# ic001372b.cif _publ_contact_author ; Professor Mark R. Mason Department of Chemistry University of Toledo Toledo, OH 43606, USA ; _publ_contact_author_email 'mmason5@uoft02.utoledo.edu' _publ_contact_author_fax '(419) 530-4033' _publ_contact_author_phone '(419) 530-1532' _publ_requested_journal 'Inorganic Chemistry' _publ_requested_coeditor_name 'Herbert D. Kaesz' _publ_contact_letter ; Please accept this CIF submission to be deposited as Supplementary Material for review in Inorganic Chemistry (manuscript number IC001372B). ; _publ_section_title ; Hindered Axial-Equatorial Carbonyl Exchange in an Fe(CO)4(PR3) Complex of a Rigid Bicyclic Phosphine ; loop_ _publ_author_name _publ_author_address ; 'Barnard, Thomas S.' Department of Chemistry University of Toledo Toledo, OH 43606, USA ; ; 'Mason, Mark R.' Department of Chemistry University of Toledo Toledo, OH 43606, USA ; data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; P(C4H3N)3CH ; _chemical_name_common phosphatri(pyrrolyl)methane _chemical_melting_point ? _chemical_formula_moiety 'C13 H10 N3 P' _chemical_formula_sum 'C13 H10 N3 P' _chemical_formula_weight 239.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.9347(5) _cell_length_b 7.9781(5) _cell_length_c 17.9210(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1134.47(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5647 _cell_measurement_theta_min 3.80 _cell_measurement_theta_max 28.90 _exptl_crystal_description 'block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.401 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.220 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.821463 _exptl_absorpt_correction_T_max 0.991528 _exptl_absorpt_process_details ? _exptl_special_details ; The decay correction was applied simultaneously with the absorption correction in sadabs. No formal measure of the extent of decay is printed out by this program. The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 \s(I). ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '100 frames' _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'before and after data collection' _diffrn_standards_decay_% ? _diffrn_reflns_number 8037 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 29.60 _reflns_number_total 2957 _reflns_number_gt 2753 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL and the Toledo cifomatic' _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^)+(0.0499P)^2^+0.1132P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.92(8) _refine_ls_number_reflns 2957 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 P1 P 0.35284(5) 0.30714(5) 0.03935(2) 0.03920(11) Uani 1.000000 1 d . N1 N 0.20891(16) 0.20984(17) 0.09832(7) 0.0414(3) Uani 1.000000 1 d . N2 N 0.43984(16) 0.42806(17) 0.10939(8) 0.0418(3) Uani 1.000000 1 d . N3 N 0.21308(16) 0.46044(17) 0.01115(7) 0.0400(3) Uani 1.000000 1 d . C1 C 0.1484(2) 0.49327(19) 0.14391(8) 0.0406(3) Uani 1.000000 1 d . C10 C 0.11234(18) 0.3055(2) 0.14651(8) 0.0395(3) Uani 1.000000 1 d . C11 C 0.0025(2) 0.2030(2) 0.18261(9) 0.0462(4) Uani 1.000000 1 d . C12 C 0.0324(2) 0.0378(2) 0.15632(11) 0.0529(4) Uani 1.000000 1 d . C13 C 0.1581(2) 0.0439(2) 0.10431(11) 0.0484(4) Uani 1.000000 1 d . C20 C 0.3359(2) 0.51215(19) 0.15942(8) 0.0419(3) Uani 1.000000 1 d . C21 C 0.4351(3) 0.5846(3) 0.21253(10) 0.0544(4) Uani 1.000000 1 d . C22 C 0.6056(2) 0.5447(3) 0.19461(12) 0.0585(5) Uani 1.000000 1 d . C23 C 0.6060(2) 0.4474(2) 0.13221(11) 0.0489(4) Uani 1.000000 1 d . C30 C 0.11730(18) 0.54537(18) 0.06375(9) 0.0395(3) Uani 1.000000 1 d . C31 C 0.0108(2) 0.6514(2) 0.02695(12) 0.0499(4) Uani 1.000000 1 d . C32 C 0.0427(2) 0.6316(2) -0.05088(12) 0.0552(4) Uani 1.000000 1 d . C33 C 0.1650(2) 0.5132(2) -0.05934(10) 0.0478(4) Uani 1.000000 1 d . H1 H 0.082(2) 0.557(2) 0.1759(10) 0.041(5) Uiso 1.000000 1 d . H11 H -0.081(3) 0.245(3) 0.2177(11) 0.056(6) Uiso 1.000000 1 d . H12 H -0.023(3) -0.055(3) 0.1717(12) 0.062(6) Uiso 1.000000 1 d . H13 H 0.204(3) -0.044(3) 0.0744(13) 0.075(7) Uiso 1.000000 1 d . H21 H 0.385(3) 0.657(3) 0.2531(12) 0.068(6) Uiso 1.000000 1 d . H22 H 0.700(3) 0.580(3) 0.2220(13) 0.066(6) Uiso 1.000000 1 d . H23 H 0.700(3) 0.403(3) 0.1023(15) 0.083(8) Uiso 1.000000 1 d . H31 H -0.068(3) 0.719(3) 0.0476(12) 0.068(6) Uiso 1.000000 1 d . H32 H -0.006(3) 0.682(3) -0.0931(12) 0.062(6) Uiso 1.000000 1 d . H33 H 0.215(3) 0.469(3) -0.0994(12) 0.051(5) Uiso 1.000000 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 P1 0.03217(17) 0.04086(18) 0.04457(19) -0.00627(16) 0.00366(15) 0.00190(14) N1 0.0377(6) 0.0367(6) 0.0497(7) -0.0014(5) 0.0039(5) -0.0012(5) N2 0.0323(6) 0.0455(7) 0.0475(7) -0.0051(6) -0.0022(5) -0.0019(5) N3 0.0357(6) 0.0463(7) 0.0379(6) 0.0001(5) 0.0007(5) 0.0032(5) C1 0.0377(7) 0.0445(8) 0.0396(7) -0.0080(6) 0.0041(6) -0.0003(6) C10 0.0353(7) 0.0453(7) 0.0379(6) 0.0000(6) 0.0014(5) -0.0007(6) C11 0.0381(7) 0.0589(10) 0.0414(7) 0.0083(8) -0.0017(6) -0.0042(8) C12 0.0454(9) 0.0505(9) 0.0627(10) 0.0173(8) -0.0120(8) -0.0097(7) C13 0.0420(8) 0.0371(7) 0.0661(10) 0.0030(7) -0.0094(7) -0.0020(6) C20 0.0429(8) 0.0415(7) 0.0412(7) -0.0048(6) 0.0007(6) -0.0036(6) C21 0.0608(11) 0.0576(11) 0.0447(9) -0.0055(8) -0.0081(8) -0.0083(9) C22 0.0511(10) 0.0639(11) 0.0604(10) 0.0037(9) -0.0210(8) -0.0108(9) C23 0.0367(8) 0.0493(9) 0.0607(10) 