Thermally Activated Transient Dipoles and Rotational Dynamics of Hydrogen-Bonded and Charge-Transferred Diazabicyclo [2.2.2]Octane Molecular Rotors.
Jiang, Xing; Duan, Hai-Bao; Jellen, Marcus J.; Chen, Yu; Chung, Tim S.; Liang, Yong; Garcia-Garibay, Miguel A; Journal of the American Chemical Society 141 (2019) 16802–16809; doi:10.1021/jacs.9b07518

data_4127960
_publ_section_title
;
 Thermally Activated Transient Dipoles and Rotational Dynamics of
 Hydrogen-Bonded and Charge-Transferred Diazabicyclo [2.2.2]Octane
 Molecular Rotors.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16802
_journal_page_last               16809
_journal_paper_doi               10.1021/jacs.9b07518
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C20 H15 O2, C20 H16 O2, C6 H13 N2'
_chemical_formula_sum            'C46 H44 N2 O4'
_chemical_formula_weight         688.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                91.253(2)
_cell_angle_beta                 100.354(2)
_cell_angle_gamma                100.068(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7804(4)
_cell_length_b                   9.4799(4)
_cell_length_c                   21.6599(10)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.17
_cell_measurement_theta_min      4.74
_cell_volume                     1743.60(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29660
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.406
_diffrn_reflns_theta_min         2.077
_diffrn_source                   'I\mS micro--focus source'
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         6250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0525P)^2^+0.5919P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5606
_reflns_number_total             6250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07518_si_002.cif
_cod_data_source_block           cu_gg1624_100K_a
_cod_database_code               4127960
_shelx_estimated_absorpt_t_min   0.735
_shelx_estimated_absorpt_t_max   0.880
_shelxl_version_number           2014/6
_shelx_res_checksum              96032
_shelx_hkl_checksum              27333