V-shaped chiral hosts based on π-extended hematoxylin
Ma, Mingfang; Dong, Liuyang; Luo, Bo; Hao, Aiyou; Xing, Pengyao; Chemical Communications  (2023) –; doi:10.1039/D3CC03631F

data_7132022
_publ_section_title
;
 V-shaped chiral hosts based on \p-extended hematoxylin
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03631F
_journal_year                    2023
_chemical_formula_moiety         'C32 H9 F4 N4 O6'
_chemical_formula_sum            'C32 H0.25 F4 N4 O6'
_chemical_formula_weight         612.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2023-07-28 deposited with the CCDC.	2023-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4673(3)
_cell_length_b                   11.7335(6)
_cell_length_c                   28.0005(9)
_cell_measurement_reflns_used    4361
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      68.7830
_cell_measurement_theta_min      4.0660
_cell_volume                     2781.88(19)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.930
_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     34.00 103.00   1.00    5.39    --  106.65 -99.00-150.00   69
  2  \w     40.00  66.00   1.00    5.39    --  106.65 -57.00 -30.00   26
  3  \w     44.00  70.00   1.00    5.39    --  106.65 -60.00 117.00   26
  4  \w     92.00 178.00   1.00    5.39    --  106.65  57.00  60.00   86
  5  \w   -159.00 -73.00   1.00    5.39    --  -91.75 -76.00  -7.00   86
  6  \w   -163.00-138.00   1.00    5.39    --  -91.75 -57.00  60.00   25
  7  \w   -128.00 -77.00   1.00    5.39    --  -91.75 -57.00  60.00   51
  8  \w   -121.00 -26.00   1.00    0.91    --  -48.42 -76.00  -7.00   95
  9  \w    -27.00  27.00   1.00    0.91    --  -48.42  19.00 -90.00   54
 10  \w    -69.00 -31.00   1.00    5.39    --  -91.75  60.00-102.00   38
 11  \w   -117.00 -72.00   1.00    5.39    --  -91.75  88.00   4.00   45
 12  \w    -56.00 -30.00   1.00    5.39    --  -91.75  88.00   4.00   26
 13  \w    -65.00 -20.00   1.00    5.39    --  -91.75  57.00  90.00   45
;
_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      -0.0850772000
_diffrn_orient_matrix_UB_12      -0.0701611000
_diffrn_orient_matrix_UB_13      -0.0386746000
_diffrn_orient_matrix_UB_21      -0.1247641000
_diffrn_orient_matrix_UB_22      0.0948959000
_diffrn_orient_matrix_UB_23      -0.0051560000
_diffrn_orient_matrix_UB_31      0.1015159000
_diffrn_orient_matrix_UB_32      0.0574890000
_diffrn_orient_matrix_UB_33      -0.0387974000
_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  0.0627
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            13212
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.014
_diffrn_reflns_theta_min         3.157
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       plate
_exptl_crystal_F_000             1217
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Flack x determined using 1289 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.65(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.530
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.530
_refine_ls_R_factor_all          0.1581
_refine_ls_R_factor_gt           0.1410
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3637
_refine_ls_wR_factor_ref         0.3817
_reflns_Friedel_coverage         0.705
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.865
_reflns_number_gt                4032
_reflns_number_total             5247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03631f2.cif
_cod_data_source_block           20221124mmf_auto
_cod_database_code               7132022
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CNOF
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.949
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C4(H4), C27(H27), C5(H5), C26(H26)
2.d Idealised tetrahedral OH refined as rotating group:
 O42(H42)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4700
_shelx_hkl_checksum              3238
_shelx_fab_checksum              83256
_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.710