50 C49 P2 120.1(4) . . ? C49 C50 C51 120.2(5) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? C52 C51 C50 119.6(5) . . ? C52 C51 H51A 120.2 . . ? C50 C51 H51A 120.2 . . ? C53 C52 C51 120.0(5) . . ? C53 C52 H52A 120.0 . . ? C51 C52 H52A 120.0 . . ? C52 C53 C54 120.8(5) . . ? C52 C53 H53A 119.6 . . ? C54 C53 H53A 119.6 . . ? C53 C54 C49 119.9(5) . . ? C53 C54 H54A 120.0 . . ? C49 C54 H54A 120.0 . . ? C15 N1 C11 118.1(4) . . ? C15 N1 Zn1 109.9(4) . . ? C11 N1 Zn1 132.0(3) . . ? C38 N2 C42 117.8(4) . . ? C38 N2 Zn2 132.2(3) . . ? C42 N2 Zn2 110.0(3) . . ? C5 Fe1 C1 41.5(2) . . ? C5 Fe1 C10 121.3(2) . . ? C1 Fe1 C10 158.0(2) . . ? C5 Fe1 C9 155.7(3) . . ? C1 Fe1 C9 160.7(2) . . ? C10 Fe1 C9 40.3(2) . . ? C5 Fe1 C4 40.5(2) . . ? C1 Fe1 C4 69.0(2) . . ? C10 Fe1 C4 106.7(2) . . ? C9 Fe1 C4 120.1(2) . . ? C5 Fe1 C6 107.9(2) . . ? C1 Fe1 C6 122.4(2) . . ? C10 Fe1 C6 40.8(2) . . ? C9 Fe1 C6 68.6(2) . . ? C4 Fe1 C6 123.8(2) . . ? C5 Fe1 C7 126.2(2) . . ? C1 Fe1 C7 109.3(2) . . ? C10 Fe1 C7 67.6(2) . . ? C9 Fe1 C7 67.8(2) . . ? C4 Fe1 C7 161.7(2) . . ? C6 Fe1 C7 40.5(2) . . ? C5 Fe1 C2 69.0(2) . . ? C1 Fe1 C2 41.3(2) . . ? C10 Fe1 C2 159.0(2) . . ? C9 Fe1 C2 123.0(2) . . ? C4 Fe1 C2 68.3(2) . . ? C6 Fe1 C2 158.7(2) . . ? C7 Fe1 C2 123.2(2) . . ? C5 Fe1 C3 68.7(2) . . ? C1 Fe1 C3 69.2(2) . . ? C10 Fe1 C3 122.5(2) . . ? C9 Fe1 C3 105.8(2) . . ? C4 Fe1 C3 40.6(2) . . ? C6 Fe1 C3 159.6(2) . . ? C7 Fe1 C3 157.2(2) . . ? C2 Fe1 C3 40.6(2) . . ? C5 Fe1 C8 162.5(2) . . ? C1 Fe1 C8 124.7(2) . . ? C10 Fe1 C8 68.1(2) . . ? C9 Fe1 C8 40.7(2) . . ? C4 Fe1 C8 155.8(2) . . ? C6 Fe1 C8 68.7(2) . . ? C7 Fe1 C8 40.26(19) . . ? C2 Fe1 C8 107.6(2) . . ? C3 Fe1 C8 120.7(2) . . ? C29 Fe2 C32 69.3(2) . . ? C29 Fe2 C28 41.4(2) . . ? C32 Fe2 C28 41.5(2) . . ? C29 Fe2 C37 154.2(2) . . ? C32 Fe2 C37 123.6(2) . . ? C28 Fe2 C37 162.1(2) . . ? C29 Fe2 C33 163.2(2) . . ? C32 Fe2 C33 108.4(2) . . ? C28 Fe2 C33 126.00(19) . . ? C37 Fe2 C33 41.04(19) . . ? C29 Fe2 C31 68.2(2) . . ? C32 Fe2 C31 40.2(2) . . ? C28 Fe2 C31 68.5(2) . . ? C37 Fe2 C31 106.2(2) . . ? C33 Fe2 C31 121.5(2) . . ? C29 Fe2 C36 119.7(2) . . ? C32 Fe2 C36 158.7(2) . . ? C28 Fe2 C36 157.0(2) . . ? C37 Fe2 C36 40.4(2) . . ? C33 Fe2 C36 68.7(2) . . ? C31 Fe2 C36 121.9(2) . . ? C29 Fe2 C30 40.4(2) . . ? C32 Fe2 C30 68.1(2) . . ? C28 Fe2 C30 68.5(2) . . ? C37 Fe2 C30 119.2(2) . . ? C33 Fe2 C30 155.5(2) . . ? C31 Fe2 C30 40.1(2) . . ? C36 Fe2 C30 105.3(2) . . ? C29 Fe2 C34 126.3(2) . . ? C32 Fe2 C34 124.4(2) . . ? C28 Fe2 C34 110.4(2) . . ? C37 Fe2 C34 67.9(2) . . ? C33 Fe2 C34 40.37(19) . . ? C31 Fe2 C34 158.3(2) . . ? C36 Fe2 C34 68.0(2) . . ? C30 Fe2 C34 161.3(2) . . ? C29 Fe2 C35 107.9(2) . . ? C32 Fe2 C35 159.8(2) . . ? C28 Fe2 C35 123.2(2) . . ? C37 Fe2 C35 67.8(2) . . ? C33 Fe2 C35 68.2(2) . . ? C31 Fe2 C35 158.9(2) . . ? C36 Fe2 C35 40.5(2) . . ? C30 Fe2 C35 123.6(2) . . ? C34 Fe2 C35 40.21(19) . . ? N1 Zn1 Cl2 103.65(12) . . ? N1 Zn1 Cl1 104.03(12) . . ? Cl2 Zn1 Cl1 113.05(6) . . ? N1 Zn1 P1 120.42(11) . . ? Cl2 Zn1 P1 113.65(6) . . ? Cl1 Zn1 P1 101.92(5) . . ? N2 Zn2 Cl3 105.86(11) . . ? N2 Zn2 Cl4 99.65(12) . . ? Cl3 Zn2 Cl4 117.60(6) . . ? N2 Zn2 P2 124.78(11) . . ? Cl3 Zn2 P2 108.79(5) . . ? Cl4 Zn2 P2 100.68(5) . . ? C1 P1 C16 105.9(2) . . ? C1 P1 C22 103.3(2) . . ? C16 P1 C22 103.2(2) . . ? C1 P1 Zn1 111.29(17) . . ? C16 P1 Zn1 112.41(17) . . ? C22 P1 Zn1 119.48(16) . . ? C28 P2 C43 109.4(2) . . ? C28 P2 C49 102.7(2) . . ? C43 P2 C49 102.0(2) . . ? C28 P2 Zn2 107.26(16) . . ? C43 P2 Zn2 111.61(16) . . ? C49 P2 Zn2 123.04(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.901 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.085 #================================================================ data_i0544 _database_code_depnum_ccdc_archive 'CCDC 805320' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H22 Br2 Fe N P Zn' _chemical_formula_sum 'C27 H22 Br2 Fe N P Zn' _chemical_formula_weight 672.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.6245(6) _cell_length_b 9.2633(4) _cell_length_c 19.3704(7) _cell_angle_alpha 90.00 _cell_angle_beta 102.744(3) _cell_angle_gamma 90.00 _cell_volume 2559.49(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 23691 _cell_measurement_theta_min 1.43 _cell_measurement_theta_max 25.62 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 4.705 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3410 _exptl_absorpt_correction_T_max 0.4668 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 16734 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.19 _reflns_number_total 4708 _reflns_number_gt 4513 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0231P)^2^+0.5984P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00033(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.094(6) _refine_ls_number_reflns 4708 _refine_ls_number_parameters 596 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0184 _refine_ls_wR_factor_ref 0.0461 _refine_ls_wR_factor_gt 0.0457 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.3517(3) 0.8128(4) 0.7809(2) 0.0262(8) Uani 1 1 d . . . C2 C -0.3707(3) 0.6796(4) 0.7428(2) 0.0273(8) Uani 1 1 d . . . H2A H -0.3958 0.5946 0.7589 0.033 Uiso 1 1 calc R . . C3 C -0.3452(3) 0.6974(5) 0.6762(2) 0.0321(9) Uani 1 1 d . . . H3A H -0.3494 0.6257 0.6406 0.039 Uiso 1 1 calc R . . C4 C -0.3123(3) 0.8418(5) 0.6726(2) 0.0352(9) Uani 1 1 d . . . H4A H -0.2914 0.8828 0.6338 0.042 Uiso 1 1 calc R . . C5 C -0.3161(3) 0.9137(4) 0.7366(2) 0.0300(9) Uani 1 1 d . . . H5A H -0.2984 1.0109 0.7482 0.036 Uiso 1 1 calc R . . C6 C -0.3725(3) 0.8452(4) 0.8506(2) 0.0268(8) Uani 1 1 d . . . C7 C -0.3979(3) 0.9846(5) 0.8654(2) 0.0328(9) Uani 1 1 d . . . H7A H -0.3992 1.0593 0.8316 0.039 Uiso 1 1 calc R . . C8 C -0.4216(3) 1.0147(5) 0.9296(2) 0.0424(11) Uani 1 1 d . . . H8A H -0.4386 1.1097 0.9405 0.051 Uiso 1 1 calc R . . C9 C -0.4199(4) 0.9042(6) 0.9768(3) 0.0500(13) Uani 1 1 d . . . H9A H -0.4370 0.9211 1.0207 0.060 Uiso 1 1 calc R . . C10 C -0.3933(4) 0.7687(5) 0.9603(3) 0.0447(12) Uani 1 1 d . . . H10A H -0.3932 0.6931 0.9934 0.054 Uiso 1 1 calc R . . C11 C -0.1515(3) 0.5710(4) 0.8082(2) 0.0267(8) Uani 1 1 d . . . C12 C -0.1338(3) 0.7015(5) 0.8499(2) 0.0323(9) Uani 1 1 d . . . H12A H -0.1433 0.7145 0.8964 0.039 Uiso 1 1 calc R . . C13 C -0.0994(3) 0.8077(5) 0.8082(2) 0.0353(10) Uani 1 1 d . . . H13A H -0.0815 0.9035 0.8228 0.042 Uiso 1 1 calc R . . C14 C -0.0962(3) 0.7465(5) 0.7417(2) 0.0377(10) Uani 1 1 d . . . H14A H -0.0764 0.7944 0.7042 0.045 Uiso 1 1 calc R . . C15 C -0.1278(3) 0.6006(5) 0.7409(2) 0.0324(9) Uani 1 1 d . . . H15A H -0.1326 0.5344 0.7027 0.039 Uiso 1 1 calc R . . C16 C -0.1328(3) 0.2960(4) 0.8849(2) 0.0287(9) Uani 1 1 d . . . C17 C -0.1694(3) 0.1802(5) 0.9172(2) 0.0382(10) Uani 1 1 d . . . H17A H -0.2352 0.1714 0.9122 0.046 Uiso 1 1 calc R . . C18 C -0.1100(4) 0.0792(5) 0.9562(3) 0.0445(11) Uani 1 1 d . . . H18A H -0.1352 0.0013 0.9780 0.053 Uiso 1 1 calc R . . C19 C -0.0134(4) 0.0914(5) 0.9635(2) 0.0464(12) Uani 1 1 d . . . H19A H 0.0274 0.0213 0.9898 0.056 Uiso 1 1 calc R . . C20 C 0.0227(4) 0.2061(6) 0.9324(3) 0.0450(11) Uani 1 1 d . . . H20A H 0.0886 0.2151 0.9376 0.054 Uiso 1 1 calc R . . C21 C -0.0368(3) 0.3085(5) 0.8934(2) 0.0366(10) Uani 1 1 d . . . H21A H -0.0113 0.3872 0.8724 0.044 Uiso 1 1 calc R . . C22 C -0.2555(3) 0.3217(4) 0.7488(2) 0.0264(8) Uani 1 1 d . . . C23 C -0.3497(3) 0.3178(4) 0.7144(2) 0.0291(9) Uani 1 1 d . . . H23A H -0.3955 0.3609 0.7357 0.035 Uiso 1 1 calc R . . C24 C -0.3768(3) 0.2510(5) 0.6488(2) 0.0331(9) Uani 1 1 d . . . H24A H -0.4411 0.2498 0.6254 0.040 Uiso 1 1 calc R . . C25 C -0.3113(4) 0.1862(5) 0.6174(2) 0.0378(10) Uani 1 1 d . . . H25A H -0.3301 0.1429 0.5721 0.045 Uiso 1 1 calc R . . C26 C -0.2175(3) 0.1848(5) 0.6526(2) 0.0350(10) Uani 1 1 d . . . H26A H -0.1726 0.1375 0.6318 0.042 Uiso 1 1 calc R . . C27 C -0.1892(3) 0.2519(5) 0.7177(2) 0.0330(9) Uani 1 1 d . . . H27A H -0.1250 0.2508 0.7414 0.040 Uiso 1 1 calc R . . C28 C 0.3674(3) 0.0298(4) 0.7118(2) 0.0287(8) Uani 1 1 d . . . C29 C 0.3711(3) 0.1538(5) 0.7568(2) 0.0297(9) Uani 1 1 d . . . H29A H 0.3792 0.2510 0.7438 0.036 Uiso 1 1 calc R . . C30 C 0.3604(3) 0.1056(5) 0.8245(2) 0.0342(9) Uani 1 1 d . . . H30A H 0.3594 0.1653 0.8642 0.041 Uiso 1 1 calc R . . C31 C 0.3515(3) -0.0480(5) 0.8223(2) 0.0379(10) Uani 1 1 d . . . H31A H 0.3435 -0.1081 0.8603 0.046 Uiso 1 1 calc R . . C32 C 0.3566(3) -0.0953(5) 0.7538(2) 0.0348(9) Uani 1 1 d . . . H32A H 0.3535 -0.1927 0.7380 0.042 Uiso 1 1 calc R . . C33 C 0.3827(3) 0.0276(4) 0.6388(2) 0.0276(8) Uani 1 1 d . . . C34 C 0.4288(4) -0.0913(5) 0.6181(3) 0.0426(11) Uani 1 1 d . . . H34A H 0.4455 -0.1703 0.6497 0.051 Uiso 1 1 calc R . . C35 C 0.4502(4) -0.0951(6) 0.5527(2) 0.0472(12) Uani 1 1 d . . . H35A H 0.4807 -0.1766 0.5383 0.057 Uiso 1 1 calc R . . C36 C 0.4266(3) 0.0222(6) 0.5080(2) 0.0421(11) Uani 1 1 d . . . H36A H 0.4424 0.0242 0.4630 0.050 Uiso 1 1 calc R . . C37 C 0.3797(3) 0.1358(5) 0.5301(2) 0.0335(9) Uani 1 1 d . . . H37A H 0.3624 0.2151 0.4988 0.040 Uiso 1 1 calc R . . C38 C 0.1410(3) 0.1780(5) 0.7033(2) 0.0281(8) Uani 1 1 d . . . C39 C 0.1330(3) 0.1413(5) 0.7742(2) 0.0328(9) Uani 1 1 d . . . H39A H 0.1341 0.2070 0.8120 0.039 Uiso 1 1 calc R . . C40 C 0.1232(3) -0.0119(5) 0.7770(2) 0.0368(10) Uani 1 1 d . . . H40A H 0.1168 -0.0665 0.8172 0.044 Uiso 1 1 calc R . . C41 C 0.1246(3) -0.0685(5) 0.7087(2) 0.0386(10) Uani 1 1 d . . . H41A H 0.1194 -0.1676 0.6958 0.046 Uiso 1 1 calc R . . C42 C 0.1350(3) 0.0464(5) 0.6638(2) 0.0354(9) Uani 1 1 d . . . H42A H 0.1376 0.0382 0.6154 0.043 Uiso 1 1 calc R . . C43 C 0.0605(3) 0.4247(5) 0.6196(2) 0.0332(9) Uani 1 1 d . . . C44 C 0.0567(3) 0.5706(5) 0.5997(2) 0.0400(11) Uani 1 1 d . . . H44A H 0.1110 0.6291 0.6138 0.048 Uiso 1 1 calc R . . C45 C -0.0240(4) 0.6303(6) 0.5603(3) 0.0513(13) Uani 1 1 d . . . H45A H -0.0256 0.7294 0.5476 0.062 Uiso 1 1 calc R . . C46 C -0.1031(4) 0.5453(7) 0.5392(3) 0.0506(13) Uani 1 1 d . . . H46A H -0.1596 0.5867 0.5130 0.061 Uiso 1 1 calc R . . C47 C -0.0997(4) 0.4001(7) 0.5562(3) 0.0561(14) Uani 1 1 d . . . H47A H -0.1534 0.3412 0.5400 0.067 Uiso 1 1 calc R . . C48 C -0.0187(3) 0.3398(6) 0.5969(2) 0.0426(11) Uani 1 1 d . . . H48A H -0.0173 0.2404 0.6091 0.051 Uiso 1 1 calc R . . C49 C 0.1902(3) 0.4657(4) 0.7520(2) 0.0277(8) Uani 1 1 d . . . C50 C 0.2802(3) 0.5034(5) 0.7877(2) 0.0330(9) Uani 1 1 d . . . H50A H 0.3323 0.4742 0.7692 0.040 Uiso 1 1 calc R . . C51 C 0.2953(3) 0.5826(5) 0.8498(2) 0.0374(10) Uani 1 1 d . . . H51A H 0.3574 0.6068 0.8735 0.045 Uiso 1 1 calc R . . C52 C 0.2202(3) 0.6268(5) 0.8775(2) 0.0399(10) Uani 1 1 d . . . H52A H 0.2307 0.6797 0.9205 0.048 Uiso 1 1 calc R . . C53 C 0.1298(3) 0.5932(5) 0.8420(3) 0.0397(11) Uani 1 1 d . . . H53A H 0.0780 0.6257 0.8600 0.048 Uiso 1 1 calc R . . C54 C 0.1143(3) 0.5122(5) 0.7801(2) 0.0351(9) Uani 1 1 d . . . H54A H 0.0521 0.4881 0.7566 0.042 Uiso 1 1 calc R . . N1 N -0.3668(3) 0.7371(4) 0.89857(18) 0.0324(8) Uani 1 1 d . . . N2 N 0.3570(2) 0.1404(4) 0.59433(17) 0.0275(7) Uani 1 1 d . . . P1 P -0.21572(7) 0.42061(10) 0.83182(5) 0.0247(2) Uani 1 1 d . . . P2 P 0.16934(7) 0.35308(11) 0.67290(5) 0.0257(2) Uani 1 1 d . . . Fe7 Fe 0.24645(4) 0.04266(6) 0.74808(3) 0.02688(13) Uani 1 1 d . . . Fe8 Fe -0.23072(4) 0.73364(6) 0.75744(3) 0.02496(13) Uani 1 1 d . . . Zn1 Zn -0.32540(3) 0.51575(5) 0.89789(2) 0.02559(10) Uani 1 1 d . . . Zn2 Zn 0.29124(3) 0.34018(5) 0.60596(2) 0.02519(10) Uani 1 1 d . . . Br1 Br -0.47037(3) 0.39079(5) 0.86509(2) 0.03547(10) Uani 1 1 d . . . Br2 Br -0.24186(3) 0.48232(5) 1.01805(2) 0.03926(11) Uani 1 1 d . . . Br3 Br 0.20794(3) 0.40661(5) 0.48922(2) 0.03594(10) Uani 1 1 d . . . Br4 Br 0.41937(3) 0.49930(4) 0.64412(2) 0.03497(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.026(2) 0.0226(19) 0.029(2) 0.0005(15) 0.0053(17) 0.0042(16) C2 0.026(2) 0.0251(19) 0.028(2) 0.0029(15) -0.0001(17) -0.0002(16) C3 0.041(2) 0.031(2) 0.023(2) 0.0003(16) 0.0042(19) 0.0014(19) C4 0.048(3) 0.029(2) 0.030(2) 0.0053(17) 0.012(2) 0.006(2) C5 0.040(2) 0.0218(18) 0.0286(19) 0.0034(16) 0.0092(19) 0.0051(17) C6 0.027(2) 0.0274(19) 0.028(2) -0.0004(16) 0.0094(17) -0.0005(17) C7 0.033(2) 0.029(2) 0.037(2) 0.0004(17) 0.010(2) 0.0036(18) C8 0.050(3) 0.034(2) 0.048(3) -0.006(2) 0.022(2) 0.005(2) C9 0.069(4) 0.045(3) 0.043(3) -0.002(2) 0.028(3) 0.010(3) C10 0.065(3) 0.039(3) 0.037(2) 0.004(2) 0.025(2) 0.011(2) C11 0.0222(19) 0.0262(19) 0.031(2) -0.0010(16) 0.0052(17) 0.0008(16) C12 0.028(2) 0.033(2) 0.035(2) -0.0049(18) 0.0061(19) -0.0011(17) C13 0.030(2) 0.032(2) 0.044(2) -0.0022(18) 0.009(2) -0.0089(18) C14 0.037(3) 0.034(2) 0.047(3) 0.0013(19) 0.020(2) -0.0018(19) C15 0.030(2) 0.029(2) 0.041(2) -0.0014(17) 0.016(2) 0.0015(17) C16 0.032(2) 0.0265(19) 0.027(2) -0.0002(16) 0.0051(18) 0.0024(17) C17 0.036(2) 0.038(2) 0.043(2) 0.005(2) 0.013(2) -0.004(2) C18 0.056(3) 0.036(2) 0.041(3) 0.011(2) 0.010(2) 0.005(2) C19 0.058(3) 0.042(3) 0.038(2) 0.006(2) 0.007(2) 0.017(2) C20 0.037(3) 0.055(3) 0.041(3) 0.003(2) 0.006(2) 0.009(2) C21 0.039(2) 0.036(2) 0.036(2) 0.0053(18) 0.012(2) 0.003(2) C22 0.032(2) 0.0233(19) 0.026(2) 0.0033(15) 0.0111(18) -0.0013(16) C23 0.037(2) 0.0199(18) 0.030(2) -0.0005(15) 0.0070(19) 0.0009(17) C24 0.034(2) 0.028(2) 0.034(2) -0.0011(17) -0.0003(19) 0.0004(18) C25 0.056(3) 0.026(2) 0.032(2) 0.0023(17) 0.010(2) -0.006(2) C26 0.043(3) 0.031(2) 0.034(2) -0.0040(17) 0.016(2) -0.0018(19) C27 0.034(2) 0.028(2) 0.038(2) -0.0039(17) 0.010(2) -0.0028(17) C28 0.030(2) 0.027(2) 0.0287(19) 0.0019(16) 0.0062(17) -0.0002(17) C29 0.029(2) 0.031(2) 0.028(2) 0.0018(17) 0.0039(18) 0.0002(18) C30 0.036(2) 0.035(2) 0.031(2) 0.0011(17) 0.006(2) -0.0009(19) C31 0.040(3) 0.038(2) 0.036(2) 0.0110(18) 0.008(2) -0.001(2) C32 0.040(2) 0.0244(19) 0.041(2) 0.0065(19) 0.012(2) 0.0027(19) C33 0.0259(19) 0.0236(18) 0.033(2) 0.0005(16) 0.0072(17) 0.0020(16) C34 0.053(3) 0.032(2) 0.045(3) 0.001(2) 0.016(2) 0.010(2) C35 0.064(3) 0.039(2) 0.041(2) -0.004(2) 0.017(2) 0.022(2) C36 0.049(3) 0.048(3) 0.032(2) -0.002(2) 0.015(2) 0.013(2) C37 0.036(2) 0.036(2) 0.030(2) 0.0006(17) 0.0101(19) 0.0024(19) C38 0.022(2) 0.036(2) 0.027(2) 0.0004(16) 0.0063(17) -0.0016(17) C39 0.029(2) 0.038(2) 0.033(2) 0.0017(18) 0.0100(19) -0.0007(18) C40 0.035(2) 0.036(2) 0.043(2) 0.0063(19) 0.015(2) -0.0064(19) C41 0.038(2) 0.029(2) 0.048(3) -0.0022(19) 0.007(2) -0.0131(19) C42 0.036(2) 0.035(2) 0.035(2) -0.0033(18) 0.005(2) -0.0040(19) C43 0.036(2) 0.040(2) 0.0261(19) 0.0029(18) 0.0118(19) 0.002(2) C44 0.037(3) 0.039(2) 0.042(3) 0.004(2) 0.006(2) 0.008(2) C45 0.060(3) 0.053(3) 0.041(3) 0.007(2) 0.009(3) 0.017(3) C46 0.034(3) 0.079(4) 0.039(2) 0.016(3) 0.008(2) 0.016(3) C47 0.032(3) 0.081(4) 0.053(3) 0.024(3) 0.002(2) -0.003(3) C48 0.037(3) 0.050(3) 0.040(2) 0.013(2) 0.006(2) -0.001(2) C49 0.029(2) 0.0241(19) 0.033(2) 0.0031(15) 0.0132(18) 0.0021(16) C50 0.037(2) 0.0247(19) 0.038(2) 0.0010(18) 0.0107(19) 0.0054(19) C51 0.041(3) 0.031(2) 0.039(2) -0.0047(18) 0.006(2) -0.0052(19) C52 0.049(3) 0.033(2) 0.039(2) -0.0048(19) 0.013(2) 0.001(2) C53 0.043(3) 0.036(2) 0.045(3) -0.006(2) 0.022(2) 0.003(2) C54 0.033(2) 0.036(2) 0.040(2) 0.0004(19) 0.0164(19) 0.000(2) N1 0.040(2) 0.0300(17) 0.0294(18) 0.0005(15) 0.0119(16) 0.0031(16) N2 0.0260(18) 0.0277(17) 0.0298(17) -0.0022(14) 0.0082(15) -0.0013(14) P1 0.0243(5) 0.0239(5) 0.0263(5) 0.0009(4) 0.0060(4) 0.0003(4) P2 0.0238(5) 0.0276(5) 0.0264(5) 0.0014(4) 0.0074(4) 0.0009(4) Fe7 0.0303(3) 0.0237(3) 0.0274(3) 0.0015(2) 0.0081(3) -0.0032(2) Fe8 0.0286(3) 0.0217(3) 0.0263(3) -0.0002(2) 0.0096(2) -0.0016(2) Zn1 0.0275(2) 0.0249(2) 0.0251(2) 0.00084(17) 0.00716(19) -0.00141(19) Zn2 0.0272(2) 0.0230(2) 0.0266(2) 0.00060(17) 0.00861(19) -0.00071(18) Br1 0.0285(2) 0.0407(2) 0.0383(2) -0.00552(18) 0.00976(18) -0.00798(18) Br2 0.0413(2) 0.0481(3) 0.0260(2) 0.00171(18) 0.00223(19) 0.0000(2) Br3 0.0387(2) 0.0424(2) 0.0274(2) 0.00660(17) 0.00876(19) 0.00256(19) Br4 0.0302(2) 0.02987(19) 0.0453(2) -0.00252(18) 0.00946(18) -0.00644(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.433(6) . ? C1 C5 1.441(5) . ? C1 C6 1.479(5) . ? C1 Fe8 2.057(4) . ? C2 C3 1.428(6) . ? C2 Fe8 2.065(4) . ? C3 C4 1.429(6) . ? C3 Fe8 2.056(4) . ? C4 C5 1.419(6) . ? C4 Fe8 2.065(4) . ? C5 Fe8 2.069(4) . ? C6 N1 1.356(5) . ? C6 C7 1.391(6) . ? C7 C8 1.392(6) . ? C8 C9 1.370(7) . ? C9 C10 1.372(7) . ? C10 N1 1.367(5) . ? C11 C12 1.445(6) . ? C11 C15 1.447(6) . ? C11 P1 1.796(4) . ? C11 Fe8 2.019(4) . ? C12 C13 1.432(6) . ? C12 Fe8 2.045(4) . ? C13 C14 1.418(6) . ? C13 Fe8 2.073(4) . ? C14 C15 1.428(6) . ? C14 Fe8 2.060(4) . ? C15 Fe8 2.025(4) . ? C16 C21 1.383(6) . ? C16 C17 1.405(6) . ? C16 P1 1.819(4) . ? C17 C18 1.383(7) . ? C18 C19 1.393(7) . ? C19 C20 1.384(7) . ? C20 C21 1.391(7) . ? C22 C23 1.392(6) . ? C22 C27 1.407(6) . ? C22 P1 1.831(4) . ? C23 C24 1.389(6) . ? C24 C25 1.380(6) . ? C25 C26 1.390(7) . ? C26 C27 1.385(6) . ? C28 C29 1.436(6) . ? C28 C32 1.443(6) . ? C28 C33 1.481(5) . ? C28 Fe7 2.045(4) . ? C29 C30 1.426(6) . ? C29 Fe7 2.067(4) . ? C30 C31 1.429(6) . ? C30 Fe7 2.054(5) . ? C31 C32 1.417(6) . ? C31 Fe7 2.039(5) . ? C32 Fe7 2.040(4) . ? C33 N2 1.353(5) . ? C33 C34 1.395(6) . ? C34 C35 1.373(6) . ? C35 C36 1.385(7) . ? C36 C37 1.374(6) . ? C37 N2 1.358(5) . ? C38 C42 1.432(6) . ? C38 C39 1.444(6) . ? C38 P2 1.805(4) . ? C38 Fe7 2.028(4) . ? C39 C40 1.429(7) . ? C39 Fe7 2.053(4) . ? C40 C41 1.426(6) . ? C40 Fe7 2.065(4) . ? C41 C42 1.405(6) . ? C41 Fe7 2.053(4) . ? C42 Fe7 2.037(4) . ? C43 C48 1.389(7) . ? C43 C44 1.403(6) . ? C43 P2 1.820(5) . ? C44 C45 1.372(7) . ? C45 C46 1.384(8) . ? C46 C47 1.384(9) . ? C47 C48 1.388(7) . ? C49 C50 1.389(6) . ? C49 C54 1.408(5) . ? C49 P2 1.822(4) . ? C50 C51 1.384(6) . ? C51 C52 1.387(6) . ? C52 C53 1.384(7) . ? C53 C54 1.390(6) . ? N1 Zn1 2.139(4) . ? N2 Zn2 2.120(3) . ? P1 Zn1 2.4277(10) . ? P2 Zn2 2.4278(10) . ? Zn1 Br1 2.3757(6) . ? Zn1 Br2 2.3981(6) . ? Zn2 Br4 2.3704(6) . ? Zn2 Br3 2.4001(6) . ? 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 C2 C1 C5 107.8(3) . . ? C2 C1 C6 126.1(4) . . ? C5 C1 C6 125.9(3) . . ? C2 C1 Fe8 70.0(2) . . ? C5 C1 Fe8 70.0(2) . . ? C6 C1 Fe8 129.3(3) . . ? C3 C2 C1 107.8(4) . . ? C3 C2 Fe8 69.4(2) . . ? C1 C2 Fe8 69.3(2) . . ? C2 C3 C4 108.1(4) . . ? C2 C3 Fe8 70.1(2) . . ? C4 C3 Fe8 70.1(3) . . ? C5 C4 C3 108.5(4) . . ? C5 C4 Fe8 70.1(2) . . ? C3 C4 Fe8 69.4(2) . . ? C4 C5 C1 107.8(4) . . ? C4 C5 Fe8 69.8(2) . . ? C1 C5 Fe8 69.1(2) . . ? N1 C6 C7 121.6(3) . . ? N1 C6 C1 118.8(3) . . ? C7 C6 C1 119.6(4) . . ? C6 C7 C8 120.0(4) . . ? C9 C8 C7 118.4(4) . . ? C8 C9 C10 119.5(4) . . ? N1 C10 C9 123.3(4) . . ? C12 C11 C15 107.3(4) . . ? C12 C11 P1 123.1(3) . . ? C15 C11 P1 128.2(3) . . ? C12 C11 Fe8 70.1(2) . . ? C15 C11 Fe8 69.2(2) . . ? P1 C11 Fe8 115.2(2) . . ? C13 C12 C11 107.6(4) . . ? C13 C12 Fe8 70.7(3) . . ? C11 C12 Fe8 68.2(2) . . ? C14 C13 C12 108.8(4) . . ? C14 C13 Fe8 69.4(3) . . ? C12 C13 Fe8 68.6(2) . . ? C13 C14 C15 108.3(4) . . ? C13 C14 Fe8 70.4(2) . . ? C15 C14 Fe8 68.2(2) . . ? C14 C15 C11 108.0(4) . . ? C14 C15 Fe8 70.9(2) . . ? C11 C15 Fe8 68.8(2) . . ? C21 C16 C17 119.2(4) . . ? C21 C16 P1 123.2(3) . . ? C17 C16 P1 117.7(3) . . ? C18 C17 C16 120.4(4) . . ? C17 C18 C19 120.1(4) . . ? C20 C19 C18 119.6(4) . . ? C19 C20 C21 120.5(5) . . ? C16 C21 C20 120.3(4) . . ? C23 C22 C27 119.0(4) . . ? C23 C22 P1 121.6(3) . . ? C27 C22 P1 119.3(3) . . ? C24 C23 C22 120.1(4) . . ? C25 C24 C23 120.7(4) . . ? C24 C25 C26 119.6(4) . . ? C27 C26 C25 120.5(4) . . ? C26 C27 C22 120.0(4) . . ? C29 C28 C32 107.2(3) . . ? C29 C28 C33 126.7(4) . . ? C32 C28 C33 125.8(4) . . ? C29 C28 Fe7 70.4(2) . . ? C32 C28 Fe7 69.1(2) . . ? C33 C28 Fe7 130.8(3) . . ? C30 C29 C28 108.1(4) . . ? C30 C29 Fe7 69.3(2) . . ? C28 C29 Fe7 68.7(2) . . ? C29 C30 C31 108.2(4) . . ? C29 C30 Fe7 70.2(2) . . ? C31 C30 Fe7 69.0(3) . . ? C32 C31 C30 108.2(4) . . ? C32 C31 Fe7 69.7(3) . . ? C30 C31 Fe7 70.1(3) . . ? C31 C32 C28 108.3(4) . . ? C31 C32 Fe7 69.6(3) . . ? C28 C32 Fe7 69.5(2) . . ? N2 C33 C34 120.7(3) . . ? N2 C33 C28 121.2(3) . . ? C34 C33 C28 118.0(4) . . ? C35 C34 C33 120.6(4) . . ? C34 C35 C36 118.7(4) . . ? C37 C36 C35 118.6(4) . . ? N2 C37 C36 123.3(4) . . ? C42 C38 C39 107.5(4) . . ? C42 C38 P2 125.6(3) . . ? C39 C38 P2 126.5(3) . . ? C42 C38 Fe7 69.7(2) . . ? C39 C38 Fe7 70.2(2) . . ? P2 C38 Fe7 119.2(2) . . ? C40 C39 C38 107.4(4) . . ? C40 C39 Fe7 70.2(3) . . ? C38 C39 Fe7 68.4(2) . . ? C41 C40 C39 108.0(4) . . ? C41 C40 Fe7 69.3(2) . . ? C39 C40 Fe7 69.2(2) . . ? C42 C41 C40 108.8(4) . . ? C42 C41 Fe7 69.3(3) . . ? C40 C41 Fe7 70.2(2) . . ? C41 C42 C38 108.4(4) . . ? C41 C42 Fe7 70.5(3) . . ? C38 C42 Fe7 69.0(2) . . ? C48 C43 C44 118.6(5) . . ? C48 C43 P2 122.5(4) . . ? C44 C43 P2 118.9(4) . . ? C45 C44 C43 121.2(5) . . ? C44 C45 C46 119.7(5) . . ? C47 C46 C45 119.9(5) . . ? C46 C47 C48 120.5(5) . . ? C47 C48 C43 120.0(5) . . ? C50 C49 C54 118.1(4) . . ? C50 C49 P2 121.8(3) . . ? C54 C49 P2 120.0(3) . . ? C51 C50 C49 121.2(4) . . ? C50 C51 C52 120.3(4) . . ? C53 C52 C51 119.5(4) . . ? C52 C53 C54 120.4(4) . . ? C53 C54 C49 120.5(4) . . ? C6 N1 C10 117.0(4) . . ? C6 N1 Zn1 132.7(3) . . ? C10 N1 Zn1 110.2(3) . . ? C33 N2 C37 118.0(3) . . ? C33 N2 Zn2 132.4(3) . . ? C37 N2 Zn2 109.5(3) . . ? C11 P1 C16 108.38(19) . . ? C11 P1 C22 104.34(18) . . ? C16 P1 C22 102.84(18) . . ? C11 P1 Zn1 107.25(13) . . ? C16 P1 Zn1 111.57(13) . . ? C22 P1 Zn1 121.71(13) . . ? C38 P2 C43 106.1(2) . . ? C38 P2 C49 104.38(18) . . ? C43 P2 C49 103.39(19) . . ? C38 P2 Zn2 112.26(13) . . ? C43 P2 Zn2 111.59(13) . . ? C49 P2 Zn2 118.05(13) . . ? C38 Fe7 C42 41.26(17) . . ? C38 Fe7 C31 160.00(17) . . ? C42 Fe7 C31 156.53(19) . . ? C38 Fe7 C32 158.02(16) . . ? C42 Fe7 C32 122.44(18) . . ? C31 Fe7 C32 40.63(18) . . ? C38 Fe7 C28 121.53(16) . . ? C42 Fe7 C28 108.98(17) . . ? C31 Fe7 C28 69.16(17) . . ? C32 Fe7 C28 41.37(16) . . ? C38 Fe7 C39 41.44(16) . . ? C42 Fe7 C39 69.07(18) . . ? C31 Fe7 C39 122.24(18) . . ? C32 Fe7 C39 159.57(17) . . ? C28 Fe7 C39 156.60(17) . . ? C38 Fe7 C41 68.62(17) . . ? C42 Fe7 C41 40.16(18) . . ? C31 Fe7 C41 120.80(19) . . ? C32 Fe7 C41 108.43(19) . . ? C28 Fe7 C41 126.05(17) . . ? C39 Fe7 C41 68.43(18) . . ? C38 Fe7 C30 123.52(18) . . ? C42 Fe7 C30 162.04(18) . . ? C31 Fe7 C30 40.84(18) . . ? C32 Fe7 C30 68.51(18) . . ? C28 Fe7 C30 68.83(16) . . ? C39 Fe7 C30 105.50(18) . . ? C41 Fe7 C30 155.39(18) . . ? C38 Fe7 C40 68.90(17) . . ? C42 Fe7 C40 68.25(18) . . ? C31 Fe7 C40 105.96(18) . . ? C32 Fe7 C40 123.95(18) . . ? C28 Fe7 C40 162.09(17) . . ? C39 Fe7 C40 40.59(18) . . ? C41 Fe7 C40 40.52(18) . . ? C30 Fe7 C40 119.47(18) . . ? C38 Fe7 C29 107.50(16) . . ? C42 Fe7 C29 126.31(17) . . ? C31 Fe7 C29 68.54(17) . . ? C32 Fe7 C29 68.66(17) . . ? C28 Fe7 C29 40.87(16) . . ? C39 Fe7 C29 120.27(18) . . ? C41 Fe7 C29 163.18(17) . . ? C30 Fe7 C29 40.49(16) . . ? C40 Fe7 C29 155.00(18) . . ? C11 Fe8 C15 41.94(16) . . ? C11 Fe8 C12 41.64(16) . . ? C15 Fe8 C12 69.79(18) . . ? C11 Fe8 C3 122.27(17) . . ? C15 Fe8 C3 106.71(18) . . ? C12 Fe8 C3 159.38(17) . . ? C11 Fe8 C1 126.03(15) . . ? C15 Fe8 C1 163.29(16) . . ? C12 Fe8 C1 108.82(16) . . ? C3 Fe8 C1 68.40(16) . . ? C11 Fe8 C14 69.55(17) . . ? C15 Fe8 C14 40.91(18) . . ? C12 Fe8 C14 68.76(18) . . ? C3 Fe8 C14 122.65(18) . . ? C1 Fe8 C14 155.30(17) . . ? C11 Fe8 C4 156.70(17) . . ? C15 Fe8 C4 119.21(17) . . ? C12 Fe8 C4 159.15(18) . . ? C3 Fe8 C4 40.57(18) . . ? C1 Fe8 C4 68.20(16) . . ? C14 Fe8 C4 104.90(18) . . ? C11 Fe8 C2 109.36(16) . . ? C15 Fe8 C2 125.41(17) . . ? C12 Fe8 C2 124.03(16) . . ? C3 Fe8 C2 40.55(16) . . ? C1 Fe8 C2 40.68(16) . . ? C14 Fe8 C2 160.72(17) . . ? C4 Fe8 C2 68.11(17) . . ? C11 Fe8 C5 162.42(15) . . ? C15 Fe8 C5 153.81(16) . . ? C12 Fe8 C5 124.06(16) . . ? C3 Fe8 C5 68.14(17) . . ? C1 Fe8 C5 40.88(15) . . ? C14 Fe8 C5 118.66(18) . . ? C4 Fe8 C5 40.16(16) . . ? C2 Fe8 C5 68.35(16) . . ? C11 Fe8 C13 69.11(17) . . ? C15 Fe8 C13 68.50(18) . . ? C12 Fe8 C13 40.70(17) . . ? C3 Fe8 C13 158.47(17) . . ? C1 Fe8 C13 121.98(16) . . ? C14 Fe8 C13 40.14(18) . . ? C4 Fe8 C13 121.96(18) . . ? C2 Fe8 C13 158.80(16) . . ? C5 Fe8 C13 106.39(18) . . ? N1 Zn1 Br1 103.39(10) . . ? N1 Zn1 Br2 101.66(10) . . ? Br1 Zn1 Br2 115.48(2) . . ? N1 Zn1 P1 124.90(10) . . ? Br1 Zn1 P1 109.67(3) . . ? Br2 Zn1 P1 102.14(3) . . ? N2 Zn2 Br4 103.30(9) . . ? N2 Zn2 Br3 105.76(9) . . ? Br4 Zn2 Br3 109.66(2) . . ? N2 Zn2 P2 120.22(9) . . ? Br4 Zn2 P2 115.21(3) . . ? Br3 Zn2 P2 102.16(3) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.339 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.053 #====================================================================== data_i0501 _database_code_depnum_ccdc_archive 'CCDC 805321' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H22 Br2 Cd Fe N P' _chemical_formula_sum 'C27 H22 Br2 Cd Fe N P' _chemical_formula_weight 719.50 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.8184(13) _cell_length_b 9.3495(6) _cell_length_c 18.8737(17) _cell_angle_alpha 90.00 _cell_angle_beta 91.972(7) _cell_angle_gamma 90.00 _cell_volume 2613.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 10241 _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 25.58 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 4.504 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3289 _exptl_absorpt_correction_T_max 0.9124 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 16395 _diffrn_reflns_av_R_equivalents 0.0789 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4593 _reflns_number_gt 3022 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0256P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4593 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 0.766 _refine_ls_restrained_S_all 0.766 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6736(3) 0.1948(5) 0.0251(2) 0.0426(12) Uani 1 1 d . . . C2 C 0.6381(3) 0.2980(5) 0.0747(3) 0.0494(13) Uani 1 1 d . . . H2A H 0.6597 0.3915 0.0822 0.059 Uiso 1 1 calc R . . C3 C 0.5658(3) 0.2341(6) 0.1097(3) 0.0540(14) Uani 1 1 d . . . H3A H 0.5312 0.2773 0.1446 0.065 Uiso 1 1 calc R . . C4 C 0.5545(3) 0.0935(6) 0.0831(3) 0.0487(13) Uani 1 1 d . . . H4A H 0.5108 0.0274 0.0973 0.058 Uiso 1 1 calc R . . C5 C 0.6195(3) 0.0690(5) 0.0317(2) 0.0404(11) Uani 1 1 d . . . H5A H 0.6263 -0.0162 0.0060 0.048 Uiso 1 1 calc R . . C6 C 0.7581(3) -0.0464(5) 0.1640(2) 0.0390(11) Uani 1 1 d . . . C7 C 0.6961(3) -0.0046(5) 0.2157(2) 0.0404(11) Uani 1 1 d . . . H7A H 0.6508 -0.0627 0.2342 0.048 Uiso 1 1 calc R . . C8 C 0.7139(3) 0.1388(5) 0.2346(2) 0.0481(12) Uani 1 1 d . . . H8A H 0.6826 0.1926 0.2680 0.058 Uiso 1 1 calc R . . C9 C 0.7861(3) 0.1874(5) 0.1952(3) 0.0487(13) Uani 1 1 d . . . H9A H 0.8115 0.2794 0.1982 0.058 Uiso 1 1 calc R . . C10 C 0.8151(3) 0.0756(5) 0.1499(2) 0.0412(11) Uani 1 1 d . . . H10A H 0.8617 0.0802 0.1174 0.049 Uiso 1 1 calc R . . C11 C 0.7465(3) 0.2198(5) -0.0244(2) 0.0412(11) Uani 1 1 d . . . C12 C 0.7617(3) 0.3583(5) -0.0498(3) 0.0481(12) Uani 1 1 d . . . H12A H 0.7269 0.4352 -0.0340 0.058 Uiso 1 1 calc R . . C13 C 0.8276(3) 0.3812(6) -0.0979(3) 0.0568(14) Uani 1 1 d . . . H13A H 0.8388 0.4742 -0.1144 0.068 Uiso 1 1 calc R . . C14 C 0.8776(4) 0.2667(6) -0.1222(3) 0.0560(14) Uani 1 1 d . . . H14A H 0.9219 0.2793 -0.1562 0.067 Uiso 1 1 calc R . . C15 C 0.8597(3) 0.1349(6) -0.0946(3) 0.0521(13) Uani 1 1 d . . . H15A H 0.8942 0.0574 -0.1102 0.063 Uiso 1 1 calc R . . C16 C 0.6534(3) -0.2970(5) 0.1267(2) 0.0357(10) Uani 1 1 d . . . C17 C 0.5893(3) -0.3076(5) 0.0719(3) 0.0411(11) Uani 1 1 d . . . H17A H 0.6027 -0.2725 0.0268 0.049 Uiso 1 1 calc R . . C18 C 0.5060(3) -0.3690(5) 0.0824(3) 0.0462(12) Uani 1 1 d . . . H18A H 0.4633 -0.3762 0.0445 0.055 Uiso 1 1 calc R . . C19 C 0.4856(3) -0.4200(5) 0.1491(3) 0.0509(13) Uani 1 1 d . . . H19A H 0.4286 -0.4603 0.1567 0.061 Uiso 1 1 calc R . . C20 C 0.5493(3) -0.4114(6) 0.2042(3) 0.0542(14) Uani 1 1 d . . . H20A H 0.5356 -0.4467 0.2492 0.065 Uiso 1 1 calc R . . C21 C 0.6328(3) -0.3514(5) 0.1937(2) 0.0465(12) Uani 1 1 d . . . H21A H 0.6759 -0.3468 0.2313 0.056 Uiso 1 1 calc R . . C22 C 0.8458(3) -0.3211(5) 0.1599(2) 0.0375(11) Uani 1 1 d . . . C23 C 0.8703(3) -0.2957(5) 0.2310(2) 0.0409(11) Uani 1 1 d . . . H23A H 0.8430 -0.2206 0.2555 0.049 Uiso 1 1 calc R . . C24 C 0.9346(3) -0.3808(6) 0.2656(3) 0.0491(12) Uani 1 1 d . . . H24A H 0.9521 -0.3614 0.3129 0.059 Uiso 1 1 calc R . . C25 C 0.9726(3) -0.4926(6) 0.2308(3) 0.0523(13) Uani 1 1 d . . . H25A H 1.0152 -0.5510 0.2549 0.063 Uiso 1 1 calc R . . C26 C 0.9493(3) -0.5210(5) 0.1607(3) 0.0519(13) Uani 1 1 d . . . H26A H 0.9760 -0.5981 0.1373 0.062 Uiso 1 1 calc R . . C27 C 0.8861(3) -0.4349(5) 0.1248(3) 0.0448(12) Uani 1 1 d . . . H27A H 0.8706 -0.4534 0.0770 0.054 Uiso 1 1 calc R . . N1 N 0.7964(2) 0.1071(4) -0.0468(2) 0.0418(9) Uani 1 1 d . . . P1 P 0.76184(7) -0.20969(13) 0.11291(6) 0.0357(3) Uani 1 1 d . . . Fe1 Fe 0.68259(4) 0.12057(7) 0.12775(3) 0.03683(16) Uani 1 1 d . . . Br1 Br 0.96347(3) -0.20661(6) -0.03241(3) 0.05545(16) Uani 1 1 d . . . Br2 Br 0.69138(3) -0.24499(6) -0.11304(3) 0.05245(15) Uani 1 1 d . . . Cd1 Cd 0.79846(2) -0.13591(4) -0.016835(18) 0.03951(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(3) 0.039(3) 0.050(3) 0.006(2) -0.004(2) 0.004(2) C2 0.050(3) 0.033(3) 0.065(3) 0.001(3) -0.001(3) 0.006(2) C3 0.047(3) 0.047(3) 0.069(4) -0.007(3) 0.009(2) 0.009(2) C4 0.031(2) 0.052(3) 0.063(3) 0.000(3) 0.000(2) 0.003(2) C5 0.042(3) 0.034(3) 0.044(3) 0.002(2) -0.009(2) 0.002(2) C6 0.040(2) 0.035(3) 0.041(3) 0.001(2) -0.003(2) -0.001(2) C7 0.047(3) 0.032(3) 0.042(3) -0.005(2) 0.007(2) -0.001(2) C8 0.057(3) 0.042(3) 0.045(3) -0.008(3) 0.002(2) 0.002(3) C9 0.051(3) 0.040(3) 0.054(3) -0.009(2) -0.004(2) -0.004(2) C10 0.035(2) 0.044(3) 0.045(3) 0.005(2) -0.005(2) -0.007(2) C11 0.043(3) 0.038(3) 0.042(3) 0.005(2) -0.009(2) -0.002(2) C12 0.048(3) 0.036(3) 0.061(3) 0.007(3) 0.002(2) 0.000(2) C13 0.063(3) 0.041(3) 0.065(4) 0.019(3) -0.006(3) -0.008(3) C14 0.062(3) 0.058(4) 0.049(3) 0.018(3) 0.010(3) -0.002(3) C15 0.059(3) 0.048(3) 0.049(3) 0.007(3) 0.009(2) -0.003(3) C16 0.037(2) 0.027(2) 0.043(3) -0.004(2) 0.001(2) 0.000(2) C17 0.039(3) 0.034(3) 0.050(3) 0.001(2) 0.001(2) 0.003(2) C18 0.043(3) 0.038(3) 0.057(3) 0.003(3) -0.002(2) 0.000(2) C19 0.047(3) 0.042(3) 0.065(4) -0.008(3) 0.011(3) -0.008(2) C20 0.055(3) 0.056(4) 0.053(3) 0.001(3) 0.015(3) -0.015(3) C21 0.045(3) 0.051(3) 0.043(3) -0.005(3) 0.001(2) -0.001(2) C22 0.032(2) 0.033(3) 0.047(3) -0.002(2) 0.004(2) -0.0030(19) C23 0.044(3) 0.037(3) 0.042(3) -0.005(2) 0.005(2) 0.000(2) C24 0.050(3) 0.048(3) 0.049(3) 0.005(3) -0.004(2) 0.001(3) C25 0.044(3) 0.046(3) 0.067(4) 0.015(3) -0.001(3) -0.001(2) C26 0.052(3) 0.038(3) 0.066(4) -0.001(3) 0.010(3) 0.006(2) C27 0.047(3) 0.042(3) 0.046(3) -0.004(2) 0.005(2) -0.001(2) N1 0.046(2) 0.033(2) 0.047(2) 0.0049(18) 0.0038(18) 0.0023(18) P1 0.0348(6) 0.0347(7) 0.0375(7) 0.0000(5) 0.0007(5) 0.0001(5) Fe1 0.0366(3) 0.0311(4) 0.0427(4) -0.0010(3) 0.0005(3) 0.0001(3) Br1 0.0447(3) 0.0674(4) 0.0546(3) 0.0019(3) 0.0066(2) 0.0112(3) Br2 0.0522(3) 0.0605(4) 0.0444(3) -0.0060(3) -0.0015(2) -0.0071(2) Cd1 0.04013(18) 0.0369(2) 0.0416(2) -0.00001(17) 0.00272(14) 0.00065(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.431(6) . ? C1 C11 1.472(6) . ? C1 C2 1.455(7) . ? C1 Fe1 2.057(5) . ? C2 C3 1.410(7) . ? C2 Fe1 2.035(5) . ? C2 H2A 0.9400 . ? C3 C4 1.415(7) . ? C3 Fe1 2.048(5) . ? C3 H3A 0.9400 . ? C4 C5 1.408(7) . ? C4 Fe1 2.066(4) . ? C4 H4A 0.9400 . ? C5 Fe1 2.067(4) . ? C5 H5A 0.9400 . ? C6 C7 1.417(6) . ? C6 C10 1.450(6) . ? C6 P1 1.807(5) . ? C6 Fe1 2.026(4) . ? C7 C8 1.411(6) . ? C7 Fe1 2.035(5) . ? C7 H7A 0.9400 . ? C8 C9 1.400(7) . ? C8 Fe1 2.061(5) . ? C8 H8A 0.9400 . ? C9 C10 1.426(6) . ? C9 Fe1 2.056(5) . ? C9 H9A 0.9400 . ? C10 Fe1 2.037(4) . ? C10 H10A 0.9400 . ? C11 N1 1.364(6) . ? C11 C12 1.401(6) . ? C12 C13 1.372(7) . ? C12 H12A 0.9400 . ? C13 C14 1.389(7) . ? C13 H13A 0.9400 . ? C14 C15 1.368(7) . ? C14 H14A 0.9400 . ? C15 N1 1.348(6) . ? C15 H15A 0.9400 . ? C16 C17 1.383(6) . ? C16 C21 1.407(6) . ? C16 P1 1.829(4) . ? C17 C18 1.382(6) . ? C17 H17A 0.9400 . ? C18 C19 1.389(7) . ? C18 H18A 0.9400 . ? C19 C20 1.384(7) . ? C19 H19A 0.9400 . ? C20 C21 1.378(6) . ? C20 H20A 0.9400 . ? C21 H21A 0.9400 . ? C22 C27 1.398(6) . ? C22 C23 1.398(6) . ? C22 P1 1.829(4) . ? C23 C24 1.387(6) . ? C23 H23A 0.9400 . ? C24 C25 1.366(7) . ? C24 H24A 0.9400 . ? C25 C26 1.382(7) . ? C25 H25A 0.9400 . ? C26 C27 1.392(6) . ? C26 H26A 0.9400 . ? C27 H27A 0.9400 . ? N1 Cd1 2.341(4) . ? P1 Cd1 2.6189(12) . ? Br1 Cd1 2.5597(6) . ? Br2 Cd1 2.5800(6) . ? 