Uncommon Regioselectivity in the Thiacalix[4]arene Series: Gross Formylation of theConeConformer
Ondrej Kundrat; Hana Dvorakova; Vaclav Eigner; Pavel Lhotak; Journal of Organic Chemistry 75 (2010) 407–411; doi:10.1021/jo902240h

data_4025169
_publ_contact_author_address
; 
 Department of Organic Chemistry, 
 Institute of Chemical Technology, Prague,
 Technick\'a 5, 16628 
 Prague 6,
 Czech Republic 
;
_publ_contact_author_email       lhotakp@vscht.cz
_publ_contact_author_name        'Lhot\'ak, Pavel '
_publ_contact_author_phone       '+420 220445055'
_publ_section_title
;
 Uncommon Regioselectivity in the Thiacalix[4]arene Series: Gross
 Formylation of theConeConformer
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              407
_journal_page_last               411
_journal_paper_doi               10.1021/jo902240h
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C43 H44 N4 O8 S4'
_chemical_formula_sum            'C43 H44 N4 O8 S4'
_chemical_formula_weight         873.11
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             09-10-06
_audit_creation_method           CRYSTALS_ver_12.86
_audit_update_record
;
2009-11-13 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 102.535(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.859(3)
_cell_length_b                   16.8393(18)
_cell_length_c                   15.9699(17)
_cell_measurement_reflns_used    2931
_cell_measurement_temperature    150
_cell_measurement_theta_max      78
_cell_measurement_theta_min      4
_cell_volume                     8625.9(16)
_computing_cell_refinement       'CrysAlis RED, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis RED, (Oxford Diffraction, 2002)'
_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_pressure         101
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23226
_diffrn_reflns_theta_full        73.423
_diffrn_reflns_theta_max         80.684
_diffrn_reflns_theta_min         4.305
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.495
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plane
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9704
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7976
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0690
_refine_ls_shift/su_max          0.031932
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.13P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2248
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.2103
_reflns_limit_h_max              40
_reflns_limit_h_min              -41
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                4157
_reflns_number_total             9031
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.52
_oxford_diffrn_Wilson_scale      0.66
_oxford_refine_ls_r_factor_ref   0.1116
_oxford_refine_ls_scale          1.273(9)
_oxford_reflns_number_all        8996
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'JK_605 in C2/c'
_cod_data_source_file            jo902240h_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        8625.7(15)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4025169