Molecular recognition of pyrazine N,N′-dioxide using aryl extended calix[4]pyrroles
Guo, Chenxing; Wang, Hu; Lynch, Vincent M.; Ji, Xiaofan; Page, Zachariah A.; Sessler, Jonathan L.; Chemical Science 11 (2020) 5650–5657; doi:10.1039/D0SC01496F

data_1557829
_publ_section_title
;
 Molecular recognition of pyrazine N,N&#x2032;-dioxide using aryl extended
 calix[4]pyrroles
;
_journal_issue                   22
_journal_name_full               'Chemical Science'
_journal_page_first              5650
_journal_page_last               5657
_journal_paper_doi               10.1039/D0SC01496F
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         '2 C40 H38 N6, C4 H4 N2 O2, 2 C H4 O'
_chemical_formula_sum            'C86 H88 N14 O4'
_chemical_formula_weight         1381.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-02-20 deposited with the CCDC.	2020-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.327(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7110(7)
_cell_length_b                   12.6971(5)
_cell_length_c                   18.2586(7)
_cell_measurement_reflns_used    12900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      1.78
_cell_volume                     3822.9(3)
_computing_cell_refinement
'CrysAlisPro V 1.171.40.37a, Rigaku Oxford Diffraction'
_computing_data_collection       'CrystalClear 1.40 (Rigaku Inc., 2008)'
_computing_data_reduction
'CrysAlisPro V 1.171.40.37a, Rigaku Oxford Diffraction'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution
;

Sheldrick. G. M.  (2015) SHELXT. Acta Cryst. A71, 3-8.

;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Nonius Kappa CCD with a Bruker Apex II detector'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45512
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         1.804
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.37a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       prism
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         7000
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1016P)^2^+4.5981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2234
_refine_ls_wR_factor_ref         0.2381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5433
_reflns_number_total             7000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01496f3.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
;Adding full bibliography for 1557828--1557833.cif.

 Adding full bibliography for 1557828--1557833.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1557829
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              43078