Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 # SUBMISSION DETAILS _publ_contact_author_name 'Lothar Stahl' _publ_contact_author_address ; Department of Chemistry University of North Dakota Grand Forks ND 58202 USA ; _publ_contact_author_email lstahl@chem.und.edu _publ_contact_author_fax '(701) 777-2331' _publ_contact_author_phone '(701) 777-2242' # TITLE AND AUTHOR LIST _publ_section_title ; Reversal of polarization in amidophosphines:Neutral- and anionic-kappa P coordination versus anionic kappaP,N coordination and the formation of nickelaazaphosphiranes ; _publ_section_title_footnote ? loop_ _publ_author_name 'Lothar Stahl' 'Ramamoorthy Boomishankar' 'Christopher J. Carrow' 'Luke Grocholl' 'Dana C. Haagenson' ; G.R.Lief ; 'Ingo Schranz' 'Lothar Stahl' 'Richard J. Staples' 'Alexander Steiner' data_2 _database_code_depnum_ccdc_archive 'CCDC 272420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H76 Cl2 N8 Ni P4' _chemical_formula_weight 910.57 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' 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 9.541(2) _cell_length_b 10.730(2) _cell_length_c 25.185(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.92(2) _cell_angle_gamma 90.00 _cell_volume 2564.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 83 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 22.34 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8017 _exptl_absorpt_correction_T_max 0.9148 _exptl_absorpt_process_details ? _exptl_special_details ; Data was collected using a Bruker SMART CCD (charge coupled device) based diffractometer equipped with an LT-2 low-temperature apparatus operating at 213 K. A suitable crystal was chosen and mounted on a glass fiber with grease. Data were measured using omega scans of 0.3\% per frame for 30 seconds, such that a hemisphere was collected. A total of 1271 frames were collected with a final resolution of 0.80 \%A. The first 50 frames were recollected at the end of data collection to monitor for decay. Cell parameters were retrieved using SMART software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp and decay. Absorption corrections were applied using SADABS supplied by George Sheldrick. The structures are solved by the direct method using the SHELX-90 program and refined by least squares method on F2 SHELXL-97, incorporated in SHELXTL-PC V 5.10. ; _diffrn_ambient_temperature 213(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 ? _diffrn_measurement_method '\w, 0.3 deg' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.8 _diffrn_reflns_number 12945 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0948 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 24.76 _reflns_number_total 4389 _reflns_number_gt 2545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (Bruker, V4.050, 1995)' _computing_cell_refinement 'SMART (Bruker, V4.050, 1995)' _computing_data_reduction 'SAINT (Bruker, V5.A06, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1998, ver 5.10)' _computing_publication_material 'CIFTAB (Sheldrick, 1993)' _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^)+(0.0681P)^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 4389 _refine_ls_number_parameters 234 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1450 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.051 _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 0.5000 0.5000 0.0000 0.0332(2) Uani 1 2 d S . . Cl1 Cl 0.29793(12) 0.46376(13) 0.02900(5) 0.0544(4) Uani 1 1 d . . . P1 P 0.59691(12) 0.45558(10) 0.08427(5) 0.0318(3) Uani 1 1 d . . . P2 P 0.43690(12) 0.44666(11) 0.16058(5) 0.0344(3) Uani 1 1 d . . . N1 N 0.5482(4) 0.5510(3) 0.13284(13) 0.0340(9) Uani 1 1 d . . . N2 N 0.5253(3) 0.3462(3) 0.12133(13) 0.0340(9) Uani 1 1 d . . . N3 N 0.5116(4) 0.4239(3) 0.22272(13) 0.0410(10) Uani 1 1 d . . . N4 N 0.7678(3) 0.4385(3) 0.08323(14) 0.0383(9) Uani 1 1 d . . . C1 C 0.5375(5) 0.6891(4) 0.13347(18) 0.0426(12) Uani 1 1 d . . . C2 C 0.3935(6) 0.7324(5) 0.1077(3) 0.089(2) Uani 1 1 d . . . H2A H 0.3201 0.6993 0.1276 0.134 Uiso 1 1 calc R . . H2B H 0.3794 0.7025 0.0711 0.134 Uiso 1 1 calc R . . H2C H 0.3897 0.8227 0.1079 0.134 Uiso 1 1 calc R . . C3 C 0.6506(6) 0.7431(5) 0.1025(2) 0.0714(17) Uani 1 1 d . . . H3B H 0.7425 0.7173 0.1189 0.107 Uiso 1 1 calc R . . H3C H 0.6447 0.8333 0.1028 0.107 Uiso 1 1 calc R . . H3D H 0.6374 0.7133 0.0660 0.107 Uiso 1 1 calc R . . C4 C 0.5607(7) 0.7326(5) 0.1903(2) 0.091(2) Uani 1 1 d . . . H4B H 0.6529 0.7057 0.2060 0.136 Uiso 1 1 calc R . . H4C H 0.4887 0.6975 0.2104 0.136 Uiso 1 1 calc R . . H4D H 0.5555 0.8229 0.1914 0.136 Uiso 1 1 calc R . . C5 C 0.4935(5) 0.2114(4) 0.11109(19) 0.0446(12) Uani 1 1 d . . . C6 C 0.5336(6) 0.1769(5) 0.0561(2) 0.0653(16) Uani 1 1 d . . . H6A H 0.6333 0.1926 0.0546 0.098 Uiso 1 1 calc R . . H6B H 0.4792 0.2268 0.0293 0.098 Uiso 1 1 calc R . . H6C H 0.5141 0.0893 0.0494 0.098 Uiso 1 1 calc R . . C7 C 0.3375(5) 0.1866(5) 0.1141(2) 0.0625(15) Uani 1 1 d . . . H7A H 0.2824 0.2350 0.0870 0.094 Uiso 1 1 calc R . . H7B H 0.3125 0.2103 0.1491 0.094 Uiso 1 1 calc R . . H7C H 0.3183 0.0986 0.1082 0.094 Uiso 1 1 calc R . . C8 C 0.5805(6) 0.1348(5) 0.1538(2) 0.0674(17) Uani 1 1 d . . . H8A H 0.6800 0.1501 0.1517 0.101 Uiso 1 1 calc R . . H8B H 0.5607 0.0469 0.1480 0.101 Uiso 1 1 calc R . . H8C H 0.5562 0.1588 0.1888 0.101 Uiso 1 1 calc R . . C9 C 0.4358(5) 0.4120(4) 0.27138(19) 0.0480(13) Uani 1 1 d . . . C10 C 0.4331(8) 0.2768(6) 0.2886(3) 0.113(3) Uani 1 1 d . . . H10A H 0.5287 0.2455 0.2946 0.169 Uiso 1 1 calc R . . H10B H 0.3805 0.2281 0.2609 0.169 Uiso 1 1 calc R . . H10C H 0.3882 0.2704 0.3213 0.169 Uiso 1 1 calc R . . C11 C 0.2874(7) 0.4599(8) 0.2628(3) 0.135(4) Uani 1 1 d . . . H11A H 0.2884 0.5468 0.2523 0.202 Uiso 1 1 calc R . . H11B H 0.2433 0.4521 0.2957 0.202 Uiso 1 1 calc R . . H11C H 0.2346 0.4118 0.2349 0.202 Uiso 1 1 calc R . . C12 C 0.5171(9) 0.4836(8) 0.3156(3) 0.146(4) Uani 1 1 d . . . H12A H 0.6130 0.4524 0.3209 0.219 Uiso 1 1 calc R . . H12B H 0.4727 0.4733 0.3483 0.219 Uiso 1 1 calc R . . H12C H 0.5182 0.5712 0.3062 0.219 Uiso 1 1 calc R . . C13 C 0.8928(5) 0.4163(5) 0.12353(18) 0.0458(13) Uani 1 1 d . . . C14 C 0.9538(6) 0.2900(5) 0.1108(2) 0.0760(18) Uani 1 1 d . . . H14A H 0.8872 0.2249 0.1174 0.114 Uiso 1 1 calc R . . H14B H 1.0413 0.2766 0.1333 0.114 Uiso 1 1 calc R . . H14C H 0.9718 0.2879 0.0736 0.114 Uiso 1 1 calc R . . C15 C 0.8548(5) 0.4215(5) 0.18009(19) 0.0625(16) Uani 1 1 d . . . H15A H 0.7880 0.3558 0.1856 0.094 Uiso 1 1 calc R . . H15B H 0.8128 0.5018 0.1865 0.094 Uiso 1 1 calc R . . H15C H 0.9391 0.4103 0.2046 0.094 Uiso 1 1 calc R . . C16 C 0.9995(5) 0.5182(5) 0.1139(2) 0.0639(16) Uani 1 1 d . . . H16A H 0.9618 0.5989 0.1224 0.096 Uiso 1 1 calc R . . H16B H 1.0179 0.5171 0.0767 0.096 Uiso 1 1 calc R . . H16C H 1.0867 0.5033 0.1364 0.096 Uiso 1 1 calc R . . C4S C -0.0516(11) 0.1964(9) -0.0345(4) 0.185(4) Uiso 1 1 d D . . C2S C 0.1266(8) 0.0323(7) -0.0033(3) 0.114(3) Uiso 1 1 d D . . C1S C 0.1467(14) -0.0853(9) 0.0182(5) 0.087(4) Uiso 0.50 1 d PD . . C3S C -0.0137(9) 0.0716(9) -0.0127(5) 0.079(4) Uiso 0.50 1 d PD . . C5S C 0.0822(11) 0.1461(9) -0.0263(5) 0.099(4) Uiso 0.50 1 d PD . . 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 0.0288(5) 0.0435(5) 0.0271(4) 0.0001(4) 0.0021(3) 0.0025(4) Cl1 0.0315(7) 0.0974(11) 0.0344(7) 0.0131(6) 0.0043(5) 0.0008(6) P1 0.0292(7) 0.0369(7) 0.0291(6) -0.0011(5) 0.0019(5) 0.0031(5) P2 0.0326(7) 0.0402(7) 0.0305(7) 0.0020(5) 0.0029(5) 0.0028(5) N1 0.039(2) 0.033(2) 0.030(2) -0.0006(16) 0.0030(16) 0.0054(17) N2 0.035(2) 0.031(2) 0.035(2) 0.0024(16) 0.0025(17) -0.0012(17) N3 0.044(2) 0.053(3) 0.026(2) 0.0040(17) 0.0024(17) 0.0028(19) N4 0.025(2) 0.050(2) 0.038(2) -0.0005(18) -0.0045(17) 0.0061(17) C1 0.051(3) 0.037(3) 0.040(3) -0.002(2) 0.007(2) 0.001(2) C2 0.077(5) 0.054(4) 0.133(6) 0.008(4) -0.003(4) 0.026(3) C3 0.100(5) 0.039(3) 0.080(4) -0.002(3) 0.036(3) -0.008(3) C4 0.175(7) 0.046(4) 0.053(4) -0.009(3) 0.019(4) -0.009(4) C5 0.051(3) 0.036(3) 0.047(3) -0.002(2) 0.007(2) 0.000(2) C6 0.087(4) 0.047(3) 0.065(4) -0.014(3) 0.019(3) -0.004(3) C7 0.062(4) 0.057(4) 0.070(4) -0.011(3) 0.013(3) -0.019(3) C8 0.080(4) 0.040(3) 0.080(4) 0.011(3) -0.002(3) 0.008(3) C9 0.054(3) 0.052(3) 0.039(3) 0.002(2) 0.008(2) 0.004(3) C10 0.156(7) 0.083(5) 0.111(6) 0.033(4) 0.071(5) 0.005(5) C11 0.106(6) 0.224(10) 0.085(6) 0.065(6) 0.064(5) 0.084(6) C12 0.183(9) 0.209(9) 0.051(4) -0.046(5) 0.039(5) -0.093(7) C13 0.029(3) 0.072(4) 0.035(3) 0.013(2) -0.001(2) 0.005(2) C14 0.055(4) 0.087(5) 0.083(4) 0.008(3) -0.013(3) 0.031(3) C15 0.038(3) 0.107(5) 0.041(3) 0.018(3) -0.006(2) 0.006(3) C16 0.037(3) 0.101(5) 0.052(3) 0.008(3) -0.004(2) 0.000(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 Cl1 2.1662(13) . ? Ni1 Cl1 2.1662(13) 3_665 ? Ni1 P1 2.2763(13) 3_665 ? Ni1 P1 2.2763(13) . ? P1 N4 1.644(4) . ? P1 N2 1.687(4) . ? P1 N1 1.696(4) . ? P1 P2 2.5766(18) . ? P2 N3 1.669(3) . ? P2 N1 1.739(4) . ? P2 N2 1.739(4) . ? N1 C1 1.486(5) . ? N2 C5 1.495(5) . ? N3 C9 1.491(6) . ? N4 C13 1.503(5) . ? C1 C4 1.501(6) . ? C1 C3 1.511(6) . ? C1 C2 1.530(6) . ? C5 C6 1.519(6) . ? C5 C7 1.522(6) . ? C5 C8 1.529(6) . ? C9 C11 1.501(7) . ? C9 C12 1.501(8) . ? C9 C10 1.514(7) . ? C13 C15 1.507(6) . ? C13 C14 1.522(7) . ? C13 C16 1.530(6) . ? C4S C5S 1.381(5) . ? C4S C3S 1.478(5) . ? C4S C1S 1.579(13) 3 ? C2S C1S 1.378(5) . ? C2S C5S 1.398(4) . ? C2S C3S 1.400(5) . ? C2S C3S 1.630(13) 3 ? C1S C3S 1.271(14) 3 ? C1S C4S 1.579(13) 3 ? C3S C1S 1.271(14) 3 ? C3S C5S 1.288(16) . ? C3S C2S 1.630(13) 3 ? C3S C3S 1.675(18) 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 Cl1 Ni1 Cl1 180.00(6) . 3_665 ? Cl1 Ni1 P1 93.55(5) . 3_665 ? Cl1 Ni1 P1 86.45(5) 3_665 3_665 ? Cl1 Ni1 P1 86.45(5) . . ? Cl1 Ni1 P1 93.55(5) 3_665 . ? P1 Ni1 P1 180.00(6) 3_665 . ? N4 P1 N2 112.97(18) . . ? N4 P1 N1 115.11(18) . . ? N2 P1 N1 82.19(17) . . ? N4 P1 Ni1 108.47(14) . . ? N2 P1 Ni1 120.85(12) . . ? N1 P1 Ni1 115.53(12) . . ? N4 P1 P2 132.28(14) . . ? N2 P1 P2 41.99(12) . . ? N1 P1 P2 42.02(13) . . ? Ni1 P1 P2 119.23(6) . . ? N3 P2 N1 104.55(17) . . ? N3 P2 N2 104.90(17) . . ? N1 P2 N2 79.53(17) . . ? N3 P2 P1 118.44(14) . . ? N1 P2 P1 40.78(12) . . ? N2 P2 P1 40.48(12) . . ? C1 N1 P1 129.3(3) . . ? C1 N1 P2 126.3(3) . . ? P1 N1 P2 97.20(18) . . ? C5 N2 P1 131.6(3) . . ? C5 N2 P2 126.6(3) . . ? P1 N2 P2 97.54(18) . . ? C9 N3 P2 125.9(3) . . ? C13 N4 P1 136.6(3) . . ? N1 C1 C4 108.5(4) . . ? N1 C1 C3 108.8(4) . . ? C4 C1 C3 109.3(4) . . ? N1 C1 C2 111.0(4) . . ? C4 C1 C2 110.4(5) . . ? C3 C1 C2 108.8(4) . . ? N2 C5 C6 109.1(4) . . ? N2 C5 C7 110.0(4) . . ? C6 C5 C7 110.0(4) . . ? N2 C5 C8 108.2(4) . . ? C6 C5 C8 109.9(4) . . ? C7 C5 C8 109.5(4) . . ? N3 C9 C11 112.5(4) . . ? N3 C9 C12 107.9(5) . . ? C11 C9 C12 109.8(6) . . ? N3 C9 C10 110.0(4) . . ? C11 C9 C10 109.0(5) . . ? C12 C9 C10 107.5(6) . . ? N4 C13 C15 112.4(4) . . ? N4 C13 C14 107.0(4) . . ? C15 C13 C14 111.5(4) . . ? N4 C13 C16 105.9(4) . . ? C15 C13 C16 110.7(4) . . ? C14 C13 C16 109.1(4) . . ? C5S C4S C3S 53.4(7) . . ? C5S C4S C1S 102.3(8) . 3 ? C3S C4S C1S 49.0(6) . 3 ? C1S C2S C5S 170.4(10) . . ? C1S C2S C3S 115.7(9) . . ? C5S C2S C3S 54.8(7) . . ? C1S C2S C3S 49.1(6) . 3 ? C5S C2S C3S 121.4(9) . 3 ? C3S C2S C3S 66.6(7) . 3 ? C3S C1S C2S 75.8(8) 3 . ? C3S C1S C4S 61.4(6) 3 3 ? C2S C1S C4S 137.1(11) . 3 ? C1S C3S C5S 128.9(7) 3 . ? C1S C3S C2S 168.4(9) 3 . ? C5S C3S C2S 62.5(4) . . ? C1S C3S C4S 69.6(7) 3 . ? C5S C3S C4S 59.5(4) . . ? C2S C3S C4S 121.9(7) . . ? C1S C3S C2S 55.1(5) 3 3 ? C5S C3S C2S 175.2(10) . 3 ? C2S C3S C2S 113.4(7) . 3 ? C4S C3S C2S 124.7(8) . 3 ? C1S C3S C3S 105.2(9) 3 3 ? C5S C3S C3S 125.7(8) . 3 ? C2S C3S C3S 63.3(6) . 3 ? C4S C3S C3S 174.8(10) . 3 ? C2S C3S C3S 50.1(5) 3 3 ? C3S C5S C4S 67.1(5) . . ? C3S C5S C2S 62.7(4) . . ? C4S C5S C2S 129.7(9) . . ? 