Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Petr Stepnicka' _publ_contact_author_address ; Department of Inorganic Chemistry Charles University in Prague, Faculty of Science Hlavova 2030 Prague 12840 CZECH REPUBLIC ; _publ_contact_author_email STEPNIC@NATUR.CUNI.CZ _publ_section_title ; Group-12 metal complexes with isomeric 1-(diphenylphosphino)-1' [N-(pyridylmethyl)carbamoyl]ferrocenes: coordination polymers vs. finite multinuclear coordination assemblies ; loop_ _publ_author_name 'Petr Stepnicka' 'Ivana Cisarova' 'Janett Kuhnert' 'Martin Lamac' data_jk8 _database_code_depnum_ccdc_archive 'CCDC 670833' _audit_creation_method SHELXL-97 _chemical_name_systematic ; N-[(4-pyridyl)methyl]-1'-(diphenylphosphino)ferrocenecarboxamide - water (1/1) ; _chemical_formula_moiety 'C29 H25 Fe N2 O P, H2 O' _chemical_formula_sum 'C29 H27 Fe N2 O2 P' _chemical_formula_weight 522.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 7.499(3) _cell_length_b 10.682(3) _cell_length_c 16.605(5) _cell_angle_alpha 73.52(2) _cell_angle_beta 75.81(3) _cell_angle_gamma 80.84(2) _cell_volume 1230.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8082 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 26.5 _exptl_crystal_description orange _exptl_crystal_colour block _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 544 _exptl_absorpt_coefficient_mu 0.708 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford KM4 CCD diffractometer' _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 8.3438 _diffrn_standards_number 0 _diffrn_reflns_number 16816 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 26.59 _reflns_number_total 5119 _reflns_number_gt 3571 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) ; _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0341P)^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 5119 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _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 Fe Fe 0.42768(3) -0.15082(2) 0.178819(16) 0.02155(8) Uani 1 1 d . . . P P 0.42423(6) 0.13595(4) 0.23772(3) 0.02216(12) Uani 1 1 d . . . N1 N 0.5308(2) -0.31893(13) 0.41653(9) 0.0240(3) Uani 1 1 d . . . H1N H 0.6525 -0.2999 0.3987 0.038(6) Uiso 1 1 d R . . N2 N 0.1722(2) 0.01468(15) 0.57898(11) 0.0368(4) Uani 1 1 d . . . O O 0.27433(17) -0.36876(12) 0.38867(8) 0.0307(3) Uani 1 1 d . . . C1 C 0.3282(2) 0.03634(15) 0.18915(11) 0.0207(4) Uani 1 1 d . . . C2 C 0.1990(2) -0.05571(16) 0.23837(12) 0.0250(4) Uani 1 1 d . . . H2 H 0.1533 -0.0723 0.2974 0.030 Uiso 1 1 calc R . . C3 C 0.1516(2) -0.11744(17) 0.18291(12) 0.0302(5) Uani 1 1 d . . . H3 H 0.0691 -0.1810 0.1988 0.036 Uiso 1 1 calc R . . C4 C 0.2518(2) -0.06563(17) 0.09896(12) 0.0309(5) Uani 1 1 d . . . H4 H 0.2474 -0.0897 0.0499 0.037 Uiso 1 1 calc R . . C5 C 0.3602(2) 0.02923(16) 0.10221(11) 0.0238(4) Uani 1 1 d . . . H5 H 0.4387 0.0784 0.0557 0.029 Uiso 1 1 calc R . . C6 C 0.5218(2) -0.29917(15) 0.27078(11) 0.0217(4) Uani 1 1 d . . . C7 C 0.4798(2) -0.34912(16) 0.20727(11) 0.0276(4) Uani 1 1 d . . . H7 H 0.3940 -0.4085 0.2168 0.033 Uiso 1 1 calc R . . C8 C 0.5917(3) -0.29242(18) 0.12740(12) 0.0334(5) Uani 1 1 d . . . H8 H 0.5927 -0.3086 0.0751 0.040 Uiso 1 1 calc R . . C9 C 0.7015(2) -0.20727(17) 0.13999(11) 0.0292(5) Uani 1 1 d . . . H9 H 0.7867 -0.1572 0.0975 0.035 Uiso 1 1 calc R . . C10 C 0.6596(2) -0.21099(16) 0.22867(11) 0.0246(4) Uani 1 1 d . . . H10 H 0.7127 -0.1642 0.2546 0.029 Uiso 1 1 calc R . . C11 C 0.4307(2) -0.33162(15) 0.36331(11) 0.0225(4) Uani 1 1 d . . . C12 C 0.2402(2) 0.27023(16) 0.24384(11) 0.0226(4) Uani 1 1 d . . . C13 C 0.1178(2) 0.31176(17) 0.18888(12) 0.0303(4) Uani 1 1 d . . . H13 H 0.1269 0.2701 0.1457 0.036 Uiso 1 1 calc R . . C14 C -0.0178(3) 0.41450(19) 0.19750(14) 0.0405(5) Uani 1 1 d . . . H14 H -0.0997 0.4411 0.1605 0.049 Uiso 1 1 calc R . . C15 C -0.0309(3) 0.47712(19) 0.26106(16) 0.0462(6) Uani 1 1 d . . . H15 H -0.1199 0.5474 0.2660 0.055 Uiso 1 1 calc R . . C16 C 0.0868(3) 0.43636(19) 0.31701(15) 0.0459(6) Uani 1 1 d . . . H16 H 0.0757 0.4776 0.3606 0.055 Uiso 1 1 calc R . . C17 C 0.2221(3) 0.33359(18) 0.30829(13) 0.0335(5) Uani 1 1 d . . . H17 H 0.3020 0.3066 0.3462 0.040 Uiso 1 1 calc R . . C18 C 0.5975(2) 0.21427(16) 0.14588(11) 0.0226(4) Uani 1 1 d . . . C19 C 0.7651(2) 0.14022(17) 0.12427(11) 0.0237(4) Uani 1 1 d . . . H19 H 0.7845 0.0545 0.1566 0.028 Uiso 1 1 calc R . . C20 C 0.9017(2) 0.19178(18) 0.05625(11) 0.0278(4) Uani 1 1 d . . . H20 H 1.0113 0.1403 0.0425 0.033 Uiso 1 1 calc R . . C21 C 0.8774(3) 0.31901(19) 0.00828(12) 0.0349(5) Uani 1 1 d . . . H21 H 0.9689 0.3532 -0.0385 0.042 Uiso 1 1 calc R . . C22 C 0.7155(3) 0.3955(2) 0.03039(13) 0.0420(5) Uani 1 1 d . . . H22 H 0.6993 0.4824 -0.0005 0.050 Uiso 1 1 calc R . . C23 C 0.5779(3) 0.34318(18) 0.09819(13) 0.0361(5) Uani 1 1 d . . . H23 H 0.4695 0.3956 0.1122 0.043 Uiso 1 1 calc R . . C24 C 0.4529(3) -0.33577(17) 0.50781(11) 0.0292(4) Uani 1 1 d . . . H24A H 0.5512 -0.3690 0.5392 0.035 Uiso 1 1 calc R . . H24B H 0.3651 -0.4011 0.5263 0.035 Uiso 1 1 calc R . . C25 C 0.3570(2) -0.21142(17) 0.53079(11) 0.0237(4) Uani 1 1 d . . . C26 C 0.3291(3) -0.09517(18) 0.47048(12) 0.0356(5) Uani 1 1 d . . . H26 H 0.3718 -0.0900 0.4122 0.043 Uiso 1 1 calc R . . C27 C 0.2373(3) 0.01338(19) 0.49731(13) 0.0409(5) Uani 1 1 d . . . H27 H 0.2200 0.0906 0.4555 0.049 Uiso 1 1 calc R . . C28 C 0.2007(3) -0.09777(19) 0.63699(13) 0.0354(5) Uani 1 1 d . . . H28 H 0.1573 -0.1001 0.6948 0.042 Uiso 1 1 calc R . . C29 C 0.2906(2) -0.21032(18) 0.61600(11) 0.0284(4) Uani 1 1 d . . . H29 H 0.3068 -0.2860 0.6592 0.034 Uiso 1 1 calc R . . O1W O -0.10028(18) -0.26217(13) 0.38662(9) 0.0444(4) Uani 1 1 d . . . H1W H 0.0206 -0.2981 0.3905 0.070(8) Uiso 1 1 d R . . H2W H -0.1061 -0.1817 0.4003 0.094(9) Uiso 1 1 d 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 Fe 0.02180(15) 0.01843(14) 0.02304(15) -0.00672(11) -0.00352(11) 0.00274(10) P 0.0218(3) 0.0199(2) 0.0236(3) -0.0053(2) -0.0051(2) 0.00141(19) N1 0.0226(9) 0.0256(8) 0.0230(8) -0.0061(7) -0.0030(7) -0.0029(6) N2 0.0392(10) 0.0337(10) 0.0381(10) -0.0148(8) -0.0057(8) 0.0012(8) O 0.0241(7) 0.0339(8) 0.0308(7) -0.0037(6) -0.0026(6) -0.0069(6) C1 0.0183(9) 0.0162(9) 0.0254(10) -0.0048(7) -0.0050(8) 0.0044(7) C2 0.0206(10) 0.0239(10) 0.0284(10) -0.0096(8) -0.0016(8) 0.0038(8) C3 0.0204(10) 0.0267(11) 0.0441(12) -0.0116(9) -0.0068(9) 0.0006(8) C4 0.0314(11) 0.0323(11) 0.0335(11) -0.0135(9) -0.0164(9) 0.0082(9) C5 0.0254(10) 0.0201(10) 0.0238(10) -0.0040(8) -0.0067(8) 0.0036(8) C6 0.0207(10) 0.0163(9) 0.0263(10) -0.0060(8) -0.0054(8) 0.0047(7) C7 0.0337(11) 0.0175(9) 0.0328(11) -0.0104(8) -0.0072(9) 0.0014(8) C8 0.0426(12) 0.0287(11) 0.0275(11) -0.0142(9) -0.0053(10) 0.0109(9) C9 0.0229(10) 0.0267(10) 0.0262(11) -0.0025(8) 0.0057(8) 0.0065(8) C10 0.0186(9) 0.0212(10) 0.0313(11) -0.0059(8) -0.0064(8) 0.0059(7) C11 0.0234(10) 0.0142(9) 0.0275(10) -0.0040(8) -0.0050(9) 0.0021(7) C12 0.0195(10) 0.0177(9) 0.0292(10) -0.0065(8) -0.0017(8) -0.0025(7) C13 0.0276(11) 0.0270(11) 0.0316(11) -0.0046(9) -0.0035(9) 0.0009(8) C14 0.0277(12) 0.0309(12) 0.0504(14) 0.0028(10) -0.0051(10) 0.0040(9) C15 0.0292(12) 0.0215(11) 0.0786(17) -0.0128(11) 0.0032(12) 0.0021(9) C16 0.0392(13) 0.0325(12) 0.0733(17) -0.0343(12) -0.0014(12) -0.0029(10) C17 0.0293(11) 0.0303(11) 0.0463(13) -0.0185(10) -0.0068(10) -0.0040(9) C18 0.0221(10) 0.0221(10) 0.0243(10) -0.0054(8) -0.0072(8) -0.0009(7) C19 0.0249(10) 0.0209(10) 0.0258(10) -0.0056(8) -0.0088(8) 0.0009(8) C20 0.0213(10) 0.0318(11) 0.0299(11) -0.0101(9) -0.0059(9) 0.0033(8) C21 0.0289(11) 0.0369(12) 0.0304(11) -0.0004(9) 0.0009(9) -0.0051(9) C22 0.0372(13) 0.0291(11) 0.0441(13) 0.0078(10) -0.0023(10) 0.0009(9) C23 0.0277(11) 0.0274(11) 0.0432(12) -0.0024(9) -0.0021(10) 0.0057(9) C24 0.0347(11) 0.0269(10) 0.0246(10) -0.0036(8) -0.0074(9) -0.0026(8) C25 0.0235(10) 0.0236(10) 0.0248(10) -0.0056(8) -0.0048(8) -0.0058(7) C26 0.0509(13) 0.0279(11) 0.0244(11) -0.0054(9) -0.0041(10) -0.0019(9) C27 0.0574(15) 0.0245(11) 0.0360(13) -0.0033(9) -0.0100(11) 0.0022(10) C28 0.0308(11) 0.0465(13) 0.0298(11) -0.0158(10) -0.0030(9) -0.0008(10) C29 0.0259(11) 0.0335(11) 0.0245(10) -0.0066(8) -0.0035(8) -0.0034(8) O1W 0.0261(8) 0.0370(9) 0.0760(11) -0.0252(8) -0.0094(7) -0.0025(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 Fe C4 2.0289(19) . ? Fe C7 2.0302(18) . ? Fe C3 2.031(2) . ? Fe C2 2.0336(17) . ? Fe C6 2.0348(18) . ? Fe C8 2.0383(18) . ? Fe C10 2.0424(19) . ? Fe C9 2.0425(19) . ? Fe C5 2.0473(18) . ? Fe C1 2.0591(17) . ? P C1 1.8210(18) . ? P C12 1.8319(17) . ? P C18 1.8343(18) . ? N1 C11 1.337(2) . ? N1 C24 1.455(2) . ? N1 H1N 0.9244 . ? N2 C27 1.327(2) . ? N2 C28 1.334(2) . ? O C11 1.233(2) . ? C1 C2 1.426(2) . ? C1 C5 1.426(2) . ? C2 C3 1.410(2) . ? C2 H2 0.9300 . ? C3 C4 1.413(3) . ? C3 H3 0.9300 . ? C4 C5 1.416(2) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.424(2) . ? C6 C7 1.425(2) . ? C6 C11 1.485(2) . ? C7 C8 1.411(2) . ? C7 H7 0.9300 . ? C8 C9 1.407(3) . ? C8 H8 0.9300 . ? C9 C10 1.419(2) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C13 1.387(3) . ? C12 C17 1.390(2) . ? C13 C14 1.386(2) . ? C13 H13 0.9300 . ? C14 C15 1.378(3) . ? C14 H14 0.9300 . ? C15 C16 1.371(3) . ? C15 H15 0.9300 . ? C16 C17 1.385(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.385(2) . ? C18 C19 1.399(2) . ? C19 C20 1.374(2) . ? C19 H19 0.9300 . ? C20 C21 1.376(3) . ? C20 H20 0.9300 . ? C21 C22 1.383(3) . ? C21 H21 0.9300 . ? C22 C23 1.379(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.509(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.379(2) . ? C25 C29 1.383(2) . ? C26 C27 1.380(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.373(2) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? O1W H1W 0.9365 . ? O1W H2W 0.9422 . ? 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 C4 Fe C7 117.93(8) . . ? C4 Fe C3 40.72(7) . . ? C7 Fe C3 104.58(8) . . ? C4 Fe C2 68.32(8) . . ? C7 Fe C2 123.45(8) . . ? C3 Fe C2 40.59(7) . . ? C4 Fe C6 153.53(8) . . ? C7 Fe C6 41.05(7) . . ? C3 Fe C6 118.92(8) . . ? C2 Fe C6 107.42(7) . . ? C4 Fe C8 106.08(8) . . ? C7 Fe C8 40.57(7) . . ? C3 Fe C8 122.69(8) . . ? C2 Fe C8 159.86(7) . . ? C6 Fe C8 68.47(7) . . ? C4 Fe C10 163.19(7) . . ? C7 Fe C10 68.75(7) . . ? C3 Fe C10 155.74(7) . . ? C2 Fe C10 122.45(7) . . ? C6 Fe C10 40.87(7) . . ? C8 Fe C10 68.21(8) . . ? C4 Fe C9 124.98(8) . . ? C7 Fe C9 68.38(8) . . ? C3 Fe C9 160.41(7) . . ? C2 Fe C9 158.37(7) . . ? C6 Fe C9 68.55(7) . . ? C8 Fe C9 40.34(7) . . ? C10 Fe C9 40.64(7) . . ? C4 Fe C5 40.65(7) . . ? C7 Fe C5 154.16(7) . . ? C3 Fe C5 68.42(8) . . ? C2 Fe C5 68.26(7) . . ? C6 Fe C5 164.20(7) . . ? C8 Fe C5 120.92(7) . . ? C10 Fe C5 127.52(7) . . ? C9 Fe C5 109.50(8) . . ? C4 Fe C1 68.57(7) . . ? C7 Fe C1 161.94(7) . . ? C3 Fe C1 68.64(7) . . ? C2 Fe C1 40.78(7) . . ? C6 Fe C1 126.30(7) . . ? C8 Fe C1 157.11(7) . . ? C10 Fe C1 110.17(7) . . ? C9 Fe C1 123.36(7) . . ? C5 Fe C1 40.65(7) . . ? C1 P C12 101.23(8) . . ? C1 P C18 100.88(8) . . ? C12 P C18 101.73(8) . . ? C11 N1 C24 121.21(15) . . ? C11 N1 H1N 123.3 . . ? C24 N1 H1N 115.5 . . ? C27 N2 C28 116.02(16) . . ? C2 C1 C5 106.78(15) . . ? C2 C1 P 122.30(13) . . ? C5 C1 P 130.92(13) . . ? C2 C1 Fe 68.65(9) . . ? C5 C1 Fe 69.23(9) . . ? P C1 Fe 126.38(9) . . ? C3 C2 C1 108.82(16) . . ? C3 C2 Fe 69.62(10) . . ? C1 C2 Fe 70.57(10) . . ? C3 C2 H2 125.6 . . ? C1 C2 H2 125.6 . . ? Fe C2 H2 125.8 . . ? C2 C3 C4 107.83(17) . . ? C2 C3 Fe 69.79(10) . . ? C4 C3 Fe 69.55(11) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Fe C3 H3 126.2 . . ? C3 C4 C5 108.33(16) . . ? C3 C4 Fe 69.74(11) . . ? C5 C4 Fe 70.37(10) . . ? C3 C4 H4 125.8 . . ? C5 C4 H4 125.8 . . ? Fe C4 H4 125.6 . . ? C4 C5 C1 108.23(16) . . ? C4 C5 Fe 68.98(10) . . ? C1 C5 Fe 70.12(9) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Fe C5 H5 126.6 . . ? C10 C6 C7 107.63(15) . . ? C10 C6 C11 127.28(16) . . ? C7 C6 C11 125.06(16) . . ? C10 C6 Fe 69.85(10) . . ? C7 C6 Fe 69.30(10) . . ? C11 C6 Fe 124.60(11) . . ? C8 C7 C6 107.81(16) . . ? C8 C7 Fe 70.02(10) . . ? C6 C7 Fe 69.65(9) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Fe C7 H7 125.8 . . ? C9 C8 C7 108.63(16) . . ? C9 C8 Fe 69.99(10) . . ? C7 C8 Fe 69.41(10) . . ? C9 C8 H8 125.7 . . ? C7 C8 H8 125.7 . . ? Fe C8 H8 126.5 . . ? C8 C9 C10 108.14(16) . . ? C8 C9 Fe 69.67(10) . . ? C10 C9 Fe 69.68(10) . . ? C8 C9 H9 125.9 . . ? C10 C9 H9 125.9 . . ? Fe C9 H9 126.3 . . ? C9 C10 C6 107.78(16) . . ? C9 C10 Fe 69.68(10) . . ? C6 C10 Fe 69.28(10) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 126.5 . . ? O C11 N1 122.84(16) . . ? O C11 C6 121.85(16) . . ? N1 C11 C6 115.30(16) . . ? C13 C12 C17 118.21(17) . . ? C13 C12 P 124.26(14) . . ? C17 C12 P 117.53(14) . . ? C14 C13 C12 120.88(19) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.8(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 120.36(18) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 119.7(2) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 121.0(2) . . ? C16 C17 H17 119.5 . . ? C12 C17 H17 119.5 . . ? C23 C18 C19 117.31(16) . . ? C23 C18 P 124.88(13) . . ? C19 C18 P 117.76(13) . . ? C20 C19 C18 121.26(16) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 120.46(16) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 119.27(18) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 120.16(18) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 121.48(17) . . ? C22 C23 H23 119.3 . . ? C18 C23 H23 119.3 . . ? N1 C24 C25 113.83(15) . . ? N1 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? N1 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C29 116.53(16) . . ? C26 C25 C24 123.39(16) . . ? C29 C25 C24 120.07(16) . . ? C25 C26 C27 119.46(18) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? N2 C27 C26 124.23(18) . . ? N2 C27 H27 117.9 . . ? C26 C27 H27 117.9 . . ? N2 C28 C29 123.61(18) . . ? N2 C28 H28 118.2 . . ? C29 C28 H28 118.2 . . ? C28 C29 C25 120.15(18) . . ? C28 C29 H29 119.9 . . ? C25 C29 H29 119.9 . . ? H1W O1W H2W 102.2 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.59 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.349 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.047 _chemical_name_common ;N-((4-pyridyl)methyl)-1'- (diphenylphosphino)ferrocenecarboxamide - water (1/1) ; #===END data_jk106 _database_code_depnum_ccdc_archive 'CCDC 670834' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H25 Fe N2 O2 P, H2 O' _chemical_formula_sum 'C29 H27 Fe N2 O3 P' _chemical_formula_weight 538.