Electronic Supplementary Material for Dalton Transactions This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'H.G. Raubenheimer' _publ_contact_author_address ;Department of Chemistry and Polymer Science University of Stellenbosch Private Bag X1 Matieland 7602 South Africa ; _publ_contact_author_email hgr@sun.ac.za _publ_contact_author_phone '+27 21 808 3850' _publ_contact_author_fax '+27 21 808 3849' _publ_section_title ; A first structural and theoretical comparison of rNHC (remote N-heterocyclic carbene) and NHC complexes of Ni(II) obtained by oxidative substitution ; loop_ _publ_author_name 'Helgard G. Raubenheimer' 'G. Frenking' 'Wolfgang Herrmann' 'Gerrit R. Julius' 'Christoph Loschen' ; S.K.Schneider ; data_7 _database_code_depnum_ccdc_archive 'CCDC 282952' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H37 Cl N Ni P2, 2(C H2 Cl2), B F4' _chemical_formula_sum 'C44 H41 B Cl5 F4 N Ni P2' _chemical_formula_weight 968.49 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 18.114(4) _cell_length_b 21.802(5) _cell_length_c 11.028(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4355.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3812 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 25.88 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7602 _exptl_absorpt_correction_T_max 0.9175 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22684 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4250 _reflns_number_gt 3305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0627P)^2^+12.6339P] 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 4250 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1399 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Ni1 Ni 0.83771(3) 0.7500 0.20617(6) 0.01359(18) Uani 1 2 d S . . P1 P 0.82646(5) 0.64880(4) 0.18606(8) 0.0150(2) Uani 1 1 d . . . Cl1 Cl 0.75286(7) 0.7500 0.34932(11) 0.0193(3) Uani 1 2 d S . . F2 F 0.98115(18) 0.7500 0.5068(3) 0.0319(8) Uani 1 2 d S . . F1 F 0.98733(16) 0.69808(11) 0.6857(2) 0.0394(6) Uani 1 1 d . . . C3 C 1.0615(3) 0.7500 0.1625(5) 0.0229(12) Uani 1 2 d S . . H3 H 1.1025 0.7500 0.2162 0.027 Uiso 1 2 calc SR . . F3 F 0.88316(19) 0.7500 0.6329(3) 0.0412(9) Uani 1 2 d S . . N1 N 0.9431(2) 0.7500 0.0081(4) 0.0193(9) Uani 1 2 d S . . C2 C 0.9909(3) 0.7500 0.2074(5) 0.0209(11) Uani 1 2 d S . . H2 H 0.9833 0.7500 0.2926 0.025 Uiso 1 2 calc SR . . C31 C 0.72858(19) 0.63234(16) 0.1711(3) 0.0172(8) Uani 1 1 d . . . C1 C 0.9288(3) 0.7500 0.1279(5) 0.0188(11) Uani 1 2 d S . . C35 C 0.6156(2) 0.58856(18) 0.2459(4) 0.0268(9) Uani 1 1 d . . . H35 H 0.5903 0.5643 0.3040 0.032 Uiso 1 1 calc R . . C13 C 0.8693(2) 0.56562(18) -0.1423(4) 0.0273(9) Uani 1 1 d . . . H13 H 0.8425 0.5507 -0.2102 0.033 Uiso 1 1 calc R . . C34 C 0.5769(2) 0.61630(19) 0.1535(4) 0.0294(10) Uani 1 1 d . . . H34 H 0.5250 0.6107 0.1476 0.035 Uiso 1 1 calc R . . C11 C 0.8708(2) 0.61190(16) 0.0561(3) 0.0181(8) Uani 1 1 d . . . C26 C 0.88020(19) 0.63200(17) 0.4208(3) 0.0188(8) Uani 1 1 d . . . H26 H 0.8760 0.6752 0.4288 0.023 Uiso 1 1 calc R . . C6 C 0.8823(3) 0.7500 -0.0799(5) 0.0246(12) Uani 1 2 d S . . H6A H 0.8357 0.7418 -0.0378 0.037 Uiso 0.50 1 calc PR . . H6B H 0.8910 0.7181 -0.1408 0.037 Uiso 0.50 1 calc PR . . H6C H 0.8797 0.7901 -0.1198 0.037 Uiso 0.50 1 calc PR . . C21 C 0.86034(19) 0.60339(17) 0.3128(3) 0.0173(8) Uani 1 1 d . . . B1 B 0.9596(4) 0.7500 0.6272(6) 0.0256(14) Uani 1 2 d S . . C22 C 0.8671(2) 0.54011(18) 0.3022(4) 0.0236(8) Uani 1 1 d . . . H22 H 0.8542 0.5206 0.2282 0.028 Uiso 1 1 calc R . . C4 C 1.0725(3) 0.7500 0.0380(5) 0.0243(12) Uani 1 2 d S . . H4 H 1.1213 0.7500 0.0063 0.029 Uiso 1 2 calc SR . . C5 C 1.0138(3) 0.7500 -0.0388(5) 0.0220(12) Uani 1 2 d S . . H5 H 1.0214 0.7500 -0.1240 0.026 Uiso 1 2 calc SR . . C24 C 0.9119(2) 0.53390(19) 0.5060(4) 0.0259(9) Uani 1 1 d . . . H24 H 0.9292 0.5101 0.5723 0.031 Uiso 1 1 calc R . . C15 C 0.9848(2) 0.58514(18) -0.0441(4) 0.0242(9) Uani 1 1 d . . . H15 H 1.0372 0.5833 -0.0439 0.029 Uiso 1 1 calc R . . C36 C 0.6918(2) 0.59598(17) 0.2544(4) 0.0218(8) Uani 1 1 d . . . H36 H 0.7185 0.5761 0.3173 0.026 Uiso 1 1 calc R . . C16 C 0.9477(2) 0.60895(17) 0.0548(3) 0.0214(8) Uani 1 1 d . . . H16 H 0.9749 0.6235 0.1226 0.026 Uiso 1 1 calc R . . C32 C 0.6887(2) 0.66097(18) 0.0785(4) 0.0231(8) Uani 1 1 d . . . H32 H 0.7135 0.6865 0.0218 0.028 Uiso 1 1 calc R . . C14 C 0.9457(2) 0.56403(19) -0.1430(4) 0.0277(9) Uani 1 1 d . . . H14 H 0.9712 0.5484 -0.2117 0.033 Uiso 1 1 calc R . . C12 C 0.8318(2) 0.58886(17) -0.0432(3) 0.0203(8) Uani 1 1 d . . . H12 H 0.7793 0.5891 -0.0426 0.024 Uiso 1 1 calc R . . C23 C 0.8924(2) 0.50534(19) 0.3981(4) 0.0286(9) Uani 1 1 d . . . H23 H 0.8964 0.4621 0.3904 0.034 Uiso 1 1 calc R . . C33 C 0.6131(2) 0.65230(19) 0.0692(4) 0.0272(9) Uani 1 1 d . . . H33 H 0.5863 0.6710 0.0051 0.033 Uiso 1 1 calc R . . C25 C 0.9064(2) 0.59667(18) 0.5173(4) 0.0235(8) Uani 1 1 d . . . H25 H 0.9204 0.6160 0.5910 0.028 Uiso 1 1 calc R . . Cl2 Cl 0.78121(7) 0.43533(7) 0.07937(13) 0.0567(4) Uani 1 1 d . . . Cl3 Cl 0.83712(12) 0.33701(12) 0.22723(16) 0.1120(9) Uani 1 1 d . . . C7 C 0.7683(3) 0.3586(3) 0.1227(5) 0.0643(18) Uani 1 1 d . . . H7B H 0.7708 0.3318 0.0504 0.077 Uiso 1 1 calc R . . H7A H 0.7189 0.3536 0.1601 0.077 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 0.0106(3) 0.0151(3) 0.0151(3) 0.000 0.0007(3) 0.000 P1 0.0117(4) 0.0159(5) 0.0172(5) 0.0003(4) -0.0015(3) 0.0005(3) Cl1 0.0163(6) 0.0202(6) 0.0213(6) 0.000 0.0052(5) 0.000 F2 0.0294(18) 0.040(2) 0.0261(18) 0.000 0.0001(14) 0.000 F1 0.0553(17) 0.0303(14) 0.0327(14) 0.0020(11) -0.0153(12) 0.0032(12) C3 0.017(3) 0.025(3) 0.026(3) 0.000 -0.001(2) 0.000 F3 0.0251(18) 0.071(3) 0.0272(19) 0.000 -0.0012(15) 0.000 N1 0.018(2) 0.021(2) 0.019(2) 0.000 0.0006(18) 0.000 C2 0.018(3) 0.017(3) 0.028(3) 0.000 0.002(2) 0.000 C31 0.0140(17) 0.0168(18) 0.0208(18) -0.0042(15) -0.0011(14) 0.0017(14) C1 0.021(3) 0.016(3) 0.020(3) 0.000 0.005(2) 0.000 C35 0.0189(19) 0.025(2) 0.037(2) -0.0042(18) 0.0062(17) -0.0042(16) C13 0.036(2) 0.025(2) 0.021(2) -0.0035(17) -0.0047(18) 0.0033(18) C34 0.0135(18) 0.032(2) 0.042(3) -0.016(2) -0.0009(18) 0.0028(16) C11 0.0207(18) 0.0160(18) 0.0176(18) 0.0007(15) 0.0015(15) 0.0015(14) C26 0.0160(18) 0.0203(19) 0.0200(19) 0.0023(15) 0.0034(15) -0.0006(14) C6 0.025(3) 0.026(3) 0.022(3) 0.000 -0.003(2) 0.000 C21 0.0103(16) 0.0212(19) 0.0205(19) 0.0035(15) 0.0014(14) 0.0003(14) B1 0.032(4) 0.029(4) 0.015(3) 0.000 -0.002(3) 0.000 C22 0.0256(19) 0.020(2) 0.026(2) -0.0003(16) -0.0033(17) 0.0026(15) C4 0.022(3) 0.026(3) 0.025(3) 0.000 0.004(2) 0.000 C5 0.018(3) 0.022(3) 0.026(3) 0.000 0.006(2) 0.000 C24 0.022(2) 0.032(2) 0.023(2) 0.0107(18) -0.0005(16) 0.0045(17) C15 0.0202(19) 0.024(2) 0.029(2) -0.0030(17) 0.0059(16) 0.0038(16) C36 0.0180(18) 0.0188(19) 0.029(2) -0.0013(16) -0.0006(16) 0.0013(15) C16 0.0204(18) 0.0207(19) 0.023(2) -0.0022(16) -0.0022(15) -0.0001(15) C32 0.0191(18) 0.025(2) 0.025(2) -0.0033(17) -0.0043(16) 0.0030(16) C14 0.031(2) 0.026(2) 0.025(2) -0.0032(18) 0.0067(18) 0.0049(17) C12 0.0197(18) 0.0188(19) 0.023(2) -0.0009(15) -0.0029(16) 0.0002(15) C23 0.031(2) 0.021(2) 0.034(2) 0.0028(18) 0.0005(19) 0.0062(17) C33 0.0207(19) 0.028(2) 0.032(2) -0.0078(18) -0.0074(17) 0.0084(17) C25 0.0194(19) 0.031(2) 0.0202(19) 0.0005(17) -0.0010(16) 0.0022(16) Cl2 0.0426(7) 0.0769(10) 0.0507(8) -0.0228(7) -0.0095(6) -0.0117(7) Cl3 0.1179(17) 0.165(2) 0.0529(10) -0.0163(12) -0.0301(10) 0.0928(16) C7 0.076(4) 0.075(4) 0.041(3) -0.020(3) -0.020(3) 0.042(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 C1 1.861(5) . ? Ni1 Cl1 2.2034(14) . ? Ni1 P1 2.2268(10) 8_575 ? Ni1 P1 2.2268(10) . ? P1 C31 1.817(4) . ? P1 C21 1.820(4) . ? P1 C11 1.829(4) . ? F2 B1 1.383(7) . ? F1 B1 1.396(4) . ? C3 C2 1.372(7) . ? C3 C4 1.388(8) . ? C3 H3 0.9500 . ? F3 B1 1.387(8) . ? N1 C1 1.347(7) . ? N1 C5 1.382(7) . ? N1 C6 1.467(7) . ? C2 C1 1.427(7) . ? C2 H2 0.9500 . ? C31 C36 1.384(5) . ? C31 C32 1.397(5) . ? C35 C34 1.377(6) . ? C35 C36 1.393(5) . ? C35 H35 0.9500 . ? C13 C12 1.383(5) . ? C13 C14 1.384(6) . ? C13 H13 0.9500 . ? C34 C33 1.383(6) . ? C34 H34 0.9500 . ? C11 C16 1.395(5) . ? C11 C12 1.396(5) . ? C26 C21 1.392(5) . ? C26 C25 1.396(5) . ? C26 H26 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C21 C22 1.390(5) . ? B1 F1 1.396(4) 8_575 ? C22 C23 1.379(5) . ? C22 H22 0.9500 . ? C4 C5 1.359(8) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C24 C25 1.378(6) . ? C24 C23 1.389(6) . ? C24 H24 0.9500 . ? C15 C14 1.380(6) . ? C15 C16 1.382(5) . ? C15 H15 0.9500 . ? C36 H36 0.9500 . ? C16 H16 0.9500 . ? C32 C33 1.386(5) . ? C32 H32 0.9500 . ? C14 H14 0.9500 . ? C12 H12 0.9500 . ? C23 H23 0.9500 . ? C33 H33 0.9500 . ? C25 H25 0.9500 . ? Cl2 C7 1.756(7) . ? Cl3 C7 1.762(5) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 Cl1 161.85(17) . . ? C1 Ni1 P1 92.00(4) . 