Polynuclear titanocene complexes with antimony ligands: [(Cp2Ti)2(SbR2)2] (R = Et), [(Cp2Ti)3(SbR)3Sb] [R = 2-(Me2NCH2)C6H4] and [(Cp2Ti)5(SbR)2Sb7] (R = Me3SiCH2)
Breunig, Hans J.; Lork, Enno; Moldovan, Ovidiu; Raţ, Ciprian I.; Rosenthal, Uwe; Silvestru, Cristian; Dalton Transactions  (2009) 5065–5067; doi:10.1039/b904846d

data_7001552
_publ_section_title
;
 Polynuclear titanocene complexes with antimony ligands:
 [(Cp2Ti)2(SbR2)2] (R = Et), [(Cp2Ti)3(SbR)3Sb] [R = 2-(Me2NCH2)C6H4]
 and [(Cp2Ti)5(SbR)2Sb7] (R = Me3SiCH2)
;
_journal_issue                   26
_journal_name_full               'Dalton Transactions'
_journal_page_first              5065
_journal_page_last               5067
_journal_paper_doi               10.1039/b904846d
_journal_year                    2009
_chemical_formula_moiety         'C61 H75 Sb9 Si2 Ti5'
_chemical_formula_sum            'C61 H75 Sb9 Si2 Ti5'
_chemical_formula_weight         2199.64
_space_group_IT_number           102
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4n -2n'
_symmetry_space_group_name_H-M   'P 42 n m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.281(3)
_cell_length_b                   30.281(3)
_cell_length_c                   8.074(5)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      11.49
_cell_measurement_theta_min      3.50
_cell_volume                     7403(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Diamond, Crystal Impact'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            23933
_diffrn_reflns_theta_full        22.51
_diffrn_reflns_theta_max         22.51
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.795
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Stuart & Walker, Acta Cryst A, 1983'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.192
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3468
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0861P)^2^+128.1821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1771
_reflns_number_gt                3126
_reflns_number_total             3468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904846d.txt
_cod_data_source_block           om10
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'refdelF' changed to
'refdelf' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        7403(4)
_cod_database_code               7001552