Synthesis and Characterization of Indium Compounds with Phosphinothiol Ligands. The Crystal and Molecular Structures of [In{2-(Ph2P)C6H4S}3], [In{2-(Ph2P)-6-(Me3Si)C6H3S}2{2-(Ph2PO)-6-(Me3Si)C6H3S}], and [NMe4][In{PhP(C6H4S-2)2}2].CH3CN
Paulo Pérez-Lourido; Jaime Romero; José Arturo García-Vázquez; Antonio Sousa; Kevin Maresca; Jon Zubieta; Inorganic Chemistry 38 (1999) 1293–1298; doi:10.1021/ic980282s

data_4321820
_publ_section_title
;
 Synthesis and Characterization of Indium Compounds with Phosphinothiol
 Ligands. The Crystal and Molecular Structures of [In{2-(Ph2P)C6H4S}3],
 [In{2-(Ph2P)-6-(Me3Si)C6H3S}2{2-(Ph2PO)-6-(Me3Si)C6H3S}], and
 [NMe4][In{PhP(C6H4S-2)2}2].CH3CN
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1293
_journal_page_last               1298
_journal_paper_doi               10.1021/ic980282s
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C42 H41 In N2 P2 S4'
_chemical_formula_weight         878.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 93.190(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0052(2)
_cell_length_b                   11.2240(2)
_cell_length_c                   14.3070(3)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.47
_cell_volume                     2085.16(7)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL XPREP'
_computing_molecular_graphics    'Siemens SHELXTL XP'
_computing_publication_material  'Siemens SHELXTL XCIF'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       'hemisphere 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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10546
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.3229
_exptl_absorpt_correction_T_min  0.1848
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.122
_refine_ls_goodness_of_fit_obs   1.100
_refine_ls_hydrogen_treatment    idealized
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6644
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.152
_refine_ls_restrained_S_obs      1.100
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_obs          0.0352
_refine_ls_shift/esd_max         -0.076
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+1.3578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0929
_refine_ls_wR_factor_obs         0.0869
_reflns_number_observed          6404
_reflns_number_total             6651
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980282s_2.cif
_cod_data_source_block           as014
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+1.3578P] 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^)+(0.0504P)^2^+1.3578P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321820