Crystal structure of catena-{[bis(benzo-15-crown-5)ammonium][silver(I)-tetrakis(m-sulfido)tungstate(VI)], [(C14H20O5)2(NH4)][AgWS4]
Yuan Cao; Guosheng Cheng; Guozhu Shen; Zeitschrift für Kristallographie - New Crystal Structures 227 (2012) 50–; doi:

data_8103296
_publ_section_title
;
 Crystal structure of
 catena-{[bis(benzo-15-crown-5)ammonium][silver(I)-tetrakis(m-sulfido)tungstate(VI)],
 [(C14H20O5)2(NH4)][AgWS4]
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              50
_journal_volume                  227
_journal_year                    2012
_chemical_formula_moiety         '2(C14 H20 O5), Ag S4 W, N'
_chemical_formula_sum            'C28 H40 Ag N O10 S4 W'
_chemical_formula_weight         970.57
_chemical_name_systematic
; 
catena-poly[[bis(benzo-15-crown-5)ammonium]
[silver(I)-di-\m-sulfido-tungstate(VI)(Ag-W)-di-\m-sulfido]]
;
_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'
_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                 92.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.915(3)
_cell_length_b                   11.515(2)
_cell_length_c                   24.758(5)
_cell_measurement_reflns_used    28323
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.45
_cell_volume                     3679.4(13)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0785
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7509
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    3.933
_exptl_absorpt_correction_T_max  0.5068
_exptl_absorpt_correction_T_min  0.3849
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7182
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0590
_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^)+(0.0821P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1642
_reflns_number_gt                5470
_reflns_number_total             7182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-3636.cff
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               8103296