# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_niscn _database_code_CSD 161110 _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal Chemistry' loop_ _publ_author_name 'J. Pinkas' 'Z. Bastl' 'M. Slouf' 'J. Podlaha' 'P. Stepnicka' _publ_contact_author_name 'Dr P Stepnicka' _publ_contact_author_address ; Department of Inorganic Chemistry Charles University 128 40 Hlavova 2030 Prague 2 CZECH REPUBLIC ; _publ_contact_author_email 'STEPNIC@NATUR.CUNI.CZ' _publ_section_title ; Preparation and Solid-State Characterization of Nickel(II) Complexes With 1'-(Diphenylphosphino)Ferrocenecarboxylic Acid ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Ni(C23H19PO2Fe)2(NCS)2] * 2CHCl3' _chemical_formula_sum 'C50 H40 Cl6 Fe2 N2 Ni O4 P2 S2' _chemical_formula_weight 1242.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ni' 'Ni' 0.3393 1.1124 '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' 'S' 'S' 0.1246 0.1234 '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' 'C' 'C' 0.0033 0.0016 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.724(1) _cell_length_b 11.0215(6) _cell_length_c 12.758(1) _cell_angle_alpha 73.832(5) _cell_angle_beta 73.892(4) _cell_angle_gamma 71.608(4) _cell_volume 1344.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(1) _cell_measurement_reflns_used 5956 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.03 _exptl_crystal_description 'thin plate' _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 630 _exptl_absorpt_coefficient_mu 1.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.906 _exptl_absorpt_correction_T_max 0.966 _exptl_absorpt_process_details '(Blessing, 1995)' _diffrn_ambient_temperature 296(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ; CCD (rotation scans, rotation per image 2\%, exposure per frame 120 s, 108 images collected using 168\% \f and 48\% \w scans, which corresponds to the half of Ewald sphere) ; _diffrn_detector_area_resol_mean 0.110 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10558 _diffrn_reflns_av_R_equivalents 0.0781 _diffrn_reflns_av_sigmaI/netI 0.1023 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4744 _reflns_number_gt 2929 _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 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+0.9300P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4743 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1196 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.1920 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 1.0000 0.0000 0.0000 0.0339(3) Uani 1 2 d S . . Fe Fe 1.20067(9) 0.25791(8) -0.27210(8) 0.0402(3) Uani 1 1 d . . . S S 1.3688(2) -0.24856(19) 0.1458(2) 0.0633(6) Uani 1 1 d . . . P P 1.01659(16) 0.19890(14) 0.00211(14) 