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_7219367
_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         'C68 H84 N6 O11 S4, 0.5(H2 O), 1.5(C H Cl3)'
_chemical_formula_sum            'C69.5 H86.5 Cl4.5 N6 O11.5 S4'
_chemical_formula_weight         1477.71
_chemical_melting_point          479.0(10)
_chemical_name_systematic
; 
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-10-09 deposited with the CCDC.
2015-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5063(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.8935(13)
_cell_length_b                   23.9302(16)
_cell_length_c                   33.589(2)
_cell_measurement_reflns_used    23432
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      25.93
_cell_measurement_theta_min      2.26
_cell_volume                     15181.2(17)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            134900
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.479
_diffrn_reflns_theta_min         1.373
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.792
_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    1.293
_exptl_crystal_description       block
_exptl_crystal_F_000             6224
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform'
_exptl_crystal_size_max          0.710
_exptl_crystal_size_mid          0.540
_exptl_crystal_size_min          0.320
_platon_squeeze_details
;
One chloroform in each of the smaller voids, two in the larger
ones. 8 squeezed per unit cell in total.
;
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1903
_refine_ls_number_reflns         31218
_refine_ls_number_restraints     465
_refine_ls_restrained_S_all      2.451
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0991P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19539
_reflns_number_total             31218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ra15905e2.cif
_cod_data_source_block           4b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '478-480' was changed to '479.0(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        'C69.50 H86.50 Cl4.50 N6 O11.50 S4'
_cod_database_code               7219367
_shelx_estimated_absorpt_t_min   0.792
_shelx_estimated_absorpt_t_max   0.898
_shelxl_version_number           2013-4