Regiocontrolled Dimerization of Asymmetric Diazaheptacene Derivatives Toward X-shaped Porous Semiconductors
Zhang , Guowei; Zhang, Lei; Lv, Aifeng; Yang, Xingzhou; Zheng, Yonghao; Gu, Wen; Xue, Ning; Chemical Science  (2020) –; doi:10.1039/D0SC03744C

data_1559105
_publ_section_title
;
 Regiocontrolled Dimerization of Asymmetric Diazaheptacene Derivatives
 Toward X-shaped Porous Semiconductors
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03744C
_journal_year                    2020
_chemical_formula_moiety         '1(C140 H168 Br4 N8 O8 Si4), 2(C7 H8)'
_chemical_formula_sum            'C154 H184 Br4 N8 O8 Si4'
_chemical_formula_weight         2707.08
_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             2019-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-29 deposited with the CCDC.	2020-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                74.2830(10)
_cell_angle_beta                 77.959(2)
_cell_angle_gamma                68.381(2)
_cell_formula_units_Z            4
_cell_length_a                   18.8621(3)
_cell_length_b                   25.0420(3)
_cell_length_c                   34.0452(6)
_cell_measurement_reflns_used    49947
_cell_measurement_temperature    169.99(13)
_cell_measurement_theta_max      74.5190
_cell_measurement_theta_min      3.4650
_cell_volume                     14284.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_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    -71.00 -24.00   0.25    0.60    --  -46.95 -77.00-120.00  188
  2  \w   -117.00 -47.00   0.25    0.60    --  -46.95-165.00-162.00  280
  3  \w   -113.00 -74.00   0.25    4.00    --  -99.00-165.00-162.00  156
  4  \w   -118.00 -84.00   0.25    0.60    --  -46.95 -77.00-120.00  136
  5  \w   -145.00-112.00   0.25    4.00    --  -99.00-116.00 -15.00  132
  6  \w   -155.00 -82.00   0.25    4.00    --  -99.00 -61.00  60.00  292
  7  \w   -102.00 -75.00   0.25    0.60    --  -46.95-125.00  60.00  108
  8  \w   -116.00 -25.00   0.25    0.60    --  -46.95 -77.00   0.00  364
  9  \w     33.00  61.00   0.25    0.60    --   46.95-116.00 -15.00  112
 10  \w     32.00 112.00   0.25    4.00    --  103.25-116.00 -15.00  320
 11  \w     88.00 113.00   0.25    4.00    --  103.25 -45.00 -60.00  100
 12  \w     43.00 120.00   0.25    4.00    --  103.25 -61.00 -30.00  308
 13  \w    117.00 168.00   0.25    4.00    --  103.25  15.00  90.00  204
 14  \w    117.00 143.00   0.25    4.00    --  103.25 116.00  73.00  104
 15  \w     51.00 115.00   0.25    0.60    --   46.95 165.00-139.00  256
 16  \w     49.00  75.00   0.25    0.60    --   46.95  57.00-180.00  104
 17  \w     83.00 115.00   0.25    0.60    --   46.95  57.00-180.00  128
 18  \w     92.00 151.00   0.25    4.00    --  103.25  30.00-180.00  236
 19  \w    134.00 169.00   0.25    4.00    --  103.25  45.00-180.00  140
 20  \w     38.00  90.00   0.25    4.00    --  103.25 -45.00  60.00  208
 21  \w     38.00 119.00   0.25    4.00    --  103.25 -61.00 150.00  324
 22  \w     32.00  97.00   0.25    4.00    --  103.25 -77.00 -30.00  260
 23  \w     55.00  80.00   0.25    0.60    --   46.95-165.00-162.00  100
 24  \w     37.00 145.00   0.25    4.00    --  103.25-165.00-162.00  432
