Quaternary Pnictides with Complex, Noncentrosymmetric Structures. Synthesis and Structural Characterization of the New Zintl Phases Na11Ca2Al3Sb8, Na4CaGaSb3, and Na15Ca3In5Sb12.
Wang, Yi; Stoyko, Stanislav; Bobev, Svilen; Inorganic chemistry 54 (2015) 1931–1939; doi:10.1021/ic502822v

data_4342327
_publ_section_title
;
 Quaternary Pnictides with Complex, Noncentrosymmetric Structures.
 Synthesis and Structural Characterization of the New Zintl Phases
 Na11Ca2Al3Sb8, Na4CaGaSb3, and Na15Ca3In5Sb12.
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_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1931
_journal_page_last               1939
_journal_paper_doi               10.1021/ic502822v
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'Al Ca3 Na3 Sb4'
_chemical_formula_weight         703.19
_space_group_IT_number           186
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.0121(5)
_cell_length_b                   10.0121(5)
_cell_length_c                   7.6045(8)
_cell_measurement_reflns_used    852
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.95
_cell_measurement_theta_min      2.35
_cell_volume                     660.16(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1023
_diffrn_reflns_av_sigmaI/netI    0.0605
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9234
_diffrn_reflns_theta_full        29.55
_diffrn_reflns_theta_max         29.55
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    9.369
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                597
_reflns_number_total             722
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502822v_si_003.cif
_cod_data_source_block           test
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 4342324--4342327.cif.
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_cod_original_sg_symbol_H-M      P6(3)mc
_cod_database_code               4342327