0.0350(4) Uani 1 1 d . . . N N 1.1495(6) -0.0875(5) 0.0570(5) 0.0454(14) Uani 1 1 d . . . O1 O 1.5033(5) 0.3809(5) -0.3856(5) 0.0618(14) Uani 1 1 d . . . O2 O 1.4098(6) 0.4067(6) -0.5286(5) 0.0644(15) Uani 1 1 d . . . C01 C 1.0565(6) 0.2992(6) -0.1351(6) 0.0426(16) Uani 1 1 d . . . C02 C 0.9970(7) 0.3186(7) -0.2283(7) 0.0563(19) Uani 1 1 d . . . H02 H 0.9367 0.2757 -0.2319 0.068 Uiso 1 1 calc R . . C03 C 1.0468(8) 0.4144(7) -0.3132(7) 0.063(2) Uani 1 1 d . . . H03 H 1.0241 0.4468 -0.3828 0.075 Uiso 1 1 calc R . . C04 C 1.1359(8) 0.4530(7) -0.2757(7) 0.059(2) Uani 1 1 d . . . H04 H 1.1834 0.5145 -0.3169 0.071 Uiso 1 1 calc R . . C05 C 1.1425(7) 0.3848(6) -0.1668(6) 0.0471(17) Uani 1 1 d . . . H05 H 1.1938 0.3935 -0.1226 0.057 Uiso 1 1 calc R . . C06 C 1.3810(7) 0.2341(6) -0.3769(6) 0.0467(17) Uani 1 1 d . . . C07 C 1.3952(7) 0.1552(6) -0.2693(6) 0.0472(17) Uani 1 1 d . . . H07 H 1.4479 0.1608 -0.2248 0.057 Uiso 1 1 calc R . . C08 C 1.3146(7) 0.0671(6) -0.2427(7) 0.0524(18) Uani 1 1 d . . . H08 H 1.3051 0.0042 -0.1771 0.063 Uiso 1 1 calc R . . C09 C 1.2508(8) 0.0898(6) -0.3315(7) 0.057(2) Uani 1 1 d . . . H09 H 1.1917 0.0451 -0.3344 0.069 Uiso 1 1 calc R . . C10 C 1.2918(8) 0.1924(7) -0.4157(7) 0.0532(18) Uani 1 1 d . . . H10 H 1.2654 0.2265 -0.4838 0.064 Uiso 1 1 calc R . . C11 C 1.4374(7) 0.3479(7) -0.4323(6) 0.0490(18) Uani 1 1 d . . . C12 C 1.1357(7) 0.2079(6) 0.0753(6) 0.0406(15) Uani 1 1 d . . . C13 C 1.0990(8) 0.2811(7) 0.1565(7) 0.0539(19) Uani 1 1 d . . . H13 H 1.0101 0.3280 0.1754 0.065 Uiso 1 1 calc R . . C14 C 1.1940(9) 0.2854(8) 0.2100(8) 0.074(3) Uani 1 1 d . . . H14 H 1.1684 0.3342 0.2649 0.089 Uiso 1 1 calc R . . C15 C 1.3249(9) 0.2175(8) 0.1816(8) 0.073(3) Uani 1 1 d . . . H15 H 1.3877 0.2190 0.2186 0.087 Uiso 1 1 calc R . . C16 C 1.3654(7) 0.1466(7) 0.0987(8) 0.062(2) Uani 1 1 d . . . H16 H 1.4550 0.1022 0.0790 0.075 Uiso 1 1 calc R . . C17 C 1.2715(7) 0.1424(6) 0.0453(6) 0.0472(17) Uani 1 1 d . . . H17 H 1.2985 0.0956 -0.0111 0.057 Uiso 1 1 calc R . . C18 C 0.8537(6) 0.2898(6) 0.0679(6) 0.0405(15) Uani 1 1 d . . . C19 C 0.7838(7) 0.4076(6) 0.0117(6) 0.0483(17) Uani 1 1 d . . . H19 H 0.8217 0.4449 -0.0603 0.058 Uiso 1 1 calc R . . C20 C 0.6549(7) 0.4699(7) 0.0649(8) 0.061(2) Uani 1 1 d . . . H20 H 0.6074 0.5489 0.0281 0.073 Uiso 1 1 calc R . . C21 C 0.5994(8) 0.4146(7) 0.1704(8) 0.061(2) Uani 1 1 d . . . H21 H 0.5146 0.4567 0.2053 0.073 Uiso 1 1 calc R . . C22 C 0.6677(9) 0.2975(8) 0.2253(8) 0.075(3) Uani 1 1 d . . . H22 H 0.6287 0.2597 0.2966 0.090 Uiso 1 1 calc R . . C23 C 0.7943(8) 0.2361(7) 0.1745(7) 0.060(2) Uani 1 1 d . . . H23 H 0.8406 0.1571 0.2126 0.072 Uiso 1 1 calc R . . C24 C 1.2432(7) -0.1555(6) 0.0935(6) 0.0443(16) Uani 1 1 d . . . H99 H 1.429(15) 