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_7718944
_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         'C136 H104 Cd4 N16 O32, 3[C2H6O] 5[C3H7NO]'
_chemical_formula_sum            'C157 H157 Cd4 N21 O40'
_chemical_formula_weight         3427.63
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-05-19
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-05-30 deposited with the CCDC.	2025-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                63.0610(10)
_cell_angle_beta                 82.3530(10)
_cell_angle_gamma                89.181(2)
_cell_formula_units_Z            1
_cell_length_a                   13.6882(3)
_cell_length_b                   18.2052(3)
_cell_length_c                   20.0158(2)
_cell_measurement_reflns_used    101541
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.8630
_cell_measurement_theta_min      2.4990
_cell_volume                     4401.11(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.142a 64-bit (release 17-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.142a (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 0.994
_diffrn_measured_fraction_theta_max 0.958
_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    -82.00  -3.00   0.50    0.20    --  -41.71 114.00  40.00  158
  2  \w     10.00  82.00   0.50    0.20    --   41.71-114.00 -50.00  144
  3  \w     10.00  85.00   0.50    0.20    --   45.00-114.00 -50.00  150
  4  \w   -174.00 -94.00   0.50    0.50    -- -103.00-114.00 -50.00  160
  5  \w    -97.00 -31.00   0.50    0.50    -- -103.00 114.00  40.00  132
  6  \w    -40.00 -14.00   0.50    0.20    --   10.00 131.00-170.83   52
  7  \w      5.00  31.00   0.50    0.20    --   26.00  73.00-170.99   52
  8  \w      5.00  34.00   0.50    0.20    --   26.00  72.00 134.68   58
  9  \w      5.00  34.00   0.50    0.20    --   26.00  72.00  -0.10   58
 10  \w     10.00  36.00   0.50    0.20    --   30.00  71.00 -49.33   52
 11  \w     11.00  46.00   0.50    0.20    --   30.00  67.00-104.83   70
 12  \w     10.00  36.00   0.50    0.20    --   30.00  70.00  92.04   52
 13  \w    -42.00 -16.00   0.50    0.20    --  -34.00 -66.00 -53.43   52
 14  \w    -42.00 -16.00   0.50    0.20    --  -34.00 -66.00  76.90   52
 15  \w    -48.00 -21.00   0.50    0.20    --  -38.00 -63.00  45.34   54
 16  \w     28.00 119.00   0.50    0.20    --   41.71  38.00  30.00  182
 17  \w     17.00  93.00   0.50    0.20    --   45.00-126.00  60.00  152
 18  \w    -18.00  68.00   0.50    0.20    --   45.00 -77.00-120.00  172
 19  \w     32.00 122.00   0.50    0.20    --   45.00  38.00 150.00  180
 20  \w     32.00 122.00   0.50    0.20    --   45.00  38.00 150.00  180
 21  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00 163.16   52
 22  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00 -31.46   52
 23  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -60.00 -79.76   52
 24  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -60.00  13.30   52
 25  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00-145.39   52
 26  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00  83.63   52
 27  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -60.00 -14.82   52
 28  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -60.00 126.59   52
