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_4031732
_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_absolute_configuration ad
_chemical_formula_moiety         'C H2 Cl2, C47 H31 N3 O2'
_chemical_formula_sum            'C48 H33 Cl2 N3 O2'
_chemical_formula_weight         754.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-07-02
_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            4
_cell_length_a                   8.7530(18)
_cell_length_b                   14.773(3)
_cell_length_c                   28.489(6)
_cell_measurement_reflns_used    12475
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4810
_cell_measurement_theta_min      1.5527
_cell_volume                     3683.9(13)
_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 0.997
_diffrn_measured_fraction_theta_max 0.994
_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      -0.0271
_diffrn_orient_matrix_UB_12      0.0966
_diffrn_orient_matrix_UB_13      0.0547
_diffrn_orient_matrix_UB_21      0.0109
_diffrn_orient_matrix_UB_22      0.0352
_diffrn_orient_matrix_UB_23      -0.0568
_diffrn_orient_matrix_UB_31      -0.0336
_diffrn_orient_matrix_UB_32      -0.0043
_diffrn_orient_matrix_UB_33      -0.0091
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            15160
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         2.434
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       rod
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 2239 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.06(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0746
_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^)+(0.0400P)^2^+2.5229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1445
_refine_ls_wR_factor_ref         0.1532
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                7231
_reflns_number_total             8370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5b01778_si_001.cif
_cod_data_source_block           sa2384
_cod_depositor_comments
'Adding full bibliography for 4031729--4031733.cif.'
_cod_database_code               4031732
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.957
_diffrn_number_total             4757
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C35(H35)
2.b Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C3(H3A), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25),
  C26(H26), C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38),
 C39(H39), C40(H40), C43(H43), C44(H44), C45(H45), C46(H46)
;
_shelx_res_checksum              77114
_shelx_hkl_checksum              85387