0.478(14) -0.559(14) 0.19(6) Uiso 1 1 d . . . C25 C 0.8042(10) 0.1563(9) 0.5902(8) 0.080(3) Uani 1 1 d . . . H25 H 0.7331 0.2004 0.6447 0.096 Uiso 1 1 calc R . . Cl1 Cl 0.9065(3) 0.0257(3) 0.6615(3) 0.1172(11) Uani 1 1 d . . . Cl2 Cl 0.8936(6) 0.2636(4) 0.5091(5) 0.217(3) Uani 1 1 d . . . Cl3 Cl 0.7301(4) 0.0996(6) 0.5159(5) 0.213(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0341(6) 0.0282(5) 0.0388(7) -0.0055(5) -0.0109(5) -0.0055(4) Fe 0.0410(6) 0.0379(5) 0.0408(6) -0.0039(4) -0.0043(4) -0.0166(4) S 0.0469(11) 0.0584(11) 0.0826(16) -0.0138(10) -0.0316(11) 0.0040(9) P 0.0346(9) 0.0287(8) 0.0401(10) -0.0056(6) -0.0078(7) -0.0076(6) N 0.046(3) 0.033(3) 0.062(4) -0.012(3) -0.018(3) -0.008(2) O1 0.064(3) 0.065(3) 0.063(4) 0.006(3) -0.022(3) -0.035(3) O2 0.074(4) 0.071(4) 0.052(4) 0.005(3) -0.014(3) -0.038(3) C01 0.039(4) 0.035(3) 0.046(4) -0.002(3) -0.007(3) -0.006(3) C02 0.046(4) 0.063(4) 0.052(5) -0.003(4) -0.014(4) -0.007(3) C03 0.056(5) 0.054(4) 0.049(5) 0.009(4) -0.006(4) 0.002(4) C04 0.066(5) 0.042(4) 0.059(6) -0.003(4) -0.006(4) -0.011(4) C05 0.055(4) 0.039(3) 0.044(4) -0.008(3) -0.002(3) -0.015(3) C06 0.040(4) 0.043(4) 0.049(5) -0.004(3) -0.002(3) -0.011(3) C07 0.045(4) 0.043(4) 0.050(5) -0.006(3) -0.009(3) -0.010(3) C08 0.057(5) 0.041(4) 0.054(5) -0.007(3) -0.003(4) -0.015(3) C09 0.068(5) 0.042(4) 0.063(5) -0.011(3) -0.006(4) -0.023(4) C10 0.061(5) 0.057(4) 0.044(5) -0.009(3) -0.009(4) -0.021(4) C11 0.043(4) 0.053(4) 0.042(5) -0.002(3) -0.002(3) -0.014(3) C12 0.043(4) 0.036(3) 0.048(4) -0.004(3) -0.018(3) -0.014(3) C13 0.060(5) 0.048(4) 0.057(5) -0.014(3) -0.020(4) -0.007(3) C14 0.084(7) 0.068(5) 0.089(7) -0.028(5) -0.037(6) -0.019(5) C15 0.076(6) 0.068(5) 0.095(8) -0.015(5) -0.039(6) -0.030(5) C16 0.039(4) 0.065(5) 0.085(7) -0.004(4) -0.025(4) -0.015(4) C17 0.043(4) 0.046(4) 0.056(5) -0.010(3) -0.011(3) -0.015(3) C18 0.043(4) 0.032(3) 0.046(4) -0.009(3) -0.010(3) -0.008(3) C19 0.047(4) 0.044(4) 0.046(5) -0.006(3) -0.010(3) -0.005(3) C20 0.044(4) 0.048(4) 0.081(7) -0.012(4) -0.019(4) 0.007(3) C21 0.045(4) 0.057(5) 0.075(6) -0.017(4) -0.004(4) -0.009(4) C22 0.065(6) 0.070(5) 0.063(6) -0.007(4) 0.018(4) -0.015(4) C23 0.050(5) 0.043(4) 0.065(6) 0.000(4) 0.005(4) -0.009(3) C24 0.049(4) 0.036(3) 0.048(4) -0.012(3) -0.013(3) -0.006(3) C25 0.084(7) 0.089(6) 0.064(6) -0.029(5) -0.021(5) -0.001(5) Cl1 0.125(3) 0.0918(19) 0.105(2) 0.0027(16) -0.027(2) -0.0045(17) Cl2 0.297(7) 0.111(3) 0.168(4) 0.032(3) 0.029(4) -0.070(4) Cl3 0.106(3) 0.346(7) 0.238(6) -0.226(6) -0.078(3) 0.052(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 Ni N 1.819(5) . ? Ni N 1.820(5) 2_755 ? Ni P 2.2627(15) . ? Ni P 2.2627(15) 2_755 ? Fe C06 2.009(7) . ? Fe C04 2.032(7) . ? Fe C10 2.032(8) . ? Fe