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.3300(2) _cell_length_b 8.2082(2) _cell_length_c 15.2675(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.283(1) _cell_angle_gamma 90.00 _cell_volume 1242.62(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15979 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.714 _exptl_absorpt_correction_T_max 0.915 _exptl_absorpt_process_details ; numerical absorption correction from crystal shape ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 25645 _diffrn_reflns_av_R_equivalents 0.05s11 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5705 _reflns_number_gt 5308 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _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^)+(0.0386P)^2^+0.3180P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _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 -0.026(10) _chemical_absolute_configuration ad _refine_ls_number_reflns 5705 _refine_ls_number_parameters 328 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.69609(3) 0.34668(3) 0.187131(17) 0.01955(8) Uani 1 1 d . . . P P 0.86060(5) 0.70728(6) 0.20380(4) 0.02049(11) Uani 1 1 d . . . O1P O 0.73552(15) 0.80653(17) 0.17022(10) 0.0267(3) Uani 1 1 d . . . N1 N 0.49746(18) -0.0568(2) 0.18697(13) 0.0258(4) Uani 1 1 d . . . H1N H 0.5702 -0.0848 0.1708 0.032(7) Uiso 1 1 d R . . N2 N 0.6385(2) -0.1297(3) 0.53189(14) 0.0406(5) Uani 1 1 d . . . O O 0.37440(15) 0.1524(2) 0.21516(12) 0.0323(4) Uani 1 1 d . . . C1 C 0.8310(2) 0.5177(3) 0.25231(14) 0.0217(4) Uani 1 1 d . . . C2 C 0.89848(19) 0.3652(3) 0.25134(13) 0.0228(4) Uani 1 1 d . . . H2 H 0.9691 0.3471 0.2259 0.027 Uiso 1 1 calc R . . C3 C 0.8393(2) 0.2470(3) 0.29570(15) 0.0256(5) Uani 1 1 d . . . H3 H 0.8635 0.1377 0.3038 0.031 Uiso 1 1 calc R . . C4 C 0.7358(2) 0.3255(3) 0.32593(13) 0.0257(5) Uani 1 1 d . . . H4 H 0.6813 0.2760 0.3574 0.031 Uiso 1 1 calc R . . C5 C 0.7307(2) 0.4911(3) 0.29987(14) 0.0239(4) Uani 1 1 d . . . H5 H 0.6725 0.5694 0.3115 0.029 Uiso 1 1 calc R . . C6 C 0.5294(2) 0.2088(3) 0.12992(14) 0.0240(4) Uani 1 1 d . . . C7 C 0.4983(2) 0.3791(3) 0.11547(14) 0.0268(5) Uani 1 1 d . . . H7 H 0.4336 0.4360 0.1350 0.032 Uiso 1 1 calc R . . C8 C 0.5838(2) 0.4447(3) 0.06610(15) 0.0310(5) Uani 1 1 d . . . H8 H 0.5851 0.5526 0.0478 0.037 Uiso 1 1 calc R . . C9 C 0.6672(2) 0.3176(3) 0.04928(14) 0.0294(5) Uani 1 1 d . . . H9 H 0.7319 0.3278 0.0179 0.035 Uiso 1 1 calc R . . C10 C 0.6345(2) 0.1724(3) 0.08869(14) 0.0251(5) Uani 1 1 d . . . H10 H 0.6744 0.0710 0.0879 0.030 Uiso 1 1 calc R . . C11 C 0.4624(2) 0.1000(3) 0.18116(15) 0.0244(4) Uani 1 1 d . . . C12 C 0.9857(2) 0.8118(2) 0.29327(14) 0.0234(5) Uani 1 1 d . . . C13 C 1.0754(2) 0.9236(3) 0.27297(16) 0.0264(5) Uani 1 1 d . . . H13 H 1.0789 0.9352 0.2131 0.032 Uiso 1 1 calc R . . C14 C 1.1591(2) 1.0170(3) 0.34139(17) 0.0327(5) Uani 1 1 d . . . H14 H 1.2185 1.0910 0.3273 0.039 Uiso 1 1 calc R . . C15 C 1.1545(2) 1.0002(3) 0.43071(17) 0.0348(5) Uani 1 1 d . . . H15 H 1.2103 1.0633 0.4766 0.042 Uiso 1 1 calc R . . C16 C 1.0670(2) 0.8899(3) 0.45160(17) 0.0363(6) Uani 1 1 d . . . H16 H 1.0641 0.8787 0.5117 0.044 Uiso 1 1 calc R . . C17 C 0.9830(2) 0.7952(3) 0.38352(16) 0.0310(5) Uani 1 1 d . . . H17 H 0.9249 0.7204 0.3983 0.037 Uiso 1 1 calc R . . C18 C 0.9364(2) 0.6627(2) 0.11381(14) 0.0221(4) Uani 1 1 d . . . C19 C 0.8588(2) 0.6833(3) 0.02432(15) 0.0267(5) Uani 1 1 d . . . H19 H 0.7703 0.7194 0.0124 0.032 Uiso 1 1 calc R . . C20 C 0.9125(2) 0.6505(3) -0.04748(17) 0.0321(5) Uani 1 1 d . . . H20 H 0.8600 0.6635 -0.1074 0.039 Uiso 1 1 calc R . . C21 C 1.0451(2) 0.5981(3) -0.02931(17) 0.0346(5) Uani 1 1 d . . . H21 H 1.0819 0.5768 -0.0772 0.042 Uiso 1 1 calc R . . C22 C 1.1220(3) 0.5776(3) 0.05928(18) 0.0333(5) Uani 1 1 d . . . H22 H 1.2106 0.5418 0.0707 0.040 Uiso 1 1 calc R . . C23 C 1.0699(2) 0.6092(3) 0.13196(16) 0.0276(5) Uani 1 1 d . . . H23 H 1.1228 0.5952 0.1917 0.033 Uiso 1 1 calc R . . C24 C 0.4450(2) -0.1675(3) 0.24203(15) 0.0296(4) Uani 1 1 d . . . H24A H 0.4548 -0.2782 0.2225 0.035 Uiso 1 1 calc R . . H24B H 0.3494 -0.1466 0.2314 0.035 Uiso 1 1 calc R . . C25 C 0.5138(2) -0.1542(3) 0.34332(14) 0.0265(4) Uani 1 1 d . . . C26 C 0.6382(2) -0.0796(3) 0.37739(17) 0.0310(5) Uani 1 1 d . . . H26 H 0.6830 -0.0370 0.3375 0.037 Uiso 1 1 calc R . . C27 C 0.6959(3) -0.0684(3) 0.47045(17) 0.0354(5) Uani 1 1 d . . . H27 H 0.7785 -0.0157 0.4915 0.043 Uiso 1 1 calc R . . C28 C 0.5210(3) -0.2060(4) 0.4989(2) 0.0460(7) Uani 1 1 d . . . H28 H 0.4805 -0.2516 0.5404 0.055 Uiso 1 1 calc R . . C29 C 0.4554(3) -0.2217(3) 0.40691(18) 0.0376(6) Uani 1 1 d . . . H29 H 0.3735 -0.2765 0.3878 0.045 Uiso 1 1 calc R . . O1W O 0.3281(3) 0.4561(2) 0.28029(14) 0.0576(6) Uani 1 1 d . . . H1W H 0.3375 0.3548 0.2595 0.098(13) Uiso 1 1 d R . . H2W H 0.3354 0.4302 0.3428 0.110(16) Uiso 1 1 d 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 Fe 0.01706(13) 0.02069(14) 0.01940(13) 0.00098(12) 0.00266(10) 0.00089(12) P 0.0193(2) 0.0203(3) 0.0216(2) 0.0004(2) 0.00542(19) 0.0015(2) O1P 0.0224(7) 0.0273(9) 0.0304(8) 0.0031(6) 0.0075(6) 0.0065(6) N1 0.0228(9) 0.0260(10) 0.0312(10) -0.0006(8) 0.0117(8) -0.0001(7) N2 0.0481(12) 0.0410(13) 0.0344(10) 0.0010(10) 0.0144(9) 0.0052(11) O 0.0246(8) 0.0319(9) 0.0442(10) -0.0039(7) 0.0163(7) 0.0006(7) C1 0.0202(10) 0.0231(10) 0.0197(10) -0.0002(8) 0.0020(8) -0.0015(8) C2 0.0160(8) 0.0243(11) 0.0251(9) 0.0016(9) 0.0006(7) 0.0017(8) C3 0.0225(10) 0.0229(11) 0.0254(11) 0.0042(9) -0.0031(9) 0.0025(9) C4 0.0266(10) 0.0313(13) 0.0181(9) 0.0027(9) 0.0044(8) -0.0034(10) C5 0.0233(10) 0.0261(11) 0.0222(10) -0.0031(9) 0.0063(8) 0.0004(9) C6 0.0176(9) 0.0283(11) 0.0228(10) -0.0032(9) 0.0002(8) -0.0008(9) C7 0.0177(9) 0.0287(13) 0.0282(11) 0.0016(9) -0.0029(8) 0.0034(8) C8 0.0298(12) 0.0316(12) 0.0243(11) 0.0073(9) -0.0043(9) -0.0029(10) C9 0.0300(11) 0.0369(15) 0.0199(9) -0.0012(9) 0.0045(8) -0.0061(10) C10 0.0251(11) 0.0276(12) 0.0213(10) -0.0045(9) 0.0047(8) -0.0041(9) C11 0.0168(10) 0.0271(11) 0.0260(11) -0.0045(9) 0.0006(8) -0.0012(8) C12 0.0220(9) 0.0212(12) 0.0264(10) -0.0001(8) 0.0060(8) 0.0021(8) C13 0.0250(11) 0.0276(11) 0.0282(11) 0.0011(9) 0.0099(9) -0.0008(9) C14 0.0254(11) 0.0337(12) 0.0395(13) -0.0022(10) 0.0096(10) -0.0029(10) C15 0.0299(12) 0.0387(13) 0.0324(12) -0.0084(11) 0.0028(10) -0.0051(11) C16 0.0358(13) 0.0469(16) 0.0246(11) -0.0034(10) 0.0055(9) -0.0039(11) C17 0.0291(11) 0.0360(13) 0.0278(12) 0.0000(9) 0.0078(9) -0.0054(9) C18 0.0211(10) 0.0212(10) 0.0239(10) 0.0004(8) 0.0062(8) 0.0010(8) C19 0.0202(10) 0.0313(12) 0.0280(11) -0.0011(9) 0.0058(8) -0.0015(9) C20 0.0292(12) 0.0399(14) 0.0269(12) -0.0022(10) 0.0072(10) -0.0016(10) C21 0.0340(13) 0.0418(14) 0.0329(12) -0.0072(11) 0.0171(11) -0.0020(11) C22 0.0243(12) 0.0395(13) 0.0377(13) -0.0023(11) 0.0112(10) 0.0063(10) C23 0.0235(11) 0.0284(12) 0.0290(12) 0.0000(9) 0.0042(9) 0.0021(9) C24 0.0277(10) 0.0256(11) 0.0368(11) -0.0001(11) 0.0113(9) -0.0018(10) C25 0.0270(10) 0.0210(9) 0.0345(10) -0.0008(11) 0.0133(8) 0.0032(11) C26 0.0303(12) 0.0317(12) 0.0336(12) 0.0007(10) 0.0131(10) -0.0021(10) C27 0.0337(13) 0.0358(13) 0.0366(13) 0.0018(11) 0.0095(11) -0.0002(11) C28 0.0528(16) 0.0524(18) 0.0418(14) 0.0037(12) 0.0278(13) -0.0039(13) C29 0.0378(13) 0.0386(13) 0.0422(14) 0.0009(11) 0.0205(12) -0.0061(11) O1W 0.0969(18) 0.0361(11) 0.0353(11) 0.0024(8) 0.0113(11) 0.0240(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C1 2.031(2) . ? Fe C5 2.037(2) . ? Fe C6 2.041(2) . ? Fe C10 2.043(2) . ? Fe C7 2.047(2) . ? Fe C4 2.050(2) . ? Fe C8 2.051(2) . ? Fe C2 2.0508(19) . ? Fe C9 2.055(2) . ? Fe C3 2.057(2) . ? P O1P 1.4914(15) . ? P C1 1.787(2) . ? P C18 1.799(2) . ? P C12 1.811(2) . ? N1 C11 1.333(3) . ? N1 C24 1.443(3) . ? N1 H1N 0.8841 . ? N2 C28 1.332(4) . ? N2 C27 1.340(3) . ? O C11 1.243(3) . ? C1 C2 1.435(3) . ? C1 C5 1.438(3) . ? C2 C3 1.416(3) . ? C2 H2 0.9300 . ? C3 C4 1.431(3) . ? C3 H3 0.9300 . ? C4 C5 1.413(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.430(3) . ? C6 C7 1.437(3) . ? C6 C11 1.480(3) . ? C7 C8 1.418(3) . ? C7 H7 0.9300 . ? C8 C9 1.421(3) . ? C8 H8 0.9300 . ? C9 C10 1.418(3) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C17 1.392(3) . ? C12 C13 1.399(3) . ? C13 C14 1.386(3) . ? C13 H13 0.9300 . ? C14 C15 1.385(3) . ? C14 H14 0.9300 . ? C15 C16 1.378(4) . ? C15 H15 0.9300 . ? C16 C17 1.390(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.387(3) . ? C18 C23 1.399(3) . ? C19 C20 1.386(3) . ? C19 H19 0.9300 . ? C20 C21 1.387(3) . ? C20 H20 0.9300 . ? C21 C22 1.374(4) . ? C21 H21 0.9300 . ? C22 C23 1.387(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.514(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.387(3) . ? C25 C29 1.393(3) . ? C26 C27 1.381(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.384(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? O1W H1W 0.9044 . ? O1W H2W 0.9592 . ? 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 C1 Fe C5 41.41(9) . . ? C1 Fe C6 166.80(9) . . ? C5 Fe C6 127.69(9) . . ? C1 Fe C10 150.92(8) . . ? C5 Fe C10 166.80(8) . . ? C6 Fe C10 41.00(8) . . ? C1 Fe C7 128.11(9) . . ? C5 Fe C7 106.77(9) . . ? C6 Fe C7 41.16(9) . . ? C10 Fe C7 68.86(9) . . ? C1 Fe C4 68.96(9) . . ? C5 Fe C4 40.46(9) . . ? C6 Fe C4 107.21(9) . . ? C10 Fe C4 129.18(9) . . ? C7 Fe C4 116.37(9) . . ? C1 Fe C8 107.91(9) . . ? C5 Fe C8 117.00(9) . . ? C6 Fe C8 68.63(9) . . ? C10 Fe C8 68.35(10) . . ? C7 Fe C8 40.51(9) . . ? C4 Fe C8 149.72(10) . . ? C1 Fe C2 41.16(9) . . ? C5 Fe C2 68.84(9) . . ? C6 Fe C2 150.51(9) . . ? C10 Fe C2 117.98(9) . . ? C7 Fe C2 167.70(9) . . ? C4 Fe C2 68.30(8) . . ? C8 Fe C2 130.16(9) . . ? C1 Fe C9 117.71(9) . . ? C5 Fe C9 150.88(9) . . ? C6 Fe C9 68.54(9) . . ? C10 Fe C9 40.49(9) . . ? C7 Fe C9 68.35(9) . . ? C4 Fe C9 168.06(10) . . ? C8 Fe C9 40.51(10) . . ? C2 Fe C9 109.52(9) . . ? C1 Fe C3 68.92(9) . . ? C5 Fe C3 68.56(9) . . ? C6 Fe C3 117.02(9) . . ? C10 Fe C3 108.63(9) . . ? C7 Fe C3 150.13(9) . . ? C4 Fe C3 40.79(9) . . ? C8 Fe C3 168.39(10) . . ? C2 Fe C3 40.33(9) . . ? C9 Fe C3 130.10(9) . . ? O1P P C1 112.69(9) . . ? O1P P C18 111.66(9) . . ? C1 P C18 107.53(10) . . ? O1P P C12 111.51(9) . . ? C1 P C12 105.59(9) . . ? C18 P C12 107.51(10) . . ? C11 N1 C24 120.50(19) . . ? C11 N1 H1N 117.9 . . ? C24 N1 H1N 119.1 . . ? C28 N2 C27 116.5(2) . . ? C2 C1 C5 107.08(18) . . ? C2 C1 P 127.97(16) . . ? C5 C1 P 124.94(16) . . ? C2 C1 Fe 70.17(11) . . ? C5 C1 Fe 69.53(12) . . ? P C1 Fe 124.94(11) . . ? C3 C2 C1 108.46(18) . . ? C3 C2 Fe 70.07(11) . . ? C1 C2 Fe 68.67(11) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Fe C2 H2 127.1 . . ? C2 C3 C4 107.89(19) . . ? C2 C3 Fe 69.60(11) . . ? C4 C3 Fe 69.33(12) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Fe C3 H3 126.6 . . ? C5 C4 C3 108.34(19) . . ? C5 C4 Fe 69.29(12) . . ? C3 C4 Fe 69.88(12) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe C4 H4 126.6 . . ? C4 C5 C1 108.22(19) . . ? C4 C5 Fe 70.25(12) . . ? C1 C5 Fe 69.05(12) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Fe C5 H5 126.4 . . ? C10 C6 C7 107.5(2) . . ? C10 C6 C11 129.1(2) . . ? C7 C6 C11 123.4(2) . . ? C10 C6 Fe 69.59(12) . . ? C7 C6 Fe 69.65(12) . . ? C11 C6 Fe 124.85(14) . . ? C8 C7 C6 107.7(2) . . ? C8 C7 Fe 69.89(12) . . ? C6 C7 Fe 69.19(11) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? Fe C7 H7 126.4 . . ? C7 C8 C9 108.4(2) . . ? C7 C8 Fe 69.61(12) . . ? C9 C8 Fe 69.91(13) . . ? C7 C8 H8 125.8 . . ? C9 C8 H8 125.8 . . ? Fe C8 H8 126.3 . . ? C10 C9 C8 108.2(2) . . ? C10 C9 Fe 69.31(12) . . ? C8 C9 Fe 69.58(13) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Fe C9 H9 126.8 . . ? C9 C10 C6 108.1(2) . . ? C9 C10 Fe 70.20(12) . . ? C6 C10 Fe 69.40(12) . . ? C9 C10 H10 125.9 . . ? C6 C10 H10 125.9 . . ? Fe C10 H10 126.0 . . ? O C11 N1 121.5(2) . . ? O C11 C6 121.1(2) . . ? N1 C11 C6 117.34(19) . . ? C17 C12 C13 118.8(2) . . ? C17 C12 P 119.48(16) . . ? C13 C12 P 121.35(17) . . ? C14 C13 C12 120.5(2) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 120.0(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 120.0(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.4(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 120.3(2) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C19 C18 C23 119.9(2) . . ? C19 C18 P 118.19(16) . . ? C23 C18 P 121.90(16) . . ? C20 C19 C18 120.4(2) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.6(2) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 121.2(2) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.8(2) . . ? C22 C23 H23 120.6 . . ? C18 C23 H23 120.6 . . ? N1 C24 C25 113.82(19) . . ? N1 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? N1 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 C29 116.8(2) . . ? C26 C25 C24 122.38(19) . . ? C29 C25 C24 120.8(2) . