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_7705019
_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_absolute_configuration rmad
_chemical_formula_moiety         'O3 V, C6 H15 N4 O2, 0.5(H2 O)'
_chemical_formula_sum            'C6 H16 N4 O5.5 V'
_chemical_formula_weight         283.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-24 deposited with the CCDC.	2020-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.374(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8138(6)
_cell_length_b                   5.1262(2)
_cell_length_c                   17.0635(7)
_cell_measurement_reflns_used    3988
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3620
_cell_measurement_theta_min      3.4970
_cell_volume                     1117.34(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.21a (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 1.000
_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   -115.00 -28.00   0.50    0.05    --  -46.75 -63.00  26.00  174
  2  \w    -64.00  23.00   0.50    0.05    --  -46.75  63.00 162.00  174
  3  \w     13.00  53.00   0.50    0.05    --   46.75 -63.00  26.00   80
  4  \w   -139.00-114.00   0.50    0.18    --  -88.50 -63.00  26.00   50
  5  \w    -73.00 -46.00   0.50    0.18    --  -88.50  63.00 162.00   54
  6  \w     89.00 174.00   0.50    0.18    --  107.31  63.00 162.00  170
  7  \w     35.00 126.00   0.50    0.18    --  107.31 -63.00  26.00  182
  8  \w   -115.00 -71.00   0.50    0.05    --  -46.75-125.00 150.00   88
  9  \w     42.00  67.00   0.50    0.05    --   46.75  57.00-150.00   50
 10  \w     71.00  99.00   0.50    0.05    --   46.75  57.00-150.00   56
 11  \w   -116.00 -87.00   0.50    0.18    --  -88.50 -61.00 -30.00   58
 12  \w   -123.00 -75.00   0.50    0.18    --  -88.50 -30.00 -90.00   96
 13  \w   -140.00 -74.00   0.50    0.18    --  -88.50 -45.00-120.00  132
 14  \w   -149.00-122.00   0.50    0.18    --  -88.50 -61.00 -30.00   54
 15  \w    -64.00 -15.00   0.50    0.18    --  -88.50 125.00-180.00   98
 16  \w   -111.00 -86.00   0.50    0.18    --  -88.50 -77.00-120.00   50
 17  \w    148.00 176.00   0.50    0.18    --  107.31  45.00  90.00   56
 18  \w    138.00 166.00   0.50    0.18    --  107.31  45.00 -90.00   56
 19  \w     93.00 132.00   0.50    0.18    --  107.31  45.00 -90.00   78
 20  \w     36.00 114.00   0.50    0.18    --  107.31-125.00   0.00  156
 21  \w    101.00 127.00   0.50    0.18    --  107.31  45.00-120.00   52
 22  \w    100.00 141.00   0.50    0.18    --  107.31  45.00  90.00   82
 23  \w     63.00  93.00   0.50    0.18    --  107.31 -94.00 -90.00   60
 24  \w     95.00 121.00   0.50    0.18    --  107.31 125.00   0.00   52
 25  \w     71.00 117.00   0.50    0.18    --  107.31-125.00-180.00   92
 26  \w    144.00 173.00   0.50    0.18    --  107.31  77.00 -30.00   58
 27  \w     39.00  65.00   0.50    0.18    --  107.31-125.00-180.00   52
 28  \w     90.00 130.00   0.50    0.18    --  107.31  77.00 -30.00   80
 29  \w    148.00 173.00   0.50    0.18    --  107.31 125.00   0.00   50
 30  \w     96.00 123.00   0.50    0.18    --  107.31  30.00 -60.00   54
 31  \w     91.00 117.00   0.50    0.18    --  107.31  61.00 -90.00   52
 32  \w    138.00 174.00   0.50    0.18    --  107.31  45.00-120.00   72
;
_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      0.0289857000
_diffrn_orient_matrix_UB_12      0.0179681000
_diffrn_orient_matrix_UB_13      0.0964029000
_diffrn_orient_matrix_UB_21      0.0806174000
_diffrn_orient_matrix_UB_22      -0.2204089000
_diffrn_orient_matrix_UB_23      0.0138854000
_diffrn_orient_matrix_UB_31      0.0848886000
_diffrn_orient_matrix_UB_32      0.2035216000
_diffrn_orient_matrix_UB_33      0.0066919000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5491
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.660
_diffrn_reflns_theta_min         3.527
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.666
_exptl_absorpt_correction_T_max  0.216
_exptl_absorpt_correction_T_min  0.199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.21a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light gray'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 867 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2229
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0502P)^2^+5.4177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1165
_reflns_Friedel_coverage         0.732
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.897
_reflns_number_gt                2153
_reflns_number_total             2229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02150d2.cif
_cod_data_source_block           exp_3485
_cod_depositor_comments
'Adding full bibliography for 7705016--7705019.cif.'
_cod_original_formula_sum        'C6 H16 N4 O5.50 V'
_cod_database_code               7705019
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C28 H64 N12 O22 V4 '
_shelx_estimated_absorpt_t_max   0.309
_shelx_estimated_absorpt_t_min   0.207
_reflns_odcompleteness_completeness 100.00
_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 C(H,H) groups, All N(H) groups, All N(H,H) groups, All
  N(H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H00O(0.5) H00P(0.5)
3.a Free rotating group:
 O006(H00O,H00P)
3.b Rotating group:
 N007(H00A,H00B)
3.c Ternary CH refined with riding coordinates:
 C00H(H00N)
3.d Secondary CH2 refined with riding coordinates:
 C00E(H00H,H00I), C00F(H00J,H00K), C00G(H00L,H00M)
3.e Aromatic/amide H refined with riding coordinates:
 N009(H009)
3.f X=CH2 refined with riding coordinates:
 N00B(H00F,H00G)
3.g Idealised Me refined as rotating group:
 N00A(H00C,H00D,H00E)
;
_shelx_res_checksum              90474
_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 1.306
_oxdiff_exptl_absorpt_empirical_full_min 0.729