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_7054579
_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_absolute_configuration ad
_chemical_formula_moiety         'C52 H36 N4 O12 S4'
_chemical_formula_sum            'C52 H36 N4 O12 S4'
_chemical_formula_weight         1037.14
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.73537(12)
_cell_length_b                   12.73537(12)
_cell_length_c                   28.8831(3)
_cell_measurement_reflns_used    11504
_cell_measurement_temperature    190
_cell_measurement_theta_max      76
_cell_measurement_theta_min      5
_cell_volume                     4684.54(8)
_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      190
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_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  0.044
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            21324
_diffrn_reflns_theta_full        74.263
_diffrn_reflns_theta_max         75.778
_diffrn_reflns_theta_min         4.629
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.469
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details 'Flack (1983), 1962 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.65(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0794
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         4801
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.0017159
_refine_ls_shift/su_mean         0.0000570
_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: 
 648. 0.102E+04 517. 128. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1148
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1148
_reflns_limit_h_max              11
_reflns_limit_h_min              -10
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              0
_reflns_number_gt                4516
_reflns_number_total             4801
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.83
_oxford_diffrn_Wilson_scale      0.38
_oxford_refine_ls_r_factor_ref   0.0464
_oxford_refine_ls_scale          1.742(9)
_oxford_reflns_number_all        4801
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c4nj01956c1.cif
_cod_data_source_block           4g
_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_H-M      'P 41 21 2 '
_cod_database_code               7054579
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
CONT ENANTIO 
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   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) H   ( 252,X'S) 
RIDE C   (  27,X'S) H   ( 271,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,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) 
END                                                                             
;