Deprotonation of Cp2Ti(SH)2with Mononuclear Rhodium and Iridium Compounds: A New Route to Trinuclear Early−Late Heterobimetallic Complexes
Casado, Miguel A.; Pérez-Torrente, Jesús J.; Ciriano, Miguel A.; Edwards, Andrew J.; Lahoz, Fernando J.; Oro, Luis A.; Organometallics 18 (1999) 5299–; doi:10.1021/om990623p

data_4077830
_publ_section_title
;
 Deprotonation of Cp2Ti(SH)2with Mononuclear Rhodium and Iridium
 Compounds:&#x00A0; A New Route to Trinuclear Early&#x2212;Late
 Heterobimetallic Complexes
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5299
_journal_paper_doi               10.1021/om990623p
_journal_volume                  18
_journal_year                    1999
_chemical_formula_moiety         'C15 H17 O2 Ti 1+,  C6 Ir3 O6 S2 1-'
_chemical_formula_structural     '((C5 H5)2 (C5 H7 O2) Ti) (Ir S2 (CO)6)'
_chemical_formula_sum            'C21 H17 Ir3 O8 S2 Ti'
_chemical_formula_weight         1085.97
_chemical_name_systematic        '  ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.39(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.379(3)
_cell_length_b                   14.912(8)
_cell_length_c                   18.946(5)
_cell_measurement_reflns_used    44
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      17.8
_cell_measurement_theta_min      10
_cell_volume                     2645.1(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, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       '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  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5487
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.536
_exptl_absorpt_correction_T_max  0.429
_exptl_absorpt_correction_T_min  0.153
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Data corrected with XPREP program (SHELXTL v 5.0, Siemens)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.727
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'irregular prism'
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.986
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          -1.128
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.3735P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0679
_refine_ls_wR_factor_ref         0.0582
_reflns_number_gt                3433
_reflns_number_total             4682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990623p.cif
_cod_data_source_block           compound8
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0267P)^2^+0.3735P] 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^)+(0.0267P)^2^+0.3735P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4077830