Crown ether-appended calix[2]triazolium[2]arene as a macrocyclic receptor for the recognition of the H<sub>2</sub>PO<sub>4</sub><sup>-</sup> anion.
Cho, Jihee; Verwilst, Peter; Kang, Minjung; Pan, Jia-Lin; Sharma, Amit; Hong, Chang Seop; Kim, Jong Seung; Kim, Sanghee; Chemical communications (Cambridge, England) 56 (2020) 1038–1041; doi:10.1039/c9cc08906c

data_7125645
_publ_section_title
;
 Crown ether-appended calix[2]triazolium[2]arene as a macrocyclic receptor
 for the recognition of the H<sub>2</sub>PO<sub>4</sub><sup>-</sup> anion.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1038
_journal_page_last               1041
_journal_paper_doi               10.1039/c9cc08906c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C38 H52 N6 O6'
_chemical_formula_sum            'C38 H52 N6 O6'
_chemical_formula_weight         688.85
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2019-05-17 deposited with the CCDC.	2019-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.284(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4036(2)
_cell_length_b                   19.8880(4)
_cell_length_c                   18.5228(4)
_cell_measurement_reflns_used    13444
_cell_measurement_temperature    292(3)
_cell_measurement_theta_max      73.6520
_cell_measurement_theta_min      2.2060
_cell_volume                     3729.95(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2262
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -65.00  33.00   1.00    1.03    --  -41.24  38.00 -30.00   98
  2  \w     80.00 116.00   1.00    1.03    --   41.24  38.00 150.00   36
  3  \w     20.00 117.00   1.00    1.03    --   41.24  77.00 -60.00   97
  4  \w      2.00  80.00   1.00    1.03    --   41.24 -99.00 150.00   78
  5  \w      9.00  43.00   1.00    1.03    --   41.24  77.00 -90.00   34
  6  \w     45.00  89.00   1.00    1.03    --   41.24-125.00 -30.00   44
  7  \w     79.00 117.00   1.00    1.03    --   41.24  77.00 -90.00   38
  8  \w    101.00 176.00   1.00    4.11    --  106.19  79.00-132.00   75
  9  \w     80.00 178.00   1.00    4.11    --  106.19  30.00  30.00   98
 10  \w     34.00 138.00   1.00    4.11    --  106.19 -77.00  60.00  104
 11  \w     77.00 117.00   1.00    4.11    --  106.19 -61.00-120.00   40
 12  \w     33.00 131.00   1.00    4.11    --  106.19 -45.00  90.00   98
 13  \w     64.00  91.00   1.00    4.11    --  106.19 -94.00-180.00   27
 14  \w    124.00 172.00   1.00    4.11    --  106.19 125.00   0.00   48
 15  \w    115.00 148.00   1.00    4.11    --  106.19 125.00  30.00   33
 16  \w     80.00 112.00   1.00    4.11    --  106.19  61.00 -30.00   32
 17  \w     48.00 121.00   1.00    4.11    --  106.19-125.00  60.00   73
 18  \w     78.00 178.00   1.00    4.11    --  106.19  61.00-180.00  100
 19  \w     29.00 138.00   1.00    4.11    --  106.19   0.00  30.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0793376000
_diffrn_orient_matrix_UB_12      -0.0640492000
_diffrn_orient_matrix_UB_13      -0.0281009000
_diffrn_orient_matrix_UB_21      0.0078177000
_diffrn_orient_matrix_UB_22      0.0170250000
_diffrn_orient_matrix_UB_23      -0.0800152000
_diffrn_orient_matrix_UB_31      0.1295130000
_diffrn_orient_matrix_UB_32      -0.0401350000
_diffrn_orient_matrix_UB_33      0.0106596000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28406
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.921
_diffrn_reflns_theta_min         3.309
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.201
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.685
_exptl_crystal_size_mid          0.462
_exptl_crystal_size_min          0.344
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         7434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0643
_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^)+(0.1119P)^2^+1.2650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.1986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6383
_reflns_number_total             7434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08906c2.cif
_cod_data_source_block           exp_1255
_cod_depositor_comments
'Adding full bibliography for 7125644--7125647.cif.'
_cod_database_code               7125645
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'c36 H52 N6 O6'
_chemical_oxdiff_usercomment     CJH-10-118
_shelx_estimated_absorpt_t_max   0.801
_shelx_estimated_absorpt_t_min   0.654
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(O30A)=Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(H31C)=Sof(H31D)=Sof(C9B)=
 Sof(H9BA)=Sof(H9BB)=1-FVAR(1)
 Sof(O30B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H31A)=Sof(H31B)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C41(H41A,H41B), C2(H2A,H2B), C12(H12A,H12B), C40(H40A,H40B),
 C16(H16A,H16B), C38(H38A,H38B), C34(H34A,H34B), C32(H32A,H32B), C37(H37A,H37B),
  C35(H35A,H35B), C28A(H28A,H28B), C28B(H28C,H28D), C31(H31A,H31B), C31(H31C,
 H31D), C9A(H9AA,H9AB), C9B(H9BA,H9BB)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C26(H26), C4(H4), C24(H24), C18(H18)
3.c Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C45(H45A,H45B,H45C), C50(H50A,H50B,
 H50C), C46(H46A,H46B,H46C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              24743
_olex2_date_sample_data_collection 2018-05-28
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.701
_oxdiff_exptl_absorpt_empirical_full_min 0.608