A tripyridylthioether macrocycle: (14,17-dithia-22,23,24-triazatetracyclo[16.3.1.1^3,7^.1^9,13^]tetracosa-1(22),3,5,7(24),9,11,13(23),18,20-nonaene-2,8-dione
Poole, Martin C.; Fronczek, Frank R.; Newkome, George R.; Watkins, Steven F.; Acta Crystallographica Section E 62 (2006) o4952–o4954; doi:10.1107/S1600536806041262

data_2211075
_publ_section_title
;A tripyridylthioether macrocycle:
 (14,17-dithia-22,23,24-triazatetracyclo[16.3.1.1^3,7^.1^9,13^]tetracosa-1(22),3,5,7(24),9,11,13(23),18,20-nonaene-2,8-dione
;
_journal_coeditor_code           IS2084
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4952
_journal_page_last               o4954
_journal_paper_doi               10.1107/S1600536806041262
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C19 H13 N3 O2 S2'
_chemical_formula_sum            'C19 H13 N3 O2 S2'
_chemical_formula_weight         379.44
_chemical_name_systematic
;
14,17-Dithia-22,23,24-triazatetracyclo[16.3.1.13,7.19,13]tetracosa-
1(22),3,5,7(24),9,11,13(23),18,20-nonaene-2,8-dione
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.532(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7102(10)
_cell_length_b                   13.1725(13)
_cell_length_c                   15.497(2)
_cell_measurement_reflns_used    7195
_cell_measurement_temperature    110
_cell_measurement_theta_max      36.3
_cell_measurement_theta_min      2.5
_cell_volume                     1758.4(4)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Nonius KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35062
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         36.4
_diffrn_reflns_theta_min         2.8
_diffrn_standards_decay_%        <2
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.42
_refine_ls_extinction_coef       0.0054(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         8240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.7446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.108
_reflns_number_gt                6267
_reflns_number_total             8240
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is2084.cif
_cod_data_source_block           II
_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:

'_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1758.4(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2211075
_cod_database_fobs_code          2211075