8_575 ? Cl1 Ni1 P1 90.43(3) . 8_575 ? C1 Ni1 P1 92.00(4) . . ? Cl1 Ni1 P1 90.43(3) . . ? P1 Ni1 P1 164.45(5) 8_575 . ? C31 P1 C21 106.95(17) . . ? C31 P1 C11 105.68(17) . . ? C21 P1 C11 102.40(16) . . ? C31 P1 Ni1 107.10(12) . . ? C21 P1 Ni1 115.57(13) . . ? C11 P1 Ni1 118.28(12) . . ? C2 C3 C4 119.4(5) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C1 N1 C5 123.1(5) . . ? C1 N1 C6 120.3(4) . . ? C5 N1 C6 116.6(4) . . ? C3 C2 C1 121.0(5) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C36 C31 C32 119.5(3) . . ? C36 C31 P1 121.5(3) . . ? C32 C31 P1 118.8(3) . . ? N1 C1 C2 116.8(5) . . ? N1 C1 Ni1 128.7(4) . . ? C2 C1 Ni1 114.5(4) . . ? C34 C35 C36 120.3(4) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C12 C13 C14 120.3(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C35 C34 C33 120.3(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C16 C11 C12 118.7(3) . . ? C16 C11 P1 117.8(3) . . ? C12 C11 P1 123.4(3) . . ? C21 C26 C25 119.5(4) . . ? C21 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C22 C21 C26 119.6(3) . . ? C22 C21 P1 120.3(3) . . ? C26 C21 P1 120.0(3) . . ? F2 B1 F3 109.0(5) . . ? F2 B1 F1 110.1(3) . 8_575 ? F3 B1 F1 109.7(4) . 8_575 ? F2 B1 F1 110.1(3) . . ? F3 B1 F1 109.7(4) . . ? F1 B1 F1 108.3(5) 8_575 . ? C23 C22 C21 120.7(4) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 N1 119.5(5) . . ? C4 C5 H5 120.2 . . ? N1 C5 H5 120.2 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C14 C15 C16 120.0(4) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C31 C36 C35 119.9(4) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C15 C16 C11 120.8(4) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C33 C32 C31 120.2(4) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C15 C14 C13 120.0(4) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C22 C23 C24 119.7(4) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C34 C33 C32 119.8(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C24 C25 C26 120.3(4) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? Cl2 C7 Cl3 109.8(4) . . ? Cl2 C7 H7B 109.7 . . ? Cl3 C7 H7B 109.7 . . ? Cl2 C7 H7A 109.7 . . ? Cl3 C7 H7A 109.7 . . ? H7B C7 H7A 108.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ni1 P1 C31 -148.3(2) . . . . ? Cl1 Ni1 P1 C31 49.71(13) . . . . ? P1 Ni1 P1 C31 -43.5(3) 8_575 . . . ? C1 Ni1 P1 C21 92.7(2) . . . . ? Cl1 Ni1 P1 C21 -69.32(13) . . . . ? P1 Ni1 P1 C21 -162.5(2) 8_575 . . . ? C1 Ni1 P1 C11 -29.2(2) . . . . ? Cl1 Ni1 P1 C11 168.83(14) . . . . ? P1 Ni1 P1 C11 75.7(3) 8_575 . . . ? C4 C3 C2 C1 0.0 . . . . ? C21 P1 C31 C36 5.7(4) . . . . ? C11 P1 C31 C36 114.3(3) . . . . ? Ni1 P1 C31 C36 -118.7(3) . . . . ? C21 P1 C31 C32 -179.2(3) . . . . ? C11 P1 C31 C32 -70.6(3) . . . . ? Ni1 P1 C31 C32 56.3(3) . . . . ? C5 N1 C1 C2 0.0 . . . . ? C6 N1 C1 C2 180.0 . . . . ? C5 N1 C1 Ni1 180.0 . . . . ? C6 N1 C1 Ni1 0.0 . . . . ? C3 C2 C1 N1 0.0 . . . . ? C3 C2 C1 Ni1 180.0 . . . . ? Cl1 Ni1 C1 N1 180.000(2) . . . . ? P1 Ni1 C1 N1 -82.49(3) 8_575 . . . ? P1 Ni1 C1 N1 82.49(3) . . . . ? Cl1 Ni1 C1 C2 0.000(3) . . . . ? P1 Ni1 C1 C2 97.51(3) 8_575 . . . ? P1 Ni1 C1 C2 -97.51(3) . . . . ? C36 C35 C34 C33 -0.7(6) . . . . ? C31 P1 C11 C16 -170.1(3) . . . . ? C21 P1 C11 C16 -58.3(3) . . . . ? Ni1 P1 C11 C16 70.0(3) . . . . ? C31 P1 C11 C12 12.4(4) . . . . ? C21 P1 C11 C12 124.3(3) . . . . ? Ni1 P1 C11 C12 -107.4(3) . . . . ? C25 C26 C21 C22 -0.3(5) . . . . ? C25 C26 C21 P1 -179.8(3) . . . . ? C31 P1 C21 C22 71.3(3) . . . . ? C11 P1 C21 C22 -39.6(3) . . . . ? Ni1 P1 C21 C22 -169.6(3) . . . . ? C31 P1 C21 C26 -109.2(3) . . . . ? C11 P1 C21 C26 139.9(3) . . . . ? Ni1 P1 C21 C26 9.9(3) . . . . ? C26 C21 C22 C23 0.9(6) . . . . ? P1 C21 C22 C23 -179.7(3) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 N1 0.0 . . . . ? C1 N1 C5 C4 0.0 . . . . ? C6 N1 C5 C4 180.0 . . . . ? C32 C31 C36 C35 -0.4(6) . . . . ? P1 C31 C36 C35 174.6(3) . . . . ? C34 C35 C36 C31 1.3(6) . . . . ? C14 C15 C16 C11 0.1(6) . . . . ? C12 C11 C16 C15 1.6(6) . . . . ? P1 C11 C16 C15 -175.9(3) . . . . ? C36 C31 C32 C33 -0.9(6) . . . . ? P1 C31 C32 C33 -176.1(3) . . . . ? C16 C15 C14 C13 -1.3(6) . . . . ? C12 C13 C14 C15 0.6(6) . . . . ? C14 C13 C12 C11 1.1(6) . . . . ? C16 C11 C12 C13 -2.2(6) . . . . ? P1 C11 C12 C13 175.2(3) . . . . ? C21 C22 C23 C24 -0.6(6) . . . . ? C25 C24 C23 C22 -0.2(6) . . . . ? C35 C34 C33 C32 -0.6(6) . . . . ? C31 C32 C33 C34 1.5(6) . . . . ? C23 C24 C25 C26 0.8(6) . . . . ? C21 C26 C25 C24 -0.5(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.838 _refine_diff_density_min -1.222 _refine_diff_density_rms 0.094 # Attachment 'Complex 8.CIF' data_8 _database_code_depnum_ccdc_archive 'CCDC 282953' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H37 Cl N Ni P2, 1.5(C H2 Cl2), B F4' _chemical_formula_sum 'C43.50 H40 B Cl4 F4 N Ni P2' _chemical_formula_weight 926.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.7256(12) _cell_length_b 19.822(3) _cell_length_c 21.939(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.392(3) _cell_angle_gamma 90.00 _cell_volume 4225.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1334 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 18.27 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.456 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6469 _exptl_absorpt_correction_T_max 0.9208 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22008 _diffrn_reflns_av_R_equivalents 0.0918 _diffrn_reflns_av_sigmaI/netI 0.1115 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.06 _reflns_number_total 7474 _reflns_number_gt 4667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0605P)^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 7474 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1544 _refine_ls_wR_factor_gt 0.1339 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Ni1 Ni 0.81147(6) 0.24285(3) 0.18004(3) 0.02083(19) Uani 1 1 d . . . P1 P 0.81192(13) 0.24203(7) 0.07879(6) 0.0231(3) Uani 1 1 d . . . P2 P 0.84722(13) 0.25374(6) 0.28045(6) 0.0219(3) Uani 1 1 d . . . Cl1 Cl 0.90361(13) 0.14053(6) 0.18308(6) 0.0299(3) Uani 1 1 d . . . C1 C 0.7224(5) 0.3261(2) 0.1774(2) 0.0194(11) Uani 1 1 d . . . N1 N 0.5916(4) 0.4509(2) 0.1742(2) 0.0274(11) Uani 1 1 d . . . C11 C 0.7529(5) 0.3182(2) 0.0392(2) 0.0190(11) Uani 1 1 d . . . C56 C 1.0764(5) 0.1952(2) 0.3442(2) 0.0221(12) Uani 1 1 d . . . H56 H 1.0126 0.1688 0.3656 0.027 Uiso 1 1 calc R . . C15 C 0.7894(5) 0.4279(3) -0.0046(2) 0.0291(13) Uani 1 1 d . . . H15 H 0.8508 0.4616 -0.0178 0.035 Uiso 1 1 calc R . . C14 C 0.6497(5) 0.4390(2) -0.0092(2) 0.0252(12) Uani 1 1 d . . . H14 H 0.6153 0.4804 -0.0255 0.030 Uiso 1 1 calc R . . C21 C 0.7054(5) 0.1779(2) 0.0397(3) 0.0262(13) Uani 1 1 d . . . C13 C 0.5589(5) 0.3901(3) 0.0098(2) 0.0264(13) Uani 1 1 d . . . H13 H 0.4623 0.3974 0.0061 0.032 Uiso 1 1 calc R . . C62 C 0.6659(5) 0.1471(2) 0.2972(3) 0.0261(13) Uani 1 1 d . . . H62 H 0.6596 0.1443 0.2540 0.031 Uiso 1 1 calc R . . C63 C 0.5896(5) 0.1036(3) 0.3320(3) 0.0299(14) Uani 1 1 d . . . H63 H 0.5300 0.0717 0.3122 0.036 Uiso 1 1 calc R . . C66 C 0.7585(5) 0.1979(3) 0.3893(3) 0.0342(14) Uani 1 1 d . . . H66 H 0.8153 0.2308 0.4092 0.041 Uiso 1 1 calc R . . C26 C 0.6316(5) 0.1316(2) 0.0721(2) 0.0251(12) Uani 1 1 d . . . H26 H 0.6442 0.1289 0.1152 0.030 Uiso 1 1 calc R . . C61 C 0.7518(5) 0.1948(2) 0.3259(2) 0.0228(12) Uani 1 1 d . . . C51 C 1.0294(5) 0.2414(2) 0.3003(2) 0.0215(11) Uani 1 1 d . . . C2 C 0.5808(5) 0.3331(3) 0.1853(2) 0.0283(13) Uani 1 1 d . . . H2 H 0.5268 0.2940 0.1915 0.034 Uiso 1 1 calc R . . C41 C 0.8052(6) 0.3361(3) 0.3131(3) 0.0322(14) Uani 1 1 d . . . C55 C 1.2173(5) 0.1877(3) 0.3566(2) 0.0293(13) Uani 1 1 d . . . H55 H 1.2493 0.1556 0.3860 0.035 Uiso 1 1 calc R . . C33 C 1.2281(5) 0.2619(3) 0.0779(3) 0.0358(14) Uani 1 1 d . . . H33 H 1.2950 0.2889 0.0992 0.043 Uiso 1 1 calc R . . C5 C 0.7926(5) 0.3864(2) 0.1674(2) 0.0211(12) Uani 1 1 d . . . H5 H 0.8888 0.3850 0.1616 0.025 Uiso 1 1 calc R . . C32 C 1.0899(5) 0.2700(3) 0.0883(3) 0.0310(13) Uani 1 1 d . . . H32 H 1.0623 0.3033 0.1165 0.037 Uiso 1 1 calc R . . C4 C 0.7280(5) 0.4468(2) 0.1659(2) 0.0269(13) Uani 1 1 d . . . H4 H 0.7791 0.4867 0.1589 0.032 Uiso 1 1 calc R . . C12 C 0.6113(5) 0.3307(3) 0.0340(2) 0.0254(13) Uani 1 1 d . . . H12 H 0.5494 0.2973 0.0475 0.030 Uiso 1 1 calc R . . C22 C 0.6878(6) 0.1807(3) -0.0236(2) 0.0339(14) Uani 1 1 d . . . H22 H 0.7381 0.2124 -0.0463 0.041 Uiso 1 1 calc R . . C31 C 0.9899(5) 0.2300(2) 0.0583(2) 0.0270(13) Uani 1 1 d . . . C36 C 1.0306(6) 0.1833(3) 0.0164(3) 0.0441(17) Uani 1 1 d . . . H36 H 0.9640 0.1571 -0.0059 0.053 Uiso 1 1 calc R . . C46 C 0.6730(7) 0.3475(3) 0.3313(3) 0.053(2) Uani 1 1 d . . . H46 H 0.6100 0.3109 0.3322 0.064 Uiso 1 1 calc R . . C16 C 0.8410(5) 0.3677(3) 0.0194(2) 0.0246(12) Uani 