Hydrogen-Bond-Mediated Self-Assembly of 26-Membered Diaza Tetraester Crowns of 3,5-Disubstituted 1H-Pyrazole. Dimerization Study in the Solid State and in CDCl3 Solution
Felipe Reviriego; Pilar Navarro; Vicente J. Arán; Maria Luisa Jimeno; Enrique García-España; Julio Latorre; Maria J. R. Yunta; Journal of Organic Chemistry 76 (2011) 8223–8231; doi:10.1021/jo2012835

data_4026641
_publ_section_title
;
 Hydrogen-Bond-Mediated Self-Assembly of 26-Membered Diaza Tetraester
 Crowns of 3,5-Disubstituted 1H-Pyrazole. Dimerization Study in the Solid
 State and in CDCl3 Solution
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8223
_journal_page_last               8231
_journal_paper_doi               10.1021/jo2012835
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C20 H26 N6 O8, C2 H3 N'
_chemical_formula_sum            'C22 H29 N7 O8'
_chemical_formula_weight         519.52
_chemical_name_common            pzmet
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.1070(2)
_cell_length_b                   13.1070(2)
_cell_length_c                   30.3510(7)
_cell_measurement_temperature    293(2)
_cell_volume                     5214.10(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            5223
_diffrn_reflns_theta_full        26.72
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.016
_refine_diff_density_min         -0.006
_refine_diff_density_rms         0.003
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1231P)^2^+0.0022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.2266
_reflns_number_gt                1824
_reflns_number_total             2784
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo2012835_si_002.cif
_cod_data_source_block           pznoxxx
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4026641