Rotational Dynamics of Diazabicyclo[2.2.2]octane in Isomorphous Halogen-Bonded Co-crystals: Entropic and Enthalpic Effects.
Catalano, Luca; Perez-Estrada, Salvador; Wang, Hsin-Hua; Ayitou, Anoklase J.-L.; Khan, Saeed I.; Terraneo, Giancarlo; Metrangolo, Pierangelo; Brown, Stuart; Garcia-Garibay, Miguel A; Journal of the American Chemical Society 139 (2017) 843–848; doi:10.1021/jacs.6b10780

data_4125750
_publ_section_title
;
 Rotational Dynamics of Diazabicyclo[2.2.2]octane in Isomorphous
 Halogen-Bonded Co-crystals: Entropic and Enthalpic Effects.
;
_journal_issue                   2
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              843
_journal_page_last               848
_journal_paper_doi               10.1021/jacs.6b10780
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C21 H15 I, C6 H12 N2 '
_chemical_formula_sum            'C27 H27 I N2'
_chemical_formula_weight         506.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 100.278(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3106(19)
_cell_length_b                   7.0791(10)
_cell_length_c                   24.375(3)
_cell_measurement_reflns_used    4795
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.96
_cell_measurement_theta_min      2.50
_cell_volume                     2259.9(5)
_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'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            23056
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.850
_diffrn_reflns_theta_min         2.088
_diffrn_source                   'Sealed Mo X-Ray Tube'
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0254P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4040
_reflns_number_total             5559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10780_si_002.cif
_cod_data_source_block           mo_gg1521s_a
_cod_original_cell_volume        2259.9(6)
_cod_database_code               4125750
_shelx_estimated_absorpt_t_min   0.782
_shelx_estimated_absorpt_t_max   0.972
_shelxl_version_number           2014/6
_shelx_res_checksum              52799
_shelx_hkl_checksum              3327