Varying degrees of homostructurality in a series of cocrystals of antimalarial drug 11-azaartemisinin with salicylic acids
Roy, Monalisa; Li, Keyao; Nisar, Madiha; Wong, Lawrence W.-Y.; Sung, Herman H.-Y.; Haynes, Richard K.; Williams, Ian D.; Acta Crystallographica Section C 77 (2021) 262–270; doi:10.1107/S2053229621004460

data_2022371
_publ_section_title
;
 Varying degrees of homostructurality in a series of cocrystals of
 antimalarial drug 11-azaartemisinin with salicylic acids
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              262
_journal_page_last               270
_journal_paper_doi               10.1107/S2053229621004460
_journal_volume                  77
_journal_year                    2021
_chemical_formula_moiety         'C7 H5 Br O3'
_chemical_formula_sum            'C7 H5 Br O3'
_chemical_formula_weight         217.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                81.959(10)
_cell_angle_beta                 73.812(10)
_cell_angle_gamma                71.352(10)
_cell_formula_units_Z            2
_cell_length_a                   6.9581(7)
_cell_length_b                   7.1413(8)
_cell_length_c                   8.0284(9)
_cell_measurement_reflns_used    1508
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2100
_cell_measurement_theta_min      6.5420
_cell_volume                     362.44(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.69a (Rigaku OD, 2020)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1788
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.943
_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     -3.00  33.00   1.00    1.00    --  -39.95  37.00  60.00   36
  2  \w    -64.00  -7.00   1.00    1.00    --  -39.95  37.00  60.00   57
  3  \w    -19.00  73.00   1.00    1.00    --   39.95 -77.00 120.00   92
  4  \w    -36.00  60.00   1.00    1.00    --   39.95 -37.00-150.00   96
  5  \w     75.00 109.00   1.00    2.00    --  104.18-111.00  60.00   34
  6  \w    120.00 178.00   1.00    2.00    --  104.18  77.00  90.00   58
  7  \w    110.00 166.00   1.00    2.00    --  104.18  30.00 150.00   56
  8  \w     65.00  99.00   1.00    2.00    --  104.18 -61.00  60.00   34
  9  \w     64.00 145.00   1.00    2.00    --  104.18 178.00 -60.00   81
 10  \w    102.00 135.00   1.00    2.00    --  104.18 -61.00  60.00   33
 11  \w     81.00 170.00   1.00    2.00    --  104.18  30.00  60.00   89
 12  \w     78.00 107.00   1.00    2.00    --  104.18  30.00 150.00   29
 13  \w     36.00 133.00   1.00    2.00    --  104.18 -61.00 -30.00   97
 14  \w     20.00 105.00   1.00    2.00    --  104.18 -94.00 -90.00   85
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0260723000
_diffrn_orient_matrix_UB_12      -0.1542351000
_diffrn_orient_matrix_UB_13      0.1525991000
_diffrn_orient_matrix_UB_21      0.0002208000
_diffrn_orient_matrix_UB_22      0.1450881000
_diffrn_orient_matrix_UB_23      0.1249950000
_diffrn_orient_matrix_UB_31      -0.2398903000
_diffrn_orient_matrix_UB_32      0.0846204000
_diffrn_orient_matrix_UB_33      0.0337530000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1946
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.204
_diffrn_reflns_theta_min         6.552
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.364
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.69a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_colour_primary    colorless
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_description       block
_exptl_crystal_F_000             212
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0279
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0477P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1275
_reflns_number_total             1347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dv3004sup8.txt
_cod_data_source_block           mona38cult
_cod_depositor_comments
'Adding full bibliography for 2022370--2022375.cif.'
_cod_original_cell_volume        362.43(8)
_cod_database_code               2022371
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.666
_diffrn_oxdiff_digest_frames
;
01a958403cdb6a7be16caa1a06563f8f0900031d8f7
;
_diffrn_oxdiff_digest_hkl
;
012498c4f8cc137c3778ac295847ef588e53ea
;
_reflns_odcompleteness_completeness 98.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C6(H6)
;
_shelx_res_checksum              13883
_shelx_hkl_checksum              91182
_olex2_date_sample_data_collection 2020-04-29
_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 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.912