 29  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -60.00 -48.69   52
 30  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -59.00-119.22   52
 31  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00-108.83   52
 32  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00  30.85   52
 33  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00 149.35   52
 34  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -59.00  45.61   52
 35  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -60.00 103.86   52
 36  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -60.00-178.98   52
 37  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00-101.74   52
 38  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00-162.39   52
 39  \w    -56.00 -30.00   0.50    0.20    --  -46.00 -61.00  93.84   52
 40  \w   -127.00 -40.00   0.50    0.20    --  -54.00 -53.00  66.35  174
 41  \w   -127.00 -40.00   0.50    0.20    --  -54.00 -53.00 -13.80  174
 42  \w   -127.00 -40.00   0.50    0.20    --  -54.00 -54.00 -94.41  174
 43  \w   -127.00 -40.00   0.50    0.20    --  -54.00 -53.00 -13.80  174
 44  \w   -127.00 -40.00   0.50    0.20    --  -54.00 -54.00 -66.79  174
 45  \w   -127.00 -40.00   0.50    0.20    --  -54.00 -53.00  66.35  174
 46  \w   -127.00 -40.00   0.50    0.20    --  -54.00 -54.00 -94.41  174
 47  \w   -131.00 -44.00   0.50    0.20    --  -58.00 -53.00 117.24  174
 48  \w   -131.00 -44.00   0.50    0.20    --  -58.00 -54.00  28.39  174
 49  \w   -135.00 -48.00   0.50    0.20    --  -62.00 -54.00-113.04  174
 50  \w   -135.00 -48.00   0.50    0.20    --  -62.00 -54.00 -21.26  174
 51  \w   -135.00 -48.00   0.50    0.20    --  -62.00 -54.00  61.29  174
 52  \w   -136.00 -48.00   0.50    0.20    --  -62.00 -52.00  99.25  176
 53  \w   -135.00 -48.00   0.50    0.20    --  -62.00 -54.00 164.20  174
 54  \w   -139.00 -52.00   0.50    0.20    --  -66.00 -54.00-125.61  174
 55  \w   -139.00 -52.00   0.50    0.20    --  -66.00 -53.00-160.50  174
 56  \w   -143.00 -56.00   0.50    0.20    --  -70.00 -54.00 -30.44  174
 57  \w   -143.00 -56.00   0.50    0.20    --  -70.00 -54.00-138.42  174
 58  \w   -143.00 -56.00   0.50    0.20    --  -70.00 -54.00  47.05  174
 59  \w   -143.00 -56.00   0.50    0.20    --  -70.00 -54.00 -30.44  174
 60  \w   -143.00 -56.00   0.50    0.20    --  -70.00 -53.00 -56.64  174
 61  \w   -143.00 -56.00   0.50    0.20    --  -70.00 -54.00 155.57  174
 62  \w   -147.00 -60.00   0.50    0.50    --  -74.00 -53.00 -99.27  174
 63  \w   -147.00 -60.00   0.50    0.50    --  -74.00 -54.00 140.64  174
 64  \w   -147.00 -60.00   0.50    0.50    --  -74.00 -54.00  90.81  174
 65  \w   -147.00 -60.00   0.50    0.50    --  -74.00 -53.00-167.42  174
 66  \w   -148.00 -60.00   0.50    0.50    --  -74.00 -52.00   5.89  176
 67  \w   -148.00 -59.00   0.50    0.50    --  -74.00 -50.00  94.20  178
 68  \w   -151.00 -64.00   0.50    0.50    --  -78.00 -54.00 -34.73  174
 69  \w   -152.00 -63.00   0.50    0.50    --  -78.00 -50.00-109.60  178
 70  \w   -151.00 -64.00   0.50    0.50    --  -78.00 -53.00  -4.62  174
 71  \w   -152.00 -64.00   0.50    0.50    --  -78.00 -51.00 172.08  176
 72  \w   -152.00 -64.00   0.50    0.50    --  -78.00 -51.00 117.21  176
 73  \w   -151.00 -64.00   0.50    0.50    --  -78.00 -53.00  24.40  174
