The First Triple Thiol-thiolate Hydrogen Bond versus Triple Diselenide Bond That Bridges Two Metal Centers
Takumi Konno; Kazuyuki Haneishi; Masakazu Hirotsu; Tadashi Yamaguchi; Tasuku Ito; Takashi Yoshimura; Journal of the American Chemical Society 125 (2003) 9244–9245; doi:10.1021/ja0302331

data_4114007
_publ_contact_author
;
     Takumi Konno
Department of Chemistry, Graduate School Of Science, Osaka University,
Toyonaka, Osaka, 560-0043, Japan
;
_publ_contact_author_email       ' konno@ch.wani.osaka-u.ac.jp '
_publ_contact_author_fax         ' +81-6-6850-5765 '
_publ_contact_author_phone       ' +81-6-6850-5765 '
_publ_section_title
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 The First Triple Thiol-thiolate Hydrogen Bond versus Triple Diselenide
 Bond That Bridges Two Metal Centers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9244
_journal_page_last               9245
_journal_paper_doi               10.1021/ja0302331
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C12 H39 B3 F12 N6 S6 Rh2 '
_chemical_formula_sum            'C12 H39 B3 F12 N6 Rh2 S6'
_chemical_formula_weight         926.06
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.517(2)
_cell_length_b                   13.974(2)
_cell_length_c                   16.765(2)
_cell_measurement_reflns_used    1016
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.585
_cell_measurement_theta_min      2.430
_cell_volume                     3166.7(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_publication_material  teXsan
_computing_structure_refinement  SHELXL93
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         ' sealed tube'
_diffrn_radiation_type           'Mo K?a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24142
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.60
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.525
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.7215
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_description       plate
_exptl_crystal_F_000             1848.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.50
_refine_diff_density_rms         0.09
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       0.0000
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^?l^3^/sin(2?q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.563
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         0
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.563
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_obs          0.0243
_refine_ls_shift/esd_max         -0.0360
_refine_ls_shift/esd_mean        0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[?s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0688
_reflns_number_observed          7047
_reflns_number_total             7318
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            ja0302331_2.cif
_cod_data_source_block           DD-[1](BF4)3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w = 1/[?s^2^(Fo^2^) +
(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w = 1/[?s^2^(Fo^2^) +
(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3166.6(7)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C12 H39 B3 F12 N6 S6 Rh2 '
_cod_database_code               4114007