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_4323872
_publ_section_title
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 Direct Conversion of \a-Substituted Ketones to Metallo-1,2-enedithiolates
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_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            'C21 H18 B Cl2 F4 Mo N2 S2'
_chemical_formula_weight         616.14
_chemical_name_systematic
; 
 ? 
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_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
_cell_angle_alpha                81.49(2)
_cell_angle_beta                 76.14(2)
_cell_angle_gamma                85.784(10)
_cell_formula_units_Z            2
_cell_length_a                   7.4009(8)
_cell_length_b                   10.1192(13)
_cell_length_c                   15.930(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      20.2
_cell_measurement_theta_min      17.6
_cell_volume                     1144.6(4)
_computing_cell_refinement       'Enraf-Nonius CAD4 EXPRESS'
_computing_data_collection       'Enraf-Nonius CAD4 EXPRESS'
_computing_data_reduction        NRCVAX
_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      153(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  0.0882
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3177
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  0.9968
_exptl_absorpt_correction_T_min  0.5860
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_description       Needle
_exptl_crystal_F_000             614
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.611
_refine_diff_density_rms         0.185
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.113
_refine_ls_goodness_of_fit_obs   1.195
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         2911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_restrained_S_obs      1.195
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_obs          0.0764
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+4.9698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2013
_refine_ls_wR_factor_obs         0.1915
_reflns_number_observed          2336
_reflns_number_total             2911
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9602052_1.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+4.9698P] 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^)+(0.1215P)^2^+4.9698P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323872