data_blt1106_300k _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 Cl2 Fe N P2' _chemical_formula_sum 'C26 H40 Cl2 Fe N P2' _chemical_formula_weight 555.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n _symmetry_space_group_name_Hall -P2yac loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 11.442(3) _cell_length_b 9.347(2) _cell_length_c 13.087(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.491(15) _cell_angle_gamma 90.00 _cell_volume 1390.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 5675 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.35 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 586 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.660 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18708 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 28.70 _reflns_number_total 3511 _reflns_number_gt 2660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0446P)^2^+0.4934P] 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 3511 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.008 _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 0.2500 0.63788(4) 0.2500 0.03838(13) Uani 1 2 d S . . Cl1 Cl 0.25607(6) 0.50074(9) 0.10874(6) 0.0806(3) Uani 1 1 d . . . P1 P 0.04113(4) 0.68757(5) 0.21242(4) 0.03272(13) Uani 1 1 d . . . N1 N 0.2500 0.8498(2) 0.2500 0.0337(5) Uani 1 2 d S . . C1 C -0.0764(2) 0.5807(2) 0.25842(17) 0.0454(5) Uani 1 1 d . . . H1B H -0.1509 0.6304 0.2386 0.055 Uiso 1 1 calc R . . C2 C -0.0822(3) 0.4357(3) 0.2035(2) 0.0772(9) Uani 1 1 d . . . H2A H -0.1391 0.3759 0.2312 0.116 Uiso 1 1 calc R . . H2B H -0.0064 0.3906 0.2136 0.116 Uiso 1 1 calc R . . H2C H -0.1047 0.4498 0.1313 0.116 Uiso 1 1 calc R . . C3 C -0.0626(2) 0.5634(3) 0.37498(18) 0.0577(6) Uani 1 1 d . . . H3A H -0.1299 0.5144 0.3954 0.087 Uiso 1 1 calc R . . H3B H -0.0561 0.6560 0.4069 0.087 Uiso 1 1 calc R . . H3C H 0.0071 0.5088 0.3961 0.087 Uiso 1 1 calc R . . C4 C -0.0094(2) 0.7220(2) 0.07524(16) 0.0433(5) Uani 1 1 d . . . H4A H -0.0124 0.6295 0.0398 0.052 Uiso 1 1 calc R . . C5 C -0.1318(2) 0.7856(3) 0.0584(2) 0.0659(7) Uani 1 1 d . . . H5A H -0.1542 0.7990 -0.0139 0.099 Uiso 1 1 calc R . . H5B H -0.1324 0.8762 0.0929 0.099 Uiso 1 1 calc R . . H5C H -0.1865 0.7219 0.0856 0.099 Uiso 1 1 calc R . . C6 C 0.0785(2) 0.8152(3) 0.02627(19) 0.0585(6) Uani 1 1 d . . . H6A H 0.0516 0.8293 -0.0452 0.088 Uiso 1 1 calc R . . H6B H 0.1539 0.7689 0.0327 0.088 Uiso 1 1 calc R . . H6C H 0.0854 0.9062 0.0604 0.088 Uiso 1 1 calc R . . C7 C 0.04371(16) 0.85962(19) 0.27427(15) 0.0328(4) Uani 1 1 d . . . C8 C -0.05117(17) 0.9268(2) 0.31240(16) 0.0389(4) Uani 1 1 d . . . H8A H -0.1241 0.8818 0.3052 0.047 Uiso 1 1 calc R . . C9 C -0.03983(19) 1.0594(2) 0.36082(17) 0.0427(5) Uani 1 1 d . . . C10 C -0.1426(2) 1.1286(3) 0.4043(2) 0.0584(7) Uani 1 1 d . . . H10A H -0.2131 1.1125 0.3586 0.088 