Synthesis and Characterization of Three New Rare-Earth Titanium Oxyselenides: Ln~3.67~Ti~2~O~3~Se~6~ (Ln = Ce, Nd, Sm)
Tougait, Olivier; Ibers, James A.; Chemistry of Materials 12 (2000) 2653–2658; doi:10.1021/cm000203m

data_4000013
_publ_section_title
;
 Synthesis and Characterization of Three New Rare-Earth Titanium
 Oxyselenides: Ln~3.67~Ti~2~O~3~Se~6~ (Ln = Ce, Nd, Sm)
;
_journal_coden_ASTM              CMATEX
_journal_issue                   9
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2653
_journal_page_last               2658
_journal_paper_doi               10.1021/cm000203m
_journal_volume                  12
_journal_year                    2000
_chemical_formula_sum            'O3 Se6 Sm3.67 Ti2'
_chemical_formula_weight         1171.98
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_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                 90.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.961(6)
_cell_length_b                   3.7827(8)
_cell_length_c                   11.128(2)
_cell_measurement_reflns_used    3583
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.997
_cell_measurement_theta_min      2.334
_cell_volume                     1177.0(4)
_computing_cell_refinement       'SMART version 5.054 (Bruker, 1999)'
_computing_data_collection       'SMART version 5.054 (Bruker, 1999)'
_computing_data_reduction        'SAINT-Plus version 6.01 (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5380
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.46
_diffrn_standards_decay_%        <2
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    37.920
_exptl_absorpt_correction_T_max  0.6802
_exptl_absorpt_correction_T_min  0.0887
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (Sheldrick, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    6.614
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2003
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.006
_refine_diff_density_min         -1.796
_refine_diff_density_rms         0.422
_refine_ls_extinction_coef       0.00003(3)
_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   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0253
_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^)+(0.04Fo^2^)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0607
_reflns_number_gt                1412
_reflns_number_total             1589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm000203m.cif
_cod_data_source_block           Sm3.67Ti2O3Se6
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4000013