Methyl 5-carboxyl-1-methylpyrazole-3-carboxylate monohydrate
Caixia Yin; Fangjun Huo; Fei Gao; Pin Yang; Acta Crystallographica Section E 59 (2003) o1994–o1996; doi:10.1107/S1600536803026485

data_2202665
_publ_section_title
;
 Methyl 5-carboxyl-1-methylpyrazole-3-carboxylate monohydrate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1994
_journal_page_last               o1996
_journal_paper_doi               10.1107/S1600536803026485
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C7 H8 N2 O4, H2 O'
_chemical_formula_moiety         'C7 H8 N2 O4, H2 O'
_chemical_formula_sum            'C7 H10 N2 O5'
_chemical_formula_weight         202.17
_chemical_melting_point          403
_chemical_name_common
'3-Methoxycarbonyl-5-carboxyl-1-methyl-pyrazole monohydrate'
_chemical_name_systematic
;
Methyl 5-carboxyl-1-methylpyrazole-3-carboxylate monohydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.641(3)
_cell_length_b                   7.3197(15)
_cell_length_c                   18.660(4)
_cell_measurement_reflns_used    4940
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.26
_cell_volume                     1802.8(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction
'SAINT (Siemens, 1996) and SHELXTL (Siemens, 1996)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area-detector'
_diffrn_measurement_method       \W
_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  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            3564
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        2.18
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.9626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0517
_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^)+(0.078P)^2^+0.9903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                1337
_reflns_number_total             1590
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6007.cif
_cod_data_source_block           I
_cod_original_cell_volume        1802.8(6)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2202665
_cod_database_fobs_code          2202665