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_4109038
_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 0.983
_diffrn_measured_fraction_theta_max 0.971
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.1744
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5602
_diffrn_reflns_theta_full        20.50
_diffrn_reflns_theta_max         23.10
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9924
_exptl_absorpt_correction_T_min  0.9736
_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         0.182
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3274
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.1684
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                1365
_reflns_number_total             3274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja064325csi20061019_065422.cif
_cod_data_source_block           gg1503csmdis1
_cod_depositor_comments
;
 Replacing the _cod_related_optimal_structure data name with the shorter
 version (_cod_related_optimal_struct) that is formally defined in the
 'cif_cod' dictionary.

 Antanas Vaitkus,
 2018-11-16

 Removed the _cod_suboptimal_structure data item in preparation for
 its deprecation. The fact that the structure is a suboptimal one
 should be derived from the presence of the _cod_related_optimal_struct
 data item.

 Antanas Vaitkus,
 2019-05-21
;
_cod_original_cell_volume        1194.7(10)
_cod_related_optimal_struct      4109002
_cod_database_code               4109038