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_4318459
_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            'C26 H35 Mo N5 S4'
_chemical_formula_weight         641.78
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      63
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_audit_creation_date             'Sat Feb 25 15:20:51 2001'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.236(9)
_cell_length_b                   25.149(9)
_cell_length_c                   13.805(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.5
_cell_volume                     3207(4)
_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    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.03956
_diffrn_orient_matrix_UB_12      -0.02625
_diffrn_orient_matrix_UB_13      0.04753
_diffrn_orient_matrix_UB_21      -0.09407
_diffrn_orient_matrix_UB_22      0.00043
_diffrn_orient_matrix_UB_23      0.03585
_diffrn_orient_matrix_UB_31      -0.03615
_diffrn_orient_matrix_UB_32      -0.02986
_diffrn_orient_matrix_UB_33      -0.04127
_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  0.000
_diffrn_reflns_av_sigmaI/netI    0.034
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1575
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        -0.56
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.790
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Walker & Stuart, 1983)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectagle
_exptl_crystal_F_000             1328.00
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.40
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.143
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1279
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.0738
_refine_ls_shift/su_mean         0.0173
_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          0.0597
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                1279
_reflns_number_total             1575
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic025609a_s1_1.cif
_cod_data_source_block           '[Et4N][Cp*Mo(i-mnt)2]'
_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_cell_volume        3206(3)
_cod_original_sg_symbol_H-M      'C m c m '
_cod_original_formula_sum        'C26 H35 N5 Mo S4 '
_cod_database_code               4318459