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_7044865
_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         'C26 H26 Cl2 N6 O19 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C58 H98 Cl2 N8 O19 V6'
_chemical_formula_weight         1587.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-18
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-08-30 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.971(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2078(4)
_cell_length_b                   20.8402(10)
_cell_length_c                   16.9703(9)
_cell_measurement_reflns_used    3509
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.8900
_cell_measurement_theta_min      4.8140
_cell_volume                     3608.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.966
_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    -82.00  21.00   1.00    2.00    --  -40.81  19.00   0.00  103
  2  \w    -65.00   3.00   1.00    2.00    --  -40.81  38.00 -90.00   68
  3  \w    -30.00  72.00   1.00    2.00    --   40.81 -77.00  90.00  102
  4  \w     38.00 111.00   1.00   30.00    --  111.52 -45.00 -90.00   73
  5  \w     94.00 178.00   1.00   30.00    --  111.52  77.00-150.00   84
  6  \w     89.00 165.00   1.00   30.00    --  111.52  61.00  90.00   76
  7  \w     39.00 141.00   1.00   30.00    --  111.52 -61.00  90.00  102
  8  \w     53.00 102.00   1.00   30.00    --  111.52 -95.00-120.00   49
  9  \w     61.00 123.00   1.00   30.00    --  111.52 -30.00  30.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0334702000
_diffrn_orient_matrix_UB_12      -0.0344853000
_diffrn_orient_matrix_UB_13      -0.0771697000
_diffrn_orient_matrix_UB_21      0.1126107000
_diffrn_orient_matrix_UB_22      0.0478188000
_diffrn_orient_matrix_UB_23      -0.0120983000
_diffrn_orient_matrix_UB_31      0.0947173000
_diffrn_orient_matrix_UB_32      -0.0445824000
_diffrn_orient_matrix_UB_33      0.0464926000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14858
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.631
_diffrn_reflns_theta_min         4.243
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.534
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (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    1.462
_exptl_crystal_description       plate
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         7330
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1273P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4861
_reflns_number_total             7330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03822d2.cif
_cod_data_source_block           exp_1543
_cod_depositor_comments
'Adding full bibliography for 7044864--7044867.cif.'
_cod_database_code               7044865
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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. Rigid bond restraints
 C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C12(H12a,H12b), C11(H11a,H11b), C9(H9a,H9b), C26(H26a,H26b),
 C25(H25a,H25b), C18(H18a,H18b), C17(H17a,H17b), C28(H28a,H28b), C24(H24a,H24b),
  C27(H27a,H27b), C23(H23a,H23b), C16(H16a,H16b), C15(H15a,H15b), C19(H19a,
 H19b), C20(H20a,H20b)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C6(H6), C2(H2), C3(H3)
3.c Idealised Me refined as rotating group:
 C29(H29a,H29b,H29c), C22(H22a,H22b,H22c), C14(H14a,H14b,H14c), C21(H21a,H21b,
 H21c)
;
_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 1.873
_oxdiff_exptl_absorpt_empirical_full_min 0.603