0.0073(8) -0.0098(7) -0.0038(7) C30 0.0337(7) 0.0361(7) 0.0486(8) -0.0042(6) 0.0029(6) 0.0002(6) C31 0.0391(8) 0.0348(7) 0.0757(12) 0.0020(8) -0.0032(8) 0.0010(6) C32 0.0468(9) 0.0522(9) 0.0665(11) 0.0207(8) -0.0108(8) -0.0091(7) C33 0.0423(8) 0.0589(10) 0.0423(8) 0.0088(7) -0.0011(6) -0.0130(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 N1 1.7388(14) . ? P1 N2 1.7270(14) . ? P1 N3 1.7266(13) . ? N1 C10 1.3839(19) . ? N1 C13 1.388(2) . ? N2 C20 1.391(2) . ? N2 C23 1.389(2) . ? N3 C30 1.388(2) . ? N3 C33 1.385(2) . ? C1 C20 1.521(2) . ? C1 C30 1.516(2) . ? C10 C1 1.526(2) . ? C10 C11 1.359(2) . ? C11 C12 1.420(3) . ? C12 C13 1.366(3) . ? C20 C21 1.364(2) . ? C21 C22 1.426(3) . ? C22 C23 1.361(3) . ? C30 C31 1.365(2) . ? C31 C32 1.426(3) . ? C32 C33 1.363(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 P1 N2 94.03(6) . . ? N1 P1 N3 94.14(6) . . ? N2 P1 N3 94.23(7) . . ? P1 N1 C10 119.79(11) . . ? P1 N1 C13 131.57(12) . . ? C10 N1 C13 108.47(14) . . ? P1 N2 C20 120.06(11) . . ? P1 N2 C23 130.96(13) . . ? C20 N2 C23 108.62(14) . . ? P1 N3 C30 119.93(11) . . ? P1 N3 C33 131.23(12) . . ? C30 N3 C33 108.68(14) . . ? C10 C1 C20 105.95(12) . . ? C10 C1 C30 105.53(12) . . ? C20 C1 C30 107.76(13) . . ? N1 C10 C1 114.74(13) . . ? N1 C10 C11 108.69(15) . . ? C11 C10 C1 136.50(15) . . ? C10 C11 C12 107.06(15) . . ? C11 C12 C13 108.37(16) . . ? N1 C13 C12 107.40(16) . . ? N2 C20 C1 114.49(12) . . ? N2 C20 C21 108.20(16) . . ? C1 C20 C21 137.22(16) . . ? C20 C21 C22 107.19(17) . . ? C21 C22 C23 108.34(15) . . ? N2 C23 C22 107.63(16) . . ? N3 C30 C1 114.89(13) . . ? N3 C30 C31 108.26(15) . . ? C1 C30 C31 136.75(15) . . ? C30 C31 C32 107.09(16) . . ? C31 C32 C33 108.18(16) . . ? N3 C33 C32 107.78(17) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 29.60 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.169 _refine_diff_density_min -0.133 _refine_diff_density_rms 0.034 #===END data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Fe(CO)4[P(C9H7N)3CH] 0.5 CH2Cl2 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32.50 H23 Cl Fe N3 O4 P' _chemical_formula_sum 'C32.50 H23 Cl Fe N3 O4 P' _chemical_formula_weight 641.81 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' '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 10.4807(16) _cell_length_b 11.3083(14) _cell_length_c 14.506(2) _cell_angle_alpha 82.139(5) _cell_angle_beta 72.167(5) _cell_angle_gamma 62.857(4) _cell_volume 1456.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5465 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 30.09 _exptl_crystal_description 'chunk' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 658 _exptl_absorpt_coefficient_mu 0.708 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.831078 _exptl_absorpt_correction_T_max 0.991675 _exptl_absorpt_process_details ? _exptl_special_details ; The decay correction was applied simultaneously with the absorption correction in sadabs. No formal measure of the extent of decay is printed out by this program. The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 \s(I). ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD Diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '100 frames' _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'before and after data collection' _diffrn_standards_decay_% ? _diffrn_reflns_number 15824 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 29.82 _reflns_number_total 7470 _reflns_number_gt 6686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL and the Toledo cifomatic' _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^)+(0.0471P)^2^+1.2716P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 7470 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1020 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.77589(3) 0.32406(2) 0.330278(17) 0.02288(7) Uani 1.000000 1 d . Cl1 Cl 0.5799(3) 0.5469(2) 0.04188(13) 0.1697(8) Uani 1.000000 1 d . P1 P 0.67598(4) 0.24483(4) 0.26140(3) 0.01998(9) Uani 1.000000 1 d . O1 O 0.8971(2) 0.4345(2) 0.43607(13) 0.0529(4) Uani 1.000000 1 d . O2 O 0.52640(16) 0.35481(14) 0.50340(10) 0.0359(3) Uani 1.000000 1 d . O3 O 0.7607(2) 0.54196(16) 0.19024(13) 0.0498(4) Uani 1.000000 1 d . O4 O 1.05238(17) 0.07427(16) 0.28700(12) 0.0446(4) Uani 1.000000 1 d . N1 N 0.75256(16) 0.19399(15) 0.14349(10) 0.0247(3) Uani 1.000000 1 d . N2 N 0.65865(17) 0.10426(14) 0.30895(10) 0.0246(3) Uani 1.000000 1 d . N3 N 0.49543(16) 0.33820(14) 0.25733(11) 0.0241(3) Uani 1.000000 1 d . C1 C 0.8510(2) 0.3906(2) 0.39616(14) 0.0342(4) Uani 1.000000 1 d . C2 C 0.6238(2) 0.34341(17) 0.43609(13) 0.0268(3) Uani 1.000000 1 d . C3 C 0.7640(2) 0.45667(19) 0.24329(14) 0.0314(4) Uani 1.000000 1 d . C4 C 0.9445(2) 0.17138(19) 0.30368(13) 0.0304(4) Uani 1.000000 1 d . C10 C 0.5412(2) 0.13803(18) 0.17837(13) 0.0266(3) Uani 1.000000 1 d . C11 C 0.6753(2) 0.14600(17) 0.10532(12) 0.0261(3) Uani 1.000000 1 d . C12 C 0.7366(2) 0.12361(18) 0.00884(13) 0.0296(4) Uani 1.000000 1 d . C13 C 0.8600(2) 0.15802(18) -0.01823(12) 0.0298(4) Uani 1.000000 1 d . C14 C 0.9622(2) 0.1565(2) -0.10751(14) 0.0387(5) Uani 1.000000 1 d . C15 C 1.0666(2) 0.2005(2) -0.11233(15) 0.0428(5) Uani 1.000000 1 d . C16 C 1.0729(2) 0.2452(2) -0.02938(16) 0.0397(5) Uani 1.000000 1 d . C17 C 0.9746(2) 0.2460(2) 0.06081(14) 0.0317(4) Uani 1.000000 1 d . C18 C 0.86780(19) 