Tetrakis(tetrabutylammonium) tetrakis[(<i>p</i>-cyanophenyl)trioxoarsonato]tetratriacontaoxododecamolybdate(4 ‒)
Johnson, Bret J.S.; Buss, Carrie E.; Young Jr., Victor G.; Stein, Andreas; Acta Crystallographica Section C 55 (1999) 549–551; doi:10.1107/S0108270198017636

data_2008341
_publ_section_title
;Tetrakis(tetrabutylammonium)
 tetrakis[(<i>p</i>-cyanophenyl)trioxoarsonato]tetratriacontaoxododecamolybdate(4
 --)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              549
_journal_page_last               551
_journal_paper_doi               10.1107/S0108270198017636
_journal_volume                  55
_journal_year                    1999
_chemical_formula_analytical     'C92 H160 As4 Mo12 N8 O46'
_chemical_formula_iupac          '(C16 H36 N)4 [{As(C7 H4 N)}4 Mo12 O46]'
_chemical_formula_moiety         '4C16 H36 N, C28 H16 As4 Mo12 N4 O46'
_chemical_formula_structural     'C92 H160 As4 Mo12 N8 O46'
_chemical_formula_sum            'C92 H160 As4 Mo12 N8 O46'
_chemical_formula_weight         3565.24
_chemical_name_common
'dodecamolybodtetrakis(p--cyanophenyl)arsonate tetrabutylammonium salt'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.1640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.9834(6)
_cell_length_b                   16.8216(4)
_cell_length_c                   28.1000(4)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.43
_cell_volume                     12754.6(5)
_computing_cell_refinement       'SAINT  (Siemens, 1994b)'
_computing_data_collection       'SMART  (Siemens, 1994b)'
_computing_data_reduction        'SHELXTL  (Siemens, 1994a)'
_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       multi-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0744
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31322
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.248
_exptl_absorpt_correction_T_max  0.763
_exptl_absorpt_correction_T_min  0.445
_exptl_absorpt_correction_type   'empirical (SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       Block
_exptl_crystal_F_000             7088
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.947
_refine_diff_density_min         -1.051
_refine_ls_extinction_coef       'not measured'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.992
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         11061
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.158
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_obs          0.0463
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0588P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1156
_refine_ls_wR_factor_obs         0.1024
_reflns_number_observed          7586
_reflns_number_total             11061
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            da1056.cif
_cod_data_source_block           98135
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 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^)+(0.0588P)^2^] 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^)+(0.0588P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2008341
_cod_database_fobs_code          2008341