Releasing a bound molecular spring with light: a visible light-triggered photosalient effect tied to polymorphism.
McGehee, Keegan; Saito, Koichiro; Kwaria, Dennis; Minamikawa, Hiroyuki; Norikane, Yasuo; Physical chemistry chemical physics : PCCP 26 (2024) 6834–6843; doi:10.1039/d3cp04691e

data_7248109
_publ_section_title
;
 Releasing a bound molecular spring with light: a visible light-triggered
 photosalient effect tied to polymorphism.
;
_journal_issue                   8
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              6834
_journal_page_last               6843
_journal_paper_doi               10.1039/d3cp04691e
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         '1(C12 H6 Br4 N2)'
_chemical_formula_sum            'C12 H6 Br4 N2'
_chemical_formula_weight         497.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-09-15 deposited with the CCDC.	2023-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.079(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.3728(11)
_cell_length_b                   8.6091(4)
_cell_length_c                   14.1715(7)
_cell_measurement_reflns_used    12013
_cell_measurement_temperature    170.15
_cell_measurement_theta_max      32.5880
_cell_measurement_theta_min      2.6640
_cell_volume                     2788.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.50a (Rigaku OD, 2022)'
_computing_data_collection
'DTREK_VERSION=d*TREK version 9.9.9.4 W9RSSI -- Mar 27 2012'
_computing_data_reduction        'CrysAlisPro 1.171.43.50a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.15
_diffrn_detector                 'PLATUS 200K area detector'
_diffrn_detector_area_resol_mean 5.811
_diffrn_detector_type            'HPC area detector'
_diffrn_measured_fraction_theta_full 1.000
_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    -60.00 120.00   1.00   16.00    --   30.00  54.00   0.00  180
  2  \w    -60.00 120.00   1.00   16.00    --   30.00  54.00 120.00  180
  3  \w    -60.00 120.00   1.00   16.00    --   30.00  54.00 240.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0278704000
_diffrn_orient_matrix_UB_12      0.0237082000
_diffrn_orient_matrix_UB_13      -0.0069772000
_diffrn_orient_matrix_UB_21      0.0077258000
_diffrn_orient_matrix_UB_22      0.0236881000
_diffrn_orient_matrix_UB_23      0.0489601000
_diffrn_orient_matrix_UB_31      0.0112179000
_diffrn_orient_matrix_UB_32      -0.0752875000
_diffrn_orient_matrix_UB_33      0.0132205000
_diffrn_radiation_monochromator  'multi-layer mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35288
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.418
_diffrn_reflns_theta_min         2.528
_diffrn_source                   'rotating anode X-ray generator'
_diffrn_source_type              FR
_exptl_absorpt_coefficient_mu    11.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.50a (Rigaku Oxford Diffraction, 2022)
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    2.372
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         9693
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0431P)^2^+0.9475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6579
_reflns_number_total             9693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp04691e4.cif
_cod_data_source_block           4BrAzo_trans_beta
_cod_depositor_comments
'Adding full bibliography for 7248107--7248109.cif.'
_cod_database_code               7248109
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Br7 \\sim Br8 \\sim C21 \\sim C19 \\sim C20 \\sim C23 \\sim C22 \\sim C24 \\sim
N4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N4A \\sim Br8A \\sim C24A \\sim C19A \\sim C20A \\sim C21A \\sim C22A \\sim
C23A \\sim Br7A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
3. Rigid body (RIGU) restrains
 Br7, Br8, C21, C19, C20, C23, C22, C24, N4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N4A, Br8A, C24A, C19A, C20A, C21A, C22A, C23A, Br7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(N4A)=Sof(N3A)=Sof(Br8A)=Sof(C24A)=Sof(C19A)=Sof(C20A)=Sof(C21A)=Sof(H21A)=
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(Br7A)=1-FVAR(1)
 Sof(Br7)=Sof(Br8)=Sof(N3)=Sof(C21)=Sof(H21)=Sof(C19)=Sof(C20)=Sof(C23)=
 Sof(H23)=Sof(C22)=Sof(H22)=Sof(C24)=Sof(N4)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4), C11(H11), C9(H9), C21(H21), C17(H17), C10(H10),
 C15(H15), C16(H16), C23(H23), C22(H22), C21A(H21A), C22A(H22A), C23A(H23A)
;
_shelx_res_checksum              28401
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.277
_oxdiff_exptl_absorpt_empirical_full_min 0.516