Diethyl 4-iodo-1,22-dioxo-15-(4-pyridylethynyl)-1,20,12,21-tetraazahexacyclo[10.10.2.0^3,8^.0^10,23^.0^14,20^.0^21,24^]tetracosa-3,5,7,14,16,18-hexaene-23,24-dicarboxylate: a molecular clip based on bis(ethoxycarbonyl)glycoluril
Yun-Feng Chen; Jing Qin; Li-Ping Cao; Meng Gao; Acta Crystallographica Section E 62 (2006) o5881–o5882; doi:10.1107/S1600536806049853

data_2211624
_publ_section_title
;Diethyl
 4-iodo-1,22-dioxo-15-(4-pyridylethynyl)-1,20,12,21-tetraazahexacyclo[10.10.2.0^3,8^.0^10,23^.0^14,20^.0^21,24^]tetracosa-3,5,7,14,16,18-hexaene-23,24-dicarboxylate:
 a molecular clip based on bis(ethoxycarbonyl)glycoluril
;
_journal_coeditor_code           SJ2160
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o5881
_journal_page_last               o5882
_journal_paper_doi               10.1107/S1600536806049853
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C33 H28 I N5 O6'
_chemical_formula_moiety         'C33 H28 I N5 O6'
_chemical_formula_sum            'C33 H28 I N5 O6'
_chemical_formula_weight         717.50
_chemical_name_systematic
;
Diethyl 4-iodo-1,22-dioxo-15-(4-pyridylethynyl)-1,20,12,21-
tetraazahexacyclo[10.10.2.0^3,8^.0^10,23^.0^14,20^.0^21,24^]tetracosa-
3,5,7,14,16,18-hexaene-23,24-dicarboxylate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.7730(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.825(3)
_cell_length_b                   8.5516(6)
_cell_length_c                   18.8448(14)
_cell_measurement_reflns_used    2860
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      19.46
_cell_measurement_theta_min      2.19
_cell_volume                     5923.9(8)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.0761
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19410
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.22
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.137
_exptl_absorpt_correction_T_max  0.9776
_exptl_absorpt_correction_T_min  0.9145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.974
_refine_diff_density_min         -0.805
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5005
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.0942
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1787P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2427
_refine_ls_wR_factor_ref         0.2778
_reflns_number_gt                2882
_reflns_number_total             5005
_reflns_threshold_expression     I>2s(I)
_cod_data_source_file            sj2160.cif
_cod_data_source_block           I
_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        5923.9(7)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2211624
_cod_database_fobs_code          2211624