#------------------------------------------------------------------------------
#$Date: 2020-12-06 16:52:27 +0200 (Sun, 06 Dec 2020) $
#$Revision: 259625 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/13/7241380.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_7241380
loop_
_publ_author_name
'Kolesov, Boris A.'
'Chupina, Anastasia V.'
'Berezin, Alexey S.'
'Kompankov, Nikolay B.'
'Abramov, Pavel A.'
'Sokolov, Maxim N.'
_publ_section_title
;
 Proton motion inside
 [(DMF)₂H]₂[W₆Cl₁₄]:
 structural, Raman and luminescence studies.
;
_journal_issue                   43
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              25344
_journal_page_last               25352
_journal_paper_doi               10.1039/d0cp04152a
_journal_volume                  22
_journal_year                    2020
_chemical_formula_sum            'C12 H30 Cl14 N4 O4 W6'
_chemical_formula_weight         1893.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2020-07-30 deposited with the CCDC.	2020-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.9480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6059(3)
_cell_length_b                   10.3846(3)
_cell_length_c                   17.1139(5)
_cell_measurement_reflns_used    9376
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      30.4766
_cell_measurement_theta_min      2.7551
_cell_volume                     1871.05(9)
_computing_cell_refinement       'SAINT (Bruker-AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2004)'
_computing_data_reduction        'SAINT (Bruker-AXS, 2004)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49924
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.512
_diffrn_reflns_theta_min         2.755
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    19.396
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.361
_exptl_crystal_description       prism
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.559
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         5693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0064P)²+6.1393P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0411
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5204
_reflns_number_total             5693
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            d0cp04152a2.cif
_cod_data_source_block           85
_cod_depositor_comments
'Adding full bibliography for 7241380--7241382.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7241380
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.212
_shelx_estimated_absorpt_t_max   0.444
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9385(4) 0.7054(5) 0.3550(2) 0.0359(10) Uani 1 1 d . . . . .
H1 H 0.988780 0.688304 0.403677 0.043 Uiso 1 1 calc R U . . .
C6 C 0.9934(5) 0.4932(5) 0.3156(3) 0.0418(11) Uani 1 1 d . . . . .
H6A H 1.066475 0.492162 0.285588 0.063 Uiso 1 1 calc R U . . .
H6B H 0.936661 0.421370 0.298698 0.063 Uiso 1 1 calc R U . . .
H6C H 1.023077 0.484651 0.371838 0.063 Uiso 1 1 calc R U . . .
C10 C 0.7232(5) 1.0165(5) 0.6146(3) 0.0456(12) Uani 1 1 d . . . . .
H10A H 0.657119 1.033294 0.570677 0.068 Uiso 1 1 calc R U . . .
H10B H 0.750373 1.098047 0.640193 0.068 Uiso 1 1 calc R U . . .
H10C H 0.689420 0.959752 0.652835 0.068 Uiso 1 1 calc R U . . .
C5 C 0.8475(5) 0.6305(5) 0.2265(2) 0.0415(11) Uani 1 1 d . . . . .
H5A H 0.779718 0.692616 0.232514 0.062 Uiso 1 1 calc R U . . .
H5B H 0.809858 0.547771 0.208781 0.062 Uiso 1 1 calc R U . . .
H5C H 0.900229 0.662745 0.187515 0.062 Uiso 1 1 calc R U . . .
C9 C 0.9307(5) 0.9092(5) 0.6442(3) 0.0435(11) Uani 1 1 d . . . . .
H9A H 0.999076 0.872127 0.617672 0.065 Uiso 1 1 calc R U . . .
H9B H 0.896626 0.843236 0.676811 0.065 Uiso 1 1 calc R U . . .
H9C H 0.964184 0.981106 0.677591 0.065 Uiso 1 1 calc R U . . .
N1 N 0.8300(4) 0.9557(3) 0.5856(2) 0.0360(8) Uani 1 1 d . . . . .
N2 N 0.9256(4) 0.6134(4) 0.3018(2) 0.0337(8) Uani 1 1 d . . . . .
