Threading of Conformationally Stable Calix[6]arene Wheels Substituted at the Methylene Bridges.
Tranfić Bakić, Marina; Iuliano, Veronica; Talotta, Carmen; Geremia, Silvano; Hickey, Neal; Spinella, Aldo; De Rosa, Margherita; Soriente, Annunziata; Gaeta, Carmine; Neri, Placido; The Journal of organic chemistry 84 (2019) 11922–11927; doi:10.1021/acs.joc.9b01779

data_4034444
_publ_section_title
;
 Threading of Conformationally Stable Calix[6]arene Wheels Substituted at
 the Methylene Bridges.
;
_journal_issue                   18
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11922
_journal_page_last               11927
_journal_paper_doi               10.1021/acs.joc.9b01779
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C80 H112 O6'
_chemical_formula_sum            'C80 H112 O6'
_chemical_formula_weight         1169.69
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yab'
_space_group_name_H-M_alt        'P 1 21/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2019-03-29T18:13:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 108.21(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.341(6)
_cell_length_b                   16.117(4)
_cell_length_c                   17.567(6)
_cell_measurement_reflns_used    40136
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.16
_cell_measurement_theta_min      1.2
_cell_measurement_wavelength     0.7
_cell_volume                     3588(2)
_computing_cell_refinement       'XDS (Kabasch 2010)'
_computing_data_collection       'ELETTRA XRD1 Data Collection SW'
_computing_data_reduction        XDS
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-2014 (Burla et al., 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_device       'Area Detector'
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'Rotating Crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74695
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         33.165
_diffrn_reflns_theta_min         1.202
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.039
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0086(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     402
_refine_ls_number_reflns         11803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.05
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+1.2139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0
_reflns_number_gt                9445
_reflns_number_total             11803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01779_si_002.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               4034444