The Mechanism of Ureido-Pyrimidinone:2,7-Diamido-Naphthyridine Complexation and the Presence of Kinetically Controlled Pathways in Multicomponent Hydrogen-Bonded Systems
Tom F. A. de Greef; G. B. W. L. Ligthart; Martin Lutz; Anthony L. Spek; E. W. Meijer; Rint P. Sijbesma; Journal of the American Chemical Society 130 (2008) 5479–5486; doi:10.1021/ja709971y

data_4107706
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@chem.uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 The Mechanism of Ureido-Pyrimidinone:2,7-Diamido-Naphthyridine
 Complexation and the Presence of Kinetically Controlled Pathways in
 Multicomponent Hydrogen-Bonded Systems
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5479
_journal_page_last               5486
_journal_paper_doi               10.1021/ja709971y
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C25 H47 N5 O2'
_chemical_formula_sum            'C25 H47 N5 O2'
_chemical_formula_weight         449.68
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.0804(6)
_cell_angle_beta                 109.5916(7)
_cell_angle_gamma                114.8871(9)
_cell_formula_units_Z            2
_cell_length_a                   10.3030(2)
_cell_length_b                   10.9384(2)
_cell_length_c                   14.1351(3)
_cell_measurement_reflns_used    69320
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     1325.56(5)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31497
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         6043
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0606P)^2^+0.2408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                4318
_reflns_number_total             6043
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja709971y-file006.cif
_cod_data_source_block           s3803a
_cod_database_code               4107706