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_4026548
_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         'C160 H192 O8, 2.5(C2 H3 N), 3(C H Cl3)'
_chemical_formula_sum            'C168 H202.5 Cl9 N2.5 O8'
_chemical_formula_weight         2703.88
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.3920(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.8379(15)
_cell_length_b                   22.2455(14)
_cell_length_c                   31.724(2)
_cell_measurement_temperature    173(2)
_cell_volume                     16822.4(18)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0953
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            183260
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.068
_exptl_crystal_description       shapeless
_exptl_crystal_F_000             5780
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.34
_refine_diff_density_max         2.335
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1783
_refine_ls_number_reflns         36742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.289
_refine_ls_R_factor_all          0.2365
_refine_ls_R_factor_gt           0.1410
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_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          0.3818
_refine_ls_wR_factor_ref         0.4208
_reflns_number_gt                16805
_reflns_number_total             36742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2009643_si_001_2.cif
_cod_data_source_block           katya25m
_cod_original_cell_volume        16822.3(18)
_cod_original_formula_sum        'C168 H202.50 Cl9 N2.50 O8'
_cod_database_code               4026548