Stabilization of liquid active guests via nanoconfinement into a flexible microporous metal–organic framework
Mazzeo, Paolo P.; Balestri, Davide; Bacchi, Alessia; Pelagatti, Paolo; CrystEngComm 23 (2021) 7262–7269; doi:10.1039/D1CE00899D

data_7243491
_publ_section_title
;
 Stabilization of liquid active guests via nanoconfinement into a flexible
 microporous metal--organic framework
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              7262
_journal_page_last               7269
_journal_paper_doi               10.1039/D1CE00899D
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety
'0.75(C104.5 H68.5 N8 O20 Zn4), 3.25(C12 H18 O), 0.5(C9 H9.25 O0.75), 1.63(C3 H7 N O)'
_chemical_formula_sum            'C126.62 H125.75 N7.62 O20.25 Zn3'
_chemical_formula_weight         2274.45
_chemical_name_common            PUM168@propofol
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-07 deposited with the CCDC.	2021-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                89.20(3)
_cell_angle_beta                 82.16(3)
_cell_angle_gamma                87.80(3)
_cell_formula_units_Z            4
_cell_length_a                   15.263(3)
_cell_length_b                   30.497(6)
_cell_length_c                   26.950(5)
_cell_measurement_reflns_used    5323
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.153
_cell_measurement_theta_min      3.521
_cell_volume                     12418(4)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010) - CCP4 (Evans, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            296249
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.266
_diffrn_reflns_theta_min         0.751
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.618
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             4764
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.339
_refine_diff_density_min         -1.425
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3272
_refine_ls_number_reflns         46776
_refine_ls_number_restraints     2946
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0898
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1608P)^2^+41.6508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2695
_refine_ls_wR_factor_ref         0.2716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                44338
_reflns_number_total             46776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00899d2.cif
_cod_data_source_block           pum168@propofol
_cod_depositor_comments
'Adding full bibliography for 7243489--7243491.cif.'
_cod_original_cell_volume        12417(4)
_cod_database_code               7243491
