Conformational flexibility of hybrid [3]- and [4]-rotaxanes.
Lockyer, Selena J.; Nawaz, Selina; Brookfield, Adam; Fielding, Alistair J.; Vitorica-Yrezabal, Inigo J; Timco, Grigore A.; Burton, Neil A.; Bowen, Alice M.; Winpenny, Richard E. P.; McInnes, Eric J. L.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c06547

data_4135221
_publ_section_title
;
 Conformational flexibility of hybrid [3]- and [4]-rotaxanes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c06547
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety
'2(C80 H144 Cr7 F8 Ni O32), C64 H100 Cr F N4 Ni2 O13 S2'
_chemical_formula_sum            'C224 H388 Cr15 F17 N4 Ni4 O77 S2'
_chemical_formula_weight         5771.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.2999(14)
_cell_length_b                   32.5605(13)
_cell_length_c                   34.8099(18)
_cell_measurement_reflns_used    11803
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      33.5550
_cell_measurement_theta_min      1.8460
_cell_volume                     34343(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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_temperature      150.00(10)
_diffrn_measured_fraction_theta_full 0.179
_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    -75.00 -48.00   1.00    7.12    --    5.00  17.00-163.00   27
  2  \w     17.00  44.00   1.00    7.12    --  -34.00 -17.00  27.00   27
  3  \w    -17.00   8.00   1.00    7.12    --  -34.00 -17.00  27.00   25
  4  \w    -19.00   6.00   1.00    7.12    --    5.00 -17.00  27.00   25
  5  \w   -122.00  -7.00   1.00    7.12    --  -34.00 -76.00-120.00  115
  6  \w   -122.00  -5.00   1.00    7.12    --  -34.00 -38.00 -60.00  117
  7  \w    -58.00  32.00   1.00    7.12    --  -34.00  57.00   0.00   90
  8  \w    -23.00   4.00   1.00    7.12    --  -34.00  57.00 -60.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_Laue_measured_fraction_full 0.179
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40232
_diffrn_reflns_point_group_measured_fraction_full 0.171
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         30.924
_diffrn_reflns_theta_min         1.858
_exptl_absorpt_coefficient_mu    4.676
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       needle
_exptl_crystal_F_000             12132
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.122
_refine_ls_abs_structure_details
;
 Flack x determined using 3351 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.205(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1420
_refine_ls_number_reflns         10652
_refine_ls_number_restraints     10842
_refine_ls_restrained_S_all      1.432
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.1808
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_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          0.4311
_refine_ls_wR_factor_ref         0.4414
_reflns_Friedel_coverage         0.816
_reflns_Friedel_fraction_full    0.163
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8991
_reflns_number_total             10652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c06547_si_002.cif
