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_4318462
_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            'C24 H26 K Mo N5 O Se5'
_chemical_formula_weight         930.34
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Wed Mar  1 14:56:27 2001'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 93.43(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.676(7)
_cell_length_b                   27.28(3)
_cell_length_c                   15.211(8)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      6.3
_cell_measurement_theta_min      3.3
_cell_volume                     3179(5)
_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      -0.07526
_diffrn_orient_matrix_UB_12      0.00694
_diffrn_orient_matrix_UB_13      -0.05453
_diffrn_orient_matrix_UB_21      -0.02260
_diffrn_orient_matrix_UB_22      0.03376
_diffrn_orient_matrix_UB_23      0.02197
_diffrn_orient_matrix_UB_31      0.10419
_diffrn_orient_matrix_UB_32      0.01248
_diffrn_orient_matrix_UB_33      -0.02969
_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  0.293
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6016
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        -0.93
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.293
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.400
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1776.00
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.12
_refine_diff_density_min         -0.82
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.591
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3945
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.1470
_refine_ls_shift/su_mean         0.0120
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0407
_reflns_number_gt                3945
_reflns_number_total             5571
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic025609a_s1_4.cif
_cod_data_source_block           '[K(thf)(CH3CN)][Cp*Mo(i-Se-mns)'
_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        3179(4)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C24 H26 K N5 Mo O Se5 '
_cod_database_code               4318462