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_7059826
_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         'C106 H148.00 Cl4.00 O8 S4'
_chemical_formula_sum            'C106 H148 Cl4 O8 S4'
_chemical_formula_weight         1820.41
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 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                 90.249(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1174(16)
_cell_length_b                   21.497(3)
_cell_length_c                   18.729(3)
_cell_measurement_reflns_used    318
_cell_measurement_temperature    200
_cell_measurement_theta_max      52
_cell_measurement_theta_min      12
_cell_volume                     5281.2(13)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_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      200
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_unetI/netI     0.050
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            119785
_diffrn_reflns_theta_full        68.450
_diffrn_reflns_theta_max         68.450
_diffrn_reflns_theta_min         2.359
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.155
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1960.000
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.261
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.66
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 9072 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.012(2)
_refine_ls_extinction_coef       45(2)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1173
_refine_ls_number_reflns         19318
_refine_ls_number_restraints     244
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.0013923
_refine_ls_shift/su_mean         0.0000387
_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: 
 2.55 3.14 0.812 0.704E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1448
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1448
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              25
_reflns_limit_k_min              -25
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                18446
_reflns_number_total             19318
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.99
_oxford_diffrn_Wilson_scale      150.72
_oxford_refine_ls_r_factor_ref   0.0604
_oxford_refine_ls_scale          0.091510(19)
_oxford_reflns_number_all        19318
_cod_data_source_file            d0nj03468a2.cif
_cod_data_source_block           DK145_1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7059826--7059829.cif.

 Adding full bibliography for 7059826--7059829.cif.
;
_cod_original_cell_volume        5281.1(13)
_cod_original_sg_symbol_H-M      'P 21 '
_cod_original_formula_sum        'C106 H148.00 Cl4.00 O8 S4'
_cod_database_code               7059826
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_hooft_y                  0.0127(15)
_oxford_bijvoet_difference       0.012(2)
_oxford_refined_flack_x          0.018(12)