Atomically Accurate Structural Tailoring of Thiacalix[4]arene-Protected Copper(II)-Based Metallamacrocycles
Liu, Chao; Mu, Wen-Lei; Wu, Linlin; Yu, Weidong; Yi, Xiao-Yi; Yan, Jun; Dalton Transactions  (2023) –; doi:10.1039/D3DT00455D

data_7712766
_publ_section_title
;
 Atomically Accurate Structural Tailoring of Thiacalix[4]arene-Protected
 Copper(II)-Based Metallamacrocycles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00455D
_journal_year                    2023
_chemical_formula_moiety
'C172 H175 Cu12 O40 P8 S12, 3.5[C3H7O], 1[C3H7O], 2[C3H7O], 1[C3H7O], 0.5[], 1[], 0.5[]'
_chemical_formula_sum            'C212.5 H269.5 Cu12 O53.5 P8 S12'
_chemical_formula_weight         5074.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-03-13 deposited with the CCDC.	2023-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.44160(10)
_cell_length_b                   64.1367(5)
_cell_length_c                   25.1780(2)
_cell_measurement_reflns_used    68797
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      72.1110
_cell_measurement_theta_min      2.2790
_cell_volume                     21134.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -51.00 -23.64   0.38    2.89    --  -46.85 102.00 -94.00   72
  2  \w     -5.00  63.02   0.38    2.89    --   46.85-102.00 162.00  179
  3  \w   -131.00-103.64   0.38   19.95    --  -99.00-102.00 162.00   72
  4  \w   -105.00 -26.34   0.38   19.95    --  -99.00 102.00 -94.00  207
  5  \w     77.00 103.22   0.38   19.95    --   99.00-102.00 162.00   69
  6  \w     90.00 141.68   0.38   19.95    --   99.00 102.00 -94.00  136
  7  \w    -39.00  20.28   0.38    2.89    --  -46.85  37.00 150.00  156
  8  \w    -22.00  27.02   0.38    2.89    --  -46.85  19.00 -90.00  129
  9  \w   -104.00 -74.36   0.38    2.89    --  -46.85-125.00 -90.00   78
 10  \w     -9.00  26.34   0.38    2.89    --  -46.85  19.00-180.00   93
 11  \w    -82.00 -27.28   0.38    2.89    --  -46.85 125.00   0.00  144
 12  \w     17.00  61.08   0.38    2.89    --   46.85 -57.00-180.00  116
 13  \w    -24.00  15.14   0.38    2.89    --   46.85 -57.00-180.00  103
 14  \w    -26.00  42.02   0.38    2.89    --   46.85 -37.00 -90.00  179
 15  \w    -73.00 -27.78   0.38   19.95    --  -99.00  77.00 -90.00  119
 16  \w    -65.00 -29.28   0.38   19.95    --  -99.00  61.00 150.00   94
 17  \w   -112.00 -83.88   0.38   19.95    --  -99.00 125.00 -90.00   74
 18  \w    -68.00 -40.64   0.38   19.95    --  -99.00 125.00  30.00   72
 19  \w    -68.00 -40.64   0.38   19.95    --  -99.00  61.00-180.00   72
 20  \w   -112.00 -26.12   0.38   19.95    --  -99.00 125.00  60.00  226
 21  \w    -83.00 -33.98   0.38   19.95    --  -99.00  77.00 -30.00  129
 22  \w   -107.00 -40.12   0.38   19.95    --  -99.00 107.00-145.95  176
 23  \w   -158.00 -86.94   0.38   19.95    --  -99.00 -45.00  60.00  187
 24  \w   -112.00 -27.26   0.38   19.95    --  -99.00 125.00 120.00  223
 25  \w   -164.00 -83.06   0.38   19.95    --  -99.00 -61.00-120.00  213
 26  \w   -101.00 -65.66   0.38   19.95    --  -99.00  77.00  60.00   93
 27  \w   -112.00 -78.94   0.38   19.95    --  -99.00 125.00  30.00   87
 28  \w     75.00 108.82   0.38   19.95    --   99.00-125.00  30.00   89
 29  \w     70.00 103.06   0.38   19.95    --   99.00 -94.00 -60.00   87
 30  \w     27.00  79.06   0.38   19.95    --   99.00-125.00-120.00  137
 31  \w     26.00  58.30   0.38   19.95    --   99.00-125.00  30.00   85
 32  \w     27.00  52.46   0.38   19.95    --   99.00 -45.00 -60.00   67