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.941
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N1D4-C3D4 = N1D4-C2D4
 1.45 with sigma of 0.02
 C2D4-C3D4
 2.5 with sigma of 0.02
 N1DA-C2DA = N1DA-C3DA = N1D1-C3D1 = N1D1-C2D1 = N1DA-C1DA = N1D1-C1DA
 1.45 with sigma of 0.02
 C7D-C1D
 2.35 with sigma of 0.02
 C1D-C8D
 2.35 with sigma of 0.02
 C7D-C8D
 2.7 with sigma of 0.02
 C6D-C7D = C8D-C6D
 1.5 with sigma of 0.02
 OPD-C0D
 1.3 with sigma of 0.02
 O11-N21
 2.25 with sigma of 0.02
 C9D-C10D
 1.5 with sigma of 0.02
 C9D-C11D
 1.5 with sigma of 0.02
 N1DA-C3DA = N1DA-C2DA
 1.5 with sigma of 0.02
 C0F-C10F
 3.6 with sigma of 0.02
 C10F-C9F
 1.45 with sigma of 0.02
 C9F-C11F
 1.45 with sigma of 0.02
 C6F-C7F
 1.5 with sigma of 0.02
 C8F-C6F = C7F-C6F
 1.5 with sigma of 0.02
 C10C-C9C
 1.5 with sigma of 0.02
 C9C-C11C
 1.5 with sigma of 0.02
 C9C-C10C = C9C-C11C
 1.5 with sigma of 0.02
 OPC1-C0C
 1.3 with sigma of 0.02
 C131-C101 = C132-C102
 1.5 with sigma of 0.02
 O8AA-C192
 1.2 with sigma of 0.02
 O1PF-C0F
 1.3 with sigma of 0.02
 C10D-C11D
 2.5 with sigma of 0.04
 C3DA-C2DA
 2.5 with sigma of 0.04
 C1D4-C2D4
 2.4 with sigma of 0.04
 C1D4-C3D4
 2.4 with sigma of 0.04
 C8F-C7F
 2.5 with sigma of 0.04
 C11C-C10C
 2.5 with sigma of 0.04
 C1C-OPC1
 2.4 with sigma of 0.04
 C5C-OPC1
 2.4 with sigma of 0.04
 C5F-C11F
 2.6 with sigma of 0.04
 C5F-C10F
 2.6 with sigma of 0.04
 C1F-C8F
 2.6 with sigma of 0.04
 C1F-C7F
 2.6 with sigma of 0.04
 C202-O8AA
 2.36 with sigma of 0.04
 C1DI-C2DI = O1D4-N1D4
 2.2 with sigma of 0.04
 C1F-O1PF
 2.4 with sigma of 0.04
 O1PF-C5F
 2.4 with sigma of 0.04
 C55-C65A \\sim C55A-C65B
 with sigma of 0.02
 C55-C45A \\sim C55A-C45B
 with sigma of 0.02
 C55-C85 \\sim C55A-C85
 with sigma of 0.02
 C65A-C75A \\sim C65B-C75B
 with sigma of 0.02
 C75A-C25 \\sim C75B-C25A
 with sigma of 0.02
 C25-C35A \\sim C25A-C35B
 with sigma of 0.02
 C25-C15 \\sim C25A-C15
 with sigma of 0.02
 C35A-C45A \\sim C35B-C45B
 with sigma of 0.02
 C55-C75A \\sim C55A-C75B
 with sigma of 0.04
 C55-C35A \\sim C55A-C35B
 with sigma of 0.04
 C65A-C25 \\sim C65B-C25A
 with sigma of 0.04
 C65A-C45A \\sim C65B-C45B
 with sigma of 0.04
 C65A-C85 \\sim C65B-C85
 with sigma of 0.04
 C75A-C35A \\sim C75B-C35B
 with sigma of 0.04
 C75A-C15 \\sim C75B-C15
 with sigma of 0.04
 C25-C45A \\sim C25A-C45B
 with sigma of 0.04
 C35A-C15 \\sim C35B-C15
 with sigma of 0.04
 C45A-C85 \\sim C45B-C85
 with sigma of 0.04
3. Restrained planarity
 C10C, O1D4, C1D4, C2D4, N1D4, C3D4
 with sigma of 0.001
 O1D4, C1D4, N1D4, C2D4
 with sigma of 0.1
 O1PF, C0F, C5F, C1F, C2F, C4F, C3F
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
