Influence of <i>exo</i>-Adamantyl Groups and <i>endo</i>-OH Functions on the Threading of Calix[6]arene Macrocycle.
Iuliano, Veronica; Talotta, Carmen; Gaeta, Carmine; Hickey, Neal; Geremia, Silvano; Vatsouro, Ivan; Kovalev, Vladimir; Neri, Placido; The Journal of organic chemistry 85 (2020) 12585–12593; doi:10.1021/acs.joc.0c01769

data_4038798
_publ_section_title
;
 Influence of <i>exo</i>-Adamantyl Groups and <i>endo</i>-OH Functions on
 the Threading of Calix[6]arene Macrocycle.
;
_journal_issue                   19
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12585
_journal_page_last               12593
_journal_paper_doi               10.1021/acs.joc.0c01769
_journal_volume                  85
_journal_year                    2020
_chemical_formula_moiety         'C126  H168  O6,  2.25 (C H Cl3)'
_chemical_formula_sum            'C128.25 H170.25 Cl6.75 O6'
_chemical_formula_weight         2047.17
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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             2020-03-06T18:04:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-03-16 deposited with the CCDC.	2020-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                75.80(3)
_cell_angle_beta                 86.69(2)
_cell_angle_gamma                86.896(10)
_cell_formula_units_Z            2
_cell_length_a                   12.959(4)
_cell_length_b                   15.165(3)
_cell_length_c                   29.378(7)
_cell_measurement_reflns_used    12871
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.6
_cell_measurement_theta_min      1.36
_cell_measurement_wavelength     0.7
_cell_volume                     5583(3)
_computing_cell_refinement       'XDS (Kabsch, 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    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.95
_diffrn_measured_fraction_theta_max 0.95
_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  0.1038
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_Laue_measured_fraction_full 0.95
_diffrn_reflns_Laue_measured_fraction_max 0.95
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            45006
_diffrn_reflns_point_group_measured_fraction_full 0.95
_diffrn_reflns_point_group_measured_fraction_max 0.95
_diffrn_reflns_theta_full        21.601
_diffrn_reflns_theta_max         21.601
_diffrn_reflns_theta_min         1.365
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Flat rods'
_exptl_crystal_F_000             2205
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CHCl3 / CH3OH'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0042(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   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1417
_refine_ls_number_reflns         12925
_refine_ls_number_restraints     1495
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.1007
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1695P)^2^+7.6660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2737
_refine_ls_wR_factor_ref         0.3254
_reflns_Friedel_coverage         0
_reflns_number_gt                7363
_reflns_number_total             12925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01769_si_003.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4038798--4038799.cif.'
_cod_database_code               4038798