 33  \w     88.00 139.30   0.38   19.95    --   99.00  45.00   0.00  135
 34  \w     27.00  52.46   0.38   19.95    --   99.00 -45.00-120.00   67
 35  \w     35.00  65.78   0.38   19.95    --   99.00 -61.00 150.00   81
 36  \w     47.00 106.66   0.38   19.95    --   99.00 -77.00 -30.00  157
 37  \w     27.00  52.08   0.38   19.95    --   99.00 -45.00  60.00   66
 38  \w    110.00 172.70   0.38   19.95    --   99.00  30.00-120.00  165
 39  \w     79.00 111.30   0.38   19.95    --   99.00-125.00 -30.00   85
 40  \w    145.00 169.70   0.38   19.95    --   99.00  77.00   0.00   65
 41  \w     89.00 136.12   0.38   19.95    --   99.00  77.00   0.00  124
 42  \w     86.00 167.70   0.38   19.95    --   99.00  45.00 150.00  215
 43  \w     37.00 104.64   0.38   19.95    --   99.00 -77.00  30.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0705018000
_diffrn_orient_matrix_UB_12      -0.0192127000
_diffrn_orient_matrix_UB_13      0.0105168000
_diffrn_orient_matrix_UB_21      -0.0860332000
_diffrn_orient_matrix_UB_22      -0.0127088000
_diffrn_orient_matrix_UB_23      0.0159323000
_diffrn_orient_matrix_UB_31      -0.0386901000
_diffrn_orient_matrix_UB_32      -0.0067889000
_diffrn_orient_matrix_UB_33      -0.0598543000
_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  0.0703
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       76
_diffrn_reflns_limit_k_min       -76
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            260197
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.269
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       block
_exptl_crystal_F_000             10530
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2880
_refine_ls_number_reflns         37280
_refine_ls_number_restraints     2383
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1033
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1167P)^2^+55.9499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2235
_refine_ls_wR_factor_ref         0.2383
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27909
_reflns_number_total             37280
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00455d2.cif
_cod_data_source_block           Cu12L3-Sa
_cod_original_formula_sum        'C212.50 H269.50 Cu12 O53.50 P8 S12'
_cod_database_code               7712766
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.760
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C69A-C139 = C139-C17A
 1.5 with sigma of 0.02
 C169-C135 = C135-C85
 1.5 with sigma of 0.02
 C1R-C1S
 1.5 with sigma of 0.02
 C135-C171
 1.5 with sigma of 0.02
 C1T-C1R = C1R-C85A
 1.5 with sigma of 0.02
 C146-C144 = C144-C148
 1.5 with sigma of 0.02
 C155-C144
 1.5 with sigma of 0.02
 C146-C155 = C155-C148
 2.5 with sigma of 0.02
 C148-C146
 2.5 with sigma of 0.02
 C167-C21
 2.5 with sigma of 0.02
 C1I-C21A
 1.5 with sigma of 0.02
 C1G-C1I = C1I-C83A
 1.5 with sigma of 0.02
 C1S-C1T = C1T-C85A
 2.5 with sigma of 0.02
 C85A-C1S
 2.5 with sigma of 0.02
 C21-C83
 2.5 with sigma of 0.02
 C2A-C65A
 2.5 with sigma of 0.02
 C139-C176
 1.5 with sigma of 0.02
 C73A-C116
 1.5 with sigma of 0.02
 C151-C126
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C69A) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C176) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(P4) \\sim Ueq, Uanis(P8) \\sim Ueq, Uanis(P3) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O10) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O28) \\sim Ueq,
