Statistical optimization of guest uptake in crystalline sponges: grading structural outcomes.
Carroll, Robert C.; Coles, Simon J.; IUCrJ 11 (2024) –; doi:10.1107/S2052252524004871

data_1571873
_publ_section_title
;
 Statistical optimization of guest uptake in crystalline sponges: grading
 structural outcomes.
;
_journal_coeditor_code           LT5068
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524004871
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety
'C72 H48 I12 N24 Zn6, 0.959(C15 H16 O3), 2.433(C6 H12)'
_chemical_formula_sum            'C100.99 H91.97 I12 N24 O2.88 Zn6'
_chemical_formula_weight         3602.84
_chemical_name_systematic
'[1,1'-biphenyl]-2-yl)methanol (absorbed in crystalline sponge)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-22
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.5077(5)
_cell_length_b                   14.99910(10)
_cell_length_c                   34.4289(6)
_cell_measurement_reflns_used    21257
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.3540
_cell_measurement_theta_min      2.6220
_cell_volume                     15910.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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   -173.00 -86.00   0.50    2.40    -- -103.00 -10.00  46.00  174
  2  \w    -66.00 -31.00   0.50    2.40    -- -103.00  61.00 -60.00   70
  3  \w   -171.00 -91.00   0.50    2.40    -- -103.00 -45.00 150.00  160
  4  \w   -109.00 -81.00   0.50    2.40    -- -103.00 125.00  60.00   56
  5  \w   -171.00 -95.00   0.50    2.40    -- -103.00 -30.00   0.00  152
  6  \w    -66.00 -39.00   0.50    2.40    -- -103.00  61.00  90.00   54
  7  \w    -56.00 -31.00   0.50    2.40    -- -103.00 125.00  60.00   50
  8  \w    109.00 149.00   0.50    2.40    --  101.75  10.00-140.00   80
  9  \w     37.00  62.00   0.50    2.40    --  101.75 -61.00  60.00   50
 10  \w     35.00  72.00   0.50    2.40    --  101.75 -61.00 -30.00   74
 11  \w     60.00 108.00   0.50    2.40    --  101.75 -77.00-150.00   96
 12  \w     35.00  73.00   0.50    2.40    --  101.75 -61.00 -90.00   76
 13  \w     34.00  62.00   0.50    2.40    --  101.75 -61.00-150.00   56
 14  \w     56.00 105.00   0.50    2.40    --  101.75 -94.00 -30.00   98
 15  \w     29.00  90.00   0.50    2.40    --  101.75 -94.00-120.00  122
 16  \w     31.00 105.00   0.50    2.40    --  101.75 -94.00 150.00  148
 17  \w   -119.00 -44.00   0.50    0.30    --  -46.36 -10.00  46.00  150
 18  \w    -14.00  20.00   0.50    0.30    --  -46.36  10.00-140.00   68
 19  \w     40.00 119.00   0.50    0.30    --   46.36  10.00-140.00  158
 20  \w    -25.00   0.00   0.50    0.30    --   46.36 -10.00  46.00   50
 21  \w    -18.00  29.00   0.50    0.30    --  -46.36  19.00   0.00   94
 22  \w     39.00  94.00   0.50    0.30    --   46.36-125.00-120.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details
'Rigaku Oxford Difffraction, UG2 \k goniometer'
_diffrn_measurement_device_type
; Rigaku 007HF equipped with Varimax confocal mirrors and a UG2 goniometer
 and HyPix 6000HE detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0497587000
_diffrn_orient_matrix_UB_12      -0.0093679000
