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_7054577
_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'
_chemical_formula_sum            'C44 H52 N4 O12 S4'
_chemical_formula_weight         957.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2014-11-26 deposited with the CCDC.
2014-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                101.125(7)
_cell_angle_beta                 95.076(6)
_cell_angle_gamma                102.421(7)
_cell_formula_units_Z            2
_cell_length_a                   11.0672(8)
_cell_length_b                   12.3077(11)
_cell_length_c                   18.3099(11)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    170
_cell_measurement_theta_max      76
_cell_measurement_theta_min      5
_cell_volume                     2367.8(3)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         101
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.947
_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  0.039
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25548
_diffrn_reflns_theta_full        67.68
_diffrn_reflns_theta_max         76.222
_diffrn_reflns_theta_min         4.521
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.383
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         8878
_refine_ls_number_restraints     219
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.0020363
_refine_ls_shift/su_mean         0.0000763
_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: 
 0.394E+04 0.668E+04 0.417E+04 0.178E+04 409. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2130
_refine_ls_wR_factor_gt          0.1779
_refine_ls_wR_factor_ref         0.1960
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                7463
_reflns_number_total             9372
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.75
_oxford_diffrn_Wilson_scale      0.05
_oxford_refine_ls_r_factor_ref   0.0709
_oxford_refine_ls_scale          4.81(9)
_oxford_reflns_number_all        9372
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c4nj01956c1.cif
_cod_data_source_block           4c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 7054576--7054583.cif.
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7054577
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
EQUIVALENCE PART(1001, OCC) PART(1002, OCC) 
WEIGHT -1 PART(1002, OCC) 
EQUIVALENCE PART(2001, OCC) PART(2002, OCC) 
WEIGHT -1 PART(2002, OCC) 
EQUIVALENCE PART(3001, OCC) PART(3002, OCC) 
WEIGHT -1 PART(3002, OCC) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  30,X'S) H   ( 302,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) H   ( 332,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) H   ( 343,X'S) H   ( 342,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 372,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) H   ( 382,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) H   ( 392,X'S) 
RIDE C   (  40,X'S) H   ( 403,X'S) H   ( 401,X'S) H   ( 402,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) H   ( 422,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) H   ( 432,X'S) 
RIDE C   (  44,X'S) H   ( 442,X'S) H   ( 441,X'S) 
RIDE C   (  45,X'S) H   ( 452,X'S) H   ( 451,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) H   ( 463,X'S) H   ( 462,X'S) 
RIDE C   (  48,X'S) H   ( 482,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 493,X'S) H   ( 492,X'S) H   ( 491,X'S) H   ( 494,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) H   ( 502,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) H   ( 512,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) H   ( 522,X'S) H   ( 523,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) H   (1362,X'S) 
RIDE C   ( 137,X'S) H   (1372,X'S) H   (1371,X'S) 
RIDE C   ( 138,X'S) H   (1382,X'S) H   (1381,X'S) 
RIDE C   ( 139,X'S) H   (1392,X'S) H   (1391,X'S) 
RIDE C   ( 140,X'S) H   (1401,X'S) H   (1403,X'S) H   (1402,X'S) 
RIDE C   ( 142,X'S) H   (1422,X'S) H   (1421,X'S) 
RIDE C   ( 143,X'S) H   (1431,X'S) H   (1432,X'S) 
RIDE C   ( 144,X'S) H   (1441,X'S) H   (1442,X'S) 
RIDE C   ( 145,X'S) H   (1451,X'S) H   (1452,X'S) 
RIDE C   ( 146,X'S) H   (1462,X'S) H   (1461,X'S) H   (1463,X'S) 
