Synthesis, Characterization, and Chiral Properties of CoIII2AgI3 Pentanuclear, CoIII4ZnII4 Octanuclear, and CoIII Mononuclear Complexes with Aza-Capped Hexadentate-N3S3 Thiolate Ligands: Crystal Structures of [Ag3{Co(L)}2][PF6]3 and [Zn4O{Co(L)}4][PF6]6 (L = N(CH2NHCH2CH2S-)3)
Keiji Tokuda; Ken-ichi Okamoto; Takumi Konno; Inorganic Chemistry 39 (2000) 333–339; doi:10.1021/ic9906407

data_4300057
_publ_contact_author
;
Takumi Konno
Department of Chemistry, Faculty of Engineering, Gunma University, Kiryu,
Gunma 376-8515, Japan
;
_publ_contact_author_email       ' konno@chem.gunma-u.ac.jp'
_publ_contact_author_fax         '+ 81-277-30-1263'
_publ_contact_author_phone       '+ 81-277-30-1260'
_publ_section_title
;
Synthesis, Characterization, and Chiral Properties of
CoIII2AgI3 Pentanuclear, CoIII4ZnII4 Octanuclear, and CoIII Mononuclear
Complexes with Aza-Capped Hexadentate-N3S3 Thiolate Ligands: Crystal
Structures of [Ag3{Co(L)}2][PF6]3 and [Zn4O{Co(L)}4][PF6]6 (L =
N(CH2NHCH2CH2S-)3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              333
_journal_page_last               339
_journal_paper_doi               10.1021/ic9906407
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C36 H100 Co4 F36 N16 O9 P6 S12 Zn4'
_chemical_formula_weight         2653.05
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 101.3(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.33(7)
_cell_length_b                   25.76(10)
_cell_length_c                   24.83(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      13.9
_cell_volume                     8988(6)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'Direct Method (SIR92)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.02168
_diffrn_orient_matrix_UB_12      -0.03362
_diffrn_orient_matrix_UB_13      -0.01868
_diffrn_orient_matrix_UB_21      0.02536
_diffrn_orient_matrix_UB_22      -0.01930
_diffrn_orient_matrix_UB_23      0.03477
_diffrn_orient_matrix_UB_31      -0.06287
_diffrn_orient_matrix_UB_32      0.00381
_diffrn_orient_matrix_UB_33      0.01135
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.177
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21723
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        -1.85
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.290
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5336.00
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.06
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.265
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1108
_refine_ls_number_reflns         8382
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0690
_refine_ls_shift/esd_max         0.0512
_refine_ls_shift/esd_mean        0.0090
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0774
_reflns_number_observed          8382
_reflns_number_total             20899
_reflns_observed_criterion       >2.0sigma(I)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        8955(47)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C36 H100 Co4 F36 N16 O9 P6 S12 Zn4 '
_cod_database_code               4300057