Spontaneous conversions of glutamine, histidine and arginine into α-hydroxycarboxylates with NH<sub>4</sub>VO<sub>3</sub> or V<sub>2</sub>O<sub>5</sub>.
Deng, Lan; Zhou, Zhao-Hui; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11921–11930; doi:10.1039/d0dt02150d

data_7705018
_publ_section_title
;
 Spontaneous conversions of glutamine, histidine and arginine into
 \a-hydroxycarboxylates with NH<sub>4</sub>VO<sub>3</sub> or
 V<sub>2</sub>O<sub>5</sub>.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11921
_journal_page_last               11930
_journal_paper_doi               10.1039/d0dt02150d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C32 H24 N8 O8 V2, 2(C10 N2)'
_chemical_formula_sum            'C52 H24 N12 O8 V2'
_chemical_formula_weight         1046.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-16 deposited with the CCDC.	2020-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.682(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4251(6)
_cell_length_b                   15.6225(4)
_cell_length_c                   13.7562(3)
_cell_measurement_reflns_used    4144
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.5460
_cell_measurement_theta_min      4.6240
_cell_volume                     4573.1(2)
_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    'olex2.solve (Bourhis et al., 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 1.000
_diffrn_measured_fraction_theta_max 0.985
_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     14.00  46.00   0.50    9.50    --   46.62 -83.00  49.00   64
  2  \w     40.00 136.00   0.50   38.00    --  110.00 -83.00  49.00  192
  3  \w    150.00 176.00   0.50   38.00    --  110.00  19.00 120.00   52
  4  \w    146.00 172.00   0.50   38.00    --  110.00  83.00 170.00   52
  5  \w    129.00 176.00   0.50   38.00    --  110.00  37.00  90.00   94
  6  \w     96.00 121.00   0.50   38.00    --  110.00  37.00  90.00   50
  7  \w     92.00 117.00   0.50   38.00    --  110.00  83.00 170.00   50
  8  \w     86.00 177.00   0.50   38.00    --  110.00  77.00 150.00  182
  9  \w     46.00  71.00   0.50    9.50    --   46.62  83.00 170.00   50
 10  \w     36.00 124.00   0.50   38.00    --  110.00 -37.00  30.00  176
 11  \w     36.00 126.00   0.50   38.00    --  110.00 -19.00   0.00  180
 12  \w     42.00  67.00   0.50   38.00    --  110.00 -99.00-180.00   50
 13  \w     36.00 121.00   0.50   38.00    --  110.00 -37.00-180.00  170
 14  \w    -72.00  25.00   0.50    9.50    --  -46.62  83.00 170.00  194
 15  \w    -80.00 -44.00   0.50   38.00    --  -88.50  83.00 170.00   72
 16  \w    -98.00 -20.00   0.50    9.50    --  -46.62 -83.00  49.00  156
 17  \w   -106.00 -78.00   0.50    9.50    --  -46.62-125.00 150.00   56
 18  \w   -127.00 -84.00   0.50   38.00    --  -88.50 -83.00  49.00   86
 19  \w   -119.00 -71.00   0.50    9.50    --  -46.62-125.00 -60.00   96
 20  \w   -118.00 -70.00   0.50    9.50    --  -46.62-125.00-150.00   96
 21  \w   -137.00 -73.00   0.50   38.00    --  -88.50-125.00-150.00  128
;
_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      -0.0562891000
_diffrn_orient_matrix_UB_12      0.0288601000
_diffrn_orient_matrix_UB_13      0.0521282000
_diffrn_orient_matrix_UB_21      0.0062538000
_diffrn_orient_matrix_UB_22      -0.0814812000
_diffrn_orient_matrix_UB_23      0.0633506000
_diffrn_orient_matrix_UB_31      0.0451136000
_diffrn_orient_matrix_UB_32      0.0474508000
_diffrn_orient_matrix_UB_33      0.0773351000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8315
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.243
_diffrn_reflns_theta_min         3.510
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.041
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_correction_T_min  0.714
_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            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8315
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0872
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1841P)^2^+7.1314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2574
_refine_ls_wR_factor_ref         0.3036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6898
_reflns_number_total             8315
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9510\% 
 around [1.00 -0.00 0.00] (reciprocal) or [0.98 0.00 0.18] (direct)
;
_cod_data_source_file            d0dt02150d2.cif
_cod_data_source_block           vhis
_cod_depositor_comments
'Adding full bibliography for 7705016--7705019.cif.'
_cod_database_code               7705018
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C N O V'
_shelx_estimated_absorpt_t_max   0.738
_shelx_estimated_absorpt_t_min   0.688
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.495(3)
 0.505(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained planarity
 N5B, N6B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C24B, C25B, C26B
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
N5A \\sim N6A \\sim C26A \\sim C21A \\sim C19A \\sim C22A \\sim C18A \\sim C24A
\\sim C20A \\sim C25A \\sim C17A \\sim C23A: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N5B \\sim N6B \\sim C17B \\sim C18B \\sim C19B \\sim C20B \\sim C21B \\sim C22B
\\sim C23B \\sim C24B \\sim C25B \\sim C26B: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
5. Others
 Sof(C21B)=Sof(N5B)=Sof(C17B)=Sof(C18B)=Sof(C19B)=Sof(C20B)=Sof(C26B)=Sof(N6B)=
 Sof(C22B)=Sof(C23B)=Sof(C24B)=Sof(C25B)=1-FVAR(1)
 Sof(N6A)=Sof(C22A)=Sof(C23A)=Sof(C24A)=Sof(C25A)=Sof(C26A)=Sof(C18A)=
 Sof(C19A)=Sof(C20A)=Sof(C21A)=Sof(N5A)=Sof(C17A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15),
 C16(H16), C3(H3), C5(H5), C6(H6)
6.b Fitted hexagon refined as free rotating group:
 C21B(N5B,C17B,C18B,C19B,C20B), C26B(N6B,C22B,C23B,C24B,C25B), N6A(C22A,C23A,
 C24A,C25A,C26A), C18A(C19A,C20A,C21A,N5A,C17A)
;
_shelx_res_checksum              63334
_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 1.808
_oxdiff_exptl_absorpt_empirical_full_min 0.668
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2