A novel series of giant cobalt-calixarene macrocycles: ring-expansion and modulation of pore apertures through recrystallization.
Zhang, Kai; Du, Shao-Wu; Dalton transactions (Cambridge, England : 2003) 50 (2021) 6181–6187; doi:10.1039/d1dt00556a

data_7707119
_publ_section_title
;
 A novel series of giant cobalt-calixarene macrocycles: ring-expansion and
 modulation of pore apertures through recrystallization.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6181
_journal_page_last               6187
_journal_paper_doi               10.1039/d1dt00556a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C364.73 H398.5 Cl8 Co32 N17.3 O80.83 S32, 56(C3 H7 N O)'
_chemical_formula_sum            'C532.73 H790.5 Cl8 Co32 N73.3 O136.83 S32'
_chemical_formula_weight         13606.72
_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   mixed
_audit_creation_date             2021-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-06 deposited with the CCDC.	2021-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.979(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   49.3116(10)
_cell_length_b                   26.6728(4)
_cell_length_c                   56.2706(10)
_cell_measurement_reflns_used    81463
_cell_measurement_temperature    110.9(5)
_cell_measurement_theta_max      60.0390
_cell_measurement_theta_min      2.5700
_cell_volume                     73295(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.9(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.953
_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    -14.00  15.00   0.25    1.57    --   -2.81 -64.00 -76.00  116
  2  \w     43.00  75.00   0.25    6.27    --   70.78 -64.00 -76.00  128
  3  \w     27.00  53.00   0.25    1.57    --   -2.81  38.00-180.00  104
  4  \w     -5.00  26.00   0.25    6.27    --   70.78 -19.00-150.00  124
  5  \w     -5.00  26.00   0.25    6.27    --   70.78 -19.00-180.00  124
  6  \w     -4.00  25.00   0.25    6.27    --   70.78 -19.00 -30.00  116
  7  \w     73.00  98.00   0.25    6.27    --   70.78  64.00  59.00  100
  8  \w      1.00  26.00   0.25    6.27    --   70.78 -19.00  90.00  100
  9  \w     -4.00  23.00   0.25    6.27    --   70.78 -19.00 120.00  108
 10  \w     -1.00  26.00   0.25    6.27    --   70.78 -19.00 150.00  108
 11  \w    -11.00  57.00   0.25    1.57    --   -2.81  64.00  59.00  272
 12  \w    -38.00  -3.00   0.25    6.27    --  -76.40  38.00 -90.00  140
 13  \w    -43.00  -7.00   0.25    6.27    --  -76.40  38.00-150.00  144
 14  \w    -41.00 -10.00   0.25    6.27    --  -76.40  38.00-180.00  124
 15  \w    -42.00 -11.00   0.25    6.27    --  -76.40  38.00-120.00  124
 16  \w    -43.00 -17.00   0.25    6.27    --  -76.40  38.00   0.00  104
 17  \w    -37.00 -12.00   0.25    6.27    --  -76.40  38.00  30.00  100
 18  \w    -42.00 -17.00   0.25    6.27    --  -76.40  38.00  60.00  100
 19  \w    -76.00  -3.00   0.25    6.27    --  -76.40  64.00  59.00  292
 20  \w    -66.00 -20.00   0.25    6.27    --  -76.40 125.00 -90.00  184
 21  \w   -110.00 -74.00   0.25    6.27    --  -76.40 125.00 -90.00  144
 22  \w    -65.00 -27.00   0.25    1.57    --   -2.81 -64.00 -76.00  152
 23  \w   -142.00 -78.00   0.25    6.27    --  -76.40 -64.00 -76.00  256
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0140152000
_diffrn_orient_matrix_UB_12      -0.0368488000
_diffrn_orient_matrix_UB_13      -0.0089016000
_diffrn_orient_matrix_UB_21      -0.0154496000
_diffrn_orient_matrix_UB_22      0.0052512000
_diffrn_orient_matrix_UB_23      -0.0213687000
_diffrn_orient_matrix_UB_31      0.0177641000
_diffrn_orient_matrix_UB_32      0.0336839000
_diffrn_orient_matrix_UB_33      -0.0064141000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_number            293116
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         61.262
_diffrn_reflns_theta_min         1.942
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    4.883
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             23163
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
A solvent mask was calculated and 8098 electrons were found in a volume of 27486\%A^3^ in 25 void per unit cell. This is consistent with the presence of 42[C3H7NO] per Formula Unit which account for 8064 electrons per unit cell.
