Biscrown-annulated TTFAQ-dianthracene hybrid: synthesis, structure, and metal ion sensing.
Shao, Min; Dongare, Prateek; Dawe, Louise N.; Thompson, David W.; Zhao, Yuming; Organic letters 12 (2010) 3050–3053; doi:10.1021/ol1010467

data_1503038
_publ_section_title
;
 Biscrown-annulated TTFAQ-dianthracene hybrid: synthesis, structure, and
 metal ion sensing.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              3050
_journal_page_last               3053
_journal_paper_doi               10.1021/ol1010467
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C71 H62 Cl6 O6 S8, 4 (C H2 Cl2)'
_chemical_formula_sum            'C72 H64 Cl8 O6 S8'
_chemical_formula_weight         1565.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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-97
_cell_angle_alpha                81.708(12)
_cell_angle_beta                 89.14(2)
_cell_angle_gamma                85.925(19)
_cell_formula_units_Z            2
_cell_length_a                   11.535(4)
_cell_length_b                   15.772(5)
_cell_length_c                   20.813(7)
_cell_measurement_reflns_used    14643
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.6839
_cell_measurement_theta_min      1.7492
_cell_volume                     3737(2)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32342
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_correction_T_min  0.9368
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(T. Higashi, 2000)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The Platon Squeeze procedure was applied to recover 363 electrons per 
unit cell in one void (total volume 1094 ^A^3); that is 181.5 electrons 
per formula unit. Disordered solvent lattice dichloromethane molecules 
were present prior to the application of Squeeze, however, a 
satisfactory point atom model could not be achieved. The application 
of Squeeze gave a good improvement in the data statistics and allowed 
for a full anisotropic refinement of the  structure.
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         13755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0959
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2788
_refine_ls_wR_factor_ref         0.3022
_reflns_number_gt                9783
_reflns_number_total             13755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol1010467_si_002.cif
_cod_data_source_block           MS-4-79
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_database_code               1503038