data_margraf7, 2SiNi _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H70 N2 Ni O4 Si2' _chemical_formula_weight 781.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.822(5) _cell_length_b 13.0594(16) _cell_length_c 7.8033(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.953(7) _cell_angle_gamma 90.00 _cell_volume 4363.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 146(2) _cell_measurement_reflns_used 210 _cell_measurement_theta_min 3 _cell_measurement_theta_max 26 _exptl_crystal_description rod _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type 'numerical, SHELXTL (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.8605 _exptl_absorpt_correction_T_max 0.9843 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 146(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 SIEMENS_SMART_CCD _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 339 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1200 _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 18461 _diffrn_reflns_av_R_equivalents 0.1274 _diffrn_reflns_av_sigmaI/netI 0.0895 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.17 _reflns_number_total 4801 _reflns_number_gt 3556 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.03P)^2^+10.0P] 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 4801 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.1515 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.290 _refine_ls_restrained_S_all 1.290 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.0000 0.05464(4) 0.2500 0.01535(17) Uani 1 2 d S . . Si Si 0.17282(2) 0.21613(8) 0.66445(14) 0.0246(3) Uani 1 1 d . . . O1 O 0.02781(5) 0.15875(16) 0.3010(3) 0.0190(5) Uani 1 1 d . . . N N 0.02625(6) -0.0475(2) 0.3271(4) 0.0174(6) Uani 1 1 d . . . C8 C 0.05661(7) 0.1522(2) 0.3649(4) 0.0179(7) Uani 1 1 d . . . O2 O 0.14776(5) 0.13693(19) 0.5709(4) 0.0313(7) Uani 1 1 d . . . C3 C 0.06975(7) 0.0587(3) 0.4197(5) 0.0191(7) Uani 1 1 d . . . C4 C 0.10022(8) 0.0559(3) 0.4939(5) 0.0240(8) Uani 1 1 d . . . H4 H 0.1086 -0.0071 0.5346 0.029 Uiso 1 1 calc R . . C2 C 0.05347(7) -0.0365(2) 0.4005(5) 0.0199(7) Uani 1 1 d . . . H2 H 0.0634 -0.0962 0.4449 0.024 Uiso 1 1 calc R . . C5 C 0.11748(8) 0.1429(3) 0.5070(5) 0.0233(8) Uani 1 1 d . . . C7 C 0.07491(7) 0.2436(2) 0.3785(5) 0.0189(7) Uani 1 1 d . . . C9 C 0.06211(8) 0.3469(3) 0.3163(5) 0.0227(8) Uani 1 1 d . . . C6 C 0.10482(8) 0.2357(3) 0.4477(5) 0.0227(8) Uani 1 1 d . . . H6 H 0.1173 0.2957 0.4554 0.027 Uiso 1 1 calc R . . C1 C 0.01197(8) -0.1508(2) 0.3220(5) 0.0207(8) Uani 1 1 d . . . H1A H 0.0019 -0.1662 0.4323 0.025 Uiso 1 1 calc R . . H1B H 0.0281 -0.2034 0.3013 0.025 Uiso 1 1 calc R . . C10 C 0.08611(9) 0.4336(3) 0.3380(5) 0.0292(9) Uani 1 