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_1571861
_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
'C71.959 H48 I12 N24 Zn6, 0.666(C15 H16 O3), 0.408(C6 H12)'
_chemical_formula_sum            'C84.39 H63.55 I12 N24 O2 Zn6'
_chemical_formula_weight         3360.86
_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             2024-02-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.01.24 svn.r2f8d729c for OlexSys, GUI svn.r6923)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.239(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.6699(9)
_cell_length_b                   14.9780(2)
_cell_length_c                   34.5752(9)
_cell_measurement_reflns_used    13434
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.0430
_cell_measurement_theta_min      3.2150
_cell_volume                     16028.0(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.994
_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   -154.00 -92.00   0.50    5.00    -- -103.00  -4.00 118.00  124
  2  \w    -84.00 -59.00   0.50    5.00    -- -103.00  -4.00 118.00   50
  3  \w    -73.00 -45.00   0.50    5.00    -- -103.00 125.00   0.00   56
  4  \w   -110.00 -77.00   0.50    5.00    -- -103.00 125.00   0.00   66
  5  \w    -75.00 -47.00   0.50    5.00    -- -103.00 125.00 -90.00   56
  6  \w   -110.00 -84.00   0.50    5.00    -- -103.00 125.00 -90.00   52
  7  \w    -60.00 -35.00   0.50    5.00    -- -103.00  61.00   0.00   50
  8  \w     53.00 163.00   0.50    5.00    --  101.75   4.00 -63.00  220
  9  \w     70.00 106.00   0.50    5.00    --  101.75 -94.00 -30.00   72
 10  \w     29.00  75.00   0.50    5.00    --  101.75 -61.00-120.00   92
 11  \w     39.00  66.00   0.50    5.00    --  101.75 -94.00-150.00   54
 12  \w     30.00  59.00   0.50    5.00    --  101.75 -61.00 -90.00   58
 13  \w     54.00 102.00   0.50    5.00    --  101.75 -94.00 -60.00   96
 14  \w     81.00 106.00   0.50    5.00    --  101.75 -94.00-150.00   50
 15  \w     46.00  71.00   0.50    5.00    --  101.75 -61.00 -30.00   50
 16  \w     29.00  72.00   0.50    5.00    --  101.75 -61.00  30.00   86
 17  \w     89.00 144.00   0.50    5.00    --  101.75  45.00   0.00  110
 18  \w     30.00  62.00   0.50    5.00    --  101.75 -94.00 -30.00   64
 19  \w    -19.00   6.00   0.50    0.80    --  -46.48   4.00 -63.00   50
 20  \w   -119.00 -27.00   0.50    0.80    --  -46.48  -4.00 118.00  184
 21  \w     10.00 114.00   0.50    0.80    --   46.48   4.00 -63.00  208
 22  \w     27.00  90.00   0.50    0.80    --   46.48-125.00  30.00  126
 23  \w      0.00  25.00   0.50    0.80    --   46.48 -19.00 -60.00   50
 24  \w    -24.00   1.00   0.50    0.80    --   46.48  -4.00 118.00   50
;
_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      -0.0491223000
_diffrn_orient_matrix_UB_12      -0.0043903000
_diffrn_orient_matrix_UB_13      -0.0166028000
_diffrn_orient_matrix_UB_21      0.0079736000
_diffrn_orient_matrix_UB_22      -0.0022372000
_diffrn_orient_matrix_UB_23      -0.0424103000
_diffrn_orient_matrix_UB_31      0.0019447000
_diffrn_orient_matrix_UB_32      -0.1027209000
_diffrn_orient_matrix_UB_33      0.0016151000
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            101230
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.252
_diffrn_reflns_theta_min         1.719
_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    19.429
_exptl_absorpt_correction_T_max  0.406
_exptl_absorpt_correction_T_min  0.178
_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    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             6280
