Crystal structure of <i>N</i>-[(8<i>E</i>)-12-methyl-14-phenyl-10,13,14,16-tetraazatetracyclo[7.7.0.0^2,7^.0^11,15^]hexadeca-1(16),2,4,6,9,11(15),12-heptaen-8-ylidene]hydroxylamine 1,4-dioxane hemisolvate
Mohamed, Shaaban K.; Mague, Joel T.; Akkurt, Mehmet; El-Emary, Talaat I.; Albayati, Mustafa R.; Acta Crystallographica Section E 71 (2015) o75–o76; doi:10.1107/S2056989014027285

data_2240356
_publ_section_title
;
 Crystal structure of
 <i>N</i>-[(8<i>E</i>)-12-methyl-14-phenyl-10,13,14,16-tetraazatetracyclo[7.7.0.0^2,7^.0^11,15^]hexadeca-1(16),2,4,6,9,11(15),12-heptaen-8-ylidene]hydroxylamine
 1,4-dioxane hemisolvate
;
_journal_coeditor_code           HB7340
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o75
_journal_page_last               o76
_journal_paper_doi               10.1107/S2056989014027285
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C19 H13 N5 O, 0.5C4 H8 O2'
_chemical_formula_moiety         'C19 H13 N5 O, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C21 H17 N5 O2'
_chemical_formula_weight         371.40
_chemical_name_systematic
'<i>N</i>-[(8<i>E</i>)-12-Methyl-14-phenyl-10,13,14,16-tetraazatetracyclo[7.7.0.0^2,7^.0^11,15^]hexadeca-1(16),2,4,6,9,11(15),12-heptaen-8-ylidene]hydroxylamine 1,4-dioxane hemisolvate'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 102.093(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8019(4)
_cell_length_b                   5.56750(10)
_cell_length_c                   20.4756(5)
_cell_measurement_reflns_used    5735
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.034
_cell_measurement_theta_min      3.226
_cell_volume                     1761.41(7)
_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
;
SHELXL2014 (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 0.992
_diffrn_measured_fraction_theta_max 0.987
_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  0.0659
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12942
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         67.132
_diffrn_reflns_theta_min         3.226
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2014)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.493
_refine_diff_density_min         -0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         3122
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+1.2077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1658
_reflns_number_gt                1934
_reflns_number_total             3122
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb7340sup1.cif
_cod_data_source_block           I
_cod_database_code               2240356
_cod_database_fobs_code          2240356
_shelx_estimated_absorpt_t_min   0.892
_shelx_estimated_absorpt_t_max   0.969
_shelx_hkl_checksum              56400
_shelx_res_checksum              47110
_shelxl_version_number           2014/6