Effects of side chains of oxatub[4]arene on its conformational interconversion, molecular recognition and macroscopic self-assembly
Yang, Liu-Pan; Jia, Fei; Pan, Fangfang; Pan, Zhi-Sheng; Rissanen, Kari; Jiang, Wei; Chemical Communications 53 (2017) 12572–12575; doi:10.1039/C7CC07630D

data_1547870
_publ_section_title
;
 Effects of side chains of oxatub[4]arene on its conformational
 interconversion, molecular recognition and macroscopic self-assembly
;
_journal_issue                   93
_journal_name_full               'Chemical Communications'
_journal_page_first              12572
_journal_page_last               12575
_journal_paper_doi               10.1039/C7CC07630D
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C80 H104 O12'
_chemical_formula_sum            'C80 H104 O12'
_chemical_formula_weight         1257.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-09-29 deposited with the CCDC.
2017-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.169(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.8502(5)
_cell_length_b                   9.25277(17)
_cell_length_c                   20.4322(5)
_cell_measurement_reflns_used    5902
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      28.1890
_cell_measurement_theta_min      3.2330
_cell_volume                     3422.75(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
  1 omega  -19.00   24.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7586  -99.0000    0.0000 43

  2 omega  -51.00   39.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8523  -57.0000  -30.0000 90

  3 omega   -4.00   87.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8523   57.0000 -120.0000 91

  4 omega  -51.00   39.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       17.8523  -57.0000   90.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0144575000
_diffrn_orient_matrix_UB_12      -0.0390886000
_diffrn_orient_matrix_UB_13      -0.0307004000
_diffrn_orient_matrix_UB_21      -0.0046197000
_diffrn_orient_matrix_UB_22      0.0655205000
_diffrn_orient_matrix_UB_23      -0.0187438000
_diffrn_orient_matrix_UB_31      0.0361227000
_diffrn_orient_matrix_UB_32      -0.0073110000
_diffrn_orient_matrix_UB_33      -0.0037132000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20660
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.393
_diffrn_reflns_theta_min         3.026
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.3063
_exptl_crystal_size_mid          0.1467
_exptl_crystal_size_min          0.0903
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0374P)^2^+1.6568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5352
_reflns_number_total             7487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07630d2.cif
_cod_data_source_block           1a
_cod_database_code               1547870
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C50 H50 O4 N4'
_reflns_odcompleteness_completeness 98.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. 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
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C15(H15), C16(H16), C19(H19), C20(H20)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              82768
_olex2_submission_special_instructions 'No special instructions were received'