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_2022370
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 97.320(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.8053(2)
_cell_length_b                   14.6610(8)
_cell_length_c                   12.9396(7)
_cell_measurement_reflns_used    913
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2860
_cell_measurement_theta_min      6.8760
_cell_volume                     716.01(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 0.987
_diffrn_measured_fraction_theta_max 0.951
_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 103.00 160.00 1.00 3.00 -- 104.18 77.00 -30.00 57 
2 \w -52.00 -14.00 1.00 1.00 -- -40.20 -37.00 60.00 38 
3 \w -114.00 -58.00 1.00 1.00 -- -40.20 -37.00 60.00 56 
4 \w 12.00 57.00 1.00 1.00 -- 40.20 57.00-180.00 45 
5 \w 58.00 105.00 1.00 1.00 -- 40.20 57.00-180.00 47 
6 \w 33.00 102.00 1.00 3.00 -- 104.18-111.00 90.00 69 
7 \w 109.00 176.00 1.00 3.00 -- 104.18 77.00 90.00 67 
8 \w 46.00 121.00 1.00 3.00 -- 104.18 -45.00 30.00 75
;
_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      0.3249518000
_diffrn_orient_matrix_UB_12      0.0094537000
_diffrn_orient_matrix_UB_13      -0.0591250000
_diffrn_orient_matrix_UB_21      0.2411295000
_diffrn_orient_matrix_UB_22      -0.0348564000
_diffrn_orient_matrix_UB_23      0.0967109000
_diffrn_orient_matrix_UB_31      -0.0541329000
_diffrn_orient_matrix_UB_32      -0.0986421000
_diffrn_orient_matrix_UB_33      -0.0398579000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2212
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.303
_diffrn_reflns_theta_min         6.900
_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    7.455
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65868
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_description       needle
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0626P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1147
_reflns_number_total             1345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dv3004sup9.txt
_cod_data_source_block           mona39cult
_cod_depositor_comments
'Adding full bibliography for 2022370--2022375.cif.'
_cod_original_cell_volume        716.02(7)
_cod_database_code               2022370
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.587
_diffrn_oxdiff_digest_frames
;
017761e0a5a2d86baf08def9d8b4d3e99500028c205
;
_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:
 C6(H6), C5(H5), C3(H3A)
;
_shelx_res_checksum              60498
_shelx_hkl_checksum              72969
_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_min 0.714