Trimodal operation of a robust smart organic crystal.
Wu, Wenbo; Chen, Kui; Yu, Hui; Zhu, Jiaxuan; Feng, Yaoguang; Wang, Jingkang; Huang, Xin; Li, Liang; Hao, Hongxun; Wang, Ting; Wang, Na; Naumov, Panče; Chemical science 15 (2024) 9287–9297; doi:10.1039/d4sc02152e

data_1571604
_publ_section_title
;
 Trimodal operation of a robust smart organic crystal.
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_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              9287
_journal_page_last               9297
_journal_paper_doi               10.1039/d4sc02152e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C15 H10 Cl F3 N2 O2'
_chemical_formula_sum            'C15 H10 Cl F3 N2 O2'
_chemical_formula_weight         342.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
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2024-03-20 deposited with the CCDC.	2024-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.4500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5603(2)
_cell_length_b                   10.25450(10)
_cell_length_c                   7.79550(10)
_cell_measurement_reflns_used    6966
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      78.3570
_cell_measurement_theta_min      4.7980
_cell_volume                     1479.22(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_temperature      113.15
_diffrn_detector                 PILATUS
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.967
_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    -83.00 -27.00   1.00    1.00    --  -49.00 -72.00   0.00   56
  2  \w    -77.00  17.00   1.00    1.00    --  -49.00  57.00-150.00   94
  3  \w   -133.00-107.00   1.00    1.00    --  -49.00 -72.00 -30.00   26
  4  \w   -136.00 -99.00   1.00    1.00    --  -49.00 -72.00   0.00   37
  5  \w    -98.00 -17.00   1.00    1.00    --  -49.00 -72.00 -30.00   81
  6  \w   -199.00-138.00   1.00    1.00    -- -110.00 -57.00 -60.00   61
  7  \w   -128.00-101.00   1.00    1.00    -- -110.00 -72.00 150.00   27
  8  \w   -143.00 -32.00   1.00    1.00    -- -110.00  38.00  90.00  111
  9  \w   -104.00 -46.00   1.00    1.00    -- -110.00  72.00 -60.00   58
 10  \w   -129.00 -77.00   1.00    1.00    -- -110.00 -38.00  60.00   52
 11  \w   -141.00 -25.00   1.00    1.00    -- -110.00  72.00-150.00  116
 12  \w   -197.00-134.00   1.00    1.00    -- -110.00 -72.00 150.00   63
 13  \w   -173.00-132.00   1.00    1.00    -- -110.00 -38.00  60.00   41
 14  \w   -124.00 -73.00   1.00    1.00    -- -110.00  72.00-180.00   51
 15  \w   -122.00 -81.00   1.00    1.00    -- -110.00 -57.00 -60.00   41
 16  \w    -53.00 -28.00   1.00    1.00    -- -110.00  57.00 -90.00   25
 17  \w   -139.00 -86.00   1.00    1.00    -- -110.00  72.00 -90.00   53
 18  \w    -93.00 -67.00   1.00    1.00    -- -110.00  57.00-180.00   26
 19  \w   -131.00 -86.00   1.00    1.00    -- -110.00  72.00 -30.00   45
 20  \w   -118.00 -92.00   1.00    1.00    -- -110.00  57.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0224867000
_diffrn_orient_matrix_UB_12      0.1417504000
_diffrn_orient_matrix_UB_13      0.0265255000
_diffrn_orient_matrix_UB_21      -0.0151745000
_diffrn_orient_matrix_UB_22      0.0480404000
_diffrn_orient_matrix_UB_23      -0.0788313000
_diffrn_orient_matrix_UB_31      -0.1964797000
_diffrn_orient_matrix_UB_32      0.0125222000
_diffrn_orient_matrix_UB_33      0.0026862000
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10857
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.033
_diffrn_reflns_theta_min         4.780
_diffrn_source                   Rotating-anode
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3087
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+0.7653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2841
_reflns_number_total             3087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02152e19.cif
_cod_data_source_block           CTBB_113K_Form_I
_cod_depositor_comments
'Adding full bibliography for 1571604--1571609.cif.'
_cod_database_code               1571604
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.641
_shelx_estimated_absorpt_t_min   0.550
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F1A-F2A \\sim F1A-F3A \\sim F2A-F3A
 with sigma of 0.02
 C15-F1 \\sim C15-F2 \\sim C15-F3 \\sim C15-F3A \\sim C15-F2A \\sim C15-F1A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F1A \\sim F2A \\sim F3A: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F1A) \\sim
Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14)
;
_shelx_res_checksum              82449
_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 1.619
_oxdiff_exptl_absorpt_empirical_full_min 0.670