Alkylation Reactions of [WS4]2- and [(η5-C5Me5)WS3]- with 2,6-Bis(bromomethyl)pyridine: The First Isolation of Bisalkylated Tetrathiometalate WS2{2,6-(SCH2)2(C5H3N)}
Rong Cao; Kazuyuki Tatsumi; Inorganic Chemistry 41 (2002) 4102–4104; doi:10.1021/ic0256258

data_4318343
_publ_contact_author_address
;
Research Center for Materials Science, and Department of Chemistry, Graduate 
School of Science, Nagoya University, Furo-cho, Chikusa-ku, Nagoya 464-8602
;
_publ_contact_author_email       ' i45100a@nucc.cc.nagoya-u.ac.jp '
_publ_contact_author_name        ' Kazuyuki Tatsumi'
_publ_section_title
;
 Alkylation Reactions of [WS4]2- and [(\h5-C5Me5)WS3]- with
 2,6-Bis(bromomethyl)pyridine: The First Isolation of Bisalkylated
 Tetrathiometalate WS2{2,6-(SCH2)2(C5H3N)}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4102
_journal_page_last               4104
_journal_paper_doi               10.1021/ic0256258
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C7 H7 N S4 W '
_chemical_formula_sum            'C7 H7 N S4 W'
_chemical_formula_weight         417.23
_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             'Sat May 27 11:52:52 2001'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                104.44(2)
_cell_angle_beta                 115.75(2)
_cell_angle_gamma                73.60(2)
_cell_formula_units_Z            2
_cell_length_a                   8.620(2)
_cell_length_b                   9.455(2)
_cell_length_c                   7.636(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     531.9(2)
_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    SHELXS97
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.07777
_diffrn_orient_matrix_UB_12      -0.08830
_diffrn_orient_matrix_UB_13      0.06589
_diffrn_orient_matrix_UB_21      -0.02905
_diffrn_orient_matrix_UB_22      -0.06492
_diffrn_orient_matrix_UB_23      -0.13073
_diffrn_orient_matrix_UB_31      0.10191
_diffrn_orient_matrix_UB_32      0.02020
_diffrn_orient_matrix_UB_33      -0.01324
_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  0.010
_diffrn_reflns_av_sigmaI/netI    0.025
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2600
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        -1.63
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.605
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            purple-red
_exptl_crystal_density_diffrn    2.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             388.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.39
_refine_diff_density_min         -2.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.829
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2277
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00010|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0311
_refine_ls_wR_factor_ref         0.0311
_reflns_number_gt                2277
_reflns_number_total             2440
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic0256258_s1_2.cif
_cod_data_source_block           WS2(SCH2)2(2_6-C5H3N)_repe
_cod_depositor_comments
;
The following automatic conversions were performed:
'_reflns_observed_expression' tag replaced with
'_reflns_threshold_expression' tag as specified in the replacement
file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_site_calc_flags'
tag replaced with '_atom_site_calc_flag' tag as specified in the
replacement file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_type_scat_imag'
tag replaced with '_atom_type_scat_dispersion_imag' tag as specified
in the replacement file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 3137 2015-03-23 15:08:43Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C7 H7 N S4 W '
_cod_database_code               4318343