 74  \w   -151.00 -64.00   0.50    0.50    --  -78.00 -53.00-142.66  174
 75  \w   -155.00 -68.00   0.50    0.50    --  -82.00 -54.00 152.13  174
 76  \w   -155.00 -68.00   0.50    0.50    --  -82.00 -53.00 -70.41  174
 77  \w   -155.00 -68.00   0.50    0.50    --  -82.00 -53.00-113.81  174
 78  \w   -155.00 -68.00   0.50    0.50    --  -82.00 -53.00 -63.04  174
 79  \w   -155.00 -68.00   0.50    0.50    --  -82.00 -53.00  56.29  174
 80  \w   -155.00 -68.00   0.50    0.50    --  -82.00 -53.00  84.52  174
 81  \w   -155.00 -68.00   0.50    0.50    --  -82.00 -53.00 -77.55  174
 82  \w   -155.00 -68.00   0.50    0.50    --  -82.00 -54.00 -26.19  174
 83  \w   -155.00 -68.00   0.50    0.50    --  -82.00 -53.00 -54.33  174
 84  \w   -160.00 -72.00   0.50    0.50    --  -86.00 -52.00  42.98  176
 85  \w   -159.00 -72.00   0.50    0.50    --  -86.00 -53.00-164.07  174
 86  \w   -159.00 -72.00   0.50    0.50    --  -86.00 -54.00  80.21  174
 87  \w   -159.00 -72.00   0.50    0.50    --  -86.00 -53.00-120.15  174
 88  \w   -163.00 -76.00   0.50    0.50    --  -90.00 -54.00 -11.60  174
 89  \w   -163.00 -76.00   0.50    0.50    --  -90.00 -54.00  36.50  174
 90  \w   -163.00 -76.00   0.50    0.50    --  -90.00 -54.00  36.50  174
 91  \w   -168.00 -79.00   0.50    0.50    --  -94.00 -57.00-166.68  178
 92  \w   -168.00 -79.00   0.50    0.50    --  -94.00 -59.00  59.31  178
 93  \w   -168.00 -79.00   0.50    0.50    --  -94.00 -55.00-137.38  178
 94  \w   -168.00 -79.00   0.50    0.50    --  -94.00 -58.00  32.39  178
 95  \w   -171.00 -83.00   0.50    0.50    --  -98.00 -57.00 -51.64  176
 96  \w   -171.00 -82.00   0.50    0.50    --  -98.00 -56.00  22.43  178
 97  \w   -171.00 -83.00   0.50    0.50    --  -98.00 -58.00 157.71  176
 98  \w   -171.00 -83.00   0.50    0.50    --  -98.00 -58.00 -22.00  176
 99  \w   -171.00 -83.00   0.50    0.50    --  -98.00 -58.00 -27.11  176
100  \w   -171.00 -83.00   0.50    0.50    --  -98.00 -58.00 -27.11  176
101  \w   -171.00 -82.00   0.50    0.50    --  -98.00 -60.00 121.83  178
102  \w   -171.00 -82.00   0.50    0.50    --  -98.00 -60.00 121.83  178
103  \w   -171.00 -82.00   0.50    0.50    --  -98.00 -61.00 -92.70  178
104  \w   -171.00 -82.00   0.50    0.50    --  -98.00 -59.00  13.82  178
105  \w   -171.00 -82.00   0.50    0.50    --  -98.00 -61.00 -92.70  178
106  \w   -171.00 -83.00   0.50    0.50    --  -98.00 -58.00-173.19  176
107  \w   -171.00 -83.00   0.50    0.50    --  -98.00 -58.00-173.19  176
108  \w   -171.00 -83.00   0.50    0.50    --  -98.00 -57.00 -51.64  176
109  \w   -174.00 -86.00   0.50    0.50    -- -102.00 -59.00 -69.83  176
110  \w    -93.00 -29.00   0.50    0.50    -- -103.00  93.00 136.58  128
111  \w    -93.00 -29.00   0.50    0.50    -- -103.00  93.00  57.65  128
112  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -65.00-137.17  176
113  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -62.00 120.12  176
114  \w    -93.00 -29.00   0.50    0.50    -- -103.00  93.00   2.98  128
115  \w    -92.00 -29.00   0.50    0.50    -- -103.00  90.00  98.26  126
116  \w    -70.00 -29.00   0.50    0.50    -- -103.00  77.00  30.00   82
117  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -62.00 159.15  176
118  \w    -93.00 -29.00   0.50    0.50    -- -103.00  91.00 -99.05  128