 25  \w     33.00 109.00   0.25    4.00    --  103.25 -94.00-180.00  304
 26  \w    -89.00  -8.00   0.25    0.60    --  -46.95 116.00  73.00  324
 27  \w   -119.00 -83.00   0.25    0.60    --  -46.95-125.00  30.00  144
 28  \w   -156.00 -87.00   0.25    4.00    --  -99.00 -30.00  60.00  276
 29  \w   -111.00 -27.00   0.25    4.00    --  -99.00  45.00 -60.00  336
 30  \w   -105.00 -70.00   0.25    4.00    --  -99.00 116.00  73.00  140
 31  \w   -117.00 -69.00   0.25    4.00    --  -99.00 125.00  30.00  192
 32  \w   -122.00 -27.00   0.25    4.00    --  -99.00  77.00 -90.00  380
 33  \w   -108.00 -75.00   0.25    0.60    --  -46.95 165.00-139.00  132
 34  \w   -111.00 -86.00   0.25    4.00    --  -99.00 165.00-139.00  100
 35  \w   -167.00 -89.00   0.25    4.00    --  -99.00 -30.00 -30.00  312
 36  \w   -158.00-123.00   0.25    4.00    --  -99.00-165.00-162.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0185305000
_diffrn_orient_matrix_UB_12      -0.0033612000
_diffrn_orient_matrix_UB_13      -0.0410667000
_diffrn_orient_matrix_UB_21      0.0719312000
_diffrn_orient_matrix_UB_22      0.0155732000
_diffrn_orient_matrix_UB_23      -0.0224698000
_diffrn_orient_matrix_UB_31      0.0481338000
_diffrn_orient_matrix_UB_32      -0.0658342000
_diffrn_orient_matrix_UB_33      0.0071800000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            56672
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.721
_diffrn_reflns_theta_min         2.119
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.152
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       needle
_exptl_crystal_F_000             5696
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.608
_refine_diff_density_min         -1.356
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3457
_refine_ls_number_reflns         56672
_refine_ls_number_restraints     1352
_refine_ls_restrained_S_all      1.965
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.1103
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2929
_refine_ls_wR_factor_ref         0.3159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38006
_reflns_number_total             56672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03744c2.cif
_cod_data_source_block           tx667_tw
_cod_database_code               1559105
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOSiBr
_chemical_oxdiff_usercomment     CHNOSiBr
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.670(4)
 0.330(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C86-C85 = C87-C86 = C87-C88 = C88-C89 = C90-C89 = C90-C91 = C92-C91 = C98-C97
 = C99-C98 = C99-C100
 1.54 with sigma of 0.02
 C94A-C93A = C95A-C94A = C95A-C96A = C96A-C97A = C98A-C97A = C98A-C99A = C2Q-
 C99A = C88A-C87A = C88A-C89A = C90A-C89A = C91A-C90A = C92A-C91A = C20A-C19A =
 C21A-C20A = C19A-C18A = C27A-C26A = C27A-C28A = C26A-C25A = C29A-C28A = C30A-
 C29A
 1.54 with sigma of 0.02
 C21A-C22A
 1.54 with sigma of 0.02
 C155-C160 = C160-C159 = C158-C159 = C157-C158 = C157-C156 = C155-C156 = C153-
 C148 = C149-C148 = C150-C149 = C150-C151 = C152-C151 = C152-C153 = C162-C167 =
 C162-C163 = C167-C166 = C165-C166 = C165-C164 = C164-C163
