The electrosynthesis of highly encumbered biaryls from aryl <i>o</i>-iodobenzyl ethers by a radical to polar crossover sequence.
Pearce, James E.; Hodgson, Jack; Folgueiras-Amador, Ana A; Fish, Johanna A.; Carroll, Robert C.; Coles, Simon J.; Parsons, Philip J.; Brown, Richard C. D.; Harrowven, David C.; Chemical communications (Cambridge, England) 61 (2025) 4042–4045; doi:10.1039/d4cc06061j

data_7134208
_publ_section_title
;
 The electrosynthesis of highly encumbered biaryls from aryl
 <i>o</i>-iodobenzyl ethers by a radical to polar crossover sequence.
;
_journal_issue                   20
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4042
_journal_page_last               4045
_journal_paper_doi               10.1039/d4cc06061j
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C36 H24 I6 N12 Zn3, 0.836(C16 H18 O3), 0.17(C6 H12)'
_chemical_formula_sum            'C50.41 H41.1 I6 N12 O2.51 Zn3'
_chemical_formula_weight         1812.58
_chemical_name_common
'BBA-(1-Me)-8,12-OMe (absorbed in crystalline sponge)'
_chemical_name_systematic
'(2',6'-dimethoxy-4-methyl-[1,1'-biphenyl]-2-yl)methanol absored in crystalline sponge'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-31 deposited with the CCDC.	2025-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.865(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.3966(12)
_cell_length_b                   14.9997(4)
_cell_length_c                   31.701(2)
_cell_measurement_reflns_used    12591
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.4140
_cell_measurement_theta_min      2.5540
_cell_volume                     16006.3(13)
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix Arc-100'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_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     17.00  43.00   0.50    1.50    --   83.47 -37.00-120.00   52
  2  \w     28.00 134.00   0.50    1.50    --   83.47   0.00 -60.00  212
  3  \w     14.00  40.00   0.50    1.50    --   83.47 -37.00 -30.00   52
  4  \w     16.00  65.00   0.50    1.50    --   83.47 -57.00-120.00   98
  5  \w     36.00  95.00   0.50    1.50    --   83.47-125.00   0.00  118
  6  \w     19.00  44.00   0.50    1.50    --   83.47 -37.00 120.00   50
  7  \w     39.00 100.00   0.50    1.50    --   83.47 -77.00-150.00  122
  8  \w     17.00  43.00   0.50    1.50    --   83.47 -57.00-150.00   52
  9  \w     36.00  61.00   0.50    1.50    --   83.47 -57.00 -30.00   50
 10  \w     15.00  40.00   0.50    1.50    --   83.47 -37.00-180.00   50
 11  \w     12.00  41.00   0.50    1.50    --   83.47 -37.00  60.00   58
 12  \w     12.00  44.00   0.50    1.50    --   83.47 -37.00 -90.00   64
 13  \w     16.00  44.00   0.50    1.50    --   83.47 -37.00   0.00   56
 14  \w     87.00 133.00   0.50    1.50    --   83.47  92.00 -55.00   92
 15  \w     24.00  82.00   0.50    1.50    --   83.47 -92.00-167.00  116
 16  \w    -76.00 -36.00   0.50    1.50    --  -79.37  92.00 -55.00   80
 17  \w   -114.00 -88.00   0.50    1.50    --  -79.37 -92.00-167.00   52
 18  \w    -38.00  -8.00   0.50    1.50    --  -79.37  37.00 -90.00   60
 19  \w    -34.00  -8.00   0.50    1.50    --  -79.37  37.00 150.00   52
 20  \w    -39.00 -11.00   0.50    1.50    --  -79.37  37.00 -60.00   56
 21  \w    -38.00 -13.00   0.50    0.50    --  -55.01  92.00 -55.00   50
 22  \w    -39.00   3.00   0.50    0.50    --  -55.01  37.00 120.00   84
 23  \w    -24.00   1.00   0.50    0.50    --  -55.01  19.00-180.00   50
 24  \w     -3.00  75.00   0.50    0.50    --   51.26 -92.00-167.00  156
 25  \w    -19.00  27.00   0.50    0.50    --   51.26 -19.00 -90.00   92
 26  \w    -10.00  16.00   0.50    0.50    --   51.26 -19.00  60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, UG2 \k goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF diffractometer equipped with Arc)Sec VHF Varimax confocal mirrors and a UG2 goniometer and HyPix Arc-100 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      -0.0060643000
_diffrn_orient_matrix_UB_12      -0.0349157000
_diffrn_orient_matrix_UB_13      0.0438590000
_diffrn_orient_matrix_UB_21      -0.0167400000
_diffrn_orient_matrix_UB_22      -0.0879532000
_diffrn_orient_matrix_UB_23      -0.0215063000
_diffrn_orient_matrix_UB_31      0.0421690000
_diffrn_orient_matrix_UB_32      -0.0399421000
_diffrn_orient_matrix_UB_33      0.0088717000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Arc)Sec VHF Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            59435
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.248
_diffrn_reflns_theta_min         2.625
_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    19.516
_exptl_absorpt_correction_T_max  0.282
_exptl_absorpt_correction_T_min  0.108
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             6845
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.872
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1104
_refine_ls_number_reflns         14515
_refine_ls_number_restraints     1058
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.1124
_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^)+(0.1416P)^2^+287.1909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3185
_refine_ls_wR_factor_ref         0.3370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9896
_reflns_number_total             14515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06061j2.cif
_cod_data_source_block           BBA_1_Me_8_12_OMe_CrystallineSponge
_cod_depositor_comments
'Adding full bibliography for 7134208--7134209.cif.'