1 1 d . . . H16 H 0.9376 0.3605 0.0223 0.029 Uiso 1 1 calc R . . C34 C 1.2684(6) 0.2141(3) 0.0361(3) 0.0388(15) Uani 1 1 d . . . H34 H 1.3630 0.2086 0.0281 0.047 Uiso 1 1 calc R . . C64 C 0.5990(5) 0.1060(3) 0.3946(3) 0.0336(14) Uani 1 1 d . . . H64 H 0.5480 0.0752 0.4180 0.040 Uiso 1 1 calc R . . C65 C 0.6842(6) 0.1539(3) 0.4236(3) 0.0393(16) Uani 1 1 d . . . H65 H 0.6908 0.1562 0.4669 0.047 Uiso 1 1 calc R . . C54 C 1.3099(6) 0.2263(3) 0.3269(3) 0.0433(17) Uani 1 1 d . . . H54 H 1.4057 0.2217 0.3362 0.052 Uiso 1 1 calc R . . C35 C 1.1709(6) 0.1748(3) 0.0066(3) 0.0498(18) Uani 1 1 d . . . H35 H 1.1989 0.1410 -0.0210 0.060 Uiso 1 1 calc R . . C23 C 0.5968(6) 0.1371(3) -0.0532(3) 0.0418(16) Uani 1 1 d . . . H23 H 0.5862 0.1381 -0.0964 0.050 Uiso 1 1 calc R . . C24 C 0.5214(6) 0.0920(3) -0.0204(3) 0.0380(16) Uani 1 1 d . . . H24 H 0.4571 0.0630 -0.0409 0.046 Uiso 1 1 calc R . . C6 C 0.5271(6) 0.5188(3) 0.1747(3) 0.0504(18) Uani 1 1 d . . . H6A H 0.5536 0.5418 0.2129 0.076 Uiso 1 1 calc R . . H6B H 0.4267 0.5140 0.1715 0.076 Uiso 1 1 calc R . . H6C H 0.5582 0.5452 0.1402 0.076 Uiso 1 1 calc R . . C44 C 0.7212(12) 0.4651(4) 0.3462(4) 0.091(4) Uani 1 1 d . . . H44 H 0.6933 0.5090 0.3580 0.109 Uiso 1 1 calc R . . C45 C 0.6298(8) 0.4120(4) 0.3485(4) 0.081(3) Uani 1 1 d . . . H45 H 0.5390 0.4190 0.3614 0.097 Uiso 1 1 calc R . . C3 C 0.5192(5) 0.3946(3) 0.1842(3) 0.0335(14) Uani 1 1 d . . . H3 H 0.4234 0.3979 0.1906 0.040 Uiso 1 1 calc R . . C42 C 0.8953(7) 0.3907(3) 0.3111(3) 0.0498(19) Uani 1 1 d . . . H42 H 0.9868 0.3839 0.2988 0.060 Uiso 1 1 calc R . . C52 C 1.1250(6) 0.2780(3) 0.2686(3) 0.0408(16) Uani 1 1 d . . . H52 H 1.0951 0.3075 0.2366 0.049 Uiso 1 1 calc R . . C25 C 0.5393(5) 0.0893(3) 0.0414(3) 0.0326(14) Uani 1 1 d . . . H25 H 0.4876 0.0578 0.0638 0.039 Uiso 1 1 calc R . . F1 F 0.1635(3) 0.40349(16) 0.17722(15) 0.0434(9) Uani 1 1 d . . . F4 F 0.1980(3) 0.51428(16) 0.15522(18) 0.0531(10) Uani 1 1 d . . . F3 F 0.0442(3) 0.45413(16) 0.09862(17) 0.0501(10) Uani 1 1 d . . . F2 F 0.2731(3) 0.43298(16) 0.09223(16) 0.0455(9) Uani 1 1 d . . . B1 B 0.1693(6) 0.4507(3) 0.1305(4) 0.0396(19) Uani 1 1 d . . . Cl2 Cl 0.38545(17) 0.12607(10) 0.18307(8) 0.0607(5) Uani 1 1 d . . . Cl3 Cl 0.2288(3) 0.00191(15) 0.18209(16) 0.1365(12) Uani 1 1 d . . . Cl4 Cl 0.8178(5) 0.0054(3) -0.0208(3) 0.0767(15) Uani 0.50 1 d P A -1 C53 C 1.2636(6) 0.2715(3) 0.2837(3) 0.0491(18) Uani 1 1 d . . . H53 H 1.3279 0.2990 0.2637 0.059 Uiso 1 1 calc R . . C43 C 0.8524(10) 0.4549(3) 0.3270(3) 0.074(3) Uani 1 1 d . . . H43 H 0.9139 0.4920 0.3246 0.088 Uiso 1 1 calc R . . C8 C 0.2455(7) 0.0840(4) 0.2108(5) 0.090(3) Uani 1 1 d . . . H8B H 0.1607 0.1097 0.1998 0.108 Uiso 1 1 calc R . . H8A H 0.2551 0.0821 0.2558 0.108 Uiso 1 1 calc R . . C7 C 0.9734(16) -0.0232(9) -0.0492(8) 0.103(7) Uani 0.50 1 d P A -1 H7A H 0.9612 -0.0700 -0.0642 0.124 Uiso 0.50 1 calc PR A -1 H7B H 0.9977 0.0054 -0.0842 0.124 Uiso 0.50 1 calc PR A -1 Cl5 Cl 1.1060(5) -0.0213(2) 0.0049(3) 0.0865(19) Uani 0.50 1 d P A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0222(3) 0.0134(3) 0.0266(4) 0.0035(3) -0.0027(3) 0.0011(3) P1 0.0237(7) 0.0172(7) 0.0281(8) 0.0009(6) -0.0014(6) 0.0043(6) P2 0.0225(7) 0.0146(7) 0.0282(8) 0.0022(6) -0.0037(6) -0.0008(6) Cl1 0.0358(8) 0.0160(7) 0.0370(9) 0.0014(6) -0.0082(7) 0.0062(6) C1 0.017(3) 0.021(3) 0.020(3) 0.001(2) 0.001(2) 0.001(2) N1 0.031(3) 0.024(2) 0.027(3) 0.001(2) -0.005(2) 0.011(2) C11 0.020(3) 0.018(3) 0.020(3) 0.001(2) 0.003(2) 0.006(2) C56 0.024(3) 0.022(3) 0.020(3) 0.000(2) 0.001(2) -0.001(2) C15 0.030(3) 0.025(3) 0.034(4) 0.008(3) 0.015(3) 0.003(2) C14 0.032(3) 0.019(3) 0.025(3) 0.003(2) 0.008(3) 0.008(2) C21 0.030(3) 0.015(3) 0.034(4) -0.003(2) -0.006(3) 0.005(2) C13 0.017(3) 0.033(3) 0.029(3) 0.004(3) -0.005(2) 0.008(2) C62 0.021(3) 0.023(3) 0.034(3) 0.001(3) -0.001(3) 0.001(2) C63 0.021(3) 0.021(3) 0.048(4) 0.000(3) 0.000(3) 0.001(2) C66 0.028(3) 0.041(4) 0.034(4) -0.011(3) 0.010(3) -0.008(3) C26 0.028(3) 0.021(3) 0.025(3) 0.002(2) -0.006(2) 0.008(2) C61 0.017(3) 0.022(3) 0.030(3) 0.000(2) 0.005(2) 0.003(2) C51 0.018(2) 0.019(3) 0.027(3) 0.002(2) -0.001(2) -0.005(2) C2 0.018(3) 0.033(3) 0.034(3) 0.013(3) 0.003(2) 0.000(2) C41 0.041(3) 0.023(3) 0.031(4) -0.004(3) -0.015(3) 0.009(3) C55 0.031(3) 0.031(3) 0.024(3) -0.001(3) -0.009(3) 0.004(3) C33 0.026(3) 0.035(3) 0.046(4) 0.002(3) -0.004(3) 0.009(3) C5 0.019(3) 0.021(3) 0.023(3) 0.000(2) 0.001(2) 0.001(2) C32 0.035(3) 0.025(3) 0.033(3) -0.001(3) 0.003(3) 0.005(2) C4 0.029(3) 0.015(3) 0.036(3) 0.001(2) -0.005(3) 0.001(2) C12 0.022(3) 0.024(3) 0.030(3) 0.000(2) -0.001(2) 0.003(2) C22 0.057(4) 0.020(3) 0.024(3) 0.009(3) -0.011(3) 0.002(3) C31 0.030(3) 0.022(3) 0.029(3) 0.000(2) 0.000(3) 0.006(2) C36 0.033(3) 0.064(4) 0.035(4) -0.019(3) -0.004(3) 0.014(3) C46 0.051(4) 0.039(4) 0.068(5) -0.023(3) -0.026(4) 0.021(3) C16 0.020(3) 0.028(3) 0.025(3) 0.003(2) 0.005(2) 0.006(2) C34 0.027(3) 0.043(4) 0.047(4) 0.012(3) 0.005(3) 0.018(3) C64 0.026(3) 0.035(3) 0.041(4) 0.006(3) 0.020(3) -0.002(3) C65 0.038(3) 0.049(4) 0.032(4) -0.010(3) 0.020(3) -0.002(3) C54 0.018(3) 0.048(4) 0.063(5) -0.015(3) -0.004(3) 0.003(3) C35 0.045(4) 0.062(5) 0.043(4) -0.012(3) 0.005(3) 0.027(4) C23 0.065(4) 0.025(3) 0.033(4) -0.006(3) -0.015(3) 0.004(3) C24 0.049(4) 0.019(3) 0.044(4) -0.007(3) -0.020(3) 0.001(3) C6 0.053(4) 0.034(4) 0.064(5) 0.002(3) -0.006(4) 0.029(3) C44 0.153(9) 0.032(5) 0.081(7) -0.027(4) -0.075(7) 0.032(6) C45 0.082(6) 0.064(6) 0.093(7) -0.037(5) -0.033(5) 0.047(5) C3 0.017(3) 0.048(4) 0.037(4) 0.013(3) 0.009(3) 0.010(3) C42 0.084(5) 0.025(3) 0.038(4) -0.003(3) -0.027(4) -0.005(3) C52 0.032(3) 0.052(4) 0.038(4) 0.019(3) -0.004(3) -0.009(3) C25 0.036(3) 0.017(3) 0.044(4) -0.001(3) -0.003(3) 0.005(2) F1 0.0410(19) 0.037(2) 0.053(2) 0.0179(17) 0.0052(17) -0.0034(16) F4 0.039(2) 0.028(2) 0.092(3) 0.0013(19) 0.006(2) -0.0030(16) F3 0.0239(17) 0.047(2) 0.079(3) 0.0269(19) -0.0072(18) -0.0059(16) F2 0.0372(18) 0.040(2) 0.061(2) 0.0207(17) 0.0189(18) 0.0050(16) B1 0.021(3) 0.020(4) 0.079(6) 0.018(4) 0.009(4) 0.001(3) Cl2 0.0539(10) 0.0780(13) 0.0505(11) 0.0052(10) 0.0063(9) 0.0094(10) Cl3 0.0879(18) 0.112(2) 0.207(3) -0.065(2) -0.014(2) -0.0296(16) Cl4 0.058(3) 0.059(3) 0.115(4) -0.016(3) 0.025(3) 0.014(3) C53 0.028(3) 0.066(5) 0.054(5) 0.016(4) 0.019(3) -0.014(3) C43 0.136(8) 0.026(4) 0.054(5) -0.001(4) -0.047(6) -0.004(5) C8 0.030(4) 0.089(6) 0.153(9) -0.030(6) 0.018(5) 0.005(4) C7 0.081(12) 0.094(14) 0.139(17) 0.073(12) 0.051(12) 0.056(10) Cl5 0.057(3) 0.037(3) 0.167(6) 0.020(3) 0.024(4) 0.012(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 Ni1 C1 1.863(5) . ? Ni1 Cl1 2.2172(13) . ? Ni1 P1 2.2217(16) . ? Ni1 P2 2.2262(15) . ? P1 C31 1.822(5) . ? P1 C11 1.823(5) . ? P1 C21 1.830(5) . ? P2 C61 1.816(5) . ? P2 C51 1.823(5) . ? P2 C41 1.836(5) . ? C1 C5 1.399(6) . ? C1 C2 1.402(6) . ? N1 C3 1.343(7) . ? N1 C4 1.348(6) . ? N1 C6 1.484(6) . ? C11 C16 1.384(7) . ? C11 C12 1.400(6) . ? C56 C51 1.393(7) . ? C56 C55 1.394(7) . ? C56 H56 0.9500 . ? C15 C14 1.376(7) . ? C15 C16 1.389(7) . ? C15 H15 0.9500 . ? C14 C13 1.386(7) . ? C14 H14 0.9500 . ? C21 C26 1.381(7) . ? C21 C22 1.393(7) . ? C13 C12 1.381(7) . ? C13 H13 0.9500 . ? C62 C63 1.385(7) . ? C62 C61 1.394(7) . ? C62 H62 0.9500 . ? C63 C64 1.374(7) . ? C63 H63 0.9500 . ? C66 C65 1.376(7) . ? C66 C61 1.392(7) . ? C66 H66 0.9500 . ? C26 C25 1.383(7) . ? C26 H26 0.9500 . ? C51 C52 1.389(7) . ? C2 C3 1.359(7) . ? C2 H2 0.9500 . ? C41 C46 1.380(8) . ? C41 C42 1.395(8) . ? C55 C54 1.367(8) . ? C55 H55 0.9500 . ? C33 C32 1.382(7) . ? C33 C34 1.387(8) . ? C33 H33 0.9500 . ? C5 C4 1.351(6) . ? C5 H5 0.9500 . ? C32 C31 1.398(7) . ? C32 H32 0.9500 . ? C4 H4 0.9500 . ? C12 H12 0.9500 . ? C22 C23 1.379(7) . ? C22 H22 0.9500 . ? C31 C36 1.375(7) . ? C36 C35 1.400(8) . ? C36 H36 0.9500 . ? C46 C45 1.402(9) . ? C46 H46 0.9500 . ? C16 H16 0.9500 . ? C34 C35 1.369(8) . ? C34 H34 0.9500 . ? C64 C65 1.397(7) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C54 C53 1.368(8) . ? C54 H54 0.9500 . ? C35 H35 0.9500 . ? C23 C24 1.376(8) . ? C23 H23 0.9500 . ? C24 C25 1.362(7) . ? C24 H24 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C44 C43 1.375(12) . ? C44 C45 1.380(12) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C3 H3 0.9500 . ? C42 C43 1.389(9) . ? C42 H42 0.9500 . ? C52 C53 1.380(8) . ? C52 H52 0.9500 . ? C25 H25 0.9500 . ? F1 B1 1.391(7) . ? F4 B1 1.395(8) . ? F3 B1 1.380(7) . ? F2 B1 1.385(7) . ? Cl2 C8 1.728(7) . ? Cl3 C8 1.750(8) . ? Cl4 C7 1.755(15) . ? C53 H53 0.9500 . ? C43 H43 0.9500 . ? C8 H8B 0.9900 . ? C8 H8A 0.9900 . ? C7 Cl5 1.716(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 Cl1 176.14(15) . . ? C1 Ni1 P1 89.78(16) . . ? Cl1 Ni1 P1 90.32(5) . . ? C1 Ni1 P2 89.86(16) . . ? Cl1 Ni1 P2 90.73(5) . . ? P1 Ni1 P2 169.53(6) . . ? C31 