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_7044866
_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         'C28 H32 N6 O19 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C60 H104 N8 O19 V6'
_chemical_formula_weight         1547.15
_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
_audit_creation_date             2017-08-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2017-08-31 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.666(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2063(5)
_cell_length_b                   21.4566(18)
_cell_length_c                   16.8058(12)
_cell_measurement_reflns_used    3924
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.9290
_cell_measurement_theta_min      4.7820
_cell_volume                     3678.8(4)
_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)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.971
_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   -115.00 -18.00   1.00    1.00    --  -40.81 -38.00  90.00   97
  2  \w      6.00  33.00   1.00    1.00    --  -40.81  38.00 150.00   27
  3  \w    -96.00  -8.00   1.00    1.00    --  -40.81 125.00  30.00   88
  4  \w     24.00  80.00   1.00    1.00    --   40.81-125.00 -30.00   56
  5  \w     88.00 114.00   1.00   15.00    --  110.27  45.00 -60.00   26
  6  \w     37.00 137.00   1.00   15.00    --  110.27 -30.00 120.00  100
  7  \w     37.00 131.00   1.00   15.00    --  110.27 -45.00 -90.00   94
  8  \w     98.00 143.00   1.00   15.00    --  110.27 125.00-180.00   45
  9  \w    113.00 174.00   1.00   15.00    --  110.27  45.00  90.00   61
 10  \w    127.00 178.00   1.00   15.00    --  110.27  45.00 -60.00   51
 11  \w     97.00 161.00   1.00   15.00    --  110.27  45.00   0.00   64
;
_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      0.0708099000
_diffrn_orient_matrix_UB_12      0.0551405000
_diffrn_orient_matrix_UB_13      0.0414040000
_diffrn_orient_matrix_UB_21      -0.0775739000
_diffrn_orient_matrix_UB_22      -0.0119380000
_diffrn_orient_matrix_UB_23      0.0758045000
_diffrn_orient_matrix_UB_31      0.1086439000
_diffrn_orient_matrix_UB_32      -0.0443649000
_diffrn_orient_matrix_UB_33      0.0307186000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.549
_diffrn_reflns_theta_min         4.121
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.721
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56099
_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    1.397
_exptl_crystal_description       block
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7404
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0774
_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^)+(0.1750P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2241
_refine_ls_wR_factor_ref         0.2525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5029
_reflns_number_total             7404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03822d2.cif
_cod_data_source_block           exp_1529
_cod_depositor_comments
'Adding full bibliography for 7044864--7044867.cif.'
_cod_database_code               7044866
_chemical_oxdiff_formula         V6CHNO
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C30A-C29 = C29-C30B = C28-C29
 1.54 with sigma of 0.02
 C29-C30B = C30A-C29 = C28-C29 = C28-C27
 1.54 with sigma of 0.02
 C26-C25B = C25B-C24B = C24B-C23B = C24A-C23A
 1.54 with sigma of 0.02
 C26-C25A = C24A-C25A
 1.54 with sigma of 0.02
 C26-C25B = C26-C25A = C24A-C25A = C25B-C24B = C24A-C23A = C24B-C23B
 1.54 with sigma of 0.02
 C30B-C28
 2.34 with sigma of 0.04
 C30A-C28
 2.34 with sigma of 0.04
 C29-C27
 2.34 with sigma of 0.04
 C25B-C23B
 2.34 with sigma of 0.04
 C23B-C25B
 2.34 with sigma of 0.04
 C24B-C26
 2.34 with sigma of 0.04
 C23A-C25A
 2.34 with sigma of 0.04
 C24A-C26
 2.34 with sigma of 0.04
3. Rigid bond restraints
 C28, C29, C30A, C30B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25B, C25A, C24A, C24B, C23B, C23A, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C30B) = Uanis(C30A)
Uanis(C25A) = Uanis(C25B)
Uanis(C24B) = Uanis(C24A)
Uanis(C23B) = Uanis(C23A)
5. Others
 Fixed Sof: H29A(0.75) H29B(0.75) H29C(0.25) H29D(0.25) H26A(0.75) H26B(0.75)
 H26C(0.25) H26D(0.25) C24B(0.75) H24A(0.75) H24B(0.75) C25B(0.75) H25A(0.75)
 H25B(0.75) C23B(0.75) H23A(0.75) H23B(0.75) H23C(0.75) C30A(0.75) H30A(0.75)
 H30B(0.75) H30C(0.75) C30B(0.25) H30D(0.25) H30E(0.25) H30F(0.25) C24A(0.25)
 H24C(0.25) H24D(0.25) C23A(0.25) H23D(0.25) H23E(0.25) H23F(0.25) C25A(0.25)
 H25C(0.25) H25D(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C10(H10A,H10B), C14(H14A,H14B), C19(H19A,
 H19B), C18(H18A,H18B), C27(H27A,H27B), C29(H29A,H29B), C29(H29C,H29D),
 C26(H26A,H26B), C26(H26C,H26D), C28(H28A,H28B), C20(H20A,H20B), C17(H17A,H17B),
  C24B(H24A,H24B), C21(H21A,H21B), C25B(H25A,H25B), C16(H16A,H16B), C24A(H24C,
 H24D), C25A(H25C,H25D)
6.b Me refined with riding coordinates:
 C30B(H30D,H30E,H30F)
6.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C6(H6), C7(H7), C3(H3), C4(H4)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C22(H22A,H22B,H22C), C23B(H23A,H23B,H23C), C15(H15A,H15B,
 H15C), C30A(H30A,H30B,H30C), C23A(H23D,H23E,H23F)
;
_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 1.495
_oxdiff_exptl_absorpt_empirical_full_min 0.653