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_4077829
_publ_section_title
;
 Deprotonation of Cp2Ti(SH)2with Mononuclear Rhodium and Iridium
 Compounds:&#x00A0; A New Route to Trinuclear Early&#x2212;Late
 Heterobimetallic Complexes
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_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         'C26 H36 O2 Rh2 S2 Ti'
_chemical_formula_structural     '(C5 H5) (C5 H7 O2) Ti S2 (Rh (C8 H12))2'
_chemical_formula_sum            'C26 H36 O2 Rh2 S2 Ti'
_chemical_formula_weight         698.39
_chemical_name_systematic        '  ?'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.593(2)
_cell_length_b                   11.6592(7)
_cell_length_c                   12.9790(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      10
_cell_volume                     2662.3(4)
_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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2681
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.696
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'Data corrected with XPREP program (SHELXTL v 5.0, Siemens)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       cubes
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.00075(9)
_refine_ls_extinction_expression Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          -0.048
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0276P)^2^+4.3535P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0620
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                2261
_reflns_number_total             2466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om990623p.cif
_cod_data_source_block           compound1
_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^)+(0.0276P)^2^+4.3535P] 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^)+(0.0276P)^2^+4.3535P] 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_database_code               4077829