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 C5 C1 C11 127.7(4) . . ? C5 C1 C2 105.9(4) . . ? C11 C1 C2 126.4(4) . . ? C5 C1 Fe1 70.1(3) . . ? C11 C1 Fe1 128.8(3) . . ? C2 C1 Fe1 68.4(3) . . ? C3 C2 C1 108.5(4) . . ? C3 C2 Fe1 70.3(3) . . ? C1 C2 Fe1 70.0(3) . . ? C3 C2 H2A 125.8 . . ? C1 C2 H2A 125.8 . . ? Fe1 C2 H2A 125.5 . . ? C4 C3 C2 108.1(4) . . ? C4 C3 Fe1 70.6(3) . . ? C2 C3 Fe1 69.3(3) . . ? C4 C3 H3A 126.0 . . ? C2 C3 H3A 126.0 . . ? Fe1 C3 H3A 125.8 . . ? C5 C4 C3 108.6(4) . . ? C5 C4 Fe1 70.1(2) . . ? C3 C4 Fe1 69.2(3) . . ? C5 C4 H4A 125.7 . . ? C3 C4 H4A 125.7 . . ? Fe1 C4 H4A 126.6 . . ? C4 C5 C1 108.9(4) . . ? C4 C5 Fe1 70.0(3) . . ? C1 C5 Fe1 69.3(3) . . ? C4 C5 H5A 125.5 . . ? C1 C5 H5A 125.5 . . ? Fe1 C5 H5A 126.7 . . ? C7 C6 C10 107.8(4) . . ? C7 C6 P1 129.2(3) . . ? C10 C6 P1 122.5(3) . . ? C7 C6 Fe1 69.9(3) . . ? C10 C6 Fe1 69.5(2) . . ? P1 C6 Fe1 119.8(2) . . ? C8 C7 C6 108.5(4) . . ? C8 C7 Fe1 70.9(3) . . ? C6 C7 Fe1 69.2(3) . . ? C8 C7 H7A 125.8 . . ? C6 C7 H7A 125.8 . . ? Fe1 C7 H7A 125.7 . . ? C9 C8 C7 108.2(4) . . ? C9 C8 Fe1 69.9(3) . . ? C7 C8 Fe1 68.9(3) . . ? C9 C8 H8A 125.9 . . ? C7 C8 H8A 125.9 . . ? Fe1 C8 H8A 126.9 . . ? C8 C9 C10 109.5(4) . . ? C8 C9 Fe1 70.3(3) . . ? C10 C9 Fe1 68.9(2) . . ? C8 C9 H9A 125.3 . . ? C10 C9 H9A 125.3 . . ? Fe1 C9 H9A 127.1 . . ? C9 C10 C6 106.0(4) . . ? C9 C10 Fe1 70.3(3) . . ? C6 C10 Fe1 68.7(2) . . ? C9 C10 H10A 127.0 . . ? C6 C10 H10A 127.0 . . ? Fe1 C10 H10A 125.6 . . ? N1 C11 C12 120.8(4) . . ? N1 C11 C1 119.5(4) . . ? C12 C11 C1 119.7(4) . . ? C13 C12 C11 119.8(5) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 119.9(5) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C15 C14 C13 117.1(5) . . ? C15 C14 H14A 121.5 . . ? C13 C14 H14A 121.5 . . ? N1 C15 C14 125.3(5) . . ? N1 C15 H15A 117.4 . . ? C14 C15 H15A 117.4 . . ? C17 C16 C21 118.8(4) . . ? C17 C16 P1 120.6(3) . . ? C21 C16 P1 120.5(3) . . ? C16 C17 C18 121.1(4) . . ? C16 C17 H17A 119.4 . . ? C18 C17 H17A 119.4 . . ? C17 C18 C19 119.7(4) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C20 C19 C18 119.8(4) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C21 C20 C19 120.6(5) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C16 120.0(4) . . ? C20 C21 H21A 120.0 . . ? C16 C21 H21A 120.0 . . ? C27 C22 C23 118.8(4) . . ? C27 C22 P1 119.9(3) . . ? C23 C22 P1 121.2(3) . . ? C24 C23 C22 120.4(4) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C25 C24 C23 120.0(5) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.9(5) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C27 119.7(5) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C22 C27 C26 120.1(5) . . ? C22 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C15 N1 C11 117.1(4) . . ? C15 N1 Cd1 110.2(3) . . ? C11 N1 Cd1 132.7(3) . . ? C6 P1 C22 104.8(2) . . ? C6 P1 C16 105.0(2) . . ? C22 P1 C16 105.3(2) . . ? C6 P1 Cd1 106.70(15) . . ? C22 P1 Cd1 116.36(15) . . ? C16 P1 Cd1 117.50(15) . . ? C6 Fe1 C7 40.85(17) . . ? C6 Fe1 C2 163.70(19) . . ? C7 Fe1 C2 153.00(19) . . ? C6 Fe1 C3 155.4(2) . . ? C7 Fe1 C3 119.5(2) . . ? C2 Fe1 C3 40.40(19) . . ? C6 Fe1 C10 41.80(17) . . ? C7 Fe1 C10 69.33(18) . . ? C2 Fe1 C10 124.22(19) . . ? C3 Fe1 C10 160.7(2) . . ? C6 Fe1 C9 68.49(19) . . ? C7 Fe1 C9 67.62(19) . . ? C2 Fe1 C9 106.2(2) . . ? C3 Fe1 C9 123.6(2) . . ? C10 Fe1 C9 40.78(18) . . ? C6 Fe1 C8 68.31(19) . . ? C7 Fe1 C8 40.28(18) . . ? C2 Fe1 C8 118.2(2) . . ? C3 Fe1 C8 106.3(2) . . ? C10 Fe1 C8 68.53(19) . . ? C9 Fe1 C8 39.74(19) . . ? C6 Fe1 C4 122.17(19) . . ? C7 Fe1 C4 109.0(2) . . ? C2 Fe1 C4 67.8(2) . . ? C3 Fe1 C4 40.24(19) . . ? C10 Fe1 C4 157.5(2) . . ? C9 Fe1 C4 160.9(2) . . ? C8 Fe1 C4 125.6(2) . . ? C6 Fe1 C5 110.12(18) . . ? C7 Fe1 C5 127.56(18) . . ? C2 Fe1 C5 68.29(19) . . ? C3 Fe1 C5 67.7(2) . . ? C10 Fe1 C5 122.34(19) . . ? C9 Fe1 C5 156.73(19) . . ? C8 Fe1 C5 163.11(19) . . ? C4 Fe1 C5 39.85(18) . . ? C6 Fe1 C1 126.51(18) . . ? C7 Fe1 C1 164.38(19) . . ? C2 Fe1 C1 41.64(19) . . ? C3 Fe1 C1 68.98(19) . . ? C10 Fe1 C1 107.06(18) . . ? C9 Fe1 C1 120.2(2) . . ? C8 Fe1 C1 154.0(2) . . ? C4 Fe1 C1 68.17(19) . . ? C5 Fe1 C1 40.60(18) . . ? N1 Cd1 Br1 103.13(9) . . ? N1 Cd1 Br2 102.18(9) . . ? Br1 Cd1 Br2 112.58(2) . . ? N1 Cd1 P1 118.71(10) . . ? Br1 Cd1 P1 105.60(3) . . ? Br2 Cd1 P1 114.31(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.730 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.089 #================================================================= data_i0731 _database_code_depnum_ccdc_archive 'CCDC 805322' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H22 Cd Fe I2 N P' _chemical_formula_sum 'C27 H22 Cd Fe I2 N P' _chemical_formula_weight 813.48 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' 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4638(10) _cell_length_b 10.5429(8) _cell_length_c 14.1699(11) _cell_angle_alpha 72.904(6) _cell_angle_beta 69.694(7) _cell_angle_gamma 70.125(7) _cell_volume 1351.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 12579 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 25.59 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 3.684 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2744 _exptl_absorpt_correction_T_max 0.8511 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 8799 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4481 _reflns_number_gt 3978 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.5229P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0041(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4481 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0835 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6107(4) 0.7162(4) 0.1238(3) 0.0312(9) Uani 1 1 d . . . C2 C 0.4692(4) 0.7543(5) 0.1132(3) 0.0407(10) Uani 1 1 d . . . H2A H 0.4035 0.8421 0.1162 0.049 Uiso 1 1 calc R . . C3 C 0.4453(5) 0.6395(5) 0.0977(4) 0.0430(11) Uani 1 1 d . . . H3A H 0.3610 0.6368 0.0881 0.052 Uiso 1 1 calc R . . C4 C 0.5687(5) 0.5282(5) 0.0989(4) 0.0433(11) Uani 1 1 d . . . H4A H 0.5808 0.4384 0.0904 0.052 Uiso 1 1 calc R . . C5 C 0.6712(4) 0.5743(4) 0.1152(3) 0.0348(9) Uani 1 1 d . . . H5A H 0.7633 0.5207 0.1195 0.042 Uiso 1 1 calc R . . C6 C 0.5416(4) 0.4699(4) 0.3651(3) 0.0355(9) Uani 1 1 d . . . C7 C 0.4923(4) 0.6126(5) 0.3756(3) 0.0379(10) Uani 1 1 d . . . H7A H 0.5439 0.6615 0.3885 0.045 Uiso 1 1 calc R . . C8 C 0.3539(5) 0.6665(5) 0.3633(3) 0.0472(12) Uani 1 1 d . . . H8A H 0.2972 0.7582 0.3658 0.057 Uiso 1 1 calc R . . C9 C 0.3145(5) 0.5610(6) 0.3466(4) 0.0539(13) Uani 1 1 d . . . H9A H 0.2267 0.5694 0.3364 0.065 Uiso 1 1 calc R . . C10 C 0.4296(5) 0.4394(5) 0.3477(4) 0.0449(11) Uani 1 1 d . . . H10A H 0.4314 0.3531 0.3383 0.054 Uiso 1 1 calc R . . C11 C 0.6765(4) 0.3727(4) 0.3766(3) 0.0334(9) Uani 1 1 d . . . C12 C 0.6915(5) 0.2314(5) 0.4009(4) 0.0450(11) Uani 1 1 d . . . H12A H 0.6156 0.1979 0.4053 0.054 Uiso 1 1 calc R . . C13 C 0.8142(6) 0.1401(5) 0.4186(4) 0.0517(13) Uani 1 1 d . . . H13A H 0.8248 0.0438 0.4327 0.062 Uiso 1 1 calc R . . C14 C 0.9223(5) 0.1897(5) 0.4157(4) 0.0476(12) Uani 1 1 d . . . H14A H 1.0067 0.1291 0.4309 0.057 Uiso 1 1 calc R . . C15 C 0.9030(5) 0.3316(5) 0.3897(4) 0.0412(10) Uani 1 1 d . . . H15A H 0.9762 0.3670 0.3880 0.049 Uiso 1 1 calc R . . C16 C 0.5555(4) 0.9526(4) 0.2092(3) 0.0343(9) Uani 1 1 d . . . C17 C 0.5271(4) 0.9609(4) 0.3106(3) 0.0378(10) Uani 1 1 d . . . H17A H 0.5830 0.8944 0.3525 0.045 Uiso 1 1 calc R . . C18 C 0.4180(5) 1.0652(5) 0.3512(4) 0.0453(11) Uani 1 1 d . . . H18A H 0.3988 1.0690 0.4211 0.054 Uiso 1 1 calc R . . C19 C 0.3366(5) 1.1638(5) 0.2917(4) 0.0471(12) Uani 1 1 d . . . H19A H 0.2608 1.2346 0.3204 0.057 Uiso 1 1 calc R . . C20 C 0.3669(5) 1.1583(5) 0.1889(5) 0.0522(13) Uani 1 1 d . . . H20A H 0.3129 1.2272 0.1468 0.063 Uiso 1 1 calc R . . C21 C 0.4745(5) 1.0539(5) 0.1479(4) 0.0442(11) Uani 1 1 d . . . H21A H 0.4939 1.0506 0.0779 0.053 Uiso 1 1 calc R . . C22 C 0.7975(4) 0.8927(4) 0.0333(3) 0.0339(9) Uani 1 1 d . . . C23 C 0.8734(5) 0.8136(5) -0.0410(4) 0.0466(12) Uani 1 1 d . . . H23A H 0.8695 0.7210 -0.0268 0.056 Uiso 1 1 calc R . . C24 C 0.9549(6) 0.8663(7) -0.1356(4) 0.0663(16) Uani 1 1 d . . . H24A H 1.0066 0.8106 -0.1856 0.080 Uiso 1 1 calc R . . C25 C 0.9596(6) 1.0012(7) -0.1557(5) 0.0666(17) Uani 1 1 d . . . H25A H 1.0133 1.0394 -0.2206 0.080 Uiso 1 1 calc R . . C26 C 0.8869(5) 1.0808(5) -0.0823(5) 0.0611(16) Uani 1 1 d . . . H26A H 0.8919 1.1731 -0.0965 0.073 Uiso 1 1 calc R . . C27 C 0.8059(5) 1.0264(5) 0.0128(5) 0.0503(13) Uani 1 1 d . . . H27A H 0.7565 1.0813 0.0635 0.060 Uiso 1 1 calc R . . N1 N 0.7850(3) 0.4213(3) 0.3668(3) 0.0336(8) Uani 1 1 d . . . P1 P 0.69590(10) 0.81209(10) 0.15654(8) 0.0289(2) Uani 1 1 d . . . Fe1 Fe 0.49336(6) 0.59651(6) 0.23471(5) 0.03223(16) Uani 1 1 d . . . Cd1 Cd 0.84082(3) 0.63296(3) 0.27681(2) 0.02893(11) Uani 1 1 d . . . I1 I 0.86281(3) 0.72827(3) 0.42870(2) 0.04081(12) Uani 1 1 d . . . I2 I 1.08915(3) 0.52017(3) 0.14282(2) 0.04028(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(2) 0.042(2) 0.020(2) -0.0033(17) -0.0068(15) -0.0111(17) C2 0.036(2) 0.055(3) 0.029(3) 0.000(2) -0.0125(18) -0.015(2) C3 0.044(2) 0.057(3) 0.035(3) -0.004(2) -0.0135(19) -0.025(2) C4 0.057(3) 0.042(2) 0.039(3) -0.012(2) -0.007(2) -0.026(2) C5 0.037(2) 0.038(2) 0.028(2) -0.0091(18) -0.0012(17) -0.0140(18) C6 0.042(2) 0.036(2) 0.027(2) -0.0005(18) -0.0033(17) -0.0206(19) C7 0.036(2) 0.048(3) 0.024(2) -0.0080(19) -0.0003(17) -0.0120(19) C8 0.038(2) 0.060(3) 0.027(3) -0.004(2) 0.0002(19) -0.005(2) C9 0.033(2) 0.081(4) 0.043(3) -0.004(3) -0.001(2) -0.026(2) C10 0.043(2) 0.055(3) 0.040(3) -0.002(2) -0.006(2) -0.029(2) C11 0.039(2) 0.039(2) 0.022(2) -0.0009(17) -0.0087(17) -0.0138(18) C12 0.061(3) 0.034(2) 0.045(3) -0.004(2) -0.011(2) -0.024(2) C13 0.068(3) 0.031(2) 0.049(3) -0.004(2) -0.014(2) -0.010(2) C14 0.053(3) 0.038(2) 0.042(3) 0.005(2) -0.017(2) -0.009(2) C15 0.046(2) 0.037(2) 0.039(3) 0.0033(19) -0.0161(19) -0.0134(19) C16 0.034(2) 0.031(2) 0.036(3) -0.0067(18) -0.0137(17) -0.0023(16) C17 0.039(2) 0.033(2) 0.039(3) -0.0085(19) -0.0117(18) -0.0034(17) C18 0.046(3) 0.044(2) 0.045(3) -0.021(2) -0.005(2) -0.010(2) C19 0.034(2) 0.043(2) 0.065(4) -0.024(2) -0.015(2) 0.0029(19) C20 0.048(3) 0.036(2) 0.072(4) -0.011(2) -0.033(2) 0.006(2) C21 0.046(3) 0.041(2) 0.043(3) -0.009(2) -0.019(2) 0.000(2) C22 0.034(2) 0.033(2) 0.035(2) 0.0032(18) -0.0158(17) -0.0112(17) C23 0.061(3) 0.051(3) 0.034(3) -0.009(2) -0.004(2) -0.031(2) C24 0.070(4) 0.091(4) 0.041(3) -0.009(3) 0.000(3) -0.045(3) C25 0.068(3) 0.075(4) 0.056(4) 0.019(3) -0.018(3) -0.044(3) C26 0.053(3) 0.034(2) 0.093(5) 0.022(3) -0.033(3) -0.024(2) C27 0.036(2) 0.040(2) 0.072(4) -0.003(2) -0.017(2) -0.011(2) N1 0.0388(18) 0.0293(17) 0.034(2) 0.0011(14) -0.0136(15) -0.0131(14) P1 0.0296(5) 0.0265(5) 0.0289(6) -0.0045(4) -0.0101(4) -0.0042(4) Fe1 0.0295(3) 0.0396(3) 0.0276(3) -0.0050(3) -0.0053(2) -0.0132(2) Cd1 0.02921(18) 0.02674(17) 0.0298(2) -0.00471(12) -0.00925(12) -0.00582(12) I1 0.0512(2) 0.04024(18) 0.0366(2) -0.01047(13) -0.01679(13) -0.01176(14) I2 0.03248(17) 0.03488(17) 0.0460(2) -0.01283(13) -0.00207(12) -0.00468(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.436(6) . ? C1 C2 1.446(6) . ? C1 P1 1.791(4) . ? C1 Fe1 2.029(4) . ? C2 C3 1.406(7) . ? C2 Fe1 2.032(5) . ? C2 H2A 0.9500 . ? C3 C4 1.421(7) . ? C3 Fe1 2.057(5) . ? C3 H3A 0.9500 . ? C4 C5 1.425(6) . ? C4 Fe1 2.054(5) . ? C4 H4A 0.9500 . ? C5 Fe1 2.034(4) . ? C5 H5A 0.9500 . ? C6 C10 1.429(6) . ? C6 C7 1.450(6) . ? C6 C11 1.466(6) . ? C6 Fe1 2.047(5) . ? C7 C8 1.418(7) . ? C7 Fe1 2.049(5) . ? C7 H7A 0.9500 . ? C8 C9 1.413(8) . ? C8 Fe1 2.051(4) . ? C8 H8A 0.9500 . ? C9 C10 1.431(7) . ? C9 Fe1 2.055(4) . ? C9 H9A 0.9500 . ? C10 Fe1 2.050(5) . ? C10 H10A 0.9500 . ? C11 N1 1.348(5) . ? C11 C12 1.392(6) . ? C12 C13 1.370(7) . ? C12 H12A 0.9500 . ? C13 C14 1.383(8) . ? C13 H13A 0.9500 . ? C14 C15 1.392(6) . ? C14 H14A 0.9500 . ? C15 N1 1.352(6) . ? C15 H15A 0.9500 . ? C16 C17 1.386(6) . ? C16 C21 1.400(6) . ? C16 P1 1.822(4) . ? C17 C18 1.380(6) . ? C17 H17A 0.9500 . ? C18 C19 1.378(7) . ? C18 H18A 0.9500 . ? C19 C20 1.394(8) . ? C19 H19A 0.9500 . ? C20 C21 1.377(7) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C27 1.380(6) . ? C22 C23 1.385(6) . ? C22 P1 1.832(4) . ? C23 C24 1.387(7) . ? C23 H23A 0.9500 . ? C24 C25 1.381(9) . ? C24 H24A 0.9500 . ? C25 C26 1.376(9) . ? C25 H25A 0.9500 . ? C26 C27 1.396(8) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N1 Cd1 2.375(3) . ? P1 Cd1 2.5932(11) . ? Cd1 I1 2.7326(4) . ? Cd1 I2 2.7520(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 106.8(4) . . ? C5 C1 P1 123.4(3) . . ? C2 C1 P1 129.4(3) . . ? C5 C1 Fe1 69.5(2) . . ? C2 C1 Fe1 69.2(2) . . ? P1 C1 Fe1 120.8(2) . . ? C3 C2 C1 108.5(4) . . ? C3 C2 Fe1 70.9(3) . . ? C1 C2 Fe1 69.0(3) . . ? C3 C2 H2A 125.8 . . ? C1 C2 H2A 125.8 . . ? Fe1 C2 H2A 125.9 . . ? C2 C3 C4 108.5(4) . . ? C2 C3 Fe1 68.9(3) . . ? C4 C3 Fe1 69.7(3) . . ? C2 C3 H3A 125.8 . . ? C4 C3 H3A 125.8 . . ? Fe1 C3 H3A 127.2 . . ? C3 C4 C5 108.3(4) . . ? C3 C4 Fe1 69.9(3) . . ? C5 C4 Fe1 68.8(2) . . ? C3 C4 H4A 125.9 . . ? C5 C4 H4A 125.9 . . ? Fe1 C4 H4A 127.0 . . ? C4 C5 C1 108.0(4) . . ? C4 C5 Fe1 70.4(2) . . ? C1 C5 Fe1 69.1(2) . . ? C4 C5 H5A 126.0 . . ? C1 C5 H5A 126.0 . . ? Fe1 C5 H5A 126.1 . . ? C10 C6 C7 106.8(4) . . ? C10 C6 C11 126.3(4) . . ? C7 C6 C11 126.8(4) . . ? C10 C6 Fe1 69.7(3) . . ? C7 C6 Fe1 69.3(3) . . ? C11 C6 Fe1 128.8(3) . . ? C8 C7 C6 108.1(4) . . ? C8 C7 Fe1 69.8(3) . . ? C6 C7 Fe1 69.2(3) . . ? C8 C7 H7A 125.9 . . ? C6 C7 H7A 125.9 . . ? Fe1 C7 H7A 126.6 . . ? C9 C8 C7 108.5(4) . . ? C9 C8 Fe1 70.0(3) . . ? C7 C8 Fe1 69.7(2) . . ? C9 C8 H8A 125.8 . . ? C7 C8 H8A 125.8 . . ? Fe1 C8 H8A 126.1 . . ? C8 C9 C10 108.3(4) . . ? C8 C9 Fe1 69.7(2) . . ? C10 C9 Fe1 69.4(2) . . ? C8 C9 H9A 125.9 . . ? C10 C9 H9A 125.9 . . ? Fe1 C9 H9A 126.6 . . ? C6 C10 C9 108.3(4) . . ? C6 C10 Fe1 69.5(2) . . ? C9 C10 Fe1 69.8(3) . . ? C6 C10 H10A 125.9 . . ? C9 C10 H10A 125.9 . . ? Fe1 C10 H10A 126.4 . . ? N1 C11 C12 120.1(4) . . ? N1 C11 C6 119.3(4) . . ? C12 C11 C6 120.5(4) . . ? C13 C12 C11 120.9(4) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C13 C14 C15 117.6(5) . . ? C13 C14 H14A 121.2 . . ? C15 C14 H14A 121.2 . . ? N1 C15 C14 123.0(4) . . ? N1 C15 H15A 118.5 . . ? C14 C15 H15A 118.5 . . ? C17 C16 C21 118.9(4) . . ? C17 C16 P1 120.5(3) . . ? C21 C16 P1 120.6(3) . . ? C18 C17 C16 120.4(4) . . ? C18 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C20 119.1(4) . . ? C18 C19 H19A 120.5 . . ? C20 C19 H19A 120.5 . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C16 120.2(5) . . ? C20 C21 H21A 119.9 . . ? C16 C21 H21A 119.9 . . ? C27 C22 C23 118.8(4) . . ? C27 C22 P1 122.9(4) . . ? C23 C22 P1 118.2(3) . . ? C22 C23 C24 121.7(5) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C25 C24 C23 118.7(6) . . ? C25 C24 H24A 120.6 . . ? C23 C24 H24A 120.6 . . ? C26 C25 C24 120.5(5) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 120.2(5) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C22 C27 C26 120.0(5) . . ? C22 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C11 N1 C15 118.8(4) . . ? C11 N1 Cd1 131.8(3) . . ? C15 N1 Cd1 107.6(3) . . ? C1 P1 C16 105.95(19) . . ? C1 P1 C22 104.95(19) . . ? C16 P1 C22 105.70(19) . . ? C1 P1 Cd1 104.99(14) . . ? C16 P1 Cd1 117.71(15) . . ? C22 P1 Cd1 116.36(13) . . ? C1 Fe1 C2 41.72(17) . . ? C1 Fe1 C5 41.41(16) . . ? C2 Fe1 C5 69.38(18) . . ? C1 Fe1 C6 126.92(17) . . ? C2 Fe1 C6 164.82(18) . . ? C5 Fe1 C6 108.61(18) . . ? C1 Fe1 C7 108.96(17) . . ? C2 Fe1 C7 126.07(19) . . ? C5 Fe1 C7 122.83(18) . . ? C6 Fe1 C7 41.47(17) . . ? C1 Fe1 C10 163.93(18) . . ? C2 Fe1 C10 152.63(18) . . ? C5 Fe1 C10 125.46(19) . . ? C6 Fe1 C10 40.82(18) . . ? C7 Fe1 C10 68.67(19) . . ? C1 Fe1 C8 120.84(19) . . ? C2 Fe1 C8 106.7(2) . . ? C5 Fe1 C8 157.35(19) . . ? C6 Fe1 C8 69.02(19) . . ? C7 Fe1 C8 40.46(19) . . ? C10 Fe1 C8 68.4(2) . . ? C1 Fe1 C4 69.07(17) . . ? C2 Fe1 C4 68.3(2) . . ? C5 Fe1 C4 40.81(18) . . ? C6 Fe1 C4 120.67(19) . . ? C7 Fe1 C4 157.55(19) . . ? C10 Fe1 C4 106.71(19) . . ? C8 Fe1 C4 160.2(2) . . ? C1 Fe1 C9 154.5(2) . . ? C2 Fe1 C9 118.0(2) . . ? C5 Fe1 C9 161.6(2) . . ? C6 Fe1 C9 68.79(19) . . ? C7 Fe1 C9 68.1(2) . . ? C10 Fe1 C9 40.8(2) . . ? C8 Fe1 C9 40.3(2) . . ? C4 Fe1 C9 123.6(2) . . ? C1 Fe1 C3 68.99(17) . . ? C2 Fe1 C3 40.21(19) . . ? C5 Fe1 C3 68.65(18) . . ? C6 Fe1 C3 154.31(18) . . ? C7 Fe1 C3 161.45(19) . . ? C10 Fe1 C3 118.52(19) . . ? C8 Fe1 C3 123.6(2) . . ? C4 Fe1 C3 40.4(2) . . ? C9 Fe1 C3 105.4(2) . . ? N1 Cd1 P1 121.60(9) . . ? N1 Cd1 I1 102.22(9) . . ? P1 Cd1 I1 115.64(3) . . ? N1 Cd1 I2 96.02(8) . . ? P1 Cd1 I2 103.49(3) . . ? I1 Cd1 I2 116.990(15) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.793 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.114 #================================================================== data_i0507a _database_code_depnum_ccdc_archive 'CCDC 805323' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H22 Br2 Fe Hg N P' _chemical_formula_sum 'C27 H22 Br2 Fe Hg N P' _chemical_formula_weight 807.69 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1471(10) _cell_length_b 10.3258(10) _cell_length_c 13.6179(13) _cell_angle_alpha 104.921(8) _cell_angle_beta 92.316(8) _cell_angle_gamma 110.214(8) _cell_volume 1280.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13800 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.66 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 9.752 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2161 _exptl_absorpt_correction_T_max 0.5998 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 208 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 9514 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4485 _reflns_number_gt 4156 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4485 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0536 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.2609(4) 0.1202(4) 0.3776(3) 0.0199(7) Uani 1 1 d . . . C2 C -0.2932(5) -0.0227(4) 0.3898(3) 0.0244(8) Uani 1 1 d . . . H2A H -0.3853 -0.0911 0.3874 0.029 Uiso 1 1 calc R . . C3 C -0.1626(5) -0.0422(4) 0.4059(3) 0.0265(8) Uani 1 1 d . . . H3A H -0.1525 -0.1263 0.4158 0.032 Uiso 1 1 calc R . . C4 C -0.0493(5) 0.0863(4) 0.4046(3) 0.0278(9) Uani 1 1 d . . . H4A H 0.0489 0.1020 0.4141 0.033 Uiso 1 1 calc R . . C5 C -0.1072(4) 0.1870(4) 0.3870(3) 0.0226(8) Uani 1 1 d . . . H5A H -0.0551 0.2807 0.3821 0.027 Uiso 1 1 calc R . . C6 C -0.1175(4) 0.0455(4) 0.1364(3) 0.0204(7) Uani 1 1 d . . . C7 C -0.2702(4) -0.0132(4) 0.1237(3) 0.0221(8) Uani 1 1 d . . . H7A H -0.3317 0.0327 0.1085 0.026 Uiso 1 1 calc R . . C8 C -0.3124(5) -0.1542(4) 0.1384(3) 0.0295(9) Uani 1 1 d . . . H8A H -0.4074 -0.2183 0.1336 0.035 Uiso 1 1 calc R . . C9 C -0.1891(5) -0.1818(4) 0.1611(3) 0.0309(10) Uani 1 1 d . . . H9A H -0.1871 -0.2668 0.1748 0.037 Uiso 1 1 calc R . . C10 C -0.0685(5) -0.0597(4) 0.1599(3) 0.0269(9) Uani 1 1 d . . . H10A H 0.0279 -0.0496 0.1725 0.032 Uiso 1 1 calc R . . C11 C -0.0262(4) 0.1865(4) 0.1247(3) 0.0203(7) Uani 1 1 d . . . C12 C 0.1112(4) 0.2072(4) 0.1010(3) 0.0250(8) Uani 1 1 d . . . H12A H 0.1494 0.1346 0.0984 0.030 Uiso 1 1 calc R . . C13 C 0.1915(4) 0.3355(4) 0.0812(3) 0.0283(9) Uani 1 1 d . . . H13A H 0.2854 0.3517 0.0658 0.034 Uiso 1 1 calc R . . C14 C 0.1327(4) 0.4390(4) 0.0843(3) 0.0261(8) Uani 1 1 d . . . H14A H 0.1841 0.5262 0.0694 0.031 Uiso 1 1 calc R . . C15 C -0.0034(4) 0.4119(4) 0.1099(3) 0.0258(8) Uani 1 1 d . . . H15A H -0.0436 0.4829 0.1118 0.031 Uiso 1 1 calc R . . C16 C -0.4079(4) 0.3048(4) 0.4694(3) 0.0206(8) Uani 1 1 d . . . C17 C -0.2884(5) 0.3870(4) 0.5439(3) 0.0282(9) Uani 1 1 d . . . H17A H -0.1972 0.3886 0.5292 0.034 Uiso 1 1 calc R . . C18 C -0.3033(6) 0.4670(5) 0.6404(3) 0.0365(10) Uani 1 1 d . . . H18A H -0.2226 0.5216 0.6913 0.044 Uiso 1 1 calc R . . C19 C -0.4360(6) 0.4660(5) 0.6612(3) 0.0354(10) Uani 1 1 d . . . H19A H -0.4463 0.5195 0.7265 0.042 Uiso 1 1 calc R . . C20 C -0.5542(5) 0.3867(4) 0.5867(4) 0.0344(10) Uani 1 1 d . . . H20A H -0.6449 0.3868 0.6016 0.041 Uiso 1 1 calc R . . C21 C -0.5413(4) 0.3068(4) 0.4899(3) 0.0263(8) Uani 1 1 d . . . H21A H -0.6221 0.2545 0.4388 0.032 Uiso 1 1 calc R . . C22 C -0.5473(4) 0.0553(4) 0.2882(3) 0.0219(8) Uani 1 1 d . . . C23 C -0.5963(4) 0.0241(4) 0.1838(3) 0.0238(8) Uani 1 1 d . . . H23A H -0.5459 0.0842 0.1447 0.029 Uiso 1 1 calc R . . C24 C -0.7189(5) -0.0953(4) 0.1374(3) 0.0310(9) Uani 1 1 d . . . H24A H -0.7502 -0.1188 0.0662 0.037 Uiso 1 1 calc R . . C25 C -0.7956(5) -0.1802(4) 0.1955(4) 0.0357(10) Uani 1 1 d . . . H25A H -0.8797 -0.2610 0.1638 0.043 Uiso 1 1 calc R . . C26 C -0.7499(5) -0.1474(4) 0.3007(4) 0.0345(10) Uani 1 1 d . . . H26A H -0.8033 -0.2049 0.3402 0.041 Uiso 1 1 calc R . . C27 C -0.6264(5) -0.0307(4) 0.3465(3) 0.0294(9) Uani 1 1 d . . . H27A H -0.5948 -0.0085 0.4176 0.035 Uiso 1 1 calc R . . N N -0.0822(3) 0.2902(3) 0.1323(2) 0.0219(7) Uani 1 1 d . . . P P -0.38003(10) 0.20165(9) 0.34683(7) 0.01793(19) Uani 1 1 d . . . Fe Fe -0.18571(6) 0.00062(5) 0.26828(4) 0.01930(12) Uani 1 1 d . . . Br1 Br -0.07987(4) 0.59051(4) 0.34909(3) 0.02411(9) Uani 1 1 d . . . Br2 Br -0.39384(4) 0.38367(4) 0.08057(3) 0.02650(10) Uani 1 1 d . . . Hg Hg -0.273067(14) 0.347555(13) 0.234406(10) 0.01858(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(2) 0.0218(17) 0.0142(17) 0.0053(14) 0.0021(15) 0.0086(15) C2 0.031(2) 0.0275(18) 0.0167(18) 0.0089(15) 0.0053(16) 0.0111(17) C3 0.038(2) 0.0307(19) 0.0162(18) 0.0070(15) 0.0020(16) 0.0192(18) C4 0.030(2) 0.033(2) 0.021(2) 0.0029(16) -0.0027(17) 0.0169(18) C5 0.023(2) 0.0249(18) 0.0156(17) -0.0006(14) 0.0008(15) 0.0091(16) C6 0.025(2) 0.0254(17) 0.0114(17) 0.0020(14) 0.0056(14) 0.0124(16) C7 0.0200(19) 0.0251(18) 0.0159(18) 0.0037(14) 0.0001(15) 0.0040(15) C8 0.038(2) 0.0220(18) 0.0183(19) 0.0006(15) 0.0023(17) 0.0025(17) C9 0.049(3) 0.0216(18) 0.021(2) 0.0011(15) 0.0069(19) 0.0159(18) C10 0.034(2) 0.0288(19) 0.0195(19) 0.0028(15) 0.0060(17) 0.0166(18) C11 0.0215(19) 0.0244(17) 0.0115(16) 0.0009(13) 0.0017(14) 0.0074(15) C12 0.023(2) 0.0315(19) 0.0201(19) 0.0032(15) 0.0057(16) 0.0129(17) C13 0.021(2) 0.036(2) 0.0187(19) -0.0013(16) 0.0054(16) 0.0067(17) C14 0.026(2) 0.0267(18) 0.0196(19) 0.0025(15) 0.0053(16) 0.0049(16) C15 0.027(2) 0.0258(18) 0.0225(19) 0.0066(15) 0.0104(16) 0.0073(16) C16 0.026(2) 0.0222(17) 0.0183(18) 0.0090(14) 0.0069(15) 0.0116(15) C17 0.034(2) 0.036(2) 0.0180(19) 0.0031(16) 0.0041(17) 0.0198(18) C18 0.051(3) 0.042(2) 0.019(2) 0.0006(18) 0.003(2) 0.027(2) C19 0.055(3) 0.036(2) 0.025(2) 0.0111(18) 0.018(2) 0.026(2) C20 0.041(3) 0.028(2) 0.046(3) 0.0187(19) 0.030(2) 0.0198(19) C21 0.026(2) 0.0221(17) 0.031(2) 0.0091(16) 0.0085(17) 0.0081(16) C22 0.021(2) 0.0204(17) 0.0234(19) 0.0058(15) 0.0059(16) 0.0062(15) C23 0.0173(19) 0.0259(18) 0.025(2) 0.0041(15) 0.0034(16) 0.0073(15) C24 0.025(2) 0.029(2) 0.033(2) -0.0006(17) -0.0029(18) 0.0101(17) C25 0.019(2) 0.0203(18) 0.059(3) 0.0030(19) 0.000(2) 0.0038(16) C26 0.021(2) 0.027(2) 0.060(3) 0.022(2) 0.009(2) 0.0062(17) C27 0.028(2) 0.0265(19) 0.033(2) 0.0120(17) 0.0073(18) 0.0060(17) N 0.0203(16) 0.0233(15) 0.0213(16) 0.0067(12) 0.0053(13) 0.0069(13) P 0.0179(5) 0.0184(4) 0.0157(4) 0.0050(3) 0.0036(4) 0.0043(4) Fe 0.0229(3) 0.0191(2) 0.0152(2) 0.0027(2) 0.0015(2) 0.0086(2) Br1 0.01829(19) 0.02104(17) 0.02496(19) 0.00105(14) 0.00197(15) 0.00173(14) Br2 0.0220(2) 0.0383(2) 0.02095(19) 0.01212(16) 0.00298(15) 0.01062(16) Hg 0.01802(9) 0.01849(8) 0.01699(8) 0.00573(5) 0.00353(5) 0.00349(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.452(5) . ? C1 C5 1.456(5) . ? C1 P 1.785(4) . ? C1 Fe 2.030(4) . ? C2 C3 1.425(6) . ? C2 Fe 2.038(4) . ? C2 H2A 0.9500 . ? C3 C4 1.429(6) . ? C3 Fe 2.056(4) . ? C3 H3A 0.9500 . ? C4 C5 1.422(6) . ? C4 Fe 2.061(4) . ? C4 H4A 0.9500 . ? C5 Fe 2.045(4) . ? C5 H5A 0.9500 . ? C6 C10 1.439(5) . ? C6 C7 1.439(5) . ? C6 C11 1.485(5) . ? C6 Fe 2.055(4) . ? C7 C8 1.438(5) . ? C7 Fe 2.065(4) . ? C7 H7A 0.9500 . ? C8 C9 1.415(7) . ? C8 Fe 2.069(4) . ? C8 H8A 0.9500 . ? C9 C10 1.426(6) . ? C9 Fe 2.053(4) . ? C9 H9A 0.9500 . ? C10 Fe 2.040(4) . ? C10 H10A 0.9500 . ? C11 N 1.360(5) . ? C11 C12 1.399(6) . ? C12 C13 1.395(6) . ? C12 H12A 0.9500 . ? C13 C14 1.385(6) . ? C13 H13A 0.9500 . ? C14 C15 1.389(6) . ? C14 H14A 0.9500 . ? C15 N 1.354(5) . ? C15 H15A 0.9500 . ? C16 C21 1.399(6) . ? C16 C17 1.403(6) . ? C16 P 1.825(4) . ? C17 C18 1.406(6) . ? C17 H17A 0.9500 . ? C18 C19 1.384(7) . ? C18 H18A 0.9500 . ? C19 C20 1.390(7) . ? C19 H19A 0.9500 . ? C20 C21 1.402(6) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.403(6) . ? C22 C27 1.409(5) . ? C22 P 1.817(4) . ? C23 C24 1.394(6) . ? C23 H23A 0.9500 . ? C24 C25 1.391(6) . ? C24 H24A 0.9500 . ? C25 C26 1.403(7) . ? C25 H25A 0.9500 . ? C26 C27 1.385(6) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N Hg 2.573(3) . ? P Hg 2.4462(9) . ? Br1 Hg 2.6291(5) . ? Br2 Hg 2.5574(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.1(3) . . ? C2 C1 P 128.9(3) . . ? C5 C1 P 123.8(3) . . ? C2 C1 Fe 69.4(2) . . ? C5 C1 Fe 69.6(2) . . ? P C1 Fe 122.46(19) . . ? C3 C2 C1 108.0(3) . . ? C3 C2 Fe 70.3(2) . . ? C1 C2 Fe 68.8(2) . . ? C3 C2 H2A 126.0 . . ? C1 C2 H2A 126.0 . . ? Fe C2 H2A 126.5 . . ? C2 C3 C4 108.3(3) . . ? C2 C3 Fe 69.0(2) . . ? C4 C3 Fe 69.9(2) . . ? C2 C3 H3A 125.9 . . ? C4 C3 H3A 125.9 . . ? Fe C3 H3A 126.9 . . ? C5 C4 C3 109.0(4) . . ? C5 C4 Fe 69.2(2) . . ? C3 C4 Fe 69.5(2) . . ? C5 C4 H4A 125.5 . . ? C3 C4 H4A 125.5 . . ? Fe C4 H4A 127.5 . . ? C4 C5 C1 107.5(3) . . ? C4 C5 Fe 70.3(2) . . ? C1 C5 Fe 68.5(2) . . ? C4 C5 H5A 126.2 . . ? C1 C5 H5A 126.2 . . ? Fe C5 H5A 126.5 . . ? C10 C6 C7 107.4(3) . . ? C10 C6 C11 125.7(4) . . ? C7 C6 C11 126.8(3) . . ? C10 C6 Fe 68.9(2) . . ? C7 C6 Fe 69.9(2) . . ? C11 C6 Fe 127.8(2) . . ? C8 C7 C6 107.4(4) . . ? C8 C7 Fe 69.8(2) . . ? C6 C7 Fe 69.2(2) . . ? C8 C7 H7A 126.3 . . ? C6 C7 H7A 126.3 . . ? Fe C7 H7A 126.3 . . ? C9 C8 C7 108.7(4) . . ? C9 C8 Fe 69.3(2) . . ? C7 C8 Fe 69.5(2) . . ? C9 C8 H8A 125.7 . . ? C7 C8 H8A 125.7 . . ? Fe C8 H8A 127.1 . . ? C8 C9 C10 108.1(3) . . ? C8 C9 Fe 70.5(2) . . ? C10 C9 Fe 69.1(2) . . ? C8 C9 H9A 125.9 . . ? C10 C9 H9A 125.9 . . ? Fe C9 H9A 126.0 . . ? C9 C10 C6 108.3(4) . . ? C9 C10 Fe 70.1(2) . . ? C6 C10 Fe 70.0(2) . . ? C9 C10 H10A 125.8 . . ? C6 C10 H10A 125.8 . . ? Fe C10 H10A 125.7 . . ? N C11 C12 121.7(3) . . ? N C11 C6 118.3(3) . . ? C12 C11 C6 120.0(3) . . ? C13 C12 C11 119.5(4) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C14 C13 C12 119.1(4) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C15 118.2(4) . . ? C13 C14 H14A 120.9 . . ? C15 C14 H14A 120.9 . . ? N C15 C14 123.9(4) . . ? N C15 H15A 118.1 . . ? C14 C15 H15A 118.1 . . ? C21 C16 C17 119.8(3) . . ? C21 C16 P 122.7(3) . . ? C17 C16 P 117.4(3) . . ? C16 C17 C18 120.1(4) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C19 C18 C17 119.8(4) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C21 120.8(4) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C16 C21 C20 119.2(4) . . ? C16 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C23 C22 C27 119.6(4) . . ? C23 C22 P 120.3(3) . . ? C27 C22 P 120.1(3) . . ? C24 C23 C22 119.9(4) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C27 C26 C25 119.6(4) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C22 120.3(4) . . ? C26 C27 H27A 119.9 . . ? C22 C27 H27A 119.9 . . ? C15 N C11 117.5(3) . . ? C15 N Hg 107.1(2) . . ? C11 N Hg 132.2(2) . . ? C1 P C22 106.49(17) . . ? C1 P C16 105.95(17) . . ? C22 P C16 107.76(18) . . ? C1 P Hg 107.98(12) . . ? C22 P Hg 113.92(13) . . ? C16 P Hg 114.18(11) . . ? C1 Fe C2 41.82(14) . . ? C1 Fe C10 162.77(15) . . ? C2 Fe C10 152.73(15) . . ? C1 Fe C5 41.86(15) . . ? C2 Fe C5 69.91(15) . . ? C10 Fe C5 123.38(16) . . ? C1 Fe C9 156.16(17) . . ? C2 Fe C9 118.36(16) . . ? C10 Fe C9 40.77(17) . . ? C5 Fe C9 158.72(18) . . ? C1 Fe C6 126.92(14) . . ? C2 Fe C6 164.59(16) . . ? C10 Fe C6 41.13(15) . . ? C5 Fe C6 108.56(15) . . ? C9 Fe C6 68.84(15) . . ? C1 Fe C3 69.45(15) . . ? C2 Fe C3 40.74(17) . . ? C10 Fe C3 117.27(17) . . ? C5 Fe C3 68.95(15) . . ? C9 Fe C3 103.77(16) . . ? C6 Fe C3 154.16(17) . . ? C1 Fe C4 69.16(16) . . ? C2 Fe C4 68.70(17) . . ? C10 Fe C4 104.94(18) . . ? C5 Fe C4 40.52(16) . . ? C9 Fe C4 121.28(17) . . ? C6 Fe C4 120.73(17) . . ? C3 Fe C4 40.62(17) . . ? C1 Fe C7 110.30(16) . . ? C2 Fe C7 126.50(16) . . ? C10 Fe C7 68.81(17) . . ? C5 Fe C7 124.24(15) . . ? C9 Fe C7 68.53(16) . . ? C6 Fe C7 40.89(15) . . ? C3 Fe C7 161.19(16) . . ? C4 Fe C7 158.04(15) . . ? C1 Fe C8 123.25(17) . . ? C2 Fe C8 107.53(17) . . ? C10 Fe C8 68.08(18) . . ? C5 Fe C8 160.25(17) . . ? C9 Fe C8 40.16(19) . . ? C6 Fe C8 68.43(15) . . ? C3 Fe C8 122.63(16) . . ? C4 Fe C8 158.24(16) . . ? C7 Fe C8 40.72(15) . . ? P Hg Br2 128.72(3) . . ? P Hg N 118.87(7) . . ? Br2 Hg N 92.37(7) . . ? P Hg Br1 108.03(2) . . ? Br2 Hg Br1 111.667(16) . . ? N Hg Br1 90.12(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.628 _refine_diff_density_min -1.305 _refine_diff_density_rms 0.123 #=============================================================== data_i0609a _database_code_depnum_ccdc_archive 'CCDC 805324' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H44 Cd Cl2 Fe2 N2 P2' _chemical_formula_sum 'C54 H44 Cd Cl2 Fe2 N2 P2' _chemical_formula_weight 1077.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 49.456(5) _cell_length_b 22.4070(14) _cell_length_c 8.2534(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9146.0(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9720 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 25.44 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4368 _exptl_absorpt_coefficient_mu 1.314 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6208 _exptl_absorpt_correction_T_max 0.9679 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 14627 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -58 _diffrn_reflns_limit_h_max 58 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3764 _reflns_number_gt 2968 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 3764 _refine_ls_number_parameters 285 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0759 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.10955(12) -0.0465(3) 0.1267(8) 0.0375(17) Uani 1 1 d . . . C2 C 0.08309(11) -0.0536(3) 0.0579(7) 0.0387(16) Uani 1 1 d . . . H2A H 0.0760 -0.0311 -0.0300 0.046 Uiso 1 1 calc R . . C3 C 0.06919(13) -0.0992(3) 0.1410(8) 0.0433(17) Uani 1 1 d . . . H3A H 0.0513 -0.1123 0.1199 0.052 Uiso 1 1 calc R . . C4 C 0.08673(12) -0.1220(3) 0.2617(9) 0.0434(17) Uani 1 1 d . . . H4A H 0.0824 -0.1530 0.3357 0.052 Uiso 1 1 calc R . . C5 C 0.11150(12) -0.0915(3) 0.2545(8) 0.0394(16) Uani 1 1 d . . . H5A H 0.1268 -0.0988 0.3209 0.047 Uiso 1 1 calc R . . C6 C 0.05550(11) 0.0393(3) 0.3213(7) 0.0336(15) Uani 1 1 d . . . C7 C 0.04769(11) -0.0065(3) 0.4335(7) 0.0378(16) Uani 1 1 d . . . H7A H 0.0306 -0.0258 0.4379 0.045 Uiso 1 1 calc R . . C8 C 0.06989(12) -0.0179(3) 0.5361(9) 0.0448(18) Uani 1 1 d . . . H8A H 0.0702 -0.0462 0.6216 0.054 Uiso 1 1 calc R . . C9 C 0.09143(12) 0.0192(3) 0.4920(7) 0.0391(17) Uani 1 1 d . . . H9A H 0.1087 0.0202 0.5418 0.047 Uiso 1 1 calc R . . C10 C 0.08296(12) 0.0551(3) 0.3604(7) 0.0378(16) Uani 1 1 d . . . H10A H 0.0935 0.0845 0.3071 0.045 Uiso 1 1 calc R . . C11 C 0.13049(12) -0.0030(4) 0.0862(7) 0.0384(16) Uani 1 1 d . . . C12 C 0.12489(13) 0.0455(3) -0.0167(8) 0.0429(17) Uani 1 1 d . . . H12A H 0.1074 0.0500 -0.0633 0.051 Uiso 1 1 calc R . . C13 C 0.14493(13) 0.0865(4) -0.0493(8) 0.0483(19) Uani 1 1 d . . . H13A H 0.1414 0.1200 -0.1167 0.058 Uiso 1 1 calc R . . C14 C 0.17045(13) 0.0782(4) 0.0179(10) 0.0508(19) Uani 1 1 d . . . H14A H 0.1848 0.1051 -0.0037 0.061 Uiso 1 1 calc R . . C15 C 0.17402(13) 0.0295(4) 0.1166(9) 0.050(2) Uani 1 1 d . . . H15A H 0.1914 0.0245 0.1637 0.060 Uiso 1 1 calc R . . C16 C 0.01344(10) 0.1270(3) 0.2691(8) 0.0330(14) Uani 1 1 d . . . C17 C 0.00040(12) 0.1702(3) 0.1770(7) 0.0381(15) Uani 1 1 d . . . H17A H 0.0032 0.1714 0.0633 0.046 Uiso 1 1 calc R . . C18 C -0.01656(12) 0.2114(3) 0.2478(9) 0.0450(17) Uani 1 1 d . . . H18A H -0.0251 0.2410 0.1831 0.054 Uiso 1 1 calc R . . C19 C -0.02126(12) 0.2096(4) 0.4149(9) 0.0449(18) Uani 1 1 d . . . H19A H -0.0331 0.2377 0.4639 0.054 Uiso 1 1 calc R . . C20 C -0.00850(12) 0.1667(3) 0.5088(10) 0.0444(17) Uani 1 1 d . . . H20A H -0.0116 0.1656 0.6224 0.053 Uiso 1 1 calc R . . C21 C 0.00829(12) 0.1263(4) 0.4393(8) 0.0412(17) Uani 1 1 d . . . H21A H 0.0168 0.0970 0.5052 0.049 Uiso 1 1 calc R . . C22 C 0.05370(9) 0.1118(3) 0.0269(8) 0.0292(13) Uani 1 1 d . . . C23 C 0.06935(12) 0.1601(3) 0.0804(8) 0.0372(16) Uani 1 1 d . . . H23A H 0.0705 0.1687 0.1929 0.045 Uiso 1 1 calc R . . C24 C 0.08318(12) 0.1954(3) -0.0302(8) 0.0418(17) Uani 1 1 d . . . H24A H 0.0938 0.2280 0.0070 0.050 Uiso 1 1 calc R . . C25 C 0.08152(12) 0.1833(3) -0.1972(9) 0.0431(17) Uani 1 1 d . . . H25A H 0.0907 0.2078 -0.2730 0.052 Uiso 1 1 calc R . . C26 C 0.06652(11) 0.1356(3) -0.2494(8) 0.0434(17) Uani 1 1 d . . . H26A H 0.0654 0.1273 -0.3621 0.052 Uiso 1 1 calc R . . C27 C 0.05280(12) 0.0991(3) -0.1400(7) 0.0389(17) Uani 1 1 d . . . H27A H 0.0429 0.0657 -0.1781 0.047 Uiso 1 1 calc R . . N1 N 0.15516(10) -0.0118(3) 0.1528(7) 0.0451(16) Uani 1 1 d . . . P1 P 0.03317(3) 0.06918(8) 0.1684(2) 0.0307(4) Uani 1 1 d . . . Cl1 Cl 0.02154(3) -0.07150(9) -0.1664(2) 0.0430(4) Uani 1 1 d . . . Fe1 Fe 0.080300(15) -0.03259(4) 0.29917(10) 0.0329(2) Uani 1 1 d . . . Cd1 Cd 0.0000 0.0000 0.01696(7) 0.03251(16) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(3) 0.039(5) 0.043(4) -0.008(3) 0.001(3) 0.007(3) C2 0.032(3) 0.046(5) 0.038(4) -0.005(3) 0.002(3) 0.001(3) C3 0.038(3) 0.028(5) 0.063(5) -0.005(3) 0.004(3) -0.003(3) C4 0.040(3) 0.041(5) 0.050(4) 0.001(4) -0.004(3) 0.002(3) C5 0.037(3) 0.031(4) 0.049(4) -0.004(3) -0.006(3) 0.011(3) C6 0.033(3) 0.029(4) 0.039(3) -0.005(3) 0.005(3) 0.001(3) C7 0.029(3) 0.040(5) 0.044(3) 0.003(3) 0.006(3) 0.003(3) C8 0.051(4) 0.044(6) 0.040(4) 0.012(3) 0.004(3) 0.010(3) C9 0.044(3) 0.034(5) 0.039(4) 0.000(3) -0.010(3) 0.011(3) C10 0.036(3) 0.043(5) 0.034(3) -0.006(3) -0.005(3) 0.000(3) C11 0.033(3) 0.038(5) 0.044(3) -0.009(3) 0.003(2) 0.007(3) C12 0.036(3) 0.039(5) 0.054(4) -0.003(3) 0.003(3) 0.004(3) C13 0.042(4) 0.048(6) 0.055(4) 0.000(3) 0.008(3) 0.001(3) C14 0.047(4) 0.045(6) 0.061(5) -0.010(4) 0.006(4) -0.010(3) C15 0.033(3) 0.058(6) 0.061(4) -0.011(4) -0.007(3) -0.006(3) C16 0.023(3) 0.040(4) 0.036(3) 0.001(3) -0.003(3) -0.003(2) C17 0.031(3) 0.040(5) 0.043(3) 0.001(3) -0.002(3) 0.006(3) C18 0.041(3) 0.037(5) 0.057(4) 0.003(4) 0.002(3) 0.008(3) C19 0.036(3) 0.038(5) 0.060(4) -0.015(4) 0.009(3) 0.003(3) C20 0.048(4) 0.041(5) 0.044(4) -0.002(4) 0.011(4) 0.007(3) C21 0.034(3) 0.045(5) 0.045(4) 0.003(3) 0.001(3) -0.004(3) C22 0.023(2) 0.032(4) 0.032(3) -0.003(3) 0.005(3) 0.000(2) C23 0.036(3) 0.037(5) 0.039(4) 0.000(3) -0.003(3) 0.004(3) C24 0.038(3) 0.039(5) 0.048(4) -0.003(3) -0.002(3) -0.007(3) C25 0.031(3) 0.048(5) 0.051(4) 0.004(4) 0.012(3) 0.002(3) C26 0.035(3) 0.058(6) 0.037(4) -0.001(3) 0.006(3) -0.001(3) C27 0.032(3) 0.040(5) 0.045(4) -0.008(3) -0.005(3) 0.008(3) N1 0.032(3) 0.053(5) 0.050(3) -0.007(3) -0.006(2) -0.001(3) P1 0.0238(8) 0.0303(12) 0.0381(9) -0.0017(7) 0.0013(7) -0.0006(7) Cl1 0.0357(8) 0.0483(13) 0.0449(10) -0.0108(8) 0.0036(7) 0.0036(7) Fe1 0.0270(4) 0.0326(6) 0.0391(5) -0.0007(4) 0.0000(4) 0.0018(4) Cd1 0.0264(3) 0.0333(4) 0.0378(3) 0.000 0.000 -0.0026(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 C1 C2 1.435(8) . ? C1 C11 1.461(10) . ? C1 C5 1.463(10) . ? C1 Fe1 2.054(6) . ? C2 C3 1.409(9) . ? C2 Fe1 2.051(6) . ? C2 H2A 0.9500 . ? C3 C4 1.416(9) . ? C3 Fe1 2.058(7) . ? C3 H3A 0.9500 . ? C4 C5 1.404(9) . ? C4 Fe1 2.052(8) . ? C4 H4A 0.9500 . ? C5 Fe1 2.064(6) . ? C5 H5A 0.9500 . ? C6 C7 1.436(9) . ? C6 C10 1.440(8) . ? C6 P1 1.805(6) . ? C6 Fe1 2.033(6) . ? C7 C8 1.409(9) . ? C7 Fe1 2.042(6) . ? C7 H7A 0.9500 . ? C8 C9 1.399(9) . ? C8 Fe1 2.049(7) . ? C8 H8A 0.9500 . ? C9 C10 1.415(9) . ? C9 Fe1 2.046(7) . ? C9 H9A 0.9500 . ? C10 Fe1 2.033(8) . ? C10 H10A 0.9500 . ? C11 N1 1.353(8) . ? C11 C12 1.407(10) . ? C12 C13 1.377(10) . ? C12 H12A 0.9500 . ? C13 C14 1.391(10) . ? C13 H13A 0.9500 . ? C14 C15 1.373(11) . ? C14 H14A 0.9500 . ? C15 N1 1.348(10) . ? C15 H15A 0.9500 . ? C16 C17 1.390(9) . ? C16 C21 1.428(9) . ? C16 P1 1.822(6) . ? C17 C18 1.377(9) . ? C17 H17A 0.9500 . ? C18 C19 1.400(9) . ? C18 H18A 0.9500 . ? C19 C20 1.386(10) . ? C19 H19A 0.9500 . ? C20 C21 1.355(10) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.402(9) . ? C22 C27 1.407(8) . ? C22 P1 1.819(6) . ? C23 C24 1.388(9) . ? C23 H23A 0.9500 . ? C24 C25 1.407(9) . ? C24 H24A 0.9500 . ? C25 C26 1.370(10) . ? C25 H25A 0.9500 . ? C26 C27 1.395(9) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? P1 Cd1 2.5800(17) . ? Cl1 Cd1 2.4478(17) . ? Cd1 Cl1 2.4479(17) 2 ? Cd1 P1 2.5798(17) 2 ? 