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_1563140
_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
'C78 H72 O12, C8 H20 N, C32 H12 B F24, 3.575(C H2 Cl2)'
_chemical_formula_sum            'C121.57 H111.15 B Cl7.15 F24 N O12'
_chemical_formula_weight         2498.44
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      64
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c e'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-12-15T15:13:41-00:00
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.824(14)
_cell_length_b                   30.10(3)
_cell_length_c                   26.489(7)
_cell_measurement_reflns_used    27088
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.578
_cell_measurement_theta_min      0.891
_cell_volume                     27766(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.71
_diffrn_measured_fraction_theta_max 0.71
_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  0.046
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.71
_diffrn_reflns_Laue_measured_fraction_max 0.71
_diffrn_reflns_number            79718
_diffrn_reflns_point_group_measured_fraction_full 0.71
_diffrn_reflns_point_group_measured_fraction_max 0.71
_diffrn_reflns_theta_full        21.578
_diffrn_reflns_theta_max         21.578
_diffrn_reflns_theta_min         1.161
_exptl_absorpt_coefficient_mu    0.225
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_description       prism
_exptl_crystal_F_000             10289
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane/dichloromethane'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0030(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.607
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         6110
_refine_ls_number_restraints     804
_refine_ls_restrained_S_all      1.545
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.176
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+56.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4399
_refine_ls_wR_factor_ref         0.4581
_reflns_Friedel_coverage         0
_reflns_number_gt                4689
_reflns_number_total             6110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02199k2.cif
_cod_data_source_block           platon_sq_CCDC2
_cod_original_cell_volume        27770(30)
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_sg_symbol_H-M      'C m c a'
_cod_database_code               1563140
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.996
_shelx_shelxl_version_number     2018/3
_platon_squeeze_void_probe_radius 1.2