_cod_original_cell_volume        16006.1(14)
_cod_original_formula_sum        'C50.41 H41.10 I6 N12 O2.51 Zn3'
_cod_database_code               7134208
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C16 H18 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     JP-9444-42
_shelx_estimated_absorpt_t_max   0.246
_shelx_estimated_absorpt_t_min   0.136
_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
 C13B-C5B = C16B-C1B
 1.51 with sigma of 0.02
 C4B-C7B
 1.5 with sigma of 0.01
 O3B-C12B = O2B-C8B
 1.38 with sigma of 0.02
 O3B-C15B = O2B-C14B
 1.43 with sigma of 0.02
 O1B-C13B
 1.43 with sigma of 0.01
 C9A-C8A = C10A-C9A = C10A-C11A = C12A-C11A = C12A-C7A = C7A-C8A
 1.39 with sigma of 0.02
 C805-C804 = C805-C806 = C804-C803 = C803-C802 = C802-C801 = C801-C806
 1.54 with sigma of 0.02
 O1A-C13A
 1.43 with sigma of 0.02
 O3A-C15A = O2A-C14A
 1.43 with sigma of 0.02
 C2B-C16B = C6B-C16B
 2.5 with sigma of 0.04
 C11B-O3B
 2.45 with sigma of 0.04
 C12B-C15B
 2.4 with sigma of 0.04
 C10A-C8A = C9A-C7A
 2.4 with sigma of 0.04
 C805-C803 = C805-C801 = C804-C802 = C803-C801 = C802-C806
 2.54 with sigma of 0.04
 C5A-C4A \\sim C6A-C5A \\sim C6A-C1A \\sim C1A-C2A \\sim C3A-C2A \\sim C3A-C4A
 with sigma of 0.02
 C1A-C3A \\sim C2A-C4A \\sim C3A-C5A \\sim C4A-C6A \\sim C5A-C1A \\sim C6A-C2A
 with sigma of 0.04
 O3A-C12A \\sim O2A-C8A
 with sigma of 0.02
 C4A-C7A \\sim C5A-C13A \\sim C1A-C16A
 with sigma of 0.02
 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
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 Zn33-N307 \\sim Zn43-N307
 with sigma of 0.02
 Zn33-N306 \\sim Zn43-N306
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N307 \\sim I406-N307
 with sigma of 0.04
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 I305-N307 \\sim I405-N307
 with sigma of 0.04
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I402-Zn41 \\sim I302-Zn31
 with sigma of 0.02
 I401-Zn41 \\sim I301-Zn31
 with sigma of 0.02
 Zn41-N301 \\sim Zn31-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
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 Zn32-N305 \\sim Zn42-N305
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I303-N305 \\sim I403-N305
 with sigma of 0.04
 I304-N305 \\sim I404-N305
 with sigma of 0.04
 I601-Zn61 \\sim I401-Zn41
 with sigma of 0.02
 I602-Zn61 \\sim I402-Zn41
 with sigma of 0.02
 Zn31-N301 \\sim Zn61-N301
 with sigma of 0.02
 I505-Zn53 \\sim I405-Zn43
 with sigma of 0.02
 I506-Zn53 \\sim I406-Zn43
 with sigma of 0.02
 C327-C325 \\sim C427-C325
 with sigma of 0.02
 C327-C331 \\sim C427-C431
 with sigma of 0.02
 C327-C328 \\sim C427-C428
 with sigma of 0.02
 N311-C329 \\sim N411-C429
 with sigma of 0.02
 N311-C330 \\sim N411-C430
 with sigma of 0.02
 C331-C330 \\sim C431-C430
 with sigma of 0.02
 C328-C329 \\sim C428-C429
 with sigma of 0.02
 C327-C329 \\sim C427-C429
 with sigma of 0.04
 C327-C330 \\sim C427-C430
 with sigma of 0.04
 C325-C331 \\sim C325-C431
 with sigma of 0.04
 C325-C328 \\sim C325-C428
 with sigma of 0.04
 N311-C331 \\sim N411-C431
 with sigma of 0.04
 N311-C328 \\sim N411-C428
