Croconic Acid Doped Glycine Single Crystals: Growth, Crystal Structure, UV-Vis, FTIR, Raman and Photoluminescence Spectroscopy
Balashova, Elena; Levin, Aleksandr A.; Davydov, Valery; Smirnov, Alexander; Starukhin, Anatoly; Pavlov, Sergey; Krichevtsov, Boris; Zolotarev, Andrey; Zhang, Hongjun; Li, Fangzhe; Ke, Hua; Crystals 12 (2022) 1342–; doi:10.3390/cryst12101342

data_1567735
_publ_section_title
;
 Croconic Acid Doped Glycine Single Crystals: Growth, Crystal Structure,
 UV-Vis, FTIR, Raman and Photoluminescence Spectroscopy
;
_journal_issue                   10
_journal_name_full               Crystals
_journal_page_first              1342
_journal_paper_doi               10.3390/cryst12101342
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C2 H5 N O2'
_chemical_formula_sum            'C2 H5 N O2'
_chemical_formula_weight         75.07
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   6.9848(3)
_cell_length_b                   6.9848(3)
_cell_length_c                   5.4744(2)
_cell_measurement_reflns_used    1040
_cell_measurement_temperature    100.0(7)
_cell_measurement_theta_max      76.8740
_cell_measurement_theta_min      7.3130
_cell_volume                     231.300(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_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      100.0(7)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_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     26.00  70.00   0.50    0.05    --   47.35  77.00-150.00   88
  2  \w     31.00  72.00   0.50    0.05    --   47.35  77.00 -60.00   82
  3  \w    -23.00  25.00   0.50    0.05    --  -47.35  19.00 -60.00   96
  4  \w    -26.00  -1.00   0.50    0.05    --  -47.35  19.00 150.00   50
  5  \w    -37.00  -3.00   0.50    0.05    --  -47.35  40.00 157.00   68
  6  \w     41.00  91.00   0.50    0.05    --   47.35  40.00 157.00  100
  7  \w    103.00 133.00   0.50    0.06    --  113.25  40.00 157.00   60
  8  \w    141.00 167.00   0.50    0.06    --  113.25  40.00 157.00   52
  9  \w    104.00 147.00   0.50    0.06    --  113.25  15.00-150.00   86
 10  \w     78.00 119.00   0.50    0.05    --   47.35 125.00 -60.00   82
 11  \w     10.00  42.00   0.50    0.05    --   47.35 -40.00   3.00   64
 12  \w     45.00  71.00   0.50    0.06    --  113.25 -61.00   0.00   52
 13  \w     44.00  71.00   0.50    0.06    --  113.25 -61.00  30.00   54
 14  \w     42.00  67.00   0.50    0.06    --  113.25 -61.00  90.00   50
 15  \w     45.00  70.00   0.50    0.06    --  113.25 -61.00 120.00   50
 16  \w     48.00  76.00   0.50    0.06    --  113.25 -94.00  90.00   56
 17  \w     43.00  69.00   0.50    0.06    --  113.25-125.00 150.00   52
 18  \w     81.00 106.00   0.50    0.06    --  113.25 -94.00  90.00   50
 19  \w     79.00 104.00   0.50    0.06    --  113.25 -94.00  30.00   50
 20  \w     48.00  92.00   0.50    0.06    --  113.25 -94.00   0.00   88
 21  \w   -105.00 -79.00   0.50    0.06    -- -106.00  77.00 -60.00   52
 22  \w    -68.00 -38.00   0.50    0.06    -- -106.00  77.00 -60.00   60
 23  \w    -70.00 -44.00   0.50    0.06    -- -106.00  61.00 -30.00   52
 24  \w    -69.00 -34.00   0.50    0.06    -- -106.00  61.00   0.00   70
 25  \w    -69.00 -44.00   0.50    0.06    -- -106.00  61.00 -60.00   50
 26  \w    -68.00 -41.00   0.50    0.06    -- -106.00  61.00 -90.00   54
 27  \w    -70.00 -38.00   0.50    0.06    -- -106.00  61.00-120.00   64
 28  \w    -66.00 -38.00   0.50    0.06    -- -106.00  61.00-180.00   56
 29  \w   -135.00-101.00   0.50    0.06    -- -106.00 -40.00   3.00   68
 30  \w   -163.00-131.00   0.50    0.06    -- -106.00 -77.00 -60.00   64
 31  \w   -117.00 -92.00   0.50    0.06    -- -106.00 -77.00 -90.00   50
 32  \w   -121.50 -84.00   0.50    0.06    -- -106.00 -77.00-120.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1907910000
_diffrn_orient_matrix_UB_12      0.0764160000
_diffrn_orient_matrix_UB_13      -0.1845784000
_diffrn_orient_matrix_UB_21      -0.1534137000
_diffrn_orient_matrix_UB_22      -0.1869926000
_diffrn_orient_matrix_UB_23      -0.1751576000
_diffrn_orient_matrix_UB_31      -0.0699186000
_diffrn_orient_matrix_UB_32      0.1552976000
_diffrn_orient_matrix_UB_33      -0.1198695000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3120
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.178
_diffrn_reflns_theta_min         7.322
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       prism
_exptl_crystal_F_000             120
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 315 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.07(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         645
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0442P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                645
_reflns_number_total             645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            gamma_GlyCA.cif
_cod_data_source_block           g_GlyCA
_cod_original_cell_volume        231.30(2)
_cod_database_code               1567735
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C10 H10 N5 O5'
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.500(5)
 0.500(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              24266
_shelx_hkl_checksum              30118
_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 1.494
_oxdiff_exptl_absorpt_empirical_full_min 0.700