Photoswitching of Co(ii)-based coordination cages containing azobenzene backbones.
Tipping, Max B.; Pruñonosa Lara, Lidón; Solea, Atena B.; von Krbek, Larissa K. S.; Ward, Michael D.; Chemical science 15 (2024) 8488–8499; doi:10.1039/d4sc01575d

data_1571545
_publ_section_title
;
 Photoswitching of Co(ii)-based coordination cages containing azobenzene
 backbones.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              8488
_journal_page_last               8499
_journal_paper_doi               10.1039/d4sc01575d
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C30 H24 N8'
_chemical_formula_sum            'C30 H24 N8'
_chemical_formula_weight         496.57
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-06 deposited with the CCDC.	2024-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.563(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4889(8)
_cell_length_b                   4.8850(3)
_cell_length_c                   20.2570(12)
_cell_measurement_reflns_used    4252
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.0840
_cell_measurement_theta_min      4.0840
_cell_volume                     1234.61(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.904
_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    -44.00  25.00   0.50    1.04    --  -48.18  40.00 -29.00  138
  2  \w    -24.00  44.00   0.50    1.04    --   48.18 -40.00 176.00  136
  3  \w     36.00 121.00   0.50    1.04    --   48.18  40.00 -29.00  170
  4  \w   -164.00 -78.00   0.50    4.15    --  -91.75 -40.00 176.00  172
  5  \w     95.00 178.00   0.50    4.15    --  108.13  40.00 -29.00  166
  6  \w    -86.00 -13.00   0.50    1.04    --  -48.18 125.00  90.00  146
  7  \w   -121.00 -36.00   0.50    1.04    --  -48.18 -40.00 176.00  170
  8  \w    -85.00 -19.00   0.50    4.15    --  -91.75 125.00   0.00  132
  9  \w    -66.00 -19.00   0.50    4.15    --  -91.75  57.00-120.00   94
 10  \w    -66.00 -19.00   0.50    4.15    --  -91.75  57.00 120.00   94
 11  \w   -163.00 -86.00   0.50    4.15    --  -91.75 -99.00 -60.00  154
 12  \w     36.00  66.00   0.50    4.15    --  108.13 -57.00-120.00   60
 13  \w     36.00  66.00   0.50    4.15    --  108.13 -57.00  60.00   60
 14  \w     36.00 106.00   0.50    4.15    --  108.13 -99.00-120.00  140
 15  \w     36.00  66.00   0.50    4.15    --  108.13 -57.00 120.00   60
 16  \w     36.00  66.00   0.50    4.15    --  108.13 -57.00  90.00   60
 17  \w     36.00 112.00   0.50    4.15    --  108.13-125.00  90.00  152
 18  \w     36.00  66.00   0.50    4.15    --  108.13 -57.00 -90.00   60
 19  \w     36.00  66.00   0.50    4.15    --  108.13 -57.00   0.00   60
 20  \w   -120.00 -25.00   0.50    1.04    --  -48.18 -77.00 -60.00  190
 21  \w   -119.00 -33.00   0.50    1.04    --  -48.18 -57.00 150.00  172
 22  \w   -119.00 -88.00   0.50    1.04    --  -48.18 -57.00  30.00   62
 23  \w   -121.00 -36.00   0.50    1.04    --  -48.18 -37.00  60.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1565
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10836
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.145
_diffrn_reflns_theta_min         4.079
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.779
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
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            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_preparation       'reflux in THF'
_exptl_crystal_recrystallization_method 'EtOAc/hexane vapour diffusion'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2364
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0736
_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^)+(0.1547P)^2^+0.2539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1982
_refine_ls_wR_factor_ref         0.2539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1618
_reflns_number_total             2364
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01575d2.cif
_cod_data_source_block           lm-azo_trans
_cod_depositor_comments
'Adding full bibliography for 1571545--1571546.cif.'
_cod_database_code               1571545
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.896
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
2. Rigid bond restraints
 C6A, C4A, C2A, C3A, C5A, C7A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C6A \\sim C4A \\sim C2A \\sim C3A \\sim C5A \\sim C7A: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H8BC)=Sof(H8BD)=Sof(C7)=Sof(H7)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=Sof(C6)=Sof(N1)=1-FVAR(1)
 Sof(C6A)=Sof(H8AA)=Sof(H8AB)=Sof(C4A)=Sof(H4A)=Sof(C2A)=Sof(C3A)=Sof(H3A)=
 Sof(C5A)=Sof(H5A)=Sof(C7A)=Sof(H7A)=Sof(N1A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8BC,H8BD), C8(H8AA,H8AB)
6.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C12(H12), C17(H17), C19(H19), C18(H18), C13(H13), C4A(H4A),
 C3A(H3A), C5A(H5A), C7A(H7A), C7(H7), C3(H3), C4(H4), C5(H5)
6.c Fitted hexagon refined as free rotating group:
 C7(C2,C3,C4,C5,C6)
;
_shelx_res_checksum              48457
_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
;