Tridentate Coordination Modes of Functionalized Titanocene Thiolates. Crystal Structure of [(η5-C5H4SiMe3)Ti(μ-η5:κ-P-C5H4PPh2)(μ-SPh)2W(CO)3]
Esther Delgado; M. Angeles García; Enrique Gutierrez-Puebla; Elisa Hernández; Noelia Mansilla; Félix Zamora; Inorganic Chemistry 37 (1998) 6684–6689; doi:10.1021/ic9804972

data_4323250
_publ_contact_author
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        E. Guti\'errez Puebla
        Instituto de Ciencia de Materiales
        CSIC
        Campus de Cantoblanco
        28049 MADRID
        Spain
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_publ_contact_author_email       enrique@immrx1.icmm.csic.es
_publ_contact_author_fax         '34 1 372-0623'
_publ_contact_author_phone       '34 1 334-9024'
_publ_section_title
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 Tridentate Coordination Modes of Functionalized Titanocene Thiolates.
 Crystal Structure of
 [(\h5-C5H4SiMe3)Ti(\m-\h5:\k-P-C5H4PPh2)(\m-SPh)2W(CO)3]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6684
_journal_page_last               6689
_journal_paper_doi               10.1021/ic9804972
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C40 H37 O3 P S2 Si Ti W'
_chemical_formula_weight         920.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                   23.0811(15)
_cell_length_b                   14.3046(9)
_cell_length_c                   11.6892(8)
_cell_measurement_temperature    293(2)
_cell_volume                     3859.4(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens SMART'
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            8423
_diffrn_reflns_theta_max         23.38
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    3.402
_exptl_absorpt_correction_T_max  0.112
_exptl_absorpt_correction_T_min  0.037
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.376
_refine_diff_density_min         -2.281
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.040
_refine_ls_goodness_of_fit_obs   1.058
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         3125
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_obs          0.0462
_refine_ls_shift/esd_max         -0.023
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+4.0331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1237
_refine_ls_wR_factor_obs         0.1214
_reflns_number_observed          2935
_reflns_number_total             3125
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9804972.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+4.0331P] where P=(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=1/[\s^2^(Fo^2^)+(0.0868P)^2^+4.0331P] where P=(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               4323250