Organoamine silver(i) decatungstate structures: remarkable chemoselectivity and the exploration of the intramolecular redox reaction upon thermolysis
Kulikov, Vladislav; Meyer, Gerd; New Journal of Chemistry 38 (2014) 3408–; doi:10.1039/C4NJ00172A

data_7054342
_publ_section_title
;
 Organoamine silver(i) decatungstate structures: remarkable
 chemoselectivity and the exploration of the intramolecular redox reaction
 upon thermolysis
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3408
_journal_paper_doi               10.1039/C4NJ00172A
_journal_volume                  38
_journal_year                    2014
_chemical_formula_moiety         '2(C16 H36 N),2(C21 H15 N3 Ag), W10 O32'
_chemical_formula_sum            'C74 H102 Ag2 N8 O32 W10'
_chemical_formula_weight         3669.89
_chemical_melting_point          ?
_chemical_name_common
;
Bis(n-tetrabutylammonium)bis(tribenzonitrilesilver)decatungstate
;
_chemical_name_systematic
; 
Bis(n-tetrabutylammonium)bis(tribenzonitrilesilver)di-mu5-oxo
-icosa-mu-oxo-decaoxodecatungstate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0555(6)
_cell_length_b                   24.2744(9)
_cell_length_c                   25.2143(12)
_cell_measurement_reflns_used    'not measured'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      'not measured'
_cell_measurement_theta_min      'not measured'
_cell_volume                     9827.0(7)
_computing_cell_refinement       'X-Area, (Stoe, 2001)'
_computing_data_collection       'X-Area, (Stoe, 2001)'
_computing_data_reduction        'X-Area, (Stoe, 2001)'
_computing_molecular_graphics    'Diamond v3.2 (Crystal Impact 2011)'
_computing_publication_material  'Diamond v3.2 (Crystal Impact 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'IPDS II (Stoe & Cie)'
_diffrn_measurement_method       '\w and \f 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  0.0694
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            149947
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         1.615
_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    12.115
_exptl_absorpt_correction_T_max  0.5998
_exptl_absorpt_correction_T_min  0.1930
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
The absorption correction (X-RED; Stoe & Cie, 2001) 
was performed after optimizing the crystal shape 
using X-SHAPE (Stoe & Cie, 1999).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6768
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.546
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.4831
_refine_ls_extinction_coef       0.00078(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         11088
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                8411
_reflns_number_total             11088
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            c4nj00172a2.cif
_cod_data_source_block           AGNBU
_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.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

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 
;
_cod_database_code               7054342