 with sigma of 0.04
 C331-C328 \\sim C431-C428
 with sigma of 0.04
 C329-C330 \\sim C429-C430
 with sigma of 0.04
 N307-C423 \\sim N307-C323
 with sigma of 0.02
 N307-C319 \\sim N307-C419
 with sigma of 0.02
 C321-C422 \\sim C321-C322
 with sigma of 0.02
 C321-C320 \\sim C321-C420
 with sigma of 0.02
 C423-C422 \\sim C323-C322
 with sigma of 0.02
 C319-C320 \\sim C419-C420
 with sigma of 0.02
 N307-C422 \\sim N307-C322
 with sigma of 0.04
 N307-C320 \\sim N307-C420
 with sigma of 0.04
 C321-C423 \\sim C321-C323
 with sigma of 0.04
 C321-C319 \\sim C321-C419
 with sigma of 0.04
 N301-C305 \\sim N301-C405
 with sigma of 0.02
 C305-C304 \\sim C405-C404
 with sigma of 0.02
 C303-C304 \\sim C303-C404
 with sigma of 0.02
 N301-C304 \\sim N301-C404
 with sigma of 0.04
 C305-C303 \\sim C405-C303
 with sigma of 0.04
3. Restrained planarity
 C4B, C5B, C6B, C13B
 with sigma of 0.1
 C3A, C4A, C5A, C6A, C1A, C2A
 with sigma of 0.1
 C11A, C12A, C7A, C8A, C9A, C10A
 with sigma of 0.1
 O3A, C12A, C7A, C8A, O2A
 with sigma of 0.1
 C16A, C1A, C6A, C5A, C13A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C4B \\sim O2B \\sim C8B \\sim C14B \\sim C9B \\sim C7B \\sim C10B \\sim C12B
\\sim C11B \\sim O3B \\sim C3B \\sim C5B \\sim C15B \\sim C2B \\sim C6B \\sim
C13B \\sim C1B \\sim O1B \\sim C16B: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
C7A \\sim C2A \\sim C3A \\sim C1A \\sim C4A \\sim C6A \\sim C16A \\sim C5A
\\sim C13A \\sim C8A \\sim C12A \\sim O1A \\sim O2A \\sim C9A \\sim O3A \\sim
C11A \\sim C14A \\sim C10A \\sim C15A: 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
C319 \\sim C419 \\sim C420 \\sim C320 \\sim C422 \\sim C322 \\sim C323 \\sim
C423: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
C327 \\sim N311 \\sim C331 \\sim C328 \\sim C329 \\sim C330 \\sim N411 \\sim
C430 \\sim C431 \\sim C429 \\sim C428 \\sim C427: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Zn31 \\sim Zn41 \\sim Zn51: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
I302 \\sim I502 \\sim I301 \\sim I501: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C305) = Uanis(C405) = Uanis(C404) = Uanis(C304)
5. Rigid body (RIGU) restrains
 C4B, O2B, C8B, C14B, C9B, C7B, C10B, C12B, C11B, O3B, C3B, C5B, C15B, C2B,
 C6B, C13B, C1B, O1B, C16B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A, C13A, C14A,
 C15A, C16A, O1A, O2A, O3A
 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
 Sof(N411)=Sof(C430)=Sof(H430)=Sof(C431)=Sof(H431)=Sof(C429)=Sof(H429)=
 Sof(C428)=Sof(H428)=Sof(C427)=1-FVAR(1)
 Sof(C327)=Sof(N311)=Sof(C331)=Sof(H331)=Sof(C328)=Sof(H328)=Sof(C329)=
 Sof(H329)=Sof(C330)=Sof(H330)=FVAR(1)
 Sof(C420)=Sof(H420)=Sof(C419)=Sof(H419)=Sof(C322)=Sof(H322)=Sof(C323)=
 Sof(H323)=1-FVAR(2)
 Sof(C423)=Sof(H423)=Sof(C319)=Sof(H319)=Sof(C422)=Sof(H422)=Sof(C320)=
 Sof(H320)=FVAR(2)
 Fixed Sof: I303(0.56594) I304(0.56594) I306(0.48222) I305(0.48222)
 Zn32(0.56594) Zn33(0.48222) I402(0.1256) I401(0.1256) Zn41(0.1256)
 C305(0.56334) H305(0.56334) C304(0.56334) H304(0.56334) I406(0.46038)
 Zn43(0.46038) I405(0.46038) I301(0.53989) Zn31(0.53989) I302(0.53989)
