A theoretical and experimental NMR study of the tautomerism of two phenylene-bis-C-substituted pyrazoles
Sanz, Dionisia; Claramunt, Rosa M.; Alkorta, Ibon; Elguero, José; Thiel, Werner R.; Rüffer, Tobias; New Journal of Chemistry 32 (2008) 2225–; doi:10.1039/b803855d

data_7051974
_publ_section_title
;
 A theoretical and experimental NMR study of the tautomerism of two
 phenylene-bis-C-substituted pyrazoles
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2225
_journal_paper_doi               10.1039/b803855d
_journal_volume                  32
_journal_year                    2008
_chemical_formula_sum            'C40 H40 N12 O'
_chemical_formula_weight         704.84
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.190(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3449(19)
_cell_length_b                   9.6588(12)
_cell_length_c                   26.538(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3777.3(8)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        XPREP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.1093
_diffrn_reflns_av_sigmaI/netI    0.2019
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            13355
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9952
_exptl_absorpt_correction_T_min  0.9317
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0041(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.801
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         6804
_refine_ls_number_restraints     218
_refine_ls_restrained_S_all      0.795
_refine_ls_R_factor_all          0.2399
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0526P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                2313
_reflns_number_total             6804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b803855d.txt
_cod_data_source_block           ii229a
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7051974