Uanis(O32) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O25)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O35) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C38) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C90) \\sim Ueq,
Uanis(C92) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C106)
\\sim Ueq, Uanis(C110) \\sim Ueq, Uanis(C112) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C118) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C132) \\sim Ueq,
Uanis(C136) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C103)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C27) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C129) \\sim Ueq, Uanis(C131) \\sim Ueq,
Uanis(C33) \\sim Ueq, Uanis(C135) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C139) \\sim Ueq, Uanis(C141) \\sim Ueq, Uanis(C71) \\sim Ueq,
Uanis(C143) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C147) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C153) \\sim Ueq, Uanis(C77) \\sim Ueq,
Uanis(C159) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C161) \\sim Ueq, Uanis(C81)
\\sim Ueq, Uanis(C163) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C165) \\sim Ueq,
Uanis(O37) \\sim Ueq, Uanis(P7) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(C83)
\\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(C167) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C169) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C171) \\sim Ueq, Uanis(S9A)
\\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C173) \\sim Ueq, Uanis(C1A) \\sim Ueq,
Uanis(C1B) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C72A)
\\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1E) \\sim Ueq, Uanis(S11A) \\sim Ueq,
Uanis(C77A) \\sim Ueq, Uanis(C1F) \\sim Ueq, Uanis(C1G) \\sim Ueq, Uanis(C1H)
\\sim Ueq, Uanis(C1I) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C83A) \\sim Ueq,
Uanis(C37A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C1J) \\sim Ueq, Uanis(Cu6A)
\\sim Ueq, Uanis(O38A) \\sim Ueq, Uanis(Cu4A) \\sim Ueq, Uanis(S5A) \\sim Ueq,
Uanis(O19A) \\sim Ueq, Uanis(P7A) \\sim Ueq, Uanis(O37A) \\sim Ueq, Uanis(O39A)
\\sim Ueq, Uanis(Cu1A) \\sim Ueq, Uanis(O33A) \\sim Ueq, Uanis(O9A) \\sim Ueq,
Uanis(P3A) \\sim Ueq, Uanis(O35A) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(C4A)
\\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C10A) \\sim Ueq,
Uanis(C12A) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C1M)
\\sim Ueq, Uanis(C81A) \\sim Ueq, Uanis(C1L) \\sim Ueq, Uanis(C41A) \\sim Ueq,
Uanis(C1K) \\sim Ueq, Uanis(C94A) \\sim Ueq, Uanis(C1N) \\sim Ueq, Uanis(C1O)
\\sim Ueq, Uanis(C1P) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C1Q) \\sim Ueq,
Uanis(C13A) \\sim Ueq, Uanis(O20A) \\sim Ueq, Uanis(C85A) \\sim Ueq, Uanis(C1R)
\\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(C1T) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C146) \\sim Ueq, Uanis(C144) \\sim Ueq, Uanis(C148) \\sim Ueq,
Uanis(C155) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C75A) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C65A) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C175) \\sim Ueq,
Uanis(C115) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C57A)
\\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C67A) \\sim Ueq, Uanis(C73A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C119, C144, C146, C148, C155
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cu1, Cu1A, Cu4, Cu4A, Cu6, Cu6A, Cu10, S5, S5A, S9, S9A, S10, S11, S11A, P3,
