# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Rosenthal, Uwe' _publ_contact_author_name 'Rosenthal, Uwe' _publ_contact_author_email uwe.rosenthal@catalysis.de _publ_section_title ; Coordination Chemistry of new Selective Ethylene Trimerisation Ligand Ph2PN(iPr)P(Ph)NH(R) (R = iPr, Et) and Tests in Catalysis ; # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 780221' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H28 N2 P2' _chemical_formula_weight 394.41 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 8.9016(18) _cell_length_b 9.978(2) _cell_length_c 24.459(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2172.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7937 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 27.31 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE-IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28706 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0302 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4279 _reflns_number_gt 3836 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2005)' _computing_cell_refinement X-AREA _computing_data_reduction X-AREA _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0427P)^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 mixed _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 -0.06(7) _refine_ls_number_reflns 4279 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.6036(2) -0.40182(18) -0.17166(7) 0.0357(4) Uani 1 1 d . . . C2 C -0.7256(2) -0.48801(19) -0.16956(8) 0.0412(4) Uani 1 1 d . . . H2A H -0.8244 -0.4523 -0.1710 0.049 Uiso 1 1 calc R . . C3 C -0.7058(3) -0.62571(19) -0.16539(9) 0.0491(5) Uani 1 1 d . . . H3A H -0.7906 -0.6834 -0.1638 0.059 Uiso 1 1 calc R . . C4 C -0.5632(3) -0.6781(2) -0.16359(8) 0.0492(5) Uani 1 1 d . . . H4A H -0.5490 -0.7722 -0.1606 0.059 Uiso 1 1 calc R . . C5 C -0.4412(2) -0.5940(2) -0.16612(8) 0.0480(5) Uani 1 1 d . . . H5A H -0.3427 -0.6305 -0.1651 0.058 Uiso 1 1 calc R . . C6 C -0.4602(2) -0.4572(2) -0.17005(7) 0.0418(4) Uani 1 1 d . . . H6A H -0.3747 -0.4004 -0.1717 0.050 Uiso 1 1 calc R . . C7 C -0.4778(2) -0.13979(18) -0.15497(7) 0.0345(4) Uani 1 1 d . . . C8 C -0.4134(2) -0.03590(18) -0.18400(8) 0.0418(4) Uani 1 1 d . . . H8A H -0.4469 -0.0177 -0.2201 0.050 Uiso 1 1 calc R . . C9 C -0.3009(2) 0.0423(2) -0.16135(10) 0.0537(5) Uani 1 1 d . . . H9A H -0.2581 0.1134 -0.1820 0.064 Uiso 1 1 calc R . . C10 C -0.2510(2) 0.0175(2) -0.10916(10) 0.0533(6) Uani 1 1 d . . . H10A H -0.1755 0.0722 -0.0932 0.064 Uiso 1 1 calc R . . C11 C -0.3124(2) -0.0884(2) -0.08010(9) 0.0524(5) Uani 1 1 d . . . H11A H -0.2778 -0.1070 -0.0441 0.063 Uiso 1 1 calc R . . C12 C -0.4226(2) -0.1668(2) -0.10288(8) 0.0450(5) Uani 1 1 d . . . H12A H -0.4617 -0.2405 -0.0828 0.054 Uiso 1 1 calc R . . C13 C -0.8509(2) -0.07411(17) -0.04749(7) 0.0338(4) Uani 1 1 d . . . C14 C -0.7714(2) 0.04098(19) -0.06027(8) 0.0437(5) Uani 1 1 d . . . H14A H -0.6949 0.0370 -0.0873 0.052 Uiso 1 1 calc R . . C15 C -0.8008(3) 0.1610(2) -0.03462(9) 0.0541(5) Uani 1 1 d . . . H15A H -0.7466 0.2393 -0.0447 0.065 Uiso 1 1 calc R . . C16 C -0.9092(3) 0.1677(2) 0.00583(9) 0.0560(6) Uani 1 1 d . . . H16A H -0.9292 0.2502 0.0238 0.067 Uiso 1 1 calc R . . C17 C -0.9877(2) 0.0540(2) 0.01977(8) 0.0482(5) Uani 1 1 d . . . H17A H -1.0622 0.0579 0.0475 0.058 Uiso 1 1 calc R . . C18 C -0.9586(2) -0.06585(19) -0.00652(7) 0.0375(4) Uani 1 1 d . . . H18A H -1.0131 -0.1438 0.0036 0.045 Uiso 1 1 calc R . . C19 C -0.9158(2) -0.11674(19) -0.17323(8) 0.0402(4) Uani 1 1 d . . . H19A H -0.9873 -0.0898 -0.1437 0.048 Uiso 1 1 calc R . . C20 C -1.0012(2) -0.2094(2) -0.21190(9) 0.0557(6) Uani 1 1 d . . . H20A H -1.0309 -0.2909 -0.1923 0.084 Uiso 1 1 calc R . . H20B H -0.9364 -0.2334 -0.2428 0.084 Uiso 1 1 calc R . . H20C H -1.0911 -0.1635 -0.2255 0.084 Uiso 1 1 calc R . . C21 C -0.8682(3) 0.0099(2) -0.20228(10) 0.0622(6) Uani 1 1 d . . . H21A H -0.8141 0.0681 -0.1767 0.093 Uiso 1 1 calc R . . H21B H -0.9572 0.0568 -0.2160 0.093 Uiso 1 1 calc R . . H21C H -0.8022 -0.0130 -0.2330 0.093 Uiso 1 1 calc R . . C22 C -0.9765(2) -0.4572(2) -0.05715(8) 0.0478(5) Uani 1 1 d . . . H22A H -1.0057 -0.4643 -0.0182 0.057 Uiso 1 1 calc R . . H22B H -0.8768 -0.5000 -0.0614 0.057 Uiso 1 1 calc R . . C23 C -1.0891(3) -0.5318(2) -0.09138(10) 0.0618(6) Uani 1 1 d . . . H23A H -1.0919 -0.6259 -0.0800 0.093 Uiso 1 1 calc R . . H23B H -1.0601 -0.5264 -0.1300 0.093 Uiso 1 1 calc R . . H23C H -1.1887 -0.4917 -0.0865 0.093 Uiso 1 1 calc R . . N1 N -0.78775(16) -0.18620(14) -0.14637(5) 0.0319(3) Uani 1 1 d . . . N2 N -0.96455(19) -0.31682(16) -0.07171(7) 0.0440(4) Uani 1 1 d . . . P1 P -0.63785(5) -0.22530(5) -0.187022(16) 0.03376(11) Uani 1 1 d . . . P2 P -0.80116(5) -0.23498(4) -0.079291(16) 0.03127(10) Uani 1 1 d . . . H2 H -1.049(2) -0.2816(18) -0.0791(7) 0.032(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0415(10) 0.0349(9) 0.0305(8) -0.0059(7) 0.0008(7) 0.0045(8) C2 0.0408(11) 0.0349(9) 0.0480(10) -0.0064(8) 0.0000(8) 0.0034(8) C3 0.0544(12) 0.0365(10) 0.0564(12) -0.0078(9) 0.0011(10) -0.0028(10) C4 0.0630(13) 0.0337(10) 0.0508(11) -0.0093(9) -0.0027(10) 0.0101(9) C5 0.0454(11) 0.0482(12) 0.0503(11) -0.0132(9) -0.0029(9) 0.0143(9) C6 0.0400(10) 0.0430(11) 0.0423(10) -0.0086(8) -0.0011(8) 0.0046(8) C7 0.0318(9) 0.0358(10) 0.0361(9) -0.0005(7) 0.0049(7) 0.0025(7) C8 0.0408(10) 0.0374(10) 0.0473(10) 0.0058(9) 0.0008(9) 0.0036(8) C9 0.0409(10) 0.0362(10) 0.0839(15) 0.0079(10) 0.0055(11) 0.0013(9) C10 0.0355(10) 0.0472(12) 0.0772(15) -0.0174(11) 0.0003(10) 0.0025(9) C11 0.0376(10) 0.0756(14) 0.0440(10) -0.0085(11) -0.0025(9) 0.0009(10) C12 0.0404(10) 0.0582(12) 0.0365(9) 0.0040(9) 0.0028(8) -0.0058(9) C13 0.0335(9) 0.0359(9) 0.0319(8) -0.0017(7) -0.0069(7) 0.0017(8) C14 0.0448(11) 0.0402(10) 0.0460(10) -0.0054(8) 0.0017(8) -0.0076(9) C15 0.0604(13) 0.0410(11) 0.0607(13) -0.0085(10) -0.0037(11) -0.0096(11) C16 0.0638(14) 0.0475(12) 0.0567(13) -0.0203(10) -0.0091(11) 0.0114(11) C17 0.0477(11) 0.0581(13) 0.0389(10) -0.0082(9) -0.0016(8) 0.0101(10) C18 0.0382(10) 0.0429(10) 0.0314(9) 0.0016(8) -0.0036(7) 0.0032(8) C19 0.0396(9) 0.0393(10) 0.0416(10) -0.0029(8) -0.0089(8) 0.0097(8) C20 0.0532(12) 0.0571(14) 0.0569(12) -0.0079(10) -0.0249(10) 0.0070(10) C21 0.0739(15) 0.0465(12) 0.0661(14) 0.0173(10) -0.0134(12) 0.0120(12) C22 0.0523(12) 0.0404(11) 0.0507(11) 0.0043(9) 0.0024(9) -0.0098(9) C23 0.0616(14) 0.0481(13) 0.0758(15) -0.0028(11) -0.0045(11) -0.0182(11) N1 0.0340(8) 0.0301(7) 0.0316(7) -0.0009(6) -0.0040(6) 0.0045(6) N2 0.0336(9) 0.0345(8) 0.0639(10) 0.0026(8) 0.0026(8) -0.0011(7) P1 0.0373(2) 0.0349(2) 0.02906(19) 0.00032(18) -0.00034(17) 0.0011(2) P2 0.0312(2) 0.0295(2) 0.0331(2) 0.00083(18) -0.00052(17) 0.00082(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.386(3) . ? C1 C6 1.392(3) . ? C1 P1 1.8265(19) . ? C2 C3 1.389(3) . ? C3 C4 1.373(3) . ? C4 C5 1.374(3) . ? C5 C6 1.379(3) . ? C7 C8 1.381(3) . ? C7 C12 1.392(3) . ? C7 P1 1.8362(19) . ? C8 C9 1.386(3) . ? C9 C10 1.374(3) . ? C10 C11 1.386(3) . ? C11 C12 1.373(3) . ? C13 C14 1.385(3) . ? C13 C18 1.389(2) . ? C13 P2 1.8380(18) . ? C14 C15 1.377(3) . ? C15 C16 1.384(3) . ? C16 C17 1.376(3) . ? C17 C18 1.382(3) . ? C19 N1 1.487(2) . ? C19 C21 1.511(3) . ? C19 C20 1.526(3) . ? C22 N2 1.449(3) . ? C22 C23 1.503(3) . ? N1 P1 1.7092(15) . ? N1 P2 1.7155(14) . ? N2 P2 1.6782(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.09(17) . . ? C2 C1 P1 118.38(13) . . ? C6 C1 P1 122.82(15) . . ? C1 C2 C3 121.15(18) . . ? C4 C3 C2 119.75(19) . . ? C3 C4 C5 119.78(19) . . ? C4 C5 C6 120.71(18) . . ? C5 C6 C1 120.52(19) . . ? C8 C7 C12 118.01(18) . . ? C8 C7 P1 116.82(14) . . ? C12 C7 P1 125.07(14) . . ? C7 C8 C9 121.15(19) . . ? C10 C9 C8 120.2(2) . . ? C9 C10 C11 119.1(2) . . ? C12 C11 C10 120.5(2) . . ? C11 C12 C7 120.89(19) . . ? C14 C13 C18 117.81(17) . . ? C14 C13 P2 120.36(14) . . ? C18 C13 P2 121.56(14) . . ? C15 C14 C13 121.41(19) . . ? C14 C15 C16 120.0(2) . . ? C17 C16 C15 119.47(19) . . ? C16 C17 C18 120.20(19) . . ? C17 C18 C13 121.08(18) . . ? N1 C19 C21 112.48(17) . . ? N1 C19 C20 111.91(15) . . ? C21 C19 C20 110.82(17) . . ? N2 C22 C23 113.00(18) . . ? C19 N1 P1 116.61(11) . . ? C19 N1 P2 120.09(12) . . ? P1 N1 P2 123.09(8) . . ? C22 N2 P2 124.13(14) . . ? N1 P1 C1 103.34(7) . . ? N1 P1 C7 104.55(7) . . ? C1 P1 C7 103.35(8) . . ? N2 P2 N1 107.70(8) . . ? N2 P2 C13 99.75(8) . . ? N1 P2 C13 100.01(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.232 _refine_diff_density_min -0.180 _refine_diff_density_rms 0.032 # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 780222' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 Cr N2 O4 P2' _chemical_formula_weight 572.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-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 15.5122(10) _cell_length_b 17.7614(12) _cell_length_c 21.5240(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5930.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4758 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 26.26 _exptl_crystal_description prism _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7582 _exptl_absorpt_correction_T_max 0.9287 _exptl_absorpt_process_details 'X-SHAPE and X-RED32 (Stoe & Cie, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5827 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5827 _reflns_number_gt 3721 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2005)' _computing_cell_refinement X-AREA _computing_data_reduction X-AREA _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0281P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5827 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0605 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 0.786 _refine_ls_restrained_S_all 0.786 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.65151(13) 0.15326(13) 0.71397(10) 0.0313(5) Uani 1 1 d . A 1 C2 C 0.70508(14) 0.08129(12) 0.61677(10) 0.0323(5) Uani 1 1 d . A 1 C3 C 0.55648(13) 0.02699(13) 0.59337(10) 0.0294(5) Uani 1 1 d . A 1 C4 C 0.58958(14) 0.01955(13) 0.70621(10) 0.0345(5) Uani 1 1 d . A 1 C5 C 0.60076(13) 0.21938(12) 0.51095(9) 0.0328(5) Uani 1 1 d . A 1 C6 C 0.60119(15) 0.15388(13) 0.47559(10) 0.0400(5) Uani 1 1 d . A 1 H6A H 0.5928 0.1066 0.4953 0.048 Uiso 1 1 calc R A 1 C7 C 0.61371(16) 0.15675(15) 0.41198(10) 0.0479(6) Uani 1 1 d . A 1 H7A H 0.6124 0.1118 0.3881 0.057 Uiso 1 1 calc R A 1 C8 C 0.62791(16) 0.22457(17) 0.38366(11) 0.0485(7) Uani 1 1 d . A 1 H8A H 0.6366 0.2265 0.3400 0.058 Uiso 1 1 calc R A 1 C9 C 0.62970(16) 0.28986(17) 0.41784(12) 0.0525(7) Uani 1 1 d . A 1 H9A H 0.6409 0.3366 0.3980 0.063 Uiso 1 1 calc R A 1 C10 C 0.61520(14) 0.28752(14) 0.48118(11) 0.0428(6) Uani 1 1 d . A 1 H10A H 0.6151 0.3329 0.5045 0.051 Uiso 1 1 calc R A 1 C11 C 0.62725(13) 0.29509(12) 0.62754(10) 0.0299(5) Uani 1 1 d . A 1 C12 C 0.70957(14) 0.31890(13) 0.61138(10) 0.0360(5) Uani 1 1 d . A 1 H12A H 0.7399 0.2938 0.5791 0.043 Uiso 1 1 calc R A 1 C13 C 0.74774(14) 0.37867(13) 0.64188(11) 0.0426(6) Uani 1 1 d . A 1 H13A H 0.8037 0.3949 0.6300 0.051 Uiso 1 1 calc R A 1 C14 C 0.70530(16) 0.41478(14) 0.68930(12) 0.0487(7) Uani 1 1 d . A 1 H14A H 0.7319 0.4558 0.7101 0.058 Uiso 1 1 calc R A 1 C15 C 0.62424(16) 0.39133(14) 0.70656(12) 0.0482(6) Uani 1 1 d . A 1 H15A H 0.5949 0.4159 0.7396 0.058 Uiso 1 1 calc R A 1 C16 C 0.58537(15) 0.33179(13) 0.67576(11) 0.0403(6) Uani 1 1 d . A 1 H16A H 0.5293 0.3159 0.6878 0.048 Uiso 1 1 calc R A 1 C17 C 0.36491(12) 0.09264(12) 0.62483(9) 0.0283(5) Uani 1 1 d . A 1 C18 C 0.35851(14) 0.08315(12) 0.56063(10) 0.0345(5) Uani 1 1 d . A 1 H18A H 0.4002 0.1055 0.5341 0.041 Uiso 1 1 calc R A 1 C19 C 0.29213(15) 0.04159(13) 0.53535(11) 0.0410(6) Uani 1 1 d . A 1 H19A H 0.2879 0.0362 0.4915 0.049 Uiso 1 1 calc R A 1 C20 C 0.23224(16) 0.00796(14) 0.57309(12) 0.0476(7) Uani 1 1 d . A 1 H20A H 0.1862 -0.0200 0.5554 0.057 Uiso 1 1 calc R A 1 C21 C 0.23879(15) 0.01473(14) 0.63644(12) 0.0484(7) Uani 1 1 d . A 1 H21A H 0.1980 -0.0095 0.6626 0.058 Uiso 1 1 calc R A 1 C22 C 0.30469(14) 0.05675(13) 0.66229(10) 0.0375(5) Uani 1 1 d . A 1 H22A H 0.3088 0.0611 0.7062 0.045 Uiso 1 1 calc R A 1 C23 C 0.45442(15) 0.19091(15) 0.78136(10) 0.0444(7) Uani 1 1 d . A 1 H23A H 0.5158 0.2041 0.7722 0.053 Uiso 1 1 calc R A 1 C24 C 0.4540(2) 0.1223(2) 0.82274(13) 0.0849(11) Uani 1 1 d . A 1 H24A H 0.4821 0.0803 0.8012 0.127 Uiso 1 1 calc R A 1 H24B H 0.3943 0.1085 0.8326 0.127 Uiso 1 1 calc R A 1 H24C H 0.4851 0.1334 0.8613 0.127 Uiso 1 1 calc R A 1 C25 C 0.4128(2) 0.2579(2) 0.81257(15) 0.0892(12) Uani 1 1 d . A 1 H25A H 0.4143 0.3012 0.7844 0.134 Uiso 1 1 calc R A 1 H25B H 0.4444 0.2701 0.8507 0.134 Uiso 1 1 calc R A 1 H25C H 0.3529 0.2458 0.8229 0.134 Uiso 1 1 calc R A 1 C26 C 0.41698(16) 0.28115(15) 0.58204(12) 0.0533(7) Uani 1 1 d . A 1 H26A H 0.4571 0.3247 0.5767 0.064 Uiso 1 1 calc R A 1 C27 C 0.37930(18) 0.26667(17) 0.51859(14) 0.0692(9) Uani 1 1 d . A 1 H27A H 0.4253 0.2515 0.4900 0.104 Uiso 1 1 calc R A 1 H27B H 0.3518 0.3127 0.5032 0.104 Uiso 1 1 calc R A 1 H27C H 0.3363 0.2264 0.5214 0.104 Uiso 1 1 calc R A 1 C28 C 0.35137(18) 0.30642(18) 0.62880(15) 0.0741(10) Uani 1 1 d . A 1 H28A H 0.3798 0.3154 0.6688 0.111 Uiso 1 1 calc R A 1 H28B H 0.3074 0.2673 0.6337 0.111 Uiso 1 1 calc R A 1 H28C H 0.3241 0.3531 0.6144 0.111 Uiso 1 1 calc R A 1 N1 N 0.47159(10) 0.21791(10) 0.60551(8) 0.0312(4) Uani 1 1 d . A 1 N2 N 0.41114(13) 0.17534(12) 0.72248(8) 0.0411(5) Uani 1 1 d . A 1 H2 H 0.3588(15) 0.1838(13) 0.7224(10) 0.038(7) Uiso 1 1 d . B 1 O1 O 0.69072(10) 0.18206(10) 0.75274(7) 0.0466(4) Uani 1 1 d . A 1 O2 O 0.77082(10) 0.07235(10) 0.59260(8) 0.0524(5) Uani 1 1 d . A 1 O3 O 0.58484(12) -0.03023(10) 0.74060(8) 0.0558(5) Uani 1 1 d . A 1 O4 O 0.53626(11) -0.02318(10) 0.56318(7) 0.0460(4) Uani 1 1 d . A 1 P1 P 0.57934(3) 0.21038(3) 0.59394(2) 0.02743(12) Uani 1 1 d . A 1 P2 P 0.45504(3) 0.14590(3) 0.65726(3) 0.02707(12) Uani 1 1 d . A 1 Cr1 Cr 0.597032(19) 0.098893(18) 0.650343(14) 0.02462(8) Uani 1 1 d . A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0285(12) 0.0334(13) 0.0319(12) -0.0012(10) 0.0013(9) 0.0078(10) C2 0.0328(12) 0.0317(14) 0.0323(11) -0.0031(10) -0.0046(10) 0.0018(10) C3 0.0269(11) 0.0328(13) 0.0286(11) 0.0022(10) 0.0015(9) 0.0022(9) C4 0.0285(12) 0.0418(14) 0.0333(11) -0.0033(11) -0.0018(10) 0.0035(11) C5 0.0305(11) 0.0336(13) 0.0342(11) 0.0058(10) -0.0040(9) -0.0020(11) C6 0.0502(14) 0.0345(14) 0.0353(12) 0.0049(10) -0.0003(11) -0.0038(12) C7 0.0571(16) 0.0516(17) 0.0350(13) 0.0007(12) -0.0007(11) -0.0014(13) C8 0.0464(15) 0.067(2) 0.0323(13) 0.0115(13) -0.0031(11) -0.0058(13) C9 0.0551(16) 0.0528(18) 0.0495(16) 0.0240(14) -0.0085(12) -0.0119(14) C10 0.0466(14) 0.0352(14) 0.0465(14) 0.0101(12) -0.0079(11) -0.0057(11) C11 0.0298(11) 0.0227(12) 0.0372(12) 0.0011(10) -0.0050(9) 0.0000(9) C12 0.0329(12) 0.0332(14) 0.0420(13) 0.0015(10) -0.0016(10) -0.0012(10) C13 0.0338(12) 0.0391(15) 0.0550(15) 0.0040(12) -0.0048(11) -0.0104(10) C14 0.0522(16) 0.0336(16) 0.0602(16) -0.0111(12) -0.0090(13) -0.0099(12) C15 0.0505(15) 0.0381(15) 0.0559(15) -0.0159(13) 0.0023(12) -0.0030(13) C16 0.0325(12) 0.0345(14) 0.0540(14) -0.0088(11) 0.0019(11) -0.0040(11) C17 0.0254(10) 0.0244(12) 0.0350(11) -0.0003(9) -0.0004(9) 0.0001(10) C18 0.0345(12) 0.0344(14) 0.0346(12) -0.0028(10) -0.0005(10) -0.0028(10) C19 0.0479(14) 0.0369(15) 0.0382(13) -0.0066(11) -0.0085(11) -0.0016(12) C20 0.0400(14) 0.0390(16) 