Stepwise syntheses and supramolecular assemblies of a series of polyoxovanadate hybrids with various architectures
Huang, Bo; Wang, Nan; Yang, Kang; Ke, Degang; Fang, Yajun; Hu, Xunliang; Wu, Baolin; Xiao, Zicheng; Wu, Pingfan; Wei, Yongge; New Journal of Chemistry 42 (2018) 5853–; doi:10.1039/C7NJ04727D

data_7057099
_publ_section_title
;
 Stepwise syntheses and supramolecular assemblies of a series of
 polyoxovanadate hybrids with various architectures
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5853
_journal_paper_doi               10.1039/C7NJ04727D
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C38 H36 N2 O25 V6, C32 H72 N2'
_chemical_formula_sum            'C70 H108 N4 O25 V6'
_chemical_formula_weight         1711.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-05-03
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_audit_update_record
;
2017-08-17 deposited with the CCDC.
2018-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                66.339(6)
_cell_angle_beta                 78.031(5)
_cell_angle_gamma                67.630(7)
_cell_formula_units_Z            1
_cell_length_a                   12.0059(8)
_cell_length_b                   13.8979(12)
_cell_length_c                   14.0548(7)
_cell_measurement_reflns_used    4396
_cell_measurement_temperature    107.2
_cell_measurement_theta_max      29.3056
_cell_measurement_theta_min      2.9921
_cell_volume                     1982.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      107.2
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -40.00  -15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046   77.0000 -180.0000 25

  2 omega  -72.00  -45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9046  -37.0000    0.0000 27

  3 omega   -5.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000   90.0000 30

  4 omega   20.00   48.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -77.0000  120.0000 28

  5 omega  -50.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -37.0000   60.0000 89

  6 omega  -46.00  -20.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -77.0000  120.0000 26

  7 omega  -42.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390  -77.0000 -150.0000 93

  8 omega   -4.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.1390   77.0000  -30.0000 95
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0119413000
_diffrn_orient_matrix_UB_12      -0.0491072000
_diffrn_orient_matrix_UB_13      0.0085117000
_diffrn_orient_matrix_UB_21      -0.0626384000
_diffrn_orient_matrix_UB_22      0.0305079000
_diffrn_orient_matrix_UB_23      -0.0030383000
_diffrn_orient_matrix_UB_31      0.0057564000
_diffrn_orient_matrix_UB_32      0.0119824000
_diffrn_orient_matrix_UB_33      -0.0544683000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14862
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             894
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         7776
_refine_ls_number_restraints     564
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0673
_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^)+(0.0000P)^2^+11.1045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1614
_reflns_number_gt                6740
_reflns_number_total             7776
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj04727d2.cif
_cod_data_source_block           exp_4931
_cod_depositor_comments
'Adding full bibliography for 7057098--7057101.cif.'
_cod_original_cell_volume        1982.2(2)
_cod_database_code               7057099
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32