Molecular Precursors for Ferroelectric Materials: Synthesis and Characterization of Bi2M2(μ-O)(sal)4(Hsal)4(OEt)2 and BiM4(μ-O)4(sal)4(Hsal)3(OiPr)4 (sal = O2CC6H4O, Hsal = O2CC6H4OH) (M = Nb, Ta)
John H. Thurston; Kenton H. Whitmire; Inorganic Chemistry 42 (2003) 2014–2023; doi:10.1021/ic026108s

data_4313395
_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
;
 Molecular Precursors for Ferroelectric Materials: Synthesis and
 Characterization of Bi2M2(\m-O)(sal)4(Hsal)4(OEt)2 and
 BiM4(\m-O)4(sal)4(Hsal)3(OiPr)4 (sal = O2CC6H4O, Hsal = O2CC6H4OH) (M =
 Nb, Ta)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2014
_journal_page_last               2023
_journal_paper_doi               10.1021/ic026108s
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C81 H66 Bi2 Mg0 Nb2 O28'
_chemical_formula_weight         2091.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 100.18(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.038(5)
_cell_length_b                   15.004(3)
_cell_length_c                   23.183(5)
_cell_measurement_reflns_used    4268
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.515
_cell_measurement_theta_min      4.591
_cell_volume                     7887(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker AXS SMART 1k, CCD'
_diffrn_measurement_method       '2 theta, omega'
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0299
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16759
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    4.815
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.837566
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             4096
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.455
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         5672
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0725P)^2^+28.7272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                4731
_reflns_number_total             5672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic026108ssi20021216_054950_2.cif
_cod_data_source_block           compound_1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        7888(3)
_cod_database_code               4313395