0.20328(17) 0.06532(12) 0.0257(3) Uani 1.000000 1 d . C19 C 0.6858(3) 0.0764(3) -0.05844(16) 0.0423(5) Uani 1.000000 1 d . C21 C 0.5909(2) 0.05551(17) 0.26272(12) 0.0256(3) Uani 1.000000 1 d . C22 C 0.5852(2) -0.05697(17) 0.30576(13) 0.0277(3) Uani 1.000000 1 d . C23 C 0.65321(19) -0.08452(17) 0.38378(13) 0.0284(4) Uani 1.000000 1 d . C24 C 0.6792(2) -0.1876(2) 0.45186(16) 0.0383(4) Uani 1.000000 1 d . C25 C 0.7447(2) -0.1879(2) 0.52125(16) 0.0424(5) Uani 1.000000 1 d . C26 C 0.7851(2) -0.0868(2) 0.52324(15) 0.0388(5) Uani 1.000000 1 d . C27 C 0.7630(2) 0.01635(19) 0.45610(13) 0.0306(4) Uani 1.000000 1 d . C28 C 0.69731(18) 0.01600(17) 0.38574(12) 0.0247(3) Uani 1.000000 1 d . C29 C 0.5201(3) -0.1364(2) 0.27925(19) 0.0407(5) Uani 1.000000 1 d . C31 C 0.4344(2) 0.27694(18) 0.21581(12) 0.0259(3) Uani 1.000000 1 d . C32 C 0.2903(2) 0.35877(19) 0.21951(13) 0.0288(4) Uani 1.000000 1 d . C33 C 0.25354(19) 0.47982(19) 0.26609(13) 0.0282(3) Uani 1.000000 1 d . C34 C 0.1216(2) 0.5978(2) 0.28947(15) 0.0360(4) Uani 1.000000 1 d . C35 C 0.1209(2) 0.7009(2) 0.33112(15) 0.0375(4) Uani 1.000000 1 d . C36 C 0.2502(2) 0.68848(19) 0.34903(14) 0.0339(4) Uani 1.000000 1 d . C37 C 0.3826(2) 0.57133(18) 0.32800(13) 0.0289(3) Uani 1.000000 1 d . C38 C 0.38229(18) 0.46672(17) 0.28771(12) 0.0241(3) Uani 1.000000 1 d . C39 C 0.1888(3) 0.3337(3) 0.17977(19) 0.0434(5) Uani 1.000000 1 d . C40 C 0.4465(14) 0.5284(6) 0.0261(10) 0.194(8) Uani 0.500000 1 d P H10 H 0.496(2) 0.102(2) 0.1504(16) 0.028(5) Uiso 1.000000 1 d . H11 H 0.599(4) 0.061(4) -0.024(3) 0.085(11) Uiso 1.000000 1 d . H12 H 0.760(4) -0.008(4) -0.090(2) 0.076(10) Uiso 1.000000 1 d . H13 H 0.666(3) 0.138(3) -0.112(2) 0.064(9) Uiso 1.000000 1 d . H14 H 0.958(3) 0.128(3) -0.163(2) 0.052(8) Uiso 1.000000 1 d . H15 H 1.136(3) 0.199(3) -0.1731(19) 0.045(7) Uiso 1.000000 1 d . H16 H 1.146(3) 0.274(2) -0.0341(18) 0.041(6) Uiso 1.000000 1 d . H17 H 0.979(3) 0.275(3) 0.1174(19) 0.043(7) Uiso 1.000000 1 d . H21 H 0.588(4) -0.215(4) 0.254(3) 0.090(12) Uiso 1.000000 1 d . H22 H 0.458(4) -0.159(4) 0.335(3) 0.091(12) Uiso 1.000000 1 d . H23 H 0.457(5) -0.090(5) 0.238(3) 0.117(15) Uiso 1.000000 1 d . H24 H 0.649(3) -0.255(3) 0.4477(19) 0.044(7) Uiso 1.000000 1 d . H25 H 0.760(3) -0.257(3) 0.569(2) 0.048(7) Uiso 1.000000 1 d . H26 H 0.834(3) -0.087(3) 0.570(2) 0.051(7) Uiso 1.000000 1 d . H27 H 0.792(3) 0.085(2) 0.4573(17) 0.037(6) Uiso 1.000000 1 d . H31 H 0.099(4) 0.339(3) 0.230(2) 0.067(9) Uiso 1.000000 1 d . H32 H 0.158(4) 0.399(3) 0.133(3) 0.072(10) Uiso 1.000000 1 d . H33 H 0.240(4) 0.251(4) 0.150(3) 0.087(12) Uiso 1.000000 1 d . H34 H 0.034(3) 0.604(3) 0.2766(18) 0.044(7) Uiso 1.000000 1 d . H35 H 0.036(3) 0.777(3) 0.3503(19) 0.044(7) Uiso 1.000000 1 d . H36 H 0.249(3) 0.762(2) 0.3757(17) 0.037(6) Uiso 1.000000 1 d . H37 H 0.472(3) 0.563(2) 0.3399(18) 0.039(6) Uiso 1.000000 1 d . H40A H 0.4050 0.5001 0.0897 0.233 Uiso 0.500000 1 caPR PR H40B H 0.3747 0.6194 0.0204 0.233 Uiso 0.500000 1 caPR PR loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02194(12) 0.02573(13) 0.02435(12) -0.00377(9) -0.00734(9) -0.01166(10) Cl1 0.1703(16) 0.232(2) 0.1151(11) 0.0396(13) -0.1012(12) -0.0671(15) P1 0.02079(19) 0.02109(19) 0.01998(18) -0.00159(14) -0.00653(14) -0.00979(15) O1 0.0661(11) 0.0726(12) 0.0492(9) -0.0047(8) -0.0220(8) -0.0498(10) O2 0.0388(7) 0.0405(8) 0.0321(7) -0.0100(6) -0.0007(6) -0.0235(6) O3 0.0594(10) 0.0361(8) 0.0510(9) 0.0076(7) -0.0106(8) -0.0236(8) O4 0.0318(7) 0.0424(8) 0.0501(9) -0.0089(7) -0.0136(7) -0.0045(6) N1 0.0277(7) 0.0302(7) 0.0198(6) -0.0028(5) -0.0055(5) -0.0156(6) N2 0.0305(7) 0.0241(7) 0.0240(6) 0.0014(5) -0.0104(6) -0.0146(6) N3 0.0225(7) 0.0236(7) 0.0296(7) -0.0025(5) -0.0112(5) -0.0099(5) C1 0.0356(10) 0.0416(10) 0.0326(9) -0.0027(8) -0.0085(8) -0.0227(8) C2 0.0299(9) 0.0275(8) 0.0278(8) -0.0057(6) -0.0091(7) -0.0143(7) C3 0.0301(9) 0.0300(9) 0.0351(9) -0.0038(7) -0.0079(7) -0.0136(7) C4 0.0272(9) 0.0359(9) 0.0304(9) -0.0035(7) -0.0099(7) -0.0137(7) C10 0.0322(9) 0.0295(8) 0.0267(8) -0.0016(6) -0.0111(7) -0.0183(7) C11 0.0327(9) 0.0265(8) 0.0247(8) -0.0010(6) -0.0110(7) -0.0154(7) C12 0.0376(10) 0.0274(8) 0.0240(8) -0.0008(6) -0.0127(7) -0.0116(7) C13 0.0326(9) 0.0287(8) 0.0217(8) 0.0004(6) -0.0075(7) -0.0082(7) C14 0.0410(11) 0.0402(11) 0.0217(8) 0.0000(7) -0.0056(8) -0.0088(9) C15 0.0344(10) 0.0494(12) 0.0266(9) 0.0054(8) 0.0006(8) -0.0105(9) C16 0.0275(9) 0.0472(12) 0.0371(10) 0.0062(9) -0.0026(8) -0.0159(9) C17 0.0268(9) 0.0366(10) 0.0294(9) 0.0008(7) -0.0052(7) -0.0139(8) C18 0.0254(8) 0.0249(8) 0.0217(7) 0.0012(6) -0.0050(6) -0.0081(6) C19 0.0556(14) 0.0467(12) 0.0303(10) -0.0063(9) -0.0191(9) -0.0210(11) C21 0.0283(8) 0.0251(8) 0.0264(8) -0.0034(6) -0.0062(6) -0.0142(7) C22 0.0258(8) 0.0237(8) 0.0308(8) -0.0033(6) -0.0006(6) -0.0122(7) C23 0.0238(8) 0.0239(8) 0.0294(8) 0.0001(6) 0.0008(6) -0.0088(6) C24 0.0322(10) 0.0310(9) 0.0429(11) 0.0086(8) -0.0023(8) -0.0138(8) C25 0.0361(11) 0.0383(11) 0.0388(11) 0.0155(9) -0.0070(8) -0.0109(9) C26 0.0336(10) 0.0419(11) 0.0282(9) 0.0066(8) -0.0097(8) -0.0071(8) C27 0.0289(9) 0.0312(9) 0.0251(8) -0.0004(7) -0.0072(7) -0.0078(7) C28 0.0220(7) 0.0235(7) 0.0221(7) -0.0002(6) -0.0026(6) -0.0065(6) C29 0.0418(12) 0.0344(10) 0.0527(13) -0.0047(9) -0.0073(10) -0.0246(9) C31 0.0284(8) 0.0300(8) 0.0268(8) 