 P3A, P7, P7A, O2, O4, O4A, O9, O9A, O19, O19A, O20, O20A, O32, O33, O33A, O34,
 O35, O35A, O37, O37A, O38, O38A, O39, O39A, C1A, C1B, C1C, C1D, C1E, C1F, C1G,
 C1H, C1I, C1J, C1K, C1L, C1M, C1N, C1O, C1P, C1Q, C1R, C1S, C1T, C4, C4A, C5,
 C5A, C6, C6A, C8, C8A, C9, C9A, C10, C10A, C12, C12A, C13, C13A, C14, C14A,
 C15, C15A, C17, C19, C19A, C21, C21A, C24, C27, C27A, C33, C37, C37A, C38, C41,
  C41A, C54, C68, C69, C70, C71, C72, C72A, C77, C77A, C81, C81A, C83, C83A,
 C85, C85A, C86, C90, C92, C94, C94A, C99, C100, C101, C103, C105, C106, C109,
 C110, C111, C112, C114, C118, C121, C129, C130, C131, C132, C135, C136, C139,
 C141, C143, C147, C153, C159, C161, C163, C165, C167, C169, C171, C173
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Cu1A)=Sof(Cu4A)=Sof(Cu6A)=Sof(S5A)=Sof(S9A)=Sof(S11A)=Sof(P3A)=Sof(P7A)=
 Sof(O4A)=Sof(O9A)=Sof(O19A)=Sof(O20A)=Sof(O33A)=Sof(O35A)=Sof(O37A)=Sof(O38A)=
 Sof(O39A)=Sof(C1A)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C1C)=Sof(C1D)=
 Sof(C1E)=Sof(H1E)=Sof(C1F)=Sof(H1F)=Sof(C1G)=Sof(H1GA)=Sof(H1GB)=Sof(H1GC)=
 Sof(C1H)=Sof(C1I)=Sof(C1J)=Sof(C1N)=Sof(C1O)=Sof(C1P)=Sof(H1P)=Sof(C1Q)=
 Sof(H1Q)=Sof(C1R)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C1T)=Sof(H1TA)=
 Sof(H1TB)=Sof(H1TC)=Sof(C4A)=Sof(C6A)=Sof(H6A)=Sof(C8A)=Sof(H8A)=Sof(C10A)=
 Sof(H10A)=Sof(C12A)=Sof(H12A)=Sof(C14A)=Sof(H14A)=Sof(C5A)=Sof(C1M)=Sof(H1M)=
 Sof(C81A)=Sof(H81A)=Sof(C1L)=Sof(H1L)=Sof(C41A)=Sof(H41A)=Sof(C1K)=Sof(H1K)=
 Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C13A)=Sof(C15A)=Sof(C19A)=Sof(C21A)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C27A)=Sof(C37A)=Sof(H37A)=Sof(C72A)=
 Sof(C77A)=Sof(C83A)=Sof(H83D)=Sof(H83E)=Sof(H83F)=Sof(C85A)=Sof(H85D)=
 Sof(H85E)=Sof(H85F)=Sof(C94A)=Sof(H94A)=Sof(C173)=Sof(H17J)=Sof(H17K)=
 Sof(H17L)=1-FVAR(1)
 Sof(Cu1)=Sof(Cu4)=Sof(Cu6)=Sof(S5)=Sof(S9)=Sof(S11)=Sof(P3)=Sof(P7)=Sof(O4)=
 Sof(O9)=Sof(O19)=Sof(O20)=Sof(O33)=Sof(O35)=Sof(O37)=Sof(O38)=Sof(O39)=Sof(C4)=
 Sof(C6)=Sof(H6)=Sof(C8)=Sof(H8)=Sof(C10)=Sof(H10)=Sof(C12)=Sof(H12)=Sof(C14)=
 Sof(H14)=Sof(C5)=Sof(C161)=Sof(H161)=Sof(C81)=Sof(H81)=Sof(C163)=Sof(H163)=
 Sof(C41)=Sof(H41)=Sof(C165)=Sof(H165)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C13)=Sof(C15)=Sof(C19)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C27)=
 Sof(C37)=Sof(H37)=Sof(C72)=Sof(C77)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=
 Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(H85C)=Sof(C94)=Sof(H94)=Sof(C103)=Sof(C105)=
 Sof(H105)=Sof(C109)=Sof(H109)=Sof(C111)=Sof(C112)=Sof(H112)=Sof(C118)=
 Sof(C121)=Sof(C129)=Sof(C130)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C132)=
 Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C135)=Sof(C136)=Sof(C141)=Sof(H141)=
 Sof(C153)=Sof(C159)=Sof(C167)=Sof(H16G)=Sof(H16H)=Sof(H16I)=Sof(C169)=
 Sof(H16J)=Sof(H16K)=Sof(H16L)=Sof(C171)=Sof(H17G)=Sof(H17H)=Sof(H17I)=FVAR(1)
 Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=Sof(C79A)=Sof(H79D)=Sof(H79E)=
 Sof(H79F)=Sof(C174)=Sof(H17M)=Sof(H17N)=Sof(H17O)=1-FVAR(2)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=
 Sof(C157)=Sof(H15D)=Sof(H15E)=Sof(H15F)=FVAR(2)
 Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C65A)=Sof(H65D)=Sof(H65E)=
 Sof(H65F)=Sof(C75A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=1-FVAR(3)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(H65C)=
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=FVAR(3)
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C57A)=Sof(H57D)=Sof(H57E)=
