Synthesis of the First Complex with a Hypercoordinate Ylidic Carbon Atom. Crystal and Molecular Structure of [{Au(PPh3)}4CS(O)Me2](ClO4)2
José Vicente; M. Teresa Chicote; Rita Guerrero; Peter G. Jones; Journal of the American Chemical Society 118 (1996) 699–700; doi:10.1021/ja953504j

data_4117102
_publ_section_title
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 Synthesis of the First Complex with a Hypercoordinate Ylidic Carbon Atom.
 Crystal and Molecular Structure of [{Au(PPh3)}4CS(O)Me2](ClO4)2
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              699
_journal_page_last               700
_journal_paper_doi               10.1021/ja953504j
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C78 H72 Au4 Cl2 O10 P4 S'
_chemical_formula_weight         2184.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.07(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.520(2)
_cell_length_b                   21.394(4)
_cell_length_c                   22.860(4)
_cell_measurement_reflns_used    57
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      5
_cell_volume                     7495(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14848
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_diffrn_reflns_theta_min         3.07
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.047
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             4184
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.403
_refine_diff_density_min         -1.482
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
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_refine_ls_R_factor_obs          0.0432
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0895
_refine_ls_wR_factor_obs         0.0766
_reflns_number_observed          6915
_reflns_number_total             12922
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja953504j.cif
_cod_data_source_block           jacks
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.0000P] 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^)+(0.0346P)^2^+0.0000P] 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_original_cell_volume        7495.4(21)
_cod_database_code               4117102