Chiral anion recognition by a ureido-thiacalix[4]arene ligand immobilized in the 1,3-alternate conformation
Mačková, Michaela; Mikšátko, Jiří; Budka, Jan; Eigner, Václav; Cuřínová, Petra; Lhoták, Pavel; New J. Chem. 39 (2015) 1382–; doi:10.1039/C4NJ01956C

data_7054581
_publ_section_title
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 Chiral anion recognition by a ureido-thiacalix[4]arene ligand immobilized
 in the 1,3-alternate conformation
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_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1382
_journal_paper_doi               10.1039/C4NJ01956C
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C36 H20.00 N4 O12 S4'
_chemical_formula_sum            'C36 H20 N4 O12 S4'
_chemical_formula_weight         828.84
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.953(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2845(12)
_cell_length_b                   18.1827(17)
_cell_length_c                   18.8706(19)
_cell_measurement_reflns_used    15913
_cell_measurement_temperature    180
_cell_measurement_theta_max      77
_cell_measurement_theta_min      5
_cell_volume                     3722.8(7)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.111
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            41863
_diffrn_reflns_theta_full        73.144
_diffrn_reflns_theta_max         76.994
_diffrn_reflns_theta_min         4.746
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.951
_exptl_absorpt_correction_T_max  0.65
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.145
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.75
_refine_ls_extinction_coef       42(4)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9798
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3857
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.1094
_refine_ls_shift/su_max          0.0035863
_refine_ls_shift/su_mean         0.0005259
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.247E+04 0.388E+04 0.223E+04 843. 160. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2180
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2180
_reflns_limit_h_max              13
_reflns_limit_h_min              -14
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                3203
_reflns_number_total             3857
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.55
_oxford_diffrn_Wilson_scale      0.15
_oxford_refine_ls_r_factor_ref   0.1203
_oxford_refine_ls_scale          2.47(5)
_oxford_reflns_number_all        3857
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c4nj01956c1.cif
_cod_data_source_block           4f
_cod_depositor_comments
'Adding full bibliography for 7054576--7054583.cif.'
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C36 H20.00 N4 O12 S4'
_cod_database_code               7054581
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
CONT EXTPARAM 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 211,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   ( 121,X'S) H   (1212,X'S) H   (1211,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.440000 , 0.050000 = O(20) TO C(21) 
DISTANCE 1.460000 , 0.050000 = C(21) TO C(22) 
DISTANCE 1.160000 , 0.050000 = C(22) TO C(23) 
ANGLE 109.000000 , 1.000000 = O(20) TO C(21) TO C(22) 
DISTANCE 2.620000 , 0.050000 = C(21) TO C(23) 
DISTANCE 1.440000 , 0.050000 = O(20) TO C(121) 
DISTANCE 1.460000 , 0.050000 = C(121) TO C(122) 
DISTANCE 1.160000 , 0.050000 = C(122) TO C(123) 
ANGLE 109.000000 , 1.000000 = O(20) TO C(121) TO C(122) 
DISTANCE 2.620000 , 0.050000 = C(121) TO C(123) 
U(IJ)'S  0.0, 0.001000 = C(21) TO C(121) 
END                                                                             
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