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 C2 C1 C11 129.1(6) . . ? C2 C1 C5 105.6(6) . . ? C11 C1 C5 125.3(5) . . ? C2 C1 Fe1 69.4(3) . . ? C11 C1 Fe1 123.8(5) . . ? C5 C1 Fe1 69.6(3) . . ? C3 C2 C1 109.4(6) . . ? C3 C2 Fe1 70.2(4) . . ? C1 C2 Fe1 69.6(3) . . ? C3 C2 H2A 125.3 . . ? C1 C2 H2A 125.3 . . ? Fe1 C2 H2A 126.5 . . ? C2 C3 C4 107.8(6) . . ? C2 C3 Fe1 69.7(4) . . ? C4 C3 Fe1 69.7(4) . . ? C2 C3 H3A 126.1 . . ? C4 C3 H3A 126.1 . . ? Fe1 C3 H3A 126.1 . . ? C5 C4 C3 109.2(7) . . ? C5 C4 Fe1 70.5(4) . . ? C3 C4 Fe1 70.1(4) . . ? C5 C4 H4A 125.4 . . ? C3 C4 H4A 125.4 . . ? Fe1 C4 H4A 125.6 . . ? C4 C5 C1 108.0(6) . . ? C4 C5 Fe1 69.6(4) . . ? C1 C5 Fe1 68.8(3) . . ? C4 C5 H5A 126.0 . . ? C1 C5 H5A 126.0 . . ? Fe1 C5 H5A 127.1 . . ? C7 C6 C10 106.5(5) . . ? C7 C6 P1 123.5(4) . . ? C10 C6 P1 130.0(5) . . ? C7 C6 Fe1 69.7(4) . . ? C10 C6 Fe1 69.3(4) . . ? P1 C6 Fe1 126.9(3) . . ? C8 C7 C6 107.9(5) . . ? C8 C7 Fe1 70.1(4) . . ? C6 C7 Fe1 69.0(3) . . ? C8 C7 H7A 126.1 . . ? C6 C7 H7A 126.1 . . ? Fe1 C7 H7A 126.4 . . ? C9 C8 C7 109.3(6) . . ? C9 C8 Fe1 69.9(4) . . ? C7 C8 Fe1 69.6(4) . . ? C9 C8 H8A 125.4 . . ? C7 C8 H8A 125.4 . . ? Fe1 C8 H8A 126.7 . . ? C8 C9 C10 108.1(6) . . ? C8 C9 Fe1 70.1(4) . . ? C10 C9 Fe1 69.2(4) . . ? C8 C9 H9A 125.9 . . ? C10 C9 H9A 125.9 . . ? Fe1 C9 H9A 126.3 . . ? C9 C10 C6 108.2(6) . . ? C9 C10 Fe1 70.2(4) . . ? C6 C10 Fe1 69.2(4) . . ? C9 C10 H10A 125.9 . . ? C6 C10 H10A 125.9 . . ? Fe1 C10 H10A 126.2 . . ? N1 C11 C12 122.4(7) . . ? N1 C11 C1 116.7(6) . . ? C12 C11 C1 121.0(5) . . ? C13 C12 C11 119.4(6) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C14 119.1(7) . . ? C12 C13 H13A 120.5 . . ? C14 C13 H13A 120.5 . . ? C15 C14 C13 117.3(7) . . ? C15 C14 H14A 121.3 . . ? C13 C14 H14A 121.3 . . ? N1 C15 C14 126.1(6) . . ? N1 C15 H15A 117.0 . . ? C14 C15 H15A 117.0 . . ? C17 C16 C21 117.5(6) . . ? C17 C16 P1 119.6(5) . . ? C21 C16 P1 122.5(5) . . ? C18 C17 C16 121.2(6) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C17 C18 C19 120.0(6) . . ? C17 C18 H18A 120.0 . . ? C19 C18 H18A 120.0 . . ? C20 C19 C18 119.6(6) . . ? C20 C19 H19A 120.2 . . ? C18 C19 H19A 120.2 . . ? C21 C20 C19 120.4(7) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C16 121.2(7) . . ? C20 C21 H21A 119.4 . . ? C16 C21 H21A 119.4 . . ? C23 C22 C27 118.8(6) . . ? C23 C22 P1 120.7(5) . . ? C27 C22 P1 120.3(5) . . ? C24 C23 C22 120.3(6) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C23 C24 C25 120.3(6) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C26 C25 C24 119.4(6) . . ? C26 C25 H25A 120.3 . . ? C24 C25 H25A 120.3 . . ? C25 C26 C27 121.1(7) . . ? C25 C26 H26A 119.5 . . ? C27 C26 H26A 119.5 . . ? C26 C27 C22 120.0(6) . . ? C26 C27 H27A 120.0 . . ? C22 C27 H27A 120.0 . . ? C15 N1 C11 115.7(7) . . ? C6 P1 C22 107.6(3) . . ? C6 P1 C16 105.8(3) . . ? C22 P1 C16 102.7(3) . . ? C6 P1 Cd1 120.3(2) . . ? C22 P1 Cd1 111.0(2) . . ? C16 P1 Cd1 107.91(18) . . ? C6 Fe1 C10 41.5(2) . . ? C6 Fe1 C7 41.3(3) . . ? C10 Fe1 C7 68.9(3) . . ? C6 Fe1 C9 69.1(2) . . ? C10 Fe1 C9 40.6(2) . . ? C7 Fe1 C9 68.1(3) . . ? C6 Fe1 C8 68.6(2) . . ? C10 Fe1 C8 67.9(3) . . ? C7 Fe1 C8 40.3(2) . . ? C9 Fe1 C8 40.0(3) . . ? C6 Fe1 C2 108.0(3) . . ? C10 Fe1 C2 117.3(3) . . ? C7 Fe1 C2 130.2(2) . . ? C9 Fe1 C2 150.2(3) . . ? C8 Fe1 C2 168.7(2) . . ? C6 Fe1 C4 151.7(2) . . ? C10 Fe1 C4 166.2(2) . . ? C7 Fe1 C4 118.9(3) . . ? C9 Fe1 C4 129.0(3) . . ? C8 Fe1 C4 109.9(3) . . ? C2 Fe1 C4 67.6(3) . . ? C6 Fe1 C1 127.4(3) . . ? C10 Fe1 C1 105.9(3) . . ? C7 Fe1 C1 167.4(3) . . ? C9 Fe1 C1 115.8(3) . . ? C8 Fe1 C1 149.7(2) . . ? C2 Fe1 C1 40.9(2) . . ? C4 Fe1 C1 68.8(3) . . ? C6 Fe1 C3 118.1(3) . . ? C10 Fe1 C3 151.2(3) . . ? C7 Fe1 C3 109.9(3) . . ? C9 Fe1 C3 167.7(3) . . ? C8 Fe1 C3 130.9(3) . . ? C2 Fe1 C3 40.1(3) . . ? C4 Fe1 C3 40.3(3) . . ? C1 Fe1 C3 68.8(3) . . ? C6 Fe1 C5 166.9(3) . . ? C10 Fe1 C5 127.9(2) . . ? C7 Fe1 C5 150.5(3) . . ? C9 Fe1 C5 107.5(3) . . ? C8 Fe1 C5 117.5(3) . . ? C2 Fe1 C5 68.2(3) . . ? C4 Fe1 C5 39.9(2) . . ? C1 Fe1 C5 41.6(3) . . ? C3 Fe1 C5 67.8(3) . . ? Cl1 Cd1 Cl1 103.63(9) . 2 ? Cl1 Cd1 P1 100.55(6) . 2 ? Cl1 Cd1 P1 114.59(5) 2 2 ? Cl1 Cd1 P1 114.59(5) . . ? Cl1 Cd1 P1 100.55(6) 2 . ? P1 Cd1 P1 122.04(8) 2 . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.470 _refine_diff_density_min -0.950 _refine_diff_density_rms 0.082 #============================================================= data_i0528 _database_code_depnum_ccdc_archive 'CCDC 805325' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H44 Cl2 Fe2 Hg N2 P2' _chemical_formula_sum 'C54 H44 Cl2 Fe2 Hg N2 P2' _chemical_formula_weight 1166.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.1944(5) _cell_length_b 15.4843(5) _cell_length_c 17.6894(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.045(2) _cell_angle_gamma 90.00 _cell_volume 4706.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 68022 _cell_measurement_theta_min 1.16 _cell_measurement_theta_max 26.33 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.460 _exptl_crystal_size_min 0.130 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 4.083 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0689 _exptl_absorpt_correction_T_max 0.3889 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2003)' _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 203(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 360 frames, detector distance = 130 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 63890 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.73 _reflns_number_total 8920 _reflns_number_gt 7954 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8920 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0720 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.27356(14) 0.96361(15) -0.14517(15) 0.0314(5) Uani 1 1 d . . . C2 C 0.26000(16) 1.03216(16) -0.19971(15) 0.0361(6) Uani 1 1 d . . . H2A H 0.2238 1.0772 -0.1959 0.043 Uiso 1 1 calc R . . C3 C 0.31126(17) 1.01922(18) -0.26009(16) 0.0414(6) Uani 1 1 d . . . H3A H 0.3148 1.0546 -0.3030 0.050 Uiso 1 1 calc R . . C4 C 0.35605(16) 0.94394(19) -0.24465(16) 0.0427(6) Uani 1 1 d . . . H4A H 0.3944 0.9210 -0.2755 0.051 Uiso 1 1 calc R . . C5 C 0.33305(15) 0.90913(17) -0.17455(16) 0.0371(6) Uani 1 1 d . . . H5A H 0.3533 0.8590 -0.1513 0.044 Uiso 1 1 calc R . . C6 C 0.21659(16) 0.84716(17) -0.34738(16) 0.0387(6) Uani 1 1 d . . . C7 C 0.15896(16) 0.91352(19) -0.33821(17) 0.0429(6) Uani 1 1 d . . . H7A H 0.1485 0.9595 -0.3717 0.051 Uiso 1 1 calc R . . C8 C 0.12060(17) 0.8973(2) -0.26960(18) 0.0488(7) Uani 1 1 d . . . H8A H 0.0805 0.9308 -0.2499 0.059 Uiso 1 1 calc R . . C9 C 0.15335(19) 0.8221(2) -0.23617(19) 0.0490(8) Uani 1 1 d . . . H9A H 0.1384 0.7970 -0.1905 0.059 Uiso 1 1 calc R . . C10 C 0.21283(19) 0.79054(17) -0.28314(17) 0.0431(7) Uani 1 1 d . . . H10A H 0.2440 0.7415 -0.2738 0.052 Uiso 1 1 calc R . . C11 C 0.27045(17) 0.83893(17) -0.41009(16) 0.0398(6) Uani 1 1 d . . . C12 C 0.2656(2) 0.8941(2) -0.4720(2) 0.0566(8) Uani 1 1 d . . . H12A H 0.2294 0.9397 -0.4737 0.068 Uiso 1 1 calc R . . C13 C 0.3154(2) 0.8809(2) -0.5316(2) 0.0639(9) Uani 1 1 d . . . H13A H 0.3120 0.9161 -0.5749 0.077 Uiso 1 1 calc R . . C14 C 0.3692(2) 0.8155(2) -0.5260(2) 0.0573(9) Uani 1 1 d . . . H14A H 0.4040 0.8056 -0.5649 0.069 Uiso 1 1 calc R . . C15 C 0.3710(2) 0.76517(19) -0.4626(2) 0.0545(8) Uani 1 1 d . . . H15A H 0.4082 0.7207 -0.4595 0.065 Uiso 1 1 calc R . . C16 C 0.25789(13) 1.03191(18) 0.00679(14) 0.0313(6) Uani 1 1 d . . . C17 C 0.29230(17) 1.10762(17) -0.01788(17) 0.0428(6) Uani 1 1 d . . . H17A H 0.3039 1.1141 -0.0691 0.051 Uiso 1 1 calc R . . C18 C 0.3096(2) 1.17415(19) 0.0335(2) 0.0516(8) Uani 1 1 d . . . H18A H 0.3336 1.2249 0.0167 0.062 Uiso 1 1 calc R . . C19 C 0.29179(19) 1.1658(2) 0.1082(2) 0.0529(8) Uani 1 1 d . . . H19A H 0.3010 1.2120 0.1419 0.063 Uiso 1 1 calc R . . C20 C 0.2603(2) 1.0895(2) 0.13378(19) 0.0537(8) Uani 1 1 d . . . H20A H 0.2505 1.0829 0.1854 0.064 Uiso 1 1 calc R . . C21 C 0.24324(17) 1.02244(18) 0.08367(17) 0.0424(6) Uani 1 1 d . . . H21A H 0.2218 0.9707 0.1014 0.051 Uiso 1 1 calc R . . C22 C 0.12228(14) 0.96619(16) -0.07650(14) 0.0320(5) Uani 1 1 d . . . C23 C 0.09619(16) 1.04909(17) -0.09668(16) 0.0382(6) Uani 1 1 d . . . H23A H 0.1318 1.0950 -0.0984 0.046 Uiso 1 1 calc R . . C24 C 0.01779(17) 1.0635(2) -0.11412(18) 0.0478(7) Uani 1 1 d . . . H24A H 0.0004 1.1192 -0.1275 0.057 Uiso 1 1 calc R . . C25 C -0.03473(16) 0.9959(2) -0.11181(18) 0.0498(7) Uani 1 1 d . . . H25A H -0.0875 1.0056 -0.1249 0.060 Uiso 1 1 calc R . . C26 C -0.01020(17) 0.9140(2) -0.09040(18) 0.0460(7) Uani 1 1 d . . . H26A H -0.0466 0.8689 -0.0879 0.055 Uiso 1 1 calc R . . C27 C 0.06839(16) 0.89816(18) -0.07254(16) 0.0375(6) Uani 1 1 d . . . H27A H 0.0850 0.8426 -0.0580 0.045 Uiso 1 1 calc R . . C28 C 0.44571(16) 0.79994(15) 0.07318(16) 0.0336(6) Uani 1 1 d . . . C29 C 0.43371(17) 0.89084(18) 0.08637(16) 0.0383(6) Uani 1 1 d . . . H29A H 0.3910 0.9238 0.0684 0.046 Uiso 1 1 calc R . . C30 C 0.49797(18) 0.92163(19) 0.13148(18) 0.0444(7) Uani 1 1 d . . . H30A H 0.5050 0.9787 0.1485 0.053 Uiso 1 1 calc R . . C31 C 0.54996(16) 0.8517(2) 0.14657(17) 0.0452(7) Uani 1 1 d . . . H31A H 0.5969 0.8547 0.1753 0.054 Uiso 1 1 calc R . . C32 C 0.51853(16) 0.77593(19) 0.11044(16) 0.0396(6) Uani 1 1 d . . . H32A H 0.5412 0.7207 0.1109 0.048 Uiso 1 1 calc R . . C33 C 0.41595(16) 0.86944(17) 0.29020(15) 0.0376(6) Uani 1 1 d . . . C34 C 0.4609(2) 0.79101(18) 0.29647(17) 0.0449(7) Uani 1 1 d . . . H34A H 0.5100 0.7851 0.3210 0.054 Uiso 1 1 calc R . . C35 C 0.4179(2) 0.72408(19) 0.25883(18) 0.0484(7) Uani 1 1 d . . . H35A H 0.4336 0.6662 0.2542 0.058 Uiso 1 1 calc R . . C36 C 0.34642(19) 0.7602(2) 0.22929(17) 0.0464(7) Uani 1 1 d . . . H36A H 0.3071 0.7302 0.2020 0.056 Uiso 1 1 calc R . . C37 C 0.34540(17) 0.84952(19) 0.24857(17) 0.0407(6) Uani 1 1 d . . . H37A H 0.3052 0.8887 0.2361 0.049 Uiso 1 1 calc R . . C38 C 0.43615(16) 0.95467(17) 0.32307(16) 0.0390(6) Uani 1 1 d . . . C39 C 0.49944(18) 0.9660(2) 0.37322(18) 0.0480(7) Uani 1 1 d . . . H39A H 0.5334 0.9199 0.3847 0.058 Uiso 1 1 calc R . . C40 C 0.5117(2) 1.0463(2) 0.4060(2) 0.0596(9) Uani 1 1 d . . . H40A H 0.5542 1.0553 0.4400 0.072 Uiso 1 1 calc R . . C41 C 0.4610(2) 1.1133(2) 0.3881(2) 0.0634(10) Uani 1 1 d . . . H41A H 0.4676 1.1682 0.4101 0.076 Uiso 1 1 calc R . . C42 C 0.3999(2) 1.0965(2) 0.3368(2) 0.0600(9) Uani 1 1 d . . . H42A H 0.3658 1.1421 0.3240 0.072 Uiso 1 1 calc R . . C43 C 0.37879(16) 0.62636(16) 0.06192(16) 0.0377(6) Uani 1 1 d . . . C44 C 0.31220(17) 0.59932(17) 0.09879(17) 0.0423(6) Uani 1 1 d . . . H44A H 0.2666 0.6329 0.0953 0.051 Uiso 1 1 calc R . . C45 C 0.3131(2) 0.52297(18) 0.14066(19) 0.0517(7) Uani 1 1 d . . . H45A H 0.2688 0.5056 0.1663 0.062 Uiso 1 1 calc R . . C46 C 0.3803(2) 0.4726(2) 0.1441(2) 0.0616(9) Uani 1 1 d . . . H46A H 0.3815 0.4214 0.1726 0.074 Uiso 1 1 calc R . . C47 C 0.4448(2) 0.4974(2) 0.1060(2) 0.0641(10) Uani 1 1 d . . . H47A H 0.4893 0.4621 0.1077 0.077 Uiso 1 1 calc R . . C48 C 0.44548(19) 0.57412(19) 0.0649(2) 0.0518(8) Uani 1 1 d . . . H48A H 0.4901 0.5907 0.0394 0.062 Uiso 1 1 calc R . . C49 C 0.42330(15) 0.72158(17) -0.07336(16) 0.0364(6) Uani 1 1 d . . . C50 C 0.38766(18) 0.66841(19) -0.12901(18) 0.0464(7) Uani 1 1 d . . . H50A H 0.3448 0.6339 -0.1172 0.056 Uiso 1 1 calc R . . C51 C 0.4161(2) 0.6673(3) -0.2015(2) 0.0620(9) Uani 1 1 d . . . H51A H 0.3931 0.6307 -0.2383 0.074 Uiso 1 1 calc R . . C52 C 0.4783(2) 0.7196(3) -0.2202(2) 0.0661(10) Uani 1 1 d . . . H52A H 0.4964 0.7191 -0.2697 0.079 Uiso 1 1 calc R . . C53 C 0.5133(2) 0.7720(3) -0.16629(19) 0.0599(9) Uani 1 1 d . . . H53A H 0.5554 0.8074 -0.1789 0.072 Uiso 1 1 calc R . . C54 C 0.48645(17) 0.7727(2) -0.09285(17) 0.0472(7) Uani 1 1 d . . . H54A H 0.5111 0.8080 -0.0560 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.16949(4) 0.80676(4) 0.11809(5) 0.04609(17) Uani 1 1 d . . . Cl2 Cl 0.17678(5) 0.67764(5) -0.07186(5) 0.05427(19) Uani 1 1 d . . . Fe1 Fe 0.23831(2) 0.91450(2) -0.24858(2) 0.03291(9) Uani 1 1 d . . . Fe2 Fe 0.44154(2) 0.82288(2) 0.18563(2) 0.03353(9) Uani 1 1 d . . . Hg1 Hg 0.248241(5) 0.799816(6) -0.001568(5) 0.03430(5) Uani 1 1 d . . . N1 N 0.32358(16) 0.77441(16) -0.40443(15) 0.0480(6) Uani 1 1 d . . . N2 N 0.38642(15) 1.01984(16) 0.30425(16) 0.0507(6) Uani 1 1 d . . . P1 P 0.22552(3) 0.94572(4) -0.05793(4) 0.02866(13) Uani 1 1 d . . . P2 P 0.37947(4) 0.73311(4) 0.01826(4) 0.03203(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0295(12) 0.0348(12) 0.0301(14) -0.0015(10) 0.0030(10) -0.0029(9) C2 0.0390(13) 0.0350(12) 0.0342(15) 0.0010(11) 0.0011(11) -0.0034(10) C3 0.0475(15) 0.0460(14) 0.0312(15) 0.0026(11) 0.0059(12) -0.0162(12) C4 0.0319(13) 0.0583(16) 0.0388(16) -0.0052(13) 0.0111(11) -0.0086(12) C5 0.0295(12) 0.0423(13) 0.0394(16) -0.0013(11) 0.0018(11) -0.0004(10) C6 0.0422(14) 0.0426(13) 0.0314(15) -0.0038(11) 0.0028(11) -0.0096(11) C7 0.0397(15) 0.0517(15) 0.0369(16) -0.0044(12) -0.0039(12) -0.0034(12) C8 0.0317(14) 0.0692(19) 0.0456(18) -0.0135(15) 0.0023(12) -0.0094(13) C9 0.0473(17) 0.0599(17) 0.0407(18) -0.0101(15) 0.0141(14) -0.0254(15) C10 0.0537(17) 0.0393(13) 0.0364(16) -0.0041(11) 0.0042(13) -0.0130(12) C11 0.0488(16) 0.0400(14) 0.0308(15) -0.0038(11) 0.0032(12) -0.0073(12) C12 0.060(2) 0.069(2) 0.0413(18) 0.0127(16) 0.0103(15) 0.0084(16) C13 0.071(2) 0.082(2) 0.0400(19) 0.0163(17) 0.0133(16) 0.0034(19) C14 0.070(2) 0.0630(18) 0.0404(19) -0.0054(15) 0.0207(16) -0.0052(17) C15 0.067(2) 0.0419(15) 0.056(2) -0.0053(14) 0.0226(16) -0.0004(14) C16 0.0240(11) 0.0374(14) 0.0325(14) -0.0018(10) 0.0003(10) 0.0038(9) C17 0.0487(16) 0.0394(13) 0.0404(17) 0.0004(12) 0.0014(12) -0.0076(12) C18 0.0580(19) 0.0400(14) 0.056(2) -0.0008(14) -0.0072(15) -0.0096(14) C19 0.0525(18) 0.0500(17) 0.056(2) -0.0184(15) -0.0074(15) -0.0014(14) C20 0.0597(19) 0.0643(19) 0.0373(17) -0.0135(14) 0.0057(14) -0.0062(15) C21 0.0442(15) 0.0471(15) 0.0363(16) -0.0044(12) 0.0066(12) -0.0035(12) C22 0.0283(12) 0.0411(13) 0.0268(13) -0.0017(10) 0.0051(9) 0.0008(10) C23 0.0362(13) 0.0399(13) 0.0388(15) 0.0012(11) 0.0054(11) 0.0037(11) C24 0.0422(15) 0.0566(17) 0.0448(18) 0.0061(14) 0.0055(13) 0.0172(13) C25 0.0281(13) 0.076(2) 0.0455(18) -0.0016(15) 0.0001(12) 0.0081(13) C26 0.0325(14) 0.0643(18) 0.0416(17) -0.0067(14) 0.0062(12) -0.0088(13) C27 0.0363(14) 0.0423(14) 0.0341(15) -0.0031(11) 0.0058(11) -0.0031(11) C28 0.0326(13) 0.0397(13) 0.0289(14) -0.0003(10) 0.0042(10) 0.0015(10) C29 0.0434(15) 0.0382(13) 0.0336(15) 0.0020(11) 0.0035(11) -0.0002(11) C30 0.0490(16) 0.0458(15) 0.0386(17) -0.0016(12) 0.0059(13) -0.0134(13) C31 0.0310(13) 0.0678(18) 0.0369(16) -0.0061(13) 0.0020(11) -0.0065(13) C32 0.0322(13) 0.0548(15) 0.0322(15) -0.0029(12) 0.0048(11) 0.0051(12) C33 0.0399(14) 0.0454(14) 0.0280(14) -0.0009(11) 0.0072(11) 0.0048(11) C34 0.0551(18) 0.0504(16) 0.0295(15) 0.0026(12) 0.0065(13) 0.0135(13) C35 0.067(2) 0.0403(14) 0.0393(17) 0.0032(13) 0.0151(14) 0.0035(14) C36 0.0515(17) 0.0489(16) 0.0400(17) -0.0064(13) 0.0177(13) -0.0110(14) C37 0.0366(14) 0.0500(15) 0.0362(16) -0.0036(12) 0.0099(12) 0.0011(12) C38 0.0390(14) 0.0463(14) 0.0323(15) -0.0040(11) 0.0107(11) 0.0007(11) C39 0.0431(16) 0.0587(17) 0.0426(18) -0.0015(14) 0.0060(13) -0.0012(13) C40 0.0553(19) 0.074(2) 0.049(2) -0.0128(17) 0.0010(15) -0.0168(17) C41 0.066(2) 0.0567(19) 0.069(2) -0.0242(17) 0.0190(19) -0.0126(17) C42 0.057(2) 0.0459(16) 0.078(3) -0.0125(16) 0.0187(18) 0.0035(14) C43 0.0380(14) 0.0348(12) 0.0403(16) -0.0062(11) 0.0016(11) 0.0037(10) C44 0.0448(15) 0.0363(13) 0.0458(17) -0.0030(12) 0.0014(12) -0.0009(11) C45 0.0590(19) 0.0423(15) 0.054(2) 0.0023(13) 0.0015(15) -0.0063(13) C46 0.074(2) 0.0415(15) 0.069(2) 0.0107(15) -0.0008(19) 0.0049(15) C47 0.063(2) 0.0484(17) 0.081(3) 0.0068(17) 0.0022(19) 0.0237(16) C48 0.0472(17) 0.0449(15) 0.064(2) -0.0005(14) 0.0078(15) 0.0137(13) C49 0.0339(13) 0.0417(13) 0.0337(15) -0.0053(11) -0.0006(11) 0.0082(11) C50 0.0453(16) 0.0504(16) 0.0433(18) -0.0147(13) -0.0012(13) 0.0040(13) C51 0.058(2) 0.083(2) 0.045(2) -0.0256(18) -0.0028(15) 0.0047(18) C52 0.058(2) 0.104(3) 0.0366(19) -0.0143(19) 0.0104(16) 0.005(2) C53 0.0469(18) 0.093(2) 0.0408(19) -0.0079(18) 0.0119(14) -0.0056(17) C54 0.0396(15) 0.0657(18) 0.0364(17) -0.0074(14) 0.0011(12) -0.0021(14) Cl1 0.0452(4) 0.0430(3) 0.0513(5) 0.0075(3) 0.0180(3) 0.0040(3) Cl2 0.0536(4) 0.0440(3) 0.0647(5) -0.0119(3) -0.0055(4) -0.0086(3) Fe1 0.03160(18) 0.03876(19) 0.0286(2) -0.00190(14) 0.00470(14) -0.00545(14) Fe2 0.03362(19) 0.03885(18) 0.0283(2) -0.00260(15) 0.00406(15) 0.00239(15) Hg1 0.03117(7) 0.03331(8) 0.03850(8) 0.00019(4) 0.00254(5) 0.00258(3) N1 0.0602(16) 0.0425(12) 0.0421(15) -0.0004(11) 0.0138(12) -0.0055(11) N2 0.0455(14) 0.0502(13) 0.0568(17) -0.0083(12) 0.0063(12) 0.0067(11) P1 0.0269(3) 0.0309(3) 0.0283(3) -0.0004(2) 0.0033(2) 0.0000(2) P2 0.0292(3) 0.0343(3) 0.0327(4) -0.0025(3) 0.0023(2) 0.0038(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 C1 C5 1.437(3) . ? C1 C2 1.448(4) . ? C1 P1 1.798(3) . ? C1 Fe1 2.052(3) . ? C2 C3 1.423(4) . ? C2 Fe1 2.045(3) . ? C2 H2A 0.9400 . ? C3 C4 1.418(4) . ? C3 Fe1 2.065(3) . ? C3 H3A 0.9400 . ? C4 C5 1.421(4) . ? C4 Fe1 2.074(3) . ? C4 H4A 0.9400 . ? C5 Fe1 2.055(3) . ? C5 H5A 0.9400 . ? C6 C10 1.439(4) . ? C6 C7 1.441(4) . ? C6 C11 1.476(4) . ? C6 Fe1 2.058(3) . ? C7 C8 1.424(4) . ? C7 Fe1 2.055(3) . ? C7 H7A 0.9400 . ? C8 C9 1.415(5) . ? C8 Fe1 2.062(3) . ? C8 H8A 0.9400 . ? C9 C10 1.427(4) . ? C9 Fe1 2.062(3) . ? C9 H9A 0.9400 . ? C10 Fe1 2.057(3) . ? C10 H10A 0.9400 . ? C11 N1 1.355(4) . ? C11 C12 1.389(4) . ? C12 C13 1.397(5) . ? C12 H12A 0.9400 . ? C13 C14 1.374(5) . ? C13 H13A 0.9400 . ? C14 C15 1.364(5) . ? C14 H14A 0.9400 . ? C15 N1 1.344(4) . ? C15 H15A 0.9400 . ? C16 C17 1.390(4) . ? C16 C21 1.400(4) . ? C16 P1 1.832(3) . ? C17 C18 1.398(4) . ? C17 H17A 0.9400 . ? C18 C19 1.374(5) . ? C18 H18A 0.9400 . ? C19 C20 1.383(5) . ? C19 H19A 0.9400 . ? C20 C21 1.390(4) . ? C20 H20A 0.9400 . ? C21 H21A 0.9400 . ? C22 C23 1.402(4) . ? C22 C27 1.406(4) . ? C22 P1 1.821(3) . ? C23 C24 1.390(4) . ? C23 H23A 0.9400 . ? C24 C25 1.385(5) . ? C24 H24A 0.9400 . ? C25 C26 1.384(5) . ? C25 H25A 0.9400 . ? C26 C27 1.399(4) . ? C26 H26A 0.9400 . ? C27 H27A 0.9400 . ? C28 C32 1.443(4) . ? C28 C29 1.443(4) . ? C28 P2 1.798(3) . ? C28 Fe2 2.024(3) . ? C29 C30 1.422(4) . ? C29 Fe2 2.047(3) . ? C29 H29A 0.9400 . ? C30 C31 1.424(4) . ? C30 Fe2 2.065(3) . ? C30 H30A 0.9400 . ? C31 C32 1.432(4) . ? C31 Fe2 2.060(3) . ? C31 H31A 0.9400 . ? C32 Fe2 2.044(3) . ? C32 H32A 0.9400 . ? C33 C37 1.430(4) . ? C33 C34 1.442(4) . ? C33 C38 1.478(4) . ? C33 Fe2 2.048(3) . ? C34 C35 1.425(5) . ? C34 Fe2 2.038(3) . ? C34 H34A 0.9400 . ? C35 C36 1.431(5) . ? C35 Fe2 2.054(3) . ? C35 H35A 0.9400 . ? C36 C37 1.425(4) . ? C36 Fe2 2.075(3) . ? C36 H36A 0.9400 . ? C37 Fe2 2.067(3) . ? C37 H37A 0.9400 . ? C38 N2 1.356(4) . ? C38 C39 1.390(4) . ? C39 C40 1.385(5) . ? C39 H39A 0.9400 . ? C40 C41 1.384(5) . ? C40 H40A 0.9400 . ? C41 C42 1.388(6) . ? C41 H41A 0.9400 . ? C42 N2 1.336(4) . ? C42 H42A 0.9400 . ? C43 C44 1.402(4) . ? C43 C48 1.403(4) . ? C43 P2 1.825(3) . ? C44 C45 1.395(4) . ? C44 H44A 0.9400 . ? C45 C46 1.395(5) . ? C45 H45A 0.9400 . ? C46 C47 1.372(5) . ? C46 H46A 0.9400 . ? C47 C48 1.393(5) . ? C47 H47A 0.9400 . ? C48 H48A 0.9400 . ? C49 C54 1.397(4) . ? C49 C50 1.407(4) . ? C49 P2 1.820(3) . ? C50 C51 1.388(5) . ? C50 H50A 0.9400 . ? C51 C52 1.390(6) . ? C51 H51A 0.9400 . ? C52 C53 1.375(5) . ? C52 H52A 0.9400 . ? C53 C54 1.394(4) . ? C53 H53A 0.9400 . ? C54 H54A 0.9400 . ? Cl1 Hg1 2.5554(7) . ? Cl2 Hg1 2.5546(7) . ? Hg1 P1 2.4946(6) . ? Hg1 P2 2.4949(6) . ? 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 C5 C1 C2 106.8(2) . . ? C5 C1 P1 125.1(2) . . ? C2 C1 P1 128.11(19) . . ? C5 C1 Fe1 69.61(15) . . ? C2 C1 Fe1 69.04(15) . . ? P1 C1 Fe1 125.30(13) . . ? C3 C2 C1 107.9(2) . . ? C3 C2 Fe1 70.47(15) . . ? C1 C2 Fe1 69.59(14) . . ? C3 C2 H2A 126.0 . . ? C1 C2 H2A 126.0 . . ? Fe1 C2 H2A 125.5 . . ? C4 C3 C2 108.5(2) . . ? C4 C3 Fe1 70.32(15) . . ? C2 C3 Fe1 69.01(14) . . ? C4 C3 H3A 125.7 . . ? C2 C3 H3A 125.7 . . ? Fe1 C3 H3A 126.5 . . ? C3 C4 C5 108.3(2) . . ? C3 C4 Fe1 69.60(15) . . ? C5 C4 Fe1 69.15(15) . . ? C3 C4 H4A 125.9 . . ? C5 C4 H4A 125.9 . . ? Fe1 C4 H4A 127.0 . . ? C4 C5 C1 108.5(2) . . ? C4 C5 Fe1 70.59(16) . . ? C1 C5 Fe1 69.42(15) . . ? C4 C5 H5A 125.8 . . ? C1 C5 H5A 125.8 . . ? Fe1 C5 H5A 125.8 . . ? C10 C6 C7 107.2(2) . . ? C10 C6 C11 126.0(3) . . ? C7 C6 C11 126.8(3) . . ? C10 C6 Fe1 69.50(16) . . ? C7 C6 Fe1 69.37(16) . . ? C11 C6 Fe1 125.62(19) . . ? C8 C7 C6 108.2(3) . . ? C8 C7 Fe1 70.04(17) . . ? C6 C7 Fe1 69.62(16) . . ? C8 C7 H7A 125.9 . . ? C6 C7 H7A 125.9 . . ? Fe1 C7 H7A 126.0 . . ? C9 C8 C7 108.2(3) . . ? C9 C8 Fe1 69.96(17) . . ? C7 C8 Fe1 69.48(16) . . ? C9 C8 H8A 125.9 . . ? C7 C8 H8A 125.9 . . ? Fe1 C8 H8A 126.2 . . ? C8 C9 C10 108.7(3) . . ? C8 C9 Fe1 69.92(17) . . ? C10 C9 Fe1 69.53(15) . . ? C8 C9 H9A 125.6 . . ? C10 C9 H9A 125.6 . . ? Fe1 C9 H9A 126.5 . . ? C9 C10 C6 107.8(3) . . ? C9 C10 Fe1 69.95(16) . . ? C6 C10 Fe1 69.57(15) . . ? C9 C10 H10A 126.1 . . ? C6 C10 H10A 126.1 . . ? Fe1 C10 H10A 125.9 . . ? N1 C11 C12 122.2(3) . . ? N1 C11 C6 116.6(2) . . ? C12 C11 C6 121.2(3) . . ? C11 C12 C13 118.9(3) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 118.8(3) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C15 C14 C13 118.5(3) . . ? C15 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? N1 C15 C14 124.9(3) . . ? N1 C15 H15A 117.6 . . ? C14 C15 H15A 117.6 . . ? C17 C16 C21 119.1(3) . . ? C17 C16 P1 122.8(2) . . ? C21 C16 P1 118.0(2) . . ? C16 C17 C18 120.0(3) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C19 C18 C17 120.4(3) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C18 C19 C20 119.9(3) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C20 C21 C16 120.0(3) . . ? C20 C21 H21A 120.0 . . ? C16 C21 H21A 120.0 . . ? C23 C22 C27 119.5(2) . . ? C23 C22 P1 120.41(19) . . ? C27 C22 P1 120.0(2) . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C26 C25 C24 120.5(3) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 120.3(3) . . ? C25 C26 H26A 119.8 . . ? C27 C26 H26A 119.8 . . ? C26 C27 C22 119.4(3) . . ? C26 C27 H27A 120.3 . . ? C22 C27 H27A 120.3 . . ? C32 C28 C29 107.7(2) . . ? C32 C28 P2 128.4(2) . . ? C29 C28 P2 123.9(2) . . ? C32 C28 Fe2 69.94(16) . . ? C29 C28 Fe2 70.10(16) . . ? P2 C28 Fe2 126.01(14) . . ? C30 C29 C28 107.8(3) . . ? C30 C29 Fe2 70.43(17) . . ? C28 C29 Fe2 68.40(16) . . ? C30 C29 H29A 126.1 . . ? C28 C29 H29A 126.1 . . ? Fe2 C29 H29A 126.6 . . ? C29 C30 C31 108.7(2) . . ? C29 C30 Fe2 69.11(16) . . ? C31 C30 Fe2 69.63(16) . . ? C29 C30 H30A 125.7 . . ? C31 C30 H30A 125.7 . . ? Fe2 C30 H30A 127.2 . . ? C30 C31 C32 108.4(3) . . ? C30 C31 Fe2 69.99(16) . . ? C32 C31 Fe2 68.95(15) . . ? C30 C31 H31A 125.8 . . ? C32 C31 H31A 125.8 . . ? Fe2 C31 H31A 126.8 . . ? C31 C32 C28 107.5(2) . . ? C31 C32 Fe2 70.19(15) . . ? C28 C32 Fe2 68.52(15) . . ? C31 C32 H32A 126.3 . . ? C28 C32 H32A 126.3 . . ? Fe2 C32 H32A 126.6 . . ? C37 C33 C34 107.5(3) . . ? C37 C33 C38 125.3(3) . . ? C34 C33 C38 127.1(3) . . ? C37 C33 Fe2 70.40(15) . . ? C34 C33 Fe2 68.96(15) . . ? C38 C33 Fe2 127.92(19) . . ? C35 C34 C33 107.9(3) . . ? C35 C34 Fe2 70.25(18) . . ? C33 C34 Fe2 69.70(16) . . ? C35 C34 H34A 126.0 . . ? C33 C34 H34A 126.0 . . ? Fe2 C34 H34A 125.6 . . ? C34 C35 C36 108.1(3) . . ? C34 C35 Fe2 68.99(16) . . ? C36 C35 Fe2 70.48(17) . . ? C34 C35 H35A 125.9 . . ? C36 C35 H35A 125.9 . . ? Fe2 C35 H35A 126.2 . . ? C37 C36 C35 108.0(3) . . ? C37 C36 Fe2 69.60(16) . . ? C35 C36 Fe2 68.96(17) . . ? C37 C36 H36A 126.0 . . ? C35 C36 H36A 126.0 . . ? Fe2 C36 H36A 127.0 . . ? C36 C37 C33 108.4(3) . . ? C36 C37 Fe2 70.15(15) . . ? C33 C37 Fe2 68.93(15) . . ? C36 C37 H37A 125.8 . . ? C33 C37 H37A 125.8 . . ? Fe2 C37 H37A 126.7 . . ? N2 C38 C39 122.3(3) . . ? N2 C38 C33 115.5(3) . . ? C39 C38 C33 122.1(3) . . ? C40 C39 C38 119.0(3) . . ? C40 C39 H39A 120.5 . . ? C38 C39 H39A 120.5 . . ? C41 C40 C39 119.4(3) . . ? C41 C40 H40A 120.3 . . ? C39 C40 H40A 120.3 . . ? C40 C41 C42 117.7(3) . . ? C40 C41 H41A 121.1 . . ? C42 C41 H41A 121.1 . . ? N2 C42 C41 124.3(3) . . ? N2 C42 H42A 117.8 . . ? C41 C42 H42A 117.8 . . ? C44 C43 C48 119.4(3) . . ? C44 C43 P2 119.0(2) . . ? C48 C43 P2 121.4(2) . . ? C45 C44 C43 120.4(3) . . ? C45 C44 H44A 119.8 . . ? C43 C44 H44A 119.8 . . ? C46 C45 C44 119.3(3) . . ? C46 C45 H45A 120.3 . . ? C44 C45 H45A 120.3 . . ? C47 C46 C45 120.4(3) . . ? C47 C46 H46A 119.8 . . ? C45 C46 H46A 119.8 . . ? C46 C47 C48 121.1(3) . . ? C46 C47 H47A 119.4 . . ? C48 C47 H47A 119.4 . . ? C47 C48 C43 119.3(3) . . ? C47 C48 H48A 120.4 . . ? C43 C48 H48A 120.4 . . ? C54 C49 C50 118.8(3) . . ? C54 C49 P2 121.0(2) . . ? C50 C49 P2 119.8(2) . . ? C51 C50 C49 119.6(3) . . ? C51 C50 H50A 120.2 . . ? C49 C50 H50A 120.2 . . ? C50 C51 C52 120.8(3) . . ? C50 C51 H51A 119.6 . . ? C52 C51 H51A 119.6 . . ? C53 C52 C51 120.0(3) . . ? C53 C52 H52A 120.0 . . ? C51 C52 H52A 120.0 . . ? C52 C53 C54 120.0(3) . . ? C52 C53 H53A 120.0 . . ? C54 C53 H53A 120.0 . . ? C53 C54 C49 120.8(3) . . ? C53 C54 H54A 119.6 . . ? C49 C54 H54A 119.6 . . ? C2 Fe1 C1 41.37(10) . . ? C2 Fe1 C7 116.03(11) . . ? C1 Fe1 C7 149.02(11) . . ? C2 Fe1 C5 68.79(11) . . ? C1 Fe1 C5 40.97(10) . . ? C7 Fe1 C5 168.79(11) . . ? C2 Fe1 C10 172.15(11) . . ? C1 Fe1 C10 131.58(11) . . ? C7 Fe1 C10 68.61(12) . . ? C5 Fe1 C10 107.89(12) . . ? C2 Fe1 C6 146.64(11) . . ? C1 Fe1 C6 169.59(11) . . ? C7 Fe1 C6 41.02(11) . . ? C5 Fe1 C6 129.52(11) . . ? C10 Fe1 C6 40.93(11) . . ? C2 Fe1 C8 110.74(12) . . ? C1 Fe1 C8 117.73(11) . . ? C7 Fe1 C8 40.48(12) . . ? C5 Fe1 C8 149.36(12) . . ? C10 Fe1 C8 68.21(13) . . ? C6 Fe1 C8 68.55(12) . . ? C2 Fe1 C9 133.82(12) . . ? C1 Fe1 C9 110.49(11) . . ? C7 Fe1 C9 67.89(13) . . ? C5 Fe1 C9 116.90(13) . . ? C10 Fe1 C9 40.53(13) . . ? C6 Fe1 C9 68.35(11) . . ? C8 Fe1 C9 40.12(14) . . ? C2 Fe1 C3 40.52(11) . . ? C1 Fe1 C3 68.64(10) . . ? C7 Fe1 C3 108.58(12) . . ? C5 Fe1 C3 67.92(11) . . ? C10 Fe1 C3 145.82(12) . . ? C6 Fe1 C3 113.99(11) . . ? C8 Fe1 C3 132.79(13) . . ? C9 Fe1 C3 172.18(14) . . ? C2 Fe1 C4 68.09(11) . . ? C1 Fe1 C4 68.40(10) . . ? C7 Fe1 C4 130.39(11) . . ? C5 Fe1 C4 40.26(11) . . ? C10 Fe1 C4 114.35(12) . . ? C6 Fe1 C4 106.69(11) . . ? C8 Fe1 C4 170.10(13) . . ? C9 Fe1 C4 147.49(14) . . ? C3 Fe1 C4 40.08(12) . . ? C28 Fe2 C34 153.20(10) . . ? C28 Fe2 C32 41.54(11) . . ? C34 Fe2 C32 116.90(12) . . ? C28 Fe2 C29 41.50(10) . . ? C34 Fe2 C29 162.40(12) . . ? C32 Fe2 C29 69.44(12) . . ? C28 Fe2 C33 164.95(11) . . ? C34 Fe2 C33 41.34(11) . . ? C32 Fe2 C33 151.44(12) . . ? C29 Fe2 C33 125.74(11) . . ? C28 Fe2 C35 120.22(11) . . ? C34 Fe2 C35 40.76(13) . . ? C32 Fe2 C35 107.03(12) . . ? C29 Fe2 C35 156.18(13) . . ? C33 Fe2 C35 68.84(11) . . ? C28 Fe2 C31 69.16(11) . . ? C34 Fe2 C31 104.83(13) . . ? C32 Fe2 C31 40.86(12) . . ? C29 Fe2 C31 68.51(12) . . ? C33 Fe2 C31 116.93(12) . . ? C35 Fe2 C31 125.08(13) . . ? C28 Fe2 C30 68.92(11) . . ? C34 Fe2 C30 124.21(13) . . ? C32 Fe2 C30 68.62(12) . . ? C29 Fe2 C30 40.46(12) . . ? C33 Fe2 C30 106.14(11) . . ? C35 Fe2 C30 161.96(14) . . ? C31 Fe2 C30 40.38(12) . . ? C28 Fe2 C37 128.41(12) . . ? C34 Fe2 C37 68.70(13) . . ? C32 Fe2 C37 166.07(12) . . ? C29 Fe2 C37 109.27(12) . . ? C33 Fe2 C37 40.67(12) . . ? C35 Fe2 C37 68.22(12) . . ? C31 Fe2 C37 152.63(12) . . ? C30 Fe2 C37 120.00(12) . . ? C28 Fe2 C36 109.86(12) . . ? C34 Fe2 C36 68.45(14) . . ? C32 Fe2 C36 127.84(12) . . ? C29 Fe2 C36 122.09(13) . . ? C33 Fe2 C36 68.34(11) . . ? C35 Fe2 C36 40.56(14) . . ? C31 Fe2 C36 163.96(13) . . ? C30 Fe2 C36 155.37(13) . . ? C37 Fe2 C36 40.25(12) . . ? P1 Hg1 P2 123.99(2) . . ? P1 Hg1 Cl2 114.23(2) . . ? P2 Hg1 Cl2 100.29(2) . . ? P1 Hg1 Cl1 102.29(2) . . ? P2 Hg1 Cl1 113.85(2) . . ? Cl2 Hg1 Cl1 100.04(3) . . ? C15 N1 C11 116.6(3) . . ? C42 N2 C38 117.2(3) . . ? C1 P1 C22 107.04(12) . . ? C1 P1 C16 106.59(11) . . ? C22 P1 C16 104.97(11) . . ? C1 P1 Hg1 114.36(8) . . ? C22 P1 Hg1 111.56(8) . . ? C16 P1 Hg1 111.73(9) . . ? C28 P2 C49 105.25(12) . . ? C28 P2 C43 107.82(13) . . ? C49 P2 C43 107.29(12) . . ? C28 P2 Hg1 112.95(8) . . ? C49 P2 Hg1 108.45(9) . . ? C43 P2 Hg1 114.53(9) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.73 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.864 _refine_diff_density_min -2.387 _refine_diff_density_rms 0.095 #====================================================================== data_i0634 _database_code_depnum_ccdc_archive 'CCDC 805326' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H44 Br2 Fe2 Hg N2 P2' _chemical_formula_weight 1254.96 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.4068(8) _cell_length_b 15.5806(5) _cell_length_c 17.5380(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.161(4) _cell_angle_gamma 90.00 _cell_volume 4753.