Sulfido-Bridged Tetranuclear Titanium−Iridium Complexes with an Unconventional Tetrahedral Iridium Center
Casado, Miguel A.; Ciriano, Miguel A.; Edwards, Andrew J.; Lahoz, Fernando J.; Oro, Luis A.; Pérez-Torrente, Jesús J.; Organometallics 18 (1999) 3025–; doi:10.1021/om990154r

data_4077783
_publ_section_title
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 Sulfido-Bridged Tetranuclear Titanium&#x2212;Iridium Complexes with an
 Unconventional Tetrahedral Iridium Center
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_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3025
_journal_paper_doi               10.1021/om990154r
_journal_volume                  18
_journal_year                    1999
_chemical_formula_moiety         'C18 H32 Ir3 O13 P3 S3 Ti'
_chemical_formula_sum            'C18 H32 Ir3 O13 P3 S3 Ti'
_chemical_formula_weight         1270.03
_chemical_name_systematic
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 ?
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_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.1800(10)
_cell_length_b                   25.012(4)
_cell_length_c                   26.110(5)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      10
_cell_volume                     6617.5(18)
_computing_cell_refinement       'XSCANS v. 2.1 (Siemens)'
_computing_data_collection       'XSCANS v. 2.1 (Siemens)'
_computing_data_reduction        'XSCANS v. 2.1 (Siemens)'
_computing_molecular_graphics    'XP, SHELXTL v. 5 (Siemens)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'Four circle Siemens P4 diffractometer'
_diffrn_measurement_method       '\w/2\q 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  0.0911
_diffrn_reflns_av_sigmaI/netI    0.1600
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14009
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  55
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    12.650
_exptl_absorpt_correction_T_max  0.1512
_exptl_absorpt_correction_T_min  0.1068
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'XPREP, SHELXTL v. 5 (Siemens)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.807
_refine_diff_density_min         -2.284
_refine_diff_density_rms         0.376
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         11283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.0000P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1578
_reflns_number_gt                6246
_reflns_number_total             11283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990154r.cif
_cod_data_source_block           compound7
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.0000P] where P=3D(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=3D1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.0000P] where
P=3D(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_sg_symbol_H-M      P21/c
_cod_database_code               4077783