O3 O 0.8882(3) 0.8147(3) 0.34505(18) 0.0401(7) Uani 1 1 d . . . . .
Cl1 Cl 0.84951(10) 0.31702(12) 0.46491(6) 0.0383(2) Uani 1 1 d . . . . .
Cl2 Cl 0.75740(9) 0.63529(9) 0.51191(5) 0.02670(18) Uani 1 1 d . . . . .
Cl3 Cl 0.68393(9) 0.37572(9) 0.62958(5) 0.02343(17) Uani 1 1 d . . . . .
Cl6 Cl 0.67524(10) 0.69411(10) 0.70483(5) 0.0323(2) Uani 1 1 d . . . . .
Cl5 Cl 0.60858(9) 0.47914(10) 0.34300(5) 0.02777(19) Uani 1 1 d . . . . .
Cl4 Cl 0.58162(11) 0.81990(12) 0.35898(7) 0.0425(3) Uani 1 1 d . . . . .
Cl7 Cl 0.46696(9) 0.78465(9) 0.53936(5) 0.02608(18) Uani 1 1 d . . . . .
W2 W 0.65204(2) 0.42268(2) 0.48548(2) 0.01868(4) Uani 1 1 d . . . . .
W1 W 0.53813(2) 0.63713(2) 0.43842(2) 0.01923(4) Uani 1 1 d . . . . .
W3 W 0.57789(2) 0.58300(2) 0.58839(2) 0.01820(4) Uani 1 1 d . . . . .
C11 C 0.8811(14) 0.9153(13) 0.5204(8) 0.028(3) Uiso 0.3 1 d . . P A 1
H11 H 0.959016 0.869417 0.523127 0.033 Uiso 0.3 1 calc R U P A 1
O2 O 0.8187(10) 0.9431(10) 0.4587(6) 0.032(2) Uiso 0.3 1 d . . P A 1
C3 C 0.8201(6) 0.9508(6) 0.5072(3) 0.0257(11) Uiso 0.7 1 d . . P A 2
H3 H 0.746855 0.983768 0.476180 0.031 Uiso 0.7 1 calc R U P A 2
O1 O 0.9109(4) 0.9010(4) 0.4745(3) 0.0322(9) Uiso 0.7 1 d . . P A 2
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 C1 N2 123.7(4) . . ?
O3 C1 H1 118.1 . . ?
N2 C1 H1 118.1 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 N1 C10 113.3(4) . . ?
C11 N1 C10 145.7(7) . . ?
C3 N1 C9 130.0(5) . . ?
C11 N1 C9 97.5(7) . . ?
C10 N1 C9 116.8(4) . . ?
C1 N2 C6 120.4(4) . . ?
C1 N2 C5 121.6(4) . . ?
C6 N2 C5 118.0(4) . . ?
W2 Cl2 W3 63.17(2) . . ?
W2 Cl2 W1 63.07(2) . . ?
W3 Cl2 W1 62.92(2) . . ?
W3 Cl3 W2 63.19(2) . . ?
W3 Cl3 W1 63.05(2) . 3_666 ?
W2 Cl3 W1 62.83(2) . 3_666 ?
W1 Cl5 W2 63.20(2) . . ?
W1 Cl5 W3 63.00(2) . 3_666 ?
W2 Cl5 W3 62.89(2) . 3_666 ?
W1 Cl7 W3 63.11(2) . . ?
W1 Cl7 W2 62.81(2) . 3_666 ?
W3 Cl7 W2 62.84(2) . 3_666 ?
Cl1 W2 Cl2 92.92(4) . . ?
Cl1 W2 Cl5 91.44(3) . . ?
Cl2 W2 Cl5 89.71(3) . . ?
Cl1 W2 Cl3 92.22(3) . . ?
Cl2 W2 Cl3 89.40(3) . . ?
Cl5 W2 Cl3 176.27(3) . . ?
Cl1 W2 Cl7 90.73(4) . 3_666 ?
Cl2 W2 Cl7 176.35(3) . 3_666 ?