O19 \\sim O29 \\sim N29 \\sim N39 \\sim C59 \\sim C49 \\sim C39 \\sim C29 \\sim
C19 \\sim N19 \\sim C69 \\sim C129 \\sim C119 \\sim C109 \\sim C99 \\sim C89
\\sim C79 \\sim C149 \\sim C159 \\sim C169 \\sim C179 \\sim C189 \\sim C139
\\sim C199 \\sim C249 \\sim C239 \\sim N49 \\sim C229 \\sim C219 \\sim C209:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C11B \\sim O1PB \\sim C0B \\sim C5B \\sim C1B \\sim C4B \\sim C6B \\sim C2B
\\sim C9B \\sim C3B \\sim C8B \\sim C7B \\sim C10B: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
O1PG \\sim C0G \\sim C5G \\sim C1G \\sim C10G \\sim C4G \\sim C2G \\sim C6G
\\sim C11G \\sim C9G \\sim C3G \\sim C7G \\sim C8G: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C5HA \\sim OPG \\sim C1IA \\sim C4AA \\sim C0AA \\sim C158 \\sim C205 \\sim
C6HA \\sim C1MA \\sim C269 \\sim C369 \\sim C3BA \\sim C2MA: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C11D \\sim C7D \\sim C6D \\sim C8D \\sim C1D \\sim C0D \\sim C2D \\sim OPD
\\sim C5D \\sim C3D \\sim C9D \\sim C4D \\sim C10D: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
O21 \\sim N31 \\sim N41 \\sim C7GA \\sim C201 \\sim C241 \\sim C231 \\sim C141
\\sim C151 \\sim C161 \\sim C172 \\sim C182 \\sim C131 \\sim C191 \\sim C221
\\sim C81 \\sim C91 \\sim C101 \\sim C3GA \\sim C121 \\sim C71 \\sim O11 \\sim
N21 \\sim C51 \\sim N11 \\sim C11 \\sim C21 \\sim C31 \\sim C41 \\sim C61:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
O7AA \\sim N22 \\sim C52 \\sim C42 \\sim C32 \\sim C22 \\sim C12 \\sim N12
\\sim C62 \\sim C122 \\sim C72 \\sim O8AA \\sim C9HA \\sim C202 \\sim N32 \\sim
C192 \\sim C82 \\sim C92 \\sim C102 \\sim C181 \\sim C171 \\sim C162 \\sim C152
\\sim C142 \\sim C132 \\sim N42 \\sim C222 \\sim C242 \\sim C232: within 1.7A
with sigma of 0.004 and sigma for terminal atoms of 0.008
O16 \\sim N26 \\sim C46 \\sim C36 \\sim C26 \\sim C16 \\sim N16 \\sim C56 \\sim
C66 \\sim C156 \\sim C146 \\sim C136 \\sim C186 \\sim C176 \\sim C166 \\sim C96
\\sim C86 \\sim C76 \\sim C126 \\sim C116 \\sim C106 \\sim O26 \\sim N36 \\sim
C196 \\sim C216 \\sim C226 \\sim N46 \\sim C236 \\sim C246 \\sim C206: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C1I \\sim OPI \\sim C0I \\sim C5I \\sim C2I \\sim C9I \\sim C4I \\sim C6I \\sim
C3I \\sim C11I \\sim C10I \\sim C8I \\sim C7I: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
O1D1 \\sim C1DA \\sim C1D1 \\sim N1DA \\sim N1D1 \\sim C2DA \\sim C3DA \\sim
C3D1 \\sim C2D1: within 1.7A with sigma of 0.004 and sigma for terminal atoms
of 0.008
O1DI \\sim C1DI \\sim N2DI \\sim C3DI \\sim C2DI: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C60 \\sim C50 \\sim C40 \\sim C30 \\sim C20 \\sim C70: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C100 \\sim C110 \\sim C120 \\sim C130 \\sim C80 \\sim C90: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