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? N2 C27 C26 123.2(2) . . ? N2 C27 H27 118.4 . . ? C26 C27 H27 118.4 . . ? N2 C28 C29 124.2(2) . . ? N2 C28 H28 117.9 . . ? C29 C28 H28 117.9 . . ? C28 C29 C25 119.1(2) . . ? C28 C29 H29 120.5 . . ? C25 C29 H29 120.5 . . ? H1W O1W H2W 99.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.299 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.054 #===END data_jk81x _database_code_depnum_ccdc_archive 'CCDC 670835' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H25 Br2 Cd Fe N2 O P' _chemical_formula_sum 'C29 H25 Br2 Cd Fe N2 O P' _chemical_formula_weight 776.55 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' 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' O O 0.0106 0.0060 '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' Cd Cd -0.8075 1.2024 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2861(2) _cell_length_b 14.8660(3) _cell_length_c 20.5346(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.294(1) _cell_angle_gamma 90.00 _cell_volume 2830.06(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30360 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.10 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 4.170 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.540 _exptl_absorpt_correction_T_max 0.744 _exptl_absorpt_process_details ; gaussian absorption correction based on indexed crystal shape ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 41043 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6237 _reflns_number_gt 4876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _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^)+(0.0302P)^2^+3.7097P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6237 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0334 _refine_ls_wR_factor_ref 0.0767 _refine_ls_wR_factor_gt 0.0692 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.60661(3) 0.267758(17) 0.359572(13) 0.02981(8) Uani 1 1 d . . . Br1 Br 0.41824(4) 0.39089(2) 0.35134(2) 0.04047(11) Uani 1 1 d . . . Br2 Br 0.55280(4) 0.11066(2) 0.31500(2) 0.03960(11) Uani 1 1 d . . . Fe Fe 0.52256(5) 0.21565(3) 0.57868(2) 0.02306(11) Uani 1 1 d . . . P P 0.76885(9) 0.24580(5) 0.46437(5) 0.02425(19) Uani 1 1 d . . . O O 0.1236(3) 0.14977(16) 0.59747(13) 0.0362(6) Uani 1 1 d . . . N1 N 0.2553(3) 0.1292(2) 0.69166(16) 0.0346(7) Uani 1 1 d . . . H1N H 0.3390 0.1303 0.7276 0.12(2) Uiso 1 1 d R . . N2 N -0.2257(3) 0.1732(2) 0.79322(15) 0.0340(7) Uani 1 1 d . . . C1 C 0.6850(3) 0.1759(2) 0.52210(17) 0.0244(7) Uani 1 1 d . . . C2 C 0.5572(4) 0.1236(2) 0.50787(18) 0.0284(8) Uani 1 1 d . . . H2 H 0.5064 0.1193 0.4676 0.034 Uiso 1 1 calc R . . C3 C 0.5220(4) 0.0792(2) 0.56636(19) 0.0314(8) Uani 1 1 d . . . H3 H 0.4443 0.0407 0.5709 0.038 Uiso 1 1 calc R . . C4 C 0.6245(4) 0.1037(2) 0.61589(19) 0.0338(8) Uani 1 1 d . . . H4 H 0.6260 0.0841 0.6589 0.041 Uiso 1 1 calc R . . C5 C 0.7256(4) 0.1632(2) 0.58997(19) 0.0309(8) Uani 1 1 d . . . H5 H 0.8042 0.1894 0.6128 0.037 Uiso 1 1 calc R . . C6 C 0.3304(4) 0.2418(2) 0.61622(19) 0.0305(8) Uani 1 1 d . . . C7 C 0.4441(4) 0.2824(2) 0.6560(2) 0.0371(9) Uani 1 1 d . . . H7 H 0.4664 0.2706 0.6999 0.044 Uiso 1 1 calc R . . C8 C 0.5165(4) 0.3440(2) 0.6163(2) 0.0405(10) Uani 1 1 d . . . H8 H 0.5955 0.3794 0.6297 0.049 Uiso 1 1 calc R . . C9 C 0.4482(4) 0.3425(2) 0.5531(2) 0.0357(9) Uani 1 1 d . . . H9 H 0.4743 0.3769 0.5178 0.043 Uiso 1 1 calc R . . C10 C 0.3339(4) 0.2801(2) 0.55243(19) 0.0316(8) Uani 1 1 d . . . H10 H 0.2716 0.2662 0.5167 0.038 Uiso 1 1 calc R . . C11 C 0.2284(4) 0.1698(2) 0.63344(18) 0.0300(8) Uani 1 1 d . . . C12 C 0.9293(3) 0.1862(2) 0.44132(17) 0.0258(7) Uani 1 1 d . . . C13 C 0.9344(4) 0.0928(2) 0.44107(18) 0.0303(8) Uani 1 1 d . . . H13 H 0.8577 0.0598 0.4559 0.036 Uiso 1 1 calc R . . C14 C 1.0535(4) 0.0487(2) 0.4187(2) 0.0372(9) Uani 1 1 d . . . H14 H 1.0571 -0.0138 0.4192 0.045 Uiso 1 1 calc R . . C15 C 1.1673(4) 0.0972(2) 0.3957(2) 0.0345(8) Uani 1 1 d . . . H15 H 1.2473 0.0674 0.3809 0.041 Uiso 1 1 calc R . . C16 C 1.1612(4) 0.1894(2) 0.3947(2) 0.0362(9) Uani 1 1 d . . . H16 H 1.2368 0.2221 0.3786 0.043 Uiso 1 1 calc R . . C17 C 1.0436(4) 0.2343(2) 0.41756(19) 0.0321(8) Uani 1 1 d . . . H17 H 1.0410 0.2969 0.4170 0.039 Uiso 1 1 calc R . . C18 C 0.8368(3) 0.3438(2) 0.50893(18) 0.0263(7) Uani 1 1 d . . . C19 C 0.9488(4) 0.3354(2) 0.55659(19) 0.0314(8) Uani 1 1 d . . . H19 H 0.9949 0.2804 0.5631 0.038 Uiso 1 1 calc R . . C20 C 0.9915(4) 0.4086(2) 0.5940(2) 0.0368(9) Uani 1 1 d . . . H20 H 1.0660 0.4028 0.6260 0.044 Uiso 1 1 calc R . . C21 C 0.9232(4) 0.4911(2) 0.5841(2) 0.0378(9) Uani 1 1 d . . . H21 H 0.9504 0.5400 0.6103 0.045 Uiso 1 1 calc R . . C22 C 0.8160(4) 0.5006(2) 0.53589(19) 0.0338(8) Uani 1 1 d . . . H22 H 0.7726 0.5564 0.5287 0.041 Uiso 1 1 calc R . . C23 C 0.7720(4) 0.4276(2) 0.49770(19) 0.0301(8) Uani 1 1 d . . . H23 H 0.6998 0.4343 0.4648 0.036 Uiso 1 1 calc R . . C24 C 0.1558(4) 0.0628(2) 0.7144(2) 0.0355(8) Uani 1 1 d . . . H24A H 0.2043 0.0280 0.7491 0.043 Uiso 1 1 calc R . . H24B H 0.1296 0.0218 0.6789 0.043 Uiso 1 1 calc R . . C25 C 0.0194(4) 0.1030(2) 0.73931(18) 0.0314(8) Uani 1 1 d . . . C26 C -0.0927(4) 0.0481(2) 0.75649(19) 0.0348(8) Uani 1 1 d . . . H26 H -0.0876 -0.0136 0.7494 0.042 Uiso 1 1 calc R . . C27 C -0.2111(4) 0.0838(2) 0.78385(18) 0.0333(8) Uani 1 1 d . . . H27 H -0.2836 0.0453 0.7963 0.040 Uiso 1 1 calc R . . C28 C -0.1218(4) 0.2268(3) 0.7733(2) 0.0424(10) Uani 1 1 d . . . H28 H -0.1329 0.2886 0.7774 0.051 Uiso 1 1 calc R . . C29 C 0.0016(4) 0.1945(3) 0.7469(2) 0.0408(10) Uani 1 1 d . . . H29 H 0.0723 0.2343 0.7344 0.049 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 Cd 0.02503(13) 0.03248(14) 0.03238(16) 0.00437(11) 0.00562(10) 0.00207(10) Br1 0.0339(2) 0.0372(2) 0.0504(3) 0.00319(17) 0.00331(17) 0.00958(16) Br2 0.0512(2) 0.03150(19) 0.0364(2) 0.00224(16) 0.00554(17) -0.00076(16) Fe 0.0212(2) 0.0224(2) 0.0258(3) -0.00128(19) 0.00303(19) 0.00244(18) P 0.0198(4) 0.0236(4) 0.0297(5) 0.0006(3) 0.0045(3) 0.0024(3) O 0.0325(14) 0.0355(13) 0.0402(17) 0.0052(12) -0.0006(12) -0.0017(11) N1 0.0280(15) 0.0429(17) 0.0336(19) 0.0070(14) 0.0078(14) 0.0037(13) N2 0.0322(16) 0.0379(17) 0.0327(18) -0.0019(14) 0.0100(13) -0.0003(13) C1 0.0211(16) 0.0256(16) 0.0269(19) 0.0013(14) 0.0057(13) 0.0059(13) C2 0.0299(18) 0.0231(16) 0.033(2) -0.0052(14) 0.0097(15) 0.0008(14) C3 0.0349(19) 0.0185(15) 0.042(2) -0.0010(14) 0.0157(17) 0.0014(14) C4 0.0337(19) 0.0327(18) 0.035(2) 0.0097(16) 0.0056(16) 0.0108(15) C5 0.0233(17) 0.0311(18) 0.038(2) 0.0061(15) -0.0002(15) 0.0083(14) C6 0.0249(17) 0.0304(17) 0.037(2) -0.0036(15) 0.0100(15) 0.0055(14) C7 0.045(2) 0.0345(19) 0.033(2) -0.0120(16) 0.0114(17) -0.0002(16) C8 0.040(2) 0.0278(18) 0.055(3) -0.0141(18) 0.0113(19) -0.0025(16) C9 0.0332(19) 0.0254(17) 0.049(3) 0.0074(16) 0.0099(17) 0.0102(15) C10 0.0236(17) 0.0321(18) 0.039(2) 0.0046(16) 0.0053(15) 0.0096(14) C11 0.0273(18) 0.0306(17) 0.033(2) -0.0017(15) 0.0101(16) 0.0075(15) C12 0.0213(16) 0.0281(17) 0.028(2) 0.0008(14) 0.0008(14) 0.0036(13) C13 0.0275(17) 0.0273(17) 0.037(2) -0.0003(15) 0.0067(15) -0.0013(14) C14 0.036(2) 0.0263(18) 0.050(3) -0.0021(17) 0.0075(18) 0.0076(15) C15 0.0248(17) 0.0369(19) 0.042(2) -0.0058(17) 0.0061(16) 0.0073(15) C16 0.0245(17) 0.039(2) 0.046(2) -0.0022(17) 0.0110(16) -0.0025(15) C17 0.0274(17) 0.0274(17) 0.042(2) -0.0020(16) 0.0080(16) 0.0005(14) C18 0.0203(16) 0.0230(16) 0.036(2) 0.0000(14) 0.0076(14) 0.0006(13) C19 0.0274(18) 0.0252(17) 0.041(2) 0.0014(15) 0.0012(16) 0.0038(14) C20 0.034(2) 0.0355(19) 0.041(2) -0.0016(17) -0.0035(17) -0.0007(16) C21 0.042(2) 0.0279(18) 0.044(3) -0.0090(16) 0.0058(18) -0.0019(16) C22 0.036(2) 0.0220(16) 0.044(2) -0.0004(15) 0.0085(17) 0.0047(15) C23 0.0251(17) 0.0287(17) 0.037(2) 0.0041(15) 0.0047(15) 0.0035(14) C24 0.0315(19) 0.040(2) 0.036(2) 0.0059(17) 0.0084(16) 0.0041(16) C25 0.0316(18) 0.0372(19) 0.026(2) 0.0019(15) 0.0066(15) 0.0036(15) C26 0.038(2) 0.0300(18) 0.037(2) 0.0006(16) 0.0086(17) 0.0006(15) C27 0.0331(19) 0.0371(19) 0.031(2) -0.0008(15) 0.0079(16) -0.0059(16) C28 0.044(2) 0.037(2) 0.047(3) -0.0045(18) 0.0177(19) 0.0012(18) C29 0.038(2) 0.037(2) 0.049(3) -0.0045(18) 0.0211(18) -0.0077(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 Cd N2 2.301(3) 4_665 ? Cd Br1 2.5308(4) . ? Cd Br2 2.5475(5) . ? Cd P 2.5758(10) . ? Fe C6 2.022(3) . ? Fe C2 2.036(3) . ? Fe C4 2.041(3) . ? Fe C5 2.041(3) . ? Fe C10 2.042(3) . ? Fe C7 2.042(4) . ? Fe C1 2.043(3) . ? Fe C3 2.044(3) . ? Fe C8 2.061(4) . ? Fe C9 2.065(3) . ? P C1 1.788(3) . ? P C18 1.814(3) . ? P C12 1.820(3) . ? O C11 1.224(4) . ? N1 C11 1.350(5) . ? N1 C24 1.448(5) . ? N1 H1N 1.0402 . ? N2 C28 1.333(5) . ? N2 C27 1.352(5) . ? N2 Cd 2.301(3) 4_466 ? C1 C2 1.435(5) . ? C1 C5 1.435(5) . ? C2 C3 1.425(5) . ? C2 H2 0.9300 . ? C3 C4 1.401(5) . ? C3 H3 0.9300 . ? C4 C5 1.415(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.430(5) . ? C6 C7 1.431(5) . ? C6 C11 1.486(5) . ? C7 C8 1.421(5) . ? C7 H7 0.9300 . ? C8 C9 1.412(6) . ? C8 H8 0.9300 . ? C9 C10 1.410(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C13 1.389(5) . ? C12 C17 1.391(5) . ? C13 C14 1.387(5) . ? C13 H13 0.9300 . ? C14 C15 1.384(5) . ? C14 H14 0.9300 . ? C15 C16 1.373(5) . ? C15 H15 0.9300 . ? C16 C17 1.385(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.393(5) . ? C18 C23 1.396(5) . ? C19 C20 1.377(5) . ? C19 H19 0.9300 . ? C20 C21 1.391(5) . ? C20 H20 0.9300 . ? C21 C22 1.370(6) . ? C21 H21 0.9300 . ? C22 C23 1.388(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.516(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C29 1.381(5) . ? C25 C26 1.385(5) . ? C26 C27 1.370(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.381(5) . ? C28 H28 0.9300 . ? C29 H29 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 N2 Cd Br1 99.99(8) 4_665 . ? N2 Cd Br2 105.20(8) 4_665 . ? Br1 Cd Br2 121.233(17) . . ? N2 Cd P 99.19(8) 4_665 . ? Br1 Cd P 121.09(2) . . ? Br2 Cd P 106.10(2) . . ? C6 Fe C2 125.51(14) . . ? C6 Fe C4 114.50(15) . . ? C2 Fe C4 68.30(15) . . ? C6 Fe C5 149.30(15) . . ? C2 Fe C5 68.99(15) . . ? C4 Fe C5 40.57(14) . . ? C6 Fe C10 41.21(15) . . ? C2 Fe C10 107.17(15) . . ? C4 Fe C10 148.63(14) . . ? C5 Fe C10 169.17(14) . . ? C6 Fe C7 41.22(15) . . ? C2 Fe C7 163.77(14) . . ? C4 Fe C7 106.48(16) . . ? C5 Fe C7 117.77(16) . . ? C10 Fe C7 68.79(16) . . ? C6 Fe C1 165.68(15) . . ? C2 Fe C1 41.20(13) . . ? C4 Fe C1 68.63(14) . . ? C5 Fe C1 41.14(14) . . ? C10 Fe C1 129.47(14) . . ? C7 Fe C1 152.95(15) . . ? C6 Fe C3 104.00(14) . . ? C2 Fe C3 40.87(14) . . ? C4 Fe C3 40.12(15) . . ? C5 Fe C3 68.34(14) . . ? C10 Fe C3 115.88(15) . . ? C7 Fe C3 125.45(15) . . ? C1 Fe C3 68.88(13) . . ? C6 Fe C8 68.61(14) . . ? C2 Fe C8 154.06(15) . . ? C4 Fe C8 129.53(17) . . ? C5 Fe C8 110.85(16) . . ? C10 Fe C8 67.88(16) . . ? C7 Fe C8 40.52(15) . . ? C1 Fe C8 121.17(14) . . ? C3 Fe C8 164.88(16) . . ? C6 Fe C9 68.40(14) . . ? C2 Fe C9 119.77(16) . . ? C4 Fe C9 168.66(16) . . ? C5 Fe C9 132.12(14) . . ? C10 Fe C9 40.14(14) . . ? C7 Fe C9 67.97(16) . . ? C1 Fe C9 111.48(14) . . ? C3 Fe C9 151.16(16) . . ? C8 Fe C9 40.01(17) . . ? C1 P C18 106.51(16) . . ? C1 P C12 106.50(15) . . ? C18 P C12 104.84(15) . . ? C1 P Cd 111.81(11) . . ? C18 P Cd 119.29(12) . . ? C12 P Cd 107.03(12) . . ? C11 N1 C24 120.1(3) . . ? C11 N1 H1N 135.6 . . ? C24 N1 H1N 104.3 . . ? C28 N2 C27 117.6(3) . . ? C28 N2 Cd 118.7(2) . 4_466 ? C27 N2 Cd 122.4(2) . 4_466 ? C2 C1 C5 107.1(3) . . ? C2 C1 P 124.5(3) . . ? C5 C1 P 128.3(3) . . ? C2 C1 Fe 69.14(17) . . ? C5 C1 Fe 69.35(18) . . ? P C1 Fe 124.97(16) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 Fe 69.86(19) . . ? C1 C2 Fe 69.67(18) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Fe C2 H2 126.0 . . ? C4 C3 C2 108.2(3) . . ? C4 C3 Fe 69.83(19) . . ? C2 C3 Fe 69.27(18) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe C3 H3 126.6 . . ? C3 C4 C5 109.1(3) . . ? C3 C4 Fe 70.06(19) . . ? C5 C4 Fe 69.72(19) . . ? C3 C4 H4 125.4 . . ? C5 C4 H4 125.4 . . ? Fe C4 H4 126.4 . . ? C4 C5 C1 107.7(3) . . ? C4 C5 Fe 69.71(19) . . ? C1 C5 Fe 69.51(18) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe C5 H5 126.2 . . ? C10 C6 C7 107.5(3) . . ? C10 C6 C11 123.5(3) . . ? C7 C6 C11 128.9(4) . . ? C10 C6 Fe 70.15(19) . . ? C7 C6 Fe 70.2(2) . . ? C11 C6 Fe 122.7(2) . . ? C8 C7 C6 107.6(4) . . ? C8 C7 Fe 70.5(2) . . ? C6 C7 Fe 68.6(2) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? Fe C7 H7 126.3 . . ? C9 C8 C7 108.3(3) . . ? C9 C8 Fe 70.2(2) . . ? C7 C8 Fe 69.0(2) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe C8 H8 126.5 . . ? C10 C9 C8 108.6(3) . . ? C10 C9 Fe 69.02(19) . . ? C8 C9 Fe 69.8(2) . . ? C10 C9 H9 125.7 . . ? C8 C9 H9 125.7 . . ? Fe C9 H9 127.0 . . ? C9 C10 C6 108.0(3) . . ? C9 C10 Fe 70.84(19) . . ? C6 C10 Fe 68.64(19) . . ? C9 C10 H10 126.0 . . ? C6 C10 H10 126.0 . . ? Fe C10 H10 126.1 . . ? O C11 N1 121.8(3) . . ? O C11 C6 121.8(3) . . ? N1 C11 C6 116.4(3) . . ? C13 C12 C17 119.1(3) . . ? C13 C12 P 121.1(2) . . ? C17 C12 P 119.5(2) . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 120.2(3) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C19 C18 C23 119.5(3) . . ? C19 C18 P 120.4(2) . . ? C23 C18 P 119.9(3) . . ? C20 C19 C18 120.1(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.1(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.2(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 119.7(3) . . ? C22 C23 H23 120.2 . . ? C18 C23 H23 120.2 . . ? N1 C24 C25 113.6(3) . . ? N1 C24 H24A 108.8 . . ? C25 C24 H24A 108.8 . . ? N1 C24 H24B 108.8 . . ? C25 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C29 C25 C26 117.1(3) . . ? C29 C25 C24 122.3(3) . . ? C26 C25 C24 120.6(3) . . ? C27 C26 C25 120.6(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? N2 C27 C26 121.9(3) . . ? N2 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? N2 C28 C29 123.0(4) . . ? N2 C28 H28 118.5 . . ? C29 C28 H28 118.5 . . ? C28 C29 C25 119.6(3) . . ? C28 C29 H29 120.2 . . ? C25 C29 H29 120.