0.0006(6) -0.0111(6) -0.0170(7) C32 0.0273(8) 0.0359(9) 0.0298(8) 0.0049(7) -0.0120(7) -0.0180(7) C33 0.0240(8) 0.0322(9) 0.0283(8) 0.0052(7) -0.0094(6) -0.0124(7) C34 0.0241(9) 0.0401(10) 0.0389(10) 0.0055(8) -0.0116(8) -0.0096(8) C35 0.0288(9) 0.0318(9) 0.0374(10) 0.0014(8) -0.0071(8) -0.0030(8) C36 0.0337(10) 0.0269(9) 0.0340(9) -0.0022(7) -0.0076(8) -0.0080(7) C37 0.0264(8) 0.0269(8) 0.0312(9) -0.0021(7) -0.0080(7) -0.0092(7) C38 0.0220(7) 0.0241(8) 0.0241(7) 0.0017(6) -0.0062(6) -0.0090(6) C39 0.0341(11) 0.0567(14) 0.0528(13) -0.0004(11) -0.0203(10) -0.0259(10) C40 0.151(8) 0.023(2) 0.183(9) 0.043(4) 0.136(7) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 P1 2.1539(5) . ? Fe1 C1 1.8151(19) . ? Fe1 C2 1.7943(18) . ? Fe1 C3 1.807(2) . ? Fe1 C4 1.7983(19) . ? Cl1 C40 1.54(2) 2_665 ? Cl1 C40 1.59(2) . ? P1 N1 1.7051(14) . ? P1 N2 1.7095(15) . ? P1 N3 1.7110(15) . ? O1 C1 1.133(2) . ? O2 C2 1.147(2) . ? O3 C3 1.143(3) . ? O4 C4 1.147(2) . ? N1 C11 1.419(2) . ? N1 C18 1.414(2) . ? N2 C21 1.417(2) . ? N2 C28 1.416(2) . ? N3 C31 1.416(2) . ? N3 C38 1.413(2) . ? C10 C11 1.512(2) . ? C10 C21 1.508(2) . ? C10 C31 1.507(3) . ? C11 C12 1.354(2) . ? C12 C13 1.444(3) . ? C12 C19 1.498(3) . ? C13 C14 1.401(3) . ? C13 C18 1.416(2) . ? C14 C15 1.376(3) . ? C15 C16 1.397(3) . ? C16 C17 1.394(3) . ? C17 C18 1.389(3) . ? C21 C22 1.357(2) . ? C22 C23 1.443(3) . ? C22 C29 1.495(3) . ? C23 C24 1.403(3) . ? C23 C28 1.415(2) . ? C24 C25 1.380(3) . ? C25 C26 1.395(3) . ? C26 C27 1.394(3) . ? C27 C28 1.396(3) . ? C31 C32 1.352(3) . ? C32 C33 1.446(3) . ? C32 C39 1.496(3) . ? C33 C34 1.400(3) . ? C33 C38 1.416(2) . ? C34 C35 1.381(3) . ? C35 C36 1.398(3) . ? C36 C37 1.395(3) . ? C37 C38 1.391(2) . ? C40 Cl1 1.54(2) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Fe1 C1 176.06(6) . . ? P1 Fe1 C2 86.09(6) . . ? P1 Fe1 C3 93.31(6) . . ? P1 Fe1 C4 89.26(6) . . ? C1 Fe1 C2 90.02(8) . . ? C1 Fe1 C3 89.22(9) . . ? C1 Fe1 C4 92.30(9) . . ? C2 Fe1 C3 121.18(8) . . ? C2 Fe1 C4 122.00(9) . . ? C3 Fe1 C4 116.79(9) . . ? C40 Cl1 C40 40.9(4) 2_665 . ? Fe1 P1 N1 121.55(5) . . ? Fe1 P1 N2 117.95(5) . . ? Fe1 P1 N3 119.67(5) . . ? N1 P1 N2 97.17(7) . . ? N1 P1 N3 98.03(7) . . ? N2 P1 N3 97.36(7) . . ? P1 N1 C11 116.55(12) . . ? P1 N1 C18 135.62(12) . . ? C11 N1 C18 107.16(14) . . ? P1 N2 C21 116.59(11) . . ? P1 N2 C28 136.57(12) . . ? C21 N2 C28 106.83(14) . . ? P1 N3 C31 116.57(12) . . ? P1 N3 C38 136.21(12) . . ? C31 N3 C38 107.21(13) . . ? Fe1 C1 O1 178.5(2) . . ? Fe1 C2 O2 179.32(15) . . ? Fe1 C3 O3 176.61(19) . . ? Fe1 C4 O4 179.63(18) . . ? C11 C10 C21 108.35(15) . . ? C11 C10 C31 107.09(14) . . ? C21 C10 C31 107.25(14) . . ? N1 C11 C10 114.38(14) . . ? N1 C11 C12 110.97(16) . . ? C10 C11 C12 134.56(16) . . ? C11 C12 C13 106.47(16) . . ? C11 C12 C19 127.55(19) . . ? C13 C12 C19 125.96(18) . . ? C12 C13 C14 132.11(18) . . ? C12 C13 C18 108.61(15) . . ? C14 C13 C18 119.27(19) . . ? C13 C14 C15 119.3(2) . . ? C14 C15 C16 120.85(19) . . ? C15 C16 C17 121.3(2) . . ? C16 C17 C18 117.76(19) . . ? N1 C18 C13 106.77(15) . . ? N1 C18 C17 131.74(16) . . ? C13 C18 C17 121.49(17) . . ? N2 C21 C10 114.45(14) . . ? N2 C21 C22 111.28(16) . . ? C10 C21 C22 134.27(16) . . ? C21 C22 C23 106.25(15) . . ? C21 C22 C29 127.33(19) . . ? C23 C22 C29 126.42(18) . . ? C22 C23 C24 131.61(18) . . ? C22 C23 C28 108.64(15) . . ? C24 C23 C28 119.75(19) . . ? C23 C24 C25 119.4(2) . . ? C24 C25 C26 120.18(19) . . ? C25 C26 C27 122.2(2) . . ? C26 C27 C28 117.48(19) . . ? N2 C28 C23 106.99(15) . . ? N2 C28 C27 131.96(17) . . ? C23 C28 C27 121.04(17) . . ? N3 C31 C10 114.49(14) . . ? N3 C31 C32 111.00(16) . . ? C10 C31 C32 134.51(16) . . ? C31 C32 C33 106.52(15) . . ? C31 C32 C39 127.55(19) . . ? C33 C32 C39 125.87(18) . . ? C32 C33 C34 131.88(18) . . ? C32 C33 C38 108.36(15) . . ? C34 C33 C38 119.76(18) . . ? C33 C34 C35 119.06(18) . . ? C34 C35 C36 120.65(18) . . ? C35 C36 C37 121.57(19) . . ? C36 C37 C38 117.66(18) . . ? N3 C38 C33 106.88(15) . . ? N3 C38 C37 131.84(16) . . ? C33 C38 C37 121.24(16) . . ? Cl1 C40 Cl1 139.1(4) 2_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 P1 N1 C18 -9.7(2) . . . . ? Fe1 P1 N2 C28 -1.9(2) . . . . ? Fe1 P1 N3 C38 1.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 29.82 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.811 _refine_diff_density_min -1.209 _refine_diff_density_rms 0.058 #===END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Fe(CO)4[P(C9H8N)3] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H24 Fe N3 O4 P' _chemical_formula_sum 'C31 H24 Fe N3 O4 P' _chemical_formula_weight 589.35 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 Orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 8.7425(7) _cell_length_b 18.0742(13) _cell_length_c 35.872(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5668.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 21.52 _exptl_crystal_description 'chunk' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.853452 _exptl_absorpt_correction_T_max 0.991571 _exptl_absorpt_process_details ? _exptl_special_details ; The decay correction was applied simultaneously with the absorption correction in sadabs. No formal measure of the extent of decay is printed out by this program. The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 \s(I). ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD Diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '100 frames' _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'before and after data collection' _diffrn_standards_decay_% ? _diffrn_reflns_number 37447 _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 29.71 _reflns_number_total 7544 _reflns_number_gt 4326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL and the Toledo cifomatic' _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^)+(0.0324P)^2^+3.4320P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 7544 _refine_ls_number_parameters 506 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1137 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.0944 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.01978(5) 0.58819(2) 0.111655(10) 0.04576(12) Uani 1 1 d . A . P1 P 0.23915(8) 0.53323(4) 0.122879(17) 0.04280(17) Uani 1 1 d . . . O1 O -0.2609(3) 0.67440(13) 0.10230(7) 0.0800(7) Uani 1 1 d . A . O2 O 0.1188(4) 0.71334(12) 0.15785(7) 0.0988(9) Uani 1 1 d . A . O3 O -0.1533(3) 0.46253(13) 0.14145(6) 0.0801(7) Uani 1 1 d . A . O4 O 0.0511(3) 0.58375(13) 0.03046(5) 0.0777(7) Uani 1 1 d . A . N1 N 0.3344(3) 0.56247(12) 0.16133(5) 0.0483(6) Uani 1 1 d . A . N2 N 0.2367(3) 0.44074(11) 0.13132(5) 0.0482(5) Uani 1 1 d . A . N3A N 0.3808(5) 0.5327(2) 0.08972(11) 0.0421(8) Uani 0.82 1 d P A 1 N3B N 0.355(2) 0.5660(8) 0.0903(5) 0.040(4) Uani 0.18 1 d PD A 2 C1 C -0.1533(4) 0.63978(16) 0.10557(8) 0.0564(7) Uani 1 1 d . . . C2 C 0.0845(4) 0.66439(17) 0.13985(8) 0.0625(8) Uani 1 1 d . . . C3 C -0.0844(3) 0.51071(17) 0.13030(8) 0.0536(7) Uani 1 1 d . . . C4 C 0.0445(3) 0.58519(15) 0.06208(8) 0.0547(7) Uani 1 1 d . . . C11 C 0.4893(4) 0.58316(17) 0.16317(8) 0.0570(7) Uani 1 1 d . . . H11 H 0.548(3) 0.5819(14) 0.1404(8) 0.057(8) Uiso 1 1 d . . . C12 C 0.5274(4) 0.60401(16) 0.19777(8) 0.0591(8) Uani 1 1 d . A . C13 C 0.3935(4) 0.59579(15) 0.22048(7) 0.0528(7) Uani 1 1 d . . . C14 C 0.3653(5) 0.60647(18) 0.25878(8) 0.0661(9) Uani 1 1 d . A . H14 H 0.445(4) 0.6235(17) 0.2738(9) 0.081(10) Uiso 1 1 d . . . C15 C 0.2221(5) 0.59101(19) 0.27239(9) 0.0724(10) Uani 1 1 d . . . H15 H 0.206(4) 0.5954(17) 0.2987(10) 0.090(11) Uiso 1 1 d . . . C16 C 0.1078(5) 0.56494(19) 0.24955(8) 0.0678(9) Uani 1 1 d . A . H16 H 0.010(3) 0.5538(15) 0.2585(8) 0.060(9) Uiso 1 1 d . . . C17 C 0.1324(4) 0.55300(18) 0.21187(8) 0.0608(8) Uani 1 1 d . . . H17 H 0.061(3) 0.5335(14) 0.1980(7) 0.050(8) Uiso 1 1 d . . . C18 C 0.2752(3) 0.56992(14) 0.19784(7) 0.0474(7) Uani 1 1 d . A . C19 C 0.6821(6) 0.6299(4) 0.21090(15) 0.0945(14) Uani 1 1 d . . . H19C H 0.666(5) 0.672(2) 0.2241(12) 0.115(18) Uiso 1 1 d . . . H19B H 0.712(6) 0.601(3) 0.2300(14) 0.135(19) Uiso 1 1 d . . . H19A H 0.746(6) 0.638(3) 0.1924(14) 0.14(2) Uiso 1 1 d . . . C21 C 0.3083(4) 0.40387(18) 0.16189(8) 0.0595(8) Uani 1 1 d . . . H21 H 0.364(3) 0.4329(15) 0.1800(8) 0.065(9) Uiso 1 1 d . . . C22 C 0.2892(4) 0.33156(18) 0.15903(9) 0.0702(9) Uani 1 1 d . A . C23 C 0.2068(4) 0.31686(15) 0.12509(8) 0.0587(8) Uani 1 1 d . . . C24 C 0.1551(5) 0.2525(2) 0.10816(11) 0.0879(12) Uani 1 1 d . A . H24 H 0.189(5) 0.204(2) 0.1220(11) 0.130(15) Uiso 1 1 d . . . C25 C 0.0790(5) 0.2584(2) 0.07433(11) 0.0950(14) Uani 1 1 d . . . H25 H 0.048(4) 0.214(2) 0.0621(10) 0.103(12) Uiso 1 1 d . . . C26 C 0.0560(5) 0.3254(2) 0.05775(10) 0.0794(11) Uani 1 1 d . A . H26 H 0.001(4) 0.3297(18) 0.0330(10) 0.097(12) Uiso 1 1 d . . . C27 C 0.1037(4) 0.39089(18) 0.07458(9) 0.0625(8) Uani 1 1 d . . . H27 H 0.089(3) 0.4377(16) 0.0646(8) 0.065(9) Uiso 1 1 d . . . C28 C 0.1762(3) 0.38533(15) 0.10822(7) 0.0516(7) Uani 1 1 d . A . C29 C 0.3477(9) 0.2737(3) 0.18576(17) 0.1103(19) Uani 1 1 d . . . H29B H 0.406(5) 0.296(2) 0.2027(12) 0.104(16) Uiso 1 1 d . . . H29A H 0.394(4) 0.236(2) 0.1698(10) 0.093(14) Uiso 1 1 d . . . H29C H 0.264(5) 0.252(3) 0.1957(13) 0.14(2) Uiso 1 1 d . . . C31A C 0.4830(7) 0.4725(4) 0.0825(2) 0.0493(14) Uani 0.82 1 d P A 1 H31A H 0.4791 0.4271 0.0946 0.059 Uiso 0.82 1 calc PR A 1 C31B C 0.351(2) 0.6351(9) 0.0720(5) 0.038(4) Uani 0.18 1 d PD A 2 H31B H 0.2817 0.6728 0.0768 0.045 Uiso 0.18 1 calc PR A 2 C32A C 0.5841(4) 0.4900(2) 0.05632(9) 0.0486(8) Uani 0.82 1 d P A 1 C32B C 0.4626(15) 0.6380(9) 0.0471(4) 0.053(5) Uani 0.18 1 d PD A 2 C33 C 0.5514(3) 0.56636(15) 0.04552(7) 0.0457(6) Uani 1 1 d D . . C34A C 0.6243(4) 0.6120(2) 0.01989(9) 0.0580(9) Uani 0.82 1 d P A 1 H34A H 0.7061 0.5949 0.0057 0.070 Uiso 0.82 1 calc PR A 1 C34B C 0.6705(17) 0.5472(11) 0.0252(4) 0.066(5) Uani 0.18 1 d PD A 2 H34B H 0.7110 0.5790 0.0073 0.079 Uiso 0.18 1 calc PR A 2 C35A C 0.5710(6) 0.6834(3) 0.01623(13) 0.0636(13) Uani 0.82 1 d P A 1 H35A H 0.6163 0.7150 -0.0010 0.076 Uiso 0.82 1 calc PR A 1 C35B C 0.731(3) 0.4794(11) 0.0314(7) 0.071(7) Uani 0.18 1 d PD A 2 H35B H 0.8148 0.4620 0.0179 0.085 Uiso 0.18 1 calc PR A 2 C36A C 0.4497(6) 0.7089(3) 0.03813(13) 0.0601(12) Uani 0.82 1 d P A 1 H36A H 0.4167 0.7575 0.0355 0.072 Uiso 0.82 1 calc PR A 1 C36B C 0.661(2) 0.4366(13) 0.0597(6) 0.064(6) Uani 0.18 1 d PD A 2 H36B H 0.6999 0.3895 0.0639 0.077 Uiso 0.18 1 calc PR A 2 C37A C 0.3779(6) 0.6630(2) 0.06365(14) 0.0508(11) Uani 0.82 1 d P A 1 H37A H 0.2977 0.6801 0.0783 0.061 Uiso 0.82 1 calc PR A 1 C37B C 0.539(3) 0.4582(16) 0.0816(10) 0.047(7) Uani 0.18 1 d PD A 2 H37B H 0.5014 0.4276 0.1003 