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_1558837
_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, 2(C5 H10 O)'
_chemical_formula_sum            'C50 H62 Br6 N6 O8 Zn3'
_chemical_formula_weight         1550.62
_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             2020-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-01 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                   15.889(2)
_cell_length_b                   13.4934(13)
_cell_length_c                   33.290(8)
_cell_measurement_reflns_used    25648
_cell_measurement_temperature    100.0(6)
_cell_measurement_theta_max      59.5170
_cell_measurement_theta_min      2.3420
_cell_volume                     7137(2)
_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      100.0(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     33.00 130.00   0.50    0.20    --   72.34-151.00 -30.00  194
  2  \w     62.00 145.00   0.50    0.20    --   72.34 151.00  14.00  166
  3  \w     19.00 110.00   0.50    0.20    --   72.34-122.00 131.00  182
  4  \w     81.00 145.00   0.50    0.20    --   72.34 122.00-147.00  128
  5  \w   -148.00 -61.00   0.50    0.20    --  -75.15-151.00 -30.00  174
  6  \w   -109.00 -18.00   0.50    0.20    --  -75.15 122.00-147.00  182
  7  \w   -148.00 -81.00   0.50    0.20    --  -75.15-122.00 131.00  134
  8  \w    -74.00  15.00   0.50    0.05    --   -1.41 -57.00 -60.00  178
  9  \w    -75.00  13.00   0.50    0.05    --   -1.41 -38.00-180.00  176
 10  \w    -75.00  13.00   0.50    0.05    --   -1.41 -38.00 -90.00  176
 11  \w    -16.00  72.00   0.50    0.05    --   -1.41  38.00 -90.00  176
 12  \w    -75.00  13.00   0.50    0.05    --   -1.41 -38.00  90.00  176
 13  \w    -74.00  15.00   0.50    0.05    --   -1.41 -57.00 -90.00  178
 14  \w    -75.00  13.00   0.50    0.05    --   -1.41 -38.00  30.00  176
 15  \w    -74.00  22.00   0.50    0.05    --   -1.41 -77.00-150.00  192
 16  \w    -48.00 -18.00   0.50    0.05    --   -1.41 122.00 113.87   60
 17  \w     49.00 145.00   0.50    0.20    --   72.34  77.00-150.00  192
 18  \w     49.00 145.00   0.50    0.20    --   72.34  77.00  90.00  192
 19  \w      0.00  66.00   0.50    0.20    --   72.34 -57.00 150.00  132
 20  \w     56.00 145.00   0.50    0.20    --   72.34  54.00 145.31  178
 21  \w     49.00 145.00   0.50    0.20    --   72.34  77.00  30.00  192
 22  \w     51.00 145.00   0.50    0.20    --   72.34  71.00  80.53  188
 23  \w     56.00 145.00   0.50    0.20    --   72.34  57.00  80.18  178
 24  \w     49.00 145.00   0.50    0.20    --   72.34  77.00 -60.00  192
 25  \w      0.00  96.00   0.50    0.20    --   72.34 -77.00 150.00  192
 26  \w     49.00 145.00   0.50    0.20    --   72.34  77.00 150.00  192
 27  \w      1.00  63.00   0.50    0.20    --   72.34 -57.00  90.00  124
 28  \w     49.00  75.00   0.50    0.20    --   72.34  77.00-120.00   52
 29  \w     49.00  89.00   0.50    0.20    --   72.34  77.00 -90.00   80
 30  \w     50.00  75.00   0.50    0.20    --   72.34  77.00  60.00   50
 31  \w      0.00  96.00   0.50    0.20    --   72.34 -77.00 -30.00  192
 32  \w     47.00  73.00   0.50    0.20    --   72.34  80.00  -4.03   52
 33  \w     49.00  75.00   0.50    0.20    --   72.34  77.00 117.09   52
 34  \w     50.00 115.00   0.50    0.20    --   72.34  73.00-135.07  130
 35  \w     55.00  88.00   0.50    0.20    --   72.34  61.00  35.95   66
 36  \w     50.00  76.00   0.50    0.20    --   72.34  73.00  87.95   52
 37  \w     49.00  75.00   0.50    0.20    --   72.34  77.00 -30.00   52
 38  \w      1.00  94.00   0.50    0.20    --   72.34 -77.00-120.00  186
