Large, larger, largest ‒ a family of cluster-based tantalum copper aluminides with giant unit cells. I. Structure solution and refinement
Weber, Thomas; Dshemuchadse, Julia; Kobas, Miroslav; Conrad, Matthias; Harbrecht, Bernd; Steurer, Walter; Acta Crystallographica Section B 65 (2009) 308–317; doi:10.1107/S0108768109014001

data_2104374
_publ_section_title
;
 Large, larger, largest -- a family of cluster-based tantalum copper
 aluminides with giant unit cells. I. Structure solution and refinement
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              308
_journal_page_last               317
_journal_paper_doi               10.1107/S0108768109014001
_journal_volume                  65
_journal_year                    2009
_chemical_formula_sum            'Al3339.8 Cu231.95 Ta2336'
_chemical_formula_weight         527545.12
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           216
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F -4 2 3'
_symmetry_space_group_name_H-M   'F -4 3 m'
_atom_sites_solution_primary     'charge flipping'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   45.3760(10)
_cell_length_b                   45.3760(10)
_cell_length_c                   45.3760(10)
_cell_measurement_reflns_used    81399
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      2.77
_cell_volume                     93428(4)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       \f-scans
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         'bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69260
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -59
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            157953
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    70.113
_exptl_absorpt_correction_T_max  0.4194
_exptl_absorpt_correction_T_min  0.2731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            'metallic light grey'
_exptl_crystal_density_diffrn    9.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             220672
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.335
_refine_diff_density_min         -2.793
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 5798 Friedel pairs'
_refine_ls_abs_structure_Flack   0.376(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         12010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0186
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+3145.4670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                11816
_reflns_number_total             12010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sn5082.cif
_cod_data_source_block           act45
_cod_original_formula_sum        'Al3339.80 Cu231.95 Ta2336'
_cod_database_code               2104374
_cod_database_fobs_code          2104374