Reactions of Phenylhydrosilanes with Pincer-Nickel Complexes: Evidence for New Si-O and Si-C Bond Formation Pathways.
Hao, Jingjun; Vabre, Boris; Zargarian, Davit; Journal of the American Chemical Society 137 (2015) 15287–15298; doi:10.1021/jacs.5b10066

data_4129737
_publ_section_title
;
 Reactions of Phenylhydrosilanes with Pincer-Nickel Complexes: Evidence
 for New Si-O and Si-C Bond Formation Pathways.
;
_journal_issue                   48
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15287
_journal_page_last               15298
_journal_paper_doi               10.1021/jacs.5b10066
_journal_volume                  137
_journal_year                    2015
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C30 H52 Ni O4 P2 Si2'
_chemical_formula_sum            'C30 H52 Ni O4 P2 Si2'
_chemical_formula_weight         653.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.634(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5124(6)
_cell_length_b                   12.2425(4)
_cell_length_c                   18.1131(6)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.26
_cell_measurement_theta_min      2.78
_cell_volume                     3529.9(2)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45537
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.924
_diffrn_reflns_theta_min         2.776
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.539
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.5651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       Block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         6703
_refine_ls_number_restraints     250
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+4.9585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5612
_reflns_number_total             6703
_cod_data_source_file            ja5b10066_si_001.cif
_cod_data_source_block           BER121
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129737
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.581
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4A(0.15) H4B(0.15) H4C(0.15) H5(0.068) H6A(0.109) H6B(0.109)
 H6C(0.109) H7A(0.153) H7B(0.153) H7C(0.153) H8(0.086) H9A(0.17) H9B(0.17)
 H9C(0.17) H1A(0.095) H1B(0.095) H2A(0.116) H3A(0.102) H3B(0.102) H10A(0.14)
 H10B(0.14) H10C(0.14) H11A(0.063) H12A(0.08) H12B(0.08) H12C(0.08) H13A(0.126)
 H13B(0.126) H13C(0.126) H14A(0.065) H15A(0.103) H15B(0.103) H15C(0.103)
 H1C(0.095) H1D(0.095) H2B(0.116) H3C(0.102) H3D(0.102) H10D(0.14) H10E(0.14)
 H10F(0.14) H11B(0.063) H12D(0.08) H12E(0.08) H12F(0.08) H13D(0.126)
 H13E(0.126) H13F(0.126) H14B(0.065) H15D(0.103) H15E(0.103) H15F(0.103)
 H16A(0.13) H16B(0.13) H16C(0.13) H17A(0.114) H17B(0.114) H17C(0.114)
 H18A(0.134) H18B(0.134) H18C(0.134) H19(0.078) H21(0.057) H22(0.066)
 H23(0.079) H24(0.091) H26(0.075) H27(0.096) H28(0.096) H29(0.082) H30(0.06)