P1 C11 105.9(2) . . ? C31 P1 C21 108.6(2) . . ? C11 P1 C21 101.0(2) . . ? C31 P1 Ni1 106.82(18) . . ? C11 P1 Ni1 117.15(17) . . ? C21 P1 Ni1 116.70(19) . . ? C61 P2 C51 107.3(2) . . ? C61 P2 C41 103.3(3) . . ? C51 P2 C41 104.8(2) . . ? C61 P2 Ni1 114.72(18) . . ? C51 P2 Ni1 109.45(17) . . ? C41 P2 Ni1 116.41(18) . . ? C5 C1 C2 115.0(4) . . ? C5 C1 Ni1 122.2(3) . . ? C2 C1 Ni1 122.8(4) . . ? C3 N1 C4 119.8(4) . . ? C3 N1 C6 121.8(5) . . ? C4 N1 C6 118.4(5) . . ? C16 C11 C12 118.0(4) . . ? C16 C11 P1 123.4(4) . . ? C12 C11 P1 118.3(4) . . ? C51 C56 C55 119.7(5) . . ? C51 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C14 C15 C16 120.4(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C14 C13 120.4(5) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C26 C21 C22 119.6(5) . . ? C26 C21 P1 121.1(4) . . ? C22 C21 P1 119.0(4) . . ? C12 C13 C14 118.8(4) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C63 C62 C61 119.9(5) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C64 C63 C62 120.9(5) . . ? C64 C63 H63 119.5 . . ? C62 C63 H63 119.5 . . ? C65 C66 C61 121.0(5) . . ? C65 C66 H66 119.5 . . ? C61 C66 H66 119.5 . . ? C21 C26 C25 119.6(5) . . ? C21 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C66 C61 C62 118.8(5) . . ? C66 C61 P2 121.1(4) . . ? C62 C61 P2 120.0(4) . . ? C52 C51 C56 118.8(5) . . ? C52 C51 P2 118.4(4) . . ? C56 C51 P2 122.7(4) . . ? C3 C2 C1 121.5(5) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C46 C41 C42 118.4(6) . . ? C46 C41 P2 119.0(4) . . ? C42 C41 P2 121.8(5) . . ? C54 C55 C56 120.7(5) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C32 C33 C34 119.5(5) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C4 C5 C1 122.1(5) . . ? C4 C5 H5 119.0 . . ? C1 C5 H5 119.0 . . ? C33 C32 C31 121.2(5) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? N1 C4 C5 120.7(5) . . ? N1 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C13 C12 C11 121.9(5) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C23 C22 C21 119.6(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C36 C31 C32 118.9(5) . . ? C36 C31 P1 123.8(4) . . ? C32 C31 P1 117.3(4) . . ? C31 C36 C35 119.6(6) . . ? C31 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C41 C46 C45 121.4(7) . . ? C41 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C11 C16 C15 120.6(4) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C35 C34 C33 119.5(5) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C63 C64 C65 119.5(5) . . ? C63 C64 H64 120.3 . . ? C65 C64 H64 120.3 . . ? C66 C65 C64 119.8(6) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C55 C54 C53 119.5(5) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C34 C35 C36 121.3(6) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C24 C23 C22 120.4(6) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 119.8(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C43 C44 C45 120.4(7) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? C44 C45 C46 119.0(8) . . ? C44 C45 H45 120.5 . . ? C46 C45 H45 120.5 . . ? N1 C3 C2 121.0(5) . . ? N1 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C43 C42 C41 120.5(7) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C53 C52 C51 120.0(5) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C24 C25 C26 120.9(5) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? F3 B1 F2 110.8(6) . . ? F3 B1 F1 110.1(5) . . ? F2 B1 F1 109.2(5) . . ? F3 B1 F4 108.1(5) . . ? F2 B1 F4 109.0(5) . . ? F1 B1 F4 109.6(6) . . ? C54 C53 C52 121.2(6) . . ? C54 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? C44 C43 C42 120.3(8) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? Cl2 C8 Cl3 112.6(4) . . ? Cl2 C8 H8B 109.1 . . ? Cl3 C8 H8B 109.1 . . ? Cl2 C8 H8A 109.1 . . ? Cl3 C8 H8A 109.1 . . ? H8B C8 H8A 107.8 . . ? Cl5 C7 Cl4 112.4(11) . . ? Cl5 C7 H7A 109.1 . . ? Cl4 C7 H7A 109.1 . . ? Cl5 C7 H7B 109.1 . . ? Cl4 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ni1 P1 C31 125.4(2) . . . . ? Cl1 Ni1 P1 C31 -58.48(18) . . . . ? P2 Ni1 P1 C31 37.3(4) . . . . ? C1 Ni1 P1 C11 6.9(2) . . . . ? Cl1 Ni1 P1 C11 -176.94(18) . . . . ? P2 Ni1 P1 C11 -81.2(4) . . . . ? C1 Ni1 P1 C21 -113.0(2) . . . . ? Cl1 Ni1 P1 C21 63.16(18) . . . . ? P2 Ni1 P1 C21 159.0(3) . . . . ? C1 Ni1 P2 C61 112.0(2) . . . . ? Cl1 Ni1 P2 C61 -64.18(18) . . . . ? P1 Ni1 P2 C61 -159.9(3) . . . . ? C1 Ni1 P2 C51 -127.4(2) . . . . ? Cl1 Ni1 P2 C51 56.41(17) . . . . ? P1 Ni1 P2 C51 -39.3(4) . . . . ? C1 Ni1 P2 C41 -8.8(3) . . . . ? Cl1 Ni1 P2 C41 175.0(2) . . . . ? P1 Ni1 P2 C41 79.3(4) . . . . ? Cl1 Ni1 C1 C5 -170(2) . . . . ? P1 Ni1 C1 C5 -78.4(4) . . . . ? P2 Ni1 C1 C5 91.1(4) . . . . ? Cl1 Ni1 C1 C2 10(3) . . . . ? P1 Ni1 C1 C2 101.6(4) . . . . ? P2 Ni1 C1 C2 -88.9(4) . . . . ? C31 P1 C11 C16 -22.4(5) . . . . ? C21 P1 C11 C16 -135.6(4) . . . . ? Ni1 P1 C11 C16 96.5(4) . . . . ? C31 P1 C11 C12 164.3(4) . . . . ? C21 P1 C11 C12 51.1(4) . . . . ? Ni1 P1 C11 C12 -76.8(4) . . . . ? C16 C15 C14 C13 -0.3(8) . . . . ? C31 P1 C21 C26 119.2(4) . . . . ? C11 P1 C21 C26 -129.7(4) . . . . ? Ni1 P1 C21 C26 -1.5(5) . . . . ? C31 P1 C21 C22 -67.6(5) . . . . ? C11 P1 C21 C22 43.5(5) . . . . ? Ni1 P1 C21 C22 171.7(4) . . . . ? C15 C14 C13 C12 0.8(8) . . . . ? C61 C62 C63 C64 -1.1(7) . . . . ? C22 C21 C26 C25 -1.1(7) . . . . ? P1 C21 C26 C25 172.1(4) . . . . ? C65 C66 C61 C62 1.3(8) . . . . ? C65 C66 C61 P2 178.8(4) . . . . ? C63 C62 C61 C66 -0.3(7) . . . . ? C63 C62 C61 P2 -177.8(4) . . . . ? C51 P2 C61 C66 61.5(5) . . . . ? C41 P2 C61 C66 -49.0(5) . . . . ? Ni1 P2 C61 C66 -176.7(4) . . . . ? C51 P2 C61 C62 -121.0(4) . . . . ? C41 P2 C61 C62 128.5(4) . . . . ? Ni1 P2 C61 C62 0.8(4) . . . . ? C55 C56 C51 C52 1.7(8) . . . . ? C55 C56 C51 P2 179.3(4) . . . . ? C61 P2 C51 C52 176.0(4) . . . . ? C41 P2 C51 C52 -74.6(5) . . . . ? Ni1 P2 C51 C52 51.0(5) . . . . ? C61 P2 C51 C56 -1.6(5) . . . . ? C41 P2 C51 C56 107.8(5) . . . . ? Ni1 P2 C51 C56 -126.6(4) . . . . ? C5 C1 C2 C3 -1.1(8) . . . . ? Ni1 C1 C2 C3 178.8(4) . . . . ? C61 P2 C41 C46 -38.4(5) . . . . ? C51 P2 C41 C46 -150.6(5) . . . . ? Ni1 P2 C41 C46 88.3(5) . . . . ? C61 P2 C41 C42 152.2(5) . . . . ? C51 P2 C41 C42 40.0(5) . . . . ? Ni1 P2 C41 C42 -81.1(5) . . . . ? C51 C56 C55 C54 1.2(8) . . . . ? C2 C1 C5 C4 0.4(7) . . . . ? Ni1 C1 C5 C4 -179.6(4) . . . . ? C34 C33 C32 C31 1.1(8) . . . . ? C3 N1 C4 C5 0.2(8) . . . . ? C6 N1 C4 C5 177.4(5) . . . . ? C1 C5 C4 N1 0.1(8) . . . . ? C14 C13 C12 C11 -0.8(8) . . . . ? C16 C11 C12 C13 0.3(8) . . . . ? P1 C11 C12 C13 173.9(4) . . . . ? C26 C21 C22 C23 0.0(8) . . . . ? P1 C21 C22 C23 -173.4(4) . . . . ? C33 C32 C31 C36 -1.9(8) . . . . ? C33 C32 C31 P1 176.7(4) . . . . ? C11 P1 C31 C36 -103.1(5) . . . . ? C21 P1 C31 C36 4.7(6) . . . . ? Ni1 P1 C31 C36 131.3(5) . . . . ? C11 P1 C31 C32 78.4(5) . . . . ? C21 P1 C31 C32 -173.8(4) . . . . ? Ni1 P1 C31 C32 -47.1(4) . . . . ? C32 C31 C36 C35 2.7(9) . . . . ? P1 C31 C36 C35 -175.8(5) . . . . ? C42 C41 C46 C45 -1.1(10) . . . . ? P2 C41 C46 C45 -170.9(5) . . . . ? C12 C11 C16 C15 0.3(8) . . . . ? P1 C11 C16 C15 -173.1(4) . . . . ? C14 C15 C16 C11 -0.2(8) . . . . ? C32 C33 C34 C35 -1.1(9) . . . . ? C62 C63 C64 C65 1.5(8) . . . . ? C61 C66 C65 C64 -0.9(8) . . . . ? C63 C64 C65 C66 -0.5(8) . . . . ? C56 C55 C54 C53 -1.4(9) . . . . ? C33 C34 C35 C36 2.0(10) . . . . ? C31 C36 C35 C34 -2.8(10) . . . . ? C21 C22 C23 C24 1.5(8) . . . . ? C22 C23 C24 C25 -1.7(9) . . . . ? C43 C44 C45 C46 0.4(12) . . . . ? C41 C46 C45 C44 0.9(11) . . . . ? C4 N1 C3 C2 -1.0(8) . . . . ? C6 N1 C3 C2 -178.1(5) . . . . ? C1 C2 C3 N1 1.5(9) . . . . ? C46 C41 C42 C43 -0.1(9) . . . . ? P2 C41 C42 C43 169.4(5) . . . . ? C56 C51 C52 C53 -4.3(9) . . . . ? P2 C51 C52 C53 178.0(5) . . . . ? C23 C24 C25 C26 0.6(8) . . . . ? C21 C26 C25 C24 0.9(8) . . . . ? C55 C54 C53 C52 -1.3(10) . . . . ? C51 C52 C53 C54 4.3(10) . . . . ? C45 C44 C43 C42 -1.6(12) . . . . ? C41 C42 C43 C44 1.4(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.800 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.090 # Attachment 'Complex 9.CIF' data_9 _database_code_depnum_ccdc_archive 'CCDC 282954' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H41 Cl N Ni O P2, 2(C H2 Cl2), B F4' _chemical_formula_sum 'C49 H45 B Cl5 F4 N Ni O P2' _chemical_formula_weight 1048.57 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8783(9) _cell_length_b 19.9993(16) _cell_length_c 22.3327(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4858.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1358 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 20.