 39  \w     47.00  94.00   0.50    0.20    --   72.34  80.00-112.36   94
 40  \w     49.00  75.00   0.50    0.20    --   72.34  77.00-180.00   52
 41  \w      0.00 105.00   0.50    0.20    --   72.34 -99.00 -30.00  210
 42  \w    -79.00 -51.00   0.50    0.20    --  -75.15 -77.00-120.00   56
 43  \w   -115.00 -84.00   0.50    0.20    --  -75.15 -77.00-120.00   62
 44  \w   -135.00 -54.00   0.50    0.20    --  -75.15 -70.00 -24.73  162
 45  \w   -147.00 -51.00   0.50    0.20    --  -75.15 -77.00 -30.00  192
 46  \w    -85.00 -54.00   0.50    0.20    --  -75.15 -70.00-143.01   62
 47  \w   -148.00 -99.00   0.50    0.20    --  -75.15 -70.00-143.01   98
 48  \w   -148.00 -57.00   0.50    0.20    --  -75.15 -62.00 -99.30  182
 49  \w    -77.00 -51.00   0.50    0.20    --  -75.15 -77.00  90.00   52
 50  \w    -61.00  -2.00   0.50    0.20    --  -75.15  57.00  60.00  118
 51  \w   -112.00 -50.00   0.50    0.20    --  -75.15 -80.00 173.23  124
 52  \w    -77.00 -51.00   0.50    0.20    --  -75.15 -77.00 -90.00   52
 53  \w    -80.00 -54.00   0.50    0.20    --  -75.15 -70.00   5.88   52
 54  \w   -147.00 -51.00   0.50    0.20    --  -75.15 -77.00 -53.39  192
 55  \w    -76.00 -51.00   0.50    0.20    --  -75.15 -77.00   0.00   50
 56  \w   -120.00 -89.00   0.50    0.20    --  -75.15 -77.00   0.00   62
 57  \w    -75.00 -50.00   0.50    0.20    --  -75.15 -81.00  48.62   50
 58  \w   -143.00 -94.00   0.50    0.20    --  -75.15 -81.00  48.62   98
 59  \w    -83.00 -51.00   0.50    0.20    --  -75.15 -77.00  58.89   64
 60  \w   -147.00-102.00   0.50    0.20    --  -75.15 -77.00  58.89   90
 61  \w   -102.00 -51.00   0.50    0.20    --  -75.15 -77.00 150.00  102
 62  \w    -77.00 -51.00   0.50    0.20    --  -75.15 -77.00-150.00   52
 63  \w   -148.00 -92.00   0.50    0.20    --  -75.15 -77.00-150.00  112
 64  \w    -77.00 -51.00   0.50    0.20    --  -75.15 -77.00-171.65   52
 65  \w    -36.00  -6.00   0.50    0.20    --  -75.15  38.00  60.00   60
 66  \w   -122.00 -72.00   0.50    0.20    --  -75.15 151.00  14.00  100
;
_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      -0.0397707000
_diffrn_orient_matrix_UB_12      0.0075616000
_diffrn_orient_matrix_UB_13      -0.0142508000
_diffrn_orient_matrix_UB_21      0.0055590000
_diffrn_orient_matrix_UB_22      -0.0064079000
_diffrn_orient_matrix_UB_23      -0.0978860000
_diffrn_orient_matrix_UB_31      -0.0040422000
_diffrn_orient_matrix_UB_32      -0.0834952000
_diffrn_orient_matrix_UB_33      0.0062513000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.1214
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            252053
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.907
_diffrn_reflns_theta_min         2.308
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.675
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63052
_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    1.443
_exptl_crystal_description       plate
_exptl_crystal_F_000             3072
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         14560
_refine_ls_number_restraints     698
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.1125
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1052P)^2^+44.1124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2757
_refine_ls_wR_factor_ref         0.2923
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                11582
_reflns_number_total             14560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01176b2.cif
_cod_data_source_block           190927-5
_cod_depositor_comments
'Adding full bibliography for 1558835--1558840.cif.'