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.407
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1521
_refine_ls_number_reflns         29170
_refine_ls_number_restraints     606
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0913
_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^)+(0.1472P)^2^+76.6313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2718
_refine_ls_wR_factor_ref         0.2939
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19768
_reflns_number_total             29170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_1_96a
_cod_database_code               1571861
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)3'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.389
_shelx_estimated_absorpt_t_min   0.159
_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
 O1A-C13A
 1.43 with sigma of 0.01
 O2A-C14A = O3A-C15A
 1.43 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 C7A-C4A
 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
 C4B-C7B
 1.5 with sigma of 0.02
 C5B-C13B
 1.51 with sigma of 0.02
 C808-C809 = C808-C807 = C809-C810 = C810-C811 = C811-C812 = C812-C807
 1.54 with sigma of 0.02
 C805-C804 = C805-C806 = C804-C803 = C803-C802 = C802-C801 = C801-C806
 1.54 with sigma of 0.02
 C5A-O1A
 2.4 with sigma of 0.01
 C6A-C13A = C13A-C4A
 2.5 with sigma of 0.04
 C5B-O1B
 2.4 with sigma of 0.04
 C4B-C13B
 2.5 with sigma of 0.04
 O1B-C5B
 2.4 with sigma of 0.04
 C6B-C13B = C13B-C4B
 2.5 with sigma of 0.04
 C8B-C14B
 2.4 with sigma of 0.04
 C12B-C15B
 2.4 with sigma of 0.02
 C808-C810 = C808-C812 = C809-C811 = C810-C812 = C811-C807
 2.54 with sigma of 0.04
 C805-C803 = C805-C801 = C804-C802 = C803-C801 = C802-C806
 2.54 with sigma of 0.04
 C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim C7A-C12A \\sim C8A-C7A \\sim
C9A-C8A
 with sigma of 0.02
 C5B-C7B \\sim C7B-C3B
 with sigma of 0.04
 C7A-C9A \\sim C8A-C10A \\sim C9A-C11A \\sim C10A-C12A \\sim C11A-C7A \\sim
C12A-C8A
 with sigma of 0.04
 O3A-C15A \\sim O2A-C14A
 with sigma of 0.02
 C12B-C4B \\sim C4B-C8B
 with sigma of 0.04
 C14B-C8B \\sim C12B-C15B
 with sigma of 0.04
 C9B-O2B \\sim O2B-C7B
 with sigma of 0.04
 C7B-O3B \\sim O3B-C11B
 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-N318 \\sim Zn46-N318
 with sigma of 0.02
 Zn36-N319 \\sim Zn46-N319
 with sigma of 0.02
 I312-I311 \\sim I412-I411
 with sigma of 0.04
 I312-N318 \\sim I412-N318
 with sigma of 0.04
 I312-N319 \\sim I412-N319
 with sigma of 0.04
 I311-N318 \\sim I411-N318
 with sigma of 0.04
 I311-N319 \\sim I411-N319
 with sigma of 0.04
 I405-Zn43 \\sim I305-Zn33
 with sigma of 0.02
 I406-Zn43 \\sim I306-Zn33
 with sigma of 0.02
 Zn43-N306 \\sim Zn33-N306
 with sigma of 0.02
 Zn43-N307 \\sim Zn33-N307
 with sigma of 0.02
 I405-I406 \\sim I305-I306
 with sigma of 0.04
 I405-N306 \\sim I305-N306
 with sigma of 0.04
 I405-N307 \\sim I305-N307
 with sigma of 0.04
 I406-N306 \\sim I306-N306
 with sigma of 0.04
 I406-N307 \\sim I306-N307
 with sigma of 0.04
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn41-N301
 with sigma of 0.02
 I301-I302 \\sim I401-I402
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 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-N317 \\sim Zn35-N317
 with sigma of 0.02
 I409-I410 \\sim I309-I310
 with sigma of 0.04
 I409-N317 \\sim I309-N317
 with sigma of 0.04
 I410-N317 \\sim I310-N317
 with sigma of 0.04
 I304-Zn32 \\sim I504-Zn52
 with sigma of 0.02
 I303-Zn32 \\sim I503-Zn52
 with sigma of 0.02
 Zn32-N305 \\sim Zn52-N305
