2,6-Pyridodicarboxamide-Bridged Triptycene Molecular Transmission Devices: Converting Rotation to Rocking Vibration.
Wang, Guangxia; Ma, Lishuang; Xiang, Junfeng; Wang, Ying; Chen, Xuebo; Che, Yanke; Jiang, Hua; The Journal of organic chemistry 80 (2015) 11302–11312; doi:10.1021/acs.joc.5b01778

data_4031730
_publ_section_title
;
 2,6-Pyridodicarboxamide-Bridged Triptycene Molecular Transmission
 Devices: Converting Rotation to Rocking Vibration.
;
_journal_issue                   22
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11302
_journal_page_last               11312
_journal_paper_doi               10.1021/acs.joc.5b01778
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C59 H55 N3 O2'
_chemical_formula_sum            'C59 H55 N3 O2'
_chemical_formula_weight         838.06
_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             2015-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.06(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.930(3)
_cell_length_b                   16.114(3)
_cell_length_c                   20.594(4)
_cell_measurement_reflns_used    12741
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      26.0095
_cell_measurement_theta_min      1.6643
_cell_volume                     5130(2)
_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  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
    Number of images: 330
               Slice: -110.0000 - 55.0000
         Image width: 0.5000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9143
              2theta: -19.9901
scan:
    Number of images: 240
               Slice: -110.0000 - 10.0000
         Image width: 0.5000
            Exp time: 20.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9143
              2theta: -19.9901
;
_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      0.0559
_diffrn_orient_matrix_UB_12      0.0324
_diffrn_orient_matrix_UB_13      -0.0022
_diffrn_orient_matrix_UB_21      0.0173
_diffrn_orient_matrix_UB_22      -0.0263
_diffrn_orient_matrix_UB_23      0.0535
_diffrn_orient_matrix_UB_31      0.0390
_diffrn_orient_matrix_UB_32      -0.0258
_diffrn_orient_matrix_UB_33      -0.0253
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28054
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.828
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.52069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.451
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.863
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         9523
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.863
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.1194
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3010
_refine_ls_wR_factor_ref         0.3404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7241
_reflns_number_total             9523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5b01778_si_003.cif
_cod_data_source_block           sa3038_sq
_cod_depositor_comments
'Adding full bibliography for 4031729--4031733.cif.'
_cod_database_code               4031730
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.971
_diffrn_number_total             10470
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C22, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Ternary CH refined with riding coordinates:
 C13(H13), C39(H39)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), C1(H1A), C2(H2A), C3(H3), C14(H14), C17(H17), C20(H20),
 C21(H21), C28(H28), C29(H29), C40(H40), C41(H41), C48(H48), C49(H49), C54(H54),
  C55(H55)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C)
;
_shelx_res_checksum              5359
_shelx_hkl_checksum              58417
_shelx_fab_checksum              2143
_olex2_submission_special_instructions 'No special instructions were received'