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_1572124
_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      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-11-28
_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                82.822(5)
_cell_angle_beta                 80.835(6)
_cell_angle_gamma                65.136(7)
_cell_formula_units_Z            2
_cell_length_a                   6.6355(5)
_cell_length_b                   7.3234(5)
_cell_length_c                   15.7183(10)
_cell_measurement_reflns_used    4225
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      77.2210
_cell_measurement_theta_min      2.8600
_cell_volume                     682.74(9)
_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 0.978
_diffrn_measured_fraction_theta_max 0.925
_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     95.00 121.00   0.50    0.09    --  108.21  57.00   0.00   52
  2  \w    142.00 170.00   0.50    0.09    --  108.21  57.00   0.00   56
  3  \w     93.00 167.00   0.50    0.09    --  108.21  19.00   0.00  148
  4  \w     98.00 137.00   0.50    0.09    --  108.21  38.00 -60.00   78
  5  \w    142.00 171.00   0.50    0.09    --  108.21  38.00 -60.00   58
  6  \w     89.00 118.00   0.50    0.05    --   47.23 125.00   0.00   58
  7  \w     64.00 115.00   0.50    0.05    --   47.23 145.00 100.00  102
  8  \w     91.00 116.00   0.50    0.09    --  108.21 145.00 100.00   50
  9  \w     94.00 119.00   0.50    0.05    --   47.23 127.00 -68.00   50
 10  \w     98.00 133.00   0.50    0.09    --  108.21 127.00 -68.00   70
 11  \w     47.00 103.00   0.50    0.09    --  108.21 -77.00  90.00  112
 12  \w     67.00 103.00   0.50    0.09    --  108.21 -77.00  30.00   72
 13  \w     37.00  63.00   0.50    0.09    --  108.21 -57.00   0.00   52
 14  \w     36.00  61.00   0.50    0.09    --  108.21 -57.00 -90.00   50
 15  \w     43.00  88.00   0.50    0.09    --  108.21 -77.00-150.00   90
 16  \w     37.00  93.00   0.50    0.09    --  108.21 -77.00-120.00  112
 17  \w    -20.00  24.00   0.50    0.05    --   47.23 -19.00-150.00   88
 18  \w    -28.00  25.00   0.50    0.05    --   47.23 -19.00  90.00  106
 19  \w     40.00  65.00   0.50    0.09    --  108.21 -57.00  90.00   50
 20  \w     40.00  65.00   0.50    0.09    --  108.21 -57.00 150.00   50
 21  \w     45.00  70.00   0.50    0.05    --   47.23-145.00  47.00   50
 22  \w     60.00 102.00   0.50    0.09    --  108.21-145.00  47.00   84
 23  \w     77.00 102.00   0.50    0.09    --  108.21-127.00-144.00   50
 24  \w     38.00  63.00   0.50    0.05    --   47.23-127.00-144.00   50
 25  \w    -25.00  27.00   0.50    0.05    --  -47.23  19.00  60.00  104
 26  \w     -1.00  27.00   0.50    0.05    --  -47.23  38.00 120.00   56
 27  \w    -42.00 -10.00   0.50    0.05    --  -47.23  38.00 120.00   64
 28  \w   -112.00 -39.00   0.50    0.09    -- -106.00 127.00 -68.00  146
 29  \w    -96.00 -45.00   0.50    0.05    --  -47.23 127.00 -68.00  102
 30  \w   -110.00 -33.00   0.50    0.09    -- -106.00 125.00   0.00  154
 31  \w   -104.00 -79.00   0.50    0.09    -- -106.00 145.00 100.00   50
 32  \w   -101.00 -62.00   0.50    0.05    --  -47.23 145.00 100.00   78
 33  \w    -60.00 -35.00   0.50    0.09    -- -106.00  57.00 -30.00   50
 34  \w    -65.00 -37.00   0.50    0.09    -- -106.00  57.00-120.00   56
 35  \w    -66.00 -41.00   0.50    0.09    -- -106.00  57.00  90.00   50
 36  \w    -64.00 -34.00   0.50    0.09    -- -106.00  57.00 120.00   60
 37  \w   -172.00 -93.00   0.50    0.09    -- -106.00 -38.00 120.00  158
 38  \w   -177.00-101.00   0.50    0.09    -- -106.00 -38.00  90.00  152
 39  \w   -177.00-149.00   0.50    0.09    -- -106.00 -38.00-120.00   56
 40  \w   -132.00-107.00   0.50    0.09    -- -106.00 -38.00-120.00   50
 41  \w   -120.00 -95.00   0.50    0.05    --  -47.23-127.00-144.00   50
 42  \w   -149.00-124.00   0.50    0.09    -- -106.00-127.00-144.00   50
 43  \w   -110.00 -60.00   0.50    0.05    --  -47.23-145.00  47.00  100
 44  \w   -127.00 -97.00   0.50    0.09    -- -106.00-145.00  47.00   60
;
_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      0.1288884000
_diffrn_orient_matrix_UB_12      -0.2242416000
_diffrn_orient_matrix_UB_13      0.0274036000
_diffrn_orient_matrix_UB_21      -0.0554677000
_diffrn_orient_matrix_UB_22      0.0507737000
_diffrn_orient_matrix_UB_23      0.0954553000
_diffrn_orient_matrix_UB_31      -0.2161579000
_diffrn_orient_matrix_UB_32      -0.0334579000
_diffrn_orient_matrix_UB_33      0.0059095000
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6755
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.477
_diffrn_reflns_theta_min         2.854
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59321
_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    1.436
_exptl_crystal_description       plate
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0614
_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^)+(0.1315P)^2^+0.0951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2303
_reflns_number_total             2658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02918f3.cif
_cod_data_source_block           ffa4ch3-2wb-231128_auto
_cod_depositor_comments
'Adding full bibliography for 1572123--1572125.cif.'
_cod_database_code               1572124
_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), C00B(H00B), C00D(H00D), C00E(H00E), C00F(H00F), C00H(H00H),
 C00I(H00I), C00J(H00J)
2.b Idealised Me refined as rotating group:
 C00L(H00A,H00C,H00G)
2.c Idealised tetrahedral OH refined as rotating group:
 O002(H002)
;
_shelx_res_checksum              31612
_shelx_hkl_checksum              56573
_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 2.057
_oxdiff_exptl_absorpt_empirical_full_min 0.445