O17 \\sim N27 \\sim N17 \\sim C17 \\sim C27 \\sim C37 \\sim C47 \\sim C57 \\sim
C67 \\sim C107 \\sim C97 \\sim C87 \\sim C77 \\sim C127 \\sim C117 \\sim C177
\\sim C187 \\sim C137 \\sim C147 \\sim C157 \\sim C167 \\sim O26 \\sim N36
\\sim C196 \\sim C216 \\sim C226 \\sim N46 \\sim C236 \\sim C246 \\sim C206:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
C611 \\sim C511 \\sim C411 \\sim C311 \\sim C211 \\sim C711: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C65A \\sim C75A \\sim C25 \\sim C35A \\sim C45A \\sim C55: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
O17 \\sim N27 \\sim N17 \\sim C17 \\sim C27 \\sim C37 \\sim C47 \\sim C57 \\sim
C67 \\sim O16 \\sim N26 \\sim C46 \\sim C36 \\sim C26 \\sim C16 \\sim N16 \\sim
C56 \\sim C66 \\sim C107 \\sim C97 \\sim C87 \\sim C77 \\sim C127 \\sim C117
\\sim C96 \\sim C86 \\sim C76 \\sim C126 \\sim C116 \\sim C106 \\sim C177 \\sim
C187 \\sim C137 \\sim C147 \\sim C157 \\sim C167 \\sim C156 \\sim C146 \\sim
C136 \\sim C186 \\sim C176 \\sim C166 \\sim O26 \\sim N36 \\sim C196 \\sim C216
\\sim C226 \\sim N46 \\sim C236 \\sim C246 \\sim C206: within 1.7A with sigma
of 0.002 and sigma for terminal atoms of 0.004
C11H \\sim OPH \\sim C0H \\sim C1H \\sim C5H \\sim C2H \\sim C9H \\sim C6H
\\sim C4H \\sim C3H \\sim C10H \\sim C7H \\sim C8H: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C9H \\sim OPH \\sim C0H \\sim C1H \\sim C5H \\sim C2H \\sim C6H \\sim C4H \\sim
C3H \\sim C11H \\sim C10H \\sim C7H \\sim C8H: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008
C412 \\sim C512 \\sim C612 \\sim C712 \\sim C212 \\sim C312: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C25C \\sim OPC2 \\sim C20C \\sim C21C \\sim C26C \\sim C22C \\sim C24C \\sim
C29C \\sim C28C \\sim C27C \\sim C23C \\sim C30C \\sim C31C: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.008
C11C \\sim OPC1 \\sim C0C \\sim C1C \\sim C5C \\sim C2C \\sim C6C \\sim C4C
\\sim C9C \\sim C3C \\sim C7C \\sim C8C \\sim C10C: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C24C \\sim OPC1 \\sim C0C \\sim C1C \\sim C5C \\sim C2C \\sim C6C \\sim C4C
\\sim C9C \\sim C3C \\sim C7C \\sim C8C \\sim C11C \\sim C10C \\sim C30C \\sim
C25C \\sim C29C \\sim C28C \\sim C27C \\sim C23C \\sim C20C \\sim C31C \\sim
C26C \\sim C22C \\sim OPC2 \\sim C21C: within 1.7A with sigma of 0.004 and
sigma for terminal atoms of 0.008
C25 \\sim C25A \\sim C55 \\sim C55A \\sim C35A \\sim C45A \\sim C45B \\sim C35B
