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_4133961
_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, 3 (C H2 Cl2)'
_chemical_formula_sum            'C68 H66 Cl6 O10'
_chemical_formula_weight         1255.9
_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
_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             2019-09-02T12:16:24-00:00
_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                76.093(7)
_cell_angle_beta                 80.772(6)
_cell_angle_gamma                88.492(4)
_cell_formula_units_Z            2
_cell_length_a                   13.171(3)
_cell_length_b                   13.4040(13)
_cell_length_c                   17.6730(11)
_cell_measurement_reflns_used    39323
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      1.18
_cell_measurement_wavelength     0.7
_cell_volume                     2989.2(8)
_computing_cell_refinement       'XDS (kabasch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection 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 0.935
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device       'Area Detector'
_diffrn_measurement_device_type  'Dectril 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  0.0169
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47654
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         27.937
_diffrn_reflns_theta_min         1.184
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.33
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Flat Bars'
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0070(5)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     768
_refine_ls_number_reflns         13771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0540P)^2^+2.3805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0
_reflns_number_gt                12630
_reflns_number_total             13771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12216_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4133958--4133962.cif.'
_cod_original_cell_volume        2989.2(7)
_cod_database_code               4133961
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.993