Heterobimetallic Bi(III)-Ti(IV) Coordination Complexes: Synthesis and Solid-State Structures of BiTi4(sal)6(μ-OiPr)3(OiPr)4, and the Cyclic Isomers Bi4Ti4(sal)10(μ-OiPr)4(OiPr)4 and Bi8Ti8(sal)20(μ-OiPr)8(OiPr)8
John H. Thurston; Arvind Kumar; Cristina Hofmann; Kenton H. Whitmire; Inorganic Chemistry 43 (2004) 8427–8436; doi:10.1021/ic049061e

data_4312253
_publ_section_title
;
 Heterobimetallic Bi(III)-Ti(IV) Coordination Complexes: Synthesis and
 Solid-State Structures of BiTi4(sal)6(\m-OiPr)3(OiPr)4, and the Cyclic
 Isomers Bi4Ti4(sal)10(\m-OiPr)4(OiPr)4 and Bi8Ti8(sal)20(\m-OiPr)8(OiPr)8
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8427
_journal_page_last               8436
_journal_paper_doi               10.1021/ic049061e
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C63 H73 Bi O25 Ti4'
_chemical_formula_weight         1630.79
_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                98.62(3)
_cell_angle_beta                 101.38(3)
_cell_angle_gamma                113.55(3)
_cell_formula_units_Z            2
_cell_length_a                   12.130(2)
_cell_length_b                   15.073(3)
_cell_length_c                   23.789(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3780.1(19)
_computing_cell_refinement       'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_data_collection       'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_data_reduction        'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker SMART 1k, CCD'
_diffrn_measurement_method       '2theta, omega'
_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  0.0638
_diffrn_reflns_av_sigmaI/netI    0.1663
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16174
_diffrn_reflns_theta_full        23.34
_diffrn_reflns_theta_max         23.34
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    2.795
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.860929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.329
_refine_diff_density_min         -1.422
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         10620
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1242P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1876
_refine_ls_wR_factor_ref         0.2166
_reflns_number_gt                5993
_reflns_number_total             10620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049061esi20040715_041825.cif
_cod_data_source_block           5
_cod_original_cell_volume        3779.9(13)
_cod_database_code               4312253