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_4026640
_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_sum            'C26 H37 N6 O8.5'
_chemical_formula_weight         569.62
_chemical_name_systematic
;
 ?
;
_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                 119.4050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.8510(3)
_cell_length_b                   31.3650(10)
_cell_length_c                   13.6220(4)
_cell_measurement_temperature    293(2)
_cell_volume                     5899.9(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11478
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6471
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1168P)^2^+2.7736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.2075
_reflns_number_gt                4320
_reflns_number_total             6471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2012835_si_001.cif
_cod_data_source_block           pzl
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C26 H37 N6 O8.50'
_cod_database_code               4026640