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_7714264
_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 rm
_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
_audit_creation_date             2023-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2023-09-05 deposited with the CCDC.	2023-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.9070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.88630(10)
_cell_length_b                   19.59970(10)
_cell_length_c                   9.86860(10)
_cell_measurement_reflns_used    16104
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.3400
_cell_measurement_theta_min      4.5070
_cell_volume                     1626.07(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_temperature      100
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_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    -60.00  22.00   0.50    0.30    --  -47.96  37.00 150.00  164
  2  \w   -119.00 -73.00   0.50    0.30    --  -47.96-125.00 -60.00   92
  3  \w   -117.00 -35.00   0.50    0.30    --  -47.96 -37.00-120.00  164
  4  \w   -117.00 -36.00   0.50    0.30    --  -47.96 -37.00 -30.00  162
  5  \w     20.00  45.00   0.50    0.30    --   47.96 -37.00 -60.00   50
  6  \w     64.00  90.00   0.50    0.30    --   47.96  37.00 -30.00   52
  7  \w    -21.00  15.00   0.50    0.30    --   47.96 -37.00 -60.00   72
  8  \w    -76.00 -23.00   0.50    0.80    --  -86.25  77.00-120.00  106
  9  \w   -143.00 -75.00   0.50    0.80    --  -86.25-125.00-120.00  136
 10  \w     54.00 122.00   0.50    0.80    --  107.75 -57.00  90.00  136
 11  \w     52.00 127.00   0.50    0.80    --  107.75 -77.00  60.00  150
 12  \w     40.00  78.00   0.50    0.80    --  107.75 -99.00  30.00   76
 13  \w     73.00  99.00   0.50    0.80    --  107.75 -99.00-120.00   52
 14  \w    129.00 155.00   0.50    0.80    --  107.75  37.00-150.00   52
 15  \w     36.00  80.00   0.50    0.80    --  107.75 -99.00 -60.00   88
 16  \w     83.00 114.00   0.50    0.80    --  107.75-125.00 -60.00   62
 17  \w     36.00 114.00   0.50    0.80    --  107.75-125.00-120.00  156
 18  \w     38.00  76.00   0.50    0.80    --  107.75-125.00 -60.00   76
 19  \w     32.00 121.00   0.50    0.80    --  107.75 -19.00 -90.00  178
 20  \w     43.00 121.00   0.50    0.80    --  107.75 -19.00   0.00  156
 21  \w     49.00 117.00   0.50    0.80    --  107.75-125.00   0.00  136
 22  \w     98.00 123.00   0.50    0.80    --  107.75 -57.00 -90.00   50
 23  \w     44.00  78.00   0.50    0.80    --  107.75 -57.00 -90.00   68
 24  \w     42.00 106.00   0.50    0.80    --  107.75 -99.00  60.00  128
 25  \w     42.00 176.00   0.50    0.80    --  107.75   0.00 -30.00  268
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16285
_diffrn_reflns_point_group_measured_fraction_full 0.729
_diffrn_reflns_point_group_measured_fraction_max 0.702
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.532
_diffrn_reflns_theta_min         4.737
_exptl_absorpt_coefficient_mu    5.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.009(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         4870
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+0.5916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.399
_reflns_Friedel_fraction_full    0.444
_reflns_Friedel_fraction_max     0.412
_reflns_number_gt                4801
_reflns_number_total             4870
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02903d2.cif
_cod_data_source_block           exp_1815
_cod_database_code               7714264
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.404
_shelx_estimated_absorpt_t_min   0.404
_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
 O8-H8
 0.85 with sigma of 0.01
 C8-H8
 1.867285 with sigma of 0.02
 V2-H8
 2.798769 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C3(H3), C8(H8A), C10(H10), C1(H1A)
4.b Aromatic/amide H refined with riding coordinates:
 N7(H7A), N4(H4), N8(H8B), N6(H6A), N10(H10A), N2(H2), N5(H5A), C11(H11),
 C15(H15), C21(H21), C18(H18), C13(H13), C16(H16), C17(H17), C14(H14), C22(H22),
  C5(H5), C20(H20), C19(H19), C23(H23), C7(H7), C6(H6)
;
_shelx_res_checksum              23466
_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
;