;
_refine_diff_density_max         1.688
_refine_diff_density_min         -2.039
_refine_diff_density_rms         0.259
_refine_ls_extinction_coef       0.000134(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2939
_refine_ls_number_reflns         81929
_refine_ls_number_restraints     7783
_refine_ls_restrained_S_all      11.231
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.1000
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2885
_refine_ls_wR_factor_ref         0.3256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                53545
_reflns_number_total             81929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00556a2.cif
_cod_data_source_block           Co32-C
_cod_depositor_comments
'Adding full bibliography for 7707115--7707120.cif.'
_cod_original_formula_sum        'C532.73 H790.50 Cl8 Co32 N73.30 O136.83 S32'
_cod_database_code               7707119
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H O N S Co Cl'
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.696
_diffrn_oxdiff_digest_frames
;
01aa904149bee2ce44d21490c4ac319ceb03264c45e
;
_diffrn_oxdiff_digest_hkl
;
01f96dc048892ebbf8f454f61f6bb4776d5774
;
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Shared sites
{O34, N15}
3. Restrained distances
 C95-C186 = C95-C168 = C95-C185 = C95-C173 = C95-C187 = C95-C169
 1.54 with sigma of 0.01
 C185-C186 = C186-C187
 2.5 with sigma of 0.01
 C168-C169 = C169-C173
 2.5 with sigma of 0.01
 C191-C189 = C189-C190 = C192-C189
 1.54 with sigma of 0.01
 C192-C191 = C191-C190
 2.5 with sigma of 0.01
 N9-C183 = N9-C138
 1.47 with sigma of 0.01
 O44-C197
 1.21 with sigma of 0.01
 N13-C196 = N13-C197 = N13-C198_$1
 1.47 with sigma of 0.01
 C198-O49
 1.21 with sigma of 0.01
 N13-O49
 2 with sigma of 0.01
 N15-C204
 1.47 with sigma of 0.01
 O50-N16
 2.3 with sigma of 0.01
 N16-C208 = N16-C206 = N16-C207
 1.47 with sigma of 0.01
 C207-O50
 1.21 with sigma of 0.01
 C175-C177 = C177-C176
 2.5 with sigma of 0.01
 C176-C105 = C105-C177 = C105-C175
 1.54 with sigma of 0.01
 N18-C213 = N18-C212 = N18-C214
 1.47 with sigma of 0.01
 N17-C210 = N17-C211 = N17-C209
 1.47 with sigma of 0.01
 N19-C210 = N19-C216 = N19-C215
 1.47 with sigma of 0.01
 O51-C216
 1.21 with sigma of 0.01
 N22-C222 = N22-C221 = N22-C224
 1.47 with sigma of 0.01
 O56-C221
 1.21 with sigma of 0.01
 N21-C220 = N21-C223 = N21-C219
 1.47 with sigma of 0.01
 O55-C220
 1.21 with sigma of 0.01
 O55-N21
 2.5 with sigma of 0.01
 N20-C218 = N20-C225 = N20-C217
 1.47 with sigma of 0.01
 C217-O53
 1.21 with sigma of 0.01
 C218-O53
 2.7 with sigma of 0.01
 C206-C208 \\sim C208-C207 \\sim C207-C206
 with sigma of 0.02
 C213-C212 \\sim C212-C214 \\sim C214-C213
 with sigma of 0.02
 C211-C209 \\sim C209-C210 \\sim C210-C211
 with sigma of 0.02
 C216-C210 \\sim C210-C215 \\sim C215-C216
 with sigma of 0.02
 C221-C222 \\sim C222-C224 \\sim C224-C221
 with sigma of 0.02
 C220-C223 \\sim C223-C219 \\sim C219-C220
 with sigma of 0.02
