Synthesis, structural determination and dynamic behavior of 2-chloro-4,6-bis(pyrazolylamino)-1,3,5-triazines
Angel Díaz-Ortiz; José Elguero; Concepción Foces-Foces; Antonio de la Hoz; Andrés Moreno; Sergio Moreno; Ana Sánchez-Migallón; Gema Valiente; Org. Biomol. Chem. 1 (2003) 4451–4457; doi:10.1039/b310693d

data_7151579
_publ_section_title
;
 Synthesis, structural determination and dynamic behavior of
 2-chloro-4,6-bis(pyrazolylamino)-1,3,5-triazines
;
_journal_issue                   24
_journal_name_full               'Org. Biomol. Chem.'
_journal_page_first              4451
_journal_page_last               4457
_journal_paper_doi               10.1039/b310693d
_journal_volume                  1
_journal_year                    2003
_chemical_formula_moiety         'C21 H16 CL1 N9'
_chemical_formula_sum            'C21 H16 Cl N9'
_chemical_formula_weight         429.88
_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'
_cell_angle_alpha                90
_cell_angle_beta                 98.529(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0587(8)
_cell_length_b                   11.2534(11)
_cell_length_c                   22.104(3)
_cell_measurement_reflns_used    74
_cell_measurement_temperature    293
_cell_measurement_theta_max      35
_cell_measurement_theta_min      2
_cell_volume                     1982.4(4)
_computing_cell_refinement       'LSUCRE (Appleman, 1984)'
_computing_data_collection       'Seifert XRD3000-S, 1996'
_computing_data_reduction        'xtal ADDREF DIFDAT ABSCAL SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type  'Four circle diffractometer'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_type           'Cu K\\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  .053
_diffrn_reflns_av_sigmaI/netI    .014
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3374
_diffrn_reflns_reduction_process 'equatorial monochr Lp'
_diffrn_reflns_theta_max         66.94
_diffrn_reflns_theta_min         4.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  100
_exptl_absorpt_coefficient_mu    1.956
_exptl_absorpt_correction_T_max  1.203
_exptl_absorpt_correction_T_min  0.992
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North el al.,1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.44
_exptl_crystal_density_meas      ?
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.33
_refine_diff_density_max         .336
_refine_diff_density_min         -.271
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       3690(309)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     '(Zachariasen, 1967)'
_refine_ls_goodness_of_fit_all   .984
_refine_ls_goodness_of_fit_ref   .972
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2480
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .054
_refine_ls_R_factor_gt           .043
_refine_ls_shift/su_max          .001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = k/[(A+B Fo)^2^(C+D(sin\q)/\l)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .062
_refine_ls_wR_factor_ref         .055
_reflns_d_resolution_high        .838
_reflns_d_resolution_low         10.93
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                2480
_reflns_number_total             3002
_reflns_threshold_expression     'I > 2.00 sig(I )'
_cod_data_source_file            b310693d.txt
_cod_data_source_block           g34
_cod_original_sg_symbol_Hall     -P_2yn
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C21 H16 CL1 N9'
_cod_database_code               7151579