# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dirk Walther' _publ_contact_author_address ; Dirk Walther Friedrich-Schiller-Universitat Jena Institut fur Anorganische und Analytische Chemie August-Bebel-Str. 2 D-07743 Jena Germany ; _publ_contact_author_phone '03641 9-48110 ' _publ_contact_author_fax '03641 9-48102 ' _publ_contact_author_email cdw@rz.uni-jena.de.de # 2. TITLE AND AUTHOR LIST _publ_section_title ; A Key Step of the Formation of Acrylic Acid from CO~2~ and Ethylene: The Transformation of a Nickelalactone into a Nickel-acrylate Complex ; loop_ _publ_author_name 'Dirk Walther' 'Reinald Fischer' 'Helmar Gorls' 'Jens Langer' 'Astrid Malassa' 'Gavin Vaughan' # data_FO1772 _database_code_depnum_ccdc_archive 'CCDC 600545' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H28 N2 Ni O2' _chemical_formula_weight 423.18 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' Ni Ni 0.3393 1.1124 '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 13.3813(3) _cell_length_b 15.6376(3) _cell_length_c 20.5571(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4301.60(16) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.922 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8988 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4887 _reflns_number_gt 3432 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0373P)^2^+2.3076P] 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 4887 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.70010(2) 0.231895(17) 0.675589(13) 0.02473(9) Uani 1 1 d . . . O1 O 0.83453(12) 0.23378(11) 0.69268(8) 0.0357(4) Uani 1 1 d . . . O2 O 0.98322(13) 0.18252(15) 0.66504(9) 0.0583(6) Uani 1 1 d . . . N1 N 0.56110(13) 0.22946(11) 0.66311(8) 0.0256(4) Uani 1 1 d . . . N2 N 0.66254(13) 0.30486(11) 0.75070(8) 0.0264(4) Uani 1 1 d . . . C1 C 0.73032(17) 0.15906(16) 0.60346(11) 0.0352(5) Uani 1 1 d . . . H1A H 0.6905 0.1058 0.6065 0.042 Uiso 1 1 calc R . . H1B H 0.7128 0.1882 0.5623 0.042 Uiso 1 1 calc R . . C2 C 0.83990(17) 0.13787(15) 0.60396(11) 0.0335(5) Uani 1 1 d . . . H2A H 0.8487 0.0757 0.6112 0.040 Uiso 1 1 calc R . . H2B H 0.8694 0.1523 0.5612 0.040 Uiso 1 1 calc R . . C3 C 0.89318(17) 0.18664(16) 0.65651(11) 0.0339(5) Uani 1 1 d . . . C4 C 0.50930(17) 0.26731(15) 0.70751(11) 0.0320(5) Uani 1 1 d . . . H4A H 0.4383 0.2673 0.7075 0.038 Uiso 1 1 calc R . . C5 C 0.56786(16) 0.30998(15) 0.75754(11) 0.0329(5) Uani 1 1 d . . . H5A H 0.5378 0.3396 0.7928 0.040 Uiso 1 1 calc R . . C6 C 0.50809(15) 0.18785(14) 0.61081(10) 0.0276(5) Uani 1 1 d . . . C7 C 0.50762(17) 0.22709(15) 0.55003(11) 0.0344(5) Uani 1 1 d . . . C8 C 0.4593(2) 0.18495(19) 0.49940(12) 0.0481(7) Uani 1 1 d . . . H8A H 0.4589 0.2102 0.4574 0.058 Uiso 1 1 calc R . . C9 C 0.4117(2) 0.10738(19) 0.50841(14) 0.0512(8) Uani 1 1 d . . . C10 C 0.41445(19) 0.07044(17) 0.56922(14) 0.0465(7) Uani 1 1 d . . . H10A H 0.3824 0.0169 0.5756 0.056 Uiso 1 1 calc R . . C11 C 0.46278(17) 0.10899(15) 0.62187(12) 0.0358(5) Uani 1 1 d . . . C12 C 0.5558(2) 0.31231(17) 0.53953(13) 0.0486(7) Uani 1 1 d . . . H12A H 0.5248 0.3547 0.5683 0.073 Uiso 1 1 calc R . . H12B H 0.5468 0.3298 0.4941 0.073 Uiso 1 1 calc R . . H12C H 0.6273 0.3082 0.5493 0.073 Uiso 1 1 calc R . . C13 C 0.3576(3) 0.0647(3) 0.45213(18) 0.0862(13) Uani 1 1 d . . . H13A H 0.3393 0.0062 0.4644 0.129 Uiso 1 1 calc R . . H13B H 0.4016 0.0633 0.4140 0.129 Uiso 1 1 calc R . . H13C H 0.2971 0.0972 0.4417 0.129 Uiso 1 1 calc R . . C14 C 0.4664(2) 0.06576(18) 0.68724(14) 0.0547(8) Uani 1 1 d . . . H14A H 0.4379 0.0082 0.6837 0.082 Uiso 1 1 calc R . . H14B H 0.4276 0.0992 0.7187 0.082 Uiso 1 1 calc R . . H14C H 0.5359 0.0618 0.7019 0.082 Uiso 1 1 calc R . . C15 C 0.72494(15) 0.35201(14) 0.79547(10) 0.0254(5) Uani 1 1 d . . . C16 C 0.74772(16) 0.31884(14) 0.85631(11) 0.0292(5) Uani 1 1 d . . . C17 C 0.80329(17) 0.37003(15) 0.89873(11) 0.0337(5) Uani 1 1 d . . . H17A H 0.8188 0.3488 0.9408 0.040 Uiso 1 1 calc R . . C18 C 0.83644(18) 0.45081(15) 0.88128(12) 0.0341(5) Uani 1 1 d . . . C19 C 0.81623(18) 0.47977(15) 0.81906(12) 0.0375(6) Uani 1 1 d . . . H19A H 0.8416 0.5338 0.8058 0.045 Uiso 1 1 calc R . . C20 C 0.75985(19) 0.43194(15) 0.77548(11) 0.0337(5) Uani 1 1 d . . . C21 C 0.7161(2) 0.22983(16) 0.87594(14) 0.0469(7) Uani 1 1 d . . . H21A H 0.7386 0.1888 0.8430 0.070 Uiso 1 1 calc R . . H21B H 0.6431 0.2275 0.8795 0.070 Uiso 1 1 calc R . . H21C H 0.7461 0.2154 0.9180 0.070 Uiso 1 1 calc R . . C22 C 0.8908(2) 0.50767(17) 0.92900(13) 0.0514(7) Uani 1 1 d . . . H22A H 0.9145 0.4733 0.9658 0.077 Uiso 1 1 calc R . . H22B H 0.8453 0.5521 0.9449 0.077 Uiso 1 1 calc R . . H22C H 0.9481 0.5345 0.9073 0.077 Uiso 1 1 calc R . . C23 C 0.7348(3) 0.46604(19) 0.70890(12) 0.0560(8) Uani 1 1 d . . . H23A H 0.7592 0.4262 0.6757 0.084 Uiso 1 1 calc R . . H23B H 0.7667 0.5219 0.7029 0.084 Uiso 1 1 calc R . . H23C H 0.6622 0.4722 0.7048 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.02074(14) 0.02935(16) 0.02411(14) -0.00282(12) -0.00080(11) -0.00059(12) O1 0.0219(8) 0.0504(10) 0.0347(8) -0.0111(8) -0.0016(7) 0.0010(8) O2 0.0248(9) 0.0953(16) 0.0549(12) -0.0269(11) -0.0006(8) 0.0047(10) N1 0.0234(9) 0.0278(9) 0.0255(9) 0.0008(8) -0.0016(7) -0.0034(8) N2 0.0258(9) 0.0285(9) 0.0249(9) -0.0018(8) -0.0004(8) -0.0007(8) C1 0.0316(12) 0.0423(14) 0.0317(12) -0.0113(10) -0.0052(10) 0.0059(11) C2 0.0329(12) 0.0367(13) 0.0310(12) -0.0025(10) 0.0040(10) -0.0008(11) C3 0.0244(12) 0.0480(14) 0.0294(12) 0.0026(11) 0.0045(9) 0.0009(11) C4 0.0226(11) 0.0410(14) 0.0322(12) -0.0016(11) 0.0003(9) -0.0003(10) C5 0.0290(12) 0.0398(13) 0.0301(12) -0.0059(10) 0.0035(10) 0.0018(10) C6 0.0232(11) 0.0316(12) 0.0280(11) -0.0015(9) -0.0050(9) 0.0011(10) C7 0.0312(12) 0.0393(13) 0.0327(12) 0.0005(11) -0.0030(10) 0.0064(11) C8 0.0473(16) 0.0648(19) 0.0322(13) -0.0082(13) -0.0125(12) 0.0208(15) C9 0.0371(15) 0.0586(18) 0.0578(18) -0.0307(15) -0.0215(13) 0.0164(14) C10 0.0295(13) 0.0386(14) 0.071(2) -0.0178(13) -0.0108(13) -0.0006(11) C11 0.0252(12) 0.0359(13) 0.0465(14) -0.0027(11) -0.0038(11) -0.0023(10) C12 0.0538(17) 0.0475(15) 0.0446(15) 0.0186(12) -0.0003(13) 0.0027(13) C13 0.068(2) 0.104(3) 0.087(3) -0.061(2) -0.039(2) 0.020(2) C14 0.0559(18) 0.0439(16) 0.0641(19) 0.0145(14) -0.0014(15) -0.0148(14) C15 0.0234(11) 0.0283(12) 0.0245(10) -0.0052(9) 0.0023(8) 0.0001(9) C16 0.0258(11) 0.0288(12) 0.0329(12) 0.0005(10) -0.0024(10) -0.0002(10) C17 0.0311(12) 0.0396(13) 0.0304(12) 0.0007(10) -0.0052(10) 0.0002(11) C18 0.0327(12) 0.0325(13) 0.0371(13) -0.0096(10) -0.0024(10) -0.0028(11) C19 0.0448(15) 0.0265(12) 0.0413(14) -0.0006(10) 0.0020(11) -0.0092(11) C20 0.0409(14) 0.0331(13) 0.0269(11) 0.0005(10) 0.0043(11) -0.0037(11) C21 0.0468(16) 0.0374(14) 0.0565(16) 0.0137(12) -0.0181(13) -0.0095(12) C22 0.0581(19) 0.0424(15) 0.0536(17) -0.0113(13) -0.0158(14) -0.0070(14) C23 0.081(2) 0.0542(18) 0.0323(14) 0.0099(12) -0.0020(14) -0.0182(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.8330(16) . ? Ni N1 1.8780(18) . ? Ni C1 1.913(2) . ? Ni N2 1.9846(17) . ? O1 C3 1.309(3) . ? O2 C3 1.219(3) . ? N1 C4 1.290(3) . ? N1 C6 1.443(3) . ? N2 C5 1.277(3) . ? N2 C15 1.445(3) . ? C1 C2 1.503(3) . ? C2 C3 1.502(3) . ? C4 C5 1.455(3) . ? C6 C7 1.392(3) . ? C6 C11 1.393(3) . ? C7 C8 1.391(3) . ? C7 C12 1.496(4) . ? C8 C9 1.382(4) . ? C9 C10 1.378(4) . ? C9 C13 1.519(4) . ? C10 C11 1.398(3) . ? C11 C14 1.505(4) . ? C15 C16 1.388(3) . ? C15 C20 1.396(3) . ? C16 C17 1.398(3) . ? C16 C21 1.510(3) . ? C17 C18 1.386(3) . ? C18 C19 1.383(3) . ? C18 C22 1.511(3) . ? C19 C20 1.390(3) . ? C20 C23 1.507(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni N1 176.79(7) . . ? O1 Ni C1 87.18(8) . . ? N1 Ni C1 95.25(9) . . ? O1 Ni N2 95.17(7) . . ? N1 Ni N2 82.36(7) . . ? C1 Ni N2 177.32(9) . . ? C3 O1 Ni 118.07(14) . . ? C4 N1 C6 118.02(18) . . ? C4 N1 Ni 115.24(15) . . ? C6 N1 Ni 126.71(14) . . ? C5 N2 C15 118.11(18) . . ? C5 N2 Ni 111.90(15) . . ? C15 N2 Ni 129.98(14) . . ? C2 C1 Ni 109.39(15) . . ? C3 C2 C1 110.85(19) . . ? O2 C3 O1 122.7(2) . . ? O2 C3 C2 123.1(2) . . ? O1 C3 C2 114.20(19) . . ? N1 C4 C5 114.9(2) . . ? N2 C5 C4 115.3(2) . . ? C7 C6 C11 122.3(2) . . ? C7 C6 N1 118.18(19) . . ? C11 C6 N1 119.44(19) . . ? C8 C7 C6 117.7(2) . . ? C8 C7 C12 120.9(2) . . ? C6 C7 C12 121.3(2) . . ? C9 C8 C7 122.0(2) . . ? C10 C9 C8 118.5(2) . . ? C10 C9 C13 121.3(3) . . ? C8 C9 C13 120.2(3) . . ? C9 C10 C11 122.3(2) . . ? C6 C11 C10 117.2(2) . . ? C6 C11 C14 122.0(2) . . ? C10 C11 C14 120.8(2) . . ? C16 C15 C20 121.8(2) . . ? C16 C15 N2 120.68(19) . . ? C20 C15 N2 117.56(19) . . ? C15 C16 C17 117.7(2) . . ? C15 C16 C21 121.6(2) . . ? C17 C16 C21 120.7(2) . . ? C18 C17 C16 122.0(2) . . ? C19 C18 C17 118.4(2) . . ? C19 C18 C22 120.1(2) . . ? C17 C18 C22 121.5(2) . . ? C18 C19 C20 121.7(2) . . ? C19 C20 C15 118.3(2) . . ? C19 C20 C23 121.1(2) . . ? C15 C20 C23 120.7(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.319 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.055 #===== END data_FO1727 _database_code_depnum_ccdc_archive 'CCDC 600546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H22 N2 Ni O3' _chemical_formula_weight 385.10 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' Ni Ni 0.3393 1.1124 '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 8.6500(3) _cell_length_b 14.8065(6) _cell_length_c 13.6843(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.718(2) _cell_angle_gamma 90.00 _cell_volume 1740.60(12) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.135 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6956 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0957 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.04 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3972 _reflns_number_gt 2775 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0927P)^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 3972 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1531 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.11756(5) 0.60347(3) 0.75258(3) 0.02650(19) Uani 1 1 d . . . O1 O -0.0697(3) 0.6617(2) 0.76349(19) 0.0342(6) Uani 1 1 d . . . O2 O -0.3031(3) 0.6972(3) 0.6888(2) 0.0525(9) Uani 1 1 d . . . N1 N 0.3034(3) 0.5333(2) 0.7495(2) 0.0298(7) Uani 1 1 d . . . N2 N 0.1677(3) 0.5930(2) 0.8989(2) 0.0282(7) Uani 1 1 d . . . C1 C 0.0415(5) 0.5944(3) 0.6145(3) 0.0323(8) Uani 1 1 d . . . H1A H 0.0817 0.6449 0.5773 0.039 Uiso 1 1 calc R . . H1B H 0.0752 0.5367 0.5870 0.039 Uiso 1 1 calc R . . C2 C -0.1348(5) 0.5985(3) 0.6079(3) 0.0393(9) Uani 1 1 d . . . H2A H -0.1783 0.6240 0.5437 0.047 Uiso 1 1 calc R . . H2B H -0.1777 0.5370 0.6137 0.047 Uiso 1 1 calc R . . C3 C -0.1777(5) 0.6570(3) 0.6903(3) 0.0343(9) Uani 1 1 d . . . C4 C 0.3951(4) 0.5164(3) 0.6786(3) 0.0340(9) Uani 1 1 d . . . C5 C 0.4999(5) 0.4433(3) 0.6882(3) 0.0419(10) Uani 1 1 d . . . H5A H 0.5623 0.4315 0.6369 0.050 Uiso 1 1 calc R . . C6 C 0.5140(5) 0.3892(3) 0.7689(4) 0.0433(10) Uani 1 1 d . . . H6A H 0.5818 0.3386 0.7725 0.052 Uiso 1 1 calc R . . C7 C 0.4276(5) 0.4087(3) 0.8471(3) 0.0365(9) Uani 1 1 d . . . C8 C 0.4405(5) 0.3611(3) 0.9387(4) 0.0442(11) Uani 1 1 d . . . H8A H 0.5046 0.3089 0.9469 0.053 Uiso 1 1 calc R . . C9 C 0.3634(5) 0.3888(3) 1.0140(4) 0.0442(11) Uani 1 1 d . . . H9A H 0.3715 0.3546 1.0731 0.053 Uiso 1 1 calc R . . C10 C 0.2696(5) 0.4691(3) 1.0055(3) 0.0376(9) Uani 1 1 d . . . C11 C 0.1978(5) 0.5075(3) 1.0822(3) 0.0436(11) Uani 1 1 d . . . H11A H 0.2006 0.4772 1.1436 0.052 Uiso 1 1 calc R . . C12 C 0.1238(5) 0.5889(3) 1.0682(3) 0.0406(10) Uani 1 1 d . . . H12A H 0.0810 0.6170 1.1214 0.049 Uiso 1 1 calc R . . C13 C 0.1103(4) 0.6315(3) 0.9748(3) 0.0330(9) Uani 1 1 d . . . C14 C 0.2495(4) 0.5144(3) 0.9148(3) 0.0293(8) Uani 1 1 d . . . C15 C 0.3266(4) 0.4834(3) 0.8352(3) 0.0305(8) Uani 1 1 d . . . C16 C 0.3912(5) 0.5770(3) 0.5912(3) 0.0420(10) Uani 1 1 d . . . H16A H 0.3130 0.6243 0.5954 0.063 Uiso 1 1 calc R . . H16B H 0.3642 0.5416 0.5310 0.063 Uiso 1 1 calc R . . H16C H 0.4937 0.6047 0.5897 0.063 Uiso 1 1 calc R . . C17 C 0.0344(5) 0.7225(3) 0.9624(3) 0.0387(9) Uani 1 1 d . . . H17A H 0.0336 0.7425 0.8941 0.058 Uiso 1 1 calc R . . H17B H 0.0927 0.7660 1.0064 0.058 Uiso 1 1 calc R . . H17C H -0.0728 0.7185 0.9786 0.058 Uiso 1 1 calc R . . O3 O -0.3243(4) 0.8126(3) 0.8486(3) 0.0660(11) Uani 1 1 d . . . C18 C -0.4727(6) 0.8521(4) 0.8375(4) 0.0557(13) Uani 1 1 d . . . H18A H -0.4758 0.8988 0.7855 0.067 Uiso 1 1 calc R . . H18B H -0.4887 0.8830 0.8997 0.067 Uiso 1 1 calc R . . C19 C -0.6003(6) 0.7901(5) 0.8124(6) 0.0780(19) Uani 1 1 d . . . H19A H -0.6989 0.8233 0.8067 0.117 Uiso 1 1 calc R . . H19B H -0.6002 0.7442 0.8641 0.117 Uiso 1 1 calc R . . H19C H -0.5883 0.7607 0.7496 0.117 Uiso 1 1 calc R . . H1O3 H -0.319(6) 0.774(5) 0.794(5) 0.064(17) 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 Ni 0.0316(3) 0.0221(3) 0.0255(3) -0.00024(19) 0.00178(18) 0.00057(18) O1 0.0346(13) 0.0375(16) 0.0299(13) -0.0025(12) 0.0015(11) 0.0074(11) O2 0.0404(16) 0.063(2) 0.0512(18) -0.0088(17) -0.0063(14) 0.0141(16) N1 0.0287(15) 0.0258(16) 0.0337(16) 0.0005(14) -0.0013(13) -0.0026(12) N2 0.0290(15) 0.0246(17) 0.0305(16) -0.0013(13) 0.0013(12) -0.0017(12) C1 0.041(2) 0.030(2) 0.0261(17) -0.0015(15) 0.0020(15) -0.0002(15) C2 0.040(2) 0.040(2) 0.037(2) -0.0025(18) -0.0043(17) 0.0005(17) C3 0.038(2) 0.030(2) 0.034(2) 0.0039(17) 0.0017(16) 0.0030(16) C4 0.0348(19) 0.032(2) 0.036(2) -0.0097(17) 0.0053(16) -0.0034(16) C5 0.038(2) 0.036(2) 0.053(3) -0.015(2) 0.0112(19) -0.0037(18) C6 0.034(2) 0.031(2) 0.063(3) -0.011(2) 0.002(2) 0.0018(17) C7 0.035(2) 0.023(2) 0.051(2) -0.0012(18) 0.0000(18) -0.0002(15) C8 0.041(2) 0.023(2) 0.065(3) 0.009(2) -0.009(2) -0.0008(17) C9 0.044(2) 0.037(2) 0.049(3) 0.016(2) -0.005(2) -0.0076(19) C10 0.038(2) 0.039(2) 0.034(2) 0.0077(18) -0.0019(17) -0.0080(17) C11 0.044(2) 0.056(3) 0.030(2) 0.0150(19) 0.0003(17) -0.015(2) C12 0.041(2) 0.054(3) 0.0280(19) -0.0007(19) 0.0051(17) -0.0067(19) C13 0.0328(19) 0.039(2) 0.0271(18) -0.0034(16) 0.0041(15) -0.0064(16) C14 0.0297(18) 0.0250(19) 0.0317(18) 0.0024(15) -0.0026(15) -0.0044(14) C15 0.0291(18) 0.0232(19) 0.038(2) 0.0012(16) -0.0012(15) -0.0036(14) C16 0.045(2) 0.046(3) 0.037(2) 0.0002(19) 0.0101(18) -0.0080(19) C17 0.046(2) 0.035(2) 0.035(2) -0.0104(18) 0.0061(17) 0.0038(18) O3 0.0485(19) 0.070(3) 0.081(3) -0.019(2) 0.0136(18) -0.0077(18) C18 0.076(3) 0.044(3) 0.049(3) 0.002(2) 0.017(2) 0.012(2) C19 0.042(3) 0.069(4) 0.122(6) 0.016(4) 0.005(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.857(3) . ? Ni N1 1.919(3) . ? Ni C1 1.932(4) . ? Ni N2 2.005(3) . ? O1 C3 1.289(4) . ? O2 C3 1.236(5) . ? N1 C4 1.347(5) . ? N1 C15 1.380(5) . ? N2 C13 1.330(5) . ? N2 C14 1.367(5) . ? C1 C2 1.518(6) . ? C2 C3 1.502(6) . ? C4 C5 1.408(6) . ? C4 C16 1.493(6) . ? C5 C6 1.358(7) . ? C6 C7 1.404(7) . ? C7 C15 1.408(5) . ? C7 C8 1.431(6) . ? C8 C9 1.355(7) . ? C9 C10 1.437(6) . ? C10 C11 1.401(7) . ? C10 C14 1.404(5) . ? C11 C12 1.368(7) . ? C12 C13 1.419(6) . ? C13 C17 1.499(6) . ? C14 C15 1.418(5) . ? O3 C18 1.403(6) . ? C18 C19 1.446(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 O1 Ni N1 173.96(13) . . ? O1 Ni C1 84.87(14) . . ? N1 Ni C1 97.54(15) . . ? O1 Ni N2 92.55(12) . . ? N1 Ni N2 84.03(13) . . ? C1 Ni N2 168.83(15) . . ? C3 O1 Ni 118.2(2) . . ? C4 N1 C15 118.3(3) . . ? C4 N1 Ni 133.0(3) . . ? C15 N1 Ni 108.1(2) . . ? C13 N2 C14 118.4(3) . . ? C13 N2 Ni 133.6(3) . . ? C14 N2 Ni 105.8(2) . . ? C2 C1 Ni 106.2(3) . . ? C3 C2 C1 108.3(3) . . ? O2 C3 O1 122.8(4) . . ? O2 C3 C2 124.0(3) . . ? O1 C3 C2 113.2(3) . . ? N1 C4 C5 120.2(4) . . ? N1 C4 C16 120.4(4) . . ? C5 C4 C16 119.4(4) . . ? C6 C5 C4 121.6(4) . . ? C5 C6 C7 119.6(4) . . ? C6 C7 C15 116.9(4) . . ? C6 C7 C8 124.9(4) . . ? C15 C7 C8 118.1(4) . . ? C9 C8 C7 121.5(4) . . ? C8 C9 C10 120.8(4) . . ? C11 C10 C14 116.7(4) . . ? C11 C10 C9 124.8(4) . . ? C14 C10 C9 118.5(4) . . ? C12 C11 C10 119.6(4) . . ? C11 C12 C13 120.4(4) . . ? N2 C13 C12 120.9(4) . . ? N2 C13 C17 119.7(3) . . ? C12 C13 C17 119.4(4) . . ? N2 C14 C10 123.7(4) . . ? N2 C14 C15 115.8(3) . . ? C10 C14 C15 120.3(4) . . ? N1 C15 C7 123.0(4) . . ? N1 C15 C14 116.4(3) . . ? C7 C15 C14 120.5(4) . . ? O3 C18 C19 115.1(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.058 _refine_diff_density_min -0.888 _refine_diff_density_rms 0.132 #===== END data_FO1150 _database_code_depnum_ccdc_archive 'CCDC 600547' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H28 Ni O2 P2' _chemical_formula_weight 529.16 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' 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' Ni Ni 0.3393 1.1124 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5487(3) _cell_length_b 14.9037(8) _cell_length_c 9.8115(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.807(3) _cell_angle_gamma 90.00 _cell_volume 1257.0(1) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 0.924 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5291 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5291 _reflns_number_gt 4871 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0312P)^2^+0.4064P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _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 -0.007(11) _refine_ls_number_reflns 5291 _refine_ls_number_parameters 418 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.71773(4) 0.14930(2) 0.07176(4) 0.01914(9) Uani 1 1 d . . . P1 P 0.83867(8) 0.10796(5) 0.30199(8) 0.01950(15) Uani 1 1 d . . . P2 P 0.59793(8) 0.25108(5) 0.14919(8) 0.01944(16) Uani 1 1 d . . . O1 O 0.6310(2) 0.19538(16) -0.1276(2) 0.0278(5) Uani 1 1 d . . . O2 O 0.6727(3) 0.2033(2) -0.3335(3) 0.0401(6) Uani 1 1 d . . . C1 C 0.8352(4) 0.0646(3) 0.0076(4) 0.0332(8) Uani 1 1 d . . . H1A H 0.825(5) 0.001(3) 0.030(5) 0.060(14) Uiso 1 1 d . . . H1B H 0.953(6) 0.091(3) 0.062(6) 0.069(14) Uiso 1 1 d . . . C2 C 0.7777(5) 0.0779(3) -0.1625(4) 0.0400(9) Uani 1 1 d . . . H2A H 0.860(5) 0.074(3) -0.200(5) 0.054(12) Uiso 1 1 d . . . H2B H 0.699(6) 0.026(3) -0.230(6) 0.067(14) Uiso 1 1 d . . . C3 C 0.6904(3) 0.1654(2) -0.2159(3) 0.0247(7) Uani 1 1 d . . . C4 C 0.8251(3) 0.2001(2) 0.4226(3) 0.0233(6) Uani 1 1 d . . . H4A H 0.862(4) 0.181(2) 0.521(4) 0.028 Uiso 1 1 d . . . H4B H 0.893(4) 0.246(2) 0.413(3) 0.020(8) Uiso 1 1 d . . . C5 C 0.6547(3) 0.2328(2) 0.3512(3) 0.0236(6) Uani 1 1 d . . . H5A H 0.591(4) 0.187(2) 0.359(4) 0.027(9) Uiso 1 1 d . . . H5B H 0.645(5) 0.292(3) 0.396(5) 0.051(12) Uiso 1 1 d . . . C6 C 1.0458(3) 0.0815(2) 0.3752(3) 0.0232(6) Uani 1 1 d . . . C7 C 1.1603(3) 0.1464(3) 0.4418(3) 0.0278(6) Uani 1 1 d . . . H7 H 1.131(4) 0.202(3) 0.460(4) 0.037(10) Uiso 1 1 d . . . C8 C 1.3165(4) 0.1260(2) 0.4857(4) 0.0361(8) Uani 1 1 d . . . H8 H 1.390(4) 0.165(3) 0.533(4) 0.044(11) Uiso 1 1 d . . . C9 C 1.3591(4) 0.0407(3) 0.4616(4) 0.0350(8) Uani 1 1 d . . . H9 H 1.474(5) 0.028(3) 0.498(5) 0.043(11) Uiso 1 1 d . . . C10 C 1.2459(4) -0.0258(2) 0.3963(4) 0.0332(7) Uani 1 1 d . . . H10 H 1.277(4) -0.089(3) 0.371(4) 0.033(9) Uiso 1 1 d . . . C11 C 1.0898(4) -0.0051(2) 0.3531(4) 0.0280(7) Uani 1 1 d . . . H11 H 1.012(4) -0.053(2) 0.302(4) 0.023(8) Uiso 1 1 d . . . C12 C 0.7581(3) 0.0122(2) 0.3600(3) 0.0227(6) Uani 1 1 d . . . C13 C 0.8341(4) -0.0234(2) 0.5067(4) 0.0295(7) Uani 1 1 d . . . H13 H 0.933(6) 0.003(3) 0.572(6) 0.076(16) Uiso 1 1 d . . . C14 C 0.7680(4) -0.0936(2) 0.5508(4) 0.0362(8) Uani 1 1 d . . . H14 H 0.822(5) -0.113(3) 0.655(5) 0.041(11) Uiso 1 1 d . . . C15 C 0.6253(4) -0.1290(2) 0.4489(4) 0.0358(8) Uani 1 1 d . . . H15 H 0.581(4) -0.173(3) 0.485(4) 0.042(11) Uiso 1 1 d . . . C16 C 0.5507(4) -0.0952(3) 0.3053(4) 0.0344(8) Uani 1 1 d . . . H16 H 0.454(5) -0.120(3) 0.230(4) 0.040(10) Uiso 1 1 d . . . C17 C 0.6152(3) -0.0244(2) 0.2591(4) 0.0263(6) Uani 1 1 d . . . H17 H 0.561(5) -0.001(3) 0.156(5) 0.044(11) Uiso 1 1 d . . . C18 C 0.3854(3) 0.2617(2) 0.0577(3) 0.0221(6) Uani 1 1 d . . . C19 C 0.2941(4) 0.2573(3) 0.1357(4) 0.0379(8) Uani 1 1 d . . . H19 H 0.341(5) 0.248(3) 0.239(5) 0.050(12) Uiso 1 1 d . . . C20 C 0.1332(4) 0.2649(3) 0.0582(5) 0.0442(9) Uani 1 1 d . . . H20 H 0.072(5) 0.257(3) 0.112(5) 0.055(12) Uiso 1 1 d . . . C21 C 0.0624(4) 0.2783(3) -0.0973(5) 0.0411(9) Uani 1 1 d . . . H21 H -0.048(5) 0.284(3) -0.156(4) 0.045(11) Uiso 1 1 d . . . C22 C 0.1524(4) 0.2822(2) -0.1761(4) 0.0353(8) Uani 1 1 d . . . H22 H 0.109(5) 0.288(3) -0.285(5) 0.048(12) Uiso 1 1 d . . . C23 C 0.3142(4) 0.2728(2) -0.0988(4) 0.0282(7) Uani 1 1 d . . . H23 H 0.380(4) 0.270(3) -0.151(4) 0.036(10) Uiso 1 1 d . . . C24 C 0.6673(3) 0.3640(2) 0.1376(3) 0.0206(6) Uani 1 1 d . . . C25 C 0.6119(4) 0.4411(2) 0.1797(4) 0.0319(7) Uani 1 1 d . . . H25 H 0.532(5) 0.440(3) 0.224(5) 0.057(13) Uiso 1 1 d . . . C26 C 0.6657(4) 0.5247(3) 0.1664(4) 0.0374(8) Uani 1 1 d . . . H26 H 0.631(5) 0.576(3) 0.195(5) 0.062(14) Uiso 1 1 d . . . C27 C 0.7770(4) 0.5341(3) 0.1127(4) 0.0370(8) Uani 1 1 d . . . H27 H 0.802(5) 0.590(3) 0.093(5) 0.052(13) Uiso 1 1 d . . . C28 C 0.8332(4) 0.4592(3) 0.0696(5) 0.0407(9) Uani 1 1 d . . . H28 H 0.904(4) 0.470(3) 0.030(4) 0.036(10) Uiso 1 1 d . . . C29 C 0.7788(4) 0.3739(2) 0.0819(4) 0.0311(7) Uani 1 1 d . . . H29 H 0.816(5) 0.316(3) 0.050(5) 0.058(13) 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 Ni 0.02115(16) 0.02178(19) 0.01647(16) 0.00076(16) 0.01004(13) 0.00308(15) P1 0.0201(3) 0.0207(4) 0.0176(3) 0.0008(3) 0.0081(3) 0.0019(3) P2 0.0200(4) 0.0227(4) 0.0181(4) 0.0014(3) 0.0106(3) 0.0031(3) O1 0.0308(11) 0.0342(13) 0.0233(11) 0.0029(9) 0.0163(9) 0.0080(9) O2 0.0314(12) 0.0695(19) 0.0209(12) 0.0118(12) 0.0126(10) 0.0043(12) C1 0.043(2) 0.034(2) 0.0260(18) 0.0016(15) 0.0179(15) 0.0153(16) C2 0.0407(19) 0.053(2) 0.0316(19) -0.0073(17) 0.0206(17) 0.0101(17) C3 0.0178(12) 0.041(2) 0.0134(12) -0.0033(13) 0.0053(10) -0.0054(12) C4 0.0246(14) 0.0290(18) 0.0156(15) -0.0021(12) 0.0080(12) 0.0026(12) C5 0.0250(14) 0.0256(18) 0.0228(15) 0.0004(12) 0.0129(12) 0.0031(12) C6 0.0228(13) 0.0254(16) 0.0216(15) 0.0010(12) 0.0099(12) 0.0026(11) C7 0.0254(13) 0.0247(16) 0.0324(15) 0.0010(16) 0.0118(12) 0.0020(15) C8 0.0268(15) 0.036(2) 0.0404(19) 0.0008(15) 0.0100(15) -0.0042(13) C9 0.0241(16) 0.042(2) 0.038(2) 0.0017(16) 0.0125(14) 0.0043(14) C10 0.0303(16) 0.0315(19) 0.0369(19) 0.0011(15) 0.0137(14) 0.0098(13) C11 0.0236(15) 0.0260(17) 0.0312(18) 0.0017(13) 0.0090(13) 0.0027(12) C12 0.0242(14) 0.0233(16) 0.0232(15) 0.0015(12) 0.0127(12) 0.0015(11) C13 0.0304(16) 0.0314(19) 0.0244(16) 0.0019(14) 0.0097(13) 0.0004(14) C14 0.050(2) 0.0301(19) 0.032(2) 0.0083(15) 0.0206(17) 0.0040(16) C15 0.045(2) 0.0266(19) 0.049(2) -0.0024(16) 0.0329(18) -0.0031(15) C16 0.0302(17) 0.036(2) 0.041(2) -0.0102(16) 0.0199(16) -0.0079(14) C17 0.0234(14) 0.0319(18) 0.0242(16) -0.0042(13) 0.0108(12) -0.0026(12) C18 0.0203(13) 0.0189(15) 0.0271(15) -0.0016(12) 0.0103(12) 0.0012(11) C19 0.0300(17) 0.057(2) 0.0317(19) 0.0000(18) 0.0184(15) 0.0041(16) C20 0.0286(18) 0.061(3) 0.049(2) -0.0056(19) 0.0225(17) 0.0037(16) C21 0.0200(16) 0.038(2) 0.058(2) -0.0038(18) 0.0100(16) 0.0038(13) C22 0.0300(17) 0.0305(19) 0.035(2) 0.0044(15) 0.0047(15) 0.0013(13) C23 0.0242(15) 0.0302(19) 0.0290(17) 0.0029(14) 0.0105(14) -0.0008(12) C24 0.0210(13) 0.0213(16) 0.0180(14) 0.0023(11) 0.0069(11) 0.0026(11) C25 0.0344(17) 0.0288(18) 0.0362(18) -0.0034(14) 0.0189(15) 0.0031(13) C26 0.046(2) 0.0243(19) 0.042(2) -0.0009(16) 0.0191(17) 0.0036(15) C27 0.0372(19) 0.026(2) 0.042(2) 0.0012(16) 0.0122(17) -0.0064(15) C28 0.0390(18) 0.037(2) 0.055(2) 0.0000(17) 0.0278(18) -0.0093(15) C29 0.0254(15) 0.0284(18) 0.044(2) -0.0033(15) 0.0194(15) -0.0023(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.890(2) . ? Ni C1 1.965(3) . ? Ni P1 2.1318(8) . ? Ni P2 2.2233(8) . ? P1 C6 1.829(3) . ? P1 C12 1.825(3) . ? P1 C4 1.854(3) . ? P2 C24 1.830(3) . ? P2 C5 1.834(3) . ? P2 C18 1.834(3) . ? O1 C3 1.304(3) . ? O2 C3 1.228(4) . ? C1 C2 1.526(5) . ? C2 C3 1.514(5) . ? C4 C5 1.544(4) . ? C6 C7 1.392(5) . ? C6 C11 1.403(5) . ? C7 C8 1.394(4) . ? C8 C9 1.386(5) . ? C9 C10 1.398(5) . ? C10 C11 1.396(4) . ? C12 C17 1.401(4) . ? C12 C13 1.404(4) . ? C13 C14 1.385(5) . ? C14 C15 1.396(5) . ? C15 C16 1.369(5) . ? C16 C17 1.393(5) . ? C18 C19 1.390(4) . ? C18 C23 1.392(4) . ? C19 C20 1.390(5) . ? C20 C21 1.388(6) . ? C21 C22 1.386(6) . ? C22 C23 1.400(5) . ? C24 C25 1.400(4) . ? C24 C29 1.400(4) . ? C25 C26 1.377(5) . ? C26 C27 1.384(6) . ? C27 C28 1.382(6) . ? C28 C29 1.398(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 O1 Ni C1 87.48(12) . . ? O1 Ni P1 173.07(7) . . ? C1 Ni P1 91.86(11) . . ? O1 Ni P2 92.68(7) . . ? C1 Ni P2 176.28(13) . . ? P1 Ni P2 87.54(3) . . ? C6 P1 C12 103.85(14) . . ? C6 P1 C4 105.87(14) . . ? C12 P1 C4 102.95(15) . . ? C6 P1 Ni 118.21(10) . . ? C12 P1 Ni 116.66(10) . . ? C4 P1 Ni 107.81(10) . . ? C24 P2 C5 105.00(14) . . ? C24 P2 C18 104.11(13) . . ? C5 P2 C18 106.58(14) . . ? C24 P2 Ni 110.62(9) . . ? C5 P2 Ni 108.32(10) . . ? C18 P2 Ni 121.05(10) . . ? C3 O1 Ni 116.23(19) . . ? C2 C1 Ni 106.4(2) . . ? C3 C2 C1 111.8(3) . . ? O2 C3 O1 123.1(3) . . ? O2 C3 C2 123.4(3) . . ? O1 C3 C2 113.5(3) . . ? C5 C4 P1 107.3(2) . . ? C4 C5 P2 107.1(2) . . ? C7 C6 C11 119.0(3) . . ? C7 C6 P1 121.9(2) . . ? C11 C6 P1 118.9(2) . . ? C6 C7 C8 120.6(3) . . ? C9 C8 C7 120.1(3) . . ? C8 C9 C10 120.1(3) . . ? C9 C10 C11 119.6(3) . . ? C10 C11 C6 120.6(3) . . ? C17 C12 C13 119.1(3) . . ? C17 C12 P1 119.8(2) . . ? C13 C12 P1 121.0(2) . . ? C14 C13 C12 120.2(3) . . ? C13 C14 C15 119.8(3) . . ? C16 C15 C14 120.4(3) . . ? C15 C16 C17 120.5(3) . . ? C16 C17 C12 119.9(3) . . ? C19 C18 C23 119.4(3) . . ? C19 C18 P2 123.5(2) . . ? C23 C18 P2 117.1(2) . . ? C18 C19 C20 120.3(3) . . ? C19 C20 C21 120.4(3) . . ? C22 C21 C20 119.7(3) . . ? C21 C22 C23 120.0(3) . . ? C18 C23 C22 120.2(3) . . ? C25 C24 C29 118.6(3) . . ? C25 C24 P2 122.9(2) . . ? C29 C24 P2 118.6(2) . . ? C26 C25 C24 120.7(3) . . ? C25 C26 C27 120.5(4) . . ? C28 C27 C26 120.0(3) . . ? C27 C28 C29 120.0(3) . . ? C28 C29 C24 120.3(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.453 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.060 #===== END data_FO1337 _database_code_depnum_ccdc_archive 'CCDC 600548' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H44 Ni O2 P2' _chemical_formula_weight 497.25 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' 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.4910(8) _cell_length_b 14.8852(6) _cell_length_c 17.1908(4) _cell_angle_alpha 90.00 _cell_angle_beta 125.904(2) _cell_angle_gamma 90.00 _cell_volume 5076.