Metal‒organic tube or layered assembly: reversible sheet-to-tube transformation and adaptive recognition
Tian, Jiayue; Liu, Luyao; Zhou, Kang; Hong, Zixiao; Chen, Qihui; Jiang, Feilong; Yuan, Daqiang; Sun, Qingfu; Hong, Maochun; Chemical Science 11 (2020) 9818–9826; doi:10.1039/D0SC01176B

data_1558838
_publ_section_title
;
 Metal--organic tube or layered assembly: reversible sheet-to-tube
 transformation and adaptive recognition
;
_journal_issue                   36
_journal_name_full               'Chemical Science'
_journal_page_first              9818
_journal_page_last               9826
_journal_paper_doi               10.1039/D0SC01176B
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C40 H42 Br6 N6 O6 Zn3, 4(C4 H8 O2)'
_chemical_formula_sum            'C56 H74 Br6 N6 O14 Zn3'
_chemical_formula_weight         1730.78
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-29 deposited with the CCDC.	2020-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.659(3)
_cell_length_b                   13.6267(18)
_cell_length_c                   32.010(2)
_cell_measurement_reflns_used    55460
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      60.0290
_cell_measurement_theta_min      2.3800
_cell_volume                     6830.3(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.59a (Rigaku OD, 2019)'
_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      99.9(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -82.00  26.00   0.50    0.10    --   -1.41 -19.00 -84.00  216
  2  \w     44.00 156.00   0.50    0.40    --   75.22  19.00  82.00  224
  3  \w   -159.00 -47.00   0.50    0.40    --  -78.03 -19.00 -84.00  224
  4  \w    -26.00   3.00   0.50    0.40    --  -78.03  19.00  82.00   58
  5  \w    -26.00  79.00   0.50    0.10    --   -1.41  19.00  82.00  210
  6  \w    -75.00  22.00   0.50    0.10    --   -1.41 -57.00-150.00  194
  7  \w     -8.00  38.00   0.50    0.10    --   -1.41 -99.00 150.00   92
  8  \w     -8.00  38.00   0.50    0.10    --   -1.41 -99.00  30.00   92
  9  \w     -8.00  38.00   0.50    0.10    --   -1.41 -99.00 -60.00   92
 10  \w    -78.00  22.00   0.50    0.10    --   -1.41 -38.00 -30.00  200
 11  \w     -8.00  38.00   0.50    0.10    --   -1.41 -99.00  90.00   92
 12  \w    -78.00  22.00   0.50    0.10    --   -1.41 -38.00 120.00  200
 13  \w    -75.00  28.00   0.50    0.10    --   -1.41 -77.00-120.00  206
 14  \w     -8.00  38.00   0.50    0.10    --   -1.41 -99.00-150.00   92
 15  \w     52.00 149.00   0.50    0.40    --   75.22  57.00   0.00  194
 16  \w     46.00 149.00   0.50    0.40    --   75.22  77.00-150.00  206
 17  \w      1.00 104.00   0.50    0.40    --   75.22 -77.00-180.00  206
 18  \w     45.00 149.00   0.50    0.40    --   75.22  80.00 157.16  208
 19  \w     46.00 149.00   0.50    0.40    --   75.22  77.00  90.00  206
 20  \w     20.00 112.00   0.50    0.40    --   75.22-125.00 -60.00  184
 21  \w     20.00 112.00   0.50    0.40    --   75.22-125.00-120.00  184
 22  \w     20.00 112.00   0.50    0.40    --   75.22-125.00 150.00  184
 23  \w     46.00 149.00   0.50    0.40    --   75.22  77.00-180.00  206
 24  \w     46.00 149.00   0.50    0.40    --   75.22  77.00 150.00  206
 25  \w     46.00 149.00   0.50    0.40    --   75.22  77.00   0.00  206
 26  \w     46.00 149.00   0.50    0.40    --   75.22  77.00  60.00  206
 27  \w     46.00 149.00   0.50    0.40    --   75.22  77.00-120.00  206
 28  \w     46.00 149.00   0.50    0.40    --   75.22  77.00 120.00  206
 29  \w     47.00  73.00   0.50    0.40    --   75.22  75.00 -14.35   52
 30  \w    115.00 148.00   0.50    0.40    --   75.22  77.00  30.00   66
 31  \w     46.00  72.00   0.50    0.40    --   75.22  77.00  30.00   52
 32  \w     46.00 140.00   0.50    0.40    --   75.22  77.00 -60.00  188
 33  \w    109.00 149.00   0.50    0.40    --   75.22 125.00  90.00   80
 34  \w     -4.00  26.00   0.50    0.40    --   75.22 -19.00 -84.00   60
