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_4119292
_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            'C61 H94 Ni2 O2 P2'
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_chemical_name_systematic
; 
 ? 
;
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_cell_angle_alpha                88.462(11)
_cell_angle_beta                 85.951(11)
_cell_angle_gamma                86.210(11)
_cell_formula_units_Z            1
_cell_length_a                   9.438(3)
_cell_length_b                   10.735(3)
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_cell_measurement_temperature    100(2)
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_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    Sir2011
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_diffrn_detector_type            '4K CCD area detector APEX II'
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_diffrn_measured_fraction_theta_max 0.906
_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'
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_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -16
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_diffrn_reflns_theta_max         26.57
_diffrn_reflns_theta_min         1.90
_diffrn_source                   'Micorfocus source E025 IuS'
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_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    0.788
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_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            yellow
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_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.405
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5174
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_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1502
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_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_total             5174
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           mo_jc224_0m
_cod_original_cell_volume        1368.7(8)
_cod_database_code               4119292