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6287 _exptl_absorpt_correction_T_max 0.9249 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25905 _diffrn_reflns_av_R_equivalents 0.1096 _diffrn_reflns_av_sigmaI/netI 0.0801 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.68 _reflns_number_total 4735 _reflns_number_gt 3121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Methyl hydrogen atoms were calculated using a staggered geometry (HFIX 33) as refinement of the torsion angles (HFIX 137) did not give satisfactory results. ; _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^)+(0.0645P)^2^+4.6755P] 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 4735 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1520 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Ni1 Ni 0.52302(7) 0.99041(4) 0.2500 0.0170(2) Uani 1 2 d S . . P1 P 0.52042(10) 0.98968(6) 0.35005(5) 0.0195(3) Uani 1 1 d . . . Cl1 Cl 0.68635(13) 1.05661(8) 0.2500 0.0239(3) Uani 1 2 d S . . O1 O 0.0494(4) 0.9375(2) 0.2500 0.0266(10) Uani 1 2 d S . . C1 C 0.3846(5) 0.9346(3) 0.2500 0.0163(12) Uani 1 2 d S . . C2 C 0.2667(5) 0.9597(3) 0.2500 0.0174(13) Uani 1 2 d S . . H2 H 0.2542 1.0067 0.2500 0.021 Uiso 1 2 calc SR . . N1 N 0.1791(4) 0.8499(2) 0.2500 0.0210(11) Uani 1 2 d S . . C41 C 0.3910(4) 0.9467(2) 0.38594(17) 0.0208(9) Uani 1 1 d . . . C5 C 0.3113(7) 0.7520(3) 0.2500 0.0304(16) Uani 1 2 d S . . H5 H 0.2412 0.7237 0.2500 0.036 Uiso 1 2 calc SR . . C9 C 0.4001(6) 0.8637(3) 0.2500 0.0208(13) Uani 1 2 d S . . C21 C 0.5129(4) 1.0743(2) 0.37933(18) 0.0243(10) Uani 1 1 d . . . C10 C 0.0711(6) 0.8053(3) 0.2500 0.0340(16) Uani 1 2 d S . . H10A H 0.0700 0.7791 0.2871 0.051 Uiso 0.50 1 calc PR . . H10B H 0.0757 0.7750 0.2156 0.051 Uiso 0.50 1 calc PR . . H10C H -0.0041 0.8321 0.2474 0.051 Uiso 0.50 1 calc PR . . C31 C 0.6502(4) 0.9471(2) 0.38497(19) 0.0239(10) Uani 1 1 d . . . C24 C 0.4802(5) 1.2037(2) 0.42404(19) 0.0333(12) Uani 1 1 d . . . H24 H 0.4688 1.2473 0.4399 0.040 Uiso 1 1 calc R . . C42 C 0.2879(4) 0.9808(2) 0.4069(2) 0.0314(11) Uani 1 1 d . . . H42 H 0.2854 1.0283 0.4060 0.038 Uiso 1 1 calc R . . C3 C 0.1663(5) 0.9173(3) 0.2500 0.0202(13) Uani 1 2 d S . . C8 C 0.5169(6) 0.8337(3) 0.2500 0.0244(14) Uani 1 2 d S . . H8 H 0.5878 0.8614 0.2500 0.029 Uiso 1 2 calc SR . . C45 C 0.2910(4) 0.8421(2) 0.40770(19) 0.0313(11) Uani 1 1 d . . . H45 H 0.2918 0.7946 0.4070 0.038 Uiso 1 1 calc R . . C4 C 0.2968(5) 0.8213(3) 0.2500 0.0189(13) Uani 1 2 d S . . C22 C 0.5883(4) 1.0988(2) 0.42512(18) 0.0268(10) Uani 1 1 d . . . H22 H 0.6506 1.0711 0.4416 0.032 Uiso 1 1 calc R . . C23 C 0.5725(5) 1.1626(2) 0.44629(19) 0.0319(11) Uani 1 1 d . . . H23 H 0.6257 1.1790 0.4767 0.038 Uiso 1 1 calc R . . C32 C 0.6460(4) 0.9308(2) 0.44549(19) 0.0285(11) Uani 1 1 d . . . H32 H 0.5783 0.9453 0.4691 0.034 Uiso 1 1 calc R . . C46 C 0.3919(4) 0.8777(2) 0.38750(18) 0.0255(10) Uani 1 1 d . . . H46 H 0.4630 0.8543 0.3745 0.031 Uiso 1 1 calc R . . C44 C 0.1894(5) 0.8757(3) 0.4289(2) 0.0401(13) Uani 1 1 d . . . H44 H 0.1202 0.8516 0.4433 0.048 Uiso 1 1 calc R . . C25 C 0.4046(4) 1.1804(2) 0.37845(19) 0.0315(11) Uani 1 1 d . . . H25 H 0.3412 1.2081 0.3628 0.038 Uiso 1 1 calc R . . C6 C 0.4265(7) 0.7251(3) 0.2500 0.0353(17) Uani 1 2 d S . . H6 H 0.4355 0.6778 0.2500 0.042 Uiso 1 2 calc SR . . C11 C 0.0263(6) 1.0087(3) 0.2500 0.0362(17) Uani 1 2 d S . . H11A H 0.0682 1.0293 0.2158 0.054 Uiso 0.50 1 calc PR . . H11B H 0.0575 1.0283 0.2873 0.054 Uiso 0.50 1 calc PR . . H11C H -0.0623 1.0168 0.2469 0.054 Uiso 0.50 1 calc PR . . C35 C 0.8415(5) 0.8874(3) 0.3776(2) 0.0428(14) Uani 1 1 d . . . H35 H 0.9093 0.8727 0.3542 0.051 Uiso 1 1 calc R . . C26 C 0.4223(4) 1.1166(2) 0.35593(19) 0.0271(10) Uani 1 1 d . . . H26 H 0.3720 1.1012 0.3240 0.033 Uiso 1 1 calc R . . C33 C 0.7386(4) 0.8939(2) 0.4717(2) 0.0344(12) Uani 1 1 d . . . H33 H 0.7358 0.8842 0.5134 0.041 Uiso 1 1 calc R . . C34 C 0.8356(5) 0.8710(3) 0.4374(2) 0.0415(13) Uani 1 1 d . . . H34 H 0.8979 0.8440 0.4550 0.050 Uiso 1 1 calc R . . C7 C 0.5313(7) 0.7651(3) 0.2500 0.0325(16) Uani 1 2 d S . . H7 H 0.6110 0.7456 0.2500 0.039 Uiso 1 2 calc SR . . C43 C 0.1887(4) 0.9447(3) 0.4291(2) 0.0410(13) Uani 1 1 d . . . H43 H 0.1194 0.9678 0.4447 0.049 Uiso 1 1 calc R . . C36 C 0.7503(4) 0.9250(2) 0.3513(2) 0.0315(11) Uani 1 1 d . . . H36 H 0.7555 0.9359 0.3100 0.038 Uiso 1 1 calc R . . Cl3 Cl 0.06508(17) 0.56390(8) 0.41179(7) 0.0715(5) Uani 1 1 d . . . Cl2 Cl 0.06836(19) 0.70743(8) 0.42681(8) 0.0778(6) Uani 1 1 d . . . C12 C 0.0990(6) 0.6408(3) 0.3785(2) 0.0540(16) Uani 1 1 d . . . H12B H 0.1868 0.6418 0.3670 0.065 Uiso 1 1 calc R . . H12A H 0.0494 0.6460 0.3416 0.065 Uiso 1 1 calc R . . F1 F -0.0179(3) 0.65790(18) 0.2500 0.0332(9) Uani 1 2 d S . . F2 F -0.2217(3) 0.63080(19) 0.2500 0.0411(10) Uani 1 2 d S . . F3 F -0.1537(3) 0.7218(2) 0.20111(19) 0.0959(15) Uani 1 1 d . . . B1 B -0.1367(8) 0.6816(4) 0.2500 0.041(2) Uani 1 2 d S . . 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 0.0159(4) 0.0195(4) 0.0156(4) 0.000 0.000 -0.0010(3) P1 0.0180(6) 0.0244(6) 0.0162(5) -0.0008(5) -0.0006(4) 0.0007(5) Cl1 0.0187(8) 0.0273(8) 0.0257(8) 0.000 0.000 -0.0045(6) O1 0.017(2) 0.024(2) 0.039(3) 0.000 0.000 -0.0022(18) C1 0.018(3) 0.023(3) 0.008(3) 0.000 0.000 -0.002(2) C2 0.019(3) 0.011(3) 0.022(3) 0.000 0.000 -0.001(2) N1 0.023(3) 0.023(3) 0.017(3) 0.000 0.000 -0.010(2) C41 0.020(2) 0.027(3) 0.015(2) -0.0016(19) 0.0020(17) 0.0021(19) C5 0.041(4) 0.017(3) 0.033(4) 0.000 0.000 -0.005(3) C9 0.029(4) 0.018(3) 0.016(3) 0.000 0.000 0.001(3) C21 0.025(2) 0.030(3) 0.018(2) 0.0012(19) 0.0010(19) -0.004(2) C10 0.031(4) 0.030(4) 0.041(4) 0.000 0.000 -0.011(3) C31 0.019(2) 0.030(3) 0.023(2) 0.000(2) -0.0045(18) 0.0009(19) C24 0.051(3) 0.029(3) 0.020(2) -0.005(2) 0.006(2) -0.006(2) C42 0.031(3) 0.036(3) 0.028(3) 0.004(2) 0.004(2) 0.005(2) C3 0.025(4) 0.022(3) 0.013(3) 0.000 0.000 0.000(3) C8 0.024(3) 0.030(4) 0.018(3) 0.000 0.000 0.002(3) C45 0.033(3) 0.033(3) 0.027(2) 0.004(2) 0.000(2) -0.002(2) C4 0.029(4) 0.018(3) 0.009(3) 0.000 0.000 0.004(3) C22 0.027(3) 0.032(3) 0.022(2) 0.003(2) -0.0037(19) 0.000(2) C23 0.039(3) 0.037(3) 0.021(2) -0.003(2) -0.003(2) -0.006(2) C32 0.023(2) 0.036(3) 0.026(3) 0.001(2) -0.0010(19) 0.002(2) C46 0.024(3) 0.033(3) 0.019(2) 0.000(2) 0.0042(19) 0.003(2) C44 0.029(3) 0.047(3) 0.045(3) 0.013(3) 0.004(2) -0.009(2) C25 0.039(3) 0.029(3) 0.026(3) 0.004(2) 0.002(2) 0.007(2) C6 0.060(5) 0.016(4) 0.030(4) 0.000 0.000 0.004(3) C11 0.018(3) 0.035(4) 0.056(5) 0.000 0.000 0.007(3) C35 0.035(3) 0.059(4) 0.035(3) 0.006(3) 0.005(2) 0.021(3) C26 0.030(3) 0.030(3) 0.021(2) -0.001(2) -0.004(2) 0.000(2) C33 0.033(3) 0.049(3) 0.021(2) 0.008(2) -0.002(2) 0.004(2) C34 0.033(3) 0.054(4) 0.037(3) 0.007(3) -0.001(2) 0.014(3) C7 0.035(4) 0.037(4) 0.026(4) 0.000 0.000 0.012(3) C43 0.024(3) 0.055(4) 0.044(3) 0.006(3) 0.012(2) 0.008(2) C36 0.027(3) 0.045(3) 0.022(2) 0.006(2) 0.002(2) 0.011(2) Cl3 0.0967(13) 0.0475(9) 0.0704(11) 0.0064(8) -0.0009(10) -0.0250(9) Cl2 0.1100(15) 0.0460(10) 0.0775(12) 0.0027(9) -0.0050(11) -0.0134(10) C12 0.066(4) 0.059(4) 0.037(3) 0.009(3) -0.006(3) -0.013(3) F1 0.020(2) 0.032(2) 0.047(2) 0.000 0.000 -0.0030(16) F2 0.029(2) 0.039(2) 0.055(3) 0.000 0.000 -0.0122(18) F3 0.050(2) 0.092(3) 0.146(4) 0.078(3) -0.041(2) -0.027(2) B1 0.026(5) 0.037(5) 0.060(6) 0.000 0.000 -0.005(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 C1 1.874(6) . ? Ni1 Cl1 2.2158(16) . ? Ni1 P1 2.2346(10) . ? Ni1 P1 2.2346(10) 6_556 ? P1 C21 1.816(4) . ? P1 C31 1.824(4) . ? P1 C41 1.833(4) . ? O1 C3 1.334(7) . ? O1 C11 1.447(7) . ? C1 C2 1.378(8) . ? C1 C9 1.429(8) . ? C2 C3 1.383(8) . ? C2 H2 0.9500 . ? N1 C3 1.355(7) . ? N1 C4 1.403(8) . ? N1 C10 1.475(7) . ? C41 C46 1.381(6) . ? C41 C42 1.393(6) . ? C5 C6 1.365(9) . ? C5 C4 1.394(8) . ? C5 H5 0.9500 . ? C9 C8 1.405(8) . ? C9 C4 1.407(8) . ? C21 C26 1.399(6) . ? C21 C22 1.399(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C31 C32 1.391(6) . ? C31 C36 1.395(6) . ? C24 C25 1.389(6) . ? C24 C23 1.390(7) . ? C24 H24 0.9500 . ? C42 C43 1.391(7) . ? C42 H42 0.9500 . ? C8 C7 1.380(9) . ? C8 H8 0.9500 . ? C45 C44 1.379(7) . ? C45 C46 1.384(6) . ? C45 H45 0.9500 . ? C22 C23 1.372(6) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C32 C33 1.381(6) . ? C32 H32 0.9500 . ? C46 H46 0.9500 . ? C44 C43 1.379(7) . ? C44 H44 0.9500 . ? C25 C26 1.386(6) . ? C25 H25 0.9500 . ? C6 C7 1.393(10) . ? C6 H6 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C35 C36 1.376(6) . ? C35 C34 1.377(7) . ? C35 H35 0.9500 . ? C26 H26 0.9500 . ? C33 C34 1.382(7) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C7 H7 0.9500 . ? C43 H43 0.9500 . ? C36 H36 0.9500 . ? Cl3 C12 1.748(5) . ? Cl2 C12 1.746(6) . ? C12 H12B 0.9900 . ? C12 H12A 0.9900 . ? F1 B1 1.377(9) . ? F2 B1 1.374(9) . ? F3 B1 1.368(6) . ? B1 F3 1.368(6) 6_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 C1 Ni1 Cl1 179.85(19) . . ? C1 Ni1 P1 89.19(4) . . ? Cl1 Ni1 P1 90.81(4) . . ? C1 Ni1 P1 89.19(4) . 6_556 ? Cl1 Ni1 P1 90.81(4) . 6_556 ? P1 Ni1 P1 178.37(7) . 