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_1572123
_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      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-04
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.3091(2)
_cell_length_b                   5.07340(10)
_cell_length_c                   41.7053(4)
_cell_measurement_reflns_used    24943
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.9450
_cell_measurement_theta_min      2.0780
_cell_volume                     2604.45(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.985
_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     37.00 106.00   0.50    0.16    --  107.12 -99.00  90.00  138
  2  \w     37.00 106.00   0.50    0.16    --  107.12 -99.00  60.00  138
  3  \w     38.00 112.00   0.50    0.16    --  107.12-125.00 -30.00  148
  4  \w     37.00 106.00   0.50    0.16    --  107.12 -99.00-120.00  138
  5  \w     19.00  93.00   0.50    0.05    --   47.44-125.00 -90.00  148
  6  \w     37.00 106.00   0.50    0.16    --  107.12 -99.00  90.00  138
  7  \w     35.00 109.00   0.50    0.16    --  107.12 -77.00 120.00  148
  8  \w     35.00  69.00   0.50    0.16    --  107.12 -57.00  90.00   68
  9  \w     35.00  69.00   0.50    0.16    --  107.12 -57.00  30.00   68
 10  \w     35.00  69.00   0.50    0.16    --  107.12 -57.00 -30.00   68
 11  \w    -27.00  30.00   0.50    0.05    --   47.44 -19.00   0.00  114
 12  \w     35.00  69.00   0.50    0.16    --  107.12 -57.00-120.00   68
 13  \w     35.00  69.00   0.50    0.16    --  107.12 -57.00 -90.00   68
 14  \w     94.00 178.00   0.50    0.16    --  107.12  38.00-150.00  168
 15  \w     92.00 178.00   0.50    0.16    --  107.12  57.00  90.00  172
 16  \w     85.00 178.00   0.50    0.16    --  107.12  77.00 150.00  186
 17  \w     85.00 178.00   0.50    0.16    --  107.12  77.00 150.00  186
 18  \w     25.00 120.00   0.50    0.05    --   47.44  77.00 -60.00  190
 19  \w     25.00 120.00   0.50    0.05    --   47.44  77.00-120.00  190
 20  \w     25.00 120.00   0.50    0.05    --   47.44  77.00-180.00  190
 21  \w    -23.00  28.00   0.50    0.05    --  -47.44  19.00 -90.00  102
 22  \w    -39.00  26.00   0.50    0.05    --  -47.44  38.00-120.00  130
 23  \w    -62.00  25.00   0.50    0.05    --  -47.44  57.00-150.00  174
 24  \w    -39.00  26.00   0.50    0.05    --  -47.44  38.00   0.00  130
 25  \w    -62.00 -32.00   0.50    0.16    -- -104.50  57.00-120.00   60
 26  \w    -62.00 -32.00   0.50    0.16    -- -104.50  57.00 -90.00   60
 27  \w   -107.00 -34.00   0.50    0.16    -- -104.50 104.00-155.00  146
 28  \w   -111.00 -35.00   0.50    0.16    -- -104.50 125.00 -60.00  152
 29  \w   -111.00 -35.00   0.50    0.16    -- -104.50 125.00 120.00  152
 30  \w   -174.00 -91.00   0.50    0.16    -- -104.50 -38.00 -30.00  166
 31  \w   -174.00 -91.00   0.50    0.16    -- -104.50 -38.00 -30.00  166
 32  \w   -174.00 -89.00   0.50    0.16    -- -104.50 -57.00 120.00  170
 33  \w   -174.00 -91.00   0.50    0.16    -- -104.50 -49.00  38.40  166
 34  \w   -174.00-106.00   0.50    0.16    -- -104.50 -51.00 -50.71  136
 35  \w   -174.00 -89.00   0.50    0.16    -- -104.50 -57.00-180.00  170
 36  \w   -120.00 -34.00   0.50    0.05    --  -47.44 -38.00-180.00  172
 37  \w   -119.00 -25.00   0.50    0.05    --  -47.44 -77.00  30.00  188
 38  \w   -119.00 -32.00   0.50    0.05    --  -47.44 -57.00  60.00  174
 39  \w   -120.00 -34.00   0.50    0.05    --  -47.44 -38.00  90.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0310431000
_diffrn_orient_matrix_UB_12      -0.0313673000
_diffrn_orient_matrix_UB_13      -0.1416575000
_diffrn_orient_matrix_UB_21      -0.1203999000
_diffrn_orient_matrix_UB_22      0.0058995000
_diffrn_orient_matrix_UB_23      0.0670075000
_diffrn_orient_matrix_UB_31      -0.0141180000
_diffrn_orient_matrix_UB_32      0.0185781000
_diffrn_orient_matrix_UB_33      -0.2602354000
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            45890
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.721
_diffrn_reflns_theta_min         2.119
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       needle
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 2351 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5415
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0540P)^2^+1.1426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                5152
_reflns_number_total             5415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02918f3.cif
_cod_data_source_block           kby-ffa4ch3-y_auto
_cod_depositor_comments
'Adding full bibliography for 1572123--1572125.cif.'
_cod_database_code               1572123
_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:
 N00A(H00A), N00C(H00C), C00D(H00D), C00G(H00G), C00M(H00M), C00P(H00P),
 C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00W(H00W), C00Y(H00Y),
 C00Z(H00Z), C011(H011), C012(H012), C013(H013)
2.b Idealised Me refined as rotating group:
 C014(H01D,H01E,H01F), C015(H01A,H01B,H01C)
2.c Idealised tetrahedral OH refined as rotating group:
 O007(H007)
;
_shelx_res_checksum              67787
_shelx_hkl_checksum              96552
_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 1.356
_oxdiff_exptl_absorpt_empirical_full_min 0.601