_diffrn_orient_matrix_UB_13      0.0113803000
_diffrn_orient_matrix_UB_21      -0.0016605000
_diffrn_orient_matrix_UB_22      0.0099043000
_diffrn_orient_matrix_UB_23      0.0442172000
_diffrn_orient_matrix_UB_31      -0.0047604000
_diffrn_orient_matrix_UB_32      -0.1017250000
_diffrn_orient_matrix_UB_33      0.0032803000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            105993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         2.137
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    19.618
_exptl_absorpt_correction_T_max  0.341
_exptl_absorpt_correction_T_min  0.076
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             6820
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.940
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1990
_refine_ls_number_reflns         29014
_refine_ls_number_restraints     1288
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1123P)^2^+55.1760P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2089
_refine_ls_wR_factor_ref         0.2208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22573
_reflns_number_total             29014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_10_48a
_cod_database_code               1571873
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     'JP-9300-04 '
_shelx_estimated_absorpt_t_max   0.340
_shelx_estimated_absorpt_t_min   0.073
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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, All O(H) groups
2. Restrained distances
 C5B-C13B
 1.51 with sigma of 0.02
 C4B-C7B
 1.5 with sigma of 0.02
 O1B-C13B = O2B-C14B = O3B-C15B
 1.43 with sigma of 0.02
 O2B-C8B = O3B-C12B
 1.37 with sigma of 0.02
 C818-C813 = C818-C817 = C813-C814 = C814-C815 = C815-C816 = C816-C817
 1.54 with sigma of 0.02
 C861-C862 = C861-C866 = C862-C863 = C863-C864 = C864-C865 = C865-C866
 1.54 with sigma of 0.02
 C839-C840 = C839-C838 = C840-C841 = C841-C842 = C842-C837 = C837-C838
 1.54 with sigma of 0.02
 C851-C852 = C851-C850 = C852-C853 = C853-C854 = C854-C849 = C849-C850
 1.54 with sigma of 0.02
 C832-C831 = C832-C833 = C831-C836 = C836-C835 = C835-C834 = C834-C833
 1.54 with sigma of 0.02
 C843-C844 = C843-C848 = C844-C845 = C845-C846 = C846-C847 = C847-C848
 1.54 with sigma of 0.02
 C856-C855 = C856-C857 = C855-C860 = C860-C859 = C859-C858 = C858-C857
 1.54 with sigma of 0.02
 C829-C830 = C829-C828 = C830-C825 = C825-C826 = C826-C827 = C827-C828
 1.54 with sigma of 0.02
 C807-C808 = C807-C812 = C808-C809 = C809-C810 = C810-C811 = C811-C812
 1.54 with sigma of 0.02
 C5B-O1B
 2.4 with sigma of 0.02
 C14B-C8B = C15B-C12B
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.02
 C7B-O2B = C7B-O3B
 2.35 with sigma of 0.04
 C4B-C13B = C13B-C6B
 2.5 with sigma of 0.04
 C11B-O3B
 2.4 with sigma of 0.04
 C818-C814 = C818-C816 = C813-C815 = C814-C816 = C815-C817
 2.54 with sigma of 0.04
 C839-C841 = C839-C837 = C840-C842 = C841-C837 = C842-C838
 2.54 with sigma of 0.04
 C861-C863 = C861-C865 = C862-C864 = C863-C865 = C864-C866
 2.54 with sigma of 0.04
 C851-C853 = C851-C849 = C852-C854 = C853-C849 = C854-C850
 2.54 with sigma of 0.04
 C832-C836 = C832-C834 = C831-C835 = C836-C834 = C835-C833