 1.39 with sigma of 0.01
 C55A-C54A = C2P-C2I = C67A-C65A
 1.54 with sigma of 0.02
 C2K-C4BA = C6AA-C5AA = C2M-C4BA = C7AA-C5AA = C2N-C2S = C2N-C2R = C126-C124 =
 C125-C124 = C2T-C122 = C3AA-C2F = C2U-C2T = C4AA-C3AA
 1.54 with sigma of 0.01
 C8AA-C0BA = C9AA-C8AA = C53-C51 = C52-C51 = C3BA-C1BA = C55-C54 = C2BA-C1BA =
 C56-C54
 1.54 with sigma of 0.01
 Si4-C57 = Si4-C0AA
 1.87 with sigma of 0.01
 C2AA-C0AA = C59-C57 = C1AA-C0AA = C58-C57
 1.54 with sigma of 0.01
 C5BA-C2C = C98-C5BA
 1.54 with sigma of 0.01
 C155-C161 = C154-C148 = C168-C162
 1.51 with sigma of 0.01
 C90-C92
 2.5 with sigma of 0.02
 C148-C152
 2.4 with sigma of 0.02
 C3BA-C2BA
 2.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C91 \\sim C92:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C96 \\sim C97 \\sim C98 \\sim C99 \\sim C100 \\sim C2C \\sim C5BA: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
C85A \\sim C86A \\sim C87A \\sim C88A \\sim C89A \\sim C90A \\sim C91A \\sim
C92A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C2Q \\sim C93A \\sim C94A \\sim C95A \\sim C96A \\sim C97A \\sim C98A \\sim
C99A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim C30A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C18A \\sim C19A \\sim C20A \\sim C21A \\sim C22A: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166 \\sim C167 \\sim C168: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C3AA \\sim C4AA \\sim C2F \\sim C2T \\sim C2U \\sim C122 \\sim C124 \\sim C125
\\sim C126 \\sim C2N \\sim C2R \\sim C2S \\sim C2K \\sim C2M \\sim C4BA \\sim
C5AA \\sim C6AA \\sim C7AA: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C2AA \\sim C59 \\sim C0AA \\sim C57 \\sim C58 \\sim C1AA: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
C51 \\sim C52 \\sim C53 \\sim C57 \\sim C58 \\sim C59 \\sim C0AA \\sim C1AA
\\sim C2AA \\sim C8AA \\sim C9AA \\sim C0BA \\sim C54 \\sim C55 \\sim C56 \\sim
C1BA \\sim C2BA \\sim C3BA: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C155 \\sim C156 \\sim C157 \\sim C158 \\sim C159 \\sim C160 \\sim C161: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
C148 \\sim C149 \\sim C150 \\sim C151 \\sim C152 \\sim C153 \\sim C154: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C88)
\\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C92) \\sim Ueq,
Uanis(C90) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq, Uanis(C100)
\\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C95) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C87A) \\sim Ueq, Uanis(C89A) \\sim Ueq, Uanis(C88A) \\sim Ueq,
Uanis(C90A) \\sim Ueq, Uanis(C91A) \\sim Ueq, Uanis(C92A) \\sim Ueq,
Uanis(C86A) \\sim Ueq, Uanis(C94A) \\sim Ueq, Uanis(C97A) \\sim Ueq,
Uanis(C99A) \\sim Ueq, Uanis(C96A) \\sim Ueq, Uanis(C98A) \\sim Ueq,
Uanis(C95A) \\sim Ueq, Uanis(C2Q) \\sim Ueq, Uanis(C28A) \\sim Ueq, Uanis(C26A)
\\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C27A) \\sim Ueq, Uanis(C30A) \\sim Ueq,
Uanis(C19A) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C21A) \\sim Ueq,
Uanis(C22A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C124) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(C2N)