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 Cl1 Ni1 P1 N4 167.40(14) . . . . ? Cl1 Ni1 P1 N4 -12.60(14) 3_665 . . . ? P1 Ni1 P1 N4 -94(75) 3_665 . . . ? Cl1 Ni1 P1 N2 34.66(15) . . . . ? Cl1 Ni1 P1 N2 -145.34(15) 3_665 . . . ? P1 Ni1 P1 N2 134(72) 3_665 . . . ? Cl1 Ni1 P1 N1 -61.66(15) . . . . ? Cl1 Ni1 P1 N1 118.34(15) 3_665 . . . ? P1 Ni1 P1 N1 37(75) 3_665 . . . ? Cl1 Ni1 P1 P2 -14.20(7) . . . . ? Cl1 Ni1 P1 P2 165.80(7) 3_665 . . . ? P1 Ni1 P1 P2 85(26) 3_665 . . . ? N4 P1 P2 N3 2.2(3) . . . . ? N2 P1 P2 N3 79.4(2) . . . . ? N1 P1 P2 N3 -79.0(2) . . . . ? Ni1 P1 P2 N3 -175.73(15) . . . . ? N4 P1 P2 N1 81.2(2) . . . . ? N2 P1 P2 N1 158.4(2) . . . . ? Ni1 P1 P2 N1 -96.71(17) . . . . ? N4 P1 P2 N2 -77.2(2) . . . . ? N1 P1 P2 N2 -158.4(2) . . . . ? Ni1 P1 P2 N2 104.88(17) . . . . ? N4 P1 N1 C1 82.8(4) . . . . ? N2 P1 N1 C1 -165.5(4) . . . . ? Ni1 P1 N1 C1 -44.9(4) . . . . ? P2 P1 N1 C1 -151.1(4) . . . . ? N4 P1 N1 P2 -126.14(18) . . . . ? N2 P1 N1 P2 -14.39(16) . . . . ? Ni1 P1 N1 P2 106.16(13) . . . . ? N3 P2 N1 C1 -90.7(4) . . . . ? N2 P2 N1 C1 166.4(4) . . . . ? P1 P2 N1 C1 152.4(4) . . . . ? N3 P2 N1 P1 116.90(18) . . . . ? N2 P2 N1 P1 14.06(16) . . . . ? N4 P1 N2 C5 -74.4(4) . . . . ? N1 P1 N2 C5 171.6(4) . . . . ? Ni1 P1 N2 C5 56.5(4) . . . . ? P2 P1 N2 C5 157.2(5) . . . . ? N4 P1 N2 P2 128.42(18) . . . . ? N1 P1 N2 P2 14.40(16) . . . . ? Ni1 P1 N2 P2 -100.75(14) . . . . ? N3 P2 N2 C5 84.6(4) . . . . ? N1 P2 N2 C5 -173.0(3) . . . . ? P1 P2 N2 C5 -158.9(4) . . . . ? N3 P2 N2 P1 -116.57(18) . . . . ? N1 P2 N2 P1 -14.15(16) . . . . ? N1 P2 N3 C9 140.7(4) . . . . ? N2 P2 N3 C9 -136.5(4) . . . . ? P1 P2 N3 C9 -177.8(3) . . . . ? N2 P1 N4 C13 -47.3(5) . . . . ? N1 P1 N4 C13 44.7(5) . . . . ? Ni1 P1 N4 C13 175.9(4) . . . . ? P2 P1 N4 C13 -2.2(5) . . . . ? P1 N1 C1 C4 -152.5(4) . . . . ? P2 N1 C1 C4 64.0(5) . . . . ? P1 N1 C1 C3 -33.7(5) . . . . ? P2 N1 C1 C3 -177.2(3) . . . . ? P1 N1 C1 C2 86.0(5) . . . . ? P2 N1 C1 C2 -57.4(5) . . . . ? P1 N2 C5 C6 -1.5(6) . . . . ? P2 N2 C5 C6 149.9(3) . . . . ? P1 N2 C5 C7 -122.3(4) . . . . ? P2 N2 C5 C7 29.1(5) . . . . ? P1 N2 C5 C8 118.0(4) . . . . ? P2 N2 C5 C8 -90.5(4) . . . . ? P2 N3 C9 C11 -17.3(7) . . . . ? P2 N3 C9 C12 -138.6(5) . . . . ? P2 N3 C9 C10 104.4(5) . . . . ? P1 N4 C13 C15 -6.4(7) . . . . ? P1 N4 C13 C14 116.3(5) . . . . ? P1 N4 C13 C16 -127.4(4) . . . . ? C5S C2S C1S C3S -9(7) . . . 3 ? C3S C2S C1S C3S 1.0(15) . . . 3 ? C5S C2S C1S C4S -7(7) . . . 3 ? C3S C2S C1S C4S 3(2) . . . 3 ? C3S C2S C1S C4S 1.6(13) 3 . . 3 ? C1S C2S C3S C1S -5(7) . . . 3 ? C5S C2S C3S C1S 173(7) . . . 3 ? C3S C2S C3S C1S -4(6) 3 . . 3 ? C1S C2S C3S C5S -178.0(12) . . . . ? C3S C2S C3S C5S -177.2(14) 3 . . . ? C1S C2S C3S C4S 178.7(11) . . . . ? C5S C2S C3S C4S -3.3(11) . . . . ? C3S C2S C3S C4S 179.5(17) 3 . . . ? C1S C2S C3S C2S -0.8(12) . . . 3 ? C5S C2S C3S C2S 177.2(14) . . . 3 ? C3S C2S C3S C2S 0.0 3 . . 3 ? C1S C2S C3S C3S -0.8(12) . . . 3 ? C5S C2S C3S C3S 177.2(14) . . . 3 ? C5S C4S C3S C1S -175.8(14) . . . 3 ? C1S C4S C3S C5S 175.8(14) 3 . . . ? C5S C4S C3S C2S 3.4(11) . . . . ? C1S C4S C3S C2S 179.2(16) 3 . . . ? C5S C4S C3S C2S -177.1(15) . . . 3 ? C1S C4S C3S C2S -1.3(10) 3 . . 3 ? C5S C4S C3S C3S 179(100) . . . 3 ? C1S C4S C3S C3S -5(16) 3 . . 3 ? C1S C3S C5S C4S 5.0(17) 3 . . . ? C2S C3S C5S C4S -176.7(11) . . . . ? C2S C3S C5S C4S 150(14) 3 . . . ? C3S C3S C5S C4S -179.9(18) 3 . . . ? C1S C3S C5S C2S -178.2(18) 3 . . . ? C4S C3S C5S C2S 176.7(11) . . . . ? C2S C3S C5S C2S -33(14) 3 . . . ? C3S C3S C5S C2S -3.1(15) 3 . . . ? C1S C4S C5S C3S -3.2(11) 3 . . . ? C3S C4S C5S C2S -3.8(13) . . . . ? C1S C4S C5S C2S -7.0(18) 3 . . . ? C1S C2S C5S C3S 11(7) . . . . ? C3S C2S C5S C3S 3.1(15) 3 . . . ? C1S C2S C5S C4S 15(7) . . . . ? C3S C2S C5S C4S 3.9(13) . . . . ? C3S C2S C5S C4S 7(2) 3 . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.76 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.192 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.083 #===END=== data_3 _database_code_depnum_ccdc_archive 'CCDC 272421' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H30 Cl2 Ni P2' _chemical_formula_weight 365.91 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' 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 7.3453(10) _cell_length_b 11.4847(15) _cell_length_c 10.8061(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.990(2) _cell_angle_gamma 90.00 _cell_volume 911.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description chunk _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data was collected using a BRUKER SMART CCD (charge coupled device) based diffractometer equipped with an LT-2 low-temperature apparatus operating at 213 K. A suitable crystal was chosen and mounted on a glass fiber with grease. Data were measured using omega scans of 0.3\% per frame for 30 s , such that a hemisphere was collected. A total of 1271 frames were collected with a final resolution of 0.75 \%A. The first 50 frames were recollected at the end of data collection to monitor for decay. Cell parameters were retrieved using SMART software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp and decay. Absorption corrections were applied using SADABS based on Blessing, (1995). The structures are solved by the direct method using the SHELX-90 program and refined by least squares method on F2 SHELXL-93, incorporated in SHELXTL V5.1. Carbon-bound H atoms were placed in idealized positions and refined as a riding model. ; _diffrn_ambient_temperature 213(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5935 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2211 _reflns_number_gt 2011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (BRUKER, V5.007, 1997)' _computing_cell_refinement 'SMART (BRUKER, V5.054, 1998)' _computing_data_reduction 'SAINT (BRUKER, V6.01, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (BRUKER, 1998, V5.1)' _computing_publication_material 'XCIF (Sheldrick and BRUKER, 1997, V5.1)' _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^)+(0.1031P)^2^+0.3789P] 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 2211 _refine_ls_number_parameters 79 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 0.753 _refine_ls_restrained_S_all 0.753 _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 0.0000 1.0000 0.0000 0.03223(13) Uani 1 2 d S . . P1 P 0.11617(7) 0.83381(4) 0.07394(4) 0.03761(15) Uani 1 1 d . . . Cl1 Cl 0.06138(9) 0.95460(5) -0.18899(4) 0.05337(18) Uani 1 1 d . . . C1 C 0.2306(3) 0.73834(19) -0.0358(2) 0.0462(5) Uani 1 1 d . . . H1A H 0.1533 0.7317 -0.1103 0.055 Uiso 1 1 calc R . . H1B H 0.3443 0.7760 -0.0601 0.055 Uiso 1 1 calc R . . C2 C 0.2759(4) 0.6155(2) 0.0097(3) 0.0616(6) Uani 1 1 d . . . H2A H 0.3359 0.5727 -0.0554 0.092 Uiso 1 1 calc R . . H2B H 0.1645 0.5757 0.0315 0.092 Uiso 1 1 calc R . . H2C H 0.3560 0.6201 0.0818 0.092 Uiso 1 1 calc R . . C3 C 0.2791(4) 0.8521(2) 0.2014(2) 0.0632(7) Uani 1 1 d . . . H3A H 0.2142 0.8794 0.2744 0.076 Uiso 1 1 calc R . . H3B H 0.3328 0.7762 0.2217 0.076 Uiso 1 1 calc R . . C4 C 0.4289(4) 0.9362(3) 0.1737(4) 0.0859(10) Uani 1 1 d . . . H4A H 0.5107 0.9420 0.2449 0.129 Uiso 1 1 calc R . . H4B H 0.3772 1.0121 0.1556 0.129 Uiso 1 1 calc R . . H4C H 0.4959 0.9088 0.1028 0.129 Uiso 1 1 calc R . . C5 C -0.0644(4) 0.7452(2) 0.1399(2) 0.0567(6) Uani 1 1 d . . . H5A H -0.0105 0.6749 0.1763 0.068 Uiso 1 1 calc R . . H5B H -0.1219 0.7891 0.2065 0.068 Uiso 1 1 calc R . . C6 C -0.2085(4) 0.7102(3) 0.0460(3) 0.0719(8) Uani 1 1 d . . . H6A H -0.3004 0.6635 0.0861 0.108 Uiso 1 1 calc R . . H6B H -0.1532 0.6651 -0.0192 0.108 Uiso 1 1 calc R . . H6C H -0.2646 0.7794 0.0109 0.108 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 0.0452(2) 0.0277(2) 0.02370(19) 0.00036(10) -0.00196(13) 0.00061(11) P1 0.0555(3) 0.0298(3) 0.0274(2) 0.00069(16) -0.0032(2) 0.00397(19) Cl1 0.0870(4) 0.0469(3) 0.0262(3) -0.00088(19) 0.0025(2) 0.0175(3) C1 0.0622(12) 0.0363(10) 0.0402(10) -0.0027(8) 0.0021(9) 0.0099(9) C2 0.0809(16) 0.0418(12) 0.0620(15) -0.0031(10) -0.0026(12) 0.0203(11) C3 0.0891(18) 0.0503(12) 0.0490(13) -0.0095(10) -0.0305(12) 0.0193(13) C4 0.0779(19) 0.078(2) 0.101(3) -0.0217(19) -0.0384(18) 0.0071(16) C5 0.0887(17) 0.0383(11) 0.0437(11) 0.0104(9) 0.0188(11) 0.0007(11) C6 0.0745(17) 0.0577(16) 0.084(2) 0.0045(14) 0.0130(15) -0.0201(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 Ni1 Cl1 2.1628(5) 3_575 ? Ni1 Cl1 2.1628(5) . ? Ni1 P1 2.2329(5) 3_575 ? Ni1 P1 2.2329(5) . ? P1 C3 1.822(2) . ? P1 C5 1.826(2) . ? P1 C1 1.830(2) . ? C1 C2 1.529(3) . ? C3 C4 1.498(5) . ? C5 C6 1.507(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 Cl1 Ni1 Cl1 180.0 3_575 . ? Cl1 Ni1 P1 92.70(2) 3_575 3_575 ? Cl1 Ni1 P1 87.30(2) . 3_575 ? Cl1 Ni1 P1 87.30(2) 3_575 . ? Cl1 Ni1 P1 92.70(2) . . ? P1 Ni1 P1 180.0 3_575 . ? C3 P1 C5 103.97(14) . . ? C3 P1 C1 104.83(12) . . ? C5 P1 C1 105.31(12) . . ? C3 P1 Ni1 114.47(9) . . ? C5 P1 Ni1 109.88(9) . . ? C1 P1 Ni1 117.21(7) . . ? C2 C1 P1 116.38(17) . . ? C4 C3 P1 113.5(2) . . ? C6 C5 P1 113.11(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Ni1 P1 C3 -50.56(12) 3_575 . . . ? Cl1 Ni1 P1 C3 129.44(12) . . . . ? P1 Ni1 P1 C3 134(74) 3_575 . . . ? Cl1 Ni1 P1 C5 65.96(9) 3_575 . . . ? Cl1 Ni1 P1 C5 -114.04(9) . . . . ? P1 Ni1 P1 C5 -110(71) 3_575 . . . ? Cl1 Ni1 P1 C1 -173.94(9) 3_575 . . . ? Cl1 Ni1 P1 C1 6.06(9) . . . . ? P1 Ni1 P1 C1 10(69) 3_575 . . . ? C3 P1 C1 C2 63.5(2) . . . . ? C5 P1 C1 C2 -45.9(2) . . . . ? Ni1 P1 C1 C2 -168.38(16) . . . . ? C5 P1 C3 C4 -172.2(2) . . . . ? C1 P1 C3 C4 77.5(2) . . . . ? Ni1 P1 C3 C4 -52.4(2) . . . . ? C3 P1 C5 C6 -175.0(2) . . . . ? C1 P1 C5 C6 -65.1(2) . . . . ? Ni1 P1 C5 C6 62.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.355 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.051 #===END=== data_8 _database_code_depnum_ccdc_archive 'CCDC 272422' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H60 Cl N3 Ni P2 Si' _chemical_formula_weight 598.96 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' Si Si 0.0817 0.0704 '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 10.8581(13) _cell_length_b 21.494(3) _cell_length_c 15.1459(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.934(2) _cell_angle_gamma 90.00 _cell_volume 3526.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'red brown' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Data was collected using a BRUKER SMART CCD (charge coupled device) based diffractometer equipped with an LT-2 low-temperature apparatus operating at 213 K. A suitable crystal was chosen and mounted on a glass fiber using grease. Data were measured using omega scans of 0.3\% per frame for 10 s , such that a hemisphere was collected. A total of 1271 frames were collected with a final resolution of 0.75 \%A. The first 50 frames were recollected at the end of data collection to monitor for decay. Cell parameters were retrieved using SMART software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp and decay. Absorption corrections were applied using SADABS based on Blessing, (1995). The structures are solved by the direct method using the SHELX-90 program and refined by least squares method on F2 SHELXL-93, incorporated in SHELXTL V5.1. Carbon-bound H atoms were placed in idealized positions and refined as a riding model. ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w, 0.3 deg' _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 25345 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.31 _reflns_number_total 8743 _reflns_number_gt 6258 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (BRUKER, V5.007, 1997)' _computing_cell_refinement 'SMART (BRUKER, V5.054, 1998)' _computing_data_reduction 'SAINT (BRUKER, V6.01, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (BRUKER, 1998, V5.1)' _computing_publication_material 'XCIF (Sheldrick and BRUKER, 1997, V5.1)' _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^)+(0.1099P)^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 8743 _refine_ls_number_parameters 325 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1660 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.022 _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 0.85830(3) 0.209959(14) 0.32194(2) 0.04029(12) Uani 1 1 d . A . Cl1 Cl 0.81317(7) 0.17085(3) 0.45155(5) 0.0579(2) Uani 1 1 d . . . Si Si 0.95767(7) 0.32972(4) 0.09446(5) 0.0512(2) Uani 1 1 d . . . P1 P 0.90181(6) 0.28228(3) 0.23943(4) 0.03761(15) Uani 1 1 d . A . P2 P 0.84850(9) 0.12430(4) 0.24980(5) 0.0632(2) Uani 1 1 d D . . N1 N 0.82546(19) 0.31254(10) 0.14904(14) 0.0445(5) Uani 1 1 d . . . N2 N 1.0323(2) 0.30000(11) 0.19145(14) 0.0492(5) Uani 1 1 d . . . N3 N 0.8763(2) 0.29916(10) 0.33666(14) 0.0459(5) Uani 1 1 d . . . C1 C 0.9779(3) 0.2850(2) -0.0075(2) 0.0760(11) Uani 1 1 d . . . H1A H 0.9990 0.3131 -0.0542 0.114 Uiso 1 1 calc R . . H1B H 0.9016 0.2635 -0.0254 0.114 Uiso 1 1 calc R . . H1C H 1.0436 0.2548 0.0034 0.114 Uiso 1 1 calc R . . C2 C 0.9837(4) 0.41300(19) 0.0725(3) 0.0914(13) Uani 1 1 d . . . H2A H 1.0039 0.4183 0.0115 0.137 Uiso 1 1 calc R . . H2B H 1.0514 0.4281 0.1118 0.137 Uiso 1 1 calc R . . H2C H 0.9094 0.4363 0.0826 0.137 Uiso 1 1 calc R . . C10 C 0.6924(3) 0.32361(14) 0.12865(19) 0.0543(7) Uani 1 1 d . . . C11 C 0.6673(3) 0.3196(2) 0.0291(2) 0.0751(10) Uani 1 1 d . . . H11A H 0.6886 0.2783 0.0091 0.113 Uiso 1 1 calc R . . H11B H 0.7167 0.3503 0.0008 0.113 Uiso 1 1 calc R . . H11C H 0.5804 0.3274 0.0138 0.113 Uiso 1 1 calc R . . C12 C 0.6145(3) 0.27574(19) 0.1727(3) 0.0727(10) Uani 1 1 d . . . H12A H 0.6350 0.2345 0.1523 0.109 Uiso 1 1 calc R . . H12B H 0.5278 0.2840 0.1576 0.109 Uiso 1 1 calc R . . H12C H 0.6308 0.2781 0.2364 0.109 Uiso 1 1 calc R . . C13 C 0.6597(4) 0.38889(19) 0.1610(3) 0.0899(12) Uani 1 1 d . . . H13A H 0.6762 0.3912 0.2246 0.135 Uiso 1 1 calc R . . H13B H 0.5729 0.3971 0.1460 0.135 Uiso 1 1 calc R . . H13C H 0.7092 0.4196 0.1327 0.135 Uiso 1 1 calc R . . C20 C 1.1623(3) 0.28445(16) 0.21745(19) 0.0567(7) Uani 1 1 d . . . C21 C 1.2080(4) 0.2339(2) 0.1579(3) 0.0835(11) Uani 1 1 d . . . H21A H 1.1611 0.1961 0.1655 0.125 Uiso 1 1 calc R . . H21B H 1.2947 0.2260 0.1733 0.125 Uiso 1 1 calc R . . H21C H 1.1972 0.2473 0.0967 0.125 Uiso 1 1 calc R . . C22 C 1.1783(3) 0.2652(3) 0.3131(2) 0.1066(17) Uani 1 1 d . . . H22A H 1.1296 0.2281 0.3221 0.160 Uiso 1 1 calc R . . H22B H 1.1509 0.2985 0.3501 0.160 Uiso 1 1 calc R . . H22C H 1.2647 0.2564 0.3286 0.160 Uiso 1 1 calc R . . C23 C 1.2397(3) 0.3421(2) 0.2020(3) 0.0919(12) Uani 1 1 d . . . H23A H 1.2134 0.3759 0.2388 0.138 Uiso 1 1 calc R . . H23B H 1.2288 0.3542 0.1402 0.138 Uiso 1 1 calc R . . H23C H 1.3260 0.3330 0.2171 0.138 Uiso 1 1 calc R . . C30 C 0.8714(3) 0.34783(13) 0.40369(19) 0.0556(7) Uani 1 1 d . A . C31 C 0.9158(4) 0.40895(16) 0.3656(3) 0.0813(11) Uani 1 1 d . . . H31A H 1.0006 0.4044 0.3503 0.122 Uiso 1 1 calc R A . H31B H 0.9109 0.4417 0.4093 0.122 Uiso 1 1 calc R . . H31C H 0.8641 0.4196 0.3130 0.122 Uiso 1 1 calc R . . C32 C 0.7375(3) 0.35388(19) 0.4287(2) 0.0806(11) Uani 1 1 d . . . H32A H 0.7110 0.3148 0.4533 0.121 Uiso 1 1 calc R A . H32B H 0.6848 0.3640 0.3764 0.121 Uiso 1 1 calc R . . H32C H 0.7321 0.3866 0.4724 0.121 Uiso 1 1 calc R . . C33 C 0.9539(4) 0.32902(18) 0.4848(2) 0.0755(10) Uani 1 1 d . . . H33A H 0.9243 0.2903 0.5084 0.113 Uiso 1 1 calc R A . H33B H 0.9520 0.3613 0.5295 0.113 Uiso 1 1 calc R . . H33C H 1.0379 0.3236 0.4681 0.113 Uiso 1 1 calc R . . C40 C 0.8565(4) 0.13192(17) 0.1313(2) 0.0795(10) Uani 1 1 d . A . H40A H 0.7976 0.1643 0.1109 0.095 Uiso 1 1 calc R . . H40B H 0.9391 0.1474 0.1206 0.095 Uiso 1 1 calc R . . C41 C 0.8317(5) 0.07474(19) 0.0722(3) 0.1028(15) Uani 1 1 d . . . H41A H 0.8894 0.0417 0.0919 0.123 Uiso 1 1 calc R A . H41B H 0.7480 0.0597 0.0802 0.123 Uiso 1 1 calc R . . C42 C 0.8440(7) 0.0864(2) -0.0246(3) 0.137(2) Uani 1 1 d D A . H42A H 0.7859 0.1192 -0.0442 0.164 Uiso 1 1 calc R . . H42B H 0.9275 0.1018 -0.0323 0.164 Uiso 1 1 calc R . . C43 C 0.8215(9) 0.0323(3) -0.0815(4) 0.205(5) Uani 1 1 d D . . H43A H 0.8316 0.0439 -0.1425 0.308 Uiso 1 1 calc R A . H43B H 0.7381 0.0173 -0.0760 0.308 Uiso 1 1 calc R . . H43C H 0.8799 -0.0003 -0.0638 0.308 Uiso 1 1 calc R . . C44 C 0.7173(7) 0.0774(2) 0.2701(4) 0.126(2) Uani 1 1 d . A . H44A H 0.7178 0.0399 0.2333 0.151 Uiso 1 1 calc R . . H44B H 0.7229 0.0643 0.3323 0.151 Uiso 1 1 calc R . . C45 C 0.6045(7) 0.1101(3) 0.2513(4) 0.158(3) Uani 1 1 d . . . H45A H 0.5930 0.1160 0.1871 0.189 Uiso 1 1 calc R A . H45B H 0.6126 0.1515 0.2782 0.189 Uiso 1 1 calc R . . C46 C 0.4821(9) 0.0781(5) 0.2843(4) 0.209(5) Uani 1 1 d D A . H46A H 0.5038 0.0377 0.3111 0.250 Uiso 1 1 calc R . . H46B H 0.4486 0.1043 0.3298 0.250 Uiso 1 1 calc R . . C47 C 0.3899(8) 0.0692(8) 0.2139(7) 0.342(10) Uani 1 1 d D . . H47A H 0.3187 0.0489 0.2364 0.513 Uiso 1 1 calc R A . H47B H 0.4228 0.0435 0.1684 0.513 Uiso 1 1 calc R . . H47C H 0.3654 0.1093 0.1889 0.513 Uiso 1 1 calc R . . C48 C 0.9314(7) 0.0569(3) 0.3049(6) 0.086(2) Uani 0.50 1 d PD A 1 H48A H 0.8980 0.0496 0.3625 0.104 Uiso 0.50 1 calc PR A 1 H48B H 0.9155 0.0195 0.2688 0.104 Uiso 0.50 1 calc PR A 1 C48B C 0.9951(7) 0.0762(3) 0.2645(3) 0.0658(18) Uani 0.50 1 d PD A 2 H48C H 0.9874 0.0406 0.2240 0.079 Uiso 0.50 1 calc PR A 2 H48D H 1.0643 0.1016 0.2470 0.079 Uiso 0.50 1 calc PR A 2 C49 C 1.0641(8) 0.0662(4) 0.3180(12) 0.160(8) Uani 0.50 1 d PD A 1 H49A H 1.0790 0.1026 0.3561 0.192 Uiso 0.50 1 calc PR A 1 H49B H 1.0957 0.0759 0.2605 0.192 Uiso 0.50 1 calc PR A 1 C49B C 1.0246(5) 0.0529(3) 0.3540(3) 0.0494(14) Uani 0.50 1 d PD A 2 H49C H 0.9551 0.0285 0.3732 0.059 Uiso 0.50 1 calc PR A 2 H49D H 1.0379 0.0881 0.3948 0.059 Uiso 0.50 1 calc PR A 2 C50 C 1.1358(5) 0.0141(3) 0.3569(4) 0.143(2) Uani 1 1 d D . . H50A H 1.0996 -0.0220 0.3285 0.171 Uiso 1 1 d R A . H50B H 1.2163 0.0177 0.3347 0.171 Uiso 1 1 d R . . C51 C 1.1655(6) -0.0072(3) 0.4467(4) 0.142(2) Uani 1 1 d D A . H51A H 1.2155 -0.0445 0.4455 0.213 Uiso 1 1 calc R . . H51B H 1.0898 -0.0162 0.4747 0.213 Uiso 1 1 calc R . . H51C H 1.2110 0.0250 0.4798 0.213 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 0.0428(2) 0.04243(19) 0.03609(18) 0.00276(12) 0.00586(13) 0.00264(12) Cl1 0.0638(4) 0.0639(4) 0.0478(4) 0.0111(3) 0.0164(3) -0.0004(3) Si 0.0478(4) 0.0696(5) 0.0360(3) 0.0112(3) 0.0006(3) -0.0113(4) P1 0.0378(3) 0.0435(3) 0.0318(3) 0.0017(2) 0.0043(2) 0.0004(2) P2 0.0899(6) 0.0435(4) 0.0548(4) -0.0018(3) -0.0062(4) 0.0070(4) N1 0.0395(11) 0.0526(12) 0.0411(11) 0.0095(9) 0.0005(9) 0.0013(9) N2 0.0385(11) 0.0754(15) 0.0338(10) 0.0081(10) 0.0026(9) -0.0073(10) N3 0.0568(13) 0.0438(11) 0.0381(11) -0.0013(8) 0.0105(10) -0.0016(9) C1 0.0551(19) 0.134(3) 0.0392(15) -0.0015(17) 0.0044(14) -0.0088(19) C2 0.098(3) 0.088(3) 0.087(3) 0.034(2) -0.002(2) -0.032(2) C10 0.0464(15) 0.0589(16) 0.0572(16) 0.0116(13) 0.0000(12) 0.0084(12) C11 0.0548(18) 0.106(3) 0.0620(19) 0.0184(19) -0.0165(15) -0.0038(18) C12 0.0405(15) 0.093(2) 0.085(2) 0.0218(19) 0.0079(15) 0.0017(15) C13 0.080(3) 0.078(2) 0.110(3) 0.003(2) -0.003(2) 0.034(2) C20 0.0381(14) 0.091(2) 0.0410(14) 0.0035(13) 0.0036(11) -0.0026(13) C21 0.077(2) 0.098(3) 0.075(2) -0.006(2) 0.005(2) 0.017(2) C22 0.0494(19) 0.223(5) 0.0470(19) 0.027(3) -0.0011(15) 0.021(3) C23 0.0494(19) 0.101(3) 0.125(3) -0.007(3) 0.004(2) -0.0174(19) C30 0.0713(19) 0.0521(15) 0.0446(14) -0.0070(12) 0.0131(13) 0.0012(13) C31 0.122(3) 0.0520(18) 0.071(2) -0.0112(16) 0.014(2) -0.0101(19) C32 0.086(3) 0.087(2) 0.073(2) -0.0175(19) 0.0293(19) 0.017(2) C33 0.101(3) 0.082(2) 0.0434(16) -0.0147(15) 0.0040(17) -0.006(2) C40 0.111(3) 0.066(2) 0.0629(19) -0.0176(16) 0.016(2) -0.001(2) C41 0.159(5) 0.075(2) 0.073(2) -0.025(2) 0.000(3) 0.007(3) C42 0.240(8) 0.105(4) 0.066(3) -0.025(2) 0.008(4) 0.024(4) C43 0.383(13) 0.141(5) 0.082(3) -0.048(4) -0.055(5) 0.092(7) C44 0.194(6) 0.081(3) 0.101(3) 0.005(3) -0.017(4) -0.062(4) C45 0.172(6) 0.141(5) 0.147(5) 0.063(4) -0.081(5) -0.093(5) C46 0.263(10) 0.246(9) 0.117(5) 0.003(5) 0.017(6) -0.191(9) C47 0.133(7) 0.62(3) 0.268(13) 0.248(16) -0.013(8) -0.130(12) C48 0.107(7) 0.044(4) 0.111(7) 0.005(4) 0.033(6) 0.008(4) C48B 0.099(6) 0.048(3) 0.052(3) 0.006(3) 0.013(4) 0.023(4) C49 0.077(8) 0.088(8) 0.31(2) -0.019(12) 0.001(11) 0.007(6) C49B 0.042(3) 0.053(3) 0.052(3) -0.008(2) -0.002(3) 0.006(3) C50 0.109(4) 0.135(5) 0.187(6) 0.068(4) 0.028(4) 0.059(4) C51 0.145(6) 0.118(4) 0.165(6) -0.029(4) 0.025(5) 0.017(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 N3 1.939(2) . ? Ni P1 2.0693(7) . ? Ni P2 2.1399(8) . ? Ni Cl1 2.2209(7) . ? Si N1 1.745(2) . ? Si N2 1.749(2) . ? Si C1 1.846(3) . ? Si C2 1.846(4) . ? Si P1 2.5322(9) . ? P1 N3 1.560(2) . ? P1 N2 1.680(2) . ? P1 N1 1.682(2) . ? P2 C44 1.788(5) . ? P2 C40 1.811(4) . ? P2 C48 1.872(5) . ? P2 C48B 1.898(5) . ? N1 C10 1.475(3) . ? N2 C20 1.478(4) . ? N3 C30 1.461(3) . ? C10 C12 1.516(4) . ? C10 C11 1.516(4) . ? C10 C13 1.536(5) . ? C20 C22 1.505(4) . ? C20 C21 1.517(5) . ? C20 C23 1.524(5) . ? C30 C33 1.524(5) . ? C30 C31 1.526(5) . ? C30 C32 1.532(4) . ? C40 C41 1.533(5) . ? C41 C42 1.502(6) . ? C42 C43 1.457(4) . ? C44 C45 1.424(9) . ? C45 C46 1.606(9) . ? C46 C47 1.424(5) . ? C48 C49 1.455(5) . ? C48B C49B 1.460(4) . ? C49 C50 1.464(5) . ? C49B C50 1.466(4) . ? C50 C51 1.450(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 N3 Ni P1 45.66(6) . . ? N3 Ni P2 155.61(7) . . ? P1 Ni P2 110.08(3) . . ? N3 Ni Cl1 107.42(6) . . ? P1 Ni Cl1 153.06(3) . . ? P2 Ni Cl1 96.86(3) . . ? N1 Si N2 82.73(10) . . ? N1 Si C1 115.80(14) . . ? N2 Si C1 115.97(16) . . ? N1 Si C2 115.58(17) . . ? N2 Si C2 115.97(16) . . ? C1 Si C2 109.03(19) . . ? N1 Si P1 41.41(7) . . ? N2 Si P1 41.34(7) . . ? C1 Si P1 124.42(14) . . ? C2 Si P1 126.55(15) . . ? N3 P1 N2 124.42(12) . . ? N3 P1 N1 124.69(12) . . ? N2 P1 N1 86.75(11) . . ? N3 P1 Ni 62.74(8) . . ? N2 P1 Ni 131.75(9) . . ? N1 P1 Ni 131.44(8) . . ? N3 P1 Si 142.52(9) . . ? N2 P1 Si 43.46(8) . . ? N1 P1 Si 43.32(7) . . ? Ni P1 Si 154.74(4) . . ? C44 P2 C40 108.3(2) . . ? C44 P2 C48 81.5(3) . . ? C40 P2 C48 117.2(3) . . ? C44 P2 C48B 110.1(3) . . ? C40 P2 C48B 93.9(2) . . ? C48 P2 C48B 32.0(3) . . ? C44 P2 Ni 114.2(2) . . ? C40 P2 Ni 115.11(12) . . ? C48 P2 Ni 115.7(3) . . ? C48B P2 Ni 113.4(2) . . ? C10 N1 P1 130.81(18) . . ? C10 N1 Si 133.81(17) . . ? P1 N1 Si 95.28(11) . . ? C20 N2 P1 130.70(18) . . ? C20 N2 Si 133.26(17) . . ? P1 N2 Si 95.19(11) . . ? C30 N3 P1 147.12(19) . . ? C30 N3 Ni 141.23(17) . . ? P1 N3 Ni 71.60(9) . . ? N1 C10 C12 111.5(2) . . ? N1 C10 C11 107.8(2) . . ? C12 C10 C11 109.3(3) . . ? N1 C10 C13 109.0(3) . . ? C12 C10 C13 109.3(3) . . ? C11 C10 C13 109.8(3) . . ? N2 C20 C22 111.3(2) . . ? N2 C20 C21 110.4(3) . . ? C22 C20 C21 110.7(3) . . ? N2 C20 C23 107.6(3) . . ? C22 C20 C23 110.1(3) . . ? C21 C20 C23 106.6(3) . . ? N3 C30 C33 108.8(2) . . ? N3 C30 C31 109.0(2) . . ? C33 C30 C31 110.4(3) . . ? N3 C30 C32 108.3(3) . . ? C33 C30 C32 109.7(3) . . ? C31 C30 C32 110.5(3) . . ? C41 C40 P2 119.2(3) . . ? C42 C41 C40 114.4(4) . . ? C43 C42 C41 115.0(5) . . ? C45 C44 P2 111.8(4) . . ? C44 C45 C46 116.4(6) . . ? C47 C46 C45 112.2(6) . . ? C49 C48 P2 113.3(4) . . ? C49B C48B P2 115.1(4) . . ? C48 C49 C50 116.4(6) . . ? C48B C49B C50 110.5(5) . . ? C51 C50 C49 134.2(9) . . ? C51 C50 C49B 109.7(5) . . ? C49 C50 C49B 30.5(6) . . ? 