One-dimensional supramolecular chain based on [H2V10O28]4- units decorated with 4-dimethylaminopyridinium ions: An experimental and theoretical characterization
Gonzalez-Vergara, Enrique; Sánchez-Lara, Eduardo; Martínez-Valencia, Beatriz; Corona-Motolinia, Nidia D.; Sánchez-Gaytán, Brenda L.; Castro, María Eugenia; Bernès, Sylvain; Mendez-Rojas, Miguel; Meléndez Bustamante, Francisco; New Journal of Chemistry 43 (2019) 17746–17755; doi:10.1039/C9NJ02097G

data_7058727
_publ_section_title
;
 One-dimensional supramolecular chain based on [H2V10O28]4- units
 decorated with 4-dimethylaminopyridinium ions: An experimental and
 theoretical characterization
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17746
_journal_page_last               17755
_journal_paper_doi               10.1039/C9NJ02097G
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'H2 O28 V10, 4(C7 H11 N2), 5(H2 O)'
_chemical_formula_sum            'C28 H56 N8 O33 V10'
_chemical_formula_weight         1542.20
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-14
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-11-27 deposited with the CCDC.    2019-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.3898(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.93249(9)
_cell_length_b                   9.91005(11)
_cell_length_c                   24.12328(19)
_cell_measurement_reflns_used    19417
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      77.0060
_cell_measurement_theta_min      3.6530
_cell_volume                     2613.49(4)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    'SHELXTL and MERCURY'
_computing_publication_material  SHELXL-2014/7
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5564
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega    2.00   37.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323   77.0000 -150.0000 35

  2 omega  -50.00   30.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323   38.0000  150.0000 80

  3 omega -115.00  -13.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323  -57.0000    0.0000 102

  4 omega   73.00  110.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -       41.0323 -146.0000 -102.0000 37

  5 omega   67.00  108.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -95.0000    0.0000 41

  6 omega   41.00   97.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -45.0000    0.0000 56

  7 omega   68.00  101.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -95.0000   60.0000 33

  8 omega   54.00  104.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -77.0000  -90.0000 50

  9 omega   54.00  167.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   15.0000   30.0000 113

 10 omega  122.00  148.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -77.0000  -90.0000 26

 11 omega   79.00  144.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   15.0000  -60.0000 65

 12 omega   59.00   90.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -30.0000 -150.0000 31

 13 omega   75.00  115.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000 -111.0000  120.0000 40

 14 omega   40.00   98.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -45.0000   90.0000 58

 15 omega   38.00   86.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -30.0000 -180.0000 48

 16 omega   61.00   87.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -30.0000  -60.0000 26

 17 omega  -71.00   33.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323   57.0000  -60.0000 104

 18 omega -116.00  -60.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323 -146.0000 -102.0000 56

 19 omega -117.00  -15.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323  -38.0000  150.0000 102

 20 omega -120.00   -7.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323  -77.0000  -90.0000 113

 21 omega   81.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   77.0000  150.0000 97

 22 omega   87.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   45.0000 -150.0000 91

 23 omega   31.00  109.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -95.0000 -150.0000 78

 24 omega   40.00   98.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -45.0000  -90.0000 58

 25 omega   84.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   30.0000  150.0000 94

 26 omega   81.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   77.0000   30.0000 97

 27 omega   37.00   91.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000  -30.0000   30.0000 54

 28 omega   87.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   45.0000   90.0000 91

 29 omega  -50.00   35.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323   38.0000 -150.0000 85

 30 omega -120.00   -7.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323  -77.0000    0.0000 113

 31 omega -115.00  -11.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323  -57.0000   90.0000 104

 32 omega   18.00   98.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -       41.0323 -125.0000   60.0000 80

 33 omega   81.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   77.0000  120.0000 97

 34 omega   87.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   45.0000 -120.0000 91

 35 omega   81.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   77.0000  -30.0000 97

 36 omega   81.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   77.0000  -60.0000 97

 37 omega   81.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   77.0000  -90.0000 97

 38 omega   81.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   77.0000 -120.0000 97

 39 omega   81.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   77.0000    0.0000 97

 40 omega   37.00  116.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000 -111.0000  150.0000 79

 41 omega  -75.00   38.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323   77.0000   30.0000 113

 42 omega -120.00   -7.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323  -77.0000   90.0000 113

 43 omega -120.00   -7.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      -41.0323  -77.0000 -180.0000 113

 44 omega   18.00   98.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -       41.0323 -125.0000  150.0000 80

 45 omega   37.00  116.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000 -111.0000  -60.0000 79

 46 omega   85.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   61.0000 -180.0000 93

 47 omega   85.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   61.0000   90.0000 93

 48 omega   85.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   61.0000 -150.0000 93

 49 omega   85.00  178.00   1.0000    9.1900
omega____ theta____ kappa____ phi______ frames
    -      115.0000   61.0000   60.0000 93
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1374059000
_diffrn_orient_matrix_UB_12      -0.0047708000
_diffrn_orient_matrix_UB_13      0.0135871000
_diffrn_orient_matrix_UB_21      -0.0304915000
_diffrn_orient_matrix_UB_22      -0.0127057000
_diffrn_orient_matrix_UB_23      -0.0622191000
_diffrn_orient_matrix_UB_31      0.0067247000
_diffrn_orient_matrix_UB_32      -0.1548862000
_diffrn_orient_matrix_UB_33      0.0046912000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            50963
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         3.665
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.226
_exptl_absorpt_correction_T_max  0.258
_exptl_absorpt_correction_T_min  0.088
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlisPro (Agilent, 2013)'
_exptl_crystal_colour            dark_orange
_exptl_crystal_density_diffrn    1.960
_exptl_crystal_description       prism
_exptl_crystal_F_000             1548
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water'
_exptl_crystal_size_max          0.219
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.153
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     372
_refine_ls_number_reflns         4662
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0298
_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/[\s^2^(Fo^2^)+(0.0534P)^2^+1.0615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4217
_reflns_number_total             4662
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02097g2.cif
_cod_data_source_block           3
_cod_database_code               7058727
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.135
_shelx_estimated_absorpt_t_max   0.205
_shelx_res_checksum              17416