119  \w    -93.00 -29.00   0.50    0.50    -- -103.00  93.00  57.65  128
120  \w    -93.00 -29.00   0.50    0.50    -- -103.00  93.00 166.27  128
121  \w   -174.00 -88.00   0.50    0.50    -- -103.00 -57.00-129.76  172
122  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -63.00 -71.44  176
123  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -62.00  -0.10  176
124  \w   -174.00 -88.00   0.50    0.50    -- -103.00 -55.00 101.16  172
125  \w    -93.00 -29.00   0.50    0.50    -- -103.00  93.00-129.81  128
126  \w    -93.00 -29.00   0.50    0.50    -- -103.00  93.00-129.81  128
127  \w    -93.00 -29.00   0.50    0.50    -- -103.00  89.00 124.46  128
128  \w    -93.00 -29.00   0.50    0.50    -- -103.00  89.00 -70.11  128
129  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -65.00-103.43  176
130  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -63.00 103.65  176
131  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -63.00 103.65  176
132  \w    -93.00 -29.00   0.50    0.50    -- -103.00  91.00 -25.99  128
133  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -63.00  52.74  176
134  \w   -163.00-134.00   0.50    0.50    -- -103.00 -63.00  52.74   58
135  \w   -122.00 -87.00   0.50    0.50    -- -103.00 -65.00 -43.84   70
136  \w   -149.00-123.00   0.50    0.50    -- -103.00 -65.00 -43.84   52
137  \w    -93.00 -29.00   0.50    0.50    -- -103.00  93.00  26.43  128
138  \w    -90.00 -34.00   0.50    0.50    -- -103.00  93.00-171.17  112
139  \w    -79.00 -29.00   0.50    0.50    -- -103.00  93.00-155.58  100
140  \w   -164.00 -86.00   0.50    0.50    -- -103.00 -63.00  96.40  156
141  \w   -122.00 -86.00   0.50    0.50    -- -103.00 -63.00  27.05   72
142  \w    -92.00 -30.00   0.50    0.50    -- -103.00  96.00 -62.19  124
143  \w   -170.00 -86.00   0.50    0.50    -- -103.00 -64.00  10.48  168
144  \w   -172.00 -87.00   0.50    0.50    -- -103.00 -65.00 -26.79  170
145  \w   -120.00 -86.00   0.50    0.50    -- -103.00 -63.00 141.40   68
146  \w   -174.00-125.00   0.50    0.50    -- -103.00 -63.00 141.40   98
147  \w   -173.00 -86.00   0.50    0.50    -- -103.00 -63.00 178.84  174
148  \w   -174.00 -86.00   0.50    0.50    -- -103.00 -62.00 -57.14  176
149  \w   -170.00 -87.00   0.50    0.50    -- -103.00 -59.00  79.59  166
150  \w   -171.00 -86.00   0.50    0.50    -- -103.00 -63.00 148.06  170
151  \w   -174.00 -87.00   0.50    0.50    -- -103.00 -56.00-156.42  174
;
_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      -0.0039339000
_diffrn_orient_matrix_UB_12      -0.0280205000
_diffrn_orient_matrix_UB_13      0.0854362000
_diffrn_orient_matrix_UB_21      0.1127895000
_diffrn_orient_matrix_UB_22      -0.0071472000
_diffrn_orient_matrix_UB_23      -0.0075560000
_diffrn_orient_matrix_UB_31      0.0138985000
_diffrn_orient_matrix_UB_32      0.0905459000
_diffrn_orient_matrix_UB_33      -0.0158391000
_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  0.1266
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            302312
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.488
_diffrn_reflns_theta_min         2.502
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.454
_exptl_absorpt_correction_T_max  0.515
_exptl_absorpt_correction_T_min  0.232