Cl5 W2 Cl7 90.36(3) . 3_666 ?
Cl3 W2 Cl7 90.29(3) . 3_666 ?
Cl1 W2 W1 134.31(3) . 3_666 ?
Cl2 W2 W1 118.55(2) . 3_666 ?
Cl5 W2 W1 118.80(2) . 3_666 ?
Cl3 W2 W1 58.67(2) . 3_666 ?
Cl7 W2 W1 58.36(2) 3_666 3_666 ?
Cl1 W2 W3 133.79(3) . 3_666 ?
Cl2 W2 W3 118.73(2) . 3_666 ?
Cl5 W2 W3 58.70(2) . 3_666 ?
Cl3 W2 W3 118.78(2) . 3_666 ?
Cl7 W2 W3 58.41(2) 3_666 3_666 ?
W1 W2 W3 60.123(6) 3_666 3_666 ?
Cl1 W2 W3 136.14(3) . . ?
Cl2 W2 W3 58.53(2) . . ?
Cl5 W2 W3 118.28(2) . . ?
Cl3 W2 W3 58.30(2) . . ?
Cl7 W2 W3 118.38(2) 3_666 . ?
W1 W2 W3 60.035(5) 3_666 . ?
W3 W2 W3 90.063(6) 3_666 . ?
Cl1 W2 W1 135.65(3) . . ?
Cl2 W2 W1 58.76(2) . . ?
Cl5 W2 W1 58.33(2) . . ?
Cl3 W2 W1 118.24(2) . . ?
Cl7 W2 W1 118.37(2) 3_666 . ?
W1 W2 W1 90.015(6) 3_666 . ?
W3 W2 W1 59.981(5) 3_666 . ?
W3 W2 W1 59.951(5) . . ?
Cl4 W1 Cl5 93.20(4) . . ?
Cl4 W1 Cl7 90.09(4) . . ?
Cl5 W1 Cl7 176.67(3) . . ?
Cl4 W1 Cl3 90.76(4) . 3_666 ?
Cl5 W1 Cl3 90.01(3) . 3_666 ?
Cl7 W1 Cl3 90.47(3) . 3_666 ?
Cl4 W1 Cl2 93.43(4) . . ?
Cl5 W1 Cl2 89.44(3) . . ?
Cl7 W1 Cl2 89.84(3) . . ?
Cl3 W1 Cl2 175.80(3) 3_666 . ?
Cl4 W1 W2 133.00(3) . 3_666 ?
Cl5 W1 W2 118.83(2) . 3_666 ?
Cl7 W1 W2 58.83(2) . 3_666 ?
Cl3 W1 W2 58.50(2) 3_666 3_666 ?
Cl2 W1 W2 118.34(2) . 3_666 ?
Cl4 W1 W3 135.11(3) . 3_666 ?
Cl5 W1 W3 58.71(2) . 3_666 ?
Cl7 W1 W3 118.95(2) . 3_666 ?
Cl3 W1 W3 58.28(2) 3_666 3_666 ?
Cl2 W1 W3 118.07(2) . 3_666 ?
W2 W1 W3 60.132(5) 3_666 3_666 ?
Cl4 W1 W3 134.78(3) . . ?
Cl5 W1 W3 118.47(2) . . ?
Cl7 W1 W3 58.51(2) . . ?
Cl3 W1 W3 118.48(2) 3_666 . ?
Cl2 W1 W3 58.36(2) . . ?
W2 W1 W3 59.999(5) 3_666 . ?
W3 W1 W3 90.048(6) 3_666 . ?
Cl4 W1 W2 137.01(3) . . ?
Cl5 W1 W2 58.47(2) . . ?
Cl7 W1 W2 118.51(2) . . ?
Cl3 W1 W2 118.17(2) 3_666 . ?
Cl2 W1 W2 58.18(2) . . ?
W2 W1 W2 89.985(6) 3_666 . ?
W3 W1 W2 59.902(6) 3_666 . ?
W3 W1 W2 60.005(5) . . ?