\\sim H45B \\sim C75A \\sim C75B \\sim C65A \\sim C65B: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
C2D4 \\sim O1D4 \\sim C1D4 \\sim N1D4 \\sim C3D4: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C11A \\sim O1PA \\sim C0A \\sim C1A \\sim C5A \\sim C9A \\sim C2A \\sim C4A
\\sim C6A \\sim C10A \\sim C3A \\sim C7A \\sim C8A: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
O1PF \\sim C0F \\sim C5F \\sim C1F \\sim C9F \\sim C4F \\sim C6F \\sim C2F
\\sim C11F \\sim C10F \\sim C3F \\sim C7F \\sim C8F: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(O17) \\sim Ueq, Uanis(N27) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C47) \\sim Ueq,
Uanis(C57) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C97)
\\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C127) \\sim Ueq,
Uanis(C117) \\sim Ueq, Uanis(C177) \\sim Ueq, Uanis(C187) \\sim Ueq,
Uanis(C137) \\sim Ueq, Uanis(C147) \\sim Ueq, Uanis(C157) \\sim Ueq,
Uanis(C167) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C0F) \\sim Ueq, Uanis(O1PF) \\sim Ueq, Uanis(C5F) \\sim Ueq, Uanis(C1F)
\\sim Ueq, Uanis(C9F) \\sim Ueq, Uanis(C4F) \\sim Ueq, Uanis(C6F) \\sim Ueq,
Uanis(C2F) \\sim Ueq, Uanis(C11F) \\sim Ueq, Uanis(C10F) \\sim Ueq, Uanis(C3F)
\\sim Ueq, Uanis(C7F) \\sim Ueq, Uanis(C8F) \\sim Ueq: with sigma of 0.05 and
sigma for terminal atoms of 0.1
5. Others
 Sof(C25A)=Sof(C45B)=Sof(H45B)=Sof(C35B)=Sof(H35B)=Sof(C65B)=Sof(H65B)=
 Sof(C75B)=Sof(H75B)=Sof(C55A)=1-FVAR(1)
 Sof(C55)=Sof(C65A)=Sof(H65A)=Sof(C75A)=Sof(H75A)=Sof(C25)=Sof(C35A)=Sof(H35A)=
 Sof(C45A)=Sof(H45A)=FVAR(1)
 Fixed Sof: H36(0.25) H36A(0.75) O17(0.25) O21(0.75) O11(0.75) N27(0.25)
 H27(0.25) N31(0.75) H31(0.75) N21(0.75) H21(0.75) N17(0.25) C17(0.25)
 H17(0.25) C27(0.25) H27A(0.25) C37(0.25) C47(0.25) H47(0.25) C57(0.25)
 H57(0.25) N41(0.75) C221(0.75) H221(0.75) C7GA(0.75) H7GA(0.75) C201(0.75)
 C241(0.75) H241(0.75) C231(0.75) H231(0.75) C141(0.75) H141(0.75) C151(0.75)
 H151(0.75) C161(0.75) C172(0.75) H172(0.75) C182(0.75) H182(0.75) C131(0.75)
 C67(0.25) C107(0.25) C97(0.75) H97(0.75) C87(0.75) H87(0.75) C77(0.25)
 C127(0.25) H127(0.25) C117(0.25) H117(0.25) C177(0.25) H177(0.25) C187(0.25)
 H187(0.25) C137(0.25) C147(0.25) H147(0.25) C157(0.25) H157(0.25) C167(0.25)
 C51(0.75) H51(0.75) N11(0.75) C11(0.75) H11(0.75) C21(0.75) H21A(0.75)
 C31(0.75) C41(0.75) H41(0.75) C61(0.75) C81(0.75) H81(0.75) C91(0.75)
 H91(0.75) C101(0.75) C3GA(0.75) H3GA(0.75) C121(0.75) H121(0.75) C71(0.75)
 C191(0.75) O7AA(0.25) O8AA(0.25) O16(0.75) N26(0.75) H26(0.75) N22(0.25)
 H22(0.25) N42(0.25) C222(0.25) H222(0.25) C9HA(0.25) H9HA(0.25) C202(0.25)
 C242(0.25) H242(0.25) C232(0.25) H232(0.25) N32(0.25) H32(0.25) C192(0.25)