C02 2.035(7) . ? Fe C01 2.038(7) . ? Fe C03 2.038(7) . ? Fe C07 2.040(7) . ? Fe C05 2.045(7) . ? Fe C09 2.055(7) . ? Fe C08 2.062(7) . ? S C24 1.599(7) . ? P C01 1.809(7) . ? P C12 1.819(6) . ? P C18 1.819(6) . ? N C24 1.174(8) . ? O1 C11 1.228(9) . ? O2 C11 1.286(9) . ? O2 H99 0.84(15) . ? C01 C05 1.426(9) . ? C01 C02 1.436(10) . ? C02 C03 1.404(11) . ? C02 H02 0.9300 . ? C03 C04 1.395(11) . ? C03 H03 0.9300 . ? C04 C05 1.394(10) . ? C04 H04 0.9300 . ? C05 H05 0.9300 . ? C06 C07 1.426(10) . ? C06 C10 1.428(10) . ? C06 C11 1.478(9) . ? C07 C08 1.410(10) . ? C07 H07 0.9300 . ? C08 C09 1.407(11) . ? C08 H08 0.9300 . ? C09 C10 1.414(10) . ? C09 H09 0.9300 . ? C10 H10 0.9300 . ? C12 C13 1.384(9) . ? C12 C17 1.403(9) . ? C13 C14 1.393(10) . ? C13 H13 0.9300 . ? C14 C15 1.367(12) . ? C14 H14 0.9300 . ? C15 C16 1.381(12) . ? C15 H15 0.9300 . ? C16 C17 1.382(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.385(10) . ? C18 C19 1.388(8) . ? C19 C20 1.408(10) . ? C19 H19 0.9300 . ? C20 C21 1.366(11) . ? C20 H20 0.9300 . ? C21 C22 1.369(11) . ? C21 H21 0.9300 . ? C22 C23 1.377(10) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C25 Cl2 1.694(11) . ? C25 Cl1 1.712(9) . ? C25 Cl3 1.727(10) . ? C25 H25 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N Ni N 180.0 . 2_755 ? N Ni P 93.75(16) . . ? N Ni P 86.25(16) 2_755 . ? N Ni P 86.25(16) . 2_755 ? N Ni P 93.75(16) 2_755 2_755 ? P Ni P 180.0 . 2_755 ? C06 Fe C04 104.7(3) . . ? C06 Fe C10 41.4(3) . . ? C04 Fe C10 120.1(3) . . ? C06 Fe C02 156.1(3) . . ? C04 Fe C02 68.0(3) . . ? C10 Fe C02 121.0(3) . . ? C06 Fe C01 159.2(3) . . ? C04 Fe C01 68.1(3) . . ? C10 Fe C01 159.2(3) . . ? C02 Fe C01 41.3(3) . . ? C06 Fe C03 119.7(3) . . ? C04 Fe C03 40.1(3) . . ? C10 Fe C03 105.0(3) . . ? C02 Fe C03 40.3(3) . . ? C01 Fe C03 68.2(3) . . ? C06 Fe C07 41.2(3) . . ? C04 Fe C07 122.4(3) . . ? C10 Fe C07 69.0(3) . . ? C02 Fe C07 161.7(3) . . ? C01 Fe C07 124.9(3) . . ? C03 Fe C07 156.9(3) . . ? C06 Fe C05 121.3(3) . . ? C04 Fe C05 40.0(3) . . ? C10 Fe C05 156.5(3) . . ? C02 Fe C05 68.7(3) . . ? C01 Fe C05 40.9(3) . . ? C03 Fe C05 67.6(3) . . ? C07 Fe C05 108.6(3) . . ? C06 Fe C09 68.7(3) . . ? C04 Fe C09 157.0(3) . . ? C10 Fe C09 40.5(3) . . ? C02 Fe C09 108.6(3) . . ? C01 Fe C09 125.4(3) . . ? C03 Fe C09 122.6(4) . . ? C07 Fe C09 68.1(3) . . ? C05 Fe C09 162.1(3) . . ? C06 Fe C08 68.3(3) . . ? C04 Fe C08 159.9(3) . . ? C10 Fe C08 67.9(3) . . ? C02 Fe C08 125.8(3) . . ? C01 Fe C08 111.4(3) . . ? C03 Fe C08 159.8(3) . . ? C07 Fe C08 40.2(3) . . ? C05 Fe C08 126.3(3) . . ? C09 Fe C08 40.0(3) . . ? C01 P C12 103.9(3) . . ? C01 P C18 105.2(3) . . ? C12 P C18 105.2(3) . . ? C01 P Ni 114.0(2) . . ? C12 P Ni 118.84(19) . . ? C18 P Ni 108.5(2) . . ? C24 