0.0637(17) -0.0101(13) -0.0109(13) -0.0114(12) C21 0.0415(14) 0.0432(16) 0.0607(18) -0.0004(13) 0.0089(12) -0.0150(12) C22 0.0377(12) 0.0375(14) 0.0374(13) -0.0015(11) 0.0048(10) -0.0040(11) C23 0.0314(12) 0.0651(19) 0.0368(13) -0.0210(13) 0.0054(10) -0.0033(12) C24 0.097(3) 0.115(3) 0.0426(16) 0.0044(18) 0.0046(16) -0.022(2) C25 0.068(2) 0.124(3) 0.075(2) -0.064(2) -0.0092(18) 0.026(2) C26 0.0421(14) 0.0383(15) 0.0795(19) 0.0090(13) -0.0111(14) 0.0116(12) C27 0.0601(19) 0.057(2) 0.090(2) 0.0208(17) -0.0364(17) 0.0038(14) C28 0.0509(17) 0.061(2) 0.111(3) 0.0013(18) -0.0063(17) 0.0304(16) N1 0.0250(9) 0.0249(10) 0.0436(11) 0.0036(9) -0.0036(8) 0.0011(8) N2 0.0254(11) 0.0571(14) 0.0407(11) -0.0177(9) 0.0015(9) 0.0036(10) O1 0.0436(10) 0.0562(12) 0.0401(9) -0.0162(8) -0.0129(8) 0.0051(8) O2 0.0301(9) 0.0700(13) 0.0571(11) -0.0129(10) 0.0088(8) 0.0042(8) O3 0.0647(12) 0.0526(12) 0.0500(10) 0.0228(9) 0.0025(9) 0.0018(10) O4 0.0523(10) 0.0402(10) 0.0455(9) -0.0151(8) -0.0034(8) -0.0072(8) P1 0.0250(3) 0.0252(3) 0.0321(3) -0.0001(2) -0.0021(2) -0.0013(2) P2 0.0232(3) 0.0277(3) 0.0303(3) -0.0042(2) -0.0004(2) 0.0006(2) Cr1 0.02313(15) 0.02595(17) 0.02478(15) -0.00150(15) -0.00020(14) 0.00189(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.152(2) . ? C1 Cr1 1.877(2) . ? C2 O2 1.156(2) . ? C2 Cr1 1.852(2) . ? C3 O4 1.147(3) . ? C3 Cr1 1.879(2) . ? C4 O3 1.155(3) . ? C4 Cr1 1.856(2) . ? C5 C10 1.388(3) . ? C5 C6 1.390(3) . ? C5 P1 1.824(2) . ? C6 C7 1.384(3) . ? C7 C8 1.368(3) . ? C8 C9 1.374(4) . ? C9 C10 1.382(3) . ? C11 C16 1.387(3) . ? C11 C12 1.389(3) . ? C11 P1 1.827(2) . ? C12 C13 1.382(3) . ? C13 C14 1.373(3) . ? C14 C15 1.376(3) . ? C15 C16 1.386(3) . ? C17 C22 1.389(3) . ? C17 C18 1.396(3) . ? C17 P2 1.827(2) . ? C18 C19 1.379(3) . ? C19 C20 1.371(3) . ? C20 C21 1.373(3) . ? C21 C22 1.382(3) . ? C23 N2 1.461(3) . ? C23 C24 1.510(4) . ? C23 C25 1.511(4) . ? C26 N1 1.495(3) . ? C26 C28 1.500(4) . ? C26 C27 1.508(4) . ? N1 P1 1.6951(17) . ? N1 P2 1.7153(18) . ? N2 P2 1.6456(18) . ? P1 Cr1 2.3388(6) . ? P1 P2 2.6243(8) . ? P2 Cr1 2.3602(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Cr1 173.98(19) . . ? O2 C2 Cr1 175.9(2) . . ? O4 C3 Cr1 171.77(19) . . ? O3 C4 Cr1 179.5(2) . . ? C10 C5 C6 118.44(19) . . ? C10 C5 P1 123.92(17) . . ? C6 C5 P1 117.63(16) . . ? C7 C6 C5 120.8(2) . . ? C8 C7 C6 119.7(2) . . ? C7 C8 C9 120.5(2) . . ? C8 C9 C10 120.0(2) . . ? C9 C10 C5 120.5(2) . . ? C16 C11 C12 118.3(2) . . ? C16 C11 P1 119.51(16) . . ? C12 C11 P1 121.69(17) . . ? C13 C12 C11 120.6(2) . . ? C14 C13 C12 120.4(2) . . ? C13 C14 C15 119.8(2) . . ? C14 C15 C16 120.0(2) . . ? C15 C16 C11 120.8(2) . . ? C22 C17 C18 118.1(2) . . ? C22 C17 P2 122.05(16) . . ? C18 C17 P2 119.69(16) . . ? C19 C18 C17 120.6(2) . . ? C20 C19 C18 120.4(2) . . ? C19 C20 C21 120.0(2) . . ? C20 C21 C22 120.1(2) . . ? C21 C22 C17 120.8(2) . . ? N2 C23 C24 110.9(2) . . ? N2 C23 C25 109.8(2) . . ? C24 C23 C25 111.8(2) . . ? N1 C26 C28 112.5(2) . . ? N1 C26 C27 113.4(2) . . ? C28 C26 C27 113.3(2) . . ? C26 N1 P1 124.64(15) . . ? C26 N1 P2 134.01(15) . . ? P1 N1 P2 100.61(9) . . ? C23 N2 P2 127.60(16) . . ? N1 P1 C5 108.45(9) . . ? N1 P1 C11 106.14(9) . . ? C5 P1 C11 103.96(10) . . ? N1 P1 Cr1 96.10(6) . . ? C5 P1 Cr1 124.13(8) . . ? C11 P1 Cr1 116.36(7) . . ? N1 P1 P2 39.98(6) . . ? C5 P1 P2 132.89(7) . . ? C11 P1 P2 116.92(7) . . ? Cr1 P1 P2 56.438(18) . . ? N2 P2 N1 112.27(10) . . ? N2 P2 C17 100.01(10) . . ? N1 P2 C17 104.63(9) . . ? N2 P2 Cr1 123.53(8) . . ? N1 P2 Cr1 94.77(6) . . ? C17 P2 Cr1 120.47(7) . . ? N2 P2 P1 127.47(8) . . ? N1 P2 P1 39.41(6) . . ? C17 P2 P1 126.15(7) . . ? Cr1 P2 P1 55.663(18) . . ? C2 Cr1 C4 100.43(10) . . ? C2 Cr1 C1 87.94(9) . . ? C4 Cr1 C1 86.90(10) . . ? C2 Cr1 C3 86.19(9) . . ? C4 Cr1 C3 83.45(9) . . ? C1 Cr1 C3 167.61(9) . . ? C2 Cr1 P1 92.67(7) . . ? C4 Cr1 P1 166.35(7) . . ? C1 Cr1 P1 89.77(7) . . ? C3 Cr1 P1 101.39(7) . . ? C2 Cr1 P2 158.28(7) . . ? C4 Cr1 P2 99.76(7) . . ? C1 Cr1 P2 101.08(6) . . ? C3 Cr1 P2 88.23(6) . . ? P1 Cr1 P2 67.90(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.311 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.042 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.500 111.7 39.4 2 0.000 0.500 0.000 111.7 39.3 3 0.500 0.500 0.500 111.7 39.3 4 0.500 1.000 1.000 111.7 39.3 _platon_squeeze_details ; Contribution from the disordered solvent molecules was taken into account using the PLATON/SQUEEZE procedure. ; # Attachment '- 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 780223' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H28 Cr N2 O4 P2' _chemical_formula_weight 558.45 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' Cr Cr 0.3209 0.6236 '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(1)/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 11.262(2) _cell_length_b 14.220(3) _cell_length_c 17.443(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.91(3) _cell_angle_gamma 90.00 _cell_volume 2723.0(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 11519 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 29.61 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1160 _exptl_absorpt_coefficient_mu 0.572 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44916 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6262 _reflns_number_gt 5107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2005)' _computing_cell_refinement X-AREA _computing_data_reduction X-AREA _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0534P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6262 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0794 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.23318(13) 0.11087(11) 0.28675(9) 0.0300(3) Uani 1 1 d . . . C2 C 0.18064(17) 0.02202(13) 0.27693(11) 0.0448(4) Uani 1 1 d . . . H2A H 0.1183 0.0090 0.2317 0.054 Uiso 1 1 calc R . . C3 C 0.2180(2) -0.04758(14) 0.33225(13) 0.0567(5) Uani 1 1 d . . . H3A H 0.1817 -0.1081 0.3248 0.068 Uiso 1 1 calc R . . C4 C 0.30792(19) -0.02928(14) 0.39817(11) 0.0526(5) Uani 1 1 d . . . H4A H 0.3336 -0.0772 0.4362 0.063 Uiso 1 1 calc R . . C5 C 0.36051(17) 0.05841(14) 0.40896(10) 0.0469(4) Uani 1 1 d . . . H5A H 0.4216 0.0712 0.4549 0.056 Uiso 1 1 calc R . . C6 C 0.32459(15) 0.12822(12) 0.35299(9) 0.0375(3) Uani 1 1 d . . . H6A H 0.3628 0.1881 0.3601 0.045 Uiso 1 1 calc R . . C7 C 0.02431(13) 0.18855(11) 0.18720(9) 0.0317(3) Uani 1 1 d . . . C8 C -0.04037(15) 0.18747(14) 0.10968(10) 0.0430(4) Uani 1 1 d . . . H8A H 0.0020 0.1918 0.0684 0.052 Uiso 1 1 calc R . . C9 C -0.16655(17) 0.18016(16) 0.09170(12) 0.0512(5) Uani 1 1 d . . . H9A H -0.2100 0.1799 0.0383 0.061 Uiso 1 1 calc R . . C10 C -0.22832(15) 0.17337(14) 0.15059(12) 0.0460(4) Uani 1 1 d . . . H10A H -0.3147 0.1689 0.1382 0.055 Uiso 1 1 calc R . . C11 C -0.16529(16) 0.17298(13) 0.22804(11) 0.0439(4) Uani 1 1 d . . . H11A H -0.2084 0.1675 0.2689 0.053 Uiso 1 1 calc R . . C12 C -0.03980(15) 0.18051(13) 0.24659(10) 0.0388(4) Uani 1 1 d . . . H12A H 0.0030 0.1802 0.3001 0.047 Uiso 1 1 calc R . . C13 C 0.26476(14) 0.44899(10) 0.14400(8) 0.0306(3) Uani 1 1 d . . . C14 C 0.13839(14) 0.45965(11) 0.12233(9) 0.0362(3) Uani 1 1 d . . . H14A H 0.0870 0.4105 0.1327 0.043 Uiso 1 1 calc R . . C15 C 0.08754(17) 0.54133(13) 0.08587(10) 0.0429(4) Uani 1 1 d . . . H15A H 0.0015 0.5487 0.0725 0.052 Uiso 1 1 calc R . . C16 C 0.16141(18) 0.61188(13) 0.06898(10) 0.0465(4) Uani 1 1 d . . . H16A H 0.1263 0.6676 0.0436 0.056 Uiso 1 1 calc R . . C17 C 0.28557(19) 0.60170(12) 0.08879(10) 0.0448(4) Uani 1 1 d . . . H17A H 0.3362 0.6505 0.0769 0.054 Uiso 1 1 calc R . . C18 C 0.33790(15) 0.52052(11) 0.12616(9) 0.0361(3) Uani 1 1 d . . . H18A H 0.4240 0.5140 0.1395 0.043 Uiso 1 1 calc R . . C19 C 0.20740(16) 0.34599(12) 0.31941(9) 0.0373(3) Uani 1 1 d . . . H19A H 0.1942 0.2932 0.3544 0.045 Uiso 1 1 calc R . . C20 C 0.09227(18) 0.40425(14) 0.30198(12) 0.0507(5) Uani 1 1 d . . . H20A H 0.0246 0.3661 0.2729 0.076 Uiso 1 1 calc R . . H20B H 0.1038 0.4590 0.2703 0.076 Uiso 1 1 calc R . . H20C H 0.0738 0.4255 0.3515 0.076 Uiso 1 1 calc R . . C21 C 0.31325(19) 0.40409(15) 0.36482(11) 0.0513(5) Uani 1 1 d . . . H21A H 0.3873 0.3656 0.3759 0.077 Uiso 1 1 calc R . . H21B H 0.2952 0.4252 0.4145 0.077 Uiso 1 1 calc R . . H21C H 0.3255 0.4589 0.3334 0.077 Uiso 1 1 calc R . . C22 C 0.56222(16) 0.31060(13) 0.26991(12) 0.0489(4) Uani 1 1 d . . . H22A H 0.6040 0.2889 0.2288 0.059 Uiso 1 1 calc R . . H22B H 0.5286 0.2547 0.2915 0.059 Uiso 1 1 calc R . . C23 C 0.65321(18) 0.35854(15) 0.33483(13) 0.0567(5) Uani 1 1 d . . . H23A H 0.7183 0.3143 0.3575 0.085 Uiso 1 1 calc R . . H23B H 0.6122 0.3795 0.3758 0.085 Uiso 1 1 calc R . . H23C H 0.6882 0.4130 0.3134 0.085 Uiso 1 1 calc R . . C24 C 0.41539(15) 0.22933(12) 0.05128(9) 0.0355(3) Uani 1 1 d . . . C25 C 0.42431(14) 0.13133(11) 0.17293(9) 0.0313(3) Uani 1 1 d . . . C26 C 0.23901(15) 0.08976(12) 0.06188(9) 0.0377(3) Uani 1 1 d . . . C27 C 0.18792(14) 0.26449(12) 0.03015(9) 0.0337(3) Uani 1 1 d . . . N1 N 0.23622(11) 0.30310(9) 0.24747(7) 0.0294(3) Uani 1 1 d . . . N2 N 0.46359(12) 0.37309(10) 0.23496(8) 0.0352(3) Uani 1 1 d . . . H2B H 0.4646(18) 0.4261(16) 0.2564(12) 0.045(5) Uiso 1 1 d . . . O1 O 0.48878(12) 0.24624(11) 0.01691(8) 0.0557(4) Uani 1 1 d . . . O2 O 0.50152(11) 0.08461(9) 0.20647(8) 0.0448(3) Uani 1 1 d . . . O3 O 0.19762(15) 0.02130(10) 0.03350(8) 0.0610(4) Uani 1 1 d . . . O4 O 0.12396(12) 0.29832(10) -0.02315(7) 0.0498(3) Uani 1 1 d . . . P1 P 0.19022(3) 0.19669(3) 0.20787(2) 0.02658(9) Uani 1 1 d . . . P2 P 0.32777(3) 0.33793(3) 0.18638(2) 0.02658(9) Uani 1 1 d . . . Cr1 Cr 0.30084(2) 0.202091(16) 0.109626(13) 0.02603(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0307(7) 0.0292(7) 0.0317(7) 0.0049(6) 0.0105(6) 0.0026(6) C2 0.0442(9) 0.0350(9) 0.0519(10) 0.0093(7) 0.0038(8) -0.0034(7) C3 0.0601(12) 0.0361(10) 0.0726(13) 0.0188(9) 0.0123(10) -0.0024(9) C4 0.0600(12) 0.0493(11) 0.0505(10) 0.0241(9) 0.0166(9) 0.0139(9) C5 0.0511(10) 0.0536(11) 0.0347(8) 0.0080(8) 0.0065(7) 0.0140(8) C6 0.0404(8) 0.0362(8) 0.0351(8) 0.0025(6) 0.0066(7) 0.0041(7) C7 0.0296(7) 0.0300(8) 0.0365(8) 0.0046(6) 0.0093(6) 0.0006(6) C8 0.0345(8) 0.0576(11) 0.0368(8) 0.0031(7) 0.0075(7) -0.0078(7) C9 0.0348(9) 0.0690(13) 0.0460(10) 0.0042(9) 0.0012(7) -0.0069(8) C10 0.0280(7) 0.0464(10) 0.0637(11) 0.0056(8) 0.0103(8) -0.0011(7) C11 0.0345(8) 0.0495(10) 0.0522(10) 0.0090(8) 0.0193(7) 0.0051(7) C12 0.0346(8) 0.0438(9) 0.0394(8) 0.0046(7) 0.0112(7) 0.0023(7) C13 0.0374(8) 0.0260(7) 0.0285(7) 0.0006(5) 0.0071(6) 0.0009(6) C14 0.0375(8) 0.0316(8) 0.0376(8) 0.0019(6) 0.0044(6) 0.0025(6) C15 0.0465(9) 0.0400(9) 0.0381(8) 0.0003(7) 0.0008(7) 0.0122(7) C16 0.0659(12) 0.0324(9) 0.0384(9) 0.0068(7) 0.0054(8) 0.0108(8) C17 0.0648(11) 0.0315(8) 0.0396(9) 0.0061(7) 0.0150(8) -0.0019(8) C18 0.0418(8) 0.0319(8) 0.0355(8) 0.0005(6) 0.0108(6) -0.0016(6) C19 0.0470(9) 0.0351(8) 0.0335(8) -0.0013(6) 0.0168(7) 0.0036(7) C20 0.0559(11) 0.0449(10) 0.0559(11) -0.0048(8) 0.0227(9) 0.0130(8) C21 0.0607(12) 0.0569(12) 0.0395(9) -0.0138(8) 0.0179(8) -0.0062(9) C22 0.0360(9) 0.0411(10) 0.0622(11) -0.0073(8) -0.0048(8) 0.0063(7) C23 0.0437(10) 0.0510(12) 0.0658(13) -0.0035(9) -0.0085(9) 0.0012(8) C24 0.0359(8) 0.0376(8) 0.0322(7) 0.0047(6) 0.0059(6) 0.0041(6) C25 0.0345(7) 0.0275(7) 0.0334(7) -0.0002(6) 0.0107(6) -0.0011(6) C26 0.0453(9) 0.0364(9) 0.0313(7) 0.0007(6) 0.0083(7) 0.0012(7) C27 0.0338(8) 0.0351(8) 0.0335(7) 0.0007(6) 0.0101(6) 0.0019(6) N1 0.0342(6) 0.0256(6) 0.0303(6) 0.0000(5) 0.0112(5) 0.0001(5) N2 0.0301(6) 0.0309(7) 0.0432(7) -0.0040(6) 0.0049(5) -0.0002(5) O1 0.0428(7) 0.0779(11) 0.0521(8) 0.0145(7) 0.0227(6) 0.0007(7) O2 0.0394(6) 0.0377(6) 0.0539(7) 0.0087(5) 0.0033(5) 0.0110(5) O3 0.0845(10) 0.0412(8) 0.0539(8) -0.0126(6) 0.0083(7) -0.0157(7) O4 0.0471(7) 0.0598(8) 0.0394(6) 0.0128(6) 0.0032(5) 0.0143(6) P1 0.02733(18) 0.02535(18) 0.02753(17) 0.00249(14) 0.00714(14) 0.00073(14) P2 0.02736(17) 0.02410(18) 0.02807(17) 0.00149(14) 0.00573(13) 0.00113(14) Cr1 0.02792(12) 0.02484(12) 0.02558(12) 0.00150(8) 0.00651(9) 0.00203(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 C1 C6 1.387(2) . ? C1 C2 1.389(2) . ? C1 P1 1.8218(15) . ? C2 C3 1.381(3) . ? C3 C4 1.377(3) . ? C4 C5 1.375(3) . ? C5 C6 1.388(2) . ? C7 C8 1.385(2) . ? C7 C12 1.394(2) . ? C7 P1 1.8257(16) . ? C8 C9 1.389(2) . ? C9 C10 1.367(3) . ? C10 C11 1.379(3) . ? C11 C12 1.382(2) . ? C13 C18 1.387(2) . ? C13 C14 1.397(2) . ? C13 P2 1.8192(15) . ? C14 C15 1.385(2) . ? C15 C16 1.376(3) . ? C16 C17 1.371(3) . ? C17 C18 1.390(2) . ? C19 N1 1.4947(19) . ? C19 C20 1.511(2) . ? C19 C21 1.520(3) . ? C22 N2 1.447(2) . ? C22 C23 1.510(3) . ? C24 O1 1.150(2) . ? C24 Cr1 1.8539(17) . ? C25 O2 1.1456(19) . ? C25 Cr1 1.8654(16) . ? C26 O3 1.143(2) . ? C26 Cr1 1.8630(17) . ? C27 O4 1.1470(19) . ? C27 Cr1 1.8812(17) . ? N1 P1 1.6958(13) . ? N1 P2 1.7131(13) . ? N2 P2 1.6519(14) . ? P1 Cr1 2.3342(7) . ? P1 P2 2.6142(6) . ? P2 Cr1 2.3312(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.74(15) . . ? C6 C1 P1 122.16(12) . . ? C2 C1 P1 118.82(12) . . ? C3 C2 C1 120.71(17) . . ? C4 C3 C2 120.05(19) . . ? C5 C4 C3 119.98(17) . . ? C4 C5 C6 120.22(17) . . ? C1 C6 C5 120.27(17) . . ? C8 C7 C12 118.55(14) . . ? C8 C7 P1 119.03(12) . . ? C12 C7 P1 122.39(12) . . ? C7 C8 C9 120.64(17) . . ? C10 C9 C8 120.16(17) . . ? C9 C10 C11 119.98(16) . . ? C10 C11 C12 120.34(16) . . ? C11 C12 C7 120.32(16) . . ? C18 C13 C14 118.68(14) . . ? C18 C13 P2 122.03(12) . . ? C14 C13 P2 119.05(12) . . ? C15 C14 C13 120.47(16) . . ? C16 C15 C14 120.11(17) . . ? C17 C16 C15 120.02(16) . . ? C16 C17 C18 120.49(17) . . ? C13 C18 C17 120.21(16) . . ? N1 C19 C20 113.09(14) . . ? N1 C19 C21 111.55(14) . . ? C20 C19 C21 110.16(15) . . ? N2 C22 C23 111.56(16) . . ? O1 C24 Cr1 178.18(14) . . ? O2 C25 Cr1 174.59(14) . . ? O3 C26 Cr1 177.71(17) . . ? O4 C27 Cr1 173.70(14) . . ? C19 N1 P1 127.03(10) . . ? C19 N1 P2 132.69(11) . . ? P1 N1 P2 100.15(7) . . ? C22 N2 P2 124.48(12) . . ? N1 P1 C1 106.54(7) . . ? N1 P1 C7 110.07(7) . . ? C1 P1 C7 101.20(7) . . ? N1 P1 Cr1 96.03(4) . . ? C1 P1 Cr1 118.77(5) . . ? C7 P1 Cr1 123.20(6) . . ? C1 P1 P2 123.85(5) . . ? C7 P1 P2 129.30(5) . . ? Cr1 P1 P2 55.867(16) . . ? N2 P2 N1 112.67(7) . . ? N2 P2 C13 100.26(7) . . ? N1 P2 C13 105.63(7) . . ? N2 P2 Cr1 122.15(6) . . ? N1 P2 Cr1 95.65(5) . . ? C13 P2 Cr1 119.80(5) . . ? N2 P2 P1 132.03(5) . . ? C13 P2 P1 122.37(5) . . ? Cr1 P2 P1 55.98(2) . . ? C24 Cr1 C26 99.79(7) . . ? C24 Cr1 C25 85.38(7) . . ? C26 Cr1 C25 87.53(7) . . ? C24 Cr1 C27 86.31(7) . . ? C26 Cr1 C27 87.21(7) . . ? C25 Cr1 C27 169.28(7) . . ? C24 Cr1 P2 97.18(6) . . ? C26 Cr1 P2 162.72(5) . . ? C25 Cr1 P2 97.06(5) . . ? C27 Cr1 P2 90.70(5) . . ? C24 Cr1 P1 163.93(5) . . ? C26 Cr1 P1 95.31(5) . . ? C25 Cr1 P1 89.84(5) . . ? C27 Cr1 P1 99.95(5) . . ? P2 Cr1 P1 68.157(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.320 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.043 # Attachment '- 5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 780224' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H33 Cr N3 O3 P2' _chemical_formula_weight 585.