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_7242073
_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         'C H Cl3, C16 H22 N2 O5'
_chemical_formula_sum            'C17 H23 Cl3 N2 O5'
_chemical_formula_weight         441.72
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-23
_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                108.089(8)
_cell_angle_beta                 96.421(7)
_cell_angle_gamma                92.493(6)
_cell_formula_units_Z            2
_cell_length_a                   10.0026(7)
_cell_length_b                   10.1400(9)
_cell_length_c                   10.8176(10)
_cell_measurement_reflns_used    3130
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.7800
_cell_measurement_theta_min      4.3020
_cell_volume                     1032.86(16)
_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    'olex2.solve (Bourhis et al., 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 0.998
_diffrn_measured_fraction_theta_max 0.968
_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   -115.00 -14.00   1.00    5.00    --  -42.16 -57.00  30.00  101
  2  \w    -90.00  -4.00   1.00    5.00    --  -42.16 125.00 150.00   86
  3  \w   -113.00 -18.00   1.00    5.00    --  -42.16 -38.00 -90.00   95
  4  \w      2.00  33.00   1.00    5.00    --   42.16 -99.00 150.00   31
  5  \w     37.00 109.00   1.00   20.00    --  103.72 -94.00 150.00   72
  6  \w     28.00  91.00   1.00   20.00    --  103.72 -94.00  90.00   63
  7  \w    114.00 172.00   1.00   20.00    --  103.72 125.00 150.00   58
  8  \w     41.00 118.00   1.00   20.00    --  103.72-125.00  30.00   77
  9  \w     41.00 127.00   1.00   20.00    --  103.72 -77.00-180.00   86
 10  \w     74.00 157.00   1.00   20.00    --  103.72  77.00 -90.00   83
 11  \w     79.00 170.00   1.00   20.00    --  103.72  61.00-120.00   91
 12  \w    118.00 175.00   1.00   20.00    --  103.72  77.00 -60.00   57
 13  \w     79.00 170.00   1.00   20.00    --  103.72  45.00   0.00   91
 14  \w     95.00 143.00   1.00   20.00    --  103.72 125.00-180.00   48
 15  \w     76.00 105.00   1.00   20.00    --  103.72  77.00 -60.00   29
;
_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      0.1375196000
_diffrn_orient_matrix_UB_12      0.0851996000
_diffrn_orient_matrix_UB_13      0.0271953000
_diffrn_orient_matrix_UB_21      -0.0707178000
_diffrn_orient_matrix_UB_22      0.1358506000
_diffrn_orient_matrix_UB_23      0.0424080000
_diffrn_orient_matrix_UB_31      0.0165718000
_diffrn_orient_matrix_UB_32      -0.0026558000
_diffrn_orient_matrix_UB_33      0.1424957000
_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  0.0288
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7009
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         72.066
_diffrn_reflns_theta_min         4.338
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.285
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88850
_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    1.420
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.964
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0431P)^2^+0.8449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3187
_reflns_number_total             3933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cp06312f2.cif
_cod_data_source_block           DASA1_CHCl3
_cod_original_cell_volume        1032.86(15)
_cod_database_code               7242073
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16O4N2H22
_chemical_oxdiff_usercomment     150k
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.900
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C26(H26), C7(H7), C11(H10)
2.b Secondary CH2 refined with riding coordinates:
 C12(H11,H12), C13(H13,H14), C14(H19,H20), C15(H21,H22)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H8), C10(H9)
2.d Idealised Me refined as rotating group:
 C1(H1,H2,H3), C2(H4,H5,H6), C16(H16,H17,H18)
;
_shelx_res_checksum              84122
_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 1.203
_oxdiff_exptl_absorpt_empirical_full_min 0.844