Visible light activated energy storage in solid-state Azo-BF<sub>2</sub> switches.
Qiu, Qianfeng; Qi, Qingkai; Usuba, Junichi; Lee, Karina; Aprahamian, Ivan; Han, Grace G. D.; Chemical science 14 (2023) 11359–11364; doi:10.1039/d3sc03465h

data_1569977
_publ_section_title
;
 Visible light activated energy storage in solid-state Azo-BF<sub>2</sub>
 switches.
;
_journal_issue                   41
_journal_name_full               'Chemical science'
_journal_page_first              11359
_journal_page_last               11364
_journal_paper_doi               10.1039/d3sc03465h
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C19 H15 B F2 N4 O'
_chemical_formula_sum            'C19 H15 B F2 N4 O'
_chemical_formula_weight         364.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-20 deposited with the CCDC.	2023-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0351(2)
_cell_length_b                   7.02387(10)
_cell_length_c                   27.7571(4)
_cell_measurement_reflns_used    6612
_cell_measurement_temperature    100.09(10)
_cell_measurement_theta_max      79.0250
_cell_measurement_theta_min      3.1800
_cell_volume                     3321.20(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.09(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_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    -76.00  26.00   0.50    2.50    --  -47.10  90.00  58.00  204
  2  \w    -47.00 -18.00   0.50   10.00    --  -91.75  37.00 -68.00   58
  3  \w    -79.00 -22.00   0.50   10.00    --  -91.75 108.00 145.00  114
  4  \w    101.00 178.00   0.50   10.00    --  113.25  37.00 -68.00  154
  5  \w     42.00 104.00   0.50   10.00    --  113.25 -90.00 -56.00  124
  6  \w   -120.00 -35.00   0.50    2.50    --  -47.10 -37.00-150.00  170
  7  \w    -39.00  28.00   0.50    2.50    --  -47.10  19.00 150.00  134
  8  \w     42.00  69.00   0.50   10.00    --  113.25 -61.00 -60.00   54
  9  \w     42.00  69.00   0.50   10.00    --  113.25 -61.00 -30.00   54
 10  \w     42.00 104.00   0.50   10.00    --  113.25 -94.00-150.00  124
 11  \w     42.00  67.00   0.50   10.00    --  113.25 -61.00 150.00   50
 12  \w     77.00 103.00   0.50   10.00    --  113.25 -94.00   0.00   52
 13  \w     45.00  71.00   0.50   10.00    --  113.25 -94.00   0.00   52
 14  \w    103.00 135.00   0.50   10.00    --  113.25  45.00-150.00   64
 15  \w    148.00 174.00   0.50   10.00    --  113.25  45.00-150.00   52
 16  \w     42.00  67.00   0.50   10.00    --  113.25 -61.00-120.00   50
 17  \w     42.00  67.00   0.50   10.00    --  113.25 -61.00  30.00   50
 18  \w     42.00  67.00   0.50   10.00    --  113.25 -61.00 120.00   50
 19  \w     42.00  67.00   0.50   10.00    --  113.25 -61.00-150.00   50
 20  \w    109.00 169.00   0.50   10.00    --  113.25 108.00 145.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0356743000
_diffrn_orient_matrix_UB_12      -0.0262175000
_diffrn_orient_matrix_UB_13      0.0505653000
_diffrn_orient_matrix_UB_21      -0.0236660000
_diffrn_orient_matrix_UB_22      0.2116710000
_diffrn_orient_matrix_UB_23      0.0007470000
_diffrn_orient_matrix_UB_31      -0.0796596000
_diffrn_orient_matrix_UB_32      -0.0511083000
_diffrn_orient_matrix_UB_33      -0.0228734000
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            18821
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.464
_diffrn_reflns_theta_min         3.184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark yellow'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.037
_exptl_crystal_size_min          0.017
_refine_diff_density_max         0.232
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0371P)^2^+1.3853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3100
_reflns_number_total             3575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03465h2.cif
_cod_data_source_block           ia423c
_cod_depositor_comments
'Adding full bibliography for 1569977--1569980.cif.'
_cod_database_code               1569977
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C19H15BF2N4O
_chemical_oxdiff_usercomment     AzoBF2-2C
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.839
_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 Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16),
 C17(H17)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              33111
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop with paratone oil'
_olex2_submission_original_sample_id AzoBF2-2C
_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.762