Partially O-Alkylated Thiacalix[4]arenes: Synthesis, Molecular and Crystal Structures, Conformational Behavior
Hana Dvořáková; Jan Lang; Jiří Vlach; Jan Sýkora; Michal Čajan; Michal Himl; Michaela Pojarová; Ivan Stibor; Pavel Lhoták; Journal of Organic Chemistry 72 (2007) 7157–7166; doi:10.1021/jo070927i

data_4024162
_publ_section_title
;
 Partially O-Alkylated Thiacalix[4]arenes: Synthesis, Molecular and
 Crystal Structures, Conformational Behavior
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7157
_journal_page_last               7166
_journal_paper_doi               10.1021/jo070927i
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C42 H52 O4 S4'
_chemical_formula_sum            'C42 H52 O4 S4'
_chemical_formula_weight         749.14
_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             07-04-24
_audit_creation_method           CRYSTALS_ver_12.82
_cell_angle_alpha                90
_cell_angle_beta                 99.552(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.006(2)
_cell_length_b                   20.624(2)
_cell_length_c                   20.815(2)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    293
_cell_measurement_theta_max      38
_cell_measurement_theta_min      17
_cell_volume                     4236.1(10)
_computing_cell_refinement       'CAD4 Express, (Straver, 1992)'
_computing_data_collection       'CAD4 Express, (Straver, 1992)'
_computing_data_reduction        'RC93 (Watkin, Prout & Lilley, 1994)'
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius Mach3'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13784
_diffrn_reflns_theta_full        59.937
_diffrn_reflns_theta_max         59.937
_diffrn_reflns_theta_min         3.037
_diffrn_standards_decay_%        1.48
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.352
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
; 
 Azimutal absorption correction (North et al., 1968) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2258
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         2794
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1603
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.003279
_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: 
 1.64 -0.175 1.22 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0901
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0594
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                2794
_reflns_number_total             6274
_reflns_threshold_expression     I>1.96u(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.2768(7)
_oxford_structure_analysis_title 'DIMETHOXY TERCBUTIL 30/05/00'
_cod_data_source_file            jo070927i-File007.cif
_cod_data_source_block           CRYSTALS_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_database_code               4024162