 C52(0.25) H52(0.25) C42(0.25) H42(0.25) C32(0.25) C22(0.25) H22A(0.25)
 C12(0.25) H12(0.25) N12(0.25) C62(0.25) C82(0.25) H82(0.25) C92(0.25)
 H92(0.25) C102(0.25) C0FA(0.25) H0FA(0.25) C122(0.25) H122(0.25) C72(0.25)
 C156(0.75) H156(0.75) C146(0.75) H146(0.75) C136(0.75) C186(0.75) H186(0.75)
 C176(0.75) H176(0.75) C166(0.75) C181(0.25) H181(0.25) C171(0.25) H171(0.25)
 C162(0.25) C152(0.25) H152(0.25) C142(0.25) H142(0.25) C132(0.25) C46(0.75)
 H46(0.75) C36(0.75) C26(0.75) H26A(0.75) C16(0.75) H16(0.75) N16(0.75)
 C56(0.75) H56(0.75) C66(0.75) C96(0.5) H96(0.5) C86(0.5) H86(0.5) C76(0.75)
 C126(0.75) H126(0.75) C116(0.75) H116(0.75) C106(0.75) O1PG(0.75) H1PG(0.75)
 C7G(0.75) H7GB(0.75) H7GC(0.75) H7GD(0.75) C10G(0.75) H10G(0.75) C8G(0.75)
 H8GA(0.75) H8GB(0.75) H8GC(0.75) C5G(0.75) C4G(0.75) H4G(0.75) C3G(0.75)
 H3G(0.75) C2G(0.75) H2G(0.75) C1G(0.75) C0G(0.75) C6G(0.75) H6G(0.75)
 C11G(0.75) H11G(0.75) H11H(0.75) H11I(0.75) C9G(0.75) H9GA(0.75) H9GB(0.75)
 H9GC(0.75) C7D(0.25) H7DA(0.25) H7DB(0.25) H7DC(0.25) C11D(0.25) H11J(0.25)
 H11K(0.25) H11L(0.25) C8D(0.25) H8DA(0.25) H8DB(0.25) H8DC(0.25) C9D(0.25)
 H9D(0.25) C10D(0.25) H10H(0.25) H10I(0.25) H10J(0.25) OPD(0.25) HPD(0.25)
 C0D(0.25) C5D(0.25) C4D(0.25) H4D(0.25) C3D(0.25) H3D(0.25) C2D(0.25)
 H2D(0.25) C1D(0.25) C6D(0.25) H6D(0.25) OPC1(0.75) HPC1(0.75) C0C(0.75)
 C1C(0.75) C2C(0.75) H2C(0.5) C3C(0.75) H3C(0.5) C4C(0.75) H4C(0.5) C5C(0.75)
 C7C(0.75) H7CA(0.5) H7CB(0.5) H7CC(0.5) C11C(0.75) H11M(0.5) H11N(0.5)
 H11O(0.5) C9C(0.75) H9C(0.5) C10C(0.75) H10K(0.5) H10L(0.5) H10M(0.5)
 C6C(0.75) H6C(0.5) C8C(0.75) H8CA(0.5) H8CB(0.5) H8CC(0.5) O1PF(0.25)
 H1PF(0.25) C7F(0.25) H7FA(0.25) H7FB(0.25) H7FC(0.25) C11F(0.25) H11P(0.25)
 H11Q(0.25) H11R(0.25) C10F(0.25) H10N(0.25) H10O(0.25) H10P(0.25) C9F(0.25)
 H9F(0.25) C6F(0.25) H6F(0.25) C0F(0.25) C5F(0.25) C4F(0.25) H4F(0.25)
 C3F(0.25) H3F(0.25) C2F(0.25) H2F(0.25) C1F(0.25) C8F(0.25) H8FA(0.25)
 H8FB(0.25) H8FC(0.25) H1PA(0.5) OPC2(0.25) HPC2(0.25) C26C(0.25) H26E(0.25)
 C28C(0.25) H28A(0.25) H28B(0.25) H28C(0.25) C30C(0.25) H30A(0.25) H30B(0.25)
 H30C(0.25) C27C(0.25) H27B(0.25) H27C(0.25) H27D(0.25) C20C(0.25) C21C(0.25)
 C22C(0.25) H22C(0.25) C23C(0.25) H23C(0.25) C24C(0.25) H24C(0.25) C25C(0.25)
 C31C(0.25) H31A(0.25) H31B(0.25) H31C(0.25) C29C(0.25) H29C(0.25) N1DA(0.5)
 C2DA(0.5) H2DA(0.5) H2DB(0.5) H2DC(0.5) C3DA(0.5) H3DA(0.5) H3DB(0.5)
 H3DC(0.5) C1DA(0.5) H1DA(0.5) N1D1(0.5) C3D1(0.5) H3DD(0.5) H3DE(0.5)
 H3DF(0.5) C1D1(0.5) H1D1(0.5) C2D1(0.5) H2DD(0.5) H2DE(0.5) H2DF(0.5)
 O1D4(0.25) N1D4(0.25) C1D4(0.25) H1D4(0.25) C3D4(0.25) H3DG(0.25) H3DH(0.25)
 H3DI(0.25) C2D4(0.25) H2DG(0.25) H2DH(0.25) H2DI(0.25) H1PB(0.5)