 C218-C217 \\sim C217-C225 \\sim C225-C218
 with sigma of 0.02
4. Restrained planarity
 N18, C212, C213, C214, O52
 with sigma of 0.01
 N21, C219, C223, C220, O55
 with sigma of 0.01
 N20, C218, C217, O53, C225
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C95 \\sim C168 \\sim C169 \\sim C173 \\sim C185 \\sim C186 \\sim C187: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C189 \\sim C191 \\sim C190 \\sim C192: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O43 \\sim N9 \\sim C138 \\sim C179 \\sim C183: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
O41 \\sim C178 \\sim N11 \\sim C181 \\sim C184: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
O33 \\sim C202 \\sim O48: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
O42 \\sim C182 \\sim N10 \\sim C115 \\sim C180 \\sim O46: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002
N13 \\sim C196 \\sim C197 \\sim O44 \\sim C198 \\sim O49: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002
N15 \\sim C201 \\sim C204 \\sim O34: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C175 \\sim C105 \\sim C176 \\sim C177: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O37 \\sim C203 \\sim O47: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
O51 \\sim C209 \\sim C210 \\sim N17 \\sim C211 \\sim N19 \\sim C215 \\sim C216:
within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
O31 \\sim C193 \\sim N12 \\sim C194 \\sim C195: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
O53 \\sim C217 \\sim N20 \\sim C225 \\sim C218: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
O45 \\sim C199 \\sim C200 \\sim N14 \\sim C205: within 2A with sigma of 0.001
and sigma for terminal atoms of 0.002
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111
\\sim C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116 \\sim C117 \\sim C118
\\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim C125
\\sim C126 \\sim C127 \\sim C128 \\sim C129 \\sim C130 \\sim C131 \\sim C132
\\sim C133 \\sim C134 \\sim C135 \\sim C136 \\sim C137 \\sim C138 \\sim C139
\\sim C140 \\sim C141 \\sim C142 \\sim C143 \\sim C144 \\sim C145 \\sim C146
\\sim C147 \\sim C148 \\sim C149 \\sim C150 \\sim C151 \\sim C152 \\sim C153
\\sim C154 \\sim C155 \\sim C156 \\sim C157 \\sim C158 \\sim C159 \\sim C160
\\sim C161 \\sim C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim C167
\\sim C168 \\sim C169 \\sim C170 \\sim C171 \\sim C172 \\sim C173 \\sim C174
\\sim C175 \\sim C176 \\sim C177 \\sim C178 \\sim C179 \\sim C180 \\sim C181
\\sim C182 \\sim C183 \\sim C184 \\sim C185 \\sim C186 \\sim C187 \\sim C188
\\sim C189 \\sim C190 \\sim C191 \\sim C192 \\sim C193 \\sim C194 \\sim C195
\\sim C196 \\sim C197 \\sim C198 \\sim C199 \\sim C200 \\sim C201 \\sim C202
\\sim C203 \\sim C204 \\sim C205 \\sim C206 \\sim C207 \\sim C208 \\sim C209
\\sim C210 \\sim C211 \\sim C212 \\sim C213 \\sim C214 \\sim C215 \\sim C216
\\sim C217 \\sim C218 \\sim C219 \\sim C220 \\sim C221 \\sim C222 \\sim C223
