Molecular Compasses and Gyroscopes with Polar Rotors: Synthesis and Characterization of Crystalline Forms
Zaira Dominguez; Tinh-A. V. Khuong; Hung Dang; Carlos N. Sanrame; Jose E. Nuñez; Miguel A. Garcia-Garibay; Journal of the American Chemical Society 125 (2003) 8827–8837; doi:10.1021/ja035274b

data_4113948
_publ_section_title
;
 Molecular Compasses and Gyroscopes with Polar Rotors: Synthesis and
 Characterization of Crystalline Forms
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8827
_journal_page_last               8837
_journal_paper_doi               10.1021/ja035274b
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C49 H33 N'
_chemical_formula_weight         635.76
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 94.226(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.812(3)
_cell_length_b                   20.338(4)
_cell_length_c                   10.741(2)
_cell_measurement_reflns_used    7030
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.2685
_cell_measurement_theta_min      2.217
_cell_volume                     3444.7(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15524
_diffrn_reflns_theta_full        23.30
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8165
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Sadabs(Bruker)
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         4962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0683P)^2^+3.3372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1472
_refine_ls_wR_factor_ref         0.1521
_reflns_number_gt                4197
_reflns_number_total             4962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja035274bsi20030321_024925.cif
_cod_data_source_block           gg2001
_cod_original_cell_volume        3444.6(12)
_cod_database_code               4113948