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_1563137
_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         'C102  H120  O12, C7 H8'
_chemical_formula_sum            'C109 H128 O12'
_chemical_formula_weight         1630.11
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-07-31T11:44:21-00:00
_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                 104.36(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.308(9)
_cell_length_b                   30.108(18)
_cell_length_c                   23.23(3)
_cell_measurement_reflns_used    7807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.938
_cell_measurement_theta_min      1.332
_cell_measurement_wavelength     0.7
_cell_volume                     9017(16)
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_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  0.052
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6384
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        22.938
_diffrn_reflns_theta_max         22.938
_diffrn_reflns_theta_min         1.332
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3512
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane/toluene'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     569
_refine_ls_number_reflns         6384
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.0912
_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^)+(0.1699P)^2^+24.1533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2549
_refine_ls_wR_factor_ref         0.2983
_reflns_Friedel_coverage         0
_reflns_number_gt                4117
_reflns_number_total             6384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02199k2.cif
_cod_data_source_block           platon_tw_CCDC1
_cod_original_cell_volume        9017(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1563137
_shelx_estimated_absorpt_t_min   0.992
_shelx_estimated_absorpt_t_max   0.998
_shelx_shelxl_version_number     2018/3