Synthesis and Reactions of Group 6 Metal Half-Sandwich Complexes of 2,2-Dicyanoethylene-1,1-dichalcogenolates [(Cp*)M{E2CC(CN)2}2]- (M = Mo, W; E = S, Se)
Maochun Hong; Rong Cao; Hiroyuki Kawaguchi; Kazuyuki Tatsumi; Inorganic Chemistry 41 (2002) 4824–4833; doi:10.1021/ic025609a

data_4318465
_publ_section_title
;
 Synthesis and Reactions of Group 6 Metal Half-Sandwich Complexes of
 2,2-Dicyanoethylene-1,1-dichalcogenolates [(Cp*)M{E2CC(CN)2}2]- (M = Mo,
 W; E = S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4824
_journal_page_last               4833
_journal_paper_doi               10.1021/ic025609a
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C20 H18 Br Cu2 N5 S4 W'
_chemical_formula_weight         847.48
_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'
_cell_angle_alpha                98.21(3)
_cell_angle_beta                 90.64(6)
_cell_angle_gamma                74.84(4)
_cell_formula_units_Z            2
_cell_length_a                   11.28(2)
_cell_length_b                   14.758(6)
_cell_length_c                   9.597(3)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      11.0
_cell_volume                     1526(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    DirectMethod
_diffrn_measured_fraction_theta_full 0.9561
_diffrn_measured_fraction_theta_max 0.9561
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.007
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5443
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_standards_decay_%        0.21
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.749
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.844
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.320
_refine_diff_density_max         1.15
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.134
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4611
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.0471
_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_ref         0.0493
_reflns_number_gt                4611
_reflns_number_total             5145
_reflns_threshold_expression     F^2^>3.0\s(F^2^)
_cod_data_source_file            ic025609a_s1_7.cif
_cod_data_source_block           '[Cp*WCu2Br(i-mnt)2]n'
_cod_original_cell_volume        1525(2)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C20 H18 Br Cu2 N5 S4 W '
_cod_database_code               4318465