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 0.909 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9876 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5794 _reflns_number_gt 4799 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0448P)^2^+10.9815P] 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 5794 _refine_ls_number_parameters 271 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.194241(15) 0.98498(2) 0.16598(2) 0.02009(10) Uani 1 1 d . . . P1 P 0.16369(3) 0.91440(4) 0.03901(4) 0.02225(15) Uani 1 1 d . . . P2 P 0.29862(3) 0.94487(5) 0.22829(4) 0.02334(16) Uani 1 1 d . . . O1 O 0.22023(9) 1.05785(13) 0.27252(12) 0.0305(4) Uani 1 1 d . . . O2 O 0.18322(12) 1.15820(14) 0.32756(16) 0.0445(6) Uani 1 1 d . . . C1 C 0.10172(13) 1.0039(2) 0.12330(19) 0.0297(6) Uani 1 1 d . . . H1A H 0.0716 1.0136 0.0530 0.036 Uiso 1 1 calc R . . H1B H 0.0854 0.9510 0.1391 0.036 Uiso 1 1 calc R . . C2 C 0.10294(15) 1.0866(2) 0.1760(2) 0.0371(7) Uani 1 1 d . . . H2A H 0.0880 1.1394 0.1332 0.045 Uiso 1 1 calc R . . H2B H 0.0711 1.0781 0.1931 0.045 Uiso 1 1 calc R . . C3 C 0.17275(15) 1.10379(18) 0.26625(19) 0.0291(6) Uani 1 1 d . . . C4 C 0.23356(14) 0.84455(18) 0.06069(19) 0.0299(6) Uani 1 1 d . . . H4A H 0.2313 0.7843 0.0831 0.036 Uiso 1 1 calc R . . H4B H 0.2289 0.8369 -0.0002 0.036 Uiso 1 1 calc R . . C5 C 0.30227(14) 0.8878(2) 0.13632(19) 0.0320(6) Uani 1 1 d . . . H5A H 0.3139 0.9317 0.1049 0.038 Uiso 1 1 calc R . . H5B H 0.3377 0.8409 0.1669 0.038 Uiso 1 1 calc R . . C6 C 0.09118(15) 0.83824(19) -0.01677(18) 0.0314(6) Uani 1 1 d . A . H6A H 0.0511 0.8748 -0.0348 0.038 Uiso 1 1 calc R . . C7 C 0.07352(18) 0.7903(2) -0.1087(2) 0.0450(8) Uani 1 1 d . A . H7A H 0.0413 0.8266 -0.1663 0.054 Uiso 1 1 calc R . . H7B H 0.1146 0.7803 -0.1059 0.054 Uiso 1 1 calc R . . C8 C 0.0428(3) 0.7032(3) -0.1116(3) 0.0789(15) Uani 1 1 d D . . H8A H 0.0658 0.6535 -0.1200 0.095 Uiso 0.468(11) 1 calc PR A 1 H8B H -0.0054 0.7025 -0.1669 0.095 Uiso 0.468(11) 1 calc PR A 1 H8C H 0.0432 0.6596 -0.1547 0.095 Uiso 0.532(11) 1 calc PR A 2 H8D H -0.0040 0.7109 -0.1316 0.095 Uiso 0.532(11) 1 calc PR A 2 C9 C 0.0491(4) 0.6891(4) -0.0172(3) 0.046(2) Uiso 0.468(11) 1 d PD A 1 H9A H 0.0050 0.6968 -0.0281 0.055 Uiso 0.468(11) 1 calc PR A 1 H9B H 0.0668 0.6285 0.0096 0.055 Uiso 0.468(11) 1 calc PR A 1 C9A C 0.0903(4) 0.6753(3) -0.0070(3) 0.058(2) Uiso 0.532(11) 1 d PD A 2 H9AA H 0.1342 0.6554 0.0085 0.069 Uiso 0.532(11) 1 calc PR A 2 H9AB H 0.0706 0.6260 0.0079 0.069 Uiso 0.532(11) 1 calc PR A 2 C10 C 0.09864(19) 0.7617(2) 0.0498(2) 0.0518(9) Uani 1 1 d D . . H10A H 0.1453 0.7381 0.0890 0.062 Uiso 0.468(11) 1 calc PR A 1 H10B H 0.0875 0.7835 0.0933 0.062 Uiso 0.468(11) 1 calc PR A 1 H10C H 0.0633 0.7656 0.0607 0.062 Uiso 0.532(11) 1 calc PR A 2 H10D H 0.1435 0.7635 0.1125 0.062 Uiso 0.532(11) 1 calc PR A 2 C11 C 0.14196(13) 0.98652(17) -0.06181(17) 0.0242(5) Uani 1 1 d . . . H11A H 0.1297 0.9467 -0.1167 0.029 Uiso 1 1 calc R . . C12 C 0.19883(14) 1.04891(19) -0.04134(19) 0.0295(6) Uani 1 1 d . . . H12A H 0.2318 1.0158 -0.0462 0.035 Uiso 1 1 calc R . . H12B H 0.2227 1.0753 0.0237 0.035 Uiso 1 1 calc R . . C13 C 0.16351(15) 1.1224(2) -0.1188(2) 0.0370(7) Uani 1 1 d . . . H13A H 0.1816 1.1824 -0.0900 0.044 Uiso 1 1 calc R . . H13B H 0.1706 1.1122 -0.1692 0.044 Uiso 1 1 calc R . . C14 C 0.08848(15) 1.1166(2) -0.1614(2) 0.0400(7) Uani 1 1 d . . . H14A H 0.0708 1.1765 -0.1615 0.048 Uiso 1 1 calc R . . H14B H 0.0624 1.0940 -0.2282 0.048 Uiso 1 1 calc R . . C15 C 0.08310(14) 1.0516(2) -0.0975(2) 0.0339(6) Uani 1 1 d . . . H15A H 0.0394 1.0194 -0.1347 0.041 Uiso 1 1 calc R . . H15B H 0.0880 1.0835 -0.0433 0.041 Uiso 1 1 calc R . . C16 C 0.32968(13) 0.86193(19) 0.32467(18) 0.0288(6) Uani 1 1 d . . . H16A H 0.3704 0.8316 0.3366 0.035 Uiso 1 1 calc R . . C17 C 0.27746(14) 0.78996(19) 0.30317(18) 0.0301(6) Uani 1 1 d . . . H17A H 0.2731 0.7444 0.2579 0.036 Uiso 1 1 calc R . . H17B H 0.2328 0.8174 0.2755 0.036 Uiso 1 1 calc R . . C18 C 0.30608(16) 0.7479(2) 0.4020(2) 0.0378(7) Uani 1 1 d . . . H18A H 0.2692 0.7316 0.4073 0.045 Uiso 1 1 calc R . . H18B H 0.3323 0.6931 0.4117 0.045 Uiso 1 1 calc R . . C19 C 0.35153(19) 0.8195(3) 0.4763(2) 0.0546(10) Uani 1 1 d . . . H19A H 0.3985 0.7973 0.5193 0.066 Uiso 1 1 calc R . . H19B H 0.3355 0.8351 0.5158 0.066 Uiso 1 1 calc R . . C20 C 0.34791(16) 0.9021(2) 0.41944(19) 0.0402(7) Uani 1 1 d . . . H20A H 0.3129 0.9447 0.4079 0.048 Uiso 1 1 calc R . . H20B H 0.3918 0.9336 0.4540 0.048 Uiso 1 1 calc R . . C21 C 0.36581(13) 1.02943(18) 0.28500(19) 0.0290(6) Uani 1 1 d . . . H21A H 0.3663 1.0565 0.3387 0.035 Uiso 1 1 calc R . . C22 C 0.43748(15) 0.9959(2) 0.3287(3) 0.0465(8) Uani 1 1 d . . . H22A H 0.4571 0.9676 0.3920 0.056 Uiso 1 1 calc R . . H22B H 0.4377 0.9517 0.2858 0.056 Uiso 1 1 calc R . . C23 C 0.47566(19) 1.0781(4) 0.3387(4) 0.110(2) Uani 1 1 d . . . H23A H 0.5094 1.0633 0.3265 0.132 Uiso 1 1 calc R . . H23B H 0.4997 1.1020 0.4048 0.132 Uiso 1 1 calc R . . C24 C 0.42764(16) 1.1464(2) 0.2685(2) 0.0469(8) Uani 1 1 d . . . H24A H 0.4365 1.1586 0.2203 0.056 Uiso 1 1 calc R . . H24B H 0.4322 1.2032 0.3017 0.056 Uiso 1 1 calc R . . C25 C 0.35721(15) 1.1073(2) 0.2202(2) 0.0441(8) Uani 1 1 d . . . H25A H 0.3392 1.0853 0.1549 0.053 Uiso 1 1 calc R . . H25B H 0.3260 1.1532 0.2153 0.053 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01991(17) 0.02135(18) 0.01796(16) -0.00098(12) 0.01051(13) 0.00018(13) P1 0.0262(3) 0.0206(3) 0.0192(3) -0.0003(2) 0.0129(3) -0.0010(3) P2 0.0207(3) 0.0244(4) 0.0229(3) 0.0031(3) 0.0117(3) 0.0030(3) O1 0.0309(10) 0.0334(11) 0.0244(9) -0.0058(8) 0.0146(8) -0.0013(8) O2 0.0678(15) 0.0358(12) 0.0509(13) -0.0135(10) 0.0465(12) -0.0104(11) C1 0.0229(13) 0.0375(17) 0.0270(13) -0.0035(11) 0.0138(11) -0.0017(11) C2 0.0334(15) 0.0421(18) 0.0435(16) -0.0016(13) 0.0269(14) 0.0045(13) C3 0.0434(16) 0.0233(14) 0.0348(14) -0.0017(11) 0.0308(13) -0.0048(12) C4 0.0393(15) 0.0239(14) 0.0287(13) 0.0015(10) 0.0212(12) 0.0072(12) C5 0.0338(15) 0.0326(16) 0.0348(14) 0.0058(12) 0.0230(12) 0.0102(12) C6 0.0385(15) 0.0296(15) 0.0241(13) -0.0041(11) 0.0171(12) -0.0113(12) C7 0.055(2) 0.0448(19) 0.0324(15) -0.0174(14) 0.0241(15) -0.0216(16) C8 0.125(4) 0.056(3) 0.069(3) -0.029(2) 0.065(3) -0.048(3) C10 0.067(2) 0.046(2) 0.0322(16) 0.0002(14) 0.0236(16) -0.0278(18) C11 0.0278(13) 0.0236(13) 0.0193(11) -0.0001(10) 0.0127(10) -0.0020(11) C12 0.0290(14) 0.0300(15) 0.0301(13) 0.0037(11) 0.0176(12) -0.0011(12) C13 0.0395(16) 0.0344(17) 0.0338(15) 0.0073(12) 0.0196(13) -0.0058(13) C14 0.0398(17) 0.0339(17) 0.0373(16) 0.0128(13) 0.0176(14) 0.0028(14) C15 0.0282(14) 0.0348(16) 0.0339(14) 0.0110(12) 0.0157(12) 0.0025(12) C16 0.0251(13) 0.0300(15) 0.0272(13) 0.0076(11) 0.0131(11) 0.0067(11) C17 0.0342(15) 0.0266(14) 0.0274(13) 0.0010(11) 0.0169(12) 0.0007(12) C18 0.0459(17) 0.0317(16) 0.0341(15) 0.0070(12) 0.0226(14) 0.0020(13) C19 0.061(2) 0.056(2) 0.0289(16) 0.0075(15) 0.0166(15) -0.0184(18) C20 0.0432(17) 0.0415(18) 0.0229(13) 0.0014(12) 0.0122(13) -0.0092(14) C21 0.0216(13) 0.0280(15) 0.0322(14) 0.0044(11) 0.0129(11) 0.0005(11) C22 0.0224(15) 0.049(2) 0.054(2) 0.0089(15) 0.0145(14) 0.0032(14) C23 0.030(2) 0.144(5) 0.118(4) 0.092(4) 0.023(2) 0.000(2) C24 0.0426(18) 0.055(2) 0.0428(17) 0.0006(15) 0.0251(15) -0.0142(16) C25 0.0320(16) 0.0383(18) 0.0456(18) 0.0146(14) 0.0137(14) -0.0015(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.8892(18) . ? Ni C1 1.950(3) . ? Ni P1 2.1242(7) . ? Ni P2 2.1972(7) . ? P1 C11 1.832(2) . ? P1 C6 1.833(3) . ? P1 C4 1.844(3) . ? P2 C21 1.833(3) . ? P2 C16 1.836(3) . ? P2 C5 1.843(3) . ? O1 C3 1.298(3) . ? O2 C3 1.231(3) . ? C1 C2 1.518(4) . ? C2 C3 1.511(4) . ? C4 C5 1.539(4) . ? C6 C7 1.546(4) . ? C6 C10 1.548(4) . ? C7 C8 1.485(5) . ? C8 C9A 1.519(4) . ? C8 C9 1.552(4) . ? C9 C10 1.524(4) . ? C9A C10 1.553(4) . ? C11 C15 1.534(4) . ? C11 C12 1.533(4) . ? C12 C13 1.539(4) . ? C13 C14 1.530(4) . ? C14 C15 1.526(4) . ? C16 C20 1.535(4) . ? C16 C17 1.538(4) . ? C17 C18 1.541(4) . ? C18 C19 1.530(4) . ? C19 C20 1.541(4) . ? C21 C22 1.532(4) . ? C21 C25 1.535(4) . ? C22 C23 1.486(6) . ? C23 C24 1.487(5) . ? C24 C25 1.524(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni C1 86.47(10) . . ? O1 Ni P1 174.60(6) . . ? C1 Ni P1 93.06(8) . . ? O1 Ni P2 92.82(6) . . ? C1 Ni P2 170.32(9) . . ? P1 Ni P2 88.55(3) . . ? C11 P1 C6 102.28(12) . . ? C11 P1 C4 103.99(12) . . ? C6 P1 C4 104.86(14) . . ? C11 P1 Ni 114.45(9) . . ? C6 P1 Ni 119.53(9) . . ? C4 P1 Ni 110.20(9) . . ? C21 P2 C16 102.37(12) . . ? C21 P2 C5 107.04(14) . . ? C16 P2 C5 105.15(13) . . ? C21 P2 Ni 119.84(9) . . ? C16 P2 Ni 111.75(9) . . ? C5 P2 Ni 109.57(9) . . ? C3 O1 Ni 116.48(17) . . ? C2 C1 Ni 106.30(18) . . ? C3 C2 C1 111.4(2) . . ? O2 C3 O1 123.3(3) . . ? O2 C3 C2 122.2(3) . . ? O1 C3 C2 114.5(2) . . ? C5 C4 P1 111.12(18) . . ? C4 C5 P2 109.78(19) . . ? C7 C6 C10 104.8(2) . . ? C7 C6 P1 115.1(2) . . ? C10 C6 P1 114.23(19) . . ? C8 C7 C6 105.7(3) . . ? C7 C8 C9A 100.2(4) . . ? C7 C8 C9 110.2(3) . . ? C9A C8 C9 35.6(3) . . ? C10 C9 C8 104.0(3) . . ? C8 C9A C10 104.2(3) . . ? C9 C10 C6 105.5(3) . . ? C9 C10 C9A 35.5(3) . . ? C6 C10 C9A 103.3(3) . . ? C15 C11 C12 102.9(2) . . ? C15 C11 P1 115.59(18) . . ? C12 C11 P1 114.64(17) . . ? C11 C12 C13 105.0(2) . . ? C14 C13 C12 106.4(2) . . ? C15 C14 C13 106.1(2) . . ? C14 C15 C11 103.4(2) . . ? C20 C16 C17 102.1(2) . . ? C20 C16 P2 113.9(2) . . ? C17 C16 P2 113.92(18) . . ? C16 C17 C18 104.0(2) . . ? C19 C18 C17 106.0(2) . . ? C18 C19 C20 106.4(2) . . ? C16 C20 C19 103.6(3) . . ? C22 C21 C25 103.4(2) . . ? C22 C21 P2 116.7(2) . . ? C25 C21 P2 115.75(19) . . ? C23 C22 C21 104.5(3) . . ? C22 C23 C24 108.9(3) . . ? C23 C24 C25 106.6(3) . . ? C24 C25 C21 105.2(2) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.779 _refine_diff_density_min -0.640 _refine_diff_density_rms 0.081 #===== END data_FO2714 _database_code_depnum_ccdc_archive 'CCDC 600549' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H24 F4 Ni O2 P2 * 1/2 C4 H10 O * C H4 O' _chemical_formula_weight 670.23 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' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 27.6383(5) _cell_length_b 10.5990(2) _cell_length_c 22.8711(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6699.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2776 _exptl_absorpt_coefficient_mu 0.728 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14297 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0700 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7633 _reflns_number_gt 4924 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1004P)^2^+8.7725P] 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 7633 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.2092 _refine_ls_wR_factor_gt 0.1873 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.114761(18) 0.63715(5) 0.21106(3) 0.03362(19) Uani 1 1 d . . . P1 P 0.13649(4) 0.44721(10) 0.21952(5) 0.0312(3) Uani 1 1 d . . . P2 P 0.03921(4) 0.57388(10) 0.22249(5) 0.0312(3) Uani 1 1 d . . . F1 F 0.20350(15) 0.1698(4) 0.01097(15) 0.0926(13) Uani 1 1 d . . . F2 F 0.28844(11) 0.4066(3) 0.40142(13) 0.0659(9) Uani 1 1 d . . . F3 F -0.02212(16) 0.6600(4) 0.46749(15) 0.0944(13) Uani 1 1 d . . . F4 F -0.10931(11) 0.7704(3) 0.05950(13) 0.0640(9) Uani 1 1 d . . . O1 O 0.10054(11) 0.8115(3) 0.21604(15) 0.0418(8) Uani 1 1 d . . . O2 O 0.13502(12) 0.9987(3) 0.22820(18) 0.0579(10) Uani 1 1 d . . . C1 C 0.18240(18) 0.6875(5) 0.2021(3) 0.0662(18) Uani 1 1 d . . . H1A H 0.2016 0.6586 0.2361 0.079 Uiso 1 1 calc R . . H1B H 0.1962 0.6495 0.1662 0.079 Uiso 1 1 calc R . . C2 C 0.1835(2) 0.8241(5) 0.1981(4) 0.0710(19) Uani 1 1 d . . . H2A H 0.1914 0.8483 0.1574 0.085 Uiso 1 1 calc R . . H2B H 0.2098 0.8562 0.2235 0.085 Uiso 1 1 calc R . . C3 C 0.13739(17) 0.8860(5) 0.2152(2) 0.0436(12) Uani 1 1 d . . . C4 C 0.08447(15) 0.3516(4) 0.2441(2) 0.0352(10) Uani 1 1 d . . . H4A H 0.0898 0.2619 0.2339 0.042 Uiso 1 1 calc R . . H4B H 0.0809 0.3582 0.2870 0.042 Uiso 1 1 calc R . . C5 C 0.03870(15) 0.4002(4) 0.2140(2) 0.0355(10) Uani 1 1 d . . . H5A H 0.0095 0.3637 0.2325 0.043 Uiso 1 1 calc R . . H5B H 0.0388 0.3769 0.1721 0.043 Uiso 1 1 calc R . . C6 C 0.15814(15) 0.3638(4) 0.15533(19) 0.0345(10) Uani 1 1 d . . . C7 C 0.16096(19) 0.4252(5) 0.1009(2) 0.0513(13) Uani 1 1 d . . . H7A H 0.1525 0.5118 0.0972 0.062 Uiso 1 1 calc R . . C8 C 0.1763(2) 0.3566(7) 0.0525(2) 0.0699(18) Uani 1 1 d . . . H8A H 0.1783 0.3959 0.0153 0.084 Uiso 1 1 calc R . . C9 C 0.1885(2) 0.2332(6) 0.0587(2) 0.0588(15) Uani 1 1 d . . . C10 C 0.18639(19) 0.1716(5) 0.1103(2) 0.0541(14) Uani 1 1 d . . . H10A H 0.1952 0.0852 0.1131 0.065 Uiso 1 1 calc R . . C11 C 0.17093(16) 0.2379(5) 0.1591(2) 0.0424(11) Uani 1 1 d . . . H11A H 0.1691 0.1961 0.1958 0.051 Uiso 1 1 calc R . . C12 C 0.18280(15) 0.4221(4) 0.27485(18) 0.0321(9) Uani 1 1 d . . . C13 C 0.23190(15) 0.4151(4) 0.25958(19) 0.0343(10) Uani 1 1 d . . . H13A H 0.2408 0.4137 0.2195 0.041 Uiso 1 1 calc R . . C14 C 0.26769(17) 0.4102(4) 0.3019(2) 0.0403(11) Uani 1 1 d . . . H14A H 0.3009 0.4056 0.2915 0.048 Uiso 1 1 calc R . . C15 C 0.25347(18) 0.4123(5) 0.3593(2) 0.0456(11) Uani 1 1 d . . . C16 C 0.20584(19) 0.4182(6) 0.3766(2) 0.0532(13) Uani 1 1 d . . . H16A H 0.1973 0.4175 0.4168 0.064 Uiso 1 1 calc R . . C17 C 0.17089(17) 0.4252(5) 0.3339(2) 0.0437(11) Uani 1 1 d . . . H17A H 0.1379 0.4324 0.3449 0.052 Uiso 1 1 calc R . . C18 C 0.01822(16) 0.6005(4) 0.29702(19) 0.0353(10) Uani 1 1 d . . . C19 C 0.05063(18) 0.6517(5) 0.3373(2) 0.0469(12) Uani 1 1 d . . . H19A H 0.0823 0.6734 0.3248 0.056 Uiso 1 1 calc R . . C20 C 0.0376(2) 0.6716(6) 0.3949(2) 0.0579(14) Uani 1 1 d . . . H20A H 0.0601 0.7045 0.4224 0.070 Uiso 1 1 calc R . . C21 C -0.0083(2) 0.6425(6) 0.4108(2) 0.0641(16) Uani 1 1 d . . . C22 C -0.0419(2) 0.5943(5) 0.3725(2) 0.0523(13) Uani 1 1 d . . . H22A H -0.0738 0.5757 0.3852 0.063 Uiso 1 1 calc R . . C23 C -0.02826(16) 0.5737(4) 0.3156(2) 0.0393(10) Uani 1 1 d . . . H23A H -0.0511 0.5405 0.2887 0.047 Uiso 1 1 calc R . . C24 C -0.00833(15) 0.6316(4) 0.17440(18) 0.0330(9) Uani 1 1 d . . . C25 C -0.05133(16) 0.5659(5) 0.1645(2) 0.0439(11) Uani 1 1 d . . . H25A H -0.0572 0.4887 0.1843 0.053 Uiso 1 1 calc R . . C26 C -0.08543(18) 0.6127(5) 0.1259(2) 0.0511(13) Uani 1 1 d . . . H26A H -0.1148 0.5686 0.1191 0.061 Uiso 1 1 calc R . . C27 C -0.07586(17) 0.7244(5) 0.0977(2) 0.0451(12) Uani 1 1 d . . . C28 C -0.03431(18) 0.7916(5) 0.1066(2) 0.0446(11) Uani 1 1 d . . . H28A H -0.0290 0.8691 0.0867 0.054 Uiso 1 1 calc R . . C29 C 0.00010(15) 0.7449(5) 0.14529(19) 0.0374(10) Uani 1 1 d . . . H29A H 0.0293 0.7901 0.1518 0.045 Uiso 1 1 calc R . . O3 O -0.1471(3) 0.2796(7) 0.5415(3) 0.0554(18) Uiso 0.50 1 d P . . C30 C -0.1127(5) 0.3619(14) 0.4587(7) 0.084(4) Uiso 0.50 1 d P . . H30A H -0.1169 0.3664 0.4162 0.126 Uiso 0.50 1 calc PR . . H30B H -0.0819 0.3206 0.4678 0.126 Uiso 0.50 1 calc PR . . H30C H -0.1128 0.4474 0.4751 0.126 Uiso 0.50 1 calc PR . . C31 C -0.1497(5) 0.2944(14) 0.4824(6) 0.079(4) Uiso 0.50 1 d P . . H31A H -0.1503 0.2099 0.4640 0.095 Uiso 0.50 1 calc PR . . H31B H -0.1806 0.3369 0.4727 0.095 Uiso 0.50 1 calc PR . . C32 C -0.1829(6) 0.2219(17) 0.5688(7) 0.098(5) Uiso 0.50 1 d P . . H32A H -0.1868 0.1367 0.5518 0.118 Uiso 0.50 1 calc PR . . H32B H -0.2132 0.2691 0.5612 0.118 Uiso 0.50 1 calc PR . . C33 C -0.1771(4) 0.2092(11) 0.6309(5) 0.055(3) Uiso 0.50 1 d P . . H33A H -0.2048 0.1635 0.6471 0.082 Uiso 0.50 1 calc PR . . H33B H -0.1751 0.2930 0.6487 0.082 Uiso 0.50 1 calc PR . . H33C H -0.1473 0.1622 0.6392 0.082 Uiso 0.50 1 calc PR . . O1M O -0.0464(2) 0.9622(7) 0.4644(3) 0.066(2) Uiso 0.726(15) 1 d P A -1 H1M1 H -0.0273 0.9075 0.4778 0.099 Uiso 0.726(15) 1 calc PR A -1 C1M C -0.0395(5) 1.024(2) 0.4752(8) 0.105(5) Uiso 0.726(15) 1 d P A -1 H1M2 H -0.0097 1.0165 0.4983 0.158 Uiso 0.726(15) 1 calc PR A -1 H1M3 H -0.0654 1.0576 0.4998 0.158 Uiso 0.726(15) 1 calc PR A -1 H1M4 H -0.0339 1.0808 0.4421 0.158 Uiso 0.726(15) 1 calc PR A -1 O1MA O -0.0570(6) 1.0747(15) 0.4915(7) 0.058(5) Uiso 0.274(15) 1 d P A -2 H1M5 H -0.0800 1.0360 0.5074 0.087 Uiso 0.274(15) 1 calc PR A -2 C1MA C -0.0032(16) 0.963(4) 0.4826(16) 0.121(14) Uiso 0.274(15) 1 d P A -2 H1M6 H 0.0247 0.9969 0.5038 0.181 Uiso 0.274(15) 1 calc PR A -2 H1M7 H 0.0048 0.9550 0.4411 0.181 Uiso 0.274(15) 1 calc PR A -2 H1M8 H -0.0116 0.8799 0.4984 0.181 Uiso 0.274(15) 1 calc PR A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0236(3) 0.0276(3) 0.0496(4) 0.0026(2) 0.0014(2) -0.0015(2) P1 0.0265(5) 0.0301(6) 0.0369(6) 0.0016(5) 0.0018(5) -0.0002(4) P2 0.0245(5) 0.0284(6) 0.0407(6) -0.0020(5) -0.0002(4) -0.0015(4) F1 0.098(3) 0.127(3) 0.053(2) -0.041(2) 0.0016(19) 0.021(3) F2 0.0548(18) 0.088(2) 0.0550(18) 0.0101(17) -0.0230(15) -0.0103(17) F3 0.104(3) 0.130(4) 0.049(2) -0.021(2) 0.020(2) -0.003(3) F4 0.0497(17) 0.093(3) 0.0496(17) 0.0003(16) -0.0153(14) 0.0146(17) O1 0.0282(15) 0.0277(15) 0.070(2) 0.0006(15) -0.0015(15) -0.0020(13) O2 0.0387(19) 0.0331(18) 0.102(3) -0.0003(19) -0.0102(19) -0.0064(15) C1 0.031(3) 0.035(3) 0.132(6) 0.006(3) 0.017(3) -0.001(2) C2 0.037(3) 0.041(3) 0.135(6) -0.010(3) 0.013(3) -0.008(2) C3 0.030(2) 0.035(3) 0.066(3) 0.006(2) -0.006(2) -0.0053(19) C4 0.031(2) 0.030(2) 0.045(3) -0.0015(19) 0.0044(19) -0.0048(18) C5 0.030(2) 0.031(2) 0.046(3) -0.005(2) -0.0005(19) -0.0019(18) C6 0.029(2) 0.037(2) 0.037(2) -0.0026(19) -0.0011(18) 0.0000(19) C7 0.054(3) 0.060(3) 0.040(3) 0.005(2) -0.001(2) 0.009(3) C8 0.075(4) 0.105(5) 0.030(3) 0.005(3) -0.001(3) 0.003(4) C9 0.055(3) 0.079(4) 0.042(3) -0.023(3) -0.003(2) 0.015(3) C10 0.052(3) 0.053(3) 0.057(3) -0.019(3) -0.003(3) 0.010(3) C11 0.039(2) 0.043(3) 0.045(3) -0.005(2) -0.001(2) -0.001(2) C12 0.033(2) 0.029(2) 0.035(2) 0.0022(18) 0.0010(18) 0.0006(18) C13 0.036(2) 0.032(2) 0.036(2) -0.0012(19) 0.0011(19) -0.0022(19) C14 0.033(2) 0.036(2) 0.051(3) -0.001(2) -0.002(2) 0.001(2) C15 0.046(3) 0.048(3) 0.043(3) 0.003(2) -0.013(2) -0.004(2) C16 0.051(3) 0.074(4) 0.035(2) 0.006(3) 0.001(2) -0.011(3) C17 0.036(2) 0.056(3) 0.040(2) 0.002(2) 0.006(2) -0.003(2) C18 0.033(2) 0.031(2) 0.042(2) -0.0032(19) -0.0014(19) 0.0051(18) C19 0.040(3) 0.057(3) 0.044(3) -0.004(2) -0.005(2) -0.006(2) C20 0.057(3) 0.067(4) 0.050(3) -0.012(3) -0.008(3) -0.004(3) C21 0.078(4) 0.073(4) 0.041(3) -0.005(3) 0.008(3) 0.010(3) C22 0.047(3) 0.055(3) 0.054(3) 0.002(3) 0.010(3) 0.004(3) C23 0.031(2) 0.041(3) 0.046(3) 0.003(2) 0.001(2) 0.001(2) C24 0.028(2) 0.038(2) 0.033(2) -0.0058(19) 0.0027(17) 0.0000(18) C25 0.032(2) 0.051(3) 0.049(3) 0.000(2) 0.001(2) -0.004(2) C26 0.033(2) 0.067(4) 0.053(3) -0.005(3) -0.009(2) -0.006(2) C27 0.037(2) 0.065(3) 0.033(2) -0.003(2) -0.006(2) 0.011(2) C28 0.049(3) 0.047(3) 0.039(2) 0.002(2) 0.003(2) 0.008(2) C29 0.030(2) 0.044(3) 0.038(2) -0.005(2) -0.0006(18) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.892(3) . ? Ni C1 1.955(5) . ? Ni P1 2.1098(12) . ? Ni P2 2.2086(12) . ? P1 C6 1.815(4) . ? P1 C12 1.820(4) . ? P1 C4 1.846(4) . ? P2 C24 1.819(4) . ? P2 C18 1.823(5) . ? P2 C5 1.851(4) . ? F1 C9 1.347(6) . ? F2 C15 1.366(5) . ? F3 C21 1.364(6) . ? F4 C27 1.362(5) . ? O1 C3 1.289(6) . ? O2 C3 1.233(6) . ? C1 C2 1.451(7) . ? C2 C3 1.487(7) . ? C4 C5 1.529(6) . ? C6 C11 1.384(6) . ? C6 C7 1.408(6) . ? C7 C8 1.390(8) . ? C8 C9 1.358(9) . ? C9 C10 1.350(8) . ? C10 C11 1.385(7) . ? C12 C17 1.389(6) . ? C12 C13 1.403(6) . ? C13 C14 1.385(6) . ? C14 C15 1.372(7) . ? C15 C16 1.376(7) . ? C16 C17 1.376(7) . ? C18 C23 1.383(6) . ? C18 C19 1.395(6) . ? C19 C20 1.382(7) . ? C20 C21 1.356(8) . ? C21 C22 1.374(8) . ? C22 C23 1.373(7) . ? C24 C25 1.396(6) . ? C24 C29 1.393(6) . ? C25 C26 1.383(7) . ? C26 C27 1.374(7) . ? C27 C28 1.367(7) . ? C28 C29 1.390(6) . ? O3 C32 1.320(17) . ? O3 C31 1.363(14) . ? C30 C31 1.359(18) . ? C32 C33 1.434(19) . ? O1M C1M 0.724(19) . ? O1MA C1MA 1.91(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni C1 86.48(18) . . ? O1 Ni P1 170.15(11) . . ? C1 Ni P1 89.87(16) . . ? O1 Ni P2 95.34(10) . . ? C1 Ni P2 177.98(17) . . ? P1 Ni P2 88.19(4) . . ? C6 P1 C12 105.0(2) . . ? C6 P1 C4 103.6(2) . . ? C12 P1 C4 104.9(2) . . ? C6 P1 Ni 118.97(15) . . ? C12 P1 Ni 113.79(14) . . ? C4 P1 Ni 109.25(14) . . ? C24 P2 C18 106.47(19) . . ? C24 P2 C5 105.4(2) . . ? C18 P2 C5 104.5(2) . . ? C24 P2 Ni 120.61(14) . . ? C18 P2 Ni 111.39(15) . . ? C5 P2 Ni 107.27(14) . . ? C3 O1 Ni 115.7(3) . . ? C2 C1 Ni 107.4(4) . . ? C1 C2 C3 113.9(5) . . ? O2 C3 O1 123.3(5) . . ? O2 C3 C2 122.5(4) . . ? O1 C3 C2 114.3(4) . . ? C5 C4 P1 108.8(3) . . ? C4 C5 P2 106.3(3) . . ? C11 C6 C7 119.1(4) . . ? C11 C6 P1 120.3(3) . . ? C7 C6 P1 120.6(4) . . ? C8 C7 C6 118.6(5) . . ? C9 C8 C7 119.8(5) . . ? F1 C9 C10 118.7(6) . . ? F1 C9 C8 118.2(6) . . ? C10 C9 C8 123.1(5) . . ? C9 C10 C11 118.2(5) . . ? C6 C11 C10 121.2(5) . . ? C17 C12 C13 118.2(4) . . ? C17 C12 P1 120.3(3) . . ? C13 C12 P1 121.0(3) . . ? C14 C13 C12 121.3(4) . . ? C15 C14 C13 117.6(4) . . ? F2 C15 C16 118.5(4) . . ? F2 C15 C14 118.1(4) . . ? C16 C15 C14 123.4(4) . . ? C15 C16 C17 118.0(4) . . ? C16 C17 C12 121.5(4) . . ? C23 C18 C19 118.2(4) . . ? C23 C18 P2 123.5(4) . . ? C19 C18 P2 118.3(4) . . ? C20 C19 C18 121.5(5) . . ? C21 C20 C19 117.7(5) . . ? C20 C21 F3 119.1(6) . . ? C20 C21 C22 123.1(5) . . ? F3 C21 C22 117.8(6) . . ? C23 C22 C21 118.6(5) . . ? C22 C23 C18 120.9(5) . . ? C25 C24 C29 119.6(4) . . ? C25 C24 P2 123.1(4) . . ? C29 C24 P2 117.3(3) . . ? C26 C25 C24 120.4(5) . . ? C27 C26 C25 118.5(5) . . ? C28 C27 F4 118.7(5) . . ? C28 C27 C26 122.7(4) . . ? F4 C27 C26 118.6(4) . . ? C27 C28 C29 119.0(5) . . ? C28 C29 C24 119.8(4) . . ? C32 O3 C31 118.9(11) . . ? C30 C31 O3 114.6(13) . . ? O3 C32 C33 115.3(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.965 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.097 #===== END data_FO2247 _database_code_depnum_ccdc_archive 'CCDC 600550' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H16 F12 Ni O2 P2 * C4 H8 O' _chemical_formula_weight 817.17 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' O O 0.0106 0.0060 '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' Ni Ni 0.3393 1.1124 '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 13.1415(5) _cell_length_b 15.6809(7) _cell_length_c 16.0563(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.673(3) _cell_angle_gamma 90.00 _cell_volume 3261.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.797 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20802 _diffrn_reflns_av_R_equivalents 0.0968 _diffrn_reflns_av_sigmaI/netI 0.0783 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7333 _reflns_number_gt 5158 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1216P)^2^+3.6710P] 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 7333 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.2284 _refine_ls_wR_factor_gt 0.2028 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.75869(5) 0.82063(4) 0.90610(3) 0.0312(2) Uani 1 1 d . . . P1 P 0.68727(9) 0.72734(8) 0.97186(7) 0.0313(3) Uani 1 1 d . . . P2 P 0.71287(9) 0.74199(7) 0.79078(7) 0.0307(3) Uani 1 1 d . . . F1 F 0.3936(3) 0.9444(2) 0.9640(3) 0.0662(10) Uani 1 1 d . . . F2 F 0.2643(3) 0.8284(3) 1.0109(3) 0.0737(11) Uani 1 1 d . . . F3 F 0.3287(3) 0.6681(3) 1.0483(3) 0.0811(13) Uani 1 1 d . . . F4 F 0.8176(3) 0.7594(2) 1.29200(18) 0.0592(9) Uani 1 1 d . . . F5 F 0.9411(3) 0.6223(2) 1.29719(19) 0.0580(9) Uani 1 1 d . . . F6 F 0.9407(3) 0.5268(2) 1.15790(19) 0.0529(8) Uani 1 1 d . . . F7 F 0.8975(3) 0.5035(2) 0.6482(2) 0.0648(10) Uani 1 1 d . . . F8 F 1.0829(3) 0.5798(2) 0.6923(2) 0.0588(9) Uani 1 1 d . . . F9 F 1.1005(3) 0.7224(3) 0.7867(3) 0.0679(10) Uani 1 1 d . . . F10 F 0.5163(3) 0.7263(2) 0.4833(2) 0.0616(10) Uani 1 1 d . . . F11 F 0.5420(3) 0.8937(2) 0.4589(2) 0.0659(10) Uani 1 1 d . . . F12 F 0.6414(3) 0.9923(2) 0.5851(2) 0.0633(10) Uani 1 1 d . . . O1 O 0.8237(3) 0.9049(2) 0.8512(2) 0.0380(7) Uani 1 1 d . . . O2 O 0.9061(3) 1.0290(2) 0.8655(2) 0.0416(8) Uani 1 1 d . . . C1 C 0.8057(4) 0.8831(3) 1.0111(3) 0.0391(11) Uani 1 1 d . . . H1A H 0.7467 0.8952 1.0403 0.047 Uiso 1 1 calc R . . H1B H 0.8571 0.8488 1.0492 0.047 Uiso 1 1 calc R . . C2 C 0.8542(5) 0.9660(4) 0.9877(3) 0.0490(13) Uani 1 1 d . . . H2A H 0.8111 1.0145 1.0005 0.059 Uiso 1 1 calc R . . H2B H 0.9233 0.9724 1.0228 0.059 Uiso 1 1 calc R . . C3 C 0.8647(4) 0.9692(3) 0.8962(3) 0.0362(10) Uani 1 1 d . . . C4 C 0.6618(4) 0.6312(3) 0.9062(3) 0.0348(10) Uani 1 1 d . . . H4A H 0.7257 0.5970 0.9094 0.042 Uiso 1 1 calc R . . H4B H 0.6087 0.5957 0.9265 0.042 Uiso 1 1 calc R . . C5 C 0.6236(4) 0.6597(3) 0.8143(3) 0.0347(10) Uani 1 1 d . . . H5A H 0.5526 0.6828 0.8083 0.042 Uiso 1 1 calc R . . H5B H 0.6234 0.6109 0.7751 0.042 Uiso 1 1 calc R . . C6 C 0.5600(4) 0.7593(3) 0.9921(3) 0.0373(10) Uani 1 1 d . . . C7 C 0.5279(4) 0.8425(3) 0.9751(3) 0.0388(11) Uani 1 1 d . . . H7A H 0.5738 0.8836 0.9588 0.047 Uiso 1 1 calc R . . C8 C 0.4283(4) 0.8647(4) 0.9821(3) 0.0470(13) Uani 1 1 d . . . C9 C 0.3604(4) 0.8066(4) 1.0064(4) 0.0517(14) Uani 1 1 d . . . C10 C 0.3946(5) 0.7239(4) 1.0249(4) 0.0554(15) Uani 1 1 d . . . C11 C 0.4938(4) 0.6988(4) 1.0186(3) 0.0443(12) Uani 1 1 d . . . H11A H 0.5165 0.6421 1.0319 0.053 Uiso 1 1 calc R . . C12 C 0.7554(4) 0.6894(3) 1.0733(3) 0.0337(10) Uani 1 1 d . . . C13 C 0.7532(4) 0.7374(3) 1.1465(3) 0.0400(11) Uani 1 1 d . . . H13A H 0.7087 0.7853 1.1451 0.048 Uiso 1 1 calc R . . C14 C 0.8160(4) 0.7144(4) 1.2203(3) 0.0423(11) Uani 1 1 d . . . C15 C 0.8798(4) 0.6441(4) 1.2243(3) 0.0423(12) Uani 1 1 d . . . C16 C 0.8797(4) 0.5961(3) 1.1519(3) 0.0375(10) Uani 1 1 d . . . C17 C 0.8199(4) 0.6181(3) 1.0768(3) 0.0368(10) Uani 1 1 d . . . H17A H 0.8222 0.5852 1.0274 0.044 Uiso 1 1 calc R . . C18 C 0.8249(4) 0.6863(3) 0.7640(3) 0.0326(10) Uani 1 1 d . . . C19 C 0.8162(4) 0.6104(3) 0.7171(3) 0.0411(11) Uani 1 1 d . . . H19A H 0.7513 0.5831 0.7014 0.049 Uiso 1 1 calc R . . C20 C 0.9043(4) 0.5764(3) 0.6944(3) 0.0428(11) Uani 1 1 d . . . C21 C 0.9985(4) 0.6138(4) 0.7166(3) 0.0431(12) Uani 1 1 d . . . C22 C 1.0067(4) 0.6873(4) 0.7640(4) 0.0462(12) Uani 1 1 d . . . C23 C 0.9212(4) 0.7247(3) 0.7877(3) 0.0404(11) Uani 1 1 d . . . H23A H 0.9277 0.7759 0.8197 0.048 Uiso 1 1 calc R . . C24 C 0.6539(4) 0.7874(3) 0.6898(3) 0.0319(9) Uani 1 1 d . . . C25 C 0.6015(4) 0.7358(3) 0.6245(3) 0.0360(10) Uani 1 1 d . . . H25A H 0.5920 0.6766 0.6332 0.043 Uiso 1 1 calc R . . C26 C 0.5645(4) 0.7730(3) 0.5485(3) 0.0419(11) Uani 1 1 d . . . C27 C 0.5782(4) 0.8593(4) 0.5355(3) 0.0463(13) Uani 1 1 d . . . C28 C 0.6294(4) 0.9080(3) 0.5989(3) 0.0416(11) Uani 1 1 d . . . C29 C 0.6677(4) 0.8733(3) 0.6772(3) 0.0361(10) Uani 1 1 d . . . H29A H 0.7030 0.9080 0.7213 0.043 Uiso 1 1 calc R . . O1T O 0.0354(4) 0.9784(3) 0.6342(3) 0.0757(14) Uani 1 1 d . . . C1T C 0.1213(6) 1.0320(5) 0.6630(6) 0.079(2) Uani 1 1 d . . . H1TA H 0.1065 1.0913 0.6434 0.094 Uiso 1 1 calc R . . H1TB H 0.1831 1.0117 0.6412 0.094 Uiso 1 1 calc R . . C2T C 0.1391(7) 1.0281(6) 0.7587(6) 0.088(3) Uani 1 1 d . . . H2TA H 0.2132 1.0350 0.7824 0.105 Uiso 1 1 calc R . . H2TB H 0.0991 1.0728 0.7824 0.105 Uiso 1 1 calc R . . C3T C 0.1020(7) 0.9417(5) 0.7767(5) 0.079(2) Uani 1 1 d . . . H3TA H 0.0769 0.9399 0.8315 0.095 Uiso 1 1 calc R . . H3TB