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_7126850
_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, C1.5'
_chemical_formula_sum            'C15.5 H11.3 N O2'
_chemical_formula_weight         243.55
_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             2020-04-14
_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                 97.664(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.4960(3)
_cell_length_b                   17.8919(3)
_cell_length_c                   8.5454(2)
_cell_measurement_reflns_used    20036
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      31.1740
_cell_measurement_theta_min      2.3390
_cell_volume                     2348.07(8)
_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      123(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.878
_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    -16.00  14.00   0.50    5.27    --   -5.34  19.00   0.00   60
  2  \w     17.00  70.00   0.50    5.27    --   -5.34  19.00   0.00  106
  3  \w     31.00  57.00   0.50    5.27    --   -5.34  33.00 -38.91   52
  4  \w    -18.00  68.00   0.50    5.27    --   -5.34  33.00  43.00  172
  5  \w    -18.00  66.00   0.50    5.27    --   -5.34  30.00-129.86  168
  6  \w    -24.00  19.00   0.50    5.27    --   -5.34 -99.00-120.00   86
  7  \w    -25.00  28.00   0.50    5.27    --   -5.34 -99.00 -60.00  106
  8  \w    -26.00  19.00   0.50    5.27    --   -5.34 -99.00  90.00   90
  9  \w    -18.00  69.00   0.50    5.27    --   -5.34  19.00 -90.00  174
 10  \w    -18.00  60.00   0.50    5.27    --   -5.34  19.00-180.00  156
 11  \w    -18.00  24.00   0.50    5.27    --   -5.34  33.00 -38.91   84
 12  \w    -18.00  67.00   0.50    5.27    --   -5.34  36.00  88.23  170
;
_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      0.0154417000
_diffrn_orient_matrix_UB_12      0.0365850000
_diffrn_orient_matrix_UB_13      0.0196928000
_diffrn_orient_matrix_UB_21      0.0288282000
_diffrn_orient_matrix_UB_22      -0.0146360000
_diffrn_orient_matrix_UB_23      0.0641422000
_diffrn_orient_matrix_UB_31      0.0326065000
_diffrn_orient_matrix_UB_32      -0.0043546000
_diffrn_orient_matrix_UB_33      -0.0501448000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29902
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.983
_diffrn_reflns_theta_min         2.277
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87854
_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_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0623P)^2^+1.8435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3007
_reflns_number_total             3290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03408h2.cif
_cod_data_source_block           1aopen-decane
_cod_depositor_comments
'Adding full bibliography for 7126838--7126851.cif.'
_cod_original_formula_sum        'C15.50 H11.30 N O2'
_cod_database_code               7126850
_shelx_shelxl_version_number     2018/3
_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.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14)
;
_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 1.183
_oxdiff_exptl_absorpt_empirical_full_min 0.791