_cod_data_source_block           rrepw187
_cod_database_code               4135221
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.706
_shelx_estimated_absorpt_t_min   0.388
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C8-C1
 2.4 with sigma of 0.02
 O2-C9 = O2-C1O
 1.436 with sigma of 0.002
 O2-C1G = O2-C1N
 2.375 with sigma of 0.002
 C9-C1G = C1N-C1O
 1.532 with sigma of 0.002
 C9-C1N = C1G-C1O
 2.38 with sigma of 0.002
 C1G-C1N
 1.536 with sigma of 0.002
 C2_73-C1_73
 C2_74-C1_74
 C2_75-C1_75
 C2_76-C1_76
 C2_77-C1_77
 C2_78-C1_78
 C2_79-C1_79
 C2_80-C1_80
 C2_81-C1_81
 C2_82-C1_82
 C2_83-C1_83
 C2_84-C1_84
 C2_85-C1_85
 C2_86-C1_86
 C2_87-C1_87
 C2_88-C1_88
 C2_89-C1_89
 C2_90-C1_90
 C2_92-C1_92
 C2_93-C1_93
 C2_94-C1_94
 C2_95-C1_95
 C2_96-C1_96
 C2_97-C1_97
 C2_98-C1_98
 C2_99-C1_99
 C2_100-C1_100
 C2_101-C1_101
 C2_102-C1_102
 C2_103-C1_103
 C2_104-C1_104
 C2_105-C1_105
 C2_106-C1_106
 C2_107-C1_107
 C2_108-C1_108
 C2_109-C1_109
 C2_110-C1_110
 C2_91-C1_91
 1.54 with sigma of 0.02
 C1M-C1C
 1.45 with sigma of 0.02
 C2-C17
 2.4 with sigma of 0.02
 C1M-C17
 1.54 with sigma of 0.02
 N1-C7
 2.4 with sigma of 0.02
 C1I-C18 \\sim C18-C1L
 with sigma of 0.002
 C1E-Ni18 \\sim Ni18-C1A
 with sigma of 0.02
 C1B-C1M \\sim C1M-C1D
 with sigma of 0.02
 C2-C14 \\sim C1M-C1C \\sim C1H-C18 \\sim C7-C1
 with sigma of 0.002
 N9-C17 \\sim N9-C2 \\sim N1-C8 \\sim N1-C1
 with sigma of 0.002
 C1M-C17 \\sim C8-C18
 with sigma of 0.002
3. Restrained planarity
 O2_73, C1_73, O1_73, C2_73
 O2_74, C1_74, O1_74, C2_74
 O2_75, C1_75, O1_75, C2_75
 O2_76, C1_76, O1_76, C2_76
 O2_77, C1_77, O1_77, C2_77
 O2_78, C1_78, O1_78, C2_78
 O2_79, C1_79, O1_79, C2_79
 O2_80, C1_80, O1_80, C2_80
 O2_81, C1_81, O1_81, C2_81
 O2_82, C1_82, O1_82, C2_82
 O2_83, C1_83, O1_83, C2_83
 O2_84, C1_84, O1_84, C2_84
 O2_85, C1_85, O1_85, C2_85
 O2_86, C1_86, O1_86, C2_86
 O2_87, C1_87, O1_87, C2_87
 O2_88, C1_88, O1_88, C2_88
 O2_89, C1_89, O1_89, C2_89
 O2_90, C1_90, O1_90, C2_90
 O2_92, C1_92, O1_92, C2_92
 O2_93, C1_93, O1_93, C2_93
 O2_94, C1_94, O1_94, C2_94
 O2_95, C1_95, O1_95, C2_95
 O2_96, C1_96, O1_96, C2_96
 O2_97, C1_97, O1_97, C2_97
 O2_98, C1_98, O1_98, C2_98
 O2_99, C1_99, O1_99, C2_99
 O2_100, C1_100, O1_100, C2_100
 O2_101, C1_101, O1_101, C2_101
 O2_102, C1_102, O1_102, C2_102
 O2_103, C1_103, O1_103, C2_103
 O2_104, C1_104, O1_104, C2_104
 O2_105, C1_105, O1_105, C2_105
 O2_106, C1_106, O1_106, C2_106
 O2_107, C1_107, O1_107, C2_107
 O2_108, C1_108, O1_108, C2_108
 O2_109, C1_109, O1_109, C2_109
 O2_110, C1_110, O1_110, C2_110
 O2_91, C1_91, O1_91, C2_91
 with sigma of 0.1
 C18, C1H, C1I, C1L, C1K, N4, C1J
 with sigma of 0.1
 C1A, C1B, C1C, C1D, C1E, N3, C1M
 with sigma of 0.1
 C1, C7, C0AA, C6, C5, C4, C3
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O2 \\sim C9 \\sim C1G \\sim C1N \\sim C1O: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C5_73 \\sim C4_73 \\sim C3_73 \\sim C2_73 \\sim C5_74 \\sim C4_74 \\sim C3_74
\\sim C2_74 \\sim C5_75 \\sim C4_75 \\sim C3_75 \\sim C2_75 \\sim C5_76 \\sim
