A new structure type of RE4B4O11F2: High-pressure synthesis and crystal structure of La4B4O11F2
Haberer, Almut; Kaindl, Reinhard; Oeckler, Oliver; Huppertz, Hubert; Journal of Solid State Chemistry 183 (2010) 1970–1979; doi:10.1016/j.jssc.2010.06.019

data_1563516
_publ_section_title
;
 A new structure type of RE4B4O11F2: High-pressure synthesis and crystal
 structure of La4B4O11F2
;
_journal_issue                   9
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              1970
_journal_page_last               1979
_journal_paper_doi               10.1016/j.jssc.2010.06.019
_journal_volume                  183
_journal_year                    2010
_chemical_formula_moiety         'B4 F2 La4 O11'
_chemical_formula_sum            'B4 F2 La4 O11'
_chemical_formula_weight         812.88
_chemical_name_common            'lanthanum fluoride borate'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.92(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.7813(16)
_cell_length_b                   35.733(7)
_cell_length_c                   7.6572(15)
_cell_measurement_reflns_used    2335
_cell_measurement_temperature    293(2)
_cell_volume                     1946.2(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'enCIFer (Allen et al., 2004) and SHELXL97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       69
_diffrn_reflns_limit_k_min       -69
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            64178
_diffrn_reflns_theta_full        45.40
_diffrn_reflns_theta_max         45.40
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    17.299
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.667
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.776
_refine_diff_density_min         -4.379
_refine_diff_density_rms         0.457
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         15796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0188P)^2^+11.1671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                12135
_reflns_number_total             15796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2010-183-1970.cif
_cod_data_source_block           spherical
_cod_original_cell_volume        1946.3(7)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1563516