Glycoluril Dimers Bearing Hydrogen Atoms on Their Convex Face and Their Self-Assembly in the Solid State
Marek Stancl; Marek Necas; Jan Taraba; Vladimir Sindelar; Journal of Organic Chemistry 73 (2008) 4671–4675; doi:10.1021/jo800699s

data_4023492
_publ_section_title
;
 Glycoluril Dimers Bearing Hydrogen Atoms on Their Convex
 Face and Their Self-Assembly in the Solid State
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4671
_journal_page_last               4675
_journal_paper_doi               10.1021/jo800699s
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C26 H28 N8 O6'
_chemical_formula_weight         548.56
_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-97
_cell_angle_alpha                67.621(2)
_cell_angle_beta                 79.274(2)
_cell_angle_gamma                83.560(2)
_cell_formula_units_Z            4
_cell_length_a                   11.6354(2)
_cell_length_b                   14.5303(3)
_cell_length_c                   16.3846(4)
_cell_measurement_temperature    120(2)
_cell_volume                     2514.10(9)
_computing_cell_refinement       'Xcalibur (Oxford Diffraction Ltd, 2003)'
_computing_data_collection       'Xcalibur (Oxford Diffraction Ltd, 2003)'
_computing_data_reduction        'Xcalibur (Oxford Diffraction Ltd, 2003)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'
_computing_structure_refinement  'SHELXTL (Bruker, 1998)'
_computing_structure_solution    'SHELXTL (Bruker, 1998)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '0.06 mm'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Kuma KM-4 CCD diffractometer'
_diffrn_measurement_method       '\w scan'
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30368
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  1.0309
_exptl_absorpt_correction_T_min  0.9761
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.811
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         8820
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          14.999
_refine_ls_shift/su_mean         0.038
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1686
_reflns_number_gt                6001
_reflns_number_total             8820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo800699s-File004_2.cif
_cod_data_source_block           2c
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_database_code               4023492