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca 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' '-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 12.7627(2) _cell_length_b 17.6292(3) _cell_length_c 26.0903(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5870.21(18) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 50510 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 29.52 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8749 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details 'X-SHAPE and X-RED32 (Stoe & Cie, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 108511 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 29.17 _reflns_number_total 7917 _reflns_number_gt 5717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2005)' _computing_cell_refinement X-AREA _computing_data_reduction X-AREA _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0550P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7917 _refine_ls_number_parameters 352 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.42258(16) 0.19760(11) 0.51139(7) 0.0416(4) Uani 1 1 d . . . H1B H 0.4904 0.1861 0.4939 0.050 Uiso 1 1 calc R . . C2 C 0.3862(2) 0.12671(14) 0.53848(10) 0.0674(7) Uani 1 1 d . . . H2A H 0.3204 0.1371 0.5565 0.101 Uiso 1 1 calc R . . H2B H 0.4396 0.1107 0.5632 0.101 Uiso 1 1 calc R . . H2C H 0.3749 0.0863 0.5133 0.101 Uiso 1 1 calc R . . C3 C 0.4412(2) 0.26107(15) 0.54921(9) 0.0673(7) Uani 1 1 d . . . H3A H 0.4661 0.3061 0.5309 0.101 Uiso 1 1 calc R . . H3B H 0.4941 0.2452 0.5743 0.101 Uiso 1 1 calc R . . H3C H 0.3756 0.2730 0.5670 0.101 Uiso 1 1 calc R . . C4 C 0.24394(13) 0.18735(9) 0.38507(6) 0.0316(3) Uani 1 1 d . . . C5 C 0.21317(15) 0.20459(10) 0.33512(7) 0.0392(4) Uani 1 1 d . . . H5 H 0.2535 0.2392 0.3154 0.047 Uiso 1 1 calc R . . C6 C 0.12454(18) 0.17181(13) 0.31393(9) 0.0533(5) Uani 1 1 d . . . H6 H 0.1047 0.1838 0.2798 0.064 Uiso 1 1 calc R . . C7 C 0.06534(18) 0.12208(13) 0.34224(11) 0.0595(6) Uani 1 1 d . . . H7 H 0.0031 0.1011 0.3282 0.071 Uiso 1 1 calc R . . C8 C 0.09616(18) 0.10282(13) 0.39078(11) 0.0588(6) Uani 1 1 d . . . H8 H 0.0560 0.0675 0.4100 0.071 Uiso 1 1 calc R . . C9 C 0.18582(16) 0.13465(11) 0.41219(8) 0.0443(4) Uani 1 1 d . . . H9 H 0.2073 0.1201 0.4456 0.053 Uiso 1 1 calc R . . C10 C 0.29219(14) 0.38416(9) 0.39659(7) 0.0350(4) Uani 1 1 d . . . H10 H 0.3346 0.4316 0.3933 0.042 Uiso 1 1 calc R . . C11 C 0.24566(19) 0.38414(12) 0.45027(8) 0.0515(5) Uani 1 1 d . . . H11A H 0.1983 0.3408 0.4540 0.077 Uiso 1 1 calc R . . H11B H 0.2066 0.4313 0.4558 0.077 Uiso 1 1 calc R . . H11C H 0.3021 0.3804 0.4756 0.077 Uiso 1 1 calc R . . C12 C 0.20487(17) 0.38900(12) 0.35711(8) 0.0487(5) Uani 1 1 d . . . H12A H 0.2349 0.3864 0.3226 0.073 Uiso 1 1 calc R . . H12B H 0.1673 0.4371 0.3612 0.073 Uiso 1 1 calc R . . H12C H 0.1561 0.3467 0.3621 0.073 Uiso 1 1 calc R . . C13 C 0.44834(13) 0.35934(9) 0.29047(6) 0.0299(3) Uani 1 1 d . . . C14 C 0.42939(15) 0.43574(10) 0.28073(7) 0.0372(4) Uani 1 1 d . . . H14 H 0.4283 0.4709 0.3083 0.045 Uiso 1 1 calc R . . C15 C 0.41211(16) 0.46077(11) 0.23113(7) 0.0438(4) Uani 1 1 d D . . H15 H 0.4000 0.5131 0.2248 0.053 Uiso 1 1 calc R . . C16 C 0.41244(18) 0.41026(10) 0.19121(7) 0.0503(5) Uani 1 1 d D . . H16 H 0.4017 0.4278 0.1572 0.060 Uiso 1 1 calc R . . C17 C 0.4282(2) 0.33463(12) 0.20010(7) 0.0574(6) Uani 1 1 d D . . H17 H 0.4263 0.2996 0.1724 0.069 Uiso 1 1 calc R . . C18 C 0.44706(18) 0.30909(11) 0.24966(7) 0.0442(4) Uani 1 1 d . . . H18 H 0.4592 0.2567 0.2556 0.053 Uiso 1 1 calc R . . C19 C 0.55514(13) 0.39880(9) 0.38186(6) 0.0279(3) Uani 1 1 d . . . C20 C 0.63288(14) 0.43498(10) 0.35364(6) 0.0348(3) Uani 1 1 d . . . H20 H 0.6441 0.4211 0.3189 0.042 Uiso 1 1 calc R . . C21 C 0.69408(15) 0.49102(11) 0.37561(7) 0.0401(4) Uani 1 1 d . . . H21 H 0.7459 0.5160 0.3557 0.048 Uiso 1 1 calc R . . C22 C 0.68020(15) 0.51068(10) 0.42618(7) 0.0403(4) Uani 1 1 d . . . H22 H 0.7214 0.5498 0.4410 0.048 Uiso 1 1 calc R . . C23 C 0.60626(14) 0.47341(10) 0.45523(7) 0.0376(4) Uani 1 1 d . . . H23 H 0.5979 0.4858 0.4904 0.045 Uiso 1 1 calc R . . C24 C 0.54404(14) 0.41783(10) 0.43324(6) 0.0332(3) Uani 1 1 d . . . H24 H 0.4932 0.3924 0.4535 0.040 Uiso 1 1 calc R . . C25 C 0.65553(16) 0.19256(12) 0.33793(8) 0.0454(4) Uani 1 1 d . . . C26 C 0.60527(14) 0.23529(10) 0.42595(7) 0.0354(4) Uani 1 1 d . . . C27 C 0.54616(16) 0.10281(11) 0.40418(8) 0.0458(4) Uani 1 1 d . . . C28 C 0.39865(16) 0.10520(10) 0.28980(7) 0.0404(4) Uani 1 1 d . . . C29 C 0.3314(2) 0.05660(14) 0.25914(9) 0.0596(6) Uani 1 1 d . . . H29A H 0.2672 0.0453 0.2783 0.089 Uiso 1 1 calc R . . H29B H 0.3682 0.0092 0.2513 0.089 Uiso 1 1 calc R . . H29C H 0.3133 0.0825 0.2271 0.089 Uiso 1 1 calc R . . Cr1 Cr 0.52946(2) 0.196613(14) 0.373024(10) 0.02848(7) Uani 1 1 d . . . N1 N 0.34664(13) 0.22020(9) 0.47248(6) 0.0367(3) Uani 1 1 d . . . N2 N 0.36501(11) 0.31940(7) 0.38851(5) 0.0283(3) Uani 1 1 d . . . N3 N 0.44828(12) 0.14266(8) 0.31570(6) 0.0367(3) Uani 1 1 d . . . O1 O 0.73686(14) 0.19082(12) 0.31866(8) 0.0779(6) Uani 1 1 d . . . O2 O 0.65736(12) 0.25687(9) 0.45927(6) 0.0555(4) Uani 1 1 d . . . O3 O 0.55763(17) 0.04684(10) 0.42553(8) 0.0819(6) Uani 1 1 d . . . P1 P 0.36603(3) 0.22694(2) 0.410384(15) 0.02618(9) Uani 1 1 d . . . P2 P 0.47812(3) 0.32133(2) 0.354324(14) 0.02598(8) Uani 1 1 d . . . H1A H 0.2900(18) 0.2266(12) 0.4827(8) 0.039(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0403(10) 0.0522(11) 0.0321(8) 0.0118(8) -0.0005(7) 0.0018(9) C2 0.0832(19) 0.0550(13) 0.0641(14) 0.0265(11) -0.0024(13) 0.0025(12) C3 0.0796(18) 0.0763(16) 0.0460(12) 0.0003(11) -0.0186(12) -0.0160(14) C4 0.0275(8) 0.0283(7) 0.0390(8) -0.0043(6) 0.0012(6) 0.0001(6) C5 0.0357(9) 0.0395(9) 0.0425(9) -0.0048(7) -0.0062(7) 0.0006(8) C6 0.0440(12) 0.0529(11) 0.0631(13) -0.0193(10) -0.0184(10) 0.0068(10) C7 0.0368(11) 0.0509(12) 0.0909(18) -0.0298(12) -0.0099(11) -0.0051(9) C8 0.0448(12) 0.0435(11) 0.0880(17) -0.0126(11) 0.0116(12) -0.0169(9) C9 0.0413(11) 0.0375(9) 0.0541(11) -0.0021(8) 0.0062(9) -0.0077(8) C10 0.0336(9) 0.0276(7) 0.0437(9) 0.0004(6) 0.0045(7) 0.0046(7) C11 0.0546(13) 0.0507(11) 0.0492(11) -0.0046(9) 0.0134(10) 0.0175(10) C12 0.0384(11) 0.0481(11) 0.0598(12) 0.0038(9) -0.0040(9) 0.0124(9) C13 0.0294(8) 0.0344(8) 0.0258(7) 0.0027(6) -0.0003(6) -0.0014(6) C14 0.0424(10) 0.0354(9) 0.0339(8) 0.0028(7) -0.0034(7) 0.0008(8) C15 0.0431(11) 0.0453(10) 0.0431(10) 0.0128(8) -0.0034(8) 0.0037(8) C16 0.0535(13) 0.0679(13) 0.0296(9) 0.0107(8) -0.0019(8) 0.0074(10) C17 0.0821(17) 0.0619(13) 0.0282(9) -0.0061(8) -0.0001(10) 0.0080(12) C18 0.0616(13) 0.0402(9) 0.0309(8) -0.0017(7) 0.0018(8) 0.0042(9) C19 0.0270(8) 0.0278(7) 0.0291(7) 0.0019(6) -0.0013(6) 0.0006(6) C20 0.0346(9) 0.0396(9) 0.0301(7) 0.0016(7) 0.0013(7) -0.0060(7) C21 0.0357(10) 0.0427(9) 0.0419(9) 0.0036(8) 0.0012(8) -0.0097(8) C22 0.0342(10) 0.0383(9) 0.0483(10) -0.0082(7) -0.0061(8) -0.0031(7) C23 0.0363(9) 0.0427(9) 0.0339(8) -0.0087(7) -0.0037(7) 0.0033(7) C24 0.0325(9) 0.0364(8) 0.0306(8) 0.0002(6) 0.0015(6) -0.0008(7) C25 0.0385(10) 0.0483(11) 0.0494(10) -0.0069(8) 0.0069(8) 0.0020(8) C26 0.0306(9) 0.0379(9) 0.0378(8) 0.0066(7) -0.0045(7) 0.0006(7) C27 0.0428(11) 0.0367(9) 0.0579(12) 0.0054(8) 0.0029(9) 0.0097(8) C28 0.0435(11) 0.0375(9) 0.0402(9) -0.0081(7) 0.0007(8) 0.0010(8) C29 0.0587(14) 0.0559(13) 0.0641(14) -0.0195(11) -0.0083(11) -0.0059(11) Cr1 0.02672(13) 0.02712(12) 0.03161(13) -0.00016(9) 0.00115(10) 0.00192(10) N1 0.0317(8) 0.0486(8) 0.0300(7) 0.0051(6) 0.0043(6) 0.0040(7) N2 0.0279(7) 0.0269(6) 0.0302(6) 0.0009(5) 0.0022(5) 0.0006(5) N3 0.0378(8) 0.0338(7) 0.0384(7) -0.0040(6) 0.0032(6) 0.0024(6) O1 0.0475(10) 0.0982(14) 0.0879(13) -0.0151(11) 0.0292(9) -0.0014(9) O2 0.0488(9) 0.0660(9) 0.0515(8) 0.0068(7) -0.0212(7) -0.0085(7) O3 0.0889(14) 0.0469(9) 0.1097(15) 0.0315(9) 0.0078(12) 0.0217(9) P1 0.02642(19) 0.02639(18) 0.02574(17) 0.00159(14) 0.00085(15) -0.00090(15) P2 0.02730(19) 0.02613(17) 0.02450(17) 0.00046(13) 0.00071(15) -0.00087(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.459(2) . ? C1 C2 1.509(3) . ? C1 C3 1.511(3) . ? C4 C9 1.384(2) . ? C4 C5 1.394(2) . ? C4 P1 1.8306(17) . ? C5 C6 1.385(3) . ? C6 C7 1.373(4) . ? C7 C8 1.369(4) . ? C8 C9 1.391(3) . ? C10 N2 1.487(2) . ? C10 C12 1.520(3) . ? C10 C11 1.521(3) . ? C13 C18 1.385(2) . ? C13 C14 1.392(2) . ? C13 P2 1.8354(16) . ? C14 C15 1.385(2) . ? C15 C16 1.370(2) . ? C16 C17 1.368(2) . ? C17 C18 1.390(3) . ? C19 C24 1.389(2) . ? C19 C20 1.390(2) . ? C19 P2 1.8296(16) . ? C20 C21 1.384(2) . ? C21 C22 1.376(3) . ? C22 C23 1.377(3) . ? C23 C24 1.386(2) . ? C25 O1 1.154(3) . ? C25 Cr1 1.853(2) . ? C26 O2 1.159(2) . ? C26 Cr1 1.8187(18) . ? C27 O3 1.143(2) . ? C27 Cr1 1.8549(19) . ? C28 N3 1.138(2) . ? C28 C29 1.453(3) . ? Cr1 N3 2.0531(15) . ? Cr1 P2 2.3455(5) . ? Cr1 P1 2.3637(5) . ? N1 P1 1.6432(15) . ? N2 P2 1.6973(14) . ? N2 P1 1.7270(13) . ? P1 P2 2.6372(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 110.34(18) . . ? N1 C1 C3 110.92(18) . . ? C2 C1 C3 110.85(19) . . ? C9 C4 C5 118.25(17) . . ? C9 C4 P1 121.86(14) . . ? C5 C4 P1 119.59(13) . . ? C6 C5 C4 120.80(19) . . ? C7 C6 C5 120.1(2) . . ? C8 C7 C6 119.9(2) . . ? C7 C8 C9 120.5(2) . . ? C4 C9 C8 120.4(2) . . ? N2 C10 C12 113.90(14) . . ? N2 C10 C11 111.99(14) . . ? C12 C10 C11 109.73(17) . . ? C18 C13 C14 118.45(15) . . ? C18 C13 P2 117.82(13) . . ? C14 C13 P2 123.72(12) . . ? C15 C14 C13 120.44(17) . . ? C16 C15 C14 120.18(17) . . ? C17 C16 C15 120.32(17) . . ? C16 C17 C18 119.91(17) . . ? C13 C18 C17 120.66(18) . . ? C24 C19 C20 118.22(15) . . ? C24 C19 P2 120.29(12) . . ? C20 C19 P2 121.20(12) . . ? C21 C20 C19 120.73(15) . . ? C22 C21 C20 120.30(17) . . ? C21 C22 C23 119.73(17) . . ? C22 C23 C24 120.14(16) . . ? C23 C24 C19 120.79(16) . . ? O1 C25 Cr1 176.1(2) . . ? O2 C26 Cr1 176.38(17) . . ? O3 C27 Cr1 176.7(2) . . ? N3 C28 C29 176.8(2) . . ? C26 Cr1 C25 85.86(9) . . ? C26 Cr1 C27 86.58(9) . . ? C25 Cr1 C27 94.73(9) . . ? C26 Cr1 N3 174.41(7) . . ? C25 Cr1 N3 93.46(8) . . ? C27 Cr1 N3 87.95(8) . . ? C26 Cr1 P2 87.43(6) . . ? C25 Cr1 P2 100.13(7) . . ? C27 Cr1 P2 163.52(7) . . ? N3 Cr1 P2 98.15(4) . . ? C26 Cr1 P1 94.10(6) . . ? C25 Cr1 P1 168.22(7) . . ? C27 Cr1 P1 97.02(6) . . ? N3 Cr1 P1 87.70(4) . . ? P2 Cr1 P1 68.113(15) . . ? C1 N1 P1 127.28(14) . . ? C10 N2 P2 126.20(11) . . ? C10 N2 P1 133.03(11) . . ? P2 N2 P1 100.73(7) . . ? C28 N3 Cr1 169.33(15) . . ? N1 P1 N2 113.13(7) . . ? N1 P1 C4 101.54(8) . . ? N2 P1 C4 103.54(7) . . ? N1 P1 Cr1 121.54(6) . . ? N2 P1 Cr1 94.81(5) . . ? C4 P1 Cr1 121.07(5) . . ? N1 P1 P2 132.38(6) . . ? C4 P1 P2 120.15(6) . . ? Cr1 P1 P2 55.617(14) . . ? N2 P2 C19 105.41(7) . . ? N2 P2 C13 107.95(7) . . ? C19 P2 C13 101.25(7) . . ? N2 P2 Cr1 96.29(5) . . ? C19 P2 Cr1 117.90(5) . . ? C13 P2 Cr1 126.08(5) . . ? C19 P2 P1 123.01(5) . . ? C13 P2 P1 128.42(6) . . ? Cr1 P2 P1 56.270(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.17 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.432 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.051 # Attachment '- 6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 780225' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H67 N4 Ni P4' _chemical_formula_weight 918.68 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' Ni Ni 0.3393 1.1124 '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 10.8037(6) _cell_length_b 11.7151(6) _cell_length_c 21.2583(10) _cell_angle_alpha 89.596(4) _cell_angle_beta 87.817(4) _cell_angle_gamma 69.521(4) _cell_volume 2518.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3783 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.24 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 978 _exptl_absorpt_coefficient_mu 0.549 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30124 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.1029 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9886 _reflns_number_gt 5604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2005)' _computing_cell_refinement X-AREA _computing_data_reduction X-AREA _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0290P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9886 _refine_ls_number_parameters 547 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 0.783 _refine_ls_restrained_S_all 0.783 _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 C49A C 0.7467(10) 0.4707(9) 0.4494(4) 0.121(2) Uiso 0.535(5) 1 d PDU A 1 H49A H 0.6642 0.4696 0.4697 0.182 Uiso 0.535(5) 1 calc PR A 1 H49B H 0.7906 0.3938 0.4266 0.182 Uiso 0.535(5) 1 calc PR A 1 H49C H 0.7271 0.5387 0.4198 0.182 Uiso 0.535(5) 1 calc PR A 1 C50A C 0.8337(8) 0.4855(9) 0.4973(4) 0.1145(18) Uiso 0.535(5) 1 d PDU A 1 H50A H 0.8493 0.4178 0.5276 0.137 Uiso 0.535(5) 1 calc PR A 1 H50B H 0.7865 0.5622 0.5207 0.137 Uiso 0.535(5) 1 calc PR A 1 C51A C 0.9620(7) 0.4884(9) 0.4746(3) 0.1104(18) Uiso 0.535(5) 1 d PDU . 1 H51A H 1.0134 0.4093 0.4543 0.133 Uiso 0.535(5) 1 calc PR A 1 H51B H 0.9482 0.5528 0.4425 0.133 Uiso 0.535(5) 1 calc PR A 1 C49B C 0.7029(9) 0.5182(11) 0.4854(6) 0.125(2) Uiso 0.465(5) 1 d PDU A 2 H49D H 0.6396 0.5373 0.4516 0.188 Uiso 0.465(5) 1 calc PR A 2 H49E H 0.6681 0.5772 0.5198 0.188 Uiso 0.465(5) 1 calc PR A 2 H49F H 0.7166 0.4359 0.5009 0.188 Uiso 0.465(5) 1 calc PR A 2 C50B C 0.8288(8) 0.5245(10) 0.4610(5) 0.1130(18) Uiso 0.465(5) 1 d PDU A 2 H50C H 0.8614 0.4658 0.4256 0.136 Uiso 0.465(5) 1 calc PR A 2 H50D H 0.8123 0.6070 0.4437 0.136 Uiso 0.465(5) 1 calc PR A 2 C51B C 0.9333(4) 0.4992(11) 0.5063(5) 0.1116(19) Uiso 0.465(5) 1 d PDU . 