Co-crystallization of organic chromophore roseolumiflavin and effect on its optical characteristics
Haj Hassani Sohi, Takin; Maass, Felix Lasse Timon; Czekelius, Constantin; Suta, Markus; Vasylyeva, Vera; CrystEngComm  (2022) –; doi:10.1039/D2CE00589A

data_7245239
_publ_section_title
;
 Co-crystallization of organic chromophore roseolumiflavin and effect on
 its optical characteristics
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00589A
_journal_year                    2022
_chemical_formula_moiety         'C14 H15 N5 O2, C4 H2 O4'
_chemical_formula_sum            'C18 H17 N5 O6'
_chemical_formula_weight         399.36
_chemical_name_common            'roseolumiflavin acetylenedicarboxylic acid'
_chemical_name_systematic
'8-(dimethylamino)-7,10-dimethylbenzo[g]pteridine-2,4(3H,10H)-dione but-2-ynedioic acid'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-04-24 deposited with the CCDC.	2022-08-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   6.9603(4)
_cell_length_b                   18.1475(7)
_cell_length_c                   28.0356(12)
_cell_measurement_reflns_used    2174
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      69.2990
_cell_measurement_theta_min      3.1490
_cell_volume                     3541.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_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    -62.00 -27.00   0.50  250.00    --  -90.00  51.00 155.00   70
  2  \w   -156.00 -99.00   0.50  250.00    --  -90.00 -51.00   9.00  114
  3  \w   -138.00 -87.00   0.50  250.00    --  -90.00-113.00 140.00  102
  4  \w    -65.00 -24.00   0.50  250.00    --  -90.00  72.00 -10.00   82
  5  \w     37.00  86.00   0.50  250.00    --  109.41 -72.00-140.00   98
  6  \w    -25.00   1.00   0.50  100.00    --  -49.27  19.00 120.00   52
  7  \w    -29.00  25.00   0.50  100.00    --  -49.27  19.00-120.00  108
  8  \w     -5.00  24.00   0.50  100.00    --   49.27 -38.00 150.00   58
  9  \w    -23.00  21.00   0.50  100.00    --   49.27 -19.00-120.00   88
 10  \w    -13.00  17.00   0.50  100.00    --   49.27 -19.00-150.00   60
 11  \w    -44.00 -18.00   0.50  250.00    --  -90.00  38.00-180.00   52
 12  \w    -47.00 -21.00   0.50  250.00    --  -90.00  38.00 120.00   52
 13  \w    -47.00 -21.00   0.50  250.00    --  -90.00  38.00  90.00   52
 14  \w     40.00  86.00   0.50  250.00    --  109.41 -77.00 120.00   92
 15  \w    118.00 178.00   0.50  250.00    --  109.41 125.00 -60.00  120
;
_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      -0.0178223000
_diffrn_orient_matrix_UB_12      0.0830106000
_diffrn_orient_matrix_UB_13      -0.0107301000
_diffrn_orient_matrix_UB_21      -0.1361026000
_diffrn_orient_matrix_UB_22      0.0090532000
_diffrn_orient_matrix_UB_23      0.0429409000
_diffrn_orient_matrix_UB_31      0.1736478000
_diffrn_orient_matrix_UB_32      0.0154327000
_diffrn_orient_matrix_UB_33      0.0325313000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            14153
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.986
_diffrn_reflns_theta_min         3.153
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'seeding in acetonitrile after liquid-assisted grinding'
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         3325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0945P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2102
_reflns_number_total             3325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00589a2.cif
_cod_data_source_block           R_A
_cod_database_code               7245239
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C18H17N5O6
_olex2_refinement_description
;
;
_shelx_res_checksum              84208
_shelx_hkl_checksum              3482
_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 1.846
_oxdiff_exptl_absorpt_empirical_full_min 0.605