 2.54 with sigma of 0.04
 C856-C860 = C856-C858 = C855-C859 = C860-C858 = C859-C857
 2.54 with sigma of 0.04
 C843-C845 = C843-C847 = C844-C846 = C845-C847 = C846-C848
 2.54 with sigma of 0.04
 C829-C825 = C829-C827 = C830-C826 = C825-C827 = C826-C828
 2.54 with sigma of 0.04
 C807-C809 = C807-C811 = C808-C810 = C809-C811 = C810-C812
 2.54 with sigma of 0.04
 C8A-C7A \\sim C9A-C8A \\sim C10A-C9A \\sim C11A-C10A \\sim C11A-C12A \\sim
C12A-C7A
 with sigma of 0.02
 C7A-C9A \\sim C8A-C10A \\sim C9A-C11A \\sim C10A-C12A \\sim C11A-C7A \\sim
C12A-C8A
 with sigma of 0.04
 C7A-C4A \\sim C5A-C13A
 with sigma of 0.02
 O3A-C15A \\sim O2A-C14A \\sim O1A-C13A
 with sigma of 0.02
 C3B-C7B \\sim C7B-C5B
 with sigma of 0.04
 C12B-C4B \\sim C4B-C8B
 with sigma of 0.04
 C802-C803 \\sim C804-C803 \\sim C804-C805 \\sim C805-C806 \\sim C806-C801
\\sim C802-C801
 with sigma of 0.02
 C861-C865 \\sim C863-C865 \\sim C862-C866 \\sim C862-C864 \\sim C864-C866
\\sim C861-C863
 with sigma of 0.04
 C818-C813 \\sim C813-C814 \\sim C814-C815 \\sim C815-C816 \\sim C816-C817
\\sim C817-C818
 with sigma of 0.02
 C861-C862 \\sim C862-C863 \\sim C863-C864 \\sim C864-C865 \\sim C865-C866
\\sim C866-C861
 with sigma of 0.02
 C818-C816 \\sim C814-C816 \\sim C813-C817 \\sim C813-C815 \\sim C815-C817
\\sim C818-C814
 with sigma of 0.04
 C822-C821 \\sim C822-C823 \\sim C823-C824 \\sim C819-C824 \\sim C820-C819
\\sim C820-C821
 with sigma of 0.02
 C839-C837 \\sim C841-C837 \\sim C840-C838 \\sim C840-C842 \\sim C842-C838
\\sim C839-C841
 with sigma of 0.04
 C839-C840 \\sim C840-C841 \\sim C841-C842 \\sim C842-C837 \\sim C837-C838
\\sim C838-C839
 with sigma of 0.02
 C851-C852 \\sim C852-C853 \\sim C853-C854 \\sim C854-C849 \\sim C849-C850
\\sim C850-C851
 with sigma of 0.02
 C851-C849 \\sim C853-C849 \\sim C852-C850 \\sim C852-C854 \\sim C854-C850
\\sim C851-C853
 with sigma of 0.04
 C856-C855 \\sim C855-C860 \\sim C860-C859 \\sim C859-C858 \\sim C858-C857
\\sim C857-C856
 with sigma of 0.02
 C856-C858 \\sim C860-C858 \\sim C855-C857 \\sim C855-C859 \\sim C859-C857
\\sim C856-C860
 with sigma of 0.04
 C832-C831 \\sim C831-C836 \\sim C836-C835 \\sim C835-C834 \\sim C834-C833
\\sim C833-C832
 with sigma of 0.02
 C832-C834 \\sim C836-C834 \\sim C831-C833 \\sim C831-C835 \\sim C835-C833
\\sim C832-C836
 with sigma of 0.04
 C843-C844 \\sim C844-C845 \\sim C845-C846 \\sim C846-C847 \\sim C847-C848
\\sim C848-C843
 with sigma of 0.02
 C843-C847 \\sim C845-C847 \\sim C844-C848 \\sim C844-C846 \\sim C846-C848
\\sim C843-C845
 with sigma of 0.04
 C829-C830 \\sim C830-C825 \\sim C825-C826 \\sim C826-C827 \\sim C827-C828
\\sim C828-C829
 with sigma of 0.02
 C829-C827 \\sim C825-C827 \\sim C830-C828 \\sim C830-C826 \\sim C826-C828
\\sim C829-C825
 with sigma of 0.04
 C807-C808 \\sim C808-C809 \\sim C809-C810 \\sim C810-C811 \\sim C811-C812
\\sim C812-C807
 with sigma of 0.02
 C807-C811 \\sim C809-C811 \\sim C808-C812 \\sim C808-C810 \\sim C810-C812
\\sim C807-C809
 with sigma of 0.04
3. Restrained planarity
 C6B, C5B, C4B, C13B
 with sigma of 0.1
 O2B, C8B, C7B, C12B, O3B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C5B \\sim C4B \\sim C3B \\sim C7B \\sim C6B \\sim C13B \\sim C2B \\sim C12B
