Rotational Dynamics in a Crystalline Molecular Gyroscope by Variable-Temperature 13C NMR,2H NMR, X-Ray Diffraction, and Force Field Calculations
Tinh-Alfredo V. Khuong; Hung Dang; Peter D. Jarowski; Emily F. Maverick; Miguel A. Garcia-Garibay; Journal of the American Chemical Society 129 (2007) 839–845; doi:10.1021/ja064325c

data_4109002
_publ_section_title
;
 Rotational Dynamics in a Crystalline Molecular Gyroscope by
 Variable-Temperature 13C NMR,2H NMR, X-Ray Diffraction, and Force Field
 Calculations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              839
_journal_page_last               845
_journal_paper_doi               10.1021/ja064325c
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C54 H46 O6, C6 H6'
_chemical_formula_sum            'C60 H52 O6'
_chemical_formula_weight         869.02
_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
_cell_angle_alpha                77.253(9)
_cell_angle_beta                 80.996(8)
_cell_angle_gamma                73.084(8)
_cell_formula_units_Z            1
_cell_length_a                   7.116(4)
_cell_length_b                   10.145(5)
_cell_length_c                   17.823(9)
_cell_measurement_temperature    298(2)
_cell_volume                     1194.8(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0859
_diffrn_reflns_av_sigmaI/netI    0.3194
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7909
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9852
_exptl_absorpt_correction_T_min  0.9742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       Plate
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.772
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.772
_refine_ls_R_factor_all          0.2640
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1772
_reflns_number_gt                1392
_reflns_number_total             5139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064325csi20061019_065400.cif
_cod_data_source_block           gg1503csm300k
_cod_depositor_comments
;
 Adding a reference to a suboptimal entry.

 Antanas Vaitkus,
 2018-11-16
;
_cod_original_cell_volume        1194.7(10)
_cod_related_suboptimal_struct   4109038
_cod_database_code               4109002