Synthesis, Structure, and Ion Selective Complexation of Trans and Cis Isomers of Photochromic Dithia-18-crown-6 Ethers
M. V. Alfimov; S. P. Gromov; Yu. V. Fedorov; O. A. Fedorova; A. I. Vedernikov; A. V. Churakov; L. G. Kuz'mina; J. A. K. Howard; S. Bossmann; A. Braun; M. Woerner; D. F. Sears; J. Saltiel; Journal of the American Chemical Society 121 (1999) 4992–5000; doi:10.1021/ja990370r

data_4116406
_publ_section_title
;
 Synthesis, Structure, and Ion Selective Complexation of Trans and Cis
 Isomers of Photochromic Dithia-18-crown-6 Ethers
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4992
_journal_page_last               5000
_journal_paper_doi               10.1021/ja990370r
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C26 H32 I N O4 S3'
_chemical_formula_weight         645.61
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                64.01(6)
_cell_angle_beta                 85.28(9)
_cell_angle_gamma                71.29(9)
_cell_formula_units_Z            2
_cell_length_a                   9.711(13)
_cell_length_b                   12.304(9)
_cell_length_c                   13.715(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      11
_cell_volume                     1392(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            5015
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.745
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.0000(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_obs          0.0560
_refine_ls_shift/esd_max         -3.258
_refine_ls_shift/esd_mean        0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1430P)^2^+0.6437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1986
_refine_ls_wR_factor_obs         0.1779
_reflns_number_observed          3728
_reflns_number_total             4613
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ja990370r.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1430P)^2^+0.6437P] 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^)+(0.1430P)^2^+0.6437P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1391.9(23)
_cod_database_code               4116406