\\sim C8B \\sim C1B \\sim O1B \\sim C11B \\sim O3B \\sim C9B \\sim O2B \\sim
C10B \\sim C15B \\sim C14B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C861 \\sim C862 \\sim C863 \\sim C864 \\sim C865 \\sim C866: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C818 \\sim C813 \\sim C814 \\sim C815 \\sim C816 \\sim C817: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C839 \\sim C840 \\sim C841 \\sim C842 \\sim C837 \\sim C838: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C851 \\sim C852 \\sim C853 \\sim C854 \\sim C849 \\sim C850: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C832 \\sim C831 \\sim C836 \\sim C835 \\sim C834 \\sim C833: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C856 \\sim C855 \\sim C860 \\sim C859 \\sim C858 \\sim C857: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C843 \\sim C844 \\sim C845 \\sim C846 \\sim C847 \\sim C848: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C829 \\sim C830 \\sim C825 \\sim C826 \\sim C827 \\sim C828: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C823 \\sim C822 \\sim C824 \\sim C821 \\sim C819 \\sim C820: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C804 \\sim C805 \\sim C806 \\sim C801 \\sim C803 \\sim C802: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
C807 \\sim C808 \\sim C809 \\sim C810 \\sim C811 \\sim C812: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C5B, C4B, C3B, C7B, C6B, C13B, C2B, C12B, C8B, C1B, O1B, C11B, O3B, C9B, O2B,
 C10B, C15B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C818, C813, C814, C815, C816, C817
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C839, C840, C841, C842, C837, C838
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C861, C862, C863, C864, C865, C866
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C851, C852, C853, C854, C849, C850
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C843, C844, C845, C846, C847, C848
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C832, C831, C836, C835, C834, C833
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C856, C855, C860, C859, C858, C857
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C829, C830, C825, C826, C827, C828
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C807, C808, C809, C810, C811, C812
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I405)=Sof(Zn43)=Sof(I406)=1-FVAR(1)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(1)
 Sof(I409)=Sof(Zn45)=Sof(I410)=1-FVAR(2)
 Sof(I310)=Sof(I309)=Sof(Zn35)=FVAR(2)
 Sof(I303)=Sof(I304)=1-FVAR(3)
 Sof(I403)=Sof(I404)=FVAR(3)
 Sof(I407)=Sof(I408)=1-FVAR(4)
 Sof(I308)=Sof(I307)=FVAR(4)
 Sof(I411)=1-FVAR(5)
 Sof(I311)=FVAR(5)
 Sof(I412)=1-FVAR(6)
 Sof(I312)=FVAR(6)
 Fixed Sof: I302(0.59086) I301(0.59086) Zn31(0.59086) O3A(0.74448)
 O2A(0.74448) O1A(0.74448) H1A(0.74448) C1A(0.74448) H1AA(0.74448) C2A(0.74448)
 H2A(0.74448) C3A(0.74448) H3A(0.74448) C4A(0.74448) C5A(0.74448) C6A(0.74448)
 H6A(0.74448) C7A(0.74448) C12A(0.74448) C8A(0.74448) C9A(0.74448) H9A(0.74448)
 C10A(0.74448) H10A(0.74448) C11A(0.74448) H11A(0.74448) C15A(0.74448)
 H15A(0.74448) H15B(0.74448) H15C(0.74448) C13A(0.74448) H13A(0.74448)
