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_7714263
_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 rmad
_chemical_formula_moiety         'C22 H26 N12 O8 V2, 4(H2 O)'
_chemical_formula_sum            'C22 H34 N12 O12 V2'
_chemical_formula_weight         760.49
_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             2020-11-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-11-23 deposited with the CCDC.	2023-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.196(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1454(2)
_cell_length_b                   13.6326(2)
_cell_length_c                   12.7784(2)
_cell_measurement_reflns_used    9098
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.5770
_cell_measurement_theta_min      3.6540
_cell_volume                     1669.09(5)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.950
_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    -62.00  21.00   0.50    0.20    --  -46.62  59.00 -59.00  166
  2  \w   -119.00 -30.00   0.50    0.20    --  -46.62 -59.00 160.00  178
  3  \w    -45.00 -19.00   0.50    1.00    --  -88.50  59.00 -59.00   52
  4  \w   -107.00 -73.00   0.50    1.00    --  -88.50 -59.00 160.00   68
  5  \w   -158.00-112.00   0.50    1.00    --  -88.50 -59.00 160.00   92
  6  \w     93.00 122.00   0.50    1.00    --  110.00 -59.00 160.00   58
  7  \w     38.00  89.00   0.50    1.00    --  110.00 -59.00 160.00  102
  8  \w    135.00 178.00   0.50    1.00    --  110.00  59.00 -59.00   86
  9  \w   -118.00 -92.00   0.50    0.20    --  -46.62-125.00   0.00   52
 10  \w   -118.00 -72.00   0.50    0.20    --  -46.62-125.00 -60.00   92
 11  \w     51.00  76.00   0.50    0.20    --   46.62  59.00 -59.00   50
 12  \w      4.00  52.00   0.50    0.20    --   46.62 -59.00 160.00   96
 13  \w   -158.00 -95.00   0.50    1.00    --  -88.50-125.00 -90.00  126
 14  \w    -55.00 -21.00   0.50    1.00    --  -88.50 125.00 -30.00   68
 15  \w     56.00  82.00   0.50    1.00    --  110.00 -99.00-180.00   52
 16  \w     44.00 117.00   0.50    1.00    --  110.00-125.00   0.00  146
 17  \w    131.00 176.00   0.50    1.00    --  110.00  57.00  30.00   90
 18  \w     95.00 121.00   0.50    1.00    --  110.00  57.00  30.00   52
 19  \w     38.00 104.00   0.50    1.00    --  110.00-125.00-180.00  132
 20  \w     58.00 124.00   0.50    1.00    --  110.00 -57.00  30.00  132
 21  \w     46.00 107.00   0.50    1.00    --  110.00 -99.00   0.00  122
;
_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      -0.1037798000
_diffrn_orient_matrix_UB_12      -0.0506803000
_diffrn_orient_matrix_UB_13      0.0474960000
_diffrn_orient_matrix_UB_21      -0.0577841000
_diffrn_orient_matrix_UB_22      -0.0605515000
_diffrn_orient_matrix_UB_23      -0.1071654000
_diffrn_orient_matrix_UB_31      0.1084126000
_diffrn_orient_matrix_UB_32      -0.0807844000
_diffrn_orient_matrix_UB_33      0.0506065000
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11499
_diffrn_reflns_point_group_measured_fraction_full 0.800
_diffrn_reflns_point_group_measured_fraction_max 0.744
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.167
_diffrn_reflns_theta_min         3.663
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.359
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61788
_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    1.513
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 1640 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         5324
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+3.0292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.502
_reflns_Friedel_fraction_full    0.584
_reflns_Friedel_fraction_max     0.520
_reflns_number_gt                5151
_reflns_number_total             5324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02903d2.cif
_cod_data_source_block           exp_1769
_cod_database_code               7714263
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.500
_shelx_estimated_absorpt_t_min   0.414
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O2W-H2WB
 0.85 with sigma of 0.01
 O1W-H1WB
 0.85 with sigma of 0.01
 H2WB-H1WB
 2.1 with sigma of 0.02
 H1WB-H2WB
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C12(H12A), C1(H1)
4.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N10(H10), N8(H8), N2(H2), N12(H12), C17(H17), C6(H6A), C9(H9),
 C20(H20), C14(H14), C22(H22), C10(H10A), C21(H21), C11(H11), C5(H5), C8(H8A),
 C3(H3), C19(H19), C4(H4A), C18(H18), C7(H7), C16(H16), C15(H15)
;
_shelx_res_checksum              61432
_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 1.612
_oxdiff_exptl_absorpt_empirical_full_min 0.675