Synthesis and Structure of the Zintl-Phase K4Pb9 Containing Isolated Pb94- Clusters of Two Different Geometries
Virginie Queneau; Slavi C. Sevov; Inorganic Chemistry 37 (1998) 1358–1360; doi:10.1021/ic971225m

data_4322714
_publ_section_title
;
 Synthesis and Structure of the Zintl-Phase K4Pb9 Containing Isolated
 Pb94- Clusters of Two Different Geometries
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1358
_journal_page_last               1360
_journal_paper_doi               10.1021/ic971225m
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'K4 Pb9'
_chemical_formula_weight         2021.11
_chemical_name_systematic
;
 K4Pb9
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.24(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.648(3)
_cell_length_b                   13.243(5)
_cell_length_c                   15.909(8)
_cell_measurement_reflns_used    3283
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      1.32
_cell_volume                     1978.6(14)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1094
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3597
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    77.083
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_type   'SADABS + XABS'
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    6.785
_exptl_crystal_description       'triangular plate'
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.313
_refine_diff_density_min         -3.534
_refine_diff_density_rms         0.616
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.084
_refine_ls_goodness_of_fit_obs   1.200
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         3473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.200
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_obs          0.0700
_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^)+(0.0610P)^2^+9.4728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1551
_refine_ls_wR_factor_obs         0.1370
_reflns_number_observed          2280
_reflns_number_total             3597
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971225m.cif
_cod_data_source_block           K4Pb9
_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^)+(0.0610P)^2^+9.4728P] 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^)+(0.0610P)^2^+9.4728P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322714