Two <i>N</i>-aminoazolylmethylene derivatives of Meldrum's acid
Blake, Alexander J.; Gould, Robert O.; Irving, Iain; McNab, Hamish; Morrow, Mark; Acta Crystallographica Section C 50 (1994) 1935–1938; doi:10.1107/S0108270194007213

data_2010289
_publ_section_title
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 Two <i>N</i>-aminoazolylmethylene derivatives of Meldrum's acid
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1935
_journal_page_last               1938
_journal_paper_doi               10.1107/S0108270194007213
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         'C10 H11 N3 O4'
_chemical_formula_sum            'C10 H11 N3 O4'
_chemical_formula_weight         237.22
_chemical_name_common            '5-(1-aminopyrazolylmethylene)-Meldrum's acid'
_chemical_name_systematic
;
 5-(1-aminopyrazolylmethylene)-2,2-dimethyl-1,3-dioxane-4,6-dione
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                107.351(7)
_cell_angle_beta                 96.814(11)
_cell_angle_gamma                100.900(15)
_cell_formula_units_Z            2
_cell_length_a                   5.4407(10)
_cell_length_b                   10.341(2)
_cell_length_c                   10.714(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     555.04(19)
_computing_cell_refinement       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method       '\w-2\q 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  0.0079
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3031
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       Tablet
_exptl_crystal_F_000             248
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.139
_refine_ls_extinction_coef       0.030(3)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_all   0.187
_refine_ls_goodness_of_fit_obs   0.181
_refine_ls_hydrogen_treatment
'H atoms placed in fixed, calculated positions except for H8N'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.187
_refine_ls_restrained_S_obs      0.181
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_obs          0.0318
_refine_ls_shift/esd_max         0.225
_refine_ls_shift/esd_mean        0.047
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(F~o~^2^) + (0.1000P)^2^ + 10.0000P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0787
_refine_ls_wR_factor_obs         0.0691
_reflns_number_observed          1640
_reflns_number_total             1964
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ha1120.cif
_cod_data_source_block           melnpz
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        555.1(2)
_cod_database_code               2010289