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.142a (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            gold
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       rhombohedra
_exptl_crystal_F_000             1758
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.728
_refine_diff_density_min         -2.132
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.278(12)
_refine_ls_extinction_coef       0.0038(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1639
_refine_ls_number_reflns         31426
_refine_ls_number_restraints     2184
_refine_ls_restrained_S_all      1.301
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_gt           0.0991
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2952
_refine_ls_wR_factor_ref         0.3088
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    0.870
_reflns_Friedel_fraction_max     0.815
_reflns_number_gt                25192
_reflns_number_total             31426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00814j2.cif
_cod_data_source_block           dmd24_scl0456_kmc15_33_d
_cod_depositor_comments
'Adding full bibliography for 7718943--7718944.cif.'
_cod_original_cell_volume        4401.11(13)
_cod_database_code               7718944
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'Cd C24 N4 O8'
_shelx_estimated_absorpt_t_max   0.690
_shelx_estimated_absorpt_t_min   0.485
_diffrn_oxdiff_digest_hkl
;
439bcdd239d4bf0a02573312835613e94d93fd
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.722(12)
 0.278(12)
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
 O1A_9-C6A_9 = O4A_9-C11A_9 = O3A_9-C12A_9 = O2A_9-C17A_9
 O1A_10-C6A_10 = O4A_10-C11A_10 = O3A_10-C12A_10 = O2A_10-C17A_10
 O1A_11-C6A_11 = O4A_11-C11A_11 = O3A_11-C12A_11 = O2A_11-C17A_11
 O1A_12-C6A_12 = O4A_12-C11A_12 = O3A_12-C12A_12 = O2A_12-C17A_12
 1.21 with sigma of 0.01
 C28_17-C30_17
 2.45 with sigma of 0.01
 C30A-C28A
 2.3 with sigma of 0.01
 C30A-C33A
 2.5 with sigma of 0.01
 C32_17-C29_17
 2.56 with sigma of 0.01
 C30_15-C33_15
 2.52 with sigma of 0.01
 C33_17-C30_17
 2.53 with sigma of 0.01
 C30_17-C31_17
 2.42 with sigma of 0.01
 C29_16-C30_16 \\sim C29A-C30A
 with sigma of 0.02
 C32_16-C34_16 \\sim C32A-C34A
 with sigma of 0.04
 C33_16-C30_16 \\sim C33A-C30A
 with sigma of 0.04
 C28_16-C30_16 \\sim C28A-C30A
 with sigma of 0.04
 C33_16-C32_16 \\sim C33A-C32A
 with sigma of 0.02
 C33_16-C34_16 \\sim C33A-C34A
 with sigma of 0.02
 C31_16-C30_16 \\sim C31_16-C30A
 with sigma of 0.04
 C29_16-C32_16 \\sim C29A-C32A
 with sigma of 0.04
 C32_16-C26_16 \\sim C32A-C26A
 with sigma of 0.04
 C29_16-C34_16 \\sim C29A-C34A
 with sigma of 0.04
 O6_14-C25_14 \\sim O5_14-C25_14 \\sim O7_14-C31_14 \\sim O8_14-C31_14
 O6_15-C25_15 \\sim O5_15-C25_15 \\sim O7_15-C31_15 \\sim O8_15-C31_15
 O6_16-C25_16 \\sim O5_16-C25_16 \\sim O7_16-C31_16 \\sim O8_16-C31_16
 O6_17-C25_17 \\sim O5_17-C25_17 \\sim O7_17-C31_17 \\sim O8_17-C31_17
 with sigma of 0.02
 C26_16-C34_16 \\sim C26A-C34A
 with sigma of 0.04
 C26_14-C25_14 \\sim C31_14-C29_14
 C26_15-C25_15 \\sim C31_15-C29_15
 C26_16-C25_16 \\sim C31_16-C29_16
 C26_17-C25_17 \\sim C31_17-C29_17
 with sigma of 0.02
 C33_14-C26_14 \\sim C33_14-C29_14
 C33_15-C26_15 \\sim C33_15-C29_15
 C33_16-C26_16 \\sim C33_16-C29_16
 C33_17-C26_17 \\sim C33_17-C29_17
 with sigma of 0.02
