Caught in Action. The Late Rare Earths Thulium and Lutetium Substituting Aluminum Atoms in the Structure of Ca14AlBi11
Baranets, Sviatoslav; Bobev, Svilen; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11026

data_4135472
_publ_section_title
;
 Caught in Action. The Late Rare Earths Thulium and Lutetium Substituting
 Aluminum Atoms in the Structure of Ca14AlBi11
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11026
_journal_year                    2020
_chemical_formula_moiety         'Al0.855 Bi11 Ca13.952 Lu0.193'
_chemical_formula_sum            'Al0.86 Bi11 Ca13.95 Lu0.19'
_chemical_formula_weight         2914.96
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.026(2)
_cell_length_b                   17.026(2)
_cell_length_c                   22.735(3)
_cell_measurement_reflns_used    3870
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      3.38
_cell_volume                     6590.5(14)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            41324
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.667
_diffrn_reflns_theta_min         2.392
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    61.268
_exptl_absorpt_correction_T_max  0.0497
_exptl_absorpt_correction_T_min  0.0140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1606 before and 0.0836 after correction. The Ratio of minimum to maximum transmission is 0.2817. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    5.876
_exptl_crystal_description       block
_exptl_crystal_F_000             9735
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.114
_refine_diff_density_max         1.481
_refine_diff_density_min         -1.772
_refine_diff_density_rms         0.365
_refine_ls_extinction_coef       0.000012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         2340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+145.6848P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1969
_reflns_number_total             2340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11026_si_001.cif
_cod_data_source_block           mo_svib1486_0m
_cod_original_cell_volume        6590.4(18)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               4135472
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.054
_shelx_estimated_absorpt_t_min   0.048
_olex2_refinement_description
;
1. Shared sites
{Al1, Lu2}
{Ca1, Lu1}
2. Uiso/Uaniso restraints and constraints
Uanis(Al1) = Uanis(Lu2)
Uanis(Ca1) = Uanis(Lu1)
3. Others
 Sof(Lu2)=0.25*(1-FVAR(2))
 Sof(Al1)=0.25*FVAR(2)
 Sof(Lu1)=1-FVAR(2)
 Sof(Ca1)=FVAR(2)
;
_shelx_res_checksum              49047
_shelx_hkl_checksum              54810
_olex2_submission_special_instructions 'No special instructions were received'