Inherent chirality through a simple dialkylation of 2,14-dithiacalix[4]arene
Kortus, D.; Kundrát, O.; Tlustý, M.; Čejka, J.; Dvořáková, H.; Lhoták, P.; New Journal of Chemistry 44 (2020) 14496–14504; doi:10.1039/D0NJ03468A

data_7059829
_publ_section_title
;
 Inherent chirality through a simple dialkylation of
 2,14-dithiacalix[4]arene
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14496
_journal_page_last               14504
_journal_paper_doi               10.1039/D0NJ03468A
_journal_volume                  44
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48.67 H65.33 Cl1.33 O4 S2'
_chemical_formula_sum            'C48.67 H65.33 Cl1.33 O4 S2'
_chemical_formula_weight         825.79
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2020-06-29 deposited with the CCDC.	2020-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.3050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   33.6924(10)
_cell_length_b                   13.3613(4)
_cell_length_c                   35.6078(11)
_cell_measurement_reflns_used    101
_cell_measurement_temperature    180
_cell_measurement_theta_max      51
_cell_measurement_theta_min      11
_cell_volume                     14609.0(8)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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_temperature      180
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.031
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            166334
_diffrn_reflns_theta_full        70.066
_diffrn_reflns_theta_max         70.066
_diffrn_reflns_theta_min         2.723
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.963
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5328
_exptl_crystal_size_max          0.454
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_details 'Flack (1983), 13745 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.000(13)
_refine_ls_extinction_coef       101(12)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9643
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1575
_refine_ls_number_reflns         27604
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.0004644
_refine_ls_shift/su_mean         0.0000743
_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: 
 12.7 20.7 11.6 4.44 0.916 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1223
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1223
_reflns_limit_h_max              40
_reflns_limit_h_min              -41
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              43
_reflns_limit_l_min              -43
_reflns_number_gt                25985
_reflns_number_total             27607
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.65
_oxford_diffrn_Wilson_scale      385.97
_oxford_refine_ls_r_factor_ref   0.0471
_oxford_refine_ls_scale          0.050526(5)
_oxford_reflns_number_all        27605
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            d0nj03468a2.cif
_cod_data_source_block           DK69
_cod_depositor_comments
;Adding full bibliography for 7059826--7059829.cif.

 Adding full bibliography for 7059826--7059829.cif.
;
_cod_original_sg_symbol_H-M      'C 1 c 1 '
_cod_database_code               7059829