Control by one drop of solvent: selective preparation of guest release/trap-triggered interconvertible molecular crystals.
Yakiyama, Yumi; Fujinaka, Takahisa; Nishimura, Mio; Seki, Ryotaro; Sakurai, Hidehiro; Chemical communications (Cambridge, England) 56 (2020) 9687–9690; doi:10.1039/d0cc03408h

data_7126849
_publ_section_title
;
 Control by one drop of solvent: selective preparation of guest
 release/trap-triggered interconvertible molecular crystals.
;
_journal_issue                   67
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9687
_journal_page_last               9690
_journal_paper_doi               10.1039/d0cc03408h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C14 H8 N O2, C0.86 O0.21'
_chemical_formula_sum            'C14.86 H8 N O2.21'
_chemical_formula_weight         235.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-16 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.025(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.5901(3)
_cell_length_b                   18.1053(4)
_cell_length_c                   8.5158(2)
_cell_measurement_reflns_used    20330
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0820
_cell_measurement_theta_min      2.2530
_cell_volume                     2385.65(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.876
_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    -18.00  38.00   0.50   13.45    --   -5.26  19.00   0.00  112
  2  \w    -18.00  68.00   0.50   13.45    --   -5.26  37.00  32.97  172
  3  \w    -18.00  69.00   0.50   13.45    --   -5.26  31.00 -71.25  174
  4  \w    -26.00  27.00   0.50   13.45    --   -5.26 -99.00 120.00  106
  5  \w    -18.00  66.00   0.50   13.45    --   -5.26  19.00  90.00  168
  6  \w    -26.00  28.00   0.50   13.45    --   -5.26 -99.00 -60.00  108
  7  \w    -48.00  25.00   0.50   13.45    --   -5.26   7.00-128.52  146
  8  \w    -18.00  53.00   0.50   13.45    --   -5.26  19.00-120.00  142
  9  \w    -47.00  -2.00   0.50   13.45    --   -5.26 113.00 -88.71   90
 10  \w    -18.00  62.00   0.50   13.45    --   -5.26  32.00 125.71  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0377585000
_diffrn_orient_matrix_UB_12      -0.0116876000
_diffrn_orient_matrix_UB_13      0.0317045000
_diffrn_orient_matrix_UB_21      0.0142420000
_diffrn_orient_matrix_UB_22      -0.0371941000
_diffrn_orient_matrix_UB_23      -0.0014955000
_diffrn_orient_matrix_UB_31      0.0217231000
_diffrn_orient_matrix_UB_32      0.0040563000
_diffrn_orient_matrix_UB_33      0.0776480000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            29531
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.885
_diffrn_reflns_theta_min         2.250
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             975
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.743
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0551
_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^)+(0.1032P)^2^+1.7412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2943
_reflns_number_total             3302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03408h2.cif
_cod_data_source_block           1a-t-BuOH
_cod_depositor_comments
'Adding full bibliography for 7126838--7126851.cif.'
_cod_database_code               7126849
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.975
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: C1S(0.33333) C4S(0.1) C3S(0.15)
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C11(H11), C13(H13), C10(H10), C4(H4), C6(H6), C14(H14), C5(H5)
;
_olex2_exptl_crystal_mounting_method Litholoop
_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 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.749