The Preparation of (η5-C5Me5)Ir(PMe3)S4 from (η5-C5Me5)Ir(PMe3)(SH)2 and SO2
Bouchra El Mouatassim; Céline Pearson; Alan Shaver; Inorganic Chemistry 40 (2001) 5290–5291; doi:10.1021/ic001385p

data_4320274
_publ_section_title
;
 The Preparation of (\h5-C5Me5)Ir(PMe3)S4 from (\h5-C5Me5)Ir(PMe3)(SH)2
 and SO2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5290
_journal_page_last               5291
_journal_paper_doi               10.1021/ic001385p
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'synthesized by the authors, see text'
_chemical_formula_moiety         'C13 H24 Ir P S4'
_chemical_formula_structural     Ir(PCH3)(Cp*)(S4)
_chemical_formula_sum            'C13 H24 Ir P S4'
_chemical_formula_weight         531.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL96 (Sheldrick, 1996)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.767(3)
_cell_length_b                   13.443(5)
_cell_length_c                   15.447(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      12.5
_cell_volume                     1820.5(10)
_computing_molecular_graphics
'ORTEPII (Johnson (1976) in NRCVAX (Gabe et al (1989))'
_computing_publication_material
'NRCVAX (Gabe et al (1989) and SHELXL96 (Sheldrick (1996))'
_computing_structure_solution    'SHELXS96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       'omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\%a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.120
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14258
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0.8
_diffrn_standards_interval_count 250
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.826
_exptl_absorpt_correction_T_max  0.9992
_exptl_absorpt_correction_T_min  0.2626
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.294
_refine_diff_density_min         -1.788
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.010(19)
_refine_ls_extinction_coef       0.0009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL96 (Sheldrick, 1996)'
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_restrained_S_obs      1.029
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1331
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                3157
_reflns_number_total             3584
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic001385p.cif
_cod_data_source_block           complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4320274
_cod_database_fobs_code          4320274