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_7714512
_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         'C12 H19 N15 O9 V2, 5(H2 O)'
_chemical_formula_sum            'C12 H29 N15 O14 V2'
_chemical_formula_weight         709.38
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-11
_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                 106.654(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3068(2)
_cell_length_b                   16.4045(2)
_cell_length_c                   16.7884(3)
_cell_measurement_reflns_used    11378
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.1040
_cell_measurement_theta_min      3.8470
_cell_volume                     2719.48(8)
_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      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.949
_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     44.00  69.00   0.50    0.33    --   43.34  27.00 -15.00   50
  2  \w     54.00  80.00   0.50    1.31    --  108.01  15.00 120.00   52
  3  \w     93.00 177.00   0.50    1.31    --  108.01  15.00 120.00  168
  4  \w     91.00 141.00   0.50    1.31    --  108.01  27.00 -15.00  100
  5  \w    101.00 178.00   0.50    1.31    --  108.01 125.00-180.00  154
  6  \w     53.00 100.00   0.50    1.31    --  108.01 -77.00  60.00   94
  7  \w     49.00  99.00   0.50    1.31    --  108.01 -77.00 -30.00  100
  8  \w     33.00  58.00   0.50    1.31    --  108.01 -61.00 -90.00   50
  9  \w     35.00  70.00   0.50    1.31    --  108.01 -61.00-150.00   70
 10  \w    -26.00  -1.00   0.50    0.33    --   43.34 -27.00-177.00   50
 11  \w    -33.00  37.00   0.50    0.33    --  -43.34  27.00 -15.00  140
 12  \w    -64.00 -28.00   0.50    1.31    --  -96.00  61.00 -90.00   72
 13  \w    -70.00 -22.00   0.50    1.31    --  -96.00  61.00-180.00   96
 14  \w    -71.00 -46.00   0.50    1.31    --  -96.00  61.00-150.00   50
 15  \w    -65.00 -22.00   0.50    1.31    --  -96.00  61.00 -60.00   86
 16  \w     32.00  98.00   0.50    0.33    --   43.34-125.00  90.00  132
 17  \w    -48.00 -22.00   0.50    1.31    --  -96.00  45.00  60.00   52
 18  \w    -66.00 -22.00   0.50    1.31    --  -96.00  61.00  90.00   88
 19  \w    -70.00 -33.00   0.50    1.31    --  -96.00  61.00 150.00   74
 20  \w    -55.00 -29.00   0.50    1.31    --  -96.00 125.00  60.00   52
 21  \w   -124.00 -14.00   0.50    0.33    --  -43.34 -27.00-177.00  220
 22  \w   -169.00 -77.00   0.50    1.31    --  -96.00 -27.00-177.00  184
 23  \w   -118.00 -92.00   0.50    0.33    --  -43.34-125.00 -30.00   52
;
_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      0.0303643000
_diffrn_orient_matrix_UB_12      0.0039022000
_diffrn_orient_matrix_UB_13      0.0952692000
_diffrn_orient_matrix_UB_21      0.1425429000
_diffrn_orient_matrix_UB_22      0.0333962000
_diffrn_orient_matrix_UB_23      0.0070388000
_diffrn_orient_matrix_UB_31      -0.0556510000
_diffrn_orient_matrix_UB_32      0.0876923000
_diffrn_orient_matrix_UB_33      -0.0069369000
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17071
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.374
_diffrn_reflns_theta_min         3.849
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.611
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87037
_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    1.733
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         5267
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      7.160
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0482P)^2^+1.1967P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0845
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4799
_reflns_number_total             5267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03445c2.cif
_cod_data_source_block           exp_9805_auto
_cod_depositor_comments
'Adding full bibliography for 7714512--7714516.cif.'
_cod_database_code               7714512
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N V '
_shelx_estimated_absorpt_t_max   0.437
_shelx_estimated_absorpt_t_min   0.351
_reflns_odcompleteness_completeness 99.98
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3W-H = O3W-HA_$1
 0.87 with sigma of 0.02
 O4W-HG = O4W-HH
 0.87 with sigma of 0.02
 HG-HH
 1.38 with sigma of 0.04
 H-HA_$1
 1.38 with sigma of 0.04
 O3A-C4 \\sim O3-C4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5WA \\sim O5W: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O2W \\sim O2WA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O3A \\sim O3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4. Others
 Sof(O5WA)=Sof(H5WC)=Sof(H5WD)=Sof(O2WA)=Sof(H2WA)=Sof(H2WB)=Sof(O3A)=1-FVAR(1)
 Sof(O3)=Sof(O2W)=Sof(H2WC)=Sof(H2WD)=Sof(O5W)=Sof(H5WA)=Sof(H5WB)=FVAR(1)
5.a Riding coordinates:
 O3W(H,HA), O1W(HB,HC), O4W(HG,HH)
5.b Free rotating group:
 O2W(H2WC,H2WD), O5W(H5WA,H5WB), O5WA(H5WC,H5WD), O2WA(H2WA,H2WB)
5.c Rotating group:
 N14(HI,HJ), N4(HO,HP)
5.d Secondary CH2 refined with riding coordinates:
 C5(HU,HV), C2(HW,HX)
5.e Aromatic/amide H refined with riding coordinates:
 N8(HD), N12(HE), N3(HF)
5.f X=CH2 refined with riding coordinates:
 N9(HK,HL), N10(HM,HN), N5(HQ,HR), N15(HS,HT)
;
_shelx_res_checksum              69910
_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 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.847