Combined Experimental and Theoretical Study on the Reductive Cleavage of Inert C-O Bonds with Silanes: Ruling out a Classical Ni(0)/Ni(II) Catalytic Couple and Evidence for Ni(I) Intermediates
Josep Cornella; Enrique Gómez-Bengoa; Ruben Martin; Journal of the American Chemical Society 135 (2013) 1997–2009; doi:10.1021/ja311940s

data_4119293
_publ_section_title
;
 Combined Experimental and Theoretical Study on the Reductive Cleavage of
 Inert C-O Bonds with Silanes: Ruling out a Classical Ni(0)/Ni(II)
 Catalytic Couple and Evidence for Ni(I) Intermediates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1997
_journal_page_last               2009
_journal_paper_doi               10.1021/ja311940s
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C38 H70 Ni O P2'
_chemical_formula_weight         663.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.116(17)
_cell_angle_beta                 86.40(2)
_cell_angle_gamma                60.580(12)
_cell_formula_units_Z            2
_cell_length_a                   9.655(4)
_cell_length_b                   9.761(4)
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_cell_measurement_reflns_used    75
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.17
_cell_measurement_theta_min      2.55
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_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
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_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support whith MicroMount'
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
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_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         0.92
_diffrn_source                   'Micorfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    0.650
_exptl_absorpt_correction_T_max  0.9935
_exptl_absorpt_correction_T_min  0.9498
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 TWINABS Version 2008/0 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       plate
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_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+3.9197P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1582
_refine_ls_wR_factor_ref         0.1740
_reflns_number_gt                4843
_reflns_number_total             6657
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311940s_si_003.cif
_cod_data_source_block           mo_jc241b_05
_cod_original_cell_volume        1815.0(14)
_cod_database_code               4119293