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_1571867
_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, 0.828(C15 H16 O3), 0.66(C6 H12)'
_chemical_formula_sum            'C88.38 H69.11 I12 N24 O2.48 Zn6'
_chemical_formula_weight         3422.02
_chemical_name_systematic
; 
(2',6'-dimethoxy-[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             2024-01-23
_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                 102.066(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.5448(8)
_cell_length_b                   14.9824(2)
_cell_length_c                   34.3898(8)
_cell_measurement_reflns_used    19094
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.2040
_cell_measurement_theta_min      2.6130
_cell_volume                     15894.1(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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 2014/5 (Sheldrick, 2014)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.993
_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   -118.00 -92.00   0.50    3.50    -- -103.00 -31.00-175.00   52
  2  \w    -99.00 -74.00   0.50    3.50    -- -103.00 125.00  90.00   50
  3  \w    -66.00 -39.00   0.50    3.50    -- -103.00  61.00  60.00   54
  4  \w    -56.00 -30.00   0.50    3.50    -- -103.00  61.00-180.00   52
  5  \w    -60.00 -33.00   0.50    3.50    -- -103.00  61.00 120.00   54
  6  \w    -57.00 -32.00   0.50    3.50    -- -103.00  61.00-120.00   50
  7  \w    -69.00 -30.00   0.50    3.50    -- -103.00 125.00  90.00   78
  8  \w    -57.00 -32.00   0.50    3.50    -- -103.00  61.00  90.00   50
  9  \w     89.00 175.00   0.50    3.50    --  101.75  31.00 -16.00  172
 10  \w     34.00  69.00   0.50    3.50    --  101.75 -61.00-120.00   70
 11  \w     33.00  75.00   0.50    3.50    --  101.75 -61.00 -90.00   84
 12  \w     35.00  75.00   0.50    3.50    --  101.75 -61.00 150.00   80
 13  \w     89.00 170.00   0.50    3.50    --  101.75  30.00  90.00  162
 14  \w     45.00  72.00   0.50    3.50    --  101.75 -61.00  30.00   54
 15  \w     35.00  67.00   0.50    3.50    --  101.75 -61.00-180.00   64
 16  \w     34.00 106.00   0.50    3.50    --  101.75-125.00-180.00  144
 17  \w     46.00  75.00   0.50    3.50    --  101.75 -61.00  60.00   58
 18  \w     29.00  71.00   0.50    3.50    --  101.75 -61.00-150.00   84
 19  \w    -28.00  17.00   0.50    0.40    --  -46.36  31.00 -16.00   90
 20  \w   -107.00 -35.00   0.50    0.40    --  -46.36 -31.00-175.00  144
 21  \w    -18.00  31.00   0.50    0.40    --   46.36 -31.00-175.00   98
 22  \w     34.00 117.00   0.50    0.40    --   46.36  31.00 -16.00  166
 23  \w     -4.00  29.00   0.50    0.40    --  -46.36  19.00 120.00   66
 24  \w    -26.00  39.00   0.50    0.40    --   46.36 -37.00  30.00  130
;
_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      -0.0497879000
_diffrn_orient_matrix_UB_12      0.0044712000
_diffrn_orient_matrix_UB_13      -0.0126682000
_diffrn_orient_matrix_UB_21      -0.0023037000
_diffrn_orient_matrix_UB_22      0.0414541000
_diffrn_orient_matrix_UB_23      0.0404785000
_diffrn_orient_matrix_UB_31      0.0033978000
_diffrn_orient_matrix_UB_32      0.0939927000
_diffrn_orient_matrix_UB_33      -0.0172706000
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            100011
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         1.729
_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    19.606
_exptl_absorpt_correction_T_max  0.289
_exptl_absorpt_correction_T_min  0.051
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