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 P2 Ni P1 N3 176.98(10) . . . . ? Cl1 Ni P1 N3 -2.58(12) . . . . ? N3 Ni P1 N2 113.10(15) . . . . ? P2 Ni P1 N2 -69.92(12) . . . . ? Cl1 Ni P1 N2 110.52(13) . . . . ? N3 Ni P1 N1 -113.52(15) . . . . ? P2 Ni P1 N1 63.46(12) . . . . ? Cl1 Ni P1 N1 -116.11(12) . . . . ? N3 Ni P1 Si -179.74(13) . . . . ? P2 Ni P1 Si -2.76(9) . . . . ? Cl1 Ni P1 Si 177.67(7) . . . . ? N1 Si P1 N3 -88.86(19) . . . . ? N2 Si P1 N3 88.5(2) . . . . ? C1 Si P1 N3 179.9(2) . . . . ? C2 Si P1 N3 -0.5(2) . . . . ? N1 Si P1 N2 -177.39(17) . . . . ? C1 Si P1 N2 91.42(19) . . . . ? C2 Si P1 N2 -89.0(2) . . . . ? N2 Si P1 N1 177.39(17) . . . . ? C1 Si P1 N1 -91.19(18) . . . . ? C2 Si P1 N1 88.4(2) . . . . ? N1 Si P1 Ni 90.76(14) . . . . ? N2 Si P1 Ni -91.85(15) . . . . ? C1 Si P1 Ni -0.43(17) . . . . ? C2 Si P1 Ni 179.15(19) . . . . ? N3 Ni P2 C44 -129.6(3) . . . . ? P1 Ni P2 C44 -134.8(2) . . . . ? Cl1 Ni P2 C44 45.0(2) . . . . ? N3 Ni P2 C40 -3.4(3) . . . . ? P1 Ni P2 C40 -8.62(17) . . . . ? Cl1 Ni P2 C40 171.19(16) . . . . ? N3 Ni P2 C48 138.4(3) . . . . ? P1 Ni P2 C48 133.2(3) . . . . ? Cl1 Ni P2 C48 -47.0(3) . . . . ? N3 Ni P2 C48B 103.2(3) . . . . ? P1 Ni P2 C48B 98.0(2) . . . . ? Cl1 Ni P2 C48B -82.2(2) . . . . ? N3 P1 N1 C10 -44.2(3) . . . . ? N2 P1 N1 C10 -174.7(3) . . . . ? Ni P1 N1 C10 38.2(3) . . . . ? Si P1 N1 C10 -176.5(3) . . . . ? N3 P1 N1 Si 132.28(12) . . . . ? N2 P1 N1 Si 1.80(12) . . . . ? Ni P1 N1 Si -145.30(7) . . . . ? N2 Si N1 C10 174.6(3) . . . . ? C1 Si N1 C10 -70.1(3) . . . . ? C2 Si N1 C10 59.2(3) . . . . ? P1 Si N1 C10 176.3(3) . . . . ? N2 Si N1 P1 -1.74(12) . . . . ? C1 Si N1 P1 113.64(17) . . . . ? C2 Si N1 P1 -117.10(17) . . . . ? N3 P1 N2 C20 57.1(3) . . . . ? N1 P1 N2 C20 -172.2(3) . . . . ? Ni P1 N2 C20 -25.3(3) . . . . ? Si P1 N2 C20 -170.4(3) . . . . ? N3 P1 N2 Si -132.50(12) . . . . ? N1 P1 N2 Si -1.79(12) . . . . ? Ni P1 N2 Si 145.13(7) . . . . ? N1 Si N2 C20 171.7(3) . . . . ? C1 Si N2 C20 56.5(3) . . . . ? C2 Si N2 C20 -73.3(3) . . . . ? P1 Si N2 C20 170.0(3) . . . . ? N1 Si N2 P1 1.74(12) . . . . ? C1 Si N2 P1 -113.47(16) . . . . ? C2 Si N2 P1 116.70(19) . . . . ? N2 P1 N3 C30 53.9(4) . . . . ? N1 P1 N3 C30 -59.1(4) . . . . ? Ni P1 N3 C30 177.6(4) . . . . ? Si P1 N3 C30 -2.6(5) . . . . ? N2 P1 N3 Ni -123.71(12) . . . . ? N1 P1 N3 Ni 123.29(11) . . . . ? Si P1 N3 Ni 179.82(9) . . . . ? P1 Ni N3 C30 -177.9(4) . . . . ? P2 Ni N3 C30 175.2(2) . . . . ? Cl1 Ni N3 C30 0.9(3) . . . . ? P2 Ni N3 P1 -6.9(2) . . . . ? Cl1 Ni N3 P1 178.77(6) . . . . ? P1 N1 C10 C12 -31.3(4) . . . . ? Si N1 C10 C12 153.5(3) . . . . ? P1 N1 C10 C11 -151.3(2) . . . . ? Si N1 C10 C11 33.5(4) . . . . ? P1 N1 C10 C13 89.5(3) . . . . ? Si N1 C10 C13 -85.7(3) . . . . ? P1 N2 C20 C22 -18.1(5) . . . . ? Si N2 C20 C22 175.1(3) . . . . ? P1 N2 C20 C21 105.3(3) . . . . ? Si N2 C20 C21 -61.5(4) . . . . ? P1 N2 C20 C23 -138.8(3) . . . . ? Si N2 C20 C23 54.4(4) . . . . ? P1 N3 C30 C33 -125.2(4) . . . . ? Ni N3 C30 C33 51.2(4) . . . . ? P1 N3 C30 C31 -4.7(5) . . . . ? Ni N3 C30 C31 171.7(3) . . . . ? P1 N3 C30 C32 115.6(4) . . . . ? Ni N3 C30 C32 -68.1(4) . . . . ? C44 P2 C40 C41 -42.1(5) . . . . ? C48 P2 C40 C41 47.5(5) . . . . ? C48B P2 C40 C41 70.6(4) . . . . ? Ni P2 C40 C41 -171.3(3) . . . . ? P2 C40 C41 C42 -178.6(4) . . . . ? C40 C41 C42 C43 179.6(6) . . . . ? C40 P2 C44 C45 -72.7(5) . . . . ? C48 P2 C44 C45 171.3(5) . . . . ? C48B P2 C44 C45 -174.2(4) . . . . ? Ni P2 C44 C45 56.9(5) . . . . ? P2 C44 C45 C46 -168.6(4) . . . . ? C44 C45 C46 C47 -124.3(12) . . . . ? C44 P2 C48 C49 -175.9(11) . . . . ? C40 P2 C48 C49 77.8(11) . . . . ? C48B P2 C48 C49 30.4(10) . . . . ? Ni P2 C48 C49 -63.2(11) . . . . ? C44 P2 C48B C49B -64.1(6) . . . . ? C40 P2 C48B C49B -175.2(6) . . . . ? C48 P2 C48B C49B -36.2(6) . . . . ? Ni P2 C48B C49B 65.2(6) . . . . ? P2 C48 C49 C50 -177.2(10) . . . . ? P2 C48B C49B C50 177.3(5) . . . . ? C48 C49 C50 C51 -83.7(17) . . . . ? C48 C49 C50 C49B -39.9(7) . . . . ? C48B C49B C50 C51 178.5(6) . . . . ? C48B C49B C50 C49 30.3(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.840 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.077 #===END=== data_9a _database_code_depnum_ccdc_archive 'CCDC 272423' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H54 N6 P2 Si2' _chemical_formula_weight 568.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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 9.2122(13) _cell_length_b 33.045(5) _cell_length_c 12.3486(16) _cell_angle_alpha 90.00 _cell_angle_beta 109.808(10) _cell_angle_gamma 90.00 _cell_volume 3536.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 52 _cell_measurement_theta_min 5.20 _cell_measurement_theta_max 12.48 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.8 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.214 _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 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5826 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4593 _reflns_number_gt 3849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0965P)^2^+2.4714P] 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 4593 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1772 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.036 _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 P1 P 0.11862(12) 0.44715(3) 0.76602(8) 0.0700(3) Uani 1 1 d . . . P2 P 0.50123(11) 0.31539(3) 1.06885(8) 0.0657(3) Uani 1 1 d . . . Si1 Si 0.17411(13) 0.42669(3) 0.58424(8) 0.0695(3) Uani 1 1 d . . . Si2 Si 0.62672(13) 0.28173(3) 0.93641(10) 0.0736(3) Uani 1 1 d . . . N1 N 0.1890(4) 0.41011(10) 0.8662(2) 0.0868(10) Uani 1 1 d . . . H1 H 0.2072 0.3872 0.8402 0.104 Uiso 1 1 calc R . . N2 N 0.4074(4) 0.35838(9) 1.0097(2) 0.0775(9) Uani 1 1 d . . . H2N H 0.4084 0.3643 0.9422 0.093 Uiso 1 1 calc R . . N3 N 0.0351(4) 0.41849(9) 0.6454(2) 0.0722(8) Uani 1 1 d . . . N4 N 0.2582(4) 0.45523(9) 0.7054(2) 0.0706(8) Uani 1 1 d . . . N5 N 0.4527(4) 0.28118(9) 0.9579(3) 0.0743(8) Uani 1 1 d . . . N6 N 0.6695(3) 0.31892(9) 1.0399(3) 0.0693(8) Uani 1 1 d . . . C1 C 0.2211(4) 0.41207(10) 0.9857(3) 0.0643(9) Uani 1 1 d . . . C2 C 0.1456(5) 0.43926(11) 1.0335(3) 0.0764(10) Uani 1 1 d . . . H2 H 0.0748 0.4573 0.9860 0.092 Uiso 1 1 calc R . . C3 C 0.1736(5) 0.44008(12) 1.1501(3) 0.0819(11) Uani 1 1 d . . . H3 H 0.1229 0.4587 1.1811 0.098 Uiso 1 1 calc R . . C4 C 0.2760(5) 0.41346(13) 1.2201(3) 0.0832(11) Uani 1 1 d . . . H4 H 0.2931 0.4134 1.2987 0.100 Uiso 1 1 calc R . . C5 C 0.3538(4) 0.38675(12) 1.1748(3) 0.0762(10) Uani 1 1 d . . . H5 H 0.4251 0.3691 1.2236 0.091 Uiso 1 1 calc R . . C6 C 0.3283(4) 0.38551(10) 1.0573(3) 0.0603(8) Uani 1 1 d . . . C7 C 0.2797(7) 0.38077(15) 0.5662(5) 0.1200(18) Uani 1 1 d . . . H7A H 0.3095 0.3652 0.6359 0.180 Uiso 1 1 calc R . . H7B H 0.3702 0.3886 0.5494 0.180 Uiso 1 1 calc R . . H7C H 0.2141 0.3648 0.5039 0.180 Uiso 1 1 calc R . . C8 C 0.1106(6) 0.45416(13) 0.4451(3) 0.0922(13) Uani 1 1 d . . . H8A H 0.0415 0.4374 0.3868 0.138 Uiso 1 1 calc R . . H8B H 0.1989 0.4607 0.4239 0.138 Uiso 1 1 calc R . . H8C H 0.0587 0.4786 0.4526 0.138 Uiso 1 1 calc R . . C9 C 0.6254(6) 0.29614(17) 0.7917(4) 0.1087(15) Uani 1 1 d . . . H9A H 0.5872 0.2740 0.7396 0.163 Uiso 1 1 calc R . . H9B H 0.7284 0.3027 0.7952 0.163 Uiso 1 1 calc R . . H9C H 0.5599 0.3193 0.7652 0.163 Uiso 1 1 calc R . . C10 C 0.7428(7) 0.23449(15) 0.9792(5) 0.1273(19) Uani 1 1 d . . . H10A H 0.7412 0.2256 1.0528 0.191 Uiso 1 1 calc R . . H10B H 0.8473 0.2397 0.9840 0.191 Uiso 1 1 calc R . . H10C H 0.6996 0.2138 0.9228 0.191 Uiso 1 1 calc R . . C11 C -0.1178(5) 0.40010(14) 0.6099(4) 0.0949(13) Uani 1 1 d . . . C12 C -0.1563(12) 0.3833(5) 0.4926(8) 0.313(9) Uani 1 1 d . . . H12A H -0.2546 0.3700 0.4711 0.469 Uiso 1 1 calc R . . H12B H -0.0785 0.3642 0.4911 0.469 Uiso 1 1 calc R . . H12C H -0.1607 0.4049 0.4394 0.469 Uiso 1 1 calc R . . C13 C -0.2286(9) 0.4295(3) 0.6051(18) 0.427(14) Uani 1 1 d . . . H13A H -0.2048 0.4539 0.5723 0.641 Uiso 1 1 calc R . . H13B H -0.2289 0.4349 0.6814 0.641 Uiso 1 1 calc R . . H13C H -0.3285 0.4199 0.5582 0.641 Uiso 1 1 calc R . . C14 C -0.1265(13) 0.3681(4) 0.6812(9) 0.335(10) Uani 1 1 d . . . H14A H -0.1381 0.3786 0.7503 0.502 Uiso 1 1 calc R . . H14B H -0.0338 0.3523 0.7005 0.502 Uiso 1 1 calc R . . H14C H -0.2137 0.3514 0.6418 0.502 Uiso 1 1 calc R . . C15 C 0.3995(5) 0.47873(13) 0.7548(4) 0.0905(12) Uani 1 1 d . . . C16 C 0.5202(6) 0.4533(2) 0.8450(6) 0.150(3) Uani 1 1 d . . . H16A H 0.4847 0.4477 0.9081 0.225 Uiso 1 1 calc R . . H16B H 0.6157 0.4680 0.8724 0.225 Uiso 1 1 calc R . . H16C H 0.5359 0.4283 0.8109 0.225 Uiso 1 1 calc R . . C17 C 0.3664(8) 0.51733(17) 0.8091(6) 0.142(2) Uani 1 1 d . . . H17A H 0.2927 0.5334 0.7514 0.213 Uiso 1 1 calc R . . H17B H 0.4602 0.5324 0.8416 0.213 Uiso 1 1 calc R . . H17C H 0.3253 0.5106 0.8687 0.213 Uiso 1 1 calc R . . C18 C 0.4618(7) 0.4893(2) 0.6600(5) 0.133(2) Uani 1 1 d . . . H18A H 0.4717 0.4651 0.6200 0.199 Uiso 1 1 calc R . . H18B H 0.5611 0.5019 0.6926 0.199 Uiso 1 1 calc R . . H18C H 0.3922 0.5077 0.6071 0.199 Uiso 1 1 calc R . . C19 C 0.3078(5) 0.25860(13) 0.9105(4) 0.0831(11) Uani 1 1 d . . . C20 C 0.1954(8) 0.2825(2) 0.8189(7) 0.186(4) Uani 1 1 d . . . H20A H 0.1443 0.3014 0.8528 0.278 Uiso 1 1 calc R . . H20B H 0.1204 0.2646 0.7683 0.278 Uiso 1 1 calc R . . H20C H 0.2482 0.2969 0.7759 0.278 Uiso 1 1 calc R . . C21 C 0.3413(8) 0.2180(2) 0.8615(8) 0.182(3) Uani 1 1 d . . . H21A H 0.3831 0.2232 0.8015 0.272 Uiso 1 1 calc R . . H21B H 0.2473 0.2029 0.8309 0.272 Uiso 1 1 calc R . . H21C H 0.4144 0.2028 0.9218 0.272 Uiso 1 1 calc R . . C22 C 0.2433(7) 0.2473(2) 1.0027(6) 0.153(3) Uani 1 1 d . . . H22A H 0.3186 0.2320 1.0613 0.230 Uiso 1 1 calc R . . H22B H 0.1520 0.2312 0.9699 0.230 Uiso 1 1 calc R . . H22C H 0.2179 0.2714 1.0359 0.230 Uiso 1 1 calc R . . C23 C 0.8105(5) 0.33982(13) 1.1103(4) 0.0869(12) Uani 1 1 d . . . C24 C 0.7761(7) 0.38339(17) 1.1323(7) 0.156(3) Uani 1 1 d . . . H24A H 0.7412 0.3979 1.0606 0.233 Uiso 1 1 calc R . . H24B H 0.8681 0.3959 1.1831 0.233 Uiso 1 1 calc R . . H24C H 0.6973 0.3840 1.1669 0.233 Uiso 1 1 calc R . . C26 C 0.9287(7) 0.3371(2) 1.0526(6) 0.169(3) Uani 1 1 d . . . H26A H 0.9500 0.3092 1.0425 0.254 Uiso 1 1 calc R . . H26B H 1.0217 0.3503 1.0993 0.254 Uiso 1 1 calc R . . H26C H 0.8903 0.3502 0.9788 0.254 Uiso 1 1 calc R . . C25 C 0.8746(8) 0.3192(2) 1.2276(6) 0.174(3) Uani 1 1 d . . . H25A H 0.7982 0.3197 1.2646 0.260 Uiso 1 1 calc R . . H25B H 0.9652 0.3333 1.2745 0.260 Uiso 1 1 calc R . . H25C H 0.9007 0.2917 1.2176 0.260 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 P1 0.0932(7) 0.0632(6) 0.0584(6) 0.0042(4) 0.0322(5) 0.0180(5) P2 0.0747(6) 0.0668(6) 0.0590(6) 0.0046(4) 0.0272(4) 0.0040(4) Si1 0.0913(7) 0.0615(6) 0.0596(6) -0.0038(4) 0.0306(5) 0.0102(5) Si2 0.0839(7) 0.0643(6) 0.0826(7) -0.0003(5) 0.0413(6) 0.0049(5) N1 0.137(3) 0.073(2) 0.0534(17) 0.0075(15) 0.0362(18) 0.0391(19) N2 0.099(2) 0.085(2) 0.0583(17) 0.0148(15) 0.0404(16) 0.0290(18) N3 0.081(2) 0.0746(19) 0.0598(17) 0.0002(14) 0.0221(15) -0.0037(16) N4 0.082(2) 0.0711(18) 0.0600(17) -0.0074(14) 0.0258(15) -0.0014(15) N5 0.083(2) 0.0719(19) 0.0755(19) -0.0110(15) 0.0370(16) -0.0117(16) N6 0.0663(18) 0.0685(18) 0.0732(19) -0.0013(14) 0.0238(15) 0.0025(14) C1 0.080(2) 0.063(2) 0.0559(19) -0.0013(16) 0.0307(17) 0.0016(17) C2 0.101(3) 0.067(2) 0.070(2) -0.0016(18) 0.042(2) 0.016(2) C3 0.108(3) 0.077(2) 0.077(3) -0.013(2) 0.054(2) 0.003(2) C4 0.106(3) 0.097(3) 0.056(2) -0.008(2) 0.039(2) 0.000(2) C5 0.085(2) 0.088(3) 0.058(2) 0.0009(19) 0.0272(19) 0.007(2) C6 0.066(2) 0.066(2) 0.0556(19) 0.0003(16) 0.0285(16) -0.0005(16) C7 0.153(5) 0.093(3) 0.121(4) -0.009(3) 0.057(4) 0.039(3) C8 0.132(4) 0.087(3) 0.065(2) 0.000(2) 0.042(2) 0.011(3) C9 0.125(4) 0.131(4) 0.088(3) -0.005(3) 0.059(3) -0.012(3) C10 0.144(5) 0.085(3) 0.169(5) 0.004(3) 0.074(4) 0.032(3) C11 0.095(3) 0.080(3) 0.107(3) 0.008(2) 0.032(3) -0.011(2) C12 0.240(11) 0.53(2) 0.152(7) -0.095(11) 0.046(7) -0.251(14) C13 0.089(5) 0.196(10) 0.95(4) -0.214(17) 0.119(12) -0.032(6) C14 0.280(12) 0.382(17) 0.232(10) 0.183(11) -0.058(9) -0.225(13) C15 0.088(3) 0.087(3) 0.090(3) -0.001(2) 0.021(2) -0.007(2) C16 0.105(4) 0.157(6) 0.146(5) 0.030(4) -0.013(4) -0.015(4) C17 0.155(5) 0.101(4) 0.169(6) -0.048(4) 0.052(4) -0.032(4) C18 0.120(4) 0.153(5) 0.133(5) -0.003(4) 0.051(4) -0.044(4) C19 0.086(3) 0.083(3) 0.084(3) -0.004(2) 0.033(2) -0.017(2) C20 0.137(5) 0.147(6) 0.194(7) 0.036(5) -0.046(5) -0.042(4) C21 0.160(6) 0.141(6) 0.272(9) -0.104(6) 0.110(6) -0.067(5) C22 0.126(5) 0.191(7) 0.149(5) -0.014(5) 0.055(4) -0.070(5) C23 0.070(2) 0.086(3) 0.097(3) -0.004(2) 0.018(2) -0.003(2) C24 0.122(4) 0.105(4) 0.215(7) -0.055(4) 0.026(4) -0.018(3) C26 0.101(4) 0.227(8) 0.203(7) -0.091(6) 0.083(4) -0.061(5) C25 0.126(5) 0.215(8) 0.130(5) 0.021(5) -0.022(4) -0.024(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 P1 N1 1.704(3) . ? P1 N3 1.712(3) . ? P1 N4 1.714(3) . ? P1 Si1 2.5564(13) . ? P2 N2 1.694(3) . ? P2 N6 1.709(3) . ? P2 N5 1.715(3) . ? P2 Si2 2.5553(14) . ? Si1 N3 1.715(3) . ? Si1 N4 1.716(3) . ? Si1 C8 1.854(4) . ? Si1 C7 1.856(4) . ? Si2 N5 1.712(3) . ? Si2 N6 1.720(3) . ? Si2 C9 1.845(4) . ? Si2 C10 1.865(5) . ? N1 C1 1.405(4) . ? N2 C6 1.404(4) . ? N3 C11 1.459(5) . ? N4 C15 1.460(5) . ? N5 C19 1.467(5) . ? N6 C23 1.468(5) . ? C1 C2 1.385(5) . ? C1 C6 1.391(5) . ? C2 C3 1.373(5) . ? C3 C4 1.363(6) . ? C4 C5 1.370(5) . ? C5 C6 1.390(5) . ? C11 C14 1.395(8) . ? C11 C13 1.395(9) . ? C11 C12 1.478(10) . ? C15 C18 1.510(7) . ? C15 