A simple strategy to overcome concentration dependence of photoswitching properties in donor-acceptor Stenhouse adducts
Connolly, Sean; Tiwari, Rahul; Holder, Simon J.; Shepherd, Helena Jane; Physical Chemistry Chemical Physics  (2021) –; doi:10.1039/D0CP06312F

data_7242076
_publ_section_title
;
 A simple strategy to overcome concentration dependence of photoswitching
 properties in donor-acceptor Stenhouse adducts
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D0CP06312F
_journal_year                    2021
_chemical_formula_moiety         'C15 H19 N O5'
_chemical_formula_sum            'C15 H19 N O5'
_chemical_formula_weight         293.31
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-07-13 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.121(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9743(4)
_cell_length_b                   17.9548(7)
_cell_length_c                   10.8807(4)
_cell_measurement_reflns_used    1827
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.7940
_cell_measurement_theta_min      4.8780
_cell_volume                     1480.60(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_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    -53.00  30.00   1.00    3.00    --  -42.16  38.00  30.00   83
  2  \w     40.00  72.00   1.00    3.00    --   42.16-125.00-150.00   32
  3  \w     32.00  86.00   1.00    3.00    --   42.16-125.00   0.00   54
  4  \w     67.00 106.00   1.00    3.00    --   42.16  38.00 120.00   39
  5  \w     31.00  97.00   1.00   12.00    --  103.72-125.00  90.00   66
  6  \w     75.00 122.00   1.00   12.00    --  103.72  61.00 -90.00   47
  7  \w    140.00 166.00   1.00   12.00    --  103.72  61.00 -60.00   26
  8  \w    109.00 176.00   1.00   12.00    --  103.72  87.00 -96.00   67
  9  \w    144.00 175.00   1.00   12.00    --  103.72 125.00 -60.00   31
 10  \w     32.00 106.00   1.00   12.00    --  103.72 -61.00 150.00   74
 11  \w     95.00 155.00   1.00   12.00    --  103.72 125.00-150.00   60
 12  \w     96.00 159.00   1.00   12.00    --  103.72  61.00-150.00   63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0013252000
_diffrn_orient_matrix_UB_12      -0.0696842000
_diffrn_orient_matrix_UB_13      -0.0828705000
_diffrn_orient_matrix_UB_21      0.1563819000
_diffrn_orient_matrix_UB_22      -0.0322881000
_diffrn_orient_matrix_UB_23      0.1087202000
_diffrn_orient_matrix_UB_31      -0.1298671000
_diffrn_orient_matrix_UB_32      -0.0381778000
_diffrn_orient_matrix_UB_33      0.0593056000
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5777
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.998
_diffrn_reflns_theta_min         4.926
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2826
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0415
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2248
_reflns_number_total             2826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cp06312f2.cif
_cod_data_source_block           DASA4
_cod_database_code               7242076
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C15O5NH19
_chemical_oxdiff_usercomment     '150 K'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;
_shelx_res_checksum              90610
_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 1.147
_oxdiff_exptl_absorpt_empirical_full_min 0.915