Bisthioxanthylidene biscrown ethers as potential stereodivergent chiral ligands
Geertsema, Edzard M.; Schoevaars, Anne Marie; Meetsma, Auke; Feringa, Ben L.; Organic & Biomolecular Chemistry 4 (2006) 4101–; doi:10.1039/b609271c

data_7151297
_publ_section_title
;
 Bisthioxanthylidene biscrown ethers as potential stereodivergent
 chiral ligands
;
_journal_issue                   22
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              4101
_journal_paper_doi               10.1039/b609271c
_journal_volume                  4
_journal_year                    2006
_chemical_compound_source        'by syntheses / see text'
_chemical_formula_moiety         'C44 H48 O10 S2'
_chemical_formula_sum            'C44 H48 O10 S2'
_chemical_formula_weight         800.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 95.882(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.617(1)
_cell_length_b                   9.336(1)
_cell_length_c                   20.742(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    130
_cell_measurement_theta_max      20.21
_cell_measurement_theta_min      14.96
_cell_volume                     3971.4(6)
_computing_cell_refinement       'SET4 (de Boer & Duisenberg, 1984)'
_computing_data_collection       'CAD4-UNIX Software Version 5.1, 1994'
_computing_data_reduction        'HELENA (Spek, 1993)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 1997)
 ORTEP (Burnett et al., 1996)
 PLATON (Spek, 1994, 1996)
;
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-97 (Beurskens et al., 1997)
;
_diffrn_ambient_temperature      130
_diffrn_measurement_device_type
;
     Enraf Nonius CAD-4F diffractometer
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_detector
;
     scintillation NaI crystal with photomultiplier
;
_diffrn_radiation_monochromator  'perpendicular mounted graphite'
_diffrn_radiation_source         'fine focus sealed Philips Mo tube '
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7158
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization effects, scale
 variation, but not for absorption and reduced to F~o~^2^
;
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .19
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       needle
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.874
_refine_diff_density_min         -.903
_refine_diff_density_rms         .124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         6952
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.1148
_refine_ls_shift/su_max          0.714
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1984P)^2^+9.9659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3048
_refine_ls_wR_factor_ref         0.3425
_reflns_number_gt                4456
_reflns_number_total             6952
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b609271c.txt
_cod_data_source_block           c44h48o1
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1984P)^2^+9.9659P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1984P)^2^+9.9659P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7151297