Synthesis, crystal structures and tautomerism in novel oximes based on hydroxyalkylpyrazolones
Belmar, Julio; Quezada, José; Jiménez, Claudio A.; Díaz-Gallifa, Pau; Pasán, Jorge; Ruiz-Pérez, Catalina; New Journal of Chemistry 37 (2013) 2002–; doi:10.1039/c3nj00163f

data_7053051
_publ_section_title
;
 Synthesis, crystal structures and tautomerism in novel oximes based on
 hydroxyalkylpyrazolones
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2002
_journal_paper_doi               10.1039/c3nj00163f
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C11 H11 N3 O3'
_chemical_formula_sum            'C11 H11 N3 O3'
_chemical_formula_weight         233.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 116.696(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8072(7)
_cell_length_b                   4.92528(15)
_cell_length_c                   16.3792(7)
_cell_measurement_reflns_used    2756
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.1159
_cell_measurement_theta_min      5.2396
_cell_volume                     1139.27(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5953
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5877
_diffrn_reflns_theta_full        70.11
_diffrn_reflns_theta_max         70.11
_diffrn_reflns_theta_min         5.24
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.5402
_exptl_crystal_size_mid          0.0831
_exptl_crystal_size_min          0.0413
_refine_diff_density_max         0.141
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0333P)^2^+0.5913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                1626
_reflns_number_total             2105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj00163f.txt
_cod_data_source_block           compound4
_cod_original_cell_volume        1139.26(8)
_cod_database_code               7053051