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_1563135
_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         'C85 H100 O10'
_chemical_formula_sum            'C85 H100 O10'
_chemical_formula_weight         1281.64
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-08-26T18:18:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-09-21 deposited with the CCDC.	2021-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.334(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.909(5)
_cell_length_b                   34.548(3)
_cell_length_c                   18.6270(7)
_cell_measurement_reflns_used    53245
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.74
_cell_measurement_theta_min      1.161
_cell_volume                     7018(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_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  0.0488
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            121074
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         1.161
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       needle
_exptl_crystal_F_000             2760
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/dichloromethane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0025(2)
_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   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         20580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+11.5003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1869
_refine_ls_wR_factor_ref         0.2038
_reflns_Friedel_coverage         0
_reflns_number_gt                15686
_reflns_number_total             20580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02199k2.cif
_cod_data_source_block           x4esxt-28jan232052_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1563135
_shelx_estimated_absorpt_t_min   0.993
_shelx_estimated_absorpt_t_max   0.999
_shelx_shelxl_version_number     2018/3