_cod_database_code               1558837
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O N Zn Br'
_diffrn_oxdiff_digest_frames
;
013c418a6824137a9a1d9e89a9b1cd4ac60821694f2
;
_diffrn_oxdiff_digest_hkl
;
014c56eb9671e66eb3b773a6f35c903b4fb969
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(8)
 0.51(8)
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
 O5-C36 = O5-C35 = O6-C29 = O6-C30 = O4-C26 = O4-C23 = C50-C49 = C50-O8 = O7-
 C41 = O7-C45 = O1-C3 = O1-C6 = O3-C10 = O3-C9 = O2-C15 = O2-C16
 1.44 with sigma of 0.02
 C29-C27 = C26-C27 = C27-C35 = C28-C27 = C7-C9 = C15-C7 = C6-C7 = C8-C7 = C46-
 O8 = C46-C47 = C47-C48 = C49-C48 = C42-C41 = C42-C43 = C43-C44 = C44-C45
 1.53 with sigma of 0.02
 C46-C47
 1.55 with sigma of 0.02
 C47-C48
 1.53 with sigma of 0.02
 C50-O8
 1.44 with sigma of 0.02
 C50-C49
 1.58 with sigma of 0.04
 C47-C46
 1.6 with sigma of 0.02
 C49-C50
 1.65 with sigma of 0.02
 C48-C49
 1.6 with sigma of 0.02
 C46-O8
 1.4 with sigma of 0.02
 O5-C35
 1.4 with sigma of 0.02
 O6-C29
 1.35 with sigma of 0.02
 C30-O6
 1.55 with sigma of 0.02
 C36-O5
 1.55 with sigma of 0.02
 C27-C28
 1.55 with sigma of 0.02
 C28-C27
 1.6 with sigma of 0.02
 C50-C46
 2.48 with sigma of 0.04
 C49-O8
 2.5 with sigma of 0.04
 C30-C29
 2.8 with sigma of 0.04
 O6-C27
 2.8 with sigma of 0.04
 O5-C27
 2.8 with sigma of 0.04
 C27-O5
 2.9 with sigma of 0.04
 C27-O4
 2.9 with sigma of 0.04
4. Rigid bond restraints
 N3, C12, C11, C10, C14, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O8, C48, C47, C49, C46, C50
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Br6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Uiso/Uaniso restraints and constraints
C35 \\sim N6 \\sim C32 \\sim N2 \\sim C26 \\sim C41 \\sim Br1 \\sim C17 \\sim
Br3 \\sim O3 \\sim N5 \\sim C37 \\sim Zn1 \\sim C4 \\sim C10 \\sim C5 \\sim C14
\\sim C13 \\sim N4 \\sim N1 \\sim Br5 \\sim C45 \\sim C27 \\sim C30 \\sim Zn2
\\sim C16 \\sim C31 \\sim O1 \\sim C38 \\sim C1 \\sim C44 \\sim Br2 \\sim C39
\\sim C12 \\sim C11 \\sim C34 \\sim C24 \\sim C40 \\sim C19 \\sim O5 \\sim C28
\\sim Br4 \\sim C25 \\sim C21 \\sim C3 \\sim O2 \\sim C23 \\sim C7 \\sim O8
\\sim Zn3 \\sim Br6 \\sim O7 \\sim C2 \\sim C33 \\sim O6 \\sim C18 \\sim C9
\\sim N3 \\sim O4 \\sim C20 \\sim C36 \\sim C6 \\sim C29 \\sim C15 \\sim C48
\\sim C22 \\sim C42 \\sim C43 \\sim C46 \\sim C50 \\sim C8 \\sim C47 \\sim C49:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.005
N3 \\sim C12 \\sim C11 \\sim C10 \\sim C14 \\sim C13: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
O8 \\sim C48 \\sim C47 \\sim C49 \\sim C46 \\sim C50: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002
Br6: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C49)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Br5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Br6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
6.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C35(H35A,H35B), C44(H44A,H44B), C26(H26A,H26B), C9(H9A,H9B),
 C41(H41A,H41B), C29(H29A,H29B), C15(H15A,H15B), C48(H48A,H48B), C6(H6A,H6B),
 C43(H43A,H43B), C42(H42A,H42B), C47(H47A,H47B), C49(H49A,H49B), C46(H46A,H46B),
  C50(H50A,H50B)
6.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C20(H20), C19(H19), C18(H18), C38(H38), C37(H37), C40(H40),
 C39(H39), C4(H4), C5(H5), C1(H1), C2(H2), C12(H12), C11(H11), C14(H14),
 C13(H13), C25(H25), C31(H31), C34(H34), C33(H33), C32(H32), C24(H24), C21(H21),
  C22(H22)
6.c Fitted hexagon refined as free rotating group:
 C17(C16,C20,C19,N2,C18), N5(C38,C37,C36,C40,C39), C3(C4,C5,N1,C1,C2), N3(C12,
 C11,C10,C14,C13), C31(C30,C34,C33,N6,C32)
6.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              20758
_shelx_fab_checksum              37564
_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 2.395
_oxdiff_exptl_absorpt_empirical_full_min 0.414