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_4133960
_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_sum            'C65 H60 O10'
_chemical_formula_weight         1001.13
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_creation_date             2019-03-07T18:51:14-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-03-07 deposited with the CCDC.	2019-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.3(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.777(8)
_cell_length_b                   32.962(13)
_cell_length_c                   19.166(7)
_cell_measurement_reflns_used    47231
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      24.43
_cell_measurement_theta_min      1.2
_cell_measurement_wavelength     0.7
_cell_volume                     10596(8)
_computing_cell_refinement       'XDS, Kabasch 2010'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        XDS
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_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      373(2)
_diffrn_measured_fraction_theta_full 0.8
_diffrn_measured_fraction_theta_max 0.794
_diffrn_measurement_device       'Area Dettector'
_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  0.063
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_Laue_measured_fraction_full 0.8
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            106357
_diffrn_reflns_point_group_measured_fraction_full 0.8
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.435
_diffrn_reflns_theta_min         1.196
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.08
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             4240
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0146(10)
_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   1.02
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1406
_refine_ls_number_reflns         106357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.089
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1009P)^2^+6.6166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2247
_refine_ls_wR_factor_ref         0.2667
_reflns_Friedel_coverage         0
_reflns_number_gt                57727
_reflns_number_total             106357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12216_si_005.cif
_cod_data_source_block           shelxt_a
_cod_depositor_comments
'Adding full bibliography for 4133958--4133962.cif.'
_cod_original_cell_volume        10596(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4133960