 C27_14-C26_14 \\sim C29_14-C28_14
 C27_15-C26_15 \\sim C29_15-C28_15
 C27_16-C26_16 \\sim C29_16-C28_16
 C27_17-C26_17 \\sim C29_17-C28_17
 with sigma of 0.02
 C28_14-C27_14
 C28_15-C27_15
 C28_16-C27_16
 C28_17-C27_17
 with sigma of 0.02
 C34_14-C33_14 \\sim C33_14-C32_14
 C34_15-C33_15 \\sim C33_15-C32_15
 C34_16-C33_16 \\sim C33_16-C32_16
 C34_17-C33_17 \\sim C33_17-C32_17
 with sigma of 0.02
 N3A_9-C11A_9 \\sim N3A_9-C12A_9 \\sim N2A_9-C6A_9 \\sim N2A_9-C17A_9
 N3A_10-C11A_10 \\sim N3A_10-C12A_10 \\sim N2A_10-C6A_10 \\sim N2A_10-C17A_10
 N3A_11-C11A_11 \\sim N3A_11-C12A_11 \\sim N2A_11-C6A_11 \\sim N2A_11-C17A_11
 N3A_12-C11A_12 \\sim N3A_12-C12A_12 \\sim N2A_12-C6A_12 \\sim N2A_12-C17A_12
 with sigma of 0.02
 C30_14-C29_14
 C30_15-C29_15
 C30_16-C29_16
 C30_17-C29_17
 with sigma of 0.02
 N3A_9-C20A_9 \\sim N2A_9-C3A_9
 N3A_10-C20A_10 \\sim N2A_10-C3A_10
 N3A_11-C20A_11 \\sim N2A_11-C3A_11
 N3A_12-C20A_12 \\sim N2A_12-C3A_12
 with sigma of 0.02
 C26_14-C28_14 \\sim C27_14-C29_14
 C26_15-C28_15 \\sim C27_15-C29_15
 C26_16-C28_16 \\sim C27_16-C29_16
 C26_17-C28_17 \\sim C27_17-C29_17
 with sigma of 0.02
 C7A_9-C6A_9 \\sim C17A_9-C16A_9 \\sim C13A_9-C12A_9 \\sim C11A_9-C10A_9
 C7A_10-C6A_10 \\sim C17A_10-C16A_10 \\sim C13A_10-C12A_10 \\sim C11A_10-C10A_10
 C7A_11-C6A_11 \\sim C17A_11-C16A_11 \\sim C13A_11-C12A_11 \\sim C11A_11-C10A_11
 C7A_12-C6A_12 \\sim C17A_12-C16A_12 \\sim C13A_12-C12A_12 \\sim C11A_12-C10A_12
 with sigma of 0.02
 C24A_9-C23A_9 \\sim C22A_9-C21A_9 \\sim C2A_9-C1A_9 \\sim C5A_9-C4A_9
 C24A_10-C23A_10 \\sim C22A_10-C21A_10 \\sim C2A_10-C1A_10 \\sim C5A_10-C4A_10
 C24A_11-C23A_11 \\sim C22A_11-C21A_11 \\sim C2A_11-C1A_11 \\sim C5A_11-C4A_11
 C24A_12-C23A_12 \\sim C22A_12-C21A_12 \\sim C2A_12-C1A_12 \\sim C5A_12-C4A_12
 with sigma of 0.02
 C34_14-C32_14
 C34_15-C32_15
 C34_16-C32_16
 C34_17-C32_17
 with sigma of 0.02
 C26_14-C29_14
 C26_15-C29_15
 C26_16-C29_16
 C26_17-C29_17
 with sigma of 0.02
 N4A_9-C23A_9 \\sim N4A_9-C22A_9 \\sim N1A_9-C5A_9 \\sim N1A_9-C1A_9
 N4A_10-C23A_10 \\sim N4A_10-C22A_10 \\sim N1A_10-C5A_10 \\sim N1A_10-C1A_10
 N4A_11-C23A_11 \\sim N4A_11-C22A_11 \\sim N1A_11-C5A_11 \\sim N1A_11-C1A_11
 N4A_12-C23A_12 \\sim N4A_12-C22A_12 \\sim N1A_12-C5A_12 \\sim N1A_12-C1A_12
 with sigma of 0.02
 O6_14-O5_14
 O6_15-O5_15
 O6_16-O5_16
 O6_17-O5_17
 with sigma of 0.02
 C21A_9-C20A_9 \\sim C24A_9-C20A_9 \\sim C4A_9-C3A_9 \\sim C3A_9-C2A_9
 C21A_10-C20A_10 \\sim C24A_10-C20A_10 \\sim C4A_10-C3A_10 \\sim C3A_10-C2A_10
 C21A_11-C20A_11 \\sim C24A_11-C20A_11 \\sim C4A_11-C3A_11 \\sim C3A_11-C2A_11
 C21A_12-C20A_12 \\sim C24A_12-C20A_12 \\sim C4A_12-C3A_12 \\sim C3A_12-C2A_12
 with sigma of 0.02
 O8_14-O7_14
 O8_15-O7_15
 O8_16-O7_16
 O8_17-O7_17
 with sigma of 0.02
 N4A_9-C24A_9 \\sim C23A_9-C20A_9 \\sim C22A_9-C20A_9 \\sim N4A_9-C21A_9 \\sim
C24A_9-C21A_9 ~
 C23A_9-C22A_9
 N4A_10-C24A_10 \\sim C23A_10-C20A_10 \\sim C22A_10-C20A_10 \\sim
N4A_10-C21A_10 \\sim C24A_10-
 C21A_10 \\sim C23A_10-C22A_10
 N4A_11-C24A_11 \\sim C23A_11-C20A_11 \\sim C22A_11-C20A_11 \\sim
N4A_11-C21A_11 \\sim C24A_11-
 C21A_11 \\sim C23A_11-C22A_11
 N4A_12-C24A_12 \\sim C23A_12-C20A_12 \\sim C22A_12-C20A_12 \\sim
N4A_12-C21A_12 \\sim C24A_12-
 C21A_12 \\sim C23A_12-C22A_12
 with sigma of 0.02
 C29_16-C33_16 \\sim C29A-C33A
