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_4318335
_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            'C68 H64 Bi2 O28 Ta2'
_chemical_formula_weight         2109.05
_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                66.06(3)
_cell_angle_beta                 71.89(3)
_cell_angle_gamma                84.27(3)
_cell_formula_units_Z            1
_cell_length_a                   11.361(2)
_cell_length_b                   13.090(3)
_cell_length_c                   13.675(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1765.8(8)
_computing_cell_refinement       'SHELXTL 5.10 (Bruker AXS,1997)'
_computing_data_collection       'SHELXTL 5.10 (Bruker AXS,1997)'
_computing_data_reduction        'SHELXTL 5.10 (Bruker AXS,1997)'
_computing_molecular_graphics    'SHELXTL 5.10 (Bruker AXS,1997)'
_computing_publication_material  'SHELXTL 5.10 (Bruker AXS,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius kappa diffractometer'
_diffrn_measurement_method       Denzo
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14424
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    8.140
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Square Prism'
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.568
_refine_diff_density_min         -3.292
_refine_diff_density_rms         0.614
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0937P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1536
_reflns_number_gt                6307
_reflns_number_total             8146
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0255454_s2_3.cif
_cod_data_source_block           compound2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1765.9(6)
_cod_database_code               4318335