Ancillary ligand-regulated Ti(iv)-based metallocalixarene coordination cages for photocatalytic H2 evolution
Tian, Yi-Qi; Cui, Yun-Shu; Zhu, Jia-Hui; Xu, Cong-Qiao; Yi, Xiao-Yi; Li, Jun; Liu, Chao; Chemical Communications  (2022) –; doi:10.1039/D2CC03131K

data_7130395
_publ_section_title
;
 Ancillary ligand-regulated Ti(iv)-based metallocalixarene coordination
 cages for photocatalytic H2 evolution
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03131K
_journal_year                    2022
_chemical_formula_moiety
'C376 H434 N6 O60 Ti12, 10(C2 H3 N), 2(C1.5 H1.5 N), 2[C2H3N], 10[C2H3N], 10[C2H3N]'
_chemical_formula_sum            'C443 H533 N40 O60 Ti12'
_chemical_formula_weight         7952.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-06-28 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.417(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.2214(6)
_cell_length_b                   21.6454(4)
_cell_length_c                   42.7779(8)
_cell_measurement_reflns_used    39170
_cell_measurement_temperature    149.99(11)
_cell_measurement_theta_max      72.4600
_cell_measurement_theta_min      2.0670
_cell_volume                     22240.0(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      149.99(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -61.00  31.00   0.50    4.00    --  -43.05  51.00-131.00  184
  2  \w    -52.00 -26.00   0.50   14.00    -- -100.00  45.00  30.00   52
  3  \w    -53.00 -26.00   0.50   14.00    -- -100.00  45.00   0.00   54
  4  \w    -54.00 -29.00   0.50   14.00    -- -100.00  45.00  60.00   50
  5  \w    -59.00 -26.00   0.50   14.00    -- -100.00  61.00  60.00   66
  6  \w    -50.00 -25.00   0.50   14.00    -- -100.00  45.00  90.00   50
  7  \w    -67.00 -41.00   0.50   14.00    -- -100.00  61.00  30.00   52
  8  \w    -60.00 -33.00   0.50   14.00    -- -100.00  61.00   0.00   54
  9  \w    -51.00 -26.00   0.50   14.00    -- -100.00  45.00 -30.00   50
 10  \w    -61.00 -27.00   0.50   14.00    -- -100.00  51.00-131.00   68
 11  \w    -53.00 -28.00   0.50   14.00    -- -100.00  45.00-150.00   50
 12  \w    -68.00 -43.00   0.50   14.00    -- -100.00  61.00-120.00   50
 13  \w    -72.00 -37.00   0.50   14.00    -- -100.00  61.00 -30.00   70
 14  \w   -116.00 -50.00   0.50    4.00    --  -43.05 -51.00  82.00  132
 15  \w     45.00  70.00   0.50    4.00    --   43.05  51.00-131.00   50
 16  \w    143.00 169.00   0.50   14.00    --  109.26  51.00-131.00   52
 17  \w     73.00  98.00   0.50   14.00    --  109.26 -77.00 -90.00   50
 18  \w     38.00 103.00   0.50   14.00    --  109.26 -77.00-180.00  130
 19  \w     35.00  64.00   0.50   14.00    --  109.26 -61.00-150.00   58
 20  \w     51.00  93.00   0.50   14.00    --  109.26 -77.00  30.00   84
 21  \w     46.00  77.00   0.50   14.00    --  109.26 -94.00 120.00   62
 22  \w     45.00 104.00   0.50   14.00    --  109.26 -94.00 150.00  118
 23  \w    115.00 172.00   0.50   14.00    --  109.26  30.00 150.00  114
 24  \w    -15.00  12.00   0.50    4.00    --   43.05 -19.00  90.00   54
 25  \w    -31.00  22.00   0.50    4.00    --   43.05 -51.00  82.00  106
 26  \w    -33.00  37.00   0.50    4.00    --   43.05 -37.00 -60.00  140
 27  \w    -17.00  12.00   0.50    4.00    --   43.05 -19.00 -60.00   58
 28  \w   -104.00 -79.00   0.50   14.00    -- -100.00 -45.00 -30.00   50
 29  \w   -174.00 -78.00   0.50   14.00    -- -100.00 -51.00  82.00  192
 30  \w   -175.00-115.00   0.50   14.00    -- -100.00 -45.00 -30.00  120
;
_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      -0.0157385000
_diffrn_orient_matrix_UB_12      -0.0403158000
_diffrn_orient_matrix_UB_13      0.0271935000
_diffrn_orient_matrix_UB_21      -0.0616241000
_diffrn_orient_matrix_UB_22      0.0180078000
_diffrn_orient_matrix_UB_23      -0.0087335000
