Diversified polyoxovanadate derivatives obtained by copper(i)-catalysed azide-alkyne cycloaddition reaction: their synthesis and structural characterization.
Jia, Hongli; Li, Qi; Bayaguud, Aruuhan; Huang, Yichao; She, Shan; Chen, Kun; Wei, Yongge; Dalton transactions (Cambridge, England : 2003) 47 (2018) 577–584; doi:10.1039/c7dt03822d

data_7044864
_publ_section_title
;
 Diversified polyoxovanadate derivatives obtained by copper(i)-catalysed
 azide-alkyne cycloaddition reaction: their synthesis and structural
 characterization.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              577
_journal_page_last               584
_journal_paper_doi               10.1039/c7dt03822d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C20 H28 N6 O23 V6, 2(C16 H36 N), 2(C2 H3 N)'
_chemical_formula_sum            'C56 H106 N10 O23 V6'
_chemical_formula_weight         1593.14
_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     iterative
_audit_creation_date             2017-07-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-07-05 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                109.899(3)
_cell_angle_beta                 108.196(3)
_cell_angle_gamma                91.399(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4326(3)
_cell_length_b                   11.8963(3)
_cell_length_c                   16.2638(5)
_cell_measurement_reflns_used    7451
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.5580
_cell_measurement_theta_min      5.5560
_cell_volume                     1783.66(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -67.00  28.00   1.00    1.00    --  -40.81  57.00  30.00   95
  2  \w     17.00 111.00   1.00    1.00    --   40.81  38.00-180.00   94
  3  \w     85.00 158.00   1.00    8.00    --  112.00  30.00-150.00   73
  4  \w    116.00 165.00   1.00    8.00    --  112.00  45.00-120.00   49
  5  \w    135.00 162.00   1.00    8.00    --  112.00  61.00 -60.00   27
  6  \w    114.00 169.00   1.00    8.00    --  112.00 125.00  60.00   55
  7  \w    102.00 129.00   1.00    8.00    --  112.00  45.00 -30.00   27
  8  \w     98.00 178.00   1.00    8.00    --  112.00  30.00 120.00   80
  9  \w     73.00 106.00   1.00    8.00    --  112.00 -95.00 120.00   33
 10  \w     71.00 121.00   1.00    8.00    --  112.00-125.00  60.00   50
 11  \w     40.00 132.00   1.00    8.00    --  112.00 -45.00 150.00   92
 12  \w     40.00 141.00   1.00    8.00    --  112.00 -61.00  30.00  101
 13  \w     64.00 108.00   1.00    8.00    --  112.00 -95.00-120.00   44
 14  \w     75.00 111.00   1.00    8.00    --  112.00-125.00-150.00   36
 15  \w     49.00  96.00   1.00    1.00    --   40.81-125.00-150.00   47
 16  \w     36.00 117.00   1.00    8.00    --  112.00 -30.00 -60.00   81
 17  \w     31.00  87.00   1.00    8.00    --  112.00 -95.00   0.00   56
 18  \w      8.00  60.00   1.00    1.00    --   40.81 -99.00  90.00   52
 19  \w   -113.00 -18.00   1.00    1.00    --  -40.81 -57.00-120.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0499487000
_diffrn_orient_matrix_UB_12      -0.1179321000
_diffrn_orient_matrix_UB_13      -0.0861540000
_diffrn_orient_matrix_UB_21      -0.0899335000
_diffrn_orient_matrix_UB_22      0.0681023000
_diffrn_orient_matrix_UB_23      -0.0560495000
_diffrn_orient_matrix_UB_31      0.1187748000
_diffrn_orient_matrix_UB_32      0.0289171000
_diffrn_orient_matrix_UB_33      -0.0303234000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12780
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.930
_diffrn_reflns_theta_min         3.995
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.998
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       block
_exptl_crystal_F_000             834
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+1.3080P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1654
_refine_ls_wR_factor_ref         0.1729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6398
_reflns_number_total             7279
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03822d2.cif
_cod_data_source_block           exp_460
_cod_depositor_comments
'Adding full bibliography for 7044864--7044867.cif.'
_cod_original_cell_volume        1783.67(9)
_cod_database_code               7044864
_chemical_oxdiff_formula         'V O N C H'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C2(H2A,H2B), C7(H7A,H7B), C6(H6A,H6B), C10(H10A,H10B), C21(H21A,
 H21B), C16(H16A,H16B), C17(H17A,H17B), C25(H25A,H25B), C22(H22A,H22B),
 C23(H23A,H23B), C15(H15A,H15B), C24(H24A,H24B), C14(H14A,H14B), C12(H12A,H12B),
  C20(H20A,H20B), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C26(H26A,H26B,
 H26C), C18(H18A,H18B,H18C), C27(H27A,H27B,H27C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.018
_oxdiff_exptl_absorpt_empirical_full_min 0.695