1 d . . . H10A H 0.1049 0.4172 0.2732 0.044 Uiso 1 1 calc R . . H10B H 0.0917 0.4412 0.4597 0.044 Uiso 1 1 calc R . . H10C H 0.0771 0.4978 0.2951 0.044 Uiso 1 1 calc R . . C15 C 0.19748(10) 0.0178(3) 0.7524(6) 0.0367(10) Uani 1 1 d . . . H15A H 0.2163 -0.0225 0.7783 0.055 Uiso 1 1 calc R . . H15B H 0.1868 -0.0106 0.6510 0.055 Uiso 1 1 calc R . . H15C H 0.1835 0.0155 0.8503 0.055 Uiso 1 1 calc R . . C13 C 0.20674(8) 0.1292(3) 0.7172(5) 0.0298(9) Uani 1 1 d . . . H13 H 0.2202 0.1281 0.6138 0.036 Uiso 1 1 calc R . . C14 C 0.22745(10) 0.1681(4) 0.8675(6) 0.0458(12) Uani 1 1 d . . . H14A H 0.2446 0.1196 0.8885 0.069 Uiso 1 1 calc R . . H14B H 0.2149 0.1740 0.9708 0.069 Uiso 1 1 calc R . . H14C H 0.2361 0.2353 0.8386 0.069 Uiso 1 1 calc R . . C20 C 0.21205(10) 0.3850(4) 0.5790(7) 0.0487(12) Uani 1 1 d . . . H20A H 0.2171 0.4381 0.4951 0.073 Uiso 1 1 calc R . . H20B H 0.2303 0.3411 0.5982 0.073 Uiso 1 1 calc R . . H20C H 0.2062 0.4172 0.6872 0.073 Uiso 1 1 calc R . . C11 C 0.03316(8) 0.3760(3) 0.4214(6) 0.0285(9) Uani 1 1 d . . . H11A H 0.0390 0.3803 0.5431 0.043 Uiso 1 1 calc R . . H11B H 0.0170 0.3238 0.4053 0.043 Uiso 1 1 calc R . . H11C H 0.0251 0.4425 0.3824 0.043 Uiso 1 1 calc R . . C19 C 0.18472(9) 0.3201(3) 0.5107(6) 0.0333(9) Uani 1 1 d . . . H19 H 0.1664 0.3671 0.4968 0.040 Uiso 1 1 calc R . . C12 C 0.05357(9) 0.3404(3) 0.1238(5) 0.0272(8) Uani 1 1 d . . . H12A H 0.0722 0.3227 0.0590 0.041 Uiso 1 1 calc R . . H12B H 0.0455 0.4068 0.0844 0.041 Uiso 1 1 calc R . . H12C H 0.0376 0.2877 0.1057 0.041 Uiso 1 1 calc R . . C18 C 0.13856(14) 0.3721(4) 0.8397(8) 0.0649(16) Uani 1 1 d . . . H18A H 0.1309 0.3962 0.9504 0.097 Uiso 1 1 calc R . . H18B H 0.1208 0.3609 0.7611 0.097 Uiso 1 1 calc R . . H18C H 0.1525 0.4237 0.7913 0.097 Uiso 1 1 calc R . . C21 C 0.19198(12) 0.2781(4) 0.3319(6) 0.0550(13) Uani 1 1 d . . . H21A H 0.1979 0.3347 0.2566 0.083 Uiso 1 1 calc R . . H21B H 0.1734 0.2437 0.2843 0.083 Uiso 1 1 calc R . . H21C H 0.2093 0.2291 0.3408 0.083 Uiso 1 1 calc R . . C17 C 0.13707(10) 0.1960(3) 0.9620(6) 0.0402(11) Uani 1 1 d . . . H17A H 0.1287 0.2279 1.0653 0.060 Uiso 1 1 calc R . . H17B H 0.1504 0.1380 0.9948 0.060 Uiso 1 1 calc R . . H17C H 0.1198 0.1716 0.8892 0.060 Uiso 1 1 calc R . . C16 C 0.15601(10) 0.2736(3) 0.8647(6) 0.0385(10) Uani 1 1 d . . . H16 H 0.1743 0.2905 0.9407 0.046 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 0.0136(3) 0.0109(3) 0.0214(4) 0.000 -0.0025(2) 0.000 Si 0.0173(5) 0.0292(5) 0.0271(6) -0.0046(4) -0.0002(4) -0.0051(4) O1 0.0151(11) 0.0128(11) 0.0290(14) -0.0003(10) -0.0043(10) -0.0007(9) N 0.0165(14) 0.0140(13) 0.0216(16) 0.0001(12) -0.0010(11) 0.0000(11) C8 0.0150(16) 0.0177(16) 0.0209(18) -0.0017(14) -0.0021(13) -0.0010(13) O2 0.0178(13) 