6_556 ? C21 P1 C31 108.4(2) . . ? C21 P1 C41 104.14(19) . . ? C31 P1 C41 100.88(19) . . ? C21 P1 Ni1 110.77(14) . . ? C31 P1 Ni1 114.89(15) . . ? C41 P1 Ni1 116.74(14) . . ? C3 O1 C11 117.6(5) . . ? C2 C1 C9 118.1(5) . . ? C2 C1 Ni1 122.1(4) . . ? C9 C1 Ni1 119.8(4) . . ? C1 C2 C3 120.8(5) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C3 N1 C4 120.0(5) . . ? C3 N1 C10 121.3(5) . . ? C4 N1 C10 118.7(5) . . ? C46 C41 C42 119.1(4) . . ? C46 C41 P1 118.3(3) . . ? C42 C41 P1 122.4(4) . . ? C6 C5 C4 119.8(6) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C8 C9 C4 117.7(5) . . ? C8 C9 C1 122.0(6) . . ? C4 C9 C1 120.3(5) . . ? C26 C21 C22 118.3(4) . . ? C26 C21 P1 117.4(3) . . ? C22 C21 P1 124.2(3) . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C32 C31 C36 118.3(4) . . ? C32 C31 P1 119.9(3) . . ? C36 C31 P1 121.5(3) . . ? C25 C24 C23 119.5(4) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C43 C42 C41 119.4(5) . . ? C43 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? O1 C3 N1 113.5(5) . . ? O1 C3 C2 124.5(5) . . ? N1 C3 C2 122.0(5) . . ? C7 C8 C9 121.8(6) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C44 C45 C46 119.8(5) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C5 C4 N1 120.6(6) . . ? C5 C4 C9 120.6(6) . . ? N1 C4 C9 118.9(5) . . ? C23 C22 C21 120.3(4) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 121.1(4) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C33 C32 C31 120.9(4) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C41 C46 C45 121.2(4) . . ? C41 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C45 C44 C43 119.6(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C26 C25 C24 119.5(4) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C5 C6 C7 121.7(6) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C36 C35 C34 120.7(5) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C25 C26 C21 121.3(4) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? C32 C33 C34 119.9(4) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 119.7(5) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C8 C7 C6 118.5(6) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C44 C43 C42 120.9(5) . . ? C44 C43 H43 119.5 . . ? C42 C43 H43 119.5 . . ? C35 C36 C31 120.5(4) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? Cl2 C12 Cl3 111.6(3) . . ? Cl2 C12 H12B 109.3 . . ? Cl3 C12 H12B 109.3 . . ? Cl2 C12 H12A 109.3 . . ? Cl3 C12 H12A 109.3 . . ? H12B C12 H12A 108.0 . . ? F3 B1 F3 105.9(7) 6_556 . ? F3 B1 F2 110.1(4) 6_556 . ? F3 B1 F2 110.1(4) . . ? F3 B1 F1 109.2(4) 6_556 . ? F3 B1 F1 109.2(4) . . ? F2 B1 F1 112.1(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ni1 P1 C21 -124.0(2) . . . . ? Cl1 Ni1 P1 C21 55.81(16) . . . . ? P1 Ni1 P1 C21 -115(3) 6_556 . . . ? C1 Ni1 P1 C31 112.7(2) . . . . ? Cl1 Ni1 P1 C31 -67.44(17) . . . . ? P1 Ni1 P1 C31 122(3) 6_556 . . . ? C1 Ni1 P1 C41 -5.1(2) . . . . ? Cl1 Ni1 P1 C41 174.73(16) . . . . ? P1 Ni1 P1 C41 4(3) 6_556 . . . ? Cl1 Ni1 C1 C2 0(27) . . . . ? P1 Ni1 C1 C2 89.87(4) . . . . ? P1 Ni1 C1 C2 -89.87(4) 6_556 . . . ? Cl1 Ni1 C1 C9 180(27) . . . . ? P1 Ni1 C1 C9 -90.13(4) . . . . ? P1 Ni1 C1 C9 90.13(4) 6_556 . . . ? C9 C1 C2 C3 0.0 . . . . ? Ni1 C1 C2 C3 180.0 . . . . ? C21 P1 C41 C46 -160.9(3) . . . . ? C31 P1 C41 C46 -48.6(4) . . . . ? Ni1 P1 C41 C46 76.6(4) . . . . ? C21 P1 C41 C42 24.7(4) . . . . ? C31 P1 C41 C42 137.0(4) . . . . ? Ni1 P1 C41 C42 -97.7(4) . . . . ? C2 C1 C9 C8 180.0 . . . . ? Ni1 C1 C9 C8 0.0 . . . . ? C2 C1 C9 C4 0.0 . . . . ? Ni1 C1 C9 C4 180.0 . . . . ? C31 P1 C21 C26 177.1(3) . . . . ? C41 P1 C21 C26 -76.1(4) . . . . ? Ni1 P1 C21 C26 50.2(4) . . . . ? C31 P1 C21 C22 -5.5(4) . . . . ? C41 P1 C21 C22 101.3(4) . . . . ? Ni1 P1 C21 C22 -132.4(3) . . . . ? C21 P1 C31 C32 69.3(4) . . . . ? C41 P1 C31 C32 -39.7(4) . . . . ? Ni1 P1 C31 C32 -166.2(3) . . . . ? C21 P1 C31 C36 -116.5(4) . . . . ? C41 P1 C31 C36 134.5(4) . . . . ? Ni1 P1 C31 C36 8.0(4) . . . . ? C46 C41 C42 C43 0.3(7) . . . . ? P1 C41 C42 C43 174.7(4) . . . . ? C11 O1 C3 N1 180.0 . . . . ? C11 O1 C3 C2 0.0 . . . . ? C4 N1 C3 O1 180.0 . . . . ? C10 N1 C3 O1 0.0 . . . . ? C4 N1 C3 C2 0.0 . . . . ? C10 N1 C3 C2 180.0 . . . . ? C1 C2 C3 O1 180.0 . . . . ? C1 C2 C3 N1 0.0 . . . . ? C4 C9 C8 C7 0.0 . . . . ? C1 C9 C8 C7 180.0 . . . . ? C6 C5 C4 N1 180.0 . . . . ? C6 C5 C4 C9 0.0 . . . . ? C3 N1 C4 C5 180.0 . . . . ? C10 N1 C4 C5 0.0 . . . . ? C3 N1 C4 C9 0.0 . . . . ? C10 N1 C4 C9 180.0 . . . . ? C8 C9 C4 C5 0.0 . . . . ? C1 C9 C4 C5 180.0 . . . . ? C8 C9 C4 N1 180.0 . . . . ? C1 C9 C4 N1 0.0 . . . . ? C26 C21 C22 C23 0.2(6) . . . . ? P1 C21 C22 C23 -177.1(3) . . . . ? C21 C22 C23 C24 1.6(7) . . . . ? C25 C24 C23 C22 -1.8(7) . . . . ? C36 C31 C32 C33 0.3(7) . . . . ? P1 C31 C32 C33 174.7(4) . . . . ? C42 C41 C46 C45 2.0(6) . . . . ? P1 C41 C46 C45 -172.6(3) . . . . ? C44 C45 C46 C41 -2.6(7) . . . . ? C46 C45 C44 C43 0.8(7) . . . . ? C23 C24 C25 C26 0.1(7) . . . . ? C4 C5 C6 C7 0.0 . . . . ? C24 C25 C26 C21 1.7(7) . . . . ? C22 C21 C26 C25 -1.9(6) . . . . ? P1 C21 C26 C25 175.7(3) . . . . ? C31 C32 C33 C34 -1.9(7) . . . . ? C36 C35 C34 C33 -1.7(8) . . . . ? C32 C33 C34 C35 2.5(8) . . . . ? C9 C8 C7 C6 0.0 . . . . ? C5 C6 C7 C8 0.0 . . . . ? C45 C44 C43 C42 1.6(8) . . . . ? C41 C42 C43 C44 -2.1(7) . . . . ? C34 C35 C36 C31 0.1(8) . . . . ? C32 C31 C36 C35 0.6(7) . . . . ? P1 C31 C36 C35 -173.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.788 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.089 # Attachment 'Complex 12.CIF' data_12 _database_code_depnum_ccdc_archive 'CCDC 282955' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H38 Cl N2 Ni P2, 2(C H2 Cl2), B F4' _chemical_formula_sum 'C43 H42 B Cl5 F4 N2 Ni P2' _chemical_formula_weight 971.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 9.0700(7) _cell_length_b 21.5846(17) _cell_length_c 11.4543(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.326(2) _cell_angle_gamma 90.00 _cell_volume 2236.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3341 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 24.70 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6312 _exptl_absorpt_correction_T_max 0.9194 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12489 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6454 _reflns_number_gt 5849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0654P)^2^+3.6111P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 6454 _refine_ls_number_parameters 516 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Ni1 Ni 0.88731(7) 1.00081(3) 0.88346(5) 0.01350(16) Uani 1 1 d . . . P2 P 0.83449(14) 0.99628(8) 0.69019(11) 0.0162(3) Uani 1 1 d . . . P1 P 0.94388(14) 1.00558(8) 1.07668(11) 0.0148(3) Uani 1 1 d . . . Cl1 Cl 1.11339(14) 0.96948(7) 0.86337(12) 0.0186(3) Uani 1 1 d . . . C21 C 1.0673(6) 1.0693(3) 1.1194(5) 0.0195(13) Uani 1 1 d . . . N2 N 0.6570(5) 1.0929(2) 0.8954(4) 0.0161(10) Uani 1 1 d . . . C51 C 0.9052(6) 1.0662(3) 0.6223(5) 0.0170(13) Uani 1 1 d . . . C3 C 0.5094(6) 1.0993(3) 0.9147(5) 0.0206(13) Uani 1 1 d . . . H3 H 0.4544 1.1368 0.9151 0.025 Uiso 1 1 calc R . . N1 N 0.5742(4) 1.0021(3) 0.9238(4) 0.0157(9) Uani 1 1 d . . . C1 C 0.6983(6) 1.0337(3) 0.9007(5) 0.0153(12) Uani 1 1 d . . . C11 C 0.7907(6) 1.0167(3) 1.1706(5) 0.0174(13) Uani 1 1 d . . . C62 C 0.5709(8) 0.9353(4) 0.6202(6) 0.0330(17) Uani 1 1 d . . . H62 H 0.6286 0.8986 0.6248 0.040 Uiso 1 1 calc R . . C4 C 0.7546(6) 1.1458(3) 0.8714(5) 0.0199(13) Uani 1 1 d . . . H4C H 0.7675 1.1478 0.7873 0.030 Uiso 1 1 calc R . . H4B H 0.8511 1.1402 0.9146 0.030 Uiso 1 1 calc R . . H4A H 0.7096 1.1844 0.8965 0.030 Uiso 1 1 calc R . . C61 C 0.6370(6) 0.9933(3) 0.6403(4) 0.0209(13) Uani 1 1 d . . . C63 C 0.4194(9) 0.9326(4) 0.5934(7) 0.046(2) Uani 1 1 d . . . H63 H 0.3723 0.8937 0.5796 0.055 Uiso 1 1 calc R . . C2 C 0.4594(6) 1.0420(3) 0.9329(5) 0.0220(13) Uani 1 1 d . . . H2 H 0.3615 1.0311 0.9492 0.026 Uiso 1 1 calc R . . C41 C 0.9156(7) 0.9316(3) 0.6143(5) 0.0185(13) Uani 1 1 d . . . C31 C 1.0382(6) 0.9345(3) 1.1258(5) 0.0165(13) Uani 1 1 d . . . C66 C 0.5518(7) 1.0473(4) 0.6337(5) 0.0273(15) Uani 1 1 d . . . H66 H 0.5967 1.0865 0.6482 0.033 Uiso 1 1 calc R . . C65 C 0.4002(8) 1.0428(4) 0.6055(6) 0.040(2) Uani 1 1 d . . . H65 H 0.3415 1.0793 0.5995 0.047 Uiso 1 1 calc R . . C64 C 0.3362(7) 0.9868(4) 0.5867(6) 0.046(2) Uani 1 1 d . . . H64 H 0.2324 0.9844 0.5685 0.056 Uiso 1 1 calc R . . C55 C 0.9021(7) 1.1407(3) 0.4657(6) 0.0272(15) Uani 1 1 d . . . H55 H 0.8619 1.1554 0.3918 0.033 Uiso 1 1 calc R . . C16 C 0.7277(6) 0.9697(3) 1.2307(5) 0.0195(12) Uani 1 1 d . . . H16 H 0.7685 0.9292 1.2296 0.023 Uiso 1 1 calc R . . C56 C 0.8443(7) 1.0882(3) 0.5145(5) 0.0206(13) Uani 1 1 d . . . H56 H 0.7633 1.0672 0.4748 0.025 Uiso 1 1 calc R . . C54 C 1.0184(7) 1.1717(3) 0.5246(6) 0.0247(14) Uani 1 1 d . . . H54 H 1.0566 1.2082 