0.057 Uiso 0.18 1 calc PR A 2 C38A C 0.4293(4) 0.5913(2) 0.06656(8) 0.0423(7) Uani 0.82 1 d P A 1 C38B C 0.474(2) 0.5261(10) 0.0750(4) 0.044(4) Uani 0.18 1 d PD A 2 C39A C 0.7082(6) 0.4421(3) 0.04085(16) 0.0621(14) Uani 0.82 1 d P A 1 H39C H 0.7046 0.3944 0.0526 0.093 Uiso 0.82 1 calc PR A 1 H39B H 0.8057 0.4646 0.0455 0.093 Uiso 0.82 1 calc PR A 1 H39A H 0.6938 0.4364 0.0145 0.093 Uiso 0.82 1 calc PR A 1 C39B C 0.497(3) 0.7055(16) 0.0238(6) 0.067(8) Uani 0.18 1 d P A 2 H39F H 0.4279 0.7446 0.0303 0.101 Uiso 0.18 1 calc PR A 2 H39E H 0.4856 0.6936 -0.0021 0.101 Uiso 0.18 1 calc PR A 2 H39D H 0.6004 0.7213 0.0284 0.101 Uiso 0.18 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0546(2) 0.0436(2) 0.03901(19) 0.00075(16) 0.00138(18) -0.00066(19) P1 0.0487(4) 0.0475(4) 0.0322(3) 0.0019(3) 0.0039(3) -0.0065(3) O1 0.0727(16) 0.0768(15) 0.0904(17) -0.0075(12) -0.0071(14) 0.0190(14) O2 0.152(3) 0.0546(14) 0.0902(17) -0.0195(12) -0.0204(17) -0.0137(16) O3 0.0833(18) 0.0782(16) 0.0789(15) 0.0125(12) 0.0208(13) -0.0244(14) O4 0.0903(17) 0.1045(18) 0.0385(11) 0.0030(11) 0.0009(11) 0.0039(14) N1 0.0512(15) 0.0599(14) 0.0337(11) -0.0004(10) 0.0008(10) -0.0104(12) N2 0.0583(15) 0.0456(11) 0.0408(11) 0.0001(9) -0.0013(11) 0.0029(12) N3A 0.047(2) 0.042(2) 0.0366(16) 0.0010(19) 0.0129(16) 0.003(2) N3B 0.045(9) 0.031(9) 0.044(8) -0.014(8) 0.008(7) 0.016(8) C1 0.064(2) 0.0538(17) 0.0519(17) -0.0014(13) -0.0010(15) 0.0025(16) C2 0.080(2) 0.0498(17) 0.0574(17) 0.0018(14) -0.0064(16) 0.0018(17) C3 0.0552(19) 0.0606(18) 0.0451(15) -0.0004(13) 0.0052(14) 0.0027(15) C4 0.0573(18) 0.0564(17) 0.0505(16) 0.0039(14) 0.0000(14) 0.0042(15) C11 0.0511(19) 0.0668(19) 0.0531(16) 0.0005(14) -0.0019(15) -0.0055(16) C12 0.0555(19) 0.0642(19) 0.0575(17) 0.0005(14) -0.0105(15) -0.0068(16) C13 0.066(2) 0.0481(16) 0.0444(14) -0.0036(12) -0.0078(14) 0.0013(15) C14 0.085(3) 0.066(2) 0.0469(17) -0.0138(15) -0.0157(18) 0.008(2) C15 0.099(3) 0.079(2) 0.0385(16) -0.0048(15) 0.0026(18) 0.009(2) C16 0.078(3) 0.082(2) 0.0433(16) -0.0027(15) 0.0103(17) -0.005(2) C17 0.068(2) 0.077(2) 0.0372(15) -0.0057(14) 0.0033(15) -0.0158(18) C18 0.0573(18) 0.0511(15) 0.0337(12) 0.0021(11) -0.0014(12) -0.0017(14) C19 0.074(3) 0.134(5) 0.075(3) -0.007(3) -0.019(2) -0.023(3) C21 0.068(2) 0.064(2) 0.0466(16) 0.0025(14) -0.0052(15) -0.0015(17) C22 0.089(3) 0.062(2) 0.0597(18) 0.0121(15) -0.0059(18) 0.0017(18) C23 0.071(2) 0.0494(16) 0.0554(16) 0.0036(14) -0.0058(15) -0.0019(15) C24 0.117(3) 0.053(2) 0.094(3) 0.000(2) -0.022(3) -0.005(2) C25 0.130(4) 0.062(2) 0.093(3) -0.020(2) -0.034(3) 0.000(2) C26 0.098(3) 0.071(2) 0.070(2) -0.0193(18) -0.026(2) 0.009(2) C27 0.076(2) 0.0549(19) 0.0565(17) -0.0056(15) -0.0138(16) 0.0107(17) C28 0.0563(18) 0.0557(16) 0.0429(14) -0.0050(13) 0.0005(13) 0.0025(14) C29 0.162(6) 0.081(3) 0.088(3) 0.025(3) -0.040(4) 0.008(4) C31A 0.050(4) 0.047(4) 0.051(2) -0.004(2) 0.006(3) 0.004(3) C31B 0.035(10) 0.023(10) 0.054(11) 0.015(8) -0.003(8) -0.002(8) C32A 0.046(2) 0.054(2) 0.0452(19) -0.0102(17) -0.0001(16) 0.0021(19) C32B 0.028(9) 0.098(14) 0.034(7) 0.021(9) -0.006(7) -0.030(10) C33 0.0411(16) 0.0603(17) 0.0358(13) 0.0002(12) -0.0037(12) -0.0054(13) C34A 0.048(2) 0.083(3) 0.0428(19) 0.0076(19) 0.0040(16) -0.004(2) C34B 0.068(12) 0.100(16) 0.029(7) -0.014(9) 0.013(8) -0.040(12) C35A 0.055(3) 0.083(4) 0.053(3) 0.022(2) 0.003(2) -0.017(3) C35B 0.083(16) 0.060(15) 0.069(16) -0.026(12) 0.009(12) -0.017(15) C36A 0.058(3) 0.059(3) 0.064(3) 0.018(3) 0.005(2) -0.001(2) C36B 0.052(14) 0.053(11) 0.086(16) -0.021(12) 0.017(11) 0.000(10) C37A 0.049(3) 0.047(3) 0.056(3) 0.010(2) 0.003(2) -0.004(2) C37B 0.05(2) 0.044(13) 0.046(11) 0.003(9) 0.008(13) 0.008(11) C38A 0.043(2) 0.050(2) 0.0343(17) 0.0018(17) 0.0018(15) -0.006(2) C38B 0.060(12) 0.035(10) 0.038(8) -0.013(7) -0.009(9) -0.012(9) C39A 0.049(3) 0.067(4) 0.070(4) -0.015(3) 0.010(2) 0.004(3) C39B 0.059(18) 0.091(18) 0.051(13) 0.017(12) 0.048(11) -0.009(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C1 1.791(3) . ? Fe1 C4 1.792(3) . ? Fe1 C3 1.799(3) . ? Fe1 C2 1.800(3) . ? Fe1 P1 2.1970(8) . ? P1 N3B 1.65(2) . ? P1 N1 1.696(2) . ? P1 N2 1.699(2) . ? P1 N3A 1.717(4) . ? O1 C1 1.136(3) . ? O2 C2 1.135(3) . ? O3 C3 1.132(3) . ? O4 C4 1.136(3) . ? N1 C11 1.407(4) . ? N1 C18 1.415(3) . ? N2 C28 1.404(3) . ? N2 C21 1.428(3) . ? N3A C38A 1.410(5) . ? N3A C31A 1.432(6) . ? N3B C38B 1.39(2) . ? N3B C31B 1.410(15) . ? C11 C12 1.339(4) . ? C12 C13 1.434(4) . ? C12 C19 1.506(5) . ? C13 C18 1.396(4) . ? C13 C14 1.409(4) . ? C14 C15 1.373(5) . ? C15 C16 1.375(5) . ? C16 C17 1.386(4) . ? C17 C18 1.380(4) . ? C21 C22 1.322(4) . ? C22 C23 1.439(4) . ? C22 C29 1.508(5) . ? C23 C24 1.388(4) . ? C23 C28 1.403(4) . ? C24 C25 1.388(5) . ? C25 C26 1.364(5) . ? C26 C27 1.393(4) . ? C27 C28 1.367(4) . ? C31A C32A 1.328(7) . ? C31B C32B 1.323(17) . ? C32A C33 1.461(5) . ? C32A C39A 1.496(7) . ? C32B C39B 1.51(3) . ? C32B C33 1.511(15) . ? C33 C34B 1.317(13) . ? C33 C38A 1.383(4) . ? C33 C34A 1.390(4) . ? C33 C38B 1.448(19) . ? C34A C35A 1.379(6) . ? C34B C35B 1.355(17) . ? C35A C36A 1.398(6) . ? C35B C36B 1.42(3) . ? C36A C37A 1.386(6) . ? C36B C37B 1.379(18) . ? C37A C38A 1.376(5) . ? C37B C38B 1.370(18) . ? 