_diffrn_orient_matrix_UB_31      -0.0084757000
_diffrn_orient_matrix_UB_32      -0.0557499000
_diffrn_orient_matrix_UB_33      -0.0224532000
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            150080
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         2.083
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             7462
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.234
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.267
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2660
_refine_ls_number_reflns         39089
_refine_ls_number_restraints     1048
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.1058
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3227
_refine_ls_wR_factor_ref         0.3413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28972
_reflns_number_total             39089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03131k2.cif
_cod_data_source_block           Ti12L6-2
_cod_database_code               7130395
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 C179-O7
 1.4 with sigma of 0.01
 C41-C173 = C173-C75
 2.5 with sigma of 0.02
 C1M-C1L = C1L-C63A
 2.5 with sigma of 0.02
 C41-C209 = C209-C75
 2.5 with sigma of 0.02
 C167-C171 = C171-C21
 2.5 with sigma of 0.02
 C167-C39 = C39-C171
 1.5 with sigma of 0.02
 C212-C63A
 1.5 with sigma of 0.02
 C1M-C79A = C79A-C63A
 2.5 with sigma of 0.02
 C198-C185 = C185-C200
 1.5 with sigma of 0.02
 C43-C173
 1.5 with sigma of 0.02
 C173-C77
 2.5 with sigma of 0.02
 C179-Ti5
 3.1 with sigma of 0.02
 C208-C198
 1.5 with sigma of 0.02
 C155-C5 = C5-C151
 1.5 with sigma of 0.02
 C210-C198
 2.5 with sigma of 0.02
 O25-C5
 1.4 with sigma of 0.02
 C210-C1J = C1J-C198
 2.5 with sigma of 0.02
 C125-C137
 1.5 with sigma of 0.02
 C177-C125 = C125-C37
 1.5 with sigma of 0.02
 C199-C185
 1.5 with sigma of 0.02
 C209-C43A
 1.5 with sigma of 0.02
 C1J-C208 = C208-C210
 1.5 with sigma of 0.02
 C208-C91A
 1.5 with sigma of 0.02
 C1M-C212 = C212-C1L
 1.5 with sigma of 0.02
 C161-C85
 2.5 with sigma of 0.02
 C73A-C79A = C79A-C201
 1.4 with sigma of 0.02
 C1L-C79A
 2.5 with sigma of 0.02
 C212-C79A
 1.5 with sigma of 0.02
 C212-C201
 2.5 with sigma of 0.02
 C1L-C201
 2.8 with sigma of 0.02
 C201-C73A
 2.5 with sigma of 0.02
 C149-C83 = C83-C169
 1.5 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C75) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C173)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C167) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C171) \\sim Ueq, Uanis(C200) \\sim Ueq, Uanis(C185) \\sim Ueq,
Uanis(C199) \\sim Ueq, Uanis(C198) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C45A)
\\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C214) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C39) \\sim Ueq, Uanis(C167) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C171)
\\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C211) \\sim Ueq, Uanis(C1K) \\sim Ueq,
Uanis(C21A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C63A) \\sim Ueq, Uanis(C212) \\sim Ueq, Uanis(C1M) \\sim Ueq, Uanis(C1L)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C179) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C181) \\sim Ueq, Uanis(C91)
