Discovery and exploration of new solid forms of dipeptide: l-alanyl-l-glutamine
Fu, Jinqiu; Cai, Mengyang; Shi, Yuzhong; Hou, Yihang; Guo, Rongxi; Wang, Chiyi; Zhao, Jingjing; Zhuang, Wei; Ying, Hanjie; Yang, Pengpeng; Zhang, Keke; CrystEngComm 26 (2024) 943–950; doi:10.1039/D3CE00957B

data_7247955
_publ_section_title
;
 Discovery and exploration of new solid forms of dipeptide:
 l-alanyl-l-glutamine
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              943
_journal_page_last               950
_journal_paper_doi               10.1039/D3CE00957B
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C8 H15 N3 O4'
_chemical_formula_sum            'C8 H15 N3 O4'
_chemical_formula_weight         217.23
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-11-10 deposited with the CCDC.	2024-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                96.682(4)
_cell_angle_beta                 95.901(4)
_cell_angle_gamma                106.738(3)
_cell_formula_units_Z            2
_cell_length_a                   5.02400(10)
_cell_length_b                   8.6623(3)
_cell_length_c                   14.2346(9)
_cell_measurement_reflns_used    4830
_cell_measurement_temperature    294.15
_cell_measurement_theta_max      31.4340
_cell_measurement_theta_min      2.4730
_cell_volume                     583.12(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      294.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_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   -110.00  70.00   0.50    2.00    --  -20.00   0.00  90.00  360
  2  \w   -110.00  55.00   0.50    2.00    --  -20.00   0.00 180.00  330
  3  \w   -110.00   7.00   0.50    2.00    --  -20.00 -70.00 180.00  234
  4  \w   -110.00   7.00   0.50    2.00    --  -20.00 -70.00   0.00  234
  5  \w   -110.00  -2.00   0.50    2.00    --  -20.00 -70.00  90.00  216
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku mm007 Saturn 944+'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0407743000
_diffrn_orient_matrix_UB_12      -0.0347775000
_diffrn_orient_matrix_UB_13      -0.0488742000
_diffrn_orient_matrix_UB_21      -0.0389247000
_diffrn_orient_matrix_UB_22      -0.0791176000
_diffrn_orient_matrix_UB_23      0.0131434000
_diffrn_orient_matrix_UB_31      -0.1378895000
_diffrn_orient_matrix_UB_32      0.0042369000
_diffrn_orient_matrix_UB_33      0.0028931000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9754
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.485
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_description       block
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 1382 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4307
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0771
_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^)+(0.1551P)^2^+0.0507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2056
_refine_ls_wR_factor_ref         0.2189
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.833
_reflns_Friedel_fraction_max     0.813
_reflns_number_gt                3808
_reflns_number_total             4307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00957b2.cif
_cod_data_source_block           r20230406b_autored
_cod_depositor_comments
;
Adding full bibliography for 7247952--7247957.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C16 H30 N6 O8'
_cod_original_formula_weight         434.46
_cod_original_formula_moiety         '2(C8 H15 N3 O4)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        583.12(4)
_cod_database_code               7247955
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.972
_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 C(H,H,H) groups
2. Restrained distances
 N2-H2
 0.9 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7), C12(H12), C15(H15)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3D,H3E), C10(H10A,H10B), C11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
 N5(H5)
3.d X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N4(H4A,H4B)
3.e Idealised Me refined as rotating group:
 N3(H3A,H3B,H3C), C8(H8A,H8B,H8C), N6(H6A,H6B,H6C), C16(H16A,H16B,H16C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69923
_shelx_fab_checksum              96847
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.430
_oxdiff_exptl_absorpt_empirical_full_min 0.518