Synthesis and crystallographic characterization of a mononuclear cobalt(III) complex possessing both thiolate and thioether donors: reactivity of an thiolate-bridged pentanuclear Co~2~Ag~3~ complex with iodomethane
Fukuda, Yosuke; Yoshinari, Nobuto; Konno, Takumi; Acta Crystallographica Section E 73 (2017) 678–681; doi:10.1107/S2056989017005229

data_2242222
_publ_section_title
;
 Synthesis and crystallographic characterization of a mononuclear
 cobalt(III) complex possessing both thiolate and thioether donors:
 reactivity of an thiolate-bridged pentanuclear Co~2~Ag~3~ complex with
 iodomethane
;
_journal_coeditor_code           IS5473
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              678
_journal_page_last               681
_journal_paper_doi               10.1107/S2056989017005229
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Co (C11 H27 N4 S3)], 2P F6'
_chemical_formula_moiety         'C11 H27 Co N4 S3 2+, 2(F6 P -)'
_chemical_formula_sum            'C11 H27 Co F12 N4 P2 S3'
_chemical_formula_weight         660.41
_chemical_name_systematic
'{2-[(Bis{[2-(methylsulfanyl)ethyl]aminomethyl}aminomethyl)amino]ethanethiolato}cobalt(III) bis(hexafluoridophosphate)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 110.629(8)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   32.440(3)
_cell_length_b                   10.3197(8)
_cell_length_c                   29.869(2)
_cell_measurement_reflns_used    27114
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.09
_cell_volume                     9358.1(14)
_computing_cell_refinement
;
PROCESS-AUTO (Rigaku, 2000)
;
_computing_data_collection
;
PROCESS-AUTO (Rigaku, 2000)
;
_computing_data_reduction
;
PROCESS-AUTO (Rigaku, 2000)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
<i>SHELXL2014/7</i> (Sheldrick, 2015) and Mercury (Macrae <i>et al.</i>,
 2006)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>SHELXS2014/7</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            44747
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.438
_diffrn_reflns_theta_min         3.084
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            purple--brown
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_description       block
_exptl_crystal_F_000             5344
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.256
_refine_diff_density_min         -0.658
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         10620
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0556
_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^)+(0.0690P)^2^+65.6905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1409
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                8276
_reflns_number_total             10620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            is5473sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        9358.1(13)
_cod_database_code               2242222
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.940
_shelx_hkl_checksum              86728
_shelx_res_checksum              87477
_cod_database_fobs_code 2242222