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_7054578
_publ_section_title
;
 Chiral anion recognition by a ureido-thiacalix[4]arene ligand immobilized
 in the 1,3-alternate conformation
;
_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         'C44 H52 N4 O12 S4, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H58 N6 O12 S4'
_chemical_formula_weight         1039.29
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.24520(12)
_cell_length_b                   13.24520(12)
_cell_length_c                   14.9787(2)
_cell_measurement_reflns_used    6670
_cell_measurement_temperature    170
_cell_measurement_theta_max      77
_cell_measurement_theta_min      4
_cell_volume                     2627.79(5)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_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      170
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11942
_diffrn_reflns_theta_full        73.941
_diffrn_reflns_theta_max         77.022
_diffrn_reflns_theta_min         4.456
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.201
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096.000
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0650
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2754
_refine_ls_number_restraints     80
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.0180496
_refine_ls_shift/su_mean         0.0022868
_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: 
 0.435E+04 0.738E+04 0.448E+04 0.181E+04 381. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2601
_refine_ls_wR_factor_gt          0.2505
_refine_ls_wR_factor_ref         0.2601
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                2451
_reflns_number_total             2754
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.70
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0851
_oxford_refine_ls_scale          4.39(19)
_oxford_reflns_number_all        2754
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c4nj01956c1.cif
_cod_data_source_block           4c_solv
_cod_depositor_comments
'Adding full bibliography for 7054576--7054583.cif.'
_cod_original_sg_symbol_Hall     '-P 4bc '
_cod_original_sg_symbol_H-M      'P 42/n '
_cod_database_code               7054578
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  92,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) H   ( 122,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) H   ( 133,X'S) 
RIDE C   ( 109,X'S) H   (1092,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1102,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) H   (1112,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1122,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) H   (1133,X'S) H   (1132,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) H   ( 193,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DISTANCE 1.441000 , 0.005000 = O(8) TO C(9) 
DISTANCE 1.525000 , 0.005000 = C(9) TO C(10) 
DISTANCE 1.539000 , 0.005000 = C(10) TO C(11) 
DISTANCE 1.539000 , 0.005000 = C(11) TO C(12) 
DISTANCE 1.539000 , 0.005000 = C(12) TO C(13) 
ANGLE 109.000000 , 1.000000 = O(8) TO C(9) TO C(10) 
ANGLE 109.000000 , 1.000000 = C(9) TO C(10) TO C(11) 
ANGLE 109.000000 , 1.000000 = C(10) TO C(11) TO C(12) 
ANGLE 109.000000 , 1.000000 = C(11) TO C(12) TO C(13) 
DISTANCE 1.441000 , 0.005000 = O(8) TO C(109) 
DISTANCE 1.525000 , 0.005000 = C(109) TO C(110) 
DISTANCE 1.539000 , 0.005000 = C(110) TO C(111) 
DISTANCE 1.539000 , 0.005000 = C(111) TO C(112) 
DISTANCE 1.539000 , 0.005000 = C(112) TO C(113) 
ANGLE 109.000000 , 1.000000 = O(8) TO C(109) TO C(110) 
ANGLE 109.000000 , 1.000000 = C(109) TO C(110) TO C(111) 
ANGLE 109.000000 , 1.000000 = C(110) TO C(111) TO C(112) 
ANGLE 109.000000 , 1.000000 = C(111) TO C(112) TO C(113) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(9) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(10) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(11) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(12) 
U(IJ)'S  0.0, 0.010000 = O(8) TO C(13) 
U(IJ)'S  0.0, 0.001000 = C(9) TO C(109) 
U(IJ)'S  0.0, 0.010000 = C(10) TO C(110) 
U(IJ)'S  0.0, 0.010000 = C(11) TO C(111) 
U(IJ)'S  0.0, 0.001000 = C(12) TO C(112) 
U(IJ)'S  0.0, 0.001000 = C(13) TO C(113) 
END                                                                             
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