Synthesis of Unique Cagelike Thiacalix[4]arene Derivatives in a 1,3-Alternate Conformation
Václav Št'astný; Ivan Stibor; Ivana Císarřová; Jan Sýkora; Michaela Pojarová; Pavel Lhoták; Journal of Organic Chemistry 71 (2006) 5404–5406; doi:10.1021/jo0607358

data_4021794
_publ_section_title
;
 Synthesis of Unique Cagelike Thiacalix[4]arene Derivatives
 in a 1,3-Alternate Conformation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5404
_journal_page_last               5406
_journal_paper_doi               10.1021/jo0607358
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C64 H57.20 N4 O10 S4'
_chemical_formula_sum            'C64 H57.2 N4 O10 S4'
_chemical_formula_weight         1170.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-03-17
_audit_creation_method           CRYSTALS_ver_12.83
_cell_angle_alpha                78.8310(14)
_cell_angle_beta                 70.9650(11)
_cell_angle_gamma                87.1330(14)
_cell_formula_units_Z            2
_cell_length_a                   13.3800(3)
_cell_length_b                   14.4440(3)
_cell_length_c                   15.9270(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2854.36(12)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'USER DEFINED DATA REDUCTION'
_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      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Unknown
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19210
_diffrn_reflns_theta_full        25.075
_diffrn_reflns_theta_max         25.075
_diffrn_reflns_theta_min         1.610
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       prism
_exptl_crystal_F_000             1226.400
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.00
_refine_diff_density_min         -0.25
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1044
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         7516
_refine_ls_number_restraints     56
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000579
_refine_ls_structure_factor_coef F
_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: 
 0.749 0.568 0.445 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0652
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0486
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -16
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7516
_reflns_number_total             10090
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            jo0607358si20060406_083622.cif
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-06-10

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_formula_sum        'C64 H57.20 N4 O10 S4'
_cod_database_code               4021794