Synthesis and Characterization of Transition-Metal Zintl Phases: Cs24Nb2In12As18 and Cs13Nb2In6As10 with Isolated Complex Anions
Franck Gascoin; Slavi C. Sevov; Inorganic Chemistry 42 (2003) 8567–8571; doi:10.1021/ic034680t

data_4312690
_publ_section_title
;
 Synthesis and Characterization of Transition-Metal Zintl Phases:
 Cs24Nb2In12As18 and Cs13Nb2In6As10 with Isolated Complex Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8567
_journal_page_last               8571
_journal_paper_doi               10.1021/ic034680t
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         cs24nb2in12as18
_chemical_formula_sum            'As18 Cs24 In12 Nb2'
_chemical_formula_weight         6102.06
_chemical_name_common            cs24nb2in12as18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.87(4)
_cell_angle_beta                 87.20(4)
_cell_angle_gamma                63.81(4)
_cell_formula_units_Z            1
_cell_length_a                   9.519(4)
_cell_length_b                   9.540(5)
_cell_length_c                   25.156(13)
_cell_measurement_reflns_used    15043
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.64
_cell_measurement_theta_min      2.38
_cell_volume                     2046.1(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL-V5.1'
_computing_molecular_graphics    'Bruker SHELXTL-V5.1'
_computing_publication_material  'Bruker SHELXTL-V5.1'
_computing_structure_refinement  'Bruker SHELXTL-V5.1'
_computing_structure_solution    'Bruker SHELXTL-V5.1'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17527
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    21.334
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7172
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.952
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.063
_refine_diff_density_max         6.218
_refine_diff_density_min         -2.627
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       0.000069(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         7217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+30.9846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                6465
_reflns_number_total             7217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034680tsi20030929_123318_1.cif
_cod_data_source_block           cs24nb2in12as18
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2046.0(16)
_cod_database_code               4312690