Synthesis and Hydride Transfer Reactions of Cobalt and Nickel Hydride Complexes to BX3 Compounds
Michael T. Mock; Robert G. Potter; Molly J. O'Hagan; Donald M. Camaioni; William G. Dougherty; W. Scott Kassel; Daniel L. DuBois; Inorganic Chemistry 50 (2011) 11914–11928; doi:10.1021/ic200857x

data_4326960
_publ_section_title
;
 Synthesis and Hydride Transfer Reactions of Cobalt and Nickel Hydride
 Complexes to BX3 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11914
_journal_page_last               11928
_journal_paper_doi               10.1021/ic200857x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C12 H34 B Co F4 P4'
_chemical_formula_weight         448.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.625(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2170(10)
_cell_length_b                   19.204(2)
_cell_length_c                   12.2850(14)
_cell_measurement_reflns_used    7286
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      32.02
_cell_measurement_theta_min      2.60
_cell_volume                     2155.3(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      135(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24450
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.26
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  0.8592
_exptl_absorpt_correction_T_min  0.8414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         8190
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0574P)^2^+0.1554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                5128
_reflns_number_total             8190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200857x_si_001_07.cif
_cod_data_source_block           pnl043_H2Co(dmpe)2_BF4
_cod_original_cell_volume        2155.2(4)
_cod_database_code               4326960