An Intramolecularly Self-Templated Synthesis of Macrocycles: The Self-Filling Effects on the Formation of Prismarenes
DELLA SALA, PAOLO; Del Regno, Rocco; Di Marino, Luca; Calabrese, Carmela; Palo, Carmine; Talotta, Carmen; Geremia, Silvano; Hickey, Neal; Capobianco, Amedeo; Neri, Placido; Gaeta, Carmine; Chemical Science  (2021) –; doi:10.1039/D1SC02199K

data_1563138
_publ_section_title
;
 An Intramolecularly Self-Templated Synthesis of Macrocycles: The
 Self-Filling Effects on the Formation of Prismarenes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02199K
_journal_year                    2021
_chemical_formula_moiety
'C65 H60 O10, C4 H12 N, C32 H12 B F24, 1.1(C H2 Cl2)'
_chemical_formula_sum            'C102.1 H86.2 B Cl2.2 F24 N O10'
_chemical_formula_weight         2031.92
_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   geom
_audit_creation_date             2020-12-15T11:52:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-12-16 deposited with the CCDC.	2021-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                81.367(6)
_cell_angle_beta                 80.862(14)
_cell_angle_gamma                68.83(3)
_cell_formula_units_Z            4
_cell_length_a                   21.686(11)
_cell_length_b                   22.528(10)
_cell_length_c                   22.906(7)
_cell_measurement_reflns_used    21249
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.674
_cell_measurement_theta_min      0.891
_cell_volume                     10250(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.94
_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  0.0993
_diffrn_reflns_av_unetI/netI     0.1006
_diffrn_reflns_Laue_measured_fraction_full 0.931
_diffrn_reflns_Laue_measured_fraction_max 0.94
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            82571
_diffrn_reflns_point_group_measured_fraction_full 0.931
_diffrn_reflns_point_group_measured_fraction_max 0.94
_diffrn_reflns_theta_full        21.689
_diffrn_reflns_theta_max         21.689
_diffrn_reflns_theta_min         0.891
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       prism
_exptl_crystal_F_000             4177
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane/dichloromethane'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2470
_refine_ls_number_reflns         23532
_refine_ls_number_restraints     3486
_refine_ls_restrained_S_all      1.13
_refine_ls_R_factor_all          0.2416
_refine_ls_R_factor_gt           0.1565
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+36.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3939
_refine_ls_wR_factor_ref         0.4607
_reflns_Friedel_coverage         0
_reflns_number_gt                12438
_reflns_number_total             23532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02199k2.cif
_cod_data_source_block           platon_sq_CCDC1
_cod_original_cell_volume        10251(8)
_cod_original_formula_sum        'C102.10 H86.20 B Cl2.20 F24 N O10'
_cod_database_code               1563138
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.997
_shelx_shelxl_version_number     2018/3
_platon_squeeze_void_probe_radius 1.2