#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:25:36 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179663 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/16/4511647.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4511647
loop_
_publ_author_name
'Podgajny, Robert'
'Pinkowicz, Dawid'
'Czarnecki, Bernard'
'Kozieł, Marcin'
'Chorąży, Szymon'
'Wis, Magdalena'
'Nitek, Wojciech'
'Rams, Michał'
'Sieklucka, Barbara'
_publ_section_title
;
 Role of Pyrazine-N,N′-dioxide in [W(CN)8]n−-Based Hybrid
 Networks: Anion−π Interactions
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              4030
_journal_paper_doi               10.1021/cg500636m
_journal_volume                  14
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '3K, 2(C4 H4 N2 O2), W C8 N8, 4(H2 O)'
_chemical_formula_sum            'C16 H16 K3 N12 O8 W'
_chemical_formula_weight         805.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      43
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-08-13T16:26:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.57900(10)
_cell_length_b                   25.2880(3)
_cell_length_c                   9.7880(4)
_cell_measurement_reflns_used    7088
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     5341.2(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.896592E-1
_diffrn_orient_matrix_UB_12      0.481901E-1
_diffrn_orient_matrix_UB_13      -0.87403E-2
_diffrn_orient_matrix_UB_21      -0.204766E-1
_diffrn_orient_matrix_UB_22      0.40092E-1
_diffrn_orient_matrix_UB_23      0.109973E-1
_diffrn_orient_matrix_UB_31      0.73534E-2
_diffrn_orient_matrix_UB_32      -0.67408E-2
_diffrn_orient_matrix_UB_33      0.382663E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3906
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.859
_exptl_absorpt_correction_T_max  0.7932
_exptl_absorpt_correction_T_min  0.7273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3127
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.85
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.386(5)
_refine_ls_extinction_coef       0.000325(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.1
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3906
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0069P)²+25.0708P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                3766
_reflns_number_total             3906
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            cg500636m_si_002.cif
_cod_data_source_block           mk103
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 4511646--4511649.cif.
;
_cod_database_code               4511647
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W 0.75 0.25 0.299 0.00885(5) Uani 1 2 d S
C1 C 0.77279(13) 0.30300(12) 0.1329(3) 0.0121(6) Uani 1 1 d .
N1 N 0.78252(11) 0.33058(10) 0.0418(4) 0.0177(5) Uani 1 1 d .
C2 C 0.82583(14) 0.29723(13) 0.3778(4) 0.0138(6) Uani 1 1 d .
N2 N 0.86714(12) 0.32005(12) 0.4236(3) 0.0199(6) Uani 1 1 d .
C3 C 0.78434(14) 0.20457(13) 0.4696(4) 0.0134(6) Uani 1 1 d .
N3 N 0.80014(11) 0.18263(10) 0.5667(3) 0.0164(5) Uani 1 1 d .
C4 C 0.66501(13) 0.28451(13) 0.2199(3) 0.0128(6) Uani 1 1 d .
N4 N 0.61993(12) 0.30153(11) 0.1744(3) 0.0183(5) Uani 1 1 d .
K2 K 0.75 0.25 -0.1961(5) 0.0118(2) Uani 1 2 d S
K3 K 0.73827(2) 0.39383(2) -0.20153(17) 0.01586(11) Uani 1 1 d .
N11 N 0.72032(11) 0.44302(10) 0.1570(3) 0.0137(5) Uani 1 1 d .
O11 O 0.70205(9) 0.44487(9) 0.0297(3) 0.0178(5) Uani 1 1 d .
C12 C 0.77832(13) 0.45786(14) 0.1919(3) 0.0200(6) Uani 1 1 d .
H12 H 0.8058 0.4703 0.1233 0.024 Uiso 1 1 calc R
C13 C 0.79804(12) 0.45522(13) 0.3241(3) 0.0190(6) Uani 1 1 d .
H13 H 0.839 0.4659 0.3464 0.023 Uiso 1 1 calc R
N14 N 0.75951(12) 0.43735(11) 0.4246(3) 0.0123(5) Uani 1 1 d .
O14 O 0.77891(9) 0.43360(8) 0.5505(3) 0.0184(4) Uani 1 1 d .
C15 C 0.70110(13) 0.42338(12) 0.3893(3) 0.0149(5) Uani 1 1 d .
H15 H 0.6732 0.4116 0.4579 0.018 Uiso 1 1 calc R
C16 C 0.68175(13) 0.42594(11) 0.2567(3) 0.0146(5) Uani 1 1 d .
H16 H 0.6407 0.4156 0.2341 0.018 Uiso 1 1 calc R
O1 O 0.67071(10) 0.17478(10) -0.2805(3) 0.0166(5) Uani 1 1 d .
