Oxo Sulfido Heteronuclear Titanium−Rhodium Clusters with an Incomplete Doubly-Fused Cubane Structure
Casado, Miguel A.; Ciriano, Miguel A.; Edwards, Andrew J.; Lahoz, Fernando J.; Pérez-Torrente, Jesús J.; Oro, Luis A.; Organometallics 17 (1998) 3414–; doi:10.1021/om980307v

data_4078404
_publ_section_title
;
 Oxo Sulfido Heteronuclear Titanium&#x2212;Rhodium Clusters with an
 Incomplete Doubly-Fused Cubane Structure
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3414
_journal_paper_doi               10.1021/om980307v
_journal_volume                  17
_journal_year                    1998
_chemical_formula_moiety         'C50 H40 O11 P2 Rh4 S4 Ti2'
_chemical_formula_structural
'[{CpTi}~2~(\m~4~-O)(\m~3~-S)~4~{Rh~4~(CO)~4~(P(OPh)~3~)2}]'
_chemical_formula_sum            'C50 H40 O11 P2 Rh4 S4 Ti2'
_chemical_formula_weight         1514.44
_chemical_name_systematic
;
tetrakis-mu!3$-sulfido-mu!4$-oxide-bis(eta$5!-cyclopentadienyl-titanium(iv))-
bis(carbonyl-rhodium(i))-bis(carbonyl-triphenylphosphite-rhodium(i))
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                96.796(2)
_cell_angle_beta                 101.292(2)
_cell_angle_gamma                98.2540(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5709(6)
_cell_length_b                   14.1410(9)
_cell_length_c                   18.9384(11)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      1.70
_cell_volume                     2716.0(3)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        "'Siemens SAINT"
_computing_molecular_graphics    'SHELXTL v5 (Siemens, 1994)'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL, Siemens 1994)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.867
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0914
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19306
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.737
_exptl_absorpt_correction_T_max  0.8736
_exptl_absorpt_correction_T_min  0.7118
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_meas      ?
_exptl_crystal_description       slab
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.620
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.144
_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     658
_refine_ls_number_reflns         11848
_refine_ls_number_restraints     450
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+0.0000P] where
 P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                7543
_reflns_number_total             11848
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om980307v.cif
_cod_data_source_block           comp5
_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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4078404