5,5'-Dimethyl-<i>N</i>,<i>N</i>'-(iminodiethylene)bis(1<i>H</i>-pyrazole-3-carboxamide)
Jing Hu; Guofeng Chen; Guochun Ma; Hongguang Song; Acta Crystallographica Section E 63 (2007) o4806–o4806; doi:10.1107/S1600536807059387

data_2216228
_publ_section_title
5,5'-Dimethyl-<i>N</i>,<i>N</i>'-(iminodiethylene)bis(1<i>H</i>-pyrazole-3-carboxamide)
_journal_coeditor_code           AT2491
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4806
_journal_page_last               o4806
_journal_paper_doi               10.1107/S1600536807059387
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C14 H21 N7 O2'
_chemical_formula_moiety         'C14 H21 N7 O2'
_chemical_formula_sum            'C14 H21 N7 O2'
_chemical_formula_weight         319.38
_chemical_melting_point          484(5)
_chemical_name_systematic
;
5,5'-Dimethyl-N,N'-(iminodiethylene)di-1<i>H</i>-pyrazole-3-carboxamide
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.874(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   37.091(6)
_cell_length_b                   7.5543(12)
_cell_length_c                   11.6123(18)
_cell_measurement_reflns_used    3176
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.75
_cell_volume                     3205.5(9)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8706
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9870
_exptl_absorpt_correction_T_min  0.9760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+1.2780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1169
_reflns_number_gt                2386
_reflns_number_total             3303
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            at2491.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2216228
_cod_database_fobs_code          2216228