Ultra-fast Rotors for Molecular Machines and Functional Materials via Halogen Bonding: Crystals of 1,4-Bis(iodoethynyl)bicyclo[2.2.2]octane with Distinct Gigahertz Rotation at Two Sites
Cyprien Lemouchi; Cortnie S. Vogelsberg; Leokadiya Zorina; Sergey Simonov; Patrick Batail; Stuart E. Brown; Miguel A. Garcia-Garibay; Journal of the American Chemical Society 133 (2011) 6371–6379; doi:10.1021/ja200503j

data_4106038
_publ_contact_author_address
;
Laboratoire de Chimie et Ing\'enierie Mol\'eculaire d'Angers,
CNRS-Universit\'e d'Angers, 49045 Angers, France
;
_publ_contact_author_email       patrick.batail@univ-angers.fr
_publ_contact_author_name        'Dr. Patrick Batail'
_publ_section_title
;
 Ultra-fast Rotors for Molecular Machines and Functional Materials via
 Halogen Bonding: Crystals of 1,4-Bis(iodoethynyl)bicyclo[2.2.2]octane
 with Distinct Gigahertz Rotation at Two Sites
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6371
_journal_page_last               6379
_journal_paper_doi               10.1021/ja200503j
_journal_volume                  133
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C12 H12 I2'
_chemical_formula_sum            'C12 H12 I2'
_chemical_formula_weight         410.02
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and WinGX routine-INITIALISE'
_cell_angle_alpha                79.081(7)
_cell_angle_beta                 65.960(7)
_cell_angle_gamma                60.573(6)
_cell_formula_units_Z            8
_cell_length_a                   13.9129(10)
_cell_length_b                   13.9129(10)
_cell_length_c                   16.236(2)
_cell_measurement_reflns_used    21275
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     2499.7(4)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND 3.1 (Crystal Impact GbR 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Bruker KappaCCD'
_diffrn_measurement_method       'combined \f/\w-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            78664
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         35.08
_diffrn_reflns_theta_min         4.53
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.994
_exptl_absorpt_correction_T_max  0.6617
_exptl_absorpt_correction_T_min  0.4414
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.179
_exptl_crystal_description       plate
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.729
_refine_diff_density_min         -2.201
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         78664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+10.9279P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                58417
_reflns_number_total             78664
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja200503j_si_002.cif
_cod_data_source_block           cl339-90K-final
_cod_database_code               4106038