Synthesis and Characterization of the "Metallic Salts" A5Pn4 (A = K, Rb, Cs and Pn = As, Sb, Bi) with Isolated Zigzag Tetramers of Pn44- and an Extra Delocalized Electron
Franck Gascoin; Slavi C. Sevov; Inorganic Chemistry 40 (2001) 5177–5181; doi:10.1021/ic0104499

data_4320325
_publ_section_title
;
 Synthesis and Characterization of the "Metallic Salts" A5Pn4 (A = K, Rb,
 Cs and Pn = As, Sb, Bi) with Isolated Zigzag Tetramers of Pn44- and an
 Extra Delocalized Electron
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5177
_journal_page_last               5181
_journal_paper_doi               10.1021/ic0104499
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         K5As4
_chemical_formula_sum            'As4 K5'
_chemical_formula_weight         495.18
_chemical_melting_point          ?
_chemical_name_common            K5As4
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.421(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.592(2)
_cell_length_b                   5.2114(5)
_cell_length_c                   10.383(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16.29
_cell_measurement_theta_min      11.78
_cell_volume                     575.6(2)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        SDS_Package_(Enraf-Nonius,_1985)
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXTL (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Enraf_Nonius_CAD4
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            569
_diffrn_reflns_theta_full        24.93
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         2.14
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    13.249
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6678
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Xabs
_exptl_crystal_colour            'gray, metallic luster'
_exptl_crystal_density_diffrn    2.857
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             454
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.0009(5)
_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   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0422P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0812
_reflns_number_gt                443
_reflns_number_total             569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0104499_1.cif
_cod_data_source_block           K5As4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

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_database_code               4320325