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_7054344
_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         '4(C21 H18 N6 O2 Ag), W10 O32, C7 H5 N'
_chemical_formula_sum            'C91 H77 Ag4 N25 O40 W10'
_chemical_formula_weight         4430.76
_chemical_melting_point          ?
_chemical_name_common
;
Tetrakis(dibenzonitriletheobrominesilver(I))decatungstate
benzonitrile
;
_chemical_name_systematic
; 
Tetrakis(dibenzonitriletheobrominesilver(I))di-mu5-oxo-icosa-
mu-oxo-decaoxodecatungstate benzonitrile 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.929(3)
_cell_angle_beta                 93.069(3)
_cell_angle_gamma                110.612(3)
_cell_formula_units_Z            1
_cell_length_a                   10.7971(5)
_cell_length_b                   14.5000(6)
_cell_length_c                   20.1073(8)
_cell_measurement_reflns_used    'not measured'
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      26.94
_cell_measurement_theta_min      1.69
_cell_volume                     2900.5(2)
_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      170(2)
_diffrn_detector_area_resol_mean 'not measured'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'IPDS 2T (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  0.0996
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44202
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.83
_diffrn_reflns_theta_min         1.69
_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    10.616
_exptl_absorpt_correction_T_max  0.5720
_exptl_absorpt_correction_T_min  0.4294
_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            yellow
_exptl_crystal_density_diffrn    2.537
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2046
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.348
_refine_diff_density_min         -2.092
_refine_diff_density_rms         0.224
_refine_ls_extinction_coef       0.00030(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   0.846
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         12299
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.845
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                6727
_reflns_number_total             12299
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            c4nj00172a2.cif
_cod_data_source_block           AGTHWB
_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               7054344