Formation of Mono(dithiolene)-Thiocarboxamido Complexes in Reactions of Thio(dithiocarbamato)-Mo/W Complexes and Dimethyl Acetylenedicarboxylate
Patrick J. Lim; Damian A. Slizys; Edward R. T. Tiekink; Charles G. Young; Inorganic Chemistry 44 (2005) 114–121; doi:10.1021/ic048882g

data_4308338
_publ_section_title
;
Formation of Mono(dithiolene)-Thiocarboxamido Complexes in Reactions of
Thio(dithiocarbamato)-Mo/W Complexes and Dimethyl Acetylenedicarboxylate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              114
_journal_page_last               121
_journal_paper_doi               10.1021/ic048882g
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C26 H38 B N7 O4 S3 W '
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_atom_sites_solution_secondary   difmap
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_cell_angle_gamma                91.56(1)
_cell_formula_units_Z            2
_cell_length_a                   12.219(2)
_cell_length_b                   13.088(2)
_cell_length_c                   11.403(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      20.9
_cell_volume                     1677.7(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et. al. 1993)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.02899
_diffrn_orient_matrix_UB_12      -0.04016
_diffrn_orient_matrix_UB_13      0.05141
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_diffrn_orient_matrix_UB_22      0.05342
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_diffrn_orient_matrix_UB_32      -0.04136
_diffrn_orient_matrix_UB_33      -0.07964
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8096
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.6
_diffrn_reflns_theta_max         27.6
_diffrn_reflns_theta_min         3.0
_diffrn_standards_decay_%        -11.0
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.671
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type
;
\DF (DIFABS; Walker & Stuart, 1983)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.99
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.070
_refine_ls_R_factor_gt           0.038
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+1.5791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.089
_refine_ls_wR_factor_ref         0.099
_reflns_number_gt                6077
_reflns_number_total             7733
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic048882gsi20040817_084428_2.cif
_cod_data_source_block           Tp*W{S2C2(CO2Me)2}(SCNEt2-?2S,C)
_cod_original_cell_volume        1677.8(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C26 H38 B N7 O4 S3 W '
_cod_database_code               4308338