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_4318334
_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_moiety         Bi2Nb2(sal)4(Hsal)4(OiPr)4
_chemical_formula_sum            'C68 H64 Bi2 Nb2 O28'
_chemical_formula_weight         1932.97
_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                65.83(3)
_cell_angle_beta                 72.49(3)
_cell_angle_gamma                85.07(3)
_cell_formula_units_Z            1
_cell_length_a                   11.231(2)
_cell_length_b                   12.997(3)
_cell_length_c                   13.615(3)
_cell_measurement_reflns_used    5664
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      46.582
_cell_measurement_theta_min      4.315
_cell_volume                     1727.5(8)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7551
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    5.487
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.456419
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.33
_refine_diff_density_max         2.499
_refine_diff_density_min         -1.743
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         4899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                4482
_reflns_number_total             4899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255454_s2_2.cif
_cod_data_source_block           compound1a
_cod_original_cell_volume        1727.5(6)
_cod_database_code               4318334