 Sof(H57F)=Sof(C175)=Sof(H17P)=Sof(H17Q)=Sof(H17R)=1-FVAR(4)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=
 Sof(C115)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(4)
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C67A)=Sof(H67D)=Sof(H67E)=
 Sof(H67F)=Sof(C73A)=Sof(H73D)=Sof(H73E)=Sof(H73F)=1-FVAR(5)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=FVAR(5)
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C69A)=Sof(H69D)=Sof(H69E)=
 Sof(H69F)=Sof(C176)=Sof(H17S)=Sof(H17T)=Sof(H17U)=1-FVAR(6)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)=
 Sof(C143)=Sof(H14E)=Sof(H14F)=Sof(H14G)=FVAR(6)
6.a Riding coordinates:
 O21(H21), C17A(H17D,H17E,H17F), C35A(H35D,H35E,H35F), C69A(H69D,H69E,H69F)
6.b Aromatic/amide H refined with riding coordinates:
 C1E(H1E), C1F(H1F), C1P(H1P), C1Q(H1Q), C3(H3), C6(H6), C8(H8), C10(H10),
 C12(H12), C14(H14), C6A(H6A), C8A(H8A), C10A(H10A), C12A(H12A), C14A(H14A),
 C161(H161), C81(H81), C163(H163), C41(H41), C165(H165), C1M(H1M), C81A(H81A),
 C1L(H1L), C41A(H41A), C1K(H1K), C25(H25), C29(H29), C33(H33), C36(H36),
 C37(H37), C37A(H37A), C40(H40), C42(H42), C47(H47), C50(H50), C51(H51),
 C53(H53), C56(H56), C59(H59), C60(H60), C64(H64), C68(H68), C70(H70), C71(H71),
  C74(H74), C82(H82), C84(H84), C86(H86), C88(H88), C89(H89), C90(H90),
 C91(H91), C92(H92), C93(H93), C94(H94), C94A(H94A), C96(H96), C98(H98),
 C100(H100), C101(H101), C104(H104), C105(H105), C106(H106), C109(H109),
 C110(H110), C112(H112), C113(H113), C114(H114), C120(H120), C122(H122),
 C124(H124), C126(H126), C128(H128), C134(H134), C141(H141), C142(H142),
 C149(H149), C150(H150), C151(H151), C168(H168)
6.c Fitted hexagon refined as free rotating group:
 C4(C6,C8,C10,C12,C14), C4A(C6A,C8A,C10A,C12A,C14A), C5(C161,C81,C163,C41,
 C165), C5A(C1M,C81A,C1L,C41A,C1K)
6.d Idealised Me refined as rotating group:
 C1B(H1BA,H1BB,H1BC), C1G(H1GA,H1GB,H1GC), C1S(H1SA,H1SB,H1SC), C1T(H1TA,H1TB,
 H1TC), C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC), C7(H7A,H7B,H7C), C7A(H7AA,H7AB,
 H7AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC), C17(H17A,H17B,H17C), C21(H21A,
 H21B,H21C), C21A(H21D,H21E,H21F), C31(H31A,H31B,H31C), C35(H35A,H35B,H35C),
 C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F), C57(H57A,H57B,H57C), C57A(H57D,H57E,
 H57F), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C), C65(H65A,H65B,H65C),
 C65A(H65D,H65E,H65F), C67(H67A,H67B,H67C), C67A(H67D,H67E,H67F), C69(H69A,H69B,
 H69C), C73(H73A,H73B,H73C), C73A(H73D,H73E,H73F), C75(H75A,H75B,H75C),
 C75A(H75D,H75E,H75F), C79(H79A,H79B,H79C), C79A(H79D,H79E,H79F), C83(H83A,H83B,
 H83C), C83A(H83D,H83E,H83F), C85(H85A,H85B,H85C), C85A(H85D,H85E,H85F),
 C115(H11A,H11B,H11C), C130(H13A,H13B,H13C), C132(H13D,H13E,H13F), C138(H13G,
 H13H,H13I), C140(H14B,H14C,H14D), C143(H14E,H14F,H14G), C145(H14H,H14I,H14J),
 C146(H14K,H14L,H14M), C148(H14N,H14O,H14P), C155(H15A,H15B,H15C), C157(H15D,
 H15E,H15F), C158(H15G,H15H,H15I), C160(H16A,H16B,H16C), C164(H16D,H16E,H16F),
 C167(H16G,H16H,H16I), C169(H16J,H16K,H16L), C171(H17G,H17H,H17I), C173(H17J,
 H17K,H17L), C174(H17M,H17N,H17O), C175(H17P,H17Q,H17R), C176(H17S,H17T,H17U)
6.e Idealised tetrahedral OH refined as rotating group:
 O11(H11), O17(H17)
;
_shelx_res_checksum              45522
_shelx_fab_checksum              16265
_platon_squeeze_void_probe_radius 1.20
_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 1.632
_oxdiff_exptl_absorpt_empirical_full_min 0.607