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_2104375
_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            'Al12827.56 Cu1244.05 Ta9063'
_chemical_formula_weight         2065084.38
_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                   71.490(4)
_cell_length_b                   71.490(4)
_cell_length_c                   71.490(4)
_cell_measurement_reflns_used    106757
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.44
_cell_measurement_theta_min      1.24
_cell_volume                     365373(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 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'PILATUS 6M pixel detector'
_diffrn_measurement_method       \f-scans
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_source         undulator
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.70850
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       102
_diffrn_reflns_limit_h_min       -102
_diffrn_reflns_limit_k_max       101
_diffrn_reflns_limit_k_min       -101
_diffrn_reflns_limit_l_max       99
_diffrn_reflns_limit_l_min       -99
_diffrn_reflns_number            1759829
_diffrn_reflns_theta_full        30.44
_diffrn_reflns_theta_max         30.44
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    70.037
_exptl_absorpt_correction_T_max  0.7209
_exptl_absorpt_correction_T_min  0.5410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            'metallic light grey'
_exptl_crystal_density_diffrn    9.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             864435
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         6.772
_refine_diff_density_min         -4.385
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.499(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1393
_refine_ls_number_reflns         48023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0237
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+32396.1992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                47991
_reflns_number_total             48023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sn5082.cif
_cod_data_source_block           act71
_cod_original_cell_volume        36537E1(4)
_cod_database_code               2104375
_cod_database_fobs_code          2104375