 Fixed X: H4A(0.7317) H4B(0.7156) H4C(0.677) H5(0.8503) H6A(0.7498)
 H6B(0.7768) H6C(0.8466) H7A(1.0062) H7B(1.0493) H7C(0.9785) H8(0.9128)
 H9A(0.9175) H9B(1.0108) H9C(0.9769) H1A(0.7748) H1B(0.7093) H2A(0.729)
 H3A(0.8216) H3B(0.8879) H10A(0.5452) H10B(0.4634) H10C(0.5504) H11A(0.5168)
 H12A(0.5332) H12B(0.4665) H12C(0.5616) H13A(0.7772) H13B(0.7866) H13C(0.8082)
 H14A(0.6747) H15A(0.5621) H15B(0.6346) H15C(0.6221) H1C(0.7266) H1D(0.6577)
 H2B(0.6959) H3C(0.788) H3D(0.8427) H10D(0.5406) H10E(0.446) H10F(0.5137)
 H11B(0.489) H12D(0.5316) H12E(0.4603) H12F(0.5567) H13D(0.75) H13E(0.7595)
 H13F(0.7881) H14B(0.6581) H15D(0.5365) H15E(0.6071) H15F(0.5901) H16A(1.0243)
 H16B(1.0505) H16C(1.0088) H17A(0.8667) H17B(0.9073) H17C(0.8118) H18A(0.8559)
 H18B(0.9554) H18C(0.9171) H19(0.8445) H21(0.6097) H22(0.5902) H23(0.695)
 H24(0.8231) H26(0.7019) H27(0.6092) H28(0.5156) H29(0.5134) H30(0.6087)
 Fixed Y: H4A(0.6019) H4B(0.492) H4C(0.5054) H5(0.4819) H6A(0.3416)
 H6B(0.3143) H6C(0.3218) H7A(0.5377) H7B(0.4436) H7C(0.4131) H8(0.4073)
 H9A(0.5501) H9B(0.509) H9C(0.6201) H1A(0.8535) H1B(0.869) H2A(0.735)
 H3A(0.818) H3B(0.7831) H10A(0.5846) H10B(0.6512) H10C(0.7139) H11A(0.6818)
 H12A(0.508) H12B(0.4958) H12C(0.4574) H13A(0.7555) H13B(0.6615) H13C(0.6362)
 H14A(0.5648) H15A(0.6835) H15B(0.705) H15C(0.7877) H1C(0.8641) H1D(0.853)
 H2B(0.71) H3C(0.7917) H3D(0.8078) H10D(0.5425) H10E(0.5755) H10F(0.6684)
 H11B(0.6535) H12D(0.4911) H12E(0.4651) H12F(0.44) H13D(0.7818) H13E(0.7132)
 H13F(0.6609) H14B(0.5858) H15D(0.6939) H15E(0.7283) H15F(0.8029) H16A(0.2936)
 H16B(0.1711) H16C(0.2483) H17A(0.1035) H17B(0.0119) H17C(0.0486) H18A(0.0893)
 H18B(0.0753) H18C(0.1874) H19(0.4208) H21(0.3016) H22(0.3448) H23(0.4336)
 H24(0.4673) H26(0.1105) H27(-0.0279) H28(-0.0072) H29(0.1558) H30(0.2953)
 Fixed Z: H4A(0.7105) H4B(0.7498) H4C(0.6531) H5(0.7588) H6A(0.6283)
 H6B(0.7223) H6C(0.6871) H7A(0.753) H7B(0.7221) H7C(0.7528) H8(0.6128)
 H9A(0.5278) H9B(0.5829) H9C(0.605) H1A(0.479) H1B(0.5185) H2A(0.5708)
 H3A(0.649) H3B(0.6134) H10A(0.4768) H10B(0.4191) H10C(0.4669) H11A(0.322)
 H12A(0.2773) H12B(0.3161) H12C(0.3663) H13A(0.3447) H13B(0.2876) H13C(0.3809)
 H14A(0.2924) H15A(0.2222) H15B(0.192) H15C(0.2545) H1C(0.4964) H1D(0.5321)
 H2B(0.5829) H3C(0.6688) H3D(0.618) H10D(0.4791) H10E(0.4213) H10F(0.4663)
 H11B(0.3273) H12D(0.2866) H12E(0.3177) H12F(0.375) H13D(0.3621) H13E(0.2912)
 H13F(0.3797) H14B(0.2938) H15D(0.2273) H15E(0.1973) H15F(0.2614) H16A(0.5593)
 H16B(0.5904) H16C(0.6348) H17A(0.6124) H17B(0.5768) H17C(0.5263) H18A(0.3852)
 H18B(0.4332) H18C(0.3873) H19(0.3591) H21(0.273) H22(0.1416) H23(0.1194)
 H24(0.2269) H26(0.3666) H27(0.3583) H28(0.4178) H29(0.484) H30(0.4942)
;
_olex2_submission_special_instructions 'No special instructions were received'