 H13B(0.74448) C14A(0.74448) H14A(0.74448) H14B(0.74448) H14C(0.74448)
 I402(0.36257) Zn41(0.36257) I401(0.36257) C4B(0.21484) C5B(0.21484)
 C6B(0.21484) H6B(0.21484) C1B(0.21484) H1B(0.21484) C2B(0.21484) H2B(0.21484)
 C3B(0.21484) H3B(0.21484) C7B(0.21484) C12B(0.21484) C11B(0.21484)
 H11B(0.21484) C10B(0.21484) H10B(0.21484) C9B(0.21484) H9B(0.21484)
 C8B(0.21484) O2B(0.21484) O3B(0.21484) C805(0.31325) H80A(0.31325)
 H80B(0.31325) C801(0.31325) H80C(0.31325) H80D(0.31325) C803(0.31325)
 H80E(0.31325) H80F(0.31325) C806(0.31325) H80G(0.31325) H80H(0.31325)
 C823(0.28233) H82A(0.28233) H82B(0.28233) C822(0.28233) H82C(0.28233)
 H82D(0.28233) C821(0.28233) H82E(0.28233) H82F(0.28233) C819(0.28233)
 H81A(0.28233) H81B(0.28233) C820(0.28233) H82G(0.28233) H82H(0.28233)
 C824(0.28233) H82I(0.28233) H82J(0.28233) C804(0.31325) H80I(0.31325)
 H80J(0.31325) C802(0.31325) H80K(0.31325) H80L(0.31325) C15B(0.21484)
 H15D(0.21484) H15E(0.21484) H15F(0.21484) C14B(0.21484) H14D(0.21484)
 H14E(0.21484) H14F(0.21484) O1B(0.21484) H1BA(0.21484) C13B(0.21484)
 H13C(0.21484) H13D(0.21484) C851(0.17616) H85A(0.17616) H85B(0.17616)
 C852(0.17616) H85C(0.17616) H85D(0.17616) C853(0.17616) H85E(0.17616)
 H85F(0.17616) C854(0.17616) H85G(0.17616) H85H(0.17616) C849(0.17616)
 H84A(0.17616) H84B(0.17616) C850(0.17616) H85I(0.17616) H85J(0.17616)
 C839(0.18714) H83A(0.18714) H83B(0.18714) C840(0.18714) H84C(0.18714)
 H84D(0.18714) C841(0.18714) H84E(0.18714) H84F(0.18714) C842(0.18714)
 H84G(0.18714) H84H(0.18714) C837(0.18714) H83C(0.18714) H83D(0.18714)
 C838(0.18714) H83E(0.18714) H83F(0.18714) C832(0.20221) H83G(0.20221)
 H83H(0.20221) C831(0.20221) H83I(0.20221) H83J(0.20221) C836(0.20221)
 H83K(0.20221) H83L(0.20221) C835(0.20221) H83M(0.20221) H83N(0.20221)
 C834(0.20221) H83O(0.20221) H83P(0.20221) C833(0.20221) H83Q(0.20221)
 H83R(0.20221) C856(0.23754) H85K(0.23754) H85L(0.23754) C855(0.23754)
 H85M(0.23754) H85N(0.23754) C860(0.23754) H86A(0.23754) H86B(0.23754)
 C859(0.23754) H85O(0.23754) H85P(0.23754) C858(0.23754) H85Q(0.23754)
 H85R(0.23754) C857(0.23754) H85S(0.23754) H85T(0.23754) C843(0.1672)
 H84I(0.1672) H84J(0.1672) C844(0.1672) H84K(0.1672) H84L(0.1672) C845(0.1672)
 H84M(0.1672) H84N(0.1672) C846(0.1672) H84O(0.1672) H84P(0.1672) C847(0.1672)
 H84Q(0.1672) H84R(0.1672) C848(0.1672) H84S(0.1672) H84T(0.1672) C861(0.2481)
 H86C(0.2481) H86D(0.2481) C862(0.2481) H86E(0.2481) H86F(0.2481) C863(0.2481)
 H86G(0.2481) H86H(0.2481) C864(0.2481) H86I(0.2481) H86J(0.2481) C865(0.2481)
 H86K(0.2481) H86L(0.2481) C866(0.2481) H86M(0.2481) H86N(0.2481) C829(0.13065)
 H82K(0.13065) H82L(0.13065) C830(0.13065) H83S(0.13065) H83T(0.13065)
 C825(0.13065) H82M(0.13065) H82N(0.13065) C826(0.13065) H82O(0.13065)
 H82P(0.13065) C827(0.13065) H82Q(0.13065) H82R(0.13065) C828(0.13065)
 H82S(0.13065) H82T(0.13065) I502(0.04655) I501(0.04655) Zn51(0.04655)
 C818(0.31531) H81C(0.31531) H81D(0.31531) C813(0.31531) H81E(0.31531)
 H81F(0.31531) C814(0.31531) H81G(0.31531) H81H(0.31531) C815(0.31531)
 H81I(0.31531) H81J(0.31531) C816(0.31531) H81K(0.31531) H81L(0.31531)
 C817(0.31531) H81M(0.31531) H81N(0.31531) C807(0.17269) H80M(0.17269)