RIDE C   ( 150,X'S) H   (1502,X'S) H   (1501,X'S) 
RIDE C   ( 151,X'S) H   (1511,X'S) H   (1512,X'S) 
RIDE C   ( 152,X'S) H   (1522,X'S) H   (1523,X'S) H   (1521,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(35) TO C(36) 
DISTANCE 1.525000 , 0.005000 = C(36) TO C(37) 
DISTANCE 1.539000 , 0.005000 = C(37) TO C(38) 
DISTANCE 1.539000 , 0.005000 = C(38) TO C(39) 
DISTANCE 1.539000 , 0.005000 = C(39) TO C(40) 
ANGLE 109.000000 , 1.000000 = O(35) TO C(36) TO C(37) 
ANGLE 109.000000 , 1.000000 = C(36) TO C(37) TO C(38) 
ANGLE 109.000000 , 1.000000 = C(37) TO C(38) TO C(39) 
ANGLE 109.000000 , 1.000000 = C(38) TO C(39) TO C(40) 
DISTANCE 1.441000 , 0.005000 = O(35) TO C(136) 
DISTANCE 1.525000 , 0.005000 = C(136) TO C(137) 
DISTANCE 1.539000 , 0.005000 = C(137) TO C(138) 
DISTANCE 1.539000 , 0.005000 = C(138) TO C(139) 
DISTANCE 1.539000 , 0.005000 = C(139) TO C(140) 
ANGLE 109.000000 , 1.000000 = O(35) TO C(136) TO C(137) 
ANGLE 109.000000 , 1.000000 = C(136) TO C(137) TO C(138) 
ANGLE 109.000000 , 1.000000 = C(137) TO C(138) TO C(139) 
ANGLE 109.000000 , 1.000000 = C(138) TO C(139) TO C(140) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(36) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(37) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(38) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(39) 
U(IJ)'S  0.0, 0.010000 = O(35) TO C(40) 
U(IJ)'S  0.0, 0.001000 = C(36) TO C(136) 
U(IJ)'S  0.0, 0.001000 = C(37) TO C(137) 
U(IJ)'S  0.0, 0.001000 = C(38) TO C(138) 
U(IJ)'S  0.0, 0.010000 = C(39) TO C(139) 
U(IJ)'S  0.0, 0.010000 = C(40) TO C(140) 
DISTANCE 1.441000 , 0.005000 = O(41) TO C(42) 
DISTANCE 1.525000 , 0.005000 = C(42) TO C(43) 
DISTANCE 1.539000 , 0.005000 = C(43) TO C(44) 
DISTANCE 1.539000 , 0.005000 = C(44) TO C(45) 
DISTANCE 1.539000 , 0.005000 = C(45) TO C(46) 
ANGLE 109.000000 , 1.000000 = O(41) TO C(42) TO C(43) 
ANGLE 109.000000 , 1.000000 = C(42) TO C(43) TO C(44) 
ANGLE 109.000000 , 1.000000 = C(43) TO C(44) TO C(45) 
ANGLE 109.000000 , 1.000000 = C(44) TO C(45) TO C(46) 
DISTANCE 1.441000 , 0.005000 = O(41) TO C(142) 
DISTANCE 1.525000 , 0.005000 = C(142) TO C(143) 
DISTANCE 1.539000 , 0.005000 = C(143) TO C(144) 
DISTANCE 1.539000 , 0.005000 = C(144) TO C(145) 
DISTANCE 1.539000 , 0.005000 = C(145) TO C(146) 
ANGLE 109.000000 , 1.000000 = O(41) TO C(142) TO C(143) 
ANGLE 109.000000 , 1.000000 = C(142) TO C(143) TO C(144) 
ANGLE 109.000000 , 1.000000 = C(143) TO C(144) TO C(145) 
ANGLE 109.000000 , 1.000000 = C(144) TO C(145) TO C(146) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(42) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(43) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(44) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(45) 
U(IJ)'S  0.0, 0.010000 = O(41) TO C(46) 
U(IJ)'S  0.0, 0.001000 = C(42) TO C(142) 
U(IJ)'S  0.0, 0.001000 = C(43) TO C(143) 
U(IJ)'S  0.0, 0.001000 = C(44) TO C(144) 
U(IJ)'S  0.0, 0.001000 = C(45) TO C(145) 
U(IJ)'S  0.0, 0.001000 = C(46) TO C(146) 
DISTANCE 1.441000 , 0.005000 = O(47) TO C(48) 
DISTANCE 1.525000 , 0.005000 = C(48) TO C(49) 
DISTANCE 1.539000 , 0.005000 = C(49) TO C(50) 
DISTANCE 1.539000 , 0.005000 = C(50) TO C(51) 
DISTANCE 1.539000 , 0.005000 = C(51) TO C(52) 
ANGLE 109.000000 , 1.000000 = O(47) TO C(48) TO C(49) 
ANGLE 109.000000 , 1.000000 = C(48) TO C(49) TO C(50) 
ANGLE 109.000000 , 1.000000 = C(49) TO C(50) TO C(51) 
ANGLE 109.000000 , 1.000000 = C(50) TO C(51) TO C(52) 
DISTANCE 1.539000 , 0.005000 = C(49) TO C(150) 
DISTANCE 1.539000 , 0.005000 = C(150) TO C(151) 
DISTANCE 1.539000 , 0.005000 = C(151) TO C(152) 
ANGLE 109.000000 , 1.000000 = C(48) TO C(49) TO C(150) 
ANGLE 109.000000 , 1.000000 = C(49) TO C(150) TO C(151) 
ANGLE 109.000000 , 1.000000 = C(150) TO C(151) TO C(152) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(48) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(49) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(50) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(51) 
U(IJ)'S  0.0, 0.010000 = O(47) TO C(52) 
U(IJ)'S  0.0, 0.001000 = C(50) TO C(150) 
U(IJ)'S  0.0, 0.001000 = C(51) TO C(151) 
U(IJ)'S  0.0, 0.001000 = C(52) TO C(152) 
END                                                                             
;