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_4021795
_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         'C52.50 H65 Cl1 N4 O8 S4'
_chemical_formula_sum            'C52.5 H65 Cl N4 O8 S4'
_chemical_formula_weight         1043.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             06-04-05
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 107.4920(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.51800(10)
_cell_length_b                   27.6200(2)
_cell_length_c                   18.6860(2)
_cell_measurement_reflns_used    24595
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     10592.06(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT. Nonius (1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.013
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47674
_diffrn_reflns_theta_full        27.480
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         1.360
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.9310
_exptl_absorpt_correction_T_min  0.9283
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.93
_refine_diff_density_min         -1.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1252
_refine_ls_number_reflns         17432
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.000967
_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: 
 1.16 1.09 0.758 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0758
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0590
_reflns_limit_h_max              26
_reflns_limit_h_min              -27
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                17432
_reflns_number_total             24236
_reflns_threshold_expression     I>1.96u(I)
_cod_data_source_file            jo0607358si20060505_041746.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C52.50 H65 Cl1 N4 O8 S4'
_cod_database_code               4021795