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_7001553
_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         'C57 H66 N3 Sb4 Ti3, 2.5(C6 H6)'
_chemical_formula_sum            'C72 H81 N3 Sb4 Ti3'
_chemical_formula_weight         1619.10
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.2155(14)
_cell_length_b                   15.2155(14)
_cell_length_c                   50.767(6)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.498
_cell_measurement_theta_min      2.401
_cell_volume                     10178.5(18)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Diamond, Crystal Impact'
_computing_publication_material  'Siemens 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 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       65
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6156
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        'random variation +/-2.0'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.945
_exptl_absorpt_correction_T_max  0.8293
_exptl_absorpt_correction_T_min  0.3882
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Stuart & Walker, Acta Cryst A, 1983'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.161
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.00015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5038
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+32.9537P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                4220
_reflns_number_total             5038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904846d.txt
_cod_data_source_block           om20
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Rhombohedral' changed to 'rhombohedral'
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_sg_symbol_H-M      'R -3'
_cod_database_code               7001553