Uiso 1 1 calc R . . H10B H -0.1289 1.2296 0.4117 0.088 Uiso 1 1 calc R . . H10C H -0.1513 1.0878 0.4703 0.088 Uiso 1 1 calc R . . C11 C 0.0703(2) 1.1236(2) 0.36870(17) 0.0456(5) Uani 1 1 d . . . H11A H 0.0800 1.2128 0.4000 0.055 Uiso 1 1 calc R . . C12 C 0.16588(18) 1.0596(2) 0.33161(16) 0.0420(5) Uani 1 1 d . . . H12A H 0.2382 1.1063 0.3382 0.050 Uiso 1 1 calc R . . C13 C 0.15493(16) 0.9251(2) 0.28409(14) 0.0326(4) 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 Fe1 0.0297(2) 0.0406(2) 0.0446(3) 0.000 0.00326(17) 0.000 Cl1 0.0572(4) 0.0904(5) 0.0911(6) -0.0555(4) -0.0049(4) 0.0121(3) P1 0.0344(3) 0.0322(2) 0.0322(3) 0.00156(19) 0.0061(2) 0.00176(19) N1 0.0264(10) 0.0372(12) 0.0376(13) 0.000 0.0036(9) 0.000 C1 0.0489(12) 0.0433(11) 0.0454(13) 0.0032(9) 0.0111(10) -0.0076(9) C2 0.119(3) 0.0500(14) 0.0662(18) -0.0080(13) 0.0282(17) -0.0354(16) C3 0.0700(16) 0.0588(14) 0.0477(14) 0.0088(11) 0.0217(12) -0.0044(12) C4 0.0577(13) 0.0376(10) 0.0336(11) 0.0012(8) 0.0011(10) -0.0036(9) C5 0.0565(15) 0.0756(18) 0.0604(17) 0.0173(14) -0.0168(13) -0.0037(13) C6 0.0749(17) 0.0612(14) 0.0396(13) 0.0125(11) 0.0077(12) -0.0099(13) C7 0.0311(9) 0.0348(9) 0.0328(10) -0.0012(7) 0.0043(8) 0.0001(7) C8 0.0327(10) 0.0395(10) 0.0456(12) -0.0009(9) 0.0090(9) 0.0022(8) C9 0.0467(12) 0.0405(11) 0.0429(12) 0.0005(9) 0.0138(9) 0.0080(9) C10 0.0622(15) 0.0491(13) 0.0692(17) -0.0030(12) 0.0306(13) 0.0130(11) C11 0.0543(13) 0.0375(11) 0.0460(13) -0.0084(9) 0.0094(10) -0.0001(9) C12 0.0397(11) 0.0441(11) 0.0422(12) -0.0076(9) 0.0043(9) -0.0060(9) C13 0.0294(9) 0.0382(10) 0.0299(10) -0.0004(8) 0.0022(7) 0.0017(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 Fe1 N1 1.981(2) . ? Fe1 Cl1 2.2570(8) 2 ? Fe1 Cl1 2.2570(8) . ? Fe1 P1 2.4297(8) . ? Fe1 P1 2.4297(8) 2 ? P1 C7 1.7991(19) . ? P1 C1 1.830(2) . ? P1 C4 1.851(2) . ? N1 C13 1.410(2) . ? N1 C13 1.410(2) 2 ? C1 C3 1.524(3) . ? C1 C2 1.532(3) . ? C1 H1B 0.9800 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.515(3) . ? C4 C6 1.526(3) . ? C4 H4A 0.9800 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.395(3) . ? C7 C13 1.405(3) . ? C8 C9 1.391(3) . ? C8 H8A 0.9300 . ? C9 C11 1.389(3) . ? C9 C10 1.509(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.382(3) . ? C11 H11A 0.9300 . ? C12 C13 1.402(3) . ? C12 H12A 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 N1 Fe1 Cl1 124.60(3) . 2 ? N1 Fe1 Cl1 124.60(3) . . ? Cl1 Fe1 Cl1 110.79(6) 2 . ? N1 Fe1 P1 78.978(16) . . ? Cl1 Fe1 P1 98.84(3) 2 . ? Cl1 Fe1 P1 93.63(3) . . ? N1 Fe1 P1 78.978(16) . 2 ? Cl1 Fe1 P1 93.63(3) 2 2 ? Cl1 Fe1 P1 98.84(3) . 2 ? P1 Fe1 P1 157.96(3) . 2 ? C7 P1 C1 108.36(10) . . ? C7 P1 C4 105.56(9) . . ? C1 P1 C4 104.69(10) . . ? C7 P1 Fe1 96.55(6) . . ? C1 P1 Fe1 124.85(8) . . ? C4 P1 Fe1 114.94(7) . . ? C13 N1 C13 120.1(2) . 