Supramolecular assembly of diethyl 1<i>H</i>-pyrazole-3,5-dicarboxylate 0.33-hydrate
Foces-Foces, Concepción; Rodríguez, Matias L.; Elguero, José; Acta Crystallographica Section E 62 (2006) o3351–o3353; doi:10.1107/S1600536806025918

data_2209833
_publ_section_title
;
 Supramolecular assembly of diethyl
 1<i>H</i>-pyrazole-3,5-dicarboxylate 0.33-hydrate
;
_journal_coeditor_code           FB2003
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3351
_journal_page_last               o3353
_journal_paper_doi               10.1107/S1600536806025918
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C9 H12 N2 O4, 0.33H2 O'
_chemical_formula_moiety         'C9 H12 N2 O4, 0.33H2 O'
_chemical_formula_sum            'C9 H12.67 N2 O4.33'
_chemical_formula_weight         218.21
_chemical_melting_point          325.3(4)
_chemical_name_systematic
;
diethyl 1H-pyrazole-3,5-dicarboxylate 0.33-hydrate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            72
_cell_length_a                   16.3410(14)
_cell_length_b                   16.3410(14)
_cell_length_c                   88.12(6)
_cell_measurement_reflns_used    34593
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      5.0
_cell_volume                     20378(14)
_computing_cell_refinement       'Please supply'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97, WinGX (Farrugia, 1999) and PLATON'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1057
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       105
_diffrn_reflns_limit_l_min       -100
_diffrn_reflns_number            34593
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         5.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sphere
_exptl_crystal_F_000             8304
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_exptl_crystal_size_rad          0.25
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    124
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4028
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.2229
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+45.7496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1983
_reflns_number_gt                2091
_reflns_number_total             4028
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fb2003.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '324.9-325.7' was changed to
'325.3(4)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '324.9-325.7' was changed to
'325.3(4)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        20379(13)
_cod_original_sg_symbol_H-M      'R -3c'
_cod_database_code               2209833
_cod_database_fobs_code          2209833