Heterobimetallic Bismuth-Transition Metal Salicylate Complexes as Molecular Precursors for Ferroelectric Materials. Synthesis and Structure of Bi2M2(sal)4(Hsal)4(OR)4 (M = Nb, Ta; R = CH2CH3, CH(CH3)2), Bi2Ti3(sal)8(Hsal)2, and Bi2Ti4(OiPr)(sal)10(Hsal) (sal = O2CC6H4-2-O; Hsal = O2CC6H4-2-OH)
John H. Thurston; Kenton H. Whitmire; Inorganic Chemistry 41 (2002) 4194–4205; doi:10.1021/ic0255454

data_4318336
_publ_contact_author
;
       Kenton H. Whitmire
       Department of Chemistry MS-60
       Rice University
       1600 Main St.
       Houtson Tx. 77005
       United States of America
;
_publ_contact_author_email       whitmir@rice.edu
_publ_contact_author_fax         '713 737 5652'
_publ_contact_author_phone       '713 737 5650'
_publ_section_title
;
 Heterobimetallic Bismuth-Transition Metal Salicylate Complexes as
 Molecular Precursors for Ferroelectric Materials. Synthesis and Structure
 of Bi2M2(sal)4(Hsal)4(OR)4 (M = Nb, Ta; R = CH2CH3, CH(CH3)2),
 Bi2Ti3(sal)8(Hsal)2, and Bi2Ti4(OiPr)(sal)10(Hsal) (sal = O2CC6H4-2-O;
 Hsal = O2CC6H4-2-OH)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4194
_journal_page_last               4205
_journal_paper_doi               10.1021/ic0255454
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C80 H52 Bi2 O35 Ti4'
_chemical_formula_weight         2182.78
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 108.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.143(3)
_cell_length_b                   33.020(7)
_cell_length_c                   19.147(4)
_cell_measurement_reflns_used    2886
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      33.438
_cell_measurement_theta_min      4.329
_cell_volume                     9066(4)
_computing_cell_refinement       'SHELXTL 6.10 (Bruker, 2001)'
_computing_data_collection       'SHELXTL 6.10 (Bruker, 2001)'
_computing_data_reduction        'SHELXTL 6.10 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL 6.10 (Bruker, 2001)'
_computing_publication_material  'SHELXTL 6.10 (Bruker, 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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker AXS SMART 1K CCD'
_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  0.0962
_diffrn_reflns_av_sigmaI/netI    0.2091
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40482
_diffrn_reflns_theta_full        23.36
_diffrn_reflns_theta_max         23.36
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    4.286
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.851223
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedron
_exptl_crystal_F_000             4264
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.933
_refine_diff_density_min         -1.938
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         13023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.853
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                4955
_reflns_number_total             13023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255454_s2_4.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        9066(3)
_cod_database_code               4318336