Conformationally Restricted Calix[8]arenes Substituted at All Methylene Bridges
Katerina Kogan; Silvio E. Biali; Journal of Organic Chemistry 76 (2011) 7240–7244; doi:10.1021/jo2009643

data_4026549
_publ_section_title
;
 Conformationally Restricted Calix[8]arenes Substituted at All Methylene
 Bridges
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7240
_journal_page_last               7244
_journal_paper_doi               10.1021/jo2009643
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C168 H208 O8, 5(C8 H10)'
_chemical_formula_sum            'C208 H258 O8'
_chemical_formula_weight         2886.14
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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                 91.265(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.177(8)
_cell_length_b                   25.438(6)
_cell_length_c                   23.549(5)
_cell_measurement_temperature    173(2)
_cell_volume                     19869(8)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.1613
_diffrn_reflns_av_sigmaI/netI    0.1666
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            98334
_diffrn_reflns_theta_full        28.15
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.965
_exptl_crystal_description       plate
_exptl_crystal_F_000             6280
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.183
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0018(2)
_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   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1073
_refine_ls_number_reflns         23390
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.2710
_refine_ls_R_factor_gt           0.1273
_refine_ls_shift/su_max          0.003
_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          0.3232
_refine_ls_wR_factor_ref         0.4101
_reflns_number_gt                8354
_reflns_number_total             23390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2009643_si_001_3.cif
_cod_data_source_block           katya24m
_cod_original_cell_volume        19870(8)
_cod_database_code               4026549