 35  \w      1.00 101.00   0.50    0.40    --   75.22 -99.00 -30.00  200
 36  \w     46.00 139.00   0.50    0.40    --   75.22  77.00 -90.00  186
 37  \w    -42.00  -1.00   0.50    0.40    --  -78.03  38.00  90.00   82
 38  \w    -80.00 -49.00   0.50    0.40    --  -78.03 -77.00  30.00   62
 39  \w    -78.00 -50.00   0.50    0.40    --  -78.03 -74.00 135.26   56
 40  \w   -152.00 -88.00   0.50    0.40    --  -78.03 -74.00 135.26  128
 41  \w   -152.00 -52.00   0.50    0.40    --  -78.03 -72.00-168.33  200
 42  \w    -96.00 -21.00   0.50    0.40    --  -78.03 125.00  90.00  150
 43  \w    -75.00 -49.00   0.50    0.40    --  -78.03 -77.00   0.00   52
 44  \w   -150.00 -50.00   0.50    0.40    --  -78.03 -76.00 112.67  200
 45  \w    -75.00 -49.00   0.50    0.40    --  -78.03 -77.00 -30.00   52
 46  \w    -83.00 -49.00   0.50    0.40    --  -78.03 -77.00-150.00   68
 47  \w   -124.00 -49.00   0.50    0.40    --  -78.03 -77.00-180.00  150
 48  \w   -151.00 -49.00   0.50    0.40    --  -78.03 -77.00  60.00  204
 49  \w    -75.00 -50.00   0.50    0.40    --  -78.03 -75.00-115.26   50
 50  \w   -143.00 -83.00   0.50    0.40    --  -78.03 -75.00-115.26  120
 51  \w    -42.00  -1.00   0.50    0.40    --  -78.03  38.00  30.00   82
 52  \w   -152.00-114.00   0.50    0.40    --  -78.03-125.00  90.00   76
 53  \w   -100.00 -47.00   0.50    0.40    --  -78.03 -81.00 166.88  106
 54  \w   -114.00 -48.00   0.50    0.40    --  -78.03 -79.00  -8.58  132
 55  \w    -74.00 -47.00   0.50    0.40    --  -78.03 -81.00 -74.01   54
 56  \w   -149.00 -48.00   0.50    0.40    --  -78.03 -80.00-121.10  202
 57  \w    -75.00 -49.00   0.50    0.40    --  -78.03 -78.00 -40.56   52
 58  \w   -104.00 -39.00   0.50    0.40    --  -78.03  77.00  60.00  130
 59  \w    -79.00 -50.00   0.50    0.40    --  -78.03 -75.00  80.76   58
 60  \w   -150.00 -96.00   0.50    0.40    --  -78.03 -75.00  80.76  108
 61  \w   -151.00 -79.00   0.50    0.40    --  -78.03 -78.00  15.52  144
 62  \w    -75.00 -49.00   0.50    0.40    --  -78.03 -78.00  15.52   52
 63  \w    -88.00 -49.00   0.50    0.40    --  -78.03 -77.00 -60.00   78
 64  \w   -151.00 -96.00   0.50    0.40    --  -78.03 -77.00 -60.00  110
 65  \w    -98.00 -15.00   0.50    0.40    --  -78.03  77.00 120.00  166
;
_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      -0.0830592000
_diffrn_orient_matrix_UB_12      -0.0403093000
_diffrn_orient_matrix_UB_13      -0.0107951000
_diffrn_orient_matrix_UB_21      0.0477863000
_diffrn_orient_matrix_UB_22      -0.0747146000
_diffrn_orient_matrix_UB_23      0.0001472000
_diffrn_orient_matrix_UB_31      -0.0219594000
_diffrn_orient_matrix_UB_32      -0.0104595000
_diffrn_orient_matrix_UB_33      0.0404002000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.1056
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            230666
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        52.928
_diffrn_reflns_theta_max         52.928
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.929
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.59a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       plate
_exptl_crystal_F_000             3456
_refine_diff_density_max         2.303
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.234
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(14)
_refine_ls_extinction_coef       0.000045(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         11948
_refine_ls_number_restraints     904
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.1275
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+264.7582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2571
_refine_ls_wR_factor_ref         0.2600
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                11060
_reflns_number_total             11948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01176b2.cif
_cod_data_source_block           190927-4
_cod_depositor_comments
'Adding full bibliography for 1558835--1558840.cif.'
