Lead Rare-Earth Oxyhalides: Syntheses and Characterization of Pb6LaO7X (X = Cl, Br)
Oleg I. Siidra; Sergey V. Krivovichev; Thomas Armbruster; Wulf Depmeier; Inorganic Chemistry 46 (2007) 1523–1525; doi:10.1021/ic062191y

data_4307697
_publ_section_title
;
Lead Rare-Earth Oxyhalides: Syntheses and Characterization of Pb6LaO7X (X
= Cl, Br)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1523
_journal_page_last               1525
_journal_paper_doi               10.1021/ic062191y
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         Pb6LaO7Br
_chemical_formula_sum            'Br0.4 La0.4 O2.8 Pb2.4'
_chemical_formula_weight         629.58
_chemical_melting_point          ?
_chemical_name_common            'lead lanthanum oxide bromide'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5896(17)
_cell_length_b                   16.146(3)
_cell_length_c                   8.1459(15)
_cell_measurement_reflns_used    750
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.502
_cell_measurement_theta_min      4.940
_cell_volume                     1261.3(4)
_computing_cell_refinement       'SMART (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'Atoms 5.1 (Dowty, 2000)'
_computing_publication_material  'WINGX (Farrugia, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1087
_diffrn_reflns_av_sigmaI/netI    0.0807
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3537
_diffrn_reflns_theta_full        27.75
_diffrn_reflns_theta_max         27.75
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    86.273
_exptl_absorpt_correction_T_max  0.45071
_exptl_absorpt_correction_T_min  0.08360
_exptl_absorpt_correction_type   'semi-empirical (XPREP, Bruker 2003)'
_exptl_absorpt_process_details   'as ellipsoid'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    8.289
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.484
_refine_diff_density_min         -2.224
_refine_diff_density_rms         0.722
_refine_ls_extinction_coef       0.000082(12)
_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   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         810
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                569
_reflns_number_total             810
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062191ysi20061228_055939.cif
_cod_data_source_block           cmcm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'unknown' was changed to '?' - the
value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1261.2(4)
_cod_original_formula_sum        'Br0.40 La0.40 O2.80 Pb2.40'
_cod_database_code               4307697