\\sim C224 \\sim C225 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6
\\sim N7 \\sim N8 \\sim N9 \\sim N10 \\sim N11 \\sim N12 \\sim N13 \\sim N14
\\sim N15 \\sim N16 \\sim N17 \\sim N18 \\sim N19 \\sim N20 \\sim N21 \\sim N22
\\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim
O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim
O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim
O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30 \\sim O31 \\sim O32 \\sim
O33 \\sim O34 \\sim O35 \\sim O36 \\sim O37 \\sim O38 \\sim O39 \\sim O40 \\sim
O41 \\sim O42 \\sim O43 \\sim O44 \\sim O45 \\sim O46 \\sim O47 \\sim O48 \\sim
O49 \\sim O50 \\sim O51 \\sim O52 \\sim O53 \\sim O55 \\sim O56: within -3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N15) = Uanis(O34)
Uanis(O34) = Uanis(N15)
6. Rigid body (RIGU) restrains
 C173, C169, C168, C95
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C95, C187, C186, C185
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C192, C189, C191, C190
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O41, C178, N11, C181, C184
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C182, O42, N10, C115, C180, O46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N13, C197, C196, O44, C198, O49, O49
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N16, C206, C207, C208
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C175, C105, C176, C177
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O51, C209, C211, C210, N17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O51, C209, C210, N17, C211, N19, C215, C216
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N21, O55, C220, H220, C219, C223, H21V, H21W, H21X, H22D, H22E, H22F
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N20, C218, C217, C225
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O45, C199, C200, N14, C205
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
7. Others
 Sof(C185)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C186)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=Sof(C187)=Sof(H18G)=Sof(H18H)=Sof(H18I)=1-FVAR(1)
 Sof(C168)=Sof(H16Y)=Sof(H)=Sof(HA)=Sof(C169)=Sof(H16Z)=Sof(HB)=Sof(HC)=
 Sof(C173)=Sof(H17J)=Sof(H17K)=Sof(H17L)=FVAR(1)
 Fixed Sof: H31A(0.6) H31B(0.6) H33A(0.66667) H33B(0.66667) O34(0.75)
 H34A(0.75) H34B(0.75) H37A(0.66667) H37B(0.66667) H18M(0.5) H18N(0.5)
 H18O(0.5) H18P(0.5) O42(0.5) C193(0.4) H193(0.4) N12(0.4) C194(0.4) H19J(0.4)
 H19K(0.4) H19L(0.4) C195(0.4) H19M(0.4) H19N(0.4) H19O(0.4) H19S(0.5)
 H19T(0.5) H19U(0.5) O44(0.5) H19V(0.5) H19W(0.5) H19X(0.5) O46(0.5) C201(0.25)
 H20A(0.25) H20B(0.25) H20C(0.25) C202(0.33333) H202(0.33333) C203(0.33333)
 H203(0.33333) O47(0.33333) H47(0.33333) C204(0.25) H20D(0.25) H20E(0.25)
 H20F(0.25) O48(0.33333) H48(0.33333) N15(0.25) H15(0.25) O49(0.5) H20J(0.5)
 H20K(0.5) C209(0.5) H209(0.5) H21D(0.5) H21E(0.5) H21F(0.5) H21A(0.5)
 H21B(0.5) H21C(0.5) N17(0.5) C211(0.5) H21G(0.5) H21H(0.5) H21I(0.5) N19(0.5)