C4_76 \\sim C3_76 \\sim C2_76 \\sim C5_77 \\sim C4_77 \\sim C3_77 \\sim C2_77
\\sim C5_78 \\sim C4_78 \\sim C3_78 \\sim C2_78 \\sim C5_79 \\sim C4_79 \\sim
C3_79 \\sim C2_79 \\sim C5_80 \\sim C4_80 \\sim C3_80 \\sim C2_80 \\sim C5_81
\\sim C4_81 \\sim C3_81 \\sim C2_81 \\sim C5_82 \\sim C4_82 \\sim C3_82 \\sim
C2_82 \\sim C5_83 \\sim C4_83 \\sim C3_83 \\sim C2_83 \\sim C5_84 \\sim C4_84
\\sim C3_84 \\sim C2_84 \\sim C5_85 \\sim C4_85 \\sim C3_85 \\sim C2_85 \\sim
C5_86 \\sim C4_86 \\sim C3_86 \\sim C2_86 \\sim C5_87 \\sim C4_87 \\sim C3_87
\\sim C2_87 \\sim C5_88 \\sim C4_88 \\sim C3_88 \\sim C2_88 \\sim C5_89 \\sim
C4_89 \\sim C3_89 \\sim C2_89 \\sim C5_90 \\sim C4_90 \\sim C3_90 \\sim C2_90
\\sim C5_92 \\sim C4_92 \\sim C3_92 \\sim C2_92 \\sim C5_93 \\sim C4_93 \\sim
C3_93 \\sim C2_93 \\sim C5_94 \\sim C4_94 \\sim C3_94 \\sim C2_94 \\sim C5_95
\\sim C4_95 \\sim C3_95 \\sim C2_95 \\sim C5_96 \\sim C4_96 \\sim C3_96 \\sim
C2_96 \\sim C5_97 \\sim C4_97 \\sim C3_97 \\sim C2_97 \\sim C5_98 \\sim C4_98
\\sim C3_98 \\sim C2_98 \\sim C5_99 \\sim C4_99 \\sim C3_99 \\sim C2_99 \\sim
C5_100 \\sim C4_100 \\sim C3_100 \\sim C2_100 \\sim C5_101 \\sim C4_101 \\sim
C3_101 \\sim C2_101 \\sim C5_102 \\sim C4_102 \\sim C3_102 \\sim C2_102 \\sim
C5_103 \\sim C4_103 \\sim C3_103 \\sim C2_103 \\sim C5_104 \\sim C4_104 \\sim
C3_104 \\sim C2_104 \\sim C5_105 \\sim C4_105 \\sim C3_105 \\sim C2_105 \\sim
C5_106 \\sim C4_106 \\sim C3_106 \\sim C2_106 \\sim C5_107 \\sim C4_107 \\sim
C3_107 \\sim C2_107 \\sim C5_108 \\sim C4_108 \\sim C3_108 \\sim C2_108 \\sim
C5_109 \\sim C4_109 \\sim C3_109 \\sim C2_109 \\sim C5_110 \\sim C4_110 \\sim
C3_110 \\sim C2_110 \\sim C5_91 \\sim C4_91 \\sim C3_91 \\sim C2_91: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
C1_91 \\sim C2_91: within 2A with sigma of 0.005 and sigma for terminal atoms
of 0.01
C1_75 \\sim C2_75: within 2A with sigma of 0.005 and sigma for terminal atoms
of 0.01
N4 \\sim C1K \\sim C1H \\sim C1L \\sim C1I \\sim C1J: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C18 \\sim C8 \\sim N1 \\sim C1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C7 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C0AA: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
C12 \\sim C13 \\sim C11 \\sim C10 \\sim C15 \\sim C14: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C2 \\sim C14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
N9 \\sim C1M \\sim C1C \\sim C1D \\sim C1E \\sim N3 \\sim C1A \\sim C1B: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01
N9 \\sim C17 \\sim C1M \\sim C2: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O1_99 \\sim C1_99 \\sim O2_99: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C1_86 \\sim O2_86 \\sim O1_86 \\sim C2_86: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C1_109 \\sim C2_109 \\sim C4_109 \\sim C5_109 \\sim C3_109 \\sim O1_109 \\sim
O2_109: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C2_94 \\sim C5_94 \\sim C3_94 \\sim C4_94 \\sim C1_94 \\sim O2_94 \\sim O1_94:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N4, C1J, C1H, C1L, C1K, C1I, C18, C8, N1, C1, C7, C6, C0AA, C3, C5, C4, S3, C19