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 37628 _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 25.73 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.420 _exptl_crystal_size_mid 0.283 _exptl_crystal_size_min 0.170 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 5.612 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3150 _exptl_absorpt_correction_T_max 0.7179 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% ? _diffrn_reflns_number 30291 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8305 _reflns_number_gt 7436 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00075(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8305 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9469(3) 0.2001(3) 0.5772(3) 0.0292(10) Uani 1 1 d . . . C2 C 1.0201(3) 0.2237(4) 0.6144(3) 0.0353(11) Uani 1 1 d . . . H2A H 1.0424 0.2793 0.6152 0.042 Uiso 1 1 calc R . . C3 C 1.0521(3) 0.1495(4) 0.6491(3) 0.0398(13) Uani 1 1 d . . . H3A H 1.0999 0.1467 0.6769 0.048 Uiso 1 1 calc R . . C4 C 1.0006(3) 0.0795(4) 0.6357(3) 0.0403(12) Uani 1 1 d . . . H4A H 1.0081 0.0223 0.6533 0.048 Uiso 1 1 calc R . . C5 C 0.9361(3) 0.1101(4) 0.5910(3) 0.0362(12) Uani 1 1 d . . . H5A H 0.8933 0.0767 0.5735 0.043 Uiso 1 1 calc R . . C6 C 0.9213(3) 0.1298(4) 0.7964(3) 0.0334(11) Uani 1 1 d . . . C7 C 0.9691(3) 0.2066(4) 0.8030(3) 0.0384(12) Uani 1 1 d . . . H7A H 1.0189 0.2102 0.8269 0.046 Uiso 1 1 calc R . . C8 C 0.9271(3) 0.2752(4) 0.7670(3) 0.0416(12) Uani 1 1 d . . . H8A H 0.9443 0.3329 0.7631 0.050 Uiso 1 1 calc R . . C9 C 0.8548(3) 0.2431(4) 0.7377(3) 0.0397(12) Uani 1 1 d . . . H9A H 0.8161 0.2753 0.7110 0.048 Uiso 1 1 calc R . . C10 C 0.8514(3) 0.1538(4) 0.7558(3) 0.0341(11) Uani 1 1 d . . . H10A H 0.8097 0.1165 0.7431 0.041 Uiso 1 1 calc R . . C11 C 0.9394(3) 0.0441(4) 0.8271(3) 0.0349(11) Uani 1 1 d . . . C12 C 1.0023(3) 0.0299(4) 0.8765(3) 0.0450(13) Uani 1 1 d . . . H12A H 1.0372 0.0750 0.8889 0.054 Uiso 1 1 calc R . . C13 C 1.0134(4) -0.0518(5) 0.9077(3) 0.0517(15) Uani 1 1 d . . . H13A H 1.0554 -0.0629 0.9425 0.062 Uiso 1 1 calc R . . C14 C 0.9621(4) -0.1164(5) 0.8870(4) 0.0548(16) Uani 1 1 d . . . H14A H 0.9680 -0.1727 0.9072 0.066 Uiso 1 1 calc R . . C15 C 0.9015(4) -0.0967(5) 0.8359(4) 0.0572(16) Uani 1 1 d . . . H15A H 0.8675 -0.1417 0.8206 0.069 Uiso 1 1 calc R . . C16 C 0.8790(3) 0.3718(4) 0.5665(3) 0.0356(11) Uani 1 1 d . . . C17 C 0.9448(3) 0.4251(4) 0.5676(4) 0.0472(14) Uani 1 1 d . . . H17A H 0.9892 0.4083 0.5414 0.057 Uiso 1 1 calc R . . C18 C 0.9440(4) 0.5024(5) 0.6074(4) 0.0584(17) Uani 1 1 d . . . H18A H 0.9878 0.5389 0.6075 0.070 Uiso 1 1 calc R . . C19 C 0.8801(4) 0.5267(4) 0.6469(4) 0.0565(16) Uani 1 1 d . . . H19A H 0.8811 0.5781 0.6760 0.068 Uiso 1 1 calc R . . C20 C 0.8142(3) 0.4758(4) 0.6440(3) 0.0464(13) Uani 1 1 d . . . H20A H 0.7697 0.4934 0.6696 0.056 Uiso 1 1 calc R . . C21 C 0.8140(3) 0.3985(4) 0.6029(3) 0.0369(11) Uani 1 1 d . . . H21A H 0.7689 0.3642 0.6000 0.044 Uiso 1 1 calc R . . C22 C 0.9228(3) 0.2769(4) 0.4294(3) 0.0316(10) Uani 1 1 d . . . C23 C 0.9838(3) 0.2254(4) 0.4088(3) 0.0417(13) Uani 1 1 d . . . H23A H 1.0080 0.1887 0.4457 0.050 Uiso 1 1 calc R . . C24 C 1.0098(3) 0.2269(5) 0.3349(3) 0.0520(16) Uani 1 1 d . . . H24A H 1.0511 0.1909 0.3212 0.062 Uiso 1 1 calc R . . C25 C 0.9750(4) 0.2814(5) 0.2809(3) 0.0576(17) Uani 1 1 d . . . H25A H 0.9922 0.2826 0.2301 0.069 Uiso 1 1 calc R . . C26 C 0.9146(3) 0.3344(5) 0.3020(3) 0.0547(17) Uani 1 1 d . . . H26A H 0.8918 0.3726 0.2655 0.066 Uiso 1 1 calc R . . C27 C 0.8875(3) 0.3321(4) 0.3753(3) 0.0419(13) Uani 1 1 d . . . H27A H 0.8456 0.3673 0.3887 0.050 Uiso 1 1 calc R . . C28 C 0.7743(2) 0.0378(3) 0.3566(2) 0.0283(10) Uani 1 1 d . . . C29 C 0.8315(3) 0.0943(4) 0.3271(3) 0.0349(11) Uani 1 1 d . . . H29A H 0.8504 0.1451 0.3510 0.042 Uiso 1 1 calc R . . C30 C 0.8549(3) 0.0611(4) 0.2560(3) 0.0400(12) Uani 1 1 d . . . H30A H 0.8923 0.0854 0.2244 0.048 Uiso 1 1 calc R . . C31 C 0.8119(3) -0.0153(4) 0.2407(3) 0.0385(12) Uani 1 1 d . . . H31A H 0.8159 -0.0503 0.1967 0.046 Uiso 1 1 calc R . . C32 C 0.7624(3) -0.0309(3) 0.3015(3) 0.0328(11) Uani 1 1 d . . . H32A H 0.7278 -0.0777 0.3055 0.039 Uiso 1 1 calc R . . C33 C 0.7144(3) 0.1522(4) 0.1529(3) 0.0363(11) Uani 1 1 d . . . C34 C 0.6590(3) 0.0855(4) 0.1627(3) 0.0401(12) Uani 1 1 d . . . H34A H 0.6493 0.0390 0.1286 0.048 Uiso 1 1 calc R . . C35 C 0.6208(3) 0.1000(4) 0.2320(3) 0.0429(13) Uani 1 1 d . . . H35A H 0.5814 0.0653 0.2518 0.051 Uiso 1 1 calc R . . C36 C 0.6521(3) 0.1757(4) 0.2663(3) 0.0428(13) Uani 1 1 d . . . H36A H 0.6373 0.2001 0.3132 0.051 Uiso 1 1 calc R . . C37 C 0.7094(3) 0.2087(4) 0.2184(3) 0.0368(12) Uani 1 1 d . . . H37A H 0.7392 0.2590 0.2277 0.044 Uiso 1 1 calc R . . C38 C 0.7673(3) 0.1620(4) 0.0904(3) 0.0372(12) Uani 1 1 d . . . C39 C 0.7630(3) 0.1084(5) 0.0264(3) 0.0473(14) Uani 1 1 d . . . H39A H 0.7271 0.0624 0.0239 0.057 Uiso 1 1 calc R . . C40 C 0.8110(4) 0.1226(5) -0.0328(3) 0.0569(17) Uani 1 1 d . . . H40A H 0.8078 0.0876 -0.0771 0.068 Uiso 1 1 calc R . . C41 C 0.8647(4) 0.1892(4) -0.0269(4) 0.0529(16) Uani 1 1 d . . . H41A H 0.8989 0.2007 -0.0666 0.063 Uiso 1 1 calc R . . C42 C 0.8657(4) 0.2368(4) 0.0378(3) 0.0498(14) Uani 1 1 d . . . H42A H 0.9026 0.2816 0.0419 0.060 Uiso 1 1 calc R . . C43 C 0.6258(2) 0.0337(3) 0.4270(2) 0.0284(10) Uani 1 1 d . . . C44 C 0.6000(3) -0.0480(4) 0.4040(3) 0.0357(11) Uani 1 1 d . . . H44A H 0.6355 -0.0941 0.4007 0.043 Uiso 1 1 calc R . . C45 C 0.5222(3) -0.0613(4) 0.3861(3) 0.0418(12) Uani 1 1 d . . . H45A H 0.5049 -0.1168 0.3708 0.050 Uiso 1 1 calc R . . C46 C 0.4696(3) 0.0056(4) 0.3904(3) 0.0429(14) Uani 1 1 d . . . H46A H 0.4168 -0.0038 0.3772 0.051 Uiso 1 1 calc R . . C47 C 0.4949(3) 0.0858(4) 0.4139(3) 0.0388(12) Uani 1 1 d . . . H47A H 0.4590 0.1315 0.4172 0.047 Uiso 1 1 calc R . . C48 C 0.5727(3) 0.1007(4) 0.4331(3) 0.0342(11) Uani 1 1 d . . . H48A H 0.5893 0.1558 0.4502 0.041 Uiso 1 1 calc R . . C49 C 0.7602(2) -0.0337(4) 0.5087(3) 0.0300(11) Uani 1 1 d . . . C50 C 0.7981(3) -0.1062(4) 0.4823(3) 0.0388(12) Uani 1 1 d . . . H50A H 0.8120 -0.1093 0.4305 0.047 Uiso 1 1 calc R . . C51 C 0.8157(3) -0.1746(4) 0.5321(4) 0.0463(14) Uani 1 1 d . . . H51A H 0.8415 -0.2238 0.5138 0.056 Uiso 1 1 calc R . . C52 C 0.7957(3) -0.1710(4) 0.6073(3) 0.0463(14) Uani 1 1 d . . . H52A H 0.8066 -0.2180 0.6404 0.056 Uiso 1 1 calc R . . C53 C 0.7596(4) -0.0985(4) 0.6343(3) 0.0493(14) Uani 1 1 d . . . H53A H 0.7467 -0.0953 0.6863 0.059 Uiso 1 1 calc R . . C54 C 0.7423(3) -0.0301(4) 0.5855(3) 0.0403(12) Uani 1 1 d . . . H54A H 0.7181 0.0196 0.6048 0.048 Uiso 1 1 calc R . . N36 N 0.8880(3) -0.0183(3) 0.8068(3) 0.0468(12) Uani 1 1 d . . . N54 N 0.8192(3) 0.2265(3) 0.0968(3) 0.0430(11) Uani 1 1 d . . . P1 P 0.88060(6) 0.26553(9) 0.52295(7) 0.0284(3) Uani 1 1 d . . . P2 P 0.72789(6) 0.05345(8) 0.44590(6) 0.0255(3) Uani 1 1 d . . . Fe1 Fe 0.94615(4) 0.17768(5) 0.69110(4) 0.02951(17) Uani 1 1 d . . . Fe2 Fe 0.73773(4) 0.08605(5) 0.25304(4) 0.03018(17) Uani 1 1 d . . . Br1 Br 0.67098(3) 0.18749(3) 0.63292(3) 0.03784(15) Uani 1 1 d . . . Br2 Br 0.67720(3) 0.32645(4) 0.43384(3) 0.04460(16) Uani 1 1 d . . . Hg1 Hg 0.751025(9) 0.197136(13) 0.505513(10) 0.02986(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(2) 0.032(3) 0.026(2) 0.0002(18) -0.0029(18) -0.0028(19) C2 0.025(2) 0.050(3) 0.031(2) 0.004(2) -0.0021(18) -0.004(2) C3 0.025(2) 0.063(4) 0.031(2) 0.001(2) -0.0038(18) 0.004(2) C4 0.045(3) 0.038(3) 0.038(3) 0.001(2) -0.004(2) 0.015(2) C5 0.039(3) 0.040(3) 0.029(2) -0.005(2) -0.0053(19) -0.001(2) C6 0.036(2) 0.038(3) 0.026(2) 0.004(2) 0.0005(18) -0.007(2) C7 0.043(3) 0.044(3) 0.028(2) -0.001(2) -0.002(2) -0.011(2) C8 0.059(3) 0.032(3) 0.034(3) -0.003(2) 0.006(2) -0.005(3) C9 0.041(3) 0.042(4) 0.037(3) 0.002(2) 0.009(2) 0.005(2) C10 0.030(2) 0.041(3) 0.031(2) 0.004(2) 0.0021(18) -0.001(2) C11 0.036(2) 0.038(3) 0.031(2) 0.003(2) 0.0032(19) -0.005(2) C12 0.040(3) 0.052(4) 0.042(3) 0.003(3) -0.005(2) 0.000(3) C13 0.052(3) 0.056(4) 0.046(3) 0.011(3) -0.005(3) 0.014(3) C14 0.062(4) 0.044(4) 0.060(4) 0.016(3) 0.010(3) 0.006(3) C15 0.048(3) 0.042(4) 0.082(4) 0.014(3) 0.002(3) -0.008(3) C16 0.038(3) 0.032(3) 0.035(2) 0.003(2) -0.011(2) -0.003(2) C17 0.041(3) 0.044(4) 0.057(3) 0.000(3) -0.003(2) -0.010(3) C18 0.060(4) 0.040(4) 0.074(4) -0.005(3) -0.007(3) -0.018(3) C19 0.071(4) 0.034(4) 0.064(4) -0.008(3) -0.005(3) -0.005(3) C20 0.053(3) 0.034(3) 0.051(3) -0.005(3) -0.005(2) 0.003(3) C21 0.037(3) 0.036(3) 0.037(2) 0.006(2) -0.005(2) -0.005(2) C22 0.029(2) 0.033(3) 0.032(2) 0.003(2) -0.0087(18) -0.007(2) C23 0.034(3) 0.057(4) 0.033(2) 0.007(2) -0.005(2) 0.002(2) C24 0.040(3) 0.078(5) 0.037(3) 0.004(3) 0.002(2) 0.001(3) C25 0.051(3) 0.087(5) 0.034(3) 0.015(3) 0.003(2) -0.009(3) C26 0.049(3) 0.075(5) 0.039(3) 0.023(3) -0.006(2) -0.008(3) C27 0.042(3) 0.041(3) 0.042(3) 0.013(2) -0.008(2) -0.005(2) C28 0.026(2) 0.033(3) 0.026(2) 0.0003(19) -0.0036(17) 0.0040(19) C29 0.029(2) 0.045(3) 0.031(2) -0.001(2) -0.0031(18) 0.002(2) C30 0.033(2) 0.055(4) 0.032(2) 0.001(2) 0.0038(19) 0.008(2) C31 0.039(3) 0.046(4) 0.030(2) -0.001(2) -0.004(2) 0.011(2) C32 0.035(2) 0.029(3) 0.034(2) -0.002(2) -0.0081(19) 0.006(2) C33 0.041(3) 0.038(3) 0.029(2) 0.006(2) -0.0041(19) 0.010(2) C34 0.037(3) 0.047(4) 0.035(2) 0.006(2) -0.010(2) 0.005(2) C35 0.030(2) 0.060(4) 0.039(3) 0.012(3) -0.002(2) 0.010(2) C36 0.043(3) 0.051(4) 0.034(3) 0.006(2) 0.001(2) 0.020(3) C37 0.043(3) 0.035(3) 0.032(2) 0.001(2) -0.005(2) 0.010(2) C38 0.041(3) 0.036(3) 0.034(2) 0.005(2) -0.006(2) 0.008(2) C39 0.049(3) 0.054(4) 0.039(3) -0.006(3) -0.001(2) 0.000(3) C40 0.065(4) 0.067(5) 0.039(3) -0.013(3) 0.002(3) -0.003(3) C41 0.060(4) 0.059(5) 0.041(3) 0.008(3) 0.013(3) 0.005(3) C42 0.059(4) 0.038(4) 0.053(3) 0.004(3) 0.012(3) -0.001(3) C43 0.026(2) 0.036(3) 0.023(2) 0.0036(18) -0.0001(16) -0.0022(19) C44 0.032(2) 0.037(3) 0.038(2) -0.003(2) -0.0003(19) -0.004(2) C45 0.038(3) 0.042(3) 0.044(3) -0.006(2) -0.003(2) -0.013(2) C46 0.026(2) 0.063(4) 0.039(3) 0.003(3) -0.004(2) -0.005(2) C47 0.027(2) 0.054(4) 0.036(2) 0.004(2) -0.0049(19) 0.005(2) C48 0.029(2) 0.042(3) 0.032(2) 0.002(2) 0.0009(18) 0.003(2) C49 0.025(2) 0.032(3) 0.032(2) 0.0017(19) -0.0073(17) -0.0031(19) C50 0.039(3) 0.041(3) 0.036(2) 0.000(2) -0.006(2) 0.007(2) C51 0.046(3) 0.034(3) 0.057(3) -0.001(3) -0.013(3) 0.011(3) C52 0.050(3) 0.037(3) 0.051(3) 0.014(3) -0.012(3) 0.002(3) C53 0.057(3) 0.054(4) 0.037(3) 0.013(3) 0.002(2) 0.007(3) C54 0.043(3) 0.038(3) 0.040(3) 0.000(2) 0.000(2) 0.010(2) N36 0.048(3) 0.036(3) 0.056(3) 0.008(2) -0.006(2) -0.010(2) N54 0.053(3) 0.036(3) 0.040(2) -0.002(2) 0.007(2) -0.001(2) P1 0.0249(5) 0.0303(7) 0.0297(6) 0.0014(5) -0.0044(4) -0.0033(5) P2 0.0236(5) 0.0271(7) 0.0257(5) 0.0000(5) -0.0031(4) -0.0005(4) Fe1 0.0293(3) 0.0327(4) 0.0263(3) 0.0013(3) -0.0027(3) -0.0017(3) Fe2 0.0289(3) 0.0348(4) 0.0267(3) 0.0014(3) -0.0021(2) 0.0050(3) Br1 0.0363(3) 0.0357(3) 0.0418(3) -0.0045(2) 0.0064(2) -0.0032(2) Br2 0.0418(3) 0.0366(3) 0.0543(3) 0.0097(2) -0.0121(2) 0.0039(2) Hg1 0.02686(14) 0.02901(16) 0.03331(14) 0.00021(7) -0.00406(8) -0.00221(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.436(8) . ? C1 C2 1.456(6) . ? C1 P1 1.787(5) . ? C1 Fe1 2.028(5) . ? C2 C3 1.411(8) . ? C2 Fe1 2.027(5) . ? C2 H2A 0.9500 . ? C3 C4 1.426(8) . ? C3 Fe1 2.058(5) . ? C3 H3A 0.9500 . ? C4 C5 1.427(7) . ? C4 Fe1 2.063(6) . ? C4 H4A 0.9500 . ? C5 Fe1 2.048(5) . ? C5 H5A 0.9500 . ? C6 C10 1.436(7) . ? C6 C7 1.458(7) . ? C6 C11 1.470(8) . ? C6 Fe1 2.052(5) . ? C7 C8 1.430(8) . ? C7 Fe1 2.039(5) . ? C7 H7A 0.9500 . ? C8 C9 1.431(8) . ? C8 Fe1 2.056(6) . ? C8 H8A 0.9500 . ? C9 C10 1.428(9) . ? C9 Fe1 2.082(5) . ? C9 H9A 0.9500 . ? C10 Fe1 2.071(5) . ? C10 H10A 0.9500 . ? C11 N36 1.360(7) . ? C11 C12 1.388(7) . ? C12 C13 1.396(9) . ? C12 H12A 0.9500 . ? C13 C14 1.385(10) . ? C13 H13A 0.9500 . ? C14 C15 1.392(9) . ? C14 H14A 0.9500 . ? C15 N36 1.340(8) . ? C15 H15A 0.9500 . ? C16 C21 1.384(8) . ? C16 C17 1.414(8) . ? C16 P1 1.824(6) . ? C17 C18 1.393(9) . ? C17 H17A 0.9500 . ? C18 C19 1.386(10) . ? C18 H18A 0.9500 . ? C19 C20 1.393(9) . ? C19 H19A 0.9500 . ? C20 C21 1.404(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C23 1.389(8) . ? C22 C27 1.405(7) . ? C22 P1 1.832(5) . ? C23 C24 1.390(8) . ? C23 H23A 0.9500 . ? C24 C25 1.393(9) . ? C24 H24A 0.9500 . ? C25 C26 1.397(11) . ? C25 H25A 0.9500 . ? C26 C27 1.387(8) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C29 1.439(7) . ? C28 C32 1.451(7) . ? C28 P2 1.806(5) . ? C28 Fe2 2.045(4) . ? C29 C30 1.423(7) . ? C29 Fe2 2.051(5) . ? C29 H29A 0.9500 . ? C30 C31 1.425(8) . ? C30 Fe2 2.075(5) . ? C30 H30A 0.9500 . ? C31 C32 1.417(7) . ? C31 Fe2 2.057(5) . ? C31 H31A 0.9500 . ? C32 Fe2 2.050(5) . ? C32 H32A 0.9500 . ? C33 C34 1.433(8) . ? C33 C37 1.452(8) . ? C33 C38 1.465(7) . ? C33 Fe2 2.063(5) . ? C34 C35 1.425(8) . ? C34 Fe2 2.055(5) . ? C34 H34A 0.9500 . ? C35 C36 1.422(9) . ? C35 Fe2 2.066(5) . ? C35 H35A 0.9500 . ? C36 C37 1.423(8) . ? C36 Fe2 2.062(6) . ? C36 H36A 0.9500 . ? C37 Fe2 2.059(5) . ? C37 H37A 0.9500 . ? C38 N54 1.352(8) . ? C38 C39 1.399(8) . ? C39 C40 1.375(9) . ? C39 H39A 0.9500 . ? C40 C41 1.397(10) . ? C40 H40A 0.9500 . ? C41 C42 1.354(9) . ? C41 H41A 0.9500 . ? C42 N54 1.347(8) . ? C42 H42A 0.9500 . ? C43 C48 1.401(7) . ? C43 C44 1.403(7) . ? C43 P2 1.822(4) . ? C44 C45 1.394(7) . ? C44 H44A 0.9500 . ? C45 C46 1.392(9) . ? C45 H45A 0.9500 . ? C46 C47 1.383(9) . ? C46 H46A 0.9500 . ? C47 C48 1.403(7) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C50 1.395(8) . ? C49 C54 1.396(7) . ? C49 P2 1.824(5) . ? C50 C51 1.405(8) . ? C50 H50A 0.9500 . ? C51 C52 1.377(9) . ? C51 H51A 0.9500 . ? C52 C53 1.385(9) . ? C52 H52A 0.9500 . ? C53 C54 1.391(8) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? P1 Hg1 2.5029(11) . ? P2 Hg1 2.4971(12) . ? Br1 Hg1 2.6818(6) . ? Br2 Hg1 2.6775(6) . ? 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 C5 C1 C2 106.8(4) . . ? C5 C1 P1 124.1(4) . . ? C2 C1 P1 129.1(4) . . ? C5 C1 Fe1 70.1(3) . . ? C2 C1 Fe1 68.9(3) . . ? P1 C1 Fe1 126.4(3) . . ? C3 C2 C1 108.1(5) . . ? C3 C2 Fe1 71.0(3) . . ? C1 C2 Fe1 69.0(3) . . ? C3 C2 H2A 125.9 . . ? C1 C2 H2A 125.9 . . ? Fe1 C2 H2A 125.6 . . ? C2 C3 C4 108.7(4) . . ? C2 C3 Fe1 68.6(3) . . ? C4 C3 Fe1 69.9(3) . . ? C2 C3 H3A 125.7 . . ? C4 C3 H3A 125.7 . . ? Fe1 C3 H3A 127.4 . . ? C3 C4 C5 108.1(5) . . ? C3 C4 Fe1 69.6(3) . . ? C5 C4 Fe1 69.1(3) . . ? C3 C4 H4A 125.9 . . ? C5 C4 H4A 125.9 . . ? Fe1 C4 H4A 126.9 . . ? C4 C5 C1 108.3(5) . . ? C4 C5 Fe1 70.2(3) . . ? C1 C5 Fe1 68.6(3) . . ? C4 C5 H5A 125.9 . . ? C1 C5 H5A 125.9 . . ? Fe1 C5 H5A 126.8 . . ? C10 C6 C7 107.3(5) . . ? C10 C6 C11 125.7(5) . . ? C7 C6 C11 127.0(4) . . ? C10 C6 Fe1 70.3(3) . . ? C7 C6 Fe1 68.6(3) . . ? C11 C6 Fe1 127.6(4) . . ? C8 C7 C6 107.3(5) . . ? C8 C7 Fe1 70.2(3) . . ? C6 C7 Fe1 69.6(3) . . ? C8 C7 H7A 126.3 . . ? C6 C7 H7A 126.3 . . ? Fe1 C7 H7A 125.4 . . ? C7 C8 C9 108.9(5) . . ? C7 C8 Fe1 68.9(3) . . ? C9 C8 Fe1 70.7(3) . . ? C7 C8 H8A 125.5 . . ? C9 C8 H8A 125.5 . . ? Fe1 C8 H8A 126.4 . . ? C10 C9 C8 107.8(5) . . ? C10 C9 Fe1 69.5(3) . . ? C8 C9 Fe1 68.8(3) . . ? C10 C9 H9A 126.1 . . ? C8 C9 H9A 126.1 . . ? Fe1 C9 H9A 127.2 . . ? C9 C10 C6 108.7(5) . . ? C9 C10 Fe1 70.3(3) . . ? C6 C10 Fe1 68.9(3) . . ? C9 C10 H10A 125.6 . . ? C6 C10 H10A 125.6 . . ? Fe1 C10 H10A 126.8 . . ? N36 C11 C12 123.0(5) . . ? N36 C11 C6 115.1(4) . . ? C12 C11 C6 121.8(5) . . ? C11 C12 C13 119.0(6) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 118.8(5) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C13 C14 C15 118.2(6) . . ? C13 C14 H14A 120.9 . . ? C15 C14 H14A 120.9 . . ? N36 C15 C14 124.3(6) . . ? N36 C15 H15A 117.8 . . ? C14 C15 H15A 117.8 . . ? C21 C16 C17 119.5(5) . . ? C21 C16 P1 119.4(4) . . ? C17 C16 P1 120.9(4) . . ? C18 C17 C16 119.5(6) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C19 C18 C17 120.6(6) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 120.2(6) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C19 C20 C21 119.5(6) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C16 C21 C20 120.6(5) . . ? C16 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C23 C22 C27 119.8(5) . . ? C23 C22 P1 120.9(4) . . ? C27 C22 P1 118.9(4) . . ? C22 C23 C24 120.8(5) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C23 C24 C25 119.7(6) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 119.5(5) . . ? C24 C25 H25A 120.2 . . ? C26 C25 H25A 120.2 . . ? C27 C26 C25 121.1(6) . . ? C27 C26 H26A 119.5 . . ? C25 C26 H26A 119.5 . . ? C26 C27 C22 119.1(6) . . ? C26 C27 H27A 120.5 . . ? C22 C27 H27A 120.5 . . ? C29 C28 C32 107.2(4) . . ? C29 C28 P2 124.6(4) . . ? C32 C28 P2 128.3(4) . . ? C29 C28 Fe2 69.7(3) . . ? C32 C28 Fe2 69.4(3) . . ? P2 C28 Fe2 125.9(2) . . ? C30 C29 C28 108.5(5) . . ? C30 C29 Fe2 70.7(3) . . ? C28 C29 Fe2 69.2(2) . . ? C30 C29 H29A 125.7 . . ? C28 C29 H29A 125.7 . . ? Fe2 C29 H29A 125.9 . . ? C29 C30 C31 107.6(5) . . ? C29 C30 Fe2 68.9(3) . . ? C31 C30 Fe2 69.2(3) . . ? C29 C30 H30A 126.2 . . ? C31 C30 H30A 126.2 . . ? Fe2 C30 H30A 127.3 . . ? C32 C31 C30 109.3(5) . . ? C32 C31 Fe2 69.5(3) . . ? C30 C31 Fe2 70.5(3) . . ? C32 C31 H31A 125.3 . . ? C30 C31 H31A 125.3 . . ? Fe2 C31 H31A 126.2 . . ? C31 C32 C28 107.4(5) . . ? C31 C32 Fe2 70.1(3) . . ? C28 C32 Fe2 69.1(3) . . ? C31 C32 H32A 126.3 . . ? C28 C32 H32A 126.3 . . ? Fe2 C32 H32A 126.1 . . ? C34 C33 C37 106.5(5) . . ? C34 C33 C38 127.6(5) . . ? C37 C33 C38 125.9(5) . . ? C34 C33 Fe2 69.3(3) . . ? C37 C33 Fe2 69.2(3) . . ? C38 C33 Fe2 125.5(3) . . ? C35 C34 C33 108.9(5) . . ? C35 C34 Fe2 70.2(3) . . ? C33 C34 Fe2 69.9(3) . . ? C35 C34 H34A 125.5 . . ? C33 C34 H34A 125.5 . . ? Fe2 C34 H34A 125.9 . . ? C36 C35 C34 108.0(5) . . ? C36 C35 Fe2 69.7(3) . . ? C34 C35 Fe2 69.4(3) . . ? C36 C35 H35A 126.0 . . ? C34 C35 H35A 126.0 . . ? Fe2 C35 H35A 126.5 . . ? C35 C36 C37 108.4(5) . . ? C35 C36 Fe2 70.0(3) . . ? C37 C36 Fe2 69.7(3) . . ? C35 C36 H36A 125.8 . . ? C37 C36 H36A 125.8 . . ? Fe2 C36 H36A 126.1 . . ? C36 C37 C33 108.2(5) . . ? C36 C37 Fe2 69.9(3) . . ? C33 C37 Fe2 69.5(3) . . ? C36 C37 H37A 125.9 . . ? C33 C37 H37A 125.9 . . ? Fe2 C37 H37A 126.3 . . ? N54 C38 C39 121.7(5) . . ? N54 C38 C33 116.9(5) . . ? C39 C38 C33 121.4(5) . . ? C40 C39 C38 119.6(6) . . ? C40 C39 H39A 120.2 . . ? C38 C39 H39A 120.2 . . ? C39 C40 C41 119.2(6) . . ? C39 C40 H40A 120.4 . . ? C41 C40 H40A 120.4 . . ? C42 C41 C40 117.1(6) . . ? C42 C41 H41A 121.5 . . ? C40 C41 H41A 121.5 . . ? N54 C42 C41 126.1(6) . . ? N54 C42 H42A 116.9 . . ? C41 C42 H42A 116.9 . . ? C48 C43 C44 119.6(4) . . ? C48 C43 P2 120.1(4) . . ? C44 C43 P2 120.3(4) . . ? C45 C44 C43 119.8(5) . . ? C45 C44 H44A 120.1 . . ? C43 C44 H44A 120.1 . . ? C46 C45 C44 120.8(5) . . ? C46 C45 H45A 119.6 . . ? C44 C45 H45A 119.6 . . ? C47 C46 C45 119.4(5) . . ? C47 C46 H46A 120.3 . . ? C45 C46 H46A 120.3 . . ? C46 C47 C48 121.0(5) . . ? C46 C47 H47A 119.5 . . ? C48 C47 H47A 119.5 . . ? C43 C48 C47 119.5(5) . . ? C43 C48 H48A 120.3 . . ? C47 C48 H48A 120.3 . . ? C50 C49 C54 118.6(5) . . ? C50 C49 P2 122.8(4) . . ? C54 C49 P2 118.6(4) . . ? C49 C50 C51 120.1(5) . . ? C49 C50 H50A 119.9 . . ? C51 C50 H50A 119.9 . . ? C52 C51 C50 120.5(6) . . ? C52 C51 H51A 119.8 . . ? C50 C51 H51A 119.8 . . ? C51 C52 C53 119.6(5) . . ? C51 C52 H52A 120.2 . . ? C53 C52 H52A 120.2 . . ? C52 C53 C54 120.4(5) . . ? C52 C53 H53A 119.8 . . ? C54 C53 H53A 119.8 . . ? C53 C54 C49 120.7(5) . . ? C53 C54 H54A 119.6 . . ? C49 C54 H54A 119.6 . . ? C15 N36 C11 116.6(5) . . ? C42 N54 C38 116.3(5) . . ? C1 P1 C16 108.4(2) . . ? C1 P1 C22 105.0(2) . . ? C16 P1 C22 107.5(2) . . ? C1 P1 Hg1 112.53(16) . . ? C16 P1 Hg1 114.19(17) . . ? C22 P1 Hg1 108.77(14) . . ? C28 P2 C43 106.6(2) . . ? C28 P2 C49 106.6(2) . . ? C43 P2 C49 105.1(2) . . ? C28 P2 Hg1 114.44(17) . . ? C43 P2 Hg1 111.63(17) . . ? C49 P2 Hg1 111.96(16) . . ? C2 Fe1 C1 42.07(18) . . ? C2 Fe1 C7 117.1(2) . . ? C1 Fe1 C7 154.4(2) . . ? C2 Fe1 C5 69.5(2) . . ? C1 Fe1 C5 41.3(2) . . ? C7 Fe1 C5 161.0(2) . . ? C2 Fe1 C6 152.38(19) . . ? C1 Fe1 C6 163.3(2) . . ? C7 Fe1 C6 41.8(2) . . ? C5 Fe1 C6 124.8(2) . . ? C2 Fe1 C8 106.9(2) . . ? C1 Fe1 C8 121.2(2) . . ? C7 Fe1 C8 40.9(2) . . ? C5 Fe1 C8 157.5(2) . . ? C6 Fe1 C8 69.0(2) . . ? C2 Fe1 C3 40.4(2) . . ? C1 Fe1 C3 69.22(19) . . ? C7 Fe1 C3 104.2(2) . . ? C5 Fe1 C3 68.5(2) . . ? C6 Fe1 C3 117.8(2) . . ? C8 Fe1 C3 123.9(2) . . ? C2 Fe1 C4 68.6(2) . . ? C1 Fe1 C4 69.1(2) . . ? C7 Fe1 C4 122.7(2) . . ? C5 Fe1 C4 40.6(2) . . ? C6 Fe1 C4 105.7(2) . . ? C8 Fe1 C4 160.4(2) . . ? C3 Fe1 C4 40.5(2) . . ? C2 Fe1 C10 165.0(2) . . ? C1 Fe1 C10 127.28(19) . . ? C7 Fe1 C10 69.1(2) . . ? C5 Fe1 C10 109.5(2) . . ? C6 Fe1 C10 40.75(19) . . ? C8 Fe1 C10 68.1(2) . . ? C3 Fe1 C10 154.2(2) . . ? C4 Fe1 C10 121.0(2) . . ? C2 Fe1 C9 126.9(2) . . ? C1 Fe1 C9 109.7(2) . . ? C7 Fe1 C9 68.8(2) . . ? C5 Fe1 C9 123.1(2) . . ? C6 Fe1 C9 68.5(2) . . ? C8 Fe1 C9 40.5(2) . . ? C3 Fe1 C9 162.3(3) . . ? C4 Fe1 C9 156.9(2) . . ? C10 Fe1 C9 40.2(2) . . ? C28 Fe2 C32 41.50(19) . . ? C28 Fe2 C29 41.1(2) . . ? C32 Fe2 C29 69.1(2) . . ? C28 Fe2 C34 149.2(2) . . ? C32 Fe2 C34 116.1(2) . . ? C29 Fe2 C34 168.5(2) . . ? C28 Fe2 C31 68.59(19) . . ? C32 Fe2 C31 40.4(2) . . ? C29 Fe2 C31 68.1(2) . . ? C34 Fe2 C31 108.6(2) . . ? C28 Fe2 C37 131.8(2) . . ? C32 Fe2 C37 172.5(2) . . ? C29 Fe2 C37 107.8(2) . . ? C34 Fe2 C37 68.4(2) . . ? C31 Fe2 C37 145.7(2) . . ? C28 Fe2 C36 110.6(2) . . ? C32 Fe2 C36 134.2(2) . . ? C29 Fe2 C36 116.6(2) . . ? C34 Fe2 C36 68.0(2) . . ? C31 Fe2 C36 172.5(3) . . ? C37 Fe2 C36 40.4(2) . . ? C28 Fe2 C33 169.8(2) . . ? C32 Fe2 C33 146.0(2) . . ? C29 Fe2 C33 129.3(2) . . ? C34 Fe2 C33 40.7(2) . . ? C31 Fe2 C33 113.5(2) . . ? C37 Fe2 C33 41.3(2) . . ? C36 Fe2 C33 68.8(2) . . ? C28 Fe2 C35 117.99(19) . . ? C32 Fe2 C35 111.0(2) . . ? C29 Fe2 C35 149.5(2) . . ? C34 Fe2 C35 40.5(2) . . ? C31 Fe2 C35 132.9(3) . . ? C37 Fe2 C35 68.0(2) . . ? C36 Fe2 C35 40.3(3) . . ? C33 Fe2 C35 68.6(2) . . ? C28 Fe2 C30 68.64(19) . . ? C32 Fe2 C30 68.4(2) . . ? C29 Fe2 C30 40.4(2) . . ? C34 Fe2 C30 130.1(2) . . ? C31 Fe2 C30 40.4(2) . . ? C37 Fe2 C30 113.9(2) . . ? C36 Fe2 C30 146.9(3) . . ? C33 Fe2 C30 106.0(2) . . ? C35 Fe2 C30 170.0(2) . . ? P2 Hg1 P1 124.28(4) . . ? P2 Hg1 Br2 114.27(3) . . ? P1 Hg1 Br2 98.71(3) . . ? P2 Hg1 Br1 102.59(3) . . ? P1 Hg1 Br1 114.59(3) . . ? Br2 Hg1 Br1 100.257(19) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 4.258 _refine_diff_density_min -2.843 _refine_diff_density_rms 0.212 #=================================================================== data_i0800 _database_code_depnum_ccdc_archive 'CCDC 805327' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H44 Fe2 Hg2 I4 N2 P2, 2(C H Cl3)' _chemical_formula_sum 'C56 H46 Cl6 Fe2 Hg2 I4 N2 P2' _chemical_formula_weight 2042.07 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' P P 0.1023 0.0942 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5405(11) _cell_length_b 9.8309(13) _cell_length_c 16.591(2) _cell_angle_alpha 79.405(11) _cell_angle_beta 86.852(10) _cell_angle_gamma 89.624(10) _cell_volume 1527.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9481 _cell_measurement_theta_min 1.25 _cell_measurement_theta_max 25.59 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 7.851 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4544 _exptl_absorpt_correction_T_max 0.9181 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 129 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 10365 _diffrn_reflns_av_R_equivalents 0.0879 _diffrn_reflns_av_sigmaI/netI 0.0967 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5303 _reflns_number_gt 3609 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5303 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1345 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0464(13) 0.1964(12) 0.3040(8) 0.041(3) Uani 1 1 d . . . C2 C 0.9356(15) 0.1160(14) 0.3513(10) 0.054(3) Uani 1 1 d . . . H2A H 0.8851 0.1395 0.3977 0.065 Uiso 1 1 calc R . . C3 C 0.9138(14) -0.0023(12) 0.3186(8) 0.042(3) Uani 1 1 d . . . H3A H 0.8472 -0.0731 0.3396 0.050 Uiso 1 1 calc R . . C4 C 1.0069(14) 0.0003(13) 0.2489(9) 0.046(3) Uani 1 1 d . . . H4A H 1.0128 -0.0666 0.2142 0.055 Uiso 1 1 calc R . . C5 C 1.0905(14) 0.1232(12) 0.2409(8) 0.043(3) Uani 1 1 d . . . H5A H 1.1635 0.1511 0.2000 0.051 Uiso 1 1 calc R . . C6 C 0.6849(13) 0.1624(13) 0.1934(8) 0.041(3) Uani 1 1 d . . . C7 C 0.7879(14) 0.1733(13) 0.1265(8) 0.043(3) Uani 1 1 d . . . H7A H 0.8044 0.1062 0.0926 0.052 Uiso 1 1 calc R . . C8 C 0.8617(14) 0.3005(13) 0.1190(9) 0.046(3) Uani 1 1 d . . . H8A H 0.9341 0.3345 0.0789 0.055 Uiso 1 1 calc R . . C9 C 0.8063(14) 0.3679(12) 0.1832(8) 0.044(3) Uani 1 1 d . . . H9A H 0.8372 0.4543 0.1936 0.053 Uiso 1 1 calc R . . C10 C 0.6958(12) 0.2834(12) 0.2296(8) 0.039(3) Uani 1 1 d . . . H10A H 0.6409 0.3039 0.2753 0.047 Uiso 1 1 calc R . . C11 C 0.5788(13) 0.0492(13) 0.2221(8) 0.042(3) Uani 1 1 d . . . C12 C 0.4820(12) 0.0530(13) 0.2862(8) 0.039(3) Uani 1 1 d . . . H12A H 0.4838 0.1262 0.3165 0.047 Uiso 1 1 calc R . . C13 C 0.3828(14) -0.0496(13) 0.3061(9) 0.047(3) Uani 1 1 d . . . H13A H 0.3157 -0.0502 0.3506 0.057 Uiso 1 1 calc R . . C14 C 0.3835(14) -0.1546(14) 0.2581(9) 0.051(3) Uani 1 1 d . . . H14A H 0.3136 -0.2250 0.2679 0.061 Uiso 1 1 calc R . . C15 C 0.4873(13) -0.1530(13) 0.1969(9) 0.046(3) Uani 1 1 d . . . H15A H 0.4896 -0.2275 0.1676 0.055 Uiso 1 1 calc R . . C16 C 1.1959(14) 0.4510(14) 0.2308(8) 0.046(3) Uani 1 1 d . . . C17 C 1.1237(15) 0.5721(13) 0.1917(10) 0.051(3) Uani 1 1 d . . . H17A H 1.0390 0.6021 0.2157 0.062 Uiso 1 1 calc R . . C18 C 1.1807(15) 0.6424(14) 0.1192(10) 0.056(4) Uani 1 1 d . . . H18A H 1.1335 0.7218 0.0921 0.067 Uiso 1 1 calc R . . C19 C 1.3061(17) 0.6019(16) 0.0831(10) 0.062(4) Uani 1 1 d . . . H19A H 1.3420 0.6531 0.0320 0.074 Uiso 1 1 calc R . . C20 C 1.3782(17) 0.4879(14) 0.1213(10) 0.059(4) Uani 1 1 d . . . H20A H 1.4650 0.4619 0.0977 0.070 Uiso 1 1 calc R . . C21 C 1.3214(14) 0.4108(13) 0.1957(9) 0.048(3) Uani 1 1 d . . . H21A H 1.3689 0.3310 0.2220 0.058 Uiso 1 1 calc R . . C22 C 1.2590(11) 0.2950(12) 0.3949(8) 0.037(3) Uani 1 1 d . . . C23 C 1.3767(14) 0.3817(14) 0.3950(8) 0.048(3) Uani 1 1 d . . . H23A H 1.3834 0.4685 0.3586 0.057 Uiso 1 1 calc R . . C24 C 1.4816(12) 0.3399(13) 0.4479(8) 0.042(3) Uani 1 1 d . . . H24A H 1.5603 0.3985 0.4484 0.050 Uiso 1 1 calc R . . C25 C 1.4726(13) 0.2109(13) 0.5012(8) 0.043(3) Uani 1 1 d . . . H25A H 1.5455 0.1827 0.5373 0.052 Uiso 1 1 calc R . . C26 C 1.3585(15) 0.1248(15) 0.5015(9) 0.051(3) Uani 1 1 d . . . H26A H 1.3530 0.0373 0.5371 0.061 Uiso 1 1 calc R . . C27 C 1.2496(12) 0.1688(12) 0.4478(8) 0.039(3) Uani 1 1 d . . . H27A H 1.1698 0.1113 0.4482 0.046 Uiso 1 1 calc R . . C28 C 1.2813(15) 0.1705(16) -0.0250(9) 0.056(4) Uani 1 1 d . . . H28A H 1.3115 0.1289 -0.0738 0.067 Uiso 1 1 calc R . . N1 N 0.5858(11) -0.0533(10) 0.1755(7) 0.044(2) Uani 1 1 d . . . P1 P 1.1176(3) 0.3523(3) 0.3267(2) 0.0401(7) Uani 1 1 d . . . Fe1 Fe 0.88421(18) 0.17445(17) 0.23291(12) 0.0403(4) Uani 1 1 d . . . I1 I 0.72276(9) 0.63737(8) 0.32449(6) 0.0467(2) Uani 1 1 d . . . I2 I 0.87373(9) 0.31475(8) 0.54978(5) 0.0443(2) Uani 1 1 d . . . Hg1 Hg 0.93456(5) 0.48403(5) 0.39090(3) 0.04428(19) Uani 1 1 d . . . Cl1 Cl 1.2501(5) 0.3484(4) -0.0571(3) 0.0769(12) Uani 1 1 d . . . Cl2 Cl 1.4154(5) 0.1460(5) 0.0465(3) 0.0753(12) Uani 1 1 d . . . Cl3 Cl 1.1251(5) 0.0880(5) 0.0220(3) 0.0845(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.034(6) 0.039(6) 0.051(8) -0.010(5) -0.004(6) 0.002(5) C2 0.048(8) 0.053(8) 0.058(9) -0.003(7) -0.007(7) -0.014(6) C3 0.048(7) 0.038(6) 0.038(7) 0.001(5) -0.013(6) -0.005(5) C4 0.044(7) 0.036(6) 0.058(8) -0.006(6) -0.005(6) -0.003(5) C5 0.043(7) 0.030(6) 0.053(8) -0.002(5) -0.005(6) 0.002(5) C6 0.039(7) 0.043(6) 0.039(7) -0.006(5) -0.004(5) 0.003(5) C7 0.045(7) 0.039(6) 0.047(7) -0.011(5) -0.006(6) -0.006(5) C8 0.046(7) 0.043(7) 0.048(8) -0.003(6) -0.009(6) -0.001(5) C9 0.049(7) 0.029(6) 0.054(8) -0.004(5) -0.013(6) 0.004(5) C10 0.024(6) 0.043(6) 0.050(7) -0.004(5) -0.010(5) 0.001(5) C11 0.033(6) 0.044(7) 0.048(7) -0.003(6) -0.012(6) 0.010(5) C12 0.035(6) 0.043(6) 0.040(7) -0.003(5) -0.010(5) 0.009(5) C13 0.042(7) 0.043(7) 0.050(8) 0.006(6) -0.002(6) -0.002(6) C14 0.043(7) 0.042(7) 0.059(9) 0.016(6) 0.000(7) 0.001(6) C15 0.034(7) 0.042(7) 0.061(9) -0.006(6) -0.004(6) -0.007(5) C16 0.044(7) 0.055(8) 0.040(7) -0.008(6) -0.013(6) 0.010(6) C17 0.046(8) 0.037(7) 0.070(10) -0.007(6) -0.010(7) -0.004(6) C18 0.047(8) 0.044(7) 0.073(10) -0.001(7) -0.006(7) -0.004(6) C19 0.066(10) 0.062(9) 0.058(9) -0.014(7) 0.009(8) -0.032(8) C20 0.062(9) 0.047(8) 0.061(10) -0.001(7) 0.011(8) -0.003(7) C21 0.040(7) 0.036(6) 0.069(9) -0.007(6) -0.015(6) 0.002(5) C22 0.018(5) 0.048(7) 0.043(7) -0.003(5) 0.010(5) -0.016(5) C23 0.046(7) 0.049(7) 0.047(8) -0.006(6) -0.003(6) 0.013(6) C24 0.023(6) 0.053(7) 0.054(8) -0.016(6) -0.010(5) -0.012(5) C25 0.038(7) 0.046(7) 0.047(7) -0.012(6) -0.002(6) 0.010(5) C26 0.046(8) 0.058(8) 0.052(8) -0.019(7) -0.001(6) 0.007(6) C27 0.029(6) 0.035(6) 0.051(7) -0.007(5) 0.000(5) 0.001(5) C28 0.046(8) 0.075(9) 0.047(8) -0.012(7) 0.002(6) -0.015(7) N1 0.041(6) 0.043(6) 0.046(6) -0.007(5) -0.003(5) -0.002(5) P1 0.0338(16) 0.0375(16) 0.0479(19) -0.0036(14) -0.0062(14) 0.0031(12) Fe1 0.0346(9) 0.0375(9) 0.0480(11) -0.0055(8) -0.0048(8) 0.0024(7) I1 0.0406(5) 0.0387(4) 0.0603(6) -0.0068(4) -0.0083(4) 0.0054(3) I2 0.0395(4) 0.0409(4) 0.0511(5) -0.0037(4) -0.0041(4) -0.0040(3) Hg1 0.0371(3) 0.0413(3) 0.0539(3) -0.0067(2) -0.0048(2) 0.00417(19) Cl1 0.088(3) 0.062(2) 0.079(3) -0.003(2) -0.021(2) 0.009(2) Cl2 0.076(3) 0.076(3) 0.072(3) -0.005(2) -0.014(2) 0.019(2) Cl3 0.075(3) 0.083(3) 0.097(4) -0.029(3) 0.027(3) -0.013(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 C1 C5 1.420(18) . ? C1 C2 1.431(19) . ? C1 P1 1.791(12) . ? C1 Fe1 2.032(12) . ? C2 C3 1.392(19) . ? C2 Fe1 2.029(15) . ? C2 H2A 0.9500 . ? C3 C4 1.415(19) . ? C3 Fe1 2.061(12) . ? C3 H3A 0.9500 . ? C4 C5 1.434(17) . ? C4 Fe1 2.052(13) . ? C4 H4A 0.9500 . ? C5 Fe1 2.034(13) . ? C5 H5A 0.9500 . ? C6 C7 1.430(18) . ? C6 C10 1.434(17) . ? C6 C11 1.503(18) . ? C6 Fe1 2.056(13) . ? C7 C8 1.421(18) . ? C7 Fe1 2.036(13) . ? C7 H7A 0.9500 . ? C8 C9 1.430(19) . ? C8 Fe1 2.082(14) . ? C8 H8A 0.9500 . ? C9 C10 1.442(18) . ? C9 Fe1 2.079(12) . ? C9 H9A 0.9500 . ? C10 Fe1 2.084(11) . ? C10 H10A 0.9500 . ? C11 C12 1.376(18) . ? C11 N1 1.377(16) . ? C12 C13 1.370(18) . ? C12 H12A 0.9500 . ? C13 C14 1.41(2) . ? C13 H13A 0.9500 . ? C14 C15 1.38(2) . ? C14 H14A 0.9500 . ? C15 N1 1.349(16) . ? C15 H15A 0.9500 . ? C16 C21 1.390(19) . ? C16 C17 1.438(18) . ? C16 P1 1.828(14) . ? C17 C18 1.36(2) . ? C17 H17A 0.9500 . ? C18 C19 1.40(2) . ? C18 H18A 0.9500 . ? C19 C20 1.38(2) . ? C19 H19A 0.9500 . ? C20 C21 1.41(2) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C27 1.382(17) . ? C22 C23 1.414(18) . ? C22 P1 1.827(12) . ? C23 C24 1.379(18) . ? C23 H23A 0.9500 . ? C24 C25 1.407(18) . ? C24 H24A 0.9500 . ? C25 C26 1.383(19) . ? C25 H25A 0.9500 . ? C26 C27 1.419(19) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 Cl1 1.760(17) . ? C28 Cl3 1.773(15) . ? C28 Cl2 1.778(16) . ? C28 H28A 1.0000 . ? P1 Hg1 2.477(3) . ? I1 Hg1 2.6765(10) . ? I2 Hg1 2.8785(11) . ? I2 Hg1 3.0312(10) 2_766 ? Hg1 I2 3.0312(10) 2_766 ? 