2,14-Dithiacalix[4]arene and its homooxa analogues: synthesis and dynamic NMR study of conformational behaviour
Michal Hucko; Hana Dvorakova; Vaclav Eigner; Pavel Lhotak; Chem.Commun. 51 (2015) 7051–; doi:10.1039/C5cc00819K

data_7116973
_publ_section_title
;
 2,14-Dithiacalix[4]arene and its homooxa analogues: synthesis and dynamic
 NMR study of conformational behaviour
;
_journal_name_full               Chem.Commun.
_journal_page_first              7051
_journal_paper_doi               10.1039/C5cc00819K
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration .
_chemical_formula_moiety         'C44 H56 O6 S2'
_chemical_formula_sum            'C44 H56 O6 S2'
_chemical_formula_weight         745.06
_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     direct
_audit_update_record
;
2014-11-03 deposited with the CCDC.
2015-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                81.533(3)
_cell_angle_beta                 81.481(3)
_cell_angle_gamma                87.419(3)
_cell_formula_units_Z            1
_cell_length_a                   9.2441(3)
_cell_length_b                   9.4374(3)
_cell_length_c                   11.5116(4)
_cell_measurement_reflns_used    11928
_cell_measurement_temperature    180
_cell_measurement_theta_max      76
_cell_measurement_theta_min      5
_cell_volume                     982.09(6)
_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 0.964
_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     1.54180
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20648
_diffrn_reflns_theta_full        67.676
_diffrn_reflns_theta_max         76.041
_diffrn_reflns_theta_min         4.739
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.29
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3937
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.0007679
_refine_ls_shift/su_mean         0.0000414
_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: 
 0.112E+04 0.183E+04 0.106E+04 410. 82.0 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0890
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0890
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3471
_reflns_number_total             3952
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.88
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0453
_oxford_refine_ls_scale          6.68(11)
_oxford_reflns_number_all        3937
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_cod_data_source_file            c5cc00819k2.cif
_cod_data_source_block           1
_cod_original_cell_volume        982.10(6)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7116973
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE O   (  17,X'S) H   ( 171,X'S) 
RIDE O   (  18,X'S) H   ( 181,X'S) 
RIDE C   (  20,X'S) H   ( 203,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 213,X'S) H   ( 212,X'S) 
RIDE C   (  22,X'S) H   ( 222,X'S) H   ( 221,X'S) H   ( 223,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 243,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 253,X'S) H   ( 252,X'S) H   ( 251,X'S) 
RIDE C   (  26,X'S) H   ( 261,X'S) H   ( 262,X'S) H   ( 263,X'S) 
RIDE C   ( 120,X'S) H   (1203,X'S) H   (1201,X'S) H   (1202,X'S) 
RIDE C   ( 121,X'S) H   (1211,X'S) H   (1213,X'S) H   (1212,X'S) 
RIDE C   ( 122,X'S) H   (1222,X'S) H   (1221,X'S) H   (1223,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 1.540000 , 0.050000 = C(19) TO C(20) 
DISTANCE 1.540000 , 0.050000 = C(19) TO C(21) 
DISTANCE 1.540000 , 0.050000 = C(19) TO C(22) 
DISTANCE 2.340000 , 0.050000 = C(20) TO C(21) 
DISTANCE 2.340000 , 0.050000 = C(21) TO C(22) 
DISTANCE 2.340000 , 0.050000 = C(22) TO C(20) 
DISTANCE 1.540000 , 0.050000 = C(119) TO C(120) 
DISTANCE 1.540000 , 0.050000 = C(119) TO C(121) 
DISTANCE 1.540000 , 0.050000 = C(119) TO C(122) 
DISTANCE 2.340000 , 0.050000 = C(120) TO C(121) 
DISTANCE 2.340000 , 0.050000 = C(121) TO C(122) 
DISTANCE 2.340000 , 0.050000 = C(122) TO C(120) 
U(IJ)'S  0.0, 0.001000 = C(19) TO C(119) 
U(IJ)'S  0.0, 0.001000 = C(20) TO C(120) 
U(IJ)'S  0.0, 0.001000 = C(21) TO C(121) 
U(IJ)'S  0.0, 0.001000 = C(22) TO C(122) 
END                                                                             
;