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_4300056
_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            'C18 H44 Ag3 Co2 F18 N8 O P3 S6'
_chemical_formula_weight         1457.32
_space_group_IT_number           121
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      121
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.012(1)
_cell_length_b                   13.0115
_cell_length_c                   24.707(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.8
_cell_measurement_theta_min      11.6
_cell_volume                     4183.0(5)
_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    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7S'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00941
_diffrn_orient_matrix_UB_12      -0.07626
_diffrn_orient_matrix_UB_13      0.00090
_diffrn_orient_matrix_UB_21      0.07509
_diffrn_orient_matrix_UB_22      -0.00896
_diffrn_orient_matrix_UB_23      0.00722
_diffrn_orient_matrix_UB_31      -0.01340
_diffrn_orient_matrix_UB_32      0.00335
_diffrn_orient_matrix_UB_33      0.03982
_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  0.000
_diffrn_reflns_av_sigmaI/netI    0.079
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1413
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        -0.49
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.681
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   '\y scans(North,Phillips & Mathews,1968)'
_exptl_crystal_colour            black
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_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2856.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.86
_refine_diff_density_min         -1.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.027
_refine_ls_matrix_type           full
_refine_ls_number_constraints    27
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1025
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0546
_refine_ls_shift/esd_max         0.2230
_refine_ls_shift/esd_mean        0.0100
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0574
_reflns_number_observed          1025
_reflns_number_total             1413
_reflns_observed_criterion       >1.5sigma(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        4182.8(8)
_cod_original_sg_symbol_H-M      'I -4 2 m '
_cod_original_formula_sum        'C18 H44 Ag3 Co2 F18 N8 O P3 S6 '
_cod_database_code               4300056