A Ni0(η2-(Si–H))(η2-H2) Complex That Mediates Facile H Atom Exchange between Two σ-Ligands
Connor, Bridget A.; Rittle, Jonathan; VanderVelde, David; Peters, Jonas C.; Organometallics 35 (2016) 686–; doi:10.1021/acs.organomet.5b00985

data_4088281
_publ_section_title
;
 A Ni0(\h2-(Si--H))(\h2-H2) Complex That Mediates Facile H Atom Exchange
 between Two \s-Ligands
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              686
_journal_paper_doi               10.1021/acs.organomet.5b00985
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C48 H72 Ni2 O P4 Si2'
_chemical_formula_weight         962.53
_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
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 109.523(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4925(11)
_cell_length_b                   11.0111(5)
_cell_length_c                   19.1787(9)
_cell_measurement_reflns_used    9145
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.30
_cell_measurement_theta_min      2.50
_cell_volume                     4675.9(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker KAPPA APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            183284
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.066
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.6566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         14271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+2.3848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12637
_reflns_number_total             14271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00985_si_002.cif
_cod_data_source_block           a14225
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088281
_shelxl_version_number           2013-3
_shelx_res_checksum              87322
_shelx_hkl_checksum              46664