A second monoclinic polymorph of 2-(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)-2-hydroxyimino-<i>N</i>'-[1-(pyridin-2-yl)ethylidene]acetohydrazide
Plutenko, Maxym O.; Lampeka, Rostislav D.; Haukka, Matti; Nordlander, Ebbe; Acta Crystallographica Section E 69 (2013) o765–o766; doi:10.1107/S1600536813009628

data_2237823
_publ_section_title
;
 A second monoclinic polymorph of
 2-(3,5-dimethyl-1<i>H</i>-pyrazol-1-yl)-2-hydroxyimino-<i>N</i>'-[1-(pyridin-2-yl)ethylidene]acetohydrazide
;
_journal_coeditor_code           FK2070
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o765
_journal_page_last               o766
_journal_paper_doi               10.1107/S1600536813009628
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C14 H16 N6 O2'
_chemical_formula_moiety         'C14 H16 N6 O2'
_chemical_formula_sum            'C14 H16 N6 O2'
_chemical_formula_weight         300.33
_chemical_name_systematic
2-(3,5-Dimethyl-1<i>H</i>-pyrazol-1-yl)-2-hydroxyimino-<i>N</i>'-[1-(pyridin-2-yl)ethylidene]acetohydrazide
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.5520(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.4734(4)
_cell_length_b                   7.7679(2)
_cell_length_c                   19.8042(4)
_cell_measurement_reflns_used    9866
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.57
_cell_measurement_theta_min      2.82
_cell_volume                     2969.75(11)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '62mm x 62mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker Kappa APEXII DUO CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_monochromator  'curved graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            64574
_diffrn_reflns_theta_full        31.67
_diffrn_reflns_theta_max         31.67
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.9737
_exptl_absorpt_correction_T_min  0.9637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         9973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.8835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                8213
_reflns_number_total             9973
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fk2070.cif
_cod_data_source_block           I
_cod_original_cell_volume        2969.74(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2237823
_cod_database_fobs_code          2237823