 with sigma of 0.02
 I304-I303 \\sim I504-I503
 with sigma of 0.04
 I304-N305 \\sim I504-N305
 with sigma of 0.04
 I303-N305 \\sim I503-N305
 with sigma of 0.04
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 I307-Zn34 \\sim I407-Zn44
 with sigma of 0.02
 Zn34-N313 \\sim Zn44-N313
 with sigma of 0.02
 Zn34-N312 \\sim Zn44-N312
 with sigma of 0.02
 I308-I307 \\sim I408-I407
 with sigma of 0.04
 I308-N313 \\sim I408-N313
 with sigma of 0.04
 I308-N312 \\sim I408-N312
 with sigma of 0.04
 I307-N313 \\sim I407-N313
 with sigma of 0.04
 I307-N312 \\sim I407-N312
 with sigma of 0.04
 N307-C323 \\sim N307-C423
 with sigma of 0.02
 C321-C322 \\sim C321-C422
 with sigma of 0.02
 C322-C323 \\sim C422-C423
 with sigma of 0.02
 N307-C322 \\sim N307-C422
 with sigma of 0.04
 C321-C323 \\sim C321-C423
 with sigma of 0.04
 N317-C347 \\sim N317-C0
 with sigma of 0.02
 C345-C346 \\sim C345-C3
 with sigma of 0.02
 C346-C347 \\sim C3-C0
 with sigma of 0.02
 N317-C346 \\sim N317-C3
 with sigma of 0.04
 C345-C347 \\sim C345-C0
 with sigma of 0.04
 I510-Zn55 \\sim I410-Zn45
 with sigma of 0.02
 I409-Zn45 \\sim I509-Zn55
 with sigma of 0.02
 C808-C809 \\sim C809-C810 \\sim C810-C811 \\sim C811-C812 \\sim C812-C807
\\sim C807-C808
 with sigma of 0.02
 C808-C812 \\sim C810-C812 \\sim C809-C807 \\sim C809-C811 \\sim C811-C807
\\sim C808-C810
 with sigma of 0.04
 C805-C804 \\sim C804-C803 \\sim C803-C802 \\sim C802-C801 \\sim C801-C806
\\sim C806-C805
 with sigma of 0.02
 C805-C801 \\sim C803-C801 \\sim C804-C806 \\sim C804-C802 \\sim C802-C806
\\sim C805-C803
 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 C3A \\sim C5A \\sim O2A \\sim C9A \\sim C2A \\sim C6A \\sim C13A \\sim
C14A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
I303 \\sim I403 \\sim I304 \\sim I404: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C808 \\sim C809 \\sim C810 \\sim C811 \\sim C812 \\sim C807: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C805 \\sim C804 \\sim C803 \\sim C802 \\sim C801 \\sim C806: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C3) = Uanis(C346) = Uanis(C0) = Uanis(C347)
Uanis(C322) = Uanis(C323) = Uanis(C422) = Uanis(C423)
5. Rigid body (RIGU) restrains
 C8A, O3A, C12A, C15A, C7A, C11A, C4A, C10A, C3A, C5A, O2A, C9A, C2A, C6A,
 C13A, C14A, C1A, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I303, I403, I404, I304
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C808, C809, C810, C811, C812, C807
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C805, C804, C803, C802, C801, C806
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 1*[Sof(I304)+Sof(I303)+Sof(Zn32)]+1*[Sof(I504)+Sof(Zn52)+Sof(I503)]+1*
 [Sof(I403)+Sof(I404)+Sof(Zn42)]=1 with esd of 0.00001
 1*[Sof(I308)+Sof(I307)+Sof(Zn34)]+1*[Sof(I408)+Sof(Zn44)+Sof(I407)]=1 with
 esd of 0.00001
 Sof(I304)=Sof(I303)=Sof(Zn32)=FVAR(1)
 Sof(I504)=Sof(Zn52)=Sof(I503)=FVAR(2)
 Sof(I403)=Sof(I404)=Sof(Zn42)=FVAR(3)
 Sof(I308)=Sof(I307)=Sof(Zn34)=FVAR(4)
 Sof(I408)=Sof(Zn44)=Sof(I407)=FVAR(5)
 Sof(C422)=Sof(H422)=Sof(C423)=Sof(H423)=1-FVAR(6)
 Sof(C322)=Sof(H322)=Sof(C323)=Sof(H323)=FVAR(6)
 Sof(C3)=Sof(H3)=Sof(C0)=Sof(H0)=1-FVAR(7)
 Sof(C346)=Sof(H346)=Sof(C347)=Sof(H347)=FVAR(7)
 Fixed Sof: I312(0.49025) I301(0.52977) I311(0.49025) I405(0.54166)
 I302(0.52977) I409(0.35602) I406(0.54166) I410(0.35602) Zn36(0.49025)
 Zn31(0.52977) Zn43(0.54166) Zn45(0.35602) O3A(0.50301) O2A(0.50301)
 O1A(0.50301) H1A(0.50301) C4A(0.50301) C3A(0.50301) H3A(0.50301) C2A(0.50301)
 H2A(0.50301) C1A(0.50301) H1AA(0.50301) C6A(0.50301) H6A(0.50301) C5A(0.50301)
