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_7714265
_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             2018-08-12
_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                 109.4050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.16620(10)
_cell_length_b                   13.61250(10)
_cell_length_c                   12.80470(10)
_cell_measurement_reflns_used    19341
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.4960
_cell_measurement_theta_min      4.5920
_cell_volume                     1671.35(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 (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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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    -56.00  24.00   0.50    0.10    --  -47.96  57.00  30.00  160
  2  \w    -59.00  25.00   0.50    0.10    --  -47.96  57.00 150.00  168
  3  \w    -60.00  22.00   0.50    0.10    --  -47.96  57.00 -90.00  164
  4  \w   -115.00 -85.00   0.50    0.10    --  -47.96-125.00 150.00   60
  5  \w     49.00  78.00   0.50    0.10    --   47.96  57.00 -30.00   58
  6  \w     80.00 120.00   0.50    0.10    --   47.96  57.00 -30.00   80
  7  \w     14.00  55.00   0.50    0.10    --   47.96 -19.00  30.00   82
  8  \w   -113.00 -87.00   0.50    0.39    --  -86.25 -94.00-120.00   52
  9  \w   -130.00 -91.00   0.50    0.39    --  -86.25-125.00  60.00   78
 10  \w     38.00  64.00   0.50    0.39    --  107.75-125.00-150.00   52
 11  \w     92.00 165.00   0.50    0.39    --  107.75  61.00-150.00  146
 12  \w     38.00 112.00   0.50    0.39    --  107.75 -77.00 150.00  148
 13  \w     35.00  65.00   0.50    0.39    --  107.75-125.00  90.00   60
 14  \w    115.00 167.00   0.50    0.39    --  107.75  15.00  90.00  104
 15  \w    102.00 170.00   0.50    0.39    --  107.75 125.00  90.00  136
 16  \w     83.00 109.00   0.50    0.39    --  107.75 -94.00   0.00   52
 17  \w     89.00 121.00   0.50    0.39    --  107.75 -15.00-120.00   64
 18  \w     37.00  63.00   0.50    0.39    --  107.75 -94.00   0.00   52
 19  \w     92.00 162.00   0.50    0.39    --  107.75 125.00  30.00  140
 20  \w     35.00  68.00   0.50    0.39    --  107.75 -61.00   0.00   66
 21  \w     77.00 122.00   0.50    0.39    --  107.75 -61.00   0.00   90
 22  \w     35.00 114.00   0.50    0.39    --  107.75 -30.00 150.00  158
 23  \w     35.00  65.00   0.50    0.39    --  107.75 -15.00-120.00   60
 24  \w     81.00 117.00   0.50    0.39    --  107.75-125.00-180.00   72
 25  \w     96.00 168.00   0.50    0.39    --  107.75  15.00 150.00  144
 26  \w     68.00 117.00   0.50    0.39    --  107.75-125.00   0.00   98
 27  \w     39.00  64.00   0.50    0.39    --  107.75-125.00-180.00   50
 28  \w     77.00 106.00   0.50    0.39    --  107.75-125.00  90.00   58
 29  \w     56.00  83.00   0.50    0.39    --  107.75-125.00 -30.00   54
 30  \w     92.00 121.00   0.50    0.39    --  107.75 125.00 120.00   58
 31  \w    136.00 174.00   0.50    0.39    --  107.75 125.00 120.00   76
 32  \w     38.00  81.00   0.50    0.39    --  107.75 -94.00-120.00   86
 33  \w     88.00 117.00   0.50    0.39    --  107.75-125.00 -30.00   58
 34  \w     77.00 102.00   0.50    0.39    --  107.75 -94.00  90.00   50
 35  \w    100.00 125.00   0.50    0.39    --  107.75  61.00-180.00   50
 36  \w    143.00 170.00   0.50    0.39    --  107.75  61.00-180.00   54
 37  \w     82.00 116.00   0.50    0.39    --  107.75-125.00-150.00   68
 38  \w     39.00  70.00   0.50    0.39    --  107.75 -94.00 150.00   62
 39  \w     83.00 116.00   0.50    0.39    --  107.75-125.00 -60.00   66
 40  \w     99.00 124.00   0.50    0.39    --  107.75  61.00 -60.00   50
 41  \w    148.00 173.00   0.50    0.39    --  107.75  61.00 -60.00   50
 42  \w     79.00 108.00   0.50    0.39    --  107.75 -94.00  60.00   58
 43  \w     45.00 121.00   0.50    0.39    --  107.75 -45.00   0.00  152
;
_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      0.0490683000
_diffrn_orient_matrix_UB_12      -0.1048780000
_diffrn_orient_matrix_UB_13      -0.0134726000
_diffrn_orient_matrix_UB_21      -0.1127018000
_diffrn_orient_matrix_UB_22      -0.0424005000
_diffrn_orient_matrix_UB_23      0.0431872000
_diffrn_orient_matrix_UB_31      -0.1034435000
_diffrn_orient_matrix_UB_32      -0.0035623000
_diffrn_orient_matrix_UB_33      -0.1192663000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22233
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.854
_diffrn_reflns_theta_min         3.660
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69398
_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    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2992 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0019(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6846
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0317P)^2^+1.0622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    0.965
_reflns_Friedel_fraction_max     0.929
_reflns_number_gt                6676
_reflns_number_total             6846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02903d2.cif
_cod_data_source_block           exp_673
_cod_database_code               7714265
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C46 H64 N22 O24 V4 '
_shelx_estimated_absorpt_t_max   0.617
_shelx_estimated_absorpt_t_min   0.617
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O3W-H3WB
 0.85 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C12(H12A), C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N10(H10), N8(H8), N4(H4), N12(H12), C17(H17), C6(H6A), C20(H20),
 C9(H9), C14(H14), C22(H22), C11(H11), C21(H21), C10(H10A), C3(H3), C8(H8A),
 C5(H5), C19(H19), C4(H4A), C18(H18), C7(H7), C16(H16), C15(H15)
;
_shelx_res_checksum              60865
_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 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.715