First single crystal growth and structural analysis of superconducting layered bismuth oxyselenide; La(O,F)BiSe2
Tanaka, Masashi; Nagao, Masanori; Matsushita, Yoshitaka; Fujioka, Masaya; Denholme, Saleem J.; Yamaguchi, Takahide; Takeya, Hiroyuki; Takano, Yoshihiko; Journal of Solid State Chemistry 219 (2014) 168–172; doi:10.1016/j.jssc.2014.07.026

data_1562265
_publ_section_title
;
 First single crystal growth and structural analysis of superconducting
 layered bismuth oxyselenide; La(O,F)BiSe2
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              168
_journal_page_last               172
_journal_paper_doi               10.1016/j.jssc.2014.07.026
_journal_volume                  219
_journal_year                    2014
_chemical_formula_moiety         'Bi1.98 F0.36 La2.02 O1.64 Se4'
_chemical_formula_sum            'Bi1.98 F0.36 La2.02 O1.64 Se4'
_chemical_formula_weight         1043.29
_space_group_crystal_system      tetragonal
_space_group_IT_number           129
_space_group_name_Hall           '-P 4a 2a'
_space_group_name_H-M_alt        'P 4/n m m :2'
_atom_sites_solution_hydrogens   .
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   4.1408(2)
_cell_length_b                   4.1408(2)
_cell_length_c                   14.1096(6)
_cell_measurement_reflns_used    8879
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      46.18
_cell_measurement_theta_min      2.89
_cell_volume                     241.926(19)
_computing_cell_refinement       'CrystalClear (Rigaku, 1997--2012)'
_computing_data_collection       'CrystalClear (Rigaku, 1997--2012)'
_computing_data_reduction        'CrystalClear (Rigaku, 1997--2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      160(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device
;
Rigaku AFC11 Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9173
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         46.242
_diffrn_reflns_theta_min         5.131
_exptl_absorpt_coefficient_mu    59.900
_exptl_absorpt_correction_T_max  0.0769
_exptl_absorpt_correction_T_min  0.0109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear (Rigaku, 1997--2002)
;
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    7.174
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_refine_diff_density_max         4.923
_refine_diff_density_min         -2.039
_refine_diff_density_rms         0.476
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         700
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+0.9988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                694
_reflns_number_total             700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2014-219-168.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        241.93(3)
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               1562265
_shelx_estimated_absorpt_t_min   0.066
_shelx_estimated_absorpt_t_max   0.267
_shelxl_version_number           2014-3
_shelx_res_checksum              85527
_shelx_hkl_checksum              65352