Dihydrogen Binding to Isostructural S=1/2 and S= 0 Cobalt Complexes
Daniel L. M. Suess; Charlene Tsay; Jonas C. Peters; Journal of the American Chemical Society 134 (2012) 14158–14164; doi:10.1021/ja305248f

data_4118552
_publ_section_title
;
 Dihydrogen Binding to Isostructural S=1/2 and S= 0 Cobalt Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14158
_journal_page_last               14164
_journal_paper_doi               10.1021/ja305248f
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C36 H54 B Br Co P3'
_chemical_formula_sum            'C36 H54 B Br Co P3'
_chemical_formula_weight         729.35
_chemical_name_common            (TPB)CoBr
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.488(3)
_cell_angle_beta                 97.701(3)
_cell_angle_gamma                117.196(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8175(6)
_cell_length_b                   11.5615(7)
_cell_length_c                   15.9277(9)
_cell_measurement_reflns_used    9002
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      42.42
_cell_measurement_theta_min      2.58
_cell_volume                     1747.20(18)
_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_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      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            147389
_diffrn_reflns_theta_full        44.17
_diffrn_reflns_theta_max         44.17
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_T_max  0.6523
_exptl_absorpt_correction_T_min  0.5562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1 (Bruker-AXS, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         27532
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0354P)^2^+0.3754P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                20889
_reflns_number_total             27532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja305248f_si_002_4.cif
_cod_data_source_block           dlms69
_cod_original_cell_volume        1747.20(17)
_cod_database_code               4118552