Reversible H2 Addition across a Nickel-Borane Unit as a Promising Strategy for Catalysis
W. Hill Harman; Jonas C. Peters; Journal of the American Chemical Society 134 (2012) 5080–5082; doi:10.1021/ja211419t

data_4117705
_publ_contact_author_email       jpeters@caltech.edu
_publ_contact_author_name        'Jonas Peters'
_publ_section_title
;
 Reversible H2 Addition across a Nickel-Borane Unit as a Promising
 Strategy for Catalysis
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5080
_journal_page_last               5082
_journal_paper_doi               10.1021/ja211419t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C46 H41 B Ni O P2'
_chemical_formula_sum            'C46 H41 B Ni O P2'
_chemical_formula_weight         741.25
_chemical_name_common            PhDPBPhNiTHF
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 129.973(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.7152(11)
_cell_length_b                   11.0648(5)
_cell_length_c                   18.3257(8)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.9
_cell_measurement_theta_min      2.2
_cell_volume                     3685.2(3)
_computing_cell_refinement       'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2010.7-0 (Bruker-AXS, 2010)'
_computing_data_reduction        'SAINT-Plus v7.66A (Bruker-AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45429
_diffrn_reflns_theta_full        32.57
_diffrn_reflns_theta_max         32.61
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  0.9377
_exptl_absorpt_correction_T_min  0.8646
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.186
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         13192
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                11245
_reflns_number_total             13192
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja211419t_si_001_2.cif
_cod_data_source_block           PhDPBPhNiTHF
_cod_original_cell_volume        3685.3(2)
_cod_database_code               4117705