_cod_original_cell_volume        6830.2(18)
_cod_database_code               1558838
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O N Zn Br'
_diffrn_oxdiff_digest_frames
;
0112fe5bd17e856d53ce614232041c4f45090088a6f
;
_diffrn_oxdiff_digest_hkl
;
01ec7d7124a29ae5edda82bfc4c06e6e538e9d
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(14)
 0.51(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C42-O12 = C42-C41 = C44-O11 = C44-C43 = O13-C47 = O13-C46 = O14-C45 = O14-C48
 = O6-C29 = O6-C30 = O5-C35 = O5-C36 = O4-C26 = O4-C23 = O2-C15 = O2-C16 = O3-
 C10 = O3-C9 = O1-C3 = O1-C6 = C50-C49 = C50-O7 = C52-O8 = C52-C51 = C54-O10 =
 C54-C53 = C56-O9 = C56-C55
 1.44 with sigma of 0.08
 C49-O8 = O7-C51 = O9-C53 = C55-O10 = C46-C45 = C47-C48 = C41-O11 = O12-C43 =
 C35-C27 = C29-C27 = C26-C27 = C28-C27 = C7-C9 = C7-C6 = C7-C8 = C7-C15
 1.53 with sigma of 0.08
 C44-C43 = C44-O11 = C42-O12 = C42-C41
 1.44 with sigma of 0.08
 C41-O11 = O12-C43
 1.53 with sigma of 0.08
 C42-C41 = C43-C44
 1.53 with sigma of 0.08
 O14-C45 = O14-C48 = O13-C46 = O13-C47 = C42-C41 = C42-O12 = C44-C43 = C44-O11
 1.44 with sigma of 0.08
 C41-O11 = C43-O12 = C46-C45 = C47-C48
 1.53 with sigma of 0.08
 C44-C43 = C42-C41
 1.44 with sigma of 0.08
 O14-C48
 1.46 with sigma of 0.08
 C42-O12
 1.45 with sigma of 0.08
 O12-C43 = O12-C42 = O11-C41 = O11-C44
 1.44 with sigma of 0.08
 C41-C42 = C43-C44
 1.53 with sigma of 0.08
 C46-C45 = C46-O13 = C48-C47 = C48-O14
 1.44 with sigma of 0.08
 O13-C47 = O14-C45
 1.55 with sigma of 0.08
 C46-C45 = C48-C47
 1.42 with sigma of 0.08
 O13-C47
 1.55 with sigma of 0.08
 O3-C10
 1.48 with sigma of 0.08
 O5-C35 = O5-C36
 1.48 with sigma of 0.08
 O2-C16
 1.48 with sigma of 0.08
 O6-C29
 1.4 with sigma of 0.08
 O13-C46 = O14-C45 = O14-C48 = O13-C47
 1.4 with sigma of 0.08
 C47-C48 = C45-C46
 1.6 with sigma of 0.08
 C48-O14 = O14-C45
 1.4 with sigma of 0.08
 C46-C45
 1.6 with sigma of 0.08
 C47-C48
 1.6 with sigma of 0.08
 C48-O14
 1.35 with sigma of 0.08
 O14-C45
 1.35 with sigma of 0.08
 C47-O13
 1.35 with sigma of 0.08
 O6-C30
 1.6 with sigma of 0.08
 O9-C53
 1.45 with sigma of 0.08
 C55-C56
 1.5 with sigma of 0.08
 C53-O9
 1.5 with sigma of 0.08
 O10-C55
 1.5 with sigma of 0.08
 C56-O9
 1.35 with sigma of 0.08
 C16-O2
 1.55 with sigma of 0.08
 O2-C15
 1.35 with sigma of 0.08
 C35-C27
 1.75 with sigma of 0.08
 C36-O5
 1.55 with sigma of 0.08
 C35-O5
 1.3 with sigma of 0.08
 C8-C7
 1.8 with sigma of 0.8
 C6-O1
 1.6 with sigma of 0.8
 C26-C27
 2 with sigma of 0.8
 C27-C29
 1.1 with sigma of 0.8
 C29-O6
 1.1 with sigma of 0.8
 C15-O2
 1.1 with sigma of 0.8
 C9-C7
 1.1 with sigma of 0.8
 C7-C15
 1.2 with sigma of 0.8
 C45-O14
 1.2 with sigma of 0.1
 C27-C35
 2.5 with sigma of 0.1
 C6-C7
 1 with sigma of 0.1
 O1-C6
 2 with sigma of 0.1
 C3-O1
 2 with sigma of 0.1
 O7-C51 = O7-C50 = O8-C52 = O8-C49