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 C5 C1 C2 106.2(11) . . ? C5 C1 P1 128.6(10) . . ? C2 C1 P1 125.1(10) . . ? C5 C1 Fe1 69.6(7) . . ? C2 C1 Fe1 69.2(8) . . ? P1 C1 Fe1 128.5(7) . . ? C3 C2 C1 109.3(13) . . ? C3 C2 Fe1 71.4(8) . . ? C1 C2 Fe1 69.5(8) . . ? C3 C2 H2A 125.4 . . ? C1 C2 H2A 125.4 . . ? Fe1 C2 H2A 125.4 . . ? C2 C3 C4 108.9(12) . . ? C2 C3 Fe1 68.9(8) . . ? C4 C3 Fe1 69.6(7) . . ? C2 C3 H3A 125.6 . . ? C4 C3 H3A 125.6 . . ? Fe1 C3 H3A 127.6 . . ? C3 C4 C5 106.8(12) . . ? C3 C4 Fe1 70.2(7) . . ? C5 C4 Fe1 68.7(7) . . ? C3 C4 H4A 126.6 . . ? C5 C4 H4A 126.6 . . ? Fe1 C4 H4A 126.0 . . ? C1 C5 C4 108.9(12) . . ? C1 C5 Fe1 69.5(7) . . ? C4 C5 Fe1 70.1(7) . . ? C1 C5 H5A 125.6 . . ? C4 C5 H5A 125.6 . . ? Fe1 C5 H5A 126.4 . . ? C7 C6 C10 108.0(11) . . ? C7 C6 C11 128.1(11) . . ? C10 C6 C11 123.9(11) . . ? C7 C6 Fe1 68.8(7) . . ? C10 C6 Fe1 70.8(7) . . ? C11 C6 Fe1 127.2(8) . . ? C8 C7 C6 109.1(12) . . ? C8 C7 Fe1 71.6(7) . . ? C6 C7 Fe1 70.3(7) . . ? C8 C7 H7A 125.4 . . ? C6 C7 H7A 125.4 . . ? Fe1 C7 H7A 124.3 . . ? C7 C8 C9 107.0(12) . . ? C7 C8 Fe1 68.1(8) . . ? C9 C8 Fe1 69.8(7) . . ? C7 C8 H8A 126.5 . . ? C9 C8 H8A 126.5 . . ? Fe1 C8 H8A 127.2 . . ? C8 C9 C10 109.0(11) . . ? C8 C9 Fe1 70.0(7) . . ? C10 C9 Fe1 70.0(7) . . ? C8 C9 H9A 125.5 . . ? C10 C9 H9A 125.5 . . ? Fe1 C9 H9A 126.1 . . ? C6 C10 C9 106.8(11) . . ? C6 C10 Fe1 68.7(7) . . ? C9 C10 Fe1 69.5(7) . . ? C6 C10 H10A 126.6 . . ? C9 C10 H10A 126.6 . . ? Fe1 C10 H10A 126.7 . . ? C12 C11 N1 124.6(12) . . ? C12 C11 C6 122.4(11) . . ? N1 C11 C6 113.0(11) . . ? C13 C12 C11 119.4(12) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C12 C13 C14 117.9(13) . . ? C12 C13 H13A 121.1 . . ? C14 C13 H13A 121.1 . . ? C15 C14 C13 118.8(13) . . ? C15 C14 H14A 120.6 . . ? C13 C14 H14A 120.6 . . ? N1 C15 C14 124.7(13) . . ? N1 C15 H15A 117.7 . . ? C14 C15 H15A 117.7 . . ? C21 C16 C17 120.2(13) . . ? C21 C16 P1 121.5(10) . . ? C17 C16 P1 118.3(11) . . ? C18 C17 C16 117.8(14) . . ? C18 C17 H17A 121.1 . . ? C16 C17 H17A 121.1 . . ? C17 C18 C19 122.3(14) . . ? C17 C18 H18A 118.8 . . ? C19 C18 H18A 118.8 . . ? C20 C19 C18 120.4(14) . . ? C20 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? C19 C20 C21 119.1(14) . . ? C19 C20 H20A 120.5 . . ? C21 C20 H20A 120.5 . . ? C16 C21 C20 120.2(12) . . ? C16 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C27 C22 C23 119.9(11) . . ? C27 C22 P1 120.2(8) . . ? C23 C22 P1 119.9(9) . . ? C24 C23 C22 119.8(12) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C23 C24 C25 120.2(11) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C26 C25 C24 120.6(12) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 119.1(13) . . ? C25 C26 H26A 120.5 . . ? C27 C26 H26A 120.5 . . ? C22 C27 C26 120.3(11) . . ? C22 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? Cl1 C28 Cl3 109.6(9) . . ? Cl1 C28 Cl2 110.0(8) . . ? Cl3 C28 Cl2 109.3(8) . . ? Cl1 C28 H28A 109.3 . . ? Cl3 C28 H28A 109.3 . . ? Cl2 C28 H28A 109.3 . . ? C15 N1 C11 114.6(11) . . ? C1 P1 C22 104.9(6) . . ? C1 P1 C16 107.5(6) . . ? C22 P1 C16 108.1(5) . . ? C1 P1 Hg1 110.9(4) . . ? C22 P1 Hg1 112.5(4) . . ? C16 P1 Hg1 112.6(4) . . ? C2 Fe1 C1 41.3(5) . . ? C2 Fe1 C5 68.3(6) . . ? C1 Fe1 C5 40.9(5) . . ? C2 Fe1 C7 159.6(5) . . ? C1 Fe1 C7 156.3(5) . . ? C5 Fe1 C7 120.0(5) . . ? C2 Fe1 C4 68.0(6) . . ? C1 Fe1 C4 69.3(5) . . ? C5 Fe1 C4 41.1(5) . . ? C7 Fe1 C4 105.1(5) . . ? C2 Fe1 C6 124.2(5) . . ? C1 Fe1 C6 162.1(5) . . ? C5 Fe1 C6 155.1(5) . . ? C7 Fe1 C6 40.9(5) . . ? C4 Fe1 C6 119.0(5) . . ? C2 Fe1 C3 39.8(5) . . ? C1 Fe1 C3 68.4(5) . . ? C5 Fe1 C3 67.9(5) . . ? C7 Fe1 C3 122.9(5) . . ? C4 Fe1 C3 40.2(5) . . ? C6 Fe1 C3 106.8(5) . . ? C2 Fe1 C9 124.7(6) . . ? C1 Fe1 C9 109.8(5) . . ? C5 Fe1 C9 125.8(5) . . ? C7 Fe1 C9 67.7(5) . . ? C4 Fe1 C9 161.0(6) . . ? C6 Fe1 C9 67.9(5) . . ? C3 Fe1 C9 158.4(5) . . ? C2 Fe1 C8 159.4(5) . . ? C1 Fe1 C8 122.3(5) . . ? C5 Fe1 C8 107.6(5) . . ? C7 Fe1 C8 40.4(5) . . ? C4 Fe1 C8 123.1(6) . . ? C6 Fe1 C8 68.3(5) . . ? C3 Fe1 C8 159.3(5) . . ? C9 Fe1 C8 40.2(5) . . ? C2 Fe1 C10 109.3(6) . . ? C1 Fe1 C10 126.1(5) . . ? C5 Fe1 C10 162.9(5) . . ? C7 Fe1 C10 68.4(5) . . ? C4 Fe1 C10 155.2(5) . . ? C6 Fe1 C10 40.5(5) . . ? C3 Fe1 C10 121.9(5) . . ? C9 Fe1 C10 40.5(5) . . ? C8 Fe1 C10 68.3(5) . . ? Hg1 I2 Hg1 84.11(3) . 2_766 ? P1 Hg1 I1 130.37(8) . . ? P1 Hg1 I2 103.75(8) . . ? I1 Hg1 I2 116.30(3) . . ? P1 Hg1 I2 97.99(8) . 2_766 ? I1 Hg1 I2 105.40(3) . 2_766 ? I2 Hg1 I2 95.89(3) . 2_766 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.149 _refine_diff_density_min -1.866 _refine_diff_density_rms 0.238 #====================================================================== data_i0772 _database_code_depnum_ccdc_archive 'CCDC 805328' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Br2 Fe N P Zn' _chemical_formula_sum 'C28 H24 Br2 Fe N P Zn' _chemical_formula_weight 686.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.2769(5) _cell_length_b 18.5543(9) _cell_length_c 15.1266(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.655(4) _cell_angle_gamma 90.00 _cell_volume 2598.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 13120 _cell_measurement_theta_min 1.74 _cell_measurement_theta_max 25.54 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.755 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 4.636 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2810 _exptl_absorpt_correction_T_max 0.7870 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 156 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 14373 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4562 _reflns_number_gt 3659 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4562 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0021(3) 0.13370(17) 0.3508(2) 0.0303(7) Uani 1 1 d . . . C2 C -0.0147(4) 0.0925(2) 0.4315(2) 0.0374(8) Uani 1 1 d . . . H2A H -0.0766 0.0531 0.4388 0.045 Uiso 1 1 calc R . . C3 C 0.0836(4) 0.1226(2) 0.4976(2) 0.0475(10) Uani 1 1 d . . . H3A H 0.0985 0.1060 0.5562 0.057 Uiso 1 1 calc R . . C4 C 0.1553(4) 0.1817(2) 0.4605(3) 0.0481(10) Uani 1 1 d . . . H4A H 0.2248 0.2112 0.4905 0.058 Uiso 1 1 calc R . . C5 C 0.1040(4) 0.18896(19) 0.3698(2) 0.0385(8) Uani 1 1 d . . . H5A H 0.1344 0.2237 0.3298 0.046 Uiso 1 1 calc R . . C6 C 0.2774(3) 0.02865(17) 0.2913(2) 0.0309(7) Uani 1 1 d . . . C7 C 0.2471(4) -0.01590(19) 0.3651(2) 0.0408(8) Uani 1 1 d . . . H7A H 0.1848 -0.0559 0.3634 0.049 Uiso 1 1 calc R . . C8 C 0.3272(4) 0.0106(2) 0.4413(2) 0.0451(9) Uani 1 1 d . . . H8A H 0.3272 -0.0090 0.4985 0.054 Uiso 1 1 calc R . . C9 C 0.4073(4) 0.0720(2) 0.4166(2) 0.0426(9) Uani 1 1 d . . . H9A H 0.4690 0.1001 0.4544 0.051 Uiso 1 1 calc R . . C10 C 0.3767(3) 0.0830(2) 0.3235(2) 0.0352(7) Uani 1 1 d . . . H10A H 0.4153 0.1198 0.2894 0.042 Uiso 1 1 calc R . . C11 C 0.2230(4) 0.01674(18) 0.1966(2) 0.0333(7) Uani 1 1 d . . . H11A H 0.1194 0.0274 0.1906 0.040 Uiso 1 1 calc R . . H11B H 0.2356 -0.0342 0.1815 0.040 Uiso 1 1 calc R . . C12 C 0.2998(3) 0.06280(18) 0.1314(2) 0.0308(7) Uani 1 1 d . . . C13 C 0.4366(4) 0.0436(2) 0.1086(2) 0.0391(8) Uani 1 1 d . . . H13A H 0.4810 0.0019 0.1330 0.047 Uiso 1 1 calc R . . C14 C 0.5081(4) 0.0858(2) 0.0498(2) 0.0458(9) Uani 1 1 d . . . H14A H 0.6010 0.0732 0.0337 0.055 Uiso 1 1 calc R . . C15 C 0.4404(4) 0.1465(2) 0.0154(2) 0.0460(9) Uani 1 1 d . . . H15A H 0.4854 0.1755 -0.0257 0.055 Uiso 1 1 calc R . . C16 C 0.3055(4) 0.1641(2) 0.0421(2) 0.0406(8) Uani 1 1 d . . . H16A H 0.2611 0.2065 0.0199 0.049 Uiso 1 1 calc R . . C17 C -0.2584(3) 0.18800(16) 0.2606(2) 0.0281(7) Uani 1 1 d . . . C18 C -0.3057(4) 0.20312(17) 0.3448(2) 0.0328(7) Uani 1 1 d . . . H18A H -0.2544 0.1850 0.3956 0.039 Uiso 1 1 calc R . . C19 C -0.4282(4) 0.2448(2) 0.3534(2) 0.0398(8) Uani 1 1 d . . . H19A H -0.4601 0.2545 0.4099 0.048 Uiso 1 1 calc R . . C20 C -0.5038(4) 0.27203(19) 0.2787(3) 0.0421(9) Uani 1 1 d . . . H20A H -0.5876 0.2996 0.2847 0.051 Uiso 1 1 calc R . . C21 C -0.4562(4) 0.25868(19) 0.1953(3) 0.0405(8) Uani 1 1 d . . . H21A H -0.5066 0.2780 0.1449 0.049 Uiso 1 1 calc R . . C22 C -0.3335(4) 0.21658(18) 0.1862(2) 0.0340(7) Uani 1 1 d . . . H22A H -0.3015 0.2075 0.1296 0.041 Uiso 1 1 calc R . . C23 C -0.1891(3) 0.03845(17) 0.2418(2) 0.0278(6) Uani 1 1 d . . . C24 C -0.2848(3) 0.01712(17) 0.3049(2) 0.0317(7) Uani 1 1 d . . . H24A H -0.3083 0.0494 0.3496 0.038 Uiso 1 1 calc R . . C25 C -0.3451(4) -0.05148(19) 0.3018(2) 0.0388(8) Uani 1 1 d . . . H25A H -0.4089 -0.0654 0.3445 0.047 Uiso 1 1 calc R . . C26 C -0.3117(4) -0.09918(18) 0.2361(3) 0.0416(8) Uani 1 1 d . . . H26A H -0.3507 -0.1459 0.2349 0.050 Uiso 1 1 calc R . . C27 C -0.2199(4) -0.07775(19) 0.1716(2) 0.0398(8) Uani 1 1 d . . . H27A H -0.1983 -0.1100 0.1264 0.048 Uiso 1 1 calc R . . C28 C -0.1606(3) -0.00965(18) 0.1735(2) 0.0321(7) Uani 1 1 d . . . H28A H -0.1007 0.0047 0.1288 0.039 Uiso 1 1 calc R . . N1 N 0.2340(3) 0.12273(15) 0.09923(17) 0.0315(6) Uani 1 1 d . . . P1 P -0.10582(8) 0.12747(4) 0.24641(5) 0.02624(17) Uani 1 1 d . . . Fe1 Fe 0.19180(5) 0.08900(3) 0.39110(3) 0.03003(12) Uani 1 1 d . . . Zn1 Zn 0.02655(4) 0.16083(2) 0.11832(2) 0.03163(11) Uani 1 1 d . . . Br1 Br -0.11143(4) 0.12156(2) -0.01279(2) 0.04287(11) Uani 1 1 d . . . Br2 Br 0.06300(5) 0.28824(2) 0.12673(3) 0.05465(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0250(15) 0.0355(17) 0.0304(16) -0.0024(14) 0.0028(13) 0.0046(13) C2 0.0302(17) 0.053(2) 0.0294(18) 0.0025(15) 0.0061(14) 0.0076(16) C3 0.041(2) 0.076(3) 0.0250(17) -0.0069(18) 0.0009(15) 0.016(2) C4 0.041(2) 0.055(2) 0.046(2) -0.0224(19) -0.0131(18) 0.0097(18) C5 0.0338(18) 0.0344(18) 0.047(2) -0.0083(16) -0.0028(16) 0.0014(15) C6 0.0263(16) 0.0324(17) 0.0345(17) -0.0001(14) 0.0050(13) 0.0067(13) C7 0.041(2) 0.0365(19) 0.046(2) 0.0068(16) 0.0097(16) 0.0088(16) C8 0.041(2) 0.060(2) 0.0342(19) 0.0115(17) 0.0068(16) 0.0186(19) C9 0.0264(17) 0.069(3) 0.0322(18) -0.0001(17) -0.0025(14) 0.0103(17) C10 0.0273(17) 0.047(2) 0.0321(17) -0.0011(15) 0.0088(14) 0.0011(15) C11 0.0305(17) 0.0337(18) 0.0362(18) -0.0070(14) 0.0059(14) -0.0002(14) C12 0.0297(17) 0.0378(18) 0.0251(16) -0.0077(13) 0.0018(13) 0.0009(14) C13 0.0327(18) 0.049(2) 0.0362(18) -0.0082(16) 0.0054(15) 0.0064(16) C14 0.0306(18) 0.065(3) 0.043(2) -0.0171(19) 0.0106(16) 0.0001(18) C15 0.0387(19) 0.064(3) 0.036(2) -0.0034(17) 0.0111(16) -0.0148(19) C16 0.0387(19) 0.049(2) 0.0347(18) 0.0024(16) 0.0031(15) -0.0026(17) C17 0.0248(15) 0.0244(15) 0.0354(17) -0.0027(13) 0.0031(13) -0.0020(12) C18 0.0357(18) 0.0311(17) 0.0314(17) -0.0048(13) 0.0003(14) 0.0020(14) C19 0.040(2) 0.0394(19) 0.0404(19) -0.0115(16) 0.0075(16) 0.0007(16) C20 0.0317(18) 0.0345(19) 0.060(2) -0.0065(17) 0.0018(17) 0.0052(15) C21 0.0363(19) 0.0349(18) 0.050(2) 0.0037(16) -0.0036(16) 0.0041(15) C22 0.0341(18) 0.0351(17) 0.0327(17) -0.0007(14) 0.0009(14) 0.0028(15) C23 0.0225(15) 0.0322(16) 0.0283(16) 0.0022(13) -0.0009(12) 0.0033(13) C24 0.0306(17) 0.0342(18) 0.0309(17) -0.0008(14) 0.0054(13) -0.0004(14) C25 0.0333(18) 0.0389(19) 0.045(2) 0.0074(16) 0.0057(15) -0.0026(15) C26 0.043(2) 0.0271(17) 0.054(2) 0.0049(16) -0.0019(17) -0.0028(15) C27 0.042(2) 0.0331(18) 0.044(2) -0.0072(16) 0.0015(16) 0.0025(16) C28 0.0264(16) 0.0375(18) 0.0326(17) -0.0017(14) 0.0028(13) 0.0002(14) N1 0.0256(14) 0.0391(15) 0.0300(14) -0.0028(12) 0.0036(11) 0.0007(12) P1 0.0247(4) 0.0276(4) 0.0266(4) -0.0003(3) 0.0030(3) 0.0006(3) Fe1 0.0250(2) 0.0376(3) 0.0274(2) -0.00123(19) 0.00118(18) 0.00322(19) Zn1 0.0294(2) 0.0333(2) 0.0327(2) 0.00043(16) 0.00575(16) 0.00169(16) Br1 0.03810(19) 0.0591(2) 0.03154(18) 0.00271(16) 0.00306(14) -0.01160(17) Br2 0.0685(3) 0.03184(19) 0.0656(3) -0.00179(17) 0.0199(2) 0.00138(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 C1 C5 1.438(5) . ? C1 C2 1.452(5) . ? C1 P1 1.800(3) . ? C1 Fe1 2.038(3) . ? C2 C3 1.424(5) . ? C2 Fe1 2.049(3) . ? C2 H2A 0.9400 . ? C3 C4 1.417(6) . ? C3 Fe1 2.049(4) . ? C3 H3A 0.9400 . ? C4 C5 1.429(5) . ? C4 Fe1 2.055(4) . ? C4 H4A 0.9400 . ? C5 Fe1 2.043(4) . ? C5 H5A 0.9400 . ? C6 C10 1.430(5) . ? C6 C7 1.431(5) . ? C6 C11 1.505(5) . ? C6 Fe1 2.078(3) . ? C7 C8 1.418(5) . ? C7 Fe1 2.057(4) . ? C7 H7A 0.9400 . ? C8 C9 1.422(6) . ? C8 Fe1 2.036(4) . ? C8 H8A 0.9400 . ? C9 C10 1.434(5) . ? C9 Fe1 2.037(3) . ? C9 H9A 0.9400 . ? C10 Fe1 2.055(3) . ? C10 H10A 0.9400 . ? C11 C12 1.516(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 N1 1.344(4) . ? C12 C13 1.383(5) . ? C13 C14 1.386(5) . ? C13 H13A 0.9400 . ? C14 C15 1.376(6) . ? C14 H14A 0.9400 . ? C15 C16 1.378(5) . ? C15 H15A 0.9400 . ? C16 N1 1.360(5) . ? C16 H16A 0.9400 . ? C17 C22 1.390(5) . ? C17 C18 1.402(5) . ? C17 P1 1.830(3) . ? C18 C19 1.387(5) . ? C18 H18A 0.9400 . ? C19 C20 1.387(5) . ? C19 H19A 0.9400 . ? C20 C21 1.385(5) . ? C20 H20A 0.9400 . ? C21 C22 1.395(5) . ? C21 H21A 0.9400 . ? C22 H22A 0.9400 . ? C23 C24 1.401(4) . ? C23 C28 1.404(4) . ? C23 P1 1.823(3) . ? C24 C25 1.390(5) . ? C24 H24A 0.9400 . ? C25 C26 1.380(5) . ? C25 H25A 0.9400 . ? C26 C27 1.393(5) . ? C26 H26A 0.9400 . ? C27 C28 1.378(5) . ? C27 H27A 0.9400 . ? C28 H28A 0.9400 . ? N1 Zn1 2.087(3) . ? P1 Zn1 2.4389(9) . ? Zn1 Br2 2.3904(5) . ? Zn1 Br1 2.4040(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 107.3(3) . . ? C5 C1 P1 122.9(3) . . ? C2 C1 P1 129.6(3) . . ? C5 C1 Fe1 69.53(18) . . ? C2 C1 Fe1 69.58(18) . . ? P1 C1 Fe1 130.43(17) . . ? C3 C2 C1 107.6(3) . . ? C3 C2 Fe1 69.7(2) . . ? C1 C2 Fe1 68.81(18) . . ? C3 C2 H2A 126.2 . . ? C1 C2 H2A 126.2 . . ? Fe1 C2 H2A 126.8 . . ? C4 C3 C2 108.7(3) . . ? C4 C3 Fe1 70.0(2) . . ? C2 C3 Fe1 69.65(19) . . ? C4 C3 H3A 125.6 . . ? C2 C3 H3A 125.6 . . ? Fe1 C3 H3A 126.3 . . ? C3 C4 C5 108.5(3) . . ? C3 C4 Fe1 69.6(2) . . ? C5 C4 Fe1 69.2(2) . . ? C3 C4 H4A 125.7 . . ? C5 C4 H4A 125.7 . . ? Fe1 C4 H4A 127.1 . . ? C4 C5 C1 107.9(3) . . ? C4 C5 Fe1 70.0(2) . . ? C1 C5 Fe1 69.21(19) . . ? C4 C5 H5A 126.1 . . ? C1 C5 H5A 126.1 . . ? Fe1 C5 H5A 126.3 . . ? C10 C6 C7 107.2(3) . . ? C10 C6 C11 126.7(3) . . ? C7 C6 C11 126.0(3) . . ? C10 C6 Fe1 68.89(18) . . ? C7 C6 Fe1 68.97(19) . . ? C11 C6 Fe1 130.6(2) . . ? C8 C7 C6 108.3(3) . . ? C8 C7 Fe1 68.9(2) . . ? C6 C7 Fe1 70.52(19) . . ? C8 C7 H7A 125.8 . . ? C6 C7 H7A 125.8 . . ? Fe1 C7 H7A 126.3 . . ? C7 C8 C9 108.7(3) . . ? C7 C8 Fe1 70.5(2) . . ? C9 C8 Fe1 69.6(2) . . ? C7 C8 H8A 125.7 . . ? C9 C8 H8A 125.7 . . ? Fe1 C8 H8A 125.8 . . ? C8 C9 C10 107.3(3) . . ? C8 C9 Fe1 69.5(2) . . ? C10 C9 Fe1 70.17(18) . . ? C8 C9 H9A 126.3 . . ? C10 C9 H9A 126.3 . . ? Fe1 C9 H9A 125.5 . . ? C6 C10 C9 108.5(3) . . ? C6 C10 Fe1 70.61(18) . . ? C9 C10 Fe1 68.81(19) . . ? C6 C10 H10A 125.8 . . ? C9 C10 H10A 125.8 . . ? Fe1 C10 H10A 126.4 . . ? C6 C11 C12 113.2(3) . . ? C6 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C6 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.8 . . ? N1 C12 C13 121.7(3) . . ? N1 C12 C11 118.7(3) . . ? C13 C12 C11 119.5(3) . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C15 C14 C13 118.7(3) . . ? C15 C14 H14A 120.7 . . ? C13 C14 H14A 120.7 . . ? C14 C15 C16 119.0(3) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? N1 C16 C15 122.8(4) . . ? N1 C16 H16A 118.6 . . ? C15 C16 H16A 118.6 . . ? C22 C17 C18 119.3(3) . . ? C22 C17 P1 119.4(2) . . ? C18 C17 P1 121.2(2) . . ? C19 C18 C17 120.2(3) . . ? C19 C18 H18A 119.9 . . ? C17 C18 H18A 119.9 . . ? C20 C19 C18 120.1(3) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C22 120.0(3) . . ? C20 C21 H21A 120.0 . . ? C22 C21 H21A 120.0 . . ? C17 C22 C21 120.3(3) . . ? C17 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C28 118.7(3) . . ? C24 C23 P1 121.0(2) . . ? C28 C23 P1 120.3(2) . . ? C25 C24 C23 120.4(3) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C26 C25 C24 120.2(3) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C25 C26 C27 119.8(3) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27A 119.7 . . ? C26 C27 H27A 119.7 . . ? C27 C28 C23 120.3(3) . . ? C27 C28 H28A 119.9 . . ? C23 C28 H28A 119.9 . . ? C12 N1 C16 117.9(3) . . ? C12 N1 Zn1 129.1(2) . . ? C16 N1 Zn1 112.8(2) . . ? C1 P1 C23 107.04(15) . . ? C1 P1 C17 103.41(14) . . ? C23 P1 C17 103.38(14) . . ? C1 P1 Zn1 114.37(11) . . ? C23 P1 Zn1 115.69(10) . . ? C17 P1 Zn1 111.69(11) . . ? C8 Fe1 C9 40.89(16) . . ? C8 Fe1 C1 156.00(15) . . ? C9 Fe1 C1 163.06(15) . . ? C8 Fe1 C5 159.59(16) . . ? C9 Fe1 C5 123.16(16) . . ? C1 Fe1 C5 41.26(13) . . ? C8 Fe1 C2 118.54(15) . . ? C9 Fe1 C2 150.89(14) . . ? C1 Fe1 C2 41.61(13) . . ? C5 Fe1 C2 69.34(15) . . ? C8 Fe1 C3 104.22(15) . . ? C9 Fe1 C3 114.98(15) . . ? C1 Fe1 C3 69.16(14) . . ? C5 Fe1 C3 68.73(16) . . ? C2 Fe1 C3 40.65(15) . . ? C8 Fe1 C4 121.69(16) . . ? C9 Fe1 C4 102.99(16) . . ? C1 Fe1 C4 68.96(14) . . ? C5 Fe1 C4 40.81(15) . . ? C2 Fe1 C4 68.47(16) . . ? C3 Fe1 C4 40.41(18) . . ? C8 Fe1 C10 68.44(14) . . ? C9 Fe1 C10 41.02(14) . . ? C1 Fe1 C10 128.43(13) . . ? C5 Fe1 C10 107.90(15) . . ? C2 Fe1 C10 167.47(13) . . ? C3 Fe1 C10 150.91(15) . . ? C4 Fe1 C10 117.98(16) . . ? C8 Fe1 C7 40.55(16) . . ? C9 Fe1 C7 68.64(16) . . ? C1 Fe1 C7 123.64(14) . . ? C5 Fe1 C7 158.55(15) . . ? C2 Fe1 C7 109.67(15) . . ? C3 Fe1 C7 125.37(16) . . ? C4 Fe1 C7 160.24(16) . . ? C10 Fe1 C7 68.15(14) . . ? C8 Fe1 C6 68.32(14) . . ? C9 Fe1 C6 68.77(14) . . ? C1 Fe1 C6 111.90(13) . . ? C5 Fe1 C6 122.82(14) . . ? C2 Fe1 C6 129.96(14) . . ? C3 Fe1 C6 164.69(16) . . ? C4 Fe1 C6 154.90(16) . . ? C10 Fe1 C6 40.50(13) . . ? C7 Fe1 C6 40.50(13) . . ? N1 Zn1 Br2 102.34(8) . . ? N1 Zn1 Br1 103.32(7) . . ? Br2 Zn1 Br1 114.19(2) . . ? N1 Zn1 P1 122.64(8) . . ? Br2 Zn1 P1 106.58(3) . . ? Br1 Zn1 P1 108.05(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.999 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.069 #==================================================================== data_i0682 _database_code_depnum_ccdc_archive 'CCDC 805329' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 Br4 Fe2 N2 P2 Zn2, 2(C H2 Cl2)' _chemical_formula_sum 'C58 H52 Br4 Cl4 Fe2 N2 P2 Zn2' _chemical_formula_weight 1542.84 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.0066(9) _cell_length_b 14.5539(7) _cell_length_c 18.3142(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.865(6) _cell_angle_gamma 90.00 _cell_volume 3028.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12652 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 25.48 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 4.159 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5191 _exptl_absorpt_correction_T_max 0.8180 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 19330 _diffrn_reflns_av_R_equivalents 0.1594 _diffrn_reflns_av_sigmaI/netI 0.1104 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5342 _reflns_number_gt 3458 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0967P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5342 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0983 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.1777 _refine_ls_wR_factor_gt 0.1610 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7552(6) 0.3232(5) 0.4979(4) 0.0436(16) Uani 1 1 d . . . C2 C 0.7368(7) 0.4020(5) 0.5397(4) 0.0460(17) Uani 1 1 d . . . H2A H 0.6897 0.4538 0.5177 0.055 Uiso 1 1 calc R . . C3 C 0.8006(7) 0.3896(6) 0.6194(4) 0.0521(18) Uani 1 1 d . . . H3A H 0.8023 0.4310 0.6599 0.062 Uiso 1 1 calc R . . C4 C 0.8618(7) 0.3036(6) 0.6277(4) 0.0533(19) Uani 1 1 d . . . H4A H 0.9114 0.2781 0.6748 0.064 Uiso 1 1 calc R . . C5 C 0.8354(7) 0.2630(6) 0.5534(4) 0.0522(19) Uani 1 1 d . . . H5A H 0.8652 0.2062 0.5421 0.063 Uiso 1 1 calc R . . C6 C 0.5163(7) 0.3011(5) 0.5847(4) 0.0478(17) Uani 1 1 d . . . C7 C 0.5958(8) 0.2711(9) 0.6565(5) 0.079(3) Uani 1 1 d . . . H7A H 0.6143 0.3033 0.7040 0.095 Uiso 1 1 calc R . . C8 C 0.6424(8) 0.1856(9) 0.6452(8) 0.089(4) Uani 1 1 d . . . H8A H 0.6969 0.1500 0.6841 0.107 Uiso 1 1 calc R . . C9 C 0.5956(9) 0.1614(7) 0.5675(8) 0.083(3) Uani 1 1 d . . . H9A H 0.6136 0.1075 0.5442 0.099 Uiso 1 1 calc R . . C10 C 0.5174(7) 0.2310(5) 0.5301(5) 0.0521(18) Uani 1 1 d . . . H10A H 0.4722 0.2316 0.4769 0.062 Uiso 1 1 calc R . . C11 C 0.4461(7) 0.3890(6) 0.5673(5) 0.056(2) Uani 1 1 d . . . H11A H 0.4149 0.3981 0.5107 0.067 Uiso 1 1 calc R . . H11B H 0.4982 0.4415 0.5900 0.067 Uiso 1 1 calc R . . C12 C 0.3447(7) 0.3868(5) 0.5995(4) 0.0478(17) Uani 1 1 d . . . C13 C 0.2622(7) 0.3197(7) 0.5801(5) 0.061(2) Uani 1 1 d . . . H13A H 0.2690 0.2728 0.5457 0.073 Uiso 1 1 calc R . . C14 C 0.1675(7) 0.3168(6) 0.6085(5) 0.059(2) Uani 1 1 d . . . H14A H 0.1095 0.2700 0.5932 0.070 Uiso 1 1 calc R . . C15 C 0.1616(7) 0.3844(5) 0.6597(5) 0.0525(19) Uani 1 1 d . . . H15A H 0.0995 0.3851 0.6812 0.063 Uiso 1 1 calc R . . C16 C 0.2485(7) 0.4516(6) 0.6791(5) 0.055(2) Uani 1 1 d . . . H16A H 0.2445 0.4981 0.7146 0.066 Uiso 1 1 calc R . . C17 C 0.8392(6) 0.3235(5) 0.3699(4) 0.0447(16) Uani 1 1 d . . . C18 C 0.9373(7) 0.3720(6) 0.4183(5) 0.0550(19) Uani 1 1 d . . . H18A H 0.9370 0.3935 0.4672 0.066 Uiso 1 1 calc R . . C19 C 1.0341(8) 0.3882(7) 0.3943(6) 0.068(2) Uani 1 1 d . . . H19A H 1.1012 0.4189 0.4276 0.082 Uiso 1 1 calc R . . C20 C 1.0332(8) 0.3599(7) 0.3221(6) 0.069(3) Uani 1 1 d . . . H20A H 1.0981 0.3735 0.3050 0.083 Uiso 1 1 calc R . . C21 C 0.9398(8) 0.3127(6) 0.2756(5) 0.062(2) Uani 1 1 d . . . H21A H 0.9421 0.2910 0.2272 0.074 Uiso 1 1 calc R . . C22 C 0.8396(7) 0.2951(6) 0.2972(4) 0.0518(18) Uani 1 1 d . . . H22A H 0.7734 0.2644 0.2629 0.062 Uiso 1 1 calc R . . C23 C 0.6571(7) 0.1935(5) 0.3729(4) 0.0486(18) Uani 1 1 d . . . C24 C 0.7393(8) 0.1205(6) 0.3859(5) 0.059(2) Uani 1 1 d . . . H24A H 0.8213 0.1331 0.4023 0.070 Uiso 1 1 calc R . . C25 C 0.6992(10) 0.0304(6) 0.3746(6) 0.073(3) Uani 1 1 d . . . H25A H 0.7544 -0.0185 0.3842 0.088 Uiso 1 1 calc R . . C26 C 0.5785(11) 0.0106(6) 0.3490(6) 0.073(3) Uani 1 1 d . . . H26A H 0.5516 -0.0512 0.3415 0.088 Uiso 1 1 calc R . . C27 C 0.4979(9) 0.0838(6) 0.3349(5) 0.066(2) Uani 1 1 d . . . H27A H 0.4157 0.0717 0.3167 0.079 Uiso 1 1 calc R . . C28 C 0.5383(7) 0.1738(6) 0.3473(5) 0.0519(18) Uani 1 1 d . . . H28A H 0.4830 0.2227 0.3381 0.062 Uiso 1 1 calc R . . C29 C 0.1072(16) 0.1091(14) 0.3935(10) 0.150(7) Uani 1 1 d . . . H29A H 0.0955 0.0452 0.3739 0.180 Uiso 1 1 calc R . . H29B H 0.0478 0.1476 0.3559 0.180 Uiso 1 1 calc R . . N1 N 0.3387(5) 0.4541(4) 0.6498(3) 0.0460(14) Uani 1 1 d . . . P1 P 0.70497(17) 0.31171(13) 0.39553(11) 0.0431(4) Uani 1 1 d . . . Fe1 Fe 0.68418(9) 0.28358(8) 0.57990(6) 0.0476(3) Uani 1 1 d . . . Zn1 Zn 0.56197(8) 0.42497(6) 0.32055(5) 0.0473(3) Uani 1 1 d . . . Br1 Br 0.55134(8) 0.39900(6) 0.18904(5) 0.0602(3) Uani 1 1 d . . . Br2 Br 0.37527(8) 0.41082(6) 0.33869(6) 0.0635(3) Uani 1 1 d . . . Cl1 Cl 0.2397(5) 0.1433(6) 0.3935(4) 0.226(4) Uani 1 1 d . . . Cl2 Cl 0.0769(3) 0.1117(3) 0.4779(2) 0.1182(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(4) 0.047(4) 0.049(4) 0.003(3) 0.020(3) 0.000(3) C2 0.046(4) 0.047(4) 0.051(4) 0.002(3) 0.024(3) -0.007(3) C3 0.055(5) 0.057(5) 0.048(4) -0.007(4) 0.023(4) -0.008(4) C4 0.049(4) 0.072(5) 0.042(4) 0.003(4) 0.019(3) 0.001(4) C5 0.051(4) 0.066(5) 0.049(4) 0.001(4) 0.029(4) 0.007(4) C6 0.048(4) 0.054(4) 0.050(4) 0.001(3) 0.029(4) -0.003(3) C7 0.063(6) 0.129(10) 0.052(5) 0.025(6) 0.029(5) -0.002(6) C8 0.048(5) 0.117(9) 0.105(9) 0.065(8) 0.027(6) 0.007(6) C9 0.060(6) 0.064(6) 0.137(11) 0.024(6) 0.048(7) 0.009(5) C10 0.049(4) 0.047(4) 0.066(5) -0.007(4) 0.026(4) -0.004(3) C11 0.048(4) 0.059(5) 0.074(5) -0.009(4) 0.037(4) -0.003(4) C12 0.051(4) 0.048(4) 0.050(4) 0.000(3) 0.024(4) 0.003(3) C13 0.057(5) 0.070(5) 0.067(5) -0.017(4) 0.035(4) -0.012(4) C14 0.045(4) 0.062(5) 0.069(5) -0.003(4) 0.020(4) -0.010(4) C15 0.044(4) 0.054(4) 0.068(5) 0.002(4) 0.030(4) -0.001(3) C16 0.051(4) 0.062(5) 0.063(5) -0.002(4) 0.036(4) 0.002(4) C17 0.048(4) 0.040(4) 0.053(4) 0.004(3) 0.026(4) 0.001(3) C18 0.050(5) 0.065(5) 0.055(5) 0.000(4) 0.024(4) -0.004(4) C19 0.056(5) 0.083(6) 0.074(6) 0.010(5) 0.033(5) -0.007(5) C20 0.060(6) 0.079(6) 0.086(7) 0.018(5) 0.049(5) 0.000(5) C21 0.071(6) 0.067(5) 0.066(5) 0.002(4) 0.047(5) 0.004(4) C22 0.051(4) 0.066(5) 0.043(4) 0.003(4) 0.021(4) 0.006(4) C23 0.059(5) 0.051(4) 0.042(4) -0.004(3) 0.025(4) -0.005(4) C24 0.063(5) 0.060(5) 0.059(5) 0.006(4) 0.029(4) 0.003(4) C25 0.104(8) 0.046(5) 0.087(7) 0.006(5) 0.055(6) 0.005(5) C26 0.119(9) 0.044(5) 0.073(6) -0.010(4) 0.056(6) -0.014(5) C27 0.072(6) 0.070(6) 0.060(5) -0.017(4) 0.028(5) -0.022(5) C28 0.048(4) 0.054(4) 0.057(5) -0.010(4) 0.021(4) -0.005(3) C29 0.128(13) 0.174(17) 0.135(14) -0.019(12) 0.024(11) -0.075(12) N1 0.052(4) 0.049(4) 0.045(3) 0.001(3) 0.025(3) -0.005(3) P1 0.0441(10) 0.0450(10) 0.0457(10) 0.0013(8) 0.0223(8) -0.0001(8) Fe1 0.0441(6) 0.0581(7) 0.0472(6) 0.0104(5) 0.0240(5) 0.0028(5) Zn1 0.0474(5) 0.0507(5) 0.0499(5) -0.0030(4) 0.0241(4) -0.0038(4) Br1 0.0724(6) 0.0630(5) 0.0470(4) -0.0039(4) 0.0219(4) -0.0034(4) Br2 0.0499(5) 0.0698(6) 0.0779(6) -0.0107(4) 0.0305(4) -0.0078(4) Cl1 0.122(4) 0.341(9) 0.243(7) -0.149(7) 0.099(4) -0.078(5) Cl2 0.095(2) 0.128(3) 0.125(3) -0.018(2) 0.026(2) -0.008(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 C1 C2 1.436(10) . ? C1 C5 1.446(11) . ? C1 P1 1.782(8) . ? C1 Fe1 2.036(7) . ? C2 C3 1.425(11) . ? C2 Fe1 2.052(7) . ? C2 H2A 0.9500 . ? C3 C4 1.435(12) . ? C3 Fe1 2.051(8) . ? C3 H3A 0.9500 . ? C4 C5 1.423(11) . ? C4 Fe1 2.048(8) . ? C4 H4A 0.9500 . ? C5 Fe1 2.047(7) . ? C5 H5A 0.9500 . ? C6 C7 1.421(12) . ? C6 C10 1.432(11) . ? C6 C11 1.508(11) . ? C6 Fe1 2.061(7) . ? C7 C8 1.407(17) . ? C7 Fe1 2.022(9) . ? C7 H7A 0.9500 . ? C8 C9 1.395(17) . ? C8 Fe1 2.026(9) . ? C8 H8A 0.9500 . ? C9 C10 1.400(13) . ? C9 Fe1 2.046(10) . ? C9 H9A 0.9500 . ? C10 Fe1 2.061(8) . ? C10 H10A 0.9500 . ? C11 C12 1.515(10) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.353(11) . ? C12 N1 1.362(10) . ? C13 C14 1.396(11) . ? C13 H13A 0.9500 . ? C14 C15 1.376(12) . ? C14 H14A 0.9500 . ? C15 C16 1.390(11) . ? C15 H15A 0.9500 . ? C16 N1 1.356(9) . ? C16 H16A 0.9500 . ? C17 C22 1.397(11) . ? C17 C18 1.412(11) . ? C17 P1 1.827(7) . ? C18 C19 1.390(11) . ? C18 H18A 0.9500 . ? C19 C20 1.382(13) . ? C19 H19A 0.9500 . ? C20 C21 1.355(13) . ? C20 H20A 0.9500 . ? C21 C22 1.406(11) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C28 1.381(11) . ? C23 C24 1.416(12) . ? C23 P1 1.819(8) . ? C24 C25 1.389(13) . ? C24 H24A 0.9500 . ? C25 C26 1.402(15) . ? C25 H25A 0.9500 . ? C26 C27 1.406(14) . ? C26 H26A 0.9500 . ? C27 C28 1.390(12) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 Cl1 1.667(16) . ? C29 Cl2 1.698(18) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? N1 Zn1 2.097(6) 3_666 ? P1 Zn1 2.455(2) . ? Zn1 N1 2.097(6) 3_666 ? Zn1 Br2 2.3790(12) . ? Zn1 Br1 2.4003(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 C2 C1 C5 107.0(7) . . ? C2 C1 P1 125.3(6) . . ? C5 C1 P1 127.2(6) . . ? C2 C1 Fe1 70.1(4) . . ? C5 C1 Fe1 69.7(4) . . ? P1 C1 Fe1 132.0(4) . . ? C3 C2 C1 108.7(7) . . ? C3 C2 Fe1 69.6(4) . . ? C1 C2 Fe1 68.8(4) . . ? C3 C2 H2A 125.6 . . ? C1 C2 H2A 125.6 . . ? Fe1 C2 H2A 127.5 . . ? C2 C3 C4 107.8(7) . . ? C2 C3 Fe1 69.7(4) . . ? C4 C3 Fe1 69.4(5) . . ? C2 C3 H3A 126.1 . . ? C4 C3 H3A 126.1 . . ? Fe1 C3 H3A 126.4 . . ? C5 C4 C3 108.2(7) . . ? C5 C4 Fe1 69.6(4) . . ? C3 C4 Fe1 69.6(4) . . ? C5 C4 H4A 125.9 . . ? C3 C4 H4A 125.9 . . ? Fe1 C4 H4A 126.4 . . ? C4 C5 C1 108.3(7) . . ? C4 C5 Fe1 69.7(4) . . ? C1 C5 Fe1 68.8(4) . . ? C4 C5 H5A 125.9 . . ? C1 C5 H5A 125.9 . . ? Fe1 C5 H5A 127.2 . . ? C7 C6 C10 105.8(8) . . ? C7 C6 C11 128.2(8) . . ? C10 C6 C11 126.0(7) . . ? C7 C6 Fe1 68.2(5) . . ? C10 C6 Fe1 69.7(4) . . ? C11 C6 Fe1 125.7(5) . . ? C8 C7 C6 108.4(10) . . ? C8 C7 Fe1 69.8(5) . . ? C6 C7 Fe1 71.1(4) . . ? C8 C7 H7A 125.8 . . ? C6 C7 H7A 125.8 . . ? Fe1 C7 H7A 124.9 . . ? C9 C8 C7 109.0(9) . . ? C9 C8 Fe1 70.8(6) . . ? C7 C8 Fe1 69.5(6) . . ? C9 C8 H8A 125.5 . . ? C7 C8 H8A 125.5 . . ? Fe1 C8 H8A 125.8 . . ? C8 C9 C10 107.6(10) . . ? C8 C9 Fe1 69.2(7) . . ? C10 C9 Fe1 70.6(5) . . ? C8 C9 H9A 126.2 . . ? C10 C9 H9A 126.2 . . ? Fe1 C9 H9A 125.6 . . ? C9 C10 C6 109.2(9) . . ? C9 C10 Fe1 69.5(6) . . ? C6 C10 Fe1 69.7(4) . . ? C9 C10 H10A 125.4 . . ? C6 C10 H10A 125.4 . . ? Fe1 C10 H10A 127.0 . . ? C6 C11 C12 111.4(6) . . ? C6 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C6 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 N1 120.2(7) . . ? C13 C12 C11 121.6(7) . . ? N1 C12 C11 118.2(7) . . ? C12 C13 C14 122.5(8) . . ? C12 C13 H13A 118.7 . . ? C14 C13 H13A 118.7 . . ? C15 C14 C13 117.4(8) . . ? C15 C14 H14A 121.3 . . ? C13 C14 H14A 121.3 . . ? C14 C15 C16 118.5(7) . . ? C14 C15 H15A 120.7 . . ? C16 C15 H15A 120.7 . . ? N1 C16 C15 123.2(7) . . ? N1 C16 H16A 118.4 . . ? C15 C16 H16A 118.4 . . ? C22 C17 C18 119.2(7) . . ? C22 C17 P1 119.5(6) . . ? C18 C17 P1 120.8(6) . . ? C19 C18 C17 119.9(8) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C20 C19 C18 120.2(9) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C21 C20 C19 120.1(8) . . ? C21 C20 H20A 120.0 . . ? C19 C20 H20A 120.0 . . ? C20 C21 C22 121.7(8) . . ? C20 C21 H21A 119.1 . . ? C22 C21 H21A 119.1 . . ? C17 C22 C21 118.8(8) . . ? C17 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C28 C23 C24 119.2(8) . . ? C28 C23 P1 119.3(6) . . ? C24 C23 P1 121.3(6) . . ? C25 C24 C23 119.6(9) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 121.0(9) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C27 118.8(8) . . ? C25 C26 H26A 120.6 . . ? C27 C26 H26A 120.6 . . ? C28 C27 C26 120.1(9) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C23 C28 C27 121.3(8) . . ? C23 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? Cl1 C29 Cl2 118.6(10) . . ? Cl1 C29 H29A 107.7 . . ? Cl2 C29 H29A 107.7 . . ? Cl1 C29 H29B 107.7 . . ? Cl2 C29 H29B 107.7 . . ? H29A C29 H29B 107.1 . . ? C16 N1 C12 118.2(7) . . ? C16 N1 Zn1 112.3(5) . 3_666 ? C12 N1 Zn1 129.0(5) . 3_666 ? C1 P1 C23 107.6(3) . . ? C1 P1 C17 103.6(3) . . ? C23 P1 C17 105.7(3) . . ? C1 P1 Zn1 117.6(2) . . ? C23 P1 Zn1 113.3(3) . . ? C17 P1 Zn1 108.0(2) . . ? C7 Fe1 C8 40.7(5) . . ? C7 Fe1 C1 167.5(4) . . ? C8 Fe1 C1 151.3(5) . . ? C7 Fe1 C9 68.2(5) . . ? C8 Fe1 C9 40.1(5) . . ? C1 Fe1 C9 119.4(4) . . ? C7 Fe1 C5 148.9(4) . . ? C8 Fe1 C5 116.4(4) . . ? C1 Fe1 C5 41.5(3) . . ? C9 Fe1 C5 108.4(4) . . ? C7 Fe1 C4 115.1(4) . . ? C8 Fe1 C4 105.7(4) . . ? C1 Fe1 C4 69.4(3) . . ? C9 Fe1 C4 127.1(4) . . ? C5 Fe1 C4 40.7(3) . . ? C7 Fe1 C3 105.9(4) . . ? C8 Fe1 C3 126.3(5) . . ? C1 Fe1 C3 69.3(3) . . ? C9 Fe1 C3 164.5(4) . . ? C5 Fe1 C3 68.8(3) . . ? C4 Fe1 C3 41.0(3) . . ? C7 Fe1 C2 128.0(4) . . ? C8 Fe1 C2 165.2(5) . . ? C1 Fe1 C2 41.1(3) . . ? C9 Fe1 C2 154.0(5) . . ? C5 Fe1 C2 68.8(3) . . ? C4 Fe1 C2 68.6(3) . . ? C3 Fe1 C2 40.6(3) . . ? C7 Fe1 C10 67.7(4) . . ? C8 Fe1 C10 67.0(4) . . ? C1 Fe1 C10 110.9(3) . . ? C9 Fe1 C10 39.9(4) . . ? C5 Fe1 C10 130.5(3) . . ? C4 Fe1 C10 166.1(3) . . ? C3 Fe1 C10 152.8(3) . . ? C2 Fe1 C10 121.4(3) . . ? C7 Fe1 C6 40.7(4) . . ? C8 Fe1 C6 68.3(4) . . ? C1 Fe1 C6 130.2(3) . . ? C9 Fe1 C6 68.4(3) . . ? C5 Fe1 C6 169.2(3) . . ? C4 Fe1 C6 149.5(3) . . ? C3 Fe1 C6 117.1(3) . . ? C2 Fe1 C6 109.3(3) . . ? C10 Fe1 C6 40.7(3) . . ? N1 Zn1 Br2 121.28(17) 3_666 . ? N1 Zn1 Br1 103.48(16) 3_666 . ? Br2 Zn1 Br1 112.31(5) . . ? N1 Zn1 P1 100.53(18) 3_666 . ? Br2 Zn1 P1 112.58(6) . . ? Br1 Zn1 P1 104.85(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.307 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.135 data_i0569 # CCDC 805330 _database_code_depnum_ccdc_archive 'CCDC 805330' #TrackingRef 'publus86_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Br2 Cd Fe N P' _chemical_formula_sum 'C28 H24 Br2 Cd Fe N P' _chemical_formula_weight 733.52 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 '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' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1388(11) _cell_length_b 9.5318(10) _cell_length_c 16.6270(17) _cell_angle_alpha 84.260(9) _cell_angle_beta 74.946(9) _cell_angle_gamma 77.441(9) _cell_volume 1363.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9790 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 25.58 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 4.317 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2698 _exptl_absorpt_correction_T_max 0.6328 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; Although the R(int) is 0.1210, the choice of the space group P-1 is unambingous. The crystal system is clearly triclinic and the e-statistic and the refined structure clearly show centrosymmetric symmetry. ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 8927 _diffrn_reflns_av_R_equivalents 0.1210 _diffrn_reflns_av_sigmaI/netI 0.1208 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.19 _reflns_number_total 4563 _reflns_number_gt 3667 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4563 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0877 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.2059 _refine_ls_wR_factor_gt 0.1969 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0552(10) 0.5377(8) 0.6680(5) 0.0314(17) Uani 1 1 d . . . C2 C -0.0294(11) 0.6436(8) 0.6196(6) 0.0357(18) Uani 1 1 d . . . H2A H -0.1024 0.6276 0.5917 0.043 Uiso 1 1 calc R . . C3 C 0.0174(11) 0.7784(9) 0.6214(6) 0.0390(19) Uani 1 1 d . . . H3A H -0.0203 0.8670 0.5950 0.047 Uiso 1 1 calc R . . C4 C 0.1288(11) 0.7563(9) 0.6693(6) 0.0386(19) Uani 1 1 d . . . H4A H 0.1784 0.8274 0.6805 0.046 Uiso 1 1 calc R . . C5 C 0.1542(10) 0.6065(8) 0.6983(5) 0.0334(17) Uani 1 1 d . . . H5A H 0.2236 0.5619 0.7314 0.040 Uiso 1 1 calc R . . C6 C -0.1487(10) 0.8447(9) 0.8331(6) 0.039(2) Uani 1 1 d . . . C7 C -0.1272(12) 0.7011(9) 0.8674(6) 0.043(2) Uani 1 1 d . . . H7A H -0.0589 0.6610 0.9019 0.051 Uiso 1 1 calc R . . C8 C -0.2266(12) 0.6269(10) 0.8410(6) 0.045(2) Uani 1 1 d . . . H8A H -0.2353 0.5294 0.8545 0.054 Uiso 1 1 calc R . . C9 C -0.3089(12) 0.7256(11) 0.7913(7) 0.050(3) Uani 1 1 d . . . H9A H -0.3823 0.7059 0.7649 0.061 Uiso 1 1 calc R . . C10 C -0.2621(11) 0.8615(9) 0.7876(6) 0.041(2) Uani 1 1 d . . . H10A H -0.3010 0.9476 0.7594 0.050 Uiso 1 1 calc R . . C11 C -0.0629(11) 0.9593(9) 0.8436(6) 0.039(2) Uani 1 1 d . . . H11A H 0.0389 0.9108 0.8532 0.047 Uiso 1 1 calc R . . H11B H -0.0436 1.0182 0.7908 0.047 Uiso 1 1 calc R . . C12 C -0.1460(10) 1.0591(9) 0.9142(6) 0.0367(19) Uani 1 1 d . . . C13 C -0.2807(12) 1.0369(10) 0.9738(6) 0.044(2) Uani 1 1 d . . . H13A H -0.3235 0.9551 0.9723 0.053 Uiso 1 1 calc R . . C14 C -0.3502(12) 1.1367(10) 1.0349(7) 0.049(2) Uani 1 1 d . . . H14A H -0.4419 1.1241 1.0753 0.058 Uiso 1 1 calc R . . C15 C -0.2854(13) 1.2539(10) 1.0365(7) 0.050(2) Uani 1 1 d . . . H15A H -0.3325 1.3234 1.0774 0.060 Uiso 1 1 calc R . . C16 C -0.1504(11) 1.2687(10) 0.9775(6) 0.041(2) Uani 1 1 d . . . H16A H -0.1042 1.3480 0.9796 0.049 Uiso 1 1 calc R . . C17 C 0.1807(10) 0.2696(9) 0.5895(5) 0.0347(18) Uani 1 1 d . . . C18 C 0.1790(13) 0.1278(9) 0.5712(7) 0.049(2) Uani 1 1 d . . . H18A H 0.1087 0.0762 0.6080 0.059 Uiso 1 1 calc R . . C19 C 0.2779(14) 0.0629(11) 0.5005(7) 0.057(3) Uani 1 1 d . . . H19A H 0.2748 -0.0319 0.4891 0.068 Uiso 1 1 calc R . . C20 C 0.3809(14) 0.1375(14) 0.4470(8) 0.063(3) Uani 1 1 d . . . H20A H 0.4470 0.0943 0.3980 0.075 Uiso 1 1 calc R . . C21 C 0.3886(12) 0.2737(12) 0.4640(7) 0.052(2) Uani 1 1 d . . . H21A H 0.4620 0.3221 0.4272 0.063 Uiso 1 1 calc R . . C22 C 0.2885(11) 0.3435(10) 0.5357(6) 0.0382(19) Uani 1 1 d . . . H22A H 0.2943 0.4377 0.5470 0.046 Uiso 1 1 calc R . . C23 C -0.1390(10) 0.3284(8) 0.6743(5) 0.0319(17) Uani 1 1 d . . . C24 C -0.1724(12) 0.3345(10) 0.5972(6) 0.042(2) Uani 1 1 d . . . H24A H -0.0967 0.3501 0.5478 0.051 Uiso 1 1 calc R . . C25 C -0.3190(12) 0.3176(10) 0.5926(7) 0.047(2) Uani 1 1 d . . . H25A H -0.3435 0.3263 0.5400 0.056 Uiso 1 1 calc R . . C26 C -0.4272(12) 0.2887(10) 0.6632(7) 0.047(2) Uani 1 1 d . . . H26A H -0.5253 0.2755 0.6594 0.057 Uiso 1 1 calc R . . C27 C -0.3927(12) 0.2792(12) 0.7385(7) 0.052(3) Uani 1 1 d . . . H27A H -0.4666 0.2568 0.7872 0.063 Uiso 1 1 calc R . . C28 C -0.2516(11) 0.3017(8) 0.7457(6) 0.0376(19) Uani 1 1 d . . . H28A H -0.2317 0.2988 0.7992 0.045 Uiso 1 1 calc R . . N1 N -0.0823(9) 1.1732(7) 0.9169(5) 0.0348(15) Uani 1 1 d . . . P1 P 0.0493(2) 0.3487(2) 0.68422(13) 0.0296(5) Uani 1 1 d . . . Fe1 Fe -0.07478(13) 0.70336(11) 0.73990(8) 0.0307(3) Uani 1 1 d . . . Br2 Br 0.33753(10) 1.00519(9) 0.76019(6) 0.0406(3) Uani 1 1 d . . . Br1 Br 0.22267(11) 1.38849(9) 0.90231(6) 0.0429(3) Uani 1 1 d . . . Cd1 Cd 0.13358(7) 1.22617(6) 0.81892(4) 0.0326(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(4) 0.028(4) 0.028(5) -0.010(3) -0.002(3) -0.008(3) C2 0.044(5) 0.024(4) 0.038(5) -0.010(3) -0.007(4) -0.003(3) C3 0.048(5) 0.028(4) 0.039(6) -0.005(3) -0.006(4) -0.008(4) C4 0.043(5) 0.037(4) 0.037(5) -0.010(3) -0.001(4) -0.015(4) C5 0.031(4) 0.033(4) 0.035(5) -0.002(3) -0.006(3) -0.008(3) C6 0.031(4) 0.038(4) 0.045(6) -0.014(4) 0.004(4) -0.010(3) C7 0.055(6) 0.029(4) 0.041(6) -0.005(3) -0.009(4) -0.004(4) C8 0.049(6) 0.045(5) 0.038(6) -0.009(4) 0.006(4) -0.018(4) C9 0.039(5) 0.049(5) 0.061(7) -0.026(5) 0.006(5) -0.015(4) C10 0.038(5) 0.031(4) 0.046(6) -0.017(3) 0.001(4) 0.004(3) C11 0.036(5) 0.036(4) 0.045(6) -0.022(4) 0.001(4) -0.008(4) C12 0.033(4) 0.042(4) 0.032(5) -0.007(3) 0.000(4) -0.008(3) C13 0.050(6) 0.044(5) 0.036(6) -0.015(4) 0.005(4) -0.017(4) C14 0.045(5) 0.048(5) 0.046(7) -0.022(4) 0.008(4) -0.011(4) C15 0.054(6) 0.044(5) 0.048(7) -0.024(4) 0.002(5) -0.011(4) C16 0.044(5) 0.040(4) 0.038(6) -0.014(4) -0.002(4) -0.011(4) C17 0.037(5) 0.035(4) 0.030(5) -0.010(3) -0.009(4) 0.001(3) C18 0.063(7) 0.033(4) 0.049(6) -0.016(4) -0.010(5) -0.001(4) C19 0.070(7) 0.042(5) 0.051(7) -0.029(4) -0.017(6) 0.019(5) C20 0.050(6) 0.082(8) 0.048(7) -0.023(6) -0.015(5) 0.016(6) C21 0.038(5) 0.068(6) 0.040(6) -0.014(5) -0.001(4) 0.006(5) C22 0.038(5) 0.043(4) 0.031(5) -0.008(3) -0.004(4) -0.006(4) C23 0.033(4) 0.025(4) 0.040(5) -0.008(3) -0.010(4) -0.006(3) C24 0.047(5) 0.046(5) 0.035(6) -0.005(4) -0.006(4) -0.014(4) C25 0.055(6) 0.047(5) 0.047(6) -0.001(4) -0.021(5) -0.020(4) C26 0.041(5) 0.044(5) 0.062(7) 0.001(4) -0.021(5) -0.013(4) C27 0.044(5) 0.059(6) 0.056(7) 0.005(5) -0.008(5) -0.021(5) C28 0.043(5) 0.031(4) 0.036(5) -0.009(3) -0.004(4) -0.007(3) N1 0.037(4) 0.033(3) 0.033(4) -0.011(3) -0.003(3) -0.008(3) P1 0.0291(10) 0.0255(9) 0.0327(12) -0.0091(7) -0.0036(8) -0.0034(7) Fe1 0.0327(6) 0.0252(6) 0.0326(7) -0.0096(4) -0.0034(5) -0.0046(4) Br2 0.0337(5) 0.0357(5) 0.0482(6) -0.0116(4) -0.0033(4) -0.0016(3) Br1 0.0470(6) 0.0440(5) 0.0410(6) -0.0156(4) -0.0084(4) -0.0132(4) Cd1 0.0335(4) 0.0311(3) 0.0322(4) -0.0096(2) -0.0036(3) -0.0060(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 C1 C5 1.437(11) . ? C1 C2 1.444(12) . ? C1 P1 1.806(7) . ? C1 Fe1 2.039(8) . ? C2 C3 1.445(11) . ? C2 Fe1 2.047(9) . ? C2 H2A 0.9500 . ? C3 C4 1.418(14) . ? C3 Fe1 2.054(9) . ? C3 H3A 0.9500 . ? C4 C5 1.450(12) . ? C4 Fe1 2.061(9) . ? C4 H4A 0.9500 . ? C5 Fe1 2.060(9) . ? C5 H5A 0.9500 . ? C6 C10 1.407(14) . ? C6 C7 1.422(13) . ? C6 C11 1.524(11) . ? C6 Fe1 2.037(9) . ? C7 C8 1.437(14) . ? C7 Fe1 2.047(10) . ? C7 H7A 0.9500 . ? C8 C9 1.412(16) . ? C8 Fe1 2.065(9) . ? C8 H8A 0.9500 . ? C9 C10 1.441(12) . ? C9 Fe1 2.059(10) . ? C9 H9A 0.9500 . ? C10 Fe1 2.060(9) . ? C10 H10A 0.9500 . ? C11 C12 1.519(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N1 1.350(11) . ? C12 C13 1.407(13) . ? C13 C14 1.391(13) . ? C13 H13A 0.9500 . ? C14 C15 1.379(13) . ? C14 H14A 0.9500 . ? C15 C16 1.386(14) . ? C15 H15A 0.9500 . ? C16 N1 1.358(12) . ? C16 H16A 0.9500 . ? C17 C22 1.410(13) . ? C17 C18 1.419(12) . ? C17 P1 1.831(9) . ? C18 C19 1.389(15) . ? C18 H18A 0.9500 . ? C19 C20 1.383(19) . ? C19 H19A 0.9500 . ? C20 C21 1.376(17) . ? C20 H20A 0.9500 . ? C21 C22 1.424(14) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.385(13) . ? C23 C28 1.397(13) . ? C23 P1 1.823(8) . ? C24 C25 1.406(14) . ? C24 H24A 0.9500 . ? C25 C26 1.371(15) . ? C25 H25A 0.9500 . ? C26 C27 1.358(16) . ? C26 H26A 0.9500 . ? C27 C28 1.388(14) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? N1 Cd1 2.323(7) . ? P1 Cd1 2.637(2) 1_545 ? Br2 Cd1 2.5734(10) . ? Br1 Cd1 2.5578(10) . ? Cd1 P1 2.637(2) 1_565 ? 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 C5 C1 C2 108.2(6) . . ? C5 C1 P1 124.6(6) . . ? C2 C1 P1 127.1(6) . . ? C5 C1 Fe1 70.3(5) . . ? C2 C1 Fe1 69.6(5) . . ? P1 C1 Fe1 128.3(4) . . ? C1 C2 C3 107.4(8) . . ? C1 C2 Fe1 69.0(5) . . ? C3 C2 Fe1 69.6(5) . . ? C1 C2 H2A 126.3 . . ? C3 C2 H2A 126.3 . . ? Fe1 C2 H2A 126.6 . . ? C4 C3 C2 108.5(7) . . ? C4 C3 Fe1 70.1(5) . . ? C2 C3 Fe1 69.1(5) . . ? C4 C3 H3A 125.7 . . ? C2 C3 H3A 125.7 . . ? Fe1 C3 H3A 126.6 . . ? C3 C4 C5 108.3(7) . . ? C3 C4 Fe1 69.6(5) . . ? C5 C4 Fe1 69.4(5) . . ? C3 C4 H4A 125.8 . . ? C5 C4 H4A 125.8 . . ? Fe1 C4 H4A 126.8 . . ? C1 C5 C4 107.5(7) . . ? C1 C5 Fe1 68.7(5) . . ? C4 C5 Fe1 69.4(5) . . ? C1 C5 H5A 126.2 . . ? C4 C5 H5A 126.2 . . ? Fe1 C5 H5A 127.2 . . ? C10 C6 C7 108.0(8) . . ? C10 C6 C11 126.3(8) . . ? C7 C6 C11 125.7(9) . . ? C10 C6 Fe1 70.8(5) . . ? C7 C6 Fe1 70.0(5) . . ? C11 C6 Fe1 124.5(6) . . ? C6 C7 C8 108.3(9) . . ? C6 C7 Fe1 69.2(5) . . ? C8 C7 Fe1 70.2(6) . . ? C6 C7 H7A 125.9 . . ? C8 C7 H7A 125.9 . . ? Fe1 C7 H7A 126.3 . . ? C9 C8 C7 107.4(8) . . ? C9 C8 Fe1 69.8(6) . . ? C7 C8 Fe1 68.9(5) . . ? C9 C8 H8A 126.3 . . ? C7 C8 H8A 126.3 . . ? Fe1 C8 H8A 126.6 . . ? C8 C9 C10 108.1(9) . . ? C8 C9 Fe1 70.2(6) . . ? C10 C9 Fe1 69.6(5) . . ? C8 C9 H9A 126.0 . . ? C10 C9 H9A 126.0 . . ? Fe1 C9 H9A 125.9 . . ? C6 C10 C9 108.1(9) . . ? C6 C10 Fe1 69.0(5) . . ? C9 C10 Fe1 69.5(5) . . ? C6 C10 H10A 125.9 . . ? C9 C10 H10A 125.9 . . ? Fe1 C10 H10A 127.1 . . ? C12 C11 C6 115.1(7) . . ? C12 C11 H11A 108.5 . . ? C6 C11 H11A 108.5 . . ? C12 C11 H11B 108.5 . . ? C6 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? N1 C12 C13 121.0(8) . . ? N1 C12 C11 115.6(7) . . ? C13 C12 C11 123.4(8) . . ? C14 C13 C12 118.9(8) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C15 C14 C13 119.7(9) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 119.0(8) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? N1 C16 C15 122.0(8) . . ? N1 C16 H16A 119.0 . . ? C15 C16 H16A 119.0 . . ? C22 C17 C18 118.7(9) . . ? C22 C17 P1 121.7(6) . . ? C18 C17 P1 119.5(7) . . ? C19 C18 C17 121.4(10) . . ? C19 C18 H18A 119.3 . . ? C17 C18 H18A 119.3 . . ? C20 C19 C18 119.5(10) . . ? C20 C19 H19A 120.3 . . ? C18 C19 H19A 120.3 . . ? C21 C20 C19 120.7(11) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 121.3(11) . . ? C20 C21 H21A 119.4 . . ? C22 C21 H21A 119.4 . . ? C17 C22 C21 118.4(9) . . ? C17 C22 H22A 120.8 . . ? C21 C22 H22A 120.8 . . ? C24 C23 C28 118.7(8) . . ? C24 C23 P1 121.7(7) . . ? C28 C23 P1 119.6(7) . . ? C23 C24 C25 119.7(9) . . ? C23 C24 H24A 120.2 . . ? C25 C24 H24A 120.2 . . ? C26 C25 C24 120.8(9) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C27 C26 C25 119.3(9) . . ? C27 C26 H26A 120.3 . . ? C25 C26 H26A 120.3 . . ? C26 C27 C28 121.4(10) . . ? C26 C27 H27A 119.3 . . ? C28 C27 H27A 119.3 . . ? C27 C28 C23 120.0(9) . . ? C27 C28 H28A 120.0 . . ? C23 C28 H28A 120.0 . . ? C12 N1 C16 119.4(7) . . ? C12 N1 Cd1 124.1(6) . . ? C16 N1 Cd1 116.5(5) . . ? C1 P1 C23 107.3(4) . . ? C1 P1 C17 103.6(4) . . ? C23 P1 C17 102.7(4) . . ? C1 P1 Cd1 114.4(3) . 1_545 ? C23 P1 Cd1 116.2(3) . 1_545 ? C17 P1 Cd1 111.3(3) . 1_545 ? C1 Fe1 C6 160.7(4) . . ? C1 Fe1 C2 41.4(3) . . ? C6 Fe1 C2 155.0(4) . . ? C1 Fe1 C7 125.8(3) . . ? C6 Fe1 C7 40.8(4) . . ? C2 Fe1 C7 163.0(3) . . ? C1 Fe1 C3 69.3(3) . . ? C6 Fe1 C3 118.3(3) . . ? C2 Fe1 C3 41.3(3) . . ? C7 Fe1 C3 154.9(4) . . ? C1 Fe1 C9 123.9(4) . . ? C6 Fe1 C9 68.5(4) . . ? C2 Fe1 C9 108.3(4) . . ? C7 Fe1 C9 68.0(5) . . ? C3 Fe1 C9 123.3(4) . . ? C1 Fe1 C4 69.2(3) . . ? C6 Fe1 C4 104.5(3) . . ? C2 Fe1 C4 68.9(4) . . ? C7 Fe1 C4 121.0(4) . . ? C3 Fe1 C4 40.3(4) . . ? C9 Fe1 C4 158.2(4) . . ? C1 Fe1 C10 158.7(4) . . ? C6 Fe1 C10 40.2(4) . . ? C2 Fe1 C10 121.1(4) . . ? C7 Fe1 C10 67.8(4) . . ? C3 Fe1 C10 105.2(4) . . ? C9 Fe1 C10 40.9(4) . . ? C4 Fe1 C10 120.7(4) . . ? C1 Fe1 C5 41.0(3) . . ? C6 Fe1 C5 122.5(4) . . ? C2 Fe1 C5 69.2(4) . . ? C7 Fe1 C5 108.2(4) . . ? C3 Fe1 C5 68.8(3) . . ? C9 Fe1 C5 159.8(4) . . ? C4 Fe1 C5 41.2(3) . . ? C10 Fe1 C5 157.9(3) . . ? C1 Fe1 C8 110.1(4) . . ? C6 Fe1 C8 68.8(4) . . ? C2 Fe1 C8 125.7(4) . . ? C7 Fe1 C8 40.9(4) . . ? C3 Fe1 C8 160.9(4) . . ? C9 Fe1 C8 40.0(5) . . ? C4 Fe1 C8 158.6(4) . . ? C10 Fe1 C8 68.1(4) . . ? C5 Fe1 C8 124.1(4) . . ? N1 Cd1 Br1 100.34(17) . . ? N1 Cd1 Br2 114.82(17) . . ? Br1 Cd1 Br2 115.36(4) . . ? N1 Cd1 P1 109.13(19) . 1_565 ? Br1 Cd1 P1 115.59(5) . 1_565 ? Br2 Cd1 P1 102.02(5) . 1_565 ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 3.222 _refine_diff_density_min -1.885 _refine_diff_density_rms 0.317 #===================================================================== data_i0791 _database_code_depnum_ccdc_archive 'CCDC 805331' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Cd Fe I2 N P' _chemical_formula_sum 'C28 H24 Cd Fe I2 N P' _chemical_formula_weight 827.50 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' 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4757(8) _cell_length_b 19.0085(11) _cell_length_c 15.4717(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.513(6) _cell_angle_gamma 90.00 _cell_volume 2778.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11155 _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 25.53 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 3.585 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5150 _exptl_absorpt_correction_T_max 0.8484 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 146 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 14403 _diffrn_reflns_av_R_equivalents 0.1141 _diffrn_reflns_av_sigmaI/netI 0.1033 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4897 _reflns_number_gt 3388 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4897 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5051(8) 0.1319(4) 0.1422(6) 0.0279(18) Uani 1 1 d . . . C2 C 0.5121(8) 0.0903(5) 0.0648(6) 0.0300(18) Uani 1 1 d . . . H2A H 0.5678 0.0493 0.0590 0.036 Uiso 1 1 calc R . . C3 C 0.4181(9) 0.1229(5) -0.0028(6) 0.034(2) Uani 1 1 d . . . H3A H 0.4030 0.1075 -0.0613 0.041 Uiso 1 1 calc R . . C4 C 0.3530(9) 0.1819(5) 0.0345(6) 0.036(2) Uani 1 1 d . . . H4A H 0.2862 0.2124 0.0047 0.043 Uiso 1 1 calc R . . C5 C 0.4024(9) 0.1882(4) 0.1221(6) 0.0308(19) Uani 1 1 d . . . H5A H 0.3742 0.2229 0.1614 0.037 Uiso 1 1 calc R . . C6 C 0.2192(8) 0.0321(4) 0.1986(6) 0.0261(17) Uani 1 1 d . . . C7 C 0.1268(9) 0.0887(4) 0.1686(6) 0.0305(18) Uani 1 1 d . . . H7A H 0.0926 0.1252 0.2032 0.037 Uiso 1 1 calc R . . C8 C 0.0956(8) 0.0801(5) 0.0768(6) 0.035(2) Uani 1 1 d . . . H8A H 0.0366 0.1101 0.0406 0.042 Uiso 1 1 calc R . . C9 C 0.1668(9) 0.0197(5) 0.0488(6) 0.034(2) Uani 1 1 d . . . H9A H 0.1634 0.0019 -0.0088 0.041 Uiso 1 1 calc R . . C10 C 0.2461(9) -0.0102(5) 0.1244(6) 0.034(2) Uani 1 1 d . . . H10A H 0.3053 -0.0505 0.1247 0.041 Uiso 1 1 calc R . . C11 C 0.2745(8) 0.0154(4) 0.2888(6) 0.0279(18) Uani 1 1 d . . . H11A H 0.3756 0.0287 0.2970 0.033 Uiso 1 1 calc R . . H11B H 0.2675 -0.0359 0.2986 0.033 Uiso 1 1 calc R . . C12 C 0.1920(8) 0.0544(4) 0.3555(5) 0.0245(17) Uani 1 1 d . . . C13 C 0.0560(8) 0.0306(4) 0.3737(6) 0.0298(18) Uani 1 1 d . . . H13A H 0.0151 -0.0093 0.3445 0.036 Uiso 1 1 calc R . . C14 C -0.0176(8) 0.0662(5) 0.4351(6) 0.033(2) Uani 1 1 d . . . H14A H -0.1089 0.0508 0.4483 0.040 Uiso 1 1 calc R . . C15 C 0.0446(9) 0.1247(5) 0.4768(6) 0.037(2) Uani 1 1 d . . . H15A H -0.0036 0.1495 0.5190 0.045 Uiso 1 1 calc R . . C16 C 0.1729(9) 0.1457(5) 0.4569(7) 0.036(2) Uani 1 1 d . . . H16A H 0.2131 0.1862 0.4851 0.043 Uiso 1 1 calc R . . C17 C 0.7568(8) 0.1845(4) 0.2346(5) 0.0256(17) Uani 1 1 d . . . C18 C 0.8319(9) 0.2081(4) 0.3096(6) 0.0317(19) Uani 1 1 d . . . H18A H 0.8015 0.1965 0.3649 0.038 Uiso 1 1 calc R . . C19 C 0.9539(8) 0.2497(4) 0.3027(6) 0.0318(19) Uani 1 1 d . . . H19A H 1.0071 0.2651 0.3538 0.038 Uiso 1 1 calc R . . C20 C 0.9975(8) 0.2685(4) 0.2210(6) 0.032(2) Uani 1 1 d . . . H20A H 1.0787 0.2972 0.2168 0.039 Uiso 1 1 calc R . . C21 C 0.9211(9) 0.2448(5) 0.1473(7) 0.039(2) Uani 1 1 d . . . H21A H 0.9510 0.2573 0.0921 0.046 Uiso 1 1 calc R . . C22 C 0.7996(8) 0.2026(4) 0.1518(6) 0.0270(17) Uani 1 1 d . . . H22A H 0.7477 0.1867 0.1005 0.032 Uiso 1 1 calc R . . C23 C 0.6874(8) 0.0372(4) 0.2508(5) 0.0246(17) Uani 1 1 d . . . C24 C 0.6542(8) -0.0120(4) 0.3145(5) 0.0275(18) Uani 1 1 d . . . H24A H 0.5906 0.0009 0.3562 0.033 Uiso 1 1 calc R . . C25 C 0.7131(9) -0.0794(4) 0.3173(7) 0.036(2) Uani 1 1 d . . . H25A H 0.6909 -0.1118 0.3610 0.043 Uiso 1 1 calc R . . C26 C 0.8068(9) -0.0990(4) 0.2538(6) 0.034(2) Uani 1 1 d . . . H26A H 0.8457 -0.1451 0.2541 0.041 Uiso 1 1 calc R . . C27 C 0.8415(9) -0.0505(4) 0.1910(6) 0.035(2) Uani 1 1 d . . . H27A H 0.9054 -0.0637 0.1495 0.042 Uiso 1 1 calc R . . C28 C 0.7837(8) 0.0171(4) 0.1882(6) 0.0259(17) Uani 1 1 d . . . H28A H 0.8080 0.0496 0.1451 0.031 Uiso 1 1 calc R . . N1 N 0.2509(7) 0.1108(3) 0.3967(5) 0.0275(15) Uani 1 1 d . . . P1 P 0.6059(2) 0.12485(11) 0.24492(14) 0.0256(4) Uani 1 1 d . . . Fe1 Fe 0.30867(11) 0.09202(6) 0.10112(8) 0.0262(3) Uani 1 1 d . . . I1 I 0.62719(6) 0.11576(3) 0.52757(4) 0.03254(15) Uani 1 1 d . . . I2 I 0.39384(6) 0.29942(3) 0.37026(4) 0.03436(16) Uani 1 1 d . . . Cd1 Cd 0.47008(6) 0.15929(3) 0.37881(4) 0.02716(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.029(4) 0.029(4) 0.025(5) 0.001(3) -0.001(3) -0.002(3) C2 0.024(4) 0.041(5) 0.026(5) -0.001(4) 0.011(4) 0.001(3) C3 0.030(4) 0.050(5) 0.023(5) 0.000(4) 0.005(4) -0.012(4) C4 0.032(4) 0.041(5) 0.035(5) 0.010(4) 0.005(4) 0.006(4) C5 0.031(4) 0.026(4) 0.035(5) 0.000(4) 0.000(4) 0.001(3) C6 0.020(4) 0.035(4) 0.023(4) 0.008(4) 0.001(3) -0.001(3) C7 0.029(4) 0.032(4) 0.032(5) -0.005(4) 0.009(4) 0.001(3) C8 0.021(4) 0.049(5) 0.034(5) 0.006(4) 0.002(4) -0.007(4) C9 0.038(5) 0.041(5) 0.025(5) -0.001(4) 0.013(4) -0.006(4) C10 0.031(4) 0.035(4) 0.036(5) -0.004(4) -0.001(4) -0.005(3) C11 0.022(4) 0.032(4) 0.031(5) -0.001(4) 0.006(3) 0.003(3) C12 0.022(4) 0.034(4) 0.017(4) 0.005(3) -0.002(3) -0.001(3) C13 0.026(4) 0.031(4) 0.032(5) 0.008(4) 0.001(4) -0.006(3) C14 0.021(4) 0.043(5) 0.035(5) 0.012(4) 0.001(4) -0.006(3) C15 0.029(4) 0.048(5) 0.035(5) 0.003(4) 0.006(4) -0.001(4) C16 0.031(4) 0.032(4) 0.045(6) 0.000(4) 0.005(4) 0.002(4) C17 0.022(4) 0.029(4) 0.026(5) -0.007(3) 0.002(3) 0.006(3) C18 0.033(4) 0.025(4) 0.035(5) 0.004(4) -0.007(4) -0.001(3) C19 0.029(4) 0.031(4) 0.034(5) -0.006(4) -0.008(4) -0.005(3) C20 0.023(4) 0.026(4) 0.048(6) -0.004(4) 0.003(4) -0.008(3) C21 0.029(4) 0.043(5) 0.044(6) 0.006(4) 0.001(4) 0.000(4) C22 0.028(4) 0.025(4) 0.028(5) 0.005(4) 0.003(3) 0.003(3) C23 0.025(4) 0.027(4) 0.022(4) 0.000(3) 0.005(3) -0.001(3) C24 0.022(4) 0.039(4) 0.022(5) -0.001(4) 0.001(3) 0.000(3) C25 0.033(4) 0.028(4) 0.044(6) 0.003(4) -0.006(4) -0.009(3) C26 0.034(4) 0.030(4) 0.036(5) -0.008(4) -0.005(4) 0.000(3) C27 0.033(4) 0.029(4) 0.042(6) -0.011(4) 0.001(4) 0.008(3) C28 0.022(4) 0.029(4) 0.026(5) 0.000(3) 0.004(3) -0.005(3) N1 0.022(3) 0.028(3) 0.032(4) 0.006(3) 0.001(3) -0.008(3) P1 0.0230(9) 0.0273(10) 0.0265(12) 0.0018(9) 0.0023(8) -0.0006(8) Fe1 0.0228(5) 0.0294(6) 0.0264(7) 0.0005(5) 0.0018(5) -0.0018(4) I1 0.0291(3) 0.0404(3) 0.0286(3) 0.0002(3) 0.0047(2) 0.0073(2) I2 0.0335(3) 0.0285(3) 0.0414(4) -0.0004(2) 0.0043(2) -0.0008(2) Cd1 0.0224(3) 0.0301(3) 0.0294(3) -0.0004(3) 0.0050(2) -0.0003(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 C1 C2 1.440(12) . ? C1 C5 1.464(11) . ? C1 P1 1.794(9) . ? C1 Fe1 2.063(8) . ? C2 C3 1.457(13) . ? C2 Fe1 2.050(8) . ? C2 H2A 0.9500 . ? C3 C4 1.425(13) . ? C3 Fe1 2.066(8) . ? C3 H3A 0.9500 . ? C4 C5 1.403(13) . ? C4 Fe1 2.055(9) . ? C4 H4A 0.9500 . ? C5 Fe1 2.047(8) . ? C5 H5A 0.9500 . ? C6 C7 1.441(11) . ? C6 C10 1.442(12) . ? C6 C11 1.486(12) . ? C6 Fe1 2.120(8) . ? C7 C8 1.437(13) . ? C7 Fe1 2.085(8) . ? C7 H7A 0.9500 . ? C8 C9 1.417(13) . ? C8 Fe1 2.037(8) . ? C8 H8A 0.9500 . ? C9 C10 1.454(13) . ? C9 Fe1 2.045(9) . ? C9 H9A 0.9500 . ? C10 Fe1 2.071(9) . ? C10 H10A 0.9500 . ? C11 C12 1.533(11) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N1 1.346(10) . ? C12 C13 1.415(11) . ? C13 C14 1.398(13) . ? C13 H13A 0.9500 . ? C14 C15 1.393(13) . ? C14 H14A 0.9500 . ? C15 C16 1.338(12) . ? C15 H15A 0.9500 . ? C16 N1 1.401(11) . ? C16 H16A 0.9500 . ? C17 C18 1.388(12) . ? C17 C22 1.416(12) . ? C17 P1 1.841(8) . ? C18 C19 1.411(11) . ? C18 H18A 0.9500 . ? C19 C20 1.406(13) . ? C19 H19A 0.9500 . ? C20 C21 1.378(13) . ? C20 H20A 0.9500 . ? C21 C22 1.410(12) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.413(11) . ? C23 C28 1.434(11) . ? C23 P1 1.835(8) . ? C24 C25 1.396(12) . ? C24 H24A 0.9500 . ? C25 C26 1.426(14) . ? C25 H25A 0.9500 . ? C26 C27 1.397(13) . ? C26 H26A 0.9500 . ? C27 C28 1.396(11) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? N1 Cd1 2.309(6) . ? P1 Cd1 2.607(2) . ? I1 Cd1 2.7675(9) . ? I2 Cd1 2.7605(8) . ? 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 C2 C1 C5 107.3(7) . . ? C2 C1 P1 129.8(6) . . ? C5 C1 P1 122.8(6) . . ? C2 C1 Fe1 69.0(4) . . ? C5 C1 Fe1 68.5(4) . . ? P1 C1 Fe1 130.6(5) . . ? C1 C2 C3 107.4(8) . . ? C1 C2 Fe1 70.0(4) . . ? C3 C2 Fe1 69.9(5) . . ? C1 C2 H2A 126.3 . . ? C3 C2 H2A 126.3 . . ? Fe1 C2 H2A 125.4 . . ? C4 C3 C2 107.6(8) . . ? C4 C3 Fe1 69.4(5) . . ? C2 C3 Fe1 68.7(5) . . ? C4 C3 H3A 126.2 . . ? C2 C3 H3A 126.2 . . ? Fe1 C3 H3A 127.3 . . ? C5 C4 C3 109.7(8) . . ? C5 C4 Fe1 69.7(5) . . ? C3 C4 Fe1 70.2(5) . . ? C5 C4 H4A 125.2 . . ? C3 C4 H4A 125.2 . . ? Fe1 C4 H4A 126.6 . . ? C4 C5 C1 108.0(8) . . ? C4 C5 Fe1 70.3(5) . . ? C1 C5 Fe1 69.7(4) . . ? C4 C5 H5A 126.0 . . ? C1 C5 H5A 126.0 . . ? Fe1 C5 H5A 125.5 . . ? C7 C6 C10 107.4(7) . . ? C7 C6 C11 128.6(8) . . ? C10 C6 C11 123.9(7) . . ? C7 C6 Fe1 68.7(5) . . ? C10 C6 Fe1 68.0(5) . . ? C11 C6 Fe1 130.7(5) . . ? C6 C7 C8 107.9(7) . . ? C6 C7 Fe1 71.3(5) . . ? C8 C7 Fe1 67.8(5) . . ? C6 C7 H7A 126.1 . . ? C8 C7 H7A 126.1 . . ? Fe1 C7 H7A 126.4 . . ? C9 C8 C7 109.2(8) . . ? C9 C8 Fe1 70.0(5) . . ? C7 C8 Fe1 71.4(5) . . ? C9 C8 H8A 125.4 . . ? C7 C8 H8A 125.4 . . ? Fe1 C8 H8A 124.8 . . ? C8 C9 C10 107.4(8) . . ? C8 C9 Fe1 69.4(5) . . ? C10 C9 Fe1 70.2(5) . . ? C8 C9 H9A 126.3 . . ? C10 C9 H9A 126.3 . . ? Fe1 C9 H9A 125.6 . . ? C6 C10 C9 108.1(8) . . ? C6 C10 Fe1 71.7(5) . . ? C9 C10 Fe1 68.4(5) . . ? C6 C10 H10A 125.9 . . ? C9 C10 H10A 125.9 . . ? Fe1 C10 H10A 125.5 . . ? C6 C11 C12 111.5(6) . . ? C6 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C6 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? N1 C12 C13 120.7(7) . . ? N1 C12 C11 119.3(7) . . ? C13 C12 C11 120.0(7) . . ? C14 C13 C12 119.4(8) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? C15 C14 C13 119.1(7) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? C16 C15 C14 119.4(9) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C15 C16 N1 123.3(8) . . ? C15 C16 H16A 118.4 . . ? N1 C16 H16A 118.4 . . ? C18 C17 C22 120.9(8) . . ? C18 C17 P1 118.5(7) . . ? C22 C17 P1 120.5(6) . . ? C17 C18 C19 119.1(9) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C20 C19 C18 120.7(8) . . ? C20 C19 H19A 119.6 . . ? C18 C19 H19A 119.6 . . ? C21 C20 C19 119.3(8) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C22 121.5(9) . . ? C20 C21 H21A 119.2 . . ? C22 C21 H21A 119.2 . . ? C21 C22 C17 118.4(8) . . ? C21 C22 H22A 120.8 . . ? C17 C22 H22A 120.8 . . ? C24 C23 C28 118.8(7) . . ? C24 C23 P1 121.4(6) . . ? C28 C23 P1 119.8(6) . . ? C25 C24 C23 121.3(8) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C24 C25 C26 119.2(9) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? C27 C26 C25 120.0(8) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C28 121.0(8) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? C27 C28 C23 119.6(8) . . ? C27 C28 H28A 120.2 . . ? C23 C28 H28A 120.2 . . ? C12 N1 C16 118.1(7) . . ? C12 N1 Cd1 127.2(5) . . ? C16 N1 Cd1 114.7(5) . . ? C1 P1 C23 107.7(4) . . ? C1 P1 C17 103.9(4) . . ? C23 P1 C17 103.7(3) . . ? C1 P1 Cd1 115.1(3) . . ? C23 P1 Cd1 114.9(3) . . ? C17 P1 Cd1 110.5(3) . . ? C8 Fe1 C9 40.6(4) . . ? C8 Fe1 C5 122.7(4) . . ? C9 Fe1 C5 157.9(4) . . ? C8 Fe1 C2 152.5(4) . . ? C9 Fe1 C2 118.9(3) . . ? C5 Fe1 C2 69.6(3) . . ? C8 Fe1 C4 103.8(4) . . ? C9 Fe1 C4 120.9(4) . . ? C5 Fe1 C4 40.0(4) . . ? C2 Fe1 C4 69.0(3) . . ? C8 Fe1 C1 162.7(4) . . ? C9 Fe1 C1 156.6(3) . . ? C5 Fe1 C1 41.7(3) . . ? C2 Fe1 C1 41.0(3) . . ? C4 Fe1 C1 68.5(3) . . ? C8 Fe1 C3 116.0(4) . . ? C9 Fe1 C3 103.7(3) . . ? C5 Fe1 C3 68.4(4) . . ? C2 Fe1 C3 41.5(4) . . ? C4 Fe1 C3 40.5(4) . . ? C1 Fe1 C3 68.9(3) . . ? C8 Fe1 C10 68.6(4) . . ? C9 Fe1 C10 41.4(4) . . ? C5 Fe1 C10 159.5(4) . . ? C2 Fe1 C10 108.7(4) . . ? C4 Fe1 C10 159.9(4) . . ? C1 Fe1 C10 123.7(3) . . ? C3 Fe1 C10 124.7(4) . . ? C8 Fe1 C7 40.8(4) . . ? C9 Fe1 C7 68.5(3) . . ? C5 Fe1 C7 108.3(3) . . ? C2 Fe1 C7 165.7(4) . . ? C4 Fe1 C7 119.1(3) . . ? C1 Fe1 C7 128.2(4) . . ? C3 Fe1 C7 152.1(4) . . ? C10 Fe1 C7 68.0(3) . . ? C8 Fe1 C6 68.0(3) . . ? C9 Fe1 C6 68.5(3) . . ? C5 Fe1 C6 124.1(4) . . ? C2 Fe1 C6 128.6(3) . . ? C4 Fe1 C6 155.8(3) . . ? C1 Fe1 C6 112.3(3) . . ? C3 Fe1 C6 163.7(3) . . ? C10 Fe1 C6 40.2(3) . . ? C7 Fe1 C6 40.1(3) . . ? N1 Cd1 P1 120.02(19) . . ? N1 Cd1 I2 99.00(17) . . ? P1 Cd1 I2 110.36(5) . . ? N1 Cd1 I1 102.18(17) . . ? P1 Cd1 I1 108.59(5) . . ? I2 Cd1 I1 116.74(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.765 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.182 #========================================================================== data_i0776 _database_code_depnum_ccdc_archive 'CCDC 805332' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Br2 Fe Hg N P' _chemical_formula_sum 'C28 H24 Br2 Fe Hg N P' _chemical_formula_weight 821.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3132(8) _cell_length_b 18.5685(17) _cell_length_c 15.3200(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.473(7) _cell_angle_gamma 90.00 _cell_volume 2641.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 218(2) _cell_measurement_reflns_used 7174 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 25.62 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.066 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 9.459 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3539 _exptl_absorpt_correction_T_max 0.7314 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 218(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 304 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 11523 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0932 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4552 _reflns_number_gt 2932 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4552 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 0.884 _refine_ls_restrained_S_all 0.884 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5091(10) 0.1355(5) 0.1457(5) 0.030(2) Uani 1 1 d . . . C2 C 0.5150(10) 0.0942(6) 0.0659(5) 0.038(2) Uani 1 1 d . . . H2A H 0.5744 0.0537 0.0573 0.046 Uiso 1 1 calc R . . C3 C 0.4132(13) 0.1266(7) 0.0024(6) 0.053(3) Uani 1 1 d . . . H3A H 0.3956 0.1111 -0.0566 0.063 Uiso 1 1 calc R . . C4 C 0.3431(12) 0.1846(6) 0.0403(6) 0.048(3) Uani 1 1 d . . . H4A H 0.2701 0.2142 0.0122 0.058 Uiso 1 1 calc R . . C5 C 0.4024(12) 0.1908(6) 0.1288(6) 0.043(3) Uani 1 1 d . . . H5A H 0.3757 0.2258 0.1699 0.051 Uiso 1 1 calc R . . C6 C 0.2237(10) 0.0298(5) 0.2056(5) 0.033(2) Uani 1 1 d . . . C7 C 0.2541(12) -0.0130(6) 0.1337(6) 0.044(3) Uani 1 1 d . . . H7A H 0.3177 -0.0531 0.1356 0.052 Uiso 1 1 calc R . . C8 C 0.1736(13) 0.0137(7) 0.0576(6) 0.048(3) Uani 1 1 d . . . H8A H 0.1722 -0.0061 0.0004 0.058 Uiso 1 1 calc R . . C9 C 0.0956(11) 0.0755(7) 0.0825(6) 0.045(3) Uani 1 1 d . . . H9A H 0.0342 0.1046 0.0448 0.054 Uiso 1 1 calc R . . C10 C 0.1269(11) 0.0856(6) 0.1749(5) 0.039(2) Uani 1 1 d . . . H10A H 0.0898 0.1227 0.2095 0.047 Uiso 1 1 calc R . . C11 C 0.2759(11) 0.0160(6) 0.3004(5) 0.036(2) Uani 1 1 d . . . H11A H 0.2650 -0.0359 0.3131 0.043 Uiso 1 1 calc R . . H11B H 0.3797 0.0278 0.3088 0.043 Uiso 1 1 calc R . . C12 C 0.1972(11) 0.0585(5) 0.3642(5) 0.034(2) Uani 1 1 d . . . C13 C 0.0601(11) 0.0384(6) 0.3854(6) 0.042(2) Uani 1 1 d . . . H13A H 0.0156 -0.0031 0.3591 0.050 Uiso 1 1 calc R . . C14 C -0.0114(11) 0.0782(7) 0.4444(6) 0.048(3) Uani 1 1 d . . . H14A H -0.1049 0.0646 0.4590 0.057 Uiso 1 1 calc R . . C15 C 0.0554(12) 0.1384(7) 0.4821(6) 0.049(3) Uani 1 1 d . . . H15A H 0.0097 0.1664 0.5238 0.059 Uiso 1 1 calc R . . C16 C 0.1902(10) 0.1568(6) 0.4576(5) 0.039(2) Uani 1 1 d . . . H16A H 0.2362 0.1982 0.4832 0.047 Uiso 1 1 calc R . . C17 C 0.7694(11) 0.1885(5) 0.2345(5) 0.033(2) Uani 1 1 d . . . C18 C 0.8464(11) 0.2168(5) 0.3087(6) 0.038(2) Uani 1 1 d . . . H18A H 0.8155 0.2073 0.3652 0.045 Uiso 1 1 calc R . . C19 C 0.9670(12) 0.2584(6) 0.3001(6) 0.042(3) Uani 1 1 d . . . H19A H 1.0195 0.2765 0.3511 0.051 Uiso 1 1 calc R . . C20 C 1.0123(12) 0.2740(6) 0.2189(6) 0.045(3) Uani 1 1 d . . . H20A H 1.0960 0.3026 0.2142 0.053 Uiso 1 1 calc R . . C21 C 0.9367(12) 0.2483(6) 0.1443(6) 0.041(2) Uani 1 1 d . . . H21A H 0.9675 0.2597 0.0883 0.050 Uiso 1 1 calc R . . C22 C 0.8152(11) 0.2057(5) 0.1514(5) 0.035(2) Uani 1 1 d . . . H22A H 0.7628 0.1881 0.1001 0.042 Uiso 1 1 calc R . . C23 C 0.6982(10) 0.0385(5) 0.2520(5) 0.030(2) Uani 1 1 d . . . C24 C 0.7884(11) 0.0169(6) 0.1911(5) 0.036(2) Uani 1 1 d . . . H24A H 0.8108 0.0490 0.1458 0.043 Uiso 1 1 calc R . . C25 C 0.8492(12) -0.0534(6) 0.1949(6) 0.042(3) Uani 1 1 d . . . H25A H 0.9126 -0.0682 0.1526 0.050 Uiso 1 1 calc R . . C26 C 0.8156(13) -0.0998(6) 0.2600(7) 0.049(3) Uani 1 1 d . . . H26A H 0.8547 -0.1471 0.2620 0.059 Uiso 1 1 calc R . . C27 C 0.7254(14) -0.0784(6) 0.3228(7) 0.053(3) Uani 1 1 d . . . H27A H 0.7030 -0.1108 0.3677 0.063 Uiso 1 1 calc R . . C28 C 0.6673(11) -0.0088(6) 0.3201(5) 0.037(2) Uani 1 1 d . . . H28A H 0.6072 0.0065 0.3639 0.045 Uiso 1 1 calc R . . N1 N 0.2585(8) 0.1190(5) 0.3996(4) 0.0347(19) Uani 1 1 d . . . P1 P 0.6190(3) 0.12832(14) 0.24638(13) 0.0284(5) Uani 1 1 d . . . Fe1 Fe 0.31139(15) 0.09126(8) 0.10801(7) 0.0334(3) Uani 1 1 d . . . Br1 Br 0.41805(15) 0.29694(6) 0.38490(7) 0.0560(3) Uani 1 1 d . . . Br2 Br 0.62380(12) 0.11815(7) 0.52228(6) 0.0533(3) Uani 1 1 d . . . Hg1 Hg 0.49150(4) 0.16168(2) 0.37385(2) 0.03640(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(5) 0.035(5) 0.036(5) 0.004(3) 0.002(4) -0.005(4) C2 0.027(6) 0.058(7) 0.031(4) -0.002(4) 0.005(4) -0.002(5) C3 0.053(8) 0.076(9) 0.029(5) 0.017(5) -0.001(4) -0.024(7) C4 0.033(6) 0.057(8) 0.054(6) 0.025(5) -0.007(5) -0.002(6) C5 0.047(7) 0.035(6) 0.046(5) 0.005(4) 0.002(4) -0.009(5) C6 0.029(5) 0.040(6) 0.032(4) 0.007(4) 0.008(4) -0.005(5) C7 0.041(7) 0.041(6) 0.050(5) -0.004(5) 0.012(5) -0.005(6) C8 0.049(7) 0.063(8) 0.033(5) -0.003(5) 0.002(4) -0.019(6) C9 0.023(5) 0.075(8) 0.035(5) 0.007(5) -0.007(4) -0.003(6) C10 0.037(6) 0.047(6) 0.033(4) -0.003(4) 0.004(4) -0.001(5) C11 0.033(6) 0.040(6) 0.034(4) 0.000(4) 0.002(4) -0.002(5) C12 0.036(6) 0.035(6) 0.031(4) 0.004(4) -0.002(4) -0.007(5) C13 0.036(6) 0.052(7) 0.038(5) 0.001(4) 0.003(4) -0.008(5) C14 0.029(6) 0.074(9) 0.041(5) 0.017(5) 0.003(4) -0.010(6) C15 0.043(7) 0.069(9) 0.038(5) 0.006(5) 0.010(4) 0.006(6) C16 0.030(5) 0.052(6) 0.034(4) -0.003(5) 0.001(4) -0.004(6) C17 0.032(6) 0.029(5) 0.036(4) -0.002(4) 0.001(4) 0.004(4) C18 0.039(6) 0.037(6) 0.035(4) 0.002(4) -0.002(4) 0.002(5) C19 0.040(6) 0.041(6) 0.045(5) -0.001(4) -0.003(4) -0.008(5) C20 0.036(7) 0.040(6) 0.058(6) 0.004(5) 0.003(5) -0.008(5) C21 0.040(6) 0.042(6) 0.043(5) 0.012(4) 0.013(4) 0.001(6) C22 0.040(6) 0.035(6) 0.029(4) 0.009(4) -0.001(4) 0.006(5) C23 0.029(5) 0.026(5) 0.034(4) -0.002(4) -0.001(4) 0.002(4) C24 0.036(6) 0.039(6) 0.032(4) 0.003(4) -0.001(4) 0.001(5) C25 0.042(7) 0.039(6) 0.044(5) -0.013(4) 0.001(4) -0.003(5) C26 0.052(7) 0.031(6) 0.061(6) -0.003(5) -0.011(5) -0.003(6) C27 0.072(9) 0.039(7) 0.046(5) 0.014(5) -0.003(5) -0.003(6) C28 0.031(6) 0.044(6) 0.036(4) 0.006(4) -0.005(4) -0.007(5) N1 0.024(4) 0.046(5) 0.035(4) -0.001(3) 0.003(3) -0.005(4) P1 0.0266(13) 0.0332(14) 0.0254(10) 0.0005(9) 0.0017(9) 0.0010(11) Fe1 0.0281(8) 0.0433(9) 0.0281(6) 0.0010(5) -0.0013(5) -0.0029(7) Br1 0.0709(9) 0.0365(6) 0.0617(6) -0.0009(5) 0.0128(5) -0.0026(6) Br2 0.0516(7) 0.0742(8) 0.0337(4) -0.0028(5) -0.0001(4) 0.0229(6) Hg1 0.0338(2) 0.0435(2) 0.03245(16) -0.00379(18) 0.00650(12) -0.0022(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 C1 C5 1.438(14) . ? C1 C2 1.447(12) . ? C1 P1 1.788(8) . ? C1 Fe1 2.057(9) . ? C2 C3 1.437(15) . ? C2 Fe1 2.050(9) . ? C3 C4 1.408(17) . ? C3 Fe1 2.046(9) . ? C4 C5 1.428(14) . ? C4 Fe1 2.054(10) . ? C5 Fe1 2.048(10) . ? C6 C7 1.405(13) . ? C6 C10 1.428(14) . ? C6 C11 1.518(11) . ? C6 Fe1 2.096(8) . ? C7 C8 1.426(15) . ? C7 Fe1 2.054(11) . ? C8 C9 1.424(16) . ? C8 Fe1 2.040(11) . ? C9 C10 1.436(12) . ? C9 Fe1 2.038(10) . ? C10 Fe1 2.071(10) . ? C11 C12 1.493(13) . ? C12 N1 1.354(12) . ? C12 C13 1.393(14) . ? C13 C14 1.379(15) . ? C14 C15 1.382(16) . ? C15 C16 1.381(14) . ? C16 N1 1.333(12) . ? C17 C18 1.398(13) . ? C17 C22 1.410(12) . ? C17 P1 1.812(10) . ? C18 C19 1.377(14) . ? C19 C20 1.376(14) . ? C20 C21 1.380(14) . ? C21 C22 1.393(14) . ? C23 C24 1.364(13) . ? C23 C28 1.410(12) . ? C23 P1 1.823(9) . ? C24 C25 1.423(14) . ? C25 C26 1.372(15) . ? C26 C27 1.385(16) . ? C27 C28 1.400(15) . ? N1 Hg1 2.372(7) . ? P1 Hg1 2.443(2) . ? Br1 Hg1 2.6120(13) . ? Br2 Hg1 2.6278(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 C5 C1 C2 107.3(8) . . ? C5 C1 P1 123.3(7) . . ? C2 C1 P1 129.2(7) . . ? C5 C1 Fe1 69.2(5) . . ? C2 C1 Fe1 69.1(5) . . ? P1 C1 Fe1 130.7(5) . . ? C3 C2 C1 106.5(10) . . ? C3 C2 Fe1 69.3(6) . . ? C1 C2 Fe1 69.6(5) . . ? C4 C3 C2 110.1(9) . . ? C4 C3 Fe1 70.2(6) . . ? C2 C3 Fe1 69.6(5) . . ? C3 C4 C5 107.2(9) . . ? C3 C4 Fe1 69.6(6) . . ? C5 C4 Fe1 69.4(6) . . ? C4 C5 C1 108.9(9) . . ? C4 C5 Fe1 69.8(6) . . ? C1 C5 Fe1 69.8(6) . . ? C7 C6 C10 108.3(8) . . ? C7 C6 C11 125.8(9) . . ? C10 C6 C11 125.7(8) . . ? C7 C6 Fe1 68.6(5) . . ? C10 C6 Fe1 69.0(5) . . ? C11 C6 Fe1 131.4(7) . . ? C6 C7 C8 108.6(10) . . ? C6 C7 Fe1 71.8(6) . . ? C8 C7 Fe1 69.1(6) . . ? C9 C8 C7 107.9(8) . . ? C9 C8 Fe1 69.5(6) . . ? C7 C8 Fe1 70.2(6) . . ? C8 C9 C10 107.5(9) . . ? C8 C9 Fe1 69.6(6) . . ? C10 C9 Fe1 70.8(5) . . ? C6 C10 C9 107.6(9) . . ? C6 C10 Fe1 70.9(5) . . ? C9 C10 Fe1 68.3(5) . . ? C12 C11 C6 113.6(8) . . ? N1 C12 C13 119.7(9) . . ? N1 C12 C11 119.2(9) . . ? C13 C12 C11 121.1(9) . . ? C14 C13 C12 120.5(10) . . ? C13 C14 C15 118.8(10) . . ? C16 C15 C14 118.5(10) . . ? N1 C16 C15 122.8(10) . . ? C18 C17 C22 118.5(9) . . ? C18 C17 P1 120.1(7) . . ? C22 C17 P1 121.4(7) . . ? C19 C18 C17 120.3(9) . . ? C20 C19 C18 120.9(9) . . ? C19 C20 C21 120.2(10) . . ? C20 C21 C22 119.8(9) . . ? C21 C22 C17 120.3(9) . . ? C24 C23 C28 119.7(9) . . ? C24 C23 P1 120.3(7) . . ? C28 C23 P1 120.0(7) . . ? C23 C24 C25 120.4(9) . . ? C26 C25 C24 119.6(10) . . ? C25 C26 C27 120.6(10) . . ? C26 C27 C28 119.9(10) . . ? C27 C28 C23 119.8(9) . . ? C16 N1 C12 119.7(8) . . ? C16 N1 Hg1 115.2(6) . . ? C12 N1 Hg1 125.0(6) . . ? C1 P1 C17 105.2(4) . . ? C1 P1 C23 108.2(4) . . ? C17 P1 C23 104.8(4) . . ? C1 P1 Hg1 112.9(3) . . ? C17 P1 Hg1 110.6(3) . . ? C23 P1 Hg1 114.5(3) . . ? C9 Fe1 C8 40.9(5) . . ? C9 Fe1 C3 113.9(4) . . ? C8 Fe1 C3 104.1(4) . . ? C9 Fe1 C5 123.3(5) . . ? C8 Fe1 C5 159.4(4) . . ? C3 Fe1 C5 67.8(4) . . ? C9 Fe1 C2 149.9(4) . . ? C8 Fe1 C2 118.0(4) . . ? C3 Fe1 C2 41.1(4) . . ? C5 Fe1 C2 69.1(4) . . ? C9 Fe1 C4 101.7(4) . . ? C8 Fe1 C4 121.0(4) . . ? C3 Fe1 C4 40.2(5) . . ? C5 Fe1 C4 40.8(4) . . ? C2 Fe1 C4 69.2(4) . . ? C9 Fe1 C7 68.6(5) . . ? C8 Fe1 C7 40.8(4) . . ? C3 Fe1 C7 126.7(5) . . ? C5 Fe1 C7 158.6(4) . . ? C2 Fe1 C7 110.2(4) . . ? C4 Fe1 C7 160.4(4) . . ? C9 Fe1 C1 163.5(4) . . ? C8 Fe1 C1 155.6(5) . . ? C3 Fe1 C1 68.5(4) . . ? C5 Fe1 C1 41.0(4) . . ? C2 Fe1 C1 41.3(3) . . ? C4 Fe1 C1 69.1(4) . . ? C7 Fe1 C1 124.2(4) . . ? C9 Fe1 C10 40.9(4) . . ? C8 Fe1 C10 68.3(4) . . ? C3 Fe1 C10 149.4(4) . . ? C5 Fe1 C10 108.5(4) . . ? C2 Fe1 C10 168.6(3) . . ? C4 Fe1 C10 116.8(4) . . ? C7 Fe1 C10 67.6(4) . . ? C1 Fe1 C10 129.8(3) . . ? C9 Fe1 C6 68.0(4) . . ? C8 Fe1 C6 67.5(4) . . ? C3 Fe1 C6 165.7(5) . . ? C5 Fe1 C6 124.0(4) . . ? C2 Fe1 C6 131.3(4) . . ? C4 Fe1 C6 154.1(4) . . ? C7 Fe1 C6 39.5(4) . . ? C1 Fe1 C6 114.0(3) . . ? C10 Fe1 C6 40.1(4) . . ? N1 Hg1 P1 123.79(18) . . ? N1 Hg1 Br1 93.6(2) . . ? P1 Hg1 Br1 116.21(6) . . ? N1 Hg1 Br2 97.27(17) . . ? P1 Hg1 Br2 112.92(6) . . ? Br1 Hg1 Br2 110.31(4) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.067 _refine_diff_density_min -1.043 _refine_diff_density_rms 0.194 #===================================================================== data_i0573 # CCDC 805333 _database_code_depnum_ccdc_archive 'CCDC 805333' #TrackingRef 'publus86_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 Br4 Fe Hg2 N P' _chemical_formula_weight 1182.12 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' Br Br -0.2901 2.4595 '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' Hg Hg -2.3894 9.2266 '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' N N 0.0061 0.0033 '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 c c n' _symmetry_Int_Tables_number 56 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 34.9720(12) _cell_length_b 9.9410(5) _cell_length_c 18.1638(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6314.8(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31703 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 25.74 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4320 _exptl_absorpt_coefficient_mu 15.286 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0059 _exptl_absorpt_correction_T_max 0.1673 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 37537 _diffrn_reflns_av_R_equivalents 0.0981 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.26 _reflns_number_total 5554 _reflns_number_gt 4561 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some residual electron densities, which have to be considered as peaks resulting from a disordered solvent molecule, after refinement did not give a chemical meaningful result. Therefor, these electron densities were removed from the Fo list using the SQUEEZE routine from PLATON. