Crystal structure of (<i>E</i>)-<i>N</i>-{[3-methyl-1-phenyl-5-(1<i>H</i>-pyrrol-1-yl)-1<i>H</i>-pyrazol-4-yl]methylidene}hydroxylamine
Mague, Joel T.; Mohamed, Shaaban K.; Akkurt, Mehmet; El-Emary, Talaat I.; Albayati, Mustafa R.; Acta Crystallographica Section E 70 (2014) o1216–o1217; doi:10.1107/S1600536814023514

data_2240152
_publ_section_title
;
 Crystal structure of
 (<i>E</i>)-<i>N</i>-{[3-methyl-1-phenyl-5-(1<i>H</i>-pyrrol-1-yl)-1<i>H</i>-pyrazol-4-yl]methylidene}hydroxylamine
;
_journal_coeditor_code           HB7307
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1216
_journal_page_last               o1217
_journal_paper_doi               10.1107/S1600536814023514
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C15 H14 N4 O'
_chemical_formula_moiety         'C15 H14 N4 O'
_chemical_formula_sum            'C15 H14 N4 O'
_chemical_formula_weight         266.30
_chemical_name_systematic
(<i>E</i>)-<i>N</i>-{[3-Methyl-1-phenyl-5-(1<i>H</i>-pyrrol-1-yl)-1<i>H</i>-pyrazol-4-yl]methylidene}hydroxylamine
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                87.4070(11)
_cell_angle_beta                 82.6740(12)
_cell_angle_gamma                75.0190(12)
_cell_formula_units_Z            4
_cell_length_a                   9.1497(2)
_cell_length_b                   12.3932(3)
_cell_length_c                   12.7294(3)
_cell_measurement_reflns_used    8765
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.18
_cell_measurement_theta_min      3.50
_cell_volume                     1382.88(6)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2014)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2014)
;
_computing_data_reduction
;
<i>SAINT</i>  (Bruker, 2014)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2008)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15570
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         72.357
_diffrn_reflns_theta_min         3.501
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+0.4010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                4088
_reflns_number_total             5370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7307sup1.cif
_cod_data_source_block           I
_cod_database_code               2240152
_cod_database_fobs_code          2240152
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.967
_shelx_hkl_checksum              30172
_shelx_res_checksum              78116
_shelxl_version_number           2014/6