Nickel-Catalyzed Hydrosilylation of CO2in the Presence of Et3B for the Synthesis of Formic Acid and Related Formates
González-Sebastián, Lucero; Flores-Alamo, Marcos; Garc\?ía, Juventino J.; Organometallics 32 (2013) 7186–; doi:10.1021/om400876j

data_4081994
_publ_section_title
;
 Nickel-Catalyzed Hydrosilylation of CO2in the Presence of Et3B for the
 Synthesis of Formic Acid and Related Formates
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              7186
_journal_paper_doi               10.1021/om400876j
_journal_volume                  32
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C16 H32 Ni O2 P2'
_chemical_formula_sum            'C16 H32 Ni O2 P2'
_chemical_formula_weight         377.07
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-05-29T15:27:23-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 100.957(12)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   32.567(5)
_cell_length_b                   11.0531(8)
_cell_length_c                   16.7505(13)
_cell_measurement_reflns_used    2337
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      25.9982
_cell_measurement_theta_min      3.6691
_cell_measurement_wavelength     0.71073
_cell_volume                     5919.7(11)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0025762
_diffrn_orient_matrix_UB_12      0.0616107
_diffrn_orient_matrix_UB_13      0.011621
_diffrn_orient_matrix_UB_21      -0.0220147
_diffrn_orient_matrix_UB_22      0.0074057
_diffrn_orient_matrix_UB_23      -0.0078855
_diffrn_orient_matrix_UB_31      -0.0004862
_diffrn_orient_matrix_UB_32      -0.0162017
_diffrn_orient_matrix_UB_33      0.0407859
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12682
_diffrn_reflns_theta_full        26.11
_diffrn_reflns_theta_max         26.11
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'trigonal prism'
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.5524
_exptl_crystal_size_mid          0.2151
_exptl_crystal_size_min          0.1237
_refine_diff_density_max         1.632
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         5855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+15.4469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1144
_reflns_number_gt                4160
_reflns_number_total             5855
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400876j_si_002.cif
_cod_data_source_block           lu184b
_cod_original_cell_volume        5919.8(11)
_cod_database_code               4081994