\\sim Ueq, Uanis(C2K) \\sim Ueq, Uanis(C2M) \\sim Ueq, Uanis(C4BA) \\sim Ueq,
Uanis(C5AA) \\sim Ueq, Uanis(C6AA) \\sim Ueq, Uanis(C7AA) \\sim Ueq, Uanis(C2S)
\\sim Ueq, Uanis(C2R) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C4AA) \\sim Ueq,
Uanis(C2F) \\sim Ueq, Uanis(C2T) \\sim Ueq, Uanis(C2U) \\sim Ueq, Uanis(C122)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C1BA)
\\sim Ueq, Uanis(C2BA) \\sim Ueq, Uanis(C3BA) \\sim Ueq, Uanis(C51) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C1AA) \\sim Ueq,
Uanis(C2AA) \\sim Ueq, Uanis(C8AA) \\sim Ueq, Uanis(C9AA) \\sim Ueq,
Uanis(C0BA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2C) \\sim Ueq, Uanis(C5BA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C157) \\sim Ueq, Uanis(C156) \\sim Ueq, Uanis(C155) \\sim Ueq,
Uanis(C158) \\sim Ueq, Uanis(C160) \\sim Ueq, Uanis(C161) \\sim Ueq,
Uanis(C159) \\sim Ueq, Uanis(C154) \\sim Ueq, Uanis(C148) \\sim Ueq,
Uanis(C153) \\sim Ueq, Uanis(C149) \\sim Ueq, Uanis(C152) \\sim Ueq,
Uanis(C150) \\sim Ueq, Uanis(C151) \\sim Ueq, Uanis(C165) \\sim Ueq,
Uanis(C163) \\sim Ueq, Uanis(C164) \\sim Ueq, Uanis(C162) \\sim Ueq,
Uanis(C167) \\sim Ueq, Uanis(C168) \\sim Ueq, Uanis(C166) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C0AA)=Sof(H0AA)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2AA)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C8AA)=Sof(H8AA)=Sof(C9AA)=Sof(H9AA)=
 Sof(H9AB)=Sof(H9AC)=Sof(C0BA)=Sof(H0BA)=Sof(H0BB)=Sof(H0BC)=Sof(C1BA)=
 Sof(H1BA)=Sof(C2BA)=Sof(H2BC)=Sof(H2BD)=Sof(H2BE)=Sof(C3BA)=Sof(H3BA)=
 Sof(H3BB)=Sof(H3BC)=1-FVAR(1)
 Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C53)=Sof(H53A)=
 Sof(H53B)=Sof(H53C)=Sof(C54)=Sof(H54)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=
 Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(H58C)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(1)
 Sof(C3AA)=Sof(H3AA)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=Sof(C2F)=
 Sof(H2FA)=Sof(H2FB)=Sof(H2FC)=Sof(C2N)=Sof(H2N)=Sof(C2R)=Sof(H2RA)=Sof(H2RB)=
 Sof(H2RC)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=Sof(C5AA)=Sof(H5AA)=Sof(C6AA)=
 Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7AA)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=1-FVAR(2)
 Sof(C2K)=Sof(H2KA)=Sof(H2KB)=Sof(H2KC)=Sof(C2M)=Sof(H2MA)=Sof(H2MB)=Sof(H2MC)=
 Sof(C4BA)=Sof(H4BA)=Sof(C124)=Sof(H124)=Sof(C125)=Sof(H12J)=Sof(H12K)=
 Sof(H12L)=Sof(C126)=Sof(H12M)=Sof(H12N)=Sof(H12O)=Sof(C2T)=Sof(H2T)=Sof(C2U)=
 Sof(H2UA)=Sof(H2UB)=Sof(H2UC)=Sof(C122)=Sof(H12P)=Sof(H12Q)=Sof(H12R)=FVAR(2)
 Sof(H98C)=Sof(H98D)=Sof(C2C)=Sof(H2CA)=Sof(H2CB)=Sof(H2CC)=Sof(C5BA)=
 Sof(H5BA)=Sof(H5BB)=1-FVAR(3)
 Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(C100)=Sof(H10A)=
 Sof(H10B)=Sof(H10C)=FVAR(3)
 Fixed X: C154(0.904169)
6.a Riding coordinates:
 C161(H16C,H16D,H16E), C168(H16F,H16G,H16H), C1AA(H1AA,H1AB,H1AC), C0BA(H0BA,
 H0BB,H0BC)
6.b Ternary CH refined with riding coordinates:
 C1G(H1G), C1Z(H1Z), C2I(H2I), C33(H33), C36(H36), C51(H51), C54(H54),
 C57(H57), C63(H63), C65(H65), C68(H68), C106(H106), C121(H121), C127(H127),
 C132(H132), C135(H135), C1U(H1U), C1W(H1W), C3AA(H3AA), C6(H6), C4BA(H4BA),