H 0.1564 0.8981 0.7765 0.095 Uiso 1 1 calc R . . C4T C 0.0150(7) 0.9301(5) 0.7035(4) 0.073(2) Uani 1 1 d . . . H4TA H 0.0083 0.8691 0.6877 0.087 Uiso 1 1 calc R . . H4TB H -0.0508 0.9490 0.7198 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0381(4) 0.0352(3) 0.0212(3) -0.0010(2) 0.0075(2) -0.0007(2) P1 0.0366(6) 0.0369(6) 0.0209(5) 0.0015(4) 0.0063(4) 0.0032(5) P2 0.0374(6) 0.0354(6) 0.0200(5) 0.0005(4) 0.0064(4) -0.0005(5) F1 0.072(2) 0.061(2) 0.071(2) 0.0086(18) 0.0267(19) 0.0265(18) F2 0.046(2) 0.101(3) 0.080(3) 0.009(2) 0.0276(19) 0.0156(19) F3 0.061(2) 0.091(3) 0.101(3) 0.027(2) 0.041(2) -0.006(2) F4 0.080(2) 0.073(2) 0.0224(14) -0.0109(14) 0.0026(14) 0.0154(18) F5 0.066(2) 0.077(2) 0.0268(15) 0.0018(14) -0.0046(13) 0.0161(18) F6 0.064(2) 0.0540(18) 0.0378(16) 0.0032(14) 0.0013(14) 0.0203(15) F7 0.065(2) 0.059(2) 0.071(2) -0.0263(18) 0.0146(18) 0.0098(17) F8 0.0484(18) 0.065(2) 0.069(2) 0.0032(17) 0.0250(16) 0.0134(16) F9 0.0397(19) 0.077(3) 0.089(3) -0.016(2) 0.0157(18) -0.0083(17) F10 0.079(2) 0.064(2) 0.0340(17) 0.0029(15) -0.0133(16) -0.0097(18) F11 0.083(3) 0.071(2) 0.0370(17) 0.0242(16) -0.0089(16) 0.0002(19) F12 0.080(2) 0.0447(18) 0.061(2) 0.0220(16) 0.0002(18) -0.0086(17) O1 0.048(2) 0.0409(18) 0.0261(16) -0.0021(13) 0.0095(14) -0.0079(15) O2 0.049(2) 0.0389(18) 0.0357(18) 0.0004(14) 0.0040(15) -0.0051(15) C1 0.043(3) 0.047(3) 0.028(2) -0.003(2) 0.0050(19) -0.005(2) C2 0.066(4) 0.050(3) 0.033(3) -0.006(2) 0.010(2) -0.010(3) C3 0.037(3) 0.037(2) 0.034(2) -0.0027(19) 0.0040(19) 0.0038(19) C4 0.046(3) 0.037(2) 0.022(2) -0.0006(17) 0.0080(18) -0.002(2) C5 0.040(3) 0.042(2) 0.023(2) 0.0024(18) 0.0077(18) -0.003(2) C6 0.038(3) 0.054(3) 0.022(2) 0.0020(19) 0.0098(18) 0.002(2) C7 0.046(3) 0.046(3) 0.026(2) 0.0025(19) 0.0097(19) 0.003(2) C8 0.053(3) 0.058(3) 0.031(3) 0.003(2) 0.014(2) 0.017(3) C9 0.039(3) 0.080(4) 0.039(3) 0.001(3) 0.016(2) 0.010(3) C10 0.056(4) 0.064(4) 0.050(3) 0.010(3) 0.019(3) -0.003(3) C11 0.044(3) 0.055(3) 0.036(3) 0.009(2) 0.015(2) 0.002(2) C12 0.040(3) 0.040(3) 0.022(2) 0.0028(18) 0.0079(18) -0.0024(19) C13 0.051(3) 0.044(3) 0.028(2) 0.000(2) 0.015(2) 0.003(2) C14 0.051(3) 0.054(3) 0.023(2) -0.004(2) 0.008(2) -0.004(2) C15 0.048(3) 0.056(3) 0.022(2) 0.006(2) 0.0018(19) 0.002(2) C16 0.040(3) 0.042(3) 0.031(2) 0.0068(19) 0.0054(19) 0.006(2) C17 0.043(3) 0.044(3) 0.024(2) 0.0009(19) 0.0067(18) 0.002(2) C18 0.039(3) 0.038(2) 0.022(2) 0.0023(17) 0.0080(18) 0.0024(19) C19 0.046(3) 0.040(3) 0.036(3) -0.005(2) 0.004(2) 0.004(2) C20 0.055(3) 0.041(3) 0.035(3) -0.001(2) 0.012(2) 0.006(2) C21 0.039(3) 0.053(3) 0.039(3) 0.005(2) 0.010(2) 0.009(2) C22 0.033(3) 0.054(3) 0.052(3) 0.004(2) 0.009(2) -0.006(2) C23 0.040(3) 0.046(3) 0.035(3) 0.001(2) 0.008(2) 0.002(2) C24 0.035(2) 0.036(2) 0.025(2) 0.0011(17) 0.0078(17) 0.0038(18) C25 0.047(3) 0.035(2) 0.025(2) 0.0025(18) 0.0058(19) 0.003(2) C26 0.041(3) 0.053(3) 0.027(2) 0.001(2) -0.0049(19) 0.002(2) C27 0.049(3) 0.056(3) 0.032(3) 0.015(2) 0.001(2) 0.003(2) C28 0.046(3) 0.042(3) 0.037(3) 0.010(2) 0.005(2) -0.003(2) C29 0.039(3) 0.041(2) 0.028(2) 0.0011(19) 0.0039(18) 0.001(2) O1T 0.107(4) 0.069(3) 0.053(3) -0.005(2) 0.021(3) -0.013(3) C1T 0.077(5) 0.069(5) 0.098(6) -0.008(4) 0.037(4) 0.000(4) C2T 0.078(5) 0.098(6) 0.080(5) -0.018(5) -0.006(4) 0.018(5) C3T 0.096(6) 0.083(5) 0.062(5) -0.005(4) 0.024(4) 0.016(4) C4T 0.106(6) 0.065(4) 0.051(4) -0.011(3) 0.023(4) -0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.872(3) . ? Ni C1 1.957(5) . ? Ni P1 2.1141(13) . ? Ni P2 2.2218(12) . ? P1 C12 1.821(5) . ? P1 C6 1.827(5) . ? P1 C4 1.838(5) . ? P2 C24 1.820(5) . ? P2 C18 1.825(5) . ? P2 C5 1.826(5) . ? F1 C8 1.345(6) . ? F2 C9 1.323(6) . ? F3 C10 1.330(7) . ? F4 C14 1.347(6) . ? F5 C15 1.349(5) . ? F6 C16 1.345(6) . ? F7 C20 1.357(6) . ? F8 C21 1.345(6) . ? F9 C22 1.343(6) . ? F10 C26 1.345(6) . ? F11 C27 1.354(6) . ? F12 C28 1.353(6) . ? O1 C3 1.303(6) . ? O2 C3 1.228(6) . ? C1 C2 1.522(7) . ? C2 C3 1.500(7) . ? C4 C5 1.544(6) . ? C6 C7 1.383(7) . ? C6 C11 1.401(7) . ? C7 C8 1.377(7) . ? C8 C9 1.377(8) . ? C9 C10 1.387(9) . ? C10 C11 1.382(8) . ? C12 C13 1.399(7) . ? C12 C17 1.399(7) . ? C13 C14 1.374(7) . ? C14 C15 1.381(8) . ? C15 C16 1.383(7) . ? C16 C17 1.369(6) . ? C18 C23 1.395(7) . ? C18 C19 1.403(7) . ? C19 C20 1.378(7) . ? C20 C21 1.362(8) . ? C21 C22 1.376(8) . ? C22 C23 1.376(7) . ? C24 C29 1.379(7) . ? C24 C25 1.409(7) . ? C25 C26 1.366(7) . ? C26 C27 1.385(8) . ? C27 C28 1.358(8) . ? C28 C29 1.384(7) . ? O1T C4T 1.408(8) . ? O1T C1T 1.422(9) . ? C1T C2T 1.517(12) . ? C2T C3T 1.485(12) . ? C3T C4T 1.507(11) . ? 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 Ni C1 87.09(18) . . ? O1 Ni P1 178.15(11) . . ? C1 Ni P1 91.07(15) . . ? O1 Ni P2 94.62(10) . . ? C1 Ni P2 175.81(16) . . ? P1 Ni P2 87.21(5) . . ? C12 P1 C6 104.9(2) . . ? C12 P1 C4 105.1(2) . . ? C6 P1 C4 104.1(2) . . ? C12 P1 Ni 118.69(16) . . ? C6 P1 Ni 113.29(17) . . ? C4 P1 Ni 109.53(15) . . ? C24 P2 C18 102.6(2) . . ? C24 P2 C5 105.6(2) . . ? C18 P2 C5 106.4(2) . . ? C24 P2 Ni 122.69(16) . . ? C18 P2 Ni 110.22(16) . . ? C5 P2 Ni 108.30(15) . . ? C3 O1 Ni 117.7(3) . . ? C2 C1 Ni 107.5(3) . . ? C3 C2 C1 112.4(4) . . ? O2 C3 O1 122.6(4) . . ? O2 C3 C2 122.5(4) . . ? O1 C3 C2 114.8(4) . . ? C5 C4 P1 108.1(3) . . ? C4 C5 P2 106.5(3) . . ? C7 C6 C11 120.9(5) . . ? C7 C6 P1 118.8(4) . . ? C11 C6 P1 120.1(4) . . ? C8 C7 C6 119.0(5) . . ? F1 C8 C7 120.7(5) . . ? F1 C8 C9 117.7(5) . . ? C7 C8 C9 121.6(5) . . ? F2 C9 C8 121.0(6) . . ? F2 C9 C10 120.5(6) . . ? C8 C9 C10 118.6(5) . . ? F3 C10 C11 120.1(6) . . ? F3 C10 C9 118.2(5) . . ? C11 C10 C9 121.7(5) . . ? C10 C11 C6 118.1(5) . . ? C13 C12 C17 119.6(4) . . ? C13 C12 P1 119.9(4) . . ? C17 C12 P1 120.0(3) . . ? C14 C13 C12 119.3(5) . . ? F4 C14 C13 121.4(5) . . ? F4 C14 C15 117.2(4) . . ? C13 C14 C15 121.4(5) . . ? F5 C15 C14 120.8(5) . . ? F5 C15 C16 120.5(5) . . ? C14 C15 C16 118.7(4) . . ? F6 C16 C17 120.9(4) . . ? F6 C16 C15 117.6(4) . . ? C17 C16 C15 121.5(5) . . ? C16 C17 C12 119.4(4) . . ? C23 C18 C19 120.1(5) . . ? C23 C18 P2 117.4(4) . . ? C19 C18 P2 122.4(4) . . ? C20 C19 C18 118.3(5) . . ? F7 C20 C21 118.6(5) . . ? F7 C20 C19 119.3(5) . . ? C21 C20 C19 122.0(5) . . ? F8 C21 C20 120.7(5) . . ? F8 C21 C22 120.0(5) . . ? C20 C21 C22 119.3(5) . . ? F9 C22 C23 120.3(5) . . ? F9 C22 C21 118.5(5) . . ? C23 C22 C21 121.2(5) . . ? C22 C23 C18 119.1(5) . . ? C29 C24 C25 120.8(4) . . ? C29 C24 P2 117.8(4) . . ? C25 C24 P2 121.3(4) . . ? C26 C25 C24 118.4(5) . . ? F10 C26 C25 120.9(5) . . ? F10 C26 C27 118.0(4) . . ? C25 C26 C27 121.0(5) . . ? F11 C27 C28 120.7(5) . . ? F11 C27 C26 119.4(5) . . ? C28 C27 C26 119.9(4) . . ? F12 C28 C27 118.9(5) . . ? F12 C28 C29 119.9(5) . . ? C27 C28 C29 121.2(5) . . ? C24 C29 C28 118.7(5) . . ? C4T O1T C1T 107.9(6) . . ? O1T C1T C2T 106.5(7) . . ? C3T C2T C1T 103.6(7) . . ? C2T C3T C4T 100.9(7) . . ? O1T C4T C3T 109.4(7) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.533 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.136 #===== END data_FO1656 _database_code_depnum_ccdc_archive 'CCDC 600551' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H32 Ni O2 P2 * C3 H7 N O' _chemical_formula_weight 630.31 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' 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 10.0133(9) _cell_length_b 10.9437(9) _cell_length_c 16.2880(1) _cell_angle_alpha 82.934(6) _cell_angle_beta 72.900(7) _cell_angle_gamma 66.730(8) _cell_volume 1567.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green-yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.756 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9865 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6467 _reflns_number_gt 4289 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0542P)^2^+0.1761P] 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 6467 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.57901(4) 0.02973(4) 0.26117(3) 0.02237(14) Uani 1 1 d . . . P1 P 0.76846(9) -0.03535(9) 0.31434(5) 0.0233(2) Uani 1 1 d . . . P2 P 0.64035(9) 0.19199(9) 0.18160(5) 0.0219(2) Uani 1 1 d . . . O1 O 0.4082(2) 0.0860(2) 0.21780(15) 0.0281(6) Uani 1 1 d . . . O2 O 0.1869(2) 0.0718(3) 0.23347(16) 0.0378(7) Uani 1 1 d . . . C1 C 0.5029(4) -0.1012(4) 0.3274(2) 0.0337(9) Uani 1 1 d . . . H1A H 0.5631 -0.1904 0.3014 0.040 Uiso 1 1 calc R . . H1B H 0.5100 -0.1057 0.3871 0.040 Uiso 1 1 calc R . . C2 C 0.3391(4) -0.0581(4) 0.3266(2) 0.0309(8) Uani 1 1 d . . . H2A H 0.3188 -0.1373 0.3198 0.037 Uiso 1 1 calc R . . H2B H 0.2722 -0.0163 0.3821 0.037 Uiso 1 1 calc R . . C3 C 0.3043(3) 0.0389(3) 0.2547(2) 0.0250(8) Uani 1 1 d . . . C4 C 0.9548(3) -0.0910(4) 0.2346(2) 0.0267(8) Uani 1 1 d . . . H4A H 1.0186 -0.0530 0.2505 0.032 Uiso 1 1 calc R . . H4B H 1.0027 -0.1889 0.2392 0.032 Uiso 1 1 calc R . . C5 C 0.9573(4) -0.0551(3) 0.1399(2) 0.0279(8) Uani 1 1 d . . . H5A H 1.0490 -0.1210 0.1033 0.034 Uiso 1 1 calc R . . H5B H 0.8689 -0.0635 0.1292 0.034 Uiso 1 1 calc R . . C6 C 0.9549(3) 0.0837(4) 0.1120(2) 0.0288(8) Uani 1 1 d . . . H6A H 0.9503 0.0976 0.0515 0.035 Uiso 1 1 calc R . . H6B H 1.0515 0.0868 0.1137 0.035 Uiso 1 1 calc R . . C7 C 0.8258(3) 0.1997(3) 0.1650(2) 0.0266(8) Uani 1 1 d . . . H7A H 0.8258 0.2843 0.1355 0.032 Uiso 1 1 calc R . . H7B H 0.8437 0.1996 0.2217 0.032 Uiso 1 1 calc R . . C8 C 0.7933(3) -0.1761(3) 0.3905(2) 0.0273(8) Uani 1 1 d . . . C9 C 0.8289(4) -0.3022(4) 0.3606(2) 0.0332(9) Uani 1 1 d . . . H9A H 0.8440 -0.3143 0.3013 0.040 Uiso 1 1 calc R . . C10 C 0.8425(4) -0.4093(4) 0.4162(3) 0.0412(10) Uani 1 1 d . . . H10A H 0.8674 -0.4950 0.3951 0.049 Uiso 1 1 calc R . . C11 C 0.8199(4) -0.3922(4) 0.5025(3) 0.0439(11) Uani 1 1 d . . . H11A H 0.8295 -0.4660 0.5409 0.053 Uiso 1 1 calc R . . C12 C 0.7832(4) -0.2677(4) 0.5326(3) 0.0416(10) Uani 1 1 d . . . H12A H 0.7678 -0.2561 0.5920 0.050 Uiso 1 1 calc R . . C13 C 0.7685(4) -0.1592(4) 0.4774(2) 0.0337(9) Uani 1 1 d . . . H13A H 0.7414 -0.0734 0.4990 0.040 Uiso 1 1 calc R . . C14 C 0.7575(3) 0.0962(3) 0.3774(2) 0.0255(8) Uani 1 1 d . . . C15 C 0.8830(4) 0.1039(4) 0.3948(2) 0.0412(10) Uani 1 1 d . . . H15A H 0.9813 0.0407 0.3707 0.049 Uiso 1 1 calc R . . C16 C 0.8641(5) 0.2029(5) 0.4466(3) 0.0492(11) Uani 1 1 d . . . H16A H 0.9499 0.2067 0.4582 0.059 Uiso 1 1 calc R . . C17 C 0.7235(5) 0.2964(4) 0.4820(3) 0.0431(10) Uani 1 1 d . . . H17A H 0.7124 0.3650 0.5169 0.052 Uiso 1 1 calc R . . C18 C 0.5996(4) 0.2895(4) 0.4661(2) 0.0417(10) Uani 1 1 d . . . H18A H 0.5020 0.3530 0.4909 0.050 Uiso 1 1 calc R . . C19 C 0.6152(4) 0.1909(4) 0.4142(2) 0.0313(8) Uani 1 1 d . . . H19A H 0.5283 0.1877 0.4035 0.038 Uiso 1 1 calc R . . C20 C 0.5084(3) 0.3540(3) 0.2256(2) 0.0240(8) Uani 1 1 d . . . C21 C 0.5508(4) 0.4438(4) 0.2555(2) 0.0304(8) Uani 1 1 d . . . H21A H 0.6543 0.4234 0.2506 0.036 Uiso 1 1 calc R . . C22 C 0.4428(4) 0.5623(4) 0.2924(2) 0.0372(9) Uani 1 1 d . . . H22A H 0.4727 0.6217 0.3136 0.045 Uiso 1 1 calc R . . C23 C 0.2908(4) 0.5955(4) 0.2988(2) 0.0367(9) Uani 1 1 d . . . H23A H 0.2174 0.6774 0.3238 0.044 Uiso 1 1 calc R . . C24 C 0.2481(4) 0.5089(4) 0.2687(2) 0.0338(9) Uani 1 1 d . . . H24A H 0.1448 0.5315 0.2720 0.041 Uiso 1 1 calc R . . C25 C 0.3551(4) 0.3884(4) 0.2335(2) 0.0296(8) Uani 1 1 d . . . H25A H 0.3236 0.3281 0.2144 0.036 Uiso 1 1 calc R . . C26 C 0.6262(3) 0.2009(3) 0.0713(2) 0.0231(7) Uani 1 1 d . . . C27 C 0.6217(4) 0.3136(4) 0.0202(2) 0.0305(8) Uani 1 1 d . . . H27A H 0.6217 0.3889 0.0436 0.037 Uiso 1 1 calc R . . C28 C 0.6171(4) 0.3170(4) -0.0640(2) 0.0358(9) Uani 1 1 d . . . H28A H 0.6140 0.3942 -0.0984 0.043 Uiso 1 1 calc R . . C29 C 0.6170(4) 0.2074(4) -0.0980(2) 0.0351(9) Uani 1 1 d . . . H29A H 0.6131 0.2098 -0.1558 0.042 Uiso 1 1 calc R . . C30 C 0.6224(4) 0.0945(4) -0.0488(2) 0.0315(9) Uani 1 1 d . . . H30A H 0.6233 0.0190 -0.0725 0.038 Uiso 1 1 calc R . . C31 C 0.6265(4) 0.0922(4) 0.0357(2) 0.0281(8) Uani 1 1 d . . . H31A H 0.6294 0.0147 0.0698 0.034 Uiso 1 1 calc R . . N1 N 0.0966(4) 0.4282(5) 0.1060(3) 0.0672(12) Uani 1 1 d . . . O3 O -0.1008(4) 0.4773(4) 0.2227(3) 0.0895(13) Uani 1 1 d . . . C32 C 0.0135(5) 0.3964(5) 0.1780(3) 0.0540(12) Uani 1 1 d . . . H32A H 0.0442 0.3058 0.1959 0.065 Uiso 1 1 calc R . . C33 C 0.2276(5) 0.3295(7) 0.0575(4) 0.099(2) Uani 1 1 d . . . H33A H 0.2378 0.2423 0.0844 0.148 Uiso 1 1 calc R . . H33B H 0.3163 0.3486 0.0555 0.148 Uiso 1 1 calc R . . H33C H 0.2196 0.3293 -0.0010 0.148 Uiso 1 1 calc R . . C34 C 0.0533(7) 0.5711(6) 0.0776(4) 0.094(2) Uani 1 1 d . . . H34A H -0.0406 0.6256 0.1179 0.141 Uiso 1 1 calc R . . H34B H 0.0382 0.5796 0.0200 0.141 Uiso 1 1 calc R . . H34C H 0.1338 0.6014 0.0762 0.141 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0181(2) 0.0239(3) 0.0270(3) 0.00357(19) -0.00930(17) -0.00877(18) P1 0.0185(4) 0.0252(5) 0.0261(5) 0.0018(4) -0.0082(4) -0.0071(4) P2 0.0173(4) 0.0228(5) 0.0270(5) 0.0015(4) -0.0084(4) -0.0077(4) O1 0.0206(11) 0.0319(14) 0.0384(14) 0.0092(11) -0.0142(10) -0.0149(10) O2 0.0251(13) 0.0548(18) 0.0433(16) 0.0093(13) -0.0182(12) -0.0215(12) C1 0.0284(18) 0.035(2) 0.044(2) 0.0139(18) -0.0167(17) -0.0183(17) C2 0.0285(18) 0.037(2) 0.031(2) 0.0059(17) -0.0093(15) -0.0170(17) C3 0.0206(17) 0.025(2) 0.0295(19) -0.0050(15) -0.0052(14) -0.0086(15) C4 0.0186(16) 0.027(2) 0.0279(19) -0.0002(15) -0.0057(14) -0.0025(14) C5 0.0191(16) 0.031(2) 0.031(2) -0.0049(16) -0.0066(14) -0.0052(15) C6 0.0189(17) 0.039(2) 0.0266(19) 0.0006(16) -0.0036(14) -0.0110(16) C7 0.0216(17) 0.029(2) 0.032(2) 0.0023(16) -0.0112(15) -0.0100(15) C8 0.0196(16) 0.030(2) 0.033(2) 0.0049(16) -0.0104(15) -0.0087(15) C9 0.0270(19) 0.035(2) 0.031(2) 0.0049(17) -0.0055(16) -0.0074(16) C10 0.033(2) 0.034(2) 0.047(3) 0.010(2) -0.0089(18) -0.0075(18) C11 0.031(2) 0.046(3) 0.049(3) 0.026(2) -0.0150(18) -0.0138(19) C12 0.039(2) 0.060(3) 0.034(2) 0.016(2) -0.0191(18) -0.025(2) C13 0.034(2) 0.039(2) 0.033(2) 0.0060(18) -0.0132(16) -0.0164(17) C14 0.0259(17) 0.029(2) 0.0233(18) 0.0032(15) -0.0080(14) -0.0120(15) C15 0.0264(19) 0.059(3) 0.045(2) -0.009(2) -0.0117(17) -0.0191(19) C16 0.049(3) 0.068(3) 0.047(3) -0.010(2) -0.013(2) -0.036(2) C17 0.056(3) 0.043(3) 0.038(2) -0.009(2) -0.009(2) -0.027(2) C18 0.048(2) 0.035(2) 0.034(2) -0.0051(18) -0.0079(18) -0.0079(19) C19 0.0266(18) 0.038(2) 0.030(2) -0.0044(17) -0.0081(15) -0.0120(16) C20 0.0196(16) 0.026(2) 0.0239(18) 0.0025(15) -0.0064(14) -0.0069(14) C21 0.0268(18) 0.032(2) 0.034(2) 0.0029(17) -0.0114(15) -0.0109(16) C22 0.045(2) 0.030(2) 0.038(2) -0.0026(18) -0.0144(18) -0.0129(18) C23 0.035(2) 0.029(2) 0.033(2) -0.0008(17) -0.0054(17) -0.0017(17) C24 0.0277(19) 0.032(2) 0.033(2) -0.0012(17) -0.0061(16) -0.0038(16) C25 0.0259(18) 0.033(2) 0.031(2) 0.0046(17) -0.0104(15) -0.0125(16) C26 0.0172(16) 0.024(2) 0.0276(19) 0.0028(15) -0.0071(13) -0.0075(14) C27 0.0305(19) 0.029(2) 0.031(2) -0.0010(17) -0.0083(16) -0.0102(16) C28 0.037(2) 0.033(2) 0.030(2) 0.0094(17) -0.0097(17) -0.0085(17) C29 0.034(2) 0.044(3) 0.026(2) 0.0014(18) -0.0098(16) -0.0118(18) C30 0.0306(19) 0.031(2) 0.034(2) -0.0054(17) -0.0088(16) -0.0118(16) C31 0.0254(17) 0.028(2) 0.030(2) 0.0018(16) -0.0080(15) -0.0096(15) N1 0.043(2) 0.090(3) 0.079(3) -0.006(3) -0.028(2) -0.026(2) O3 0.067(2) 0.089(3) 0.109(3) -0.042(3) -0.004(2) -0.028(2) C32 0.048(3) 0.064(3) 0.066(3) -0.008(3) -0.016(2) -0.036(3) C33 0.043(3) 0.167(7) 0.075(4) -0.019(4) -0.015(3) -0.024(4) C34 0.120(5) 0.085(5) 0.127(5) 0.038(4) -0.073(4) -0.072(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.891(2) . ? Ni C1 1.949(4) . ? Ni P1 2.1454(9) . ? Ni P2 2.2444(10) . ? P1 C14 1.820(3) . ? P1 C8 1.839(4) . ? P1 C4 1.848(3) . ? P2 C20 1.819(3) . ? P2 C7 1.830(3) . ? P2 C26 1.831(3) . ? O1 C3 1.300(4) . ? O2 C3 1.226(4) . ? C1 C2 1.521(4) . ? C2 C3 1.504(5) . ? C4 C5 1.539(5) . ? C5 C6 1.524(5) . ? C6 C7 1.531(4) . ? C8 C13 1.385(5) . ? C8 C9 1.393(5) . ? C9 C10 1.378(5) . ? C10 C11 1.381(6) . ? C11 C12 1.376(6) . ? C12 C13 1.385(5) . ? C14 C19 1.396(4) . ? C14 C15 1.402(4) . ? C15 C16 1.375(5) . ? C16 C17 1.375(5) . ? C17 C18 1.372(5) . ? C18 C19 1.384(5) . ? C20 C21 1.397(5) . ? C20 C25 1.398(4) . ? C21 C22 1.383(5) . ? C22 C23 1.392(5) . ? C23 C24 1.371(5) . ? C24 C25 1.387(5) . ? C26 C31 1.385(5) . ? C26 C27 1.392(5) . ? C27 C28 1.382(5) . ? C28 C29 1.382(5) . ? C29 C30 1.379(5) . ? C30 C31 1.385(5) . ? N1 C32 1.320(6) . ? N1 C33 1.410(6) . ? N1 C34 1.501(6) . ? O3 C32 1.222(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 O1 Ni C1 85.88(12) . . ? O1 Ni P1 178.14(8) . . ? C1 Ni P1 92.60(10) . . ? O1 Ni P2 87.58(7) . . ? C1 Ni P2 173.31(10) . . ? P1 Ni P2 93.91(4) . . ? C14 P1 C8 102.12(16) . . ? C14 P1 C4 107.84(16) . . ? C8 P1 C4 101.31(15) . . ? C14 P1 Ni 110.61(11) . . ? C8 P1 Ni 118.80(11) . . ? C4 P1 Ni 114.87(11) . . ? C20 P2 C7 103.83(15) . . ? C20 P2 C26 103.78(15) . . ? C7 P2 C26 101.95(15) . . ? C20 P2 Ni 110.34(11) . . ? C7 P2 Ni 121.28(12) . . ? C26 P2 Ni 113.84(11) . . ? C3 O1 Ni 117.6(2) . . ? C2 C1 Ni 107.6(2) . . ? C3 C2 C1 111.3(3) . . ? O2 C3 O1 123.0(3) . . ? O2 C3 C2 122.8(3) . . ? O1 C3 C2 114.3(3) . . ? C5 C4 P1 117.0(2) . . ? C6 C5 C4 115.3(3) . . ? C5 C6 C7 116.4(3) . . ? C6 C7 P2 113.1(2) . . ? C13 C8 C9 119.1(3) . . ? C13 C8 P1 122.0(3) . . ? C9 C8 P1 118.8(3) . . ? C10 C9 C8 120.6(4) . . ? C9 C10 C11 120.0(4) . . ? C12 C11 C10 119.7(4) . . ? C11 C12 C13 120.8(4) . . ? C12 C13 C8 119.7(4) . . ? C19 C14 C15 118.1(3) . . ? C19 C14 P1 118.1(2) . . ? C15 C14 P1 123.7(3) . . ? C16 C15 C14 120.1(4) . . ? C15 C16 C17 121.4(4) . . ? C18 C17 C16 119.1(4) . . ? C17 C18 C19 120.8(4) . . ? C18 C19 C14 120.5(3) . . ? C21 C20 C25 118.0(3) . . ? C21 C20 P2 123.7(2) . . ? C25 C20 P2 118.2(3) . . ? C22 C21 C20 120.3(3) . . ? C21 C22 C23 120.9(3) . . ? C24 C23 C22 119.3(3) . . ? C23 C24 C25 120.3(3) . . ? C24 C25 C20 121.1(3) . . ? C31 C26 C27 118.5(3) . . ? C31 C26 P2 120.1(3) . . ? C27 C26 P2 121.3(3) . . ? C28 C27 C26 120.7(3) . . ? C27 C28 C29 119.6(4) . . ? C30 C29 C28 120.6(3) . . ? C29 C30 C31 119.4(3) . . ? C26 C31 C30 121.1(3) . . ? C32 N1 C33 120.4(5) . . ? C32 N1 C34 119.3(5) . . ? C33 N1 C34 120.2(5) . . ? O3 C32 N1 123.4(5) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.906 _refine_diff_density_max 0.690 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.080 #===== END data_FO2378 _database_code_depnum_ccdc_archive 'CCDC 600552' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H40 N Ni O2 P3' _chemical_formula_weight 742.37 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' Ni Ni 0.3393 1.1124 '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 19.0310(5) _cell_length_b 16.9081(4) _cell_length_c 23.1607(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7452.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 0.686 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45196 _diffrn_reflns_av_R_equivalents 0.1435 _diffrn_reflns_av_sigmaI/netI 0.0903 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8459 _reflns_number_gt 5010 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0595P)^2^+7.0849P] 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 8459 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1271 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1560 _refine_ls_wR_factor_gt 0.1266 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.17817(2) 0.74481(3) 0.20062(2) 0.03300(14) Uani 1 1 d . . . P1 P 0.12139(5) 0.81180(6) 0.13911(4) 0.0312(2) Uani 1 1 d . . . P2 P 0.07989(5) 0.68398(6) 0.22889(5) 0.0315(2) Uani 1 1 d . . . P3 P -0.12313(5) 0.85137(6) 0.10634(5) 0.0373(3) Uani 1 1 d . . . O1 O 0.23798(13) 0.67888(16) 0.24462(13) 0.0437(7) Uani 1 1 d . . . O2 O 0.34973(14) 0.64325(17) 0.25843(14) 0.0485(8) Uani 1 1 d . . . N1 N -0.01729(15) 0.78395(18) 0.17408(14) 0.0319(7) Uani 1 1 d . . . C1 C 0.26510(19) 0.7977(3) 0.1774(2) 0.0434(10) Uani 1 1 d . . . H1A H 0.2619 0.8152 0.1367 0.052 Uiso 1 1 calc R . . H1B H 0.2737 0.8445 0.2021 0.052 Uiso 1 1 calc R . . C2 C 0.3236(2) 0.7386(2) 0.1844(2) 0.0434(10) Uani 1 1 d . . . H2A H 0.3681 0.7663 0.1932 0.052 Uiso 1 1 calc R . . H2B H 0.3299 0.7084 0.1482 0.052 Uiso 1 1 calc R . . C3 C 0.3050(2) 0.6828(2) 0.2332(2) 0.0399(10) Uani 1 1 d . . . C4 C 0.03324(19) 0.8467(2) 0.16002(18) 0.0336(9) Uani 1 1 d . . . H4A H 0.0380 0.8818 0.1940 0.040 Uiso 1 1 calc R . . H4B H 0.0138 0.8787 0.1280 0.040 Uiso 1 1 calc R . . C5 C 0.1078(2) 0.7511(2) 0.07533(18) 0.0347(8) Uani 1 1 d . . . C6 C 0.1609(3) 0.7035(4) 0.0578(3) 0.107(3) Uani 1 1 d . . . H6A H 0.2035 0.7029 0.0791 0.128 Uiso 1 1 calc R . . C7 C 0.1544(4) 0.6561(5) 0.0100(3) 0.128(4) Uani 1 1 d . . . H7A H 0.1935 0.6256 -0.0026 0.153 Uiso 1 1 calc R . . C8 C 0.0931(3) 0.6524(3) -0.0196(3) 0.0774(18) Uani 1 1 d . . . H8A H 0.0874 0.6166 -0.0508 0.093 Uiso 1 1 calc R . . C9 C 0.0400(3) 0.7008(4) -0.0035(3) 0.094(2) Uani 1 1 d . . . H9A H -0.0025 0.7012 -0.0250 0.113 Uiso 1 1 calc R . . C10 C 0.0471(2) 0.7496(4) 0.0439(2) 0.0746(18) Uani 1 1 d . . . H10A H 0.0091 0.7828 0.0548 0.089 Uiso 1 1 calc R . . C11 C 0.15426(19) 0.9060(2) 0.11203(17) 0.0326(8) Uani 1 1 d . . . C12 C 0.1823(2) 0.9610(3) 0.1509(2) 0.0492(11) Uani 1 1 d . . . H12A H 0.1864 0.9477 0.1906 0.059 Uiso 1 1 calc R . . C13 C 0.2039(3) 1.0340(3) 0.1319(3) 0.0592(14) Uani 1 1 d . . . H13A H 0.2231 1.0709 0.1585 0.071 Uiso 1 1 calc R . . C14 C 0.1978(2) 1.0542(3) 0.0743(3) 0.0546(13) Uani 1 1 d . . . H14A H 0.2129 1.1047 0.0613 0.066 Uiso 1 1 calc R . . C15 C 0.1702(3) 1.0016(3) 0.0362(2) 0.0551(12) Uani 1 1 d . . . H15A H 0.1655 1.0157 -0.0033 0.066 Uiso 1 1 calc R . . C16 C 0.1486(2) 0.9269(2) 0.05480(19) 0.0437(10) Uani 1 1 d . . . H16A H 0.1300 0.8902 0.0278 0.052 Uiso 1 1 calc R . . C17 C -0.00102(19) 0.7436(2) 0.22803(17) 0.0316(8) Uani 1 1 d . . . H17A H -0.0410 0.7085 0.2378 0.038 Uiso 1 1 calc R . . H17C H 0.0025 0.7838 0.2589 0.038 Uiso 1 1 calc R . . C18 C 0.0614(2) 0.5975(2) 0.18495(18) 0.0369(9) Uani 1 1 d . . . C19 C 0.1093(2) 0.5353(3) 0.1868(2) 0.0609(14) Uani 1 1 d . . . H19A H 0.1491 0.5389 0.2114 0.073 Uiso 1 1 calc R . . C20 C 0.0999(3) 0.4688(3) 0.1537(3) 0.081(2) Uani 1 1 d . . . H20A H 0.1325 0.4264 0.1560 0.097 Uiso 1 1 calc R . . C21 C 0.0427(3) 0.4639(3) 0.1170(3) 0.0749(18) Uani 1 1 d . . . H21A H 0.0358 0.4179 0.0941 0.090 Uiso 1 1 calc R . . C22 C -0.0038(3) 0.5250(3) 0.1137(3) 0.0712(17) Uani 1 1 d . . . H22A H -0.0424 0.5220 0.0877 0.085 Uiso 1 1 calc R . . C23 C 0.0049(2) 0.5912(3) 0.1477(2) 0.0549(13) Uani 1 1 d . . . H23B H -0.0284 0.6330 0.1456 0.066 Uiso 1 1 calc R . . C24 C 0.0714(2) 0.6462(2) 0.30255(18) 0.0365(9) Uani 1 1 d . . . C25 C 0.0124(2) 0.6013(3) 0.3183(2) 0.0457(11) Uani 1 1 d . . . H25A H -0.0216 0.5878 0.2899 0.055 Uiso 1 1 calc R . . C26 C 0.0034(2) 0.5768(3) 0.3743(2) 0.0497(11) Uani 1 1 d . . . H26A H -0.0370 0.5470 0.3847 0.060 Uiso 1 1 calc R . . C27 C 0.0528(3) 0.5952(3) 0.4153(2) 0.0633(14) Uani 1 1 d . . . H27A H 0.0462 0.5785 0.4541 0.076 Uiso 1 1 calc R . . C28 C 0.1125(3) 0.6383(3) 0.4003(2) 0.0651(15) Uani 1 1 d . . . H28A H 0.1468 0.6504 0.4288 0.078 Uiso 1 1 calc R . . C29 C 0.1218(2) 0.6636(3) 0.3439(2) 0.0479(11) Uani 1 1 d . . . H29A H 0.1626 0.6928 0.3336 0.058 Uiso 1 1 calc R . . C30 C -0.08877(18) 0.8165(2) 0.17685(18) 0.0349(9) Uani 1 1 d . . . H30A H -0.0892 0.8612 0.2044 0.042 Uiso 1 1 calc R . . H30B H -0.1207 0.7753 0.1921 0.042 Uiso 1 1 calc R . . C31 C -0.1466(2) 0.7593(2) 0.06912(19) 0.0395(10) Uani 1 1 d . . . C32 C -0.1386(2) 0.7603(3) 0.0089(2) 0.0490(11) Uani 1 1 d . . . H32A H -0.1231 0.8074 -0.0095 0.059 Uiso 1 1 calc R . . C33 C -0.1527(3) 0.6942(3) -0.0244(2) 0.0611(14) Uani 1 1 d . . . H33A H -0.1471 0.6962 -0.0652 0.073 Uiso 1 1 calc R . . C34 C -0.1750(3) 0.6258(3) 0.0017(3) 0.0634(14) Uani 1 1 d . . . H34A H -0.1856 0.5806 -0.0211 0.076 Uiso 1 1 calc R . . C35 C -0.1819(3) 0.6225(3) 0.0612(2) 0.0571(13) Uani 1 1 d . . . H35A H -0.1962 0.5748 0.0794 0.069 Uiso 1 1 calc R . . C36 C -0.1681(2) 0.6893(3) 0.0943(2) 0.0477(11) Uani 1 1 d . . . H36A H -0.1735 0.6867 0.1350 0.057 Uiso 1 1 calc R . . C37 C -0.2060(2) 0.8896(2) 0.13574(19) 0.0385(9) Uani 1 1 d . . . C38 C -0.2697(2) 0.8499(3) 0.1363(2) 0.0538(12) Uani 1 1 d . . . H38A H -0.2730 0.7989 0.1194 0.065 Uiso 1 1 calc R . . C39 C -0.3290(3) 0.8842(3) 0.1615(3) 0.0635(14) Uani 1 1 d . . . H39A H -0.3723 0.8564 0.1620 0.076 Uiso 1 1 calc R . . C40 C -0.3246(3) 0.9575(3) 0.1853(2) 0.0613(14) Uani 1 1 d . . . H40A H -0.3652 0.9815 0.2017 0.074 Uiso 1 1 calc R . . C41 C -0.2615(3) 0.9971(3) 0.1857(2) 0.0620(14) Uani 1 1 d . . . H41A H -0.2580 1.0477 0.2033 0.074 Uiso 1 1 calc R . . C42 C -0.2039(3) 0.9633(3) 0.1608(2) 0.0559(13) Uani 1 1 d . . . H42A H -0.1608 0.9917 0.1607 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0234(2) 0.0385(3) 0.0371(3) 0.0040(2) -0.0020(2) 0.0003(2) P1 0.0251(5) 0.0344(5) 0.0341(6) 0.0012(4) -0.0003(4) -0.0016(4) P2 0.0235(4) 0.0345(5) 0.0364(6) 0.0036(4) -0.0024(4) -0.0009(4) P3 0.0322(5) 0.0394(5) 0.0403(6) 0.0009(5) -0.0029(5) 0.0049(4) O1 0.0260(14) 0.0487(16) 0.0564(19) 0.0148(15) -0.0022(13) 0.0017(12) O2 0.0303(14) 0.0537(18) 0.061(2) 0.0141(16) -0.0053(14) -0.0039(13) N1 0.0219(15) 0.0357(16) 0.0381(19) 0.0029(15) -0.0001(14) 0.0013(13) C1 0.0249(19) 0.056(3) 0.049(3) 0.008(2) -0.0028(18) -0.0023(18) C2 0.031(2) 0.049(2) 0.050(3) 0.007(2) -0.0008(19) -0.0047(19) C3 0.030(2) 0.041(2) 0.049(3) 0.009(2) -0.0106(18) -0.0042(18) C4 0.0307(19) 0.0314(19) 0.039(2) 0.0003(17) -0.0013(17) 0.0018(16) C5 0.0310(18) 0.0354(19) 0.038(2) -0.0053(18) 0.0004(17) -0.0051(17) C6 0.081(4) 0.143(6) 0.095(5) -0.078(5) -0.053(4) 0.073(4) C7 0.110(6) 0.155(7) 0.119(6) -0.090(6) -0.058(5) 0.090(5) C8 0.086(4) 0.072(4) 0.075(4) -0.038(3) -0.008(3) 0.002(3) C9 0.043(3) 0.154(6) 0.086(5) -0.068(5) 0.002(3) -0.016(4) C10 0.031(2) 0.126(5) 0.067(4) -0.055(4) 0.000(2) 0.000(3) C11 0.0252(18) 0.037(2) 0.036(2) -0.0008(17) -0.0007(16) -0.0009(15) C12 0.052(3) 0.047(2) 0.049(3) -0.005(2) -0.011(2) -0.002(2) C13 0.055(3) 0.043(3) 0.080(4) -0.006(3) -0.015(3) -0.010(2) C14 0.045(3) 0.041(2) 0.078(4) 0.007(3) 0.003(2) -0.009(2) C15 0.067(3) 0.046(3) 0.053(3) 0.010(2) 0.010(3) -0.005(2) C16 0.046(2) 0.043(2) 0.042(3) 0.003(2) 0.000(2) -0.006(2) C17 0.0246(17) 0.0368(19) 0.033(2) 0.0017(17) -0.0009(15) 0.0013(16) C18 0.0290(19) 0.037(2) 0.045(2) 0.0027(18) -0.0020(17) -0.0014(17) C19 0.038(2) 0.063(3) 0.082(4) -0.022(3) -0.015(2) 0.016(2) C20 0.059(3) 0.061(3) 0.122(6) -0.035(4) -0.023(3) 0.029(3) C21 0.062(3) 0.058(3) 0.104(5) -0.041(3) -0.015(3) 0.010(3) C22 0.053(3) 0.061(3) 0.099(5) -0.029(3) -0.033(3) 0.010(3) C23 0.042(2) 0.042(2) 0.081(4) -0.013(2) -0.022(2) 0.006(2) C24 0.033(2) 0.041(2) 0.036(2) 0.0064(18) -0.0023(17) -0.0025(17) C25 0.035(2) 0.053(3) 0.048(3) 0.007(2) -0.008(2) -0.008(2) C26 0.045(2) 0.057(3) 0.047(3) 0.015(2) 0.001(2) -0.010(2) C27 0.067(3) 0.082(4) 0.042(3) 0.024(3) -0.004(3) -0.023(3) C28 0.063(3) 0.088(4) 0.044(3) 0.013(3) -0.017(3) -0.027(3) C29 0.040(2) 0.058(3) 0.046(3) 0.008(2) -0.003(2) -0.012(2) C30 0.0251(18) 0.038(2) 0.042(2) 0.0009(18) -0.0040(16) 0.0035(16) C31 0.0290(19) 0.046(2) 0.044(2) -0.007(2) -0.0044(17) 0.0109(18) C32 0.043(2) 0.055(3) 0.049(3) -0.002(2) -0.007(2) 0.012(2) C33 0.057(3) 0.080(4) 0.046(3) -0.015(3) -0.012(2) 0.008(3) C34 0.049(3) 0.065(3) 0.076(4) -0.028(3) -0.013(3) 0.004(3) C35 0.051(3) 0.052(3) 0.069(4) -0.009(2) -0.001(3) -0.003(2) C36 0.045(2) 0.049(2) 0.050(3) -0.007(2) -0.001(2) 0.000(2) C37 0.037(2) 0.039(2) 0.040(2) 0.0003(19) -0.0056(18) 0.0101(17) C38 0.039(2) 0.050(3) 0.073(4) -0.009(2) 0.007(2) 0.003(2) C39 0.040(3) 0.074(3) 0.077(4) -0.006(3) 0.011(3) 0.005(2) C40 0.055(3) 0.077(4) 0.052(3) -0.005(3) 0.001(2) 0.030(3) C41 0.063(3) 0.057(3) 0.065(3) -0.017(3) -0.005(3) 0.023(3) C42 0.046(3) 0.050(3) 0.071(4) -0.012(2) -0.007(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.891(3) . ? Ni C1 1.955(4) . ? Ni P1 2.1166(11) . ? Ni P2 2.2327(11) . ? P1 C5 1.818(4) . ? P1 C11 1.823(4) . ? P1 C4 1.843(4) . ? P2 C18 1.815(4) . ? P2 C24 1.828(4) . ? P2 C17 1.840(4) . ? P3 C31 1.834(4) . ? P3 C37 1.836(4) . ? P3 C30 1.855(4) . ? O1 C3 1.305(5) . ? O2 C3 1.231(5) . ? N1 C17 1.457(5) . ? N1 C4 1.468(5) . ? N1 C30 1.469(4) . ? C1 C2 1.504(6) . ? C2 C3 1.512(6) . ? C5 C6 1.352(6) . ? C5 C10 1.366(6) . ? C6 C7 1.374(8) . ? C7 C8 1.355(9) . ? C8 C9 1.351(8) . ? C9 C10 1.380(7) . ? C11 C16 1.376(6) . ? C11 C12 1.399(6) . ? C12 C13 1.375(6) . ? C13 C14 1.382(7) . ? C14 C15 1.358(7) . ? C15 C16 1.396(6) . ? C18 C23 1.383(6) . ? C18 C19 1.393(6) . ? C19 C20 1.371(7) . ? C20 C21 1.384(8) . ? C21 C22 1.363(7) . ? C22 C23 1.379(7) . ? C24 C29 1.387(6) . ? C24 C25 1.404(6) . ? C25 C26 1.373(6) . ? C26 C27 1.370(7) . ? C27 C28 1.395(7) . ? C28 C29 1.385(7) . ? C31 C36 1.382(6) . ? C31 C32 1.404(6) . ? C32 C33 1.384(7) . ? C33 C34 1.372(7) . ? C34 C35 1.387(8) . ? C35 C36 1.389(6) . ? C37 C42 1.375(6) . ? C37 C38 1.385(6) . ? C38 C39 1.397(6) . ? C39 C40 1.359(7) . ? C40 C41 1.375(7) . ? C41 C42 1.364(7) . ? 