Triazole-bearing calixpyrroles: strong halide binding affinities through multiple N-H and C-H hydrogen bonds.
Kim, Hyeongcheol; Hong, Kyeong-Im; Lee, Jeong Heon; Kang, Philjae; Choi, Moon-Gun; Jang, Woo-Dong; Chemical communications (Cambridge, England) 54 (2018) 10863–10865; doi:10.1039/c8cc06385k

data_7122307
_publ_section_title
;
 Triazole-bearing calixpyrroles: strong halide binding affinities through
 multiple N-H and C-H hydrogen bonds.
;
_journal_issue                   77
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10863
_journal_page_last               10865
_journal_paper_doi               10.1039/c8cc06385k
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C44 H46 N10'
_chemical_formula_sum            'C44 H46 N10'
_chemical_formula_weight         714.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     direct
_audit_creation_date             2017-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-06-16 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.95(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.546(3)
_cell_length_b                   27.351(6)
_cell_length_c                   11.169(2)
_cell_measurement_reflns_used    70848
_cell_measurement_temperature    100
_cell_measurement_theta_max      50.00
_cell_measurement_theta_min      0.57
_cell_volume                     3823.5(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.749
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.749
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            29162
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.749
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         33.325
_diffrn_reflns_theta_min         1.749
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   Multi-scans
_exptl_absorpt_process_details   HKL3000
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         15928
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1158P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1509
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11445
_reflns_number_total             15928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06385k2.cif
_cod_data_source_block           calixpyrrole_trans
_cod_depositor_comments
'Adding full bibliography for 7122306--7122307.cif.'
_cod_original_cell_volume        3823.5(13)
_cod_database_code               7122307
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of
0.00001
Uanis(C2) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of 0
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C40(H40A,H40B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N8(H8), N14(H14), N20(H20), C3(H3), C4(H4), C10(H10), C11(H11),
 C16(H16), C17(H17), C22(H22), C23(H23), C30(H30), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51)
3.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C)
;
_olex2_submission_special_instructions 'No special instructions were received'