2 H51C H 0.8956 0.5572 0.5416 0.134 Uiso 0.465(5) 1 calc PR A 2 H51D H 0.9451 0.4173 0.5232 0.134 Uiso 0.465(5) 1 calc PR A 2 C1 C 0.6853(3) -0.0734(2) 0.13606(12) 0.0339(6) Uani 1 1 d . . . C2 C 0.6036(3) -0.0019(3) 0.09153(12) 0.0444(7) Uani 1 1 d . . . H2A H 0.5142 0.0438 0.1031 0.053 Uiso 1 1 calc R . . C3 C 0.6497(3) 0.0043(3) 0.03067(13) 0.0589(9) Uani 1 1 d . . . H3A H 0.5923 0.0550 0.0010 0.071 Uiso 1 1 calc R . . C4 C 0.7776(3) -0.0621(3) 0.01273(14) 0.0599(9) Uani 1 1 d . . . H4A H 0.8092 -0.0585 -0.0293 0.072 Uiso 1 1 calc R . . C5 C 0.8591(3) -0.1335(3) 0.05607(14) 0.0591(9) Uani 1 1 d . . . H5A H 0.9480 -0.1799 0.0439 0.071 Uiso 1 1 calc R . . C6 C 0.8146(3) -0.1393(3) 0.11729(13) 0.0496(8) Uani 1 1 d . . . H6A H 0.8733 -0.1891 0.1468 0.060 Uiso 1 1 calc R . . C7 C 0.7623(3) -0.0996(3) 0.26038(12) 0.0369(7) Uani 1 1 d . . . C8 C 0.8304(3) -0.0191(3) 0.25070(13) 0.0495(8) Uani 1 1 d . . . H8A H 0.8018 0.0430 0.2200 0.059 Uiso 1 1 calc R . . C9 C 0.9393(3) -0.0291(4) 0.28534(16) 0.0675(10) Uani 1 1 d . . . H9A H 0.9854 0.0259 0.2781 0.081 Uiso 1 1 calc R . . C10 C 0.9810(3) -0.1173(4) 0.32980(16) 0.0686(11) Uani 1 1 d . . . H10A H 1.0566 -0.1241 0.3531 0.082 Uiso 1 1 calc R . . C11 C 0.9144(3) -0.1963(3) 0.34115(14) 0.0602(9) Uani 1 1 d . . . H11A H 0.9430 -0.2571 0.3726 0.072 Uiso 1 1 calc R . . C12 C 0.8050(3) -0.1871(3) 0.30646(12) 0.0452(7) Uani 1 1 d . . . H12A H 0.7588 -0.2417 0.3145 0.054 Uiso 1 1 calc R . . C13 C 0.3387(3) -0.2174(2) 0.18951(13) 0.0382(7) Uani 1 1 d . . . C14 C 0.2536(3) -0.2786(3) 0.20609(16) 0.0579(9) Uani 1 1 d . . . H14A H 0.2370 -0.2915 0.2493 0.069 Uiso 1 1 calc R . . C15 C 0.1920(4) -0.3217(3) 0.16029(19) 0.0743(11) Uani 1 1 d . . . H15A H 0.1353 -0.3649 0.1724 0.089 Uiso 1 1 calc R . . C16 C 0.2126(4) -0.3021(3) 0.09819(18) 0.0682(10) Uani 1 1 d . . . H16A H 0.1719 -0.3332 0.0671 0.082 Uiso 1 1 calc R . . C17 C 0.2922(3) -0.2377(3) 0.08066(15) 0.0638(9) Uani 1 1 d . . . H17A H 0.3047 -0.2219 0.0374 0.077 Uiso 1 1 calc R . . C18 C 0.3540(3) -0.1959(3) 0.12590(13) 0.0524(8) Uani 1 1 d . . . H18A H 0.4087 -0.1510 0.1132 0.063 Uiso 1 1 calc R . . C19 C 0.3751(3) -0.1692(3) 0.37448(13) 0.0514(8) Uani 1 1 d . . . H19A H 0.3098 -0.0843 0.3723 0.062 Uiso 1 1 calc R . . C20 C 0.3162(4) -0.2426(4) 0.41829(15) 0.0821(12) Uani 1 1 d . . . H20A H 0.2340 -0.2446 0.4012 0.123 Uiso 1 1 calc R . . H20B H 0.2976 -0.2043 0.4601 0.123 Uiso 1 1 calc R . . H20C H 0.3794 -0.3260 0.4216 0.123 Uiso 1 1 calc R . . C21 C 0.4992(3) -0.1633(4) 0.40092(16) 0.0726(11) Uani 1 1 d . . . H21A H 0.5358 -0.1153 0.3730 0.109 Uiso 1 1 calc R . . H21B H 0.5638 -0.2460 0.4044 0.109 Uiso 1 1 calc R . . H21C H 0.4792 -0.1249 0.4427 0.109 Uiso 1 1 calc R . . C22 C 0.6757(3) -0.3314(3) 0.20488(13) 0.0449(7) Uani 1 1 d . . . H22A H 0.7670 -0.3318 0.2113 0.054 Uiso 1 1 calc R . . C23 C 0.6697(3) -0.3646(3) 0.13571(15) 0.0603(9) Uani 1 1 d . . . H23A H 0.6831 -0.3016 0.1086 0.090 Uiso 1 1 calc R . . H23B H 0.5830 -0.3703 0.1283 0.090 Uiso 1 1 calc R . . H23C H 0.7391 -0.4432 0.1260 0.090 Uiso 1 1 calc R . . C24 C 0.6554(3) -0.4287(3) 0.24743(15) 0.0562(8) Uani 1 1 d . . . H24A H 0.6583 -0.4063 0.2915 0.084 Uiso 1 1 calc R . . H24B H 0.7256 -0.5071 0.2383 0.084 Uiso 1 1 calc R . . H24C H 0.5693 -0.4354 0.2399 0.084 Uiso 1 1 calc R . . C25 C 0.3549(3) 0.2815(2) 0.14395(12) 0.0382(7) Uani 1 1 d . . . C26 C 0.3443(3) 0.2881(3) 0.07944(13) 0.0542(8) Uani 1 1 d . . . H26A H 0.2857 0.2560 0.0599 0.065 Uiso 1 1 calc R . . C27 C 0.4186(4) 0.3414(3) 0.04270(14) 0.0664(10) Uani 1 1 d D . . H27A H 0.4105 0.3452 -0.0017 0.080 Uiso 1 1 calc R . . C28 C 0.5029(4) 0.3879(3) 0.06997(13) 0.0657(10) Uani 1 1 d D . . H28A H 0.5525 0.4251 0.0448 0.079 Uiso 1 1 calc R . . C29 C 0.5156(4) 0.3809(3) 0.13354(14) 0.0641(9) Uani 1 1 d D . . H29A H 0.5751 0.4125 0.1525 0.077 Uiso 1 1 calc R . . C30 C 0.4429(3) 0.3285(3) 0.17039(14) 0.0518(8) Uani 1 1 d . . . H30A H 0.4530 0.3244 0.2146 0.062 Uiso 1 1 calc R . . C31 C 0.1322(3) 0.2039(3) 0.15682(12) 0.0421(7) Uani 1 1 d . . . C32 C 0.0523(3) 0.3050(3) 0.12535(15) 0.0646(10) Uani 1 1 d . . . H32A H 0.0744 0.3767 0.1233 0.078 Uiso 1 1 calc R . . C33 C -0.0607(4) 0.3024(4) 0.09657(17) 0.0854(13) Uani 1 1 d . . . H33A H -0.1161 0.3727 0.0758 0.102 Uiso 1 1 calc R . . C34 C -0.0921(4) 0.1979(5) 0.09820(18) 0.0828(13) Uani 1 1 d . . . H34A H -0.1687 0.1961 0.0784 0.099 Uiso 1 1 calc R . . C35 C -0.0125(4) 0.0973(4) 0.12834(16) 0.0730(11) Uani 1 1 d . . . H35A H -0.0337 0.0251 0.1290 0.088 Uiso 1 1 calc R . . C36 C 0.0981(3) 0.0992(3) 0.15774(13) 0.0518(8) Uani 1 1 d . . . H36A H 0.1519 0.0285 0.1789 0.062 Uiso 1 1 calc R . . C37 C 0.2276(3) 0.1717(2) 0.38184(12) 0.0381(7) Uani 1 1 d . . . C38 C 0.1056(3) 0.1627(3) 0.37011(14) 0.0519(8) Uani 1 1 d . . . H38A H 0.0755 0.1702 0.3283 0.062 Uiso 1 1 calc R . . C39 C 0.0279(3) 0.1429(3) 0.41929(17) 0.0655(10) Uani 1 1 d . . . H39A H -0.0556 0.1374 0.4109 0.079 Uiso 1 1 calc R . . C40 C 0.0695(4) 0.1313(3) 0.47954(16) 0.0700(10) Uani 1 1 d . . . H40A H 0.0149 0.1183 0.5129 0.084 Uiso 1 1 calc R . . C41 C 0.1902(4) 0.1382(3) 0.49187(14) 0.0637(10) Uani 1 1 d . . . H41A H 0.2196 0.1300 0.5338 0.076 Uiso 1 1 calc R . . C42 C 0.2688(3) 0.1573(3) 0.44344(13) 0.0493(8) Uani 1 1 d . . . H42A H 0.3530 0.1607 0.4523 0.059 Uiso 1 1 calc R . . C43 C 0.5780(3) 0.1969(3) 0.34258(14) 0.0487(8) Uani 1 1 d . . . H43A H 0.6043 0.1426 0.3046 0.058 Uiso 1 1 calc R . . C44 C 0.6266(4) 0.3019(4) 0.3313(2) 0.0980(15) Uani 1 1 d . . . H44A H 0.5837 0.3484 0.2948 0.147 Uiso 1 1 calc R . . H44B H 0.7226 0.2703 0.3233 0.147 Uiso 1 1 calc R . . H44C H 0.6051 0.3552 0.3685 0.147 Uiso 1 1 calc R . . C45 C 0.6426(3) 0.1232(3) 0.39812(16) 0.0751(11) Uani 1 1 d . . . H45A H 0.6105 0.0552 0.4042 0.113 Uiso 1 1 calc R . . H45B H 0.6207 0.1749 0.4359 0.113 Uiso 1 1 calc R . . H45C H 0.7387 0.0914 0.3905 0.113 Uiso 1 1 calc R . . C46 C 0.1536(3) 0.4064(3) 0.26729(14) 0.0521(8) Uani 1 1 d . . . H46A H 0.1572 0.4415 0.2245 0.063 Uiso 1 1 calc R . . C47 C 0.2036(4) 0.4783(3) 0.31220(15) 0.0663(10) Uani 1 1 d . . . H47A H 0.2961 0.4667 0.3009 0.099 Uiso 1 1 calc R . . H47B H 0.1974 0.4498 0.3553 0.099 Uiso 1 1 calc R . . H47C H 0.1499 0.5649 0.3096 0.099 Uiso 1 1 calc R . . C48 C 0.0088(3) 0.4253(3) 0.28269(18) 0.0750(11) Uani 1 1 d . . . H48A H -0.0224 0.3794 0.2526 0.112 Uiso 1 1 calc R . . H48B H -0.0441 0.5122 0.2799 0.112 Uiso 1 1 calc R . . H48C H -0.0003 0.3966 0.3254 0.112 Uiso 1 1 calc R . . N1 N 0.5830(2) -0.20832(19) 0.22185(10) 0.0344(5) Uani 1 1 d . . . N2 N 0.3940(3) -0.2229(2) 0.31167(11) 0.0482(7) Uani 1 1 d . . . H2 H 0.417(3) -0.306(3) 0.3139(15) 0.075(11) Uiso 1 1 d . . . N3 N 0.2390(2) 0.27615(19) 0.26317(9) 0.0369(6) Uani 1 1 d . . . N4 N 0.4343(3) 0.2390(2) 0.35009(12) 0.0459(6) Uani 1 1 d . . . H4 H 0.403(3) 0.294(3) 0.3796(13) 0.050(9) Uiso 1 1 d . . . P1 P 0.61323(7) -0.07473(6) 0.21571(3) 0.03135(17) Uani 1 1 d . . . P2 P 0.41818(7) -0.15166(6) 0.24634(3) 0.03385(17) Uani 1 1 d . . . P3 P 0.28505(7) 0.19137(6) 0.19565(3) 0.03414(17) Uani 1 1 d . . . P4 P 0.33914(7) 0.17490(6) 0.31510(3) 0.03407(17) Uani 1 1 d . . . Ni1 Ni 0.41281(3) 0.03414(3) 0.244229(15) 0.02993(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0351(16) 0.0361(16) 0.0330(14) -0.0047(12) 0.0016(12) -0.0158(14) C2 0.0433(18) 0.0499(19) 0.0359(16) 0.0000(14) 0.0012(14) -0.0114(15) C3 0.061(2) 0.080(3) 0.0349(17) 0.0113(16) -0.0022(16) -0.024(2) C4 0.063(2) 0.085(3) 0.0352(17) -0.0091(18) 0.0139(17) -0.033(2) C5 0.0428(19) 0.084(3) 0.0468(19) -0.0129(18) 0.0111(16) -0.0185(19) C6 0.0411(18) 0.062(2) 0.0436(17) -0.0034(15) 0.0001(14) -0.0150(16) C7 0.0331(16) 0.0460(18) 0.0298(14) -0.0067(13) 0.0020(12) -0.0117(14) C8 0.0492(19) 0.070(2) 0.0392(16) -0.0007(15) -0.0017(14) -0.0326(18) C9 0.058(2) 0.109(3) 0.052(2) -0.012(2) 0.0008(18) -0.050(2) C10 0.038(2) 0.109(3) 0.053(2) -0.017(2) -0.0126(17) -0.017(2) C11 0.050(2) 0.068(2) 0.0426(18) -0.0061(17) -0.0105(16) 0.0049(19) C12 0.0412(18) 0.0474(19) 0.0386(16) -0.0068(14) -0.0044(14) -0.0046(15) C13 0.0379(16) 0.0324(16) 0.0461(16) -0.0035(13) -0.0007(13) -0.0147(14) C14 0.062(2) 0.059(2) 0.060(2) 0.0090(17) -0.0077(17) -0.0304(19) C15 0.075(3) 0.073(3) 0.098(3) 0.015(2) -0.028(2) -0.053(2) C16 0.070(3) 0.060(2) 0.080(3) -0.006(2) -0.033(2) -0.026(2) C17 0.068(2) 0.081(3) 0.0480(19) -0.0052(18) -0.0122(17) -0.031(2) C18 0.059(2) 0.066(2) 0.0441(18) -0.0008(16) -0.0055(16) -0.0366(19) C19 0.060(2) 0.052(2) 0.0386(16) 0.0072(15) -0.0003(15) -0.0156(17) C20 0.075(3) 0.137(4) 0.051(2) 0.029(2) -0.0012(19) -0.059(3) C21 0.075(3) 0.095(3) 0.055(2) 0.000(2) -0.0015(19) -0.040(2) C22 0.0419(18) 0.0328(17) 0.0562(18) -0.0039(14) -0.0055(15) -0.0078(15) C23 0.068(2) 0.0407(19) 0.066(2) -0.0149(16) -0.0008(18) -0.0108(18) C24 0.057(2) 0.0346(18) 0.072(2) 0.0077(16) -0.0103(18) -0.0093(16) C25 0.0505(18) 0.0294(15) 0.0307(14) 0.0013(12) -0.0032(13) -0.0089(14) C26 0.075(2) 0.054(2) 0.0424(17) 0.0055(15) -0.0106(16) -0.0326(19) C27 0.101(3) 0.070(2) 0.0364(17) 0.0118(17) -0.0018(19) -0.041(2) C28 0.091(3) 0.062(2) 0.056(2) 0.0103(18) 0.006(2) -0.042(2) C29 0.083(3) 0.067(2) 0.057(2) -0.0038(18) 0.0045(19) -0.046(2) C30 0.067(2) 0.058(2) 0.0391(16) 0.0003(15) -0.0001(16) -0.0325(19) C31 0.0375(17) 0.0503(19) 0.0324(15) -0.0034(14) -0.0041(13) -0.0071(15) C32 0.060(2) 0.056(2) 0.065(2) -0.0095(18) -0.0198(19) -0.0014(18) C33 0.055(2) 0.101(3) 0.069(3) -0.021(2) -0.027(2) 0.014(2) C34 0.040(2) 0.138(4) 0.066(3) -0.026(3) -0.0049(19) -0.025(3) C35 0.058(2) 0.123(4) 0.057(2) -0.002(2) 0.0011(19) -0.055(3) C36 0.0462(19) 0.077(2) 0.0386(16) 0.0047(16) -0.0013(14) -0.0304(18) C37 0.0402(17) 0.0358(16) 0.0333(14) -0.0048(12) 0.0018(13) -0.0074(14) C38 0.053(2) 0.061(2) 0.0448(17) -0.0089(16) 0.0049(15) -0.0246(18) C39 0.055(2) 0.082(3) 0.069(2) -0.013(2) 0.0163(19) -0.038(2) C40 0.076(3) 0.087(3) 0.051(2) -0.0048(19) 0.0269(19) -0.036(2) C41 0.073(3) 0.076(3) 0.0341(17) 0.0029(16) 0.0072(17) -0.017(2) C42 0.0511(19) 0.056(2) 0.0366(16) -0.0006(14) 0.0004(14) -0.0142(17) C43 0.051(2) 0.057(2) 0.0451(17) -0.0029(15) -0.0063(15) -0.0279(17) C44 0.101(3) 0.111(4) 0.117(3) 0.037(3) -0.035(3) -0.078(3) C45 0.060(2) 0.089(3) 0.076(2) 0.020(2) -0.017(2) -0.024(2) C46 0.064(2) 0.0363(19) 0.0424(17) -0.0036(14) 0.0001(16) -0.0007(17) C47 0.084(3) 0.0384(19) 0.062(2) -0.0093(17) -0.0024(19) -0.0030(19) C48 0.050(2) 0.068(3) 0.085(3) -0.014(2) -0.002(2) 0.0076(19) N1 0.0367(13) 0.0272(13) 0.0387(13) -0.0011(10) -0.0037(10) -0.0102(11) N2 0.0701(19) 0.0389(16) 0.0390(14) 0.0075(12) 0.0022(13) -0.0238(15) N3 0.0397(14) 0.0309(13) 0.0324(12) -0.0010(10) -0.0021(10) -0.0025(11) N4 0.0471(16) 0.0477(16) 0.0440(15) -0.0121(13) -0.0037(13) -0.0176(14) P1 0.0338(4) 0.0319(4) 0.0287(4) 0.0004(3) -0.0025(3) -0.0118(4) P2 0.0391(4) 0.0324(4) 0.0317(4) 0.0023(3) -0.0014(3) -0.0146(4) P3 0.0372(4) 0.0325(4) 0.0303(4) -0.0005(3) -0.0034(3) -0.0089(4) P4 0.0382(4) 0.0332(4) 0.0295(4) -0.0018(3) -0.0022(3) -0.0108(4) Ni1 0.0329(2) 0.0285(2) 0.02819(18) 0.00017(15) -0.00124(15) -0.01046(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 C49A C50A 1.462(4) . ? C50A C51A 1.462(4) . ? C51A C51A 1.462(4) 2_766 ? C49B C50B 1.463(4) . ? C50B C51B 1.462(4) . ? C51B C51B 1.462(4) 2_766 ? C1 C2 1.382(4) . ? C1 C6 1.384(4) . ? C1 P1 1.839(3) . ? C2 C3 1.379(4) . ? C3 C4 1.368(4) . ? C4 C5 1.363(4) . ? C5 C6 1.380(4) . ? C7 C12 1.383(4) . ? C7 C8 1.395(4) . ? C7 P1 1.834(3) . ? C8 C9 1.381(4) . ? C9 C10 1.363(5) . ? C10 C11 1.372(5) . ? C11 C12 1.389(4) . ? C13 C14 1.385(4) . ? C13 C18 1.388(4) . ? C13 P2 1.829(3) . ? C14 C15 1.391(4) . ? C15 C16 1.362(5) . ? C16 C17 1.368(5) . ? C17 C18 1.377(4) . ? C19 N2 1.457(4) . ? C19 C21 1.497(4) . ? C19 C20 1.529(4) . ? C22 N1 1.477(3) . ? C22 C24 1.520(4) . ? C22 C23 1.533(4) . ? C25 C26 1.380(4) . ? C25 C30 1.392(4) . ? C25 P3 1.835(3) . ? C26 C27 1.393(4) . ? C27 C28 1.361(3) . ? C28 C29 1.363(3) . ? C29 C30 1.374(4) . ? C31 C32 1.383(4) . ? C31 C36 1.400(4) . ? C31 P3 1.833(3) . ? C32 C33 1.396(5) . ? C33 C34 1.379(5) . ? C34 C35 1.365(5) . ? C35 C36 1.377(4) . ? C37 C42 1.389(4) . ? C37 C38 1.391(4) . ? C37 P4 1.835(3) . ? C38 C39 1.385(4) . ? C39 C40 1.364(4) . ? C40 C41 1.370(4) . ? C41 C42 1.376(4) . ? C43 N4 1.458(4) . ? C43 C45 1.501(4) . ? C43 C44 1.512(4) . ? C46 N3 1.482(3) . ? C46 C47 1.511(4) . ? C46 C48 1.524(4) . ? N1 P1 1.710(2) . ? N1 P2 1.729(2) . ? N2 P2 1.674(2) . ? N3 P3 1.707(2) . ? N3 P4 1.723(2) . ? N4 P4 1.668(2) . ? P1 Ni1 2.1590(8) . ? P1 P2 2.6255(10) . ? P2 Ni1 2.1573(8) . ? P3 Ni1 2.1603(8) . ? P3 P4 2.6180(9) . ? P4 Ni1 2.1558(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C49A C50A C51A 116.4(7) . . ? C51A C51A C50A 112.3(8) 2_766 . ? C51B C50B C49B 115.8(8) . . ? C51B C51B C50B 126.2(11) 2_766 . ? C2 C1 C6 117.7(3) . . ? C2 C1 P1 117.4(2) . . ? C6 C1 P1 124.9(2) . . ? C3 C2 C1 121.2(3) . . ? C4 C3 C2 120.4(3) . . ? C5 C4 C3 119.0(3) . . ? C4 C5 C6 121.1(3) . . ? C5 C6 C1 120.6(3) . . ? C12 C7 C8 118.1(3) . . ? C12 C7 P1 123.9(2) . . ? C8 C7 P1 117.8(2) . . ? C9 C8 C7 120.5(3) . . ? C10 C9 C8 120.4(3) . . ? C9 C10 C11 120.4(3) . . ? C10 C11 C12 119.7(3) . . ? C7 C12 C11 120.9(3) . . ? C14 C13 C18 117.1(3) . . ? C14 C13 P2 123.9(2) . . ? C18 C13 P2 118.7(2) . . ? C13 C14 C15 120.9(3) . . ? C16 C15 C14 120.3(3) . . ? C15 C16 C17 120.0(3) . . ? C16 C17 C18 119.7(3) . . ? C17 C18 C13 121.9(3) . . ? N2 C19 C21 113.7(3) . . ? N2 C19 C20 108.6(3) . . ? C21 C19 C20 109.8(2) . . ? N1 C22 C24 112.0(2) . . ? N1 C22 C23 113.0(2) . . ? C24 C22 C23 110.0(2) . . ? C26 C25 C30 117.6(3) . . ? C26 C25 P3 124.5(2) . . ? C30 C25 P3 116.88(19) . . ? C25 C26 C27 120.6(3) . . ? C28 C27 C26 120.4(3) . . ? C27 C28 C29 119.7(3) . . ? C28 C29 C30 120.6(3) . . ? C29 C30 C25 121.1(3) . . ? C32 C31 C36 118.2(3) . . ? C32 C31 P3 125.9(3) . . ? C36 C31 P3 115.9(2) . . ? C31 C32 C33 120.4(4) . . ? C34 C33 C32 120.2(4) . . ? C35 C34 C33 119.7(4) . . ? C34 C35 C36 120.7(4) . . ? C35 C36 C31 120.8(3) . . ? C42 C37 C38 117.9(3) . . ? C42 C37 P4 122.1(2) . . ? C38 C37 P4 119.1(2) . . ? C39 C38 C37 120.0(3) . . ? C40 C39 C38 121.0(3) . . ? C39 C40 C41 119.8(3) . . ? C40 C41 C42 119.9(3) . . ? C41 C42 C37 121.4(3) . . ? N4 C43 C45 111.3(3) . . ? N4 C43 C44 111.4(3) . . ? C45 C43 C44 110.8(3) . . ? N3 C46 C47 112.7(2) . . ? N3 C46 C48 113.2(3) . . ? C47 C46 C48 110.6(3) . . ? C22 N1 P1 126.73(18) . . ? C22 N1 P2 133.56(18) . . ? P1 N1 P2 99.54(11) . . ? C19 N2 P2 123.9(2) . . ? C46 N3 P3 125.73(18) . . ? C46 N3 P4 134.01(18) . . ? P3 N3 P4 99.49(11) . . ? C43 N4 P4 124.3(2) . . ? N1 P1 C7 104.94(12) . . ? N1 P1 C1 106.34(11) . . ? C7 P1 C1 98.55(12) . . ? N1 P1 Ni1 93.00(8) . . ? C7 P1 Ni1 126.90(9) . . ? C1 P1 Ni1 123.90(9) . . ? C7 P1 P2 126.26(9) . . ? C1 P1 P2 126.16(8) . . ? Ni1 P1 P2 52.51(2) . . ? N2 P2 N1 110.18(12) . . ? N2 P2 C13 99.85(13) . . ? N1 P2 C13 103.27(11) . . ? N2 P2 Ni1 124.14(10) . . ? N1 P2 Ni1 92.53(8) . . ? C13 P2 Ni1 124.31(9) . . ? N2 P2 P1 129.15(10) . . ? C13 P2 P1 123.28(9) . . ? Ni1 P2 P1 52.56(2) . . ? N3 P3 C31 106.64(12) . . ? N3 P3 C25 104.05(11) . . ? C31 P3 C25 102.28(13) . . ? N3 P3 Ni1 92.93(8) . . ? C31 P3 Ni1 126.64(10) . . ? C25 P3 Ni1 120.64(9) . . ? C31 P3 P4 130.58(9) . . ? C25 P3 P4 118.87(9) . . ? Ni1 P3 P4 52.58(2) . . ? N4 P4 N3 109.79(12) . . ? N4 P4 C37 99.66(13) . . ? N3 P4 C37 104.45(12) . . ? N4 P4 Ni1 123.38(10) . . ? N3 P4 Ni1 92.63(8) . . ? C37 P4 Ni1 124.73(9) . . ? N4 P4 P3 125.85(9) . . ? C37 P4 P3 127.02(9) . . ? Ni1 P4 P3 52.74(2) . . ? P4 Ni1 P2 129.35(3) . . ? P4 Ni1 P1 130.35(3) . . ? P2 Ni1 P1 74.93(3) . . ? P4 Ni1 P3 74.68(3) . . ? P2 Ni1 P3 130.64(3) . . ? P1 Ni1 P3 126.17(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.382 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.045 # Attachment '- 7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 780226' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H32 Cl4 N2 Ni P2' _chemical_formula_weight 622.98 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' Ni Ni 0.3393 1.1124 '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 8.5768(2) _cell_length_b 18.4703(5) _cell_length_c 18.9358(5) _cell_angle_alpha 97.413(2) _cell_angle_beta 91.558(2) _cell_angle_gamma 96.707(2) _cell_volume 2951.58(13) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9128 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 29.62 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6400 _exptl_absorpt_correction_T_max 0.7753 _exptl_absorpt_process_details 'X-SHAPE and X-RED32 (Stoe & Cie, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49081 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13536 _reflns_number_gt 9487 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2005)' _computing_cell_refinement X-AREA _computing_data_reduction X-AREA _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0425P)^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 13536 _refine_ls_number_parameters 589 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 0.867 _refine_ls_restrained_S_all 0.891 _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 C49 C 0.1998(4) 0.84543(17) 0.1192(2) 0.0829(12) Uani 1 1 d D . . H49A H 0.2034 0.8635 0.1708 0.099 Uiso 0.701(7) 1 calc PR A 1 H49B H 0.0938 0.8191 0.1057 0.099 Uiso 0.701(7) 1 calc PR A 1 H49C H 0.1013 0.8159 0.1297 0.099 Uiso 0.299(7) 1 calc PR A 2 H49D H 0.2353 0.8790 0.1632 0.099 Uiso 0.299(7) 1 calc PR A 2 C50 C 0.7514(5) 0.34589(17) 0.12288(18) 0.0753(11) Uani 1 1 d D . . H50A H 0.7971 0.3720 0.1691 0.090 Uiso 0.534(12) 1 calc PR B 1 H50B H 0.6434 