Asymmetric dinuclear, hexanuclear and octanuclear oxovanadium citrates with triazolates: novel mixed-ligands and mixed-valence complexes.
Xie, Zhen-Lang; Zhou, Zhao-Hui; Dalton transactions (Cambridge, England : 2003) 53 (2023) 186–195; doi:10.1039/d3dt03445c

data_7714515
_publ_section_title
;
 Asymmetric dinuclear, hexanuclear and octanuclear oxovanadium citrates
 with triazolates: novel mixed-ligands and mixed-valence complexes.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              186
_journal_page_last               195
_journal_paper_doi               10.1039/d3dt03445c
_journal_volume                  53
_journal_year                    2023
_chemical_formula_moiety         'C40 H59 K2 N40 O43.5 V8, 20[H2O]'
_chemical_formula_sum            'C40 H99 K2 N40 O63.5 V8'
_chemical_formula_weight         2642.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-07-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2023-07-24 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.30450(10)
_cell_length_b                   18.4546(2)
_cell_length_c                   26.9082(2)
_cell_measurement_reflns_used    31273
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.2920
_cell_measurement_theta_min      2.8160
_cell_volume                     10062.49(14)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.990
_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   -114.00 -69.00   0.50    0.60    --  -42.99-147.00-117.00   90
  2  \w    -92.00 -46.00   0.50    0.60    --  -42.99 125.00 125.00   92
  3  \w    -98.00 -71.00   0.50    0.60    --  -42.99-125.00  47.00   54
  4  \w     54.00  80.00   0.50    0.60    --   45.49-125.00  47.00   52
  5  \w     54.00  79.00   0.50    0.60    --   45.49-147.00-117.00   50
  6  \w    -81.00 -56.00   0.50    2.40    --  -95.46 125.00 125.00   50
  7  \w    -96.00 -61.00   0.50    2.40    --  -95.46-147.00-117.00   70
  8  \w   -143.00-118.00   0.50    2.40    --  -95.46-125.00  47.00   50
  9  \w     46.00 132.00   0.50    2.40    --   97.96-147.00-117.00  172
 10  \w     31.00 108.00   0.50    2.40    --   97.96-125.00  47.00  154
 11  \w    -17.00  15.00   0.50    0.60    --  -42.99  19.00-120.00   64
 12  \w    -25.00  38.00   0.50    0.60    --  -42.99  19.00 -30.00  126
 13  \w   -116.00 -76.00   0.50    0.60    --  -42.99-125.00 120.00   80
 14  \w    -24.00  17.00   0.50    0.60    --  -42.99  19.00-150.00   82
 15  \w    -51.00 -26.00   0.50    2.40    --  -95.46  45.00  60.00   50
 16  \w   -105.00 -74.00   0.50    2.40    --  -95.46  77.00 120.00   62
 17  \w    -86.00 -22.00   0.50    2.40    --  -95.46 125.00  90.00  128
 18  \w    -50.00 -22.00   0.50    2.40    --  -95.46 125.00-120.00   56
 19  \w    -51.00 -26.00   0.50    2.40    --  -95.46  45.00 -30.00   50
 20  \w    -51.00 -26.00   0.50    2.40    --  -95.46  45.00 -60.00   50
 21  \w    -67.00 -30.00   0.50    2.40    --  -95.46  77.00 120.00   74
 22  \w    -91.00 -57.00   0.50    2.40    --  -95.46 125.00-120.00   68
 23  \w   -167.00 -80.00   0.50    2.40    --  -95.46 -95.00-180.00  174
 24  \w     21.00  99.00   0.50    2.40    --   97.96 -95.00  60.00  156
 25  \w     25.00  51.00   0.50    2.40    --   97.96 -45.00-150.00   52
 26  \w     38.00  63.00   0.50    2.40    --   97.96 -61.00-180.00   50
 27  \w     80.00 171.00   0.50    2.40    --   97.96  45.00 -60.00  182
 28  \w     23.00  48.00   0.50    2.40    --   97.96 -45.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0536972000
_diffrn_orient_matrix_UB_12      0.0049892000
_diffrn_orient_matrix_UB_13      -0.0429801000
_diffrn_orient_matrix_UB_21      0.0073765000
_diffrn_orient_matrix_UB_22      0.0830940000
_diffrn_orient_matrix_UB_23      -0.0003235000
_diffrn_orient_matrix_UB_31      0.0533099000
_diffrn_orient_matrix_UB_32      -0.0064170000
_diffrn_orient_matrix_UB_33      -0.0379900000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            71737
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.730
_diffrn_reflns_theta_min         2.647
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             5396
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1256
_refine_ls_number_reflns         18443
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0785P)^2^+16.6432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15885
_reflns_number_total             18443
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03445c2.cif
_cod_data_source_block           exp_13142_k2v8_auto
_cod_depositor_comments
'Adding full bibliography for 7714512--7714516.cif.'
_cod_original_formula_sum        'C40 H99 K2 N40 O63.50 V8'
_cod_database_code               7714515
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.509
_shelx_estimated_absorpt_t_min   0.304
_reflns_odcompleteness_completeness 98.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 K2A-O31 \\sim K2-O31
 with sigma of 0.02
 O22A-C40 \\sim O22-C40
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O9W \\sim O9WA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
K2 \\sim K2A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
O22 \\sim O22A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O2W) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O3W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O10W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(K2) \\sim Ueq, Uanis(K2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9W) \\sim Ueq, Uanis(O9WA) \\sim Ueq, Uanis(O8W) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 K2A, O31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 K2, O31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Others
 Sof(K2)=Sof(H6WC)=Sof(H6WD)=Sof(O9WA)=Sof(O22)=1-FVAR(1)
 Sof(K2A)=Sof(H6WA)=Sof(H6WB)=Sof(O9W)=Sof(O22A)=FVAR(1)
 Fixed Sof: O2W(0.5) H2WA(0.5) H2WB(0.5) O3W(0.25) O5W(0.25) O8W(0.5)
6.a Riding coordinates:
 O6W(H6WA,H6WB), O6W(H6WC,H6WD)
6.b Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O10W(H10C,H10D)
6.c Secondary CH2 refined with riding coordinates:
 C15(H15C,H15D), C18(H18A,H18B), C23(H23A,H23B), C30(H30C,H30D), C32(H32A,
 H32B), C34(H34C,H34D), C37(H37A,H37B), C39(H39C,H39D)
6.d Aromatic/amide H refined with riding coordinates:
 N3(H3), N13(H13), N23(H23), N33(H33)
6.e X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B), N9(H9A,H9B), N10(H10A,H10B), N14(H14A,H14B),
 N15(H15A,H15B), N19(H19A,H19B), N20(H20A,H20B), N24(H24A,H24B), N25(H25A,H25B),
  N29(H29A,H29B), N30(H30A,H30B), N34(H34A,H34B), N35(H35A,H35B), N39(H39A,
 H39B), N40(H40A,H40B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40347
_shelx_fab_checksum              97827
_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 1.339
_oxdiff_exptl_absorpt_empirical_full_min 0.768