New [4.4]Cyclophanes: Molecular Parallelograms, Triangles, Rhombuses, Pentagons, and Supramolecular Constructions
Niculina Bogdan; Eric Condamine; Loïc Toupet; Yvan Ramondenc; Elena Bogdan; Ion Grosu; Journal of Organic Chemistry 73 (2008) 5831–5838; doi:10.1021/jo8006489

data_4023575
_publ_section_title
;
 New [4.4]Cyclophanes: Molecular Parallelograms, Triangles,
 Rhombuses, Pentagons, and Supramolecular Constructions
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5831
_journal_page_last               5838
_journal_paper_doi               10.1021/jo8006489
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C84 H96 O24'
_chemical_formula_weight         1489.61
_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                59.980(2)
_cell_angle_beta                 90.024(2)
_cell_angle_gamma                90.006(2)
_cell_formula_units_Z            2
_cell_length_a                   6.4201(6)
_cell_length_b                   26.907(2)
_cell_length_c                   26.903(2)
_cell_measurement_temperature    120(1)
_cell_volume                     4023.9(6)
_computing_cell_refinement       'Bruker AXS, 2003'
_computing_data_collection       'Bruker AXS, 2003'
_computing_data_reduction        'Bruker AXS, 2003'
_computing_molecular_graphics    'PLATON_(Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97_(Altomare & al., 1998)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 19.24
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  X8-APEX
_diffrn_measurement_method       'Area detector scans (see text)'
_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  0.0810
_diffrn_reflns_av_sigmaI/netI    0.3011
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30894
_diffrn_reflns_theta_full        29.77
_diffrn_reflns_theta_max         29.77
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         20097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.2534
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0923P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.2435
_reflns_number_gt                6569
_reflns_number_total             20097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8006489-File004.cif
_cod_data_source_block           nbm6f2
_cod_database_code               4023575