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 Ni C1 84.73(15) . . ? O1 Ni P1 170.18(10) . . ? C1 Ni P1 90.15(13) . . ? O1 Ni P2 94.27(9) . . ? C1 Ni P2 178.81(14) . . ? P1 Ni P2 90.93(4) . . ? C5 P1 C11 105.25(18) . . ? C5 P1 C4 105.37(18) . . ? C11 P1 C4 97.08(17) . . ? C5 P1 Ni 108.49(14) . . ? C11 P1 Ni 121.60(13) . . ? C4 P1 Ni 117.32(14) . . ? C18 P2 C24 103.00(19) . . ? C18 P2 C17 105.82(18) . . ? C24 P2 C17 97.33(18) . . ? C18 P2 Ni 111.64(14) . . ? C24 P2 Ni 120.55(13) . . ? C17 P2 Ni 116.45(12) . . ? C31 P3 C37 105.32(18) . . ? C31 P3 C30 103.26(19) . . ? C37 P3 C30 95.07(18) . . ? C3 O1 Ni 116.7(3) . . ? C17 N1 C4 112.9(3) . . ? C17 N1 C30 109.6(3) . . ? C4 N1 C30 110.3(3) . . ? C2 C1 Ni 107.0(3) . . ? C1 C2 C3 108.8(4) . . ? O2 C3 O1 123.5(4) . . ? O2 C3 C2 122.2(4) . . ? O1 C3 C2 114.3(3) . . ? N1 C4 P1 115.1(2) . . ? C6 C5 C10 117.5(4) . . ? C6 C5 P1 118.2(3) . . ? C10 C5 P1 124.3(3) . . ? C5 C6 C7 121.4(5) . . ? C8 C7 C6 120.8(6) . . ? C7 C8 C9 118.5(5) . . ? C8 C9 C10 120.5(6) . . ? C5 C10 C9 121.2(5) . . ? C16 C11 C12 118.7(4) . . ? C16 C11 P1 121.9(3) . . ? C12 C11 P1 119.3(3) . . ? C13 C12 C11 120.3(5) . . ? C12 C13 C14 120.3(5) . . ? C15 C14 C13 119.9(4) . . ? C14 C15 C16 120.3(5) . . ? C11 C16 C15 120.4(4) . . ? N1 C17 P2 116.3(3) . . ? C23 C18 C19 118.0(4) . . ? C23 C18 P2 124.2(3) . . ? C19 C18 P2 117.7(3) . . ? C20 C19 C18 121.1(5) . . ? C19 C20 C21 119.7(5) . . ? C22 C21 C20 120.0(5) . . ? C21 C22 C23 120.4(5) . . ? C18 C23 C22 120.8(4) . . ? C29 C24 C25 119.2(4) . . ? C29 C24 P2 120.7(3) . . ? C25 C24 P2 120.1(3) . . ? C26 C25 C24 120.6(4) . . ? C27 C26 C25 120.0(4) . . ? C26 C27 C28 120.3(5) . . ? C29 C28 C27 120.0(5) . . ? C28 C29 C24 119.8(4) . . ? N1 C30 P3 114.0(3) . . ? C36 C31 C32 117.4(4) . . ? C36 C31 P3 127.0(4) . . ? C32 C31 P3 115.5(3) . . ? C33 C32 C31 121.6(5) . . ? C34 C33 C32 119.6(5) . . ? C33 C34 C35 120.1(5) . . ? C34 C35 C36 119.8(5) . . ? C31 C36 C35 121.4(5) . . ? C42 C37 C38 117.4(4) . . ? C42 C37 P3 116.8(3) . . ? C38 C37 P3 125.8(3) . . ? C37 C38 C39 120.7(4) . . ? C40 C39 C38 119.9(5) . . ? C39 C40 C41 120.0(5) . . ? C42 C41 C40 119.7(5) . . ? C41 C42 C37 122.3(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.458 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.076 #===== END data_FO1676 _database_code_depnum_ccdc_archive 'CCDC 600553' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24 N4 Ni' _chemical_formula_weight 475.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.7003(4) _cell_length_b 22.7328(4) _cell_length_c 18.2480(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.915(1) _cell_angle_gamma 90.00 _cell_volume 8960.1(3) _cell_formula_units_Z 16 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3968 _exptl_absorpt_coefficient_mu 0.890 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21970 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.46 _reflns_number_total 9693 _reflns_number_gt 7905 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0975P)^2^+80.8569P] 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 9693 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0893 _refine_ls_wR_factor_ref 0.2523 _refine_ls_wR_factor_gt 0.2335 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.082 _refine_ls_shift/su_mean 0.002 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 Ni1 Ni -0.69294(3) 0.05729(3) -0.26279(4) 0.02473(19) Uani 1 1 d . . . N1 N -0.6226(2) 0.0683(2) -0.1704(3) 0.0298(10) Uani 1 1 d . . . N2 N -0.7261(2) 0.12652(17) -0.2255(2) 0.0223(8) Uani 1 1 d . . . N3 N -0.6751(2) 0.0440(2) -0.3602(3) 0.0254(9) Uani 1 1 d . . . N4 N -0.74500(19) -0.01273(19) -0.2945(2) 0.0231(8) Uani 1 1 d . . . C1 C -0.5691(3) 0.0364(3) -0.1453(4) 0.0400(14) Uani 1 1 d . . . C2 C -0.5242(3) 0.0505(3) -0.0774(4) 0.0511(19) Uani 1 1 d . . . H2A H -0.4879 0.0270 -0.0608 0.061 Uiso 1 1 calc R . . C3 C -0.5304(3) 0.0983(4) -0.0324(4) 0.0512(19) Uani 1 1 d . . . H3A H -0.4990 0.1073 0.0143 0.061 Uiso 1 1 calc R . . C4 C -0.5838(3) 0.1324(3) -0.0576(3) 0.0371(14) Uani 1 1 d . . . C5 C -0.5966(3) 0.1838(3) -0.0191(4) 0.0500(19) Uani 1 1 d . . . H5A H -0.5669 0.1961 0.0275 0.060 Uiso 1 1 calc R . . C6 C -0.6490(4) 0.2153(3) -0.0469(4) 0.0479(18) Uani 1 1 d . . . H6A H -0.6551 0.2494 -0.0200 0.057 Uiso 1 1 calc R . . C7 C -0.6956(3) 0.1983(3) -0.1165(3) 0.0338(12) Uani 1 1 d . . . C8 C -0.7506(3) 0.2287(3) -0.1499(4) 0.0426(15) Uani 1 1 d . . . H8A H -0.7602 0.2631 -0.1265 0.051 Uiso 1 1 calc R . . C9 C -0.7907(3) 0.2076(3) -0.2178(4) 0.0377(13) Uani 1 1 d . . . H9A H -0.8282 0.2282 -0.2409 0.045 Uiso 1 1 calc R . . C10 C -0.7782(2) 0.1571(3) -0.2536(3) 0.0301(11) Uani 1 1 d . . . C11 C -0.6844(2) 0.1482(2) -0.1562(3) 0.0251(10) Uani 1 1 d . . . C12 C -0.6288(2) 0.1154(3) -0.1271(3) 0.0293(11) Uani 1 1 d . . . C13 C -0.5619(3) -0.0134(3) -0.1942(5) 0.061(2) Uani 1 1 d . . . H13A H -0.5207 -0.0309 -0.1724 0.091 Uiso 1 1 calc R . . H13B H -0.5666 0.0008 -0.2464 0.091 Uiso 1 1 calc R . . H13C H -0.5935 -0.0432 -0.1961 0.091 Uiso 1 1 calc R . . C14 C -0.8232(3) 0.1332(3) -0.3256(4) 0.0449(16) Uani 1 1 d . . . H14A H -0.8277 0.0907 -0.3202 0.067 Uiso 1 1 calc R . . H14B H -0.8079 0.1410 -0.3694 0.067 Uiso 1 1 calc R . . H14C H -0.8635 0.1524 -0.3343 0.067 Uiso 1 1 calc R . . C15 C -0.6386(3) 0.0749(3) -0.3930(3) 0.0328(12) Uani 1 1 d . . . C16 C -0.6322(3) 0.0584(3) -0.4640(4) 0.0376(13) Uani 1 1 d . . . H16A H -0.6078 0.0820 -0.4865 0.045 Uiso 1 1 calc R . . C17 C -0.6607(3) 0.0086(3) -0.5021(4) 0.0393(14) Uani 1 1 d . . . H17A H -0.6552 -0.0027 -0.5496 0.047 Uiso 1 1 calc R . . C18 C -0.6975(3) -0.0248(3) -0.4697(3) 0.0314(12) Uani 1 1 d . . . C19 C -0.7304(3) -0.0765(3) -0.5036(3) 0.0362(13) Uani 1 1 d . . . H19A H -0.7271 -0.0902 -0.5513 0.043 Uiso 1 1 calc R . . C20 C -0.7662(3) -0.1064(3) -0.4693(3) 0.0375(13) Uani 1 1 d . . . H20A H -0.7871 -0.1409 -0.4932 0.045 Uiso 1 1 calc R . . C21 C -0.7735(3) -0.0872(2) -0.3971(3) 0.0285(11) Uani 1 1 d . . . C22 C -0.8093(3) -0.1157(3) -0.3582(3) 0.0337(12) Uani 1 1 d . . . H22A H -0.8315 -0.1505 -0.3789 0.040 Uiso 1 1 calc R . . C23 C -0.8124(3) -0.0930(3) -0.2891(4) 0.0366(13) Uani 1 1 d . . . H23A H -0.8359 -0.1128 -0.2617 0.044 Uiso 1 1 calc R . . C24 C -0.7812(2) -0.0413(3) -0.2596(3) 0.0305(11) Uani 1 1 d . . . C25 C -0.7420(2) -0.0361(2) -0.3636(3) 0.0238(10) Uani 1 1 d . . . C26 C -0.7041(2) -0.0049(2) -0.3988(3) 0.0259(10) Uani 1 1 d . . . C27 C -0.6047(3) 0.1269(3) -0.3491(4) 0.0502(17) Uani 1 1 d . . . H27A H -0.5835 0.1154 -0.2957 0.075 Uiso 1 1 calc R . . H27B H -0.6343 0.1584 -0.3497 0.075 Uiso 1 1 calc R . . H27C H -0.5742 0.1409 -0.3731 0.075 Uiso 1 1 calc R . . C28 C -0.7863(3) -0.0144(3) -0.1861(4) 0.0418(15) Uani 1 1 d . . . H28A H -0.7448 -0.0076 -0.1504 0.063 Uiso 1 1 calc R . . H28B H -0.8090 -0.0412 -0.1624 0.063 Uiso 1 1 calc R . . H28C H -0.8086 0.0231 -0.1979 0.063 Uiso 1 1 calc R . . NiA Ni 0.0000 -0.12902(4) -0.2500 0.0273(2) Uani 1 2 d S . . N1A N 0.07720(19) -0.17376(19) -0.2163(3) 0.0253(9) Uani 1 1 d . . . N2A N 0.0381(2) -0.0840(2) -0.1558(3) 0.0342(11) Uani 1 1 d . . . C1A C 0.0972(3) -0.2206(2) -0.2475(3) 0.0291(11) Uani 1 1 d . . . C2A C 0.1558(3) -0.2442(3) -0.2158(4) 0.0385(13) Uani 1 1 d . . . H2AA H 0.1686 -0.2757 -0.2415 0.046 Uiso 1 1 calc R . . C3A C 0.1965(3) -0.2228(3) -0.1474(4) 0.0386(13) Uani 1 1 d . . . H3AA H 0.2363 -0.2399 -0.1255 0.046 Uiso 1 1 calc R . . C4A C 0.1772(3) -0.1759(3) -0.1123(3) 0.0335(12) Uani 1 1 d . . . C5A C 0.2148(3) -0.1493(3) -0.0413(4) 0.0425(15) Uani 1 1 d . . . H5AA H 0.2547 -0.1648 -0.0159 0.051 Uiso 1 1 calc R . . C6A C 0.1943(3) -0.1036(3) -0.0113(4) 0.0465(17) Uani 1 1 d . . . H6AA H 0.2204 -0.0868 0.0350 0.056 Uiso 1 1 calc R . . C7A C 0.1346(3) -0.0786(3) -0.0457(4) 0.0393(14) Uani 1 1 d . . . C8A C 0.1102(4) -0.0308(3) -0.0163(5) 0.056(2) Uani 1 1 d . . . H8AA H 0.1334 -0.0120 0.0302 0.067 Uiso 1 1 calc R . . C9A C 0.0512(4) -0.0116(3) -0.0570(5) 0.059(2) Uani 1 1 d . . . H9AA H 0.0339 0.0201 -0.0366 0.071 Uiso 1 1 calc R . . C10A C 0.0161(3) -0.0366(3) -0.1261(4) 0.0454(16) Uani 1 1 d . . . C11A C 0.0959(3) -0.1038(2) -0.1156(3) 0.0297(11) Uani 1 1 d . . . C12A C 0.1177(2) -0.1524(2) -0.1484(3) 0.0258(10) Uani 1 1 d . . . C13A C 0.0531(3) -0.2450(3) -0.3187(3) 0.0404(14) Uani 1 1 d . . . H13D H 0.0119 -0.2480 -0.3123 0.061 Uiso 1 1 calc R . . H13E H 0.0670 -0.2841 -0.3287 0.061 Uiso 1 1 calc R . . H13F H 0.0512 -0.2190 -0.3621 0.061 Uiso 1 1 calc R . . C14A C -0.0465(4) -0.0138(4) -0.1714(6) 0.067(2) Uani 1 1 d . . . H14D H -0.0503 -0.0141 -0.2264 0.100 Uiso 1 1 calc R . . H14E H -0.0514 0.0265 -0.1553 0.100 Uiso 1 1 calc R . . H14F H -0.0786 -0.0389 -0.1622 0.100 Uiso 1 1 calc R . . NiB Ni 0.0000 0.24673(4) -0.2500 0.0262(2) Uani 1 2 d S . . N1B N -0.06262(19) 0.2898(2) -0.2185(2) 0.0259(9) Uani 1 1 d . . . N2B N 0.0124(2) 0.20529(19) -0.1524(3) 0.0264(9) Uani 1 1 d . . . C1B C -0.1028(2) 0.3315(2) -0.2552(3) 0.0303(11) Uani 1 1 d . . . C2B C -0.1462(3) 0.3551(3) -0.2231(4) 0.0363(13) Uani 1 1 d . . . H2BA H -0.1744 0.3840 -0.2512 0.044 Uiso 1 1 calc R . . C3B C -0.1494(3) 0.3379(3) -0.1519(4) 0.0352(13) Uani 1 1 d . . . H3BA H -0.1785 0.3552 -0.1305 0.042 Uiso 1 1 calc R . . C4B C -0.1090(3) 0.2946(3) -0.1123(3) 0.0311(11) Uani 1 1 d . . . C5B C -0.1087(3) 0.2702(3) -0.0389(3) 0.0372(13) Uani 1 1 d . . . H5BA H -0.1370 0.2849 -0.0144 0.045 Uiso 1 1 calc R . . C6B C -0.0692(3) 0.2272(3) -0.0046(3) 0.0385(14) Uani 1 1 d . . . H6BA H -0.0700 0.2126 0.0438 0.046 Uiso 1 1 calc R . . C7B C -0.0255(3) 0.2024(3) -0.0392(3) 0.0322(12) Uani 1 1 d . . . C8B C 0.0169(3) 0.1590(3) -0.0063(4) 0.0422(15) Uani 1 1 d . . . H8BA H 0.0194 0.1432 0.0428 0.051 Uiso 1 1 calc R . . C9B C 0.0560(3) 0.1389(3) -0.0468(4) 0.0427(15) Uani 1 1 d . . . H9BA H 0.0860 0.1095 -0.0244 0.051 Uiso 1 1 calc R . . C10B C 0.0521(3) 0.1610(3) -0.1196(4) 0.0371(13) Uani 1 1 d . . . C11B C -0.0259(2) 0.2256(2) -0.1117(3) 0.0244(10) Uani 1 1 d . . . C12B C -0.0668(2) 0.2712(2) -0.1474(3) 0.0239(10) Uani 1 1 d . . . C13B C -0.0979(3) 0.3511(3) -0.3310(4) 0.0464(17) Uani 1 1 d . . . H13G H -0.1035 0.3173 -0.3657 0.070 Uiso 1 1 calc R . . H13J H -0.0570 0.3685 -0.3238 0.070 Uiso 1 1 calc R . . H13H H -0.1300 0.3805 -0.3534 0.070 Uiso 1 1 calc R . . C14B C 0.0903(4) 0.1365(3) -0.1657(5) 0.0547(19) Uani 1 1 d . . . H14J H 0.0632 0.1241 -0.2163 0.082 Uiso 1 1 calc R . . H14G H 0.1140 0.1026 -0.1388 0.082 Uiso 1 1 calc R . . H14H H 0.1190 0.1668 -0.1725 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0230(3) 0.0254(4) 0.0260(3) -0.0006(2) 0.0079(2) -0.0002(2) N1 0.024(2) 0.032(2) 0.029(2) 0.0074(18) 0.0026(17) -0.0007(18) N2 0.033(2) 0.0148(19) 0.025(2) 0.0024(15) 0.0167(17) 0.0045(16) N3 0.024(2) 0.026(2) 0.028(2) 0.0007(17) 0.0110(17) 0.0049(17) N4 0.023(2) 0.022(2) 0.024(2) 0.0005(16) 0.0067(16) 0.0030(16) C1 0.029(3) 0.042(3) 0.049(4) 0.013(3) 0.011(3) 0.001(2) C2 0.025(3) 0.057(5) 0.060(4) 0.018(4) -0.003(3) -0.002(3) C3 0.029(3) 0.071(5) 0.041(4) 0.015(3) -0.009(3) -0.017(3) C4 0.036(3) 0.047(4) 0.023(3) 0.007(2) 0.001(2) -0.016(3) C5 0.057(4) 0.064(5) 0.024(3) 0.000(3) 0.005(3) -0.034(4) C6 0.073(5) 0.040(4) 0.035(3) -0.011(3) 0.022(3) -0.030(3) C7 0.044(3) 0.028(3) 0.034(3) -0.003(2) 0.019(2) -0.011(2) C8 0.062(4) 0.024(3) 0.050(4) -0.007(3) 0.031(3) -0.002(3) C9 0.038(3) 0.029(3) 0.049(4) 0.002(2) 0.017(3) 0.008(2) C10 0.027(3) 0.031(3) 0.032(3) 0.005(2) 0.010(2) 0.003(2) C11 0.026(2) 0.029(3) 0.020(2) 0.0036(19) 0.0067(19) -0.008(2) C12 0.026(3) 0.033(3) 0.028(3) 0.008(2) 0.006(2) -0.011(2) C13 0.038(4) 0.044(4) 0.098(7) 0.002(4) 0.018(4) 0.010(3) C14 0.034(3) 0.056(4) 0.037(3) 0.002(3) -0.001(3) 0.012(3) C15 0.031(3) 0.033(3) 0.038(3) 0.004(2) 0.015(2) 0.001(2) C16 0.032(3) 0.050(4) 0.037(3) 0.009(3) 0.021(2) 0.005(3) C17 0.038(3) 0.050(4) 0.036(3) 0.008(3) 0.020(3) 0.012(3) C18 0.030(3) 0.038(3) 0.028(3) 0.004(2) 0.011(2) 0.009(2) C19 0.043(3) 0.038(3) 0.029(3) -0.008(2) 0.013(2) 0.009(3) C20 0.041(3) 0.035(3) 0.034(3) -0.010(2) 0.008(2) 0.005(3) C21 0.032(3) 0.023(3) 0.030(3) -0.002(2) 0.008(2) 0.003(2) C22 0.032(3) 0.026(3) 0.040(3) -0.002(2) 0.006(2) -0.006(2) C23 0.037(3) 0.035(3) 0.042(3) 0.005(2) 0.019(3) -0.006(2) C24 0.027(3) 0.034(3) 0.032(3) 0.002(2) 0.010(2) 0.002(2) C25 0.022(2) 0.024(2) 0.022(2) 0.0019(18) 0.0027(18) 0.0033(19) C26 0.025(2) 0.026(3) 0.026(3) 0.0035(19) 0.0085(19) 0.008(2) C27 0.054(4) 0.045(4) 0.061(4) -0.007(3) 0.033(4) -0.016(3) C28 0.045(4) 0.048(4) 0.039(3) -0.004(3) 0.024(3) -0.011(3) NiA 0.0268(5) 0.0215(5) 0.0349(5) 0.000 0.0116(4) 0.000 N1A 0.024(2) 0.024(2) 0.032(2) 0.0057(17) 0.0142(17) 0.0008(16) N2A 0.038(3) 0.025(2) 0.046(3) -0.012(2) 0.022(2) -0.008(2) C1A 0.037(3) 0.029(3) 0.024(2) -0.001(2) 0.013(2) -0.003(2) C2A 0.043(3) 0.037(3) 0.043(3) -0.001(3) 0.023(3) 0.009(3) C3A 0.034(3) 0.038(3) 0.042(3) 0.008(3) 0.009(2) 0.004(2) C4A 0.028(3) 0.040(3) 0.030(3) 0.004(2) 0.006(2) -0.007(2) C5A 0.033(3) 0.055(4) 0.035(3) -0.003(3) 0.004(2) -0.015(3) C6A 0.050(4) 0.059(4) 0.030(3) -0.010(3) 0.011(3) -0.028(3) C7A 0.050(4) 0.040(3) 0.037(3) -0.012(3) 0.026(3) -0.019(3) C8A 0.069(5) 0.048(4) 0.064(5) -0.037(4) 0.039(4) -0.030(4) C9A 0.080(6) 0.035(4) 0.081(6) -0.032(4) 0.051(5) -0.018(4) C10A 0.058(4) 0.026(3) 0.067(4) -0.016(3) 0.041(4) -0.007(3) C11A 0.037(3) 0.026(3) 0.032(3) -0.008(2) 0.020(2) -0.015(2) C12A 0.025(2) 0.031(3) 0.024(2) 0.0013(19) 0.0114(19) -0.007(2) C13A 0.045(3) 0.043(4) 0.032(3) -0.010(3) 0.010(3) 0.007(3) C14A 0.055(5) 0.043(4) 0.108(7) -0.022(4) 0.032(5) 0.012(3) NiB 0.0260(5) 0.0278(5) 0.0258(5) 0.000 0.0097(4) 0.000 N1B 0.0194(19) 0.029(2) 0.025(2) -0.0110(17) 0.0005(16) 0.0016(17) N2B 0.024(2) 0.022(2) 0.032(2) 0.0035(17) 0.0062(17) -0.0028(16) C1B 0.028(3) 0.029(3) 0.032(3) 0.004(2) 0.007(2) 0.005(2) C2B 0.031(3) 0.031(3) 0.045(3) 0.007(2) 0.009(2) 0.010(2) C3B 0.031(3) 0.037(3) 0.042(3) 0.000(2) 0.017(2) 0.006(2) C4B 0.030(3) 0.034(3) 0.031(3) -0.005(2) 0.011(2) -0.006(2) C5B 0.036(3) 0.050(4) 0.030(3) -0.004(3) 0.017(2) -0.004(3) C6B 0.042(3) 0.048(4) 0.026(3) 0.005(2) 0.012(2) -0.013(3) C7B 0.033(3) 0.035(3) 0.025(3) 0.006(2) 0.004(2) -0.011(2) C8B 0.046(4) 0.035(3) 0.038(3) 0.014(3) 0.003(3) -0.007(3) C9B 0.038(3) 0.031(3) 0.054(4) 0.014(3) 0.006(3) 0.005(3) C10B 0.029(3) 0.030(3) 0.051(4) 0.008(3) 0.010(3) 0.001(2) C11B 0.023(2) 0.025(3) 0.022(2) 0.0037(18) 0.0017(18) -0.0077(19) C12B 0.021(2) 0.028(3) 0.023(2) 0.0002(19) 0.0059(18) -0.0066(19) C13B 0.052(4) 0.058(4) 0.032(3) 0.021(3) 0.017(3) 0.022(3) C14B 0.056(4) 0.047(4) 0.069(5) 0.013(3) 0.030(4) 0.020(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 Ni1 N2 1.955(4) . ? Ni1 N1 1.949(4) . ? Ni1 N4 1.961(4) . ? Ni1 N3 1.965(4) . ? N1 C12 1.364(8) . ? N1 C1 1.366(7) . ? N2 C10 1.331(7) . ? N2 C11 1.416(6) . ? N3 C15 1.357(7) . ? N3 C26 1.371(7) . ? N4 C24 1.352(7) . ? N4 C25 1.388(6) . ? C1 C2 1.379(9) . ? C1 C13 1.482(10) . ? C2 C3 1.393(11) . ? C3 C4 1.394(10) . ? C4 C12 1.415(7) . ? C4 C5 1.439(10) . ? C5 C6 1.347(11) . ? C6 C7 1.433(9) . ? C7 C8 1.392(9) . ? C7 C11 1.415(8) . ? C8 C9 1.377(9) . ? C9 C10 1.393(8) . ? C10 C14 1.495(8) . ? C11 C12 1.421(8) . ? C15 C16 1.398(8) . ? C15 C27 1.501(9) . ? C16 C17 1.382(9) . ? C17 C18 1.388(8) . ? C18 C26 1.421(7) . ? C18 C19 1.427(9) . ? C19 C20 1.352(9) . ? C20 C21 1.445(8) . ? C21 C22 1.392(8) . ? C21 C25 1.404(7) . ? C22 C23 1.385(9) . ? C23 C24 1.391(8) . ? C24 C28 1.510(8) . ? C25 C26 1.412(7) . ? NiA N1A 1.955(4) 2_554 ? NiA N1A 1.955(4) . ? NiA N2A 1.958(5) . ? NiA N2A 1.958(5) 2_554 ? N1A C1A 1.350(7) . ? N1A C12A 1.384(7) . ? N2A C10A 1.368(7) . ? N2A C11A 1.368(8) . ? C1A C2A 1.386(8) . ? C1A C13A 1.482(8) . ? C2A C3A 1.393(9) . ? C3A C4A 1.383(9) . ? C4A C12A 1.413(8) . ? C4A C5A 1.446(8) . ? C5A C6A 1.324(10) . ? C6A C7A 1.425(10) . ? C7A C8A 1.400(9) . ? C7A C11A 1.428(8) . ? C8A C9A 1.388(12) . ? C9A C10A 1.389(11) . ? C10A C14A 1.499(11) . ? C11A C12A 1.417(8) . ? NiB N1B 1.953(4) 2_554 ? NiB N1B 1.953(4) . ? NiB N2B 1.957(4) 2_554 ? NiB N2B 1.957(4) . ? N1B C1B 1.342(7) . ? N1B C12B 1.395(7) . ? N2B C10B 1.362(7) . ? N2B C11B 1.386(7) . ? C1B C2B 1.400(8) . ? C1B C13B 1.490(8) . ? C2B C3B 1.380(8) . ? C3B C4B 1.387(8) . ? C4B C12B 1.411(7) . ? C4B C5B 1.448(8) . ? C5B C6B 1.345(9) . ? C6B C7B 1.442(9) . ? C7B C8B 1.380(9) . ? C7B C11B 1.422(7) . ? C8B C9B 1.397(10) . ? C9B C10B 1.397(9) . ? C10B C14B 1.489(9) . ? C11B C12B 1.409(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N1 84.09(19) . . ? N2 Ni1 N4 119.64(18) . . ? N1 Ni1 N4 128.18(18) . . ? N2 Ni1 N3 130.35(18) . . ? N1 Ni1 N3 117.40(19) . . ? N4 Ni1 N3 83.19(18) . . ? C12 N1 C1 117.5(5) . . ? C12 N1 Ni1 113.5(3) . . ? C1 N1 Ni1 129.0(4) . . ? C10 N2 C11 115.7(4) . . ? C10 N2 Ni1 132.7(4) . . ? C11 N2 Ni1 111.6(3) . . ? C15 N3 C26 117.2(5) . . ? C15 N3 Ni1 130.0(4) . . ? C26 N3 Ni1 112.8(3) . . ? C24 N4 C25 116.8(4) . . ? C24 N4 Ni1 130.5(4) . . ? C25 N4 Ni1 112.6(3) . . ? N1 C1 C2 120.8(7) . . ? N1 C1 C13 117.1(6) . . ? C2 C1 C13 122.1(6) . . ? C1 C2 C3 122.0(6) . . ? C2 C3 C4 118.3(6) . . ? C3 C4 C12 117.3(6) . . ? C3 C4 C5 125.2(6) . . ? C12 C4 C5 117.5(6) . . ? C6 C5 C4 122.4(6) . . ? C5 C6 C7 121.1(6) . . ? C8 C7 C11 116.9(5) . . ? C8 C7 C6 125.0(6) . . ? C11 C7 C6 118.1(6) . . ? C9 C8 C7 118.5(6) . . ? C8 C9 C10 122.4(6) . . ? N2 C10 C9 122.3(5) . . ? N2 C10 C14 115.8(5) . . ? C9 C10 C14 121.9(5) . . ? N2 C11 C7 124.2(5) . . ? N2 C11 C12 115.2(5) . . ? C7 C11 C12 120.7(5) . . ? N1 C12 C4 124.0(5) . . ? N1 C12 C11 115.7(5) . . ? C4 C12 C11 120.3(6) . . ? N3 C15 C16 121.3(6) . . ? N3 C15 C27 117.0(5) . . ? C16 C15 C27 121.6(5) . . ? C17 C16 C15 121.3(6) . . ? C16 C17 C18 119.0(6) . . ? C17 C18 C26 117.4(6) . . ? C17 C18 C19 124.6(6) . . ? C26 C18 C19 118.0(5) . . ? C20 C19 C18 121.5(5) . . ? C19 C20 C21 121.6(6) . . ? C22 C21 C25 117.6(5) . . ? C22 C21 C20 124.9(5) . . ? C25 C21 C20 117.5(5) . . ? C21 C22 C23 119.4(5) . . ? C24 C23 C22 120.4(5) . . ? N4 C24 C23 122.3(5) . . ? N4 C24 C28 116.6(5) . . ? C23 C24 C28 121.1(5) . . ? N4 C25 C21 123.5(5) . . ? N4 C25 C26 115.4(5) . . ? C21 C25 C26 121.2(5) . . ? N3 C26 C18 123.8(5) . . ? N3 C26 C25 115.9(5) . . ? C18 C26 C25 120.3(5) . . ? N1A NiA N1A 117.3(3) 2_554 . ? N1A NiA N2A 131.20(19) 2_554 . ? N1A NiA N2A 83.4(2) . . ? N1A NiA N2A 83.4(2) 2_554 2_554 ? N1A NiA N2A 131.20(19) . 2_554 ? N2A NiA N2A 117.0(3) . 2_554 ? C1A N1A C12A 115.9(5) . . ? C1A N1A NiA 131.5(4) . . ? C12A N1A NiA 112.6(4) . . ? C10A N2A C11A 116.9(5) . . ? C10A N2A NiA 130.1(5) . . ? C11A N2A NiA 113.0(4) . . ? N1A C1A C2A 122.2(5) . . ? N1A C1A C13A 116.2(5) . . ? C2A C1A C13A 121.6(5) . . ? C1A C2A C3A 121.8(6) . . ? C4A C3A C2A 117.8(6) . . ? C3A C4A C12A 118.0(5) . . ? C3A C4A C5A 123.6(6) . . ? C12A C4A C5A 118.4(6) . . ? C6A C5A C4A 120.8(6) . . ? C5A C6A C7A 122.6(6) . . ? C8A C7A C11A 116.6(7) . . ? C8A C7A C6A 125.1(6) . . ? C11A C7A C6A 118.3(6) . . ? C9A C8A C7A 118.0(6) . . ? C8A C9A C10A 123.2(7) . . ? N2A C10A C9A 120.4(7) . . ? N2A C10A C14A 116.9(6) . . ? C9A C10A C14A 122.7(6) . . ? N2A C11A C12A 115.6(5) . . ? N2A C11A C7A 124.9(5) . . ? C12A C11A C7A 119.4(6) . . ? N1A C12A C4A 124.2(5) . . ? N1A C12A C11A 115.4(5) . . ? C4A C12A C11A 120.4(5) . . ? N1B NiB N1B 119.8(3) 2_554 . ? N1B NiB N2B 83.56(19) 2_554 2_554 ? N1B NiB N2B 126.53(17) . 2_554 ? N1B NiB N2B 126.53(17) 2_554 . ? N1B NiB N2B 83.56(19) . . ? N2B NiB N2B 122.4(3) 2_554 . ? C1B N1B C12B 116.6(4) . . ? C1B N1B NiB 130.7(4) . . ? C12B N1B NiB 112.6(3) . . ? C10B N2B C11B 116.8(5) . . ? C10B N2B NiB 130.3(4) . . ? C11B N2B NiB 112.9(3) . . ? N1B C1B C2B 121.3(5) . . ? N1B C1B C13B 116.2(5) . . ? C2B C1B C13B 122.5(5) . . ? C3B C2B C1B 122.2(5) . . ? C2B C3B C4B 118.3(5) . . ? C3B C4B C12B 117.6(5) . . ? C3B C4B C5B 124.6(5) . . ? C12B C4B C5B 117.7(5) . . ? C6B C5B C4B 121.4(5) . . ? C5B C6B C7B 122.1(5) . . ? C8B C7B C11B 118.3(6) . . ? C8B C7B C6B 124.7(6) . . ? C11B C7B C6B 117.0(5) . . ? C7B C8B C9B 118.5(6) . . ? C10B C9B C8B 121.4(6) . . ? N2B C10B C9B 121.6(6) . . ? N2B C10B C14B 116.7(6) . . ? C9B C10B C14B 121.7(6) . . ? N2B C11B C12B 115.5(4) . . ? N2B C11B C7B 123.4(5) . . ? C12B C11B C7B 121.2(5) . . ? N1B C12B C4B 123.9(5) . . ? N1B C12B C11B 115.5(4) . . ? C4B C12B C11B 120.7(5) . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.751 _refine_diff_density_min -1.132 _refine_diff_density_rms 0.230 #===== END data_FO1270 _database_code_depnum_ccdc_archive 'CCDC 600554' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H52 Ni P4' _chemical_formula_weight 883.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.1812(6) _cell_length_b 13.2156(5) _cell_length_c 19.9132(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.690(2) _cell_angle_gamma 90.00 _cell_volume 4504.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.609 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8793 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5093 _reflns_number_gt 4239 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+4.0135P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5093 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Ni Ni 0.0000 -0.00329(2) 0.2500 0.01378(10) Uani 1 2 d S . . P1 P -0.04456(3) -0.10201(4) 0.15771(2) 0.01577(12) Uani 1 1 d . . . P2 P 0.08861(3) 0.07840(4) 0.22050(2) 0.01678(12) Uani 1 1 d . . . C1 C 0.02497(11) -0.13103(16) 0.11061(10) 0.0218(4) Uani 1 1 d . . . H1B H 0.0628(13) -0.1790(17) 0.1407(11) 0.028(6) Uiso 1 1 d . . . H1A H -0.0031(13) -0.1645(16) 0.0668(11) 0.029(6) Uiso 1 1 d . . . C2 C 0.06756(12) -0.03873(17) 0.09668(10) 0.0233(4) Uani 1 1 d . . . H2B H 0.0306(12) 0.0142(16) 0.0727(11) 0.025(6) Uiso 1 1 d . . . H2A H 0.0914(13) -0.0556(17) 0.0631(11) 0.029(6) Uiso 1 1 d . . . C3 C 0.13017(11) 0.00215(16) 0.16392(10) 0.0222(4) Uani 1 1 d . . . H3B H 0.1571(12) -0.0549(17) 0.1934(11) 0.027(6) Uiso 1 1 d . . . H3A H 0.1689(13) 0.0415(17) 0.1521(11) 0.027(6) Uiso 1 1 d . . . C4 C -0.12825(10) -0.05963(15) 0.08081(9) 0.0184(4) Uani 1 1 d . . . C5 C -0.17959(13) -0.12569(18) 0.03273(11) 0.0315(5) Uani 1 1 d . . . H5 H -0.1727(13) -0.1959(19) 0.0391(11) 0.034(6) Uiso 1 1 d . . . C6 C -0.24106(13) -0.08884(19) -0.02457(12) 0.0368(6) Uani 1 1 d . . . H6 H -0.2732(15) -0.134(2) -0.0587(14) 0.050(7) Uiso 1 1 d . . . C7 C -0.25166(12) 0.01406(18) -0.03481(11) 0.0311(5) Uani 1 1 d . . . H7 H -0.2944(14) 0.0400(18) -0.0737(12) 0.038(6) Uiso 1 1 d . . . C8 C -0.20080(12) 0.08041(17) 0.01168(10) 0.0262(4) Uani 1 1 d . . . H8 H -0.2077(14) 0.156(2) 0.0062(12) 0.042(7) Uiso 1 1 d . . . C9 C -0.13973(11) 0.04314(16) 0.06907(10) 0.0221(4) Uani 1 1 d . . . H9 H -0.1077(13) 0.0903(17) 0.1012(11) 0.029(6) Uiso 1 1 d . . . C10 C -0.07692(10) -0.23021(14) 0.17086(9) 0.0182(4) Uani 1 1 d . . . C11 C -0.13472(12) -0.23918(16) 0.20214(10) 0.0235(4) Uani 1 1 d . . . H11 H -0.1565(12) -0.1812(17) 0.2123(10) 0.026(6) Uiso 1 1 d . . . C12 C -0.15942(13) -0.33260(17) 0.21763(10) 0.0293(5) Uani 1 1 d . . . H12 H -0.1966(16) -0.338(2) 0.2398(14) 0.056(8) Uiso 1 1 d . . . C13 C -0.12607(13) -0.41965(17) 0.20299(11) 0.0318(5) Uani 1 1 d . . . H13 H -0.1409(13) -0.4800(18) 0.2143(11) 0.032(6) Uiso 1 1 d . . . C14 C -0.06902(13) -0.41313(17) 0.17178(11) 0.0310(5) Uani 1 1 d . . . H14 H -0.0462(14) -0.472(2) 0.1621(12) 0.042(7) Uiso 1 1 d . . . C15 C -0.04514(12) -0.31920(16) 0.15515(10) 0.0257(4) Uani 1 1 d . . . H15 H -0.0049(14) -0.3171(18) 0.1356(12) 0.038(6) Uiso 1 1 d . . . C16 C 0.06216(11) 0.19322(15) 0.16351(10) 0.0229(4) Uani 1 1 d . . . C17 C 0.10884(15) 0.23190(18) 0.12636(12) 0.0365(5) Uani 1 1 d . . . H17 H 0.1569(14) 0.2032(18) 0.1324(11) 0.035(6) Uiso 1 1 d . . . C18 C 0.08397(18) 0.3136(2) 0.08024(14) 0.0488(7) Uani 1 1 d . . . H18 H 0.1150(15) 0.336(2) 0.0534(14) 0.055(8) Uiso 1 1 d . . . C19 C 0.01245(18) 0.3577(2) 0.07081(14) 0.0501(7) Uani 1 1 d . . . H19 H -0.0054(16) 0.411(2) 0.0405(14) 0.055(8) Uiso 1 1 d . . . C20 C -0.03383(16) 0.32181(18) 0.10796(13) 0.0413(6) Uani 1 1 d . . . H20 H -0.0825(16) 0.349(2) 0.1019(13) 0.048(7) Uiso 1 1 d . . . C21 C -0.00870(12) 0.24022(16) 0.15400(11) 0.0275(5) Uani 1 1 d . . . H21 H -0.0398(12) 0.2143(16) 0.1790(11) 0.024(5) Uiso 1 1 d . . . C22 C 0.18090(11) 0.12254(15) 0.28760(9) 0.0206(4) Uani 1 1 d . . . C23 C 0.19436(12) 0.22438(17) 0.30662(11) 0.0258(4) Uani 1 1 d . . . H23 H 0.1579(13) 0.2700(17) 0.2845(11) 0.026(6) Uiso 1 1 d . . . C24 C 0.26313(14) 0.25396(19) 0.35945(11) 0.0330(5) Uani 1 1 d . . . H24 H 0.2682(14) 0.322(2) 0.3689(12) 0.044(7) Uiso 1 1 d . . . C25 C 0.31911(13) 0.18407(19) 0.39367(11) 0.0355(5) Uani 1 1 d . . . H25 H 0.3664(15) 0.2036(19) 0.4300(13) 0.047(7) Uiso 1 1 d . . . C26 C 0.30670(13) 0.08310(19) 0.37565(11) 0.0333(5) Uani 1 1 d . . . H26 H 0.3442(15) 0.033(2) 0.3986(13) 0.044(7) Uiso 1 1 d . . . C27 C 0.23804(11) 0.05247(17) 0.32353(10) 0.0248(4) Uani 1 1 d . . . H27 H 0.2273(12) -0.0197(18) 0.3122(11) 0.029(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 Ni 0.01289(17) 0.01528(18) 0.01351(16) 0.000 0.00489(12) 0.000 P1 0.0145(2) 0.0177(2) 0.0149(2) -0.00129(17) 0.00460(17) -0.00029(19) P2 0.0152(2) 0.0180(3) 0.0180(2) 0.00023(18) 0.00679(18) -0.00115(19) C1 0.0211(10) 0.0254(11) 0.0202(9) -0.0060(8) 0.0086(8) -0.0006(9) C2 0.0230(10) 0.0317(12) 0.0187(9) -0.0031(8) 0.0115(8) -0.0014(9) C3 0.0202(10) 0.0261(11) 0.0240(10) 0.0001(8) 0.0123(8) -0.0010(9) C4 0.0177(9) 0.0225(10) 0.0154(8) -0.0010(7) 0.0061(7) -0.0002(8) C5 0.0348(12) 0.0254(12) 0.0255(10) 0.0028(9) -0.0013(9) -0.0030(10) C6 0.0327(13) 0.0368(14) 0.0279(11) 0.0020(10) -0.0071(9) -0.0089(11) C7 0.0230(11) 0.0421(14) 0.0227(10) 0.0075(9) 0.0007(8) 0.0058(10) C8 0.0302(11) 0.0271(12) 0.0222(10) 0.0034(8) 0.0101(8) 0.0079(9) C9 0.0242(10) 0.0240(11) 0.0181(9) -0.0025(8) 0.0071(8) -0.0006(9) C10 0.0185(9) 0.0196(10) 0.0134(8) -0.0014(7) 0.0013(7) -0.0009(8) C11 0.0235(10) 0.0224(11) 0.0241(10) -0.0012(8) 0.0074(8) -0.0001(9) C12 0.0296(12) 0.0311(13) 0.0263(11) 0.0022(9) 0.0081(9) -0.0093(10) C13 0.0374(13) 0.0212(12) 0.0290(11) 0.0028(9) 0.0010(9) -0.0097(10) C14 0.0336(12) 0.0189(11) 0.0337(11) -0.0027(9) 0.0025(9) 0.0021(9) C15 0.0228(10) 0.0258(11) 0.0272(10) -0.0044(8) 0.0067(8) -0.0010(9) C16 0.0253(10) 0.0208(10) 0.0222(9) 0.0011(8) 0.0076(8) -0.0024(8) C17 0.0421(14) 0.0310(13) 0.0428(13) 0.0114(10) 0.0227(11) 0.0031(11) C18 0.072(2) 0.0369(15) 0.0459(14) 0.0151(11) 0.0307(14) -0.0045(14) C19 0.070(2) 0.0257(13) 0.0481(15) 0.0158(11) 0.0109(13) 0.0028(13) C20 0.0391(14) 0.0257(13) 0.0514(15) 0.0071(10) 0.0051(11) 0.0071(11) C21 0.0282(11) 0.0202(11) 0.0330(11) 0.0007(8) 0.0088(9) -0.0021(9) C22 0.0172(9) 0.0277(11) 0.0188(9) -0.0005(8) 0.0084(7) -0.0059(8) C23 0.0259(11) 0.0268(12) 0.0275(10) -0.0039(9) 0.0126(9) -0.0039(9) C24 0.0377(13) 0.0337(13) 0.0312(11) -0.0093(10) 0.0162(10) -0.0163(11) C25 0.0281(12) 0.0497(15) 0.0252(11) -0.0040(10) 0.0046(9) -0.0165(11) C26 0.0232(11) 0.0460(15) 0.0271(11) 0.0074(10) 0.0038(9) -0.0025(11) C27 0.0213(10) 0.0262(12) 0.0265(10) 0.0027(8) 0.0075(8) -0.0050(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 Ni P1 2.1754(5) . ? Ni P1 2.1755(5) 2 ? Ni P2 2.1780(5) 2 ? Ni P2 2.1781(5) . ? P1 C10 1.8409(19) . ? P1 C4 1.8449(18) . ? P1 C1 1.8503(19) . ? P2 C3 1.8519(19) . ? P2 C22 1.8521(19) . ? P2 C16 1.858(2) . ? C1 C2 1.520(3) . ? C2 C3 1.534(3) . ? C4 C9 1.382(3) . ? C4 C5 1.396(3) . ? C5 C6 1.389(3) . ? C6 C7 1.379(3) . ? C7 C8 1.380(3) . ? C8 C9 1.388(3) . ? C10 C15 1.392(3) . ? C10 C11 1.395(3) . ? C11 C12 1.384(3) . ? C12 C13 1.377(3) . ? C13 C14 1.380(3) . ? C14 C15 1.391(3) . ? C16 C21 1.385(3) . ? C16 C17 1.397(3) . ? C17 C18 1.390(3) . ? C18 C19 1.379(4) . ? C19 C20 1.378(4) . ? C20 C21 1.389(3) . ? C22 C23 1.397(3) . ? C22 C27 1.396(3) . ? C23 C24 1.392(3) . ? C24 C25 1.373(3) . ? C25 C26 1.381(3) . ? C26 C27 1.388(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ni P1 106.30(3) . 