 with sigma of 0.02
 O3A_9-C13A_9 \\sim O4A_9-C10A_9 \\sim C7A_9-O1A_9 \\sim C16A_9-O2A_9
 O3A_10-C13A_10 \\sim O4A_10-C10A_10 \\sim C7A_10-O1A_10 \\sim C16A_10-O2A_10
 O3A_11-C13A_11 \\sim O4A_11-C10A_11 \\sim C7A_11-O1A_11 \\sim C16A_11-O2A_11
 O3A_12-C13A_12 \\sim O4A_12-C10A_12 \\sim C7A_12-O1A_12 \\sim C16A_12-O2A_12
 with sigma of 0.02
 C29_16-C28_16 \\sim C29A-C28A
 with sigma of 0.02
 C29_16-C31_16 \\sim C29A-C31_16
 with sigma of 0.02
 O1A_9-N2A_9 \\sim O2A_9-N2A_9 \\sim O3A_9-N3A_9 \\sim O4A_9-N3A_9
 O1A_10-N2A_10 \\sim O2A_10-N2A_10 \\sim O3A_10-N3A_10 \\sim O4A_10-N3A_10
 O1A_11-N2A_11 \\sim O2A_11-N2A_11 \\sim O3A_11-N3A_11 \\sim O4A_11-N3A_11
 O1A_12-N2A_12 \\sim O2A_12-N2A_12 \\sim O3A_12-N3A_12 \\sim O4A_12-N3A_12
 with sigma of 0.02
 C33_16-C26_16 \\sim C33A-C26A
 with sigma of 0.02
 C28_16-C27_16 \\sim C28A-C27A
 with sigma of 0.02
 C25_16-C26_16 \\sim C25_16-C26A
 with sigma of 0.02
 C26_16-C27_16 \\sim C26A-C27A
 with sigma of 0.02
 C29_16-C26_16 \\sim C29A-C26A
 with sigma of 0.04
 C29_16-C27_16 \\sim C29A-C27A
 with sigma of 0.04
 C33_16-C28_16 \\sim C33A-C28A
 with sigma of 0.04
 C33_16-C31_16 \\sim C33A-C31_16
 with sigma of 0.04
 C33_16-C25_16 \\sim C33A-C25_16
 with sigma of 0.04
 C33_16-C27_16 \\sim C33A-C27A
 with sigma of 0.04
 C28_16-C31_16 \\sim C28A-C31_16
 with sigma of 0.04
 C26_14-C28_14 \\sim C27_14-C29_14
 with sigma of 0.02
 C28_16-C26_16 \\sim C28A-C26A
 with sigma of 0.04
 C25_16-C27_16 \\sim C25_16-C27A
 with sigma of 0.04
4. Restrained planarity
 O6_14, C25_14, O5_14
 O6_15, C25_15, O5_15
 O6_16, C25_16, O5_16
 O6_17, C25_17, O5_17
 with sigma of 0.01
 O8_14, O7_14, C31_14
 O8_15, O7_15, C31_15
 O8_16, O7_16, C31_16
 O8_17, O7_17, C31_17
 with sigma of 0.01
 C26_14, C25_14, O6_14, O5_14
 C26_15, C25_15, O6_15, O5_15
 C26_16, C25_16, O6_16, O5_16
 C26_17, C25_17, O6_17, O5_17
 with sigma of 0.01
 C29_14, O8_14, C31_14, O7_14
 C29_15, O8_15, C31_15, O7_15
 C29_16, O8_16, C31_16, O7_16
 C29_17, O8_17, C31_17, O7_17
 with sigma of 0.01
 C5A_9, N1A_9, C4A_9, C1A_9, C3A_9, C2A_9
 C5A_10, N1A_10, C4A_10, C1A_10, C3A_10, C2A_10
 C5A_11, N1A_11, C4A_11, C1A_11, C3A_11, C2A_11
 C5A_12, N1A_12, C4A_12, C1A_12, C3A_12, C2A_12
 with sigma of 0.02
 C20A_9, C24A_9, C21A_9, C23A_9, C22A_9, N4A_9
 C20A_10, C24A_10, C21A_10, C23A_10, C22A_10, N4A_10
 C20A_11, C24A_11, C21A_11, C23A_11, C22A_11, N4A_11
 C20A_12, C24A_12, C21A_12, C23A_12, C22A_12, N4A_12
 with sigma of 0.01
 N2A_9, C17A_9, C6A_9
 N2A_10, C17A_10, C6A_10
 N2A_11, C17A_11, C6A_11
 N2A_12, C17A_12, C6A_12
 with sigma of 0.01
 N3A_9, C11A_9, C12A_9
 N3A_10, C11A_10, C12A_10
 N3A_11, C11A_11, C12A_11
 N3A_12, C11A_12, C12A_12
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C26A \\sim C30A \\sim C27A \\sim C33A \\sim C29A \\sim C32A \\sim C28A \\sim
C34A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
O8_14 \\sim O6_14 \\sim O7_14 \\sim C25_14 \\sim C31_14 \\sim C33_14 \\sim
O5_14 \\sim C32_14 \\sim C34_14 \\sim C26_14 \\sim C29_14 \\sim C27_14 \\sim
C28_14 \\sim C30_14 \\sim O8_15 \\sim O6_15 \\sim O7_15 \\sim C25_15 \\sim
C31_15 \\sim C33_15 \\sim O5_15 \\sim C32_15 \\sim C34_15 \\sim C26_15 \\sim
C29_15 \\sim C27_15 \\sim C28_15 \\sim C30_15 \\sim O8_16 \\sim O6_16 \\sim
O7_16 \\sim C25_16 \\sim C31_16 \\sim C33_16 \\sim O5_16 \\sim C32_16 \\sim
