Positive and negative allosteric effects of thiacalix[4]arene-based receptors having urea and crown‒ether moieties
Tomiyasu, Hirotsugu; Zhao, Jiang-Lin; Ni, Xin-Long; zeng, xi; Elsegood, Mark Robert James; Jones, Beth; Redshaw, Carl; Teat, Simon; Yamato, Takehiko; RSC Adv.  (2015) –; doi:10.1039/C4RA15905E

data_7219368
_publ_section_title
;
 Positive and negative allosteric effects of thiacalix[4]arene-based
 receptors having urea and crown--ether moieties
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA15905E
_journal_year                    2015
_chemical_formula_moiety         'C66 H78 N8 O15 S4, 0.5(C H Cl3), 3(C2 H3 N)'
_chemical_formula_sum            'C72.5 H87.5 Cl1.5 N11 O15 S4'
_chemical_formula_weight         1534.44
_chemical_melting_point          486.0(10)
_chemical_name_systematic
; 
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-10-09 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.384(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.7980(10)
_cell_length_b                   26.7870(16)
_cell_length_c                   32.552(2)
_cell_measurement_reflns_used    9617
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.35
_cell_measurement_theta_min      2.44
_cell_volume                     15423.1(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHTXTL'
_computing_publication_material  'Bruker SHTXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            155885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         34.779
_diffrn_reflns_theta_min         1.594
_diffrn_source                   'ALS Station 11.3.1'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.927
_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    1.322
_exptl_crystal_description       plate
_exptl_crystal_F_000             6472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chlorform/acetonitrile'
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.443
_refine_diff_density_min         -1.856
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2055
_refine_ls_number_reflns         50956
_refine_ls_number_restraints     656
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0863
_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^)+(0.1702P)^2^+8.5757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2650
_refine_ls_wR_factor_ref         0.2937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                35702
_reflns_number_total             50956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra15905e2.cif
_cod_data_source_block           4e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '485-487' was changed to '486.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C72.50 H87.50 Cl1.50 N11 O15 S4'
_cod_database_code               7219368
_shelx_estimated_absorpt_t_min   0.927
_shelx_estimated_absorpt_t_max   0.994
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014-3
_shelx_res_checksum              2723