\\sim Ueq, Uanis(C183) \\sim Ueq, Uanis(C89) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C155) \\sim Ueq, Uanis(C151) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N10) \\sim Ueq, Uanis(C196) \\sim Ueq, Uanis(C197) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C85) \\sim Ueq, Uanis(C161) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C67) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C169) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C137) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C177) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C153) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C131) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C147) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1J) \\sim Ueq, Uanis(C210) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C69) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C165) \\sim Ueq, Uanis(C202) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C209) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C79A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C208) \\sim Ueq, Uanis(C205) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C81) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C161)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C35) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C11, C13, C21, C25, C29, C35, C39, C41, C43, C45, C69, C71, C75, C77, C85,
 C101, C107, C121, C128, C131, C133, C147, C153, C161, C164, C167, C171, C173,
 C181, C185, C198, C199, C200
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1J, C41, C43, C43A, C75, C77, C77A, C91, C91A, C173, C185, C198, C199, C200,
 C205, C208, C209, C210
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O13, C1A, C1L, C1M, C9, C9A, C63, C63A, C73, C73A, C79, C79A, C135, C141,
 C143, C145, C157, C159, C175, C201, C212
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1K, C21, C21A, C29, C29A, C39, C39A, C167, C171, C211
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1J, C198, C208, C210
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O25, C5, C151, C155
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C25, C45, C89, C91, C179, C181, C183
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N10, C196, C197
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O21, C87, C165, C202, C203
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O29, C83, C149, C169
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C35, C67, C71, C81, C85, C93, C161
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C1A)=Sof(C1B)=Sof(H1B)=Sof(C1C)=Sof(H1C)=Sof(C1D)=Sof(H1D)=Sof(C1E)=
 Sof(C1F)=Sof(H1F)=Sof(C1G)=Sof(C1H)=Sof(C1I)=Sof(H1IA)=Sof(H1IB)=Sof(C1J)=
 Sof(H1JA)=Sof(H1JB)=Sof(H1JC)=Sof(C1K)=Sof(H1KA)=Sof(H1KB)=Sof(H1KC)=Sof(C1L)=
 Sof(H1LA)=Sof(H1LB)=Sof(H1LC)=Sof(C1M)=Sof(H1MA)=Sof(H1MB)=Sof(H1MC)=Sof(C9A)=
 Sof(C11A)=Sof(H11A)=Sof(C13A)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C21A)=
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C29A)=
 Sof(C39A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C43A)=Sof(C45A)=Sof(C63A)=
 Sof(H63A)=Sof(H63B)=Sof(H63C)=Sof(C69A)=Sof(H69C)=Sof(H69D)=Sof(C73A)=
 Sof(H73A)=Sof(H75D)=Sof(H75E)=Sof(H75F)=Sof(C77A)=Sof(C79A)=Sof(C89A)=
 Sof(C91A)=Sof(C175)=Sof(H19H)=Sof(H19I)=Sof(H19J)=Sof(C201)=Sof(H201)=
 Sof(C204)=Sof(C205)=Sof(H205)=Sof(C206)=Sof(C207)=Sof(C208)=Sof(C209)=
 Sof(H20I)=Sof(H20J)=Sof(H20K)=Sof(C210)=Sof(H21G)=Sof(H21H)=Sof(H21I)=
 Sof(C211)=Sof(H21J)=Sof(H21K)=Sof(H21L)=Sof(C212)=1-FVAR(1)
 Sof(C9)=Sof(C11)=Sof(H11)=Sof(C13)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C21)=
 Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C29)=Sof(C39)=
 Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C43)=Sof(C63)=Sof(C69)=Sof(H69A)=Sof(H69B)=
 Sof(C73)=Sof(H73)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C77)=Sof(C79)=Sof(H79A)=
 Sof(H79B)=Sof(H79C)=Sof(C89)=Sof(C179)=Sof(C45)=Sof(C181)=Sof(H181)=Sof(C91)=
 Sof(C183)=Sof(H183)=Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(C107)=Sof(C121)=
 Sof(C128)=Sof(C131)=Sof(C133)=Sof(H133)=Sof(C135)=Sof(C141)=Sof(C143)=
 Sof(C145)=Sof(H145)=Sof(C147)=Sof(H147)=Sof(C153)=Sof(H153)=Sof(C157)=
 Sof(H15J)=Sof(H15K)=Sof(H15L)=Sof(C159)=Sof(H15M)=Sof(H15N)=Sof(H15O)=