 Fixed X: H1PA(0.01853) O1D4(0.565361) H1PB(0.108221)
 Fixed Y: H1PA(1.00572) O1D4(0.55073) H1PB(0.99593)
 Fixed Z: H1PA(1.020821) O1D4(1.12845) H1PB(1.020821)
6.a Ternary CH refined with riding coordinates:
 C9B(H9B), C6B(H6B), C10G(H10G), C6G(H6G), C9D(H9D), C6D(H6D), C9C(H9C),
 C6C(H6C), C9F(H9F), C6F(H6F), C6HA(H6HA), C205(H205), C9A(H9A), C6A(H6A),
 C9I(H9I), C6I(H6I), C26C(H26E), C29C(H29C), C6H(H6H), C9H(H9H)
6.b Aromatic/amide H refined with riding coordinates:
 N36(H36), N36(H36A), C68(H68), C78(H78), C38(H38), C48(H48), C104(H104),
 C94(H94), C134(H134), C124(H124), C64(H64), C74(H74), C34(H34), C44(H44),
 C65A(H65A), C75A(H75A), C35A(H35A), C45A(H45A), C93(H93), C103(H103),
 C123(H123), C133(H133), C33(H33), C43(H43), C63(H63), C73(H73), C128(H128),
 C138(H138), C98(H98), C108(H108), C125(H125), C135(H135), C95(H95), C105(H105),
  C216(H216), C226(H226), C236(H236), C246(H246), N27(H27), N31(H31), N21(H21),
 C17(H17), C27(H27A), C47(H47), C57(H57), C221(H221), C7GA(H7GA), C241(H241),
 C231(H231), C141(H141), C151(H151), C172(H172), C182(H182), C97(H97), C87(H87),
  C127(H127), C117(H117), C177(H177), C187(H187), C147(H147), C157(H157),
 C51(H51), C11(H11), C21(H21A), C41(H41), C81(H81), C91(H91), C3GA(H3GA),
 C121(H121), N26(H26), N22(H22), C222(H222), C9HA(H9HA), C242(H242), C232(H232),
  N32(H32), C52(H52), C42(H42), C22(H22A), C12(H12), C82(H82), C92(H92),
 C0FA(H0FA), C122(H122), C156(H156), C146(H146), C186(H186), C176(H176),
 C181(H181), C171(H171), C152(H152), C142(H142), C46(H46), C26(H26A), C16(H16),
 C56(H56), C96(H96), C86(H86), C126(H126), C116(H116), N29(H29), N39(H39),
 C90(H90), C100(H100), C120(H120), C130(H130), C60(H60), C70(H70), C30(H30),
 C40(H40), C711(H711), C611(H611), C411(H411), C311(H311), C312(H312),
 C412(H412), C612(H612), C712(H712), C59(H59), C49(H49), C29(H29A), C19(H19),
 C129(H129), C119(H119), C99(H99), C89(H89), C149(H149), C159(H159), C179(H179),
  C189(H189), C249(H249), C239(H239), C229(H229), C219(H219), C4B(H4B),
 C3B(H3B), C2B(H2B), C4G(H4G), C3G(H3G), C2G(H2G), C4D(H4D), C3D(H3D), C2D(H2D),
  C2C(H2C), C3C(H3C), C4C(H4C), C4F(H4F), C3F(H3F), C2F(H2F), C158(H158),
 C1MA(H1MA), C5HA(H5HA), C2A(H2A), C3A(H3A), C4A(H4A), C2I(H2I), C3I(H3I),
 C4I(H4I), C22C(H22C), C23C(H23C), C24C(H24C), C2H(H2H), C3H(H3H), C4H(H4H),
 C1DA(H1DA), C1D1(H1D1), C1D4(H1D4), C1D3(H1D3), C1DI(H1DI), C45B(H45B),
 C35B(H35B), C65B(H65B), C75B(H75B)
6.c Fitted hexagon refined as free rotating group:
 C68(C78,C28,C38,C48,C58), C104(C94,C84,C134,C124,C114), C64(C74,C24,C34,C44,
 C54), C55(C65A,C75A,C25,C35A,C45A), C93(C103,C113,C123,C133,C83), C33(C43,C53,
 C63,C73,C23), C128(C138,C88,C98,C108,C118), C125(C135,C85,C95,C105,C115),