0.3241 0.1310 0.090 Uiso 0.534(12) 1 calc PR B 1 H50C H 0.6569 0.3258 0.1462 0.090 Uiso 0.466(12) 1 calc PR B 2 H50D H 0.8143 0.3827 0.1583 0.090 Uiso 0.466(12) 1 calc PR B 2 Cl5 Cl 0.34066(12) 0.78553(6) 0.10141(5) 0.0801(3) Uani 1 1 d D A . Cl7 Cl 0.86221(13) 0.27502(6) 0.09510(6) 0.0878(3) Uani 1 1 d D B . Cl6A Cl 0.2365(5) 0.92127(16) 0.07004(15) 0.1272(11) Uiso 0.701(7) 1 d PD A 1 Cl6B Cl 0.1559(8) 0.8979(3) 0.0557(2) 0.097(2) Uiso 0.299(7) 1 d PD A 2 Cl8A Cl 0.7405(6) 0.4106(3) 0.0628(2) 0.0938(11) Uiso 0.534(12) 1 d PD B 1 Cl8B Cl 0.6947(5) 0.3879(3) 0.05165(15) 0.0756(12) Uiso 0.466(12) 1 d PD B 2 C1 C 0.30058(18) 0.18483(7) 0.32769(7) 0.0269(5) Uani 1 1 d G . . C2 C 0.2454(2) 0.16649(8) 0.39221(8) 0.0428(6) Uani 1 1 d G . . H2 H 0.2476 0.1180 0.4035 0.051 Uiso 1 1 calc R . . C3 C 0.1870(2) 0.21914(10) 0.44017(7) 0.0543(8) Uani 1 1 d G . . H3 H 0.1493 0.2066 0.4843 0.065 Uiso 1 1 calc R . . C4 C 0.1837(2) 0.29012(9) 0.42362(9) 0.0540(8) Uani 1 1 d G . . H4 H 0.1438 0.3261 0.4564 0.065 Uiso 1 1 calc R . . C5 C 0.2389(2) 0.30846(7) 0.35910(10) 0.0538(8) Uani 1 1 d G . . H5 H 0.2367 0.3570 0.3478 0.065 Uiso 1 1 calc R . . C6 C 0.2973(2) 0.25582(8) 0.31114(7) 0.0386(6) Uani 1 1 d G . . H6 H 0.3350 0.2683 0.2670 0.046 Uiso 1 1 calc R . . C7 C 0.35882(17) 0.14104(10) 0.18177(7) 0.0299(5) Uani 1 1 d G . . C8 C 0.20392(16) 0.13893(12) 0.15724(9) 0.0525(8) Uani 1 1 d G . . H8 H 0.1204 0.1283 0.1877 0.063 Uiso 1 1 calc R . . C9 C 0.17117(19) 0.15235(13) 0.08814(10) 0.0695(11) Uani 1 1 d G . . H9 H 0.0653 0.1509 0.0714 0.083 Uiso 1 1 calc R . . C10 C 0.2933(3) 0.16788(13) 0.04358(7) 0.0681(10) Uani 1 1 d G . . H10 H 0.2709 0.1770 -0.0036 0.082 Uiso 1 1 calc R . . C11 C 0.4482(2) 0.16998(13) 0.06812(8) 0.0694(10) Uani 1 1 d G . . H11 H 0.5317 0.1806 0.0377 0.083 Uiso 1 1 calc R . . C12 C 0.48097(15) 0.15656(12) 0.13721(9) 0.0486(7) Uani 1 1 d G . . H12 H 0.5868 0.1580 0.1540 0.058 Uiso 1 1 calc R . . C13 C 0.6990(3) 0.19870(13) 0.30021(13) 0.0309(5) Uani 1 1 d . . . H13A H 0.6547 0.2337 0.2713 0.037 Uiso 1 1 calc R . . C14 C 0.7184(3) 0.23561(14) 0.37643(14) 0.0419(6) Uani 1 1 d . . . H14A H 0.6154 0.2450 0.3942 0.063 Uiso 1 1 calc R . . H14B H 0.7867 0.2823 0.3786 0.063 Uiso 1 1 calc R . . H14C H 0.7658 0.2035 0.4060 0.063 Uiso 1 1 calc R . . C15 C 0.8570(3) 0.18400(17) 0.27031(17) 0.0498(7) Uani 1 1 d . . . H15A H 0.8412 0.1607 0.2207 0.075 Uiso 1 1 calc R . . H15B H 0.9057 0.1512 0.2987 0.075 Uiso 1 1 calc R . . H15C H 0.9256 0.2306 0.2723 0.075 Uiso 1 1 calc R . . C16 C 0.6866(3) -0.03985(15) 0.17479(13) 0.0389(6) Uani 1 1 d . . . H16A H 0.5705 -0.0435 0.1653 0.047 Uiso 1 1 calc R . . C17 C 0.7313(4) -0.11675(16) 0.17520(17) 0.0542(8) Uani 1 1 d . . . H17A H 0.6756 -0.1400 0.2125 0.081 Uiso 1 1 calc R . . H17B H 0.8449 -0.1141 0.1847 0.081 Uiso 1 1 calc R . . H17C H 0.7025 -0.1459 0.1287 0.081 Uiso 1 1 calc R . . C18 C 0.7688(4) -0.0012(2) 0.11703(16) 0.0654(9) Uani 1 1 d . . . H18A H 0.7335 0.0474 0.1169 0.098 Uiso 1 1 calc R . . H18B H 0.7428 -0.0306 0.0704 0.098 Uiso 1 1 calc R . . H18C H 0.8827 0.0045 0.1266 0.098 Uiso 1 1 calc R . . C19 C 0.6757(2) 0.03343(12) 0.38691(11) 0.0255(4) Uani 1 1 d . . . C20 C 0.7706(3) -0.02021(14) 0.39978(13) 0.0344(5) Uani 1 1 d . . . H20A H 0.8068 -0.0510 0.3611 0.041 Uiso 1 1 calc R . . C21 C 0.8117(3) -0.02844(16) 0.46904(14) 0.0442(6) Uani 1 1 d . . . H21A H 0.8779 -0.0644 0.4778 0.053 Uiso 1 1 calc R . . C22 C 0.7579(3) 0.01501(15) 0.52549(13) 0.0424(6) Uani 1 1 d . . . H22A H 0.7885 0.0095 0.5729 0.051 Uiso 1 1 calc R . . C23 C 0.6599(3) 0.06633(14) 0.51355(13) 0.0378(6) Uani 1 1 d . . . H23A H 0.6208 0.0954 0.5527 0.045 Uiso 1 1 calc R . . C24 C 0.6183(3) 0.07562(13) 0.44445(12) 0.0315(5) Uani 1 1 d . . . H24A H 0.5502 0.1110 0.4363 0.038 Uiso 1 1 calc R . . C25 C 0.8885(2) 0.67671(12) 0.32480(12) 0.0265(5) Uani 1 1 d . . . C26 C 0.9586(2) 0.64874(14) 0.38085(12) 0.0308(5) Uani 1 1 d . . . H26A H 0.9344 0.5984 0.3868 0.037 Uiso 1 1 calc R . . C27 C 1.0642(3) 0.69489(16) 0.42806(13) 0.0395(6) Uani 1 1 d . . . H27A H 1.1132 0.6761 0.4662 0.047 Uiso 1 1 calc R . . C28 C 1.0979(3) 0.76760(16) 0.41973(14) 0.0427(6) Uani 1 1 d . . . H28A H 1.1692 0.7989 0.4527 0.051 Uiso 1 1 calc R . . C29 C 1.0301(3) 0.79580(14) 0.36433(15) 0.0419(6) Uani 1 1 d . . . H29A H 1.0549 0.8463 0.3591 0.050 Uiso 1 1 calc R . . C30 C 0.9250(3) 0.75029(13) 0.31592(13) 0.0334(5) Uani 1 1 d . . . H30A H 0.8787 0.7693 0.2772 0.040 Uiso 1 1 calc R . . C31 C 0.7804(2) 0.64102(13) 0.17832(12) 0.0282(5) Uani 1 1 d . . . C32 C 0.9315(3) 0.64279(16) 0.15340(14) 0.0421(6) Uani 1 1 d . . . H32A H 1.0162 0.6351 0.1839 0.051 Uiso 1 1 calc R . . C33 C 0.9585(3) 0.65569(18) 0.08473(15) 0.0518(7) Uani 1 1 d . . . H33A H 1.0617 0.6560 0.0677 0.062 Uiso 1 1 calc R . . C34 C 0.8376(3) 0.66811(18) 0.04039(15) 0.0523(7) Uani 1 1 d . . . H34A H 0.8577 0.6776 -0.0068 0.063 Uiso 1 1 calc R . . C35 C 0.6876(3) 0.66672(19) 0.06442(14) 0.0518(7) Uani 1 1 d . . . H35A H 0.6041 0.6756 0.0339 0.062 Uiso 1 1 calc R . . C36 C 0.6584(3) 0.65237(15) 0.13295(13) 0.0397(6) Uani 1 1 d . . . H36A H 0.5543 0.6503 0.1491 0.048 Uiso 1 1 calc R . . C37 C 0.4944(2) 0.70488(12) 0.29591(12) 0.0268(5) Uani 1 1 d . . . H37A H 0.5530 0.7371 0.2645 0.032 Uiso 1 1 calc R . . C38 C 0.5159(3) 0.74382(14) 0.37146(13) 0.0379(6) Uani 1 1 d . . . H38A H 0.6277 0.7507 0.3861 0.057 Uiso 1 1 calc R . . H38B H 0.4569 0.7141 0.4034 0.057 Uiso 1 1 calc R . . H38C H 0.4771 0.7919 0.3738 0.057 Uiso 1 1 calc R . . C39 C 0.3230(3) 0.69264(13) 0.26973(14) 0.0349(5) Uani 1 1 d . . . H39A H 0.3144 0.6672 0.2208 0.052 Uiso 1 1 calc R . . H39B H 0.2825 0.7402 0.2708 0.052 Uiso 1 1 calc R . . H39C H 0.2617 0.6627 0.3007 0.052 Uiso 1 1 calc R . . C40 C 0.3637(3) 0.47433(14) 0.16562(12) 0.0326(5) Uani 1 1 d . . . H40A H 0.4785 0.4790 0.1565 0.039 Uiso 1 1 calc R . . C41 C 0.3033(3) 0.39339(15) 0.16042(15) 0.0485(7) Uani 1 1 d . . . H41A H 0.3592 0.3711 0.1963 0.073 Uiso 1 1 calc R . . H41B H 0.3209 0.3689 0.1128 0.073 Uiso 1 1 calc R . . H41C H 0.1905 0.3878 0.1689 0.073 Uiso 1 1 calc R . . C42 C 0.2807(4) 0.51093(18) 0.11035(14) 0.0520(7) Uani 1 1 d . . . H42A H 0.3237 0.5629 0.1141 0.078 Uiso 1 1 calc R . . H42B H 0.1680 0.5071 0.1188 0.078 Uiso 1 1 calc R . . H42C H 0.2969 0.4863 0.0625 0.078 Uiso 1 1 calc R . . C43 C 0.4011(2) 0.54625(11) 0.38092(11) 0.0227(4) Uani 1 1 d . . . C44 C 0.4858(3) 0.58473(13) 0.44116(12) 0.0306(5) Uani 1 1 d . . . H44A H 0.5860 0.6110 0.4361 0.037 Uiso 1 1 calc R . . C45 C 0.4249(3) 0.58489(14) 0.50802(12) 0.0368(6) Uani 1 1 d . . . H45A H 0.4828 0.6115 0.5485 0.044 Uiso 1 1 calc R . . C46 C 0.2803(3) 0.54649(15) 0.51597(13) 0.0376(6) Uani 1 1 d . . . H46A H 0.2379 0.5470 0.5619 0.045 Uiso 1 1 calc R . . C47 C 0.1969(3) 0.50717(14) 0.45709(13) 0.0367(6) Uani 1 1 d . . . H47A H 0.0979 0.4801 0.4628 0.044 Uiso 1 1 calc R . . C48 C 0.2562(2) 0.50692(13) 0.38986(12) 0.0281(5) Uani 1 1 d . . . H48A H 0.1978 0.4798 0.3497 0.034 Uiso 1 1 calc R . . N1 N 0.58712(19) 0.12984(10) 0.29132(10) 0.0249(4) Uani 1 1 d . . . N2 N 0.7258(2) 0.00304(11) 0.24527(10) 0.0295(4) Uani 1 1 d . . . H2B H 0.8252 0.0091 0.2601 0.035 Uiso 1 1 calc R . . N3 N 0.56127(19) 0.63332(10) 0.28796(9) 0.0234(4) Uani 1 1 d . . . N4 N 0.3431(2) 0.51167(10) 0.23756(9) 0.0263(4) Uani 1 1 d . . . H4B H 0.2465 0.5160 0.2506 0.032 Uiso 1 1 calc R . . P1 P 0.39276(6) 0.11899(3) 0.26998(3) 0.02295(11) Uani 1 1 d . . . P2 P 0.60335(6) 0.04018(3) 0.29809(3) 0.02206(11) Uani 1 1 d . . . P3 P 0.74441(6) 0.61696(3) 0.26618(3) 0.02248(11) Uani 1 1 d . . . P4 P 0.48649(6) 0.54561(3) 0.29493(3) 0.02010(11) Uani 1 1 d . . . Cl1 Cl 0.10037(6) -0.00719(4) 0.27229(4) 0.04575(16) Uani 1 1 d . . . Cl2 Cl 0.38478(7) -0.10795(3) 0.29211(3) 0.03454(13) Uani 1 1 d . . . Cl3 Cl 0.61763(7) 0.39232(3) 0.29562(3) 0.03430(13) Uani 1 1 d . . . Cl4 Cl 0.94919(6) 0.48391(4) 0.25438(4) 0.04378(16) Uani 1 1 d . . . Ni1 Ni 0.35886(3) 0.005991(15) 0.280837(14) 0.02223(7) Uani 1 1 d . . . Ni2 Ni 0.70604(3) 0.503902(15) 0.277552(14) 0.02148(7) 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 C49 0.071(2) 0.111(4) 0.063(2) 0.002(2) 0.0019(19) 0.006(2) C50 0.089(3) 0.085(3) 0.0486(19) -0.0056(19) 0.0153(18) 0.013(2) Cl5 0.0767(6) 0.1001(8) 0.0626(5) 0.0094(5) 0.0087(4) 0.0073(5) Cl7 0.0857(7) 0.0863(7) 0.0951(7) 0.0138(6) 0.0346(6) 0.0163(6) C1 0.0221(10) 0.0287(12) 0.0299(11) 0.0024(9) 0.0025(8) 0.0048(9) C2 0.0493(15) 0.0462(16) 0.0382(14) 0.0122(12) 0.0153(11) 0.0179(13) C3 0.0628(18) 0.065(2) 0.0389(15) 0.0055(14) 0.0220(13) 0.0209(16) C4 0.0559(17) 0.0468(18) 0.0554(18) -0.0143(14) 0.0171(14) 0.0094(14) C5 0.0600(18) 0.0280(14) 0.072(2) -0.0044(14) 0.0153(15) 0.0068(13) C6 0.0429(13) 0.0278(13) 0.0454(15) 0.0047(11) 0.0130(11) 0.0036(11) C7 0.0373(12) 0.0282(12) 0.0263(11) 0.0059(9) 0.0027(9) 0.0095(10) C8 0.0432(15) 0.082(2) 0.0382(15) 0.0151(15) -0.0019(12) 0.0243(15) C9 0.080(2) 0.095(3) 0.0410(17) 0.0101(17) -0.0160(16) 0.042(2) C10 0.120(3) 0.060(2) 0.0285(15) 0.0111(14) -0.0099(17) 0.025(2) C11 0.093(3) 0.079(3) 0.0343(16) 0.0142(16) 0.0169(16) -0.004(2) C12 0.0508(16) 0.0612(19) 0.0336(14) 0.0113(13) 0.0086(12) -0.0015(14) C13 0.0269(11) 0.0264(12) 0.0390(13) 0.0084(10) 0.0002(9) -0.0028(9) C14 0.0477(15) 0.0304(14) 0.0442(15) 0.0030(12) -0.0076(12) -0.0055(11) C15 0.0281(12) 0.0505(18) 0.0673(19) 0.0049(15) 0.0087(12) -0.0081(12) C16 0.0337(12) 0.0532(17) 0.0277(12) -0.0060(11) 0.0004(10) 0.0086(12) C17 0.0583(18) 0.0433(17) 0.0554(18) -0.0122(14) 0.0112(14) 0.0009(14) C18 0.091(3) 0.072(2) 0.0350(16) 0.0060(15) 0.0156(16) 0.019(2) C19 0.0228(10) 0.0270(12) 0.0256(11) 0.0049(9) -0.0014(8) -0.0026(8) C20 0.0313(11) 0.0397(14) 0.0342(13) 0.0097(11) -0.0011(10) 0.0082(10) C21 0.0393(13) 0.0533(17) 0.0437(15) 0.0214(13) -0.0081(11) 0.0069(12) C22 0.0467(14) 0.0492(17) 0.0295(13) 0.0162(12) -0.0118(11) -0.0109(12) C23 0.0456(14) 0.0348(14) 0.0280(12) 0.0005(10) 0.0002(10) -0.0120(11) C24 0.0353(12) 0.0277(12) 0.0304(12) 0.0043(10) -0.0002(9) -0.0007(10) C25 0.0201(9) 0.0279(12) 0.0296(11) -0.0008(9) 0.0043(8) -0.0003(8) C26 0.0264(11) 0.0334(13) 0.0309(12) 0.0016(10) 0.0012(9) 0.0000(9) C27 0.0328(12) 0.0532(17) 0.0289(12) -0.0022(12) -0.0018(10) -0.0011(11) C28 0.0335(12) 0.0462(17) 0.0402(14) -0.0135(12) 0.0034(11) -0.0084(11) C29 0.0351(13) 0.0280(13) 0.0572(17) -0.0072(12) 0.0129(12) -0.0068(10) C30 0.0294(11) 0.0303(13) 0.0399(13) 0.0051(11) 0.0041(10) 0.0000(10) C31 0.0272(11) 0.0295(12) 0.0269(11) 0.0036(9) 0.0038(9) -0.0011(9) C32 0.0286(12) 0.0610(18) 0.0370(14) 0.0099(13) 0.0064(10) 0.0019(12) C33 0.0380(14) 0.076(2) 0.0401(15) 0.0083(15) 0.0146(12) -0.0029(14) C34 0.0571(17) 0.069(2) 0.0285(13) 0.0103(14) 0.0082(12) -0.0082(15) C35 0.0459(15) 0.077(2) 0.0340(14) 0.0179(14) -0.0051(12) 0.0036(15) C36 0.0302(12) 0.0544(17) 0.0342(13) 0.0081(12) 0.0021(10) 0.0011(11) C37 0.0273(10) 0.0204(11) 0.0341(12) 0.0063(9) 0.0020(9) 0.0058(9) C38 0.0480(14) 0.0294(13) 0.0379(13) 0.0021(11) 0.0015(11) 0.0139(11) C39 0.0282(11) 0.0313(13) 0.0473(14) 0.0062(11) 0.0030(10) 0.0112(10) C40 0.0290(11) 0.0438(15) 0.0230(11) -0.0019(10) -0.0003(9) 0.0029(10) C41 0.0591(17) 0.0399(16) 0.0418(15) -0.0065(12) -0.0124(13) 0.0022(13) C42 0.0661(18) 0.0590(19) 0.0295(14) 0.0084(13) -0.0109(13) 0.0025(15) C43 0.0241(10) 0.0205(11) 0.0244(10) 0.0036(8) 0.0032(8) 0.0051(8) C44 0.0317(11) 0.0317(13) 0.0282(12) 0.0056(10) -0.0016(9) 0.0020(10) C45 0.0491(14) 0.0367(14) 0.0251(12) 0.0027(10) -0.0019(10) 0.0099(11) C46 0.0446(14) 0.0454(15) 0.0270(12) 0.0096(11) 0.0128(10) 0.0146(12) C47 0.0317(12) 0.0416(15) 0.0394(14) 0.0107(11) 0.0147(10) 0.0063(10) C48 0.0250(10) 0.0297(12) 0.0298(11) 0.0035(9) 0.0046(9) 0.0042(9) N1 0.0206(8) 0.0247(10) 0.0300(10) 0.0060(8) 0.0013(7) 0.0025(7) N2 0.0198(8) 0.0394(12) 0.0283(10) -0.0019(8) -0.0006(7) 0.0059(8) N3 0.0198(8) 0.0226(9) 0.0289(9) 0.0054(7) 0.0044(7) 0.0047(7) N4 0.0185(8) 0.0346(11) 0.0245(9) -0.0004(8) 0.0011(7) 0.0026(7) P1 0.0205(2) 0.0256(3) 0.0242(3) 0.0062(2) 0.0022(2) 0.0052(2) P2 0.0187(2) 0.0249(3) 0.0228(3) 0.0031(2) -0.00015(19) 0.0038(2) P3 0.0176(2) 0.0240(3) 0.0256(3) 0.0036(2) 0.0019(2) 0.0012(2) P4 0.0178(2) 0.0213(3) 0.0213(3) 0.0029(2) 0.00178(19) 0.0023(2) Cl1 0.0188(3) 0.0550(4) 0.0636(4) 0.0107(3) -0.0014(3) 0.0028(3) Cl2 0.0396(3) 0.0248(3) 0.0398(3) 0.0078(2) 0.0012(2) 0.0023(2) Cl3 0.0436(3) 0.0242(3) 0.0360(3) 0.0072(2) 0.0042(2) 0.0039(2) Cl4 0.0196(2) 0.0450(4) 0.0636(4) -0.0084(3) 0.0002(3) 0.0085(2) Ni1 0.01830(12) 0.02431(15) 0.02444(14) 0.00493(11) 0.00040(10) 0.00228(10) Ni2 0.01812(12) 0.02186(15) 0.02429(14) 0.00131(11) 0.00013(10) 0.00377(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C49 Cl6B 1.699(4) . ? C49 Cl5 1.742(3) . ? C49 Cl6A 1.782(3) . ? C50 Cl8B 1.727(3) . ? C50 Cl7 1.742(3) . ? C50 Cl8A 1.762(3) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 P1 1.7964(11) . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 P1 1.7936(12) . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 N1 1.489(3) . ? C13 C14 1.511(3) . ? C13 C15 1.523(3) . ? C16 N2 1.470(3) . ? C16 C17 1.515(4) . ? C16 C18 1.526(4) . ? C19 C24 1.392(3) . ? C19 C20 1.394(3) . ? C19 P2 1.801(2) . ? C20 C21 1.381(3) . ? C21 C22 1.376(4) . ? C22 C23 1.373(4) . ? C23 C24 1.384(3) . ? C25 C26 1.391(3) . ? C25 C30 1.391(3) . ? C25 P3 1.808(2) . ? C26 C27 1.387(3) . ? C27 C28 1.370(4) . ? C28 C29 1.375(4) . ? C29 C30 1.392(4) . ? C31 C36 1.388(3) . ? C31 C32 1.390(3) . ? C31 P3 1.802(2) . ? C32 C33 1.373(4) . ? C33 C34 1.375(4) . ? C34 C35 1.375(4) . ? C35 C36 1.381(4) . ? C37 N3 1.493(3) . ? C37 C38 1.512(3) . ? C37 C39 1.521(3) . ? C40 N4 1.470(3) . ? C40 C41 1.514(4) . ? C40 C42 1.521(3) . ? C43 C48 1.390(3) . ? C43 C44 1.400(3) . ? C43 P4 1.803(2) . ? C44 C45 1.383(3) . ? C45 C46 1.377(4) . ? C46 C47 1.381(4) . ? C47 C48 1.383(3) . ? N1 P1 1.6872(17) . ? N1 P2 1.6989(18) . ? N2 P2 1.6195(18) . ? N3 P3 1.6860(16) . ? N3 P4 1.6942(18) . ? N4 P4 1.6300(18) . ? P1 Ni1 2.1108(6) . ? P1 P2 2.5351(7) . ? P2 Ni1 2.1220(6) . ? P3 Ni2 2.1152(6) . ? P3 P4 2.5487(7) . ? P4 Ni2 2.1342(5) . ? Cl1 Ni1 2.2010(6) . ? Cl2 Ni1 2.1787(6) . ? Cl3 Ni2 2.1843(6) . ? Cl4 Ni2 2.2058(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl6B C49 Cl5 118.2(3) . . ? Cl5 C49 Cl6A 109.8(2) . . ? Cl8B C50 Cl7 111.0(2) . . ? Cl7 C50 Cl8A 114.8(2) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 119.51(8) . . ? C6 C1 P1 120.23(8) . . ? C1 C2 C3 120.0 . . ? C4 C3 C2 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C8 C7 C12 120.0 . . ? C8 C7 P1 117.75(9) . . ? C12 C7 P1 122.19(9) . . ? C9 C8 C7 120.0 . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C12 C11 C10 120.0 . . ? C11 C12 C7 120.0 . . ? N1 C13 C14 113.0(2) . . ? N1 C13 C15 110.55(19) . . ? C14 C13 C15 111.1(2) . . ? N2 C16 C17 109.3(2) . . ? N2 C16 C18 110.3(2) . . ? C17 C16 C18 111.8(2) . . ? C24 C19 C20 119.1(2) . . ? C24 C19 P2 119.08(16) . . ? C20 C19 P2 121.18(17) . . ? C21 C20 C19 119.7(2) . . ? C22 C21 C20 120.6(2) . . ? C23 C22 C21 120.2(2) . . ? C22 C23 C24 119.9(2) . . ? C23 C24 C19 120.3(2) . . ? C26 C25 C30 120.2(2) . . ? C26 C25 P3 118.95(18) . . ? C30 C25 P3 120.84(17) . . ? C27 C26 C25 119.5(2) . . ? C28 C27 C26 120.1(2) . . ? C27 C28 C29 120.9(2) . . ? C28 C29 C30 119.9(2) . . ? C25 C30 C29 119.4(2) . . ? C36 C31 C32 119.1(2) . . ? C36 C31 P3 121.33(17) . . ? C32 C31 P3 119.37(18) . . ? C33 C32 C31 120.0(2) . . ? C32 C33 C34 120.6(2) . . ? C35 C34 C33 120.0(3) . . ? C34 C35 C36 119.9(2) . . ? C35 C36 C31 120.3(2) . . ? N3 C37 C38 111.94(17) . . ? N3 C37 C39 109.79(18) . . ? C38 C37 C39 112.16(19) . . ? N4 C40 C41 110.3(2) . . ? N4 C40 C42 110.0(2) . . ? C41 C40 C42 111.2(2) . . ? C48 C43 C44 118.7(2) . . ? C48 C43 P4 121.98(16) . . ? C44 C43 P4 119.24(16) . . ? C45 C44 C43 120.6(2) . . ? C46 C45 C44 120.1(2) . . ? C45 C46 C47 119.9(2) . . ? C46 C47 C48 120.6(2) . . ? C47 C48 C43 120.2(2) . . ? C13 N1 P1 128.48(14) . . ? C13 N1 P2 134.57(14) . . ? P1 N1 P2 96.95(9) . . ? C16 N2 P2 126.12(15) . . ? C37 N3 P3 128.34(15) . . ? C37 N3 P4 133.76(14) . . ? P3 N3 P4 97.88(9) . . ? C40 N4 P4 124.62(14) . . ? N1 P1 C7 110.31(8) . . ? N1 P1 C1 108.93(9) . . ? C7 P1 C1 105.18(7) . . ? N1 P1 Ni1 94.99(6) . . ? C7 P1 Ni1 115.63(7) . . ? C1 P1 Ni1 121.12(6) . . ? C7 P1 P2 121.84(6) . . ? C1 P1 P2 130.01(6) . . ? Ni1 P1 P2 53.411(18) . . ? N2 P2 N1 115.07(10) . . ? N2 P2 C19 105.47(9) . . ? N1 P2 C19 108.75(10) . . ? N2 P2 Ni1 119.48(7) . . ? N1 P2 Ni1 94.23(6) . . ? C19 P2 Ni1 113.50(7) . . ? N2 P2 P1 128.92(7) . . ? C19 P2 P1 124.14(7) . . ? Ni1 P2 P1 53.004(19) . . ? N3 P3 C31 109.21(9) . . ? N3 P3 C25 110.34(9) . . ? C31 P3 C25 105.28(11) . . ? N3 P3 Ni2 94.53(7) . . ? C31 P3 Ni2 117.71(8) . . ? C25 P3 Ni2 119.06(8) . . ? C31 P3 P4 121.96(7) . . ? C25 P3 P4 129.80(7) . . ? Ni2 P3 P4 53.489(18) . . ? N4 P4 N3 114.62(9) . . ? N4 P4 C43 105.01(9) . . ? N3 P4 C43 107.12(9) . . ? N4 P4 Ni2 116.25(7) . . ? N3 P4 Ni2 93.60(6) . . ? C43 P4 Ni2 119.94(6) . . ? N4 P4 P3 125.56(7) . . ? C43 P4 P3 127.01(7) . . ? Ni2 P4 P3 52.805(18) . . ? P1 Ni1 P2 73.58(2) . . ? P1 Ni1 Cl2 166.32(2) . . ? P2 Ni1 Cl2 92.93(2) . . ? P1 Ni1 Cl1 96.73(3) . . ? P2 Ni1 Cl1 168.69(3) . . ? Cl2 Ni1 Cl1 96.91(3) . . ? P3 Ni2 P4 73.71(2) . . ? P3 Ni2 Cl3 168.02(2) . . ? P4 Ni2 Cl3 94.36(2) . . ? P3 Ni2 Cl4 94.43(3) . . ? P4 Ni2 Cl4 168.10(3) . . ? Cl3 Ni2 Cl4 97.52(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.080 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.057 # Attachment '- 8.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 780227' #TrackingRef '- 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 Cl2 N2 P2 Pd' _chemical_formula_weight 585.74 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' 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' Pd Pd -0.9988 1.0072 '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(1)/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 8.7588(3) _cell_length_b 14.6095(3) _cell_length_c 20.0055(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.028(2) _cell_angle_gamma 90.00 _cell_volume 2559.94(13) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4932 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 29.62 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.073 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7375 _exptl_absorpt_correction_T_max 0.9483 _exptl_absorpt_process_details 'X-SHAPE (Stoe & Cie, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS II' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37483 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5879 _reflns_number_gt 4680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Program Package (Stoe & Cie, 2005)' _computing_cell_refinement 'IPDS Program Package' _computing_data_reduction 'IPDS Program Package' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL' _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^)+(0.0305P)^2^+0.2976P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5879 _refine_ls_number_parameters 288 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0555 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.1212(2) 0.13439(15) 0.17425(11) 0.0294(4) Uani 1 1 d . . . C2 C -0.0552(3) 0.07549(17) 0.12777(13) 0.0403(5) Uani 1 1 d . . . H2 H 0.0312 0.0948 0.1027 0.048 Uiso 1 1 calc R . . C3 C -0.1153(3) -0.01119(18) 0.11794(14) 0.0498(7) Uani 1 1 d D . . H3 H -0.0720 -0.0503 0.0851 0.060 Uiso 1 1 calc R . . C4 C -0.2371(3) -0.04095(17) 0.15533(12) 0.0498(7) Uani 1 1 d D . . H4 H -0.2772 -0.1007 0.1487 0.060 Uiso 1 1 calc R . . C5 C -0.3006(3) 0.01594(18) 0.20229(14) 0.0496(7) Uani 1 1 d D . . H5 H -0.3835 -0.0052 0.2287 0.060 Uiso 1 1 calc R . . C6 C -0.2452(3) 0.10374(17) 0.21156(13) 0.0388(5) Uani 1 1 d . . . H6 H -0.2918 0.1431 0.2434 0.047 Uiso 1 1 calc R . . C7 C 0.3267(2) 0.23614(14) 0.07174(11) 0.0278(4) Uani 1 1 d . . . C8 C 0.4123(3) 0.16236(16) 0.09458(12) 0.0369(5) Uani 1 1 d . . . H8 H 0.4094 0.1456 0.1404 0.044 Uiso 1 1 calc R . . C9 C 0.5019(3) 0.11348(19) 0.05009(13) 0.0471(6) Uani 1 1 d . . . H9 H 0.5619 0.0637 0.0656 0.057 Uiso 1 1 calc R . . C10 C 0.5041(3) 0.13673(19) -0.01653(13) 0.0448(6) Uani 1 1 d . . . H10 H 0.5653 0.1026 -0.0468 0.054 Uiso 1 1 calc R . . C11 C 0.4184(3) 0.20902(18) -0.03961(12) 0.0383(5) Uani 1 1 d . . . H11 H 0.4188 0.2238 -0.0858 0.046 Uiso 1 1 calc R . . C12 C 0.3318(2) 0.26005(16) 0.00434(11) 0.0339(5) Uani 1 1 d . . . H12 H 0.2758 0.3114 -0.0113 0.041 Uiso 1 1 calc R . . C13 C 0.2633(2) 0.41800(15) 0.11773(11) 0.0287(4) Uani 1 1 d . . . C14 C 0.4159(3) 0.44079(17) 0.10884(14) 0.0442(6) Uani 1 1 d . . . H14 H 0.4901 0.3939 0.1038 0.053 Uiso 1 1 calc R . . C15 C 0.4599(3) 0.53150(19) 0.10739(16) 0.0528(7) Uani 1 1 d . . . H15 H 0.5646 0.5469 0.1022 0.063 Uiso 1 1 calc R . . C16 C 0.3528(3) 0.59936(17) 0.11346(14) 0.0471(6) Uani 1 1 d . . . H16 H 0.3835 0.6617 0.1122 0.057 Uiso 1 1 calc R . . C17 C 0.2007(3) 0.57747(18) 0.12142(15) 0.0492(7) Uani 1 1 d . . . H17 H 0.1266 0.6247 0.1249 0.059 Uiso 1 1 calc R . . C18 C 0.1563(3) 0.48725(17) 0.12432(13) 0.0407(6) Uani 1 1 d . . . H18 H 0.0518 0.4724 0.1309 0.049 Uiso 1 1 calc R . . C19 C -0.1461(2) 0.38401(16) 0.26835(11) 0.0319(5) Uani 1 1 d . . . H19 H -0.0342 0.3970 0.2709 0.038 Uiso 1 1 calc R . . C20 C -0.2021(3) 0.3618(2) 0.33799(12) 0.0454(6) Uani 1 1 d . . . H20A H -0.3104 0.3452 0.3362 0.068 Uiso 1 1 calc R . . H20B H -0.1890 0.4155 0.3668 0.068 Uiso 1 1 calc R . . H20C H -0.1431 0.3105 0.3561 0.068 Uiso 1 1 calc R . . C21 C -0.2251(3) 0.46801(18) 0.24075(15) 0.0501(6) Uani 1 1 d . . . H21A H -0.1827 0.4828 0.1967 0.075 Uiso 1 1 calc R . . H21B H -0.2090 0.5197 0.2712 0.075 Uiso 1 1 calc R . . H21C H -0.3347 0.4559 0.2365 0.075 Uiso 1 1 calc R . . C22 C -0.0587(2) 0.30850(18) 0.05048(11) 0.0363(5) Uani 1 1 d . . . H22 H -0.0010 0.3580 0.0270 0.044 Uiso 1 1 calc R . . C23 C -0.0702(3) 0.2272(2) 0.00369(13) 0.0520(7) Uani 1 1 d . . . H23A H 0.0315 0.2008 -0.0031 0.078 Uiso 1 1 calc R . . H23B H -0.1116 0.2473 -0.0394 0.078 Uiso 1 1 calc R . . H23C H -0.1378 0.1810 0.0232 0.078 Uiso 1 1 calc R . . C24 C -0.2175(3) 0.3438(3) 0.06525(14) 0.0615(9) Uani 1 1 d . . . H24A H -0.2750 0.2971 0.0898 0.092 Uiso 1 1 calc R . . H24B H -0.2700 0.3576 0.0232 0.092 Uiso 1 1 calc R . . H24C H -0.2105 0.3995 0.0923 0.092 Uiso 1 1 calc R . . Cl1 Cl 0.14094(6) 0.19736(5) 0.34182(3) 0.04026(14) Uani 1 1 d . . . Cl2 Cl 0.45891(5) 0.27154(4) 0.25802(3) 0.03864(14) Uani 1 1 d . . . N1 N -0.1686(2) 0.30463(13) 0.22487(9) 0.0295(4) Uani 1 1 d . . . N2 N 0.02298(18) 0.28709(13) 0.11406(8) 0.0277(4) Uani 1 1 d . . . P1 P -0.03585(5) 0.24511(4) 0.18924(2) 0.02394(10) Uani 1 1 d . . . P2 P 0.21099(5) 0.30031(4) 0.12985(3) 0.02414(11) Uani 1 1 d . . . Pd1 Pd 0.196830(14) 0.250808(12) 0.233561(7) 0.02268(5) Uani 1 1 d . . . H1 H -0.250(4) 0.290(2) 0.2183(15) 0.058(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0242(9) 0.0313(11) 0.0327(11) 0.0009(9) -0.0080(8) -0.0008(8) C2 0.0356(12) 0.0369(13) 0.0484(14) -0.0065(11) -0.0040(10) 0.0036(10) C3 0.0568(16) 0.0356(14) 0.0570(17) -0.0107(12) -0.0163(13) 0.0102(12) C4 0.0554(16) 0.0302(13) 0.0638(18) 0.0079(12) -0.0280(14) -0.0073(11) C5 0.0483(15) 0.0419(15) 0.0586(18) 0.0136(13) -0.0096(13) -0.0132(12) C6 0.0375(12) 0.0377(13) 0.0410(13) 0.0050(11) 0.0001(10) -0.0070(10) C7 0.0233(9) 0.0289(12) 0.0312(10) -0.0001(8) 0.0028(7) -0.0015(8) C8 0.0389(12) 0.0382(13) 0.0334(12) 0.0006(10) 0.0031(9) 0.0078(10) C9 0.0484(14) 0.0463(15) 0.0466(15) -0.0026(12) 0.0040(11) 0.0169(12) C10 0.0439(13) 0.0493(15) 0.0412(14) -0.0120(12) 0.0109(11) 0.0062(11) C11 0.0364(11) 0.0475(14) 0.0309(12) -0.0018(11) 0.0053(9) -0.0059(11) C12 0.0327(10) 0.0358(13) 0.0331(11) 0.0028(10) 0.0046(8) 0.0016(9) C13 0.0265(10) 0.0298(11) 0.0299(11) 0.0020(9) 0.0012(8) 0.0009(8) C14 0.0267(11) 0.0343(13) 0.0716(18) 0.0034(12) 0.0027(11) -0.0001(9) C15 0.0374(13) 0.0427(15) 0.078(2) 0.0094(14) -0.0003(13) -0.0121(11) C16 0.0616(17) 0.0297(12) 0.0500(16) 0.0046(11) 0.0023(13) -0.0056(11) C17 0.0567(16) 0.0344(13) 0.0566(17) 0.0080(12) 0.0158(13) 0.0122(11) C18 0.0344(12) 0.0383(13) 0.0494(15) 0.0056(11) 0.0129(10) 0.0057(10) C19 0.0237(9) 0.0366(12) 0.0356(12) -0.0055(9) 0.0012(8) -0.0030(8) C20 0.0467(14) 0.0561(16) 0.0333(13) -0.0073(12) 0.0027(10) -0.0113(12) C21 0.0548(15) 0.0380(14) 0.0577(17) 0.0004(13) 0.0004(13) 0.0030(12) C22 0.0298(10) 0.0528(15) 0.0262(11) 0.0044(10) -0.0037(8) 0.0002(10) C23 0.0535(15) 0.069(2) 0.0337(13) -0.0032(12) -0.0086(11) -0.0089(13) C24 0.0388(14) 0.108(3) 0.0379(15) 0.0038(15) -0.0086(11) 0.0220(15) Cl1 0.0380(3) 0.0550(4) 0.0278(3) 0.0065(3) -0.0002(2) -0.0069(3) Cl2 0.0188(2) 0.0538(4) 0.0433(3) -0.0039(2) -0.0044(2) -0.0012(2) N1 0.0194(8) 0.0359(10) 0.0333(10) -0.0046(8) 0.0009(7) -0.0019(7) N2 0.0203(7) 0.0388(9) 0.0240(8) 0.0021(7) -0.0013(6) -0.0013(7) P1 0.0179(2) 0.0294(2) 0.0246(2) -0.0005(2) -0.00132(16) -0.0013(2) P2 0.0184(2) 0.0289(3) 0.0252(3) 0.0011(2) 0.00157(18) 0.00070(19) Pd1 0.01752(7) 0.02702(8) 0.02349(7) -0.00084(7) -0.00168(5) -0.00041(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.393(3) . ? C1 C2 1.393(3) . ? C1 P1 1.807(2) . ? C2 C3 1.385(3) . ? C3 C4 1.374(3) . ? C4 C5 1.372(3) . ? C5 C6 1.384(3) . ? C7 C8 1.390(3) . ? C7 C12 1.394(3) . ? C7 P2 1.805(2) . ? C8 C9 1.385(3) . ? C9 C10 1.376(4) . ? C10 C11 1.376(4) . ? C11 C12 1.380(3) . ? C13 C18 1.385(3) . ? C13 C14 1.388(3) . ? C13 P2 1.796(2) . ? C14 C15 1.380(3) . ? C15 C16 1.370(4) . ? C16 C17 1.380(4) . ? C17 C18 1.375(4) . ? C19 N1 1.463(3) . ? C19 C20 1.512(3) . ? C19 C21 1.513(3) . ? C22 N2 1.492(3) . ? C22 C24 1.513(3) . ? C22 C23 1.515(4) . ? Cl1 Pd1 2.3539(6) . ? Cl2 Pd1 2.3663(5) . ? N1 P1 1.6178(18) . ? N2 P2 1.6877(16) . ? N2 P1 1.7042(18) . ? P1 Pd1 2.2237(4) . ? P1 P2 2.5958(7) . ? P2 Pd1 2.2007(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.9(2) . . ? C6 C1 P1 121.44(18) . . ? C2 C1 P1 119.49(17) . . ? C3 C2 C1 120.1(2) . . ? C4 C3 C2 120.5(2) . . ? C5 C4 C3 119.7(2) . . ? C4 C5 C6 120.7(2) . . ? C5 C6 C1 120.0(2) . . ? C8 C7 C12 119.7(2) . . ? C8 C7 P2 119.60(17) . . ? C12 C7 P2 120.74(16) . . ? C9 C8 C7 119.6(2) . . ? C10 C9 C8 120.3(2) . . ? C9 C10 C11 120.4(2) . . ? C10 C11 C12 120.1(2) . . ? C11 C12 C7 119.9(2) . . ? C18 C13 C14 119.2(2) . . ? C18 C13 P2 120.90(17) . . ? C14 C13 P2 119.51(17) . . ? C15 C14 C13 120.1(2) . . ? C16 C15 C14 120.1(2) . . ? C15 C16 C17 120.2(2) . . ? C18 C17 C16 120.0(2) . . ? C17 C18 C13 120.3(2) . . ? N1 C19 C20 109.54(19) . . ? N1 C19 C21 111.4(2) . . ? C20 C19 C21 111.2(2) . . ? N2 C22 C24 110.21(19) . . ? N2 C22 C23 113.2(2) . . ? C24 C22 C23 109.1(2) . . ? C19 N1 P1 126.26(14) . . ? C22 N2 P2 127.08(14) . . ? C22 N2 P1 133.06(14) . . ? P2 N2 P1 99.87(9) . . ? N1 P1 N2 114.40(10) . . ? N1 P1 C1 104.89(10) . . ? N2 P1 C1 107.51(10) . . ? N1 P1 Pd1 117.58(7) . . ? N2 P1 Pd1 93.50(6) . . ? C1 P1 Pd1 118.59(7) . . ? N1 P1 P2 129.32(7) . . ? N2 P1 P2 39.83(5) . . ? C1 P1 P2 123.14(8) . . ? Pd1 P1 P2 53.667(16) . . ? N2 P2 C13 109.47(9) . . ? N2 P2 C7 111.61(9) . . ? C13 P2 C7 105.47(10) . . ? N2 P2 Pd1 94.79(6) . . ? C13 P2 Pd1 117.15(7) . . ? C7 P2 Pd1 117.93(7) . . ? N2 P2 P1 40.30(6) . . ? C13 P2 P1 124.88(7) . . ? C7 P2 P1 126.98(7) . . ? Pd1 P2 P1 54.489(16) . . ? P2 Pd1 P1 71.844(18) . . ? P2 Pd1 Cl1 171.206(19) . . ? P1 Pd1 Cl1 99.41(2) . . ? P2 Pd1 Cl2 95.61(2) . . ? P1 Pd1 Cl2 167.43(2) . . ? Cl1 Pd1 Cl2 93.11(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.472 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.057 # Attachment '- 9.cif' data_9 _database_code_depnum_ccdc_archive 'CCDC 780228' #TrackingRef '- 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24.50 H31 Br2 Cl N2 P2 Pt' _chemical_formula_weight 805.81 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' P P 0.1023 0.0942 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.4775(2) _cell_length_b 13.2311(2) _cell_length_c 22.4851(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.4274(17) _cell_angle_gamma 90.00 _cell_volume 2763.68(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6755 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 29.55 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 8.198 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2645 _exptl_absorpt_correction_T_max 0.6076 _exptl_absorpt_process_details 'X-SHAPE and X-RED32 (Stoe & Cie, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42678 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6342 _reflns_number_gt 5163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2005)' _computing_cell_refinement X-AREA _computing_data_reduction X-AREA _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0182P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6342 _refine_ls_number_parameters 315 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0409 _refine_ls_wR_factor_gt 0.0393 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.926 _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 Br1 Br 0.26006(4) 1.03084(3) 0.108896(17) 0.03273(8) Uani 1 1 d . . . Br2 Br 0.45423(4) 0.92365(3) 0.249126(17) 0.03323(9) Uani 1 1 d . . . C1 C -0.0867(3) 0.8279(2) 0.09262(15) 0.0229(7) Uani 1 1 d . . . C2 C -0.1636(4) 0.7930(3) 0.13516(16) 0.0278(7) Uani 1 1 d . . . H2B H -0.1240 0.7411 0.1627 0.033 Uiso 1 1 calc R . . C3 C -0.2975(4) 0.8332(3) 0.13769(18) 0.0334(8) Uani 1 1 d . . . H3 H -0.3490 0.8094 0.1671 0.040 Uiso 1 1 calc R . . C4 C -0.3553(4) 0.9075(3) 0.09764(19) 0.0384(9) Uani 1 1 d . . . H4 H -0.4465 0.9356 0.0996 0.046 Uiso 1 1 calc R . . C5 C -0.2818(4) 0.9415(3) 0.0546(2) 0.0421(10) Uani 1 1 d . . . H5 H -0.3238 0.9914 0.0261 0.050 Uiso 1 1 calc R . . C6 C -0.1465(4) 0.9032(3) 0.05257(17) 0.0331(8) Uani 1 1 d . . . H6 H -0.0947 0.9287 0.0237 0.040 Uiso 1 1 calc R . . C7 C 0.1241(4) 0.7794(3) 0.01967(15) 0.0251(7) Uani 1 1 d . . . C8 C 0.0120(4) 0.7559(3) -0.02868(15) 0.0327(8) Uani 1 1 d D . . H8 H -0.0828 0.7465 -0.0217 0.039 Uiso 1 1 calc R . . C9 C 0.0384(4) 0.7464(3) -0.08645(15) 0.0426(10) Uani 1 1 d D . . H9 H -0.0380 0.7290 -0.1190 0.051 Uiso 1 1 calc R . . C10 C 0.1745(3) 0.7619(3) -0.09743(17) 0.0475(11) Uani 1 1 d D . . H10 H 0.1916 0.7567 -0.1375 0.057 Uiso 1 1 calc R . . C11 C 0.2856(4) 0.7851(4) -0.05004(13) 0.0492(11) Uani 1 1 d D . . H11 H 0.3798 0.7950 -0.0575 0.059 Uiso 1 1 calc R . . C12 C 0.2614(4) 0.7942(3) 0.00813(16) 0.0356(9) Uani 1 1 d D . . H12 H 0.3389 0.8105 0.0405 0.043 Uiso 1 1 calc R . . C13 C 0.0896(4) 0.5693(2) 0.11613(15) 0.0242(7) Uani 1 1 d . . . H13 H 0.1297 0.5266 0.1522 0.029 Uiso 1 1 calc R . . C14 C -0.0719(4) 0.5544(3) 0.1030(2) 0.0373(9) Uani 1 1 d . . . H14A H -0.1100 0.5712 0.1393 0.056 Uiso 1 1 calc R . . H14B H -0.0943 0.4837 0.0919 0.056 Uiso 1 1 calc R . . H14C H -0.1161 0.5985 0.0695 0.056 Uiso 1 1 calc R . . C15 C 0.1565(4) 0.5321(3) 0.06420(18) 0.0334(8) Uani 1 1 d . . . H15A H 0.1158 0.5698 0.0273 