C17 1.519(7) . ? C15 C16 1.530(7) . ? C19 C20 1.477(7) . ? C19 C22 1.499(7) . ? C19 C21 1.545(7) . ? C23 C26 1.492(7) . ? C23 C24 1.518(7) . ? C23 C25 1.526(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 N1 P1 N3 100.49(16) . . ? N1 P1 N4 105.76(17) . . ? N3 P1 N4 83.62(15) . . ? N1 P1 Si1 107.89(11) . . ? N3 P1 Si1 41.79(11) . . ? N4 P1 Si1 41.83(10) . . ? N2 P2 N6 102.65(15) . . ? N2 P2 N5 104.57(16) . . ? N6 P2 N5 83.55(15) . . ? N2 P2 Si2 111.37(11) . . ? N6 P2 Si2 41.99(10) . . ? N5 P2 Si2 41.73(11) . . ? N3 Si1 N4 83.47(15) . . ? N3 Si1 C8 115.97(19) . . ? N4 Si1 C8 116.54(18) . . ? N3 Si1 C7 115.1(2) . . ? N4 Si1 C7 117.0(2) . . ? C8 Si1 C7 107.6(2) . . ? N3 Si1 P1 41.70(10) . . ? N4 Si1 P1 41.77(11) . . ? C8 Si1 P1 126.18(14) . . ? C7 Si1 P1 126.20(18) . . ? N5 Si2 N6 83.31(14) . . ? N5 Si2 C9 117.0(2) . . ? N6 Si2 C9 117.4(2) . . ? N5 Si2 C10 115.1(2) . . ? N6 Si2 C10 115.0(2) . . ? C9 Si2 C10 107.8(3) . . ? N5 Si2 P2 41.82(10) . . ? N6 Si2 P2 41.66(10) . . ? C9 Si2 P2 130.64(18) . . ? C10 Si2 P2 121.57(19) . . ? C1 N1 P1 128.5(2) . . ? C6 N2 P2 128.0(2) . . ? C11 N3 P1 126.5(3) . . ? C11 N3 Si1 136.3(3) . . ? P1 N3 Si1 96.51(16) . . ? C15 N4 P1 126.5(3) . . ? C15 N4 Si1 137.1(3) . . ? P1 N4 Si1 96.40(16) . . ? C19 N5 Si2 135.8(3) . . ? C19 N5 P2 127.6(3) . . ? Si2 N5 P2 96.45(15) . . ? C23 N6 P2 126.3(3) . . ? C23 N6 Si2 135.3(3) . . ? P2 N6 Si2 96.35(15) . . ? C2 C1 C6 119.2(3) . . ? C2 C1 N1 121.4(3) . . ? C6 C1 N1 119.4(3) . . ? C3 C2 C1 121.1(4) . . ? C4 C3 C2 119.7(4) . . ? C3 C4 C5 120.2(4) . . ? C4 C5 C6 121.2(4) . . ? C5 C6 C1 118.6(3) . . ? C5 C6 N2 121.8(3) . . ? C1 C6 N2 119.6(3) . . ? C14 C11 C13 110.9(10) . . ? C14 C11 N3 112.5(5) . . ? C13 C11 N3 110.0(5) . . ? C14 C11 C12 106.7(8) . . ? C13 C11 C12 106.9(9) . . ? N3 C11 C12 109.7(5) . . ? N4 C15 C18 108.6(4) . . ? N4 C15 C17 110.3(4) . . ? C18 C15 C17 109.5(5) . . ? N4 C15 C16 109.7(4) . . ? C18 C15 C16 108.5(5) . . ? C17 C15 C16 110.2(5) . . ? N5 C19 C20 109.9(4) . . ? N5 C19 C22 111.4(4) . . ? C20 C19 C22 111.1(5) . . ? N5 C19 C21 108.8(4) . . ? C20 C19 C21 110.2(6) . . ? C22 C19 C21 105.3(5) . . ? N6 C23 C26 109.4(4) . . ? N6 C23 C24 110.8(4) . . ? C26 C23 C24 111.8(5) . . ? N6 C23 C25 109.4(4) . . ? C26 C23 C25 108.5(5) . . ? C24 C23 C25 106.9(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.455 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.053 #===END=== data_9b _database_code_depnum_ccdc_archive 'CCDC 272424' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H54 N6 P2 Si2' _chemical_formula_weight 568.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.225(3) _cell_length_b 16.783(4) _cell_length_c 32.714(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6712(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 4.73 _cell_measurement_theta_max 12.51 _exptl_crystal_description rhombic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.85 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2536 _exptl_absorpt_coefficient_mu 0.228 _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 293(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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5443 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 22.49 _reflns_number_total 4355 _reflns_number_gt 3477 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0663P)^2^+10.4298P] 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 4355 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1352 _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 N1 N 1.1693(2) 0.85419(18) 0.08396(9) 0.0463(7) Uani 1 1 d . . . N2 N 1.0335(2) 0.75785(18) 0.08288(9) 0.0490(8) Uani 1 1 d . . . N3 N 0.9302(2) 1.02757(17) 0.17428(9) 0.0468(7) Uani 1 1 d . . . N4 N 0.8869(2) 0.91175(18) 0.20894(9) 0.0480(8) Uani 1 1 d . . . N5 N 0.9748(2) 0.89093(17) 0.12896(9) 0.0434(7) Uani 1 1 d . . . N6A N 0.9946(5) 0.9537(4) 0.04515(19) 0.068(2) Uani 0.583(8) 1 d P A 1 H6A1 H 0.9948 0.9722 0.0206 0.081 Uiso 0.583(8) 1 calc PR A 1 H6A2 H 1.0553 0.9469 0.0580 0.081 Uiso 0.583(8) 1 calc PR A 1 N6B N 0.7400(8) 0.8641(5) 0.1438(3) 0.068(3) Uani 0.417(8) 1 d P A 2 H6B1 H 0.7822 0.8458 0.1626 0.082 Uiso 0.417(8) 1 calc PR A 2 H6B2 H 0.6702 0.8608 0.1464 0.082 Uiso 0.417(8) 1 calc PR A 2 P1 P 1.07882(8) 0.82022(6) 0.12107(3) 0.0430(3) Uani 1 1 d . . . P2 P 0.99432(7) 0.93623(6) 0.17667(3) 0.0421(3) Uani 1 1 d . . . Si1 Si 1.14022(10) 0.77802(8) 0.04956(3) 0.0601(4) Uani 1 1 d . . . Si2 Si 0.83751(9) 1.00825(7) 0.21308(4) 0.0560(3) Uani 1 1 d . . . C1 C 1.2472(5) 0.6999(4) 0.04602(18) 0.1005(18) Uani 1 1 d . . . H1A H 1.2656 0.6816 0.0730 0.151 Uiso 1 1 calc R . . H1B H 1.3112 0.7216 0.0331 0.151 Uiso 1 1 calc R . . H1C H 1.2202 0.6560 0.0301 0.151 Uiso 1 1 calc R . . C2 C 1.1025(5) 0.8053(4) -0.00335(13) 0.1021(19) Uani 1 1 d . . . H2A H 1.0906 0.7578 -0.0191 0.153 Uiso 1 1 calc R . . H2B H 1.1606 0.8357 -0.0154 0.153 Uiso 1 1 calc R . . H2C H 1.0367 0.8366 -0.0030 0.153 Uiso 1 1 calc R . . C3 C 0.8645(4) 1.0586(3) 0.26300(14) 0.0854(15) Uani 1 1 d . . . H3A H 0.9416 1.0579 0.2686 0.128 Uiso 1 1 calc R . . H3B H 0.8263 1.0311 0.2844 0.128 Uiso 1 1 calc R . . H3C H 0.8394 1.1128 0.2617 0.128 Uiso 1 1 calc R . . C4 C 0.6915(3) 1.0250(3) 0.20093(19) 0.0868(16) Uani 1 1 d . . . H4A H 0.6782 1.0810 0.1979 0.130 Uiso 1 1 calc R . . H4B H 0.6469 1.0044 0.2227 0.130 Uiso 1 1 calc R . . H4C H 0.6734 0.9981 0.1759 0.130 Uiso 1 1 calc R . . C10 C 1.2747(3) 0.8933(3) 0.09336(13) 0.0558(10) Uani 1 1 d . . . C11 C 1.2553(4) 0.9653(3) 0.12014(19) 0.0987(18) Uani 1 1 d . . . H11A H 1.2115 1.0034 0.1056 0.148 Uiso 1 1 calc R . . H11B H 1.3242 0.9890 0.1272 0.148 Uiso 1 1 calc R . . H11C H 1.2179 0.9492 0.1446 0.148 Uiso 1 1 calc R . . C12 C 1.3296(4) 0.9176(4) 0.05399(16) 0.1006(19) Uani 1 1 d . . . H12A H 1.3390 0.8717 0.0369 0.151 Uiso 1 1 calc R . . H12B H 1.3997 0.9406 0.0599 0.151 Uiso 1 1 calc R . . H12C H 1.2849 0.9561 0.0401 0.151 Uiso 1 1 calc R . . C13 C 1.3511(4) 0.8374(4) 0.11712(16) 0.0894(16) Uani 1 1 d . . . H13A H 1.3149 0.8192 0.1414 0.134 Uiso 1 1 calc R . . H13B H 1.4165 0.8656 0.1245 0.134 Uiso 1 1 calc R . . H13C H 1.3698 0.7926 0.1003 0.134 Uiso 1 1 calc R . . C20 C 0.9668(4) 0.6849(2) 0.08731(14) 0.0648(12) Uani 1 1 d . . . C21 C 1.0145(5) 0.6318(3) 0.1210(2) 0.116(2) Uani 1 1 d . . . H21A H 1.0903 0.6216 0.1154 0.174 Uiso 1 1 calc R . . H21B H 0.9752 0.5823 0.1218 0.174 Uiso 1 1 calc R . . H21C H 1.0079 0.6583 0.1469 0.174 Uiso 1 1 calc R . . C22 C 0.9688(7) 0.6398(4) 0.0475(2) 0.135(3) Uani 1 1 d . . . H22A H 0.9512 0.6754 0.0254 0.203 Uiso 1 1 calc R . . H22B H 0.9161 0.5975 0.0484 0.203 Uiso 1 1 calc R . . H22C H 1.0404 0.6179 0.0432 0.203 Uiso 1 1 calc R . . C23 C 0.8510(4) 0.7052(3) 0.0982(2) 0.113(2) Uani 1 1 d . . . H23A H 0.8500 0.7357 0.1230 0.169 Uiso 1 1 calc R . . H23B H 0.8100 0.6570 0.1020 0.169 Uiso 1 1 calc R . . H23C H 0.8189 0.7358 0.0765 0.169 Uiso 1 1 calc R . . C30 C 0.9762(3) 1.1032(2) 0.15953(13) 0.0562(10) Uani 1 1 d . . . C31 C 0.8981(4) 1.1705(3) 0.17095(17) 0.0809(14) Uani 1 1 d . . . H31A H 0.8263 1.1585 0.1609 0.121 Uiso 1 1 calc R . . H31B H 0.9233 1.2194 0.1590 0.121 Uiso 1 1 calc R . . H31C H 0.8957 1.1759 0.2002 0.121 Uiso 1 1 calc R . . C32 C 0.9869(4) 1.1013(3) 0.11296(14) 0.0758(13) Uani 1 1 d . . . H32A H 1.0347 1.0586 0.1051 0.114 Uiso 1 1 calc R . . H32B H 1.0165 1.1510 0.1036 0.114 Uiso 1 1 calc R . . H32C H 0.9161 1.0932 0.1010 0.114 Uiso 1 1 calc R . . C33 C 1.0879(4) 1.1194(3) 0.17900(15) 0.0737(13) Uani 1 1 d . . . H33A H 1.0809 1.1193 0.2082 0.111 Uiso 1 1 calc R . . H33B H 1.1145 1.1703 0.1701 0.111 Uiso 1 1 calc R . . H33C H 1.1385 1.0786 0.1709 0.111 Uiso 1 1 calc R . . C40 C 0.8888(3) 0.8443(2) 0.23825(12) 0.0559(10) Uani 1 1 d . . . C41 C 0.7734(4) 0.8329(3) 0.25493(17) 0.0880(16) Uani 1 1 d . . . H41A H 0.7503 0.8806 0.2686 0.132 Uiso 1 1 calc R . . H41B H 0.7729 0.7893 0.2739 0.132 Uiso 1 1 calc R . . H41C H 0.7243 0.8216 0.2328 0.132 Uiso 1 1 calc R . . C42 C 0.9659(4) 0.8619(3) 0.27384(13) 0.0777(14) Uani 1 1 d . . . H42A H 1.0380 0.8724 0.2635 0.116 Uiso 1 1 calc R . . H42B H 0.9683 0.8167 0.2918 0.116 Uiso 1 1 calc R . . H42C H 0.9400 0.9076 0.2886 0.116 Uiso 1 1 calc R . . C43 C 0.9258(5) 0.7688(3) 0.21704(15) 0.0867(16) Uani 1 1 d . . . H43A H 0.8767 0.7568 0.1950 0.130 Uiso 1 1 calc R . . H43B H 0.9257 0.7255 0.2362 0.130 Uiso 1 1 calc R . . H43C H 0.9983 0.7762 0.2065 0.130 Uiso 1 1 calc R . . C50 C 0.8847(3) 0.9071(2) 0.10192(11) 0.0475(9) Uani 1 1 d . A . C51 C 0.7784(3) 0.8941(3) 0.11402(18) 0.0696(13) Uani 1 1 d . . . C52 C 0.6925(5) 0.9106(4) 0.0875(3) 0.120(3) Uani 1 1 d . A . H52 H 0.6208 0.9023 0.0959 0.144 Uiso 1 1 calc R . . C53 C 0.7119(9) 0.9382(5) 0.0501(3) 0.148(5) Uani 1 1 d . . . H53 H 0.6535 0.9487 0.0327 0.178 Uiso 1 1 calc R A . C54 C 0.8148(8) 0.9513(4) 0.03697(19) 0.113(3) Uani 1 1 d . A . H54 H 0.8262 0.9705 0.0106 0.136 Uiso 1 1 calc R . . C55 C 0.9048(4) 0.9364(3) 0.06237(13) 0.0657(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0440(17) 0.0516(18) 0.0433(17) 0.0052(14) 0.0039(13) -0.0009(15) N2 0.0539(18) 0.0437(17) 0.0493(17) -0.0049(14) -0.0024(15) -0.0010(15) N3 0.0474(17) 0.0380(17) 0.0552(18) -0.0021(14) 0.0017(14) 0.0034(14) N4 0.0452(17) 0.0509(19) 0.0478(17) 0.0063(15) 0.0036(14) 0.0058(15) N5 0.0404(16) 0.0431(17) 0.0467(17) -0.0011(14) -0.0043(13) 0.0041(14) N6A 0.070(5) 0.069(4) 0.064(4) 0.023(3) -0.004(3) 0.006(3) N6B 0.060(5) 0.073(6) 0.072(6) -0.004(5) -0.007(5) -0.008(5) P1 0.0430(5) 0.0411(5) 0.0450(5) 0.0010(4) 0.0010(4) 0.0038(4) P2 0.0397(5) 0.0411(5) 0.0454(5) -0.0002(4) -0.0017(4) 0.0034(4) Si1 0.0601(7) 0.0708(8) 0.0495(6) -0.0099(6) 0.0052(5) -0.0008(6) Si2 0.0471(6) 0.0556(7) 0.0653(7) -0.0029(6) 0.0051(5) 0.0121(5) C1 0.087(4) 0.109(4) 0.106(4) -0.046(4) 0.016(3) 0.014(3) C2 0.114(4) 0.143(5) 0.049(3) -0.004(3) -0.008(3) -0.028(4) C3 0.098(4) 0.083(3) 0.075(3) -0.016(3) 0.015(3) 0.018(3) C4 0.049(3) 0.075(3) 0.136(5) 0.009(3) 0.017(3) 0.019(2) C10 0.042(2) 0.062(3) 0.064(2) 0.002(2) 0.0063(18) -0.0045(19) C11 0.062(3) 0.090(4) 0.144(5) -0.036(4) 0.011(3) -0.024(3) C12 0.077(3) 0.144(5) 0.081(4) 0.019(4) 0.018(3) -0.037(4) C13 0.055(3) 0.116(4) 0.097(4) 0.014(3) -0.021(3) -0.002(3) C20 0.069(3) 0.046(2) 0.079(3) -0.014(2) 0.006(2) -0.008(2) C21 0.130(5) 0.065(3) 0.154(6) 0.032(4) -0.003(4) -0.011(4) C22 0.186(7) 0.101(5) 0.119(5) -0.058(4) 0.038(5) -0.068(5) C23 0.077(4) 0.077(4) 0.184(7) -0.030(4) 0.023(4) -0.029(3) C30 0.063(3) 0.040(2) 0.066(3) -0.0029(19) -0.007(2) 0.0012(19) C31 0.082(3) 0.049(3) 0.111(4) -0.003(3) -0.009(3) 0.014(2) C32 0.099(4) 0.058(3) 0.070(3) 0.013(2) -0.002(3) -0.017(3) C33 0.066(3) 0.056(3) 0.100(4) -0.008(3) -0.010(3) -0.011(2) C40 0.049(2) 0.061(2) 0.058(2) 0.011(2) 0.0084(19) 0.002(2) C41 0.059(3) 0.107(4) 0.099(4) 0.035(3) 0.013(3) -0.006(3) C42 0.065(3) 0.102(4) 0.067(3) 0.023(3) -0.006(2) 0.002(3) C43 0.121(4) 0.060(3) 0.079(3) 0.020(3) 0.021(3) 0.014(3) C50 0.047(2) 0.040(2) 0.056(2) -0.0038(18) -0.0069(18) 0.0040(17) C51 0.046(3) 0.069(3) 0.094(4) -0.018(3) 0.001(3) -0.005(2) C52 0.054(3) 0.110(5) 0.196(8) -0.062(6) -0.040(5) 0.018(3) C53 0.152(8) 0.111(6) 0.182(9) -0.063(6) -0.112(8) 0.062(6) C54 0.193(8) 0.077(4) 0.071(4) -0.005(3) -0.057(5) 0.043(5) C55 0.093(4) 0.050(2) 0.054(3) 0.000(2) -0.010(3) 0.013(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 N1 C10 1.478(5) . ? N1 P1 1.739(3) . ? N1 Si1 1.740(3) . ? N2 C20 1.478(5) . ? N2 P1 1.721(3) . ? N2 Si1 1.733(3) . ? N3 C30 1.469(5) . ? N3 P2 1.724(3) . ? N3 Si2 1.732(3) . ? N4 C40 1.483(5) . ? N4 Si2 1.734(3) . ? N4 P2 1.734(3) . ? N5 C50 1.439(5) . ? N5 P2 1.753(3) . ? N5 P1 1.758(3) . ? N6A C55 1.267(7) . ? N6B C51 1.192(10) . ? P1 Si1 2.5570(15) . ? P2 Si2 2.5603(14) . ? Si1 C2 1.849(5) . ? Si1 C1 1.856(5) . ? Si2 C4 1.850(5) . ? Si2 C3 1.868(5) . ? C10 C12 1.508(6) . ? C10 C11 1.511(6) . ? C10 C13 1.535(6) . ? C20 C23 1.498(7) . ? C20 C22 1.507(7) . ? C20 C21 1.532(7) . ? C30 C31 1.525(6) . ? C30 C32 1.529(6) . ? C30 C33 1.532(6) . ? C40 C43 1.514(6) . ? C40 C41 1.525(6) . ? C40 C42 1.527(6) . ? C50 C51 1.376(6) . ? C50 C55 1.405(6) . ? C51 C52 1.391(8) . ? C52 C53 1.328(12) . ? C53 C54 1.347(12) . ? C54 