Transformations Leading to the Generation of Dithiolene Ligands Initiated by Reactions of Sulfur-Rich WS(S2)(S2CNR2)2Complexes with Dimethyl Acetylenedicarboxylate and Phenylacetylene
Lim, Patrick J.; Cook, Vernon C.; Doonan, Christian J.; Young, Charles G.; Tiekink, Edward R. T.; Organometallics 19 (2000) 5643–; doi:10.1021/om0006561

data_4077627
_publ_section_title
;
 Transformations Leading to the Generation of Dithiolene Ligands Initiated
 by Reactions of Sulfur-Rich WS(S2)(S2CNR2)2Complexes with Dimethyl
 Acetylenedicarboxylate and Phenylacetylene
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5643
_journal_paper_doi               10.1021/om0006561
_journal_volume                  19
_journal_year                    2000
_chemical_formula_sum            'C23 H38 N2 O8 S6 W'
_chemical_formula_weight         846.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.82(3)
_cell_angle_beta                 76.68(2)
_cell_angle_gamma                78.16(3)
_cell_formula_units_Z            2
_cell_length_a                   9.278(3)
_cell_length_b                   13.794(4)
_cell_length_c                   14.174(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     1659.6(8)
_computing_data_reduction        Process-Data
_computing_molecular_graphics    ZORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius'
_diffrn_measurement_method       ?:2?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6206
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_time  '160 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.902
_exptl_absorpt_correction_T_max  0.5961
_exptl_absorpt_correction_T_min  0.4061
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.30mm
_exptl_crystal_size_mid          0.30mm
_exptl_crystal_size_min          0.14mm
_refine_diff_density_max         1.451
_refine_diff_density_min         -1.920
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0008(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.6500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                5268
_reflns_number_total             5814
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0006561.cif
_cod_data_source_block           jmwcd6
_cod_original_sg_symbol_H-M      P1_
_cod_database_code               4077627