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    1.430
_exptl_crystal_description       block
_exptl_crystal_F_000             6413
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.348
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1647
_refine_ls_number_reflns         28888
_refine_ls_number_restraints     793
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0825
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1462P)^2^+62.5282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2556
_refine_ls_wR_factor_ref         0.2729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20854
_reflns_number_total             28888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_5_96a
_cod_database_code               1571867
_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   0.271
_shelx_estimated_absorpt_t_min   0.064
_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
 O2A-C14A
 1.43 with sigma of 0.02
 O3B-C15B = C14B-O2B = C13B-O1B
 1.43 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 C7B-C4B
 1.5 with sigma of 0.02
 C13B-C5B
 1.51 with sigma of 0.02
 O3B-C12B = O2B-C8B
 1.37 with sigma of 0.02
 C4-C5 = C4-C10 = C5-C6 = C6-C7 = C7-C9 = C9-C10
 1.54 with sigma of 0.02
 C11-C12 = C11-C17 = C12-C13 = C13-C15 = C15-C16 = C16-C17
 1.54 with sigma of 0.02
 C2-C3 = C2-C18 = C3-C1 = C1-C8 = C8-C14 = C14-C18
 1.54 with sigma of 0.02
 C14B-C8B = C12B-C15B
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.02
 C5B-O1B
 2.4 with sigma of 0.04
 C4-C6 = C4-C9 = C5-C7 = C6-C9 = C7-C10
 2.54 with sigma of 0.04
 C11-C13 = C11-C16 = C12-C15 = C13-C16 = C15-C17
 2.54 with sigma of 0.04
 C2-C1 = C2-C14 = C3-C8 = C1-C14 = C8-C18
 2.54 with sigma of 0.04
 C8A-C7A \\sim C9A-C8A \\sim C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim
C7A-C12A
 with sigma of 0.02
 O1A-C13A \\sim O3A-C15A
 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
 C4B-C13B \\sim C13B-C6B
 with sigma of 0.02
 C7B-O3B \\sim O3B-C11B
 with sigma of 0.02
 C7B-O2B \\sim O2B-C9B
 with sigma of 0.02
 C4-C5 \\sim C5-C6 \\sim C6-C7 \\sim C7-C9 \\sim C9-C10 \\sim C10-C4
 with sigma of 0.02
 C4-C9 \\sim C6-C9 \\sim C5-C10 \\sim C5-C7 \\sim C7-C10 \\sim C4-C6
 with sigma of 0.04
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 Zn32-N306 \\sim Zn42-N306
 with sigma of 0.02
 Zn32-N307 \\sim Zn42-N307
 with sigma of 0.02
 I304-I303 \\sim I404-I403
 with sigma of 0.04
 I304-N306 \\sim I404-N306
 with sigma of 0.04
 I304-N307 \\sim I404-N307
 with sigma of 0.04
 I303-N306 \\sim I403-N306
 with sigma of 0.04
 I303-N307 \\sim I403-N307
 with sigma of 0.04
 I409-Zn45 \\sim I309-Zn35
 with sigma of 0.02
 I410-Zn45 \\sim I310-Zn35
 with sigma of 0.02
 Zn45-N318 \\sim Zn35-N318
 with sigma of 0.02
 Zn45-N319 \\sim Zn35-N319
 with sigma of 0.02
 I409-I410 \\sim I309-I310
 with sigma of 0.04
 I409-N318 \\sim I309-N318
 with sigma of 0.04
 I409-N319 \\sim I309-N319
 with sigma of 0.04
 I410-N318 \\sim I310-N318
 with sigma of 0.04
 I410-N319 \\sim I310-N319
 with sigma of 0.04
 I312-Zn36 \\sim I412-Zn46
 with sigma of 0.02
 I311-Zn36 \\sim I411-Zn46
 with sigma of 0.02
 Zn36-N324 \\sim Zn46-N324
 with sigma of 0.02
 I312-I311 \\sim I412-I411
 with sigma of 0.04
 I312-N324 \\sim I412-N324
 with sigma of 0.04
 I311-N324 \\sim I411-N324
 with sigma of 0.04
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 Zn43-N311 \\sim Zn33-N311
 with sigma of 0.02
 I406-I405 \\sim I306-I305
 with sigma of 0.04
 I406-N311 \\sim I306-N311
 with sigma of 0.04
 I405-N311 \\sim I305-N311
 with sigma of 0.04
 I307-Zn34 \\sim I407-Zn44