C55 1.402(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 C10 N1 P1 123.7(2) . . ? C10 N1 Si1 129.7(2) . . ? P1 N1 Si1 94.63(15) . . ? C20 N2 P1 127.6(3) . . ? C20 N2 Si1 129.7(3) . . ? P1 N2 Si1 95.49(16) . . ? C30 N3 P2 127.5(2) . . ? C30 N3 Si2 130.7(2) . . ? P2 N3 Si2 95.61(15) . . ? C40 N4 Si2 131.9(2) . . ? C40 N4 P2 124.2(2) . . ? Si2 N4 P2 95.17(15) . . ? C50 N5 P2 124.7(2) . . ? C50 N5 P1 126.2(2) . . ? P2 N5 P1 108.96(15) . . ? N2 P1 N1 84.10(15) . . ? N2 P1 N5 106.51(15) . . ? N1 P1 N5 109.96(15) . . ? N2 P1 Si1 42.43(11) . . ? N1 P1 Si1 42.70(11) . . ? N5 P1 Si1 122.23(10) . . ? N3 P2 N4 83.92(15) . . ? N3 P2 N5 106.47(14) . . ? N4 P2 N5 109.65(15) . . ? N3 P2 Si2 42.33(10) . . ? N4 P2 Si2 42.41(10) . . ? N5 P2 Si2 121.14(10) . . ? N2 Si1 N1 83.71(14) . . ? N2 Si1 C2 116.7(2) . . ? N1 Si1 C2 118.3(2) . . ? N2 Si1 C1 115.6(2) . . ? N1 Si1 C1 114.5(2) . . ? C2 Si1 C1 107.0(3) . . ? N2 Si1 P1 42.08(10) . . ? N1 Si1 P1 42.67(10) . . ? C2 Si1 P1 135.6(2) . . ? C1 Si1 P1 117.36(19) . . ? N3 Si2 N4 83.66(14) . . ? N3 Si2 C4 116.5(2) . . ? N4 Si2 C4 117.4(2) . . ? N3 Si2 C3 116.1(2) . . ? N4 Si2 C3 115.4(2) . . ? C4 Si2 C3 106.8(3) . . ? N3 Si2 P2 42.06(10) . . ? N4 Si2 P2 42.42(10) . . ? C4 Si2 P2 133.95(19) . . ? C3 Si2 P2 119.22(17) . . ? N1 C10 C12 109.3(4) . . ? N1 C10 C11 109.8(3) . . ? C12 C10 C11 110.4(4) . . ? N1 C10 C13 111.4(4) . . ? C12 C10 C13 109.1(4) . . ? C11 C10 C13 106.9(4) . . ? N2 C20 C23 110.9(4) . . ? N2 C20 C22 108.8(4) . . ? C23 C20 C22 109.5(5) . . ? N2 C20 C21 110.0(4) . . ? C23 C20 C21 108.7(5) . . ? C22 C20 C21 108.9(5) . . ? N3 C30 C31 108.7(3) . . ? N3 C30 C32 110.0(3) . . ? C31 C30 C32 108.2(4) . . ? N3 C30 C33 110.9(3) . . ? C31 C30 C33 109.0(4) . . ? C32 C30 C33 110.0(4) . . ? N4 C40 C43 110.3(3) . . ? N4 C40 C41 108.3(3) . . ? C43 C40 C41 109.6(4) . . ? N4 C40 C42 110.8(3) . . ? C43 C40 C42 109.1(4) . . ? C41 C40 C42 108.8(4) . . ? C51 C50 C55 119.1(4) . . ? C51 C50 N5 121.1(4) . . ? C55 C50 N5 119.9(4) . . ? N6B C51 C50 132.4(6) . . ? N6B C51 C52 107.3(7) . . ? C50 C51 C52 120.1(6) . . ? C53 C52 C51 120.6(7) . . ? C52 C53 C54 121.2(7) . . ? C53 C54 C55 121.0(7) . . ? N6A C55 C54 112.1(6) . . ? N6A C55 C50 129.8(5) . . ? C54 C55 C50 118.1(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.357 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.068 #===END=== data_10 _database_code_depnum_ccdc_archive 'CCDC 272425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H61 Cl N6 Ni P2 Si2' _chemical_formula_weight 754.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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 10.6331(13) _cell_length_b 15.7716(15) _cell_length_c 25.212(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.343(8) _cell_angle_gamma 90.00 _cell_volume 4220.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 ? _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 7138 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5506 _reflns_number_gt 4971 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+6.0279P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5506 _refine_ls_number_parameters 391 _refine_ls_number_restraints 831 _refine_ls_R_factor_all 0.0566 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.123 _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 0.79395(5) 0.27130(3) 0.183800(19) 0.0437(2) Uani 1 1 d . . . Cl1 Cl 0.79720(16) 0.16962(8) 0.24149(5) 0.0824(4) Uani 1 1 d . . . P1 P 0.81135(11) 0.24091(7) 0.10026(4) 0.0458(3) Uani 1 1 d . A . P2 P 0.77199(10) 0.37693(7) 0.23608(4) 0.0428(3) Uani 1 1 d . . . Si1 Si 0.83270(14) 0.18934(8) 0.00611(5) 0.0596(4) Uani 1 1 d . A . Si2 Si 0.75198(13) 0.39489(8) 0.33468(4) 0.0547(4) Uani 1 1 d . . . N1 N 0.7976(4) 0.3351(2) 0.12304(13) 0.0601(10) Uani 1 1 d . . . N2 N 0.7618(4) 0.4653(2) 0.19976(13) 0.0556(10) Uani 1 1 d . . . H2N H 0.7271 0.5079 0.2153 0.067 Uiso 1 1 calc R . . N3 N 0.9300(4) 0.2183(2) 0.06106(14) 0.0551(9) Uani 1 1 d . A . N4 N 0.7144(4) 0.2130(3) 0.04817(14) 0.0595(10) Uani 1 1 d . . . N5 N 0.8695(3) 0.3952(2) 0.29000(13) 0.0497(8) Uani 1 1 d . . . N6 N 0.6549(3) 0.3806(2) 0.27762(13) 0.0492(8) Uani 1 1 d . C . C1 C 0.8156(4) 0.4200(3) 0.11085(16) 0.0518(11) Uani 1 1 d . . . C2 C 0.8497(6) 0.4434(3) 0.06020(18) 0.0716(15) Uani 1 1 d . . . H2 H 0.8602 0.4012 0.0345 0.086 Uiso 1 1 calc R . . C3 C 0.8679(7) 0.5265(3) 0.0473(2) 0.090(2) Uani 1 1 d . . . H3 H 0.8901 0.5412 0.0130 0.108 Uiso 1 1 calc R . . C4 C 0.8535(7) 0.5882(3) 0.0849(2) 0.094(2) Uani 1 1 d . . . H4 H 0.8665 0.6454 0.0763 0.113 Uiso 1 1 calc R . . C5 C 0.8205(6) 0.5669(3) 0.13482(19) 0.0744(15) Uani 1 1 d . . . H5 H 0.8117 0.6098 0.1602 0.089 Uiso 1 1 calc R . . C6 C 0.7995(4) 0.4829(3) 0.14865(16) 0.0498(10) Uani 1 1 d . . . C11 C 0.8400(7) 0.2557(4) -0.0541(2) 0.0921(19) Uani 1 1 d . . . H11A H 0.7736 0.2388 -0.0800 0.138 Uiso 1 1 calc R B . H11B H 0.9212 0.2482 -0.0692 0.138 Uiso 1 1 calc R . . H11C H 0.8291 0.3148 -0.0448 0.138 Uiso 1 1 calc R . . C12 C 0.8422(6) 0.0770(3) -0.0151(2) 0.0858(17) Uani 1 1 d . . . H12A H 0.8430 0.0405 0.0158 0.129 Uiso 1 1 calc R B . H12B H 0.9188 0.0684 -0.0335 0.129 Uiso 1 1 calc R . . H12C H 0.7698 0.0635 -0.0388 0.129 Uiso 1 1 calc R . . C21 C 0.7291(6) 0.4944(4) 0.3716(2) 0.0880(18) Uani 1 1 d . . . H21A H 0.7982 0.5019 0.3981 0.132 Uiso 1 1 calc R . . H21B H 0.6503 0.4916 0.3891 0.132 Uiso 1 1 calc R . . H21C H 0.7268 0.5418 0.3471 0.132 Uiso 1 1 calc R . . C22 C 0.7582(6) 0.3042(4) 0.3814(2) 0.0888(18) Uani 1 1 d . . . H22A H 0.7743 0.2524 0.3622 0.133 Uiso 1 1 calc R . . H22B H 0.6784 0.2995 0.3980 0.133 Uiso 1 1 calc R . . H22C H 0.8253 0.3133 0.4086 0.133 Uiso 1 1 calc R . . C30 C 1.0642(4) 0.2114(3) 0.07658(18) 0.0628(12) Uani 1 1 d DU . . C31 C 1.0898(16) 0.1590(14) 0.1273(7) 0.104(6) Uiso 0.44(2) 1 d PDU A 1 H31A H 1.0592 0.1016 0.1214 0.157 Uiso 0.44(2) 1 calc PR A 1 H31B H 1.0467 0.1845 0.1562 0.157 Uiso 0.44(2) 1 calc PR A 1 H31C H 1.1797 0.1577 0.1364 0.157 Uiso 0.44(2) 1 calc PR A 1 C32 C 1.1135(14) 0.3003(7) 0.0875(9) 0.087(5) Uiso 0.44(2) 1 d PDU A 1 H32A H 1.0981 0.3350 0.0560 0.130 Uiso 0.44(2) 1 calc PR A 1 H32B H 1.2033 0.2980 0.0967 0.130 Uiso 0.44(2) 1 calc PR A 1 H32C H 1.0706 0.3248 0.1168 0.130 Uiso 0.44(2) 1 calc PR A 1 C33 C 1.1334(13) 0.1720(13) 0.0310(5) 0.082(5) Uiso 0.44(2) 1 d PDU A 1 H33A H 1.1010 0.1154 0.0238 0.123 Uiso 0.44(2) 1 calc PR A 1 H33B H 1.2228 0.1688 0.0410 0.123 Uiso 0.44(2) 1 calc PR A 1 H33C H 1.1203 0.2067 -0.0006 0.123 Uiso 0.44(2) 1 calc PR A 1 C31' C 1.0856(11) 0.1278(7) 0.1057(6) 0.085(4) Uiso 0.56(2) 1 d PDU A 2 H31D H 1.0571 0.0814 0.0827 0.127 Uiso 0.56(2) 1 calc PR A 2 H31E H 1.0388 0.1275 0.1375 0.127 Uiso 0.56(2) 1 calc PR A 2 H31F H 1.1747 0.1210 0.1153 0.127 Uiso 0.56(2) 1 calc PR A 2 C32' C 1.1081(12) 0.2837(8) 0.1122(7) 0.094(4) Uiso 0.56(2) 1 d PDU A 2 H32D H 1.0963 0.3369 0.0931 0.141 Uiso 0.56(2) 1 calc PR A 2 H32E H 1.1966 0.2764 0.1227 0.141 Uiso 0.56(2) 1 calc PR A 2 H32F H 1.0595 0.2845 0.1435 0.141 Uiso 0.56(2) 1 calc PR A 2 C33' C 1.1360(12) 0.2134(13) 0.0255(4) 0.098(4) Uiso 0.56(2) 1 d PDU A 2 H33D H 1.1075 0.1671 0.0025 0.147 Uiso 0.56(2) 1 calc PR A 2 H33E H 1.2256 0.2073 0.0345 0.147 Uiso 0.56(2) 1 calc PR A 2 H33F H 1.1204 0.2669 0.0074 0.147 Uiso 0.56(2) 1 calc PR A 2 C40 C 0.5708(13) 0.2088(8) 0.0428(4) 0.065(5) Uiso 0.535(16) 1 d PDU B 1 C41 C 0.5341(15) 0.2916(9) 0.0154(7) 0.124(6) Uiso 0.535(16) 1 d PDU B 1 H41A H 0.5679 0.2930 -0.0195 0.186 Uiso 0.535(16) 1 calc PR B 1 H41B H 0.5680 0.3388 0.0364 0.186 Uiso 0.535(16) 1 calc PR B 1 H41C H 0.4430 0.2960 0.0118 0.186 Uiso 0.535(16) 1 calc PR B 1 C42 C 0.5189(14) 0.2028(11) 0.0970(5) 0.094(4) Uiso 0.535(16) 1 d PDU B 1 H42A H 0.5435 0.1491 0.1132 0.141 Uiso 0.535(16) 1 calc PR B 1 H42B H 0.4277 0.2064 0.0935 0.141 Uiso 0.535(16) 1 calc PR B 1 H42C H 0.5519 0.2489 0.1191 0.141 Uiso 0.535(16) 1 calc PR B 1 C43 C 0.5283(11) 0.1374(8) 0.0062(5) 0.088(4) Uiso 0.535(16) 1 d PDU B 1 H43A H 0.5523 0.0836 0.0224 0.132 Uiso 0.535(16) 1 calc PR B 1 H43B H 0.5679 0.1432 -0.0273 0.132 Uiso 0.535(16) 1 calc PR B 1 H43C H 0.4375 0.1395 -0.0001 0.132 Uiso 0.535(16) 1 calc PR B 1 C40' C 0.5815(15) 0.2260(9) 0.0444(5) 0.067(6) Uiso 0.465(16) 1 d PDU B 2 C41' C 0.5355(14) 0.3158(8) 0.0506(7) 0.098(5) Uiso 0.465(16) 1 d PDU B 2 H41D H 0.5672 0.3380 0.0847 0.147 Uiso 0.465(16) 1 calc PR B 2 H41E H 0.4441 0.3164 0.0488 0.147 Uiso 0.465(16) 1 calc PR B 2 H41F H 0.5657 0.3507 0.0224 0.147 Uiso 0.465(16) 1 calc PR B 2 C42' C 0.5243(15) 0.1700(11) 0.0885(6) 0.090(5) Uiso 0.465(16) 1 d PDU B 2 H42D H 0.5519 0.1118 0.0848 0.135 Uiso 0.465(16) 1 calc PR B 2 H42E H 0.4331 0.1724 0.0846 0.135 Uiso 0.465(16) 1 calc PR B 2 H42F H 0.5526 0.1913 0.1232 0.135 Uiso 0.465(16) 1 calc PR B 2 C43' C 0.5304(16) 0.1937(14) -0.0096(6) 0.122(6) Uiso 0.465(16) 1 d PDU B 2 H43D H 0.5559 0.1351 -0.0140 0.182 Uiso 0.465(16) 1 calc PR B 2 H43E H 0.5637 0.2280 -0.0374 0.182 Uiso 0.465(16) 1 calc PR B 2 H43F H 0.4392 0.1972 -0.0117 0.182 Uiso 0.465(16) 1 calc PR B 2 C50 C 0.0014(13) 0.4216(8) 0.2897(5) 0.072(5) Uiso 0.59(3) 1 d PDU . 1 C51 C 0.0140(12) 0.5164(7) 0.2829(6) 0.091(4) Uiso 0.59(3) 1 d PDU . 1 H51A H -0.0241 0.5329 0.2486 0.136 Uiso 0.59(3) 1 calc PR . 1 H51B H 0.1025 0.5317 0.2850 0.136 Uiso 0.59(3) 1 calc PR . 1 H51C H -0.0284 0.5452 0.3108 0.136 Uiso 0.59(3) 1 calc PR . 1 C52 C 0.0601(12) 0.4000(13) 0.3448(4) 0.099(4) Uiso 0.59(3) 1 d PDU . 1 H52A H 0.0536 0.3394 0.3508 0.149 Uiso 0.59(3) 1 calc PR . 1 H52B H 0.0160 0.4303 0.3715 0.149 Uiso 0.59(3) 1 calc PR . 1 H52C H 0.1482 0.4164 0.3469 0.149 Uiso 0.59(3) 1 calc PR . 1 C53 C 0.0671(12) 0.3640(10) 0.2500(6) 0.089(4) Uiso 0.59(3) 1 d PDU . 1 H53A H 0.0514 0.3050 0.2583 0.134 Uiso 0.59(3) 1 calc PR . 1 H53B H 0.1571 0.3747 0.2527 0.134 Uiso 0.59(3) 1 calc PR . 1 H53C H 0.0339 0.3762 0.2141 0.134 Uiso 0.59(3) 1 calc PR . 1 C50' C 0.0082(15) 0.4051(10) 0.2944(5) 0.050(5) Uiso 0.41(3) 1 d PDU . 2 C51' C 0.038(2) 0.4994(12) 0.3040(11) 0.113(7) Uiso 0.41(3) 1 d PDU . 2 H51D H -0.0016 0.5329 0.2754 0.169 Uiso 0.41(3) 1 calc PR . 2 H51E H 0.1282 0.5080 0.3053 0.169 Uiso 0.41(3) 1 calc PR . 2 H51F H 0.0053 0.5169 0.3375 0.169 Uiso 0.41(3) 1 calc PR . 2 C52' C 0.0687(15) 0.3567(16) 0.3402(6) 0.088(6) Uiso 0.41(3) 1 d PDU . 2 H52D H 0.0274 0.3706 0.3723 0.132 Uiso 0.41(3) 1 calc PR . 2 H52E H 0.1572 0.3717 0.3445 0.132 Uiso 0.41(3) 1 calc PR . 2 H52F H 0.0608 0.2964 0.3333 0.132 Uiso 0.41(3) 1 calc PR . 2 C53' C 0.0620(15) 0.3938(13) 0.2400(5) 0.071(5) Uiso 0.41(3) 1 d PDU . 2 H53D H 0.0189 0.4317 0.2146 0.107 Uiso 0.41(3) 1 calc PR . 2 H53E H 0.0500 0.3356 0.2283 0.107 Uiso 0.41(3) 1 calc PR . 2 H53F H 0.1512 0.4071 0.2425 0.107 Uiso 0.41(3) 1 calc PR . 