 C216(C226,N46,C236,C246,C206), N17(C17,C27,C37,C47,C57), N41(C221,C7GA,C201,
 C241,C231), C141(C151,C161,C172,C182,C131), C107(C97,C87,C77,C127,C117),
 C177(C187,C137,C147,C157,C167), C51(N11,C11,C21,C31,C41), C81(C91,C101,C3GA,
 C121,C71), N42(C222,C9HA,C202,C242,C232), C52(C42,C32,C22,C12,N12), C82(C92,
 C102,C0FA,C122,C72), C156(C146,C136,C186,C176,C166), C181(C171,C162,C152,C142,
 C132), C46(C36,C26,C16,N16,C56), C96(C86,C76,C126,C116,C106), C90(C100,C110,
 C120,C130,C80), C60(C70,C20,C30,C40,C50), C711(C611,C511,C411,C311,C211),
 C312(C412,C512,C612,C712,C212), C59(C49,C39,C29,C19,N19), C129(C119,C109,C99,
 C89,C79), C149(C159,C169,C179,C189,C139), C249(C239,N49,C229,C219,C209),
 C5B(C4B,C3B,C2B,C1B,C0B), C5G(C4G,C3G,C2G,C1G,C0G), C0D(C5D,C4D,C3D,C2D,C1D),
 C0C(C1C,C2C,C3C,C4C,C5C), C0F(C5F,C4F,C3F,C2F,C1F), C4AA(C158,C1MA,C5HA,C0AA,
 C1IA), C1A(C2A,C3A,C4A,C5A,C0A), C1I(C2I,C3I,C4I,C5I,C0I), C20C(C21C,C22C,C23C,
 C24C,C25C), C1H(C2H,C3H,C4H,C5H,C0H)
6.d Tetrahedral OH refined with riding coordinates:
 OPC1(HPC1), O1PF(H1PF)
6.e Idealised Me refined with everything fixed:
 C7G(H7GB,H7GC,H7GD), C8G(H8GA,H8GB,H8GC), C11G(H11G,H11H,H11I), C9G(H9GA,H9GB,
 H9GC), C7D(H7DA,H7DB,H7DC), C11D(H11J,H11K,H11L), C8D(H8DA,H8DB,H8DC),
 C10D(H10H,H10I,H10J), C7C(H7CA,H7CB,H7CC), C11C(H11M,H11N,H11O), C10C(H10K,
 H10L,H10M), C8C(H8CA,H8CB,H8CC), C7F(H7FA,H7FB,H7FC), C11F(H11P,H11Q,H11R),
 C10F(H10N,H10O,H10P), C8F(H8FA,H8FB,H8FC), C28C(H28A,H28B,H28C), C30C(H30A,
 H30B,H30C), C27C(H27B,H27C,H27D), C31C(H31A,H31B,H31C), C2DA(H2DA,H2DB,H2DC),
 C3DA(H3DA,H3DB,H3DC), C2D1(H2DD,H2DE,H2DF), C3D4(H3DG,H3DH,H3DI), C2D4(H2DG,
 H2DH,H2DI)
6.f Idealised Me refined as rotating group:
 C8B(H8BA,H8BB,H8BC), C7B(H7BA,H7BB,H7BC), C11B(H11D,H11E,H11F), C10B(H10D,
 H10E,H10F), C3BA(H3BA,H3BB,H3BC), C2MA(H2MA,H2MB,H2MC), C269(H26B,H26C,H26D),
 C369(H36B,H36C,H36D), C7A(H7AA,H7AB,H7AC), C10A(H10A,H10B,H10C), C11A(H11A,
 H11B,H11C), C8A(H8AA,H8AB,H8AC), C8I(H8IA,H8IB,H8IC), C11I(H11S,H11T,H11U),
 C10I(H10Q,H10R,H10S), C7I(H7IA,H7IB,H7IC), C7H(H7HA,H7HB,H7HC), C8H(H8HA,H8HB,
 H8HC), C11H(H11V,H11W,H11X), C10H(H10T,H10U,H10V), C3D1(H3DD,H3DE,H3DF),
 C3D3(H3DJ,H3DK,H3DL), C2D3(H2DJ,H2DK,H2DL), C3DI(H3DM,H3DN,H3DO), C2DI(H2DM,
 H2DN,H2DO)
6.g Idealised tetrahedral OH refined with everything fixed:
 O1PG(H1PG), OPD(HPD), OPC2(HPC2)
6.h Idealised tetrahedral OH refined as rotating group:
 O1PB(H1PC), OPG(HPG), OPI(HPI), OPH(HPH)
;
_shelx_res_checksum              90198
_shelx_hkl_checksum              93475
_olex2_exptl_crystal_mounting_method CryoLoop
_olex2_submission_special_instructions 'No special instructions were received'