Benzenebistriazole-strapped calix[4]pyrrole: a neutral anion receptor with CH and NH donor groups that exhibits high sulfate binding affinity and selectivity in aqueous solutions.
He, Ying-Chun; Yan, Yan-Mei; Tong, Hong-Bo; Ren, Zhen-Xing; Wang, Jun-Hong; Zhang, Yong-Bin; Chao, Jian-Bin; Wang, Meng-Liang; Chemical communications (Cambridge, England) 56 (2020) 9364–9367; doi:10.1039/d0cc03655b

data_7126788
_publ_section_title
;
 Benzenebistriazole-strapped calix[4]pyrrole: a neutral anion receptor
 with CH and NH donor groups that exhibits high sulfate binding affinity
 and selectivity in aqueous solutions.
;
_journal_issue                   65
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9364
_journal_page_last               9367
_journal_paper_doi               10.1039/d0cc03655b
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C44 H52 N10, 2(C3 H7 N O), H2 O'
_chemical_formula_sum            'C50 H68 N12 O3'
_chemical_formula_weight         885.16
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-12-10
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-12 deposited with the CCDC.	2020-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                77.860(2)
_cell_angle_beta                 79.348(2)
_cell_angle_gamma                82.174(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4540(4)
_cell_length_b                   11.2457(5)
_cell_length_c                   22.6586(9)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      3.05
_cell_volume                     2546.20(18)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      297.09
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40084
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         3.020
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0908 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.9246.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.054(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         8916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+1.4684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7156
_reflns_number_total             8916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03655b2.cif
_cod_data_source_block           test-2_a
_cod_depositor_comments
'Adding full bibliography for 7126788--7126789.cif.'
_cod_database_code               7126788
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 C50(H3B,H3C)
2.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C9(H9), C10(H10), C15(H15), C16(H16), C22(H22), C23(H23),
 C31(H31), C34(H34), C36(H36), C37(H37), C38(H38), C40(H40), C45(H45), C48(H48)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              82064
_shelx_hkl_checksum              81090
_olex2_submission_special_instructions 'No special instructions were received'