0.0258(13) 0.0500(19) -0.0083(13) -0.0137(12) -0.0001(10) C3 0.0148(15) 0.0177(15) 0.0247(19) -0.0009(15) -0.0013(13) -0.0023(13) C4 0.0190(17) 0.0200(16) 0.033(2) -0.0025(16) -0.0062(15) 0.0044(15) C2 0.0169(16) 0.0171(17) 0.026(2) 0.0015(14) -0.0013(14) 0.0019(13) C5 0.0154(17) 0.0243(18) 0.030(2) -0.0050(16) -0.0071(15) -0.0005(14) C7 0.0161(16) 0.0192(16) 0.0213(18) -0.0054(14) 0.0011(13) -0.0012(13) C9 0.0214(18) 0.0170(16) 0.030(2) -0.0009(15) -0.0010(15) -0.0025(14) C6 0.0198(17) 0.0185(17) 0.030(2) -0.0043(15) -0.0014(15) -0.0044(14) C1 0.0226(18) 0.0100(15) 0.029(2) 0.0014(14) -0.0019(15) -0.0015(13) C10 0.0285(19) 0.0187(18) 0.040(2) -0.0019(16) -0.0047(17) -0.0043(15) C15 0.036(2) 0.040(2) 0.034(2) -0.0012(19) -0.0114(19) 0.0068(19) C13 0.0188(18) 0.048(2) 0.023(2) -0.0021(18) -0.0033(15) -0.0030(17) C14 0.035(2) 0.058(3) 0.044(3) -0.001(2) -0.014(2) -0.006(2) C20 0.032(2) 0.051(3) 0.062(3) 0.010(2) -0.003(2) -0.015(2) C11 0.0257(19) 0.0176(17) 0.042(2) -0.0033(17) 0.0028(17) 0.0021(15) C19 0.026(2) 0.036(2) 0.037(2) 0.0010(19) -0.0014(17) -0.0069(17) C12 0.0278(19) 0.0236(18) 0.030(2) 0.0057(16) -0.0056(16) -0.0047(15) C18 0.085(4) 0.046(3) 0.064(4) 0.005(3) 0.029(3) 0.024(3) C21 0.065(3) 0.068(3) 0.032(3) 0.003(2) 0.010(2) -0.010(3) C17 0.033(2) 0.044(2) 0.044(3) 0.001(2) 0.010(2) 0.0037(19) C16 0.039(2) 0.035(2) 0.042(3) -0.009(2) 0.011(2) -0.0051(19) _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 N 1.839(3) 2 ? Ni N 1.839(3) . ? Ni O1 1.846(2) . ? Ni O1 1.846(2) 2 ? Si O2 1.652(2) . ? Si C13 1.883(4) . ? Si C16 1.887(4) . ? Si C19 1.888(4) . ? O1 C8 1.325(4) . ? N C2 1.298(4) . ? N C1 1.482(4) . ? C8 C3 1.407(5) . ? C8 C7 1.431(4) . ? O2 C5 1.384(4) . ? C3 C4 1.419(4) . ? C3 C2 1.432(4) . ? C4 C5 1.359(5) . ? C5 C6 1.402(5) . ? C7 C6 1.386(5) . ? C7 C9 1.533(5) . ? C9 C10 1.537(4) . ? C9 C12 1.543(5) . ? C9 C11 1.545(5) . ? C1 C1 1.509(6) 2 ? C15 C13 1.534(6) . ? C13 C14 1.544(5) . ? C20 C19 1.533(5) . ? C19 C21 1.535(6) . ? C18 C16 1.499(6) . ? C17 C16 1.511(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 N Ni N 87.02(16) 2 . ? N Ni O1 173.26(12) 2 . ? N Ni O1 94.30(10) . . ? N Ni O1 94.30(10) 2 2 ? N Ni O1 173.26(12) . 2 ? O1 Ni O1 85.16(13) . 2 ? O2 Si C13 102.25(15) . . ? O2 Si C16 111.17(17) . . ? C13 Si C16 111.2(2) . . ? O2 Si C19 110.46(16) . . ? C13 Si C19 110.92(18) . . ? C16 Si C19 110.55(19) . . ? C8 O1 Ni 128.8(2) . . ? C2 N C1 118.7(3) . . ? C2 N Ni 127.1(2) . . ? C1 N Ni 113.70(19) . . ? O1 C8 C3 122.4(3) . . ? O1 C8 C7 118.6(3) . . ? C3 C8 C7 119.0(3) . . ? C5 O2 Si 136.2(2) . . ? C8 C3 C4 120.4(3) . . ? C8 C3 C2 122.0(3) . . ? C4 C3 C2 117.6(3) . . ? C5 C4 C3 120.3(3) . . ? N C2 C3 125.0(3) . . ? C4 C5 O2 119.0(3) . . ? C4 C5 C6 119.4(3) . . ? O2 C5 C6 121.5(3) . . ? C6 C7 C8 117.9(3) . . ? C6 C7 C9 120.8(3) . . ? C8 C7 C9 121.3(3) . . ? C7 C9 C10 112.3(3) . . ? C7 C9 C12 109.7(3) . . ? C10 C9 C12 107.2(3) . . ? C7 C9 C11 109.5(3) . . ? C10 C9 C11 107.5(3) . . ? C12 C9 C11 110.5(3) . . ? C7 C6 C5 122.9(3) . . ? N C1 C1 107.2(2) . 