 with sigma of 0.02
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 Zn34-N312 \\sim Zn44-N312
 with sigma of 0.02
 Zn34-N313 \\sim Zn44-N313
 with sigma of 0.02
 I307-I308 \\sim I407-I408
 with sigma of 0.04
 I307-N312 \\sim I407-N312
 with sigma of 0.04
 I307-N313 \\sim I407-N313
 with sigma of 0.04
 I308-N312 \\sim I408-N312
 with sigma of 0.04
 I308-N313 \\sim I408-N313
 with sigma of 0.04
 I402-Zn31 \\sim I302-Zn41
 with sigma of 0.02
 I401-Zn31 \\sim I301-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I402-I401 \\sim I302-I301
 with sigma of 0.04
 I402-N301 \\sim I302-N301
 with sigma of 0.04
 I401-N301 \\sim I301-N301
 with sigma of 0.04
 I305-Zn33 \\sim I505-Zn53
 with sigma of 0.02
 I506-Zn53 \\sim I406-Zn43
 with sigma of 0.02
 C11-C12 \\sim C12-C13 \\sim C13-C15 \\sim C15-C16 \\sim C16-C17 \\sim C17-C11
 with sigma of 0.02
 C11-C16 \\sim C13-C16 \\sim C12-C17 \\sim C12-C15 \\sim C15-C17 \\sim C11-C13
 with sigma of 0.04
 C2-C3 \\sim C3-C1 \\sim C1-C8 \\sim C8-C14 \\sim C14-C18 \\sim C18-C2
 with sigma of 0.02
 C2-C14 \\sim C1-C14 \\sim C3-C18 \\sim C3-C8 \\sim C8-C18 \\sim C2-C1
 with sigma of 0.04
3. Restrained planarity
 C4B, C5B, C6B, C13B
 with sigma of 0.1
 O2B, C8B, C7B, C12B, O3B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C8A \\sim O3A \\sim C12A \\sim C15A \\sim C7A \\sim C11A \\sim C4A \\sim C10A
\\sim C5A \\sim C3A \\sim O2A \\sim C9A \\sim C6A \\sim C13A \\sim C2A \\sim
C14A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C8B \\sim C4B \\sim C5B \\sim C3B \\sim C7B \\sim C6B \\sim C13B \\sim C2B
\\sim C12B \\sim C1B \\sim O1B \\sim C9B \\sim O2B \\sim O3B \\sim C11B \\sim
C10B \\sim C14B \\sim C15B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C4 \\sim C5 \\sim C6 \\sim C7 \\sim C9 \\sim C10: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C350 \\sim N318 \\sim C354 \\sim C353 \\sim C352 \\sim C351: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C11 \\sim C12 \\sim C13 \\sim C15 \\sim C16 \\sim C17: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C2 \\sim C3 \\sim C1 \\sim C8 \\sim C14 \\sim C18: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn55) = Uanis(Zn45) = Uanis(Zn35)
5. Rigid body (RIGU) restrains
 C8B, C4B, C5B, C3B, C7B, C6B, C13B, C2B, C12B, C1B, O1B, C9B, O2B, O3B, C11B,
 C10B, C14B, C15B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, C5, C6, C7, C9, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C350, N318, C354, C353, C352, C351
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C12, C13, C15, C16, C17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C3, C1, C8, C14, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(I307)+Sof(I308)+Sof(Zn34)]+1*[Sof(I407)+Sof(Zn44)+Sof(I408)]=1 with
 esd of 0.00001
 Sof(I307)=Sof(I308)=Sof(Zn34)=FVAR(1)
 Sof(I407)=Sof(Zn44)=Sof(I408)=FVAR(2)
 Fixed Sof: I304(0.52) I312(0.56109) I409(0.4293) I311(0.56109) I406(0.48556)
 I402(0.38253) I401(0.38253) I303(0.52) I410(0.4293) I405(0.48556)
 Zn36(0.56109) Zn32(0.52) Zn45(0.4293) Zn43(0.48556) Zn31(0.38253) O3A(0.64176)
 O2A(0.64176) O1A(0.64176) H1A(0.64176) C4A(0.64176) C5A(0.64176) C6A(0.64176)
 H6A(0.64176) C1A(0.64176) H1AA(0.64176) C2A(0.64176) H2A(0.64176) C3A(0.64176)
 H3A(0.64176) C7A(0.64176) C8A(0.64176) C12A(0.64176) C9A(0.64176) H9A(0.64176)
 C10A(0.64176) H10A(0.64176) C11A(0.64176) H11A(0.64176) C15A(0.64176)
 H15A(0.64176) H15B(0.64176) H15C(0.64176) C13A(0.64176) H13A(0.64176)
 H13B(0.64176) C14A(0.64176) H14A(0.64176) H14B(0.64176) H14C(0.64176)
 I404(0.48) Zn42(0.48) I403(0.48) I309(0.43419) Zn35(0.43419) I310(0.43419)
