Elucidation of a Low Spin Cobalt(II) System in a Distorted Tetrahedral Geometry
David M. Jenkins; Angel J. Di Bilio; Matthew J. Allen; Theodore A. Betley; Jonas C. Peters; Journal of the American Chemical Society 124 (2002) 15336–15350; doi:10.1021/ja026433e

data_4115403
_publ_section_title
;
 Elucidation of a Low Spin Cobalt(II) System in a Distorted Tetrahedral
 Geometry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15336
_journal_page_last               15350
_journal_paper_doi               10.1021/ja026433e
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'C53 H50 B Co O P3'
_chemical_formula_weight         865.58
_space_group_IT_number           9
_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                 109.1810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2447(14)
_cell_length_b                   16.4840(13)
_cell_length_c                   16.4939(13)
_cell_measurement_temperature    96(2)
_cell_volume                     4428.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      96(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45708
_diffrn_reflns_theta_full        28.61
_diffrn_reflns_theta_max         28.61
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.661
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         10456
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.660
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0612
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                9359
_reflns_number_total             10456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja026433e-2_s2_5.cif
_cod_data_source_block           dmj11
_cod_database_code               4115403