2 ? C13 N1 Fe1 119.96(11) . . ? C13 N1 Fe1 119.96(11) 2 . ? C3 C1 C2 111.7(2) . . ? C3 C1 P1 112.98(16) . . ? C2 C1 P1 108.85(16) . . ? C3 C1 H1B 107.7 . . ? C2 C1 H1B 107.7 . . ? P1 C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C6 111.0(2) . . ? C5 C4 P1 113.04(17) . . ? C6 C4 P1 111.00(16) . . ? C5 C4 H4A 107.2 . . ? C6 C4 H4A 107.2 . . ? P1 C4 H4A 107.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C13 120.31(17) . . ? C8 C7 P1 126.15(15) . . ? C13 C7 P1 113.53(13) . . ? C9 C8 C7 121.87(19) . . ? C9 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? C11 C9 C8 117.14(18) . . ? C11 C9 C10 121.7(2) . . ? C8 C9 C10 121.1(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 122.27(19) . . ? C12 C11 H11A 118.9 . . ? C9 C11 H11A 118.9 . . ? C11 C12 C13 120.62(19) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C12 C13 C7 117.77(17) . . ? C12 C13 N1 123.70(17) . . ? C7 C13 N1 118.47(17) . . ? 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 N1 Fe1 P1 C7 -26.59(6) . . . . ? Cl1 Fe1 P1 C7 97.14(7) 2 . . . ? Cl1 Fe1 P1 C7 -151.15(7) . . . . ? P1 Fe1 P1 C7 -26.59(6) 2 . . . ? N1 Fe1 P1 C1 -144.38(9) . . . . ? Cl1 Fe1 P1 C1 -20.65(9) 2 . . . ? Cl1 Fe1 P1 C1 91.06(9) . . . . ? P1 Fe1 P1 C1 -144.38(9) 2 . . . ? N1 Fe1 P1 C4 83.98(7) . . . . ? Cl1 Fe1 P1 C4 -152.29(8) 2 . . . ? Cl1 Fe1 P1 C4 -40.59(8) . . . . ? P1 Fe1 P1 C4 83.98(7) 2 . . . ? Cl1 Fe1 N1 C13 -60.10(9) 2 . . . ? Cl1 Fe1 N1 C13 119.90(9) . . . . ? P1 Fe1 N1 C13 33.10(9) . . . . ? P1 Fe1 N1 C13 -146.90(9) 2 . . . ? Cl1 Fe1 N1 C13 119.90(9) 2 . . 2 ? Cl1 Fe1 N1 C13 -60.10(9) . . . 2 ? P1 Fe1 N1 C13 -146.90(9) . . . 2 ? P1 Fe1 N1 C13 33.10(9) 2 . . 2 ? C7 P1 C1 C3 -57.25(19) . . . . ? C4 P1 C1 C3 -169.54(17) . . . . ? Fe1 P1 C1 C3 54.9(2) . . . . ? C7 P1 C1 C2 178.09(18) . . . . ? C4 P1 C1 C2 65.8(2) . . . . ? Fe1 P1 C1 C2 -69.7(2) . . . . ? C7 P1 C4 C5 -61.53(19) . . . . ? C1 P1 C4 C5 52.73(19) . . . . ? Fe1 P1 C4 C5 -166.61(15) . . . . ? C7 P1 C4 C6 63.89(18) . . . . ? C1 P1 C4 C6 178.16(17) . . . . ? Fe1 P1 C4 C6 -41.19(18) . . . . ? C1 P1 C7 C8 -26.1(2) . . . . ? C4 P1 C7 C8 85.58(19) . . . . ? Fe1 P1 C7 C8 -156.21(17) . . . . ? C1 P1 C7 C13 152.71(15) . . . . ? C4 P1 C7 C13 -95.59(16) . . . . ? Fe1 P1 C7 C13 22.61(15) . . . . ? C13 C7 C8 C9 0.1(3) . . . . ? P1 C7 C8 C9 178.82(16) . . . . ? C7 C8 C9 C11 0.8(3) . . . . ? C7 C8 C9 C10 -178.2(2) . . . . ? C8 C9 C11 C12 -0.8(3) . . . . ? C10 C9 C11 C12 178.3(2) . . . . ? C9 C11 C12 C13 -0.1(3) . . . . ? C11 C12 C13 C7 1.0(3) . . . . ? C11 C12 C13 N1 -176.09(18) . . . . ? C8 C7 C13 C12 -1.0(3) . . . . ? P1 C7 C13 C12 -179.86(15) . . . . ? C8 C7 C13 N1 176.29(16) . . . . ? P1 C7 C13 N1 -2.6(2) . . . . ? C13 N1 C13 C12 -30.71(16) 2 . . . ? Fe1 N1 C13 C12 149.29(16) . . . . ? C13 N1 C13 C7 152.22(19) 2 . . . ? Fe1 N1 C13 C7 -27.78(19) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.542 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.053