Photoswitching chiroptical response in camphorate-based chiral metal-organic frameworks.
Clutterbuck, Katelyn M.; Windsor, Hunter J.; D'Alessandro, Deanna M; Lakhwani, Girish; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11089–11094; doi:10.1039/d5dt00814j

data_7718943
_publ_section_title
;
 Photoswitching chiroptical response in camphorate-based chiral
 metal-organic frameworks.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11089
_journal_page_last               11094
_journal_paper_doi               10.1039/d5dt00814j
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C22 H20 N2 O6 Zn, 3.325[C3H7NO]'
_chemical_formula_sum            'C31.98 H43.28 N5.33 O9.33 Zn'
_chemical_formula_weight         717.03
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-05-30 deposited with the CCDC.	2025-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2755(5)
_cell_length_b                   13.2994(5)
_cell_length_c                   22.3069(10)
_cell_measurement_reflns_used    3371
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      58.8970
_cell_measurement_theta_min      1.9880
_cell_volume                     3938.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.137a 64-bit (release 10-09-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -38.00  53.00   0.50    1.47    --    0.00  60.00 -77.00  182
  2  \w    -18.00   7.00   0.50    1.47    --    0.00 -70.00 -70.00   50
  3  \w     -7.00  18.00   0.50    1.47    --    0.00  70.00  60.00   50
  4  \w    -17.00   8.00   0.50    5.88    --   45.00 -60.00 143.00   50
  5  \w     38.00  69.00   0.50    5.88    --   45.00 -70.00 -70.00   62
  6  \w     45.00  82.00   0.50    5.88    --   45.00 -97.00  47.00   74
  7  \w     28.00  60.00   0.50    5.88    --   45.00  60.00 -77.00   64
  8  \w    -67.00 -41.00   0.50    5.88    --  -51.50  97.00 155.00   52
  9  \w    -44.00  24.00   0.50    5.88    --  -51.50  60.00 -77.00  136
 10  \w    -48.00  14.00   0.50    5.88    --  -51.50  70.00  60.00  124
 11  \w   -152.00-126.00   0.50    5.88    -- -103.00 -97.00  47.00   52
 12  \w   -157.00-121.00   0.50    5.88    -- -103.00 -70.00 -70.00   72
 13  \w    -83.00 -57.00   0.50    5.88    -- -103.00  97.00 155.00   52
 14  \w   -144.00 -81.00   0.50    5.88    -- -103.00 -60.00 143.00  126
 15  \w    -54.00 -24.00   0.50    5.88    -- -103.00  70.00  60.00   60
 16  \w    -50.00 -16.00   0.50    5.88    --   45.00 -19.00  90.00   68
 17  \w    -47.00 -15.00   0.50    5.88    --   45.00 -19.00  30.00   64
 18  \w    -49.00 -19.00   0.50    5.88    --   45.00 -19.00-180.00   60
 19  \w   -130.00 -80.00   0.50    5.88    --  -51.50 -57.00-180.00  100
 20  \w    -55.00 -18.00   0.50    5.88    --  -51.50 -57.00-150.00   74
 21  \w   -170.00-109.00   0.50    5.88    -- -103.00 -99.00-120.00  122
 22  \w    -53.00 -21.00   0.50    5.88    -- -103.00  77.00-120.00   64
 23  \w   -144.00-109.00   0.50    5.88    -- -103.00 -77.00-150.00   70
 24  \w   -146.00 -55.00   0.50    5.88    -- -103.00 -38.00 150.00  182
 25  \w   -111.00 -85.00   0.50    5.88    -- -103.00 -19.00 -90.00   52
 26  \w   -145.00-115.00   0.50    5.88    -- -103.00 -60.00  68.58   60
 27  \w   -106.00 -81.00   0.50    5.88    -- -103.00 -60.00  68.58   50
 28  \w    -77.00 -51.00   0.50    5.88    -- -103.00 126.00  90.00   52
 29  \w   -165.00-101.00   0.50    5.88    -- -103.00 -99.00  60.00  128
 30  \w   -172.00 -80.00   0.50    5.88    -- -103.00 -57.00 -90.00  184
 31  \w   -170.00-119.00   0.50    5.88    -- -103.00 -87.00-159.30  102
 32  \w   -174.00-130.00   0.50    5.88    -- -103.00 -99.00  30.00   88
 33  \w    -98.00 -72.00   0.50    5.88    -- -103.00 -38.00 -30.00   52
 34  \w    -77.00 -23.00   0.50    5.88    -- -103.00 126.00-120.00  108
 35  \w   -129.00 -87.00   0.50    5.88    -- -103.00-126.00  90.00   84
 36  \w   -104.00 -78.00   0.50    5.88    -- -103.00 -19.00 -60.00   52
 37  \w   -143.00-109.00   0.50    5.88    -- -103.00 -77.00  30.00   68
 38  \w   -163.00-128.00   0.50    5.88    -- -103.00 -99.00   0.00   70
 39  \w   -168.00-139.00   0.50    5.88    -- -103.00 -92.00 -16.78   58
 40  \w   -146.00-120.00   0.50    5.88    -- -103.00 -38.00 -30.00   52
