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_4115402
_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_moiety         'C45 H41 B Co I O2 P3, 2(C6 H6)'
_chemical_formula_sum            'C57 H53 B Co I O2 P3'
_chemical_formula_weight         1059.54
_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                 106.262(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.916(3)
_cell_length_b                   18.582(4)
_cell_length_c                   21.674(5)
_cell_measurement_temperature    98(2)
_cell_volume                     4994(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      98(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0773
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54319
_diffrn_reflns_theta_full        23.32
_diffrn_reflns_theta_max         23.32
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Electric Blue'
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       Shard
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.755
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         7213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.755
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.001
_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          0.0602
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                5722
_reflns_number_total             7213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja026433e-2_s2_4.cif
_cod_data_source_block           dmj02
_cod_original_cell_volume        4993.7(18)
_cod_database_code               4115402