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 Fe1 C4 89.80(13) . . ? C1 Fe1 C3 91.32(13) . . ? C4 Fe1 C3 113.97(13) . . ? C1 Fe1 C2 86.30(14) . . ? C4 Fe1 C2 122.88(13) . . ? C3 Fe1 C2 123.07(13) . . ? C1 Fe1 P1 174.48(10) . . ? C4 Fe1 P1 93.62(10) . . ? C3 Fe1 P1 91.25(10) . . ? C2 Fe1 P1 88.20(11) . . ? N3B P1 N1 99.5(7) . . ? N3B P1 N2 119.1(4) . . ? N1 P1 N2 99.66(11) . . ? N1 P1 N3A 102.18(17) . . ? N2 P1 N3A 97.32(15) . . ? N3B P1 Fe1 103.9(6) . . ? N1 P1 Fe1 115.91(9) . . ? N2 P1 Fe1 117.81(9) . . ? N3A P1 Fe1 120.32(14) . . ? C11 N1 C18 106.5(2) . . ? C11 N1 P1 126.45(19) . . ? C18 N1 P1 127.07(19) . . ? C28 N2 C21 106.6(2) . . ? C28 N2 P1 126.98(18) . . ? C21 N2 P1 126.2(2) . . ? C38A N3A C31A 106.0(4) . . ? C38A N3A P1 128.4(3) . . ? C31A N3A P1 125.4(4) . . ? C38B N3B C31B 107.0(17) . . ? C38B N3B P1 123.7(12) . . ? C31B N3B P1 129.2(13) . . ? O1 C1 Fe1 177.8(3) . . ? O2 C2 Fe1 177.0(3) . . ? O3 C3 Fe1 178.1(3) . . ? O4 C4 Fe1 176.0(3) . . ? C12 C11 N1 111.0(3) . . ? C11 C12 C13 107.1(3) . . ? C11 C12 C19 126.9(4) . . ? C13 C12 C19 126.0(3) . . ? C18 C13 C14 118.9(3) . . ? C18 C13 C12 108.0(2) . . ? C14 C13 C12 133.1(3) . . ? C15 C14 C13 118.6(3) . . ? C14 C15 C16 121.4(3) . . ? C15 C16 C17 121.4(4) . . ? C18 C17 C16 117.5(3) . . ? C17 C18 C13 122.2(2) . . ? C17 C18 N1 130.4(3) . . ? C13 C18 N1 107.4(2) . . ? C22 C21 N2 110.3(3) . . ? C21 C22 C23 108.1(3) . . ? C21 C22 C29 126.4(4) . . ? C23 C22 C29 125.4(4) . . ? C24 C23 C28 119.2(3) . . ? C24 C23 C22 133.5(3) . . ? C28 C23 C22 107.3(2) . . ? C23 C24 C25 118.3(4) . . ? C26 C25 C24 121.3(4) . . ? C25 C26 C27 121.4(3) . . ? C28 C27 C26 117.3(3) . . ? C27 C28 C23 122.3(3) . . ? C27 C28 N2 130.1(3) . . ? C23 C28 N2 107.6(2) . . ? C32A C31A N3A 111.2(5) . . ? C32B C31B N3B 109.5(17) . . ? C31A C32A C33 106.4(4) . . ? C31A C32A C39A 127.4(5) . . ? C33 C32A C39A 126.2(4) . . ? C31B C32B C39B 123.7(16) . . ? C31B C32B C33 111.7(12) . . ? C39B C32B C33 124.7(13) . . ? C38A C33 C34A 121.5(3) . . ? C34B C33 C38B 129.7(12) . . ? C38A C33 C32A 108.3(3) . . ? C34A C33 C32A 130.2(3) . . ? C34B C33 C32B 130.6(10) . . ? C38B C33 C32B 99.5(10) . . ? C35A C34A C33 117.6(4) . . ? C33 C34B C35B 117.2(17) . . ? C34A C35A C36A 120.7(4) . . ? C34B C35B C36B 116(2) . . ? C37A C36A C35A 121.2(5) . . ? C37B C36B C35B 126(2) . . ? C38A C37A C36A 117.8(5) . . ? C38B C37B C36B 118(3) . . ? C37A C38A C33 121.2(3) . . ? C37A C38A N3A 130.8(4) . . ? C33 C38A N3A 108.0(3) . . ? C37B C38B N3B 135.0(19) . . ? C37B C38B C33 112.7(19) . . ? N3B C38B C33 112.3(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 P1 N1 C18 50.5(2) . . . . ? Fe1 P1 N2 C28 56.0(2) . . . . ? Fe1 P1 N3A C38A 42.6(4) . . . . ? Fe1 P1 N3B C38B -148.7(15) . . . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 29.71 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.321 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.046 #===END data_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Fe(CO)4[P(NC4H4)3] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H12 Fe N3 O4 P' _chemical_formula_sum 'C16 H12 Fe N3 O4 P' _chemical_formula_weight 397.11 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 9.1920(3) _cell_length_b 10.2470(8) _cell_length_c 10.7407(3) _cell_angle_alpha 86.360(5) _cell_angle_beta 65.577(4) _cell_angle_gamma 88.141(4) _cell_volume 919.27(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3612 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 21.43 _exptl_crystal_description 'chunk' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.806106 _exptl_absorpt_correction_T_max 0.991589 _exptl_absorpt_process_details ? _exptl_special_details ; The decay correction was applied simultaneously with the absorption correction in sadabs. No formal measure of the extent of decay is printed out by this program. The final unit cell is obtained from the refinement of the XYZ weighted centroids of reflections above 20 \s(I). ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens CCD Diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '100 frames' _diffrn_standards_interval_count ? _diffrn_standards_interval_time 'before and after data collection' _diffrn_standards_decay_% ? _diffrn_reflns_number 10468 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 29.72 _reflns_number_total 4705 _reflns_number_gt 2929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL and the Toledo cifomatic' _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^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 4705 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 Fe1 Fe 0.26008(4) 0.84862(3) 0.28801(3) 0.05794(14) Uani 1.000000 1 d . P1 P 0.15488(7) 0.71635(6) 0.19926(6) 0.05622(17) Uani 1.000000 1 d . O1 O 0.3994(3) 1.0318(3) 0.4065(3) 0.1454(11) Uani 1.000000 1 d . O2 O 0.5571(3) 0.8585(2) 0.0392(2) 0.0958(6) Uani 1.000000 1 d . O3 O 0.2368(3) 0.6537(2) 0.5061(2) 0.1089(8) Uani 1.000000 1 d . O4 O -0.0085(3) 1.0308(2) 0.3371(3) 0.1112(8) Uani 1.000000 1 d . N1 N 0.1987(3) 0.7453(3) 0.0311(2) 0.0790(7) Uani 1.000000 1 d . N2 N -0.0477(2) 0.7102(2) 0.2668(2) 0.0689(6) Uani 1.000000 1 d . N3 N 0.2001(2) 0.55555(19) 0.2070(2) 0.0619(5) Uani 1.000000 1 d . C1 C 0.3449(4) 0.9613(3) 0.3603(3) 0.0888(9) Uani 1.000000 1 d . C2 C 0.4404(3) 0.8541(2) 0.1351(3) 0.0676(6) Uani 1.000000 1 d . C3 C 0.2424(3) 0.7289(3) 0.4207(3) 0.0710(7) Uani 1.000000 1 d . C4 C 0.0974(4) 0.9599(3) 0.3152(3) 0.0788(8) Uani 