2 ? C15 C13 C14 108.8(3) . . ? C15 C13 Si 114.2(3) . . ? C14 C13 Si 113.5(3) . . ? C20 C19 C21 110.4(4) . . ? C20 C19 Si 112.9(3) . . ? C21 C19 Si 112.4(3) . . ? C18 C16 C17 111.7(4) . . ? C18 C16 Si 115.5(4) . . ? C17 C16 Si 111.4(3) . . ? 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 N Ni O1 C8 -98.9(9) 2 . . . ? N Ni O1 C8 2.2(3) . . . . ? O1 Ni O1 C8 175.5(3) 2 . . . ? N Ni N C2 177.5(4) 2 . . . ? O1 Ni N C2 4.1(3) . . . . ? O1 Ni N C2 -81.1(10) 2 . . . ? N Ni N C1 -10.83(18) 2 . . . ? O1 Ni N C1 175.8(2) . . . . ? O1 Ni N C1 90.6(9) 2 . . . ? Ni O1 C8 C3 -6.0(5) . . . . ? Ni O1 C8 C7 174.1(2) . . . . ? C13 Si O2 C5 175.6(4) . . . . ? C16 Si O2 C5 56.9(4) . . . . ? C19 Si O2 C5 -66.3(4) . . . . ? O1 C8 C3 C4 -177.4(3) . . . . ? C7 C8 C3 C4 2.6(5) . . . . ? O1 C8 C3 C2 3.8(6) . . . . ? C7 C8 C3 C2 -176.3(3) . . . . ? C8 C3 C4 C5 -2.5(6) . . . . ? C2 C3 C4 C5 176.5(4) . . . . ? C1 N C2 C3 -178.1(3) . . . . ? Ni N C2 C3 -6.8(5) . . . . ? C8 C3 C2 N 2.7(6) . . . . ? C4 C3 C2 N -176.2(4) . . . . ? C3 C4 C5 O2 -176.4(3) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? Si O2 C5 C4 -156.6(3) . . . . ? Si O2 C5 C6 26.6(6) . . . . ? O1 C8 C7 C6 179.1(3) . . . . ? C3 C8 C7 C6 -0.8(5) . . . . ? O1 C8 C7 C9 -1.7(5) . . . . ? C3 C8 C7 C9 178.3(3) . . . . ? C6 C7 C9 C10 1.0(5) . . . . ? C8 C7 C9 C10 -178.1(3) . . . . ? C6 C7 C9 C12 120.1(4) . . . . ? C8 C7 C9 C12 -59.0(4) . . . . ? C6 C7 C9 C11 -118.4(4) . . . . ? C8 C7 C9 C11 62.5(4) . . . . ? C8 C7 C6 C5 -1.1(6) . . . . ? C9 C7 C6 C5 179.7(3) . . . . ? C4 C5 C6 C7 1.3(6) . . . . ? O2 C5 C6 C7 178.1(3) . . . . ? C2 N C1 C1 -158.7(4) . . . 2 ? Ni N C1 C1 28.8(4) . . . 2 ? O2 Si C13 C15 -30.3(3) . . . . ? C16 Si C13 C15 88.5(3) . . . . ? C19 Si C13 C15 -148.0(3) . . . . ? O2 Si C13 C14 -155.8(3) . . . . ? C16 Si C13 C14 -37.1(4) . . . . ? C19 Si C13 C14 86.4(3) . . . . ? O2 Si C19 C20 -170.1(3) . . . . ? C13 Si C19 C20 -57.4(4) . . . . ? C16 Si C19 C20 66.4(4) . . . . ? O2 Si C19 C21 -44.4(3) . . . . ? C13 Si C19 C21 68.2(3) . . . . ? C16 Si C19 C21 -167.9(3) . . . . ? O2 Si C16 C18 -90.4(4) . . . . ? C13 Si C16 C18 156.4(4) . . . . ? C19 Si C16 C18 32.7(4) . . . . ? O2 Si C16 C17 38.5(4) . . . . ? C13 Si C16 C17 -74.8(3) . . . . ? C19 Si C16 C17 161.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 28.17 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 0.879 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.095