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.893 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.098 #===END data_jk83c _database_code_depnum_ccdc_archive 'CCDC 670836' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H25 Br2 Fe Hg N2 O P' _chemical_formula_sum 'C29 H25 Br2 Fe Hg N2 O P' _chemical_formula_weight 864.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2514(1) _cell_length_b 14.8207(3) _cell_length_c 20.5550(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.376(1) _cell_angle_gamma 90.00 _cell_volume 2813.45(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27616 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 8.889 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.135 _exptl_absorpt_correction_T_max 0.529 _exptl_absorpt_process_details ; gaussian integration based on indexed crystal shape (Coppens, 1970) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 45710 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.53 _reflns_number_total 6456 _reflns_number_gt 5458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _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^)+(0.0309P)^2^+5.2644P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6456 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg Hg 0.607448(16) 0.270054(11) 0.371612(7) 0.03078(6) Uani 1 1 d . . . Br1 Br 0.41656(5) 0.39141(3) 0.34953(2) 0.04104(11) Uani 1 1 d . . . Br2 Br 0.54844(5) 0.11612(3) 0.31558(2) 0.04070(11) Uani 1 1 d . . . Fe Fe 0.52353(5) 0.21546(3) 0.57987(3) 0.02275(11) Uani 1 1 d . . . P P 0.77187(10) 0.24485(6) 0.46697(5) 0.02324(19) Uani 1 1 d . . . O O 0.1236(3) 0.14909(19) 0.59727(14) 0.0363(6) Uani 1 1 d . . . N1 N 0.2548(4) 0.1277(2) 0.69194(16) 0.0326(7) Uani 1 1 d . . . H1N H 0.3456 0.1461 0.7186 0.039 Uiso 1 1 d R . . N2 N -0.2274(4) 0.1695(3) 0.79440(17) 0.0374(8) Uani 1 1 d . . . C1 C 0.6864(4) 0.1746(2) 0.52424(18) 0.0245(7) Uani 1 1 d . . . C2 C 0.5581(4) 0.1223(2) 0.50967(19) 0.0284(8) Uani 1 1 d . . . H2 H 0.5077 0.1180 0.4693 0.034 Uiso 1 1 calc R . . C3 C 0.5220(5) 0.0786(3) 0.5677(2) 0.0329(9) Uani 1 1 d . . . H3 H 0.4437 0.0401 0.5720 0.039 Uiso 1 1 calc R . . C4 C 0.6251(4) 0.1034(3) 0.6179(2) 0.0339(9) Uani 1 1 d . . . H4 H 0.6259 0.0842 0.6610 0.041 Uiso 1 1 calc R . . C5 C 0.7270(4) 0.1622(3) 0.5917(2) 0.0311(8) Uani 1 1 d . . . H5 H 0.8063 0.1882 0.6144 0.037 Uiso 1 1 calc R . . C6 C 0.3302(4) 0.2415(3) 0.6174(2) 0.0304(8) Uani 1 1 d . . . C7 C 0.4451(5) 0.2818(3) 0.6569(2) 0.0358(10) Uani 1 1 d . . . H7 H 0.4682 0.2693 0.7006 0.043 Uiso 1 1 calc R . . C8 C 0.5172(5) 0.3439(3) 0.6180(2) 0.0401(10) Uani 1 1 d . . . H8 H 0.5960 0.3794 0.6318 0.048 Uiso 1 1 calc R . . C9 C 0.4495(4) 0.3430(3) 0.5547(2) 0.0365(10) Uani 1 1 d . . . H9 H 0.4763 0.3777 0.5198 0.044 Uiso 1 1 calc R . . C10 C 0.3341(4) 0.2805(3) 0.5534(2) 0.0333(9) Uani 1 1 d . . . H10 H 0.2718 0.2670 0.5176 0.040 Uiso 1 1 calc R . . C11 C 0.2288(4) 0.1695(3) 0.63380(19) 0.0296(8) Uani 1 1 d . . . C12 C 0.9312(4) 0.1857(2) 0.44197(17) 0.0243(7) Uani 1 1 d . . . C13 C 1.0451(4) 0.2346(3) 0.4188(2) 0.0317(9) Uani 1 1 d . . . H13 H 1.0421 0.2973 0.4191 0.038 Uiso 1 1 calc R . . C14 C 1.1634(4) 0.1908(3) 0.3951(2) 0.0386(10) Uani 1 1 d . . . H14 H 1.2387 0.2239 0.3789 0.046 Uiso 1 1 calc R . . C15 C 1.1688(4) 0.0973(3) 0.3958(2) 0.0350(9) Uani 1 1 d . . . H15 H 1.2489 0.0675 0.3808 0.042 Uiso 1 1 calc R . . C16 C 1.0554(4) 0.0484(3) 0.4185(2) 0.0345(9) Uani 1 1 d . . . H16 H 1.0590 -0.0143 0.4186 0.041 Uiso 1 1 calc R . . C17 C 0.9359(4) 0.0924(3) 0.44140(19) 0.0296(8) Uani 1 1 d . . . H17 H 0.8591 0.0592 0.4563 0.036 Uiso 1 1 calc R . . C18 C 0.8380(4) 0.3442(2) 0.51020(18) 0.0252(8) Uani 1 1 d . . . C19 C 0.7727(4) 0.4279(3) 0.4984(2) 0.0291(8) Uani 1 1 d . . . H19 H 0.7003 0.4343 0.4654 0.035 Uiso 1 1 calc R . . C20 C 0.8168(5) 0.5017(3) 0.5364(2) 0.0350(9) Uani 1 1 d . . . H20 H 0.7733 0.5576 0.5290 0.042 Uiso 1 1 calc R . . C21 C 0.9242(5) 0.4920(3) 0.5847(2) 0.0385(10) Uani 1 1 d . . . H21 H 0.9511 0.5411 0.6109 0.046 Uiso 1 1 calc R . . C22 C 0.9928(5) 0.4098(3) 0.5949(2) 0.0370(9) Uani 1 1 d . . . H22 H 1.0681 0.4046 0.6267 0.044 Uiso 1 1 calc R . . C23 C 0.9501(4) 0.3359(3) 0.55835(19) 0.0307(8) Uani 1 1 d . . . H23 H 0.9957 0.2806 0.5656 0.037 Uiso 1 1 calc R . . C24 C 0.1553(5) 0.0605(3) 0.7140(2) 0.0367(9) Uani 1 1 d . . . H24A H 0.2040 0.0250 0.7483 0.044 Uiso 1 1 calc R . . H24B H 0.1286 0.0202 0.6781 0.044 Uiso 1 1 calc R . . C25 C 0.0191(4) 0.1009(3) 0.73923(18) 0.0310(8) Uani 1 1 d . . . C26 C -0.0932(4) 0.0447(3) 0.75656(19) 0.0340(9) Uani 1 1 d . . . H26 H -0.0878 -0.0171 0.7493 0.041 Uiso 1 1 calc R . . C27 C -0.2126(5) 0.0807(3) 0.78452(19) 0.0355(9) Uani 1 1 d . . . H27 H -0.2852 0.0419 0.7969 0.043 Uiso 1 1 calc R . . C28 C -0.1239(5) 0.2240(3) 0.7746(2) 0.0427(11) Uani 1 1 d . . . H28 H -0.1360 0.2860 0.7787 0.051 Uiso 1 1 calc R . . C29 C 0.0010(5) 0.1921(3) 0.7483(2) 0.0403(10) Uani 1 1 d . . . H29 H 0.0724 0.2322 0.7368 0.048 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 Hg 0.02505(8) 0.03806(10) 0.02929(9) 0.00572(6) 0.00220(6) 0.00223(6) Br1 0.0349(2) 0.0385(2) 0.0492(3) 0.00339(19) -0.00141(19) 0.00981(18) Br2 0.0554(3) 0.0327(2) 0.0343(2) 0.00288(17) 0.00478(19) -0.00102(19) Fe 0.0215(2) 0.0221(3) 0.0246(3) -0.00135(19) 0.0014(2) 0.0028(2) P 0.0203(4) 0.0233(5) 0.0262(5) 0.0001(4) 0.0024(4) 0.0025(4) O 0.0342(15) 0.0352(16) 0.0388(16) 0.0054(13) -0.0041(13) -0.0006(13) N1 0.0277(17) 0.040(2) 0.0303(18) 0.0069(15) 0.0056(13) 0.0016(14) N2 0.0361(19) 0.044(2) 0.0329(19) -0.0009(16) 0.0082(15) 0.0017(16) C1 0.0229(17) 0.0217(18) 0.0295(19) -0.0021(14) 0.0053(14) 0.0059(14) C2 0.033(2) 0.0229(18) 0.030(2) -0.0038(15) 0.0061(16) -0.0004(15) C3 0.038(2) 0.0219(19) 0.040(2) -0.0030(16) 0.0146(18) 0.0008(16) C4 0.037(2) 0.032(2) 0.034(2) 0.0123(17) 0.0093(18) 0.0146(18) C5 0.0253(19) 0.034(2) 0.034(2) 0.0043(17) -0.0009(16) 0.0072(16) C6 0.027(2) 0.029(2) 0.035(2) -0.0032(16) 0.0087(16) 0.0066(16) C7 0.040(2) 0.038(2) 0.030(2) -0.0134(17) 0.0090(18) -0.0006(18) C8 0.038(2) 0.026(2) 0.057(3) -0.0109(19) 0.009(2) -0.0024(18) C9 0.032(2) 0.025(2) 0.053(3) 0.0086(18) 0.0104(19) 0.0104(17) C10 0.0240(19) 0.032(2) 0.044(2) 0.0054(17) 0.0042(17) 0.0102(16) C11 0.030(2) 0.029(2) 0.030(2) -0.0002(16) 0.0065(16) 0.0108(16) C12 0.0222(17) 0.0260(19) 0.0248(18) 0.0001(15) 0.0023(14) 0.0048(14) C13 0.0269(19) 0.025(2) 0.043(2) 0.0009(17) 0.0056(17) 0.0024(16) C14 0.0210(19) 0.043(2) 0.052(3) -0.006(2) 0.0061(18) -0.0002(18) C15 0.027(2) 0.039(2) 0.039(2) -0.0075(18) 0.0043(17) 0.0086(17) C16 0.035(2) 0.027(2) 0.042(2) -0.0041(17) 0.0039(18) 0.0062(17) C17 0.0252(18) 0.029(2) 0.035(2) 0.0014(16) 0.0044(16) 0.0014(15) C18 0.0245(18) 0.0239(18) 0.0276(19) 0.0001(15) 0.0059(15) 0.0024(14) C19 0.0266(19) 0.0248(19) 0.036(2) 0.0017(16) 0.0021(16) 0.0018(15) C20 0.037(2) 0.024(2) 0.045(2) 0.0009(17) 0.0090(19) 0.0076(17) C21 0.047(3) 0.027(2) 0.042(2) -0.0073(18) 0.002(2) -0.0032(18) C22 0.037(2) 0.034(2) 0.040(2) -0.0061(18) -0.0048(18) 0.0000(18) C23 0.030(2) 0.025(2) 0.037(2) 0.0028(16) 0.0010(17) 0.0043(16) C24 0.036(2) 0.040(2) 0.035(2) 0.0061(18) 0.0081(18) 0.0025(18) C25 0.035(2) 0.034(2) 0.0240(19) 0.0025(16) 0.0024(16) 0.0034(17) C26 0.038(2) 0.033(2) 0.032(2) 0.0024(17) 0.0077(17) 0.0017(18) C27 0.041(2) 0.038(2) 0.027(2) -0.0006(17) 0.0044(17) -0.0049(19) C28 0.050(3) 0.038(3) 0.042(3) -0.0057(19) 0.017(2) 0.003(2) C29 0.044(2) 0.037(2) 0.041(2) -0.0037(19) 0.0166(19) -0.003(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 Hg N2 2.438(3) 4_665 ? Hg P 2.4381(10) . ? Hg Br1 2.5427(4) . ? Hg Br2 2.5990(5) . ? Fe C6 2.026(4) . ? Fe C7 2.034(4) . ? Fe C2 2.036(4) . ? Fe C1 2.036(4) . ? Fe C4 2.041(4) . ? Fe C5 2.042(4) . ? Fe C3 2.044(4) . ? Fe C10 2.045(4) . ? Fe C8 2.061(4) . ? Fe C9 2.065(4) . ? P C1 1.791(4) . ? P C18 1.808(4) . ? P C12 1.815(4) . ? O C11 1.232(5) . ? N1 C11 1.355(5) . ? N1 C24 1.446(5) . ? N1 H1N 1.0136 . ? N2 C28 1.334(6) . ? N2 C27 1.341(6) . ? N2 Hg 2.438(3) 4_466 ? C1 C5 1.427(5) . ? C1 C2 1.433(5) . ? C2 C3 1.414(6) . ? C2 H2 0.9300 . ? C3 C4 1.413(6) . ? C3 H3 0.9300 . ? C4 C5 1.413(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.430(6) . ? C6 C10 1.438(6) . ? C6 C11 1.473(6) . ? C7 C8 1.413(6) . ? C7 H7 0.9300 . ? C8 C9 1.409(7) . ? C8 H8 0.9300 . ? C9 C10 1.412(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C17 1.384(5) . ? C12 C13 1.386(5) . ? C13 C14 1.385(6) . ? C13 H13 0.9300 . ? C14 C15 1.387(6) . ? C14 H14 0.9300 . ? C15 C16 1.380(6) . ? C15 H15 0.9300 . ? C16 C17 1.389(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.393(5) . ? C18 C23 1.396(5) . ? C19 C20 1.392(6) . ? C19 H19 0.9300 . ? C20 C21 1.370(6) . ? C20 H20 0.9300 . ? C21 C22 1.383(6) . ? C21 H21 0.9300 . ? C22 C23 1.373(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.514(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C29 1.376(6) . ? C25 C26 1.394(6) . ? C26 C27 1.382(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.388(6) . ? C28 H28 0.9300 . ? C29 H29 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 N2 Hg P 101.21(9) 4_665 . ? N2 Hg Br1 94.55(9) 4_665 . ? P Hg Br1 130.22(3) . . ? N2 Hg Br2 99.05(9) 4_665 . ? P Hg Br2 109.06(2) . . ? Br1 Hg Br2 114.598(16) . . ? C6 Fe C7 41.25(17) . . ? C6 Fe C2 125.30(16) . . ? C7 Fe C2 163.30(17) . . ? C6 Fe C1 165.72(16) . . ? C7 Fe C1 152.99(17) . . ? C2 Fe C1 41.21(15) . . ? C6 Fe C4 113.97(17) . . ? C7 Fe C4 105.81(18) . . ? C2 Fe C4 68.39(17) . . ? C1 Fe C4 68.51(15) . . ? C6 Fe C5 148.91(17) . . ? C7 Fe C5 117.56(18) . . ? C2 Fe C5 68.91(16) . . ? C1 Fe C5 40.97(15) . . ? C4 Fe C5 40.49(16) . . ? C6 Fe C3 103.63(16) . . ? C7 Fe C3 125.10(17) . . ? C2 Fe C3 40.57(16) . . ? C1 Fe C3 68.64(15) . . ? C4 Fe C3 40.47(17) . . ? C5 Fe C3 68.34(17) . . ? C6 Fe C10 41.37(17) . . ? C7 Fe C10 68.87(18) . . ? C2 Fe C10 107.41(17) . . ? C1 Fe C10 129.91(16) . . ? C4 Fe C10 148.58(17) . . ? C5 Fe C10 169.42(17) . . ? C3 Fe C10 115.82(18) . . ? C6 Fe C8 68.53(17) . . ? C7 Fe C8 40.38(18) . . ? C2 Fe C8 154.81(17) . . ? C1 Fe C8 121.80(17) . . ? C4 Fe C8 128.97(19) . . ? C5 Fe C8 111.00(18) . . ? C3 Fe C8 164.45(18) . . ? C10 Fe C8 67.81(18) . . ? C6 Fe C9 68.51(16) . . ? C7 Fe C9 67.93(18) . . ? C2 Fe C9 120.45(17) . . ? C1 Fe C9 112.17(16) . . ? C4 Fe C9 168.16(18) . . ? C5 Fe C9 132.32(17) . . ? C3 Fe C9 151.35(18) . . ? C10 Fe C9 40.16(16) . . ? C8 Fe C9 39.94(19) . . ? C1 P C18 107.50(17) . . ? C1 P C12 107.62(16) . . ? C18 P C12 106.02(17) . . ? C1 P Hg 109.80(12) . . ? C18 P Hg 116.56(12) . . ? C12 P Hg 108.96(12) . . ? C11 N1 C24 120.5(4) . . ? C11 N1 H1N 116.8 . . ? C24 N1 H1N 122.6 . . ? C28 N2 C27 117.9(4) . . ? C28 N2 Hg 117.7(3) . 4_466 ? C27 N2 Hg 122.2(3) . 4_466 ? C5 C1 C2 107.5(3) . . ? C5 C1 P 127.8(3) . . ? C2 C1 P 124.7(3) . . ? C5 C1 Fe 69.7(2) . . ? C2 C1 Fe 69.4(2) . . ? P C1 Fe 124.47(19) . . ? C3 C2 C1 107.8(3) . . ? C3 C2 Fe 70.0(2) . . ? C1 C2 Fe 69.4(2) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Fe C2 H2 126.0 . . ? C4 C3 C2 108.3(4) . . ? C4 C3 Fe 69.7(2) . . ? C2 C3 Fe 69.4(2) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe C3 H3 126.7 . . ? C5 C4 C3 108.6(4) . . ? C5 C4 Fe 69.8(2) . . ? C3 C4 Fe 69.9(2) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? Fe C4 H4 126.2 . . ? C4 C5 C1 107.8(4) . . ? C4 C5 Fe 69.7(2) . . ? C1 C5 Fe 69.3(2) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe C5 H5 126.4 . . ? C7 C6 C10 107.1(4) . . ? C7 C6 C11 129.3(4) . . ? C10 C6 C11 123.5(4) . . ? C7 C6 Fe 69.7(2) . . ? C10 C6 Fe 70.0(2) . . ? C11 C6 Fe 122.5(3) . . ? C8 C7 C6 108.1(4) . . ? C8 C7 Fe 70.8(2) . . ? C6 C7 Fe 69.1(2) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe C7 H7 125.7 . . ? C9 C8 C7 108.5(4) . . ? C9 C8 Fe 70.2(2) . . ? C7 C8 Fe 68.8(2) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe C8 H8 126.8 . . ? C8 C9 C10 108.6(4) . . ? C8 C9 Fe 69.8(2) . . ? C10 C9 Fe 69.2(2) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe C9 H9 126.9 . . ? C9 C10 C6 107.8(4) . . ? C9 C10 Fe 70.7(2) . . ? C6 C10 Fe 68.6(2) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 126.2 . . ? O C11 N1 121.2(4) . . ? O C11 C6 121.9(4) . . ? N1 C11 C6 116.9(4) . . ? C17 C12 C13 119.7(3) . . ? C17 C12 P 120.8(3) . . ? C13 C12 P 119.4(3) . . ? C14 C13 C12 120.6(4) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 119.6(4) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.3(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 119.9(4) . . ? C12 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C23 119.9(4) . . ? C19 C18 P 120.6(3) . . ? C23 C18 P 119.5(3) . . ? C20 C19 C18 119.5(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C21 C20 C19 120.0(4) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.6(4) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 120.3(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 119.7(4) . . ? C22 C23 H23 120.1 . . ? C18 C23 H23 120.1 . . ? N1 C24 C25 113.2(4) . . ? N1 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N1 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.8 . . ? C29 C25 C26 116.9(4) . . ? C29 C25 C24 123.0(4) . . ? C26 C25 C24 120.0(4) . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? N2 C27 C26 122.2(4) . . ? N2 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? N2 C28 C29 122.8(4) . . ? N2 C28 H28 118.6 . . ? C29 C28 H28 118.6 . . ? C25 C29 C28 119.9(4) . . ? C25 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.741 _refine_diff_density_min -1.345 _refine_diff_density_rms 0.116 #===END data_jk81f _database_code_depnum_ccdc_archive 'CCDC 670837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H26 Br3 Cd Fe N2 O P, H2 O' _chemical_formula_sum 'C29 H28 Br3 Cd Fe N2 O2 P' _chemical_formula_weight 875.48 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' 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' O O 0.0106 0.0060 '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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8247(2) _cell_length_b 9.6370(2) _cell_length_c 17.9163(4) _cell_angle_alpha 83.033(1) _cell_angle_beta 88.557(1) _cell_angle_gamma 87.229(1) _cell_volume 1510.36(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14197 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 5.235 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.611 _exptl_absorpt_process_details ; gaussian absorption correction based on indexed crystal shape ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 26533 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.56 _reflns_number_total 6960 _reflns_number_gt 5814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _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^)+(0.0266P)^2^+1.0936P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6960 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 1.24907(2) 0.20463(2) 0.241663(11) 0.02013(6) Uani 1 1 d . . . Br1 Br 1.27559(3) 0.37819(3) 0.119771(16) 0.02496(8) Uani 1 1 d . . . Br2 Br 1.50671(3) 0.07759(3) 0.272073(18) 0.02744(8) Uani 1 1 d . . . Br3 Br 1.04590(4) 0.03742(3) 0.213976(18) 0.02874(8) Uani 1 1 d . . . Fe Fe 0.81670(4) 0.51982(4) 0.27099(2) 0.01739(9) Uani 1 1 d . . . P P 1.14116(8) 0.33406(7) 0.35130(4) 0.01678(15) Uani 1 1 d . . . O O 0.6536(2) 0.4376(2) 0.07239(11) 0.0237(4) Uani 1 1 d . . . N1 N 0.8961(3) 0.3593(2) 0.08611(14) 0.0227(5) Uani 1 1 d . . . H1N H 0.9836 0.3675 0.1119 0.039(10) Uiso 1 1 d R . . N2 N 0.6574(3) -0.0905(3) 0.03326(15) 0.0287(6) Uani 1 1 d . . . H2N H 0.6080 -0.1631 0.0305 0.044(11) Uiso 1 1 d R . . C1 C 0.9434(3) 0.3875(3) 0.34644(15) 0.0176(6) Uani 1 1 d . . . C2 C 0.8262(3) 0.3134(3) 0.31624(16) 0.0204(6) Uani 1 1 d . . . H2 H 0.8407 0.2365 0.2897 0.024 Uiso 1 1 calc R . . C3 C 0.6844(3) 0.3783(3) 0.33410(17) 0.0254(7) Uani 1 1 d . . . H3 H 0.5896 0.3503 0.3219 0.030 Uiso 1 1 calc R . . C4 C 0.7114(3) 0.4926(3) 0.37363(16) 0.0264(7) Uani 1 1 d . . . H4 H 0.6374 0.5531 0.3915 0.032 Uiso 1 1 calc R . . C5 C 0.8705(3) 0.4997(3) 0.38154(15) 0.0200(6) Uani 1 1 d . . . H5 H 0.9188 0.5655 0.4053 0.024 Uiso 1 1 calc R . . C6 C 0.7992(3) 0.5450(3) 0.15617(15) 0.0199(6) Uani 1 1 d . . . C7 C 0.6770(4) 0.6202(3) 0.19028(16) 0.0260(7) Uani 1 1 d . . . H7 H 0.5740 0.6069 0.1861 0.031 Uiso 1 1 calc R . . C8 C 0.7418(4) 0.7184(3) 0.23149(17) 0.0303(7) Uani 1 1 d . . . H8 H 0.6884 0.7810 0.2591 0.036 Uiso 1 1 calc R . . C9 C 0.9013(4) 0.7048(3) 0.22349(17) 0.0295(7) Uani 1 1 d . . . H9 H 0.9706 0.7570 0.2450 0.035 Uiso 1 1 calc R . . C10 C 0.9380(3) 0.5984(3) 0.17720(15) 0.0216(6) Uani 1 1 d . . . H10 H 1.0351 0.5686 0.1630 0.026 Uiso 1 1 calc R . . C11 C 0.7766(3) 0.4424(3) 0.10294(15) 0.0190(6) Uani 1 1 d . . . C12 C 1.1555(3) 0.2280(3) 0.44275(15) 0.0189(6) Uani 1 1 d . . . C13 C 1.0329(3) 0.2136(3) 0.49284(16) 0.0243(6) Uani 1 1 d . . . H13 H 0.9395 0.2575 0.4796 0.029 Uiso 1 1 calc R . . C14 C 1.0486(4) 0.1345(3) 0.56231(17) 0.0297(7) Uani 1 1 d . . . H14 H 0.9657 0.1253 0.5953 0.036 Uiso 1 1 calc R . . C15 C 1.1866(4) 0.0691(3) 0.58295(18) 0.0314(7) Uani 1 1 d . . . H15 H 1.1973 0.0172 0.6299 0.038 Uiso 1 1 calc R . . C16 C 1.3087(4) 0.0817(4) 0.53295(19) 0.0380(8) Uani 1 1 d . . . H16 H 1.4018 0.0376 0.5464 0.046 Uiso 1 1 calc R . . C17 C 1.2934(4) 0.1596(3) 0.46287(18) 0.0313(7) Uani 1 1 d . . . H17 H 1.3756 0.1661 0.4293 0.038 Uiso 1 1 calc R . . C18 C 1.2357(3) 0.4940(3) 0.36212(16) 0.0189(6) Uani 1 1 d . . . C19 C 1.2669(3) 0.5860(3) 0.29784(17) 0.0261(7) Uani 1 1 d . . . H19 H 1.2470 0.5615 0.2505 0.031 Uiso 1 1 calc R . . C20 C 1.3275(4) 0.7142(3) 0.30442(18) 0.0299(7) Uani 1 1 d . . . H20 H 1.3446 0.7768 0.2616 0.036 Uiso 1 1 calc R . . C21 C 1.3625(3) 0.7491(3) 0.37412(19) 0.0308(7) Uani 1 1 d . . . H21 H 1.4035 0.8349 0.3782 0.037 Uiso 1 1 calc R . . C22 C 1.3368(4) 0.6568(3) 0.43805(18) 0.0304(7) Uani 1 1 d . . . H22 H 1.3620 0.6800 0.4849 0.036 Uiso 1 1 calc R . . C23 C 1.2732(3) 0.5293(3) 0.43216(16) 0.0245(6) Uani 1 1 d . . . H23 H 1.2556 0.4675 0.4752 0.029 Uiso 1 1 calc R . . C24 C 0.8965(3) 0.2843(3) 0.02074(17) 0.0261(7) Uani 1 1 d . . . H24A H 1.0012 0.2630 0.0068 0.031 Uiso 1 1 calc R . . H24B H 0.8526 0.3465 -0.0205 0.031 Uiso 1 1 calc R . . C25 C 0.8135(3) 0.1502(3) 0.02865(16) 0.0216(6) Uani 1 1 d . . . C26 C 0.7268(3) 0.1028(3) 0.09168(16) 0.0240(6) Uani 1 1 d . . . H26 H 0.7211 0.1525 0.1331 0.029 Uiso 1 1 calc R . . C27 C 0.6501(4) -0.0175(3) 0.09243(18) 0.0272(7) Uani 1 1 d . . . H27 H 0.5920 -0.0490 0.1346 0.033 Uiso 1 1 calc R . . C28 C 0.7404(4) -0.0485(3) -0.02824(18) 0.0299(7) Uani 1 1 d . . . H28 H 0.7445 -0.1007 -0.0687 0.036 Uiso 1 1 calc R . . C29 C 0.8192(4) 0.0714(3) -0.03161(18) 0.0286(7) Uani 1 1 d . . . H29 H 0.8768 0.1002 -0.0744 0.034 Uiso 1 1 calc R . . O1W O 0.4884(2) 0.6881(2) 0.03971(12) 0.0253(5) Uani 1 1 d . . . H1W H 0.4332 0.6583 0.0016 0.062(13) Uiso 1 1 d R . . H2W H 0.5144 0.6014 0.0580 0.072(14) Uiso 1 1 d 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 Cd 0.02219(11) 0.01966(11) 0.01892(11) -0.00388(8) 0.00040(8) -0.00136(8) Br1 0.02600(16) 0.02580(16) 0.02237(16) 0.00023(12) 0.00330(12) -0.00369(12) Br2 0.02380(16) 0.02677(16) 0.03113(17) -0.00238(13) -0.00095(13) 0.00253(12) Br3 0.03094(17) 0.02360(16) 0.03329(18) -0.00723(13) -0.00066(13) -0.00802(13) Fe 0.0214(2) 0.0161(2) 0.0146(2) -0.00221(15) -0.00327(16) 0.00115(16) P 0.0180(3) 0.0175(3) 0.0149(3) -0.0021(3) -0.0011(3) -0.0005(3) O 0.0236(11) 0.0246(11) 0.0237(11) -0.0053(9) -0.0086(9) 0.0016(8) N1 0.0205(13) 0.0242(13) 0.0250(13) -0.0085(10) -0.0055(10) -0.0001(10) N2 0.0303(14) 0.0195(13) 0.0371(16) -0.0058(11) -0.0094(12) 0.0008(11) C1 0.0180(14) 0.0203(14) 0.0142(13) -0.0013(11) -0.0021(11) 0.0005(11) C2 0.0235(15) 0.0167(14) 0.0205(15) 0.0013(11) -0.0034(12) -0.0046(11) C3 0.0191(15) 0.0282(16) 0.0279(16) 0.0031(13) -0.0011(12) -0.0065(12) C4 0.0230(15) 0.0351(17) 0.0196(15) -0.0003(13) 0.0034(12) 0.0062(13) C5 0.0241(15) 0.0234(15) 0.0130(13) -0.0044(11) -0.0021(11) 0.0012(12) C6 0.0277(15) 0.0164(14) 0.0147(14) 0.0019(11) -0.0037(12) 0.0003(11) C7 0.0317(17) 0.0258(16) 0.0192(15) -0.0007(12) -0.0053(13) 0.0086(13) C8 0.051(2) 0.0159(15) 0.0229(16) -0.0019(12) -0.0066(15) 0.0099(14) C9 0.048(2) 0.0175(15) 0.0233(16) 0.0015(12) -0.0084(14) -0.0070(14) C10 0.0283(16) 0.0197(14) 0.0167(14) 0.0006(11) -0.0018(12) -0.0056(12) C11 0.0217(15) 0.0175(14) 0.0170(14) 0.0011(11) -0.0026(12) -0.0007(11) C12 0.0209(14) 0.0181(14) 0.0182(14) -0.0045(11) -0.0021(11) -0.0002(11) C13 0.0237(15) 0.0250(15) 0.0235(16) -0.0007(12) -0.0024(12) 0.0005(12) C14 0.0357(18) 0.0305(17) 0.0213(16) 0.0032(13) 0.0034(14) -0.0036(14) C15 0.042(2) 0.0282(17) 0.0221(16) 0.0054(13) -0.0082(14) -0.0008(14) C16 0.0328(18) 0.044(2) 0.0328(19) 0.0090(16) -0.0070(15) 0.0128(16) C17 0.0264(16) 0.0408(19) 0.0248(17) 0.0012(14) -0.0025(13) 0.0064(14) C18 0.0168(14) 0.0200(14) 0.0207(15) -0.0059(11) 0.0017(11) -0.0005(11) C19 0.0265(16) 0.0286(16) 0.0240(16) -0.0043(13) -0.0033(13) -0.0034(13) C20 0.0330(17) 0.0242(16) 0.0312(18) 0.0031(13) -0.0010(14) -0.0051(13) C21 0.0267(17) 0.0245(16) 0.043(2) -0.0096(15) 0.0017(15) -0.0062(13) C22 0.0294(17) 0.0377(18) 0.0272(17) -0.0148(14) 0.0009(14) -0.0083(14) C23 0.0283(16) 0.0273(16) 0.0187(15) -0.0058(12) 0.0037(12) -0.0056(13) C24 0.0282(16) 0.0257(15) 0.0256(16) -0.0089(13) 0.0031(13) -0.0020(13) C25 0.0210(14) 0.0202(14) 0.0242(15) -0.0070(12) -0.0064(12) 0.0060(11) C26 0.0307(16) 0.0224(15) 0.0184(15) -0.0024(12) -0.0037(12) 0.0041(12) C27 0.0312(17) 0.0234(16) 0.0259(17) 0.0013(13) -0.0057(13) 0.0005(13) C28 0.0341(18) 0.0284(17) 0.0297(18) -0.0137(14) -0.0055(14) 0.0025(14) C29 0.0267(16) 0.0308(17) 0.0297(17) -0.0112(14) 0.0004(13) 0.0029(13) O1W 0.0289(11) 0.0186(11) 0.0294(12) -0.0048(9) -0.0089(9) -0.0006(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd Br3 2.5642(4) . ? Cd Br2 2.5683(4) . ? Cd P 2.5897(7) . ? Cd Br1 2.5976(3) . ? Fe C5 2.033(3) . ? Fe C4 2.033(3) . ? Fe C8 2.042(3) . ? Fe C7 2.045(3) . ? Fe C9 2.046(3) . ? Fe C6 2.051(3) . ? Fe C3 2.053(3) . ? Fe C2 2.054(3) . ? Fe C10 2.055(3) . ? Fe C1 2.055(3) . ? P C1 1.797(3) . ? P C18 1.821(3) . ? P C12 1.827(3) . ? O C11 1.233(3) . ? N1 C11 1.344(3) . ? N1 C24 1.448(4) . ? N1 H1N 0.9218 . ? N2 C28 1.339(4) . ? N2 C27 1.340(4) . ? N2 H2N 0.8496 . ? C1 C5 1.434(4) . ? C1 C2 1.437(4) . ? C2 C3 1.419(4) . ? C2 H2 0.9300 . ? C3 C4 1.412(4) . ? C3 H3 0.9300 . ? C4 C5 1.421(4) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C10 1.428(4) . ? C6 C7 1.435(4) . ? C6 C11 1.477(4) . ? C7 C8 1.418(4) . ? C7 H7 0.9300 . ? C8 C9 1.413(5) . ? C8 H8 0.9300 . ? C9 C10 1.416(4) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C13 1.390(4) . ? C12 C17 1.390(4) . ? C13 C14 1.385(4) . ? C13 H13 0.9300 . ? C14 C15 1.382(5) . ? C14 H14 0.9300 . ? C15 C16 1.384(5) . ? C15 H15 0.9300 . ? C16 C17 1.388(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.391(4) . ? C18 C19 1.396(4) . ? C19 C20 1.389(4) . ? C19 H19 0.9300 . ? C20 C21 1.378(5) . ? C20 H20 0.9300 . ? C21 C22 1.383(4) . ? C21 H21 0.9300 . ? C22 C23 1.392(4) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.506(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.391(4) . ? C25 C29 1.392(4) . ? C26 C27 1.369(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.372(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? O1W H1W 0.9290 . ? O1W H2W 0.8819 . ? 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 Br3 Cd Br2 112.596(12) . . ? Br3 Cd P 106.147(18) . . ? Br2 Cd P 112.434(19) . . ? Br3 Cd Br1 105.436(13) . . ? Br2 Cd Br1 109.459(12) . . ? P Cd Br1 110.513(18) . . ? C5 Fe C4 40.91(12) . . ? C5 Fe C8 112.69(12) . . ? C4 Fe C8 101.55(12) . . ? C5 Fe C7 145.27(11) . . ? C4 Fe C7 111.98(12) . . ? C8 Fe C7 40.61(12) . . ? C5 Fe C9 106.29(12) . . ? C4 Fe C9 124.16(13) . . ? C8 Fe C9 40.42(13) . . ? C7 Fe C9 68.27(13) . . ? C5 Fe C6 170.69(12) . . ? C4 Fe C6 148.38(12) . . ? C8 Fe C6 68.45(11) . . ? C7 Fe C6 41.02(11) . . ? C9 Fe C6 68.22(12) . . ? C5 Fe C3 68.50(12) . . ? C4 Fe C3 40.43(12) . . ? C8 Fe C3 123.60(13) . . ? C7 Fe C3 105.31(13) . . ? C9 Fe C3 161.45(13) . . ? C6 Fe C3 119.13(12) . . ? C5 Fe C2 68.92(11) . . ? C4 Fe C2 68.38(12) . . ? C8 Fe C2 163.43(13) . . ? C7 Fe C2 129.32(12) . . ? C9 Fe C2 156.15(12) . . ? C6 Fe C2 112.84(11) . . ? C3 Fe C2 40.42(11) . . ? C5 Fe C10 130.37(12) . . ? C4 Fe C10 164.19(12) . . ? C8 Fe C10 68.18(12) . . ? C7 Fe C10 68.62(12) . . ? C9 Fe C10 40.39(12) . . ? C6 Fe C10 40.70(11) . . ? C3 Fe C10 155.35(12) . . ? C2 Fe C10 124.35(11) . . ? C5 Fe C1 41.06(11) . . ? C4 Fe C1 68.72(11) . . ? C8 Fe C1 149.33(12) . . ? C7 Fe C1 169.99(12) . . ? C9 Fe C1 120.16(12) . . ? C6 Fe C1 134.34(11) . . ? C3 Fe C1 68.40(11) . . ? C2 Fe C1 40.95(11) . . ? C10 Fe C1 113.63(11) . . ? C1 P C18 104.22(12) . . ? C1 P C12 103.39(12) . . ? C18 P C12 105.10(13) . . ? C1 P Cd 115.86(9) . . ? C18 P Cd 114.04(9) . . ? C12 P Cd 113.01(9) . . ? C11 N1 C24 121.2(3) . . ? C11 N1 H1N 116.1 . . ? C24 N1 H1N 121.5 . . ? C28 N2 C27 121.2(3) . . ? C28 N2 H2N 114.9 . . ? C27 N2 H2N 123.9 . . ? C5 C1 C2 107.3(2) . . ? C5 C1 P 126.1(2) . . ? C2 C1 P 126.0(2) . . ? C5 C1 Fe 68.64(15) . . ? C2 C1 Fe 69.47(15) . . ? P C1 Fe 133.77(14) . . ? C3 C2 C1 107.9(2) . . ? C3 C2 Fe 69.77(16) . . ? C1 C2 Fe 69.58(15) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Fe C2 H2 126.2 . . ? C4 C3 C2 108.4(3) . . ? C4 C3 Fe 69.03(16) . . ? C2 C3 Fe 69.80(15) . . ? C4 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? Fe C3 H3 127.0 . . ? C3 C4 C5 108.5(3) . . ? C3 C4 Fe 70.53(17) . . ? C5 C4 Fe 69.52(15) . . ? C3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? Fe C4 H4 125.8 . . ? C4 C5 C1 107.9(3) . . ? C4 C5 Fe 69.57(16) . . ? C1 C5 Fe 70.30(15) . . ? C4 C5 H5 126.1 . . ? C1 C5 H5 126.1 . . ? Fe C5 H5 125.6 . . ? C10 C6 C7 107.6(3) . . ? C10 C6 C11 128.4(3) . . ? C7 C6 C11 123.6(3) . . ? C10 C6 Fe 69.79(16) . . ? C7 C6 Fe 69.26(16) . . ? C11 C6 Fe 131.07(19) . . ? C8 C7 C6 107.6(3) . . ? C8 C7 Fe 69.61(17) . . ? C6 C7 Fe 69.73(16) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? Fe C7 H7 126.0 . . ? C9 C8 C7 108.4(3) . . ? C9 C8 Fe 69.95(17) . . ? C7 C8 Fe 69.78(16) . . ? C9 C8 H8 125.8 . . ? C7 C8 H8 125.8 . . ? Fe C8 H8 126.0 . . ? C8 C9 C10 108.6(3) . . ? C8 C9 Fe 69.63(17) . . ? C10 C9 Fe 70.11(16) . . ? C8 C9 H9 125.7 . . ? C10 C9 H9 125.7 . . ? Fe C9 H9 126.1 . . ? C9 C10 C6 107.8(3) . . ? C9 C10 Fe 69.50(16) . . ? C6 C10 Fe 69.51(15) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 126.5 . . ? O C11 N1 121.0(3) . . ? O C11 C6 120.9(2) . . ? N1 C11 C6 118.0(3) . . ? C13 C12 C17 119.0(3) . . ? C13 C12 P 122.0(2) . . ? C17 C12 P 119.0(2) . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 120.1(3) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C23 C18 C19 119.2(3) . . ? C23 C18 P 122.3(2) . . ? C19 C18 P 118.5(2) . . ? C20 C19 C18 120.1(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.2(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 120.0(3) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C18 C23 C22 120.2(3) . . ? C18 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? N1 C24 C25 116.8(2) . . ? N1 C24 H24A 108.1 . . ? C25 C24 H24A 108.1 . . ? N1 C24 H24B 108.1 . . ? C25 C24 H24B 108.1 . . ? H24A C24 H24B 107.3 . . ? C26 C25 C29 117.9(3) . . ? C26 C25 C24 123.8(3) . . ? C29 C25 C24 118.2(3) . . ? C27 C26 C25 119.6(3) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? N2 C27 C26 120.9(3) . . ? N2 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? N2 C28 C29 120.0(3) . . ? N2 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C25 120.3(3) . . ? C28 C29 H29 119.8 . . ? C25 C29 H29 119.8 . . ? H1W O1W H2W 92.0 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.490 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.108 #===END data_jk82 _database_code_depnum_ccdc_archive 'CCDC 670838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C116 H100 Br8 Cd4 Fe4 N8 O4 P4' _chemical_formula_sum 'C116 H100 Br8 Cd4 Fe4 N8 O4 P4' _chemical_formula_weight 3106.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.6296(2) _cell_length_b 14.7954(3) _cell_length_c 16.0664(3) _cell_angle_alpha 106.7924(9) _cell_angle_beta 115.194(1) _cell_angle_gamma 99.039(1) _cell_volume 2850.8(1) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 34240 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 4.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.492 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_process_details ; SORTAV: multiscan Blessing, R. H. (1997). J. Appl. Cryst. 30, 421--426 ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 51514 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.51 _reflns_number_total 13060 _reflns_number_gt 10422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _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^)+(0.0617P)^2^+4.7571P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13060 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.88157(2) 0.01224(2) 0.03236(2) 0.02297(8) Uani 1 1 d . . . Cd2 Cd 1.24394(3) 0.77396(2) 0.53040(2) 0.03656(9) Uani 1 1 d . . . Br1 Br 0.94114(3) -0.13961(3) -0.05379(3) 0.02803(10) Uani 1 1 d . . . Br2 Br 1.33219(5) 0.93894(4) 0.53129(5) 0.06738(19) Uani 1 1 d . . . Br3 Br 1.33851(4) 0.72729(4) 0.67964(4) 0.05097(14) Uani 1 1 d . . . Br4 Br 1.05228(4) 0.75597(5) 0.49591(4) 0.05774(17) Uani 1 1 d . . . Fe1 Fe 0.46257(4) -0.23138(4) -0.00050(4) 0.02647(13) Uani 1 1 d . . . Fe2 Fe 1.05556(5) 0.42065(4) 0.31136(5) 0.03333(15) Uani 1 1 d . . . P1 P 0.45535(11) -0.32419(9) 0.16780(9) 0.0379(3) Uani 1 1 d . . . P2 P 1.25104(8) 0.63891(8) 0.39085(8) 0.0251(2) Uani 1 1 d . . . O1 O 0.7331(2) -0.0930(2) 0.0152(2) 0.0289(6) Uani 1 1 d . . . O2 O 0.8558(2) 0.1583(2) 0.1081(2) 0.0298(6) Uani 1 1 d . . . N11 N 0.5898(3) -0.1522(3) -0.1404(2) 0.0286(7) Uani 1 1 d . . . H1N H 0.5167 -0.1729 -0.1685 0.057(16) Uiso 1 1 d R . . N12 N 0.7599(2) 0.0266(2) -0.1159(2) 0.0250(7) Uani 1 1 d . . . N21 N 0.8770(3) 0.1764(3) 0.2609(3) 0.0300(7) Uani 1 1 d . . . H2N H 0.8968 0.2156 0.3220 0.051(16) Uiso 1 1 d R . . N22 N 0.9753(3) 0.0137(3) 0.1941(2) 0.0285(7) Uani 1 1 d . . . C1 C 0.4328(3) -0.3435(3) 0.0428(3) 0.0298(9) Uani 1 1 d . . . C2 C 0.5037(4) -0.3562(3) 0.0041(4) 0.0338(9) Uani 1 1 d . . . H2 H 0.5722 -0.3588 0.0385 0.041 Uiso 1 1 calc R . . C3 C 0.4509(4) -0.3640(3) -0.0964(4) 0.0385(10) Uani 1 1 d . . . H3 H 0.4792 -0.3722 -0.1390 0.046 Uiso 1 1 calc R . . C4 C 0.3485(4) -0.3574(3) -0.1203(3) 0.0390(10) Uani 1 1 d . . . H4 H 0.2972 -0.3612 -0.1818 0.047 Uiso 1 1 calc R . . C5 C 0.3369(3) -0.3440(3) -0.0350(3) 0.0349(10) Uani 1 1 d . . . H5 H 0.2770 -0.3368 -0.0304 0.042 Uiso 1 1 calc R . . C6 C 0.5618(3) -0.1178(3) 0.0008(3) 0.0263(8) Uani 1 1 d . . . C7 C 0.4542(3) -0.1171(3) -0.0461(3) 0.0329(9) Uani 1 1 d . . . H7 H 0.4141 -0.1231 -0.1117 0.039 Uiso 1 1 calc R . . C8 C 0.4198(4) -0.1058(3) 0.0248(4) 0.0370(10) Uani 1 1 d . . . H8 H 0.3527 -0.1032 0.0140 0.044 Uiso 1 1 calc R . . C9 C 0.5041(4) -0.0989(3) 0.1151(4) 0.0369(10) Uani 1 1 d . . . H9 H 0.5021 -0.0902 0.1739 0.044 Uiso 1 1 calc R . . C10 C 0.5925(3) -0.1073(3) 0.1014(3) 0.0315(9) Uani 1 1 d . . . H10 H 0.6580 -0.1063 0.1487 0.038 Uiso 1 1 calc R . . C11 C 0.6348(3) -0.1210(3) -0.0409(3) 0.0244(8) Uani 1 1 d . . . C12 C 0.4087(4) -0.4531(4) 0.1534(4) 0.0397(11) Uani 1 1 d . . . C13 C 0.3260(4) -0.5259(4) 0.0601(4) 0.0468(12) Uani 1 1 d . . . H13 H 0.3032 -0.5121 0.0030 0.056 Uiso 1 1 calc R . . C14 C 0.2786(5) -0.6186(4) 0.0538(6) 0.0616(16) Uani 1 1 d . . . H14 H 0.2237 -0.6665 -0.0078 0.074 Uiso 1 1 calc R . . C15 C 0.3117(5) -0.6399(5) 0.1364(6) 0.0667(19) Uani 1 1 d . . . H15 H 0.2786 -0.7019 0.1314 0.080 Uiso 1 1 calc R . . C16 C 0.3941(6) -0.5704(5) 0.2278(6) 0.0626(17) Uani 1 1 d . . . H16 H 0.4176 -0.5860 0.2839 0.075 Uiso 1 1 calc R . . C17 C 0.4416(5) -0.4776(4) 0.2360(5) 0.0499(13) Uani 1 1 d . . . H17 H 0.4968 -0.4308 0.2980 0.060 Uiso 1 1 calc R . . C18 C 0.6009(4) -0.2921(4) 0.2344(4) 0.0510(13) Uani 1 1 d . . . C19 C 0.6558(5) -0.3582(6) 0.2245(6) 0.076(2) Uani 1 1 d . . . H19 H 0.6186 -0.4262 0.1902 0.091 Uiso 1 1 calc R . . C20 C 0.7671(6) -0.3248(9) 0.2650(8) 0.122(4) Uani 1 1 d . . . H20 H 0.8035 -0.3694 0.2552 0.147 Uiso 1 1 calc R . . C21 C 0.8217(7) -0.2222(9) 0.3208(8) 0.133(5) Uani 1 1 d . . . H21 H 0.8952 -0.1984 0.3482 0.159 Uiso 1 1 calc R . . C22 C 0.7678(7) -0.1560(7) 0.3358(6) 0.097(3) Uani 1 1 d . . . H22 H 0.8054 -0.0884 0.3745 0.117 Uiso 1 1 calc R . . C23 C 0.6587(6) -0.1895(5) 0.2938(4) 0.074(2) Uani 1 1 d . . . H23 H 0.6229 -0.1446 0.3043 0.088 Uiso 1 1 calc R . . C24 C 0.6515(3) -0.1487(3) -0.1916(3) 0.0269(8) Uani 1 1 d . . . H24A H 0.6115 -0.2010 -0.2587 0.032 Uiso 1 1 calc R . . H24B H 0.7179 -0.1603 -0.1555 0.032 Uiso 1 1 calc R . . C25 C 0.6749(3) -0.0494(3) -0.1979(3) 0.0269(8) Uani 1 1 d . . . C26 C 0.7762(3) 0.1185(3) -0.1179(3) 0.0302(9) Uani 1 1 d . . . H26 H 0.8334 0.1714 -0.0623 0.036 Uiso 1 1 calc R . . C27 C 0.7114(4) 0.1370(4) -0.1991(4) 0.0385(10) Uani 1 1 d . . . H27 H 0.7249 0.2011 -0.1976 0.046 Uiso 1 1 calc R . . C28 C 0.6271(4) 0.0596(4) -0.2819(4) 0.0418(11) Uani 1 1 d . . . H28 H 0.5829 0.0707 -0.3374 0.050 Uiso 1 1 calc R . . C29 C 0.6086(3) -0.0347(4) -0.2819(3) 0.0374(10) Uani 1 1 d . . . H29 H 0.5521 -0.0880 -0.3377 0.045 Uiso 1 1 calc R . . C51 C 1.2083(3) 0.5117(3) 0.3757(3) 0.0265(8) Uani 1 1 d . . . C52 C 1.1874(3) 0.4199(3) 0.2972(3) 0.0308(9) Uani 1 1 d . . . H52 H 1.1922 0.4141 0.2401 0.037 Uiso 1 1 calc R . . C53 C 1.1585(3) 0.3403(3) 0.3223(4) 0.0379(10) Uani 1 1 d . . . H53 H 1.1413 0.2731 0.2843 0.045 Uiso 1 1 calc R . . C54 C 1.1600(4) 0.3789(3) 0.4139(4) 0.0409(11) Uani 1 1 d . . . H54 H 1.1435 0.3418 0.4465 0.049 Uiso 1 1 calc R . . C55 C 1.1911(3) 0.4848(3) 0.4481(3) 0.0332(9) Uani 1 1 d . . . H55 H 1.1988 0.5289 0.5071 0.040 Uiso 1 1 calc R . . C56 C 0.9052(3) 0.3217(3) 0.2260(4) 0.0355(10) Uani 1 1 d . . . C57 C 0.9159(4) 0.3930(3) 0.3146(4) 0.0496(14) Uani 1 1 d . . . H57 H 0.9064 0.3791 0.3638 0.060 Uiso 1 1 calc R . . C58 C 0.9435(4) 0.4881(4) 0.3133(6) 0.068(2) Uani 1 1 d . . . H58 H 0.9560 0.5482 0.3622 0.081 Uiso 1 1 calc R . . C59 C 0.9489(4) 0.4767(4) 0.2270(6) 0.065(2) Uani 1 1 d . . . H59 H 0.9647 0.5282 0.2080 0.079 Uiso 1 1 calc R . . C60 C 0.9265(3) 0.3737(4) 0.1719(4) 0.0489(13) Uani 1 1 d . . . H60 H 0.9259 0.3460 0.1118 0.059 Uiso 1 1 calc R . . C61 C 0.8782(3) 0.2130(3) 0.1945(3) 0.0285(9) Uani 1 1 d . . . C62 C 1.3921(3) 0.6682(3) 0.4287(3) 0.0292(8) Uani 1 1 d . . . C63 C 1.4552(3) 0.6231(3) 0.4832(4) 0.0368(10) Uani 1 1 d . . . H63 H 1.4238 0.5701 0.4928 0.044 Uiso 1 1 calc R . . C64 C 1.5652(4) 0.6562(4) 0.5238(4) 0.0446(12) Uani 1 1 d . . . H64 H 1.6072 0.6255 0.5603 0.054 Uiso 1 1 calc R . . C65 C 1.6124(4) 0.7349(4) 0.5099(4) 0.0454(12) Uani 1 1 d . . . H65 H 1.6860 0.7569 0.5369 0.055 Uiso 1 1 calc R . . C66 C 1.5497(4) 0.7811(4) 0.4556(4) 0.0442(11) Uani 1 1 d . . . H66 H 1.5814 0.8342 0.4464 0.053 Uiso 1 1 calc R . . C67 C 1.4404(4) 0.7482(3) 0.4152(3) 0.0373(10) Uani 1 1 d . . . H67 H 1.3986 0.7793 0.3789 0.045 Uiso 1 1 calc R . . C68 C 1.1816(3) 0.6445(3) 0.2690(3) 0.0294(9) Uani 1 1 d . . . C69 C 1.1119(3) 0.7002(3) 0.2561(3) 0.0345(9) Uani 1 1 d . . . H69 H 1.1066 0.7374 0.3104 0.041 Uiso 1 1 calc R . . C70 C 1.0508(4) 0.7004(4) 0.1628(4) 0.0436(11) Uani 1 1 d . . . H70 H 1.0039 0.7371 0.1545 0.052 Uiso 1 1 calc R . . C71 C 1.0588(4) 0.6463(4) 0.0815(4) 0.0472(13) Uani 1 1 d . . . H71 H 1.0167 0.6459 0.0187 0.057 Uiso 1 1 calc R . . C72 C 1.1294(4) 0.5927(4) 0.0938(3) 0.0428(11) Uani 1 1 d . . . H72 H 1.1354 0.5571 0.0394 0.051 Uiso 1 1 calc R . . C73 C 1.1913(4) 0.5918(3) 0.1871(3) 0.0359(10) Uani 1 1 d . . . H73 H 1.2393 0.5562 0.1952 0.043 Uiso 1 1 calc R . . C74 C 0.8497(3) 0.0714(3) 0.2411(3) 0.0284(8) Uani 1 1 d . . . H74A H 0.7960 0.0336 0.1711 0.034 Uiso 1 1 calc R . . H74B H 0.8194 0.0590 0.2814 0.034 Uiso 1 1 calc R . . C75 C 0.9454(3) 0.0358(3) 0.2640(3) 0.0314(9) Uani 1 1 d . . . C76 C 1.0635(4) -0.0122(4) 0.2166(3) 0.0397(11) Uani 1 1 d . . . H76 H 1.0852 -0.0262 0.1690 0.048 Uiso 1 1 calc R . . C77 C 1.1241(5) -0.0195(5) 0.3057(4) 0.0542(14) Uani 1 1 d . . . H77 H 1.1850 -0.0380 0.3181 0.065 Uiso 1 1 calc R . . C78 C 1.0917(5) 0.0013(6) 0.3757(4) 0.0687(19) Uani 1 1 d . . . H78 H 1.1294 -0.0049 0.4361 0.082 Uiso 1 1 calc R . . C79 C 1.0033(5) 0.0314(5) 0.3560(4) 0.0539(14) Uani 1 1 d . . . H79 H 0.9826 0.0487 0.4041 0.065 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 Cd1 0.01961(14) 0.02730(15) 0.02194(14) 0.00779(11) 0.01195(11) 0.00652(11) Cd2 0.03425(18) 0.03644(18) 0.02688(17) 0.00403(13) 0.01021(14) 0.01258(14) Br1 0.02325(19) 0.02591(19) 0.0330(2) 0.00602(16) 0.01699(17) 0.00526(15) Br2 0.0508(3) 0.0344(3) 0.0744(4) 0.0205(3) -0.0010(3) 0.0062(2) Br3 0.0353(3) 0.0693(4) 0.0276(2) 0.0182(2) 0.0051(2) -0.0013(2) Br4 0.0391(3) 0.0816(4) 0.0303(3) -0.0032(2) 0.0124(2) 0.0276(3) Fe1 0.0236(3) 0.0268(3) 0.0307(3) 0.0099(2) 0.0165(2) 0.0066(2) Fe2 0.0205(3) 0.0243(3) 0.0472(4) 0.0100(3) 0.0134(3) 0.0057(2) P1 0.0527(7) 0.0302(6) 0.0388(6) 0.0152(5) 0.0281(6) 0.0150(5) P2 0.0224(5) 0.0259(5) 0.0231(5) 0.0084(4) 0.0097(4) 0.0057(4) O1 0.0234(14) 0.0339(15) 0.0264(14) 0.0102(12) 0.0129(12) 0.0039(12) O2 0.0271(14) 0.0314(15) 0.0308(15) 0.0110(13) 0.0153(12) 0.0093(12) N11 0.0246(17) 0.0328(18) 0.0272(18) 0.0106(15) 0.0142(14) 0.0056(14) N12 0.0225(16) 0.0290(17) 0.0247(17) 0.0092(14) 0.0138(14) 0.0084(13) N21 0.0302(18) 0.0269(17) 0.0290(18) 0.0017(15) 0.0187(15) 0.0062(14) N22 0.0275(17) 0.0333(18) 0.0247(17) 0.0095(15) 0.0143(14) 0.0097(14) C1 0.031(2) 0.026(2) 0.036(2) 0.0139(18) 0.0189(18) 0.0080(17) C2 0.036(2) 0.025(2) 0.049(3) 0.0140(19) 0.027(2) 0.0134(17) C3 0.050(3) 0.030(2) 0.040(3) 0.0081(19) 0.032(2) 0.008(2) C4 0.037(2) 0.035(2) 0.029(2) 0.0079(19) 0.0106(19) -0.0026(19) C5 0.025(2) 0.034(2) 0.041(2) 0.015(2) 0.0147(19) 0.0023(17) C6 0.0232(19) 0.0227(18) 0.031(2) 0.0087(16) 0.0144(17) 0.0040(15) C7 0.037(2) 0.032(2) 0.038(2) 0.0142(19) 0.024(2) 0.0142(18) C8 0.039(2) 0.032(2) 0.054(3) 0.018(2) 0.033(2) 0.0179(19) C9 0.049(3) 0.027(2) 0.042(3) 0.0089(19) 0.034(2) 0.0068(19) C10 0.032(2) 0.028(2) 0.032(2) 0.0095(17) 0.0183(18) 0.0026(17) C11 0.0238(19) 0.0183(17) 0.028(2) 0.0062(15) 0.0133(16) 0.0024(14) C12 0.051(3) 0.038(2) 0.051(3) 0.021(2) 0.039(2) 0.021(2) C13 0.050(3) 0.033(2) 0.068(4) 0.017(2) 0.041(3) 0.014(2) C14 0.054(3) 0.042(3) 0.102(5) 0.027(3) 0.050(4) 0.016(3) C15 0.068(4) 0.050(3) 0.131(6) 0.054(4) 0.073(5) 0.031(3) C16 0.090(5) 0.062(4) 0.103(5) 0.057(4) 0.080(5) 0.051(4) C17 0.075(4) 0.044(3) 0.066(4) 0.033(3) 0.054(3) 0.032(3) C18 0.054(3) 0.050(3) 0.034(3) 0.021(2) 0.009(2) 0.010(2) C19 0.052(4) 0.071(4) 0.086(5) 0.038(4) 0.014(3) 0.021(3) C20 0.056(5) 0.145(9) 0.160(9) 0.101(8) 0.019(5) 0.045(5) C21 0.053(5) 0.131(9) 0.133(8) 0.085(7) -0.027(5) -0.017(5) C22 0.072(5) 0.087(6) 0.064(5) 0.037(4) -0.015(4) -0.016(4) C23 0.079(5) 0.063(4) 0.032(3) 0.017(3) 0.000(3) -0.007(3) C24 0.027(2) 0.0263(19) 0.0215(19) 0.0038(16) 0.0122(16) 0.0049(16) C25 0.0228(19) 0.033(2) 0.027(2) 0.0099(17) 0.0156(16) 0.0078(16) C26 0.028(2) 0.030(2) 0.035(2) 0.0123(18) 0.0192(18) 0.0099(17) C27 0.041(3) 0.037(2) 0.044(3) 0.023(2) 0.022(2) 0.013(2) C28 0.035(2) 0.051(3) 0.038(3) 0.025(2) 0.013(2) 0.013(2) C29 0.030(2) 0.045(3) 0.029(2) 0.013(2) 0.0099(18) 0.0051(19) C51 0.0201(18) 0.0267(19) 0.028(2) 0.0093(16) 0.0096(16) 0.0050(15) C52 0.0222(19) 0.031(2) 0.033(2) 0.0057(18) 0.0123(17) 0.0096(16) C53 0.026(2) 0.027(2) 0.048(3) 0.008(2) 0.013(2) 0.0091(17) C54 0.031(2) 0.036(2) 0.054(3) 0.025(2) 0.017(2) 0.0081(19) C55 0.030(2) 0.034(2) 0.031(2) 0.0128(18) 0.0130(18) 0.0080(18) C56 0.0186(19) 0.029(2) 0.051(3) 0.010(2) 0.0146(19) 0.0069(16) C57 0.030(2) 0.027(2) 0.076(4) -0.003(2) 0.029(2) 0.0042(18) C58 0.030(3) 0.029(3) 0.112(6) 0.001(3) 0.025(3) 0.012(2) C59 0.023(2) 0.039(3) 0.109(5) 0.040(3) 0.006(3) 0.009(2) C60 0.021(2) 0.041(3) 0.067(3) 0.029(3) 0.004(2) 0.0042(19) C61 0.0168(18) 0.028(2) 0.033(2) 0.0055(18) 0.0119(16) 0.0041(15) C62 0.026(2) 0.029(2) 0.026(2) 0.0064(17) 0.0111(17) 0.0053(16) C63 0.031(2) 0.037(2) 0.045(3) 0.022(2) 0.018(2) 0.0107(19) C64 0.028(2) 0.048(3) 0.053(3) 0.025(2) 0.013(2) 0.012(2) C65 0.027(2) 0.049(3) 0.049(3) 0.017(2) 0.014(2) 0.004(2) C66 0.034(2) 0.041(3) 0.051(3) 0.018(2) 0.020(2) 0.001(2) C67 0.032(2) 0.037(2) 0.038(2) 0.019(2) 0.014(2) 0.0043(19) C68 0.025(2) 0.031(2) 0.025(2) 0.0104(17) 0.0088(16) 0.0019(16) C69 