Restricted Rotation around the P-C Bond in Metalated Phosphonium Salts: A Variable-Temperature 1H NMR Study. X-ray Crystal Structures of [{AuP(C6H11)3}2{μ-C(PTo3)(py-2)}]ClO4 and [(AuPPh3)2{μ-{C(PPh3)(py-2)}(AuPPh3)}](CF3SO3)2
José Vicente; María-Teresa Chicote; María-Cristina Lagunas; Peter G. Jones; Birte Ahrens; Inorganic Chemistry 36 (1997) 4938–4944; doi:10.1021/ic970367d

data_4323642
_publ_section_title
;
 Restricted Rotation around the P-C Bond in Metalated Phosphonium Salts: A
 Variable-Temperature 1H NMR Study. X-ray Crystal Structures of
 [{AuP(C6H11)3}2{\m-C(PTo3)(py-2)}]ClO4 and
 [(AuPPh3)2{\m-{C(PPh3)(py-2)}(AuPPh3)}](CF3SO3)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4938
_journal_page_last               4944
_journal_paper_doi               10.1021/ic970367d
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C82 H68 Au3 Cl4 F6 N O6 P4 S2'
_chemical_formula_weight         2198.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 96.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.232(6)
_cell_length_b                   25.800(7)
_cell_length_c                   18.005(7)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10.5
_cell_measurement_theta_min      10
_cell_volume                     7949(5)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-92
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens R3'
_diffrn_measurement_method       Omega-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  0.0620
_diffrn_reflns_av_sigmaI/netI    0.1024
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.859
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       tablet
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.482
_refine_diff_density_min         -1.505
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.029
_refine_ls_hydrogen_treatment    riding
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_refine_ls_number_parameters     568
_refine_ls_number_reflns         10418
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.071
_refine_ls_restrained_S_obs      1.009
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_obs          0.0524
_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^)+(0.0613P)^2^+54.1631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1584
_refine_ls_wR_factor_obs         0.1138
_reflns_number_observed          6154
_reflns_number_total             10422
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970367d_2.cif
_cod_data_source_block           hauch
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (25 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (54
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+54.1631P] 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^)+(0.0613P)^2^+54.1631P] 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        7948.9(47)
_cod_database_code               4323642