2 C60 C 0.5203(4) 0.3650(3) 0.26726(19) 0.0682(13) Uani 1 1 d DU . . C61 C 0.4588(17) 0.4543(9) 0.2720(8) 0.113(6) Uiso 0.396(11) 1 d PDU C 1 H61A H 0.4827 0.4784 0.3065 0.170 Uiso 0.396(11) 1 calc PR C 1 H61B H 0.3679 0.4489 0.2681 0.170 Uiso 0.396(11) 1 calc PR C 1 H61C H 0.4876 0.4911 0.2443 0.170 Uiso 0.396(11) 1 calc PR C 1 C62 C 0.4674(17) 0.3188(12) 0.3139(6) 0.112(7) Uiso 0.396(11) 1 d PDU C 1 H62A H 0.4958 0.3466 0.3468 0.169 Uiso 0.396(11) 1 calc PR C 1 H62B H 0.4965 0.2605 0.3145 0.169 Uiso 0.396(11) 1 calc PR C 1 H62C H 0.3761 0.3197 0.3103 0.169 Uiso 0.396(11) 1 calc PR C 1 C63 C 0.4829(17) 0.3260(12) 0.2154(5) 0.102(6) Uiso 0.396(11) 1 d PDU C 1 H63A H 0.5168 0.3591 0.1871 0.153 Uiso 0.396(11) 1 calc PR C 1 H63B H 0.3918 0.3245 0.2107 0.153 Uiso 0.396(11) 1 calc PR C 1 H63C H 0.5157 0.2686 0.2144 0.153 Uiso 0.396(11) 1 calc PR C 1 C61' C 0.4455(12) 0.4105(9) 0.3069(5) 0.125(5) Uiso 0.604(11) 1 d PDU C 2 H61D H 0.4770 0.3954 0.3426 0.187 Uiso 0.604(11) 1 calc PR C 2 H61E H 0.3576 0.3943 0.3020 0.187 Uiso 0.604(11) 1 calc PR C 2 H61F H 0.4534 0.4712 0.3020 0.187 Uiso 0.604(11) 1 calc PR C 2 C62' C 0.4976(14) 0.2687(7) 0.2736(6) 0.130(5) Uiso 0.604(11) 1 d PDU C 2 H62D H 0.5442 0.2379 0.2478 0.194 Uiso 0.604(11) 1 calc PR C 2 H62E H 0.4084 0.2567 0.2677 0.194 Uiso 0.604(11) 1 calc PR C 2 H62F H 0.5260 0.2512 0.3092 0.194 Uiso 0.604(11) 1 calc PR C 2 C63' C 0.4771(10) 0.3860(8) 0.2102(4) 0.093(3) Uiso 0.604(11) 1 d PDU C 2 H63D H 0.5282 0.3550 0.1861 0.140 Uiso 0.604(11) 1 calc PR C 2 H63E H 0.4861 0.4464 0.2042 0.140 Uiso 0.604(11) 1 calc PR C 2 H63F H 0.3895 0.3699 0.2039 0.140 Uiso 0.604(11) 1 calc PR C 2 C70 C 0.6598(15) 0.3983(14) 0.8307(7) 0.146(6) Uiso 0.584(14) 1 d PDU D 1 C71 C 0.7634(14) 0.4384(10) 0.8534(6) 0.122(5) Uiso 0.584(14) 1 d PDU D 1 H71 H 0.8412 0.4377 0.8375 0.147 Uiso 0.584(14) 1 calc PR D 1 C72 C 0.7487(17) 0.4784(14) 0.8988(7) 0.136(6) Uiso 0.584(14) 1 d PDU D 1 H72 H 0.8203 0.5045 0.9152 0.164 Uiso 0.584(14) 1 calc PR D 1 C73 C 0.6390(15) 0.4850(11) 0.9237(6) 0.139(6) Uiso 0.584(14) 1 d PDU D 1 H73 H 0.6334 0.5166 0.9551 0.167 Uiso 0.584(14) 1 calc PR D 1 C74 C 0.5367(17) 0.4429(14) 0.9004(8) 0.163(7) Uiso 0.584(14) 1 d PDU D 1 H74 H 0.4587 0.4441 0.9161 0.196 Uiso 0.584(14) 1 calc PR D 1 C75 C 0.5499(13) 0.4006(10) 0.8553(6) 0.105(4) Uiso 0.584(14) 1 d PDU D 1 H75 H 0.4802 0.3711 0.8400 0.126 Uiso 0.584(14) 1 calc PR D 1 C76 C 0.674(2) 0.3574(16) 0.7798(8) 0.206(10) Uiso 0.584(14) 1 d PDU D 1 H76A H 0.5949 0.3323 0.7672 0.310 Uiso 0.584(14) 1 calc PR D 1 H76B H 0.7381 0.3135 0.7839 0.310 Uiso 0.584(14) 1 calc PR D 1 H76C H 0.7001 0.3991 0.7543 0.310 Uiso 0.584(14) 1 calc PR D 1 C70' C 0.5996(17) 0.4435(13) 0.8881(7) 0.114(6) Uiso 0.416(14) 1 d PDU D 2 C71' C 0.7081(19) 0.4807(19) 0.9048(10) 0.135(9) Uiso 0.416(14) 1 d PDU D 2 H71' H 0.7127 0.5159 0.9349 0.162 Uiso 0.416(14) 1 calc PR D 2 C72' C 0.8098(18) 0.4659(15) 0.8772(9) 0.138(8) Uiso 0.416(14) 1 d PDU D 2 H72' H 0.8866 0.4912 0.8889 0.166 Uiso 0.416(14) 1 calc PR D 2 C73' C 0.8075(18) 0.4165(13) 0.8334(8) 0.116(6) Uiso 0.416(14) 1 d PDU D 2 H73' H 0.8812 0.4073 0.8153 0.139 Uiso 0.416(14) 1 calc PR D 2 C74' C 0.699(2) 0.381(2) 0.8163(11) 0.170(11) Uiso 0.416(14) 1 d PDU D 2 H74' H 0.6954 0.3478 0.7854 0.204 Uiso 0.416(14) 1 calc PR D 2 C75' C 0.591(2) 0.3936(19) 0.8439(10) 0.144(9) Uiso 0.416(14) 1 d PDU D 2 H75' H 0.5145 0.3682 0.8324 0.172 Uiso 0.416(14) 1 calc PR D 2 C76' C 0.506(2) 0.468(2) 0.9247(11) 0.187(13) Uiso 0.416(14) 1 d PDU D 2 H76D H 0.4255 0.4420 0.9137 0.280 Uiso 0.416(14) 1 calc PR D 2 H76E H 0.4966 0.5291 0.9246 0.280 Uiso 0.416(14) 1 calc PR D 2 H76F H 0.5318 0.4487 0.9602 0.280 Uiso 0.416(14) 1 calc PR D 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 Ni1 0.0563(4) 0.0383(3) 0.0373(3) 0.0014(2) 0.0090(2) 0.0012(2) Cl1 0.1326(12) 0.0537(7) 0.0617(8) 0.0178(6) 0.0127(8) 0.0013(7) P1 0.0604(7) 0.0407(6) 0.0371(6) -0.0020(4) 0.0093(5) 0.0038(5) P2 0.0531(6) 0.0426(6) 0.0335(5) 0.0002(4) 0.0103(5) 0.0000(5) Si1 0.0841(9) 0.0559(8) 0.0398(7) -0.0068(6) 0.0116(6) 0.0076(7) Si2 0.0742(8) 0.0559(7) 0.0352(6) -0.0037(5) 0.0127(6) -0.0090(6) N1 0.102(3) 0.042(2) 0.0383(19) 0.0010(16) 0.0204(19) 0.0041(19) N2 0.090(3) 0.0394(19) 0.0401(19) -0.0003(15) 0.0219(18) 0.0087(18) N3 0.066(2) 0.055(2) 0.045(2) -0.0065(16) 0.0146(17) 0.0029(18) N4 0.066(2) 0.071(2) 0.042(2) -0.0087(18) 0.0008(17) 0.009(2) N5 0.054(2) 0.054(2) 0.0412(19) -0.0038(16) 0.0047(16) -0.0065(17) N6 0.054(2) 0.054(2) 0.0404(18) -0.0022(16) 0.0146(16) -0.0021(16) C1 0.074(3) 0.041(2) 0.042(2) 0.0031(19) 0.017(2) 0.005(2) C2 0.119(4) 0.052(3) 0.047(3) 0.002(2) 0.032(3) 0.010(3) C3 0.161(6) 0.056(3) 0.059(3) 0.012(3) 0.053(4) 0.004(3) C4 0.165(6) 0.047(3) 0.076(4) 0.010(3) 0.054(4) -0.004(3) C5 0.127(5) 0.044(3) 0.056(3) 0.001(2) 0.034(3) 0.001(3) C6 0.070(3) 0.040(2) 0.040(2) 0.0031(18) 0.017(2) 0.005(2) C11 0.143(6) 0.087(4) 0.048(3) 0.004(3) 0.018(3) 0.009(4) C12 0.124(5) 0.068(3) 0.066(3) -0.016(3) 0.013(3) 0.009(3) C21 0.119(5) 0.083(4) 0.064(3) -0.027(3) 0.024(3) -0.011(4) C22 0.126(5) 0.092(4) 0.049(3) 0.018(3) 0.008(3) -0.020(4) C30 0.064(3) 0.067(3) 0.060(3) -0.001(2) 0.017(2) 0.002(2) C60 0.057(3) 0.085(4) 0.064(3) -0.004(3) 0.018(2) -0.004(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 N1 1.835(3) . ? Ni1 P2 2.1456(11) . ? Ni1 Cl1 2.1640(13) . ? Ni1 P1 2.1783(12) . ? P1 N1 1.603(4) . ? P1 N4 1.680(4) . ? P1 N3 1.685(4) . ? P1 Si1 2.5319(16) . ? P2 N2 1.668(3) . ? P2 N6 1.674(3) . ? P2 N5 1.686(3) . ? P2 Si2 2.5232(15) . ? Si1 N4 1.732(4) . ? Si1 N3 1.741(4) . ? Si1 C11 1.850(5) . ? Si1 C12 1.855(5) . ? Si2 N5 1.730(3) . ? Si2 N6 1.736(4) . ? Si2 C21 1.848(5) . ? Si2 C22 1.852(5) . ? N1 C1 1.389(6) . ? N2 C6 1.400(5) . ? N3 C30 1.462(6) . ? N4 C40' 1.426(16) . ? N4 C40 1.526(14) . ? N5 C50 1.464(14) 1_655 ? N5 C50' 1.481(16) 1_655 ? N6 C60 1.460(6) . ? C1 C6 1.393(6) . ? C1 C2 1.397(6) . ? C2 C3 1.366(7) . ? C3 C4 1.375(7) . ? C4 C5 1.367(7) . ? C5 C6 1.391(6) . ? C30 C32' 1.508(10) . ? C30 C32 1.517(11) . ? C30 C31' 1.519(9) . ? C30 C33 1.532(10) . ? C30 C31 1.533(11) . ? C30 C33' 1.534(10) . ? C40 C42 1.506(11) . ? C40 C43 1.509(12) . ? C40 C41 1.518(12) . ? C40' C41' 1.510(13) . ? C40' C43' 1.523(13) . ? C40' C42' 1.569(13) . ? C50 N5 1.464(14) 1_455 ? C50 C51 1.511(12) . ? C50 C52 1.527(12) . ? C50 C53 1.549(11) . ? C50' N5 1.481(16) 1_455 ? C50' C52' 1.497(13) . ? C50' C53' 1.526(12) . ? C50' C51' 1.537(13) . ? C60 C63 1.478(11) . ? C60 C61' 1.497(10) . ? C60 C62 1.520(12) . ? C60 C63' 1.521(9) . ? C60 C62' 1.548(10) . ? C60 C61 1.560(12) . ? C70 C75 1.355(13) . ? C70 C71 1.366(12) . ? C70 C76 1.45(2) . ? C71 C72 1.325(13) . ? C72 C73 1.360(13) . ? C73 C74 1.376(14) . ? C74 C75 1.332(13) . ? C70' C71' 1.340(14) . ? C70' C75' 1.362(14) . ? C70' C76' 1.45(2) . ? C71' C72' 1.341(14) . ? C72' C73' 1.350(14) . ? C73' C74' 1.329(14) . ? C74' C75' 1.390(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 P2 95.46(11) . . ? N1 Ni1 Cl1 165.29(12) . . ? P2 Ni1 Cl1 99.24(5) . . ? N1 Ni1 P1 46.10(11) . . ? P2 Ni1 P1 141.56(5) . . ? Cl1 Ni1 P1 119.20(5) . . ? N1 P1 N4 117.3(2) . . ? N1 P1 N3 119.5(2) . . ? N4 P1 N3 86.11(19) . . ? N1 P1 Ni1 55.60(12) . . ? N4 P1 Ni1 136.94(14) . . ? N3 P1 Ni1 136.24(14) . . ? N1 P1 Si1 130.45(14) . . ? N4 P1 Si1 42.90(13) . . ? N3 P1 Si1 43.21(13) . . ? Ni1 P1 Si1 173.96(6) . . ? N2 P2 N6 106.73(18) . . ? N2 P2 N5 108.49(18) . . ? N6 P2 N5 86.25(17) . . ? N2 P2 Ni1 108.52(12) . . ? N6 P2 Ni1 121.51(13) . . ? N5 P2 Ni1 122.97(13) . . ? N2 P2 Si2 116.14(13) . . ? N6 P2 Si2 43.22(12) . . ? N5 P2 Si2 43.08(12) . . ? Ni1 P2 Si2 135.30(6) . . ? N4 Si1 N3 82.84(17) . . ? N4 Si1 C11 116.6(3) . . ? N3 Si1 C11 117.0(3) . . ? N4 Si1 C12 115.8(3) . . ? N3 Si1 C12 116.1(2) . . ? C11 Si1 C12 107.3(3) . . ? N4 Si1 P1 41.32(12) . . ? N3 Si1 P1 41.52(12) . . ? C11 Si1 P1 126.8(2) . . ? C12 Si1 P1 125.92(19) . . ? N5 Si2 N6 82.99(16) . . ? N5 Si2 C21 116.6(2) . . ? N6 Si2 C21 116.0(2) . . ? N5 Si2 C22 114.6(3) . . ? N6 Si2 C22 115.2(2) . . ? C21 Si2 C22 109.6(3) . . ? N5 Si2 P2 41.70(11) . . ? N6 Si2 P2 41.34(11) . . ? C21 Si2 P2 127.8(2) . . ? C22 Si2 P2 122.6(2) . . ? C1 N1 P1 142.9(3) . . ? C1 N1 Ni1 136.3(3) . . ? P1 N1 Ni1 78.30(15) . . ? C6 N2 P2 131.2(3) . . ? C30 N3 P1 127.7(3) . . ? C30 N3 Si1 136.0(3) . . ? P1 N3 Si1 95.3(2) . . ? C40' N4 C40 10.8(8) . . ? C40' N4 P1 125.1(6) . . ? C40 N4 P1 130.2(5) . . ? C40' N4 Si1 137.9(6) . . ? C40 N4 Si1 134.0(5) . . ? P1 N4 Si1 95.8(2) . . ? C50 N5 C50' 11.4(8) 1_655 1_655 ? C50 N5 P2 126.1(5) 1_655 . ? C50' N5 P2 129.9(5) 1_655 . ? C50 N5 Si2 137.1(5) 1_655 . ? C50' N5 Si2 134.9(5) 1_655 . ? P2 N5 Si2 95.22(18) . . ? C60 N6 P2 129.7(3) . . ? C60 N6 Si2 134.4(3) . . ? P2 N6 Si2 95.44(18) . . ? N1 C1 C6 120.7(4) . . ? N1 C1 C2 120.2(4) . . ? C6 C1 C2 119.0(4) . . ? C3 C2 C1 121.3(4) . . ? C2 C3 C4 119.5(5) . . ? C5 C4 C3 120.4(5) . . ? C4 C5 C6 121.2(5) . . ? C5 C6 C1 118.6(4) . . ? C5 C6 N2 118.6(4) . . ? C1 C6 N2 122.8(4) . . ? N3 C30 C32' 111.4(6) . . ? N3 C30 C32 107.5(7) . . ? C32' C30 C32 26.0(7) . . ? N3 C30 C31' 108.1(6) . . ? C32' C30 C31' 109.7(7) . . ? C32 C30 C31' 132.4(8) . . ? N3 C30 C33 109.5(6) . . ? C32' C30 C33 127.4(8) . . ? C32 C30 C33 109.6(8) . . ? C31' C30 C33 86.8(8) . . ? N3 C30 C31 112.7(7) . . ? C32' C30 C31 83.0(9) . . ? C32 C30 C31 107.7(9) . . ? C31' C30 C31 27.8(7) . . ? C33 C30 C31 109.7(9) . . ? N3 C30 C33' 107.4(6) . . ? C32' C30 C33' 109.4(8) . . ? C32 C30 C33' 87.1(8) . . ? C31' C30 C33' 110.7(7) . . ? C33 C30 C33' 25.2(7) . . ? C31 C30 C33' 129.6(9) . . ? C42 C40 C43 113.2(11) . . ? C42 C40 C41 111.6(11) . . ? C43 C40 C41 107.7(10) . . ? C42 C40 N4 109.9(9) . . ? C43 C40 N4 110.4(9) . . ? C41 C40 N4 103.5(10) . . ? N4 C40' C41' 117.0(12) . . ? N4 C40' C43' 108.2(11) . . ? C41' C40' C43' 107.8(12) . . ? N4 C40' C42' 107.2(11) . . ? C41' C40' C42' 108.2(11) . . ? C43' C40' C42' 108.2(12) . . ? N5 C50 C51 111.9(9) 1_455 . ? N5 C50 C52 105.9(9) 1_455 . ? C51 C50 C52 106.9(10) . . ? N5 C50 C53 107.7(9) 1_455 . ? C51 C50 C53 117.4(11) . . ? C52 C50 C53 106.3(10) . . ? N5 C50' C52' 112.7(11) 1_455 . ? N5 C50' C53' 110.1(10) 1_455 . ? C52' C50' C53' 117.8(13) . . ? N5 C50' C51' 107.9(12) 1_455 . ? C52' C50' C51' 107.3(12) . . ? C53' C50' C51' 99.8(12) . . ? N6 C60 C63 116.0(8) . . ? N6 C60 C61' 110.7(6) . . ? C63 C60 C61' 131.7(10) . . ? N6 C60 C62 110.2(8) . . ? C63 C60 C62 113.1(10) . . ? C61' C60 C62 58.5(8) . . ? N6 C60 C63' 111.8(5) . . ? C63 C60 C63' 37.2(7) . . ? C61' C60 C63' 112.7(7) . . ? C62 C60 C63' 137.0(9) . . ? N6 C60 C62' 107.7(7) . . ? C63 C60 C62' 69.3(9) . . ? C61' C60 C62' 108.0(8) . . ? C62 C60 C62' 51.8(8) . . ? C63' C60 C62' 105.7(7) . . ? N6 C60 C61 104.2(8) . . ? C63 C60 C61 110.6(10) . . ? C61' C60 C61 43.5(8) . . ? C62 C60 C61 101.4(10) . . ? C63' C60 C61 76.8(8) . . ? C62' C60 C61 144.0(10) . . ? C75 C70 C71 119.4(13) . . ? C75 C70 C76 123.8(14) . . ? C71 C70 C76 116.8(14) . . ? C72 C71 C70 116.8(13) . . ? C71 C72 C73 125.6(14) . . ? C72 C73 C74 116.4(14) . . ? C75 C74 C73 119.0(15) . . ? C74 C75 C70 122.7(13) . . ? C71' C70' C75' 121.6(15) . . ? C71' C70' C76' 107.2(15) . . ? C75' C70' C76' 131.1(17) . . ? C70' C71' C72' 117.8(16) . . ? C71' C72' C73' 123.2(16) . . ? C74' C73' C72' 118.7(15) . . ? C73' C74' C75' 120.3(17) . . ? C70' C75' C74' 118.3(16) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.586 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.065 #===END=== data_11 _database_code_depnum_ccdc_archive 'CCDC 272426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H67 N6 Ni P3 Si2' _chemical_formula_weight 743.72 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' Si Si 0.0817 0.0704 '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 11.4153(15) _cell_length_b 12.2457(16) _cell_length_c 16.145(2) _cell_angle_alpha 79.259(2) _cell_angle_beta 79.351(2) _cell_angle_gamma 69.353(2) _cell_volume 2057.