0.050 Uiso 1 1 calc R . . H15B H 0.1359 0.4600 0.0575 0.050 Uiso 1 1 calc R . . H15C H 0.2609 0.5426 0.0743 0.050 Uiso 1 1 calc R . . C16 C 0.3951(3) 0.6334(3) 0.21184(14) 0.0228(6) Uani 1 1 d . . . C17 C 0.4698(3) 0.6220(3) 0.16474(16) 0.0306(8) Uani 1 1 d . . . H17 H 0.4349 0.6525 0.1264 0.037 Uiso 1 1 calc R . . C18 C 0.5954(4) 0.5658(3) 0.1743(2) 0.0404(10) Uani 1 1 d . . . H18 H 0.6460 0.5571 0.1421 0.048 Uiso 1 1 calc R . . C19 C 0.6479(4) 0.5222(3) 0.2301(2) 0.0422(10) Uani 1 1 d . . . H19 H 0.7342 0.4837 0.2363 0.051 Uiso 1 1 calc R . . C20 C 0.5750(4) 0.5346(3) 0.2765(2) 0.0406(10) Uani 1 1 d . . . H20 H 0.6108 0.5045 0.3149 0.049 Uiso 1 1 calc R . . C21 C 0.4494(4) 0.5910(3) 0.26773(18) 0.0322(8) Uani 1 1 d . . . H21 H 0.4005 0.6004 0.3003 0.039 Uiso 1 1 calc R . . C22 C 0.0725(4) 0.7712(3) 0.28031(16) 0.0274(7) Uani 1 1 d . . . H22 H 0.0415 0.8229 0.2479 0.033 Uiso 1 1 calc R . . C23 C -0.0609(4) 0.7183(4) 0.2930(2) 0.0459(10) Uani 1 1 d . . . H23A H -0.1063 0.6794 0.2572 0.069 Uiso 1 1 calc R . . H23B H -0.1290 0.7687 0.3024 0.069 Uiso 1 1 calc R . . H23C H -0.0334 0.6725 0.3276 0.069 Uiso 1 1 calc R . . C24 C 0.1524(5) 0.8246(3) 0.33653(19) 0.0470(11) Uani 1 1 d . . . H24A H 0.1801 0.7754 0.3693 0.071 Uiso 1 1 calc R . . H24B H 0.0898 0.8761 0.3490 0.071 Uiso 1 1 calc R . . H24C H 0.2389 0.8569 0.3276 0.071 Uiso 1 1 calc R . . N1 N 0.1302(3) 0.6758(2) 0.13289(12) 0.0214(6) Uani 1 1 d . . . N2 N 0.1678(3) 0.6985(2) 0.25850(13) 0.0261(6) Uani 1 1 d D . . H2A H 0.175(4) 0.6385(13) 0.2747(17) 0.040(11) Uiso 1 1 d D . . P1 P 0.09777(9) 0.78837(6) 0.09678(4) 0.02054(17) Uani 1 1 d . . . P2 P 0.23843(8) 0.71421(6) 0.19904(4) 0.01951(16) Uani 1 1 d . . . Pt1 Pt 0.259569(13) 0.868348(9) 0.164730(6) 0.01978(3) Uani 1 1 d . . . C25 C 0.4672(17) 0.5697(4) 0.9727(7) 0.066(4) Uani 0.50 1 d PD A -1 H25A H 0.3691 0.5926 0.9752 0.079 Uiso 0.50 1 calc PR A -1 H25B H 0.4739 0.5685 0.9294 0.079 Uiso 0.50 1 calc PR A -1 Cl1 Cl 0.5913(3) 0.6560(2) 1.01064(13) 0.0718(8) Uani 0.50 1 d PD A -1 Cl2 Cl 0.4923(5) 0.4478(3) 1.0017(2) 0.0903(15) Uani 0.50 1 d PD A -1 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 Br1 0.0435(2) 0.02351(17) 0.03191(19) 0.00367(14) 0.00917(15) 0.00034(15) Br2 0.02855(17) 0.0392(2) 0.03030(19) -0.00810(16) 0.00178(14) -0.00775(15) C1 0.0205(15) 0.0217(16) 0.0254(17) -0.0023(13) 0.0017(13) -0.0006(12) C2 0.0285(17) 0.0271(18) 0.0271(18) -0.0024(14) 0.0039(14) 0.0002(14) C3 0.0262(17) 0.0335(19) 0.044(2) -0.0085(17) 0.0146(16) -0.0050(15) C4 0.0240(18) 0.041(2) 0.049(2) -0.0088(19) 0.0048(17) 0.0049(16) C5 0.034(2) 0.044(2) 0.045(2) 0.004(2) 0.0016(18) 0.0162(18) C6 0.0306(18) 0.036(2) 0.034(2) 0.0080(16) 0.0089(16) 0.0064(15) C7 0.0280(17) 0.0234(17) 0.0239(16) 0.0013(14) 0.0055(13) 0.0017(14) C8 0.0312(18) 0.039(2) 0.0279(18) -0.0019(16) 0.0055(15) 0.0010(16) C9 0.049(3) 0.050(3) 0.0272(19) -0.0038(17) 0.0026(18) 0.004(2) C10 0.060(3) 0.058(3) 0.029(2) -0.002(2) 0.020(2) 0.005(2) C11 0.049(3) 0.058(3) 0.048(3) -0.004(2) 0.028(2) -0.008(2) C12 0.0334(19) 0.040(2) 0.035(2) -0.0042(17) 0.0118(16) -0.0029(16) C13 0.0290(17) 0.0192(17) 0.0239(17) -0.0016(13) 0.0035(14) -0.0037(13) C14 0.0257(18) 0.031(2) 0.055(3) -0.0101(18) 0.0085(17) -0.0078(15) C15 0.0338(19) 0.0288(19) 0.038(2) -0.0065(16) 0.0082(16) 0.0007(15) C16 0.0189(13) 0.0212(15) 0.0271(16) 0.0003(15) 0.0018(12) -0.0023(14) C17 0.0218(15) 0.038(2) 0.0315(18) -0.0002(17) 0.0050(13) -0.0009(16) C18 0.0223(17) 0.045(2) 0.056(3) -0.010(2) 0.0122(17) 0.0014(16) C19 0.0210(18) 0.034(2) 0.068(3) 0.000(2) 0.0002(18) 0.0070(16) C20 0.034(2) 0.037(2) 0.046(2) 0.0107(19) -0.0037(18) 0.0055(17) C21 0.0286(18) 0.0325(19) 0.034(2) 0.0059(16) 0.0027(15) 0.0010(15) C22 0.0281(17) 0.0294(19) 0.0264(17) 0.0011(14) 0.0095(14) 0.0050(14) C23 0.033(2) 0.061(3) 0.047(2) 0.012(2) 0.0164(18) 0.005(2) C24 0.057(3) 0.048(3) 0.035(2) -0.0138(19) 0.009(2) 0.010(2) N1 0.0207(13) 0.0202(14) 0.0222(14) 0.0000(11) 0.0019(11) -0.0011(11) N2 0.0309(15) 0.0231(15) 0.0264(15) 0.0021(12) 0.0108(12) 0.0037(12) P1 0.0187(4) 0.0218(4) 0.0209(4) 0.0003(3) 0.0033(3) 0.0008(3) P2 0.0188(4) 0.0199(4) 0.0200(4) -0.0002(3) 0.0042(3) 0.0002(3) Pt1 0.01936(5) 0.01940(6) 0.02094(6) -0.00111(6) 0.00489(4) -0.00029(6) C25 0.080(9) 0.044(8) 0.066(10) 0.003(6) -0.005(7) 0.006(6) Cl1 0.0488(13) 0.092(2) 0.0674(17) -0.0102(15) -0.0065(12) 0.0133(13) Cl2 0.116(4) 0.079(2) 0.090(3) 0.025(2) 0.054(3) 0.036(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 Br1 Pt1 2.4902(4) . ? Br2 Pt1 2.4805(4) . ? C1 C6 1.387(5) . ? C1 C2 1.391(5) . ? C1 P1 1.810(3) . ? C2 C3 1.388(5) . ? C3 C4 1.371(6) . ? C4 C5 1.376(6) . ? C5 C6 1.387(5) . ? C7 C12 1.390(5) . ? C7 C8 1.397(5) . ? C7 P1 1.804(3) . ? C8 C9 1.376(2) . ? C9 C10 1.376(2) . ? C10 C11 1.376(3) . ? C11 C12 1.377(3) . ? C13 N1 1.489(4) . ? C13 C14 1.513(5) . ? C13 C15 1.517(5) . ? C16 C21 1.380(5) . ? C16 C17 1.394(5) . ? C16 P2 1.806(3) . ? C17 C18 1.383(5) . ? C18 C19 1.381(6) . ? C19 C20 1.371(6) . ? C20 C21 1.385(5) . ? C22 N2 1.469(4) . ? C22 C24 1.513(5) . ? C22 C23 1.521(5) . ? N1 P1 1.695(3) . ? N1 P2 1.708(3) . ? N2 P2 1.623(3) . ? P1 Pt1 2.2084(8) . ? P1 P2 2.6099(12) . ? P2 Pt1 2.2035(8) . ? C25 Cl2 1.737(8) . ? C25 Cl1 1.737(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.9(3) . . ? C6 C1 P1 120.5(3) . . ? C2 C1 P1 120.0(3) . . ? C3 C2 C1 120.5(3) . . ? C4 C3 C2 119.9(4) . . ? C3 C4 C5 120.3(4) . . ? C4 C5 C6 120.3(4) . . ? C1 C6 C5 120.2(4) . . ? C12 C7 C8 118.8(3) . . ? C12 C7 P1 118.9(3) . . ? C8 C7 P1 122.3(3) . . ? C9 C8 C7 120.2(3) . . ? C10 C9 C8 120.5(4) . . ? C9 C10 C11 119.7(3) . . ? C10 C11 C12 120.6(4) . . ? C11 C12 C7 120.2(3) . . ? N1 C13 C14 111.9(3) . . ? N1 C13 C15 112.0(3) . . ? C14 C13 C15 111.6(3) . . ? C21 C16 C17 119.6(3) . . ? C21 C16 P2 122.2(3) . . ? C17 C16 P2 118.0(3) . . ? C18 C17 C16 119.4(3) . . ? C19 C18 C17 120.6(4) . . ? C20 C19 C18 119.7(4) . . ? C19 C20 C21 120.3(4) . . ? C16 C21 C20 120.2(4) . . ? N2 C22 C24 110.2(3) . . ? N2 C22 C23 110.5(3) . . ? C24 C22 C23 110.8(3) . . ? C13 N1 P1 134.2(2) . . ? C13 N1 P2 125.6(2) . . ? P1 N1 P2 100.14(14) . . ? C22 N2 P2 124.9(2) . . ? N1 P1 C7 110.86(15) . . ? N1 P1 C1 111.12(15) . . ? C7 P1 C1 106.59(15) . . ? N1 P1 Pt1 93.13(10) . . ? C7 P1 Pt1 119.15(11) . . ? C1 P1 Pt1 115.38(11) . . ? C7 P1 P2 132.70(11) . . ? C1 P1 P2 118.29(11) . . ? Pt1 P1 P2 53.64(3) . . ? N2 P2 N1 113.87(15) . . ? N2 P2 C16 104.67(15) . . ? N1 P2 C16 107.20(14) . . ? N2 P2 Pt1 119.22(11) . . ? N1 P2 Pt1 92.93(10) . . ? C16 P2 Pt1 118.33(11) . . ? N2 P2 P1 123.50(11) . . ? C16 P2 P1 128.56(11) . . ? Pt1 P2 P1 53.82(3) . . ? P2 Pt1 P1 72.54(3) . . ? P2 Pt1 Br2 96.35(2) . . ? P1 Pt1 Br2 168.48(2) . . ? P2 Pt1 Br1 170.05(2) . . ? P1 Pt1 Br1 97.78(2) . . ? Br2 Pt1 Br1 93.189(13) . . ? Cl2 C25 Cl1 113.4(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.047 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.105 # Attachment '- 10.cif' data_10 _database_code_depnum_ccdc_archive 'CCDC 780229' #TrackingRef '- 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H66 B2 F8 Fe N6 P4' _chemical_formula_weight 1128.46 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.804(4) _cell_length_b 13.105(3) _cell_length_c 20.917(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.96(3) _cell_angle_gamma 90.00 _cell_volume 5534.2(19) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 50200 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 29.56 _exptl_crystal_description 'part of block' _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8906 _exptl_absorpt_correction_T_max 0.9460 _exptl_absorpt_process_details 'X-SHAPE and X-RED32 (Stoe & Cie, 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE IPDS II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9746 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1242 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9746 _reflns_number_gt 5340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2005)' _computing_cell_refinement X-AREA _computing_data_reduction X-AREA _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP in SHELXTL' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0000P)^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 9746 _refine_ls_number_parameters 610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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 1.0000 0.0000 0.5000 0.01938(17) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 1.0000 0.01987(18) Uani 1 2 d S . . P1 P 0.92469(5) 0.05155(7) 0.55403(5) 0.0228(2) Uani 1 1 d . . . P2 P 0.89741(5) -0.02529(7) 0.43388(5) 0.0224(2) Uani 1 1 d . . . P11 P 0.47728(5) 0.08629(8) 0.90448(5) 0.0221(2) Uani 1 1 d . . . P12 P 0.49857(5) 0.16916(8) 1.02222(5) 0.0227(2) Uani 1 1 d . . . N1 N 0.91628(14) 0.0006(3) 0.62407(13) 0.0332(7) Uani 1 1 d . . . H1A H 0.9311 -0.0622 0.6315 0.040 Uiso 1 1 calc R . . N2 N 0.85862(14) 0.0241(2) 0.49007(14) 0.0228(7) Uani 1 1 d . . . N3 N 0.99713(15) 0.1334(2) 0.46421(14) 0.0236(7) Uani 1 1 d . . . N11 N 0.53009(14) 0.0953(2) 0.85773(13) 0.0283(8) Uani 1 1 d . . . H11A H 0.5713 0.0791 0.8769 0.034 Uiso 1 1 calc R . . N12 N 0.46563(14) 0.1993(2) 0.94145(14) 0.0232(7) Uani 1 1 d . . . N13 N 0.40670(14) -0.0009(3) 0.99043(13) 0.0240(6) Uani 1 1 d . . . C1 C 0.8877(2) 0.0446(3) 0.67571(18) 0.0382(11) Uani 1 1 d . . . H1B H 0.8743 0.1165 0.6631 0.046 Uiso 1 1 calc R . . C2 C 0.8267(2) -0.0136(4) 0.6825(2) 0.0713(16) Uani 1 1 d . . . H2A H 0.7939 -0.0141 0.6401 0.107 Uiso 1 1 calc R . . H2B H 0.8077 0.0195 0.7158 0.107 Uiso 1 1 calc R . . H2C H 0.8390 -0.0840 0.6961 0.107 Uiso 1 1 calc R . . C3 C 0.9381(3) 0.0465(5) 0.7399(2) 0.081(2) Uani 1 1 d . . . H3A H 0.9771 0.0847 0.7350 0.121 Uiso 1 1 calc R . . H3B H 0.9511 -0.0235 0.7537 0.121 Uiso 1 1 calc R . . H3C H 0.9193 0.0795 0.7733 0.121 Uiso 1 1 calc R . . C4 C 0.92348(18) 0.1873(3) 0.57018(18) 0.0246(9) Uani 1 1 d . . . C5 C 0.87744(19) 0.2550(3) 0.53556(19) 0.0312(10) Uani 1 1 d . . . H5A H 0.8401 0.2304 0.5037 0.037 Uiso 1 1 calc R . . C6 C 0.8854(2) 0.3599(3) 0.5472(2) 0.0410(11) Uani 1 1 d . . . H6A H 0.8533 0.4063 0.5236 0.049 Uiso 1 1 calc R . . C7 C 0.9391(2) 0.3956(3) 0.5922(2) 0.0447(12) Uani 1 1 d . . . H7A H 0.9443 0.4669 0.6001 0.054 Uiso 1 1 calc R . . C8 C 0.9855(2) 0.3296(3) 0.6260(2) 0.0487(12) Uani 1 1 d . . . H8A H 1.0233 0.3552 0.6569 0.058 Uiso 1 1 calc R . . C10 C 0.78733(18) 0.0228(3) 0.49301(19) 0.0321(10) Uani 1 1 d . . . H10A H 0.7823 0.0735 0.5272 0.039 Uiso 1 1 calc R . . C9 C 0.9781(2) 0.2254(3) 0.6159(2) 0.0390(11) Uani 1 1 d . . . H9A H 1.0105 0.1798 0.6402 0.047 Uiso 1 1 calc R . . C11 C 0.74080(17) 0.0541(3) 0.4290(2) 0.0439(12) Uani 1 1 d . . . H11B H 0.7545 0.1204 0.4152 0.066 Uiso 1 1 calc R . . H11C H 0.6957 0.0594 0.4351 0.066 Uiso 1 1 calc R . . H11D H 0.7419 0.0029 0.3951 0.066 Uiso 1 1 calc R . . C12 C 0.7657(2) -0.0800(3) 0.5137(2) 0.0511(12) Uani 1 1 d . . . H12A H 0.7959 -0.1011 0.5552 0.077 Uiso 1 1 calc R . . H12B H 0.7667 -0.1306 0.4795 0.077 Uiso 1 1 calc R . . H12C H 0.7206 -0.0746 0.5198 0.077 Uiso 1 1 calc R . . C13 C 0.86233(18) -0.1507(3) 0.40965(18) 0.0280(9) Uani 1 1 d . . . C14 C 0.8650(2) -0.2238(3) 0.4568(2) 0.0395(11) Uani 1 1 d . . . H14A H 0.8830 -0.2069 0.5017 0.047 Uiso 1 1 calc R . . C15 C 0.8421(2) -0.3226(3) 0.4406(2) 0.0507(12) Uani 1 1 d . . . H15A H 0.8450 -0.3722 0.4743 0.061 Uiso 1 1 calc R . . C16 C 0.8154(2) -0.3480(4) 0.3764(3) 0.0577(14) Uani 1 1 d . . . H16A H 0.7998 -0.4154 0.3652 0.069 Uiso 1 1 calc R . . C17 C 0.8112(2) -0.2750(4) 0.3274(3) 0.0601(14) Uani 1 1 d . . . H17A H 0.7931 -0.2922 0.2825 0.072 Uiso 1 1 calc R . . C18 C 0.8334(2) -0.1784(3) 0.3442(2) 0.0443(11) Uani 1 1 d . . . H18A H 0.8292 -0.1284 0.3106 0.053 Uiso 1 1 calc R . . C19 C 0.87970(17) 0.0518(3) 0.35987(17) 0.0235(9) Uani 1 1 d . . . C20 C 0.90204(19) 0.0188(3) 0.30514(19) 0.0354(11) Uani 1 1 d . . . H20A H 0.9237 -0.0452 0.3068 0.042 Uiso 1 1 calc R . . C21 C 0.8931(2) 0.0777(3) 0.2492(2) 0.0414(11) Uani 1 1 d . . . H21A H 0.9064 0.0521 0.2118 0.050 Uiso 1 1 calc R . . C22 C 0.8656(2) 0.1718(4) 0.2469(2) 0.0474(12) Uani 1 1 d . . . H22A H 0.8605 0.2123 0.2083 0.057 Uiso 1 1 calc R . . C23 C 0.8449(2) 0.2091(3) 0.3010(2) 0.0397(11) Uani 1 1 d . . . H23A H 0.8256 0.2750 0.2996 0.048 Uiso 1 1 calc R . . C24 C 0.85270(19) 0.1493(3) 0.3567(2) 0.0319(10) Uani 1 1 d . . . H24A H 0.8393 0.1754 0.3938 0.038 Uiso 1 1 calc R . . C25 C 0.9909(2) 0.2157(3) 0.4452(2) 0.0298(10) Uani 1 1 d . . . C26 C 0.9826(2) 0.3197(3) 0.4224(2) 0.0491(13) Uani 1 1 d . . . H26A H 0.9378 0.3429 0.4222 0.074 Uiso 1 1 calc R . . H26B H 0.9893 0.3236 0.3777 0.074 Uiso 1 1 calc R . . H26C H 1.0151 0.3632 0.4518 0.074 Uiso 1 1 calc R . . C31 C 0.5182(2) 0.1266(3) 0.78797(17) 0.0340(10) Uani 1 1 d . . . H31A H 0.4694 0.1235 0.7684 0.041 Uiso 1 1 calc R . . C32 C 0.5512(2) 0.0505(3) 0.75116(19) 0.0450(12) Uani 1 1 d . . . H32A H 0.5353 -0.0184 0.7572 0.067 Uiso 1 1 calc R . . H32B H 0.5993 0.0533 0.7685 0.067 Uiso 1 1 calc R . . H32C H 0.5401 0.0675 0.7041 0.067 Uiso 1 1 calc R . . C33 C 0.5407(2) 0.2343(3) 0.7798(2) 0.0538(13) Uani 1 1 d . . . H33A H 0.5181 0.2815 0.8034 0.081 Uiso 1 1 calc R . . H33B H 0.5300 0.2521 0.7329 0.081 Uiso 1 1 calc R . . H33C H 0.5887 0.2393 0.7977 0.081 Uiso 1 1 calc R . . C34 C 0.40119(18) 0.0550(3) 0.84422(17) 0.0230(9) Uani 1 1 d . . . C35 C 0.40199(19) -0.0287(3) 0.80399(19) 0.0338(10) Uani 1 1 d . . . H35A H 0.4426 -0.0632 0.8059 0.041 Uiso 1 1 calc R . . C36 C 0.34541(19) -0.0623(3) 0.76158(19) 0.0385(11) Uani 1 1 d . . . H36A H 0.3469 -0.1191 0.7337 0.046 Uiso 1 1 calc R . . C37 C 0.28619(19) -0.0139(3) 0.75928(19) 0.0412(11) Uani 1 1 d . . . H37A H 0.2467 -0.0372 0.7299 0.049 Uiso 1 1 calc R . . C38 C 0.28436(19) 0.0678(3) 0.79937(19) 0.0404(11) Uani 1 1 d . . . H38A H 0.2434 0.1009 0.7979 0.049 Uiso 1 1 calc R . . C39 C 0.34142(19) 0.1025(3) 0.84183(18) 0.0330(10) Uani 1 1 d . . . H39A H 0.3396 0.1593 0.8696 0.040 Uiso 1 1 calc R . . C40 C 0.4456(2) 0.2993(3) 0.9071(2) 0.0353(10) Uani 1 1 d . . . H40A H 0.4351 0.2844 0.8587 0.042 Uiso 1 1 calc R . . C41 C 0.3834(2) 0.3439(3) 0.9211(2) 0.0508(12) Uani 1 1 d . . . H41A H 0.3482 0.2924 0.9123 0.076 Uiso 1 1 calc R . . H41B H 0.3693 0.4032 0.8926 0.076 Uiso 1 1 calc R . . H41C H 0.3923 0.3650 0.9673 0.076 Uiso 1 1 calc R . . C42 C 0.5017(2) 0.3769(3) 0.9200(2) 0.0500(12) Uani 1 1 d . . . H42A H 0.5411 0.3462 0.9101 0.075 Uiso 1 1 calc R . . H42B H 0.5117 0.3976 0.9664 0.075 Uiso 1 1 calc R . . H42C H 0.4883 0.4368 0.8919 0.075 Uiso 1 1 calc R . . C43 C 0.57859(18) 0.2303(3) 1.05065(18) 0.0263(9) Uani 1 1 d . . . C44 C 0.6019(2) 0.2600(3) 1.11579(19) 0.0359(10) Uani 1 1 d . . . H44A H 0.5727 0.2591 1.1443 0.043 Uiso 1 1 calc R . . C45 C 0.6664(2) 0.2907(4) 1.1401(2) 0.0545(14) Uani 1 1 d . . . H45A H 0.6809 0.3113 1.1848 0.065 Uiso 1 1 calc R . . C46 C 0.7102(2) 0.2916(4) 1.0998(2) 0.0576(14) Uani 1 1 d . . . H46A H 0.7550 0.3115 1.1165 0.069 Uiso 1 1 calc R . . C47 C 0.6873(2) 0.2632(3) 1.0349(2) 0.0469(12) Uani 1 1 d . . . H47A H 0.7168 0.2646 1.0065 0.056 Uiso 1 1 calc R . . C48 C 0.62231(19) 0.2327(3) 1.0101(2) 0.0354(10) Uani 1 1 d . . . H48A H 0.6077 0.2133 0.9651 0.042 Uiso 1 1 calc R . . C49 C 0.44888(18) 0.2255(3) 1.07396(17) 0.0252(9) Uani 1 1 d . . . C50 C 0.41097(19) 0.1641(3) 1.10408(18) 0.0336(10) Uani 1 1 d . . . H50A H 0.4124 0.0922 1.0988 0.040 Uiso 1 1 calc R . . C51 C 0.3706(2) 0.2052(4) 1.1422(2) 