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_7714516
_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         'C20 H28 N20 O22 V6, 4[H2O]'
_chemical_formula_sum            'C20 H36 N20 O26 V6'
_chemical_formula_weight         1278.33
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2023-05-13 deposited with the CCDC.	2023-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.3481(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.60453(18)
_cell_length_b                   18.2772(3)
_cell_length_c                   11.2855(2)
_cell_measurement_reflns_used    8909
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.7480
_cell_measurement_theta_min      4.7150
_cell_volume                     2098.93(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_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      99.99(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 0.952
_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    -71.00  33.00   0.50    0.12    --  -43.34  95.00 125.00  208
  2  \w     13.00  55.00   0.50    0.12    --   43.34 -95.00  15.00   84
  3  \w   -129.00 -83.00   0.50    0.48    --  -96.00 -95.00  15.00   92
  4  \w    -80.00 -19.00   0.50    0.48    --  -96.00  95.00 125.00  122
  5  \w     63.00 108.00   0.50    0.48    --  108.01 -95.00  15.00   90
  6  \w    105.00 157.00   0.50    0.48    --  108.01  95.00 125.00  104
  7  \w   -117.00 -73.00   0.50    0.12    --  -43.34-125.00-180.00   88
  8  \w   -108.00 -70.00   0.50    0.12    --  -43.34-125.00 -90.00   76
  9  \w    -26.00  25.00   0.50    0.12    --  -43.34  19.00-120.00  102
 10  \w   -116.00 -85.00   0.50    0.12    --  -43.34-125.00 150.00   62
 11  \w    -50.00 -22.00   0.50    0.48    --  -96.00  45.00-150.00   56
 12  \w    -70.00 -22.00   0.50    0.48    --  -96.00  61.00 -60.00   96
 13  \w    -90.00 -65.00   0.50    0.48    --  -96.00 125.00  30.00   50
 14  \w    -51.00 -23.00   0.50    0.48    --  -96.00  45.00 120.00   56
 15  \w    -50.00 -19.00   0.50    0.48    --  -96.00  45.00-120.00   62
 16  \w    -50.00 -25.00   0.50    0.48    --  -96.00  45.00   0.00   50
 17  \w    -69.00 -25.00   0.50    0.48    --  -96.00  61.00 -90.00   88
 18  \w    -56.00 -29.00   0.50    0.48    --  -96.00  61.00 -30.00   54
 19  \w    -50.00 -21.00   0.50    0.48    --  -96.00  45.00 150.00   58
 20  \w    -51.00 -25.00   0.50    0.48    --  -96.00  45.00  90.00   52
 21  \w     78.00 103.00   0.50    0.48    --  108.01 -77.00  30.00   50
 22  \w     33.00  63.00   0.50    0.48    --  108.01 -77.00  30.00   60
 23  \w     41.00  67.00   0.50    0.48    --  108.01 -61.00-180.00   52
 24  \w     39.00  71.00   0.50    0.48    --  108.01 -61.00 150.00   64
 25  \w     35.00 105.00   0.50    0.48    --  108.01 -77.00 -60.00  140
 26  \w     41.00  67.00   0.50    0.48    --  108.01 -61.00  90.00   52
 27  \w     35.00  61.00   0.50    0.48    --  108.01 -61.00  30.00   52
 28  \w     71.00 101.00   0.50    0.48    --  108.01 -77.00-120.00   60
 29  \w     45.00  70.00   0.50    0.48    --  108.01 -77.00-120.00   50
 30  \w     34.00  62.00   0.50    0.48    --  108.01 -61.00  60.00   56
;
_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      0.0849251000
_diffrn_orient_matrix_UB_12      0.0259764000
_diffrn_orient_matrix_UB_13      -0.0824763000
_diffrn_orient_matrix_UB_21      0.0205277000
_diffrn_orient_matrix_UB_22      0.0743029000
_diffrn_orient_matrix_UB_23      0.0671702000
_diffrn_orient_matrix_UB_31      0.1235581000
_diffrn_orient_matrix_UB_32      -0.0301795000
_diffrn_orient_matrix_UB_33      0.0945022000
_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  0.0371
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13873
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.943
_diffrn_reflns_theta_min         4.746
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00034(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0383P)^2^+1.7543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3819
_reflns_number_total             4055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03445c2.cif
_cod_data_source_block           exp_9808_auto
_cod_depositor_comments
'Adding full bibliography for 7714512--7714516.cif.'
_cod_original_cell_volume        2098.93(7)
_cod_database_code               7714516
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N V'
_shelx_estimated_absorpt_t_max   0.384
_shelx_estimated_absorpt_t_min   0.270
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4C,H4D)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N8(H8)
2.c X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N4(H4A,H4B), N10(H10A,H10B), N9(H9A,H9B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              93139
_shelx_fab_checksum              75867
_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 1.863
_oxdiff_exptl_absorpt_empirical_full_min 0.673