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 -0.250 0.824 92 46 ' ' 2 0.250 -0.250 0.324 92 47 ' ' 3 0.750 0.250 0.676 92 46 ' ' 4 0.750 0.250 0.176 92 47 ' ' _platon_squeeze_details ; ; _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^)+(0.0898P)^2^+24.9054P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00018(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5554 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0681 _refine_ls_R_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1360 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1317(3) 0.2893(9) 0.5976(6) 0.035(2) Uani 1 1 d . . . C2 C 0.1316(3) 0.1436(9) 0.5953(6) 0.039(2) Uani 1 1 d . . . H2A H 0.1454 0.0895 0.5614 0.047 Uiso 1 1 calc R . . C3 C 0.1074(3) 0.0953(11) 0.6517(7) 0.045(3) Uani 1 1 d . . . H3A H 0.1019 0.0039 0.6626 0.054 Uiso 1 1 calc R . . C4 C 0.0926(4) 0.2124(12) 0.6900(7) 0.050(3) Uani 1 1 d . . . H4A H 0.0756 0.2104 0.7307 0.060 Uiso 1 1 calc R . . C5 C 0.1078(3) 0.3322(11) 0.6565(7) 0.042(2) Uani 1 1 d . . . H5A H 0.1029 0.4224 0.6709 0.051 Uiso 1 1 calc R . . C6 C 0.0575(3) 0.1509(9) 0.4831(6) 0.035(2) Uani 1 1 d . . . C7 C 0.0564(3) 0.2950(9) 0.4825(7) 0.040(2) Uani 1 1 d . . . H7A H 0.0691 0.3518 0.4484 0.048 Uiso 1 1 calc R . . C8 C 0.0327(3) 0.3386(10) 0.5421(6) 0.039(2) Uani 1 1 d . . . H8A H 0.0271 0.4293 0.5546 0.047 Uiso 1 1 calc R . . C9 C 0.0191(3) 0.2220(10) 0.5795(7) 0.042(2) Uani 1 1 d . . . H9A H 0.0030 0.2209 0.6216 0.050 Uiso 1 1 calc R . . C10 C 0.0339(3) 0.1085(10) 0.5427(6) 0.037(2) Uani 1 1 d . . . H10A H 0.0288 0.0176 0.5556 0.045 Uiso 1 1 calc R . . C11 C 0.0772(3) 0.0589(10) 0.4281(6) 0.037(2) Uani 1 1 d . . . H11B H 0.1022 0.0983 0.4150 0.045 Uiso 1 1 calc R . . H11A H 0.0820 -0.0290 0.4520 0.045 Uiso 1 1 calc R . . C12 C 0.0548(3) 0.0351(9) 0.3583(6) 0.033(2) Uani 1 1 d . . . C13 C 0.0216(3) 0.1083(11) 0.3408(6) 0.044(2) Uani 1 1 d . . . H13A H 0.0129 0.1780 0.3724 0.052 Uiso 1 1 calc R . . C14 C 0.0019(3) 0.0771(11) 0.2766(7) 0.046(3) Uani 1 1 d . . . H14A H -0.0215 0.1213 0.2654 0.055 Uiso 1 1 calc R . . C15 C 0.0166(3) -0.0197(11) 0.2289(6) 0.044(3) Uani 1 1 d . . . H15A H 0.0041 -0.0409 0.1841 0.053 Uiso 1 1 calc R . . C16 C 0.0502(3) -0.0839(10) 0.2491(6) 0.040(2) Uani 1 1 d . . . H16A H 0.0602 -0.1508 0.2171 0.048 Uiso 1 1 calc R . . C17 C 0.2014(3) 0.4522(9) 0.5794(7) 0.040(2) Uani 1 1 d . . . C18 C 0.2137(3) 0.3903(12) 0.6449(8) 0.051(3) Uani 1 1 d . . . H18A H 0.1983 0.3242 0.6683 0.061 Uiso 1 1 calc R . . C19 C 0.2491(4) 0.4278(14) 0.6754(8) 0.059(3) Uani 1 1 d . . . H19A H 0.2574 0.3900 0.7208 0.071 Uiso 1 1 calc R . . C20 C 0.2718(4) 0.5200(13) 0.6389(9) 0.063(4) Uani 1 1 d . . . H20A H 0.2962 0.5429 0.6583 0.076 Uiso 1 1 calc R . . C21 C 0.2594(4) 0.5789(12) 0.5745(9) 0.061(4) Uani 1 1 d . . . H21A H 0.2752 0.6428 0.5502 0.073 Uiso 1 1 calc R . . C22 C 0.2242(4) 0.5461(11) 0.5447(8) 0.052(3) Uani 1 1 d . . . H22A H 0.2158 0.5881 0.5006 0.062 Uiso 1 1 calc R . . C23 C 0.1705(3) 0.3093(10) 0.4576(6) 0.040(2) Uani 1 1 d . . . C24 C 0.1543(3) 0.3355(16) 0.3897(8) 0.059(4) Uani 1 1 d . . . H24A H 0.1369 0.4078 0.3828 0.071 Uiso 1 1 calc R . . C25 C 0.1652(5) 0.247(2) 0.3295(8) 0.078(4) Uani 1 1 d . . . H25A H 0.1546 0.2610 0.2820 0.093 Uiso 1 1 calc R . . C26 C 0.1912(4) 0.1414(15) 0.3406(8) 0.061(3) Uani 1 1 d . . . H26A H 0.1973 0.0813 0.3017 0.073 Uiso 1 1 calc R . . C27 C 0.2072(4) 0.1270(11) 0.4077(7) 0.052(3) Uani 1 1 d . . . H27A H 0.2258 0.0583 0.4143 0.063 Uiso 1 1 calc R . . C28 C 0.1980(4) 0.2063(11) 0.4672(7) 0.046(3) Uani 1 1 d . . . H28A H 0.2098 0.1922 0.5136 0.055 Uiso 1 1 calc R . . Br1 Br 0.05994(3) 0.72934(11) 0.56077(7) 0.0482(3) Uani 1 1 d . . . Br2 Br 0.07916(4) 0.58576(10) 0.35908(7) 0.0493(3) Uani 1 1 d . . . Br3 Br 0.15266(4) 0.81443(13) 0.20405(8) 0.0563(3) Uani 1 1 d . . . Br4 Br 0.15760(3) 0.81371(10) 0.45616(7) 0.0445(3) Uani 1 1 d . . . Fe Fe 0.07785(4) 0.22248(13) 0.58095(8) 0.0326(3) Uani 1 1 d . . . Hg1 Hg 0.115070(14) 0.59491(4) 0.51803(3) 0.05572(19) Uani 1 1 d . . . Hg2 Hg 0.122392(14) 0.79848(4) 0.33037(3) 0.04732(17) Uani 1 1 d . . . P P 0.15645(8) 0.4032(2) 0.53761(17) 0.0374(6) Uani 1 1 d . . . N N 0.0696(2) -0.0566(7) 0.3119(5) 0.0334(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(5) 0.023(4) 0.053(7) -0.002(4) 0.001(4) 0.003(4) C2 0.041(6) 0.021(4) 0.056(7) 0.000(4) -0.005(5) 0.003(4) C3 0.050(6) 0.038(6) 0.047(7) 0.004(5) -0.004(5) -0.008(5) C4 0.054(7) 0.062(7) 0.034(7) -0.002(5) 0.008(5) -0.011(6) C5 0.038(6) 0.035(5) 0.054(7) -0.007(5) -0.002(5) 0.007(4) C6 0.048(6) 0.019(4) 0.038(6) -0.002(4) -0.006(4) 0.012(4) C7 0.046(6) 0.023(5) 0.051(7) 0.009(4) -0.001(5) 0.003(4) C8 0.040(6) 0.029(5) 0.049(7) -0.010(4) -0.003(5) 0.002(4) C9 0.033(5) 0.037(5) 0.057(8) -0.008(5) 0.005(5) 0.003(4) C10 0.034(5) 0.031(5) 0.048(7) -0.004(4) 0.004(4) 0.003(4) C11 0.046(6) 0.030(5) 0.036(6) -0.001(4) -0.009(4) 0.011(4) C12 0.038(5) 0.027(4) 0.034(6) 0.000(4) 0.004(4) 0.006(4) C13 0.049(6) 0.039(6) 0.043(7) -0.004(4) -0.006(5) 0.010(5) C14 0.045(6) 0.041(6) 0.052(7) 0.002(5) -0.007(5) 0.002(5) C15 0.054(7) 0.042(6) 0.036(7) -0.001(4) -0.011(5) -0.008(5) C16 0.044(6) 0.036(5) 0.040(6) 0.001(4) 0.008(5) 0.002(4) C17 0.036(5) 0.027(5) 0.058(8) -0.007(4) 0.013(5) -0.004(4) C18 0.038(6) 0.049(6) 0.067(9) -0.004(6) 0.003(5) 0.001(5) C19 0.046(7) 0.079(9) 0.052(8) -0.011(6) -0.001(6) -0.009(6) C20 0.045(7) 0.049(7) 0.095(12) -0.017(7) 0.003(7) -0.006(6) C21 0.045(7) 0.048(7) 0.090(11) 0.001(6) 0.026(7) -0.002(5) C22 0.048(7) 0.039(6) 0.068(9) -0.001(5) 0.021(6) -0.003(5) C23 0.047(6) 0.031(5) 0.043(7) 0.005(4) 0.003(5) -0.004(4) C24 0.036(6) 0.091(9) 0.050(8) 0.027(7) -0.003(5) 0.021(6) C25 0.073(10) 0.124(13) 0.037(8) -0.011(8) -0.016(6) 0.010(10) C26 0.068(9) 0.074(9) 0.042(8) -0.009(6) 0.010(6) 0.015(7) C27 0.060(7) 0.041(6) 0.057(8) -0.003(5) 0.012(6) 0.010(5) C28 0.059(7) 0.042(6) 0.037(7) 0.007(4) 0.000(5) 0.015(5) Br1 0.0507(6) 0.0391(5) 0.0549(7) 0.0047(5) 0.0077(5) 0.0162(5) Br2 0.0562(7) 0.0347(5) 0.0569(8) 0.0115(4) -0.0075(5) -0.0005(5) Br3 0.0590(7) 0.0589(7) 0.0511(8) 0.0133(5) 0.0128(5) 0.0142(6) Br4 0.0430(6) 0.0380(5) 0.0525(7) 0.0019(4) -0.0074(5) -0.0019(4) Fe 0.0347(7) 0.0253(6) 0.0378(8) -0.0024(5) 0.0013(6) -0.0019(5) Hg1 0.0445(3) 0.0294(2) 0.0933(4) 0.0073(2) 0.0127(2) 0.00953(17) Hg2 0.0519(3) 0.0462(3) 0.0438(3) 0.00334(17) 0.00172(18) 0.01134(18) P 0.0365(14) 0.0268(12) 0.0489(18) 0.0004(10) 0.0060(11) 0.0026(10) N 0.033(4) 0.021(4) 0.047(5) 0.001(3) 0.002(4) 0.000(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 C1 C5 1.423(15) . ? C1 C2 1.449(13) . ? C1 P 1.794(10) . ? C1 Fe 2.021(10) . ? C2 C3 1.412(17) . ? C2 Fe 2.053(10) . ? C2 H2A 0.9500 . ? C3 C4 1.451(17) . ? C3 Fe 2.078(12) . ? C3 H3A 0.9500 . ? C4 C5 1.439(16) . ? C4 Fe 2.050(13) . ? C4 H4A 0.9500 . ? C5 Fe 2.043(11) . ? C5 H5A 0.9500 . ? C6 C10 1.427(15) . ? C6 C7 1.433(13) . ? C6 C11 1.519(14) . ? C6 Fe 2.043(10) . ? C7 C8 1.429(16) . ? C7 Fe 2.069(11) . ? C7 H7A 0.9500 . ? C8 C9 1.426(16) . ? C8 Fe 2.078(11) . ? C8 H8A 0.9500 . ? C9 C10 1.409(14) . ? C9 Fe 2.055(11) . ? C9 H9A 0.9500 . ? C10 Fe 2.033(10) . ? C10 H10A 0.9500 . ? C11 C12 1.507(15) . ? C11 H11B 0.9900 . ? C11 H11A 0.9900 . ? C12 N 1.346(13) . ? C12 C13 1.406(15) . ? C13 C14 1.391(16) . ? C13 H13A 0.9500 . ? C14 C15 1.394(17) . ? C14 H14A 0.9500 . ? C15 C16 1.387(16) . ? C15 H15A 0.9500 . ? C16 N 1.354(15) . ? C16 H16A 0.9500 . ? C17 C22 1.380(15) . ? C17 C18 1.408(18) . ? C17 P 1.812(11) . ? C18 C19 1.408(18) . ? C18 H18A 0.9500 . ? C19 C20 1.38(2) . ? C19 H19A 0.9500 . ? C20 C21 1.38(2) . ? C20 H20A 0.9500 . ? C21 C22 1.38(2) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C24 1.381(17) . ? C23 C28 1.414(15) . ? C23 P 1.796(12) . ? C24 C25 1.45(2) . ? C24 H24A 0.9500 . ? C25 C26 1.40(2) . ? C25 H25A 0.9500 . ? C26 C27 1.349(19) . ? C26 H26A 0.9500 . ? C27 C28 1.375(17) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? Br1 Hg1 2.4710(11) . ? Br2 Hg2 2.6514(12) . ? Br2 Hg1 3.1498(14) . ? Br3 Hg2 2.5319(13) . ? Br4 Hg2 2.5999(12) . ? Br4 Hg1 2.8647(12) . ? Hg1 P 2.419(3) . ? Hg2 N 2.365(8) 1_565 ? N Hg2 2.365(8) 1_545 ? 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 C5 C1 C2 108.6(9) . . ? C5 C1 P 123.4(7) . . ? C2 C1 P 127.9(8) . . ? C5 C1 Fe 70.3(6) . . ? C2 C1 Fe 70.3(6) . . ? P C1 Fe 124.5(6) . . ? C3 C2 C1 108.7(10) . . ? C3 C2 Fe 71.0(7) . . ? C1 C2 Fe 68.0(5) . . ? C3 C2 H2A 125.7 . . ? C1 C2 H2A 125.7 . . ? Fe C2 H2A 126.9 . . ? C2 C3 C4 106.8(9) . . ? C2 C3 Fe 69.0(6) . . ? C4 C3 Fe 68.4(7) . . ? C2 C3 H3A 126.6 . . ? C4 C3 H3A 126.6 . . ? Fe C3 H3A 127.5 . . ? C5 C4 C3 109.2(10) . . ? C5 C4 Fe 69.1(7) . . ? C3 C4 Fe 70.5(7) . . ? C5 C4 H4A 125.4 . . ? C3 C4 H4A 125.4 . . ? Fe C4 H4A 126.6 . . ? C1 C5 C4 106.7(9) . . ? C1 C5 Fe 68.7(6) . . ? C4 C5 Fe 69.7(7) . . ? C1 C5 H5A 126.7 . . ? C4 C5 H5A 126.7 . . ? Fe C5 H5A 126.5 . . ? C10 C6 C7 106.5(9) . . ? C10 C6 C11 125.7(9) . . ? C7 C6 C11 127.6(10) . . ? C10 C6 Fe 69.1(6) . . ? C7 C6 Fe 70.6(6) . . ? C11 C6 Fe 128.7(7) . . ? C8 C7 C6 108.3(9) . . ? C8 C7 Fe 70.2(6) . . ? C6 C7 Fe 68.6(6) . . ? C8 C7 H7A 125.8 . . ? C6 C7 H7A 125.8 . . ? Fe C7 H7A 126.9 . . ? C9 C8 C7 107.9(9) . . ? C9 C8 Fe 68.9(6) . . ? C7 C8 Fe 69.5(6) . . ? C9 C8 H8A 126.1 . . ? C7 C8 H8A 126.1 . . ? Fe C8 H8A 127.1 . . ? C10 C9 C8 107.6(10) . . ? C10 C9 Fe 69.0(6) . . ? C8 C9 Fe 70.7(6) . . ? C10 C9 H9A 126.2 . . ? C8 C9 H9A 126.2 . . ? Fe C9 H9A 125.7 . . ? C9 C10 C6 109.6(9) . . ? C9 C10 Fe 70.7(6) . . ? C6 C10 Fe 69.9(6) . . ? C9 C10 H10A 125.2 . . ? C6 C10 H10A 125.2 . . ? Fe C10 H10A 125.9 . . ? C12 C11 C6 114.4(8) . . ? C12 C11 H11B 108.7 . . ? C6 C11 H11B 108.7 . . ? C12 C11 H11A 108.7 . . ? C6 C11 H11A 108.7 . . ? H11B C11 H11A 107.6 . . ? N C12 C13 121.8(10) . . ? N C12 C11 115.7(8) . . ? C13 C12 C11 122.5(9) . . ? C14 C13 C12 119.0(10) . . ? C14 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C13 C14 C15 119.4(11) . . ? C13 C14 H14A 120.3 . . ? C15 C14 H14A 120.3 . . ? C16 C15 C14 117.9(11) . . ? C16 C15 H15A 121.1 . . ? C14 C15 H15A 121.1 . . ? N C16 C15 123.6(10) . . ? N C16 H16A 118.2 . . ? C15 C16 H16A 118.2 . . ? C22 C17 C18 120.3(11) . . ? C22 C17 P 119.5(10) . . ? C18 C17 P 120.1(8) . . ? C19 C18 C17 119.1(12) . . ? C19 C18 H18A 120.5 . . ? C17 C18 H18A 120.5 . . ? C20 C19 C18 119.5(14) . . ? C20 C19 H19A 120.2 . . ? C18 C19 H19A 120.2 . . ? C21 C20 C19 120.5(13) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 120.8(12) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C17 C22 C21 119.7(13) . . ? C17 C22 H22A 120.2 . . ? C21 C22 H22A 120.2 . . ? C24 C23 C28 121.7(11) . . ? C24 C23 P 120.7(9) . . ? C28 C23 P 117.6(9) . . ? C23 C24 C25 116.7(12) . . ? C23 C24 H24A 121.7 . . ? C25 C24 H24A 121.7 . . ? C26 C25 C24 121.0(12) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C27 C26 C25 118.5(12) . . ? C27 C26 H26A 120.7 . . ? C25 C26 H26A 120.7 . . ? C26 C27 C28 123.5(12) . . ? C26 C27 H27A 118.3 . . ? C28 C27 H27A 118.3 . . ? C27 C28 C23 118.5(11) . . ? C27 C28 H28A 120.7 . . ? C23 C28 H28A 120.7 . . ? Hg2 Br2 Hg1 85.98(4) . . ? Hg2 Br4 Hg1 93.14(4) . . ? C1 Fe C10 160.1(4) . . ? C1 Fe C5 41.0(4) . . ? C10 Fe C5 156.3(5) . . ? C1 Fe C6 124.7(4) . . ? C10 Fe C6 41.0(4) . . ? C5 Fe C6 161.7(5) . . ? C1 Fe C4 68.7(5) . . ? C10 Fe C4 119.6(5) . . ? C5 Fe C4 41.2(5) . . ? C6 Fe C4 155.8(4) . . ? C1 Fe C2 41.7(4) . . ? C10 Fe C2 121.5(4) . . ? C5 Fe C2 69.4(4) . . ? C6 Fe C2 107.2(4) . . ? C4 Fe C2 68.2(5) . . ? C1 Fe C9 159.2(4) . . ? C10 Fe C9 40.3(4) . . ? C5 Fe C9 121.5(4) . . ? C6 Fe C9 68.9(4) . . ? C4 Fe C9 105.3(5) . . ? C2 Fe C9 156.3(4) . . ? C1 Fe C7 110.7(4) . . ? C10 Fe C7 67.9(4) . . ? C5 Fe C7 125.5(4) . . ? C6 Fe C7 40.8(4) . . ? C4 Fe C7 160.7(5) . . ? C2 Fe C7 125.1(5) . . ? C9 Fe C7 68.1(5) . . ? C1 Fe C8 125.2(4) . . ? C10 Fe C8 67.6(4) . . ? C5 Fe C8 108.7(4) . . ? C6 Fe C8 68.5(4) . . ? C4 Fe C8 123.1(5) . . ? C2 Fe C8 161.8(4) . . ? C9 Fe C8 40.4(4) . . ? C7 Fe C8 40.3(4) . . ? C1 Fe C3 69.1(4) . . ? C10 Fe C3 104.4(4) . . ? C5 Fe C3 69.7(4) . . ? C6 Fe C3 120.0(4) . . ? C4 Fe C3 41.2(5) . . ? C2 Fe C3 40.0(5) . . ? C9 Fe C3 120.3(5) . . ? C7 Fe C3 158.0(5) . . ? C8 Fe C3 157.7(5) . . ? P Hg1 Br1 147.85(8) . . ? P Hg1 Br4 110.20(7) . . ? Br1 Hg1 Br4 96.76(4) . . ? P Hg1 Br2 110.51(8) . . ? Br1 Hg1 Br2 89.57(4) . . ? Br4 Hg1 Br2 82.49(3) . . ? N Hg2 Br3 99.2(2) 1_565 . ? N Hg2 Br4 117.3(2) 1_565 . ? Br3 Hg2 Br4 126.49(5) . . ? N Hg2 Br2 93.93(19) 1_565 . ? Br3 Hg2 Br2 117.82(5) . . ? Br4 Hg2 Br2 98.26(4) . . ? C1 P C23 107.2(5) . . ? C1 P C17 109.5(5) . . ? C23 P C17 103.9(5) . . ? C1 P Hg1 107.4(3) . . ? C23 P Hg1 117.0(4) . . ? C17 P Hg1 111.6(3) . . ? C12 N C16 118.1(9) . . ? C12 N Hg2 128.6(7) . 1_545 ? C16 N Hg2 112.8(6) . 1_545 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.26 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 4.385 _refine_diff_density_min -2.254 _refine_diff_density_rms 0.258 #============================================================= #============================================================= data_i0683 _database_code_depnum_ccdc_archive 'CCDC 805334' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 Br2 Fe2 Hg N2 P2, C H Cl3' _chemical_formula_sum 'C57 H49 Br2 Cl3 Fe2 Hg N2 P2' _chemical_formula_weight 1402.38 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'I b a 2' _symmetry_Int_Tables_number 45 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, z+1/2' 'x, -y, z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' _cell_length_a 13.7805(6) _cell_length_b 40.4138(16) _cell_length_c 19.1500(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10665.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 40531 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 25.61 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5504 _exptl_absorpt_coefficient_mu 5.158 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4185 _exptl_absorpt_correction_T_max 0.5756 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 33209 _diffrn_reflns_av_R_equivalents 0.0850 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9405 _reflns_number_gt 8569 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(6) _refine_ls_number_reflns 9405 _refine_ls_number_parameters 622 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.5866(6) -0.38916(17) -0.2097(4) 0.0330(16) Uani 1 1 d . . . C2 C -0.5360(5) -0.40093(19) -0.1502(4) 0.0374(17) Uani 1 1 d . . . H2A H -0.5451 -0.3935 -0.1036 0.045 Uiso 1 1 calc R . . C3 C -0.4698(6) -0.4256(2) -0.1718(5) 0.048(2) Uani 1 1 d . . . H3A H -0.4273 -0.4376 -0.1421 0.057 Uiso 1 1 calc R . . C4 C -0.4776(6) -0.4296(2) -0.2463(5) 0.0457(19) Uani 1 1 d . . . H4A H -0.4413 -0.4443 -0.2746 0.055 Uiso 1 1 calc R . . C5 C -0.5503(5) -0.40704(19) -0.2692(4) 0.0360(16) Uani 1 1 d . . . H5A H -0.5714 -0.4043 -0.3161 0.043 Uiso 1 1 calc R . . C6 C -0.6938(6) -0.47283(19) -0.2509(5) 0.0407(17) Uani 1 1 d . . . C7 C -0.7552(5) -0.4497(2) -0.2168(5) 0.0412(18) Uani 1 1 d . . . H7A H -0.8019 -0.4360 -0.2389 0.049 Uiso 1 1 calc R . . C8 C -0.7349(6) -0.4506(3) -0.1428(5) 0.052(2) Uani 1 1 d . . . H8A H -0.7642 -0.4372 -0.1079 0.062 Uiso 1 1 calc R . . C9 C -0.6615(7) -0.4755(2) -0.1321(5) 0.056(2) Uani 1 1 d . . . H9A H -0.6342 -0.4817 -0.0885 0.067 Uiso 1 1 calc R . . C10 C -0.6377(6) -0.4889(2) -0.1968(6) 0.052(2) Uani 1 1 d . . . H10A H -0.5916 -0.5061 -0.2043 0.062 Uiso 1 1 calc R . . C11 C -0.6889(6) -0.4795(2) -0.3285(6) 0.057(2) Uani 1 1 d . . . H11A H -0.6226 -0.4872 -0.3400 0.068 Uiso 1 1 calc R . . H11B H -0.6996 -0.4584 -0.3535 0.068 Uiso 1 1 calc R . . C12 C -0.7612(6) -0.5049(2) -0.3561(5) 0.048(2) Uani 1 1 d . . . C13 C -0.8483(8) -0.5109(3) -0.3272(8) 0.098(5) Uani 1 1 d . . . H13A H -0.8674 -0.4993 -0.2864 0.117 Uiso 1 1 calc R . . C14 C -0.9106(9) -0.5341(3) -0.3566(8) 0.092(4) Uani 1 1 d . . . H14A H -0.9698 -0.5397 -0.3340 0.110 Uiso 1 1 calc R . . C15 C -0.8868(7) -0.5484(3) -0.4162(6) 0.064(3) Uani 1 1 d . . . H15A H -0.9306 -0.5627 -0.4398 0.077 Uiso 1 1 calc R . . C16 C -0.7966(9) -0.5419(3) -0.4428(7) 0.081(3) Uani 1 1 d . . . H16A H -0.7772 -0.5534 -0.4837 0.097 Uiso 1 1 calc R . . C17 C -0.7558(5) -0.3610(2) -0.1398(5) 0.0363(17) Uani 1 1 d . . . C18 C -0.8509(5) -0.3726(2) -0.1487(5) 0.0436(19) Uani 1 1 d . . . H18A H -0.8753 -0.3768 -0.1942 0.052 Uiso 1 1 calc R . . C19 C -0.9097(6) -0.3779(2) -0.0902(5) 0.051(2) Uani 1 1 d . . . H19A H -0.9735 -0.3863 -0.0962 0.061 Uiso 1 1 calc R . . C20 C -0.8762(7) -0.3711(2) -0.0245(5) 0.055(2) Uani 1 1 d . . . H20A H -0.9167 -0.3748 0.0149 0.066 Uiso 1 1 calc R . . C21 C -0.7828(9) -0.3588(3) -0.0155(5) 0.053(2) Uani 1 1 d . . . H21A H -0.7601 -0.3542 0.0303 0.064 Uiso 1 1 calc R . . C22 C -0.7231(8) -0.3532(2) -0.0713(6) 0.043(2) Uani 1 1 d . . . H22A H -0.6601 -0.3442 -0.0643 0.052 Uiso 1 1 calc R . . C23 C -0.6078(5) -0.31807(19) -0.1991(4) 0.0333(16) Uani 1 1 d . . . C24 C -0.5069(5) -0.3170(2) -0.2098(4) 0.0405(17) Uani 1 1 d . . . H24A H -0.4711 -0.3367 -0.2188 0.049 Uiso 1 1 calc R . . C25 C -0.4609(7) -0.2862(3) -0.2070(5) 0.052(2) Uani 1 1 d . . . H25A H -0.3931 -0.2849 -0.2156 0.063 Uiso 1 1 calc R . . C26 C -0.5118(7) -0.2577(2) -0.1919(5) 0.054(2) Uani 1 1 d . . . H26A H -0.4790 -0.2370 -0.1900 0.065 Uiso 1 1 calc R . . C27 C -0.6121(7) -0.2593(2) -0.1793(5) 0.049(2) Uani 1 1 d . . . H27A H -0.6476 -0.2398 -0.1681 0.059 Uiso 1 1 calc R . . C28 C -0.6585(6) -0.2894(2) -0.1835(5) 0.0433(18) Uani 1 1 d . . . H28A H -0.7265 -0.2906 -0.1755 0.052 Uiso 1 1 calc R . . C29 C -0.5797(5) -0.31701(19) -0.4484(4) 0.0326(16) Uani 1 1 d . . . C30 C -0.5247(5) -0.3062(2) -0.5092(4) 0.0365(16) Uani 1 1 d . . . H30A H -0.5337 -0.3135 -0.5559 0.044 Uiso 1 1 calc R . . C31 C -0.4551(5) -0.2828(2) -0.4858(5) 0.0403(18) Uani 1 1 d . . . H31A H -0.4083 -0.2721 -0.5144 0.048 Uiso 1 1 calc R . . C32 C -0.4669(5) -0.2779(2) -0.4124(5) 0.0434(19) Uani 1 1 d . . . H32A H -0.4298 -0.2634 -0.3839 0.052 Uiso 1 1 calc R . . C33 C -0.5435(5) -0.2985(2) -0.3898(4) 0.0389(17) Uani 1 1 d . . . H33A H -0.5672 -0.2999 -0.3433 0.047 Uiso 1 1 calc R . . C34 C -0.6711(5) -0.22959(19) -0.4177(4) 0.0376(16) Uani 1 1 d . . . C35 C -0.7359(5) -0.2520(2) -0.4511(5) 0.0419(18) Uani 1 1 d . . . H35A H -0.7865 -0.2641 -0.4293 0.050 Uiso 1 1 calc R . . C36 C -0.7107(6) -0.2529(2) -0.5246(4) 0.0439(18) Uani 1 1 d . . . H36A H -0.7415 -0.2658 -0.5597 0.053 Uiso 1 1 calc R . . C37 C -0.6311(7) -0.2309(2) -0.5344(5) 0.048(2) Uani 1 1 d . . . H37A H -0.5992 -0.2266 -0.5774 0.058 Uiso 1 1 calc R . . C38 C -0.6074(6) -0.21650(19) -0.4687(4) 0.0405(17) Uani 1 1 d . . . H38A H -0.5575 -0.2008 -0.4605 0.049 Uiso 1 1 calc R . . C39 C -0.6722(6) -0.2199(2) -0.3408(5) 0.048(2) Uani 1 1 d . . . H39A H -0.6072 -0.2238 -0.3203 0.057 Uiso 1 1 calc R . . H39B H -0.7195 -0.2338 -0.3154 0.057 Uiso 1 1 calc R . . C40 C -0.7003(5) -0.18258(18) -0.3324(5) 0.0385(14) Uani 1 1 d . . . C41 C -0.6279(4) -0.15862(18) -0.3298(5) 0.0399(15) Uani 1 1 d . . . H41A H -0.5613 -0.1646 -0.3315 0.048 Uiso 1 1 calc R . . C42 C -0.6561(6) -0.12560(19) -0.3245(5) 0.0473(18) Uani 1 1 d . . . H42A H -0.6090 -0.1085 -0.3222 0.057 Uiso 1 1 calc R . . C43 C -0.7534(6) -0.1183(2) -0.3228(6) 0.051(2) Uani 1 1 d . . . H43A H -0.7748 -0.0960 -0.3195 0.062 Uiso 1 1 calc R . . C44 C -0.8196(5) -0.1440(2) -0.3261(6) 0.052(2) Uani 1 1 d . . . H44A H -0.8867 -0.1386 -0.3252 0.063 Uiso 1 1 calc R . . C45 C -0.7502(5) -0.3434(2) -0.5200(5) 0.0331(16) Uani 1 1 d . . . C46 C -0.7180(8) -0.3505(2) -0.5877(5) 0.043(2) Uani 1 1 d . . . H46A H -0.6555 -0.3600 -0.5942 0.051 Uiso 1 1 calc R . . C47 C -0.7766(7) -0.3440(3) -0.6461(5) 0.048(2) Uani 1 1 d . . . H47A H -0.7542 -0.3490 -0.6918 0.058 Uiso 1 1 calc R . . C48 C -0.8684(6) -0.3299(2) -0.6363(4) 0.0438(18) Uani 1 1 d . . . H48A H -0.9085 -0.3251 -0.6754 0.053 Uiso 1 1 calc R . . C49 C -0.9004(6) -0.3230(2) -0.5694(5) 0.049(2) Uani 1 1 d . . . H49A H -0.9633 -0.3139 -0.5629 0.059 Uiso 1 1 calc R . . C50 C -0.8427(5) -0.3291(2) -0.5117(4) 0.0421(18) Uani 1 1 d . . . H50A H -0.8655 -0.3236 -0.4663 0.051 Uiso 1 1 calc R . . C51 C -0.6045(6) -0.3869(2) -0.4618(4) 0.0362(17) Uani 1 1 d . . . C52 C -0.6538(7) -0.4165(2) -0.4778(5) 0.0476(19) Uani 1 1 d . . . H52A H -0.7220 -0.4163 -0.4848 0.057 Uiso 1 1 calc R . . C53 C -0.6025(9) -0.4458(2) -0.4831(6) 0.063(3) Uani 1 1 d . . . H53A H -0.6355 -0.4656 -0.4952 0.075 Uiso 1 1 calc R . . C54 C -0.5026(8) -0.4464(2) -0.4710(5) 0.063(3) Uani 1 1 d . . . H54A H -0.4690 -0.4669 -0.4730 0.076 Uiso 1 1 calc R . . C55 C -0.4527(7) -0.4183(2) -0.4564(5) 0.055(2) Uani 1 1 d . . . H55A H -0.3846 -0.4192 -0.4492 0.066 Uiso 1 1 calc R . . C56 C -0.5022(6) -0.3878(2) -0.4522(5) 0.0456(19) Uani 1 1 d . . . H56A H -0.4674 -0.3680 -0.4429 0.055 Uiso 1 1 calc R . . C57 C -0.8823(9) -0.4640(4) -0.6301(9) 0.094(4) Uani 1 1 d . . . H57A H -0.8593 -0.4862 -0.6464 0.113 Uiso 1 1 calc R . . N1 N -0.7329(6) -0.5200(3) -0.4146(5) 0.069(2) Uani 1 1 d . . . N2 N -0.7947(4) -0.17533(16) -0.3303(4) 0.0423(13) Uani 1 1 d . . . P1 P -0.67596(15) -0.35646(5) -0.21480(11) 0.0292(4) Uani 1 1 d . . . P2 P -0.67063(15) -0.34835(5) -0.44568(11) 0.0297(4) Uani 1 1 d . . . Cl1 Cl -0.7981(3) -0.43377(13) -0.6555(3) 0.1310(17) Uani 1 1 d . . . Cl2 Cl -0.8894(5) -0.4642(3) -0.5399(4) 0.208(4) Uani 1 1 d . . . Cl3 Cl -0.9962(3) -0.45552(12) -0.6679(3) 0.1303(18) Uani 1 1 d . . . Fe1 Fe -0.61071(8) -0.43862(3) -0.19797(6) 0.0353(2) Uani 1 1 d . . . Fe2 Fe -0.59425(7) -0.26714(3) -0.46459(6) 0.0316(2) Uani 1 1 d . . . Br1 Br -0.87308(5) -0.30060(2) -0.30595(5) 0.04448(19) Uani 1 1 d . . . Br2 Br -0.88444(6) -0.40060(2) -0.35953(5) 0.0494(2) Uani 1 1 d . . . Hg1 Hg -0.758810(14) -0.352331(6) -0.33120(2) 0.03229(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.040(4) 0.021(3) 0.038(4) -0.003(3) -0.003(3) 0.000(3) C2 0.037(4) 0.037(4) 0.037(4) 0.002(3) -0.009(3) -0.001(3) C3 0.040(4) 0.050(5) 0.053(5) 0.000(4) -0.011(4) 0.008(4) C4 0.038(4) 0.045(5) 0.054(5) -0.004(4) 0.006(4) 0.007(3) C5 0.037(3) 0.039(4) 0.033(4) 0.003(3) 0.009(3) -0.002(3) C6 0.043(4) 0.032(4) 0.046(5) 0.001(3) 0.002(3) -0.005(3) C7 0.033(3) 0.040(4) 0.050(5) 0.001(4) 0.002(3) -0.002(3) C8 0.048(5) 0.062(6) 0.044(5) -0.005(4) 0.014(4) -0.008(4) C9 0.073(6) 0.052(5) 0.043(5) 0.013(4) -0.006(4) -0.014(5) C10 0.047(4) 0.033(4) 0.076(6) -0.001(4) 0.003(4) 0.002(3) C11 0.061(4) 0.058(5) 0.050(5) -0.012(5) 0.010(5) -0.013(4) C12 0.049(4) 0.050(5) 0.047(4) -0.012(4) -0.001(4) -0.001(3) C13 0.073(6) 0.121(10) 0.099(9) -0.059(9) 0.037(7) -0.052(7) C14 0.075(7) 0.082(8) 0.118(11) -0.044(8) 0.020(7) -0.028(6) C15 0.064(6) 0.059(6) 0.069(7) -0.014(5) -0.015(5) -0.009(5) C16 0.081(7) 0.092(8) 0.071(8) -0.035(7) -0.005(6) -0.008(7) C17 0.035(4) 0.031(4) 0.043(5) 0.004(4) 0.008(3) 0.000(3) C18 0.036(4) 0.042(4) 0.052(5) -0.009(4) 0.009(4) -0.001(3) C19 0.044(4) 0.048(5) 0.060(6) -0.001(4) 0.019(4) -0.002(4) C20 0.063(5) 0.055(5) 0.049(5) 0.012(4) 0.023(4) 0.011(4) C21 0.074(6) 0.055(5) 0.031(5) 0.003(4) 0.006(5) 0.017(5) C22 0.045(5) 0.047(6) 0.037(6) -0.001(3) 0.004(4) -0.001(3) C23 0.040(4) 0.040(4) 0.020(3) -0.003(3) 0.002(3) -0.002(3) C24 0.035(4) 0.051(4) 0.036(4) -0.001(4) -0.002(3) -0.001(3) C25 0.053(5) 0.075(7) 0.029(4) 0.004(5) -0.002(4) -0.027(5) C26 0.081(6) 0.048(5) 0.033(4) -0.002(4) -0.005(4) -0.020(5) C27 0.079(6) 0.032(4) 0.038(5) -0.001(4) 0.008(4) 0.000(4) C28 0.045(4) 0.040(4) 0.044(5) -0.004(4) -0.002(4) -0.001(3) C29 0.032(4) 0.039(4) 0.027(4) 0.000(3) -0.002(3) 0.007(3) C30 0.030(3) 0.045(4) 0.035(4) -0.002(3) 0.005(3) 0.004(3) C31 0.026(3) 0.049(4) 0.046(5) -0.003(4) 0.003(3) -0.003(3) C32 0.034(4) 0.047(4) 0.049(5) 0.004(4) -0.013(3) -0.004(3) C33 0.033(3) 0.047(4) 0.037(4) -0.002(3) -0.004(3) 0.002(3) C34 0.040(4) 0.040(4) 0.032(4) 0.003(3) 0.004(3) 0.004(3) C35 0.031(3) 0.045(4) 0.049(5) 0.006(4) 0.001(3) 0.010(3) C36 0.050(4) 0.048(5) 0.033(4) -0.002(4) -0.012(3) 0.011(4) C37 0.061(5) 0.050(5) 0.033(4) 0.006(4) 0.003(4) 0.012(4) C38 0.055(4) 0.032(4) 0.035(4) 0.006(3) 0.006(4) -0.005(3) C39 0.057(4) 0.052(4) 0.034(5) 0.002(4) 0.003(4) 0.014(3) C40 0.044(3) 0.047(4) 0.025(3) 0.002(4) -0.002(4) 0.003(3) C41 0.032(3) 0.051(4) 0.037(3) 0.007(5) 0.002(4) -0.001(3) C42 0.059(4) 0.040(4) 0.043(5) -0.002(4) 0.004(4) -0.002(3) C43 0.069(5) 0.046(4) 0.040(6) 0.003(4) 0.010(4) 0.012(4) C44 0.042(3) 0.077(6) 0.038(4) -0.002(5) 0.007(5) 0.020(4) C45 0.028(3) 0.035(4) 0.037(4) -0.003(4) -0.004(3) -0.004(3) C46 0.040(4) 0.063(6) 0.025(5) -0.001(4) -0.002(4) 0.008(4) C47 0.047(5) 0.067(6) 0.031(4) -0.001(5) 0.002(4) 0.002(4) C48 0.040(4) 0.055(5) 0.037(4) 0.006(4) -0.005(3) 0.001(3) C49 0.040(4) 0.065(6) 0.042(5) -0.003(4) -0.007(4) 0.009(4) C50 0.035(4) 0.056(5) 0.035(4) -0.004(4) 0.005(3) -0.001(3) C51 0.036(4) 0.041(4) 0.031(4) 0.003(4) 0.005(3) 0.010(3) C52 0.057(5) 0.044(5) 0.042(5) 0.001(4) 0.008(4) 0.003(4) C53 0.103(8) 0.031(4) 0.054(6) -0.001(4) 0.022(6) -0.001(5) C54 0.082(7) 0.052(6) 0.055(6) 0.008(5) 0.020(5) 0.032(5) C55 0.057(5) 0.055(6) 0.054(6) 0.010(5) 0.007(4) 0.024(4) C56 0.046(4) 0.049(4) 0.041(4) 0.006(4) 0.006(4) 0.012(4) C57 0.062(6) 0.077(8) 0.143(14) -0.008(9) -0.014(7) 0.001(6) N1 0.060(5) 0.087(6) 0.059(5) -0.023(5) 0.004(4) -0.019(4) N2 0.036(3) 0.054(4) 0.037(3) -0.003(4) -0.003(4) 0.000(3) P1 0.0303(9) 0.0298(9) 0.0275(11) -0.0020(7) -0.0005(8) 0.0000(7) P2 0.0290(9) 0.0337(9) 0.0265(10) 0.0003(7) -0.0004(8) 0.0001(7) Cl1 0.112(3) 0.129(4) 0.152(4) 0.023(3) -0.023(3) -0.052(3) Cl2 0.133(4) 0.362(12) 0.129(5) 0.049(6) -0.010(4) -0.070(6) Cl3 0.0707(19) 0.124(3) 0.196(5) -0.046(4) -0.041(3) 0.023(2) Fe1 0.0380(5) 0.0340(5) 0.0339(6) 0.0016(5) -0.0010(4) 0.0025(4) Fe2 0.0275(5) 0.0370(6) 0.0303(5) 0.0001(5) 0.0003(4) -0.0011(4) Br1 0.0381(3) 0.0444(4) 0.0510(4) -0.0025(3) 0.0032(3) 0.0098(3) Br2 0.0414(4) 0.0511(5) 0.0558(5) -0.0037(4) -0.0051(4) -0.0125(3) Hg1 0.03007(11) 0.03771(13) 0.02910(12) -0.00172(13) 0.00006(17) 0.00093(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.419(11) . ? C1 C5 1.439(11) . ? C1 P1 1.809(8) . ? C1 Fe1 2.038(7) . ? C2 C3 1.413(12) . ? C2 Fe1 2.053(8) . ? C2 H2A 0.9500 . ? C3 C4 1.439(14) . ? C3 Fe1 2.073(8) . ? C3 H3A 0.9500 . ? C4 C5 1.423(11) . ? C4 Fe1 2.086(8) . ? C4 H4A 0.9500 . ? C5 Fe1 2.045(7) . ? C5 H5A 0.9500 . ? C6 C7 1.420(12) . ? C6 C10 1.448(13) . ? C6 C11 1.511(15) . ? C6 Fe1 2.062(8) . ? C7 C8 1.444(14) . ? C7 Fe1 2.073(8) . ? C7 H7A 0.9500 . ? C8 C9 1.442(14) . ? C8 Fe1 2.068(8) . ? C8 H8A 0.9500 . ? C9 C10 1.391(14) . ? C9 Fe1 2.074(9) . ? C9 H9A 0.9500 . ? C10 Fe1 2.068(8) . ? C10 H10A 0.9500 . ? C11 C12 1.523(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N1 1.336(13) . ? C12 C13 1.344(13) . ? C13 C14 1.390(15) . ? C13 H13A 0.9500 . ? C14 C15 1.322(17) . ? C14 H14A 0.9500 . ? C15 C16 1.369(17) . ? C15 H15A 0.9500 . ? C16 N1 1.357(14) . ? C16 H16A 0.9500 . ? C17 C18 1.401(11) . ? C17 C22 1.422(15) . ? C17 P1 1.819(9) . ? C18 C19 1.398(12) . ? C18 H18A 0.9500 . ? C19 C20 1.369(15) . ? C19 H19A 0.9500 . ? C20 C21 1.389(16) . ? C20 H20A 0.9500 . ? C21 C22 1.368(16) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C28 1.385(11) . ? C23 C24 1.407(11) . ? C23 P1 1.838(8) . ? C24 C25 1.398(12) . ? C24 H24A 0.9500 . ? C25 C26 1.381(14) . ? C25 H25A 0.9500 . ? C26 C27 1.405(14) . ? C26 H26A 0.9500 . ? C27 C28 1.378(12) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C33 1.438(11) . ? C29 C30 1.455(11) . ? C29 P2 1.782(8) . ? C29 Fe2 2.049(8) . ? C30 C31 1.419(11) . ? C30 Fe2 2.035(8) . ? C30 H30A 0.9500 . ? C31 C32 1.428(13) . ? C31 Fe2 2.060(7) . ? C31 H31A 0.9500 . ? C32 C33 1.412(11) . ? C32 Fe2 2.066(8) . ? C32 H32A 0.9500 . ? C33 Fe2 2.037(8) . ? C33 H33A 0.9500 . ? C34 C38 1.415(11) . ? C34 C35 1.424(12) . ? C34 C39 1.524(12) . ? C34 Fe2 2.057(8) . ? C35 C36 1.451(12) . ? C35 Fe2 2.062(7) . ? C35 H35A 0.9500 . ? C36 C37 1.424(13) . ? C36 Fe2 2.056(8) . ? C36 H36A 0.9500 . ? C37 C38 1.424(13) . ? C37 Fe2 2.047(9) . ? C37 H37A 0.9500 . ? C38 Fe2 2.056(8) . ? C38 H38A 0.9500 . ? C39 C40 1.565(11) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N2 1.334(9) . ? C40 C41 1.391(10) . ? C41 C42 1.394(11) . ? C41 H41A 0.9500 . ? C42 C43 1.372(11) . ? C42 H42A 0.9500 . ? C43 C44 1.382(13) . ? C43 H43A 0.9500 . ? C44 N2 1.316(11) . ? C44 H44A 0.9500 . ? C45 C46 1.400(13) . ? C45 C50 1.408(11) . ? C45 P2 1.807(8) . ? C46 C47 1.406(14) . ? C46 H46A 0.9500 . ? C47 C48 1.400(13) . ? C47 H47A 0.9500 . ? C48 C49 1.384(13) . ? C48 H48A 0.9500 . ? C49 C50 1.384(12) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C52 1.408(13) . ? C51 C56 1.422(12) . ? C51 P2 1.831(8) . ? C52 C53 1.384(13) . ? C52 H52A 0.9500 . ? C53 C54 1.395(16) . ? C53 H53A 0.9500 . ? C54 C55 1.358(15) . ? C54 H54A 0.9500 . ? C55 C56 1.412(12) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 Cl2 1.730(19) . ? C57 Cl1 1.754(14) . ? C57 Cl3 1.762(13) . ? C57 H57A 1.0000 . ? P1 Hg1 2.510(2) . ? P2 Hg1 2.512(2) . ? Br1 Hg1 2.6615(8) . ? Br2 Hg1 2.6640(8) . ? 