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_4318342
_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_sum            'C29 H40 N2 S6 W2'
_chemical_formula_weight         976.71
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             'Sat May 27 11:17:49 2001'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 94.76(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.112(3)
_cell_length_b                   21.515(6)
_cell_length_c                   21.445(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      12.1
_cell_measurement_theta_min      3.2
_cell_volume                     6948(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      0.00200
_diffrn_orient_matrix_UB_12      -0.04644
_diffrn_orient_matrix_UB_13      -0.00104
_diffrn_orient_matrix_UB_21      0.03683
_diffrn_orient_matrix_UB_22      -0.00018
_diffrn_orient_matrix_UB_23      0.04095
_diffrn_orient_matrix_UB_31      -0.05521
_diffrn_orient_matrix_UB_32      -0.00180
_diffrn_orient_matrix_UB_33      0.02261
_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  0.089
_diffrn_reflns_av_sigmaI/netI    0.264
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11231
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        -3.74
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.006
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            violet-red
_exptl_crystal_density_diffrn    1.867
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3776.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.33
_refine_diff_density_min         -1.04
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     393
_refine_ls_number_reflns         3890
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.0670
_refine_ls_shift/su_mean         0.0040
_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          0.0562
_refine_ls_wR_factor_ref         0.0562
_reflns_number_gt                3890
_reflns_number_total             10722
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic0256258_s1_1.cif
_cod_data_source_block           (Cp*WS2(SCH2))2(2_6-C5H3N)
_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 21/a '
_cod_original_formula_sum        'C29 H40 N2 S6 W2 '
_cod_database_code               4318342