0.0470(12) Uani 1 1 d . . . H51A H 0.3442 0.1618 1.1619 0.056 Uiso 1 1 calc R . . C52 C 0.3695(2) 0.3092(4) 1.1509(2) 0.0461(12) Uani 1 1 d . . . H52A H 0.3415 0.3382 1.1758 0.055 Uiso 1 1 calc R . . C53 C 0.4094(2) 0.3715(3) 1.1235(2) 0.0419(11) Uani 1 1 d . . . H53A H 0.4102 0.4429 1.1314 0.050 Uiso 1 1 calc R . . C54 C 0.44787(19) 0.3305(3) 1.08452(19) 0.0322(9) Uani 1 1 d . . . H54A H 0.4739 0.3743 1.0647 0.039 Uiso 1 1 calc R . . C55 C 0.35070(19) 0.0025(4) 0.98046(19) 0.0323(10) Uani 1 1 d . . . C56 C 0.27845(18) 0.0099(4) 0.9684(2) 0.0606(15) Uani 1 1 d . . . H56A H 0.2647 -0.0103 1.0083 0.091 Uiso 1 1 calc R . . H56B H 0.2578 -0.0355 0.9320 0.091 Uiso 1 1 calc R . . H56C H 0.2646 0.0804 0.9569 0.091 Uiso 1 1 calc R . . B1 B 0.13532(8) 0.30273(12) 0.35643(9) 0.065(2) Uani 1 1 d G . . F1 F 0.12966(9) 0.38710(12) 0.39262(10) 0.1060(13) Uani 1 1 d G . . F2 F 0.11268(9) 0.32430(15) 0.29121(10) 0.1488(18) Uani 1 1 d G . . F3 F 0.20003(8) 0.27412(14) 0.36868(8) 0.1192(15) Uani 1 1 d G . . F4 F 0.09889(9) 0.22540(13) 0.37320(9) 0.0672(8) Uani 1 1 d G . . B2 B 0.72035(8) 0.12845(15) 0.86393(8) 0.0723(5) Uiso 0.50 1 d PG A 1 F5 F 0.73276(8) 0.06668(17) 0.81569(9) 0.0723(5) Uiso 0.50 1 d PG A 1 F6 F 0.77720(9) 0.14138(16) 0.91204(9) 0.0723(5) Uiso 0.50 1 d PG A 1 F7 F 0.69834(8) 0.22109(14) 0.83758(9) 0.0723(5) Uiso 0.50 1 d PG A 1 F8 F 0.67310(8) 0.08464(17) 0.89042(9) 0.0723(5) Uiso 0.50 1 d PG A 1 B2' B 0.72261(8) 0.11869(15) 0.86730(8) 0.0723(5) Uiso 0.50 1 d PG B 2 F5' F 0.72041(8) 0.11555(17) 0.80116(8) 0.0723(5) Uiso 0.50 1 d PG B 2 F6' F 0.68184(8) 0.04452(17) 0.88210(9) 0.0723(5) Uiso 0.50 1 d PG B 2 F7' F 0.78642(9) 0.10190(17) 0.90283(9) 0.0723(5) Uiso 0.50 1 d PG B 2 F8' F 0.70179(9) 0.21280(16) 0.88310(9) 0.0723(5) Uiso 0.50 1 d PG B 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 0.0231(4) 0.0184(4) 0.0173(4) 0.0003(4) 0.0062(3) 0.0014(4) Fe2 0.0209(4) 0.0214(4) 0.0173(4) 0.0000(4) 0.0046(3) -0.0035(4) P1 0.0262(5) 0.0226(5) 0.0204(5) 0.0000(4) 0.0074(5) 0.0040(4) P2 0.0237(5) 0.0221(6) 0.0216(5) -0.0005(4) 0.0054(4) 0.0001(4) P11 0.0233(5) 0.0246(5) 0.0182(5) 0.0010(4) 0.0047(4) -0.0026(5) P12 0.0266(6) 0.0229(5) 0.0191(5) -0.0017(4) 0.0066(5) -0.0044(5) N1 0.0364(18) 0.0333(17) 0.0332(18) 0.0057(18) 0.0151(15) 0.0075(19) N2 0.0205(16) 0.0236(19) 0.0255(18) -0.0027(14) 0.0080(14) 0.0012(14) N3 0.0250(18) 0.0253(18) 0.0197(18) -0.0042(15) 0.0037(14) -0.0014(15) N11 0.0257(16) 0.041(2) 0.0173(17) 0.0034(15) 0.0042(14) -0.0008(16) N12 0.0273(18) 0.0218(17) 0.0192(17) 0.0028(14) 0.0032(15) 0.0014(14) N13 0.0301(17) 0.0242(15) 0.0179(15) 0.0007(16) 0.0063(13) -0.0025(17) C1 0.051(3) 0.044(3) 0.022(2) 0.002(2) 0.015(2) 0.010(2) C2 0.106(4) 0.056(3) 0.073(4) -0.005(3) 0.062(3) -0.018(3) C3 0.082(4) 0.127(6) 0.034(3) -0.009(3) 0.016(3) 0.026(4) C4 0.028(2) 0.025(2) 0.025(2) -0.0059(18) 0.0132(18) 0.0022(18) C5 0.029(2) 0.031(2) 0.035(2) -0.001(2) 0.0118(19) 0.0074(19) C6 0.042(3) 0.033(3) 0.053(3) 0.003(2) 0.021(2) 0.010(2) C7 0.061(3) 0.024(3) 0.056(3) -0.011(2) 0.026(3) -0.001(2) C8 0.050(3) 0.039(3) 0.054(3) -0.017(2) 0.008(2) -0.001(3) C10 0.023(2) 0.040(3) 0.036(2) -0.006(2) 0.0125(18) -0.0035(19) C9 0.038(3) 0.037(3) 0.038(3) -0.007(2) 0.001(2) 0.010(2) C11 0.021(2) 0.064(3) 0.047(3) -0.004(2) 0.009(2) 0.001(2) C12 0.041(3) 0.056(3) 0.064(3) 0.006(3) 0.028(2) -0.004(3) C13 0.032(2) 0.027(2) 0.027(2) 0.0013(18) 0.0121(19) 0.0041(18) C14 0.035(3) 0.038(3) 0.042(3) 0.002(2) 0.003(2) -0.005(2) C15 0.047(3) 0.041(3) 0.065(3) 0.005(3) 0.015(3) -0.012(2) C16 0.067(4) 0.037(3) 0.070(4) -0.016(3) 0.017(3) -0.017(3) C17 0.068(4) 0.059(3) 0.052(3) -0.021(3) 0.012(3) -0.013(3) C18 0.045(3) 0.038(3) 0.046(3) -0.012(2) 0.001(2) -0.010(2) C19 0.019(2) 0.031(2) 0.018(2) -0.0015(17) 0.0009(16) -0.0002(17) C20 0.036(2) 0.040(3) 0.030(2) 0.005(2) 0.0067(19) 0.011(2) C21 0.045(3) 0.056(3) 0.025(2) 0.007(2) 0.011(2) 0.007(2) C22 0.047(3) 0.055(3) 0.038(3) 0.023(2) 0.006(2) 0.003(3) C23 0.040(3) 0.039(3) 0.040(3) 0.010(2) 0.009(2) 0.003(2) C24 0.032(2) 0.032(2) 0.031(3) 0.0007(19) 0.006(2) 0.000(2) C25 0.032(2) 0.027(2) 0.031(2) -0.001(2) 0.0092(19) -0.003(2) C26 0.056(3) 0.025(2) 0.068(3) 0.011(2) 0.018(3) 0.002(2) C31 0.044(3) 0.044(3) 0.017(2) 0.0057(19) 0.0124(19) -0.007(2) C32 0.058(3) 0.055(3) 0.023(2) 0.001(2) 0.012(2) -0.001(2) C33 0.083(4) 0.047(3) 0.041(3) 0.004(2) 0.034(3) -0.013(3) C34 0.028(2) 0.024(2) 0.017(2) 0.0021(17) 0.0057(17) 0.0000(17) C35 0.026(2) 0.041(3) 0.034(3) -0.001(2) 0.005(2) 0.001(2) C36 0.035(2) 0.039(3) 0.036(3) -0.012(2) -0.003(2) -0.004(2) C37 0.030(2) 0.053(3) 0.033(2) -0.004(2) -0.0060(18) -0.007(2) C38 0.028(2) 0.059(3) 0.030(2) -0.002(2) -0.001(2) 0.009(2) C39 0.033(2) 0.042(3) 0.024(2) -0.005(2) 0.0069(19) 0.002(2) C40 0.052(3) 0.024(2) 0.029(2) 0.0033(19) 0.008(2) 0.004(2) C41 0.061(3) 0.035(3) 0.053(3) -0.001(2) 0.006(3) 0.015(2) C42 0.075(3) 0.028(2) 0.046(3) 0.008(2) 0.012(3) -0.005(2) C43 0.032(2) 0.023(2) 0.024(2) 0.0027(17) 0.0074(18) -0.0046(18) C44 0.037(2) 0.043(3) 0.028(2) -0.005(2) 0.009(2) -0.011(2) C45 0.054(3) 0.070(4) 0.033(3) -0.007(2) 0.000(2) -0.028(3) C46 0.045(3) 0.068(4) 0.051(3) 0.008(3) -0.007(3) -0.027(3) C47 0.046(3) 0.052(3) 0.046(3) -0.003(2) 0.017(2) -0.019(2) C48 0.043(3) 0.032(2) 0.034(3) -0.002(2) 0.013(2) -0.015(2) C49 0.025(2) 0.029(2) 0.020(2) -0.0059(18) 0.0027(17) -0.0007(18) C50 0.040(2) 0.032(2) 0.031(2) -0.007(2) 0.015(2) -0.005(2) C51 0.054(3) 0.052(3) 0.043(3) -0.003(2) 0.029(2) -0.002(2) C52 0.043(3) 0.061(3) 0.038(3) -0.013(2) 0.017(2) 0.014(3) C53 0.046(3) 0.033(2) 0.045(3) -0.008(2) 0.007(2) 0.009(2) C54 0.034(2) 0.032(2) 0.034(2) -0.002(2) 0.0127(19) 0.004(2) C55 0.029(2) 0.040(2) 0.029(2) 0.003(2) 0.0081(18) -0.005(2) C56 0.020(2) 0.091(4) 0.072(3) 0.023(3) 0.013(2) 0.002(3) B1 0.102(6) 0.033(3) 0.083(5) 0.026(3) 0.067(5) 0.016(3) F1 0.121(3) 0.061(2) 0.156(4) -0.017(2) 0.073(3) -0.001(2) F2 0.218(5) 0.139(4) 0.079(3) 0.053(3) 0.018(3) -0.044(4) F3 0.107(3) 0.065(2) 0.212(4) 0.032(3) 0.092(3) 0.011(2) F4 0.083(2) 0.0435(16) 0.090(2) 0.0130(16) 0.0494(18) -0.0009(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 Fe1 N3 1.896(3) 3_756 ? Fe1 N3 1.896(3) . ? Fe1 P1 2.2456(10) 3_756 ? Fe1 P1 2.2456(10) . ? Fe1 P2 2.2701(12) 3_756 ? Fe1 P2 2.2701(12) . ? Fe2 N13 1.903(3) 3_657 ? Fe2 N13 1.903(3) . ? Fe2 P11 2.2446(10) 3_657 ? Fe2 P11 2.2446(10) . ? Fe2 P12 2.2666(11) . ? Fe2 P12 2.2666(11) 3_657 ? P1 N1 1.657(3) . ? P1 N2 1.709(3) . ? P1 C4 1.812(4) . ? P1 P2 2.6390(14) . ? P2 N2 1.706(3) . ? P2 C19 1.810(4) . ? P2 C13 1.820(4) . ? P11 N11 1.642(3) . ? P11 N12 1.715(3) . ? P11 C34 1.817(4) . ? P11 P12 2.6294(15) . ? P12 N12 1.709(3) . ? P12 C43 1.814(4) . ? P12 C49 1.823(3) . ? N1 C1 1.470(4) . ? N1 H1A 0.8800 . ? N2 C10 1.499(4) . ? N3 C25 1.146(4) . ? N11 C31 1.478(4) . ? N11 H11A 0.8800 . ? N12 C40 1.504(5) . ? N13 C55 1.134(4) . ? C1 C3 1.491(6) . ? C1 C2 1.518(5) . ? C1 H1B 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.377(5) . ? C4 C9 1.390(5) . ? C5 C6 1.399(5) . ? C5 H5A 0.9500 . ? C6 C7 1.358(6) . ? C6 H6A 0.9500 . ? C7 C8 1.360(6) . ? C7 H7A 0.9500 . ? C8 C9 1.385(6) . ? C8 H8A 0.9500 . ? C10 C11 1.507(5) . ? C10 C12 1.515(5) . ? C10 H10A 1.0000 . ? C9 H9A 0.9500 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.367(5) . ? C13 C18 1.404(5) . ? C14 C15 1.393(6) . ? C14 H14A 0.9500 . ? C15 C16 1.366(6) . ? C15 H15A 0.9500 . ? C16 C17 1.389(6) . ? C16 H16A 0.9500 . ? C17 C18 1.364(6) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.391(5) . ? C19 C20 1.403(5) . ? C20 C21 1.376(5) . ? C20 H20A 0.9500 . ? C21 C22 1.356(6) . ? C21 H21A 0.9500 . ? C22 C23 1.393(5) . ? C22 H22A 0.9500 . ? C23 C24 1.381(5) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.441(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C31 C33 1.509(5) . ? C31 C32 1.521(5) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C39 1.380(5) . ? C34 C35 1.385(5) . ? C35 C36 1.365(5) . ? C35 H35A 0.9500 . ? C36 C37 1.376(5) . ? C36 H36A 0.9500 . ? C37 C38 1.366(6) . ? C37 H37A 0.9500 . ? C38 C39 1.377(5) . ? C38 H38A 0.9500 . ? C39 H39A 0.9500 . ? C40 C41 1.512(5) . ? C40 C42 1.522(5) . ? C40 H40A 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C48 1.386(5) . ? C43 C44 1.387(5) . ? C44 C45 1.374(6) . ? C44 H44A 0.9500 . ? C45 C46 1.383(6) . ? C45 H45A 0.9500 . ? C46 C47 1.377(6) . ? C46 H46A 0.9500 . ? C47 C48 1.386(5) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C50 1.380(5) . ? C49 C54 1.395(5) . ? C50 C51 1.398(5) . ? C50 H50A 0.9500 . ? C51 C52 1.377(6) . ? C51 H51A 0.9500 . ? C52 C53 1.383(6) . ? C52 H52A 0.9500 . ? C53 C54 1.382(5) . ? C53 H53A 0.9500 . ? C54 H54A 0.9500 . ? C55 C56 1.466(5) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? B1 F4 1.3610 . ? B1 F1 1.3610 . ? B1 F3 1.3611 . ? B1 F2 1.3611 . ? B2 F8 1.3659 . ? B2 F5 1.3659 . ? B2 F6 1.3659 . ? B2 F7 1.3659 . ? B2' F5' 1.3736 . ? B2' F7' 1.3736 . ? B2' F8' 1.3736 . ? B2' F6' 1.3736 . ? 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 N3 Fe1 N3 180.00(17) 3_756 . ? N3 Fe1 P1 87.83(9) 3_756 3_756 ? N3 Fe1 P1 92.17(9) . 3_756 ? N3 Fe1 P1 92.17(9) 3_756 . ? N3 Fe1 P1 87.83(9) . . ? P1 Fe1 P1 180.0 3_756 . ? N3 Fe1 P2 87.62(9) 3_756 3_756 ? N3 Fe1 P2 92.38(9) . 3_756 ? P1 Fe1 P2 71.52(4) 3_756 3_756 ? P1 Fe1 P2 108.48(4) . 3_756 ? N3 Fe1 P2 92.38(9) 3_756 . ? N3 Fe1 P2 87.62(9) . . ? P1 Fe1 P2 108.48(4) 3_756 . ? P1 Fe1 P2 71.52(4) . . ? P2 Fe1 P2 180.00(4) 3_756 . ? N13 Fe2 N13 180.0(2) 3_657 . ? N13 Fe2 P11 85.36(9) 3_657 3_657 ? N13 Fe2 P11 94.64(9) . 3_657 ? N13 Fe2 P11 94.65(9) 3_657 . ? N13 Fe2 P11 85.35(9) . . ? P11 Fe2 P11 180.0 3_657 . ? N13 Fe2 P12 92.06(11) 3_657 . ? N13 Fe2 P12 87.94(11) . . ? P11 Fe2 P12 108.70(4) 3_657 . ? P11 Fe2 P12 71.30(4) . . ? N13 Fe2 P12 87.94(11) 3_657 3_657 ? N13 Fe2 P12 92.05(11) . 3_657 ? P11 Fe2 P12 71.30(4) 3_657 3_657 ? P11 Fe2 P12 108.70(4) . 3_657 ? P12 Fe2 P12 180.0 . 3_657 ? N1 P1 N2 111.77(15) . . ? N1 P1 C4 102.79(17) . . ? N2 P1 C4 107.92(17) . . ? N1 P1 Fe1 123.99(12) . . ? N2 P1 Fe1 94.00(10) . . ? C4 P1 Fe1 115.59(12) . . ? N1 P1 P2 130.09(13) . . ? C4 P1 P2 122.87(13) . . ? Fe1 P1 P2 54.67(3) . . ? N2 P2 C19 110.17(16) . . ? N2 P2 C13 108.06(15) . . ? C19 P2 C13 106.29(17) . . ? N2 P2 Fe1 93.23(11) . . ? C19 P2 Fe1 114.02(12) . . ? C13 P2 Fe1 123.81(13) . . ? C19 P2 P1 123.65(13) . . ? C13 P2 P1 126.12(12) . . ? Fe1 P2 P1 53.81(4) . . ? N11 P11 N12 113.22(15) . . ? N11 P11 C34 101.49(15) . . ? N12 P11 C34 108.26(16) . . ? N11 P11 Fe2 122.60(12) . . ? N12 P11 Fe2 93.22(10) . . ? C34 P11 Fe2 117.72(12) . . ? N11 P11 P12 122.85(12) . . ? C34 P11 P12 131.66(12) . . ? Fe2 P11 P12 54.74(3) . . ? N12 P12 C43 109.84(15) . . ? N12 P12 C49 110.10(16) . . ? C43 P12 C49 103.51(17) . . ? N12 P12 Fe2 92.60(10) . . ? C43 P12 Fe2 116.28(12) . . ? C49 P12 Fe2 123.70(13) . . ? C43 P12 P11 115.05(12) . . ? C49 P12 P11 137.02(13) . . ? Fe2 P12 P11 53.96(3) . . ? C1 N1 P1 129.7(3) . . ? C1 N1 H1A 115.1 . . ? P1 N1 H1A 115.1 . . ? C10 N2 P2 131.4(2) . . ? C10 N2 P1 125.9(2) . . ? P2 N2 P1 101.21(15) . . ? C25 N3 Fe1 173.9(3) . . ? C31 N11 P11 129.2(3) . . ? C31 N11 H11A 115.4 . . ? P11 N11 H11A 115.4 . . ? C40 N12 P12 132.3(2) . . ? C40 N12 P11 126.1(2) . . ? P12 N12 P11 100.33(15) . . ? C55 N13 Fe2 174.9(3) . . ? N1 C1 C3 110.3(3) . . ? N1 C1 C2 111.6(3) . . ? C3 C1 C2 110.2(4) . . ? N1 C1 H1B 108.2 . . ? C3 C1 H1B 108.2 . . ? C2 C1 H1B 108.2 . . ? 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 C9 118.7(4) . . ? C5 C4 P1 125.0(3) . . ? C9 C4 P1 115.8(3) . . ? C4 C5 C6 120.2(4) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C7 C6 C5 120.2(4) . . ? C7 C6 H6A 119.9 . . ? C5 C6 H6A 119.9 . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C7 C8 C9 120.7(4) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? N2 C10 C11 113.0(3) . . ? N2 C10 C12 112.7(3) . . ? C11 C10 C12 108.9(4) . . ? N2 C10 H10A 107.3 . . ? C11 C10 H10A 107.3 . . ? C12 C10 H10A 107.3 . . ? C8 C9 C4 120.1(4) . . ? C8 C9 H9A 120.0 . . ? C4 C9 H9A 120.0 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C11 H11D 109.5 . . ? H11B C11 H11D 109.5 . . ? H11C C11 H11D 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 117.1(4) . . ? C14 C13 P2 119.2(3) . . ? C18 C13 P2 123.7(3) . . ? C13 C14 C15 121.6(4) . . ? C13 C14 H14A 119.2 . . ? C15 C14 H14A 119.2 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 119.8(4) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 119.4(5) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C13 122.1(5) . . ? C17 C18 H18A 119.0 . . ? C13 C18 H18A 119.0 . . ? C24 C19 C20 116.9(3) . . ? C24 C19 P2 123.4(3) . . ? C20 C19 P2 119.1(3) . . ? C21 C20 C19 121.2(4) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C22 C21 C20 120.6(4) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C21 C22 C23 120.1(4) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C24 C23 C22 119.3(4) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C23 C24 C19 121.7(4) . . ? C23 C24 H24A 119.1 . . ? C19 C24 H24A 119.1 . . ? N3 C25 C26 178.9(4) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N11 C31 C33 112.9(3) . . ? N11 C31 C32 109.2(3) . . ? C33 C31 C32 111.5(3) . . ? N11 C31 H31A 107.7 . . ? C33 C31 H31A 107.7 . . ? C32 C31 H31A 107.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 118.5(4) . . ? C39 C34 P11 123.4(3) . . ? C35 C34 P11 117.6(3) . . ? C36 C35 C34 121.0(4) . . ? C36 C35 H35A 119.5 . . ? C34 C35 H35A 119.5 . . ? C35 C36 C37 119.9(4) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C38 C37 C36 119.8(4) . . ? C38 C37 H37A 120.1 . . ? C36 C37 H37A 120.1 . . ? C37 C38 C39 120.5(4) . . ? C37 C38 H38A 119.8 . . ? C39 C38 H38A 119.8 . . ? C38 C39 C34 120.2(4) . . ? C38 C39 H39A 119.9 . . ? C34 C39 H39A 119.9 . . ? N12 C40 C41 113.3(3) . . ? N12 C40 C42 112.6(3) . . ? C41 C40 C42 111.2(3) . . ? N12 C40 H40A 106.4 . . ? C41 C40 H40A 106.4 . . ? C42 C40 H40A 106.4 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 118.0(4) . . ? C48 C43 P12 119.7(3) . . ? C44 C43 P12 121.5(3) . . ? C45 C44 C43 121.6(4) . . ? C45 C44 H44A 119.2 . . ? C43 C44 H44A 119.2 . . ? C44 C45 C46 120.3(4) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C47 C46 C45 118.5(4) . . ? C47 C46 H46A 120.7 . . ? C45 C46 H46A 120.7 . . ? C46 C47 C48 121.3(4) . . ? C46 C47 H47A 119.3 . . ? C48 C47 H47A 119.3 . . ? C43 C48 C47 120.2(4) . . ? C43 C48 H48A 119.9 . . ? C47 C48 H48A 119.9 . . ? C50 C49 C54 118.1(3) . . ? C50 C49 P12 120.2(3) . . ? C54 C49 P12 121.7(3) . . ? C49 C50 C51 121.6(4) . . ? C49 C50 H50A 119.2 . . ? C51 C50 H50A 119.2 . . ? C52 C51 C50 119.2(4) . . ? C52 C51 H51A 120.4 . . ? C50 C51 H51A 120.4 . . ? C51 C52 C53 119.9(4) . . ? C51 C52 H52A 120.0 . . ? C53 C52 H52A 120.0 . . ? C54 C53 C52 120.4(4) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C53 C54 C49 120.7(4) . . ? C53 C54 H54A 119.7 . . ? C49 C54 H54A 119.7 . . ? N13 C55 C56 178.3(5) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? F4 B1 F1 109.5 . . ? F4 B1 F3 109.5 . . ? F1 B1 F3 109.5 . . ? F4 B1 F2 109.5 . . ? F1 B1 F2 109.5 . . ? F3 B1 F2 109.5 . . ? F8 B2 F5 109.5 . . ? F8 B2 F6 109.5 . . ? F5 B2 F6 109.5 . . ? F8 B2 F7 109.5 . . ? F5 B2 F7 109.5 . . ? F6 B2 F7 109.5 . . ? F5' B2' F7' 109.5 . . ? F5' B2' F8' 109.5 . . ? F7' B2' F8' 109.5 . . ? F5' B2' F6' 109.5 . . ? F7' B2' F6' 109.5 . . ? F8' B2' F6' 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.069 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.059