0.4916 0.030 Uiso 1 1 calc R . . C46 C 0.9445(7) 0.9374(3) 0.4979(5) 0.0228(13) Uani 1 1 d . . . H46 H 0.9190 0.9748 0.4576 0.027 Uiso 1 1 calc R . . C53 C 1.0799(7) 1.1501(3) 0.6311(6) 0.0248(14) Uani 1 1 d . . . H53 H 1.1599 1.1717 0.6710 0.030 Uiso 1 1 calc R . . C24 C 1.2425(7) 1.1708(3) 1.1878(6) 0.0290(15) Uani 1 1 d . . . H24 H 1.3017 1.2056 1.2111 0.035 Uiso 1 1 calc R . . C45 C 1.0096(8) 0.8900(3) 0.4391(6) 0.0268(15) Uani 1 1 d . . . H45 H 1.0296 0.8946 0.3593 0.032 Uiso 1 1 calc R . . C5 C 0.5632(7) 0.9349(3) 0.9366(6) 0.0249(14) Uani 1 1 d . . . H5A H 0.4819 0.9193 0.8834 0.037 Uiso 1 1 calc R . . H5B H 0.5441 0.9248 1.0175 0.037 Uiso 1 1 calc R . . H5C H 0.6561 0.9156 0.9175 0.037 Uiso 1 1 calc R . . C32 C 1.1874(6) 0.9342(3) 1.1683(5) 0.0195(12) Uani 1 1 d . . . H32 H 1.2403 0.9720 1.1781 0.023 Uiso 1 1 calc R . . C13 C 0.6067(7) 1.0872(3) 1.2348(5) 0.0277(15) Uani 1 1 d . . . H13 H 0.5649 1.1276 1.2356 0.033 Uiso 1 1 calc R . . C44 C 1.0451(7) 0.8355(3) 0.4989(6) 0.0284(15) Uani 1 1 d . . . H44 H 1.0922 0.8029 0.4602 0.034 Uiso 1 1 calc R . . C15 C 0.6040(6) 0.9810(3) 1.2932(5) 0.0210(13) Uani 1 1 d . . . H15 H 0.5617 0.9483 1.3351 0.025 Uiso 1 1 calc R . . C34 C 1.1815(7) 0.8237(3) 1.1838(6) 0.0283(15) Uani 1 1 d . . . H34 H 1.2298 0.7858 1.2054 0.034 Uiso 1 1 calc R . . C25 C 1.2048(7) 1.1605(3) 1.0712(6) 0.0271(15) Uani 1 1 d . . . H25 H 1.2376 1.1881 1.0140 0.032 Uiso 1 1 calc R . . C23 C 1.1952(7) 1.1309(3) 1.2718(6) 0.0305(16) Uani 1 1 d . . . H23 H 1.2245 1.1378 1.3521 0.037 Uiso 1 1 calc R . . C52 C 1.0246(6) 1.0970(3) 0.6793(5) 0.0204(13) Uani 1 1 d . . . H52 H 1.0682 1.0815 0.7515 0.025 Uiso 1 1 calc R . . C43 C 1.0132(7) 0.8279(3) 0.6133(6) 0.0277(15) Uani 1 1 d . . . H43 H 1.0329 0.7895 0.6516 0.033 Uiso 1 1 calc R . . C33 C 1.2569(7) 0.8787(3) 1.1957(5) 0.0241(14) Uani 1 1 d . . . H33 H 1.3584 0.8786 1.2231 0.029 Uiso 1 1 calc R . . C35 C 1.0331(7) 0.8234(3) 1.1399(6) 0.0247(14) Uani 1 1 d . . . H35 H 0.9810 0.7854 1.1307 0.030 Uiso 1 1 calc R . . C14 C 0.5432(6) 1.0395(3) 1.2942(5) 0.0248(14) Uani 1 1 d . . . H14 H 0.4580 1.0471 1.3355 0.030 Uiso 1 1 calc R . . C36 C 0.9624(7) 0.8785(3) 1.1101(5) 0.0212(13) Uani 1 1 d . . . H36 H 0.8624 0.8782 1.0789 0.025 Uiso 1 1 calc R . . C26 C 1.1183(7) 1.1095(3) 1.0372(6) 0.0234(14) Uani 1 1 d . . . H26 H 1.0937 1.1021 0.9563 0.028 Uiso 1 1 calc R . . C12 C 0.7303(6) 1.0766(3) 1.1746(5) 0.0212(13) Uani 1 1 d . . . H12 H 0.7746 1.1099 1.1356 0.025 Uiso 1 1 calc R . . C22 C 1.1056(6) 1.0809(3) 1.2398(5) 0.0217(13) Uani 1 1 d . . . H22 H 1.0699 1.0546 1.2979 0.026 Uiso 1 1 calc R . . C42 C 0.95393(13) 0.87521(6) 0.67147(10) 0.0268(15) Uani 1 1 d . . . H42 H 0.9378 0.8704 0.7520 0.032 Uiso 1 1 calc R . . Cl3 Cl 1.11982(13) 0.74488(6) 0.87749(10) 0.0388(4) Uani 1 1 d R . . Cl5 Cl 1.37032(13) 0.72098(6) 0.44350(10) 0.0618(7) Uani 1 1 d R . . Cl2 Cl 1.38423(13) 0.77928(6) 0.75988(10) 0.0505(5) Uani 1 1 d R . . Cl4 Cl 1.6557(2) 0.77314(14) 0.5325(3) 0.0757(8) Uani 1 1 d . . . F4 F 1.3860(4) 1.33223(18) 0.8080(4) 0.0381(10) Uani 1 1 d . . . F3 F 1.2918(4) 1.23529(19) 0.8291(3) 0.0381(10) Uani 1 1 d . . . F2 F 1.3354(5) 1.29763(19) 0.9865(3) 0.0380(10) Uani 1 1 d . . . F1 F 1.5254(4) 1.2562(2) 0.8949(4) 0.0466(11) Uani 1 1 d . . . B1 B 1.3834(7) 1.2808(3) 0.8790(6) 0.0218(15) Uani 1 1 d . . . C6 C 1.2655(9) 0.7988(4) 0.8710(7) 0.0403(18) Uani 1 1 d . . . H6B H 1.3236 0.8000 0.9477 0.048 Uiso 1 1 calc R . . H6A H 1.2236 0.8406 0.8553 0.048 Uiso 1 1 calc R . . C7 C 1.5245(10) 0.7656(5) 0.4154(7) 0.057(2) Uani 1 1 d . . . H7A H 1.5723 0.7468 0.3491 0.068 Uiso 1 1 calc R . . H7B H 1.4903 0.8075 0.3908 0.068 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 0.0099(3) 0.0159(4) 0.0149(3) -0.0007(3) 0.0015(2) 0.0004(3) P2 0.0128(6) 0.0200(8) 0.0160(6) -0.0018(7) 0.0018(5) -0.0022(7) P1 0.0123(6) 0.0158(8) 0.0165(6) -0.0017(7) 0.0016(5) 0.0003(6) Cl1 0.0107(6) 0.0254(8) 0.0199(7) -0.0047(6) 0.0027(5) 0.0026(6) C21 0.012(3) 0.018(3) 0.029(3) -0.001(3) 0.006(2) 0.008(2) N2 0.014(2) 0.018(3) 0.017(2) 0.002(2) 0.0034(19) 0.0040(19) C51 0.015(3) 0.013(3) 0.023(3) -0.006(2) 0.008(2) 0.003(2) C3 0.013(3) 0.025(3) 0.024(3) -0.003(3) 0.000(2) 0.008(2) N1 0.013(2) 0.017(2) 0.017(2) 0.002(2) 0.0007(17) 0.000(2) C1 0.014(3) 0.015(3) 0.017(3) 0.007(2) -0.001(2) -0.002(2) C11 0.010(2) 0.024(4) 0.018(3) -0.008(2) -0.003(2) -0.001(2) C62 0.025(4) 0.045(5) 0.029(4) -0.003(3) 0.002(3) -0.009(3) C4 0.023(3) 0.013(3) 0.023(3) 0.000(3) 0.002(2) 0.002(2) C61 0.013(3) 0.039(4) 0.010(2) -0.001(3) -0.003(2) 0.001(3) C63 0.038(4) 0.061(6) 0.038(4) 0.005(4) -0.001(4) -0.025(4) C2 0.010(3) 0.035(4) 0.021(3) -0.002(3) 0.002(2) -0.003(3) C41 0.017(3) 0.014(3) 0.025(3) -0.004(3) 0.001(2) -0.004(2) C31 0.010(3) 0.028(4) 0.012(3) 0.002(3) 0.005(2) 0.004(2) C66 0.022(3) 0.040(4) 0.020(3) -0.004(3) 0.003(3) -0.002(3) C65 0.021(4) 0.072(6) 0.026(4) 0.005(4) 0.002(3) 0.012(4) C64 0.012(3) 0.087(8) 0.041(4) -0.007(4) 0.006(3) -0.006(4) C55 0.029(3) 0.027(4) 0.026(3) 0.006(3) 0.002(3) 0.008(3) C16 0.019(3) 0.020(3) 0.019(3) 0.001(3) 0.000(2) -0.001(3) C56 0.021(3) 0.018(3) 0.024(3) -0.001(3) 0.003(2) -0.002(2) C54 0.026(3) 0.011(3) 0.038(4) 0.003(3) 0.009(3) -0.003(3) C46 0.028(3) 0.020(3) 0.021(3) 0.001(3) 0.006(3) 0.003(3) C53 0.017(3) 0.027(4) 0.031(4) -0.011(3) 0.007(3) -0.010(3) C24 0.022(3) 0.027(4) 0.039(4) -0.013(3) 0.004(3) -0.005(3) C45 0.035(4) 0.025(4) 0.022(3) -0.003(3) 0.008(3) 0.002(3) C5 0.025(3) 0.025(4) 0.024(3) 0.005(3) 0.002(3) -0.007(3) C32 0.019(3) 0.020(3) 0.019(3) -0.005(3) 0.000(2) -0.004(2) C13 0.027(3) 0.033(4) 0.024(3) -0.008(3) 0.005(3) 0.009(3) C44 0.028(3) 0.025(4) 0.032(4) -0.007(3) 0.005(3) -0.005(3) C15 0.022(3) 0.018(3) 0.024(3) -0.002(2) 0.002(2) -0.007(2) C34 0.026(3) 0.027(4) 0.033(4) 0.001(3) 0.008(3) 0.009(3) C25 0.018(3) 0.018(3) 0.047(4) -0.003(3) 0.015(3) -0.002(2) C23 0.020(3) 0.040(4) 0.031(4) -0.014(3) -0.002(3) 0.000(3) C52 0.017(3) 0.024(4) 0.020(3) -0.008(3) 0.001(2) 0.000(2) C43 0.037(4) 0.019(3) 0.026(3) -0.002(3) -0.006(3) 0.003(3) C33 0.018(3) 0.029(4) 0.025(3) -0.001(3) 0.000(3) 0.006(3) C35 0.024(3) 0.017(3) 0.033(4) -0.003(3) 0.008(3) 0.002(3) C14 0.012(3) 0.044(4) 0.019(3) -0.010(3) 0.002(2) 0.003(3) C36 0.017(3) 0.024(3) 0.024(3) 0.001(3) 0.005(3) 0.000(2) C26 0.021(3) 0.021(3) 0.028(3) -0.008(3) 0.005(3) 0.000(2) C12 0.020(3) 0.024(3) 0.019(3) 0.000(3) 0.001(2) 0.003(2) C22 0.014(3) 0.023(3) 0.028(3) -0.006(3) 0.002(2) -0.001(2) C42 0.033(4) 0.030(4) 0.016(3) 0.002(3) -0.005(3) -0.002(3) Cl3 0.0514(11) 0.0345(10) 0.0302(8) 0.0081(8) 0.0005(8) -0.0065(8) Cl5 0.0649(15) 0.0635(16) 0.0575(13) -0.0073(12) 0.0076(12) -0.0251(12) Cl2 0.0411(11) 0.0621(14) 0.0487(11) 0.0039(11) 0.0056(9) 0.0088(10) Cl4 0.0355(11) 0.086(2) 0.103(2) -0.0387(16) -0.0153(12) 0.0055(12) F4 0.042(2) 0.023(2) 0.051(2) 0.0064(19) 0.0149(19) 0.0037(17) F3 0.040(2) 0.035(2) 0.038(2) -0.0038(19) -0.0013(18) -0.0130(19) F2 0.050(3) 0.031(2) 0.034(2) -0.0055(18) 0.0062(19) 0.0023(18) F1 0.021(2) 0.038(3) 0.080(3) 0.004(2) 0.001(2) 0.0060(18) B1 0.020(3) 0.013(3) 0.033(4) 0.000(3) 0.005(3) 0.002(3) C6 0.045(4) 0.035(4) 0.040(4) -0.003(3) -0.007(4) -0.010(3) C7 0.061(6) 0.060(6) 0.050(5) 0.015(5) 0.002(4) -0.017(5) _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 C1 1.880(6) . ? Ni1 Cl1 2.1878(14) . ? Ni1 P2 2.2315(15) . ? Ni1 P1 2.2363(15) . ? P2 C41 1.829(6) . ? P2 C51 1.836(6) . ? P2 C61 1.840(5) . ? P1 C21 1.817(7) . ? P1 C31 1.825(6) . ? P1 C11 1.836(6) . ? C21 C26 1.386(9) . ? C21 C22 1.419(8) . ? N2 C1 1.331(7) . ? N2 C3 1.380(7) . ? N2 C4 1.483(7) . ? C51 C52 1.390(8) . ? C51 C56 1.398(9) . ? C3 C2 1.339(9) . ? C3 H3 0.9500 . ? N1 C1 1.359(7) . ? N1 C2 1.361(8) . ? N1 C5 1.462(8) . ? C11 C16 1.374(8) . ? C11 C12 1.407(8) . ? C62 C63 1.386(10) . ? C62 C61 1.400(10) . ? C62 H62 0.9500 . ? C4 H4C 0.9800 . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C61 C66 1.396(10) . ? C63 C64 1.392(12) . ? C63 H63 0.9500 . ? C2 H2 0.9500 . ? C41 C46 1.384(8) . ? C41 C42 1.412(6) . ? C31 C36 1.396(9) . ? C31 C32 1.403(8) . ? C66 C65 1.391(9) . ? C66 H66 0.9500 . ? C65 C64 1.351(12) . ? C65 H65 0.9500 . ? C64 H64 0.9500 . ? C55 C54 1.381(9) . ? C55 C56 1.384(9) . ? C55 H55 0.9500 . ? C16 C15 1.397(8) . ? C16 H16 0.9500 . ? C56 H56 0.9500 . ? C54 C53 1.383(9) . ? C54 H54 0.9500 . ? C46 C45 1.382(9) . ? C46 H46 0.9500 . ? C53 C52 1.383(9) . ? C53 H53 0.9500 . ? C24 C25 1.371(10) . ? C24 C23 1.384(10) . ? C24 H24 0.9500 . ? C45 C44 1.387(10) . ? C45 H45 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C32 C33 1.378(9) . ? C32 H32 0.9500 . ? C13 C12 1.379(8) . ? C13 C14 1.383(10) . ? C13 H13 0.9500 . ? C44 C43 1.372(9) . ? C44 H44 0.9500 . ? C15 C14 1.379(9) . ? C15 H15 0.9500 . ? C34 C33 1.373(9) . ? C34 C35 1.401(9) . ? C34 H34 0.9500 . ? C25 C26 1.391(9) . ? C25 H25 0.9500 . ? C23 C22 1.384(9) . ? C23 H23 0.9500 . ? C52 H52 0.9500 . ? C43 C42 1.352(7) . ? C43 H43 0.9500 . ? C33 H33 0.9500 . ? C35 C36 1.381(9) . ? C35 H35 0.9500 . ? C14 H14 0.9500 . ? C36 H36 0.9500 . ? C26 H26 0.9500 . ? C12 H12 0.9500 . ? C22 H22 0.9500 . ? C42 H42 0.9500 . ? Cl3 C6 1.767(7) . ? Cl5 C7 1.748(8) . ? Cl2 C6 1.779(8) . ? Cl4 C7 1.732(9) . ? F4 B1 1.377(8) . ? F3 B1 1.383(8) . ? F2 B1 1.385(8) . ? F1 B1 1.392(8) . ? C6 H6B 0.9900 . ? C6 H6A 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ni1 Cl1 175.81(18) . . ? C1 Ni1 P2 89.51(17) . . ? Cl1 Ni1 P2 90.85(5) . . ? C1 Ni1 P1 91.24(17) . . ? Cl1 Ni1 P1 88.36(5) . . ? P2 Ni1 P1 179.12(6) . . ? C41 P2 C51 105.1(2) . . ? C41 P2 C61 104.1(3) . . ? C51 P2 C61 105.1(3) . . ? C41 P2 Ni1 116.2(2) . . ? C51 P2 Ni1 109.2(2) . . ? C61 P2 Ni1 116.14(17) . . ? C21 P1 C31 106.8(3) . . ? C21 P1 C11 102.8(3) . . ? C31 P1 C11 106.7(3) . . ? C21 P1 Ni1 113.1(2) . . ? C31 P1 Ni1 109.5(2) . . ? C11 P1 Ni1 117.31(18) . . ? C26 C21 C22 118.7(6) . . ? C26 C21 P1 121.4(5) . . ? C22 C21 P1 119.8(5) . . ? C1 N2 C3 111.2(5) . . ? C1 N2 C4 125.3(5) . . ? C3 N2 C4 123.5(5) . . ? C52 C51 C56 119.6(6) . . ? C52 C51 P2 118.6(5) . . ? C56 C51 P2 121.7(5) . . ? C2 C3 N2 106.0(5) . . ? C2 C3 H3 127.0 . . ? N2 C3 H3 127.0 . . ? C1 N1 C2 110.3(5) . . ? C1 N1 C5 125.5(5) . . ? C2 N1 C5 124.1(5) . . ? N2 C1 N1 104.8(5) . . ? N2 C1 Ni1 127.8(4) . . ? N1 C1 Ni1 127.3(4) . . ? C16 C11 C12 119.0(5) . . ? C16 C11 P1 123.9(5) . . ? C12 C11 P1 116.9(4) . . ? C63 C62 C61 118.7(8) . . ? C63 C62 H62 120.7 . . ? C61 C62 H62 120.7 . . ? N2 C4 H4C 109.5 . . ? N2 C4 H4B 109.5 . . ? H4C C4 H4B 109.5 . . ? N2 C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? C66 C61 C62 120.5(6) . . ? C66 C61 P2 120.7(5) . . ? C62 C61 P2 118.5(5) . . ? C62 C63 C64 120.0(8) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C3 C2 N1 107.6(5) . . ? C3 C2 H2 126.2 . . ? N1 C2 H2 126.2 . . ? C46 C41 C42 117.8(5) . . ? C46 C41 P2 120.0(5) . . ? C42 C41 P2 122.1(4) . . ? C36 C31 C32 119.5(6) . . ? C36 C31 P1 118.3(4) . . ? C32 C31 P1 121.9(5) . . ? C65 C66 C61 119.2(7) . . ? C65 C66 H66 120.4 . . ? C61 C66 H66 120.4 . . ? C64 C65 C66 120.3(8) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C65 C64 C63 121.3(6) . . ? C65 C64 H64 119.4 . . ? C63 C64 H64 119.4 . . ? C54 C55 C56 119.8(6) . . ? C54 C55 H55 120.1 . . ? C56 C55 H55 120.1 . . ? C11 C16 C15 120.6(6) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C55 C56 C51 119.9(6) . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C55 C54 C53 120.7(6) . . ? C55 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C45 C46 C41 121.4(6) . . ? C45 C46 H46 119.3 . . ? C41 C46 H46 119.3 . . ? C52 C53 C54 119.8(6) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C25 C24 C23 120.6(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C46 C45 C44 118.6(6) . . ? C46 C45 H45 120.7 . . ? C44 C45 H45 120.7 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C33 C32 C31 119.7(6) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C12 C13 C14 120.5(6) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C43 C44 C45 121.0(6) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C14 C15 C16 120.0(5) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C33 C34 C35 119.8(6) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C24 C25 C26 119.7(6) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C22 C23 C24 120.5(6) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C53 C52 C51 120.1(6) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C42 C43 C44 120.0(6) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C34 C33 C32 120.9(6) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C36 C35 C34 120.1(6) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C15 C14 C13 119.8(5) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C35 C36 C31 119.9(6) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C21 C26 C25 121.0(6) . . ? C21 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C13 C12 C11 120.1(6) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C23 C22 C21 119.5(6) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C43 C42 C41 121.0(4) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? F4 B1 F3 111.4(5) . . ? F4 B1 F2 109.6(5) . . ? F3 B1 F2 109.5(5) . . ? F4 B1 F1 109.1(5) . . ? F3 B1 F1 107.7(5) . . ? F2 B1 F1 109.5(5) . . ? Cl3 C6 Cl2 111.6(4) . . ? Cl3 C6 H6B 109.3 . . ? Cl2 C6 H6B 109.3 . . ? Cl3 C6 H6A 109.3 . . ? Cl2 C6 H6A 109.3 . . ? H6B C6 H6A 108.0 . . ? Cl4 C7 Cl5 115.0(5) . . ? Cl4 C7 H7A 108.5 . . ? Cl5 C7 H7A 108.5 . . ? Cl4 C7 H7B 108.5 . . ? Cl5 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Ni1 P2 C41 -146.1(3) . . . . ? Cl1 Ni1 P2 C41 38.1(2) . . . . ? P1 Ni1 P2 C41 64(5) . . . . ? C1 Ni1 P2 C51 95.3(3) . . . . ? Cl1 Ni1 P2 C51 -80.5(2) . . . . ? P1 Ni1 P2 C51 -54(5) . . . . ? C1 Ni1 P2 C61 -23.2(3) . . . . ? Cl1 Ni1 P2 C61 161.0(3) . . . . ? P1 Ni1 P2 C61 -173(100) . . . . ? C1 Ni1 P1 C21 -104.2(3) . . . . ? Cl1 Ni1 P1 C21 71.6(2) . . . . ? P2 Ni1 P1 C21 45(5) . . . . ? C1 Ni1 P1 C31 136.9(3) . . . . ? Cl1 Ni1 P1 C31 -47.3(2) . . . . ? P2 Ni1 P1 C31 -74(5) . . . . ? C1 Ni1 P1 C11 15.2(3) . . . . ? Cl1 Ni1 P1 C11 -169.0(2) . . . . ? P2 Ni1 P1 C11 165(49) . . . . ? C31 P1 C21 C26 120.4(5) . . . . ? C11 P1 C21 C26 -127.5(5) . . . . ? Ni1 P1 C21 C26 -0.1(6) . . . . ? C31 P1 C21 C22 -63.7(5) . . . . ? C11 P1 C21 C22 48.4(5) . . . . ? Ni1 P1 C21 C22 175.9(4) . . . . ? C41 P2 C51 C52 -99.2(5) . . . . ? C61 P2 C51 C52 151.2(5) . . . . ? Ni1 P2 C51 C52 26.0(5) . . . . ? C41 P2 C51 C56 79.4(5) . . . . ? C61 P2 C51 C56 -30.1(5) . . . . ? Ni1 P2 C51 C56 -155.3(4) . . . . ? C1 N2 C3 C2 0.2(7) . . . . ? C4 N2 C3 C2 180.0(5) . . . . ? C3 N2 C1 N1 0.1(6) . . . . ? C4 N2 C1 N1 -179.7(5) . . . . ? C3 N2 C1 Ni1 -178.7(4) . . . . ? C4 N2 C1 Ni1 1.5(8) . . . . ? C2 N1 C1 N2 -0.3(6) . . . . ? C5 N1 C1 N2 179.3(5) . . . . ? C2 N1 C1 Ni1 178.5(4) . . . . ? C5 N1 C1 Ni1 -1.9(8) . . . . ? Cl1 Ni1 C1 N2 8(3) . . . . ? P2 Ni1 C1 N2 -87.3(5) . . . . ? P1 Ni1 C1 N2 92.2(5) . . . . ? Cl1 Ni1 C1 N1 -171(2) . . . . ? P2 Ni1 C1 N1 94.1(5) . . . . ? P1 Ni1 C1 N1 -86.3(5) . . . . ? C21 P1 C11 C16 -135.0(5) . . . . ? C31 P1 C11 C16 -22.8(6) . . . . ? Ni1 P1 C11 C16 100.3(5) . . . . ? C21 P1 C11 C12 49.0(5) . . . . ? C31 P1 C11 C12 161.1(4) . . . . ? Ni1 P1 C11 C12 -75.8(5) . . . . ? C63 C62 C61 C66 0.1(9) . . . . ? C63 C62 C61 P2 174.0(5) . . . . ? C41 P2 C61 C66 -150.7(5) . . . . ? C51 P2 C61 C66 -40.5(5) . . . . ? Ni1 P2 C61 C66 80.3(5) . . . . ? C41 P2 C61 C62 35.4(5) . . . . ? C51 P2 C61 C62 145.7(5) . . . . ? Ni1 P2 C61 C62 -93.6(5) . . . . ? C61 C62 C63 C64 0.1(11) . . . . ? N2 C3 C2 N1 -0.4(7) . . . . ? C1 N1 C2 C3 0.5(7) . . . . ? C5 N1 C2 C3 -179.2(5) . . . . ? C51 P2 C41 C46 -31.7(5) . . . . ? C61 P2 C41 C46 78.5(5) . . . . ? Ni1 P2 C41 C46 -152.5(4) . . . . ? C51 P2 C41 C42 146.8(5) . . . . ? C61 P2 C41 C42 -103.0(4) . . . . ? Ni1 P2 C41 C42 26.0(5) . . . . ? C21 P1 C31 C36 176.0(5) . . . . ? C11 P1 C31 C36 66.7(5) . . . . ? Ni1 P1 C31 C36 -61.2(5) . . . . ? C21 P1 C31 C32 -10.0(5) . . . . ? C11 P1 C31 C32 -119.3(5) . . . . ? Ni1 P1 C31 C32 112.8(4) . . . . ? C62 C61 C66 C65 -0.7(9) . . . . ? P2 C61 C66 C65 -174.4(5) . . . . ? C61 C66 C65 C64 1.0(10) . . . . ? C66 C65 C64 C63 -0.8(11) . . . . ? C62 C63 C64 C65 0.2(11) . . . . ? C12 C11 C16 C15 1.0(8) . . . . ? P1 C11 C16 C15 -175.0(4) . . . . ? C54 C55 C56 C51 -1.0(9) . . . . ? C52 C51 C56 C55 -0.6(9) . . . . ? P2 C51 C56 C55 -179.2(5) . . . . ? C56 C55 C54 C53 1.3(10) . . . . ? C42 C41 C46 C45 -0.4(9) . . . . ? P2 C41 C46 C45 178.1(5) . . . . ? C55 C54 C53 C52 0.0(10) . . . . ? C41 C46 C45 C44 0.5(10) . . . . ? C36 C31 C32 C33 -1.0(8) . . . . ? P1 C31 C32 C33 -174.9(5) . . . . ? C46 C45 C44 C43 1.6(10) . . . . ? C11 C16 C15 C14 0.6(9) . . . . ? C23 C24 C25 C26 0.0(10) . . . . ? C25 C24 C23 C22 -1.8(10) . . . . ? C54 C53 C52 C51 -1.6(9) . . . . ? C56 C51 C52 C53 1.8(9) . . . . ? P2 C51 C52 C53 -179.5(5) . . . . ? C45 C44 C43 C42 -3.8(10) . . . . ? C35 C34 C33 C32 2.0(10) . . . . ? C31 C32 C33 C34 -1.1(9) . . . . ? C33 C34 C35 C36 -0.8(10) . . . . ? C16 C15 C14 C13 -1.2(9) . . . . ? C12 C13 C14 C15 0.1(9) . . . . ? C34 C35 C36 C31 -1.2(9) . . . . ? C32 C31 C36 C35 2.1(9) . . . . ? P1 C31 C36 C35 176.3(5) . . . . ? C22 C21 C26 C25 -0.3(9) . . . . ? P1 C21 C26 C25 175.7(5) . . . . ? C24 C25 C26 C21 1.1(9) . . . . ? C14 C13 C12 C11 1.6(9) . . . . ? C16 C11 C12 C13 -2.1(9) . . . . ? P1 C11 C12 C13 174.2(5) . . . . ? C24 C23 C22 C21 2.6(9) . . . . ? C26 C21 C22 C23 -1.6(8) . . . . ? P1 C21 C22 C23 -177.6(5) . . . . ? C44 C43 C42 C41 3.8(8) . . . . ? C46 C41 C42 C43 -1.7(7) . . . . ? P2 C41 C42 C43 179.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.421 _refine_diff_density_min -1.934 _refine_diff_density_rms 0.094