Prismarenes: A New Class of Macrocyclic Hosts Obtained by Templation in a Thermodynamically Controlled Synthesis.
Della Sala, Paolo; Del Regno, Rocco; Talotta, Carmen; Capobianco, Amedeo; Hickey, Neal; Geremia, Silvano; De Rosa, Margherita; Spinella, Aldo; Soriente, Annunziata; Neri, Placido; Gaeta, Carmine; Journal of the American Chemical Society 142 (2020) 1752–1756; doi:10.1021/jacs.9b12216

data_4133962
_publ_section_title
;
 Prismarenes: A New Class of Macrocyclic Hosts Obtained by Templation in a
 Thermodynamically Controlled Synthesis.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1752
_journal_page_last               1756
_journal_paper_doi               10.1021/jacs.9b12216
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C65 H60 O10, 1.9 (C H2 Cl2)'
_chemical_formula_sum            'C66.9 H63.8 Cl3.8 O10'
_chemical_formula_weight         1162.49
_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
_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             2019-09-02T11:47:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-09-02 deposited with the CCDC.	2019-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                107.381(3)
_cell_angle_beta                 86.900(10)
_cell_angle_gamma                99.769(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3230(15)
_cell_length_b                   13.7720(8)
_cell_length_c                   21.1170(6)
_cell_measurement_reflns_used    41031
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.13
_cell_measurement_theta_min      0.99
_cell_measurement_wavelength     0.7
_cell_volume                     2823.5(5)
_computing_cell_refinement       'XDS (Kabasch 2010)'
_computing_data_collection       'Elettra XRD1 Data Collectipon SW'
_computing_data_reduction        XDS
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.895
_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  0.0184
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            53513
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.089
_diffrn_reflns_theta_min         0.995
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0187(9)
_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   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     765
_refine_ls_number_reflns         15564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0619P)^2^+1.5206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0
_reflns_number_gt                13742
_reflns_number_total             15564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12216_si_003.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4133958--4133962.cif.'
_cod_original_formula_sum        'C66.90 H63.80 Cl3.80 O10'
_cod_database_code               4133962