H1A H 0.6303 0.1818 -0.2564 0.025 Uiso 1 1 d R
H1B H 0.6682 0.1666 -0.3705 0.025 Uiso 1 1 d R
O2 O 0.84502(10) 0.18569(10) -0.1212(3) 0.0195(5) Uani 1 1 d .
H2A H 0.8856 0.1842 -0.1566 0.029 Uiso 1 1 d R
H2B H 0.8571 0.1884 -0.0323 0.029 Uiso 1 1 d R
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 0 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.849 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C3 W1 C3 78.63(17) . 14_655
C3 W1 C1 109.24(10) . 14_655
C3 W1 C1 146.42(10) 14_655 14_655
C3 W1 C1 146.42(10) . .
C3 W1 C1 109.24(10) 14_655 .
C1 W1 C1 82.58(17) 14_655 .
C3 W1 C2 71.97(12) . 14_655
C3 W1 C2 76.03(12) 14_655 14_655
C1 W1 C2 75.80(12) 14_655 14_655
C1 W1 C2 141.29(11) . 14_655
C3 W1 C2 76.03(12) . .
C3 W1 C2 71.97(12) 14_655 .
C1 W1 C2 141.29(12) 14_655 .
C1 W1 C2 75.80(12) . .
C2 W1 C2 138.29(18) 14_655 .
C3 W1 C4 141.19(12) . .
C3 W1 C4 76.83(12) 14_655 .
C1 W1 C4 77.83(12) 14_655 .
C1 W1 C4 71.06(11) . .
C2 W1 C4 73.21(11) 14_655 .
C2 W1 C4 122.86(12) . .
C3 W1 C4 76.83(12) . 14_655
C3 W1 C4 141.19(12) 14_655 14_655
C1 W1 C4 71.06(11) 14_655 14_655
C1 W1 C4 77.83(12) . 14_655
C2 W1 C4 122.86(12) 14_655 14_655
C2 W1 C4 73.21(11) . 14_655
C4 W1 C4 138.26(17) . 14_655
N1 C1 W1 177.0(3) . .
N2 C2 W1 176.4(3) . .
N3 C3 W1 175.0(3) . .
N4 C4 W1 177.7(3) . .
O11 N11 C12 120.7(3) . .
O11 N11 C16 120.9(2) . .
C12 N11 C16 118.5(3) . .
N11 C12 C13 121.0(3) . .
N11 C12 H12 119.5 . .
C13 C12 H12 119.5 . .
C12 C13 N14 120.7(3) . .
C12 C13 H13 119.7 . .
N14 C13 H13 119.7 . .
O14 N14 C15 121.3(2) . .
O14 N14 C13 120.6(2) . .
C15 N14 C13 118.0(3) . .
N14 C15 C16 121.0(3) . .
N14 C15 H15 119.5 . .
C16 C15 H15 119.5 . .
N11 C16 C15 120.8(3) . .
N11 C16 H16 119.6 . .
C15 C16 H16 119.6 . .
H1A O1 H1B 103.7 . .
H2A O2 H2B 95.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C3 2.158(3) .
W1 C3 2.158(3) 14_655
W1 C1 2.164(3) 14_655
W1 C1 2.164(3) .
W1 C2 2.168(3) 14_655
W1 C2 2.168(3) .
W1 C4 2.174(3) .
W1 C4 2.174(3) 14_655
C1 N1 1.151(4) .
C2 N2 1.153(4) .
C3 N3 1.153(4) .
C4 N4 1.153(4) .
N11 O11 1.308(4) .
N11 C12 1.350(4) .
N11 C16 1.353(4) .
C12 C13 1.363(4) .
C12 H12 0.95 .
C13 N14 1.365(4) .
C13 H13 0.95 .
N14 O14 1.305(4) .
N14 C15 1.354(4) .
C15 C16 1.365(4) .
C15 H15 0.95 .
C16 H16 0.95 .
O1 H1A 0.9206 .
O1 H1B 0.9064 .
O2 H2A 0.9425 .
O2 H2B 0.9117 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A O11 0.92 1.84 2.761(3) 176.1 7_644 y
O1 H1B N2 0.91 2.18 3.012(4) 152 14_654 y
O2 H2A O14 0.94 1.89 2.827(3) 171 15_644 y
O2 H2B N4 0.91 2.1 3.009(4) 176.1 14_655 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
O11 N11 C12 C13 -178.9(3)
C16 N11 C12 C13 0.7(5)
N11 C12 C13 N14 0.1(5)
C12 C13 N14 O14 178.3(3)
C12 C13 N14 C15 -1.2(5)
O14 N14 C15 C16 -178.0(3)
C13 N14 C15 C16 1.5(4)
O11 N11 C16 C15 179.2(3)
C12 N11 C16 C15 -0.5(4)
N14 C15 C16 N11 -0.7(5)
