Synthesis and Aqueous Anion Recognition of Imidazolium-Based Nonacationic Cup
Wang, Pinpin; Liu, Kai; Ma, Huanqing; Nian, Hao; Li, Yawen; Li, Qingfang; Cheng, Lin; Cao, Liping; Chemical Communications  (2021) –; doi:10.1039/D1CC05603D

data_7129273
_publ_section_title
;
 Synthesis and Aqueous Anion Recognition of Imidazolium-Based Nonacationic
 Cup
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05603D
_journal_year                    2021
_chemical_formula_moiety         'C84 H81 N18, 9(Cl), 9(C H2 Cl2)'
_chemical_formula_sum            'C93 H99 Cl27 N18'
_chemical_formula_weight         2426.05
_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
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc26yv67
_audit_creation_date             2020-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-07 deposited with the CCDC.	2021-11-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.615(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3833(6)
_cell_length_b                   20.8000(8)
_cell_length_c                   37.6802(15)
_cell_measurement_reflns_used    9613
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      54.87
_cell_measurement_theta_min      2.66
_cell_volume                     12778.8(8)
_computing_cell_refinement       'SAINT V8.38A (bruker, 2016)'
_computing_data_collection       'APEX3 v.2017.3-0 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1921
_diffrn_reflns_av_unetI/netI     0.0675
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            185754
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        52.998
_diffrn_reflns_theta_max         52.998
_diffrn_reflns_theta_min         2.050
_diffrn_source                   'Liquid METALJET D2 PLUS X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.686
_exptl_absorpt_correction_T_max  0.7365
_exptl_absorpt_correction_T_min  0.4620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for 
absorption correction. The 
Ratio of minimum to maximum transmission is 
0.6273. The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       block
_exptl_crystal_F_000             4968
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.698
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.686
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1027
_refine_ls_number_reflns         22518
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.686
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.1187
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3759
_refine_ls_wR_factor_ref         0.3936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18713
_reflns_number_total             22518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05603d2.cif
_cod_data_source_block           2
_cod_database_code               7129273
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.526
_shelx_estimated_absorpt_t_min   0.320
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl1A) = Uanis(Cl0A)
3. Others
 1*[Sof(H02V)+Sof(H02W)+Sof(H02X)+Sof(H02Y)+Sof(Cl2)]+1*[Sof(Cl0A)]+1*
 [Sof(Cl1A)]=1 with esd of 0.001
 Sof(H02X)=Sof(H02Y)=1-FVAR(1)
 Sof(H02V)=Sof(H02W)=Sof(Cl2)=FVAR(1)
 Sof(Cl3)=1-FVAR(4)
 Sof(Cl1)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C013(H01A,H01B), C01F(H01G,H01H), C01G(H01I,H01J), C01L(H01M,H01N), C01S(H01T,
 H01U), C01T(H01V,H01W), C023(H02A,H02B), C026(H02C,H02D), C02G(H02I,H02J),
 C02J(H02L,H02M), C02U(H02V,H02W), C02U(H02X,H02Y), C036(H03A,H03B)
4.b Me refined with riding coordinates:
 C01V(H01Y,H,HA)
4.c Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00S(H00S), C00T(H00T), C00V(H00V), C00W(H00W), C00Z(H00Z),
 C010(H010), C016(H016), C018(H018), C01B(H01C), C01C(H01D), C01D(H01E),
 C01E(H01F), C01H(H01K), C01J(H01L), C01N(H01O), C01O(H01P), C01P(H01Q),
 C01Q(H01R), C01R(H01S), C01U(H01X), C01X(H01Z), C01Y(H01), C01Z(H0AA),
 C020(H020), C021(H021), C024(H024), C027(H027), C028(H028), C02F(H02H),
 C02I(H02K), C02L(H02Q), C02M(H02R), C02O(H02S), C02Q(H02T), C02R(H02U),
 C02V(H02Z), C02W(H02), C02Y(H1AA), C030(H030), C031(H031), C033(H033),
 C035(H035), C037(H037), C038(H038), C03B(H03C), C03D(H03D), C03G(H03G)
4.d Idealised Me refined as rotating group:
 C02B(H02E,H02F,H02G), C02K(H02N,H02O,H02P)
;
_smtbx_masks_special_details     36(CH2Cl2)
_shelx_res_checksum              11566
_shelx_hkl_checksum              46708
_shelx_fab_checksum              84269
_olex2_submission_special_instructions 'No special instructions were received'