2 ? P1 Ni P2 115.236(17) . 2 ? P1 Ni P2 99.681(17) 2 2 ? P1 Ni P2 99.681(17) . . ? P1 Ni P2 115.235(17) 2 . ? P2 Ni P2 120.57(3) 2 . ? C10 P1 C4 100.58(8) . . ? C10 P1 C1 100.78(9) . . ? C4 P1 C1 98.95(9) . . ? C10 P1 Ni 118.53(6) . . ? C4 P1 Ni 119.17(6) . . ? C1 P1 Ni 115.40(6) . . ? C3 P2 C22 98.86(9) . . ? C3 P2 C16 98.48(9) . . ? C22 P2 C16 99.70(9) . . ? C3 P2 Ni 112.64(7) . . ? C22 P2 Ni 122.29(6) . . ? C16 P2 Ni 120.44(6) . . ? C2 C1 P1 113.79(14) . . ? C1 C2 C3 113.41(16) . . ? C2 C3 P2 112.81(13) . . ? C9 C4 C5 118.08(17) . . ? C9 C4 P1 118.30(14) . . ? C5 C4 P1 123.60(15) . . ? C6 C5 C4 120.8(2) . . ? C7 C6 C5 120.1(2) . . ? C6 C7 C8 119.92(19) . . ? C7 C8 C9 119.7(2) . . ? C4 C9 C8 121.43(18) . . ? C15 C10 C11 117.43(18) . . ? C15 C10 P1 124.68(15) . . ? C11 C10 P1 117.81(15) . . ? C12 C11 C10 121.7(2) . . ? C13 C12 C11 119.9(2) . . ? C12 C13 C14 119.7(2) . . ? C13 C14 C15 120.3(2) . . ? C14 C15 C10 120.9(2) . . ? C21 C16 C17 117.82(19) . . ? C21 C16 P2 119.16(15) . . ? C17 C16 P2 122.93(16) . . ? C18 C17 C16 120.9(2) . . ? C19 C18 C17 120.0(2) . . ? C20 C19 C18 120.0(2) . . ? C19 C20 C21 119.8(2) . . ? C16 C21 C20 121.5(2) . . ? C23 C22 C27 117.91(18) . . ? C23 C22 P2 122.16(15) . . ? C27 C22 P2 119.85(15) . . ? C22 C23 C24 120.4(2) . . ? C25 C24 C23 120.9(2) . . ? C24 C25 C26 119.5(2) . . ? C25 C26 C27 120.2(2) . . ? C26 C27 C22 121.1(2) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.309 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.055 #===== END data_FO1664 _database_code_depnum_ccdc_archive 'CCDC 600555' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H56 Ni P4' _chemical_formula_weight 911.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.9448(4) _cell_length_b 11.8350(3) _cell_length_c 20.0660(4) _cell_angle_alpha 90.00 _cell_angle_beta 110.142(2) _cell_angle_gamma 90.00 _cell_volume 4669.79(18) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.590 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9633 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 27.46 _reflns_number_total 5338 _reflns_number_gt 4257 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0420P)^2^+2.5743P] 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 5338 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.0000 0.95551(2) 0.7500 0.01985(9) Uani 1 2 d S . . P1 P 0.07778(2) 1.04944(4) 0.72139(2) 0.02380(11) Uani 1 1 d . . . P2 P -0.04523(2) 0.83862(3) 0.66037(2) 0.02231(10) Uani 1 1 d . . . C1 C 0.11104(8) 0.96967(15) 0.66090(8) 0.0293(4) Uani 1 1 d . . . H1A H 0.1503 1.0104 0.6556 0.035 Uiso 1 1 calc R . . H1B H 0.1268 0.8943 0.6813 0.035 Uiso 1 1 calc R . . C2 C 0.05478(9) 0.95599(15) 0.58725(8) 0.0307(4) Uani 1 1 d . . . H2A H 0.0145 1.0001 0.5868 0.037 Uiso 1 1 calc R . . H2B H 0.0713 0.9887 0.5508 0.037 Uiso 1 1 calc R . . C3 C 0.03283(9) 0.83428(15) 0.56671(9) 0.0317(4) Uani 1 1 d . . . H3A H 0.0709 0.7943 0.5584 0.038 Uiso 1 1 calc R . . H3B H -0.0057 0.8353 0.5211 0.038 Uiso 1 1 calc R . . C4 C 0.01130(8) 0.76555(15) 0.62022(8) 0.0283(3) Uani 1 1 d . . . H4A H 0.0529 0.7413 0.6590 0.034 Uiso 1 1 calc R . . H4B H -0.0121 0.6964 0.5962 0.034 Uiso 1 1 calc R . . C5 C 0.15892(8) 1.10078(15) 0.78754(9) 0.0303(4) Uani 1 1 d . . . C6 C 0.16417(10) 1.20985(17) 0.81454(10) 0.0417(5) Uani 1 1 d . . . H6A H 0.1269 1.2603 0.7961 0.050 Uiso 1 1 calc R . . C7 C 0.22263(11) 1.2469(2) 0.86785(12) 0.0555(6) Uani 1 1 d . . . H7A H 0.2250 1.3219 0.8855 0.067 Uiso 1 1 calc R . . C8 C 0.27687(11) 1.1751(2) 0.89486(12) 0.0556(6) Uani 1 1 d . . . H8A H 0.3165 1.1995 0.9320 0.067 Uiso 1 1 calc R . . C9 C 0.27344(10) 1.0681(2) 0.86797(11) 0.0491(5) Uani 1 1 d . . . H9A H 0.3112 1.0187 0.8861 0.059 Uiso 1 1 calc R . . C10 C 0.21508(9) 1.03098(17) 0.81437(10) 0.0385(4) Uani 1 1 d . . . H10A H 0.2137 0.9567 0.7959 0.046 Uiso 1 1 calc R . . C11 C 0.05423(9) 1.18143(15) 0.66838(9) 0.0314(4) Uani 1 1 d . . . C12 C -0.00956(10) 1.22719(16) 0.65411(9) 0.0381(4) Uani 1 1 d . . . H12A H -0.0402 1.1919 0.6732 0.046 Uiso 1 1 calc R . . C13 C -0.03037(13) 1.32362(18) 0.61253(11) 0.0522(6) Uani 1 1 d . . . H13A H -0.0747 1.3534 0.6033 0.063 Uiso 1 1 calc R . . C14 C 0.01385(15) 1.37543(18) 0.58496(12) 0.0601(7) Uani 1 1 d . . . H14A H 0.0003 1.4417 0.5569 0.072 Uiso 1 1 calc R . . C15 C 0.07769(14) 1.33107(19) 0.59812(12) 0.0567(6) Uani 1 1 d . . . H15A H 0.1081 1.3665 0.5787 0.068 Uiso 1 1 calc R . . C16 C 0.09788(11) 1.23527(19) 0.63940(11) 0.0469(5) Uani 1 1 d . . . H16A H 0.1422 1.2056 0.6482 0.056 Uiso 1 1 calc R . . C17 C -0.08903(8) 0.71561(14) 0.68193(8) 0.0272(3) Uani 1 1 d . . . C18 C -0.14662(9) 0.73685(16) 0.69954(9) 0.0327(4) Uani 1 1 d . . . H18A H -0.1639 0.8117 0.6956 0.039 Uiso 1 1 calc R . . C19 C -0.17957(10) 0.65201(17) 0.72271(9) 0.0389(4) Uani 1 1 d . . . H19A H -0.2191 0.6689 0.7339 0.047 Uiso 1 1 calc R . . C20 C -0.15473(11) 0.54273(17) 0.72948(11) 0.0446(5) Uani 1 1 d . . . H20A H -0.1763 0.4843 0.7464 0.054 Uiso 1 1 calc R . . C21 C -0.09852(12) 0.51999(17) 0.71146(12) 0.0492(5) Uani 1 1 d . . . H21A H -0.0813 0.4451 0.7159 0.059 Uiso 1 1 calc R . . C22 C -0.06632(10) 0.60481(15) 0.68683(10) 0.0390(4) Uani 1 1 d . . . H22A H -0.0284 0.5866 0.6732 0.047 Uiso 1 1 calc R . . C23 C -0.11383(8) 0.88379(15) 0.57876(8) 0.0265(3) Uani 1 1 d . . . C24 C -0.15108(9) 0.80570(17) 0.52814(9) 0.0374(4) Uani 1 1 d . . . H24A H -0.1411 0.7274 0.5354 0.045 Uiso 1 1 calc R . . C25 C -0.20272(10) 0.8416(2) 0.46725(10) 0.0456(5) Uani 1 1 d . . . H25A H -0.2273 0.7880 0.4327 0.055 Uiso 1 1 calc R . . C26 C -0.21817(10) 0.9547(2) 0.45701(10) 0.0465(5) Uani 1 1 d . . . H26A H -0.2541 0.9791 0.4159 0.056 Uiso 1 1 calc R . . C27 C -0.18152(10) 1.03270(19) 0.50641(10) 0.0442(5) Uani 1 1 d . . . H27A H -0.1918 1.1109 0.4990 0.053 Uiso 1 1 calc R . . C28 C -0.12951(9) 0.99717(16) 0.56713(9) 0.0332(4) Uani 1 1 d . . . H28A H -0.1045 1.0514 0.6010 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.02190(15) 0.02085(15) 0.01606(14) 0.000 0.00557(10) 0.000 P1 0.0250(2) 0.0258(2) 0.0208(2) -0.00036(16) 0.00809(16) -0.00325(16) P2 0.0238(2) 0.0236(2) 0.01751(19) -0.00120(16) 0.00452(15) -0.00009(16) C1 0.0278(8) 0.0375(10) 0.0254(8) -0.0031(7) 0.0127(7) -0.0029(7) C2 0.0336(9) 0.0393(10) 0.0211(8) 0.0002(7) 0.0119(7) -0.0013(7) C3 0.0338(9) 0.0395(10) 0.0232(8) -0.0045(7) 0.0118(7) 0.0008(8) C4 0.0303(8) 0.0290(9) 0.0250(8) -0.0048(7) 0.0089(6) 0.0011(7) C5 0.0286(8) 0.0355(10) 0.0278(8) -0.0012(7) 0.0108(7) -0.0074(7) C6 0.0381(10) 0.0411(11) 0.0426(11) -0.0102(9) 0.0097(8) -0.0065(8) C7 0.0491(13) 0.0536(14) 0.0568(13) -0.0228(11) 0.0094(10) -0.0156(11) C8 0.0388(11) 0.0743(17) 0.0448(12) -0.0120(12) 0.0030(9) -0.0198(11) C9 0.0328(10) 0.0588(14) 0.0479(12) 0.0053(11) 0.0038(9) -0.0062(9) C10 0.0316(9) 0.0414(11) 0.0396(10) 0.0037(8) 0.0085(8) -0.0048(8) C11 0.0404(9) 0.0279(9) 0.0264(8) -0.0008(7) 0.0121(7) -0.0063(7) C12 0.0525(11) 0.0334(10) 0.0310(9) 0.0035(8) 0.0178(8) 0.0037(9) C13 0.0772(16) 0.0388(12) 0.0437(11) 0.0099(9) 0.0246(11) 0.0202(11) C14 0.112(2) 0.0296(11) 0.0433(12) 0.0096(10) 0.0322(13) 0.0050(12) C15 0.0850(18) 0.0405(12) 0.0505(13) 0.0066(10) 0.0309(12) -0.0178(12) C16 0.0531(12) 0.0461(12) 0.0453(11) 0.0044(10) 0.0217(10) -0.0136(10) C17 0.0316(8) 0.0271(9) 0.0186(7) -0.0021(6) 0.0032(6) -0.0045(7) C18 0.0349(9) 0.0327(9) 0.0295(9) 0.0000(7) 0.0096(7) -0.0017(7) C19 0.0365(10) 0.0468(12) 0.0337(9) 0.0015(9) 0.0126(8) -0.0096(8) C20 0.0565(13) 0.0389(11) 0.0398(11) 0.0002(9) 0.0181(10) -0.0172(9) C21 0.0699(14) 0.0264(10) 0.0546(13) 0.0021(9) 0.0256(11) -0.0026(9) C22 0.0498(11) 0.0289(10) 0.0417(10) 0.0002(8) 0.0202(9) 0.0004(8) C23 0.0249(8) 0.0346(9) 0.0195(7) 0.0019(7) 0.0069(6) -0.0002(7) C24 0.0365(9) 0.0398(10) 0.0283(9) -0.0007(8) 0.0016(7) -0.0054(8) C25 0.0382(10) 0.0614(14) 0.0267(9) -0.0001(9) -0.0021(8) -0.0121(10) C26 0.0352(10) 0.0730(15) 0.0245(9) 0.0120(10) 0.0014(8) 0.0100(10) C27 0.0500(12) 0.0502(12) 0.0302(10) 0.0130(9) 0.0110(9) 0.0178(10) C28 0.0388(10) 0.0373(10) 0.0220(8) 0.0021(7) 0.0087(7) 0.0045(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni P1 2.2054(4) . ? Ni P1 2.2054(4) 2_556 ? Ni P2 2.2073(4) . ? Ni P2 2.2074(4) 2_556 ? P1 C1 1.8524(17) . ? P1 C11 1.8583(18) . ? P1 C5 1.8616(17) . ? P2 C23 1.8471(15) . ? P2 C17 1.8497(17) . ? P2 C4 1.8591(16) . ? C1 C2 1.549(2) . ? C2 C3 1.525(3) . ? C3 C4 1.533(2) . ? C5 C10 1.385(3) . ? C5 C6 1.390(3) . ? C6 C7 1.391(3) . ? C7 C8 1.372(3) . ? C8 C9 1.369(3) . ? C9 C10 1.392(3) . ? C11 C12 1.377(3) . ? C11 C16 1.395(3) . ? C12 C13 1.392(3) . ? C13 C14 1.376(3) . ? C14 C15 1.375(4) . ? C15 C16 1.382(3) . ? C17 C22 1.387(3) . ? C17 C18 1.392(2) . ? C18 C19 1.386(3) . ? C19 C20 1.383(3) . ? C20 C21 1.372(3) . ? C21 C22 1.392(3) . ? C23 C28 1.382(3) . ? C23 C24 1.396(2) . ? C24 C25 1.390(3) . ? C25 C26 1.376(3) . ? C26 C27 1.378(3) . ? C27 C28 1.391(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ni P1 119.46(2) . 2_556 ? P1 Ni P2 104.600(15) . . ? P1 Ni P2 112.318(15) 2_556 . ? P1 Ni P2 112.320(15) . 2_556 ? P1 Ni P2 104.599(15) 2_556 2_556 ? P2 Ni P2 102.38(2) . 2_556 ? C1 P1 C11 97.99(8) . . ? C1 P1 C5 100.17(8) . . ? C11 P1 C5 97.53(8) . . ? C1 P1 Ni 113.07(6) . . ? C11 P1 Ni 119.90(6) . . ? C5 P1 Ni 123.62(5) . . ? C23 P2 C17 97.94(7) . . ? C23 P2 C4 99.64(7) . . ? C17 P2 C4 100.16(8) . . ? C23 P2 Ni 121.71(6) . . ? C17 P2 Ni 114.27(5) . . ? C4 P2 Ni 119.08(5) . . ? C2 C1 P1 110.13(11) . . ? C3 C2 C1 114.58(14) . . ? C2 C3 C4 116.48(14) . . ? C3 C4 P2 116.20(12) . . ? C10 C5 C6 117.38(17) . . ? C10 C5 P1 121.79(14) . . ? C6 C5 P1 120.75(14) . . ? C5 C6 C7 121.6(2) . . ? C8 C7 C6 119.9(2) . . ? C9 C8 C7 119.57(19) . . ? C8 C9 C10 120.6(2) . . ? C5 C10 C9 120.9(2) . . ? C12 C11 C16 117.50(18) . . ? C12 C11 P1 119.79(14) . . ? C16 C11 P1 122.66(16) . . ? C11 C12 C13 121.88(19) . . ? C14 C13 C12 119.4(2) . . ? C15 C14 C13 119.8(2) . . ? C14 C15 C16 120.3(2) . . ? C15 C16 C11 121.0(2) . . ? C22 C17 C18 117.32(16) . . ? C22 C17 P2 125.11(14) . . ? C18 C17 P2 117.40(13) . . ? C19 C18 C17 121.97(18) . . ? C20 C19 C18 119.76(18) . . ? C21 C20 C19 119.05(18) . . ? C20 C21 C22 121.12(19) . . ? C17 C22 C21 120.73(19) . . ? C28 C23 C24 118.63(15) . . ? C28 C23 P2 119.85(13) . . ? C24 C23 P2 121.51(14) . . ? C25 C24 C23 120.53(19) . . ? C26 C25 C24 120.00(19) . . ? C27 C26 C25 120.00(17) . . ? C26 C27 C28 120.13(19) . . ? C23 C28 C27 120.69(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.288 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.050 #===== END data_FO1460 _database_code_depnum_ccdc_archive 'CCDC 600556' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H79 Ni2 O2 P7 * 2 C7 H8' _chemical_formula_weight 1711.01 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' 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' 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 13.8923(5) _cell_length_b 16.8347(9) _cell_length_c 24.148(1) _cell_angle_alpha 103.947(3) _cell_angle_beta 95.888(3) _cell_angle_gamma 113.132(3) _cell_volume 4915.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas green _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.542 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32946 _diffrn_reflns_av_R_equivalents 0.1049 _diffrn_reflns_av_sigmaI/netI 0.2267 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.49 _reflns_number_total 21771 _reflns_number_gt 9129 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.1308P)^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 21771 _refine_ls_number_parameters 943 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1962 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.2664 _refine_ls_wR_factor_gt 0.2219 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.007 _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 Ni1 Ni 0.49897(6) 0.28598(5) 0.17144(3) 0.0357(2) Uani 1 1 d . . . Ni2 Ni 0.48189(6) 0.20737(5) 0.25098(4) 0.0364(2) Uani 1 1 d . . . P1 P 0.39780(13) 0.28284(11) 0.23193(7) 0.0379(4) Uani 1 1 d . . . O1 O 0.4658(3) 0.0951(3) 0.1865(2) 0.0439(11) Uani 1 1 d . . . O2 O 0.4621(3) 0.1587(3) 0.11531(18) 0.0423(10) Uani 1 1 d . . . C1 C 0.4121(8) -0.0128(7) 0.0361(5) 0.096(3) Uani 1 1 d . . . H1A H 0.4114 0.0325 0.0193 0.115 Uiso 1 1 calc R . . H1B H 0.3979 -0.0714 0.0117 0.115 Uiso 1 1 calc R . . C2 C 0.4319(5) 0.0047(5) 0.0907(3) 0.0579(19) Uani 1 1 d . . . H2A H 0.4318 -0.0426 0.1057 0.069 Uiso 1 1 calc R . . C3 C 0.4556(5) 0.0931(4) 0.1340(3) 0.0431(16) Uani 1 1 d . . . C4 C 0.4230(5) 0.3881(5) 0.2876(3) 0.0434(15) Uani 1 1 d . . . C5 C 0.3807(6) 0.3888(5) 0.3372(3) 0.0578(19) Uani 1 1 d . . . H5A H 0.3303 0.3335 0.3407 0.069 Uiso 1 1 calc R . . C6 C 0.4115(7) 0.4700(6) 0.3822(4) 0.073(2) Uani 1 1 d . . . H6A H 0.3838 0.4689 0.4166 0.087 Uiso 1 1 calc R . . C7 C 0.4809(8) 0.5506(6) 0.3773(4) 0.076(2) Uani 1 1 d . . . H7A H 0.5011 0.6056 0.4078 0.091 Uiso 1 1 calc R . . C8 C 0.5223(7) 0.5514(5) 0.3264(4) 0.066(2) Uani 1 1 d . . . H8A H 0.5695 0.6070 0.3217 0.079 Uiso 1 1 calc R . . C9 C 0.4931(6) 0.4694(5) 0.2831(3) 0.0578(19) Uani 1 1 d . . . H9A H 0.5228 0.4698 0.2494 0.069 Uiso 1 1 calc R . . C10 C 0.2526(5) 0.2261(4) 0.2077(3) 0.0393(15) Uani 1 1 d . . . C11 C 0.2066(5) 0.1378(5) 0.1673(3) 0.0458(16) Uani 1 1 d . . . H11A H 0.2522 0.1113 0.1538 0.055 Uiso 1 1 calc R . . C12 C 0.0979(5) 0.0896(5) 0.1473(3) 0.0559(19) Uani 1 1 d . . . H12A H 0.0687 0.0305 0.1199 0.067 Uiso 1 1 calc R . . C13 C 0.0300(6) 0.1278(7) 0.1673(4) 0.067(2) Uani 1 1 d . . . H13A H -0.0457 0.0937 0.1551 0.081 Uiso 1 1 calc R . . C14 C 0.0729(6) 0.2135(6) 0.2041(4) 0.069(2) Uani 1 1 d . . . H14A H 0.0265 0.2398 0.2167 0.082 Uiso 1 1 calc R . . C15 C 0.1837(5) 0.2643(5) 0.2241(3) 0.0567(19) Uani 1 1 d . . . H15A H 0.2120 0.3251 0.2489 0.068 Uiso 1 1 calc R . . P1A P 0.20578(14) -0.06910(13) 0.28548(9) 0.0489(5) Uani 1 1 d . . . P2A P 0.38847(13) 0.12672(12) 0.30216(8) 0.0399(4) Uani 1 1 d . . . C1A C 0.2777(5) 0.0232(4) 0.2539(3) 0.0455(16) Uani 1 1 d . . . H1AA H 0.3055 -0.0026 0.2215 0.055 Uiso 1 1 calc R . . H1AB H 0.2240 0.0404 0.2364 0.055 Uiso 1 1 calc R . . C2A C 0.1876(5) -0.1686(5) 0.2261(3) 0.0490(17) Uani 1 1 d . . . C3A C 0.2775(6) -0.1701(6) 0.2041(4) 0.063(2) Uani 1 1 d . . . H3AA H 0.3452 -0.1188 0.2185 0.076 Uiso 1 1 calc R . . C4A C 0.2667(6) -0.2469(6) 0.1612(4) 0.075(2) Uani 1 1 d . . . H4AA H 0.3270 -0.2468 0.1459 0.089 Uiso 1 1 calc R . . C5A C 0.1702(7) -0.3229(6) 0.1406(4) 0.078(3) Uani 1 1 d . . . H5AA H 0.1636 -0.3748 0.1112 0.093 Uiso 1 1 calc R . . C6A C 0.0828(6) -0.3227(6) 0.1634(5) 0.079(3) Uani 1 1 d . . . H6AA H 0.0158 -0.3750 0.1503 0.094 Uiso 1 1 calc R . . C7A C 0.0937(6) -0.2466(5) 0.2051(4) 0.065(2) Uani 1 1 d . . . H7AA H 0.0328 -0.2478 0.2202 0.078 Uiso 1 1 calc R . . C8A C 0.0696(5) -0.0758(5) 0.2749(3) 0.0518(18) Uani 1 1 d . . . C9A C 0.0136(5) -0.0786(5) 0.2222(3) 0.0547(19) Uani 1 1 d . . . H9AA H 0.0460 -0.0785 0.1895 0.066 Uiso 1 1 calc R . . C10A C -0.0885(6) -0.0814(6) 0.2170(4) 0.068(2) Uani 1 1 d . . . H10A H -0.1255 -0.0845 0.1806 0.082 Uiso 1 1 calc R . . C11A C -0.1346(7) -0.0798(6) 0.2631(5) 0.085(3) Uani 1 1 d . . . H11B H -0.2047 -0.0826 0.2591 0.102 Uiso 1 1 calc R . . C12A C -0.0805(8) -0.0742(8) 0.3169(5) 0.096(3) Uani 1 1 d . . . H12B H -0.1126 -0.0713 0.3498 0.115 Uiso 1 1 calc R . . C13A C 0.0240(6) -0.0728(7) 0.3224(4) 0.079(3) Uani 1 1 d . . . H13B H 0.0611 -0.0698 0.3587 0.095 Uiso 1 1 calc R . . C14A C 0.4619(5) 0.0812(4) 0.3431(3) 0.0487(17) Uani 1 1 d . . . C15A C 0.5331(5) 0.0551(5) 0.3157(4) 0.059(2) Uani 1 1 d . . . H15B H 0.5389 0.0601 0.2777 0.071 Uiso 1 1 calc R . . C16A C 0.5954(6) 0.0222(6) 0.3423(5) 0.077(3) Uani 1 1 d . . . H16A H 0.6420 0.0034 0.3223 0.093 Uiso 1 1 calc R . . C17A C 0.5900(7) 0.0168(6) 0.3973(5) 0.083(3) Uani 1 1 d . . . H17A H 0.6348 -0.0031 0.4168 0.100 Uiso 1 1 calc R . . C18A C 0.5186(7) 0.0407(6) 0.4241(4) 0.078(3) Uani 1 1 d . . . H18A H 0.5130 0.0345 0.4619 0.094 Uiso 1 1 calc R . . C19A C 0.4542(6) 0.0736(5) 0.3986(4) 0.060(2) Uani 1 1 d . . . H19A H 0.4063 0.0903 0.4185 0.072 Uiso 1 1 calc R . . C20A C 0.3251(5) 0.1741(5) 0.3553(3) 0.0488(17) Uani 1 1 d . . . C21A C 0.2174(5) 0.1556(5) 0.3426(3) 0.0536(18) Uani 1 1 d . . . H21A H 0.1721 0.1129 0.3064 0.064 Uiso 1 1 calc R . . C22A C 0.1762(6) 0.1991(6) 0.3823(4) 0.071(2) Uani 1 1 d . . . H22A H 0.1022 0.1858 0.3730 0.085 Uiso 1 1 calc R . . C23A C 0.2388(8) 0.2615(7) 0.4352(4) 0.078(3) Uani 1 1 d . . . H23A H 0.2083 0.2894 0.4626 0.094 Uiso 1 1 calc R . . C24A C 0.3480(7) 0.2826(6) 0.4477(3) 0.065(2) Uani 1 1 d . . . H24A H 0.3929 0.3275 0.4832 0.078 Uiso 1 1 calc R . . C25A C 0.3907(6) 0.2399(5) 0.4097(3) 0.0571(19) Uani 1 1 d . . . H25A H 0.4647 0.2537 0.4193 0.069 Uiso 1 1 calc R . . P1B P 0.25555(13) 0.26306(12) -0.00668(8) 0.0430(4) Uani 1 1 d . . . P2B P 0.43540(12) 0.33069(11) 0.10496(7) 0.0379(4) Uani 1 1 d . . . C1B C 0.3057(4) 0.2427(5) 0.0609(3) 0.0431(16) Uani 1 1 d . . . H1BA H 0.2520 0.2366 0.0855 0.052 Uiso 1 1 calc R . . H1BB H 0.3110 0.1843 0.0494 0.052 Uiso 1 1 calc R . . C2B C 0.2951(4) 0.1924(4) -0.0615(3) 0.0409(15) Uani 1 1 d . . . C3B C 0.3543(5) 0.2331(5) -0.0985(3) 0.0509(17) Uani 1 1 d . . . H3BA H 0.3705 0.2945 -0.0958 0.061 Uiso 1 1 calc R . . C4B C 0.3900(5) 0.1823(6) -0.1401(3) 0.059(2) Uani 1 1 d . . . H4BA H 0.4285 0.2094 -0.1661 0.071 Uiso 1 1 calc R . . C5B C 0.3700(5) 0.0961(6) -0.1432(3) 0.060(2) Uani 1 1 d . . . H5BA H 0.3965 0.0634 -0.1703 0.072 Uiso 1 1 calc R . . C6B C 0.3104(6) 0.0551(5) -0.1066(3) 0.0573(19) Uani 1 1 d . . . H6BA H 0.2957 -0.0058 -0.1089 0.069 Uiso 1 1 calc R . . C7B C 0.2725(5) 0.1032(5) -0.0669(3) 0.0532(18) Uani 1 1 d . . . H7BA H 0.2301 0.0742 -0.0429 0.064 Uiso 1 1 calc R . . C8B C 0.1104(5) 0.1957(4) -0.0202(3) 0.0414(15) Uani 1 1 d . . . C9B C 0.0450(5) 0.2067(5) -0.0621(4) 0.059(2) Uani 1 1 d . . . H9BA H 0.0777 0.2449 -0.0845 0.071 Uiso 1 1 calc R . . C10B C -0.0641(6) 0.1651(6) -0.0726(4) 0.069(2) Uani 1 1 d . . . H10B H -0.1054 0.1762 -0.1011 0.082 Uiso 1 1 calc R . . C11B C -0.1151(6) 0.1070(6) -0.0423(4) 0.070(2) Uani 1 1 d . . . H11C H -0.1912 0.0769 -0.0501 0.083 Uiso 1 1 calc R . . C12B C -0.0525(6) 0.0933(6) 0.0000(4) 0.072(2) Uani 1 1 d . . . H12C H -0.0856 0.0543 0.0219 0.087 Uiso 1 1 calc R . . C13B C 0.0596(5) 0.1376(5) 0.0099(3) 0.060(2) Uani 1 1 d . . . H13C H 0.1017 0.1271 0.0383 0.072 Uiso 1 1 calc R . . C14B C 0.5145(4) 0.3494(4) 0.0492(3) 0.0390(15) Uani 1 1 d . . . C15B C 0.5409(5) 0.4236(5) 0.0273(3) 0.0460(16) Uani 1 1 d . . . H15C H 0.5147 0.4675 0.0405 0.055 Uiso 1 1 calc R . . C16B C 0.6055(5) 0.4340(5) -0.0139(3) 0.0498(18) Uani 1 1 d . . . H16B H 0.6247 0.4850 -0.0279 0.060 Uiso 1 1 calc R . . C17B C 0.6407(5) 0.3678(6) -0.0337(3) 0.058(2) Uani 1 1 d . . . H17B H 0.6830 0.3733 -0.0623 0.070 Uiso 1 1 calc R . . C18B C 0.6158(5) 0.2938(5) -0.0128(3) 0.0555(19) Uani 1 1 d . . . H18B H 0.6419 0.2499 -0.0263 0.067 Uiso 1 1 calc R . . C19B C 0.5514(5) 0.2845(5) 0.0286(3) 0.0438(15) Uani 1 1 d . . . H19B H 0.5329 0.2335 0.0426 0.053 Uiso 1 1 calc R . . C20B C 0.4104(5) 0.4309(4) 0.1285(3) 0.0395(15) Uani 1 1 d . . . C21B C 0.3081(5) 0.4253(5) 0.1312(3) 0.0544(18) Uani 1 1 d . . . H21B H 0.2474 0.3681 0.1156 0.065 Uiso 1 1 calc R . . C22B C 0.2938(6) 0.5009(6) 0.1560(4) 0.062(2) Uani 1 1 d . . . H22B H 0.2236 0.4959 0.1575 0.075 Uiso 1 1 calc R . . C23B C 0.3797(7) 0.5831(6) 0.1785(4) 0.066(2) Uani 1 1 d . . . H23B H 0.3688 0.6350 0.1957 0.079 Uiso 1 1 calc R . . C24B C 0.4829(6) 0.5928(5) 0.1768(3) 0.0521(17) Uani 1 1 d . . . H24B H 0.5425 0.6506 0.1930 0.062 Uiso 1 1 calc R . . C25B C 0.4975(5) 0.5164(4) 0.1510(3) 0.0447(16) Uani 1 1 d . . . H25B H 0.5677 0.5224 0.1487 0.054 Uiso 1 1 calc R . . P1C P 0.67363(12) 0.37043(11) 0.20293(7) 0.0384(4) Uani 1 1 d . . . P2C P 0.64938(12) 0.28751(12) 0.30086(8) 0.0397(4) Uani 1 1 d . . . C1C C 0.7117(5) 0.3933(4) 0.2821(3) 0.0416(15) Uani 1 1 d . . . H1CA H 0.6879 0.4382 0.3029 0.050 Uiso 1 1 calc R . . H1CB H 0.7908 0.4192 0.2947 0.050 Uiso 1 1 calc R . . C2C C 0.7327(4) 0.4854(4) 0.1970(3) 0.0421(15) Uani 1 1 d . . . C3C C 0.7483(5) 0.5631(5) 0.2426(3) 0.0542(18) Uani 1 1 d . . . H3CA H 0.7367 0.5577 0.2799 0.065 Uiso 1 1 calc R . . C4C C 0.7809(6) 0.6483(5) 0.2331(4) 0.062(2) Uani 1 1 d . . . H4CA H 0.7907 0.6999 0.2640 0.075 Uiso 1 1 calc R . . C5C C 0.7988(5) 0.6574(5) 0.1796(4) 0.0561(19) Uani 1 1 d . . . H5CA H 0.8215 0.7151 0.1734 0.067 Uiso 1 1 calc R . . C6C C 0.7833(5) 0.5815(5) 0.1345(3) 0.0532(18) Uani 1 1 d . . . H6CA H 0.7944 0.5872 0.0972 0.064 Uiso 1 1 calc R . . C7C C 0.7520(4) 0.4981(5) 0.1435(3) 0.0433(16) Uani 1 1 d . . . H7CA H 0.7433 0.4474 0.1122 0.052 Uiso 1 1 calc R . . C8C C 0.7690(5) 0.3296(4) 0.1736(3) 0.0414(15) Uani 1 1 d . . . C9C C 0.8788(5) 0.3784(6) 0.1950(4) 0.062(2) Uani 1 1 d . . . H9CA H 0.9069 0.4335 0.2263 0.075 Uiso 1 1 calc R . . C10C C 0.9480(6) 0.3458(6) 0.1699(4) 0.073(2) Uani 1 1 d . . . H10C H 1.0233 0.3785 0.1850 0.088 Uiso 1 1 calc R . . C11C C 0.9085(6) 0.2680(6) 0.1243(4) 0.062(2) Uani 1 1 d . . . H11D H 0.9558 0.2480 0.1061 0.074 Uiso 1 1 calc R . . C12C C 0.8010(6) 0.2194(6) 0.1051(3) 0.059(2) Uani 1 1 d . . . H12D H 0.7731 0.1633 0.0747 0.071 Uiso 1 1 calc R . . C13C C 0.7301(5) 0.2507(5) 0.1295(3) 0.0481(17) Uani 1 1 d . . . H13D H 0.6549 0.2165 0.1150 0.058 Uiso 1 1 calc R . . C14C C 0.7511(5) 0.2446(5) 0.2970(3) 0.0463(16) Uani 1 1 d . . . C15C C 0.8535(6) 0.2923(6) 0.3362(3) 0.062(2) Uani 1 1 d . . . H15D H 0.8715 0.3493 0.3641 0.074 Uiso 1 1 calc R . . C16C C 0.9273(6) 0.2550(7) 0.3336(4) 0.076(3) Uani 1 1 d . . . H16C H 0.9951 0.2864 0.3603 0.091 Uiso 1 1 calc R . . C17C C 0.9027(6) 0.1726(6) 0.2923(4) 0.067(2) Uani 1 1 d . . . H17C H 0.9516 0.1460 0.2914 0.080 Uiso 1 1 calc R . . C18C C 0.8060(6) 0.1307(6) 0.2529(3) 0.060(2) Uani 1 1 d . . . H18C H 0.7893 0.0755 0.2233 0.073 Uiso 1 1 calc R . . C19C C 0.7324(5) 0.1667(5) 0.2551(3) 0.0500(17) Uani 1 1 d . . . H19C H 0.6667 0.1362 0.2266 0.060 Uiso 1 1 calc R . . C20C C 0.6648(5) 0.3309(5) 0.3804(3) 0.0463(16) Uani 1 1 d . . . C21C C 0.6403(6) 0.4033(5) 0.4043(3) 0.060(2) Uani 1 1 d . . . H21C H 0.6215 0.4334 0.3795 0.072 Uiso 1 1 calc R . . C22C C 0.6429(7) 0.4316(6) 0.4627(4) 0.070(2) Uani 1 1 d . . . H22C H 0.6281 0.4821 0.4780 0.084 Uiso 1 1 calc R . . C23C C 0.6668(7) 0.3875(6) 0.4997(4) 0.075(2) Uani 1 1 d . . . H23C H 0.6672 0.4068 0.5401 0.089 Uiso 1 1 calc R . . C24C C 0.6900(6) 0.3154(6) 0.4775(4) 0.069(2) Uani 1 1 d . . . H24C H 0.7057 0.2857 0.5036 0.083 Uiso 1 1 calc R . . C25C C 0.6919(4) 0.2834(4) 0.4187(2) 0.0553(18) Uani 1 1 d . . . H25C H 0.7095 0.2342 0.4045 0.066 Uiso 1 1 calc R . . C16 C 1.0768(4) 0.5222(4) 0.3732(2) 0.101(2) Uiso 0.50 1 d PR . . C17 C 1.0391(4) 0.5777(4) 0.3531(2) 0.101(2) Uiso 0.50 1 d PR . . H17D H 0.9908 0.5960 0.3715 0.121 Uiso 0.50 1 calc PR . . C18 C 1.0722(4) 0.6063(4) 0.3060(2) 0.101(2) Uiso 0.50 1 d PR . . H18D H 1.0464 0.6442 0.2923 0.121 Uiso 0.50 1 calc PR . . C19 C 1.1429(4) 0.5795(4) 0.2791(2) 0.101(2) Uiso 0.50 1 d PR . . H19D H 1.1655 0.5990 0.2469 0.121 Uiso 0.50 1 calc PR . . C20 C 1.1806(4) 0.5240(4) 0.2992(2) 0.101(2) Uiso 0.50 1 d PR . . H20A H 1.2289 0.5056 0.2808 0.121 Uiso 0.50 1 calc PR . . C21 C 1.1475(4) 0.4954(4) 0.3462(2) 0.101(2) Uiso 0.50 1 d PR . . H21D H 1.1732 0.4575 0.3600 0.121 Uiso 0.50 1 calc PR . . C22 C 1.0409(10) 0.5023(9) 0.4300(5) 0.101(2) Uiso 0.50 1 d P . . H22D H 1.0807 0.5568 0.4637 0.151 Uiso 0.50 1 calc PR . . H22E H 1.0559 0.4525 0.4362 0.151 Uiso 0.50 1 calc PR . . H22F H 0.9638 0.4852 0.4254 0.151 Uiso 0.50 1 calc PR . . C23 C 0.9784(10) 0.2509(9) 0.5235(5) 0.178(5) Uiso 0.50 1 d PR . . C28 C 1.0438(10) 0.2403(9) 0.5659(5) 0.178(5) Uiso 0.50 1 d PR . . H28A H 1.0176 0.1871 0.5777 0.214 Uiso 0.50 1 calc PR . . C27 C 1.1474(10) 0.3074(9) 0.5911(5) 0.178(5) Uiso 0.50 1 d PR . . H27A H 1.1921 0.3001 0.6201 0.214 Uiso 0.50 1 calc PR . . C26 C 1.1857(10) 0.3853(9) 0.5739(5) 0.178(5) Uiso 0.50 1 d PR . . H26A H 1.2566 0.4312 0.5911 0.214 Uiso 0.50 1 calc PR . . C25 C 1.1203(10) 0.3959(9) 0.5315(5) 0.178(5) Uiso 0.50 1 d PR . . H25D H 1.1465 0.4491 0.5197 0.214 Uiso 0.50 1 calc PR . . C24 C 1.0167(10) 0.3288(9) 0.5063(5) 0.178(5) Uiso 0.50 1 d PR . . H24D H 0.9720 0.3361 0.4773 0.214 Uiso 0.50 1 calc PR . . C29 C 0.8724(6) 0.1699(5) 0.4910(4) 0.178(5) Uiso 0.50 1 d P . . H29A H 0.8669 0.1175 0.5037 0.267 Uiso 0.50 1 calc PR . . H29B H 0.8691 0.1552 0.4488 0.267 Uiso 0.50 1 calc PR . . H29C H 0.8128 0.1847 0.4994 0.267 Uiso 0.50 1 calc PR . . C30 C 0.4599(6) -0.2134(5) 0.3656(4) 0.0838(19) Uiso 0.50 1 d PR . . C31 C 0.5138(6) -0.2118(5) 0.3202(4) 0.0838(19) Uiso 0.50 1 d PR . . H31A H 0.4779 -0.2198 0.2822 0.101 Uiso 0.50 1 calc PR . . C32 C 0.6202(6) -0.1984(5) 0.3303(4) 0.0838(19) Uiso 0.50 1 d PR . . H32A H 0.6570 -0.1973 0.2993 0.101 Uiso 0.50 1 calc PR . . C33 C 0.6727(6) -0.1867(5) 0.3859(4) 0.0838(19) Uiso 0.50 1 d PR . . H33A H 0.7454 -0.1775 0.3929 0.101 Uiso 0.50 1 calc PR . . C34 C 0.6188(6) -0.1883(5) 0.4314(4) 0.0838(19) Uiso 0.50 1 d PR . . H34A H 0.6547 -0.1803 0.4694 0.101 Uiso 0.50 1 calc PR . . C35 C 0.5124(6) -0.2017(5) 0.4213(4) 0.0838(19) Uiso 0.50 1 d PR . . H35A H 0.4756 -0.2028 0.4523 0.101 Uiso 0.50 1 calc PR . . C36 C 0.3564(14) -0.2158(13) 0.3828(9) 0.0838(19) Uiso 0.50 1 d P . . H36A H 0.3088 -0.2170 0.3494 0.126 Uiso 0.50 1 calc PR . . H36B H 0.3732 -0.1617 0.4157 0.126 Uiso 0.50 1 calc PR . . H36C H 0.3206 -0.2703 0.3944 0.126 Uiso 0.50 1 calc PR . . C37 C 1.0909(15) 0.4468(14) 0.0050(9) 0.084(5) Uiso 0.50 1 d P . . C38 C 1.0098(14) 0.4687(12) 0.0074(8) 0.073(5) Uiso 0.50 1 d P . . C39 C 0.9339(14) 0.4206(13) 0.0453(9) 0.081(5) Uiso 0.50 1 d P . . C40 C 1.0244(9) 0.3985(8) 0.0338(5) 0.108(3) Uiso 1 1 d . . . C41 C 0.9224(7) 0.4873(6) 0.0200(4) 0.077(2) 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 Ni1 0.0363(4) 0.0358(5) 0.0331(5) 0.0098(4) 0.0081(3) 0.0142(3) Ni2 0.0389(4) 0.0344(5) 0.0358(5) 0.0103(4) 0.0081(3) 0.0161(3) P1 0.0453(9) 0.0384(10) 0.0340(10) 0.0118(8) 0.0115(7) 0.0209(7) O1 0.052(3) 0.039(3) 0.041(3) 0.008(2) 0.011(2) 0.023(2) O2 0.044(2) 0.043(3) 0.036(3) 0.010(2) 0.0084(19) 0.017(2) C1 0.100(7) 0.088(8) 0.090(9) 0.009(6) 0.016(6) 0.042(6) C2 0.057(4) 0.061(5) 0.042(5) -0.005(4) 0.004(3) 0.027(4) C3 0.032(3) 0.035(4) 0.050(5) 0.002(3) 0.009(3) 0.010(3) C4 0.058(4) 0.042(4) 0.036(4) 0.013(3) 0.013(3) 0.026(3) C5 0.082(5) 0.043(4) 0.049(5) 0.008(4) 0.022(4) 0.029(4) C6 0.117(7) 0.066(6) 0.054(5) 0.016(5) 0.035(5) 0.055(5) C7 0.125(7) 0.057(6) 0.054(6) 0.004(4) 0.017(5) 0.056(6) C8 0.098(6) 0.035(4) 0.054(5) 0.009(4) 0.005(4) 0.024(4) C9 0.085(5) 0.050(5) 0.046(5) 0.017(4) 0.012(4) 0.036(4) C10 0.040(3) 0.048(4) 0.044(4) 0.026(3) 0.015(3) 0.025(3) C11 0.045(4) 0.057(5) 0.045(4) 0.025(4) 0.017(3) 0.024(3) C12 0.047(4) 0.061(5) 0.058(5) 0.030(4) 0.012(3) 0.014(4) C13 0.044(4) 0.087(7) 0.079(6) 0.042(5) 0.014(4) 0.027(4) C14 0.059(5) 0.078(7) 0.086(7) 0.035(5) 0.026(4) 0.037(5) C15 0.053(4) 0.060(5) 0.068(5) 0.021(4) 0.017(4) 0.034(4) P1A 0.0452(9) 0.0470(11) 0.0512(12) 0.0202(9) 0.0097(8) 0.0140(8) P2A 0.0419(9) 0.0395(10) 0.0408(10) 0.0152(8) 0.0091(7) 0.0186(7) C1A 0.052(4) 0.042(4) 0.040(4) 0.018(3) 0.010(3) 0.014(3) C2A 0.046(4) 0.050(4) 0.053(5) 0.019(4) 0.010(3) 0.020(3) C3A 0.048(4) 0.064(5) 0.069(6) 0.013(4) 0.010(4) 0.020(4) C4A 0.056(5) 0.067(6) 0.101(7) 0.012(5) 0.023(5) 0.033(4) C5A 0.075(6) 0.069(6) 0.087(7) 0.008(5) 0.010(5) 0.040(5) C6A 0.056(5) 0.052(5) 0.121(8) 0.017(5) 0.011(5) 0.025(4) C7A 0.046(4) 0.046(5) 0.097(7) 0.014(5) 0.015(4) 0.019(4) C8A 0.051(4) 0.045(4) 0.065(5) 0.022(4) 0.024(4) 0.021(3) C9A 0.042(4) 0.059(5) 0.063(5) 0.026(4) 0.012(3) 0.018(3) C10A 0.056(5) 0.064(6) 0.083(7) 0.023(5) 0.012(4) 0.024(4) C11A 0.060(5) 0.082(7) 0.114(9) 0.027(6) 0.014(6) 0.036(5) C12A 0.078(6) 0.134(10) 0.102(9) 0.048(7) 0.056(6) 0.057(6) C13A 0.062(5) 0.115(8) 0.075(6) 0.046(6) 0.031(4) 0.038(5) C14A 0.049(4) 0.034(4) 0.053(5) 0.014(3) -0.003(3) 0.011(3) C15A 0.051(4) 0.051(5) 0.079(6) 0.027(4) 0.010(4) 0.023(4) C16A 0.067(5) 0.073(6) 0.119(9) 0.055(6) 0.023(5) 0.041(5) C17A 0.075(6) 0.063(6) 0.117(9) 0.038(6) -0.003(6) 0.035(5) C18A 0.101(7) 0.062(6) 0.066(6) 0.036(5) -0.004(5) 0.026(5) C19A 0.076(5) 0.051(5) 0.060(5) 0.027(4) 0.010(4) 0.030(4) C20A 0.058(4) 0.055(5) 0.047(5) 0.023(4) 0.021(3) 0.032(4) C21A 0.047(4) 0.063(5) 0.057(5) 0.022(4) 0.014(3) 0.027(4) C22A 0.060(5) 0.088(7) 0.083(7) 0.033(6) 0.034(5) 0.043(5) C23A 0.105(7) 0.103(8) 0.054(6) 0.025(5) 0.038(5) 0.068(6) C24A 0.084(6) 0.075(6) 0.039(5) 0.013(4) 0.018(4) 0.039(5) C25A 0.070(5) 0.073(5) 0.034(4) 0.018(4) 0.014(4) 0.035(4) P1B 0.0410(9) 0.0466(11) 0.0380(10) 0.0163(8) 0.0062(7) 0.0143(8) P2B 0.0353(8) 0.0409(10) 0.0345(10) 0.0115(8) 0.0085(7) 0.0133(7) C1B 0.035(3) 0.051(4) 0.038(4) 0.015(3) 0.012(3) 0.010(3) C2B 0.035(3) 0.045(4) 0.032(4) 0.011(3) -0.001(3) 0.010(3) C3B 0.051(4) 0.060(5) 0.041(4) 0.019(4) 0.011(3) 0.021(3) C4B 0.048(4) 0.070(6) 0.057(5) 0.024(4) 0.018(3) 0.019(4) C5B 0.053(4) 0.062(6) 0.059(5) 0.008(4) 0.011(4) 0.024(4) C6B 0.066(5) 0.041(4) 0.056(5) 0.011(4) 0.008(4) 0.018(4) C7B 0.059(4) 0.053(5) 0.047(5) 0.020(4) 0.014(3) 0.021(4) C8B 0.040(3) 0.037(4) 0.043(4) 0.009(3) 0.007(3) 0.015(3) C9B 0.051(4) 0.054(5) 0.068(6) 0.016(4) 0.003(4) 0.023(4) C10B 0.063(5) 0.077(6) 0.064(6) 0.020(5) -0.002(4) 0.033(4) C11B 0.035(4) 0.083(6) 0.066(6) -0.003(5) 0.006(4) 0.016(4) C12B 0.045(4) 0.087(6) 0.061(6) 0.024(5) 0.010(4) 0.003(4) C13B 0.041(4) 0.078(6) 0.053(5) 0.031(4) 0.004(3) 0.013(4) C14B 0.036(3) 0.047(4) 0.037(4) 0.018(3) 0.012(3) 0.017(3) C15B 0.040(3) 0.054(4) 0.044(4) 0.014(3) 0.008(3) 0.021(3) C16B 0.039(3) 0.065(5) 0.050(4) 0.031(4) 0.018(3) 0.017(3) C17B 0.044(4) 0.083(6) 0.048(5) 0.026(4) 0.018(3) 0.022(4) C18B 0.059(4) 0.063(5) 0.049(5) 0.012(4) 0.019(4) 0.033(4) C19B 0.046(4) 0.047(4) 0.039(4) 0.013(3) 0.011(3) 0.020(3) C20B 0.042(3) 0.045(4) 0.037(4) 0.021(3) 0.014(3) 0.017(3) C21B 0.051(4) 0.061(5) 0.057(5) 0.020(4) 0.018(3) 0.027(4) C22B 0.059(5) 0.059(5) 0.074(6) 0.013(4) 0.023(4) 0.033(4) C23B 0.099(6) 0.069(6) 0.061(5) 0.028(5) 0.033(5) 0.059(5) C24B 0.061(4) 0.045(4) 0.052(5) 0.018(4) 0.010(3) 0.023(3) C25B 0.046(4) 0.043(4) 0.052(4) 0.019(3) 0.013(3) 0.023(3) P1C 0.0386(8) 0.0361(9) 0.0371(10) 0.0087(8) 0.0075(7) 0.0146(7) P2C 0.0412(9) 0.0378(10) 0.0382(10) 0.0105(8) 0.0059(7) 0.0166(7) C1C 0.043(3) 0.038(4) 0.039(4) 0.011(3) 0.005(3) 0.014(3) C2C 0.034(3) 0.037(4) 0.048(4) 0.011(3) 0.006(3) 0.010(3) C3C 0.060(4) 0.038(4) 0.052(5) 0.004(4) 0.010(3) 0.015(3) C4C 0.069(5) 0.041(5) 0.068(6) 0.012(4) 0.012(4) 0.018(4) C5C 0.050(4) 0.042(4) 0.072(6) 0.024(4) 0.015(4) 0.011(3) C6C 0.040(4) 0.054(5) 0.062(5) 0.020(4) 0.016(3) 0.014(3) C7C 0.032(3) 0.041(4) 0.050(4) 0.012(3) 0.010(3) 0.010(3) C8C 0.041(3) 0.040(4) 0.039(4) 0.010(3) 0.004(3) 0.015(3) C9C 0.044(4) 0.077(6) 0.068(6) 0.015(4) 0.011(4) 0.034(4) C10C 0.048(4) 0.088(7) 0.092(7) 0.027(6) 0.016(4) 0.037(4) C11C 0.058(5) 0.072(6) 0.067(6) 0.019(5) 0.018(4) 0.041(4) C12C 0.066(5) 0.070(5) 0.054(5) 0.013(4) 0.021(4) 0.043(4) C13C 0.053(4) 0.051(5) 0.042(4) 0.016(4) 0.012(3) 0.023(3) C14C 0.046(4) 0.043(4) 0.048(4) 0.015(3) 0.009(3) 0.016(3) C15C 0.056(4) 0.067(5) 0.057(5) 0.007(4) 0.004(4) 0.031(4) C16C 0.049(4) 0.105(7) 0.078(7) 0.021(6) 0.000(4) 0.045(5) C17C 0.073(5) 0.079(6) 0.063(6) 0.020(5) 0.023(4) 0.046(5) C18C 0.059(5) 0.072(6) 0.053(5) 0.009(4) 0.010(4) 0.037(4) C19C 0.047(4) 0.055(5) 0.044(4) 0.010(4) 0.007(3) 0.021(3) C20C 0.043(4) 0.053(4) 0.036(4) 0.007(3) 0.010(3) 0.017(3) C21C 0.080(5) 0.060(5) 0.053(5) 0.017(4) 0.016(4) 0.043(4) C22C 0.096(6) 0.076(6) 0.046(5) 0.006(4) 0.017(4) 0.052(5) C23C 0.093(6) 0.082(7) 0.044(5) 0.011(5) 0.016(4) 0.038(5) C24C 0.083(6) 0.082(6) 0.043(5) 0.016(4) 0.001(4) 0.040(5) C25C 0.062(4) 0.064(5) 0.043(5) 0.017(4) 0.004(3) 0.032(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 2.071(4) . ? Ni1 P1 2.1242(17) . ? Ni1 P2B 2.1766(18) . ? Ni1 P1C 2.2083(17) . ? Ni1 Ni2 2.5630(11) . ? Ni2 O1 2.056(4) . ? Ni2 P1 2.1279(17) . ? Ni2 P2A 2.1929(18) . ? Ni2 P2C 2.2046(18) . ? P1 C10 1.816(6) . ? P1 C4 1.827(7) . ? O1 C3 1.251(8) . ? O2 C3 1.265(8) . ? C1 C2 1.254(12) . ? C2 C3 1.488(9) . ? C4 C9 1.371(10) . ? C4 C5 1.388(9) . ? C5 C6 1.401(10) . ? C6 C7 1.364(12) . ? C7 C8 1.411(11) . ? C8 C9 1.393(10) . ? C10 C15 1.386(8) . ? C10 C11 1.413(9) . ? C11 C12 1.368(9) . ? C12 C13 1.398(11) . ? C13 C14 1.351(11) . ? C14 C15 1.396(10) . ? P1A C2A 1.833(7) . ? P1A C8A 1.838(7) . ? P1A C1A 1.872(6) . ? P2A C1A 1.820(7) . ? P2A C20A 1.829(7) . ? P2A C14A 1.837(7) . ? C2A C7A 1.371(10) . ? C2A C3A 1.415(9) . ? C3A C4A 1.390(11) . ? C4A C5A 1.375(11) . ? C5A C6A 1.385(11) . ? C6A C7A 1.368(11) . ? C8A C13A 1.366(10) . ? C8A C9A 1.401(10) . ? C9A C10A 1.391(10) . ? C10A C11A 1.341(13) . ? C11A C12A 1.396(14) . ? C12A C13A 1.434(11) . ? C14A C19A 1.388(10) . ? C14A C15A 1.394(10) . ? C15A C16A 1.379(10) . ? C16A C17A 1.359(13) . ? C17A C18A 1.374(13) . ? C18A C19A 1.388(10) . ? C20A C21A 1.388(9) . ? C20A C25A 1.429(10) . ? C21A C22A 1.374(10) . ? C22A C23A 1.378(12) . ? C23A C24A 1.396(11) . ? C24A C25A 1.358(10) . ? P1B C8B 1.829(6) . ? P1B C2B 1.837(7) . ? P1B C1B 1.868(6) . ? P2B C1B 1.823(6) . ? P2B C20B 1.824(7) . ? P2B C14B 1.831(6) . ? C2B C7B 1.378(9) . ? C2B C3B 1.395(9) . ? C3B C4B 1.418(10) . ? C4B C5B 1.348(10) . ? C5B C6B 1.391(10) . ? C6B C7B 1.385(10) . ? C8B C13B 1.376(9) . ? C8B C9B 1.384(9) . ? C9B C10B 1.361(10) . ? C10B C11B 1.379(11) . ? C11B C12B 1.392(12) . ? C12B C13B 1.401(9) . ? C14B C19B 1.391(9) . ? C14B C15B 1.406(9) . ? C15B C16B 1.403(9) . ? C16B C17B 1.389(10) . ? C17B C18B 1.388(10) . ? C18B C19B 1.405(9) . ? C20B C25B 1.397(9) . ? C20B C21B 1.397(8) . ? C21B C22B 1.369(10) . ? C22B C23B 1.356(11) . ? C23B C24B 1.382(10) . ? C24B C25B 1.389(9) . ? P1C C2C 1.830(6) . ? P1C C1C 1.834(7) . ? P1C C8C 1.845(6) . ? P2C C14C 1.823(7) . ? P2C C1C 1.840(6) . ? P2C C20C 1.840(7) . ? C2C C7C 1.396(9) . ? C2C C3C 1.416(9) . ? C3C C4C 1.408(10) . ? C4C C5C 1.375(10) . ? C5C C6C 1.389(10) . ? C6C C7C 1.376(9) . ? C8C C13C 1.352(9) . ? C8C C9C 1.384(9) . ? C9C C10C 1.402(10) . ? C10C C11C 1.358(11) . ? C11C C12C 1.352(10) . ? C12C C13C 1.404(9) . ? C14C C19C 1.361(9) . ? C14C C15C 1.422(9) . ? C15C C16C 1.397(10) . ? C16C C17C 1.387(11) . ? C17C C18C 1.370(10) . ? C18C C19C 1.378(9) . ? C20C C21C 1.400(9) . ? C20C C25C 1.470(9) . ? C21C C22C 1.367(10) . ? C22C C23C 1.383(12) . ? C23C C24C 1.377(11) . ? C24C C25C 1.398(10) . ? C16 C17 1.3899 . ? C16 C21 1.3901 . ? C16 C22 1.572(13) . ? C17 C18 1.3902 . ? C18 C19 1.3900 . ? C19 C20 1.3901 . ? C20 C21 1.3899 . ? C23 C28 1.3900 . ? C23 C24 1.3900 . ? C23 C29 1.522(15) . ? C28 C27 1.3900 . ? C27 C26 1.3901 . ? C26 C25 1.3901 . ? C25 C24 1.3899 . ? C30 C31 1.3899 . ? C30 C35 1.3902 . ? C30 C36 1.526(17) . ? C31 C32 1.3901 . ? C32 C33 1.3898 . ? C33 C34 1.3903 . ? C34 C35 1.3901 . ? C37 C38 1.32(2) . ? C37 C40 1.35(2) . ? C37 C41 1.44(2) 2_765 ? C38 C41 1.299(19) 2_765 ? C38 C38 1.30(3) 2_765 ? C38 C41 1.413(18) . ? C38 C40 1.539(19) . ? C38 C39 1.58(3) . ? C39 C41 1.45(2) . ? C39 C40 1.478(19) . ? C41 C38 1.299(19) 2_765 ? C41 C37 1.44(2) 2_765 ? 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 O2 Ni1 P1 113.05(13) . . ? O2 Ni1 P2B 94.67(13) . . ? P1 Ni1 P2B 104.16(7) . . ? O2 Ni1 P1C 112.60(12) . . ? P1 Ni1 P1C 119.14(7) . . ? P2B Ni1 P1C 109.91(7) . . ? O2 Ni1 Ni2 84.42(12) . . ? P1 Ni1 Ni2 53.00(5) . . ? P2B Ni1 Ni2 153.32(6) . . ? P1C Ni1 Ni2 94.85(5) . . ? O1 Ni2 P1 118.83(13) . . ? O1 Ni2 P2A 93.53(14) . . ? P1 Ni2 P2A 104.84(7) . . ? O1 Ni2 P2C 111.28(12) . . ? P1 Ni2 P2C 116.12(7) . . ? P2A Ni2 P2C 109.03(7) . . ? O1 Ni2 Ni1 86.24(13) . . ? P1 Ni2 Ni1 52.87(5) . . ? P2A Ni2 Ni1 152.52(6) . . ? P2C Ni2 Ni1 96.52(5) . . ? C10 P1 C4 103.8(3) . . ? C10 P1 Ni1 121.4(2) . . ? C4 P1 Ni1 119.3(2) . . ? C10 P1 Ni2 119.3(2) . . ? C4 P1 Ni2 118.0(2) . . ? Ni1 P1 Ni2 74.14(6) . . ? C3 O1 Ni2 120.8(4) . . ? C3 O2 Ni1 121.9(4) . . ? C1 C2 C3 125.7(9) . . ? O1 C3 O2 125.8(6) . . ? O1 C3 C2 115.9(7) . . ? O2 C3 C2 118.3(7) . . ? C9 C4 C5 118.1(7) . . ? C9 C4 P1 119.3(5) . . ? C5 C4 P1 122.3(5) . . ? C4 C5 C6 120.8(7) . . ? C7 C6 C5 120.7(8) . . ? C6 C7 C8 119.2(8) . . ? C9 C8 C7 119.0(8) . . ? C4 C9 C8 122.1(7) . . ? C15 C10 C11 117.5(6) . . ? C15 C10 P1 125.0(6) . . ? C11 C10 P1 117.5(4) . . ? C12 C11 C10 121.5(6) . . ? C11 C12 C13 119.7(8) . . ? C14 C13 C12 119.5(7) . . ? C13 C14 C15 121.5(7) . . ? C10 C15 C14 120.2(7) . . ? C2A P1A C8A 101.1(3) . . ? C2A P1A C1A 100.0(3) . . ? C8A P1A C1A 102.0(3) . . ? C1A P2A C20A 103.8(3) . . ? C1A P2A C14A 101.6(3) . . ? C20A P2A C14A 104.2(3) . . ? C1A P2A Ni2 110.4(2) . . ? C20A P2A Ni2 120.7(2) . . ? C14A P2A Ni2 114.1(2) . . ? P2A C1A P1A 118.3(4) . . ? C7A C2A C3A 116.7(7) . . ? C7A C2A P1A 124.0(6) . . ? C3A C2A P1A 119.0(5) . . ? C4A C3A C2A 119.9(7) . . ? C5A C4A C3A 121.2(7) . . ? C4A C5A C6A 119.1(8) . . ? C7A C6A C5A 119.4(8) . . ? C6A C7A C2A 123.6(7) . . ? C13A C8A C9A 119.0(7) . . ? C13A C8A P1A 117.2(6) . . ? C9A C8A P1A 123.7(5) . . ? C10A C9A C8A 121.4(7) . . ? C11A C10A C9A 120.1(9) . . ? C10A C11A C12A 120.5(8) . . ? C11A C12A C13A 119.7(9) . . ? C8A C13A C12A 119.3(8) . . ? C19A C14A C15A 118.5(6) . . ? C19A C14A P2A 125.5(6) . . ? C15A C14A P2A 116.0(6) . . ? C16A C15A C14A 121.9(8) . . ? C17A C16A C15A 119.7(9) . . ? C16A C17A C18A 118.9(8) . . ? C17A C18A C19A 122.9(9) . . ? C14A C19A C18A 118.1(8) . . ? C21A C20A C25A 118.3(6) . . ? C21A C20A P2A 122.4(6) . . ? C25A C20A P2A 119.0(5) . . ? C22A C21A C20A 119.9(8) . . ? C21A C22A C23A 122.0(7) . . ? C22A C23A C24A 118.6(7) . . ? C25A C24A C23A 120.7(8) . . ? C24A C25A C20A 120.5(7) . . ? C8B P1B C2B 102.6(3) . . ? C8B P1B C1B 102.4(3) . . ? C2B P1B C1B 100.3(3) . . ? C1B P2B C20B 103.6(3) . . ? C1B P2B C14B 101.8(3) . . ? C20B P2B C14B 105.8(3) . . ? C1B P2B Ni1 111.1(2) . . ? C20B P2B Ni1 118.5(2) . . ? C14B P2B Ni1 114.2(2) . . ? P2B C1B P1B 115.2(3) . . ? C7B C2B C3B 118.6(7) . . ? C7B C2B P1B 123.9(5) . . ? C3B C2B P1B 117.4(5) . . ? C2B C3B C4B 119.5(7) . . ? C5B C4B C3B 120.7(7) . . ? C4B C5B C6B 119.9(7) . . ? C7B C6B C5B 119.9(7) . . ? C2B C7B C6B 121.3(7) . . ? C13B C8B C9B 116.5(6) . . ? C13B C8B P1B 125.3(5) . . ? C9B C8B P1B 118.2(5) . . ? C10B C9B C8B 123.0(7) . . ? C9B C10B C11B 120.5(7) . . ? C10B C11B C12B 118.6(7) . . ? C11B C12B C13B 119.4(7) . . ? C8B C13B C12B 122.0(7) . . ? C19B C14B C15B 119.1(5) . . ? C19B C14B P2B 115.8(5) . . ? C15B C14B P2B 125.2(5) . . ? C16B C15B C14B 121.1(6) . . ? C17B C16B C15B 118.4(6) . . ? C18B C17B C16B 121.8(6) . . ? C17B C18B C19B 119.2(6) . . ? C14B C19B C18B 120.5(6) . . ? C25B C20B C21B 117.8(6) . . ? C25B C20B P2B 119.2(4) . . ? C21B C20B P2B 122.6(5) . . ? C22B C21B C20B 121.0(7) . . ? C23B C22B C21B 120.1(7) . . ? C22B C23B C24B 121.4(7) . . ? C23B C24B C25B 118.6(7) . . ? C24B C25B C20B 120.9(6) . . ? C2C P1C C1C 101.2(3) . . ? C2C P1C C8C 99.2(3) . . ? C1C P1C C8C 103.9(3) . . ? C2C P1C Ni1 119.6(2) . . ? C1C P1C Ni1 109.9(2) . . ? C8C P1C Ni1 120.3(2) . . ? C14C P2C C1C 102.5(3) . . ? C14C P2C C20C 101.6(3) . . ? C1C P2C C20C 101.7(3) . . ? C14C P2C Ni2 123.2(2) . . ? C1C P2C Ni2 110.5(2) . . ? C20C P2C Ni2 114.7(2) . . ? P1C C1C P2C 109.8(3) . . ? C7C C2C C3C 116.8(6) . . ? C7C C2C P1C 119.8(5) . . ? C3C C2C P1C 122.9(5) . . ? C4C C3C C2C 120.5(7) . . ? C5C C4C C3C 120.5(7) . . ? C4C C5C C6C 119.3(7) . . ? C7C C6C C5C 120.6(7) . . ? C6C C7C C2C 122.2(7) . . ? C13C C8C C9C 119.6(6) . . ? C13C C8C P1C 118.7(5) . . ? C9C C8C P1C 121.7(5) . . ? C8C C9C C10C 119.5(8) . . ? C11C C10C C9C 120.6(7) . . ? C12C C11C C10C 119.3(7) . . ? C11C C12C C13C 121.0(7) . . ? C8C C13C C12C 120.0(7) . . ? C19C C14C C15C 117.6(6) . . ? C19C C14C P2C 120.7(5) . . ? C15C C14C P2C 121.6(5) . . ? C16C C15C C14C 119.8(7) . . ? C17C C16C C15C 120.6(7) . . ? C18C C17C C16C 118.4(7) . . ? C17C C18C C19C 121.5(7) . . ? C14C C19C C18C 121.8(7) . . ? C21C C20C C25C 119.2(6) . . ? C21C C20C P2C 120.6(5) . . ? C25C C20C P2C 119.8(5) . . ? C22C C21C C20C 121.4(7) . . ? C21C C22C C23C 120.7(8) . . ? C24C C23C C22C 119.5(8) . . ? C23C C24C C25C 123.7(7) . . ? C24C C25C C20C 115.6(6) . . ? C17 C16 C21 120.0 . . ? C17 C16 C22 114.4(5) . . ? C21 C16 C22 125.4(5) . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C20 C21 C16 120.0 . . ? C28 C23 C24 120.0 . . ? C28 C23 C29 117.7(6) . . ? C24 C23 C29 121.7(6) . . ? C23 C28 C27 120.0 . . ? C28 C27 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C24 C23 120.0 . . ? C31 C30 C35 120.0 . . ? C31 C30 C36 143.8(8) . . ? C35 C30 C36 95.9(8) . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C30 120.0 . . ? C38 C37 C40 70.6(13) . . ? C38 C37 C41 55.9(11) . 2_765 ? C40 C37 C41 126.5(15) . 2_765 ? C41 C38 C38 65.7(15) 2_765 2_765 ? C41 C38 C37 67.0(13) 2_765 . ? C38 C38 C37 132(2) 2_765 . ? C41 C38 C41 122.7(13) 2_765 . ? C38 C38 C41 56.9(13) 2_765 . ? C37 C38 C41 168.9(18) . . ? C41 C38 C40 122.6(14) 2_765 . ? C38 C38 C40 170(2) 2_765 . ? C37 C38 C40 55.6(11) . . ? C41 C38 C40 114.4(14) . . ? C41 C38 C39 175.5(18) 2_765 . ? C38 C38 C39 115(2) 2_765 . ? C37 C38 C39 112.0(16) . . ? C41 C38 C39 57.8(10) . . ? C40 C38 C39 56.6(10) . . ? C41 C39 C40 115.7(14) . . ? C41 C39 C38 55.3(9) . . ? C40 C39 C38 60.4(10) . . ? C37 C40 C39 116.7(14) . . ? C37 C40 C38 53.8(11) . . ? C39 C40 C38 63.0(11) . . ? C38 C41 C38 57.3(13) 2_765 . ? C38 C41 C37 57.1(10) 2_765 2_765 ? C38 C41 C37 114.1(13) . 2_765 ? C38 C41 C39 123.9(13) 2_765 . ? C38 C41 C39 66.8(10) . . ? C37 C41 C39 179.0(13) 2_765 . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.281 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.110 #===== END data_FO2394 _database_code_depnum_ccdc_archive 'CCDC 600557' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H66 Ni P6' _chemical_formula_weight 1211.81 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' 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 11.0266(1) _cell_length_b 11.1318(2) _cell_length_c 27.3260(3) _cell_angle_alpha 92.840(1) _cell_angle_beta 98.429(1) _cell_angle_gamma 106.845(1) _cell_volume 3160.52(7) _cell_formula_units_Z 2 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 0.502 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23848 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.46 _reflns_number_total 14212 _reflns_number_gt 11438 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+3.0023P] 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 14212 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1098 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.77422(3) 0.44720(3) 0.255793(10) 0.01812(8) Uani 1 1 d . . . P1A P 0.63410(6) 0.30294(6) 0.41974(2) 0.02908(14) Uani 1 1 d . . . P2A P 0.64944(5) 0.39060(5) 0.31006(2) 0.01988(12) Uani 1 1 d . . . C1A C 0.7333(2) 0.3640(2) 0.37090(8) 0.0246(5) Uani 1 1 d . . . H1AA H 0.7976 0.4450 0.3851 0.030 Uiso 1 1 calc R . . H1AB H 0.7813 0.3040 0.3643 0.030 Uiso 1 1 calc R . . C2A C 0.7175(3) 0.4226(2) 0.47216(9) 0.0315(5) Uani 1 1 d . . . C3A C 0.6706(4) 0.5245(4) 0.47772(13) 0.0650(11) Uani 1 1 d . . . H3AA H 0.5988 0.5292 0.4549 0.078 Uiso 1 1 calc R . . C4A C 0.7270(5) 0.6199(4) 0.51621(14) 0.0766(13) Uani 1 1 d . . . H4AA H 0.6938 0.6892 0.5193 0.092 Uiso 1 1 calc R . . C5A C 0.8302(4) 0.6145(3) 0.54973(12) 0.0547(9) Uani 1 1 d . . . H5AA H 0.8700 0.6806 0.5756 0.066 Uiso 1 1 calc R . . C6A C 0.8749(4) 0.5129(4) 0.54546(13) 0.0613(9) Uani 1 1 d . . . H6AA H 0.9447 0.5070 0.5691 0.074 Uiso 1 1 calc R . . C7A C 0.8193(3) 0.4184(3) 0.50698(12) 0.0517(8) Uani 1 1 d . . . H7AA H 0.8525 0.3488 0.5046 0.062 Uiso 1 1 calc R . . C8A C 0.6867(3) 0.1651(2) 0.43538(9) 0.0361(6) Uani 1 1 d . . . C9A C 0.8082(4) 0.1539(3) 0.43387(11) 0.0497(8) Uani 1 1 d . . . H9AA H 0.8741 0.2240 0.4268 0.060 Uiso 1 1 calc R . . C10A C 0.8348(5) 0.0405(4) 0.44270(12) 0.0709(13) Uani 1 1 d . . . H10A H 0.9183 0.0340 0.4415 0.085 Uiso 1 1 calc R . . C11A C 0.7405(6) -0.0609(4) 0.45311(13) 0.0799(15) Uani 1 1 d . . . H11A H 0.7585 -0.1380 0.4588 0.096 Uiso 1 1 calc R . . C12A C 0.6212(6) -0.0514(3) 0.45536(14) 0.0756(14) Uani 1 1 d . . . H12A H 0.5563 -0.1216 0.4630 0.091 Uiso 1 1 calc R . . C13A C 0.5938(4) 0.0608(3) 0.44648(11) 0.0540(9) Uani 1 1 d . . . H13A H 0.5100 0.0661 0.4480 0.065 Uiso 1 1 calc R . . C14A C 0.5648(2) 0.5013(2) 0.32900(8) 0.0250(5) Uani 1 1 d . . . C15A C 0.6122(2) 0.6267(2) 0.31996(10) 0.0316(5) Uani 1 1 d . . . H15A H 0.6832 0.6514 0.3029 0.038 Uiso 1 1 calc R . . C16A C 0.5574(3) 0.7162(3) 0.33548(12) 0.0445(7) Uani 1 1 d . . . H16A H 0.5919 0.8018 0.3295 0.053 Uiso 1 1 calc R . . C17A C 0.4525(3) 0.6808(3) 0.35964(12) 0.0473(7) Uani 1 1 d . . . H17A H 0.4152 0.7423 0.3705 0.057 Uiso 1 1 calc R . . C18A C 0.4022(3) 0.5571(3) 0.36788(11) 0.0408(7) Uani 1 1 d . . . H18A H 0.3293 0.5330 0.3840 0.049 Uiso 1 1 calc R . . C19A C 0.4574(2) 0.4665(3) 0.35287(9) 0.0325(5) Uani 1 1 d . . . H19A H 0.4221 0.3811 0.3588 0.039 Uiso 1 1 calc R . . C20A C 0.5173(2) 0.2430(2) 0.29539(8) 0.0239(5) Uani 1 1 d . . . C21A C 0.4030(2) 0.2410(2) 0.26538(9) 0.0290(5) Uani 1 1 d . . . H21A H 0.3916 0.3178 0.2550 0.035 Uiso 1 1 calc R . . C22A C 0.3056(2) 0.1290(2) 0.25034(10) 0.0334(6) Uani 1 1 d . . . H22A H 0.2281 0.1297 0.2301 0.040 Uiso 1 1 calc R . . C23A C 0.3209(3) 0.0163(2) 0.26470(10) 0.0350(6) Uani 1 1 d . . . H23A H 0.2544 -0.0606 0.2542 0.042 Uiso 1 1 calc R . . C24A C 0.4337(3) 0.0161(2) 0.29455(10) 0.0336(6) Uani 1 1 d . . . H24A H 0.4444 -0.0611 0.3047 0.040 Uiso 1 1 calc R . . C25A C 0.5312(2) 0.1282(2) 0.30972(9) 0.0271(5) Uani 1 1 d . . . H25A H 0.6083 0.1270 0.3301 0.032 Uiso 1 1 calc R . . P1B P 0.69359(6) 0.54044(6) 0.07406(2) 0.02524(13) Uani 1 1 d . . . P2B P 0.66949(5) 0.46568(5) 0.18438(2) 0.01984(12) Uani 1 1 d . . . C1B C 0.7697(2) 0.5064(2) 0.13505(8) 0.0243(5) Uani 1 1 d . . . H1BA H 0.8049 0.4358 0.1288 0.029 Uiso 1 1 calc R . . H1BB H 0.8436 0.5812 0.1485 0.029 Uiso 1 1 calc R . . C2B C 0.6660(2) 0.3984(2) 0.03184(9) 0.0284(5) Uani 1 1 d . . . C3B C 0.6656(3) 0.2803(3) 0.04561(10) 0.0363(6) Uani 1 1 d . . . H3BA H 0.6910 0.2703 0.0795 0.044 Uiso 1 1 calc R . . C4B C 0.6285(3) 0.1759(3) 0.01037(12) 0.0473(7) Uani 1 1 d . . . H4BA H 0.6287 0.0954 0.0204 0.057 Uiso 1 1 calc R . . C5B C 0.5914(3) 0.1889(3) -0.03896(13) 0.0547(9) Uani 1 1 d . . . H5BA H 0.5657 0.1177 -0.0630 0.066 Uiso 1 1 calc R . . C6B C 0.5918(4) 0.3059(4) -0.05321(12) 0.0616(10) Uani 1 1 d . . . H6BA H 0.5673 0.3157 -0.0872 0.074 Uiso 1 1 calc R . . C7B C 0.6276(3) 0.4084(3) -0.01844(10) 0.0470(7) Uani 1 1 d . . . H7BA H 0.6263 0.4883 -0.0288 0.056 Uiso 1 1 calc R . . C8B C 0.8356(2) 0.6462(2) 0.05390(8) 0.0296(5) Uani 1 1 d . . . C9B C 0.8387(3) 0.7706(3) 0.04948(10) 0.0380(6) Uani 1 1 d . . . H9BA H 0.7680 0.7976 0.0562 0.046 Uiso 1 1 calc R . . C10B C 0.9440(3) 0.8562(3) 0.03541(11) 0.0505(8) Uani 1 1 d . . . H10B H 0.9453 0.9413 0.0328 0.061 Uiso 1 1 calc R . . C11B C 1.0460(3) 0.8180(3) 0.02531(11) 0.0503(8) Uani 1 1 d . . . H11B H 1.1176 0.8767 0.0155 0.060 Uiso 1 1 calc R . . C12B C 1.0453(3) 0.6940(3) 0.02935(11) 0.0482(8) Uani 1 1 d . . . H12B H 1.1161 0.6676 0.0223 0.058 Uiso 1 1 calc R . . C13B C 0.9403(3) 0.6088(3) 0.04373(10) 0.0397(6) Uani 1 1 d . . . H13B H 0.9397 0.5240 0.0467 0.048 Uiso 1 1 calc R . . C14B C 0.5380(2) 0.3307(2) 0.15129(8) 0.0248(5) Uani 1 1 d . . . C15B C 0.4513(2) 0.3423(3) 0.11080(9) 0.0295(5) Uani 1 1 d . . . H15B H 0.4521 0.4239 0.1018 0.035 Uiso 1 1 calc R . . C16B C 0.3630(3) 0.2363(3) 0.08316(10) 0.0394(6) Uani 1 1 d . . . H16B H 0.3056 0.2455 0.0551 0.047 Uiso 1 1 calc R . . C17B C 0.3595(3) 0.1174(3) 0.09685(11) 0.0442(7) Uani 1 1 d . . . H17B H 0.2997 0.0447 0.0781 0.053 Uiso 1 1 calc R . . C18B C 0.4425(3) 0.1045(3) 0.13755(11) 0.0427(7) Uani 1 1 d . . . H18B H 0.4387 0.0228 0.1472 0.051 Uiso 1 1 calc R . . C19B C 0.5320(2) 0.2104(2) 0.16479(9) 0.0301(5) Uani 1 1 d . . . H19B H 0.5893 0.2004 0.1927 0.036 Uiso 1 1 calc R . . C20B C 0.5919(2) 0.5914(2) 0.18464(8) 0.0246(5) Uani 1 1 d . . . C21B C 0.4707(3) 0.5688(3) 0.19722(10) 0.0358(6) Uani 1 1 d . . . H21B H 0.4227 0.4851 0.2013 0.043 Uiso 1 1 calc R . . C22B C 0.4181(3) 0.6663(3) 0.20392(11) 0.0481(8) Uani 1 1 d . . . H22B H 0.3349 0.6487 0.2127 0.058 Uiso 1 1 calc R . . C23B C 0.4851(3) 0.7876(3) 0.19805(11) 0.0498(8) Uani 1 1 d . . . H23B H 0.4486 0.8540 0.2027 0.060 Uiso 1 1 calc R . . C24B C 0.6062(3) 0.8130(3) 0.18525(11) 0.0469(7) Uani 1 1 d . . . H24B H 0.6533 0.8970 0.1812 0.056 Uiso 1 1 calc R . . C25B C 0.6592(3) 0.7151(2) 0.17830(10) 0.0353(6) Uani 1 1 d . . . H25B H 0.7420 0.7328 0.1692 0.042 Uiso 1 1 calc R . . P1C P 0.95055(5) 0.60526(5) 0.27859(2) 0.02021(12) Uani 1 1 d . . . P2C P 0.92470(5) 0.35695(5) 0.25340(2) 0.02085(12) Uani 1 1 d . . . C8C C 1.0213(2) 0.7078(2) 0.33714(8) 0.0241(5) Uani 1 1 d . . . C1C C 1.0541(2) 0.4999(2) 0.28235(9) 0.0266(5) Uani 1 1 d . . . H1CA H 1.1242 0.5253 0.2625 0.032 Uiso 1 1 calc R . . H1CB H 1.0898 0.4917 0.3170 0.032 Uiso 1 1 calc R . . C2C C 1.0090(2) 0.7178(2) 0.23428(8) 0.0257(5) Uani 1 1 d . . . C9C C 0.9512(3) 0.7037(2) 0.37579(9) 0.0297(5) Uani 1 1 d . . . H9CA H 0.8638 0.6534 0.3711 0.036 Uiso 1 1 calc R . . C7C C 0.9731(2) 0.8282(2) 0.23443(10) 0.0329(6) Uani 1 1 d . . . H7CA H 0.9265 0.8460 0.2590 0.039 Uiso 1 1 calc R . . C3C C 1.0771(3) 0.6944(3) 0.19755(9) 0.0367(6) Uani 1 1 d . . . H3CA H 1.1022 0.6197 0.1964 0.044 Uiso 1 1 calc R . . C6C C 1.0045(3) 0.9121(3) 0.19925(11) 0.0458(8) Uani 1 1 d . . . H6CA H 0.9787 0.9864 0.1998 0.055 Uiso 1 1 calc R . . C5C C 1.0726(3) 0.8888(3) 0.16356(11) 0.0534(9) Uani 1 1 d . . . H5CA H 1.0949 0.9472 0.1398 0.064 Uiso 1 1 calc R . . C4C C 1.1084(3) 0.7802(3) 0.16257(10) 0.0510(9) Uani 1 1 d . . . H4CA H 1.1549 0.7636 0.1377 0.061 Uiso 1 1 calc R . . C14C C 0.9765(2) 0.3070(2) 0.19671(9) 0.0260(5) Uani 1 1 d . . . C13C C 1.1494(2) 0.7838(2) 0.34482(10) 0.0321(5) Uani 1 1 d . . . H13C H 1.1982 0.7876 0.3187 0.038 Uiso 1 1 calc R . . C20C C 0.9543(2) 0.2308(2) 0.28983(9) 0.0274(5) Uani 1 1 d . . . C19C C 0.8858(3) 0.2228(3) 0.16132(10) 0.0407(6) Uani 1 1 d . . . H19C H 0.7988 0.1956 0.1661 0.049 Uiso 1 1 calc R . . C10C C 1.0095(3) 0.7735(3) 0.42159(9) 0.0390(6) Uani 1 1 d . . . H10C H 0.9618 0.7699 0.4480 0.047 Uiso 1 1 calc R . . C21C C 0.8510(3) 0.1270(3) 0.29241(11) 0.0390(6) Uani 1 1 d . . . H21C H 0.7675 0.1237 0.2763 0.047 Uiso 1 1 calc R . . C24C C 1.0935(4) 0.1337(3) 0.33900(11) 0.0483(8) Uani 1 1 d . . . H24C H 1.1769 0.1359 0.3548 0.058 Uiso 1 1 calc R . . C12C C 1.2057(3) 0.8535(3) 0.39008(10) 0.0407(6) Uani 1 1 d . . . H12C H 1.2924 0.9056 0.3948 0.049 Uiso 1 1 calc R . . C11C C 1.1358(3) 0.8473(3) 0.42837(10) 0.0426(7) Uani 