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_7027087
_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_structural     '[Nb2 S2 (CH3 CO CH CO CH3)4] (CH2CL2)2'
_chemical_formula_sum            'C22 H32 Cl4 Nb2 O8 S2'
_chemical_formula_weight         816.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Thu May  7 1998'
_audit_creation_method           'from TEXRAY.INF file'
_audit_update_record             ' May 7 1998'
_cell_angle_alpha                101.5(1)
_cell_angle_beta                 95.69(10)
_cell_angle_gamma                73.3(2)
_cell_formula_units_Z            1
_cell_length_a                   9.00(2)
_cell_length_b                   11.15(3)
_cell_length_c                   8.868(6)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      7.9
_cell_measurement_theta_min      3.8
_cell_volume                     834(3)
_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    'SIR92 (Altomare, A. et al. 1994)'
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.07497
_diffrn_orient_matrix_UB_12      0.05305
_diffrn_orient_matrix_UB_13      0.02333
_diffrn_orient_matrix_UB_21      -0.02042
_diffrn_orient_matrix_UB_22      0.01562
_diffrn_orient_matrix_UB_23      0.11204
_diffrn_orient_matrix_UB_31      0.08630
_diffrn_orient_matrix_UB_32      -0.07746
_diffrn_orient_matrix_UB_33      0.01316
_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  0.052
_diffrn_reflns_av_sigmaI/netI    0.038
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            967
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         22.45
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        -1.86
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.170
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.444
_exptl_absorpt_correction_type   '\DF (DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             410.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.900
_refine_ls_hydrogen_treatment    'Hydrogen atoms were not included.'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     77
_refine_ls_number_reflns         784
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0737
_refine_ls_shift/esd_max         0.0020
_refine_ls_shift/esd_mean        0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + (1/4)(0.019|Fo|)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0778
_reflns_number_observed          784
_reflns_number_total             798
_reflns_observed_criterion       >2.0sigma(I)
_cod_data_source_file            806627Bsup1.cif
_cod_data_source_block           2
_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) +
(1/4)(0.019|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) + (1/4)(0.019|Fo|)^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        834(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C22 H32 Cl4 Nb2 O8 S2 '
_cod_database_code               7027087