 C33A(H33A), C36A(H36A), C51A(H51A), C54A(H54A), C57A(H57A), C63A(H63A),
 C65A(H65A), C68A(H68A), C103(H103), C124(H124), C138(H138), C0AA(H0AA),
 C2N(H2N), C2T(H2T), C5AA(H5AA), C8AA(H8AA), C1BA(H1BA)
6.c Secondary CH2 refined with riding coordinates:
 C1D(H1DA,H1DB), C1Q(H1QA,H1QB), C1R(H1RA,H1RB), C1Y(H1YA,H1YB), C2B(H2BA,
 H2BB), C29(H29A,H29B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
  C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,
 H89B), C90(H90A,H90B), C91(H91A,H91B), C93(H93A,H93B), C94(H94A,H94B),
 C95(H95A,H95B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C98(H98C,H98D),
  C99(H99A,H99B), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A,H17B), C18A(H18A,
 H18B), C19A(H19A,H19B), C20A(H20C,H20D), C21A(H21D,H21E), C23A(H23C,H23D),
 C24A(H24C,H24D), C25A(H25C,H25D), C26A(H26C,H26D), C27A(H27C,H27D), C28A(H28C,
 H28D), C29A(H29C,H29D), C85A(H85C,H85D), C86A(H86C,H86D), C87A(H87C,H87D),
 C88A(H88C,H88D), C89A(H89C,H89D), C90A(H90C,H90D), C91A(H91C,H91D), C93A(H93C,
 H93D), C94A(H94C,H94D), C95A(H95C,H95D), C96A(H96C,H96D), C97A(H97C,H97D),
 C98A(H98E,H98F), C99A(H99C,H99D), C5BA(H5BA,H5BB)
6.d Aromatic/amide H refined with riding coordinates:
 C1J(H1J), C1N(H1N), C1S(H1S), C39(H39), C41(H41), C42(H42), C43(H43),
 C44(H44), C46(H46), C111(H111), C113(H113), C114(H114), C1P(H1P), C1T(H1T),
 C1V(H1V), C39A(H39A), C41A(H41A), C42A(H42A), C43A(H43A), C44A(H44A),
 C46A(H46A), C109(H109), C112(H112), C116(H116), C142(H142), C143(H143),
 C144(H144), C145(H145), C146(H146), C149(H149), C150(H150), C151(H151),
 C152(H152), C153(H153), C156(H156), C157(H157), C158(H158), C159(H159),
 C160(H160), C163(H163), C164(H164), C165(H165), C166(H166), C167(H167)
6.e Idealised Me refined as rotating group:
 C2E(H2EA,H2EB,H2EC), C2H(H2HA,H2HB,H2HC), C2J(H2JA,H2JB,H2JC), C2O(H2OA,H2OB,
 H2OC), C2P(H2PA,H2PB,H2PC), C30(H30A,H30B,H30C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C92(H92A,
 H92B,H92C), C100(H10A,H10B,H10C), C123(H12A,H12B,H12C), C128(H12D,H12E,H12F),
 C129(H12G,H12H,H12I), C133(H13A,H13B,H13C), C134(H13D,H13E,H13F), C136(H13G,
 H13H,H13I), C137(H13J,H13K,H13L), C139(H13M,H13N,H13O), C1X(H1XA,H1XB,H1XC),
 C2D(H2DA,H2DB,H2DC), C2G(H2GA,H2GB,H2GC), C2K(H2KA,H2KB,H2KC), C2L(H2LA,H2LB,
 H2LC), C2M(H2MA,H2MB,H2MC), C4AA(H4AA,H4AB,H4AC), C2Q(H2QA,H2QB,H2QC),
 C21(H21A,H21B,H21C), C22A(H22C,H22D,H22E), C30A(H30D,H30E,H30F), C52A(H52D,
 H52E,H52F), C53A(H53D,H53E,H53F), C55A(H55D,H55E,H55F), C56A(H56D,H56E,H56F),
 C58A(H58D,H58E,H58F), C59A(H59D,H59E,H59F), C62A(H62D,H62E,H62F), C64A(H64D,
 H64E,H64F), C66A(H66D,H66E,H66F), C67A(H67D,H67E,H67F), C69A(H69D,H69E,H69F),
 C70A(H70D,H70E,H70F), C92A(H92D,H92E,H92F), C2F(H2FA,H2FB,H2FC), C125(H12J,
 H12K,H12L), C126(H12M,H12N,H12O), C140(H14A,H14B,H14C), C147(H14D,H14E,H14F),
 C154(H15C,H15D,H15E), C2AA(H2AA,H2AB,H2AC), C2R(H2RA,H2RB,H2RC), C2S(H2SA,H2SB,
 H2SC), C2U(H2UA,H2UB,H2UC), C122(H12P,H12Q,H12R), C6AA(H6AA,H6AB,H6AC),
 C7AA(H7AA,H7AB,H7AC), C9AA(H9AA,H9AB,H9AC), C2BA(H2BC,H2BD,H2BE), C3BA(H3BA,
 H3BB,H3BC), C2C(H2CA,H2CB,H2CC)
;
_shelx_res_checksum              46109
_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 2.937
_oxdiff_exptl_absorpt_empirical_full_min 0.368