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_4024159
_publ_contact_author_address
; 
Chemical Crystallography Laboratory, 
Department of Chemistry, 
University of Oxford, 
Chemistry Research Laboratory, 
Mansfield Road, 
Oxford 
OX1 3TA 
;
_publ_contact_author_email       david.watkin@chem.ox.ac.uk
_publ_contact_author_fax         '01865 272 699'
_publ_contact_author_name        'David Watkin'
_publ_contact_author_phone       '01865 270 826'
_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_compound_source
;
?
;
_chemical_formula_moiety         ' C30 H28 O4 S4 '
_chemical_formula_sum            'C30 H28 O4 S4'
_chemical_formula_weight         580.81
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             04-03-12
_audit_creation_method           CRYSTALS_ver_12.20
_cell_angle_alpha                103.7710(15)
_cell_angle_beta                 105.1480(17)
_cell_angle_gamma                109.5170(18)
_cell_formula_units_Z            1
_cell_length_a                   8.7790(3)
_cell_length_b                   9.0180(3)
_cell_length_c                   10.0710(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     677.42(5)
_computing_cell_refinement
; 
 USER DEFINED 6 
;
_computing_data_collection
; 
 DATA COLLECTION 
;
_computing_data_reduction
; 
 USER DEFINED 5 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.00
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5533
_diffrn_reflns_theta_full        27.008
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_min         2.566
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' white '
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.00
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0212
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4910
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.001040
_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: 
 0.913 0.455 0.569 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0439
_refine_ls_wR_factor_gt          0.0385
_refine_ls_wR_factor_ref         0.0385
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              11
_reflns_limit_k_min              -11
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                4910
_reflns_number_total             5533
_reflns_threshold_expression     I>1.96u(I)
_cod_data_source_file            jo070927i-File004.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
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_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C30 H28 O4 S4 '
_cod_database_code               4024159