Substitution of bridging S2 ligands in the [Nb2(μ-S2)2]4+ core: a simple route to [Nb2(Se2)2]4+, [Nb2(S)(Te2)]4+ and [Nb2(S)2]4+
Sokolov, Maxim; Imoto, Hideo; Saito, Taro; Fedorov, Vladimir; Journal of the Chemical Society, Dalton Transactions  (1999) 85–; doi:10.1039/a806627b

data_7027086
_publ_section_title
;
 Substitution of bridging S2 ligands in the [Nb2(\m-S2)2]4+ core: a simple
 route to [Nb2(Se2)2]4+, [Nb2(S)(Te2)]4+ and [Nb2(S)2]4+
;
_journal_issue                   1
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              85
_journal_paper_doi               10.1039/a806627b
_journal_year                    1999
_chemical_formula_moiety         'C20 H40 N4 Nb2 S12 '
_chemical_formula_structural     'Nb2 (S2)2 (S2 C N (C2 H5)2)4'
_chemical_formula_sum            'C20 H40 N4 Nb2 S12'
_chemical_formula_weight         907.10
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 94.460(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.010(3)
_cell_length_b                   6.957(4)
_cell_length_c                   21.172(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295.2
_cell_measurement_theta_max      16.2
_cell_measurement_theta_min      12.2
_cell_volume                     3526(2)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    'DIRDIF92 (PATTY)'
_diffrn_ambient_temperature      295.2
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.03365
_diffrn_orient_matrix_UB_12      0.01092
_diffrn_orient_matrix_UB_13      -0.03073
_diffrn_orient_matrix_UB_21      -0.02468
_diffrn_orient_matrix_UB_22      -0.02667
_diffrn_orient_matrix_UB_23      0.03491
_diffrn_orient_matrix_UB_31      -0.00206
_diffrn_orient_matrix_UB_32      0.14081
_diffrn_orient_matrix_UB_33      0.00900
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.108
_diffrn_reflns_av_sigmaI/netI    0.103
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            4479
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        -0.19
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   '\DF (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1848.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.52
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.375
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2550
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0424
_refine_ls_shift/esd_max         0.0000
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0269
_reflns_number_observed          2550
_reflns_number_total             4372
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            806627Bsup1.cif
_cod_data_source_block           mc1505
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00001|Fo|^2^]' 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) + 0.00001|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3526(1)
_cod_original_sg_symbol_H-M      'C 2/c        '
_cod_original_formula_sum        'C20 H40 N4 Nb2 S12 '
_cod_database_code               7027086