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_4342326
_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            'Ca In1.67 Na5 Sb4'
_chemical_formula_weight         833.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           26
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2'
_symmetry_space_group_name_H-M   'P m c 21'
_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                90.00
_cell_formula_units_Z            1
_cell_length_a                   4.7609(5)
_cell_length_b                   9.1680(10)
_cell_length_c                   7.8898(8)
_cell_measurement_reflns_used    1518
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      3.41
_cell_volume                     344.37(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4863
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    10.963
_exptl_absorpt_correction_T_max  0.7636
_exptl_absorpt_correction_T_min  0.3705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            grey-silver
_exptl_crystal_density_diffrn    4.020
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             361
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.045
_refine_diff_density_min         -1.884
_refine_diff_density_rms         0.235
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         1058
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+2.0041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0637
_reflns_number_gt                992
_reflns_number_total             1058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502822v_si_002.cif
_cod_data_source_block           III
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      Pmc2(1)
_cod_database_code               4342326