Cl6 W3 Cl3 92.63(3) . . ?
Cl6 W3 Cl7 90.78(3) . . ?
Cl3 W3 Cl7 176.56(3) . . ?
Cl6 W3 Cl2 92.95(3) . . ?
Cl3 W3 Cl2 89.40(3) . . ?
Cl7 W3 Cl2 89.98(3) . . ?
Cl6 W3 Cl5 91.10(3) . 3_666 ?
Cl3 W3 Cl5 89.99(3) . 3_666 ?
Cl7 W3 Cl5 90.40(3) . 3_666 ?
Cl2 W3 Cl5 175.93(3) . 3_666 ?
Cl6 W3 W2 133.62(3) . 3_666 ?
Cl3 W3 W2 118.77(2) . 3_666 ?
Cl7 W3 W2 58.75(2) . 3_666 ?
Cl2 W3 W2 118.58(2) . 3_666 ?
Cl5 W3 W2 58.41(2) 3_666 3_666 ?
Cl6 W3 W1 134.95(3) . 3_666 ?
Cl3 W3 W1 58.67(2) . 3_666 ?
Cl7 W3 W1 118.85(2) . 3_666 ?
Cl2 W3 W1 118.13(2) . 3_666 ?
Cl5 W3 W1 58.29(2) 3_666 3_666 ?
W2 W3 W1 60.118(5) 3_666 3_666 ?
Cl6 W3 W1 135.06(3) . . ?
Cl3 W3 W1 118.55(2) . . ?
Cl7 W3 W1 58.38(2) . . ?
Cl2 W3 W1 58.72(2) . . ?
Cl5 W3 W1 118.27(2) 3_666 . ?
W2 W3 W1 59.878(5) 3_666 . ?
W1 W3 W1 89.952(6) 3_666 . ?
Cl6 W3 W2 136.45(3) . . ?
Cl3 W3 W2 58.51(2) . . ?
Cl7 W3 W2 118.42(2) . . ?
Cl2 W3 W2 58.30(2) . . ?
Cl5 W3 W2 118.11(2) 3_666 . ?
W2 W3 W2 89.937(6) 3_666 . ?
W1 W3 W2 59.833(6) 3_666 . ?
W1 W3 W2 60.044(5) . . ?
O2 C11 N1 114.2(13) . . ?
O2 C11 H11 122.9 . . ?
N1 C11 H11 122.9 . . ?
O1 C3 N1 118.9(6) . . ?
O1 C3 H3 120.6 . . ?
N1 C3 H3 120.6 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O3 1.256(6) . ?
C1 N2 1.316(6) . ?
C1 H1 0.9500 . ?
C6 N2 1.446(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C10 N1 1.437(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C5 N2 1.456(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C9 N1 1.456(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N1 C3 1.334(7) . ?
N1 C11 1.365(14) . ?
Cl1 W2 2.4274(10) . ?
Cl2 W2 2.4911(9) . ?
Cl2 W3 2.4972(9) . ?
Cl2 W1 2.5066(9) . ?
Cl3 W3 2.4907(9) . ?
Cl3 W2 2.4964(8) . ?
Cl3 W1 2.5011(9) 3_666 ?
Cl6 W3 2.4230(9) . ?
Cl5 W1 2.4923(9) . ?
Cl5 W2 2.4960(8) . ?
Cl5 W3 2.5037(9) 3_666 ?
Cl4 W1 2.4115(10) . ?
Cl7 W1 2.4933(9) . ?
Cl7 W3 2.4969(9) . ?
Cl7 W2 2.5059(9) 3_666 ?
W2 W1 2.6049(2) 3_666 ?
W2 W3 2.6082(2) 3_666 ?
W2 W3 2.6128(2) . ?
W2 W1 2.6138(2) . ?
W1 W3 2.6103(2) 3_666 ?
W1 W3 2.61139(19) . ?
C11 O2 1.211(17) . ?
C11 H11 0.9500 . ?
C3 O1 1.280(7) . ?
C3 H3 0.9500 . ?
