Refinement of the crystal structure of decalanthanum monooxide tetradecaselenide, La~10~OSe~14~, at 153 K
Wu, Li-Bin; Huang, Fu-Qiang; Zeitschrift für Kristallographie - New Crystal Structures 222 (2007) 175–176; doi:

data_8102975
_publ_section_title
;
Refinement of the crystal structure of decalanthanum monooxide 
tetradecaselenide, La~10~OSe~14~, at 153 K
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              175
_journal_page_last               176
_journal_volume                  222
_journal_year                    2007
_chemical_formula_moiety         La10OSe14
_chemical_formula_sum            'La10 O Se14'
_chemical_formula_weight         2510.54
_chemical_name_common            'decalanthanum oxide tetradecaselenide'
_chemical_name_systematic
; 
decalanthanum monooxide tetradecaselenide
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.888(2)
_cell_length_b                   15.888(2)
_cell_length_c                   21.014(3)
_cell_measurement_reflns_used    13747
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.56
_cell_volume                     5304.5(12)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP in SHELXTL'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'omega, 0.3\%'
_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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30381
_diffrn_reflns_theta_full        28.95
_diffrn_reflns_theta_max         28.95
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    34.925
_exptl_absorpt_correction_T_max  0.18017
_exptl_absorpt_correction_T_min  0.03290
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (SHELXTL, Sheldrick, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    6.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8432
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.271
_refine_ls_extinction_coef       0.000113(4)
_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   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1719
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0200
_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^)+(0.0205P)^2^+42.7867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0425
_refine_ls_wR_factor_ref         0.0439
_reflns_number_gt                1557
_reflns_number_total             1719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            409927.cff
_cod_data_source_block           final
_cod_original_cell_volume        5304.4(12)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               8102975