1.000000 1 d . C10 C 0.2087(5) 0.8699(6) -0.0337(5) 0.1122(15) Uani 1.000000 1 d . C11 C 0.2322(6) 0.8510(9) -0.1637(5) 0.155(3) Uani 1.000000 1 d . C12 C 0.2351(6) 0.7194(9) -0.1824(4) 0.149(3) Uani 1.000000 1 d . C13 C 0.2160(4) 0.6538(5) -0.0646(3) 0.1024(12) Uani 1.000000 1 d . C20 C -0.1465(4) 0.7089(4) 0.1979(5) 0.0968(10) Uani 1.000000 1 d . C21 C -0.2957(5) 0.6902(5) 0.2946(6) 0.1216(17) Uani 1.000000 1 d . C22 C -0.2949(4) 0.6805(4) 0.4238(5) 0.1026(11) Uani 1.000000 1 d . C23 C -0.1434(4) 0.6945(3) 0.4062(4) 0.0860(9) Uani 1.000000 1 d . C30 C 0.1026(4) 0.4500(3) 0.2198(4) 0.0872(9) Uani 1.000000 1 d . C31 C 0.1901(4) 0.3403(4) 0.2051(4) 0.1031(12) Uani 1.000000 1 d . C32 C 0.3444(4) 0.3737(3) 0.1847(4) 0.0888(9) Uani 1.000000 1 d . C33 C 0.3492(3) 0.5045(3) 0.1866(3) 0.0720(7) Uani 1.000000 1 d . H10 H 0.207(5) 0.926(4) 0.008(4) 0.117(17) Uiso 1.000000 1 d . H11 H 0.231(5) 0.922(4) -0.208(4) 0.122(14) Uiso 1.000000 1 d . H12 H 0.258(4) 0.669(4) -0.257(4) 0.128(13) Uiso 1.000000 1 d . H13 H 0.224(3) 0.561(3) -0.045(3) 0.089(11) Uiso 1.000000 1 d . H20 H -0.090(4) 0.711(4) 0.095(4) 0.124(13) Uiso 1.000000 1 d . H21 H -0.369(5) 0.684(4) 0.288(5) 0.143(18) Uiso 1.000000 1 d . H22 H -0.382(4) 0.674(3) 0.507(4) 0.115(12) Uiso 1.000000 1 d . H23 H -0.098(3) 0.698(3) 0.467(3) 0.083(9) Uiso 1.000000 1 d . H30 H -0.007(3) 0.471(3) 0.241(3) 0.090(9) Uiso 1.000000 1 d . H31 H 0.157(5) 0.262(4) 0.214(4) 0.138(15) Uiso 1.000000 1 d . H32 H 0.427(3) 0.318(3) 0.169(3) 0.078(8) Uiso 1.000000 1 d . H33 H 0.433(3) 0.560(3) 0.162(3) 0.082(9) Uiso 1.000000 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 Fe1 0.0626(2) 0.0579(2) 0.0585(2) -0.00530(15) -0.02948(18) -0.00574(15) P1 0.0565(3) 0.0647(4) 0.0524(4) 0.0002(3) -0.0273(3) -0.0097(3) O1 0.126(2) 0.154(2) 0.168(3) -0.081(2) -0.0607(19) -0.0277(17) O2 0.0851(14) 0.0950(15) 0.0847(15) -0.0097(12) -0.0105(12) -0.0185(11) O3 0.143(2) 0.1213(19) 0.0740(14) 0.0206(13) -0.0587(15) -0.0147(15) O4 0.1126(18) 0.0887(16) 0.144(2) -0.0164(14) -0.0655(16) 0.0300(14) N1 0.0814(15) 0.1101(19) 0.0558(13) 0.0098(13) -0.0387(11) -0.0300(13) N2 0.0575(12) 0.0804(15) 0.0737(14) -0.0007(11) -0.0319(11) -0.0073(10) N3 0.0570(11) 0.0614(12) 0.0660(13) -0.0090(10) -0.0224(10) -0.0094(9) C1 0.0808(19) 0.093(2) 0.095(2) -0.0331(18) -0.0346(17) -0.0061(16) C2 0.0749(17) 0.0597(15) 0.0725(18) -0.0042(13) -0.0338(15) -0.0112(12) C3 0.0787(17) 0.0832(19) 0.0597(16) -0.0047(14) -0.0367(14) -0.0067(14) C4 0.091(2) 0.0644(17) 0.089(2) -0.0028(15) -0.0456(17) -0.0019(15) C10 0.120(3) 0.148(4) 0.087(3) 0.043(3) -0.065(2) -0.041(3) C11 0.126(3) 0.271(8) 0.093(3) 0.083(4) -0.076(3) -0.089(4) C12 0.110(3) 0.288(8) 0.058(2) 0.008(4) -0.041(2) -0.084(4) C13 0.091(2) 0.161(4) 0.062(2) -0.018(2) -0.0334(17) -0.036(2) C20 0.076(2) 0.122(3) 0.111(3) -0.003(2) -0.056(2) -0.0033(18) C21 0.060(2) 0.151(4) 0.162(5) -0.005(3) -0.054(3) -0.002(2) C22 0.062(2) 0.115(3) 0.115(3) -0.009(2) -0.020(2) -0.0038(17) C23 0.0654(18) 0.106(2) 0.079(2) -0.0009(17) -0.0224(17) -0.0074(15) C30 0.0721(19) 0.0710(19) 0.112(3) -0.0070(17) -0.0300(18) -0.0196(15) C31 0.098(2) 0.066(2) 0.128(3) -0.011(2) -0.027(2) -0.0194(19) C32 0.086(2) 0.073(2) 0.098(2) -0.0139(17) -0.0280(18) 0.0085(17) C33 0.0640(16) 0.0687(18) 0.0799(19) -0.0097(14) -0.0252(14) -0.0060(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 P1 2.1661(7) . ? Fe1 C1 1.793(3) . ? Fe1 C2 1.786(3) . ? Fe1 C3 1.778(3) . ? Fe1 C4 1.787(3) . ? P1 N1 1.688(2) . ? P1 N2 1.698(2) . ? P1 N3 1.691(2) . ? O1 C1 1.139(4) . ? O2 C2 1.139(3) . ? O3 C3 1.145(3) . ? O4 C4 1.147(3) . ? N1 C10 1.402(5) . ? N1 C13 1.393(4) . ? N2 C20 1.390(4) . ? N2 C23 1.389(4) . ? N3 C30 1.390(3) . ? N3 C33 1.386(3) . ? C10 C11 1.348(7) . ? C11 C12 1.374(9) . ? C12 C13 1.342(6) . ? C20 C21 1.346(6) . ? C21 C22 1.388(6) . ? C22 C23 1.337(4) . ? C30 C31 1.340(5) . ? C31 C32 1.393(5) . ? C32 C33 1.344(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Fe1 C1 178.64(11) . . ? P1 Fe1 C2 90.71(8) . . ? P1 Fe1 C3 90.71(9) . . ? P1 Fe1 C4 89.54(9) . . ? C1 Fe1 C2 89.43(13) . . ? C1 Fe1 C3 90.41(14) . . ? C2 Fe1 C3 118.69(12) . . ? C4 Fe1 C1 89.25(14) . . ? C4 Fe1 C2 123.00(13) . . ? C4 Fe1 C3 118.30(13) . . ? Fe1 P1 N1 116.00(9) . . ? Fe1 P1 N2 116.91(8) . . ? Fe1 P1 N3 117.31(7) . . ? N1 P1 N2 101.38(11) . . ? N1 P1 N3 102.05(12) . . ? N2 P1 N3 100.55(10) . . ? P1 N1 C10 124.7(3) . . ? P1 N1 C13 127.4(3) . . ? C10 N1 C13 107.6(3) . . ? P1 N2 C20 128.2(2) . . ? P1 N2 C23 123.9(2) . . ? C20 N2 C23 107.7(3) . . ? P1 N3 C30 127.3(2) . . ? P1 N3 C33 125.52(17) . . ? C30 N3 C33 106.8(2) . . ? Fe1 C1 O1 179.3(4) . . ? Fe1 C2 O2 178.5(2) . . ? Fe1 C3 O3 177.1(3) . . ? Fe1 C4 O4 177.8(3) . . ? N1 C10 C11 106.4(6) . . ? C10 C11 C12 109.7(5) . . ? C11 C12 C13 108.5(5) . . ? N1 C13 C12 107.7(5) . . ? N2 C20 C21 106.3(4) . . ? C20 C21 C22 110.3(4) . . ? C21 C22 C23 107.0(4) . . ? N2 C23 C22 108.7(4) . . ? N3 C30 C31 108.2(3) . . ? C30 C31 C32 108.5(3) . . ? C31 C32 C33 107.7(3) . . ? N3 C33 C32 108.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 P1 N1 C10 -39.5(3) . . . . ? Fe1 P1 N2 C23 -49.5(3) . . . . ? Fe1 P1 N3 C33 -40.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 29.72 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 0.254 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.045 #===END