Direct Conversion of α-Substituted Ketones to Metallo-1,2-enedithiolates
John K. Hsu; Cecilia J. Bonangelino; Sharada P. Kaiwar; Christine M. Boggs; James C. Fettinger; Robert S. Pilato; Inorganic Chemistry 35 (1996) 4743–4751; doi:10.1021/ic9602052

data_4323873
_publ_section_title
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 Direct Conversion of \a-Substituted Ketones to Metallo-1,2-enedithiolates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4743
_journal_page_last               4751
_journal_paper_doi               10.1021/ic9602052
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C20.5 H17 Cl Mo N2 S2'
_chemical_formula_weight         486.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.440(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.4514(15)
_cell_length_b                   15.474(2)
_cell_length_c                   12.2201(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.8
_cell_measurement_theta_min      8.8
_cell_volume                     3869.9(7)
_computing_cell_refinement       'Enraf-Nonius EXPRESS'
_computing_data_collection       'Enraf-Nonius EXPRESS'
_computing_molecular_graphics    'ORTEP NRCVAX '
_computing_publication_material  'XCIF, SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 '
_diffrn_measurement_method       'omega:2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2702
_diffrn_reflns_theta_max         22.58
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.039
_exptl_absorpt_correction_T_max  0.9952
_exptl_absorpt_correction_T_min  0.8514
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.020
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         2556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_obs          0.0275
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+3.8650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0698
_refine_ls_wR_factor_obs         0.0668
_reflns_number_observed          2157
_reflns_number_total             2556
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9602052_2.cif
_cod_data_source_block           Complex7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+3.8650P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+3.8650P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3869.8(7)
_cod_original_formula_sum        'C20.50 H17 Cl Mo N2 S2'
_cod_database_code               4323873