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_4318463
_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 H31 K N4 O2 S5 W'
_chemical_formula_weight         814.80
_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 Feb 25 15:24:02 2001'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                105.28(4)
_cell_angle_beta                 97.67(3)
_cell_angle_gamma                66.75(3)
_cell_formula_units_Z            2
_cell_length_a                   13.676(5)
_cell_length_b                   15.83(1)
_cell_length_c                   8.641(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11.0
_cell_volume                     1657.1(14)
_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
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.06475
_diffrn_orient_matrix_UB_12      -0.00429
_diffrn_orient_matrix_UB_13      0.03368
_diffrn_orient_matrix_UB_21      0.02559
_diffrn_orient_matrix_UB_22      0.01155
_diffrn_orient_matrix_UB_23      0.11466
_diffrn_orient_matrix_UB_31      -0.03865
_diffrn_orient_matrix_UB_32      0.06958
_diffrn_orient_matrix_UB_33      0.01128
_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    0.017
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6109
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        -1.24
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.959
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             808.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.90
_refine_diff_density_min         -1.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.651
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5333
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.2006
_refine_ls_shift/su_mean         0.0443
_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          0.0564
_refine_ls_wR_factor_ref         0.0564
_reflns_number_gt                5333
_reflns_number_total             5840
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic025609a_s1_5.cif
_cod_data_source_block           '[K(thf)2][Cp*W(i-mnt)(S-i-mnt)'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_reflns_observed_expression' tag replaced with
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file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_site_calc_flags'
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'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_type_scat_imag'
tag replaced with '_atom_type_scat_dispersion_imag' tag as specified
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'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        1657(1)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C26 H31 K N4 O2 S5 W '
_cod_database_code               4318463