0.036(2) 0.035(2) 0.030(2) 0.0137(19) 0.0142(19) 0.0093(18) C70 0.037(3) 0.042(3) 0.049(3) 0.026(2) 0.014(2) 0.010(2) C71 0.042(3) 0.051(3) 0.031(2) 0.022(2) 0.006(2) -0.001(2) C72 0.045(3) 0.042(3) 0.027(2) 0.009(2) 0.014(2) -0.002(2) C73 0.035(2) 0.040(2) 0.033(2) 0.015(2) 0.0172(19) 0.0086(19) C74 0.032(2) 0.029(2) 0.028(2) 0.0078(17) 0.0210(18) 0.0068(16) C75 0.037(2) 0.030(2) 0.027(2) 0.0076(17) 0.0186(19) 0.0095(18) C76 0.036(2) 0.055(3) 0.033(2) 0.016(2) 0.020(2) 0.022(2) C77 0.054(3) 0.076(4) 0.035(3) 0.021(3) 0.018(2) 0.040(3) C78 0.084(4) 0.107(5) 0.035(3) 0.038(3) 0.029(3) 0.064(4) C79 0.072(4) 0.076(4) 0.033(3) 0.024(3) 0.034(3) 0.046(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 Cd1 O1 2.324(3) . ? Cd1 O2 2.328(3) . ? Cd1 N22 2.358(3) . ? Cd1 N12 2.385(3) . ? Cd1 Br1 2.7510(5) . ? Cd1 Br1 2.7794(4) 2_755 ? Cd2 Br3 2.5638(6) . ? Cd2 Br4 2.5685(6) . ? Cd2 Br2 2.5688(7) . ? Cd2 P2 2.5894(11) . ? Br1 Cd1 2.7794(4) 2_755 ? Fe1 C5 2.025(4) . ? Fe1 C7 2.029(4) . ? Fe1 C6 2.029(4) . ? Fe1 C1 2.031(4) . ? Fe1 C8 2.039(4) . ? Fe1 C2 2.041(4) . ? Fe1 C3 2.044(4) . ? Fe1 C10 2.044(4) . ? Fe1 C4 2.045(4) . ? Fe1 C9 2.055(4) . ? Fe2 C56 2.031(4) . ? Fe2 C55 2.038(4) . ? Fe2 C60 2.038(5) . ? Fe2 C52 2.038(4) . ? Fe2 C51 2.040(4) . ? Fe2 C54 2.042(5) . ? Fe2 C53 2.043(4) . ? Fe2 C57 2.045(5) . ? Fe2 C59 2.053(5) . ? Fe2 C58 2.054(5) . ? P1 C1 1.815(4) . ? P1 C18 1.831(6) . ? P1 C12 1.832(5) . ? P2 C51 1.796(4) . ? P2 C68 1.816(4) . ? P2 C62 1.821(4) . ? O1 C11 1.243(5) . ? O2 C61 1.253(5) . ? N11 C11 1.335(5) . ? N11 C24 1.462(5) . ? N11 H1N 0.9206 . ? N12 C26 1.355(5) . ? N12 C25 1.363(5) . ? N21 C61 1.334(5) . ? N21 C74 1.444(5) . ? N21 H2N 0.8727 . ? N22 C76 1.335(6) . ? N22 C75 1.344(5) . ? C1 C5 1.424(6) . ? C1 C2 1.429(6) . ? C2 C3 1.420(7) . ? C2 H2 0.9300 . ? C3 C4 1.407(7) . ? C3 H3 0.9300 . ? C4 C5 1.414(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.431(6) . ? C6 C10 1.433(6) . ? C6 C11 1.483(5) . ? C7 C8 1.409(6) . ? C7 H7 0.9300 . ? C8 C9 1.410(7) . ? C8 H8 0.9300 . ? C9 C10 1.420(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C17 1.384(7) . ? C12 C13 1.409(7) . ? C13 C14 1.390(7) . ? C13 H13 0.9300 . ? C14 C15 1.357(9) . ? C14 H14 0.9300 . ? C15 C16 1.377(10) . ? C15 H15 0.9300 . ? C16 C17 1.380(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.376(9) . ? C18 C23 1.416(8) . ? C19 C20 1.407(10) . ? C19 H19 0.9300 . ? C20 C21 1.403(14) . ? C20 H20 0.9300 . ? C21 C22 1.381(15) . ? C21 H21 0.9300 . ? C22 C23 1.373(11) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.498(6) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C29 1.390(6) . ? C26 C27 1.381(6) . ? C26 H26 0.9300 . ? C27 C28 1.372(7) . ? C27 H27 0.9300 . ? C28 C29 1.379(7) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C51 C55 1.436(6) . ? C51 C52 1.443(6) . ? C52 C53 1.410(6) . ? C52 H52 0.9300 . ? C53 C54 1.407(7) . ? C53 H53 0.9300 . ? C54 C55 1.424(6) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? C56 C60 1.409(7) . ? C56 C57 1.432(7) . ? C56 C61 1.469(6) . ? C57 C58 1.410(8) . ? C57 H57 0.9300 . ? C58 C59 1.387(10) . ? C58 H58 0.9300 . ? C59 C60 1.425(8) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C62 C63 1.381(6) . ? C62 C67 1.402(6) . ? C63 C64 1.389(6) . ? C63 H63 0.9300 . ? C64 C65 1.382(7) . ? C64 H64 0.9300 . ? C65 C66 1.389(7) . ? C65 H65 0.9300 . ? C66 C67 1.380(6) . ? C66 H66 0.9300 . ? C67 H67 0.9300 . ? C68 C69 1.395(6) . ? C68 C73 1.400(6) . ? C69 C70 1.381(6) . ? C69 H69 0.9300 . ? C70 C71 1.384(8) . ? C70 H70 0.9300 . ? C71 C72 1.381(8) . ? C71 H71 0.9300 . ? C72 C73 1.387(6) . ? C72 H72 0.9300 . ? C73 H73 0.9300 . ? C74 C75 1.509(6) . ? C74 H74A 0.9700 . ? C74 H74B 0.9700 . ? C75 C79 1.383(7) . ? C76 C77 1.373(7) . ? C76 H76 0.9300 . ? C77 C78 1.373(8) . ? C77 H77 0.9300 . ? C78 C79 1.373(8) . ? C78 H78 0.9300 . ? C79 H79 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 O1 Cd1 O2 94.62(10) . . ? O1 Cd1 N22 86.34(10) . . ? O2 Cd1 N22 86.79(11) . . ? O1 Cd1 N12 86.24(10) . . ? O2 Cd1 N12 81.71(10) . . ? N22 Cd1 N12 165.76(11) . . ? O1 Cd1 Br1 94.90(7) . . ? O2 Cd1 Br1 170.48(7) . . ? N22 Cd1 Br1 93.82(8) . . ? N12 Cd1 Br1 98.91(8) . . ? O1 Cd1 Br1 179.49(8) . 2_755 ? O2 Cd1 Br1 84.87(7) . 2_755 ? N22 Cd1 Br1 93.60(8) . 2_755 ? N12 Cd1 Br1 93.71(8) . 2_755 ? Br1 Cd1 Br1 85.612(14) . 2_755 ? Br3 Cd2 Br4 107.76(2) . . ? Br3 Cd2 Br2 119.77(2) . . ? Br4 Cd2 Br2 111.66(2) . . ? Br3 Cd2 P2 100.90(3) . . ? Br4 Cd2 P2 112.42(3) . . ? Br2 Cd2 P2 103.82(3) . . ? Cd1 Br1 Cd1 94.388(14) . 2_755 ? C5 Fe1 C7 126.00(18) . . ? C5 Fe1 C6 165.43(17) . . ? C7 Fe1 C6 41.29(17) . . ? C5 Fe1 C1 41.10(17) . . ? C7 Fe1 C1 164.41(17) . . ? C6 Fe1 C1 152.82(17) . . ? C5 Fe1 C8 105.96(18) . . ? C7 Fe1 C8 40.54(17) . . ? C6 Fe1 C8 68.62(17) . . ? C1 Fe1 C8 126.79(17) . . ? C5 Fe1 C2 68.81(18) . . ? C7 Fe1 C2 152.72(17) . . ? C6 Fe1 C2 119.50(16) . . ? C1 Fe1 C2 41.09(16) . . ? C8 Fe1 C2 166.24(18) . . ? C5 Fe1 C3 68.36(18) . . ? C7 Fe1 C3 118.18(18) . . ? C6 Fe1 C3 109.32(17) . . ? C1 Fe1 C3 68.80(17) . . ? C8 Fe1 C3 150.7(2) . . ? C2 Fe1 C3 40.69(19) . . ? C5 Fe1 C10 151.01(17) . . ? C7 Fe1 C10 69.28(18) . . ? C6 Fe1 C10 41.18(16) . . ? C1 Fe1 C10 118.12(17) . . ? C8 Fe1 C10 68.54(19) . . ? C2 Fe1 C10 109.46(18) . . ? C3 Fe1 C10 130.29(18) . . ? C5 Fe1 C4 40.66(18) . . ? C7 Fe1 C4 106.88(19) . . ? C6 Fe1 C4 128.43(17) . . ? C1 Fe1 C4 68.72(18) . . ? C8 Fe1 C4 116.7(2) . . ? C2 Fe1 C4 68.3(2) . . ? C3 Fe1 C4 40.3(2) . . ? C10 Fe1 C4 167.69(18) . . ? C5 Fe1 C9 116.90(18) . . ? C7 Fe1 C9 68.19(18) . . ? C6 Fe1 C9 68.34(16) . . ? C1 Fe1 C9 107.72(18) . . ? C8 Fe1 C9 40.28(19) . . ? C2 Fe1 C9 129.6(2) . . ? C3 Fe1 C9 168.3(2) . . ? C10 Fe1 C9 40.53(17) . . ? C4 Fe1 C9 150.1(2) . . ? C56 Fe2 C55 146.70(19) . . ? C56 Fe2 C60 40.53(19) . . ? C55 Fe2 C60 172.17(18) . . ? C56 Fe2 C52 130.06(18) . . ? C55 Fe2 C52 69.00(17) . . ? C60 Fe2 C52 108.5(2) . . ? C56 Fe2 C51 170.36(18) . . ? C55 Fe2 C51 41.23(16) . . ? C60 Fe2 C51 132.10(19) . . ? C52 Fe2 C51 41.44(16) . . ? C56 Fe2 C54 114.04(18) . . ? C55 Fe2 C54 40.86(18) . . ? C60 Fe2 C54 146.0(2) . . ? C52 Fe2 C54 68.44(19) . . ? C51 Fe2 C54 69.17(17) . . ? C56 Fe2 C53 107.27(17) . . ? C55 Fe2 C53 68.29(18) . . ? C60 Fe2 C53 115.0(2) . . ? C52 Fe2 C53 40.44(18) . . ? C51 Fe2 C53 68.87(17) . . ? C54 Fe2 C53 40.3(2) . . ? C56 Fe2 C57 41.14(19) . . ? C55 Fe2 C57 115.3(2) . . ? C60 Fe2 C57 68.6(2) . . ? C52 Fe2 C57 169.25(18) . . ? C51 Fe2 C57 147.94(18) . . ? C54 Fe2 C57 107.8(2) . . ? C53 Fe2 C57 130.4(2) . . ? C56 Fe2 C59 67.77(19) . . ? C55 Fe2 C59 133.2(2) . . ? C60 Fe2 C59 40.8(2) . . ? C52 Fe2 C59 117.8(3) . . ? C51 Fe2 C59 110.61(19) . . ? C54 Fe2 C59 170.9(3) . . ? C53 Fe2 C59 148.7(3) . . ? C57 Fe2 C59 67.2(3) . . ? C56 Fe2 C58 68.18(19) . . ? C55 Fe2 C58 110.1(2) . . ? C60 Fe2 C58 68.1(3) . . ? C52 Fe2 C58 149.4(2) . . ? C51 Fe2 C58 117.09(19) . . ? C54 Fe2 C58 132.0(3) . . ? C53 Fe2 C58 169.7(3) . . ? C57 Fe2 C58 40.2(2) . . ? C59 Fe2 C58 39.5(3) . . ? C1 P1 C18 99.3(2) . . ? C1 P1 C12 101.0(2) . . ? C18 P1 C12 103.4(2) . . ? C51 P2 C68 108.23(19) . . ? C51 P2 C62 105.29(19) . . ? C68 P2 C62 107.53(19) . . ? C51 P2 Cd2 117.26(14) . . ? C68 P2 Cd2 113.02(15) . . ? C62 P2 Cd2 104.75(14) . . ? C11 O1 Cd1 136.1(3) . . ? C61 O2 Cd1 137.6(3) . . ? C11 N11 C24 123.1(3) . . ? C11 N11 H1N 109.1 . . ? C24 N11 H1N 127.8 . . ? C26 N12 C25 117.5(3) . . ? C26 N12 Cd1 117.1(3) . . ? C25 N12 Cd1 125.5(3) . . ? C61 N21 C74 124.1(3) . . ? C61 N21 H2N 121.3 . . ? C74 N21 H2N 114.5 . . ? C76 N22 C75 117.8(4) . . ? C76 N22 Cd1 116.9(3) . . ? C75 N22 Cd1 125.3(3) . . ? C5 C1 C2 107.3(4) . . ? C5 C1 P1 123.6(3) . . ? C2 C1 P1 129.1(3) . . ? C5 C1 Fe1 69.2(2) . . ? C2 C1 Fe1 69.8(2) . . ? P1 C1 Fe1 124.1(2) . . ? C3 C2 C1 107.8(4) . . ? C3 C2 Fe1 69.7(3) . . ? C1 C2 Fe1 69.1(2) . . ? C3 C2 H2 126.1 . . ? C1 C2 H2 126.1 . . ? Fe1 C2 H2 126.6 . . ? C4 C3 C2 108.4(4) . . ? C4 C3 Fe1 69.9(3) . . ? C2 C3 Fe1 69.6(2) . . ? C4 C3 H3 125.8 . . ? C2 C3 H3 125.8 . . ? Fe1 C3 H3 126.3 . . ? C3 C4 C5 108.3(4) . . ? C3 C4 Fe1 69.8(3) . . ? C5 C4 Fe1 68.9(2) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe1 C4 H4 127.0 . . ? C4 C5 C1 108.3(4) . . ? C4 C5 Fe1 70.4(2) . . ? C1 C5 Fe1 69.7(2) . . ? C4 C5 H5 125.8 . . ? C1 C5 H5 125.8 . . ? Fe1 C5 H5 125.6 . . ? C7 C6 C10 107.9(3) . . ? C7 C6 C11 128.0(4) . . ? C10 C6 C11 124.0(4) . . ? C7 C6 Fe1 69.3(2) . . ? C10 C6 Fe1 70.0(2) . . ? C11 C6 Fe1 129.6(3) . . ? C8 C7 C6 107.7(4) . . ? C8 C7 Fe1 70.1(2) . . ? C6 C7 Fe1 69.4(2) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? Fe1 C7 H7 125.9 . . ? C7 C8 C9 108.6(4) . . ? C7 C8 Fe1 69.3(2) . . ? C9 C8 Fe1 70.5(3) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? Fe1 C8 H8 126.1 . . ? C8 C9 C10 108.7(4) . . ? C8 C9 Fe1 69.2(3) . . ? C10 C9 Fe1 69.3(2) . . ? C8 C9 H9 125.6 . . ? C10 C9 H9 125.6 . . ? Fe1 C9 H9 127.4 . . ? C9 C10 C6 107.1(4) . . ? C9 C10 Fe1 70.1(2) . . ? C6 C10 Fe1 68.8(2) . . ? C9 C10 H10 126.5 . . ? C6 C10 H10 126.5 . . ? Fe1 C10 H10 126.1 . . ? O1 C11 N11 122.4(4) . . ? O1 C11 C6 120.9(4) . . ? N11 C11 C6 116.7(3) . . ? C17 C12 C13 118.2(5) . . ? C17 C12 P1 120.9(4) . . ? C13 C12 P1 120.2(4) . . ? C14 C13 C12 119.7(6) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C15 C14 C13 120.7(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.4(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 119.9(6) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 121.1(6) . . ? C16 C17 H17 119.5 . . ? C12 C17 H17 119.5 . . ? C19 C18 C23 119.1(6) . . ? C19 C18 P1 125.0(5) . . ? C23 C18 P1 115.7(5) . . ? C18 C19 C20 121.3(7) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 118.0(10) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C22 C21 C20 121.0(8) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C23 C22 C21 120.2(8) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 120.2(8) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? N11 C24 C25 110.5(3) . . ? N11 C24 H24A 109.5 . . ? C25 C24 H24A 109.5 . . ? N11 C24 H24B 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 108.1 . . ? N12 C25 C29 121.7(4) . . ? N12 C25 C24 117.2(3) . . ? C29 C25 C24 120.9(4) . . ? N12 C26 C27 122.8(4) . . ? N12 C26 H26 118.6 . . ? C27 C26 H26 118.6 . . ? C28 C27 C26 119.3(4) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 119.1(4) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C28 C29 C25 119.5(4) . . ? C28 C29 H29 120.2 . . ? C25 C29 H29 120.2 . . ? C55 C51 C52 106.6(4) . . ? C55 C51 P2 122.8(3) . . ? C52 C51 P2 130.5(3) . . ? C55 C51 Fe2 69.3(2) . . ? C52 C51 Fe2 69.2(2) . . ? P2 C51 Fe2 127.4(2) . . ? C53 C52 C51 108.0(4) . . ? C53 C52 Fe2 70.0(2) . . ? C51 C52 Fe2 69.4(2) . . ? C53 C52 H52 126.0 . . ? C51 C52 H52 126.0 . . ? Fe2 C52 H52 126.3 . . ? C54 C53 C52 109.1(4) . . ? C54 C53 Fe2 69.8(3) . . ? C52 C53 Fe2 69.6(2) . . ? C54 C53 H53 125.5 . . ? C52 C53 H53 125.5 . . ? Fe2 C53 H53 126.7 . . ? C53 C54 C55 108.0(4) . . ? C53 C54 Fe2 69.9(3) . . ? C55 C54 Fe2 69.4(2) . . ? C53 C54 H54 126.0 . . ? C55 C54 H54 126.0 . . ? Fe2 C54 H54 126.3 . . ? C54 C55 C51 108.2(4) . . ? C54 C55 Fe2 69.7(3) . . ? C51 C55 Fe2 69.5(2) . . ? C54 C55 H55 125.9 . . ? C51 C55 H55 125.9 . . ? Fe2 C55 H55 126.5 . . ? C60 C56 C57 108.1(4) . . ? C60 C56 C61 124.2(5) . . ? C57 C56 C61 127.7(5) . . ? C60 C56 Fe2 70.0(3) . . ? C57 C56 Fe2 70.0(2) . . ? C61 C56 Fe2 125.1(3) . . ? C58 C57 C56 107.4(6) . . ? C58 C57 Fe2 70.2(3) . . ? C56 C57 Fe2 68.9(3) . . ? C58 C57 H57 126.3 . . ? C56 C57 H57 126.3 . . ? Fe2 C57 H57 126.1 . . ? C59 C58 C57 108.5(5) . . ? C59 C58 Fe2 70.2(3) . . ? C57 C58 Fe2 69.5(3) . . ? C59 C58 H58 125.8 . . ? C57 C58 H58 125.8 . . ? Fe2 C58 H58 126.1 . . ? C58 C59 C60 109.1(5) . . ? C58 C59 Fe2 70.3(3) . . ? C60 C59 Fe2 69.0(3) . . ? C58 C59 H59 125.4 . . ? C60 C59 H59 125.4 . . ? Fe2 C59 H59 126.8 . . ? C56 C60 C59 106.9(6) . . ? C56 C60 Fe2 69.5(3) . . ? C59 C60 Fe2 70.2(3) . . ? C56 C60 H60 126.6 . . ? C59 C60 H60 126.6 . . ? Fe2 C60 H60 125.4 . . ? O2 C61 N21 122.4(4) . . ? O2 C61 C56 120.5(4) . . ? N21 C61 C56 117.1(4) . . ? C63 C62 C67 119.3(4) . . ? C63 C62 P2 121.2(3) . . ? C67 C62 P2 118.9(3) . . ? C62 C63 C64 120.4(4) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C65 C64 C63 120.1(4) . . ? C65 C64 H64 119.9 . . ? C63 C64 H64 119.9 . . ? C64 C65 C66 119.9(4) . . ? C64 C65 H65 120.0 . . ? C66 C65 H65 120.0 . . ? C67 C66 C65 120.1(4) . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C67 C62 120.2(4) . . ? C66 C67 H67 119.9 . . ? C62 C67 H67 119.9 . . ? C69 C68 C73 119.1(4) . . ? C69 C68 P2 117.9(3) . . ? C73 C68 P2 122.9(3) . . ? C70 C69 C68 120.2(4) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.9 . . ? C69 C70 C71 120.5(5) . . ? C69 C70 H70 119.7 . . ? C71 C70 H70 119.7 . . ? C72 C71 C70 119.9(4) . . ? C72 C71 H71 120.1 . . ? C70 C71 H71 120.1 . . ? C71 C72 C73 120.3(5) . . ? C71 C72 H72 119.9 . . ? C73 C72 H72 119.9 . . ? C72 C73 C68 120.0(5) . . ? C72 C73 H73 120.0 . . ? C68 C73 H73 120.0 . . ? N21 C74 C75 112.0(3) . . ? N21 C74 H74A 109.2 . . ? C75 C74 H74A 109.2 . . ? N21 C74 H74B 109.2 . . ? C75 C74 H74B 109.2 . . ? H74A C74 H74B 107.9 . . ? N22 C75 C79 121.5(4) . . ? N22 C75 C74 117.7(4) . . ? C79 C75 C74 120.8(4) . . ? N22 C76 C77 124.0(4) . . ? N22 C76 H76 118.0 . . ? C77 C76 H76 118.0 . . ? C76 C77 C78 117.8(5) . . ? C76 C77 H77 121.1 . . ? C78 C77 H77 121.1 . . ? C77 C78 C79 119.5(5) . . ? C77 C78 H78 120.3 . . ? C79 C78 H78 120.3 . . ? C78 C79 C75 119.4(5) . . ? C78 C79 H79 120.3 . . ? C75 C79 H79 120.