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_7044867
_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         'C16 H24 N6 O21 V6, 2(C16 H36 N)'
_chemical_formula_sum            'C48 H96 N8 O21 V6'
_chemical_formula_weight         1426.96
_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             2017-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-07-05 deposited with the CCDC.
2017-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.715(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1864(7)
_cell_length_b                   15.7148(5)
_cell_length_c                   25.1531(8)
_cell_measurement_reflns_used    8664
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.8910
_cell_measurement_theta_min      4.0710
_cell_volume                     6731.9(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_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 1.000
_diffrn_measured_fraction_theta_max 0.970
_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    -42.00  33.00   1.00    4.68    --  -40.81  38.00 -60.00   75
  2  \w    -46.00 -12.00   1.00    4.68    --  -40.81 125.00 -90.00   34
  3  \w    -55.00  32.00   1.00    4.68    --  -40.81  57.00  60.00   87
  4  \w     31.00  97.00   1.00    4.68    --   40.81-125.00 120.00   66
  5  \w     37.00  97.00   1.00   18.72    --  112.00 -95.00 150.00   60
  6  \w     65.00 121.00   1.00   18.72    --  112.00-125.00  90.00   56
  7  \w     59.00 118.00   1.00   18.72    --  112.00 -30.00-150.00   59
  8  \w     90.00 141.00   1.00   18.72    --  112.00 -61.00-150.00   51
  9  \w     87.00 178.00   1.00   18.72    --  112.00  61.00   0.00   91
 10  \w     96.00 133.00   1.00   18.72    --  112.00 125.00-120.00   37
 11  \w     97.00 171.00   1.00   18.72    --  112.00 125.00-150.00   74
 12  \w     40.00  79.00   1.00   18.72    --  112.00 -61.00-150.00   39
;
_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      0.0758333000
_diffrn_orient_matrix_UB_12      0.0454676000
_diffrn_orient_matrix_UB_13      -0.0107493000
_diffrn_orient_matrix_UB_21      0.0474526000
_diffrn_orient_matrix_UB_22      -0.0526150000
_diffrn_orient_matrix_UB_23      0.0448155000
_diffrn_orient_matrix_UB_31      0.0136561000
_diffrn_orient_matrix_UB_32      -0.0690989000
_diffrn_orient_matrix_UB_33      -0.0411461000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27976
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.915
_diffrn_reflns_theta_min         3.546
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20209
_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    1.408
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.781
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         13792
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1378P)^2^+0.6711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2203
_refine_ls_wR_factor_ref         0.2381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10418
_reflns_number_total             13792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03822d2.cif
_cod_data_source_block           exp_465
_cod_depositor_comments
'Adding full bibliography for 7044864--7044867.cif.'
_cod_database_code               7044867
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         V6CHON
_reflns_odcompleteness_completeness 99.93
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C15-C16C \\sim C15-C16B \\sim C15-C16A
 with sigma of 0.02
 O20C-C16C \\sim O20A-C16B \\sim O20B-C16A
 with sigma of 0.02
3. Rigid bond restraints
 C46, C48A, C47B, C48B, C47A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C32A, C32B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, C44A, C44B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, O21A, O21B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C46 \\sim C48A \\sim C47B \\sim C48B \\sim C47A: within 1.7A with sigma of 0.04
and sigma for terminal atoms of 0.08
C31 \\sim C32A \\sim C32B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C43 \\sim C44A \\sim C44B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C1 \\sim O21A \\sim O21B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C16C) = Uanis(C16B) = Uanis(C16A)
Uanis(C16C) = Uanis(O20C)
Uanis(C16B) = Uanis(O20A)
Uanis(C16A) = Uanis(O20B)
5. Others
 Fixed Sof: O20B(0.5) H20B(0.5) C16B(0.3) H16A(0.3) H16B(0.3) H1AA(0.8)
 H1AB(0.8) H1BC(0.2) H1BD(0.2) H31A(0.6) H31B(0.6) H31C(0.4) H31D(0.4)
 C32A(0.6) H32A(0.6) H32B(0.6) H32C(0.6) H46A(0.5) H46B(0.5) H46C(0.5)
 H46D(0.5) C48A(0.5) H48A(0.5) H48B(0.5) H48C(0.5) H43A(0.5) H43B(0.5)
 H43C(0.5) H43D(0.5) C44A(0.5) H44A(0.5) H44B(0.5) H44C(0.5) O21A(0.8)
 H21A(0.8) C44B(0.5) H44D(0.5) H44E(0.5) H44F(0.5) C32B(0.4) H32D(0.4)
 H32E(0.4) H32F(0.4) C47B(0.5) H47A(0.5) H47B(0.5) C48B(0.5) H48D(0.5)
 H48E(0.5) H48F(0.5) O21B(0.2) H21B(0.2) C47A(0.5) H47C(0.5) H47D(0.5)
 C16A(0.5) H16C(0.5) H16D(0.5) O20A(0.3) H20A(0.3) O20C(0.2) H20C(0.2)
 C16C(0.2) H16E(0.2) H16F(0.2)
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C0AA(H0AA,H0AB), C11(H11A,H11B), C6(H6A,H6B),
 C10(H10A,H10B), C4(H4A,H4B), C20(H20D,H20E), C29(H29A,H29B), C13(H13A,H13B),
 C30(H30A,H30B), C39(H39A,H39B), C38(H38A,H38B), C37(H37A,H37B), C16B(H16A,
 H16B), C18(H18A,H18B), C1(H1AA,H1AB), C1(H1BC,H1BD), C28(H28A,H28B), C8(H8A,
 H8B), C27(H27A,H27B), C36(H36A,H36B), C21(H21C,H21D), C41(H41A,H41B), C26(H26A,
 H26B), C22(H22A,H22B), C42(H42A,H42B), C35(H35A,H35B), C31(H31A,H31B),
 C31(H31C,H31D), C46(H46A,H46B), C46(H46C,H46D), C23(H23A,H23B), C43(H43A,H43B),
  C43(H43C,H43D), C34(H34A,H34B), C19(H19A,H19B), C47B(H47A,H47B), C47A(H47C,
 H47D), C16A(H16C,H16D), C16C(H16E,H16F)
6.b Me refined with riding coordinates:
 C44B(H44D,H44E,H44F), C32B(H32D,H32E,H32F)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C3(H3)
6.d Idealised Me refined with riding coordinates:
 C44A(H44A,H44B,H44C)
6.e Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C32A(H32A,H32B,
 H32C), C48A(H48A,H48B,H48C), C24(H24A,H24B,H24C), C33(H33A,H33B,H33C),
 C48B(H48D,H48E,H48F)
6.f Idealised tetrahedral OH refined with riding coordinates:
 O20B(H20B), O21A(H21A), O20A(H20A)
6.g Idealised tetrahedral OH refined as rotating group:
 O21B(H21B), O20C(H20C)
;
_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 2.064
_oxdiff_exptl_absorpt_empirical_full_min 0.462