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_7705016
_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         'C30 H26 N6 O11 V2, 0.5(H2 O2), 2(H2 O)'
_chemical_formula_sum            'C30 H31 N6 O14 V2'
_chemical_formula_weight         801.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_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                 103.274(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6292(3)
_cell_length_b                   18.1010(3)
_cell_length_c                   15.3035(3)
_cell_measurement_reflns_used    6015
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      67.9760
_cell_measurement_theta_min      3.8460
_cell_volume                     3944.15(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     15.00  41.00   0.50    1.14    --    0.00  28.00-104.00   52
  2  \w     58.00  83.00   0.50    1.14    --    0.00  28.00-104.00   50
  3  \w    -83.00  21.00   0.50    4.54    --  -58.33  28.00-104.00  208
  4  \w   -142.00 -63.00   0.50    4.54    --  -58.33 -28.00  93.00  158
  5  \w   -116.00 -69.00   0.50    4.54    --  -98.50 -28.00  93.00   94
  6  \w     95.00 178.00   0.50    4.54    --  116.65  28.00-104.00  166
  7  \w     32.00 111.00   0.50    4.54    --  116.65 -28.00  93.00  158
  8  \w    -84.00 -55.00   0.50    1.14    --    0.00-178.00-120.00   58
  9  \w    -69.00   4.00   0.50    1.14    --    0.00 -28.00  93.00  146
 10  \w     92.00 138.00   0.50    4.54    --   58.33 125.00  90.00   92
 11  \w    108.00 133.00   0.50    4.54    --   58.33 125.00   0.00   50
 12  \w     92.00 139.00   0.50    4.54    --   58.33 125.00 120.00   94
 13  \w    -83.00 -21.00   0.50    4.54    --  -98.50 111.00-180.00  124
 14  \w    -71.00 -46.00   0.50    4.54    --  -98.50 111.00 -30.00   50
 15  \w    -85.00 -59.00   0.50    4.54    --  -98.50 111.00   0.00   52
 16  \w   -113.00 -76.00   0.50    4.54    --  -98.50 -77.00 150.00   74
 17  \w    -68.00 -21.00   0.50    4.54    --  -98.50 111.00 -90.00   94
 18  \w   -170.00-140.00   0.50    4.54    --  -98.50 -77.00 150.00   60
 19  \w     39.00 109.00   0.50    4.54    --  116.65-111.00 -60.00  140
 20  \w    150.00 176.00   0.50    4.54    --  116.65 111.00 120.00   52
 21  \w    101.00 138.00   0.50    4.54    --  116.65 111.00 120.00   74
 22  \w     47.00  90.00   0.50    4.54    --  116.65 -94.00-120.00   86
 23  \w     34.00 109.00   0.50    4.54    --  116.65-111.00 150.00  150
 24  \w     84.00 129.00   0.50    4.54    --  116.65 -45.00-150.00   90
 25  \w     84.00 109.00   0.50    4.54    --  116.65 -94.00 -90.00   50
 26  \w     58.00  83.00   0.50    4.54    --  116.65 -94.00-180.00   50
 27  \w     38.00  63.00   0.50    4.54    --  116.65 -94.00 -90.00   50
;
_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      -0.1000147000
_diffrn_orient_matrix_UB_12      -0.0307334000
_diffrn_orient_matrix_UB_13      -0.0346651000
_diffrn_orient_matrix_UB_21      0.0132369000
_diffrn_orient_matrix_UB_22      0.0029791000
_diffrn_orient_matrix_UB_23      -0.0969496000
_diffrn_orient_matrix_UB_31      0.0392537000
_diffrn_orient_matrix_UB_32      -0.0792629000
_diffrn_orient_matrix_UB_33      0.0097684000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10637
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         3.843
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.565
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.803
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             1644
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.960
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0583P)^2^+12.9753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3395
_reflns_number_total             3605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02150d2.cif
_cod_data_source_block           vgln_sq
_cod_depositor_comments
'Adding full bibliography for 7705016--7705019.cif.'
_cod_database_code               7705016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C128 H112 N44 O56 V8 '
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.804
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: H2W(0.5)
3.a Free rotating group:
 O2W(H2W), O1W(H1Wa,H1Wb)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b), C3(H3a,H3b)
3.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C9(H9), C12(H12), C13(H13), C8(H8), C7(H7), C6(H6)
;
_shelx_res_checksum              95792
_shelx_fab_checksum              40299
_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 1.411
_oxdiff_exptl_absorpt_empirical_full_min 0.763