Syntheses and Structures of Distibene Complexes of Tungsten and Titanium: [W(CO)5{(2,6-Mes2C6H3)2Sb2}] (Mes = 2,4,6-Me3C6H2) and [Cp2Ti{(2,6-Mes2C6H3)2Sb2)}]
Breunig, Hans J.; Borrmann, Tobias; Lork, Enno; Raţ, Ciprian I.; Rosenthal, Uwe; Organometallics 26 (2007) 5364–; doi:10.1021/om700681w

data_4073852
_publ_section_title
;
 Syntheses and Structures of Distibene Complexes of Tungsten and
 Titanium:&#x00A0; [W(CO)5{(2,6-Mes2C6H3)2Sb2}] (Mes = 2,4,6-Me3C6H2) and
 [Cp2Ti{(2,6-Mes2C6H3)2Sb2)}]
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5364
_journal_paper_doi               10.1021/om700681w
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H60 Sb2 Ti, 1.5(C6 D6)'
_chemical_formula_sum            'C67 H60 D9 Sb2 Ti'
_chemical_formula_weight         1174.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-03-23T12:58:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                97.060(10)
_cell_angle_beta                 93.690(10)
_cell_angle_gamma                109.120(10)
_cell_formula_units_Z            2
_cell_length_a                   11.2720(10)
_cell_length_b                   12.836(2)
_cell_length_c                   20.263(2)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.974
_cell_measurement_theta_min      4.559
_cell_measurement_wavelength     0.71073
_cell_volume                     2731.9(6)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14678
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    1.165
_exptl_absorpt_correction_T_max  0.8446
_exptl_absorpt_correction_T_min  0.5935
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1190
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         12549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+1.5883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.088
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                8969
_reflns_number_total             12549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700681w-file009.cif
_cod_data_source_block           cr10
_cod_database_code               4073852