 1.4 with sigma of 0.04
 O7-C51 = O8-C49
 1.4 with sigma of 0.04
 O7-C51 = O8-C52
 1.4 with sigma of 0.04
 C50-C49
 1.8 with sigma of 0.04
 O7-C50
 1.5 with sigma of 0.04
 O9-C53 = O9-C56 = O10-C55
 1.4 with sigma of 0.04
 O10-C54
 1.7 with sigma of 0.04
 O10-C54 = O9-C56 = O9-C53
 1.3 with sigma of 0.04
 C56-C55 = C54-C53
 1.8 with sigma of 0.04
 C46-C47
 2.45 with sigma of 0.16
 C42-O11
 2.4 with sigma of 0.16
 C43-O11
 2.4 with sigma of 0.16
 O12-C41
 2.4 with sigma of 0.16
 C44-O12
 2.45 with sigma of 0.16
 C44-C41
 2.45 with sigma of 0.16
 O11-C42
 2.45 with sigma of 0.16
 C41-O12
 2.45 with sigma of 0.16
 C42-C43
 2.45 with sigma of 0.16
 O12-C44
 2.45 with sigma of 0.16
 O11-O12
 3 with sigma of 0.16
 O11-C40
 3.1 with sigma of 0.16
 C9-C10
 2.45 with sigma of 0.16
 C15-C16
 2.45 with sigma of 0.16
 O5-C27
 2.5 with sigma of 0.16
 O6-C27
 2.5 with sigma of 0.16
 C30-C29
 2.5 with sigma of 0.16
 C27-O6
 2.6 with sigma of 0.16
 O13-C48
 2.5 with sigma of 0.16
 C47-O14
 2.5 with sigma of 0.16
 O14-C46
 2.5 with sigma of 0.16
 C29-C30
 2.6 with sigma of 0.16
 C55-O9
 2.45 with sigma of 0.16
 O10-C53
 2.5 with sigma of 0.16
 C56-C53
 2.5 with sigma of 0.16
 C54-O9
 2.5 with sigma of 0.16
 C54-C56
 2.9 with sigma of 0.16
 C16-C15
 2.5 with sigma of 0.16
 C6-C3
 2.6 with sigma of 1.6
 O1-C2
 2.8 with sigma of 1.6
 O1-C4
 2.8 with sigma of 1.6
 C3-C6
 2.8 with sigma of 1.6
 C27-O5
 2.8 with sigma of 1.6
 C35-C36
 2.8 with sigma of 1.6
 O14-C47
 3 with sigma of 0.2
 C48-O13
 3 with sigma of 0.2
 C47-C46
 3 with sigma of 0.2
 C45-C48
 3.3 with sigma of 0.2
 C48-C45
 4 with sigma of 0.2
 C52-C49
 2.5 with sigma of 0.08
 O8-C50
 2.6 with sigma of 0.08
 C51-C50
 2.6 with sigma of 0.08
 C56-O10
 2.6 with sigma of 0.08
4. Rigid bond restraints
 C44, O11, C41, C42, O12, C43
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C13, C14, C10, C11, C12, N3
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C13, C14, C11, C12, N3, C10
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O3, C13, C14, C10, C11, C12, N3
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C13, C14, C10, C11, C12, N3, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N6, C33, C34, C30, C31, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C56, O10, C55, C53, O9, C54
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
Br2 \\sim Br5 \\sim Zn3 \\sim Zn2 \\sim Br4 \\sim O4 \\sim C3 \\sim Zn1 \\sim
Br1 \\sim O1 \\sim N1 \\sim C1 \\sim C4 \\sim C52 \\sim O3 \\sim Br3 \\sim Br6
\\sim C5 \\sim N6 \\sim C33 \\sim C2 \\sim O14 \\sim C22 \\sim O6 \\sim C26
\\sim C51 \\sim C13 \\sim C24 \\sim C35 \\sim C18 \\sim C14 \\sim N3 \\sim C11
\\sim O10 \\sim C45 \\sim C41 \\sim O5 \\sim C50 \\sim C43 \\sim C46 \\sim C42
\\sim O12 \\sim C48 \\sim C49 \\sim C39 \\sim O8 \\sim C54 \\sim C38 \\sim C10