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 C2 C1 C5 107.3(7) . . ? C2 C1 P1 128.5(6) . . ? C5 C1 P1 124.1(6) . . ? C2 C1 Fe1 70.3(4) . . ? C5 C1 Fe1 69.6(4) . . ? P1 C1 Fe1 127.7(4) . . ? C3 C2 C1 108.5(8) . . ? C3 C2 Fe1 70.7(5) . . ? C1 C2 Fe1 69.1(4) . . ? C3 C2 H2A 125.7 . . ? C1 C2 H2A 125.7 . . ? Fe1 C2 H2A 126.0 . . ? C2 C3 C4 108.7(7) . . ? C2 C3 Fe1 69.2(4) . . ? C4 C3 Fe1 70.3(5) . . ? C2 C3 H3A 125.6 . . ? C4 C3 H3A 125.6 . . ? Fe1 C3 H3A 126.4 . . ? C5 C4 C3 106.7(7) . . ? C5 C4 Fe1 68.3(4) . . ? C3 C4 Fe1 69.2(5) . . ? C5 C4 H4A 126.7 . . ? C3 C4 H4A 126.7 . . ? Fe1 C4 H4A 127.3 . . ? C4 C5 C1 108.8(7) . . ? C4 C5 Fe1 71.4(5) . . ? C1 C5 Fe1 69.1(4) . . ? C4 C5 H5A 125.6 . . ? C1 C5 H5A 125.6 . . ? Fe1 C5 H5A 125.4 . . ? C7 C6 C10 106.5(8) . . ? C7 C6 C11 126.6(8) . . ? C10 C6 C11 126.8(8) . . ? C7 C6 Fe1 70.3(5) . . ? C10 C6 Fe1 69.7(5) . . ? C11 C6 Fe1 125.4(6) . . ? C6 C7 C8 108.7(8) . . ? C6 C7 Fe1 69.5(4) . . ? C8 C7 Fe1 69.4(5) . . ? C6 C7 H7A 125.7 . . ? C8 C7 H7A 125.7 . . ? Fe1 C7 H7A 127.0 . . ? C9 C8 C7 106.9(8) . . ? C9 C8 Fe1 69.9(5) . . ? C7 C8 Fe1 69.8(5) . . ? C9 C8 H8A 126.5 . . ? C7 C8 H8A 126.5 . . ? Fe1 C8 H8A 125.4 . . ? C10 C9 C8 108.2(8) . . ? C10 C9 Fe1 70.1(5) . . ? C8 C9 Fe1 69.4(5) . . ? C10 C9 H9A 125.9 . . ? C8 C9 H9A 125.9 . . ? Fe1 C9 H9A 126.2 . . ? C9 C10 C6 109.6(8) . . ? C9 C10 Fe1 70.6(5) . . ? C6 C10 Fe1 69.3(5) . . ? C9 C10 H10A 125.2 . . ? C6 C10 H10A 125.2 . . ? Fe1 C10 H10A 126.5 . . ? C6 C11 C12 115.6(8) . . ? C6 C11 H11A 108.4 . . ? C12 C11 H11A 108.4 . . ? C6 C11 H11B 108.4 . . ? C12 C11 H11B 108.4 . . ? H11A C11 H11B 107.4 . . ? N1 C12 C13 121.5(9) . . ? N1 C12 C11 114.1(8) . . ? C13 C12 C11 124.3(9) . . ? C12 C13 C14 120.6(12) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 119.4(11) . . ? C15 C14 H14A 120.3 . . ? C13 C14 H14A 120.3 . . ? C14 C15 C16 117.6(10) . . ? C14 C15 H15A 121.2 . . ? C16 C15 H15A 121.2 . . ? N1 C16 C15 124.4(11) . . ? N1 C16 H16A 117.8 . . ? C15 C16 H16A 117.8 . . ? C18 C17 C22 118.9(8) . . ? C18 C17 P1 120.2(7) . . ? C22 C17 P1 120.9(6) . . ? C19 C18 C17 119.7(9) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? C20 C19 C18 120.7(8) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C19 C20 C21 119.9(9) . . ? C19 C20 H20A 120.1 . . ? C21 C20 H20A 120.1 . . ? C22 C21 C20 121.3(10) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C17 119.5(10) . . ? C21 C22 H22A 120.3 . . ? C17 C22 H22A 120.3 . . ? C28 C23 C24 120.3(8) . . ? C28 C23 P1 118.9(6) . . ? C24 C23 P1 120.4(6) . . ? C25 C24 C23 118.0(8) . . ? C25 C24 H24A 121.0 . . ? C23 C24 H24A 121.0 . . ? C26 C25 C24 121.5(8) . . ? C26 C25 H25A 119.3 . . ? C24 C25 H25A 119.3 . . ? C25 C26 C27 119.8(8) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C28 C27 C26 119.2(9) . . ? C28 C27 H27A 120.4 . . ? C26 C27 H27A 120.4 . . ? C27 C28 C23 121.2(8) . . ? C27 C28 H28A 119.4 . . ? C23 C28 H28A 119.4 . . ? C33 C29 C30 106.7(7) . . ? C33 C29 P2 126.2(6) . . ? C30 C29 P2 127.1(6) . . ? C33 C29 Fe2 69.0(4) . . ? C30 C29 Fe2 68.6(4) . . ? P2 C29 Fe2 129.4(4) . . ? C31 C30 C29 107.4(7) . . ? C31 C30 Fe2 70.7(5) . . ? C29 C30 Fe2 69.6(4) . . ? C31 C30 H30A 126.3 . . ? C29 C30 H30A 126.3 . . ? Fe2 C30 H30A 125.0 . . ? C30 C31 C32 108.9(7) . . ? C30 C31 Fe2 68.8(4) . . ? C32 C31 Fe2 70.0(4) . . ? C30 C31 H31A 125.5 . . ? C32 C31 H31A 125.5 . . ? Fe2 C31 H31A 127.3 . . ? C33 C32 C31 107.8(7) . . ? C33 C32 Fe2 68.8(4) . . ? C31 C32 Fe2 69.5(4) . . ? C33 C32 H32A 126.1 . . ? C31 C32 H32A 126.1 . . ? Fe2 C32 H32A 127.2 . . ? C32 C33 C29 109.0(7) . . ? C32 C33 Fe2 71.0(5) . . ? C29 C33 Fe2 69.8(4) . . ? C32 C33 H33A 125.5 . . ? C29 C33 H33A 125.5 . . ? Fe2 C33 H33A 125.3 . . ? C38 C34 C35 108.5(7) . . ? C38 C34 C39 125.2(7) . . ? C35 C34 C39 126.3(7) . . ? C38 C34 Fe2 69.9(4) . . ? C35 C34 Fe2 70.0(4) . . ? C39 C34 Fe2 128.0(5) . . ? C34 C35 C36 107.6(7) . . ? C34 C35 Fe2 69.6(4) . . ? C36 C35 Fe2 69.1(4) . . ? C34 C35 H35A 126.2 . . ? C36 C35 H35A 126.2 . . ? Fe2 C35 H35A 126.6 . . ? C37 C36 C35 107.2(8) . . ? C37 C36 Fe2 69.4(5) . . ? C35 C36 Fe2 69.6(4) . . ? C37 C36 H36A 126.4 . . ? C35 C36 H36A 126.4 . . ? Fe2 C36 H36A 126.2 . . ? C38 C37 C36 108.4(7) . . ? C38 C37 Fe2 70.0(5) . . ? C36 C37 Fe2 70.0(5) . . ? C38 C37 H37A 125.8 . . ? C36 C37 H37A 125.8 . . ? Fe2 C37 H37A 125.7 . . ? C34 C38 C37 108.3(7) . . ? C34 C38 Fe2 69.9(4) . . ? C37 C38 Fe2 69.3(5) . . ? C34 C38 H38A 125.8 . . ? C37 C38 H38A 125.8 . . ? Fe2 C38 H38A 126.5 . . ? C34 C39 C40 110.4(7) . . ? C34 C39 H39A 109.6 . . ? C40 C39 H39A 109.6 . . ? C34 C39 H39B 109.6 . . ? C40 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? N2 C40 C41 123.0(7) . . ? N2 C40 C39 117.1(7) . . ? C41 C40 C39 119.8(6) . . ? C40 C41 C42 118.0(6) . . ? C40 C41 H41A 121.0 . . ? C42 C41 H41A 121.0 . . ? C43 C42 C41 118.7(8) . . ? C43 C42 H42A 120.7 . . ? C41 C42 H42A 120.7 . . ? C42 C43 C44 118.8(8) . . ? C42 C43 H43A 120.6 . . ? C44 C43 H43A 120.6 . . ? N2 C44 C43 123.6(7) . . ? N2 C44 H44A 118.2 . . ? C43 C44 H44A 118.2 . . ? C46 C45 C50 118.4(8) . . ? C46 C45 P2 120.9(6) . . ? C50 C45 P2 120.4(6) . . ? C45 C46 C47 121.0(9) . . ? C45 C46 H46A 119.5 . . ? C47 C46 H46A 119.5 . . ? C48 C47 C46 119.4(9) . . ? C48 C47 H47A 120.3 . . ? C46 C47 H47A 120.3 . . ? C49 C48 C47 119.6(8) . . ? C49 C48 H48A 120.2 . . ? C47 C48 H48A 120.2 . . ? C48 C49 C50 121.3(8) . . ? C48 C49 H49A 119.3 . . ? C50 C49 H49A 119.3 . . ? C49 C50 C45 120.3(8) . . ? C49 C50 H50A 119.9 . . ? C45 C50 H50A 119.9 . . ? C52 C51 C56 119.0(8) . . ? C52 C51 P2 121.3(6) . . ? C56 C51 P2 119.5(7) . . ? C53 C52 C51 119.8(9) . . ? C53 C52 H52A 120.1 . . ? C51 C52 H52A 120.1 . . ? C52 C53 C54 120.4(10) . . ? C52 C53 H53A 119.8 . . ? C54 C53 H53A 119.8 . . ? C55 C54 C53 121.2(8) . . ? C55 C54 H54A 119.4 . . ? C53 C54 H54A 119.4 . . ? C54 C55 C56 120.0(9) . . ? C54 C55 H55A 120.0 . . ? C56 C55 H55A 120.0 . . ? C55 C56 C51 119.5(9) . . ? C55 C56 H56A 120.2 . . ? C51 C56 H56A 120.2 . . ? Cl2 C57 Cl1 108.6(8) . . ? Cl2 C57 Cl3 111.1(9) . . ? Cl1 C57 Cl3 109.9(9) . . ? Cl2 C57 H57A 109.1 . . ? Cl1 C57 H57A 109.1 . . ? Cl3 C57 H57A 109.1 . . ? C12 N1 C16 116.3(9) . . ? C44 N2 C40 117.9(7) . . ? C1 P1 C17 107.2(4) . . ? C1 P1 C23 105.1(4) . . ? C17 P1 C23 105.4(4) . . ? C1 P1 Hg1 113.9(3) . . ? C17 P1 Hg1 115.6(3) . . ? C23 P1 Hg1 108.8(3) . . ? C29 P2 C45 108.9(4) . . ? C29 P2 C51 104.5(4) . . ? C45 P2 C51 105.3(4) . . ? C29 P2 Hg1 114.3(3) . . ? C45 P2 Hg1 113.6(3) . . ? C51 P2 Hg1 109.5(3) . . ? C1 Fe1 C5 41.3(3) . . ? C1 Fe1 C2 40.6(3) . . ? C5 Fe1 C2 68.3(3) . . ? C1 Fe1 C6 133.9(3) . . ? C5 Fe1 C6 108.4(3) . . ? C2 Fe1 C6 174.2(3) . . ? C1 Fe1 C8 114.8(4) . . ? C5 Fe1 C8 145.4(4) . . ? C2 Fe1 C8 111.1(4) . . ? C6 Fe1 C8 68.6(4) . . ? C1 Fe1 C10 174.2(4) . . ? C5 Fe1 C10 134.0(4) . . ? C2 Fe1 C10 144.6(4) . . ? C6 Fe1 C10 41.0(4) . . ? C8 Fe1 C10 67.4(4) . . ? C1 Fe1 C7 110.5(3) . . ? C5 Fe1 C7 114.2(3) . . ? C2 Fe1 C7 136.0(3) . . ? C6 Fe1 C7 40.2(3) . . ? C8 Fe1 C7 40.8(4) . . ? C10 Fe1 C7 67.4(3) . . ? C1 Fe1 C3 68.0(3) . . ? C5 Fe1 C3 67.8(4) . . ? C2 Fe1 C3 40.1(3) . . ? C6 Fe1 C3 144.0(3) . . ? C8 Fe1 C3 135.3(4) . . ? C10 Fe1 C3 114.6(4) . . ? C7 Fe1 C3 175.3(4) . . ? C1 Fe1 C9 145.8(4) . . ? C5 Fe1 C9 172.5(4) . . ? C2 Fe1 C9 115.6(4) . . ? C6 Fe1 C9 68.2(4) . . ? C8 Fe1 C9 40.7(4) . . ? C10 Fe1 C9 39.2(4) . . ? C7 Fe1 C9 68.0(4) . . ? C3 Fe1 C9 110.6(4) . . ? C1 Fe1 C4 68.7(3) . . ? C5 Fe1 C4 40.3(3) . . ? C2 Fe1 C4 68.1(3) . . ? C6 Fe1 C4 112.8(3) . . ? C8 Fe1 C4 174.1(4) . . ? C10 Fe1 C4 109.6(3) . . ? C7 Fe1 C4 143.6(4) . . ? C3 Fe1 C4 40.5(4) . . ? C9 Fe1 C4 133.8(4) . . ? C30 Fe2 C33 69.5(3) . . ? C30 Fe2 C37 113.5(3) . . ? C33 Fe2 C37 171.8(3) . . ? C30 Fe2 C29 41.7(3) . . ? C33 Fe2 C29 41.2(3) . . ? C37 Fe2 C29 145.8(3) . . ? C30 Fe2 C36 110.5(3) . . ? C33 Fe2 C36 146.7(3) . . ? C37 Fe2 C36 40.6(4) . . ? C29 Fe2 C36 115.8(3) . . ? C30 Fe2 C38 142.9(3) . . ? C33 Fe2 C38 132.6(3) . . ? C37 Fe2 C38 40.6(4) . . ? C29 Fe2 C38 173.5(3) . . ? C36 Fe2 C38 68.4(3) . . ? C30 Fe2 C34 176.5(3) . . ? C33 Fe2 C34 109.2(3) . . ? C37 Fe2 C34 68.2(3) . . ? C29 Fe2 C34 135.3(3) . . ? C36 Fe2 C34 68.7(3) . . ? C38 Fe2 C34 40.2(3) . . ? C30 Fe2 C31 40.6(3) . . ? C33 Fe2 C31 68.1(3) . . ? C37 Fe2 C31 108.8(4) . . ? C29 Fe2 C31 68.7(3) . . ? C36 Fe2 C31 134.6(4) . . ? C38 Fe2 C31 112.4(3) . . ? C34 Fe2 C31 142.4(3) . . ? C30 Fe2 C35 136.8(3) . . ? C33 Fe2 C35 115.0(3) . . ? C37 Fe2 C35 68.5(4) . . ? C29 Fe2 C35 111.5(3) . . ? C36 Fe2 C35 41.2(3) . . ? C38 Fe2 C35 68.0(3) . . ? C34 Fe2 C35 40.4(3) . . ? C31 Fe2 C35 175.7(4) . . ? C30 Fe2 C32 68.8(3) . . ? C33 Fe2 C32 40.2(3) . . ? C37 Fe2 C32 132.7(4) . . ? C29 Fe2 C32 68.6(3) . . ? C36 Fe2 C32 172.9(4) . . ? C38 Fe2 C32 107.7(3) . . ? C34 Fe2 C32 112.5(3) . . ? C31 Fe2 C32 40.5(4) . . ? C35 Fe2 C32 143.8(4) . . ? P1 Hg1 P2 124.01(5) . . ? P1 Hg1 Br1 99.21(5) . . ? P2 Hg1 Br1 113.23(5) . . ? P1 Hg1 Br2 115.33(5) . . ? P2 Hg1 Br2 100.58(5) . . ? Br1 Hg1 Br2 103.16(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.009 _refine_diff_density_min -1.340 _refine_diff_density_rms 0.161 #====================================================================== data_i0818 _database_code_depnum_ccdc_archive 'CCDC 805335' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H22 Br2 Fe N P Zn' _chemical_formula_sum 'C27 H22 Br2 Fe N P Zn' _chemical_formula_weight 672.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3284(10) _cell_length_b 9.0578(6) _cell_length_c 18.4976(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.220(5) _cell_angle_gamma 90.00 _cell_volume 2553.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11946 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 25.66 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 4.716 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5464 _exptl_absorpt_correction_T_max 0.6663 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 16069 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4461 _reflns_number_gt 3378 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4461 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6518(3) 0.3105(5) 0.1737(3) 0.0230(10) Uani 1 1 d . . . C2 C 0.6360(3) 0.2789(5) 0.2476(3) 0.0263(11) Uani 1 1 d . . . H2A H 0.6677 0.2105 0.2793 0.032 Uiso 1 1 calc R . . C3 C 0.5646(3) 0.3682(6) 0.2647(3) 0.0303(11) Uani 1 1 d . . . H3A H 0.5405 0.3699 0.3099 0.036 Uiso 1 1 calc R . . C4 C 0.5351(3) 0.4552(6) 0.2021(3) 0.0310(12) Uani 1 1 d . . . H4A H 0.4882 0.5243 0.1987 0.037 Uiso 1 1 calc R . . C5 C 0.5880(3) 0.4205(5) 0.1458(3) 0.0266(11) Uani 1 1 d . . . H5A H 0.5826 0.4621 0.0984 0.032 Uiso 1 1 calc R . . C6 C 0.7728(3) 0.5575(5) 0.3084(3) 0.0238(10) Uani 1 1 d . . . C7 C 0.6960(3) 0.6392(5) 0.3218(3) 0.0291(11) Uani 1 1 d . . . H7A H 0.6690 0.6395 0.3657 0.035 Uiso 1 1 calc R . . C8 C 0.6677(4) 0.7204(5) 0.2570(3) 0.0324(12) Uani 1 1 d . . . H8A H 0.6187 0.7851 0.2506 0.039 Uiso 1 1 calc R . . C9 C 0.7257(3) 0.6875(5) 0.2036(3) 0.0304(11) Uani 1 1 d . . . H9A H 0.7217 0.7260 0.1556 0.037 Uiso 1 1 calc R . . C10 C 0.7902(3) 0.5870(5) 0.2350(3) 0.0242(10) Uani 1 1 d . . . H10A H 0.8368 0.5463 0.2115 0.029 Uiso 1 1 calc R . . C11 C 0.8266(3) 0.4614(5) 0.3618(3) 0.0222(10) Uani 1 1 d . . . C12 C 0.9182(3) 0.4716(5) 0.3706(3) 0.0291(11) Uani 1 1 d . . . H12A H 0.9474 0.5384 0.3418 0.035 Uiso 1 1 calc R . . C13 C 0.9661(3) 0.3825(6) 0.4221(3) 0.0311(12) Uani 1 1 d . . . H13A H 1.0283 0.3881 0.4285 0.037 Uiso 1 1 calc R . . C14 C 0.9224(3) 0.2859(6) 0.4638(3) 0.0274(11) Uani 1 1 d . . . H14A H 0.9553 0.2249 0.4985 0.033 Uiso 1 1 calc R . . C15 C 0.7874(3) 0.3632(5) 0.4057(3) 0.0262(11) Uani 1 1 d . . . H15A H 0.7252 0.3561 0.4003 0.031 Uiso 1 1 calc R . . C16 C 0.8177(3) 0.1614(5) 0.1879(3) 0.0273(11) Uani 1 1 d . . . C17 C 0.8983(3) 0.2371(6) 0.1954(3) 0.0324(12) Uani 1 1 d . . . H17A H 0.9086 0.3146 0.1628 0.039 Uiso 1 1 calc R . . C18 C 0.9625(4) 0.1979(6) 0.2504(3) 0.0399(14) Uani 1 1 d . . . H18A H 1.0172 0.2482 0.2552 0.048 Uiso 1 1 calc R . . C19 C 0.9479(4) 0.0872(6) 0.2983(3) 0.0413(14) Uani 1 1 d . . . H19A H 0.9919 0.0631 0.3367 0.050 Uiso 1 1 calc R . . C20 C 0.8683(4) 0.0094(7) 0.2909(4) 0.0465(15) Uani 1 1 d . . . H20A H 0.8584 -0.0683 0.3235 0.056 Uiso 1 1 calc R . . C21 C 0.8044(4) 0.0474(6) 0.2355(3) 0.0334(12) Uani 1 1 d . . . H21A H 0.7506 -0.0055 0.2299 0.040 Uiso 1 1 calc R . . C22 C 0.6739(3) 0.0536(5) 0.0866(3) 0.0234(10) Uani 1 1 d . . . C23 C 0.7206(3) -0.0476(5) 0.0486(3) 0.0280(11) Uani 1 1 d . . . H23A H 0.7808 -0.0306 0.0438 0.034 Uiso 1 1 calc R . . C24 C 0.6788(4) -0.1743(5) 0.0174(3) 0.0305(12) Uani 1 1 d . . . H24A H 0.7106 -0.2415 -0.0093 0.037 Uiso 1 1 calc R . . C25 C 0.5917(4) -0.2010(6) 0.0256(3) 0.0358(13) Uani 1 1 d . . . H25A H 0.5634 -0.2864 0.0044 0.043 Uiso 1 1 calc R . . C26 C 0.5453(4) -0.1022(5) 0.0650(3) 0.0313(12) Uani 1 1 d . . . H26A H 0.4857 -0.1212 0.0714 0.038 Uiso 1 1 calc R . . C27 C 0.5867(3) 0.0244(6) 0.0950(3) 0.0303(11) Uani 1 1 d . . . H27A H 0.5547 0.0915 0.1215 0.036 Uiso 1 1 calc R . . N1 N 0.8335(3) 0.2767(4) 0.4558(2) 0.0259(9) Uani 1 1 d . . . P1 P 0.72930(8) 0.22385(13) 0.12052(7) 0.0243(3) Uani 1 1 d . . . Fe1 Fe 0.66555(4) 0.49836(7) 0.23567(4) 0.02096(16) Uani 1 1 d . . . Zn1 Zn 0.76751(4) 0.37082(6) 0.01646(3) 0.02440(15) Uani 1 1 d . . . Br1 Br 0.86789(3) 0.56797(5) 0.04437(3) 0.03227(14) Uani 1 1 d . . . Br2 Br 0.63298(3) 0.41838(5) -0.05695(3) 0.02822(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(2) 0.019(2) 0.025(3) 0.0016(19) 0.003(2) -0.0012(18) C2 0.029(2) 0.024(2) 0.025(3) 0.003(2) 0.002(2) -0.006(2) C3 0.033(3) 0.034(3) 0.025(3) 0.002(2) 0.009(2) -0.004(2) C4 0.024(2) 0.036(3) 0.033(3) -0.002(2) 0.003(2) 0.004(2) C5 0.029(2) 0.029(3) 0.021(3) -0.001(2) -0.002(2) 0.001(2) C6 0.031(2) 0.019(2) 0.021(3) 0.0006(19) 0.0000(19) 0.0000(19) C7 0.042(3) 0.026(2) 0.019(3) -0.003(2) 0.002(2) 0.005(2) C8 0.044(3) 0.021(2) 0.031(3) 0.000(2) -0.001(2) 0.007(2) C9 0.044(3) 0.021(2) 0.025(3) 0.003(2) -0.002(2) -0.004(2) C10 0.032(2) 0.021(2) 0.020(3) 0.0012(19) 0.004(2) -0.0052(19) C11 0.031(2) 0.017(2) 0.018(3) -0.0022(18) 0.0008(19) -0.0001(18) C12 0.032(3) 0.027(3) 0.029(3) 0.004(2) 0.005(2) -0.004(2) C13 0.024(2) 0.035(3) 0.033(3) 0.002(2) -0.002(2) 0.001(2) C14 0.028(3) 0.029(3) 0.024(3) 0.002(2) -0.002(2) 0.002(2) C15 0.031(2) 0.023(2) 0.025(3) -0.002(2) 0.002(2) 0.0058(19) C16 0.026(2) 0.024(2) 0.031(3) -0.008(2) -0.002(2) 0.0047(19) C17 0.032(3) 0.028(3) 0.037(3) -0.009(2) 0.000(2) 0.005(2) C18 0.037(3) 0.035(3) 0.046(4) -0.009(3) -0.002(3) 0.004(2) C19 0.036(3) 0.043(3) 0.041(4) -0.011(3) -0.013(2) 0.016(2) C20 0.061(4) 0.030(3) 0.047(4) 0.001(3) -0.003(3) 0.009(3) C21 0.039(3) 0.028(3) 0.032(3) -0.003(2) -0.004(2) 0.007(2) C22 0.034(2) 0.022(2) 0.013(3) 0.0029(19) -0.0010(19) -0.0017(19) C23 0.039(3) 0.023(2) 0.021(3) 0.003(2) -0.001(2) 0.003(2) C24 0.053(3) 0.021(2) 0.016(3) 0.0012(19) -0.002(2) 0.006(2) C25 0.056(3) 0.022(2) 0.026(3) 0.003(2) -0.008(2) -0.009(2) C26 0.042(3) 0.028(3) 0.022(3) 0.004(2) -0.001(2) -0.011(2) C27 0.037(3) 0.028(3) 0.026(3) 0.000(2) 0.001(2) -0.006(2) N1 0.030(2) 0.025(2) 0.022(2) 0.0011(17) 0.0006(17) 0.0025(17) P1 0.0265(6) 0.0203(6) 0.0259(8) -0.0037(5) 0.0018(5) -0.0008(5) Fe1 0.0274(3) 0.0182(3) 0.0171(4) 0.0006(3) 0.0018(3) 0.0018(3) Zn1 0.0276(3) 0.0238(3) 0.0211(3) -0.0047(2) -0.0009(2) -0.0007(2) Br1 0.0315(3) 0.0293(3) 0.0350(3) -0.0066(2) -0.0012(2) -0.0061(2) Br2 0.0288(3) 0.0298(2) 0.0245(3) -0.0044(2) -0.00416(19) 0.00190(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.443(7) . ? C1 C5 1.451(7) . ? C1 P1 1.802(5) . ? C1 Fe1 2.050(5) . ? C2 C3 1.424(7) . ? C2 Fe1 2.056(5) . ? C2 H2A 0.9500 . ? C3 C4 1.433(8) . ? C3 Fe1 2.062(5) . ? C3 H3A 0.9500 . ? C4 C5 1.422(7) . ? C4 Fe1 2.066(5) . ? C4 H4A 0.9500 . ? C5 Fe1 2.060(5) . ? C5 H5A 0.9500 . ? C6 C7 1.435(7) . ? C6 C10 1.437(7) . ? C6 C11 1.495(7) . ? C6 Fe1 2.079(5) . ? C7 C8 1.433(7) . ? C7 Fe1 2.056(5) . ? C7 H7A 0.9500 . ? C8 C9 1.430(8) . ? C8 Fe1 2.049(5) . ? C8 H8A 0.9500 . ? C9 C10 1.421(7) . ? C9 Fe1 2.062(5) . ? C9 H9A 0.9500 . ? C10 Fe1 2.074(5) . ? C10 H10A 0.9500 . ? C11 C15 1.386(7) . ? C11 C12 1.398(7) . ? C12 C13 1.395(8) . ? C12 H12A 0.9500 . ? C13 C14 1.386(7) . ? C13 H13A 0.9500 . ? C14 N1 1.358(6) . ? C14 H14A 0.9500 . ? C15 N1 1.353(6) . ? C15 H15A 0.9500 . ? C16 C21 1.386(8) . ? C16 C17 1.406(7) . ? C16 P1 1.828(5) . ? C17 C18 1.384(8) . ? C17 H17A 0.9500 . ? C18 C19 1.372(9) . ? C18 H18A 0.9500 . ? C19 C20 1.403(9) . ? C19 H19A 0.9500 . ? C20 C21 1.381(8) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C27 1.388(7) . ? C22 C23 1.399(7) . ? C22 P1 1.838(5) . ? C23 C24 1.407(7) . ? C23 H23A 0.9500 . ? C24 C25 1.382(8) . ? C24 H24A 0.9500 . ? C25 C26 1.397(8) . ? C25 H25A 0.9500 . ? C26 C27 1.396(7) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N1 Zn1 2.077(4) 4_566 ? P1 Zn1 2.4628(14) . ? Zn1 N1 2.077(4) 4_565 ? Zn1 Br1 2.3771(7) . ? Zn1 Br2 2.3823(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.2(4) . . ? C2 C1 P1 128.2(4) . . ? C5 C1 P1 124.4(4) . . ? C2 C1 Fe1 69.6(3) . . ? C5 C1 Fe1 69.7(3) . . ? P1 C1 Fe1 129.3(2) . . ? C3 C2 C1 108.0(4) . . ? C3 C2 Fe1 70.0(3) . . ? C1 C2 Fe1 69.2(3) . . ? C3 C2 H2A 126.0 . . ? C1 C2 H2A 126.0 . . ? Fe1 C2 H2A 126.4 . . ? C2 C3 C4 108.4(5) . . ? C2 C3 Fe1 69.5(3) . . ? C4 C3 Fe1 69.8(3) . . ? C2 C3 H3A 125.8 . . ? C4 C3 H3A 125.8 . . ? Fe1 C3 H3A 126.4 . . ? C5 C4 C3 108.4(4) . . ? C5 C4 Fe1 69.6(3) . . ? C3 C4 Fe1 69.6(3) . . ? C5 C4 H4A 125.8 . . ? C3 C4 H4A 125.8 . . ? Fe1 C4 H4A 126.6 . . ? C4 C5 C1 108.0(4) . . ? C4 C5 Fe1 70.1(3) . . ? C1 C5 Fe1 69.0(3) . . ? C4 C5 H5A 126.0 . . ? C1 C5 H5A 126.0 . . ? Fe1 C5 H5A 126.5 . . ? C7 C6 C10 107.9(4) . . ? C7 C6 C11 126.2(5) . . ? C10 C6 C11 125.9(4) . . ? C7 C6 Fe1 68.8(3) . . ? C10 C6 Fe1 69.6(3) . . ? C11 C6 Fe1 128.2(3) . . ? C8 C7 C6 107.4(5) . . ? C8 C7 Fe1 69.3(3) . . ? C6 C7 Fe1 70.6(3) . . ? C8 C7 H7A 126.3 . . ? C6 C7 H7A 126.3 . . ? Fe1 C7 H7A 125.4 . . ? C9 C8 C7 108.4(4) . . ? C9 C8 Fe1 70.2(3) . . ? C7 C8 Fe1 69.8(3) . . ? C9 C8 H8A 125.8 . . ? C7 C8 H8A 125.8 . . ? Fe1 C8 H8A 125.8 . . ? C10 C9 C8 108.0(5) . . ? C10 C9 Fe1 70.3(3) . . ? C8 C9 Fe1 69.1(3) . . ? C10 C9 H9A 126.0 . . ? C8 C9 H9A 126.0 . . ? Fe1 C9 H9A 126.1 . . ? C9 C10 C6 108.2(4) . . ? C9 C10 Fe1 69.5(3) . . ? C6 C10 Fe1 69.9(3) . . ? C9 C10 H10A 125.9 . . ? C6 C10 H10A 125.9 . . ? Fe1 C10 H10A 126.3 . . ? C15 C11 C12 117.9(4) . . ? C15 C11 C6 121.1(4) . . ? C12 C11 C6 120.9(4) . . ? C13 C12 C11 119.3(5) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C14 C13 C12 119.7(5) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? N1 C14 C13 121.2(5) . . ? N1 C14 H14A 119.4 . . ? C13 C14 H14A 119.4 . . ? N1 C15 C11 123.1(4) . . ? N1 C15 H15A 118.5 . . ? C11 C15 H15A 118.5 . . ? C21 C16 C17 119.2(5) . . ? C21 C16 P1 121.0(4) . . ? C17 C16 P1 119.6(4) . . ? C18 C17 C16 119.6(5) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C19 C18 C17 120.6(5) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 120.3(5) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C21 C20 C19 119.1(6) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C16 121.0(5) . . ? C20 C21 H21A 119.5 . . ? C16 C21 H21A 119.5 . . ? C27 C22 C23 118.9(5) . . ? C27 C22 P1 122.5(4) . . ? C23 C22 P1 118.6(4) . . ? C22 C23 C24 120.4(5) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? C25 C24 C23 120.0(5) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 119.9(5) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C27 C26 C25 119.9(5) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C22 C27 C26 120.9(5) . . ? C22 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? C15 N1 C14 118.9(4) . . ? C15 N1 Zn1 119.6(3) . 4_566 ? C14 N1 Zn1 121.5(3) . 4_566 ? C1 P1 C16 104.3(2) . . ? C1 P1 C22 104.1(2) . . ? C16 P1 C22 104.7(2) . . ? C1 P1 Zn1 114.69(16) . . ? C16 P1 Zn1 118.59(17) . . ? C22 P1 Zn1 109.09(16) . . ? C8 Fe1 C1 157.1(2) . . ? C8 Fe1 C7 40.9(2) . . ? C1 Fe1 C7 161.8(2) . . ? C8 Fe1 C2 158.0(2) . . ? C1 Fe1 C2 41.2(2) . . ? C7 Fe1 C2 123.4(2) . . ? C8 Fe1 C5 119.2(2) . . ? C1 Fe1 C5 41.34(19) . . ? C7 Fe1 C5 154.3(2) . . ? C2 Fe1 C5 69.0(2) . . ? C8 Fe1 C3 120.5(2) . . ? C1 Fe1 C3 68.7(2) . . ? C7 Fe1 C3 105.5(2) . . ? C2 Fe1 C3 40.5(2) . . ? C5 Fe1 C3 68.3(2) . . ? C8 Fe1 C9 40.7(2) . . ? C1 Fe1 C9 123.4(2) . . ? C7 Fe1 C9 68.7(2) . . ? C2 Fe1 C9 160.8(2) . . ? C5 Fe1 C9 106.8(2) . . ? C3 Fe1 C9 157.0(2) . . ? C8 Fe1 C4 103.8(2) . . ? C1 Fe1 C4 68.73(19) . . ? C7 Fe1 C4 118.8(2) . . ? C2 Fe1 C4 68.4(2) . . ? C5 Fe1 C4 40.3(2) . . ? C3 Fe1 C4 40.6(2) . . ? C9 Fe1 C4 121.2(2) . . ? C8 Fe1 C10 68.0(2) . . ? C1 Fe1 C10 110.89(19) . . ? C7 Fe1 C10 68.4(2) . . ? C2 Fe1 C10 126.07(19) . . ? C5 Fe1 C10 125.4(2) . . ? C3 Fe1 C10 160.2(2) . . ? C9 Fe1 C10 40.19(19) . . ? C4 Fe1 C10 159.0(2) . . ? C8 Fe1 C6 68.1(2) . . ? C1 Fe1 C6 127.02(19) . . ? C7 Fe1 C6 40.61(19) . . ? C2 Fe1 C6 110.34(19) . . ? C5 Fe1 C6 163.16(19) . . ? C3 Fe1 C6 122.8(2) . . ? C9 Fe1 C6 68.0(2) . . ? C4 Fe1 C6 156.3(2) . . ? C10 Fe1 C6 40.50(19) . . ? N1 Zn1 Br1 105.01(11) 4_565 . ? N1 Zn1 Br2 104.51(12) 4_565 . ? Br1 Zn1 Br2 119.20(3) . . ? N1 Zn1 P1 104.22(12) 4_565 . ? Br1 Zn1 P1 116.07(4) . . ? Br2 Zn1 P1 106.18(4) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.014 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.121 #===================================================================== data_i0626 _database_code_depnum_ccdc_archive 'CCDC 805336' #TrackingRef '- publus86.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H22 Br2 Fe Hg N P' _chemical_formula_sum 'C27 H22 Br2 Fe Hg N P' _chemical_formula_weight 807.69 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' Fe Fe 0.3463 0.8444 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.0531(9) _cell_length_b 8.9781(4) _cell_length_c 19.1000(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.934(4) _cell_angle_gamma 90.00 _cell_volume 2647.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25021 _cell_measurement_theta_min 1.32 _cell_measurement_theta_max 25.78 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 9.436 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.0502 _exptl_absorpt_correction_T_max 0.3925 _exptl_absorpt_process_details 'X-red ver. 1.31 (Stoe & Cie. 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_source_power 1.50 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 135 mm ; _diffrn_standards_decay_% none _diffrn_reflns_number 16588 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.23 _reflns_number_total 4720 _reflns_number_gt 4423 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+0.5961P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00250(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4720 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0285 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1483(2) 0.2106(4) -0.1282(2) 0.0306(8) Uani 1 1 d . . . C2 C 0.0835(2) 0.1015(5) -0.1230(2) 0.0354(8) Uani 1 1 d . . . H2A H 0.0751 0.0615 -0.0794 0.042 Uiso 1 1 calc R . . C3 C 0.0350(3) 0.0657(5) -0.1948(3) 0.0434(10) Uani 1 1 d . . . H3A H -0.0121 -0.0023 -0.2076 0.052 Uiso 1 1 calc R . . C4 C 0.0684(3) 0.1484(5) -0.2448(3) 0.0409(10) Uani 1 1 d . . . H4A H 0.0477 0.1438 -0.2964 0.049 Uiso 1 1 calc R . . C5 C 0.1378(2) 0.2387(5) -0.2047(2) 0.0347(8) Uani 1 1 d . . . H5A H 0.1712 0.3055 -0.2245 0.042 Uiso 1 1 calc R . . C6 C 0.2737(2) -0.0403(4) -0.2097(2) 0.0340(8) Uani 1 1 d . . . C7 C 0.2868(3) -0.0679(4) -0.1334(2) 0.0365(9) Uani 1 1 d . . . H7A H 0.3310 -0.0256 -0.0949 0.044 Uiso 1 1 calc R . . C8 C 0.2216(3) -0.1701(5) -0.1254(3) 0.0420(10) Uani 1 1 d . . . H8A H 0.2146 -0.2067 -0.0807 0.050 Uiso 1 1 calc R . . C9 C 0.1691(3) -0.2073(5) -0.1965(3) 0.0446(10) Uani 1 1 d . . . H9A H 0.1213 -0.2739 -0.2075 0.053 Uiso 1 1 calc R . . C10 C 0.2008(3) -0.1272(4) -0.2481(3) 0.0396(10) Uani 1 1 d . . . H10A H 0.1776 -0.1309 -0.2995 0.048 Uiso 1 1 calc R . . C11 C 0.3268(2) 0.0599(4) -0.2426(2) 0.0336(8) Uani 1 1 d . . . C12 C 0.4139(2) 0.0867(5) -0.2087(2) 0.0399(9) Uani 1 1 d . . . H12A H 0.4413 0.0412 -0.1633 0.048 Uiso 1 1 calc R . . C13 C 0.4604(2) 0.1808(6) -0.2420(3) 0.0445(10) Uani 1 1 d . . . H13A H 0.5201 0.1995 -0.2197 0.053 Uiso 1 1 calc R . . C14 C 0.4190(2) 0.2469(5) -0.3077(2) 0.0405(9) Uani 1 1 d . . . H14A H 0.4510 0.3111 -0.3303 0.049 Uiso 1 1 calc R . . C15 C 0.2902(3) 0.1314(4) -0.3079(2) 0.0344(9) Uani 1 1 d . . . H15A H 0.2304 0.1154 -0.3309 0.041 Uiso 1 1 calc R . . C16 C 0.3166(3) 0.3605(4) -0.0767(3) 0.0373(10) Uani 1 1 d . . . C17 C 0.3975(2) 0.3006(5) -0.0426(3) 0.0422(10) Uani 1 1 d . . . H17A H 0.4031 0.2246 -0.0070 0.051 Uiso 1 1 calc R . . C18 C 0.4705(3) 0.3532(6) -0.0613(4) 0.0549(14) Uani 1 1 d . . . H18A H 0.5260 0.3139 -0.0377 0.066 Uiso 1 1 calc R . . C19 C 0.4626(3) 0.4606(6) -0.1131(4) 0.0630(15) Uani 1 1 d . . . H19A H 0.5125 0.4942 -0.1260 0.076 Uiso 1 1 calc R . . C20 C 0.3825(3) 0.5211(6) -0.1472(4) 0.0642(15) Uani 1 1 d . . . H20A H 0.3777 0.5964 -0.1830 0.077 Uiso 1 1 calc R . . C21 C 0.3091(3) 0.4718(5) -0.1290(3) 0.0495(11) Uani 1 1 d . . . H21A H 0.2540 0.5138 -0.1520 0.059 Uiso 1 1 calc R . . C22 C 0.1665(2) 0.4639(4) -0.0327(2) 0.0334(8) Uani 1 1 d . . . C23 C 0.2110(3) 0.5594(5) 0.0228(2) 0.0369(9) Uani 1 1 d . . . H23A H 0.2698 0.5402 0.0479 0.044 Uiso 1 1 calc R . . C24 C 0.1688(3) 0.6830(5) 0.0412(3) 0.0412(9) Uani 1 1 d . . . H24A H 0.1986 0.7472 0.0795 0.049 Uiso 1 1 calc R . . C25 C 0.0832(3) 0.7126(5) 0.0037(3) 0.0453(10) Uani 1 1 d . . . H25A H 0.0548 0.7976 0.0158 0.054 Uiso 1 1 calc R . . C26 C 0.0397(3) 0.6193(5) -0.0509(3) 0.0471(11) Uani 1 1 d . . . H26A H -0.0189 0.6399 -0.0762 0.057 Uiso 1 1 calc R . . C27 C 0.0805(3) 0.4937(5) -0.0698(2) 0.0413(9) Uani 1 1 d . . . H27A H 0.0499 0.4294 -0.1077 0.050 Uiso 1 1 calc R . . Fe1 Fe 0.16419(3) 0.01824(6) -0.17957(3) 0.03090(14) Uani 1 1 d . . . N1 N 0.3347(2) 0.2227(4) -0.34064(19) 0.0362(7) Uani 1 1 d . . . P1 P 0.22119(6) 0.29647(11) -0.05136(6) 0.0295(2) Uani 1 1 d . . . Hg1 Hg 0.254946(8) 0.131822(16) 0.054495(8) 0.03316(9) Uani 1 1 d . . . Br1 Br 0.36800(3) -0.07816(5) 0.07332(3) 0.04700(13) Uani 1 1 d . . . Br2 Br 0.13011(3) 0.07200(5) 0.11138(3) 0.04689(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0324(16) 0.0290(19) 0.032(2) 0.0015(16) 0.0109(15) 0.0054(14) C2 0.0349(18) 0.041(2) 0.033(2) -0.0003(18) 0.0151(16) -0.0012(16) C3 0.0339(18) 0.054(3) 0.041(2) -0.005(2) 0.0074(17) -0.0019(18) C4 0.040(2) 0.051(3) 0.028(2) -0.0007(19) 0.0030(17) 0.0068(17) C5 0.0398(18) 0.033(2) 0.032(2) 0.0072(17) 0.0114(16) 0.0089(15) C6 0.0399(18) 0.0309(19) 0.032(2) 0.0024(17) 0.0114(16) 0.0066(15) C7 0.045(2) 0.030(2) 0.035(2) 0.0030(17) 0.0114(17) 0.0088(16) C8 0.056(2) 0.032(2) 0.042(3) 0.0066(19) 0.020(2) 0.0066(18) C9 0.056(2) 0.029(2) 0.054(3) -0.004(2) 0.023(2) -0.0041(17) C10 0.049(2) 0.036(2) 0.035(2) -0.0052(18) 0.0131(19) 0.0014(16) C11 0.0375(18) 0.034(2) 0.032(2) -0.0038(17) 0.0139(16) 0.0075(15) C12 0.0366(19) 0.052(3) 0.031(2) 0.006(2) 0.0091(16) 0.0095(18) C13 0.0294(17) 0.058(3) 0.044(3) 0.007(2) 0.0071(17) 0.0058(18) C14 0.0331(18) 0.049(2) 0.041(2) 0.006(2) 0.0131(17) 0.0009(17) C15 0.0343(18) 0.035(2) 0.032(2) 0.0017(16) 0.0070(16) -0.0009(14) C16 0.040(2) 0.031(2) 0.045(3) -0.0067(17) 0.0178(19) 0.0002(15) C17 0.0350(19) 0.040(2) 0.054(3) -0.007(2) 0.0163(18) 0.0012(16) C18 0.038(2) 0.056(3) 0.075(4) -0.015(3) 0.022(2) 0.0005(19) C19 0.060(3) 0.056(3) 0.091(4) -0.009(3) 0.050(3) -0.012(2) C20 0.074(3) 0.048(3) 0.086(4) 0.012(3) 0.048(3) -0.005(2) C21 0.051(2) 0.040(2) 0.063(3) 0.011(2) 0.026(2) 0.0037(19) C22 0.0394(18) 0.0287(19) 0.036(2) 0.0021(17) 0.0165(16) 0.0029(15) C23 0.0426(19) 0.033(2) 0.038(2) 0.0021(18) 0.0153(17) 0.0011(16) C24 0.061(2) 0.030(2) 0.037(2) 0.0009(19) 0.021(2) -0.0020(18) C25 0.061(2) 0.036(2) 0.047(3) 0.006(2) 0.027(2) 0.0155(19) C26 0.050(2) 0.047(3) 0.046(3) 0.003(2) 0.017(2) 0.0172(19) C27 0.045(2) 0.043(2) 0.036(2) -0.0007(19) 0.0105(18) 0.0097(18) Fe1 0.0356(3) 0.0299(3) 0.0283(3) -0.0001(2) 0.0106(2) -0.0002(2) N1 0.0348(15) 0.043(2) 0.0308(18) 0.0045(15) 0.0093(13) -0.0017(14) P1 0.0311(4) 0.0277(5) 0.0307(5) 0.0003(4) 0.0102(4) 0.0041(4) Hg1 0.03564(11) 0.03383(12) 0.02928(12) 0.00047(6) 0.00769(7) 0.00527(5) Br1 0.0415(2) 0.0458(3) 0.0481(3) -0.0029(2) 0.00265(18) 0.01613(17) Br2 0.0436(2) 0.0462(3) 0.0583(3) -0.0125(2) 0.0265(2) -0.00454(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.445(6) . ? C1 C2 1.452(5) . ? C1 P1 1.782(4) . ? C1 Fe1 2.036(4) . ? C2 C3 1.416(6) . ? C2 Fe1 2.043(4) . ? C2 H2A 0.9500 . ? C3 C4 1.425(7) . ? C3 Fe1 2.059(4) . ? C3 H3A 0.9500 . ? C4 C5 1.419(6) . ? C4 Fe1 2.057(4) . ? C4 H4A 0.9500 . ? C5 Fe1 2.053(4) . ? C5 H5A 0.9500 . ? C6 C10 1.430(6) . ? C6 C7 1.435(6) . ? C6 C11 1.492(6) . ? C6 Fe1 2.062(4) . ? C7 C8 1.431(6) . ? C7 Fe1 2.072(4) . ? C7 H7A 0.9500 . ? C8 C9 1.429(7) . ? C8 Fe1 2.063(4) . ? C8 H8A 0.9500 . ? C9 C10 1.423(7) . ? C9 Fe1 2.056(4) . ? C9 H9A 0.9500 . ? C10 Fe1 2.047(4) . ? C10 H10A 0.9500 . ? C11 C15 1.382(6) . ? C11 C12 1.391(6) . ? C12 C13 1.391(7) . ? C12 H12A 0.9500 . ? C13 C14 1.384(7) . ? C13 H13A 0.9500 . ? C14 N1 1.344(5) . ? C14 H14A 0.9500 . ? C15 N1 1.349(5) . ? C15 H15A 0.9500 . ? C16 C17 1.391(6) . ? C16 C21 1.394(7) . ? C16 P1 1.822(4) . ? C17 C18 1.397(6) . ? C17 H17A 0.9500 . ? C18 C19 1.363(8) . ? C18 H18A 0.9500 . ? C19 C20 1.382(8) . ? C19 H19A 0.9500 . ? C20 C21 1.390(6) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C27 1.393(5) . ? C22 C23 1.398(6) . ? C22 P1 1.824(4) . ? C23 C24 1.395(6) . ? C23 H23A 0.9500 . ? C24 C25 1.390(6) . ? C24 H24A 0.9500 . ? C25 C26 1.369(7) . ? C25 H25A 0.9500 . ? C26 C27 1.401(6) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N1 Hg1 2.439(3) 4_565 ? P1 Hg1 2.4423(10) . ? Hg1 N1 2.439(3) 4_566 ? Hg1 Br1 2.5727(4) . ? Hg1 Br2 2.5847(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 107.4(3) . . ? C5 C1 P1 128.7(3) . . ? C2 C1 P1 123.8(3) . . ? C5 C1 Fe1 69.9(2) . . ? C2 C1 Fe1 69.4(2) . . ? P1 C1 Fe1 128.51(19) . . ? C3 C2 C1 107.5(4) . . ? C3 C2 Fe1 70.4(2) . . ? C1 C2 Fe1 68.9(2) . . ? C3 C2 H2A 126.3 . . ? C1 C2 H2A 126.3 . . ? Fe1 C2 H2A 126.0 . . ? C2 C3 C4 108.8(4) . . ? C2 C3 Fe1 69.2(2) . . ? C4 C3 Fe1 69.7(2) . . ? C2 C3 H3A 125.6 . . ? C4 C3 H3A 125.6 . . ? Fe1 C3 H3A 127.1 . . ? C5 C4 C3 108.6(4) . . ? C5 C4 Fe1 69.7(2) . . ? C3 C4 Fe1 69.8(2) . . ? C5 C4 H4A 125.7 . . ? C3 C4 H4A 125.7 . . ? Fe1 C4 H4A 126.4 . . ? C4 C5 C1 107.6(4) . . ? C4 C5 Fe1 69.9(2) . . ? C1 C5 Fe1 68.7(2) . . ? C4 C5 H5A 126.2 . . ? C1 C5 H5A 126.2 . . ? Fe1 C5 H5A 126.8 . . ? C10 C6 C7 107.4(4) . . ? C10 C6 C11 126.4(4) . . ? C7 C6 C11 126.2(4) . . ? C10 C6 Fe1 69.1(2) . . ? C7 C6 Fe1 70.1(2) . . ? C11 C6 Fe1 126.4(3) . . ? C8 C7 C6 108.2(4) . . ? C8 C7 Fe1 69.4(2) . . ? C6 C7 Fe1 69.3(2) . . ? C8 C7 H7A 125.9 . . ? C6 C7 H7A 125.9 . . ? Fe1 C7 H7A 127.0 . . ? C7 C8 C9 107.8(4) . . ? C7 C8 Fe1 70.1(2) . . ? C9 C8 Fe1 69.4(3) . . ? C7 C8 H8A 126.1 . . ? C9 C8 H8A 126.1 . . ? Fe1 C8 H8A 126.0 . . ? C10 C9 C8 108.1(4) . . ? C10 C9 Fe1 69.4(2) . . ? C8 C9 Fe1 70.0(2) . . ? C10 C9 H9A 126.0 . . ? C8 C9 H9A 126.0 . . ? Fe1 C9 H9A 126.2 . . ? C9 C10 C6 108.5(4) . . ? C9 C10 Fe1 70.0(3) . . ? C6 C10 Fe1 70.2(2) . . ? C9 C10 H10A 125.7 . . ? C6 C10 H10A 125.7 . . ? Fe1 C10 H10A 125.6 . . ? C15 C11 C12 117.6(4) . . ? C15 C11 C6 120.6(3) . . ? C12 C11 C6 121.7(4) . . ? C11 C12 C13 119.3(4) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C14 C13 C12 119.4(4) . . ? C14 C13 H13A 120.3 . . ? C12 C13 H13A 120.3 . . ? N1 C14 C13 121.8(4) . . ? N1 C14 H14A 119.1 . . ? C13 C14 H14A 119.1 . . ? N1 C15 C11 123.5(4) . . ? N1 C15 H15A 118.2 . . ? C11 C15 H15A 118.2 . . ? C17 C16 C21 119.9(4) . . ? C17 C16 P1 119.9(3) . . ? C21 C16 P1 120.1(3) . . ? C16 C17 C18 119.4(5) . . ? C16 C17 H17A 120.3 . . ? C18 C17 H17A 120.3 . . ? C19 C18 C17 120.5(5) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 120.6(4) . . ? C18 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C19 C20 C21 120.0(5) . . ? C19 C20 H20A 120.0 . . ? C21 C20 H20A 120.0 . . ? C20 C21 C16 119.6(5) . . ? C20 C21 H21A 120.2 . . ? C16 C21 H21A 120.2 . . ? C27 C22 C23 119.7(4) . . ? C27 C22 P1 121.5(3) . . ? C23 C22 P1 118.7(3) . . ? C24 C23 C22 119.8(4) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C26 C25 C24 120.1(4) . . ? C26 C25 H25A 120.0 . . ? C24 C25 H25A 120.0 . . ? C25 C26 C27 120.8(4) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C22 C27 C26 119.5(4) . . ? C22 C27 H27A 120.3 . . ? C26 C27 H27A 120.3 . . ? C1 Fe1 C2 41.71(15) . . ? C1 Fe1 C10 160.95(16) . . ? C2 Fe1 C10 155.13(17) . . ? C1 Fe1 C5 41.39(16) . . ? C2 Fe1 C5 69.54(16) . . ? C10 Fe1 C5 122.87(18) . . ? C1 Fe1 C9 157.91(18) . . ? C2 Fe1 C9 120.07(17) . . ? C10 Fe1 C9 40.59(18) . . ? C5 Fe1 C9 157.99(19) . . ? C1 Fe1 C3 68.77(17) . . ? C2 Fe1 C3 40.39(18) . . ? C10 Fe1 C3 119.80(18) . . ? C5 Fe1 C3 68.39(17) . . ? C9 Fe1 C3 105.20(19) . . ? C1 Fe1 C4 68.79(16) . . ? C2 Fe1 C4 68.61(18) . . ? C10 Fe1 C4 105.86(19) . . ? C5 Fe1 C4 40.41(17) . . ? C9 Fe1 C4 121.25(19) . . ? C3 Fe1 C4 40.53(19) . . ? C1 Fe1 C6 125.41(15) . . ? C2 Fe1 C6 162.50(16) . . ? C10 Fe1 C6 40.74(17) . . ? C5 Fe1 C6 108.53(16) . . ? C9 Fe1 C6 68.46(17) . . ? C3 Fe1 C6 156.40(18) . . ? C4 Fe1 C6 121.91(18) . . ? C1 Fe1 C8 123.46(18) . . ? C2 Fe1 C8 107.20(18) . . ? C10 Fe1 C8 68.33(19) . . ? C5 Fe1 C8 160.47(18) . . ? C9 Fe1 C8 40.6(2) . . ? C3 Fe1 C8 122.34(19) . . ? C4 Fe1 C8 157.88(18) . . ? C6 Fe1 C8 68.48(17) . . ? C1 Fe1 C7 109.97(16) . . ? C2 Fe1 C7 125.29(17) . . ? C10 Fe1 C7 68.16(18) . . ? C5 Fe1 C7 124.78(16) . . ? C9 Fe1 C7 68.07(18) . . ? C3 Fe1 C7 160.01(18) . . ? C4 Fe1 C7 159.12(18) . . ? C6 Fe1 C7 40.61(16) . . ? C8 Fe1 C7 40.48(17) . . ? C14 N1 C15 118.4(4) . . ? C14 N1 Hg1 122.1(3) . 4_565 ? C15 N1 Hg1 118.7(2) . 4_565 ? C1 P1 C22 105.93(18) . . ? C1 P1 C16 109.1(2) . . ? C22 P1 C16 106.06(17) . . ? C1 P1 Hg1 111.50(13) . . ? C22 P1 Hg1 110.27(14) . . ? C16 P1 Hg1 113.52(15) . . ? N1 Hg1 P1 107.63(9) 4_566 . ? N1 Hg1 Br1 94.97(8) 4_566 . ? P1 Hg1 Br1 123.16(3) . . ? N1 Hg1 Br2 93.37(8) 4_566 . ? P1 Hg1 Br2 116.89(3) . . ? Br1 Hg1 Br2 112.804(17) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.23 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.933 _refine_diff_density_min -0.731 _refine_diff_density_rms 0.257 #===eof======================================================