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_4114008
_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
;
 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 H52 B6 F24 N6 O8 Rh2 Se6 '
_chemical_formula_sum            'C12 H52 B6 F24 N6 O8 Rh2 Se6'
_chemical_formula_weight         1608.97
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 110.74(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.963(3)
_cell_length_b                   10.569(2)
_cell_length_c                   16.508(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     2278.3(7)
_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  SHELXL93
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       'Rigaku AFC7S'
_diffrn_measurement_method       ?w-2?q
_diffrn_orient_matrix_UB_11      -0.03494
_diffrn_orient_matrix_UB_12      0.07891
_diffrn_orient_matrix_UB_13      -0.02926
_diffrn_orient_matrix_UB_21      -0.05751
_diffrn_orient_matrix_UB_22      -0.05184
_diffrn_orient_matrix_UB_23      -0.03955
_diffrn_orient_matrix_UB_31      -0.03656
_diffrn_orient_matrix_UB_32      0.00614
_diffrn_orient_matrix_UB_33      0.04213
_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  0.024
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5757
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.52
_diffrn_standards_decay_%        -19.57
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.658
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.327
_exptl_absorpt_correction_type   'psi-scan (North,Phillips & Mathews,1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.345
_exptl_crystal_description       plate
_exptl_crystal_F_000             1540.00
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.79
_refine_diff_density_min         -1.23
_refine_diff_density_rms         0.17
_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   1.135
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         0
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_obs          0.0529
_refine_ls_shift/esd_max         0.0420
_refine_ls_shift/esd_mean        0.0020
_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         0.1761
_reflns_number_observed          3796
_reflns_number_total             5538
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            ja0302331_3.cif
_cod_data_source_block           '[2](BF4)6'
_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        2278.3(6)
_cod_original_sg_symbol_H-M      'P 2/n '
_cod_original_formula_sum        'C12 H52 B6 F24 N6 O8 Rh2 Se6 '
_cod_database_code               4114008