#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/88/2238825.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2238825
loop_
_publ_author_name
'Zhou, Lu-Jun'
'Shi, Hua-Tian'
'Xu, Chao'
'Chen, Qun'
'Zhang, Qian-Feng'
_publ_section_title
;
 catena-Poly[2-methylpyridinium
 [tungstate-di-μ-selenido-silver-di-μ-selenido] 2-methylpyridine
 monosolvate]
;
_journal_coeditor_code           XU5746
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m608
_journal_paper_doi               10.1107/S1600536813028213
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(C6 H8 N) [Ag W Se4], C6 H7 N'
_chemical_formula_moiety         'C6 H8 N +, Ag Se4 W -, C6 H7 N'
_chemical_formula_sum            'C12 H15 Ag N2 Se4 W'
_chemical_formula_weight         794.82
_chemical_name_systematic
;
catena-Poly[2-methylpyridinium
[tungstate-di-μ-selenido-silver-di-μ-selenido] 2-methylpyridine
monosolvate]
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 100.962(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.859(2)
_cell_length_b                   5.9448(15)
_cell_length_c                   19.830(5)
_cell_measurement_reflns_used    1243
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.45
_cell_measurement_theta_min      2.64
_cell_volume                     909.6(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5398
_diffrn_reflns_theta_full        27.42
_diffrn_reflns_theta_max         27.42
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    15.389
_exptl_absorpt_correction_T_max  0.6553
_exptl_absorpt_correction_T_min  0.2061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.902
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.863
_refine_diff_density_min         -1.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         2051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0337
_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/[σ²(Fo²)+(0.0357P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0778
_reflns_number_gt                1565
_reflns_number_total             2051
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5746.cif
_cod_data_source_block           I
_cod_original_cell_volume        909.5(4)
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2238825
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
W W1 0.5000 0.30930(6) 0.7500 0.03027(13) Uani d S 1 2
Ag Ag1 0.5000 0.80929(13) 0.7500 0.0524(2) Uani d S 1 2
Se Se1 0.24423(10) 0.09964(13) 0.72794(4) 0.0417(2) Uani d . 1 1
Se Se2 0.50518(11) 0.51956(12) 0.65078(4) 0.0434(2) Uani d . 1 1
N N1 0.0998(7) 0.3192(10) 0.4854(3) 0.0389(14) Uani d . 1 1
H H1N 0.0423 0.4382 0.4914 0.047 Uiso calc PR 0.50 1
C C1 0.1778(10) 0.1984(14) 0.5389(4) 0.0478(19) Uani d . 1 1
H H1 0.1711 0.2486 0.5828 0.057 Uiso calc R 1 1
C C2 0.2676(11) 0.0041(13) 0.5329(5) 0.053(2) Uani d . 1 1
H H2 0.3163 -0.0786 0.5716 0.064 Uiso calc R 1 1
C C3 0.2838(12) -0.0653(16) 0.4690(5) 0.062(2) Uani d . 1 1
H H3 0.3473 -0.1938 0.4635 0.075 Uiso calc R 1 1
C C4 0.2043(11) 0.0586(15) 0.4116(4) 0.053(2) Uani d . 1 1
H H4 0.2133 0.0114 0.3677 0.064 Uiso calc R 1 1
C C5 0.1125(10) 0.2507(14) 0.4203(4) 0.0447(19) Uani d . 1 1
C C6 0.0282(12) 0.3915(15) 0.3622(4) 0.059(2) Uani d . 1 1
H H6A 0.0500 0.3291 0.3200 0.088 Uiso calc R 1 1
H H6B 0.0741 0.5414 0.3678 0.088 Uiso calc R 1 1
H H6C -0.0945 0.3955 0.3610 0.088 Uiso calc R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
Se1 W1 Se1 . 2_656 115.47(5)
Se1 W1 Se2 . 2_656 106.92(3)
Se1 W1 Se2 2_656 2_656 106.25(3)
Se1 W1 Se2 . . 106.25(3)
Se1 W1 Se2 2_656 . 106.92(3)
Se2 W1 Se2 2_656 . 115.36(4)
Se1 W1 Ag1 . . 122.27(2)
Se1 W1 Ag1 2_656 . 122.27(2)
Se2 W1 Ag1 2_656 . 57.68(2)
Se2 W1 Ag1 . . 57.68(2)
Se1 W1 Ag1 . 1_545 57.73(2)
Se1 W1 Ag1 2_656 1_545 57.73(2)
Se2 W1 Ag1 2_656 1_545 122.32(2)
Se2 W1 Ag1 . 1_545 122.32(2)
Ag1 W1 Ag1 . 1_545 180.0000(10)
Se2 Ag1 Se2 . 2_656 97.84(4)
Se2 Ag1 Se1 . 2_666 115.91(3)
Se2 Ag1 Se1 2_656 2_666 115.35(3)
Se2 Ag1 Se1 . 1_565 115.35(3)
Se2 Ag1 Se1 2_656 1_565 115.91(3)
Se1 Ag1 Se1 2_666 1_565 97.67(5)
Se2 Ag1 W1 . . 48.92(2)
Se2 Ag1 W1 2_656 . 48.92(2)
Se1 Ag1 W1 2_666 . 131.16(2)
Se1 Ag1 W1 1_565 . 131.16(2)
Se2 Ag1 W1 . 1_565 131.08(2)
Se2 Ag1 W1 2_656 1_565 131.08(2)
Se1 Ag1 W1 2_666 1_565 48.84(2)
Se1 Ag1 W1 1_565 1_565 48.84(2)
W1 Ag1 W1 . 1_565 180.0
W1 Se1 Ag1 . 1_545 73.43(3)
W1 Se2 Ag1 . . 73.40(3)
C1 N1 C5 . . 119.0(6)
C1 N1 H1N . . 120.5
C5 N1 H1N . . 120.5
N1 C1 C2 . . 123.5(7)
N1 C1 H1 . . 118.2
C2 C1 H1 . . 118.2
C3 C2 C1 . . 118.5(8)
C3 C2 H2 . . 120.7
C1 C2 H2 . . 120.7
C2 C3 C4 . . 119.4(8)
C2 C3 H3 . . 120.3
C4 C3 H3 . . 120.3
C5 C4 C3 . . 119.8(7)
C5 C4 H4 . . 120.1
C3 C4 H4 . . 120.1
N1 C5 C4 . . 119.7(7)
N1 C5 C6 . . 117.6(7)
C4 C5 C6 . . 122.7(7)
C5 C6 H6A . . 109.5
C5 C6 H6B . . 109.5
H6A C6 H6B . . 109.5
C5 C6 H6C . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 Se1 . 2.3347(9) y
W1 Se1 2_656 2.3347(9) ?
W1 Se2 2_656 2.3379(9) ?
W1 Se2 . 2.3379(9) y
W1 Ag1 . 2.9723(11) ?
W1 Ag1 1_545 2.9725(11) ?
Ag1 Se1 2_666 2.6224(11) ?
Ag1 Se1 1_565 2.6224(11) y
Ag1 Se2 . 2.6210(10) y
Ag1 Se2 2_656 2.6210(10) ?
Ag1 W1 1_565 2.9725(11) ?
N1 C1 . 1.330(9) ?
N1 C5 . 1.376(9) ?
N1 H1N . 0.8600 ?
C1 C2 . 1.371(10) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.361(12) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.400(12) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.380(11) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.475(11) ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9600 ?
C6 H6C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1N N1 3_566 0.86 1.93 2.786(12) 172
C1 H1 Se1 . 0.93 2.96 3.732(8) 141
C4 H4 Se1 4 0.93 2.90 3.832(8) 176