C34_16 \\sim C26_16 \\sim C29_16 \\sim C27_16 \\sim C28_16 \\sim C30_16 \\sim
O8_17 \\sim O6_17 \\sim O7_17 \\sim C25_17 \\sim C31_17 \\sim C33_17 \\sim
O5_17 \\sim C32_17 \\sim C34_17 \\sim C26_17 \\sim C29_17 \\sim C27_17 \\sim
C28_17 \\sim C30_17: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
N1A_11 \\sim C5A_11 \\sim C2A_11 \\sim C3A_11 \\sim C4A_11 \\sim C1A_11: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N1A_9 \\sim C1A_9 \\sim C2A_9 \\sim C3A_9 \\sim C4A_9 \\sim C5A_9 \\sim N1A_10
\\sim C1A_10 \\sim C2A_10 \\sim C3A_10 \\sim C4A_10 \\sim C5A_10 \\sim N1A_11
\\sim C1A_11 \\sim C2A_11 \\sim C3A_11 \\sim C4A_11 \\sim C5A_11 \\sim N1A_12
\\sim C1A_12 \\sim C2A_12 \\sim C3A_12 \\sim C4A_12 \\sim C5A_12: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
6. Rigid body (RIGU) restrains
 C18A_9, C11A_9, C17A_9, C12A_9, C19A_9, C18A_10, C15A_10, C13A_10, C17A_10,
 C19A_10, C12A_10, C14A_10, C16A_10, C11A_10, C19A_11, C9A_11, C7A_11, C17A_11,
 C18A_11, C12A_11, C8A_11, C10A_11, C11A_11, C18A_12, C11A_12, C17A_12, C12A_12,
  C19A_12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Sof(C26A)=Sof(H26A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C27A)=
 Sof(H27A)=Sof(H27B)=Sof(C33A)=Sof(C29A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=1-FVAR(1)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C32)=
 Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C29)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C33)=
 Sof(C26)=Sof(H26)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
8.a Ternary CH refined with riding coordinates:
 C26A(H26A), C26(H26), C26(H26), C26(H26), C26(H26)
8.b Secondary CH2 refined with riding coordinates:
 C27A(H27A,H27B), C28A(H28A,H28B), C28(H28A,H28B), C27(H27A,H27B), C28(H28A,
 H28B), C27(H27A,H27B), C28(H28A,H28B), C27(H27A,H27B), C28(H28A,H28B),
 C27(H27A,H27B)
8.c Me refined with riding coordinates:
 C30A(H30A,H30B,H30C), C32A(H32A,H32B,H32C), C30(H30A,H30B,H30C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C30(H30A,H30B,H30C), C30(H30A,H30B,H30C),
 C32(H32A,H32B,H32C)
8.d Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C1A(H1A), C22A(H22A), C4A(H4A), C5A(H5A), C21A(H21A), C23A(H23A),
 C8A(H8A), C9A(H9A), C15A(H15A), C14A(H14A), C24A(H24A), C24A(H24A), C9A(H9A),
 C8A(H8A), C14A(H14A), C15A(H15A), C5A(H5A), C2A(H2A), C21A(H21A), C4A(H4A),
 C23A(H23A), C22A(H22A), C1A(H1A), C24A(H24A), C15A(H15A), C14A(H14A), C8A(H8A),
  C9A(H9A), C5A(H5A), C2A(H2A), C21A(H21A), C4A(H4A), C23A(H23A), C22A(H22A),
 C1A(H1A), C2A(H2A), C1A(H1A), C22A(H22A), C4A(H4A), C5A(H5A), C21A(H21A),
 C23A(H23A), C8A(H8A), C9A(H9A), C15A(H15A), C14A(H14A), C24A(H24A)
8.e Naphthalene refined as free rotating group:
 C7A(C8A,C9A,C10A,C19A,C18A,C16A,C15A,C14A,C13A), C10A(C9A,C8A,C7A,C18A,C19A,
 C13A,C14A,C15A,C16A), C16A(C15A,C14A,C13A,C19A,C18A,C7A,C8A,C9A,C10A), C7A(C8A,
 C9A,C10A,C19A,C18A,C16A,C15A,C14A,C13A)
8.f Idealised Me refined as rotating group:
 C34A(H34A,H34B,H34C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C34(H34A,H34B,H34C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96313
_shelx_hkl_checksum              33049
_shelx_fab_checksum              66085
_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 1.944
_oxdiff_exptl_absorpt_empirical_full_min 0.461