 Sof(C164)=Sof(C167)=Sof(H16O)=Sof(H16P)=Sof(H16Q)=Sof(C171)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C173)=Sof(H17G)=Sof(H17H)=Sof(H17I)=Sof(C185)=
 Sof(H19E)=Sof(H19F)=Sof(H19G)=Sof(C199)=Sof(H19K)=Sof(H19L)=Sof(H19M)=
 Sof(C200)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
 Sof(H83A)=Sof(O29A)=1-FVAR(2)
 Sof(O29)=Sof(H83)=FVAR(2)
 Sof(H49A)=Sof(C214)=Sof(H21O)=Sof(H21P)=Sof(H21Q)=1-FVAR(3)
 Sof(H49)=Sof(C163)=Sof(H16I)=Sof(H16J)=Sof(H16K)=FVAR(3)
 Fixed Sof: C87(0.5) H87A(0.5) H87B(0.5) C165(0.5) H16L(0.5) H16M(0.5)
 H16N(0.5) C202(0.5) H20D(0.5) H20E(0.5) H20F(0.5) C203(0.5) H20G(0.5)
 H20H(0.5) C189(0.5) H18H(0.5) H18I(0.5) H18J(0.5)
5.a Riding coordinates:
 C41(H41A,H41B,H41C), C41(H41D,H41E,H41F), C63A(H63A,H63B,H63C), C75(H75A,H75B,
 H75C), C75(H75D,H75E,H75F), C171(H17D,H17E,H17F), C173(H17G,H17H,H17I),
 C198(H19E,H19F,H19G), C198(H19H,H19I,H19J)
5.b Ternary CH refined with riding coordinates:
 C5(H5), C49(H49), C49(H49A), C83(H83), C83(H83A), C119(H119), C130(H130)
5.c Secondary CH2 refined with riding coordinates:
 C1I(H1IA,H1IB), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B), C19A(H19C,
 H19D), C25(H25A,H25B), C25A(H25C,H25D), C69(H69A,H69B), C69A(H69C,H69D),
 C82(H82A,H82B), C87(H87A,H87B), C101(H10A,H10B), C114(H11H,H11I), C126(H12D,
 H12E), C140(H14A,H14B), C182(H18C,H18D), C203(H20G,H20H), C213(H21M,H21N)
5.d Aromatic/amide H refined with riding coordinates:
 C1B(H1B), C1C(H1C), C1D(H1D), C1F(H1F), C3(H3), C11(H11), C11A(H11A),
 C22(H22), C23(H23), C24(H24), C27(H27), C36(H36), C40(H40), C44(H44), C53(H53),
  C56(H56), C61(H61), C62(H62), C70(H70), C73(H73), C73A(H73A), C74(H74),
 C78(H78), C84(H84), C88(H88), C181(H181), C183(H183), C90(H90), C92(H92),
 C94(H94), C99(H99), C104(H104), C108(H108), C109(H109), C133(H133), C136(H136),
  C138(H138), C145(H145), C146(H146), C147(H147), C148(H148), C150(H150),
 C153(H153), C154(H154), C158(H158), C162(H162), C166(H166), C168(H168),
 C170(H170), C178(H178), C184(H184), C201(H201), C205(H205)
5.e Fitted hexagon refined as free rotating group:
 C89(C179,C45,C181,C91,C183)
5.f Idealised Me refined as rotating group:
 C1J(H1JA,H1JB,H1JC), C1K(H1KA,H1KB,H1KC), C1L(H1LA,H1LB,H1LC), C1M(H1MA,H1MB,
 H1MC), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C21(H21A,
 H21B,H21C), C21A(H21D,H21E,H21F), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C),
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C79(H79A,
 H79B,H79C), C81(H81A,H81B,H81C), C85(H85A,H85B,H85C), C103(H10C,H10D,H10E),
 C111(H11B,H11C,H11D), C113(H11E,H11F,H11G), C115(H11J,H11K,H11L), C117(H11M,
 H11N,H11O), C123(H12A,H12B,H12C), C127(H12F,H12G,H12H), C129(H12I,H12J,H12K),
 C137(H13A,H13B,H13C), C139(H13D,H13E,H13F), C149(H14C,H14D,H14E), C151(H15D,
 H15E,H15F), C155(H15G,H15H,H15I), C157(H15J,H15K,H15L), C159(H15M,H15N,H15O),
 C160(H16C,H16D,H16E), C161(H16F,H16G,H16H), C163(H16I,H16J,H16K), C165(H16L,
 H16M,H16N), C167(H16O,H16P,H16Q), C169(H16R,H16S,H16T), C174(H17J,H17K,H17L),
 C176(H17M,H17N,H17O), C177(H17P,H17Q,H17R), C199(H19K,H19L,H19M), C200(H20A,
 H20B,H20C), C202(H20D,H20E,H20F), C209(H20I,H20J,H20K), C210(H21G,H21H,H21I),
 C211(H21J,H21K,H21L), C187(H18E,H18F,H18G), C189(H18H,H18I,H18J), C191(H19N,
 H19O,H19P), C193(H19Q,H19R,H19S), C195(H19T,H19U,H19V), C197(H19W,H19X,H19Y),
 C214(H21O,H21P,H21Q)
;
_shelx_res_checksum              49164
_shelx_hkl_checksum              48040
_shelx_fab_checksum              9471
_platon_squeeze_special_details
;
A solvent mask was calculated and 468 electrons were 
found in a volume of 3426\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 2[C2H3N], 10[C2H3N], 10[C2H3N] per Formula Unit 
which account for 484 electrons per unit cell.
;
_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 1.540
_oxdiff_exptl_absorpt_empirical_full_min 0.670