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C1E, C1D, C1A, C1B, C1C, C1M, C17, N9, C2, C14, C13, C12, C11, C10, C15,
 S2, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{O1_74, O2_74, C1_74, C2_74, C3_74, C4_74, C5_74}
{O1_75, O2_75, C1_75, C2_75, C3_75, C4_75, C5_75}
{O1_76, O2_76, C1_76, C2_76, C3_76, C4_76, C5_76}
{O1_77, O2_77, C1_77, C2_77, C3_77, C4_77, C5_77}
{O1_78, O2_78, C1_78, C2_78, C3_78, C4_78, C5_78}
{O1_79, O2_79, C1_79, C2_79, C3_79, C4_79, C5_79}
{O1_80, O2_80, C1_80, C2_80, C3_80, C4_80, C5_80}
{O1_81, O2_81, C1_81, C2_81, C3_81, C4_81, C5_81}
{O1_82, O2_82, C1_82, C2_82, C3_82, C4_82, C5_82}
{O1_83, O2_83, C1_83, C2_83, C3_83, C4_83, C5_83}
{O1_84, O2_84, C1_84, C2_84, C3_84, C4_84, C5_84}
{O1_85, O2_85, C1_85, C2_85, C3_85, C4_85, C5_85}
{O1_86, O2_86, C1_86, C2_86, C3_86, C4_86, C5_86}
{O1_87, O2_87, C1_87, C2_87, C3_87, C4_87, C5_87}
{O1_88, O2_88, C1_88, C2_88, C3_88, C4_88, C5_88}
{O1_89, O2_89, C1_89, C2_89, C3_89, C4_89, C5_89}
{O1_90, O2_90, C1_90, C2_90, C3_90, C4_90, C5_90}
{O1_92, O2_92, C1_92, C2_92, C3_92, C4_92, C5_92}
{O1_93, O2_93, C1_93, C2_93, C3_93, C4_93, C5_93}
{O1_94, O2_94, C1_94, C2_94, C3_94, C4_94, C5_94}
{O1_95, O2_95, C1_95, C2_95, C3_95, C4_95, C5_95}
{O1_96, O2_96, C1_96, C2_96, C3_96, C4_96, C5_96}
{O1_97, O2_97, C1_97, C2_97, C3_97, C4_97, C5_97}
{O1_98, O2_98, C1_98, C2_98, C3_98, C4_98, C5_98}
{O1_99, O2_99, C1_99, C2_99, C3_99, C4_99, C5_99}
{O1_100, O2_100, C1_100, C2_100, C3_100, C4_100, C5_100}
{O1_101, O2_101, C1_101, C2_101, C3_101, C4_101, C5_101}
{O1_102, O2_102, C1_102, C2_102, C3_102, C4_102, C5_102}
{O1_103, O2_103, C1_103, C2_103, C3_103, C4_103, C5_103}
{O1_104, O2_104, C1_104, C2_104, C3_104, C4_104, C5_104}
{O1_105, O2_105, C1_105, C2_105, C3_105, C4_105, C5_105}
{O1_106, O2_106, C1_106, C2_106, C3_106, C4_106, C5_106}
{O1_107, O2_107, C1_107, C2_107, C3_107, C4_107, C5_107}
{O1_108, O2_108, C1_108, C2_108, C3_108, C4_108, C5_108}
{O1_109, O2_109, C1_109, C2_109, C3_109, C4_109, C5_109}
{O1_110, O2_110, C1_110, C2_110, C3_110, C4_110, C5_110}
{O1_91, O2_91, C1_91, C2_91, C3_91, C4_91, C5_91}
as
{O1_73, O2_73, C1_73, C2_73, C3_73, C4_73, C5_73} sigma for 1-2: 0.02 1-3: 0.04
7.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C2(H2A,H2B), C1(H1C,H1D), C8(H8A,H8B), N9(H9A,H9B), C17(H17A,
 H17B), C18(H18A,H18B), C1M(H1MA,H1MB), C9(H9C,H9D), C1G(H1GA,H1GB), C1N(H1NA,
 H1NB), C1O(H1OA,H1OB)
7.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,
 H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C5(H5A,H5B,H5C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
7.c Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C3(H3), C5(H5), C6(H6), C10(H10), C12(H12), C13(H13), C15(H15),
 C1A(H1AA), C1B(H1BA), C1D(H1DA), C1E(H1E), C1I(H1I), C1J(H1J), C1K(H1K),
 C1L(H1L)
7.d Fitted hexagon refined as free rotating group:
 C0AA(C3,C4,C5,C6,C7), C10(C11,C12,C13,C14,C15), C1A(C1B,C1C,C1D,C1E,N3),
 C1H(C1I,C1J,N4,C1K,C1L)
;
_shelx_res_checksum              46138
_shelx_hkl_checksum              64077
_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
;