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_7242075
_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         '4(H2 O), C16 H22 N2 O5'
_chemical_formula_sum            'C16 H30 N2 O9'
_chemical_formula_weight         394.42
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-16
_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                 94.0935(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.92326(18)
_cell_length_b                   8.57252(8)
_cell_length_c                   15.64663(18)
_cell_measurement_reflns_used    7140
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.8280
_cell_measurement_theta_min      5.6470
_cell_volume                     1996.57(4)
_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 1.3 (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 1.000
_diffrn_measured_fraction_theta_max 0.982
_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    -92.00  -2.00   1.00    1.00    --  -42.16 125.00  60.00   90
  2  \w    -67.00  32.00   1.00    1.00    --  -42.16  38.00-120.00   99
  3  \w      1.00  83.00   1.00    1.00    --   42.16 -99.00  30.00   82
  4  \w     23.00  98.00   1.00    1.00    --   42.16-125.00-150.00   75
  5  \w     31.00 133.00   1.00    2.00    --  103.72 -61.00  30.00  102
  6  \w     31.00 118.00   1.00    2.00    --  103.72-125.00 -30.00   87
  7  \w     21.00 109.00   1.00    2.00    --  103.72 -94.00-180.00   88
  8  \w     21.00 109.00   1.00    2.00    --  103.72 -94.00 -60.00   88
  9  \w     78.00 177.00   1.00    2.00    --  103.72  45.00-180.00   99
 10  \w     75.00 178.00   1.00    2.00    --  103.72  30.00-120.00  103
 11  \w   -118.00 -46.00   1.00    1.00    --  -42.16 -77.00 120.00   72
;
_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      -0.0697017000
_diffrn_orient_matrix_UB_12      -0.0189077000
_diffrn_orient_matrix_UB_13      0.0673091000
_diffrn_orient_matrix_UB_21      0.0676944000
_diffrn_orient_matrix_UB_22      -0.0982329000
_diffrn_orient_matrix_UB_23      0.0561389000
_diffrn_orient_matrix_UB_31      0.0356957000
_diffrn_orient_matrix_UB_32      0.1492629000
_diffrn_orient_matrix_UB_33      0.0454015000
_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  0.0205
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11588
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.987
_diffrn_reflns_theta_min         3.955
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88577
_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    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_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          0.1251
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3492
_reflns_number_total             3862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cp06312f2.cif
_cod_data_source_block           DASA1_H2O
_cod_database_code               7242075
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16N2O5H21
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.899
_reflns_odcompleteness_completeness 99.95
_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, All O(H,H) groups
2.a Free rotating group:
 O8s(h8d,h8c), O6s(H6A,H6B), O9s(H7A,H7B), O7s(H10A,H10B)
2.b Ternary CH refined with riding coordinates:
 C7(H7), C11(H11)
2.c Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B)
2.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10)
2.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              28411
_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 1.200
_oxdiff_exptl_absorpt_empirical_full_min 0.736