\\sim C40 \\sim C12 \\sim C30 \\sim C9 \\sim C44 \\sim C29 \\sim C47 \\sim C8
\\sim C6 \\sim C16 \\sim O13 \\sim C37 \\sim C53 \\sim C17 \\sim C15 \\sim C23
\\sim C32 \\sim N5 \\sim O11 \\sim C31 \\sim N4 \\sim C21 \\sim C56 \\sim C25
\\sim C27 \\sim C55 \\sim C20 \\sim C34 \\sim C36 \\sim N2 \\sim O2 \\sim O9
\\sim C28 \\sim C19 \\sim C7 \\sim O7: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.005
C13 \\sim C14 \\sim C10 \\sim N3 \\sim C11 \\sim C12: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
C44 \\sim O11 \\sim C43 \\sim C41 \\sim C42 \\sim O12: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
N4 \\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
C47 \\sim O13 \\sim C46 \\sim C45 \\sim O14 \\sim C48: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
C13 \\sim C14 \\sim C11 \\sim N3 \\sim C12 \\sim C10: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
C13 \\sim C14 \\sim C10 \\sim C11 \\sim C12 \\sim N3: within 2A with sigma of
0.002 and sigma for terminal atoms of 0.004
O3 \\sim C13 \\sim C14 \\sim C10 \\sim C11 \\sim C12 \\sim N3: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C13 \\sim C14 \\sim C10 \\sim C11 \\sim C12 \\sim N3 \\sim O3: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
N6 \\sim C33 \\sim C34 \\sim C30 \\sim C31 \\sim C32: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002
C56 \\sim O10 \\sim C55 \\sim C53 \\sim O9 \\sim C54: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.01
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.01
Uanis(C26) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Br5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Br3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N3) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N6) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C56) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C54) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C6(H6A,H6B), C56(H56A,H56B), C44(H44A,H44B), C26(H26A,H26B),
 C9(H9A,H9B), C55(H55A,H55B), C15(H15A,H15B), C53(H53A,H53B), C29(H29A,H29B),
 C45(H45A,H45B), C50(H50A,H50B), C51(H51A,H51B), C43(H43A,H43B), C54(H54A,H54B),
  C49(H49A,H49B), C35(H35A,H35B), C41(H41A,H41B), C46(H46A,H46B), C47(H47A,
 H47B), C42(H42A,H42B), C48(H48A,H48B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C33(H33), C34(H34), C31(H31), C32(H32),
 C25(H25), C24(H24), C22(H22), C21(H21), C13(H13), C14(H14), C11(H11), C12(H12),
  C37(H37), C38(H38), C39(H39), C40(H40), C20(H20), C17(H17), C18(H18), C19(H19)
6.c Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N6(C33,C34,C30,C31,C32), N4(C25,C24,C23,C22,C21), C37(C38,
 N5,C39,C40,C36), C20(C16,C17,C18,N2,C19)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              98534
_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 2.284
_oxdiff_exptl_absorpt_empirical_full_min 0.480