Planar chiral tetrasubstituted [2.2]paracyclophane: optical resolution and functionalization.
Morisaki, Yasuhiro; Gon, Masayuki; Sasamori, Takahiro; Tokitoh, Norihiro; Chujo, Yoshiki; Journal of the American Chemical Society 136 (2014) 3350–3353; doi:10.1021/ja412197j

data_4121506
_publ_section_title
;
 Planar chiral tetrasubstituted [2.2]paracyclophane: optical resolution
 and functionalization.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3350
_journal_page_last               3353
_journal_paper_doi               10.1021/ja412197j
_journal_volume                  136
_journal_year                    2014
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C72 H60, 4(H2 O)'
_chemical_formula_sum            'C72 H68 O4'
_chemical_formula_weight         997.26
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 94.822(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.272(5)
_cell_length_b                   20.035(3)
_cell_length_c                   9.3941(14)
_cell_measurement_temperature    103(2)
_cell_volume                     5864.9(16)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics    'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_publication_material  'Yadokari-XG 2011 (Wakita,Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Rigaku VariMax Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'rotating-anode X-ray tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            53443
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.9980
_exptl_absorpt_correction_T_min  0.9919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 MULABS - Empirical Correction for Absorption Anisotropy.
 Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.385
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5059
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.392
_refine_ls_R_factor_all          0.1817
_refine_ls_R_factor_gt           0.1185
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3363
_refine_ls_wR_factor_ref         0.3960
_reflns_number_gt                2733
_reflns_number_total             5059
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja412197j_si_004.cif
_cod_data_source_block           rac
_cod_original_cell_volume        5864.8(14)
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4121506