Asymmetric Cationic Coordination Environments in New Oxide Materials: Synthesis and Characterization of Pb4Te6M10O41 (M = Nb5+ or Ta5+)
Kang Min Ok; P. Shiv Halasyamani; Inorganic Chemistry 43 (2004) 4248–4253; doi:10.1021/ic049534h

data_4311249
_publ_contact_author_address
;
Department of Chemistry
University of Houston
4800 Calhoun
TX 77204-5003 USA
;
_publ_contact_author_email       psh@uh.edu
_publ_contact_author_fax         1(713)7432787
_publ_contact_author_name        'Halasyamani, P. Shiv'
_publ_contact_author_phone       1(713)7433278
_publ_section_title
;
 Asymmetric Cationic Coordination Environments in New Oxide Materials:
 Synthesis and Characterization of Pb4Te6M10O41 (M = Nb5+ or Ta5+)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4248
_journal_page_last               4253
_journal_paper_doi               10.1021/ic049534h
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'Nb10 O41 Pb4 Te6'
_chemical_formula_weight         3179.46
_chemical_name_systematic
;
 Lead Niobium Tellurium Oxide
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 99.630(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.412(3)
_cell_length_b                   20.114(3)
_cell_length_c                   7.5008(10)
_cell_measurement_reflns_used    5755
_cell_measurement_temperature    293.0(2)
_cell_measurement_theta_max      27.760
_cell_measurement_theta_min      2.687
_cell_volume                     3482.4(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293.0(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10860
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    27.475
_exptl_absorpt_correction_T_max  0.414
_exptl_absorpt_correction_T_min  0.223
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'Light Yellow'
_exptl_crystal_density_diffrn    6.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5512
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.143
_refine_diff_density_min         -2.159
_refine_diff_density_rms         0.303
_refine_ls_extinction_coef       0.000484(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+87.5275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0932
_reflns_number_gt                3473
_reflns_number_total             4045
_reflns_threshold_expression     >2\(I)
_cod_data_source_file            ic049534hsi20040412_094927.cif
_cod_data_source_block           ok156
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Psi-scan' changed to
'psi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4311249