Na3PbII[B(O3POH)4]: An Alkali-Metal Lead Borophosphate with Heterocubane-like Units Na3PbO4
Stefan Hoffmann; Harold B. Tanh Jeazet; Prashanth W. Menezes; Yurii Prots; Rüdiger Kniep; Inorganic Chemistry 47 (2008) 10193–10195; doi:10.1021/ic801334g

data_4306514
_publ_contact_author_address
;
Max-Planck Institut f\"ur Chemische Physik fester Stoffe
N\"othnitzer Str. 40
D-01187 Dresden
Germany
;
_publ_contact_author_email       kniep@cpfs.mpg.de
_publ_contact_author_fax         '+49 (0)351 4646 3000'
_publ_contact_author_name        'Kniep, R\"udiger'
_publ_contact_author_phone       '+49 (0)351 4646 3002'
_publ_section_title
;
Na3PbII[B(O3POH)4]: An Alkali-Metal Lead Borophosphate with
Heterocubane-like Units Na3PbO4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10193
_journal_page_last               10195
_journal_paper_doi               10.1021/ic801334g
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'B Na3 O16 P4 Pb'
_chemical_formula_weight         666.85
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-06-24T16:22:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.9182(8)
_cell_length_b                   6.9182(8)
_cell_length_c                   27.309(3)
_cell_measurement_reflns_used    3748
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      33.4543
_cell_measurement_theta_min      1.4906
_cell_volume                     1307.0(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 91.9000
_diffrn_measured_fraction_theta_max 33.4543
_diffrn_measurement_details
;
scan:
 Number of images: 400
            Slice: -120.0000 - 120.0000
      Image width: 0.6000
         Exp time: 30.0000
    Rotation axis: Phi
            Omega: 0.0000
              Chi: 0.0000
              Phi: 0.0000
              XTD: 42.0500
           2theta: -25.0000
scan:
 Number of images: 95
            Slice: -38.0000 - 19.0000
      Image width: 0.6000
         Exp time: 30.0000
    Rotation axis: Omega
            Omega: 0.0000
              Chi: -90.0000
              Phi: 5.0000
              XTD: 42.0500
           2theta: -25.0000

;
_diffrn_measurement_device_details
;
AFC7: Eulerian 3-circle
;
_diffrn_measurement_device_type  'Rigaku AFC7'
_diffrn_measurement_method       oscillation
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.1370
_diffrn_orient_matrix_UB_12      -0.0095
_diffrn_orient_matrix_UB_13      -0.0451
_diffrn_orient_matrix_UB_21      0.0108
_diffrn_orient_matrix_UB_22      0.1441
_diffrn_orient_matrix_UB_23      0.0024
_diffrn_orient_matrix_UB_31      0.0113
_diffrn_orient_matrix_UB_32      -0.0014
_diffrn_orient_matrix_UB_33      0.0348
_diffrn_radiation_detector       'Mercury CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            4613
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        33.4543
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           48.0000
_diffrn_source_power             2.4000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    13.592
_exptl_absorpt_correction_T_max  0.542
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    3.389
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.704
_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   1.128
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+11.8233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.086
_reflns_number_gt                852
_reflns_number_total             877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801334g_si_002.cif
_cod_data_source_block           hta_0114a
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4306514