 C12A(0.50301) C7A(0.50301) C8A(0.50301) C9A(0.50301) H9A(0.50301)
 C15A(0.50301) H15A(0.50301) H15B(0.50301) H15C(0.50301) C10A(0.50301)
 H10A(0.50301) C11A(0.50301) H11A(0.50301) C13A(0.50301) H13A(0.50301)
 H13B(0.50301) I411(0.43771) I412(0.43771) Zn46(0.43771) I305(0.45832)
 Zn33(0.45832) I306(0.45832) I402(0.41907) Zn41(0.41907) I401(0.41907)
 I310(0.61662) Zn35(0.61662) I309(0.61662) I502(0.05115) I501(0.05115)
 Zn51(0.05115) I510(0.02734) I509(0.02734) Zn55(0.02734) I512(0.07207)
 Zn56(0.07207) I511(0.07207) C14A(0.50301) H14A(0.50301) H14B(0.50301)
 H14C(0.50301) C808(0.18959) H80A(0.18959) H80B(0.18959) C809(0.18959)
 H80C(0.18959) H80D(0.18959) C810(0.18959) H81A(0.18959) H81B(0.18959)
 C811(0.18959) H81C(0.18959) H81D(0.18959) C812(0.18959) H81E(0.18959)
 H81F(0.18959) C807(0.18959) H80E(0.18959) H80F(0.18959) C805(0.21796)
 H80G(0.21796) H80H(0.21796) C804(0.21796) H80I(0.21796) H80J(0.21796)
 C803(0.21796) H80K(0.21796) H80L(0.21796) C802(0.21796) H80M(0.21796)
 H80N(0.21796) C801(0.21796) H80O(0.21796) H80P(0.21796) C806(0.21796)
 H80Q(0.21796) H80R(0.21796) C4B(0.16299) C5B(0.16299) C6B(0.16299)
 H6B(0.16299) C1B(0.16299) H1B(0.16299) C2B(0.16299) H2B(0.16299) C3B(0.16299)
 H3B(0.16299) C7B(0.16299) C12B(0.16299) C11B(0.16299) H11B(0.16299)
 C10B(0.16299) H10B(0.16299) C9B(0.16299) H9B(0.16299) C8B(0.16299)
 O3B(0.16299) O2B(0.16299) C15B(0.16299) H15D(0.16299) H15E(0.16299)
 H15F(0.16299) C14B(0.16299) H14D(0.16299) H14E(0.16299) H14F(0.16299)
 O1B(0.16299) H1BA(0.16299) C13B(0.16299) H13C(0.16299) H13D(0.16299)
 Fixed Uiso: I504(0.08) Zn52(0.08) I503(0.08) I502(0.08) I501(0.08) Zn51(0.08)
 I510(0.08) I509(0.08) Zn55(0.08) I512(0.08) Zn56(0.08) I511(0.08) C4B(0.08)
 C5B(0.08) C6B(0.08) C1B(0.08) C2B(0.08) C3B(0.08) C7B(0.08) C12B(0.08)
 C11B(0.08) C10B(0.08) C9B(0.08) C8B(0.08) O3B(0.08) O2B(0.08) C15B(0.08)
 C14B(0.08) O1B(0.08) C13B(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C808(H80A,H80B), C809(H80C,H80D), C810(H81A,H81B), C811(H81C,
 H81D), C812(H81E,H81F), C807(H80E,H80F), C805(H80G,H80H), C804(H80I,H80J),
 C803(H80K,H80L), C802(H80M,H80N), C801(H80O,H80P), C806(H80Q,H80R), C13B(H13C,
 H13D)
7.b Aromatic/amide H refined with riding coordinates:
 C328(H328), C304(H304), C349(H349), C315(H315), C314(H314), C356(H356),
 C329(H329), C364(H364), C310(H310), C311(H311), C350(H350), C305(H305),
 C313(H313), C354(H354), C312(H312), C302(H302), C317(H317), C351(H351),
 C331(H331), C301(H301), C353(H353), C355(H355), C320(H320), C358(H358),
 C341(H341), C340(H340), C337(H337), C348(H348), C359(H359), C330(H330),
 C369(H369), C365(H365), C318(H318), C335(H335), C338(H338), C319(H319),
 C346(H346), C366(H366), C347(H347), C336(H336), C372(H372), C368(H368),
 C367(H367), C371(H371), C3A(H3A), C2A(H2A), C1A(H1AA), C6A(H6A), C333(H333),
 C332(H332), C9A(H9A), C322(H322), C323(H323), C10A(H10A), C11A(H11A),
 C422(H422), C423(H423), C3(H3), C0(H0), C6B(H6B), C1B(H1B), C2B(H2B), C3B(H3B),
  C11B(H11B), C10B(H10B), C9B(H9B)
7.c Fitted hexagon refined as free rotating group:
 C4A(C3A,C2A,C1A,C6A,C5A), C4B(C5B,C6B,C1B,C2B,C3B), C7B(C12B,C11B,C10B,C9B,C8B)
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), C15B(H15D,H15E,H15F), C14B(H14D,
 H14E,H14F)
;
_shelx_res_checksum              3874
_shelx_hkl_checksum              77852
_olex2_date_sample_data_collection 2022-01-31
_olex2_date_sample_submission    2022-01-31
_olex2_submission_original_sample_id 50_1_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 2.547
_oxdiff_exptl_absorpt_empirical_full_min 0.366