N Ni 173.1(5) . . ? C11 O2 H99 119(10) . . ? C05 C01 C02 107.1(6) . . ? C05 C01 P 125.9(5) . . ? C02 C01 P 126.7(5) . . ? C05 C01 Fe 69.8(4) . . ? C02 C01 Fe 69.2(4) . . ? P C01 Fe 131.1(3) . . ? C03 C02 C01 107.2(7) . . ? C03 C02 Fe 70.0(4) . . ? C01 C02 Fe 69.5(4) . . ? C03 C02 H02 126.4 . . ? C01 C02 H02 126.4 . . ? Fe C02 H02 125.8 . . ? C04 C03 C02 108.7(7) . . ? C04 C03 Fe 69.7(4) . . ? C02 C03 Fe 69.7(4) . . ? C04 C03 H03 125.6 . . ? C02 C03 H03 125.6 . . ? Fe C03 H03 126.5 . . ? C05 C04 C03 109.1(7) . . ? C05 C04 Fe 70.5(4) . . ? C03 C04 Fe 70.2(4) . . ? C05 C04 H04 125.4 . . ? C03 C04 H04 125.4 . . ? Fe C04 H04 125.4 . . ? C04 C05 C01 107.8(7) . . ? C04 C05 Fe 69.5(4) . . ? C01 C05 Fe 69.3(4) . . ? C04 C05 H05 126.1 . . ? C01 C05 H05 126.1 . . ? Fe C05 H05 126.6 . . ? C07 C06 C10 107.9(6) . . ? C07 C06 C11 125.5(7) . . ? C10 C06 C11 126.3(7) . . ? C07 C06 Fe 70.6(4) . . ? C10 C06 Fe 70.2(4) . . ? C11 C06 Fe 119.9(5) . . ? C08 C07 C06 107.4(7) . . ? C08 C07 Fe 70.7(4) . . ? C06 C07 Fe 68.2(4) . . ? C08 C07 H07 126.3 . . ? C06 C07 H07 126.3 . . ? Fe C07 H07 126.3 . . ? C09 C08 C07 108.9(7) . . ? C09 C08 Fe 69.8(4) . . ? C07 C08 Fe 69.1(4) . . ? C09 C08 H08 125.6 . . ? C07 C08 H08 125.6 . . ? Fe C08 H08 127.2 . . ? C08 C09 C10 108.3(7) . . ? C08 C09 Fe 70.3(4) . . ? C10 C09 Fe 68.9(4) . . ? C08 C09 H09 125.9 . . ? C10 C09 H09 125.9 . . ? Fe C09 H09 126.6 . . ? C09 C10 C06 107.6(7) . . ? C09 C10 Fe 70.6(5) . . ? C06 C10 Fe 68.5(4) . . ? C09 C10 H10 126.2 . . ? C06 C10 H10 126.2 . . ? Fe C10 H10 126.2 . . ? O1 C11 O2 124.8(7) . . ? O1 C11 C06 120.1(7) . . ? O2 C11 C06 115.0(7) . . ? C13 C12 C17 118.5(6) . . ? C13 C12 P 122.7(5) . . ? C17 C12 P 118.7(5) . . ? C12 C13 C14 120.7(7) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 119.7(8) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 121.0(8) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C17 119.4(7) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C12 120.7(7) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C23 C18 C19 119.1(6) . . ? C23 C18 P 119.0(5) . . ? C19 C18 P 121.9(5) . . ? C18 C19 C20 119.2(7) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C21 C20 C19 120.3(7) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.5(7) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C23 119.9(8) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C22 C23 C18 121.1(7) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? N C24 S 178.8(7) . . ? Cl2 C25 Cl1 109.7(6) . . ? Cl2 C25 Cl3 113.4(6) . . ? Cl1 C25 Cl3 108.9(6) . . ? Cl2 C25 H25 108.3 . . ? Cl1 C25 H25 108.3 . . ? Cl3 C25 H25 108.3 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.594 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.101