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 0.675 _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 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' _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 10494 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0981 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7116 _reflns_number_gt 4649 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^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 7116 _refine_ls_number_parameters 416 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0822 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _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 0.73457(4) 0.27164(4) 0.24875(3) 0.01727(15) Uani 1 1 d . . . P1 P 0.77884(9) 0.40817(8) 0.29108(6) 0.0172(2) Uani 1 1 d . . . P2 P 0.57599(10) 0.24886(9) 0.20564(6) 0.0199(3) Uani 1 1 d . . . P3 P 0.87879(10) 0.10331(9) 0.24691(7) 0.0257(3) Uani 1 1 d . . . Si1 Si 0.86599(11) 0.54295(10) 0.34289(8) 0.0286(3) Uani 1 1 d . . . Si2 Si 0.53845(12) 0.08017(10) 0.15666(8) 0.0293(3) Uani 1 1 d . . . N1 N 0.6452(3) 0.4274(3) 0.2638(2) 0.0218(8) Uani 1 1 d . . . N2 N 0.4551(3) 0.3665(3) 0.2036(2) 0.0240(8) Uani 1 1 d . . . N3 N 0.7854(3) 0.4443(3) 0.3853(2) 0.0205(7) Uani 1 1 d . . . N4 N 0.8521(3) 0.5071(3) 0.2477(2) 0.0229(8) Uani 1 1 d . . . N5 N 0.5274(3) 0.1308(3) 0.2520(2) 0.0224(8) Uani 1 1 d . . . N6 N 0.6042(3) 0.1886(3) 0.1138(2) 0.0236(8) Uani 1 1 d . . . C1 C 0.5246(3) 0.5091(3) 0.2565(2) 0.0186(9) Uani 1 1 d . . . C2 C 0.4937(4) 0.6200(3) 0.2763(2) 0.0223(9) Uani 1 1 d . . . H2 H 0.5561 0.6420 0.2942 0.027 Uiso 1 1 calc R . . C3 C 0.3750(4) 0.7013(3) 0.2714(3) 0.0267(10) Uani 1 1 d . . . H3 H 0.3552 0.7778 0.2865 0.032 Uiso 1 1 calc R . . C4 C 0.2848(4) 0.6695(3) 0.2440(2) 0.0252(10) Uani 1 1 d . . . H4 H 0.2022 0.7244 0.2404 0.030 Uiso 1 1 calc R . . C5 C 0.3144(4) 0.5594(3) 0.2222(2) 0.0218(9) Uani 1 1 d . . . H5 H 0.2512 0.5400 0.2031 0.026 Uiso 1 1 calc R . . C6 C 0.4345(4) 0.4735(3) 0.2269(2) 0.0199(9) Uani 1 1 d . . . C7 C 0.7816(5) 0.6978(4) 0.3626(3) 0.0522(14) Uani 1 1 d . . . H7A H 0.8178 0.7503 0.3208 0.078 Uiso 1 1 calc R . . H7B H 0.7907 0.7066 0.4200 0.078 Uiso 1 1 calc R . . H7C H 0.6919 0.7184 0.3575 0.078 Uiso 1 1 calc R . . C8 C 1.0294(4) 0.4961(5) 0.3688(3) 0.0513(15) Uani 1 1 d . . . H8A H 1.0746 0.4155 0.3561 0.077 Uiso 1 1 calc R . . H8B H 1.0273 0.4991 0.4293 0.077 Uiso 1 1 calc R . . H8C H 1.0727 0.5490 0.3346 0.077 Uiso 1 1 calc R . . C9 C 0.3876(5) 0.0940(4) 0.1201(3) 0.0455(13) Uani 1 1 d . . . H9A H 0.3284 0.1740 0.1237 0.068 Uiso 1 1 calc R . . H9B H 0.3510 0.0373 0.1562 0.068 Uiso 1 1 calc R . . H9C H 0.4042 0.0779 0.0610 0.068 Uiso 1 1 calc R . . C10 C 0.6464(5) -0.0741(4) 0.1489(3) 0.0448(13) Uani 1 1 d . . . H10A H 0.6650 -0.0882 0.0893 0.067 Uiso 1 1 calc R . . H10B H 0.6056 -0.1293 0.1825 0.067 Uiso 1 1 calc R . . H10C H 0.7251 -0.0858 0.1707 0.067 Uiso 1 1 calc R . . C11 C 0.7520(3) 0.3929(3) 0.4726(2) 0.0200(9) Uani 1 1 d . . . C12 C 0.7129(4) 0.4899(3) 0.5285(3) 0.0285(10) Uani 1 1 d . . . H12A H 0.7856 0.5139 0.5302 0.043 Uiso 1 1 calc R . . H12B H 0.6822 0.4608 0.5862 0.043 Uiso 1 1 calc R . . H12C H 0.6455 0.5575 0.5053 0.043 Uiso 1 1 calc R . . C13 C 0.6416(4) 0.3491(4) 0.4751(3) 0.0297(10) Uani 1 1 d . . . H13A H 0.5718 0.4132 0.4510 0.045 Uiso 1 1 calc R . . H13B H 0.6134 0.3228 0.5341 0.045 Uiso 1 1 calc R . . H13C H 0.6685 0.2833 0.4417 0.045 Uiso 1 1 calc R . . C14 C 0.8658(4) 0.2911(4) 0.5041(3) 0.0358(11) Uani 1 1 d . . . H14A H 0.8914 0.2289 0.4676 0.054 Uiso 1 1 calc R . . H14B H 0.8424 0.2595 0.5627 0.054 Uiso 1 1 calc R . . H14C H 0.9362 0.3202 0.5020 0.054 Uiso 1 1 calc R . . C15 C 0.9000(4) 0.5329(4) 0.1579(3) 0.0325(11) Uani 1 1 d . . . C16 C 0.7923(5) 0.5731(5) 0.1041(3) 0.0677(18) Uani 1 1 d . . . H16A H 0.7607 0.5079 0.1055 0.101 Uiso 1 1 calc R . . H16B H 0.8230 0.5978 0.0453 0.101 Uiso 1 1 calc R . . H16C H 0.7240 0.6394 0.1268 0.101 Uiso 1 1 calc R . . C17 C 1.0057(7) 0.4231(5) 0.1318(4) 0.113(3) Uani 1 1 d . . . H17A H 1.0638 0.3925 0.1748 0.169 Uiso 1 1 calc R . . H17B H 1.0516 0.4430 0.0768 0.169 Uiso 1 1 calc R . . H17C H 0.9697 0.3631 0.1271 0.169 Uiso 1 1 calc R . . C18 C 0.9563(5) 0.6300(4) 0.1483(3) 0.0513(14) Uani 1 1 d . . . H18A H 0.8898 0.7027 0.1629 0.077 Uiso 1 1 calc R . . H18B H 0.9947 0.6428 0.0894 0.077 Uiso 1 1 calc R . . H18C H 1.0209 0.6074 0.1864 0.077 Uiso 1 1 calc R . . C19 C 0.4475(4) 0.1234(4) 0.3338(3) 0.0288(10) Uani 1 1 d . . . C20 C 0.3074(4) 0.1921(4) 0.3237(3) 0.0385(12) Uani 1 1 d . . . H20A H 0.2975 0.2747 0.3022 0.058 Uiso 1 1 calc R . . H20B H 0.2555 0.1872 0.3790 0.058 Uiso 1 1 calc R . . H20C H 0.2803 0.1578 0.2835 0.058 Uiso 1 1 calc R . . C21 C 0.4615(4) -0.0048(4) 0.3646(3) 0.0375(11) Uani 1 1 d . . . H21A H 0.4346 -0.0369 0.3230 0.056 Uiso 1 1 calc R . . H21B H 0.4088 -0.0109 0.4195 0.056 Uiso 1 1 calc R . . H21C H 0.5500 -0.0493 0.3713 0.056 Uiso 1 1 calc R . . C22 C 0.4830(4) 0.1774(4) 0.3984(3) 0.0347(11) Uani 1 1 d . . . H22A H 0.5713 0.1350 0.4071 0.052 Uiso 1 1 calc R . . H22B H 0.4284 0.1718 0.4524 0.052 Uiso 1 1 calc R . . H22C H 0.4724 0.2603 0.3775 0.052 Uiso 1 1 calc R . . C23 C 0.6222(4) 0.2493(3) 0.0260(2) 0.0240(9) Uani 1 1 d . . . C24 C 0.6883(4) 0.3379(4) 0.0247(3) 0.0337(11) Uani 1 1 d . . . H24A H 0.6334 0.4006 0.0579 0.051 Uiso 1 1 calc R . . H24B H 0.7069 0.3719 -0.0341 0.051 Uiso 1 1 calc R . . H24C H 0.7672 0.2983 0.0495 0.051 Uiso 1 1 calc R . . C25 C 0.7045(5) 0.1559(4) -0.0304(3) 0.0424(12) Uani 1 1 d . . . H25A H 0.7890 0.1214 -0.0127 0.064 Uiso 1 1 calc R . . H25B H 0.7108 0.1923 -0.0897 0.064 Uiso 1 1 calc R . . H25C H 0.6665 0.0941 -0.0249 0.064 Uiso 1 1 calc R . . C26 C 0.4968(4) 0.3134(4) -0.0082(3) 0.0387(12) Uani 1 1 d . . . H26A H 0.4588 0.2558 -0.0152 0.058 Uiso 1 1 calc R . . H26B H 0.5108 0.3594 -0.0634 0.058 Uiso 1 1 calc R . . H26C H 0.4399 0.3661 0.0318 0.058 Uiso 1 1 calc R . . C27 C 1.0234(4) 0.1003(3) 0.2823(3) 0.0291(10) Uani 1 1 d . . . H27A H 1.0552 0.1596 0.2439 0.035 Uiso 1 1 calc R . . H27B H 1.0014 0.1249 0.3398 0.035 Uiso 1 1 calc R . . C28 C 1.1303(4) -0.0172(4) 0.2858(3) 0.0389(12) Uani 1 1 d . . . H28A H 1.0991 -0.0783 0.3206 0.058 Uiso 1 1 calc R . . H28B H 1.1992 -0.0109 0.3108 0.058 Uiso 1 1 calc R . . H28C H 1.1613 -0.0379 0.2281 0.058 Uiso 1 1 calc R . . C29 C 0.9346(4) 0.0449(4) 0.1452(3) 0.0362(11) Uani 1 1 d . . . H29A H 0.9867 -0.0391 0.1558 0.043 Uiso 1 1 calc R . . H29B H 0.8609 0.0489 0.1193 0.043 Uiso 1 1 calc R . . C30 C 1.0127(4) 0.1108(4) 0.0820(3) 0.0411(12) Uani 1 1 d . . . H30A H 0.9678 0.1957 0.0786 0.062 Uiso 1 1 calc R . . H30B H 1.0252 0.0861 0.0257 0.062 Uiso 1 1 calc R . . H30C H 1.0949 0.0927 0.1011 0.062 Uiso 1 1 calc R . . C31 C 0.8407(4) -0.0188(3) 0.3171(3) 0.0338(11) Uani 1 1 d . . . H31A H 0.7585 -0.0195 0.3061 0.041 Uiso 1 1 calc R . . H31B H 0.9055 -0.0937 0.3027 0.041 Uiso 1 1 calc R . . C32 C 0.8336(4) -0.0131(4) 0.4118(3) 0.0410(12) Uani 1 1 d . . . H32A H 0.9179 -0.0249 0.4251 0.062 Uiso 1 1 calc R . . H32B H 0.8023 -0.0749 0.4454 0.062 Uiso 1 1 calc R . . H32C H 0.7762 0.0640 0.4256 0.062 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 0.0190(3) 0.0172(3) 0.0134(3) -0.0020(2) -0.0053(2) -0.0017(2) P1 0.0182(5) 0.0195(5) 0.0119(5) -0.0017(4) -0.0033(4) -0.0034(4) P2 0.0238(6) 0.0222(6) 0.0142(6) -0.0024(4) -0.0053(5) -0.0069(5) P3 0.0250(6) 0.0216(6) 0.0257(6) -0.0009(5) -0.0051(5) -0.0019(5) Si1 0.0324(7) 0.0381(7) 0.0222(7) -0.0061(6) -0.0015(6) -0.0199(6) Si2 0.0460(8) 0.0268(7) 0.0205(7) -0.0029(5) -0.0102(6) -0.0157(6) N1 0.0199(18) 0.0212(18) 0.025(2) -0.0093(15) -0.0029(15) -0.0040(14) N2 0.0188(18) 0.0269(19) 0.027(2) -0.0057(16) -0.0089(16) -0.0038(15) N3 0.0225(18) 0.0267(18) 0.0142(18) -0.0043(15) -0.0014(15) -0.0102(15) N4 0.0250(18) 0.0321(19) 0.0118(18) -0.0022(15) -0.0017(15) -0.0103(16) N5 0.0268(19) 0.0222(18) 0.0205(19) -0.0017(15) -0.0057(16) -0.0099(15) N6 0.035(2) 0.0213(18) 0.0162(19) -0.0013(15) -0.0073(16) -0.0093(15) C1 0.015(2) 0.023(2) 0.009(2) 0.0050(17) -0.0020(16) 0.0007(17) C2 0.029(2) 0.024(2) 0.014(2) -0.0002(18) -0.0051(18) -0.0099(19) C3 0.032(2) 0.023(2) 0.020(2) -0.0015(19) -0.002(2) -0.0039(19) C4 0.023(2) 0.025(2) 0.016(2) 0.0056(19) -0.0028(18) 0.0021(18) C5 0.022(2) 0.031(2) 0.011(2) 0.0011(18) -0.0021(18) -0.0098(19) C6 0.030(2) 0.021(2) 0.005(2) 0.0002(17) 0.0035(17) -0.0071(18) C7 0.078(4) 0.038(3) 0.049(3) -0.013(3) 0.003(3) -0.031(3) C8 0.043(3) 0.107(4) 0.023(3) -0.009(3) -0.003(2) -0.047(3) C9 0.061(3) 0.061(3) 0.030(3) -0.005(2) -0.013(3) -0.037(3) C10 0.072(4) 0.031(3) 0.035(3) -0.006(2) -0.011(3) -0.017(3) C11 0.023(2) 0.025(2) 0.010(2) -0.0001(17) -0.0026(17) -0.0069(18) C12 0.031(2) 0.040(3) 0.016(2) -0.007(2) 0.0012(19) -0.013(2) C13 0.039(3) 0.040(3) 0.014(2) -0.003(2) 0.002(2) -0.021(2) C14 0.036(3) 0.036(3) 0.027(3) 0.002(2) -0.004(2) -0.006(2) C15 0.039(3) 0.034(3) 0.020(2) 0.000(2) 0.004(2) -0.012(2) C16 0.092(5) 0.114(5) 0.021(3) 0.018(3) -0.022(3) -0.070(4) C17 0.159(7) 0.051(4) 0.062(5) -0.003(3) 0.078(5) -0.003(4) C18 0.047(3) 0.072(4) 0.037(3) 0.018(3) -0.008(3) -0.033(3) C19 0.033(2) 0.034(2) 0.023(2) -0.001(2) -0.002(2) -0.016(2) C20 0.030(3) 0.044(3) 0.040(3) 0.001(2) -0.003(2) -0.013(2) C21 0.039(3) 0.041(3) 0.031(3) 0.004(2) -0.001(2) -0.018(2) C22 0.042(3) 0.049(3) 0.018(2) -0.003(2) -0.004(2) -0.021(2) C23 0.038(2) 0.024(2) 0.010(2) -0.0024(17) -0.0063(19) -0.0082(19) C24 0.047(3) 0.036(3) 0.016(2) 0.004(2) -0.004(2) -0.015(2) C25 0.063(3) 0.033(3) 0.025(3) -0.008(2) -0.004(2) -0.008(2) C26 0.046(3) 0.041(3) 0.025(3) 0.005(2) -0.015(2) -0.009(2) C27 0.025(2) 0.020(2) 0.039(3) -0.005(2) -0.008(2) 0.0001(18) C28 0.028(3) 0.034(3) 0.051(3) -0.001(2) -0.008(2) -0.007(2) C29 0.035(3) 0.031(2) 0.040(3) -0.015(2) -0.008(2) 0.000(2) C30 0.039(3) 0.041(3) 0.032(3) -0.009(2) -0.001(2) 0.000(2) C31 0.034(3) 0.022(2) 0.040(3) 0.000(2) -0.003(2) -0.005(2) C32 0.043(3) 0.036(3) 0.038(3) 0.010(2) -0.011(2) -0.011(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 N1 1.856(3) . ? Ni1 P3 2.1383(11) . ? Ni1 P1 2.1603(11) . ? Ni1 P2 2.1756(11) . ? P1 N1 1.592(3) . ? P1 N3 1.683(3) . ? P1 N4 1.685(3) . ? P1 Si1 2.5285(15) . ? P2 N2 1.605(3) . ? P2 N6 1.706(3) . ? P2 N5 1.722(3) . ? P2 Si2 2.5366(15) . ? P3 C29 1.829(4) . ? P3 C27 1.831(4) . ? P3 C31 1.831(4) . ? Si1 N4 1.723(3) . ? Si1 N3 1.737(3) . ? Si1 C8 1.851(4) . ? Si1 C7 1.858(5) . ? Si2 N6 1.723(3) . ? Si2 N5 1.732(3) . ? Si2 C9 1.865(4) . ? Si2 C10 1.869(4) . ? N1 C1 1.398(4) . ? N2 C6 1.360(5) . ? N3 C11 1.471(5) . ? N4 C15 1.470(5) . ? N5 C19 1.467(5) . ? N6 C23 1.488(5) . ? C1 C2 1.362(5) . ? C1 C6 1.432(5) . ? C2 C3 1.376(5) . ? C3 C4 1.386(5) . ? C4 C5 1.367(5) . ? C5 C6 1.409(5) . ? C11 C12 1.517(5) . ? C11 C13 1.526(5) . ? C11 C14 1.538(5) . ? C15 C18 1.512(6) . ? C15 C16 1.521(6) . ? C15 C17 1.523(7) . ? C19 C22 1.512(5) . ? C19 C21 1.516(5) . ? C19 C20 1.546(6) . ? C23 C26 1.519(5) . ? C23 C24 1.520(5) . ? C23 C25 1.527(5) . ? C27 C28 1.523(5) . ? C29 C30 1.533(6) . ? C31 C32 1.530(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 P3 162.91(10) . . ? N1 Ni1 P1 45.93(9) . . ? P3 Ni1 P1 117.01(4) . . ? N1 Ni1 P2 92.57(10) . . ? P3 Ni1 P2 104.48(4) . . ? P1 Ni1 P2 138.50(4) . . ? N1 P1 N3 119.43(17) . . ? N1 P1 N4 118.18(16) . . ? N3 P1 N4 85.81(15) . . ? N1 P1 Ni1 56.91(11) . . ? N3 P1 Ni1 136.15(12) . . ? N4 P1 Ni1 136.84(12) . . ? N1 P1 Si1 132.50(12) . . ? N3 P1 Si1 43.16(11) . . ? N4 P1 Si1 42.68(11) . . ? Ni1 P1 Si1 170.60(5) . . ? N2 P2 N6 110.38(16) . . ? N2 P2 N5 108.95(16) . . ? N6 P2 N5 85.08(15) . . ? N2 P2 Ni1 112.53(12) . . ? N6 P2 Ni1 117.65(12) . . ? N5 P2 Ni1 119.28(11) . . ? N2 P2 Si2 112.62(12) . . ? N6 P2 Si2 42.56(11) . . ? N5 P2 Si2 42.91(11) . . ? Ni1 P2 Si2 134.85(5) . . ? C29 P3 C27 103.5(2) . . ? C29 P3 C31 102.4(2) . . ? C27 P3 C31 102.9(2) . . ? C29 P3 Ni1 117.85(15) . . ? C27 P3 Ni1 112.55(13) . . ? C31 P3 Ni1 115.74(14) . . ? N4 Si1 N3 83.03(15) . . ? N4 Si1 C8 115.12(19) . . ? N3 Si1 C8 114.8(2) . . ? N4 Si1 C7 116.6(2) . . ? N3 Si1 C7 115.7(2) . . ? C8 Si1 C7 109.7(2) . . ? N4 Si1 P1 41.54(11) . . ? N3 Si1 P1 41.52(10) . . ? C8 Si1 P1 122.96(18) . . ? C7 Si1 P1 127.32(17) . . ? N6 Si2 N5 84.23(15) . . ? N6 Si2 C9 116.82(19) . . ? N5 Si2 C9 117.0(2) . . ? N6 Si2 C10 115.4(2) . . ? N5 Si2 C10 115.05(19) . . ? C9 Si2 C10 107.3(2) . . ? N6 Si2 P2 42.03(11) . . ? N5 Si2 P2 42.59(10) . . ? C9 Si2 P2 123.15(16) . . ? C10 Si2 P2 129.57(16) . . ? C1 N1 P1 143.7(3) . . ? C1 N1 Ni1 139.1(3) . . ? P1 N1 Ni1 77.16(13) . . ? C6 N2 P2 131.3(3) . . ? C11 N3 P1 130.6(2) . . ? C11 N3 Si1 133.4(2) . . ? P1 N3 Si1 95.31(16) . . ? C15 N4 P1 127.8(3) . . ? C15 N4 Si1 135.9(3) . . ? P1 N4 Si1 95.78(16) . . ? C19 N5 P2 125.8(3) . . ? C19 N5 Si2 133.0(3) . . ? P2 N5 Si2 94.50(17) . . ? C23 N6 P2 126.2(2) . . ? C23 N6 Si2 132.9(3) . . ? P2 N6 Si2 95.41(17) . . ? C2 C1 N1 121.0(3) . . ? C2 C1 C6 120.7(3) . . ? N1 C1 C6 118.3(3) . . ? C1 C2 C3 122.1(4) . . ? C2 C3 C4 118.8(4) . . ? C5 C4 C3 120.2(4) . . ? C4 C5 C6 122.8(4) . . ? N2 C6 C5 118.5(3) . . ? N2 C6 C1 126.1(3) . . ? C5 C6 C1 115.4(3) . . ? N3 C11 C12 107.2(3) . . ? N3 C11 C13 109.5(3) . . ? C12 C11 C13 109.6(3) . . ? N3 C11 C14 110.7(3) . . ? C12 C11 C14 109.6(3) . . ? C13 C11 C14 110.2(3) . . ? N4 C15 C18 109.2(4) . . ? N4 C15 C16 109.9(4) . . ? C18 C15 C16 109.0(4) . . ? N4 C15 C17 108.0(4) . . ? C18 C15 C17 107.6(4) . . ? C16 C15 C17 113.0(5) . . ? N5 C19 C22 110.8(3) . . ? N5 C19 C21 108.7(3) . . ? C22 C19 C21 110.9(3) . . ? N5 C19 C20 110.5(3) . . ? C22 C19 C20 107.2(4) . . ? C21 C19 C20 108.6(3) . . ? N6 C23 C26 111.4(3) . . ? N6 C23 C24 110.2(3) . . ? C26 C23 C24 108.8(3) . . ? N6 C23 C25 107.7(3) . . ? C26 C23 C25 109.4(3) . . ? C24 C23 C25 109.3(4) . . ? C28 C27 P3 116.3(3) . . ? C30 C29 P3 113.6(3) . . ? C32 C31 P3 114.1(3) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.987 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.094