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_7714513
_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         'C4 H11 N10 O8 V3, 0.5(H2 O), 4[H2O]'
_chemical_formula_sum            'C4 H20 N10 O12.5 V3'
_chemical_formula_weight         561.12
_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             2023-04-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2023-11-11 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.788(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3231(2)
_cell_length_b                   17.2111(3)
_cell_length_c                   10.4223(2)
_cell_measurement_reflns_used    6488
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.3320
_cell_measurement_theta_min      5.0180
_cell_volume                     1812.70(6)
_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 2018/2 (Sheldrick, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.940
_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    -51.00 -20.00   0.50    0.12    --  -98.00  45.00 150.00   62
  2  \w    -49.00 -20.00   0.50    0.12    --  -98.00  45.00 120.00   58
  3  \w    -51.00 -20.00   0.50    0.12    --  -98.00  45.00 -60.00   62
  4  \w    -47.00 -22.00   0.50    0.12    --  -98.00  45.00-180.00   50
  5  \w    -57.00 -31.00   0.50    0.12    --  -98.00  61.00 -90.00   52
  6  \w    -46.00 -21.00   0.50    0.12    --  -98.00  45.00 -90.00   50
  7  \w    -49.00 -21.00   0.50    0.12    --  -98.00  45.00 -30.00   56
  8  \w    -26.00  42.00   0.50    0.05    --  -40.63  19.00 -90.00  136
  9  \w    -51.00 -21.00   0.50    0.12    --  -98.00  45.00   0.00   60
 10  \w    -50.00 -25.00   0.50    0.12    --  -98.00  45.00  30.00   50
 11  \w    -51.00 -21.00   0.50    0.12    --  -98.00  45.00  90.00   60
 12  \w    -67.00  -3.00   0.50    0.05    --  -40.63 110.00 153.00  128
 13  \w    -77.00 -52.00   0.50    0.12    --  -98.00 110.00 153.00   50
 14  \w    -87.00 -25.00   0.50    0.12    --  -98.00 125.00-180.00  124
 15  \w   -149.00 -79.00   0.50    0.12    --  -98.00-110.00  58.00  140
 16  \w   -115.00 -62.00   0.50    0.05    --  -40.63 -38.00 -60.00  106
 17  \w    -58.00 -14.00   0.50    0.05    --  -40.63 -38.00 -60.00   88
 18  \w    -40.00  -8.00   0.50    0.05    --   40.63 -19.00  30.00   64
 19  \w     61.00  87.00   0.50    0.12    --  110.43 -77.00  60.00   52
 20  \w     46.00  71.00   0.50    0.12    --  110.43 -61.00  30.00   50
 21  \w     37.00  69.00   0.50    0.12    --  110.43 -61.00  60.00   64
 22  \w     36.00 102.00   0.50    0.12    --  110.43 -77.00 120.00  132
 23  \w     75.00 113.00   0.50    0.12    --  110.43-125.00 150.00   76
 24  \w     48.00 103.00   0.50    0.12    --  110.43-110.00  58.00  110
 25  \w     31.00  87.00   0.50    0.05    --   40.63-110.00  58.00  112
 26  \w     90.00 115.00   0.50    0.12    --  110.43  61.00  60.00   50
 27  \w    133.00 165.00   0.50    0.12    --  110.43  61.00  60.00   64
 28  \w    109.00 143.00   0.50    0.12    --  110.43 110.00 153.00   68
 29  \w     68.00  93.00   0.50    0.05    --   40.63 178.00 -30.00   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      -0.1007082000
_diffrn_orient_matrix_UB_12      -0.0244339000
_diffrn_orient_matrix_UB_13      -0.1236890000
_diffrn_orient_matrix_UB_21      -0.0033065000
_diffrn_orient_matrix_UB_22      0.0840348000
_diffrn_orient_matrix_UB_23      -0.0514979000
_diffrn_orient_matrix_UB_31      0.1143779000
_diffrn_orient_matrix_UB_32      -0.0189772000
_diffrn_orient_matrix_UB_33      -0.0694746000
_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  0.0589
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10675
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.006
_diffrn_reflns_theta_min         5.039
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06236
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.056
_exptl_crystal_description       block
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.238
_refine_diff_density_min         -1.315
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0912P)^2^+4.0553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1505
_refine_ls_wR_factor_ref         0.1536
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3203
_reflns_number_total             3504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03445c2.cif
_cod_data_source_block           exp_12327_auto
_cod_depositor_comments
'Adding full bibliography for 7714512--7714516.cif.'
_cod_original_formula_sum        'C4 H20 N10 O12.50 V3'
_cod_database_code               7714513
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N V Cl'
_shelx_estimated_absorpt_t_max   0.344
_shelx_estimated_absorpt_t_min   0.236
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
3.a Riding coordinates:
 O1W(H1WA,H1WB)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8)
3.c X=CH2 refined with riding coordinates:
 N9(H9A,H9B), N4(H4A,H4B), N5(H5A,H5B), N10(H10A,H10B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4025
_shelx_fab_checksum              22053
_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 7.500
_oxdiff_exptl_absorpt_empirical_full_min 0.527