 41  \w   -149.00-108.00   0.50    5.88    -- -103.00 -77.00  60.00   82
 42  \w   -144.00-112.00   0.50    5.88    -- -103.00 -77.00-180.00   64
 43  \w   -123.00 -97.00   0.50    5.88    -- -103.00 -57.00-150.00   52
 44  \w   -167.00-142.00   0.50    5.88    -- -103.00 -38.00-120.00   50
 45  \w   -151.00-126.00   0.50    5.88    -- -103.00 -38.00  30.00   50
 46  \w   -172.00-104.00   0.50    5.88    -- -103.00 -99.00 -30.00  136
 47  \w   -174.00-129.00   0.50    5.88    -- -103.00 -82.00-164.21   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0690542000
_diffrn_orient_matrix_UB_12      -0.0906839000
_diffrn_orient_matrix_UB_13      -0.0127195000
_diffrn_orient_matrix_UB_21      -0.0441550000
_diffrn_orient_matrix_UB_22      0.0084631000
_diffrn_orient_matrix_UB_23      0.0636138000
_diffrn_orient_matrix_UB_31      -0.0820998000
_diffrn_orient_matrix_UB_32      0.0715946000
_diffrn_orient_matrix_UB_33      -0.0237261000
_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  0.0749
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16666
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        50.425
_diffrn_reflns_theta_max         50.425
_diffrn_reflns_theta_min         3.870
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.872
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.112a (Rigaku Oxford Diffraction, 2024)
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            orange
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.167
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.19(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.388
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     275
_refine_ls_restrained_S_all      1.418
_refine_ls_R_factor_all          0.1523
_refine_ls_R_factor_gt           0.1168
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3272
_refine_ls_wR_factor_ref         0.3643
_reflns_Friedel_coverage         0.734
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                2636
_reflns_number_total             4042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00814j2.cif
_cod_data_source_block           dmd24_scl0334_kmc15_23_b
_cod_depositor_comments
'Adding full bibliography for 7718943--7718944.cif.'
_cod_database_code               7718943
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C40 H20 N10 O8 Zn2'
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.81(18)
 0.19(18)
2. 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
3. Restrained distances
 C23-C24 = C22-C23
 1.53 with sigma of 0.01
 C23-C19 = C23-C16
 1.57 with sigma of 0.01
 C17-C16 = C18-C19
 1.54 with sigma of 0.01
 C17-C18
 1.52 with sigma of 0.01
 C21-C20
 2.48 with sigma of 0.01
 C23-C21
 2.59 with sigma of 0.01
 C21-C19
 1.54 with sigma of 0.01
 C20-C19
 1.52 with sigma of 0.01
 O5-C19 = O6-C19
 2.53 with sigma of 0.01
 C24-C22
 2.48 with sigma of 0.01
 C23-C21
 2.59 with sigma of 0.01
 C22-C19
 2.59 with sigma of 0.01
 C24-C19
 2.59 with sigma of 0.01
 C21-C23
 2.59 with sigma of 0.01
 C16-C18 = C17-C19
 2.45 with sigma of 0.01
 O4-C15 \\sim O3-C15 \\sim O6-C20 \\sim O5-C20
 with sigma of 0.01
4. Restrained planarity
 N4, C10, C11_$1, C11, C12_$1, C12
 with sigma of 0.01
 N1, C1, C1_$1, C2_$1, C2, C3
 with sigma of 0.01
5. Rigid body (RIGU) restrains
 O3, O4, O5, O6, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, O2, N1, N2, N3, N4, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12,
 C13, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6.a Ternary CH refined with riding coordinates:
 C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B)
6.c Me refined with riding coordinates:
 C21(H21A,H21B,H21C)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C11(H11), C12(H12)
6.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 532 electrons were 
found in a volume of 2422\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
3.325[C3H7NO] per formula unit 
which account for 532 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27805
_shelx_hkl_checksum              39726
_shelx_fab_checksum              63685
_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 2.920
_oxdiff_exptl_absorpt_empirical_full_min 0.426