 C215(0.5) H21J(0.5) H21K(0.5) H21L(0.5) C216(0.5) H216(0.5)
8.a Riding coordinates:
 O31(H31A,H31B), O33(H33A,H33B), O34(H34A,H34B), O37(H37A,H37B), C175(H17P,
 H17Q,H17R), C176(H17S,H17T,H17U), C177(H17V,H17W,H17X), C180(H180,H18M,H18N),
 C182(H18O,H182,H18P), C194(H19J,H19K,H19L), C196(H19P,H19Q,H19R), C197(H19S,
 H19T,H19U), C198(H19V,H19W,H19X), C199(H19Y,HF,HG), C200(H20G,H20H,H20I),
 C201(H20A,H20B,H20C), O47(H47), C204(H20D,H20E,H20F), C205(H205), N15(H15),
 C206(H20J,H20K,H20L), C207(H207), C208(H20M,H20N,H20O), C217(H217), C218(H21S,
 H21T,H21U), C225(H22A,H22B,H22C)
8.b Rotating group:
 O35(H35A,H35B), O36(H36A,H36B), O38(H38A,H38B), O40(H40A,H40B)
8.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C10(H10), C19(H19), C21(H21), C24(H24), C27(H27), C38(H38),
 C41(H41), C50(H50), C57(H57), C58(H58), C59(H59), C61(H61), C62(H62), C64(H64),
  C65(H65), C66(H66), C69(H69), C70(H70), C74(H74), C77(H77), C79(H79),
 C80(H80), C82(H82), C85(H85), C90(H90), C93(H93), C96(H96), C100(H100),
 C101(H101), C103(H103), C108(H108), C110(H110), C123(H123), C127(H127),
 C179(H179), C181(H181), C193(H193), C202(H202), C203(H203), C209(H209),
 C213(H213), C216(H216), C220(H220), C221(H221)
8.d Idealised Me refined as rotating group:
 C115(H11A,H11B,H11C), C121(H12A,H12B,H12C), C122(H12D,H12E,H12F), C125(H12G,
 H12H,H12I), C126(H12J,H12K,H12L), C131(H13A,H13B,H13C), C132(H13D,H13E,H13F),
 C133(H13G,H13H,H13I), C134(H13J,H13K,H13L), C135(H13M,H13N,H13O), C137(H13P,
 H13Q,H13R), C138(H13V,H13W,H13X), C139(H13S,H13T,H13U), C141(H14A,H14B,H14C),
 C143(H14D,H14E,H14F), C144(H14G,H14H,H14I), C145(H14J,H14K,H14L), C146(H14M,
 H14N,H14O), C147(H14P,H14Q,H14R), C148(H14S,H14T,H14U), C149(H14V,H14W,H14X),
 C151(H15A,H15B,H15C), C152(H15D,H15E,H15F), C153(H15G,H15H,H15I), C154(H15J,
 H15K,H15L), C156(H15M,H15N,H15O), C157(H15P,H15Q,H15R), C159(H15S,H15T,H15U),
 C160(H16A,H16B,H16C), C161(H16D,H16E,H16F), C162(H16G,H16H,H16I), C163(H16J,
 H16K,H16L), C164(H16M,H16N,H16O), C165(H16P,H16Q,H16R), C166(H16S,H16T,H16U),
 C167(H16V,H16W,H16X), C168(H16Y,H,HA), C169(H16Z,HB,HC), C170(H17A,H17B,H17C),
 C171(H17D,H17E,H17F), C172(H17G,H17H,H17I), C173(H17J,H17K,H17L), C174(H17M,
 H17N,H17O), C178(H17Y,HD,HE), C183(H18Q,H18R,H18S), C184(H18T,H18U,H18V),
 C185(H18A,H18B,H18C), C186(H18D,H18E,H18F), C187(H18G,H18H,H18I), C188(H18J,
 H18K,H18L), C190(H19A,H19B,H19C), C191(H19D,H19E,H19F), C192(H19G,H19H,H19I),
 C195(H19M,H19N,H19O), C210(H21D,H21E,H21F), C210(H21A,H21B,H21C), C211(H21G,
 H21H,H21I), C212(H21M,H21N,H21O), C214(H21P,H21Q,H21R), C215(H21J,H21K,H21L),
 C219(H21V,H21W,H21X), C222(H22G,H22H,H22I), C223(H22D,H22E,H22F), C224(H22J,
 H22K,H22L)
8.e Idealised tetrahedral OH refined as rotating group:
 O48(H48)
;
_shelx_res_checksum              18212
_shelx_hkl_checksum              12180
_shelx_fab_checksum              89255
_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 5.079
_oxdiff_exptl_absorpt_empirical_full_min 0.647