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_7125644
_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         'C36 H48 N6 O5'
_chemical_formula_sum            'C36 H48 N6 O5'
_chemical_formula_weight         644.80
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-17 deposited with the CCDC.	2019-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.795(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4230(3)
_cell_length_b                   20.3482(7)
_cell_length_c                   17.1498(7)
_cell_measurement_reflns_used    4862
_cell_measurement_temperature    292.8(3)
_cell_measurement_theta_max      73.0560
_cell_measurement_theta_min      3.4370
_cell_volume                     3482.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      292.8(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2262
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.968
_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    -66.00  11.00   1.00    3.45    --  -41.49  38.00-120.00   77
  2  \w   -100.00 -42.00   1.00    3.45    --  -41.49 -38.00  30.00   58
  3  \w     15.00  49.00   1.00    3.45    --   41.49  57.00 -60.00   34
  4  \w     23.00  60.00   1.00    3.45    --   41.49-125.00   0.00   37
  5  \w     67.00 115.00   1.00    3.45    --   41.49  57.00 -60.00   48
  6  \w     78.00 142.00   1.00   13.80    --  106.19  30.00-180.00   64
  7  \w     82.00 177.00   1.00   13.80    --  106.19  45.00  30.00   95
  8  \w     61.00 154.00   1.00   13.80    --  106.19 -15.00-180.00   93
  9  \w     53.00 118.00   1.00   13.80    --  106.19 -30.00   0.00   65
 10  \w     34.00 127.00   1.00   13.80    --  106.19 -61.00-120.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0281364000
_diffrn_orient_matrix_UB_12      -0.0460990000
_diffrn_orient_matrix_UB_13      0.0742790000
_diffrn_orient_matrix_UB_21      0.1289369000
_diffrn_orient_matrix_UB_22      0.0387085000
_diffrn_orient_matrix_UB_23      0.0410082000
_diffrn_orient_matrix_UB_31      -0.0798024000
_diffrn_orient_matrix_UB_32      0.0460082000
_diffrn_orient_matrix_UB_33      0.0401136000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13883
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.700
_diffrn_reflns_theta_min         3.459
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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 white'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.311
_exptl_crystal_size_min          0.155
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         6803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0728
_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^)+(0.1344P)^2^+1.0817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5139
_reflns_number_total             6803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08906c2.cif
_cod_data_source_block           exp_1235
_cod_depositor_comments
'Adding full bibliography for 7125644--7125647.cif.'
_cod_database_code               7125644
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'c36 h48 n6 o5'
_chemical_oxdiff_usercomment     CJH-8-176
_reflns_odcompleteness_completeness 99.83
_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(O32B)=Sof(H30A)=Sof(H30B)=Sof(H33C)=Sof(H33D)=Sof(H31C)=Sof(H31D)=
 Sof(C45B)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C46B)=Sof(H46D)=Sof(H46E)=
 Sof(H46F)=Sof(C47B)=Sof(H47D)=Sof(H47E)=Sof(H47F)=Sof(C27B)=Sof(H27C)=
 Sof(H27D)=Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(O29B)=1-FVAR(1)
 Sof(O32A)=Sof(H30C)=Sof(H30D)=Sof(H33A)=Sof(H33B)=Sof(H31A)=Sof(H31B)=
 Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C46A)=Sof(H46A)=Sof(H46B)=
 Sof(H46C)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C27A)=Sof(H27A)=
 Sof(H27B)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(O29A)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C4(H4A,H4B), C20(H20A,H20B), C14(H14A,H14B), C37(H37A,H37B),
 C36(H36A,H36B), C30(H30C,H30D), C30(H30A,H30B), C34(H34A,H34B), C33(H33A,H33B),
  C33(H33C,H33D), C31(H31A,H31B), C31(H31C,H31D), C27A(H27A,H27B), C27B(H27C,
 H27D), C28A(H28A,H28B), C28B(H28C,H28D)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C12(H12), C8(H8), C6(H6), C16(H16), C2(H2)
3.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45A(H45A,H45B,
 H45C), C45B(H45D,H45E,H45F), C46A(H46A,H46B,H46C), C46B(H46D,H46E,H46F),
 C47A(H47A,H47B,H47C), C47B(H47D,H47E,H47F)
;
_shelx_res_checksum              78942
_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 1.625
_oxdiff_exptl_absorpt_empirical_full_min 0.565