Molecular and Electronic Structures of Homoleptic Six-Coordinate Cobalt(I) Complexes of 2,2':6',2″-Terpyridine, 2,2'-Bipyridine, and 1,10-Phenanthroline. An Experimental and Computational Study.
England, Jason; Bill, Eckhard; Weyhermüller, Thomas; Neese, Frank; Atanasov, Mihail; Wieghardt, Karl; Inorganic chemistry 54 (2015) 12002–12018; doi:10.1021/acs.inorgchem.5b02415

data_4346952
_publ_section_title
;
 Molecular and Electronic Structures of Homoleptic Six-Coordinate
 Cobalt(I) Complexes of 2,2':6',2&#x2033;-Terpyridine, 2,2'-Bipyridine,
 and 1,10-Phenanthroline. An Experimental and Computational Study.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12002
_journal_page_last               12018
_journal_paper_doi               10.1021/acs.inorgchem.5b02415
_journal_volume                  54
_journal_year                    2015
_chemical_compound_source        'acetonitrile, diethylether'
_chemical_formula_moiety         'C36 H24 Co N6, B F4, 3.5(C2 H3 N)'
_chemical_formula_sum            'C43 H34.5 B Co F4 N9.5'
_chemical_formula_weight         830.04
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_block_code                WGT-JE-096-01
_audit_creation_date             2014-02-26
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.2287(11)
_cell_length_b                   14.2287(11)
_cell_length_c                   34.0196(13)
_cell_measurement_reflns_used    28834
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.0947
_cell_measurement_theta_min      2.8633
_cell_volume                     5964.7(7)
_computing_cell_refinement       'REVALCCD V. 1.6, 2008'
_computing_data_collection       'DATCOL (Bruker AXS, 2006)'
_computing_data_reduction        'REVALCCD V. 1.6, 2008'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18.02
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios focusing multilayer optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            27336
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.091
_diffrn_reflns_theta_min         2.863
_diffrn_source                   '0.2 x 2mm^2^ focus rotating anode'
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.94317
_exptl_absorpt_correction_T_min  0.92935
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             2562
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0452P)^2^+8.8774P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4611
_reflns_number_total             5031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02415_si_002.cif
_cod_data_source_block           9
_cod_original_cell_volume        5964.7(9)
_cod_original_formula_sum        'C43 H34.50 B Co F4 N9.50'
_cod_database_code               4346952
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.934
_shelxl_version_number           2013-2
_shelx_res_checksum              7325
_shelx_hkl_checksum              80061