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.423 _refine_diff_density_min -2.139 _refine_diff_density_rms 0.125 #===END data_jk84d _database_code_depnum_ccdc_archive 'CCDC 670839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H50 Br4 Fe2 Hg2 N4 O2 P2' _chemical_formula_sum 'C58 H50 Br4 Fe2 Hg2 N4 O2 P2' _chemical_formula_weight 1729.48 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6494(1) _cell_length_b 28.7444(3) _cell_length_c 10.0076(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.8681(6) _cell_angle_gamma 90.00 _cell_volume 2779.38(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 94862 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 8.998 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.212 _exptl_absorpt_correction_T_max 0.719 _exptl_absorpt_process_details ; gaussian absorption correction from indexed crystal shape ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\w and \p scans to fill the Ewald sphere' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_reflns_number 43116 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6365 _reflns_number_gt 5358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _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^)+(0.0338P)^2^+3.3754P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6365 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0402 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hg Hg 0.967515(16) 0.067361(5) 0.496963(15) 0.02316(6) Uani 1 1 d . . . Br1 Br 1.05651(5) 0.110024(16) 0.33767(5) 0.03758(11) Uani 1 1 d . . . Br2 Br 1.17869(4) 0.008301(13) 0.67598(4) 0.02626(9) Uani 1 1 d . . . Fe Fe 1.04283(5) 0.180148(17) 0.80440(5) 0.01698(11) Uani 1 1 d . . . P P 0.84159(10) 0.08493(3) 0.64453(10) 0.01768(19) Uani 1 1 d . . . O O 0.7680(3) 0.26425(9) 0.7426(3) 0.0259(6) Uani 1 1 d . . . N1 N 0.7259(3) 0.26039(10) 0.5014(3) 0.0204(6) Uani 1 1 d . . . H1N H 0.7576 0.2546 0.4342 0.037(13) Uiso 1 1 d R . . N2 N 0.4515(4) 0.34699(11) 0.3523(4) 0.0289(8) Uani 1 1 d . . . C1 C 0.9500(4) 0.11856(12) 0.8004(4) 0.0189(7) Uani 1 1 d . . . C2 C 0.9111(4) 0.15215(12) 0.8823(4) 0.0222(8) Uani 1 1 d . . . H2 H 0.8216 0.1621 0.8606 0.027 Uiso 1 1 calc R . . C3 C 1.0325(4) 0.16730(13) 1.0014(4) 0.0249(9) Uani 1 1 d . . . H3 H 1.0369 0.1891 1.0718 0.030 Uiso 1 1 calc R . . C4 C 1.1472(4) 0.14357(12) 0.9957(4) 0.0254(9) Uani 1 1 d . . . H4 H 1.2393 0.1472 1.0618 0.031 Uiso 1 1 calc R . . C5 C 1.0977(4) 0.11343(12) 0.8726(4) 0.0218(8) Uani 1 1 d . . . H5 H 1.1512 0.0938 0.8436 0.026 Uiso 1 1 calc R . . C6 C 0.9477(4) 0.23620(12) 0.6785(4) 0.0172(7) Uani 1 1 d . . . C7 C 1.0689(4) 0.25026(12) 0.8026(4) 0.0209(8) Uani 1 1 d . . . H7 H 1.0726 0.2709 0.8758 0.025 Uiso 1 1 calc R . . C8 C 1.1834(4) 0.22698(13) 0.7943(4) 0.0241(8) Uani 1 1 d . . . H8 H 1.2755 0.2300 0.8612 0.029 Uiso 1 1 calc R . . C9 C 1.1330(4) 0.19832(13) 0.6660(4) 0.0234(8) Uani 1 1 d . . . H9 H 1.1861 0.1791 0.6353 0.028 Uiso 1 1 calc R . . C10 C 0.9874(4) 0.20424(12) 0.5937(4) 0.0201(7) Uani 1 1 d . . . H10 H 0.9283 0.1899 0.5065 0.024 Uiso 1 1 calc R . . C11 C 0.8066(4) 0.25386(12) 0.6455(4) 0.0196(7) Uani 1 1 d . . . C12 C 0.7865(4) 0.03530(12) 0.7176(4) 0.0206(8) Uani 1 1 d . . . C13 C 0.8349(5) 0.02820(14) 0.8681(4) 0.0278(9) Uani 1 1 d . . . H13 H 0.9003 0.0484 0.9333 0.033 Uiso 1 1 calc R . . C14 C 0.7863(5) -0.00878(15) 0.9221(5) 0.0349(10) Uani 1 1 d . . . H14 H 0.8184 -0.0133 1.0231 0.042 Uiso 1 1 calc R . . C15 C 0.6894(5) -0.03893(14) 0.8242(5) 0.0352(10) Uani 1 1 d . . . H15 H 0.6551 -0.0634 0.8596 0.042 Uiso 1 1 calc R . . C16 C 0.6439(5) -0.03264(14) 0.6743(5) 0.0354(10) Uani 1 1 d . . . H16 H 0.5804 -0.0533 0.6092 0.042 Uiso 1 1 calc R . . C17 C 0.6923(5) 0.00435(14) 0.6207(5) 0.0299(9) Uani 1 1 d . . . H17 H 0.6616 0.0084 0.5196 0.036 Uiso 1 1 calc R . . C18 C 0.6849(4) 0.11762(12) 0.5399(4) 0.0197(8) Uani 1 1 d . . . C19 C 0.5897(4) 0.12599(14) 0.5995(4) 0.0281(9) Uani 1 1 d . . . H19 H 0.6076 0.1153 0.6935 0.034 Uiso 1 1 calc R . . C20 C 0.4690(4) 0.15005(15) 0.5192(4) 0.0303(9) Uani 1 1 d . . . H20 H 0.4062 0.1557 0.5596 0.036 Uiso 1 1 calc R . . C21 C 0.4412(4) 0.16578(14) 0.3789(5) 0.0300(9) Uani 1 1 d . . . H21 H 0.3593 0.1817 0.3246 0.036 Uiso 1 1 calc R . . C22 C 0.5360(5) 0.15776(14) 0.3195(4) 0.0306(9) Uani 1 1 d . . . H22 H 0.5178 0.1685 0.2254 0.037 Uiso 1 1 calc R . . C23 C 0.6574(4) 0.13384(13) 0.3995(4) 0.0255(8) Uani 1 1 d . . . H23 H 0.7206 0.1286 0.3593 0.031 Uiso 1 1 calc R . . C24 C 0.5851(4) 0.27816(13) 0.4498(4) 0.0229(8) Uani 1 1 d . . . H24A H 0.5438 0.2655 0.5119 0.028 Uiso 1 1 calc R . . H24B H 0.5317 0.2668 0.3506 0.028 Uiso 1 1 calc R . . C25 C 0.5738(4) 0.33056(13) 0.4492(4) 0.0210(8) Uani 1 1 d . . . C26 C 0.4334(5) 0.39297(15) 0.3469(6) 0.0380(11) Uani 1 1 d . . . H26 H 0.3494 0.4046 0.2789 0.046 Uiso 1 1 calc R . . C27 C 0.5306(6) 0.42439(15) 0.4350(6) 0.0399(12) Uani 1 1 d . . . H27 H 0.5123 0.4562 0.4278 0.048 Uiso 1 1 calc R . . C28 C 0.6565(5) 0.40705(14) 0.5347(5) 0.0346(10) Uani 1 1 d . . . H28 H 0.7253 0.4271 0.5958 0.041 Uiso 1 1 calc R . . C29 C 0.6786(4) 0.35940(13) 0.5422(4) 0.0253(8) Uani 1 1 d . . . H29 H 0.7622 0.3470 0.6086 0.030 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 Hg 0.02718(10) 0.02309(8) 0.02270(8) -0.00166(5) 0.01390(7) 0.00052(6) Br1 0.0453(3) 0.0378(2) 0.0395(2) 0.00981(18) 0.0275(2) 0.0008(2) Br2 0.0287(2) 0.02143(18) 0.02213(19) -0.00382(14) 0.00432(16) 0.00135(15) Fe 0.0189(3) 0.0154(2) 0.0164(2) 0.00106(18) 0.0072(2) 0.00111(19) P 0.0198(5) 0.0160(4) 0.0181(4) 0.0002(3) 0.0089(4) 0.0001(4) O 0.0316(17) 0.0291(14) 0.0220(13) 0.0037(11) 0.0160(12) 0.0074(12) N1 0.0228(18) 0.0218(15) 0.0176(15) 0.0000(12) 0.0094(13) 0.0032(13) N2 0.0223(19) 0.0283(18) 0.0382(19) 0.0107(15) 0.0148(16) 0.0059(14) C1 0.022(2) 0.0198(17) 0.0169(17) 0.0021(13) 0.0108(16) 0.0018(14) C2 0.029(2) 0.0191(18) 0.0238(18) 0.0033(14) 0.0166(17) 0.0022(15) C3 0.037(3) 0.0227(19) 0.0173(18) -0.0012(14) 0.0140(18) -0.0012(17) C4 0.031(2) 0.0179(18) 0.0189(18) 0.0014(14) 0.0019(17) 0.0001(16) C5 0.026(2) 0.0179(17) 0.0193(18) 0.0029(14) 0.0075(16) 0.0050(15) C6 0.021(2) 0.0172(17) 0.0157(16) 0.0012(13) 0.0100(15) -0.0010(14) C7 0.028(2) 0.0147(17) 0.0218(17) -0.0001(13) 0.0117(16) -0.0038(14) C8 0.022(2) 0.0221(18) 0.027(2) 0.0032(15) 0.0086(17) -0.0036(15) C9 0.026(2) 0.0255(19) 0.0248(19) 0.0042(15) 0.0167(18) 0.0015(16) C10 0.020(2) 0.0215(18) 0.0175(17) 0.0046(14) 0.0071(15) 0.0020(15) C11 0.023(2) 0.0188(17) 0.0183(17) 0.0031(14) 0.0093(16) 0.0010(15) C12 0.018(2) 0.0181(17) 0.029(2) 0.0008(14) 0.0123(17) 0.0005(14) C13 0.034(3) 0.025(2) 0.024(2) 0.0016(16) 0.0119(18) -0.0031(17) C14 0.043(3) 0.032(2) 0.032(2) 0.0092(18) 0.019(2) 0.001(2) C15 0.038(3) 0.020(2) 0.052(3) 0.0119(18) 0.023(2) 0.0000(18) C16 0.032(3) 0.024(2) 0.045(3) 0.0019(18) 0.011(2) -0.0057(18) C17 0.033(3) 0.028(2) 0.027(2) 0.0012(16) 0.0115(19) -0.0014(18) C18 0.020(2) 0.0179(17) 0.0183(17) -0.0008(13) 0.0054(15) -0.0010(14) C19 0.030(2) 0.032(2) 0.0233(19) 0.0009(16) 0.0124(18) 0.0012(18) C20 0.025(2) 0.035(2) 0.029(2) -0.0012(17) 0.0098(18) 0.0070(18) C21 0.023(2) 0.024(2) 0.034(2) -0.0034(17) 0.0032(18) 0.0047(16) C22 0.033(3) 0.033(2) 0.0209(19) 0.0071(16) 0.0065(18) 0.0037(18) C23 0.029(2) 0.026(2) 0.0236(19) 0.0017(15) 0.0133(18) 0.0001(16) C24 0.018(2) 0.0230(18) 0.0235(19) 0.0007(15) 0.0044(16) 0.0010(15) C25 0.022(2) 0.0257(19) 0.0200(18) 0.0022(15) 0.0133(16) 0.0025(15) C26 0.030(3) 0.033(2) 0.057(3) 0.017(2) 0.024(2) 0.0139(19) C27 0.055(3) 0.022(2) 0.056(3) 0.003(2) 0.036(3) 0.009(2) C28 0.048(3) 0.026(2) 0.032(2) -0.0041(17) 0.020(2) -0.007(2) C29 0.033(2) 0.0234(19) 0.0199(18) -0.0014(15) 0.0121(17) -0.0008(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 Hg P 2.4291(9) . ? Hg Br1 2.4929(4) . ? Hg Br2 2.7857(4) . ? Hg Br2 2.8077(4) 3_756 ? Br2 Hg 2.8077(4) 3_756 ? Fe C1 2.020(4) . ? Fe C6 2.034(3) . ? Fe C7 2.035(3) . ? Fe C2 2.035(4) . ? Fe C5 2.037(3) . ? Fe C8 2.047(4) . ? Fe C4 2.054(4) . ? Fe C3 2.054(3) . ? Fe C10 2.056(3) . ? Fe C9 2.056(4) . ? P C1 1.785(4) . ? P C12 1.810(4) . ? P C18 1.815(4) . ? O C11 1.241(4) . ? N1 C11 1.346(5) . ? N1 C24 1.457(5) . ? N1 H1N 0.8862 . ? N2 C26 1.333(5) . ? N2 C25 1.341(5) . ? C1 C2 1.436(5) . ? C1 C5 1.436(5) . ? C2 C3 1.409(6) . ? C2 H2 0.9300 . ? C3 C4 1.421(6) . ? C3 H3 0.9300 . ? C4 C5 1.415(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.422(5) . ? C6 C10 1.430(5) . ? C6 C11 1.485(5) . ? C7 C8 1.424(6) . ? C7 H7 0.9300 . ? C8 C9 1.427(5) . ? C8 H8 0.9300 . ? C9 C10 1.419(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C12 C17 1.386(5) . ? C12 C13 1.387(5) . ? C13 C14 1.387(6) . ? C13 H13 0.9300 . ? C14 C15 1.387(6) . ? C14 H14 0.9300 . ? C15 C16 1.380(6) . ? C15 H15 0.9300 . ? C16 C17 1.385(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.390(5) . ? C18 C19 1.397(5) . ? C19 C20 1.381(6) . ? C19 H19 0.9300 . ? C20 C21 1.383(6) . ? C20 H20 0.9300 . ? C21 C22 1.390(6) . ? C21 H21 0.9300 . ? C22 C23 1.384(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.511(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C29 1.387(5) . ? C26 C27 1.377(7) . ? C26 H26 0.9300 . ? C27 C28 1.384(7) . ? C27 H27 0.9300 . ? C28 C29 1.386(6) . ? C28 H28 0.9300 . ? C29 H29 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 P Hg Br1 137.91(2) . . ? P Hg Br2 103.80(2) . . ? Br1 Hg Br2 106.850(15) . . ? P Hg Br2 103.36(2) . 3_756 ? Br1 Hg Br2 104.374(14) . 3_756 ? Br2 Hg Br2 90.734(12) . 3_756 ? Hg Br2 Hg 89.266(12) . 3_756 ? C1 Fe C6 124.74(15) . . ? C1 Fe C7 159.23(15) . . ? C6 Fe C7 40.92(15) . . ? C1 Fe C2 41.47(14) . . ? C6 Fe C2 107.85(15) . . ? C7 Fe C2 120.89(15) . . ? C1 Fe C5 41.46(15) . . ? C6 Fe C5 162.05(14) . . ? C7 Fe C5 156.09(16) . . ? C2 Fe C5 69.29(15) . . ? C1 Fe C8 159.61(15) . . ? C6 Fe C8 68.45(15) . . ? C7 Fe C8 40.83(15) . . ? C2 Fe C8 156.21(15) . . ? C5 Fe C8 121.52(16) . . ? C1 Fe C4 68.80(15) . . ? C6 Fe C4 156.43(14) . . ? C7 Fe C4 119.53(15) . . ? C2 Fe C4 68.32(16) . . ? C5 Fe C4 40.46(14) . . ? C8 Fe C4 105.20(16) . . ? C1 Fe C3 68.79(15) . . ? C6 Fe C3 121.56(15) . . ? C7 Fe C3 104.42(15) . . ? C2 Fe C3 40.32(16) . . ? C5 Fe C3 68.46(15) . . ? C8 Fe C3 120.07(16) . . ? C4 Fe C3 40.48(16) . . ? C1 Fe C10 110.35(14) . . ? C6 Fe C10 40.92(14) . . ? C7 Fe C10 68.83(15) . . ? C2 Fe C10 125.38(16) . . ? C5 Fe C10 125.36(14) . . ? C8 Fe C10 68.19(15) . . ? C4 Fe C10 159.72(16) . . ? C3 Fe C10 159.54(16) . . ? C1 Fe C9 124.91(14) . . ? C6 Fe C9 68.51(14) . . ? C7 Fe C9 68.82(15) . . ? C2 Fe C9 161.86(15) . . ? C5 Fe C9 108.37(15) . . ? C8 Fe C9 40.68(15) . . ? C4 Fe C9 122.33(17) . . ? C3 Fe C9 157.01(16) . . ? C10 Fe C9 40.36(15) . . ? C1 P C12 105.91(16) . . ? C1 P C18 108.89(16) . . ? C12 P C18 105.41(17) . . ? C1 P Hg 108.93(12) . . ? C12 P Hg 115.95(12) . . ? C18 P Hg 111.43(12) . . ? C11 N1 C24 121.8(3) . . ? C11 N1 H1N 120.7 . . ? C24 N1 H1N 117.5 . . ? C26 N2 C25 117.3(4) . . ? C2 C1 C5 107.4(3) . . ? C2 C1 P 128.9(3) . . ? C5 C1 P 123.6(3) . . ? C2 C1 Fe 69.8(2) . . ? C5 C1 Fe 69.9(2) . . ? P C1 Fe 128.57(18) . . ? C3 C2 C1 108.0(3) . . ? C3 C2 Fe 70.5(2) . . ? C1 C2 Fe 68.7(2) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe C2 H2 126.3 . . ? C2 C3 C4 108.4(3) . . ? C2 C3 Fe 69.1(2) . . ? C4 C3 Fe 69.8(2) . . ? C2 C3 H3 125.8 . . ? C4 C3 H3 125.8 . . ? Fe C3 H3 126.9 . . ? C5 C4 C3 108.5(4) . . ? C5 C4 Fe 69.1(2) . . ? C3 C4 Fe 69.8(2) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Fe C4 H4 126.9 . . ? C4 C5 C1 107.7(3) . . ? C4 C5 Fe 70.4(2) . . ? C1 C5 Fe 68.6(2) . . ? C4 C5 H5 126.2 . . ? C1 C5 H5 126.2 . . ? Fe C5 H5 126.4 . . ? C7 C6 C10 108.3(3) . . ? C7 C6 C11 124.0(3) . . ? C10 C6 C11 127.7(3) . . ? C7 C6 Fe 69.6(2) . . ? C10 C6 Fe 70.4(2) . . ? C11 C6 Fe 127.0(2) . . ? C6 C7 C8 107.5(3) . . ? C6 C7 Fe 69.5(2) . . ? C8 C7 Fe 70.0(2) . . ? C6 C7 H7 126.3 . . ? C8 C7 H7 126.3 . . ? Fe C7 H7 125.8 . . ? C7 C8 C9 108.4(3) . . ? C7 C8 Fe 69.1(2) . . ? C9 C8 Fe 70.0(2) . . ? C7 C8 H8 125.8 . . ? C9 C8 H8 125.8 . . ? Fe C8 H8 126.7 . . ? C10 C9 C8 107.9(3) . . ? C10 C9 Fe 69.8(2) . . ? C8 C9 Fe 69.3(2) . . ? C10 C9 H9 126.0 . . ? C8 C9 H9 126.0 . . ? Fe C9 H9 126.4 . . ? C9 C10 C6 107.8(3) . . ? C9 C10 Fe 69.8(2) . . ? C6 C10 Fe 68.70(19) . . ? C9 C10 H10 126.1 . . ? C6 C10 H10 126.1 . . ? Fe C10 H10 127.0 . . ? O C11 N1 122.2(3) . . ? O C11 C6 123.1(3) . . ? N1 C11 C6 114.6(3) . . ? C17 C12 C13 119.7(4) . . ? C17 C12 P 119.0(3) . . ? C13 C12 P 121.3(3) . . ? C12 C13 C14 120.4(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 119.5(4) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.3(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C12 119.9(4) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C23 C18 C19 119.4(4) . . ? C23 C18 P 120.6(3) . . ? C19 C18 P 120.0(3) . . ? C20 C19 C18 120.2(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 120.2(4) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 119.8(4) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 120.3(4) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C18 120.0(4) . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? N1 C24 C25 114.8(3) . . ? N1 C24 H24A 108.6 . . ? C25 C24 H24A 108.6 . . ? N1 C24 H24B 108.6 . . ? C25 C24 H24B 108.6 . . ? H24A C24 H24B 107.5 . . ? N2 C25 C29 122.5(4) . . ? N2 C25 C24 113.9(3) . . ? C29 C25 C24 123.6(3) . . ? N2 C26 C27 124.6(4) . . ? N2 C26 H26 117.7 . . ? C27 C26 H26 117.7 . . ? C26 C27 C28 117.7(4) . . ? C26 C27 H27 121.2 . . ? C28 C27 H27 121.2 . . ? C27 C28 C29 119.0(4) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C28 C29 C25 118.9(4) . . ? C28 C29 H29 120.5 . . ? C25 C29 H29 120.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.900 _refine_diff_density_min -2.337 _refine_diff_density_rms 0.139 #===END