 I404(0.43406) Zn42(0.43406) I403(0.43406) I502(0.29448) I501(0.29448)
 Zn51(0.29448) I506(0.0574) I505(0.0574) Zn53(0.0574) I602(0.04002)
 I601(0.04002) Zn61(0.04002) O2B(0.43058) O1B(0.43058) H1B(0.43058)
 O3B(0.43058) C8B(0.43058) C9B(0.43058) H9B(0.43058) C10B(0.43058)
 H10B(0.43058) C11B(0.43058) H11B(0.43058) C12B(0.43058) C7B(0.43058)
 C4B(0.43058) C3B(0.43058) H3B(0.43058) C2B(0.43058) H2B(0.43058) C1B(0.43058)
 C6B(0.43058) H6B(0.43058) C5B(0.43058) C15B(0.43058) H15A(0.43058)
 H15B(0.43058) H15C(0.43058) C14B(0.43058) H14A(0.43058) H14B(0.43058)
 H14C(0.43058) C13B(0.43058) H13A(0.43058) H13B(0.43058) C2A(0.40588)
 H2A(0.40588) O2A(0.40588) C4A(0.40588) C5A(0.40588) O1A(0.40588) H1A(0.40588)
 C15A(0.40588) H15D(0.40588) H15E(0.40588) H15F(0.40588) C6A(0.40588)
 H6A(0.40588) C3A(0.40588) H3A(0.40588) O3A(0.40588) C16A(0.40588)
 H16D(0.40588) H16E(0.40588) H16F(0.40588) C8A(0.40588) C13A(0.40588)
 H13C(0.40588) H13D(0.40588) C11A(0.40588) H11A(0.40588) C14A(0.40588)
 H14D(0.40588) H14E(0.40588) H14F(0.40588) C12A(0.40588) C7A(0.40588)
 C9A(0.40588) H9A(0.40588) C10A(0.40588) H10A(0.40588) C1A(0.40588)
 C16B(0.43058) H16A(0.43058) H16B(0.43058) H16C(0.43058) C805(0.17034)
 H80A(0.17034) H80B(0.17034) C804(0.17034) H80C(0.17034) H80D(0.17034)
 C803(0.17034) H80E(0.17034) H80F(0.17034) C802(0.17034) H80G(0.17034)
 H80H(0.17034) C801(0.17034) H80I(0.17034) H80J(0.17034) C806(0.17034)
 H80K(0.17034) H80L(0.17034) C405(0.43666) H405(0.43666) C404(0.43666)
 H404(0.43666)
 Fixed Uiso: I506(0.08) I505(0.08) Zn53(0.08) I602(0.08) I601(0.08) Zn61(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13B(H13A,H13B), C13A(H13C,H13D), C805(H80A,H80B), C804(H80C,H80D), C803(H80E,
 H80F), C802(H80G,H80H), C801(H80I,H80J), C806(H80K,H80L)
7.b Aromatic/amide H refined with riding coordinates:
 C313(H313), C333(H333), C332(H332), C311(H311), C317(H317), C312(H312),
 C310(H310), C305(H305), C318(H318), C423(H423), C302(H302), C319(H319),
 C315(H315), C422(H422), C314(H314), C301(H301), C304(H304), C335(H335),
 C331(H331), C328(H328), C320(H320), C329(H329), C330(H330), C336(H336),
 C9B(H9B), C10B(H10B), C11B(H11B), C3B(H3B), C2B(H2B), C6B(H6B), C2A(H2A),
 C6A(H6A), C3A(H3A), C11A(H11A), C9A(H9A), C10A(H10A), C430(H430), C431(H431),
 C429(H429), C428(H428), C420(H420), C419(H419), C322(H322), C323(H323),
 C405(H405), C404(H404)
7.c Fitted hexagon refined as free rotating group:
 C8B(C9B,C10B,C11B,C12B,C7B), C4B(C3B,C2B,C1B,C6B,C5B)
7.d Tetrahedral OH refined with riding coordinates:
 O1B(H1B), O1A(H1A)
7.e Idealised Me refined with everything fixed:
 C15B(H15A,H15B,H15C), C14B(H14A,H14B,H14C), C15A(H15D,H15E,H15F), C16A(H16D,
 H16E,H16F), C14A(H14D,H14E,H14F), C16B(H16A,H16B,H16C)
;
_shelx_res_checksum              3477
_shelx_hkl_checksum              63837
_olex2_date_sample_data_collection 2023-07-10
_olex2_date_sample_submission    2023-07-10
_olex2_submission_original_sample_id BBA-(1-Me)-8,12-OMe
_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 2.466
_oxdiff_exptl_absorpt_empirical_full_min 0.519