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_4024160
_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         ' C33 H33.25 O4 S4 '
_chemical_formula_sum            'C33 H33.25 O4 S4'
_chemical_formula_weight         622.14
_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             04-04-30
_audit_creation_method           CRYSTALS_ver_12.20
_cell_angle_alpha                90.1202(6)
_cell_angle_beta                 94.7055(8)
_cell_angle_gamma                94.9100(8)
_cell_formula_units_Z            8
_cell_length_a                   10.5160(2)
_cell_length_b                   18.8366(3)
_cell_length_c                   31.7909(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     6252.80(19)
_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 0.993
_diffrn_measured_fraction_theta_max 0.981
_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  0.02
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            49573
_diffrn_reflns_theta_full        20.566
_diffrn_reflns_theta_max         27.421
_diffrn_reflns_theta_min         1.085
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' ? '
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_description       ' ? '
_exptl_crystal_F_000             2618
_exptl_crystal_size_max          0.00
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0933
_refine_ls_number_parameters     1503
_refine_ls_number_reflns         18599
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.001057
_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: 
 1.01 0.679 0.713 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0720
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0504
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              24
_reflns_limit_k_min              -24
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                18599
_reflns_number_total             28005
_reflns_threshold_expression     I>1.96u(I)
_cod_data_source_file            jo070927i-File005.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        ' C33 H33.25 O4 S4 '
_cod_database_code               4024160