[N(CH~3~)~4~]~4~H~12~Ge~9~O~26~^.^14H~2~O
Tripathi, Akhilesh; Young Jr., Victor G.; Johnson, Geoffrey M.; Cahill, Christopher L.; Parise, John B.; Acta Crystallographica Section C 55 (1999) 496–499; doi:10.1107/S0108270198014838

data_2008331
_publ_contact_author
; Prof. John B. Parise
  Dept. of Geosciences
  SUNY Stony Brook
  NY 11794-2100
  USA
;
_publ_section_title
;
 [N(CH~3~)~4~]~4~H~12~Ge~9~O~26~^.^14H~2~O
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              496
_journal_page_last               499
_journal_paper_doi               10.1107/S0108270198014838
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[N (C H3)4]4  Ge9 O26 H12  14H2 O'
_chemical_formula_moiety         '(C4 H12 N)4  [Ge9  O14 OH12 ].14(H2 O)'
_chemical_formula_sum            'C16 H88 Ge9 N4 O40'
_chemical_formula_weight         1630.22
_chemical_name_systematic        '(C4 H12 N)4  Ge9 H12 O26  14(H2 O)'
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.6970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.8627(3)
_cell_length_b                   12.6533(3)
_cell_length_c                   16.6278(4)
_cell_measurement_reflns_used    6714
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      1.64
_cell_volume                     2710.02(11)
_computing_cell_refinement       'TWINDX  (Sparks, 1996)'
_computing_data_collection       'SMART  (Siemens, 1994)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens SMART Platform CCD'
_diffrn_measurement_method       '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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18384
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    5.021
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.998
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.002
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.970
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.149
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4763
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.140
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0443P)^2^+4.3643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1096
_refine_ls_wR_factor_ref         0.0998
_reflns_number_observed          3581
_reflns_number_total             4763
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            br1237.cif
_cod_data_source_block           attmage
_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.

'_geom_torsion_publ_flag' value
'No' changed to 'no' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (70 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0443P)^2^+4.3643P] 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^)+(0.0443P)^2^+4.3643P] where P=(Fo^2^+2Fc^2^)/3'.

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

2019-10-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         815.11
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C8 H44 Ge4.50 N2 O20'
_cod_database_code               2008331