Amphidynamic Crystals of a Steroidal Bicyclo[2.2.2]octane Rotor: A High Symmetry Group That Rotates Faster than Smaller Methyl and Methoxy Groups
Braulio Rodríguez-Molina; Salvador Pérez-Estrada; Miguel A. Garcia-Garibay; Journal of the American Chemical Society 135 (2013) 10388–10395; doi:10.1021/ja4024463

data_4120099
_publ_contact_author_address
;     
      Chemistry and Biochemistry Department
      University of California Los Angeles
      Charles E. Young Drive East
      Los Angeles, CA 90095
      USA
;
_publ_contact_author_email       mgg@chem.ucla.edu
_publ_contact_author_fax         '310 825 3159'
_publ_contact_author_name        'Miguel A. Garcia-Garibay'
_publ_contact_author_phone       '310 825 3159'
_publ_section_title
;
 Amphidynamic Crystals of a Steroidal Bicyclo[2.2.2]octane Rotor: A High
 Symmetry Group That Rotates Faster than Smaller Methyl and Methoxy Groups
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10388
_journal_page_last               10395
_journal_paper_doi               10.1021/ja4024463
_journal_volume                  135
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C50 H62 O4'
_chemical_formula_sum            'C50 H62 O4'
_chemical_formula_weight         727.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4876(7)
_cell_length_b                   7.4876(7)
_cell_length_c                   72.129(10)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      3.72
_cell_volume                     4043.9(8)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0641
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       96
_diffrn_reflns_limit_l_min       -96
_diffrn_reflns_number            51185
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.9963
_exptl_absorpt_correction_T_min  0.9387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         3118
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+1.4696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                2692
_reflns_number_total             3118
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4024463_si_002.cif
_cod_data_source_block           gg612-tetra
_cod_database_code               4120099