A study of anion binding behaviour of 1,3-alternate thiacalix[4]arene-based receptors bearing urea moieties
Rahman, Shofiur; Tomiyasu, Hirotsugu; Kawazoe, Hiroto; Zhao, Jiang-Lin; Cong, Hang; Ni, Xin-Long; Zeng, Xi; Elsegood, Mark R. J.; Warwick, Thomas G.; Teat, Simon J.; Redshaw, Carl; Georghiou, Paris E.; Yamato, Takehiko; New J. Chem. 40 (2016) 9245–; doi:10.1039/C6NJ00923A

data_7055760
_publ_section_title
;
 A study of anion binding behaviour of 1,3-alternate
 thiacalix[4]arene-based receptors bearing urea moieties
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              9245
_journal_paper_doi               10.1039/C6NJ00923A
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety
'C144 H160 N8 O12 S8, C16 H36 N 1+, Cl 1-, 0.5(C H Cl3), C2 H3 N'
_chemical_formula_sum            'C162.5 H199.5 Cl2.5 N10 O12 S8'
_chemical_formula_weight         2829.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-12 deposited with the CCDC.
2016-09-08 downloaded from the CCDC.
;
_cell_angle_alpha                104.778(2)
_cell_angle_beta                 94.065(2)
_cell_angle_gamma                92.353(2)
_cell_formula_units_Z            4
_cell_length_a                   15.1315(5)
_cell_length_b                   28.8618(11)
_cell_length_c                   35.9491(13)
_cell_measurement_reflns_used    9728
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.31
_cell_volume                     15113.8(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\w/\q shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            116001
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.291
_diffrn_reflns_theta_max         25.291
_diffrn_reflns_theta_min         2.024
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2012/1, Sheldrick, G.M., (2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6044
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform/acetonitrile'
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.781
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3705
_refine_ls_number_reflns         42128
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0834P)^2^+25.3467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27707
_reflns_number_total             42128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj00923a2.cif
_cod_data_source_block           4a
_cod_depositor_comments          'Adding full bibliography for 7055760.cif.'
_cod_original_cell_volume        15113.8(9)
_cod_original_formula_sum        'C162.50 H199.50 Cl2.50 N10 O12 S8'
_cod_database_code               7055760
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              56182