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_4308337
_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 H39.50 B Mo N7 O4.75 S3 '
_chemical_formula_sum            'C26 H39.5 B Mo N7 O4.75 S3'
_chemical_formula_weight         729.08
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.60(1)
_cell_length_b                   13.764(3)
_cell_length_c                   16.305(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      5.4
_cell_measurement_theta_min      3.9
_cell_volume                     6867(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.01106
_diffrn_orient_matrix_UB_12      -0.05362
_diffrn_orient_matrix_UB_13      0.03578
_diffrn_orient_matrix_UB_21      -0.01325
_diffrn_orient_matrix_UB_22      -0.03236
_diffrn_orient_matrix_UB_23      -0.04897
_diffrn_orient_matrix_UB_31      0.02775
_diffrn_orient_matrix_UB_32      -0.03682
_diffrn_orient_matrix_UB_33      -0.00912
_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    0.143
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8689
_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_%        -3.2
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type
;
\DF (DIFABS; Walker & Stuart, 1983)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_description       odd
_exptl_crystal_F_000             3020
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.68
_refine_diff_density_min         -1.03
_refine_diff_density_rms         0.100
_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     408
_refine_ls_number_reflns         7923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.214
_refine_ls_R_factor_gt           0.072
_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^)+(0.1037P)^2^+0.131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.179
_refine_ls_wR_factor_ref         0.229
_reflns_number_gt                3383
_reflns_number_total             7923
_reflns_threshold_expression     I>2.00\s(I)
_cod_data_source_file            ic048882gsi20040817_084428_1.cif
_cod_data_source_block           Tp*Mo{S2C2(CO2Me)2}(SCNEt2-?2S,C).0.75H2O
_cod_original_sg_symbol_H-M      'P b c n '
_cod_original_formula_sum        'C26 H39.50 B Mo N7 O4.75 S3 '
_cod_database_code               4308337