Molecular Spur Gears Based on a Switchable Quinquepyridine Foldamer Acting as a Stator.
Huang, Fu; Wang, Guangxia; Ma, Lishuang; Wang, Ying; Chen, Xuebo; Che, Yanke; Jiang, Hua; The Journal of organic chemistry 82 (2017) 12106–12111; doi:10.1021/acs.joc.7b01864

data_4033044
_publ_section_title
;
 Molecular Spur Gears Based on a Switchable Quinquepyridine Foldamer
 Acting as a Stator.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12106
_journal_page_last               12111
_journal_paper_doi               10.1021/acs.joc.7b01864
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C65 H41 N5'
_chemical_formula_sum            'C65 H41 N5'
_chemical_formula_weight         892.03
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.263(3)
_cell_length_b                   18.263(3)
_cell_length_c                   61.044(9)
_cell_measurement_reflns_used    29054
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4726
_cell_measurement_theta_min      1.4983
_cell_volume                     20360(6)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2013)'
_computing_structure_solution
;
'SHELXS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0062
_diffrn_orient_matrix_UB_12      -0.0257
_diffrn_orient_matrix_UB_13      0.0480
_diffrn_orient_matrix_UB_21      0.0255
_diffrn_orient_matrix_UB_22      0.0440
_diffrn_orient_matrix_UB_23      0.0202
_diffrn_orient_matrix_UB_31      -0.0144
_diffrn_orient_matrix_UB_32      0.0060
_diffrn_orient_matrix_UB_33      0.0051
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0758
_diffrn_reflns_av_unetI/netI     0.0985
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            34993
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.197
_diffrn_reflns_theta_min         1.164
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       Plate
_exptl_crystal_F_000             7456
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.449
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         9131
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.467
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.1042
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_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          0.2564
_refine_ls_wR_factor_ref         0.2727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6501
_reflns_number_total             9131
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b01864_si_001.cif
_cod_data_source_block           sa2790
_cod_depositor_comments          'Adding full bibliography for 4033044.cif.'
_cod_original_cell_volume        20360(7)
_cod_database_code               4033044
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.975
_diffrn_number_total             11777
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N5) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C29) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C33(H33), C53(H53)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C12(H12), C13(H13), C14(H14),
 C17(H17), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28), C29(H29),
  C30(H30), C31(H31), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41),
 C42(H42), C43(H43), C44(H44), C48(H48), C49(H49), C50(H50), C51(H51), C55(H55),
  C56(H56), C57(H57), C58(H58), C61(H61), C62(H62), C63(H63), C64(H64)
;
_shelx_res_checksum              65672
_shelx_hkl_checksum              12243