Deltahedral Clusters in Neat Solids: Synthesis and Structure of the Zintl Phase Cs4Pb9 with Discrete Pb94- Clusters
Evgeny Todorov; Slavi C. Sevov; Inorganic Chemistry 37 (1998) 3889–3891; doi:10.1021/ic980266v

data_4322916
_publ_section_title
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 Deltahedral Clusters in Neat Solids: Synthesis and Structure of the Zintl
 Phase Cs4Pb9 with Discrete Pb94- Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3889
_journal_page_last               3891
_journal_paper_doi               10.1021/ic980266v
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'Cs4 Pb9'
_chemical_formula_weight         2396.35
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.17(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.042(5)
_cell_length_b                   14.781(8)
_cell_length_c                   15.863(8)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.55
_cell_measurement_theta_min      5.85
_cell_volume                     2318(2)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        SDP_Package_(Enraf-Nonius,_1985)
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  'SHELXTL (Siemens, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       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_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.3028
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4061
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.24
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    71.284
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.099
_exptl_absorpt_correction_type   xabs
_exptl_crystal_colour            gray-metallic
_exptl_crystal_density_diffrn    6.868
_exptl_crystal_description       shapeless
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.986
_refine_diff_density_min         -3.875
_refine_diff_density_rms         0.964
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.120
_refine_ls_goodness_of_fit_obs   1.262
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         3497
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.138
_refine_ls_restrained_S_obs      1.262
_refine_ls_R_factor_all          0.1747
_refine_ls_R_factor_obs          0.0989
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2607
_refine_ls_wR_factor_obs         0.2145
_reflns_number_observed          2226
_reflns_number_total             4061
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980266v.cif
_cod_data_source_block           Cs4Pb9
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2317.6(20)
_cod_database_code               4322916