 I411(0.3876) Zn46(0.3876) I412(0.3876) I305(0.46002) Zn33(0.46002)
 I306(0.46002) I301(0.58506) Zn41(0.58506) I302(0.58506) I509(0.1365)
 I510(0.1365) Zn55(0.1365) I511(0.05131) I512(0.05131) Zn56(0.05131)
 I505(0.05441) I506(0.05441) Zn53(0.05441) I502(0.03241) I501(0.03241)
 Zn51(0.03241) C4B(0.18615) C5B(0.18615) C6B(0.18615) H6B(0.18615) C1B(0.18615)
 H1B(0.18615) C2B(0.18615) H2B(0.18615) C3B(0.18615) H3B(0.18615) O3B(0.18615)
 C7B(0.18615) C8B(0.18615) C9B(0.18615) H9B(0.18615) C10B(0.18615)
 H10B(0.18615) C11B(0.18615) H11B(0.18615) C12B(0.18615) C4(0.20925)
 H4A(0.20925) H4B(0.20925) C5(0.20925) H5A(0.20925) H5B(0.20925) C6(0.20925)
 H6C(0.20925) H6D(0.20925) C7(0.20925) H7A(0.20925) H7B(0.20925) C9(0.20925)
 H9C(0.20925) H9D(0.20925) C10(0.20925) H10C(0.20925) H10D(0.20925)
 C11(0.19701) H11C(0.19701) H11D(0.19701) C12(0.19701) H12A(0.19701)
 H12B(0.19701) C13(0.19701) H13E(0.19701) H13F(0.19701) C15(0.19701)
 H15G(0.19701) H15H(0.19701) C16(0.19701) H16A(0.19701) H16B(0.19701)
 C17(0.19701) H17A(0.19701) H17B(0.19701) O2B(0.18615) C14B(0.18615)
 H14D(0.18615) H14E(0.18615) H14F(0.18615) C15B(0.18615) H15D(0.18615)
 H15E(0.18615) H15F(0.18615) O1B(0.18615) H1BA(0.18615) C13B(0.18615)
 H13C(0.18615) H13D(0.18615) C2(0.25329) H2C(0.25329) H2D(0.25329) C3(0.25329)
 H3C(0.25329) H3D(0.25329) C1(0.25329) H1C(0.25329) H1D(0.25329) C8(0.25329)
 H8A(0.25329) H8B(0.25329) C14(0.25329) H14G(0.25329) H14H(0.25329)
 C18(0.25329) H18A(0.25329) H18B(0.25329)
 Fixed Uiso: I511(0.08) I512(0.08) Zn56(0.08) I505(0.08) I506(0.08) Zn53(0.08)
 I502(0.08) I501(0.08) Zn51(0.08) C4(0.08) H4A(0.08) H4B(0.08) C5(0.08)
 H5A(0.08) H5B(0.08) C6(0.08) H6C(0.08) H6D(0.08) C7(0.08) H7A(0.08) H7B(0.08)
 C9(0.08) H9C(0.08) H9D(0.08) C10(0.08) H10C(0.08) H10D(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C4(H4A,H4B), C5(H5A,H5B), C6(H6C,H6D), C7(H7A,H7B), C9(H9C,
 H9D), C10(H10C,H10D), C11(H11C,H11D), C12(H12A,H12B), C13(H13E,H13F), C15(H15G,
 H15H), C16(H16A,H16B), C17(H17A,H17B), C13B(H13C,H13D), C2(H2C,H2D), C3(H3C,
 H3D), C1(H1C,H1D), C8(H8A,H8B), C14(H14G,H14H), C18(H18A,H18B)
7.b Aromatic/amide H refined with riding coordinates:
 C349(H349), C315(H315), C369(H369), C367(H367), C371(H371), C348(H348),
 C317(H317), C359(H359), C313(H313), C320(H320), C372(H372), C312(H312),
 C328(H328), C358(H358), C365(H365), C366(H366), C364(H364), C314(H314),
 C353(H353), C318(H318), C368(H368), C322(H322), C332(H332), C346(H346),
 C356(H356), C319(H319), C304(H304), C335(H335), C323(H323), C333(H333),
 C354(H354), C355(H355), C305(H305), C6A(H6A), C1A(H1AA), C2A(H2A), C3A(H3A),
 C336(H336), C338(H338), C330(H330), C331(H331), C329(H329), C301(H301),
 C337(H337), C347(H347), C302(H302), C340(H340), C310(H310), C311(H311),
 C341(H341), C9A(H9A), C10A(H10A), C11A(H11A), C350(H350), C351(H351), C6B(H6B),
  C1B(H1B), C2B(H2B), C3B(H3B), C9B(H9B), C10B(H10B), C11B(H11B)
7.c Fitted hexagon refined as free rotating group:
 C4A(C5A,C6A,C1A,C2A,C3A), C4B(C5B,C6B,C1B,C2B,C3B), C7B(C8B,C9B,C10B,C11B,C12B)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1B(H1BA)
7.e Idealised Me refined with everything fixed:
 C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C), C14B(H14D,H14E,H14F), C15B(H15D,
 H15E,H15F)
;
_shelx_res_checksum              50074
_shelx_hkl_checksum              56464
_olex2_date_sample_data_collection 2022-01-31
_olex2_date_sample_submission    2022-01-31
_olex2_submission_original_sample_id 50_5_96a
_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 2.702
_oxdiff_exptl_absorpt_empirical_full_min 0.446