Preparation of intrinsically fragile bent crystals.
Seki, Tomohiro; Kobayashi, Shiori; Ishikawa, Rintaro; Yano, Keigo; Matsuo, Takumi; Hayashi, Shotaro; Chemical science 15 (2024) 12258–12263; doi:10.1039/d4sc02918f

data_1572125
_publ_section_title
;
 Preparation of intrinsically fragile bent crystals.
;
_journal_issue                   31
_journal_name_full               'Chemical science'
_journal_page_first              12258
_journal_page_last               12263
_journal_paper_doi               10.1039/d4sc02918f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C15 H12 F3 N O2'
_chemical_formula_sum            'C15 H12 F3 N O2'
_chemical_formula_weight         295.26
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-24 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.674(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.9586(2)
_cell_length_b                   11.2709(4)
_cell_length_c                   24.1190(8)
_cell_measurement_reflns_used    4251
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.0810
_cell_measurement_theta_min      3.6870
_cell_volume                     1341.36(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_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      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 0.998
_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    -66.00  -6.00   0.50    1.07    --  -47.48 103.00 -73.00  120
  2  \w     16.00  67.00   0.50    1.07    --   47.48-103.00-174.00  102
  3  \w   -176.00-114.00   0.50    4.30    -- -106.00-103.00-174.00  124
  4  \w    -98.00 -72.00   0.50    4.30    -- -106.00 103.00 -73.00   52
  5  \w     51.00 107.00   0.50    4.30    --  108.21-103.00-174.00  112
  6  \w     90.00 155.00   0.50    4.30    --  108.21 103.00 -73.00  130
  7  \w   -113.00 -74.00   0.50    1.07    --  -47.48-125.00  60.00   78
  8  \w   -104.00 -73.00   0.50    1.07    --  -47.48-125.00-120.00   62
  9  \w   -117.00 -78.00   0.50    1.07    --  -47.48-125.00 -90.00   78
 10  \w     82.00 116.00   0.50    1.07    --   47.48 125.00-150.00   68
 11  \w     82.00 107.00   0.50    1.07    --   47.48 125.00 120.00   50
 12  \w    -60.00 -34.00   0.50    4.30    -- -106.00  57.00 150.00   52
 13  \w   -164.00-138.00   0.50    4.30    -- -106.00 -99.00 120.00   52
 14  \w    -67.00 -42.00   0.50    4.30    -- -106.00  57.00  60.00   50
 15  \w    -67.00 -42.00   0.50    4.30    -- -106.00  57.00  30.00   50
 16  \w    -61.00 -35.00   0.50    4.30    -- -106.00  57.00-120.00   52
 17  \w    -67.00 -41.00   0.50    4.30    -- -106.00  57.00 120.00   52
 18  \w   -125.00 -97.00   0.50    4.30    -- -106.00 -38.00  90.00   56
 19  \w   -133.00 -91.00   0.50    4.30    -- -106.00 -99.00 120.00   84
 20  \w   -168.00-142.00   0.50    4.30    -- -106.00 -38.00  90.00   52
 21  \w    -63.00 -38.00   0.50    4.30    -- -106.00  57.00  90.00   50
 22  \w     35.00  60.00   0.50    4.30    --  108.21 -57.00-180.00   50
 23  \w     56.00  81.00   0.50    4.30    --  108.21 -77.00-150.00   50
 24  \w     72.00  98.00   0.50    4.30    --  108.21 -77.00-180.00   52
 25  \w     37.00  62.00   0.50    4.30    --  108.21 -77.00-180.00   50
 26  \w     37.00  64.00   0.50    4.30    --  108.21 -57.00-120.00   54
 27  \w     35.00  60.00   0.50    4.30    --  108.21 -57.00 -30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.2388669000
_diffrn_orient_matrix_UB_12      0.0725405000
_diffrn_orient_matrix_UB_13      0.0183552000
_diffrn_orient_matrix_UB_21      0.1860072000
_diffrn_orient_matrix_UB_22      0.1091910000
_diffrn_orient_matrix_UB_23      0.0094477000
_diffrn_orient_matrix_UB_31      -0.0760454000
_diffrn_orient_matrix_UB_32      0.0388272000
_diffrn_orient_matrix_UB_33      -0.0607787000
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            8206
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.294
_diffrn_reflns_theta_min         3.683
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.102a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       needle
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0715P)^2^+0.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2343
_reflns_number_total             2708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02918f3.cif
_cod_data_source_block           ffa4ch3-8_auto
_cod_depositor_comments
'Adding full bibliography for 1572123--1572125.cif.'
_cod_database_code               1572125
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHONF
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N006(H006), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H),
 C00I(H00I), C00L(H00L)
2.b Idealised Me refined as rotating group:
 C00K(H00A,H00B,H00C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              35127
_shelx_hkl_checksum              3109
_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 2.263
_oxdiff_exptl_absorpt_empirical_full_min 0.393