1 1 d . . . H11C H 1.1750 0.8942 0.4595 0.051 Uiso 1 1 calc R . . C25C C 1.0766(3) 0.2339(3) 0.31325(10) 0.0385(6) Uani 1 1 d . . . H25C H 1.1485 0.3046 0.3116 0.046 Uiso 1 1 calc R . . C23C C 0.9896(4) 0.0315(3) 0.34155(11) 0.0522(9) Uani 1 1 d . . . H23C H 1.0014 -0.0365 0.3594 0.063 Uiso 1 1 calc R . . C15C C 1.1023(3) 0.3433(4) 0.18908(13) 0.0578(10) Uani 1 1 d . . . H15C H 1.1669 0.4000 0.2133 0.069 Uiso 1 1 calc R . . C22C C 0.8685(4) 0.0271(3) 0.31843(13) 0.0543(9) Uani 1 1 d . . . H22C H 0.7970 -0.0439 0.3202 0.065 Uiso 1 1 calc R . . C18C C 0.9195(3) 0.1771(4) 0.11863(11) 0.0545(9) Uani 1 1 d . . . H18C H 0.8558 0.1190 0.0946 0.065 Uiso 1 1 calc R . . C17C C 1.0440(4) 0.2156(4) 0.11125(12) 0.0590(9) Uani 1 1 d . . . H17C H 1.0673 0.1856 0.0819 0.071 Uiso 1 1 calc R . . C16C C 1.1354(4) 0.2980(4) 0.14657(16) 0.0810(14) Uani 1 1 d . . . H16C H 1.2224 0.3243 0.1417 0.097 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01715(14) 0.01861(14) 0.01898(14) 0.00230(10) 0.00292(10) 0.00596(10) P1A 0.0302(3) 0.0320(3) 0.0246(3) 0.0061(2) 0.0070(2) 0.0070(3) P2A 0.0189(3) 0.0206(3) 0.0205(3) 0.0030(2) 0.0038(2) 0.0062(2) C1A 0.0242(11) 0.0275(12) 0.0212(11) 0.0064(9) 0.0025(9) 0.0062(9) C2A 0.0377(14) 0.0324(13) 0.0260(12) 0.0045(10) 0.0091(10) 0.0107(11) C3A 0.098(3) 0.060(2) 0.0452(18) -0.0075(16) -0.0111(18) 0.049(2) C4A 0.131(4) 0.052(2) 0.056(2) -0.0109(17) 0.002(2) 0.051(3) C5A 0.071(2) 0.0444(18) 0.0388(16) -0.0085(13) 0.0147(16) 0.0024(16) C6A 0.054(2) 0.069(2) 0.052(2) -0.0196(17) -0.0112(16) 0.0196(18) C7A 0.056(2) 0.053(2) 0.0460(17) -0.0111(14) -0.0076(14) 0.0279(16) C8A 0.0558(17) 0.0272(13) 0.0227(12) 0.0036(10) 0.0057(11) 0.0087(12) C9A 0.076(2) 0.0512(19) 0.0390(16) 0.0190(14) 0.0231(15) 0.0367(17) C10A 0.135(4) 0.075(3) 0.0385(17) 0.0209(17) 0.035(2) 0.074(3) C11A 0.170(5) 0.043(2) 0.0384(19) 0.0055(15) 0.018(2) 0.050(3) C12A 0.129(4) 0.0262(17) 0.052(2) 0.0069(14) 0.000(2) -0.001(2) C13A 0.075(2) 0.0319(16) 0.0394(16) 0.0067(12) 0.0002(15) -0.0046(15) C14A 0.0222(11) 0.0303(12) 0.0236(11) 0.0006(9) 0.0026(9) 0.0107(9) C15A 0.0264(12) 0.0291(13) 0.0399(14) 0.0016(10) 0.0052(10) 0.0096(10) C16A 0.0374(15) 0.0300(15) 0.067(2) -0.0038(13) 0.0066(14) 0.0146(12) C17A 0.0384(16) 0.0487(18) 0.0601(19) -0.0133(15) 0.0044(14) 0.0260(14) C18A 0.0313(14) 0.0564(19) 0.0409(15) 0.0008(13) 0.0112(12) 0.0211(13) C19A 0.0271(12) 0.0391(15) 0.0340(13) 0.0063(11) 0.0090(10) 0.0118(11) C20A 0.0225(11) 0.0249(12) 0.0231(11) 0.0015(9) 0.0064(9) 0.0042(9) C21A 0.0262(12) 0.0260(12) 0.0332(13) 0.0064(10) 0.0041(10) 0.0052(10) C22A 0.0252(12) 0.0323(14) 0.0368(14) 0.0035(11) -0.0010(10) 0.0027(10) C23A 0.0300(13) 0.0269(13) 0.0404(14) 0.0003(11) 0.0039(11) -0.0016(10) C24A 0.0373(14) 0.0235(12) 0.0387(14) 0.0041(10) 0.0051(11) 0.0076(10) C25A 0.0247(12) 0.0258(12) 0.0307(12) 0.0030(9) 0.0040(9) 0.0080(9) P1B 0.0261(3) 0.0292(3) 0.0210(3) 0.0034(2) 0.0032(2) 0.0093(2) P2B 0.0182(3) 0.0219(3) 0.0194(3) 0.0019(2) 0.0022(2) 0.0064(2) C1B 0.0219(11) 0.0297(12) 0.0220(11) 0.0044(9) 0.0034(9) 0.0087(9) C2B 0.0223(11) 0.0353(14) 0.0270(12) -0.0002(10) 0.0019(9) 0.0093(10) C3B 0.0423(15) 0.0354(15) 0.0338(14) 0.0034(11) 0.0123(11) 0.0127(12) C4B 0.0475(17) 0.0343(16) 0.060(2) -0.0048(13) 0.0179(15) 0.0100(13) C5B 0.0453(18) 0.055(2) 0.057(2) -0.0250(16) -0.0054(15) 0.0161(15) C6B 0.076(2) 0.070(2) 0.0359(16) -0.0161(15) -0.0198(16) 0.035(2) C7B 0.0595(19) 0.0489(18) 0.0310(14) -0.0037(12) -0.0103(13) 0.0240(15) C8B 0.0367(13) 0.0312(13) 0.0186(11) 0.0031(9) 0.0045(9) 0.0068(10) C9B 0.0482(16) 0.0365(15) 0.0293(13) 0.0080(11) 0.0065(12) 0.0121(12) C10B 0.071(2) 0.0342(16) 0.0370(16) 0.0092(12) 0.0086(15) 0.0000(15) C11B 0.0534(19) 0.0509(19) 0.0324(15) 0.0041(13) 0.0126(13) -0.0088(15) C12B 0.0393(16) 0.057(2) 0.0415(16) -0.0031(14) 0.0148(13) 0.0017(14) C13B 0.0381(15) 0.0387(15) 0.0405(15) 0.0006(12) 0.0123(12) 0.0066(12) C14B 0.0206(11) 0.0295(12) 0.0227(11) -0.0001(9) 0.0049(9) 0.0049(9) C15B 0.0231(12) 0.0364(14) 0.0278(12) 0.0004(10) 0.0041(9) 0.0078(10) C16B 0.0260(13) 0.0536(18) 0.0321(14) -0.0094(12) -0.0002(10) 0.0068(12) C17B 0.0343(15) 0.0404(16) 0.0465(16) -0.0176(13) 0.0046(12) -0.0018(12) C18B 0.0463(17) 0.0281(14) 0.0490(17) -0.0041(12) 0.0130(13) 0.0026(12) C19B 0.0306(13) 0.0278(13) 0.0313(12) 0.0001(10) 0.0077(10) 0.0069(10) C20B 0.0279(12) 0.0277(12) 0.0189(10) 0.0005(9) -0.0012(9) 0.0121(10) C21B 0.0368(14) 0.0412(15) 0.0374(14) 0.0111(11) 0.0109(11) 0.0209(12) C22B 0.0525(18) 0.062(2) 0.0475(17) 0.0152(15) 0.0177(14) 0.0394(16) C23B 0.071(2) 0.055(2) 0.0387(16) 0.0008(14) 0.0046(15) 0.0457(18) C24B 0.064(2) 0.0268(14) 0.0476(17) -0.0021(12) -0.0052(15) 0.0187(14) C25B 0.0354(14) 0.0285(13) 0.0383(14) -0.0016(11) -0.0028(11) 0.0092(11) P1C 0.0187(3) 0.0187(3) 0.0223(3) 0.0005(2) 0.0020(2) 0.0051(2) P2C 0.0209(3) 0.0200(3) 0.0231(3) 0.0012(2) 0.0033(2) 0.0088(2) C8C 0.0288(12) 0.0196(11) 0.0236(11) 0.0004(8) -0.0008(9) 0.0095(9) C1C 0.0231(11) 0.0263(12) 0.0299(12) -0.0010(9) -0.0011(9) 0.0102(9) C2C 0.0215(11) 0.0257(12) 0.0229(11) 0.0003(9) -0.0007(9) -0.0012(9) C9C 0.0387(14) 0.0235(12) 0.0278(12) 0.0048(9) 0.0047(10) 0.0107(10) C7C 0.0265(12) 0.0297(13) 0.0364(13) 0.0079(10) -0.0038(10) 0.0027(10) C3C 0.0321(13) 0.0395(15) 0.0300(13) -0.0030(11) 0.0073(11) -0.0025(11) C6C 0.0383(15) 0.0349(15) 0.0507(18) 0.0170(13) -0.0128(13) -0.0020(12) C5C 0.0494(18) 0.054(2) 0.0335(15) 0.0189(14) -0.0085(13) -0.0150(15) C4C 0.0426(17) 0.064(2) 0.0265(14) 0.0011(13) 0.0062(12) -0.0150(15) C14C 0.0281(12) 0.0289(12) 0.0256(11) 0.0023(9) 0.0053(9) 0.0153(10) C13C 0.0288(13) 0.0314(13) 0.0326(13) -0.0030(10) -0.0008(10) 0.0077(10) C20C 0.0379(13) 0.0252(12) 0.0252(11) 0.0038(9) 0.0077(10) 0.0177(10) C19C 0.0343(14) 0.0516(18) 0.0363(14) -0.0102(12) 0.0031(11) 0.0169(13) C10C 0.0583(18) 0.0402(16) 0.0231(12) 0.0029(11) 0.0063(12) 0.0223(14) C21C 0.0448(16) 0.0323(14) 0.0478(16) 0.0103(12) 0.0205(13) 0.0166(12) C24C 0.071(2) 0.0477(18) 0.0375(15) 0.0039(13) -0.0015(14) 0.0408(17) C12C 0.0338(14) 0.0400(16) 0.0401(15) -0.0084(12) -0.0107(12) 0.0086(12) C11C 0.0557(18) 0.0391(16) 0.0283(13) -0.0077(11) -0.0106(12) 0.0176(14) C25C 0.0462(16) 0.0330(14) 0.0388(14) 0.0023(11) -0.0030(12) 0.0213(12) C23C 0.092(3) 0.0466(18) 0.0414(16) 0.0192(14) 0.0270(17) 0.0476(19) C15C 0.0344(16) 0.069(2) 0.061(2) -0.0268(17) 0.0186(15) 0.0018(15) C22C 0.075(2) 0.0375(17) 0.066(2) 0.0216(15) 0.0387(19) 0.0253(16) C18C 0.0516(19) 0.079(2) 0.0361(15) -0.0215(15) -0.0062(14) 0.0348(18) C17C 0.062(2) 0.083(3) 0.0406(17) -0.0102(16) 0.0200(16) 0.0325(19) C16C 0.048(2) 0.104(3) 0.081(3) -0.038(2) 0.035(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni P2A 2.1627(6) . ? Ni P2B 2.1681(6) . ? Ni P2C 2.1814(6) . ? Ni P1C 2.1950(6) . ? P1A C8A 1.839(3) . ? P1A C2A 1.840(3) . ? P1A C1A 1.878(2) . ? P2A C20A 1.833(2) . ? P2A C14A 1.845(2) . ? P2A C1A 1.861(2) . ? C2A C7A 1.375(4) . ? C2A C3A 1.387(4) . ? C3A C4A 1.392(5) . ? C4A C5A 1.370(6) . ? C5A C6A 1.365(5) . ? C6A C7A 1.384(4) . ? C8A C13A 1.387(4) . ? C8A C9A 1.388(4) . ? C9A C10A 1.401(4) . ? C10A C11A 1.369(7) . ? C11A C12A 1.360(7) . ? C12A C13A 1.393(5) . ? C14A C15A 1.389(4) . ? C14A C19A 1.401(3) . ? C15A C16A 1.385(4) . ? C16A C17A 1.384(4) . ? C17A C18A 1.371(5) . ? C18A C19A 1.394(4) . ? C20A C25A 1.398(3) . ? C20A C21A 1.393(3) . ? C21A C22A 1.386(3) . ? C22A C23A 1.381(4) . ? C23A C24A 1.385(4) . ? C24A C25A 1.387(4) . ? P1B C2B 1.834(3) . ? P1B C8B 1.841(3) . ? P1B C1B 1.861(2) . ? P2B C20B 1.840(2) . ? P2B C14B 1.843(2) . ? P2B C1B 1.858(2) . ? C2B C3B 1.384(4) . ? C2B C7B 1.397(4) . ? C3B C4B 1.395(4) . ? C4B C5B 1.377(5) . ? C5B C6B 1.377(5) . ? C6B C7B 1.372(4) . ? C8B C9B 1.388(4) . ? C8B C13B 1.394(4) . ? C9B C10B 1.389(4) . ? C10B C11B 1.371(5) . ? C11B C12B 1.388(5) . ? C12B C13B 1.389(4) . ? C14B C15B 1.390(3) . ? C14B C19B 1.393(3) . ? C15B C16B 1.393(4) . ? C16B C17B 1.385(4) . ? C17B C18B 1.374(4) . ? C18B C19B 1.393(4) . ? C20B C21B 1.384(4) . ? C20B C25B 1.395(4) . ? C21B C22B 1.386(4) . ? C22B C23B 1.369(5) . ? C23B C24B 1.384(5) . ? C24B C25B 1.395(4) . ? P1C C2C 1.834(2) . ? P1C C8C 1.846(2) . ? P1C C1C 1.856(2) . ? P2C C20C 1.838(2) . ? P2C C14C 1.842(2) . ? P2C C1C 1.850(2) . ? C8C C9C 1.392(3) . ? C8C C13C 1.398(3) . ? C2C C3C 1.395(4) . ? C2C C7C 1.396(4) . ? C9C C10C 1.401(4) . ? C7C C6C 1.384(4) . ? C3C C4C 1.393(4) . ? C6C C5C 1.373(5) . ? C5C C4C 1.376(5) . ? C14C C19C 1.377(4) . ? C14C C15C 1.378(4) . ? C13C C12C 1.385(4) . ? C20C C21C 1.380(4) . ? C20C C25C 1.396(4) . ? C19C C18C 1.392(4) . ? C10C C11C 1.376(4) . ? C21C C22C 1.394(4) . ? C24C C23C 1.374(5) . ? C24C C25C 1.390(4) . ? C12C C11C 1.381(4) . ? C23C C22C 1.377(5) . ? C15C C16C 1.382(4) . ? C18C C17C 1.363(5) . ? C17C C16C 1.371(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 P2A Ni P2B 112.34(2) . . ? P2A Ni P2C 117.07(2) . . ? P2B Ni P2C 115.86(2) . . ? P2A Ni P1C 117.75(2) . . ? P2B Ni P1C 112.23(2) . . ? P2C Ni P1C 77.43(2) . . ? C8A P1A C2A 103.88(12) . . ? C8A P1A C1A 101.34(12) . . ? C2A P1A C1A 100.23(11) . . ? C20A P2A C14A 101.49(11) . . ? C20A P2A C1A 101.39(10) . . ? C14A P2A C1A 102.01(11) . . ? C20A P2A Ni 118.13(7) . . ? C14A P2A Ni 117.28(8) . . ? C1A P2A Ni 114.02(8) . . ? P2A C1A P1A 118.33(12) . . ? C7A C2A C3A 117.2(3) . . ? C7A C2A P1A 126.1(2) . . ? C3A C2A P1A 116.7(2) . . ? C2A C3A C4A 121.1(3) . . ? C5A C4A C3A 120.4(3) . . ? C6A C5A C4A 119.0(3) . . ? C5A C6A C7A 120.6(3) . . ? C2A C7A C6A 121.7(3) . . ? C13A C8A C9A 117.7(3) . . ? C13A C8A P1A 116.6(3) . . ? C9A C8A P1A 125.6(2) . . ? C8A C9A C10A 120.8(4) . . ? C11A C10A C9A 120.1(4) . . ? C12A C11A C10A 120.1(4) . . ? C11A C12A C13A 120.2(4) . . ? C8A C13A C12A 121.2(4) . . ? C15A C14A C19A 118.4(2) . . ? C15A C14A P2A 117.94(18) . . ? C19A C14A P2A 123.66(19) . . ? C16A C15A C14A 121.0(3) . . ? C15A C16A C17A 120.0(3) . . ? C18A C17A C16A 120.0(3) . . ? C17A C18A C19A 120.5(3) . . ? C18A C19A C14A 120.1(3) . . ? C25A C20A C21A 117.9(2) . . ? C25A C20A P2A 121.83(18) . . ? C21A C20A P2A 120.00(18) . . ? C22A C21A C20A 121.2(2) . . ? C23A C22A C21A 120.2(2) . . ? C22A C23A C24A 119.6(2) . . ? C23A C24A C25A 120.3(2) . . ? C24A C25A C20A 120.8(2) . . ? C2B P1B C8B 100.51(11) . . ? C2B P1B C1B 105.33(11) . . ? C8B P1B C1B 99.85(11) . . ? C20B P2B C14B 101.96(11) . . ? C20B P2B C1B 102.40(11) . . ? C14B P2B C1B 100.31(10) . . ? C20B P2B Ni 114.80(7) . . ? C14B P2B Ni 120.19(8) . . ? C1B P2B Ni 114.63(7) . . ? P2B C1B P1B 118.43(12) . . ? C3B C2B C7B 117.5(2) . . ? C3B C2B P1B 126.18(19) . . ? C7B C2B P1B 115.9(2) . . ? C2B C3B C4B 120.9(3) . . ? C5B C4B C3B 120.2(3) . . ? C6B C5B C4B 119.5(3) . . ? C7B C6B C5B 120.2(3) . . ? C6B C7B C2B 121.7(3) . . ? C9B C8B C13B 118.6(2) . . ? C9B C8B P1B 117.6(2) . . ? C13B C8B P1B 123.8(2) . . ? C8B C9B C10B 120.7(3) . . ? C11B C10B C9B 120.1(3) . . ? C10B C11B C12B 120.4(3) . . ? C11B C12B C13B 119.4(3) . . ? C12B C13B C8B 120.9(3) . . ? C15B C14B C19B 118.4(2) . . ? C15B C14B P2B 122.94(19) . . ? C19B C14B P2B 118.40(18) . . ? C14B C15B C16B 121.1(3) . . ? C15B C16B C17B 119.6(3) . . ? C18B C17B C16B 120.0(3) . . ? C17B C18B C19B 120.5(3) . . ? C18B C19B C14B 120.4(3) . . ? C21B C20B C25B 118.0(2) . . ? C21B C20B P2B 120.55(19) . . ? C25B C20B P2B 120.94(19) . . ? C20B C21B C22B 121.1(3) . . ? C23B C22B C21B 120.6(3) . . ? C22B C23B C24B 119.6(3) . . ? C23B C24B C25B 120.0(3) . . ? C20B C25B C24B 120.7(3) . . ? C2C P1C C8C 99.24(10) . . ? C2C P1C C1C 105.97(11) . . ? C8C P1C C1C 99.89(10) . . ? C2C P1C Ni 120.16(7) . . ? C8C P1C Ni 133.31(8) . . ? C1C P1C Ni 92.72(8) . . ? C20C P2C C14C 96.44(10) . . ? C20C P2C C1C 103.97(11) . . ? C14C P2C C1C 105.77(11) . . ? C20C P2C Ni 127.90(8) . . ? C14C P2C Ni 125.70(8) . . ? C1C P2C Ni 93.33(7) . . ? C9C C8C C13C 118.8(2) . . ? C9C C8C P1C 120.48(18) . . ? C13C C8C P1C 120.50(18) . . ? P2C C1C P1C 95.22(11) . . ? C3C C2C C7C 118.0(2) . . ? C3C C2C P1C 123.8(2) . . ? C7C C2C P1C 117.86(19) . . ? C8C C9C C10C 120.0(2) . . ? C6C C7C C2C 120.9(3) . . ? C4C C3C C2C 120.2(3) . . ? C5C C6C C7C 120.6(3) . . ? C6C C5C C4C 119.5(3) . . ? C5C C4C C3C 120.8(3) . . ? C19C C14C C15C 118.1(2) . . ? C19C C14C P2C 118.14(19) . . ? C15C C14C P2C 123.6(2) . . ? C12C C13C C8C 120.7(3) . . ? C21C C20C C25C 119.1(2) . . ? C21C C20C P2C 118.0(2) . . ? C25C C20C P2C 122.8(2) . . ? C14C C19C C18C 121.1(3) . . ? C11C C10C C9C 120.1(3) . . ? C20C C21C C22C 120.5(3) . . ? C23C C24C C25C 120.0(3) . . ? C11C C12C C13C 120.0(3) . . ? C12C C11C C10C 120.3(2) . . ? C24C C25C C20C 120.2(3) . . ? C24C C23C C22C 120.4(3) . . ? C14C C15C C16C 120.6(3) . . ? C23C C22C C21C 119.9(3) . . ? C17C C18C C19C 120.0(3) . . ? C18C C17C C16C 119.3(3) . . ? C17C C16C C15C 120.8(3) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.787 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.069 #===== END data_FO2190 _database_code_depnum_ccdc_archive 'CCDC 600558' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H44 Ni P4 * 1/2 C4 H8 O' _chemical_formula_weight 863.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _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 11.8283(3) _cell_length_b 22.0688(4) _cell_length_c 16.7883(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.564(1) _cell_angle_gamma 90.00 _cell_volume 4373.88(17) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.627 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30846 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10025 _reflns_number_gt 7297 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^+2.1436P] 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 10025 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0888 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.56670(2) 0.139723(12) 0.199991(16) 0.01871(8) Uani 1 1 d . . . P1 P 0.67028(5) 0.17514(2) 0.30227(3) 0.01966(13) Uani 1 1 d . . . P2 P 0.62658(5) 0.05716(2) 0.25980(3) 0.02208(13) Uani 1 1 d . . . P3 P 0.39416(5) 0.16906(2) 0.16421(3) 0.01985(13) Uani 1 1 d . . . P4 P 0.57606(5) 0.16134(2) 0.07444(3) 0.01998(13) Uani 1 1 d . . . C1 C 0.7239(2) 0.09898(9) 0.33182(14) 0.0253(5) Uani 1 1 d . . . H1A H 0.7113 0.0891 0.3881 0.030 Uiso 1 1 calc R . . H1B H 0.8047 0.0933 0.3214 0.030 Uiso 1 1 calc R . . C2 C 0.41966(19) 0.16586(10) 0.05660(13) 0.0236(5) Uani 1 1 d . . . H2A H 0.3945 0.2029 0.0274 0.028 Uiso 1 1 calc R . . H2B H 0.3866 0.1294 0.0298 0.028 Uiso 1 1 calc R . . C3 C 0.79597(19) 0.22354(10) 0.29956(13) 0.0224(5) Uani 1 1 d . . . C4 C 0.7942(2) 0.28302(10) 0.32648(14) 0.0289(5) Uani 1 1 d . . . H4A H 0.7313 0.2971 0.3539 0.035 Uiso 1 1 calc R . . C5 C 0.8834(2) 0.32226(12) 0.31380(16) 0.0366(6) Uani 1 1 d . . . H5A H 0.8804 0.3630 0.3317 0.044 Uiso 1 1 calc R . . C6 C 0.9759(2) 0.30220(13) 0.27542(16) 0.0385(6) Uani 1 1 d . . . H6A H 1.0371 0.3289 0.2674 0.046 Uiso 1 1 calc R . . C7 C 0.9795(2) 0.24309(13) 0.24864(15) 0.0380(6) Uani 1 1 d . . . H7A H 1.0438 0.2291 0.2228 0.046 Uiso 1 1 calc R . . C8 C 0.8896(2) 0.20410(11) 0.25931(14) 0.0303(5) Uani 1 1 d . . . H8A H 0.8917 0.1639 0.2392 0.036 Uiso 1 1 calc R . . C9 C 0.60961(19) 0.20391(10) 0.39269(13) 0.0212(5) Uani 1 1 d . . . C10 C 0.6642(2) 0.20078(10) 0.46866(14) 0.0270(5) Uani 1 1 d . . . H10A H 0.7381 0.1840 0.4753 0.032 Uiso 1 1 calc R . . C11 C 0.6112(2) 0.22202(11) 0.53461(14) 0.0317(6) Uani 1 1 d . . . H11A H 0.6487 0.2194 0.5862 0.038 Uiso 1 1 calc R . . C12 C 0.5047(2) 0.24686(13) 0.52558(16) 0.0405(7) Uani 1 1 d . . . H12A H 0.4686 0.2613 0.5709 0.049 Uiso 1 1 calc R . . C13 C 0.4500(2) 0.25087(15) 0.45096(17) 0.0485(8) Uani 1 1 d . . . H13A H 0.3766 0.2683 0.4446 0.058 Uiso 1 1 calc R . . C14 C 0.5030(2) 0.22931(13) 0.38508(15) 0.0369(6) Uani 1 1 d . . . H14A H 0.4650 0.2321 0.3337 0.044 Uiso 1 1 calc R . . C15 C 0.5383(2) 0.01283(10) 0.32478(14) 0.0267(5) Uani 1 1 d . . . C16 C 0.5224(2) -0.04907(11) 0.31785(16) 0.0404(7) Uani 1 1 d . . . H16A H 0.5627 -0.0712 0.2803 0.048 Uiso 1 1 calc R . . C17 C 0.4485(3) -0.07916(13) 0.36493(18) 0.0508(8) Uani 1 1 d . . . H17A H 0.4384 -0.1217 0.3591 0.061 Uiso 1 1 calc R . . C18 C 0.3899(2) -0.04852(13) 0.41963(17) 0.0452(7) Uani 1 1 d . . . H18A H 0.3394 -0.0695 0.4518 0.054 Uiso 1 1 calc R . . C19 C 0.4048(3) 0.01322(13) 0.42772(19) 0.0488(8) Uani 1 1 d . . . H19A H 0.3646 0.0350 0.4658 0.059 Uiso 1 1 calc R . . C20 C 0.4780(2) 0.04353(12) 0.38060(17) 0.0419(7) Uani 1 1 d . . . H20A H 0.4874 0.0861 0.3865 0.050 Uiso 1 1 calc R . . C21 C 0.71936(19) -0.00101(10) 0.21947(15) 0.0259(5) Uani 1 1 d . . . C22 C 0.7270(2) -0.00465(11) 0.13774(16) 0.0344(6) Uani 1 1 d . . . H22A H 0.6805 0.0206 0.1036 0.041 Uiso 1 1 calc R . . C23 C 0.8018(3) -0.04485(12) 0.10502(18) 0.0461(7) Uani 1 1 d . . . H23A H 0.8065 -0.0469 0.0488 0.055 Uiso 1 1 calc R . . C24 C 0.8693(2) -0.08177(12) 0.1545(2) 0.0460(8) Uani 1 1 d . . . H24A H 0.9209 -0.1090 0.1322 0.055 Uiso 1 1 calc R . . C25 C 0.8619(2) -0.07912(12) 0.2355(2) 0.0458(7) Uani 1 1 d . . . H25A H 0.9079 -0.1049 0.2693 0.055 Uiso 1 1 calc R . . C26 C 0.7874(2) -0.03901(11) 0.26845(17) 0.0374(6) Uani 1 1 d . . . H26A H 0.7828 -0.0374 0.3247 0.045 Uiso 1 1 calc R . . C27 C 0.25840(19) 0.13024(10) 0.17456(14) 0.0257(5) Uani 1 1 d . . . C28 C 0.2434(2) 0.09863(11) 0.24456(16) 0.0371(6) Uani 1 1 d . . . H28A H 0.3026 0.0979 0.2855 0.045 Uiso 1 1 calc R . . C29 C 0.1428(3) 0.06802(13) 0.25565(19) 0.0487(8) Uani 1 1 d . . . H29A H 0.1333 0.0473 0.3044 0.058 Uiso 1 1 calc R . . C30 C 0.0575(3) 0.06767(13) 0.1966(2) 0.0521(9) Uani 1 1 d . . . H30A H -0.0108 0.0463 0.2039 0.062 Uiso 1 1 calc R . . C31 C 0.0712(2) 0.09853(13) 0.1264(2) 0.0495(8) Uani 1 1 d . . . H31A H 0.0121 0.0984 0.0855 0.059 Uiso 1 1 calc R . . C32 C 0.1712(2) 0.13000(11) 0.11514(17) 0.0354(6) Uani 1 1 d . . . H32A H 0.1797 0.1513 0.0667 0.042 Uiso 1 1 calc R . . C33 C 0.35266(18) 0.24807(10) 0.18179(13) 0.0228(5) Uani 1 1 d . . . C34 C 0.28991(19) 0.26207(11) 0.24735(15) 0.0282(5) Uani 1 1 d . . . H34A H 0.2592 0.2303 0.2775 0.034 Uiso 1 1 calc R . . C35 C 0.2721(2) 0.32193(12) 0.26887(17) 0.0368(6) Uani 1 1 d . . . H35A H 0.2312 0.3308 0.3144 0.044 Uiso 1 1 calc R . . C36 C 0.3134(2) 0.36847(12) 0.22449(18) 0.0429(7) Uani 1 1 d . . . H36A H 0.3005 0.4094 0.2390 0.051 Uiso 1 1 calc R . . C37 C 0.3732(2) 0.35552(11) 0.15913(19) 0.0418(7) Uani 1 1 d . . . H37A H 0.4007 0.3877 0.1281 0.050 Uiso 1 1 calc R . . C38 C 0.3942(2) 0.29595(11) 0.13771(16) 0.0309(5) Uani 1 1 d . . . H38A H 0.4369 0.2877 0.0929 0.037 Uiso 1 1 calc R . . C39 C 0.62798(19) 0.23482(10) 0.03964(14) 0.0232(5) Uani 1 1 d . . . C40 C 0.6953(2) 0.27024(11) 0.09139(15) 0.0307(5) Uani 1 1 d . . . H40A H 0.7145 0.2565 0.1441 0.037 Uiso 1 1 calc R . . C41 C 0.7349(3) 0.32599(12) 0.06635(19) 0.0457(7) Uani 1 1 d . . . H41A H 0.7819 0.3500 0.1018 0.055 Uiso 1 1 calc R . . C42 C 0.7062(3) 0.34641(12) -0.0095(2) 0.0511(8) Uani 1 1 d . . . H42A H 0.7334 0.3845 -0.0264 0.061 Uiso 1 1 calc R . . C43 C 0.6378(3) 0.31172(12) -0.06159(18) 0.0449(7) Uani 1 1 d . . . H43A H 0.6174 0.3261 -0.1139 0.054 Uiso 1 1 calc R . . C44 C 0.5994(2) 0.25613(11) -0.03708(15) 0.0331(6) Uani 1 1 d . . . H44A H 0.5530 0.2321 -0.0729 0.040 Uiso 1 1 calc R . . C45 C 0.6274(2) 0.11200(10) -0.00363(13) 0.0237(5) Uani 1 1 d . . . C46 C 0.5605(2) 0.07045(11) -0.04678(15) 0.0334(6) Uani 1 1 d . . . H46A H 0.4811 0.0696 -0.0409 0.040 Uiso 1 1 calc R . . C47 C 0.6083(3) 0.02986(12) -0.09881(17) 0.0422(7) Uani 1 1 d . . . H47A H 0.5614 0.0018 -0.1284 0.051 Uiso 1 1 calc R . . C48 C 0.7229(3) 0.03030(12) -0.10744(16) 0.0429(7) Uani 1 1 d . . . H48A H 0.7552 0.0026 -0.1429 0.051 Uiso 1 1 calc R . . C49 C 0.7910(3) 0.07098(12) -0.06457(17) 0.0430(7) Uani 1 1 d . . . H49A H 0.8704 0.0713 -0.0705 0.052 Uiso 1 1 calc R . . C50 C 0.7440(2) 0.11146(11) -0.01279(16) 0.0342(6) Uani 1 1 d . . . H50A H 0.7917 0.1391 0.0168 0.041 Uiso 1 1 calc R . . O1T O 0.0903(4) 0.0056(2) 0.4375(3) 0.0684(14) Uani 0.50 1 d P . . C1T C -0.0147(4) 0.0253(3) 0.4396(3) 0.119(2) Uani 1 1 d . . . H1TA H -0.0498 0.0158 0.3860 0.142 Uiso 1 1 calc R . . H1TB H -0.0075 0.0700 0.4414 0.142 Uiso 1 1 calc R . . C2T C 0.0986(5) -0.0125(3) 0.5090(3) 0.127(2) Uani 1 1 d . . . H2TA H 0.1476 0.0178 0.5377 0.153 Uiso 1 1 calc R . . H2TB H 0.1442 -0.0501 0.5078 0.153 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.01921(15) 0.01892(14) 0.01784(14) -0.00031(11) -0.00011(11) 0.00118(11) P1 0.0198(3) 0.0197(3) 0.0192(3) -0.0008(2) -0.0009(2) 0.0013(2) P2 0.0237(3) 0.0185(3) 0.0238(3) 0.0005(2) -0.0004(2) 0.0014(2) P3 0.0186(3) 0.0205(3) 0.0205(3) -0.0009(2) 0.0012(2) 0.0008(2) P4 0.0205(3) 0.0212(3) 0.0183(3) -0.0010(2) 0.0016(2) -0.0010(2) C1 0.0282(13) 0.0205(11) 0.0262(12) 0.0002(10) -0.0047(10) 0.0034(9) C2 0.0228(12) 0.0274(12) 0.0202(11) -0.0010(9) -0.0021(9) -0.0022(9) C3 0.0203(12) 0.0278(12) 0.0186(11) 0.0024(9) -0.0025(9) -0.0003(9) C4 0.0285(13) 0.0276(12) 0.0308(13) 0.0029(10) 0.0041(10) -0.0010(10) C5 0.0373(16) 0.0290(13) 0.0432(16) 0.0073(12) -0.0008(12) -0.0064(11) C6 0.0250(14) 0.0487(16) 0.0412(15) 0.0179(13) -0.0033(12) -0.0106(12) C7 0.0215(13) 0.0617(18) 0.0312(14) 0.0107(13) 0.0035(11) 0.0048(12) C8 0.0261(13) 0.0369(13) 0.0279(13) -0.0012(11) 0.0022(10) 0.0013(10) C9 0.0220(12) 0.0221(11) 0.0194(11) -0.0007(9) 0.0009(9) -0.0029(9) C10 0.0271(13) 0.0279(12) 0.0256(12) -0.0006(10) -0.0024(10) -0.0029(10) C11 0.0394(15) 0.0367(14) 0.0189(12) -0.0007(11) -0.0006(10) -0.0085(11) C12 0.0375(16) 0.0567(17) 0.0282(14) -0.0165(13) 0.0086(12) -0.0039(13) C13 0.0293(15) 0.077(2) 0.0383(16) -0.0168(15) -0.0014(12) 0.0173(14) C14 0.0310(14) 0.0558(17) 0.0230(13) -0.0073(12) -0.0053(11) 0.0100(12) C15 0.0268(13) 0.0263(12) 0.0264(12) 0.0056(10) -0.0020(10) 0.0018(10) C16 0.0525(18) 0.0308(13) 0.0391(15) -0.0058(12) 0.0138(13) -0.0106(12) C17 0.070(2) 0.0350(15) 0.0485(18) -0.0034(14) 0.0164(16) -0.0209(14) C18 0.0437(17) 0.0481(17) 0.0450(17) 0.0100(14) 0.0130(14) -0.0110(13) C19 0.0497(19) 0.0442(16) 0.0552(19) 0.0102(14) 0.0254(15) 0.0103(14) C20 0.0474(17) 0.0270(13) 0.0533(17) 0.0089(13) 0.0182(14) 0.0072(12) C21 0.0231(12) 0.0186(11) 0.0361(13) -0.0031(10) 0.0027(10) -0.0012(9) C22 0.0413(16) 0.0256(12) 0.0369(14) 0.0031(11) 0.0066(12) 0.0046(11) C23 0.059(2) 0.0333(14) 0.0492(17) -0.0024(13) 0.0258(15) 0.0034(13) C24 0.0339(16) 0.0266(13) 0.079(2) -0.0067(14) 0.0192(15) 0.0037(11) C25 0.0322(16) 0.0311(14) 0.073(2) -0.0010(14) -0.0078(15) 0.0095(11) C26 0.0384(16) 0.0298(13) 0.0427(15) -0.0024(12) -0.0070(12) 0.0072(11) C27 0.0221(12) 0.0213(11) 0.0345(13) -0.0064(10) 0.0082(10) 0.0013(9) C28 0.0420(16) 0.0381(14) 0.0328(14) -0.0058(12) 0.0149(12) -0.0076(12) C29 0.057(2) 0.0401(16) 0.0531(19) -0.0106(14) 0.0339(17) -0.0133(14) C30 0.0336(17) 0.0354(15) 0.091(3) -0.0195(17) 0.0327(18) -0.0122(12) C31 0.0217(14) 0.0407(16) 0.085(2) -0.0119(16) -0.0038(15) -0.0033(12) C32 0.0261(14) 0.0284(13) 0.0510(16) -0.0012(12) -0.0025(12) 0.0007(10) C33 0.0184(11) 0.0234(11) 0.0258(12) -0.0038(9) -0.0059(9) 0.0026(9) C34 0.0189(12) 0.0324(13) 0.0324(13) -0.0053(11) -0.0050(10) 0.0012(10) C35 0.0250(14) 0.0415(15) 0.0434(16) -0.0178(13) -0.0032(11) 0.0073(11) C36 0.0369(16) 0.0292(14) 0.0610(19) -0.0146(14) -0.0091(14) 0.0085(11) C37 0.0358(16) 0.0262(13) 0.0626(19) 0.0047(13) -0.0040(14) 0.0005(11) C38 0.0233(13) 0.0284(12) 0.0404(14) -0.0012(11) -0.0017(11) 0.0026(10) C39 0.0225(12) 0.0220(11) 0.0255(12) -0.0008(9) 0.0050(9) -0.0004(9) C40 0.0290(14) 0.0318(13) 0.0309(13) -0.0013(11) -0.0014(11) -0.0025(10) C41 0.0497(18) 0.0316(14) 0.0551(19) -0.0039(14) -0.0029(14) -0.0157(13) C42 0.061(2) 0.0293(14) 0.064(2) 0.0093(14) 0.0126(17) -0.0153(13) C43 0.0581(19) 0.0368(15) 0.0402(16) 0.0123(13) 0.0071(14) -0.0058(13) C44 0.0403(15) 0.0329(13) 0.0260(13) 0.0030(11) 0.0021(11) -0.0069(11) C45 0.0315(13) 0.0217(11) 0.0184(11) 0.0021(9) 0.0047(9) 0.0012(9) C46 0.0362(15) 0.0329(13) 0.0307(13) -0.0060(11) -0.0007(11) 0.0015(11) C47 0.0556(19) 0.0318(14) 0.0387(16) -0.0109(12) 0.0003(13) 0.0033(13) C48 0.066(2) 0.0281(13) 0.0368(15) -0.0038(12) 0.0197(14) 0.0111(13) C49 0.0421(17) 0.0385(15) 0.0512(17) 0.0018(14) 0.0252(14) 0.0046(13) C50 0.0359(15) 0.0303(13) 0.0376(14) -0.0030(11) 0.0125(12) -0.0044(11) O1T 0.059(3) 0.091(4) 0.055(3) 0.022(3) 0.004(2) 0.014(3) C1T 0.047(3) 0.202(6) 0.107(4) 0.041(4) 0.004(3) -0.009(3) C2T 0.103(4) 0.224(7) 0.055(3) 0.005(4) 0.010(3) -0.040(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni P4 2.1706(6) . ? Ni P2 2.1774(6) . ? Ni P3 2.1892(6) . ? Ni P1 2.1906(6) . ? P1 C9 1.832(2) . ? P1 C3 1.833(2) . ? P1 C1 1.853(2) . ? P2 C15 1.838(2) . ? P2 C21 1.845(2) . ? P2 C1 1.862(2) . ? P3 C27 1.838(2) . ? P3 C33 1.840(2) . ? P3 C2 1.851(2) . ? P4 C45 1.836(2) . ? P4 C39 1.842(2) . ? P4 C2 1.858(2) . ? C3 C4 1.389(3) . ? C3 C8 1.401(3) . ? C4 C5 1.392(3) . ? C5 C6 1.377(4) . ? C6 C7 1.381(4) . ? C7 C8 1.388(4) . ? C9 C14 1.378(3) . ? C9 C10 1.395(3) . ? C10 C11 1.387(3) . ? C11 C12 1.374(4) . ? C12 C13 1.376(4) . ? C13 C14 1.389(4) . ? C15 C16 1.383(3) . ? C15 C20 1.389(3) . ? C16 C17 1.384(4) . ? C17 C18 1.363(4) . ? C18 C19 1.379(4) . ? C19 C20 1.382(4) . ? C21 C22 1.383(3) . ? C21 C26 1.395(3) . ? C22 C23 1.390(3) . ? C23 C24 1.381(4) . ? C24 C25 1.371(4) . ? C25 C26 1.387(4) . ? C27 C28 1.388(3) . ? C27 C32 1.390(4) . ? C28 C29 1.390(4) . ? C29 C30 1.370(5) . ? C30 C31 1.379(5) . ? C31 C32 1.394(4) . ? C33 C38 1.397(3) . ? C33 C34 1.400(3) . ? C34 C35 1.389(3) . ? C35 C36 1.376(4) . ? C36 C37 1.373(4) . ? C37 C38 1.389(3) . ? C39 C40 1.383(3) . ? C39 C44 1.393(3) . ? C40 C41 1.391(3) . ? C41 C42 1.374(4) . ? C42 C43 1.384(4) . ? C43 C44 1.380(3) . ? C45 C46 1.386(3) . ? C45 C50 1.398(3) . ? C46 C47 1.395(3) . ? C47 C48 1.372(4) . ? C48 C49 1.379(4) . ? C49 C50 1.387(3) . ? O1T C2T 1.263(6) . ? O1T C1T 1.319(6) . ? C1T C2T 1.383(6) 3_556 ? C2T C1T 1.383(6) 3_556 ? 