Two-Dimensional Metal NaCu6.3Sb3 and Solid-State Transformations of Sodium Copper Antimonides
Owens-Baird, Bryan; Lee, Shannon; Kovnir, Kirill; Dalton Trans.  (2017) –; doi:10.1039/C7DT02329D

data_7044014
_publ_section_title
;
 Two-Dimensional Metal NaCu6.3Sb3 and Solid-State Transformations of
 Sodium Copper Antimonides
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02329D
_journal_year                    2017
_chemical_formula_sum            'Cu6.35 Na Sb3'
_chemical_formula_weight         791.40
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   4.2166(2)
_cell_length_b                   4.2166(2)
_cell_length_c                   24.0406(10)
_cell_measurement_reflns_used    5900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.480
_cell_measurement_theta_min      5.088
_cell_volume                     370.17(3)
_computing_cell_refinement       'SAINT (8.34a) (Bruker, 2013)'
_computing_data_collection       'Apex3 (2016.9) (Bruker, 2016)'
_computing_data_reduction        'SAINT (8.34a) (Bruker, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Photon100 CMOS'
_diffrn_radiation_monochromator  Mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            8175
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.479
_diffrn_reflns_theta_min         5.088
_diffrn_source                   Micro-source
_exptl_absorpt_coefficient_mu    28.551
_exptl_absorpt_correction_type   'Empirical, SADABS (multi-scan)'
_exptl_absorpt_process_details   'SADABS 2016/2 (Sheldrick, 2016)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    7.100
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.3907
_refine_diff_density_max         1.935
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.297
_refine_ls_extinction_coef       0.0122(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     23
_refine_ls_number_reflns         265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0218
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+2.9509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                263
_reflns_number_total             265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02329d1.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        370.17(4)
_cod_database_code               7044014
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.240
_shelx_estimated_absorpt_t_max   0.763
_shelx_res_checksum              32072
_shelx_hkl_checksum              37612