Protonated and deprotonated vanadyl imidazole tartrates for the mimics of the vanadium coordination in FeV-cofactor of V-nitrogenase
Zhu, Shuang-Shuang; Xie, Zhenlang; Deng, Lan; Wang, Si-Yuan; Ni, Lubin; Zhou, Zhao-Hui; Dalton Transactions  (2023) –; doi:10.1039/D3DT02903D

data_7714262
_publ_section_title
;
 Protonated and deprotonated vanadyl imidazole tartrates for the mimics of
 the vanadium coordination in FeV-cofactor of V-nitrogenase
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02903D
_journal_year                    2023
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C14 H14 N4 O14 V2, 2(C3 H5 N2), C3 H4 N2'
_chemical_formula_sum            'C23 H28 N10 O14 V2'
_chemical_formula_weight         770.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-25 deposited with the CCDC.	2023-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.160(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9068(3)
_cell_length_b                   19.6606(6)
_cell_length_c                   9.8849(4)
_cell_measurement_reflns_used    1896
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.2580
_cell_measurement_theta_min      2.8660
_cell_volume                     1635.09(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -52.00  51.00   1.00    5.00    --  -18.45  77.00 -90.00  103
  2  \w    -52.00  49.00   1.00    5.00    --  -18.45  77.00  30.00  101
  3  \w     67.00  92.00   1.00    5.00    --   19.70  77.00  60.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0776865000
_diffrn_orient_matrix_UB_12      -0.0138934000
_diffrn_orient_matrix_UB_13      0.0263143000
_diffrn_orient_matrix_UB_21      0.0324935000
_diffrn_orient_matrix_UB_22      0.0323456000
_diffrn_orient_matrix_UB_23      -0.0059110000
_diffrn_orient_matrix_UB_31      0.0036719000
_diffrn_orient_matrix_UB_32      0.0078862000
_diffrn_orient_matrix_UB_33      0.0710825000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5991
_diffrn_reflns_point_group_measured_fraction_full 0.797
_diffrn_reflns_point_group_measured_fraction_max 0.797
_diffrn_reflns_theta_full        24.990
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         2.181
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.652
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 1411 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         4595
_refine_ls_number_restraints     188
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0423P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.545
_reflns_Friedel_fraction_full    0.581
_reflns_Friedel_fraction_max     0.581
_reflns_number_gt                4361
_reflns_number_total             4595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02903d2.cif
_cod_data_source_block           exp_18851
_cod_database_code               7714262
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.780
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.07
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O11-H11
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 C18-H18
 1 with sigma of 0.01
 C10-H11
 1.893847 with sigma of 0.02
 V2-H11
 3.018167 with sigma of 0.02
 C3-H4
 1.864024 with sigma of 0.02
 V1-H4
 2.813709 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C4 \\sim C8 \\sim C18 \\sim C3 \\sim C5 \\sim C11 \\sim C1 \\sim C9 \\sim C2
\\sim C21 \\sim C10 \\sim C6 \\sim C15 \\sim C19 \\sim C20 \\sim C7 \\sim C12
\\sim C17 \\sim C22 \\sim C23 \\sim C16 \\sim C14 \\sim C13: within 3.8A with
sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C8(H8), C3(H3), C1(H1), C10(H10)
4.b Aromatic/amide H refined with riding coordinates:
 N5(H5A), N2(H2), N6(H6A), N10(H10A), C5(H5), C21(H21), C6(H6), C15(H15),
 C19(H19), C7(H7), C12(H12), C17(H17), C22(H22), C23(H23), C14(H14), C13(H13)
;
_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 1.513
_oxdiff_exptl_absorpt_empirical_full_min 0.901