Crystal structures of η''-Cu<sub>3+x</sub>Si and η'''-Cu<sub>3+x</sub>Si.
Corrêa, Cinthia Antunes; Perez, Olivier; Kopeček, Jaromír; Brázda, Petr; Klementová, Mariana; Palatinus, Lukáš; Acta crystallographica Section B, Structural science, crystal engineering and materials 73 (2017) 767–774; doi:10.1107/S2052520617006163

data_2311716
_publ_section_title
;
 Crystal structures of \h''-Cu<sub>3+x</sub>Si and
 \h'''-Cu<sub>3+x</sub>Si.
;
_journal_coeditor_code           BP5097
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              767
_journal_page_last               774
_journal_paper_doi               10.1107/S2052520617006163
_journal_volume                  73
_journal_year                    2017
_chemical_formula_sum            'Cu3.313 Si'
_chemical_formula_weight         238.6
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            192
_cell_length_a                   16.2448(4)
_cell_length_b                   16.2448(4)
_cell_length_c                   44.017(8)
_cell_measurement_reflns_used    1361
_cell_measurement_temperature    743
_cell_measurement_theta_max      28.9115
_cell_measurement_theta_min      5.5596
_cell_volume                     10059.6(19)
_computing_cell_refinement       'Bruker SAINT, v. 8.34A'
_computing_data_collection       'Bruker SAINT, v. 8.34A'
_computing_data_reduction
'Bruker SAINT, v. 8.34A, Sadabs (Sheldrick 1996)'
_computing_structure_refinement  'Jana2006 (Petricek et al., 2014)'
_computing_structure_solution    'Supeflip (Palatinus and Chapuis, 2007)'
_diffrn_ambient_temperature      743
_diffrn_measured_fraction_theta_full 0.52
_diffrn_measured_fraction_theta_max 0.49
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'KappaCCD (Bruker-Nonius)'
_diffrn_measurement_method       phi-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2402
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            25292
_diffrn_reflns_theta_full        28.89
_diffrn_reflns_theta_max         30.39
_diffrn_reflns_theta_min         2.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    33.346
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (J.Appl.Cryst.48 (2015). )'
_exptl_crystal_colour            'metallic gray'
_exptl_crystal_density_diffrn    7.5625
_exptl_crystal_description       irregular
_exptl_crystal_F_000             21132
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.088
_refine_diff_density_max         13.76
_refine_diff_density_min         -14.71
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.35
_refine_ls_hydrogen_treatment    undef
_refine_ls_number_constraints    282
_refine_ls_number_parameters     6
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.5448
_refine_ls_R_factor_gt           0.1503
_refine_ls_shift/su_max          0.0027
_refine_ls_shift/su_mean         0.0007
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F)+0.0001F^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1468
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                624
_reflns_number_total             4996
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            bp5097sup1.cif
_cod_data_source_block           eta1
_cod_original_cell_volume        10060(2)
_cod_original_sg_symbol_Hall     '-P 3;-2c'
_cod_original_formula_sum        'Cu3.313 Si1'
_cod_database_code               2311716