The closo-Ge52- Anion: Synthesis, Crystal Structure, and Raman Spectrum of (2,2,2-crypt-K+)2Ge52-.THF
Janette Campbell; Gary J. Schrobilgen; Inorganic Chemistry 36 (1997) 4078–4081; doi:10.1021/ic970191f

data_4323565
_publ_contact_author
;
    Prof. Gary J. Schrobilgen
    Department of Chemistry
    McMaster University
    Hamilton, Ontario
    L8S 4M1
;
_publ_contact_author_email       schrobil@mcmaster.ca
_publ_contact_author_fax         905-522-2509
_publ_contact_author_phone       '905-525-9140 ext. 22537 or 23305'
_publ_section_title
;
 The closo-Ge52- Anion: Synthesis, Crystal Structure, and Raman Spectrum
 of (2,2,2-crypt-K+)2Ge52-.THF
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4078
_journal_page_last               4081
_journal_paper_doi               10.1021/ic970191f
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C40 H80 Ge5 K2 N4 O13'
_chemical_formula_weight         1266.23
_chemical_name_systematic
; 
 Bis[4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane-
 potassium(+1)] closo-pentagermanium(2-) tetrahydrofuran
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   calculated
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                62.1630(10)
_cell_angle_beta                 67.7760(10)
_cell_angle_gamma                84.1870(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9657(4)
_cell_length_b                   12.1750(5)
_cell_length_c                   12.9142(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1405.37(10)
_computing_cell_refinement       'Siemens SMART 1K CCD Area Detector Package'
_computing_data_collection       'Siemens SMART 1K CCD Area Detector Package'
_computing_data_reduction        'Siemens SMART 1K CCD Area Detector Package'
_computing_molecular_graphics    'SHELXTL PLUS (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL PLUS (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXTL PLUS (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL PLUS (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device
;
 P4 Siemens diffractometer, equipped with a Siemens SMART 1K CCD Area 
 Detector
;
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20545
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        none
_diffrn_standards_number         'not applicable'
_exptl_absorpt_coefficient_mu    2.847
_exptl_absorpt_correction_type   'redundant reflections'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             650
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.412(10)
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.017
_refine_ls_goodness_of_fit_obs   1.036
_refine_ls_hydrogen_treatment
;
 riding on parent C atom with U(iso) = 1.2 x U(eq) of the parent atom
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         11288
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.017
_refine_ls_restrained_S_obs      1.036
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_obs          0.0432
_refine_ls_shift/esd_max         0.031
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.4889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1187
_refine_ls_wR_factor_obs         0.1068
_reflns_number_observed          8898
_reflns_number_total             11288
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970191f.cif
_cod_data_source_block           ge5
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.4889P] 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^)+(0.0620P)^2^+0.4889P] 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        1405.37(9)
_cod_database_code               4323565