Spin Isomers and Ligand Isomerization in a Three-Coordinate Cobalt(I) Carbonyl Complex.
Al-Afyouni, Malik H; Suturina, Elizaveta; Pathak, Shubhrodeep; Atanasov, Mihail; Bill, Eckhard; DeRosha, Daniel E.; Brennessel, William W.; Neese, Frank; Holland, Patrick L.; Journal of the American Chemical Society 137 (2015) 10689–10699; doi:10.1021/jacs.5b06078

data_4129452
_publ_section_title
;
 Spin Isomers and Ligand Isomerization in a Three-Coordinate Cobalt(I)
 Carbonyl Complex.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10689
_journal_page_last               10699
_journal_paper_doi               10.1021/jacs.5b06078
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C36 H53 Co N2 O'
_chemical_formula_sum            'C36 H53 Co N2 O'
_chemical_formula_weight         588.73
_chemical_name_common            holma05
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.447(3)
_cell_length_b                   14.3930(19)
_cell_length_c                   10.9118(14)
_cell_measurement_reflns_used    3994
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      38.07
_cell_measurement_theta_min      2.44
_cell_volume                     3211.3(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            116867
_diffrn_reflns_theta_full        37.78
_diffrn_reflns_theta_max         37.78
_diffrn_reflns_theta_min         1.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.9354
_exptl_absorpt_correction_T_min  0.8058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            'dark red-orange'
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
'Flack H D (1983), 8235 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         17183
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                14299
_reflns_number_total             17183
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b06078_si_002.cif
_cod_data_source_block           LCo(CO)
_cod_original_cell_volume        3211.2(7)
_cod_database_code               4129452