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 P4 Ni P2 126.65(2) . . ? P4 Ni P3 76.79(2) . . ? P2 Ni P3 130.17(2) . . ? P4 Ni P1 128.53(2) . . ? P2 Ni P1 77.70(2) . . ? P3 Ni P1 125.17(2) . . ? C9 P1 C3 100.28(10) . . ? C9 P1 C1 103.75(10) . . ? C3 P1 C1 105.68(10) . . ? C9 P1 Ni 122.97(8) . . ? C3 P1 Ni 127.11(7) . . ? C1 P1 Ni 92.97(7) . . ? C15 P2 C21 102.73(10) . . ? C15 P2 C1 103.27(11) . . ? C21 P2 C1 103.02(11) . . ? C15 P2 Ni 122.58(8) . . ? C21 P2 Ni 126.65(8) . . ? C1 P2 Ni 93.15(7) . . ? C27 P3 C33 100.55(10) . . ? C27 P3 C2 105.71(10) . . ? C33 P3 C2 104.71(10) . . ? C27 P3 Ni 129.89(8) . . ? C33 P3 Ni 119.32(7) . . ? C2 P3 Ni 92.92(7) . . ? C45 P4 C39 99.45(10) . . ? C45 P4 C2 106.67(10) . . ? C39 P4 C2 104.47(10) . . ? C45 P4 Ni 127.01(7) . . ? C39 P4 Ni 122.66(8) . . ? C2 P4 Ni 93.32(7) . . ? P1 C1 P2 95.05(10) . . ? P3 C2 P4 93.77(10) . . ? C4 C3 C8 118.4(2) . . ? C4 C3 P1 120.91(17) . . ? C8 C3 P1 120.04(18) . . ? C3 C4 C5 120.7(2) . . ? C6 C5 C4 120.2(2) . . ? C5 C6 C7 119.8(2) . . ? C6 C7 C8 120.3(2) . . ? C7 C8 C3 120.5(2) . . ? C14 C9 C10 118.3(2) . . ? C14 C9 P1 117.85(17) . . ? C10 C9 P1 123.89(18) . . ? C11 C10 C9 120.5(2) . . ? C12 C11 C10 120.2(2) . . ? C11 C12 C13 120.1(2) . . ? C12 C13 C14 119.6(3) . . ? C9 C14 C13 121.4(2) . . ? C16 C15 C20 117.8(2) . . ? C16 C15 P2 123.72(19) . . ? C20 C15 P2 118.38(18) . . ? C17 C16 C15 120.9(3) . . ? C18 C17 C16 120.8(3) . . ? C17 C18 C19 119.3(3) . . ? C20 C19 C18 120.2(3) . . ? C19 C20 C15 121.1(2) . . ? C22 C21 C26 118.6(2) . . ? C22 C21 P2 118.78(18) . . ? C26 C21 P2 122.47(19) . . ? C21 C22 C23 120.7(3) . . ? C24 C23 C22 119.8(3) . . ? C25 C24 C23 120.1(2) . . ? C24 C25 C26 120.3(3) . . ? C25 C26 C21 120.4(3) . . ? C28 C27 C32 118.5(2) . . ? C28 C27 P3 118.2(2) . . ? C32 C27 P3 123.22(19) . . ? C27 C28 C29 120.9(3) . . ? C30 C29 C28 120.2(3) . . ? C29 C30 C31 119.7(3) . . ? C30 C31 C32 120.5(3) . . ? C27 C32 C31 120.1(3) . . ? C38 C33 C34 118.1(2) . . ? C38 C33 P3 121.73(17) . . ? C34 C33 P3 119.68(17) . . ? C35 C34 C33 120.7(2) . . ? C36 C35 C34 120.3(2) . . ? C37 C36 C35 119.7(2) . . ? C36 C37 C38 120.9(3) . . ? C37 C38 C33 120.3(2) . . ? C40 C39 C44 119.2(2) . . ? C40 C39 P4 119.24(18) . . ? C44 C39 P4 121.60(18) . . ? C39 C40 C41 120.1(2) . . ? C42 C41 C40 120.1(3) . . ? C41 C42 C43 120.3(2) . . ? C44 C43 C42 119.6(3) . . ? C43 C44 C39 120.7(2) . . ? C46 C45 C50 118.2(2) . . ? C46 C45 P4 124.20(18) . . ? C50 C45 P4 117.13(18) . . ? C45 C46 C47 120.8(2) . . ? C48 C47 C46 120.2(3) . . ? C47 C48 C49 119.9(2) . . ? C48 C49 C50 120.2(3) . . ? C49 C50 C45 120.8(2) . . ? C2T O1T C1T 95.5(5) . . ? O1T C1T C2T 131.5(5) . 3_556 ? O1T C2T C1T 129.9(6) . 3_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.543 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.065 #===== END data_FO2561 _database_code_depnum_ccdc_archive 'CCDC 600559' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H31 N2 Ni O2.25 P2 *C3 H7 N O' _chemical_formula_weight 671.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3147 0.7232 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting mpnoclinic _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 21.3152(9) _cell_length_b 8.0904(5) _cell_length_c 21.7217(13) _cell_angle_alpha 90.00 _cell_angle_beta 118.410(2) _cell_angle_gamma 90.00 _cell_volume 3294.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.384 _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 120(2) _diffrn_radiation_wavelength 0.46409 _diffrn_radiation_type ? _diffrn_radiation_source 'synchrotron-radiation ESRF' _diffrn_radiation_monochromator Si(111) _diffrn_measurement_device_type BRUKER-AXS _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24947 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 17.54 _reflns_number_total 7377 _reflns_number_gt 6054 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXTL-97 _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^)+(0.0678P)^2^+2.1867P] 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 SHELXL _refine_ls_extinction_coef 0.145(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7377 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0622 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1276 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.800783(16) 0.10365(4) 0.075243(15) 0.02225(13) Uani 1 1 d . . . P1 P 0.84625(3) -0.13680(8) 0.10064(3) 0.02046(15) Uani 1 1 d . . . P2 P 0.77960(4) -0.15167(9) -0.05727(3) 0.02869(17) Uani 1 1 d . . . O1 O 0.74835(10) 0.2985(2) 0.03695(10) 0.0326(4) Uani 1 1 d . . . O1P O 0.8185(4) -0.0216(9) -0.0607(4) 0.0270(14) Uiso 0.25 1 d P . . O2 O 0.64126(12) 0.4147(3) -0.00676(14) 0.0532(6) Uani 1 1 d . . . N1 N 0.88350(11) 0.2247(3) 0.08231(11) 0.0247(4) Uani 1 1 d . . . C1 C 0.71799(13) 0.0199(4) 0.07848(14) 0.0311(6) Uani 1 1 d . . . H1A H 0.7079 -0.0948 0.0605 0.037 Uiso 1 1 calc R . . H1B H 0.7260 0.0198 0.1273 0.037 Uiso 1 1 calc R . . C2 C 0.65581(14) 0.1320(4) 0.03324(14) 0.0326(6) Uani 1 1 d . . . H2A H 0.6252 0.0767 -0.0119 0.039 Uiso 1 1 calc R . . H2B H 0.6267 0.1522 0.0569 0.039 Uiso 1 1 calc R . . C3 C 0.68149(15) 0.2952(4) 0.01975(14) 0.0341(6) Uani 1 1 d . . . C4 C 0.88249(15) 0.2874(3) 0.02459(14) 0.0319(6) Uani 1 1 d . . . H4A H 0.8456 0.2546 -0.0200 0.038 Uiso 1 1 calc R . . C5 C 0.93350(16) 0.3983(4) 0.02800(16) 0.0367(6) Uani 1 1 d . . . H5A H 0.9318 0.4398 -0.0137 0.044 Uiso 1 1 calc R . . C6 C 0.98656(16) 0.4476(4) 0.09225(17) 0.0396(7) Uani 1 1 d . . . H6A H 1.0218 0.5244 0.0958 0.047 Uiso 1 1 calc R . . C7 C 0.98759(16) 0.3833(4) 0.15151(16) 0.0379(6) Uani 1 1 d . . . H7A H 1.0236 0.4161 0.1966 0.045 Uiso 1 1 calc R . . C8 C 0.93622(14) 0.2712(3) 0.14502(14) 0.0300(5) Uani 1 1 d . . . H8A H 0.9381 0.2253 0.1861 0.036 Uiso 1 1 calc R . . C9 C 0.84091(12) -0.2564(3) 0.16899(12) 0.0234(5) Uani 1 1 d . . . C10 C 0.82918(13) -0.4265(3) 0.16312(13) 0.0269(5) Uani 1 1 d . . . H10A H 0.8215 -0.4825 0.1217 0.032 Uiso 1 1 calc R . . C11 C 0.82868(15) -0.5146(4) 0.21807(15) 0.0344(6) Uani 1 1 d . . . H11A H 0.8208 -0.6306 0.2141 0.041 Uiso 1 1 calc R . . C12 C 0.83963(17) -0.4328(4) 0.27834(16) 0.0404(7) Uani 1 1 d . . . H12A H 0.8393 -0.4929 0.3158 0.048 Uiso 1 1 calc R . . C13 C 0.85093(19) -0.2649(4) 0.28420(16) 0.0432(7) Uani 1 1 d . . . H13A H 0.8586 -0.2096 0.3258 0.052 Uiso 1 1 calc R . . C14 C 0.85118(15) -0.1754(4) 0.22962(14) 0.0326(6) Uani 1 1 d . . . H14A H 0.8583 -0.0592 0.2337 0.039 Uiso 1 1 calc R . . C15 C 0.94100(13) -0.1427(3) 0.12540(12) 0.0236(5) Uani 1 1 d . . . C16 C 0.96324(14) -0.1144(3) 0.07551(14) 0.0307(5) Uani 1 1 d . . . H16A H 0.9287 -0.1012 0.0278 0.037 Uiso 1 1 calc R . . C17 C 1.03519(16) -0.1054(4) 0.09457(16) 0.0364(6) Uani 1 1 d . . . H17A H 1.0496 -0.0870 0.0599 0.044 Uiso 1 1 calc R . . C18 C 1.08603(15) -0.1231(4) 0.16395(18) 0.0429(7) Uani 1 1 d . . . H18A H 1.1353 -0.1155 0.1772 0.051 Uiso 1 1 calc R . . C19 C 1.06479(16) -0.1516(5) 0.21382(18) 0.0497(9) Uani 1 1 d . . . H19A H 1.0997 -0.1653 0.2614 0.060 Uiso 1 1 calc R . . C20 C 0.99280(15) -0.1608(4) 0.19512(15) 0.0393(7) Uani 1 1 d . . . H20A H 0.9788 -0.1794 0.2301 0.047 Uiso 1 1 calc R . . C21 C 0.80441(13) -0.2714(3) 0.02351(12) 0.0253(5) Uani 1 1 d . . . H21A H 0.7613 -0.3233 0.0212 0.030 Uiso 1 1 calc R . . H21B H 0.8380 -0.3606 0.0276 0.030 Uiso 1 1 calc R . . C22 C 0.78375(13) -0.3127(3) -0.11465(12) 0.0282(5) Uani 1 1 d . . . C23 C 0.82164(16) -0.2748(4) -0.14992(16) 0.0397(7) Uani 1 1 d . . . H23A H 0.8442 -0.1701 -0.1430 0.048 Uiso 1 1 calc R . . C24 C 0.82693(17) -0.3890(5) -0.19559(16) 0.0443(8) Uani 1 1 d . . . H24A H 0.8530 -0.3613 -0.2194 0.053 Uiso 1 1 calc R . . C25 C 0.79501(17) -0.5390(5) -0.20602(15) 0.0440(8) Uani 1 1 d . . . H25A H 0.7980 -0.6157 -0.2376 0.053 Uiso 1 1 calc R . . C26 C 0.7581(2) -0.5793(5) -0.1703(2) 0.0575(10) Uani 1 1 d . . . H26D H 0.7363 -0.6848 -0.1770 0.069 Uiso 1 1 calc R . . C27 C 0.75252(19) -0.4674(4) -0.12480(17) 0.0469(8) Uani 1 1 d . . . H27A H 0.7271 -0.4971 -0.1004 0.056 Uiso 1 1 calc R . . C28 C 0.68399(14) -0.1139(4) -0.09355(13) 0.0301(6) Uani 1 1 d . . . C29 C 0.63454(15) -0.2259(4) -0.09324(14) 0.0338(6) Uani 1 1 d . . . H29A H 0.6501 -0.3299 -0.0708 0.041 Uiso 1 1 calc R . . C30 C 0.56213(16) -0.1859(5) -0.12586(15) 0.0424(7) Uani 1 1 d . . . H30B H 0.5284 -0.2626 -0.1258 0.051 Uiso 1 1 calc R . . C31 C 0.53957(16) -0.0337(5) -0.15842(15) 0.0460(8) Uani 1 1 d . . . H31A H 0.4901 -0.0079 -0.1817 0.055 Uiso 1 1 calc R . . C32 C 0.58773(18) 0.0797(5) -0.15737(15) 0.0455(8) Uani 1 1 d . . . H32A H 0.5719 0.1853 -0.1782 0.055 Uiso 1 1 calc R . . C33 C 0.66029(16) 0.0401(4) -0.12553(14) 0.0378(6) Uani 1 1 d . . . H33A H 0.6936 0.1180 -0.1256 0.045 Uiso 1 1 calc R . . O1D O 0.94594(13) 0.1495(3) 0.30252(12) 0.0484(6) Uani 1 1 d . . . C1D C 0.96739(17) 0.1648(4) 0.36538(17) 0.0420(7) Uani 1 1 d . . . H1DA H 1.0174 0.1762 0.3944 0.050 Uiso 1 1 calc R . . N1D N 0.92678(14) 0.1667(4) 0.39681(14) 0.0418(6) Uani 1 1 d . . . C2D C 0.9567(2) 0.2016(7) 0.47153(19) 0.0666(12) Uani 1 1 d . . . H2DA H 1.0089 0.2015 0.4934 0.100 Uiso 1 1 calc R . . H2DB H 0.9411 0.1166 0.4934 0.100 Uiso 1 1 calc R . . H2DC H 0.9402 0.3102 0.4779 0.100 Uiso 1 1 calc R . . C3D C 0.85015(16) 0.1453(4) 0.35777(18) 0.0432(7) Uani 1 1 d . . . H3DA H 0.8362 0.1227 0.3086 0.065 Uiso 1 1 calc R . . H3DB H 0.8265 0.2463 0.3610 0.065 Uiso 1 1 calc R . . H3DC H 0.8359 0.0524 0.3773 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.02233(18) 0.02364(19) 0.01984(17) 0.00087(11) 0.00928(13) 0.00210(12) P1 0.0201(3) 0.0239(3) 0.0163(3) 0.0009(2) 0.0077(2) 0.0014(2) P2 0.0292(3) 0.0344(4) 0.0196(3) 0.0059(3) 0.0092(3) 0.0053(3) O1 0.0292(9) 0.0288(10) 0.0331(10) 0.0016(8) 0.0095(8) 0.0044(8) O2 0.0370(12) 0.0434(13) 0.0665(16) 0.0080(11) 0.0143(11) 0.0157(10) N1 0.0267(10) 0.0225(10) 0.0255(10) 0.0019(8) 0.0129(8) 0.0022(8) C1 0.0284(12) 0.0395(15) 0.0295(13) 0.0016(11) 0.0171(11) 0.0028(11) C2 0.0257(12) 0.0458(16) 0.0261(12) -0.0016(11) 0.0122(10) 0.0029(11) C3 0.0333(13) 0.0357(15) 0.0292(13) -0.0056(11) 0.0115(11) 0.0049(11) C4 0.0385(14) 0.0321(14) 0.0260(12) 0.0028(10) 0.0161(11) 0.0028(11) C5 0.0441(16) 0.0372(15) 0.0383(15) 0.0099(12) 0.0272(13) 0.0046(12) C6 0.0388(15) 0.0354(15) 0.0520(18) 0.0003(13) 0.0276(14) -0.0035(13) C7 0.0315(13) 0.0443(17) 0.0353(14) -0.0073(12) 0.0139(12) -0.0054(12) C8 0.0295(12) 0.0353(14) 0.0254(12) 0.0004(10) 0.0133(10) -0.0007(11) C9 0.0224(11) 0.0280(12) 0.0191(11) 0.0022(9) 0.0092(9) 0.0004(9) C10 0.0260(12) 0.0294(13) 0.0252(12) 0.0017(10) 0.0121(10) 0.0009(10) C11 0.0371(14) 0.0303(14) 0.0403(15) 0.0094(11) 0.0221(12) 0.0024(11) C12 0.0496(17) 0.0456(17) 0.0359(15) 0.0148(13) 0.0284(14) 0.0079(14) C13 0.061(2) 0.0461(18) 0.0290(14) 0.0023(13) 0.0273(14) 0.0050(15) C14 0.0415(15) 0.0317(14) 0.0244(12) 0.0004(10) 0.0156(11) -0.0004(12) C15 0.0229(11) 0.0240(12) 0.0230(11) 0.0030(9) 0.0100(9) 0.0003(9) C16 0.0309(13) 0.0348(14) 0.0291(13) 0.0024(11) 0.0165(11) 0.0022(11) C17 0.0367(14) 0.0361(15) 0.0447(16) 0.0064(12) 0.0260(13) 0.0008(12) C18 0.0239(13) 0.0467(18) 0.0558(19) 0.0186(15) 0.0171(13) 0.0046(12) C19 0.0249(13) 0.075(2) 0.0385(16) 0.0214(16) 0.0061(12) 0.0017(15) C20 0.0265(13) 0.0602(19) 0.0261(13) 0.0128(13) 0.0084(11) -0.0015(13) C21 0.0269(11) 0.0269(12) 0.0178(11) -0.0005(9) 0.0071(9) 0.0016(10) C22 0.0253(12) 0.0378(14) 0.0188(11) 0.0042(10) 0.0084(9) 0.0067(10) C23 0.0388(15) 0.0510(18) 0.0345(15) 0.0034(13) 0.0215(13) 0.0022(13) C24 0.0401(16) 0.067(2) 0.0341(15) 0.0047(14) 0.0245(13) 0.0114(15) C25 0.0490(17) 0.055(2) 0.0286(14) -0.0006(13) 0.0192(13) 0.0176(16) C26 0.083(3) 0.050(2) 0.056(2) -0.0142(17) 0.047(2) -0.0113(19) C27 0.064(2) 0.0500(19) 0.0435(17) -0.0101(15) 0.0392(16) -0.0110(16) C28 0.0304(12) 0.0404(15) 0.0163(10) -0.0001(10) 0.0085(9) 0.0078(11) C29 0.0315(13) 0.0410(16) 0.0236(12) -0.0041(11) 0.0088(10) 0.0041(12) C30 0.0321(14) 0.062(2) 0.0281(14) -0.0088(14) 0.0103(12) 0.0014(14) C31 0.0340(14) 0.069(2) 0.0244(13) -0.0010(14) 0.0051(11) 0.0184(16) C32 0.0494(18) 0.056(2) 0.0270(14) 0.0095(13) 0.0144(13) 0.0261(16) C33 0.0417(15) 0.0445(16) 0.0255(13) 0.0058(12) 0.0147(12) 0.0129(13) O1D 0.0487(13) 0.0620(15) 0.0385(12) -0.0086(11) 0.0239(10) -0.0166(11) C1D 0.0369(15) 0.0503(18) 0.0387(16) -0.0051(14) 0.0178(13) -0.0143(14) N1D 0.0398(13) 0.0508(16) 0.0357(13) -0.0082(11) 0.0187(11) -0.0108(12) C2D 0.066(2) 0.099(3) 0.0392(19) -0.021(2) 0.0285(18) -0.035(2) C3D 0.0347(15) 0.0457(18) 0.0519(18) -0.0018(14) 0.0228(14) 0.0016(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni O1 1.8821(19) . ? Ni C1 1.923(3) . ? Ni N1 1.958(2) . ? Ni P1 2.1258(7) . ? P1 C9 1.820(2) . ? P1 C15 1.827(2) . ? P1 C21 1.835(2) . ? P2 O1P 1.363(7) . ? P2 C28 1.828(3) . ? P2 C22 1.834(3) . ? P2 C21 1.848(3) . ? O1 C3 1.290(3) . ? O2 C3 1.238(4) . ? N1 C4 1.343(3) . ? N1 C8 1.343(3) . ? C1 C2 1.519(4) . ? C2 C3 1.510(4) . ? C4 C5 1.384(4) . ? C5 C6 1.373(5) . ? C6 C7 1.379(4) . ? C7 C8 1.376(4) . ? C9 C14 1.392(4) . ? C9 C10 1.394(4) . ? C10 C11 1.394(4) . ? C11 C12 1.384(4) . ? C12 C13 1.375(5) . ? C13 C14 1.391(4) . ? C15 C16 1.393(4) . ? C15 C20 1.394(4) . ? C16 C17 1.387(4) . ? C17 C18 1.383(5) . ? C18 C19 1.378(5) . ? C19 C20 1.390(4) . ? C22 C23 1.387(4) . ? C22 C27 1.385(4) . ? C23 C24 1.399(5) . ? C24 C25 1.356(5) . ? C25 C26 1.380(5) . ? C26 C27 1.387(5) . ? C28 C29 1.393(4) . ? C28 C33 1.398(4) . ? C29 C30 1.396(4) . ? C30 C31 1.387(5) . ? C31 C32 1.369(5) . ? C32 C33 1.398(4) . ? O1D C1D 1.223(4) . ? C1D N1D 1.333(4) . ? N1D C3D 1.449(4) . ? N1D C2D 1.462(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni C1 87.08(10) . . ? O1 Ni N1 86.48(9) . . ? C1 Ni N1 168.92(11) . . ? O1 Ni P1 169.37(6) . . ? C1 Ni P1 88.91(9) . . ? N1 Ni P1 98.93(6) . . ? C9 P1 C15 103.62(11) . . ? C9 P1 C21 103.73(11) . . ? C15 P1 C21 104.03(12) . . ? C9 P1 Ni 120.02(8) . . ? C15 P1 Ni 113.82(8) . . ? C21 P1 Ni 110.04(8) . . ? O1P P2 C28 115.4(3) . . ? O1P P2 C22 106.5(3) . . ? C28 P2 C22 103.31(12) . . ? O1P P2 C21 123.4(3) . . ? C28 P2 C21 104.70(12) . . ? C22 P2 C21 100.85(12) . . ? C3 O1 Ni 116.89(19) . . ? C4 N1 C8 118.4(2) . . ? C4 N1 Ni 120.12(18) . . ? C8 N1 Ni 120.48(18) . . ? C2 C1 Ni 107.41(19) . . ? C3 C2 C1 111.3(2) . . ? O2 C3 O1 122.9(3) . . ? O2 C3 C2 122.6(3) . . ? O1 C3 C2 114.5(2) . . ? N1 C4 C5 122.1(3) . . ? C6 C5 C4 119.3(3) . . ? C5 C6 C7 118.6(3) . . ? C8 C7 C6 119.6(3) . . ? N1 C8 C7 122.0(3) . . ? C14 C9 C10 119.5(2) . . ? C14 C9 P1 118.6(2) . . ? C10 C9 P1 121.90(19) . . ? C9 C10 C11 120.0(2) . . ? C12 C11 C10 120.0(3) . . ? C13 C12 C11 120.2(3) . . ? C12 C13 C14 120.4(3) . . ? C13 C14 C9 119.9(3) . . ? C16 C15 C20 118.4(2) . . ? C16 C15 P1 120.30(19) . . ? C20 C15 P1 121.1(2) . . ? C17 C16 C15 120.9(3) . . ? C18 C17 C16 120.1(3) . . ? C19 C18 C17 119.6(3) . . ? C18 C19 C20 120.6(3) . . ? C19 C20 C15 120.4(3) . . ? P1 C21 P2 110.54(13) . . ? C23 C22 C27 118.3(3) . . ? C23 C22 P2 116.6(2) . . ? C27 C22 P2 125.1(2) . . ? C22 C23 C24 120.7(3) . . ? C25 C24 C23 120.4(3) . . ? C24 C25 C26 119.5(3) . . ? C27 C26 C25 120.8(4) . . ? C26 C27 C22 120.3(3) . . ? C29 C28 C33 119.1(3) . . ? C29 C28 P2 125.5(2) . . ? C33 C28 P2 115.4(2) . . ? C28 C29 C30 120.2(3) . . ? C31 C30 C29 119.7(3) . . ? C32 C31 C30 120.8(3) . . ? C31 C32 C33 119.9(3) . . ? C32 C33 C28 120.2(3) . . ? O1D C1D N1D 125.7(3) . . ? C1D N1D C3D 121.7(3) . . ? C1D N1D C2D 121.6(3) . . ? C3D N1D C2D 116.6(3) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 17.54 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.745 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.109 #===== END data_FO2663 _database_code_depnum_ccdc_archive 'CCDC 600812' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H31 N Ni O3 P2 * C4 H 8 O' _chemical_formula_weight 682.34 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' Ni Ni 0.3393 1.1124 '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 18.3457(7) _cell_length_b 8.2770(4) _cell_length_c 22.1729(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.078(2) _cell_angle_gamma 90.00 _cell_volume 3362.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.03 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.713 _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 183(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 KappaCCD _diffrn_measurement_method 'phi- + omega-scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21829 _diffrn_reflns_av_R_equivalents 0.1376 _diffrn_reflns_av_sigmaI/netI 0.1364 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.29 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7646 _reflns_number_gt 3956 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL/PC _computing_publication_material SHELXL-97 _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^)+(0.0827P)^2^+3.8020P] 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 7646 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1679 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2182 _refine_ls_wR_factor_gt 0.1718 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Ni Ni 0.77039(4) 0.15287(8) 0.05920(3) 0.0347(2) Uani 1 1 d . . . P1 P 0.66613(8) -0.14554(19) 0.13904(7) 0.0411(4) Uani 1 1 d . . . P2 P 0.75552(7) -0.08710(17) 0.02750(6) 0.0350(3) Uani 1 1 d . . . O1 O 0.7855(2) 0.3581(5) 0.09485(19) 0.0482(10) Uani 1 1 d . . . O2 O 0.8504(3) 0.4952(6) 0.1647(3) 0.091(2) Uani 1 1 d . . . O3 O 0.6218(2) -0.0052(5) 0.1185(2) 0.0544(11) Uani 1 1 d . . . N1 N 0.6946(2) 0.2602(5) 0.0077(2) 0.0407(11) Uani 1 1 d . . . C1 C 0.8550(3) 0.0838(7) 0.1079(3) 0.0430(13) Uani 1 1 d . . . H1A H 0.8463 -0.0237 0.1257 0.052 Uiso 1 1 calc R . . H1B H 0.8981 0.0767 0.0830 0.052 Uiso 1 1 calc R . . C2 C 0.8675(3) 0.2088(7) 0.1571(3) 0.0471(14) Uani 1 1 d . . . H2A H 0.8463 0.1700 0.1946 0.057 Uiso 1 1 calc R . . H2B H 0.9206 0.2242 0.1655 0.057 Uiso 1 1 calc R . . C3 C 0.8332(4) 0.3665(7) 0.1387(3) 0.0532(16) Uani 1 1 d . . . C4 C 0.6302(4) 0.2855(12) 0.0280(4) 0.096(3) Uani 1 1 d . . . H4A H 0.6186 0.2380 0.0653 0.115 Uiso 1 1 calc R . . C5 C 0.5781(6) 0.3800(15) -0.0032(5) 0.142(6) Uani 1 1 d . . . H5A H 0.5298 0.3855 0.0101 0.170 Uiso 1 1 calc R . . C6 C 0.5963(5) 0.4633(10) -0.0520(4) 0.079(2) Uani 1 1 d . . . H6A H 0.5630 0.5368 -0.0715 0.095 Uiso 1 1 calc R . . C7 C 0.6627(5) 0.4394(9) -0.0722(3) 0.070(2) Uani 1 1 d . . . H7A H 0.6773 0.4941 -0.1073 0.085 Uiso 1 1 calc R . . C8 C 0.7089(4) 0.3359(9) -0.0421(3) 0.0624(18) Uani 1 1 d . . . H8A H 0.7550 0.3170 -0.0583 0.075 Uiso 1 1 calc R . . C9 C 0.7228(3) -0.1002(7) 0.2055(3) 0.0443(13) Uani 1 1 d . . . C10 C 0.7086(4) 0.0432(8) 0.2356(3) 0.0575(17) Uani 1 1 d . . . H10A H 0.6713 0.1134 0.2199 0.069 Uiso 1 1 calc R . . C11 C 0.7478(4) 0.0842(10) 0.2876(3) 0.069(2) Uani 1 1 d . . . H11A H 0.7368 0.1816 0.3078 0.083 Uiso 1 1 calc R . . C12 C 0.8027(4) -0.0142(10) 0.3108(3) 0.0649(19) Uani 1 1 d . . . H12A H 0.8298 0.0145 0.3470 0.078 Uiso 1 1 calc R . . C13 C 0.8180(4) -0.1551(9) 0.2809(3) 0.0601(17) Uani 1 1 d . . . H13A H 0.8564 -0.2230 0.2963 0.072 Uiso 1 1 calc R . . C14 C 0.7780(3) -0.1990(8) 0.2286(3) 0.0528(16) Uani 1 1 d . . . H14A H 0.7887 -0.2972 0.2088 0.063 Uiso 1 1 calc R . . C15 C 0.6080(3) -0.3091(7) 0.1606(3) 0.0418(13) Uani 1 1 d . . . C16 C 0.5378(3) -0.2674(8) 0.1748(3) 0.0525(15) Uani 1 1 d . . . H16A H 0.5231 -0.1574 0.1727 0.063 Uiso 1 1 calc R . . C17 C 0.4888(4) -0.3833(10) 0.1919(3) 0.068(2) Uani 1 1 d . . . H17A H 0.4408 -0.3528 0.2016 0.082 Uiso 1 1 calc R . . C18 C 0.5097(4) -0.5431(11) 0.1950(3) 0.068(2) Uani 1 1 d . . . H18A H 0.4765 -0.6221 0.2081 0.082 Uiso 1 1 calc R . . C19 C 0.5779(5) -0.5891(10) 0.1794(4) 0.086(3) Uani 1 1 d . . . H19A H 0.5912 -0.7001 0.1791 0.104 Uiso 1 1 calc R . . C20 C 0.6286(4) -0.4682(9) 0.1635(5) 0.085(3) Uani 1 1 d . . . H20A H 0.6769 -0.4979 0.1549 0.102 Uiso 1 1 calc R . . C21 C 0.7236(3) -0.2327(7) 0.0832(3) 0.0408(13) Uani 1 1 d . . . H21A H 0.6959 -0.3194 0.0614 0.049 Uiso 1 1 calc R . . H21B H 0.7666 -0.2831 0.1045 0.049 Uiso 1 1 calc R . . C22 C 0.8359(3) -0.1847(7) -0.0005(2) 0.0377(13) Uani 1 1 d . . . C23 C 0.8460(3) -0.3510(7) 0.0017(3) 0.0464(14) Uani 1 1 d . . . H23A H 0.8121 -0.4182 0.0207 0.056 Uiso 1 1 calc R . . C24 C 0.9069(4) -0.4184(9) -0.0244(3) 0.0603(18) Uani 1 1 d . . . H24A H 0.9138 -0.5321 -0.0233 0.072 Uiso 1 1 calc R . . C25 C 0.9570(4) -0.3225(11) -0.0517(3) 0.069(2) Uani 1 1 d . . . H25A H 0.9981 -0.3695 -0.0693 0.083 Uiso 1 1 calc R . . C26 C 0.9466(3) -0.1572(9) -0.0533(3) 0.0547(16) Uani 1 1 d . . . H26A H 0.9808 -0.0895 -0.0718 0.066 Uiso 1 1 calc R . . C27 C 0.8865(3) -0.0907(8) -0.0280(3) 0.0472(14) Uani 1 1 d . . . H27A H 0.8798 0.0230 -0.0295 0.057 Uiso 1 1 calc R . . C28 C 0.6886(3) -0.1070(7) -0.0363(3) 0.0430(14) Uani 1 1 d . . . C29 C 0.7109(4) -0.1195(9) -0.0952(3) 0.0590(18) Uani 1 1 d . . . H29A H 0.7613 -0.1319 -0.1020 0.071 Uiso 1 1 calc R . . C30 C 0.6607(4) -0.1140(9) -0.1439(3) 0.069(2) Uani 1 1 d . . . H30A H 0.6766 -0.1204 -0.1839 0.083 Uiso 1 1 calc R . . C31 C 0.5868(5) -0.0990(9) -0.1339(4) 0.075(2) Uani 1 1 d . . . H31A H 0.5520 -0.0980 -0.1672 0.090 Uiso 1 1 calc R . . C32 C 0.5643(4) -0.0858(9) -0.0774(4) 0.067(2) Uani 1 1 d . . . H32A H 0.5138 -0.0733 -0.0713 0.080 Uiso 1 1 calc R . . C33 C 0.6139(3) -0.0904(9) -0.0275(3) 0.0573(17) Uani 1 1 d . . . H33A H 0.5971 -0.0823 0.0122 0.069 Uiso 1 1 calc R . . O1T O 1.0891(4) -0.2137(7) 0.1240(3) 0.0938(19) Uani 1 1 d . . . C1T C 1.1101(5) -0.1193(10) 0.1718(4) 0.085(3) Uani 1 1 d . . . H1TA H 1.1376 -0.0247 0.1579 0.102 Uiso 1 1 calc R . . H1TB H 1.1422 -0.1813 0.2006 0.102 Uiso 1 1 calc R . . C2T C 1.0439(6) -0.0639(13) 0.2022(4) 0.103(4) Uani 1 1 d . . . H2TA H 1.0547 -0.0410 0.2456 0.124 Uiso 1 1 calc R . . H2TB H 1.0218 0.0327 0.1823 0.124 Uiso 1 1 calc R . . C3T C 0.9976(6) -0.2068(17) 0.1933(6) 0.119(4) Uani 1 1 d . . . H3TA H 0.9453 -0.1772 0.1938 0.143 Uiso 1 1 calc R . . H3TB H 1.0087 -0.2878 0.2253 0.143 Uiso 1 1 calc R . . C4T C 1.0155(6) -0.2729(12) 0.1314(5) 0.099(3) Uani 1 1 d . . . H4TA H 1.0140 -0.3925 0.1309 0.119 Uiso 1 1 calc R . . H4TB H 0.9811 -0.2310 0.0992 0.119 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0343(4) 0.0316(4) 0.0383(4) -0.0008(3) 0.0039(3) 0.0009(3) P1 0.0379(7) 0.0363(8) 0.0498(8) 0.0029(7) 0.0081(7) 0.0023(6) P2 0.0329(7) 0.0340(7) 0.0378(7) -0.0022(6) -0.0002(6) 0.0036(6) O1 0.045(2) 0.036(2) 0.063(3) -0.0012(19) -0.011(2) 0.0017(18) O2 0.095(4) 0.054(3) 0.119(5) -0.035(3) -0.044(4) 0.018(3) O3 0.053(2) 0.047(3) 0.063(3) 0.007(2) 0.008(2) 0.007(2) N1 0.039(3) 0.034(3) 0.049(3) -0.004(2) 0.001(2) -0.002(2) C1 0.039(3) 0.039(3) 0.051(3) -0.001(3) 0.003(3) -0.003(2) C2 0.047(3) 0.046(4) 0.047(3) -0.006(3) -0.007(3) 0.001(3) C3 0.054(4) 0.038(4) 0.067(4) -0.016(3) -0.002(3) -0.003(3) C4 0.072(5) 0.121(8) 0.099(6) 0.067(6) 0.039(5) 0.051(5) C5 0.097(7) 0.178(11) 0.157(10) 0.115(9) 0.062(7) 0.099(8) C6 0.094(6) 0.075(5) 0.068(5) 0.022(4) 0.003(5) 0.048(5) C7 0.105(6) 0.063(5) 0.043(4) 0.017(3) -0.002(4) 0.006(4) C8 0.061(4) 0.076(5) 0.051(4) 0.020(4) 0.011(3) 0.011(4) C9 0.042(3) 0.039(3) 0.052(3) 0.000(3) 0.015(3) -0.003(3) C10 0.058(4) 0.053(4) 0.063(4) -0.010(3) 0.015(3) 0.010(3) C11 0.077(5) 0.070(5) 0.062(4) -0.019(4) 0.016(4) -0.001(4) C12 0.059(4) 0.088(6) 0.048(4) -0.004(4) 0.007(3) -0.013(4) C13 0.061(4) 0.065(4) 0.054(4) 0.006(4) -0.005(3) -0.002(4) C14 0.053(4) 0.050(4) 0.055(4) -0.001(3) 0.009(3) -0.002(3) C15 0.042(3) 0.040(3) 0.042(3) 0.004(2) -0.006(3) -0.003(2) C16 0.049(4) 0.051(4) 0.059(4) -0.007(3) 0.013(3) -0.008(3) C17 0.060(4) 0.076(6) 0.071(5) -0.010(4) 0.024(4) -0.015(4) C18 0.067(5) 0.085(6) 0.052(4) 0.011(4) 0.002(4) -0.032(4) C19 0.081(6) 0.059(5) 0.118(7) 0.037(5) 0.001(5) -0.005(4) C20 0.050(4) 0.059(5) 0.144(8) 0.031(5) -0.004(5) 0.001(3) C21 0.039(3) 0.037(3) 0.047(3) 0.000(2) 0.005(3) -0.001(2) C22 0.035(3) 0.045(3) 0.033(3) -0.005(2) -0.002(2) 0.009(2) C23 0.053(3) 0.042(3) 0.045(3) -0.003(3) 0.003(3) 0.011(3) C24 0.066(4) 0.061(4) 0.054(4) -0.002(3) 0.002(4) 0.027(4) C25 0.053(4) 0.102(6) 0.053(4) -0.010(4) 0.006(3) 0.032(4) C26 0.039(3) 0.066(4) 0.061(4) -0.002(3) 0.011(3) 0.007(3) C27 0.040(3) 0.053(4) 0.049(3) -0.005(3) 0.001(3) 0.009(3) C28 0.041(3) 0.041(3) 0.046(3) -0.002(2) -0.007(3) 0.008(2) C29 0.059(4) 0.071(5) 0.046(4) -0.011(3) -0.003(3) 0.007(3) C30 0.081(5) 0.078(5) 0.048(4) -0.013(3) -0.010(4) 0.022(4) C31 0.087(6) 0.057(4) 0.075(5) -0.014(4) -0.046(5) 0.015(4) C32 0.050(4) 0.073(5) 0.076(5) -0.016(4) -0.019(4) 0.016(3) C33 0.044(3) 0.069(4) 0.058(4) -0.006(3) -0.006(3) 0.006(3) O1T 0.133(6) 0.070(4) 0.079(4) -0.002(3) 0.021(4) 0.016(4) C1T 0.091(6) 0.066(6) 0.095(6) 0.013(5) -0.015(5) -0.001(4) C2T 0.138(9) 0.100(8) 0.069(5) -0.020(5) -0.016(6) 0.050(7) C3T 0.083(7) 0.149(11) 0.123(9) 0.048(8) -0.024(7) 0.007(7) C4T 0.105(8) 0.079(6) 0.112(8) -0.023(6) -0.008(6) 0.001(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 Ni O1 1.888(4) . ? Ni C1 1.929(6) . ? Ni N1 1.964(5) . ? Ni P2 2.1197(16) . ? P1 O3 1.476(4) . ? P1 C9 1.796(6) . ? P1 C15 1.803(6) . ? P1 C21 1.817(6) . ? P2 C22 1.820(5) . ? P2 C28 1.831(5) . ? P2 C21 1.844(6) . ? O1 C3 1.275(7) . ? O2 C3 1.244(7) . ? N1 C4 1.303(9) . ? N1 C8 1.308(8) . ? C1 C2 1.512(8) . ? C2 C3 1.496(9) . ? C4 C5 1.390(10) . ? C5 C6 1.340(12) . ? C6 C7 1.336(11) . ? C7 C8 1.355(9) . ? C9 C14 1.380(9) . ? C9 C10 1.394(8) . ? C10 C11 1.367(10) . ? C11 C12 1.374(11) . ? C12 C13 1.378(10) . ? C13 C14 1.385(9) . ? C15 C20 1.370(9) . ? C15 C16 1.387(8) . ? C16 C17 1.382(9) . ? C17 C18 1.378(11) . ? C18 C19 1.371(12) . ? C19 C20 1.423(11) . ? C22 C27 1.377(8) . ? C22 C23 1.390(8) . ? C23 C24 1.402(9) . ? C24 C25 1.379(11) . ? C25 C26 1.382(10) . ? C26 C27 1.379(8) . ? C28 C29 1.394(9) . ? C28 C33 1.401(8) . ? C29 C30 1.381(9) . ? C30 C31 1.392(11) . ? C31 C32 1.344(11) . ? C32 C33 1.393(9) . ? O1T C1T 1.357(10) . ? O1T C4T 1.454(12) . ? C1T C2T 1.492(13) . ? C2T C3T 1.464(15) . ? C3T C4T 1.529(16) . ? 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 Ni C1 86.4(2) . . ? O1 Ni N1 85.42(17) . . ? C1 Ni N1 169.4(2) . . ? O1 Ni P2 174.52(13) . . ? C1 Ni P2 89.62(18) . . ? N1 Ni P2 99.00(14) . . ? O3 P1 C9 112.0(3) . . ? O3 P1 C15 110.4(3) . . ? C9 P1 C15 105.3(3) . . ? O3 P1 C21 115.6(3) . . ? C9 P1 C21 108.1(3) . . ? C15 P1 C21 104.7(3) . . ? C22 P2 C28 102.6(2) . . ? C22 P2 C21 103.4(3) . . ? C28 P2 C21 103.6(3) . . ? C22 P2 Ni 115.89(19) . . ? C28 P2 Ni 114.18(19) . . ? C21 P2 Ni 115.48(19) . . ? C3 O1 Ni 116.6(4) . . ? C4 N1 C8 116.2(6) . . ? C4 N1 Ni 119.9(5) . . ? C8 N1 Ni 122.7(4) . . ? C2 C1 Ni 106.7(4) . . ? C3 C2 C1 110.8(5) . . ? O2 C3 O1 123.2(6) . . ? O2 C3 C2 121.9(6) . . ? O1 C3 C2 114.9(5) . . ? N1 C4 C5 122.0(7) . . ? C6 C5 C4 119.8(8) . . ? C7 C6 C5 117.8(7) . . ? C6 C7 C8 119.0(7) . . ? N1 C8 C7 124.8(7) . . ? C14 C9 C10 118.5(6) . . ? C14 C9 P1 124.3(5) . . ? C10 C9 P1 117.2(5) . . ? C11 C10 C9 120.8(7) . . ? C10 C11 C12 120.7(7) . . ? C11 C12 C13 119.0(7) . . ? C12 C13 C14 120.8(7) . . ? C9 C14 C13 120.1(6) . . ? C20 C15 C16 119.0(6) . . ? C20 C15 P1 124.7(5) . . ? C16 C15 P1 116.3(4) . . ? C17 C16 C15 121.1(7) . . ? C16 C17 C18 119.8(7) . . ? C19 C18 C17 120.7(7) . . ? C18 C19 C20 119.0(8) . . ? C15 C20 C19 120.4(8) . . ? P1 C21 P2 114.4(3) . . ? C27 C22 C23 118.9(5) . . ? C27 C22 P2 118.6(4) . . ? C23 C22 P2 122.4(5) . . ? C22 C23 C24 119.1(6) . . ? C25 C24 C23 121.2(7) . . ? C24 C25 C26 119.1(6) . . ? C27 C26 C25 119.8(7) . . ? C22 C27 C26 121.8(6) . . ? C29 C28 C33 118.5(6) . . ? C29 C28 P2 120.8(5) . . ? C33 C28 P2 120.3(5) . . ? C30 C29 C28 120.8(7) . . ? C29 C30 C31 119.5(7) . . ? C32 C31 C30 120.5(6) . . ? C31 C32 C33 121.2(7) . . ? C32 C33 C28 119.6(7) . . ? C1T O1T C4T 109.3(7) . . ? O1T C1T C2T 109.1(8) . . ? C3T C2T C1T 99.9(8) . . ? C2T C3T C4T 105.0(9) . . ? O1T C4T C3T 103.1(8) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.705 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.097