 H80N(0.17269) C808(0.17269) H80O(0.17269) H80P(0.17269) C809(0.17269)
 H80Q(0.17269) H80R(0.17269) C810(0.17269) H81O(0.17269) H81P(0.17269)
 C811(0.17269) H81Q(0.17269) H81R(0.17269) C812(0.17269) H81S(0.17269)
 H81T(0.17269)
 Fixed Uiso: C856(0.08) C855(0.08) C860(0.08) C859(0.08) C858(0.08) C857(0.08)
 C861(0.08) C862(0.08) C863(0.08) C864(0.08) C865(0.08) C866(0.08) I502(0.08)
 I501(0.08) Zn51(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C805(H80A,H80B), C801(H80C,H80D), C803(H80E,H80F), C806(H80G,
 H80H), C823(H82A,H82B), C822(H82C,H82D), C821(H82E,H82F), C819(H81A,H81B),
 C820(H82G,H82H), C824(H82I,H82J), C804(H80I,H80J), C802(H80K,H80L), C13B(H13C,
 H13D), C851(H85A,H85B), C852(H85C,H85D), C853(H85E,H85F), C854(H85G,H85H),
 C849(H84A,H84B), C850(H85I,H85J), C839(H83A,H83B), C840(H84C,H84D), C841(H84E,
 H84F), C842(H84G,H84H), C837(H83C,H83D), C838(H83E,H83F), C832(H83G,H83H),
 C831(H83I,H83J), C836(H83K,H83L), C835(H83M,H83N), C834(H83O,H83P), C833(H83Q,
 H83R), C856(H85K,H85L), C855(H85M,H85N), C860(H86A,H86B), C859(H85O,H85P),
 C858(H85Q,H85R), C857(H85S,H85T), C843(H84I,H84J), C844(H84K,H84L), C845(H84M,
 H84N), C846(H84O,H84P), C847(H84Q,H84R), C848(H84S,H84T), C861(H86C,H86D),
 C862(H86E,H86F), C863(H86G,H86H), C864(H86I,H86J), C865(H86K,H86L), C866(H86M,
 H86N), C829(H82K,H82L), C830(H83S,H83T), C825(H82M,H82N), C826(H82O,H82P),
 C827(H82Q,H82R), C828(H82S,H82T), C818(H81C,H81D), C813(H81E,H81F), C814(H81G,
 H81H), C815(H81I,H81J), C816(H81K,H81L), C817(H81M,H81N), C807(H80M,H80N),
 C808(H80O,H80P), C809(H80Q,H80R), C810(H81O,H81P), C811(H81Q,H81R), C812(H81S,
 H81T)
7.b Aromatic/amide H refined with riding coordinates:
 C333(H333), C322(H322), C317(H317), C332(H332), C328(H328), C369(H369),
 C318(H318), C351(H351), C350(H350), C320(H320), C348(H348), C335(H335),
 C336(H336), C349(H349), C329(H329), C323(H323), C331(H331), C315(H315),
 C353(H353), C319(H319), C364(H364), C358(H358), C340(H340), C365(H365),
 C313(H313), C355(H355), C368(H368), C354(H354), C356(H356), C367(H367),
 C330(H330), C359(H359), C366(H366), C304(H304), C312(H312), C314(H314),
 C341(H341), C371(H371), C305(H305), C1A(H1AA), C2A(H2A), C3A(H3A), C6A(H6A),
 C337(H337), C338(H338), C347(H347), C346(H346), C372(H372), C302(H302),
 C301(H301), C9A(H9A), C10A(H10A), C11A(H11A), C310(H310), C311(H311), C6B(H6B),
  C1B(H1B), C2B(H2B), C3B(H3B), C11B(H11B), C10B(H10B), C9B(H9B)
7.c Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A), C4B(C5B,C6B,C1B,C2B,C3B), C7B(C12B,C11B,C10B,C9B,C8B)
7.d Tetrahedral OH refined with riding coordinates:
 O1B(H1BA)
7.e Idealised Me refined with everything fixed:
 C15B(H15D,H15E,H15F), C14B(H14D,H14E,H14F)
7.f Idealised Me refined as rotating group:
 C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C)
7.g Idealised tetrahedral OH refined as rotating group:
 O1A(H1A)
;
_shelx_res_checksum              7961
_shelx_hkl_checksum              60292
_olex2_date_sample_data_collection 2022-03-07
_olex2_date_sample_submission    2022-03-07
_olex2_submission_original_sample_id 50_10_48a
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.553
_oxdiff_exptl_absorpt_empirical_full_min 0.502