Cyclotridecanone 2,4-dinitrophenylhydrazone
Valente, Edward J.; Pawar, Diwaker M.; Fronczek, Frank R.; Noe, Eric A.; Acta Crystallographica Section C 64 (2008) o447–o449; doi:10.1107/S010827010802012X

data_2016715
_publ_section_title
;
 Cyclotridecanone 2,4-dinitrophenylhydrazone
;
_journal_coeditor_code           GG3158
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o447
_journal_page_last               o449
_journal_paper_doi               10.1107/S010827010802012X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C19 H28 N4 O4'
_chemical_formula_moiety         'C19 H28 N4 O4'
_chemical_formula_sum            'C19 H28 N4 O4'
_chemical_formula_weight         376.45
_chemical_melting_point          378
_chemical_name_common            'cyclotridecanone 2',4'-dinitrophenylhydrazone'
_chemical_name_systematic
;
cyclotridecanone 2,4-dinitrophenylhydrazone
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                81.979(7)
_cell_angle_beta                 77.608(8)
_cell_angle_gamma                80.234(8)
_cell_formula_units_Z            2
_cell_length_a                   7.7859(10)
_cell_length_b                   7.8937(10)
_cell_length_c                   16.130(2)
_cell_measurement_reflns_used    4832
_cell_measurement_temperature    90
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.5
_cell_volume                     948.7(2)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.87
_diffrn_measurement_device
'Nonius KappaCCD (with an Oxford Cryosystems Cryostream cooler)'
_diffrn_measurement_method       '\w scans with \k offsets'
_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  0.029
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26226
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         31.5
_diffrn_reflns_theta_min         2.6
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.34
_refine_diff_density_min         -0.26
_refine_ls_extinction_coef       0.0121(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         5518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.079
_refine_ls_R_factor_gt           0.046
_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^)+(0.0276P)^2^+0.4695P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.087
_refine_ls_wR_factor_ref         0.099
_reflns_number_gt                3974
_reflns_number_total             5518
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3158.cif
_cod_data_source_block           I
_cod_database_code               2016715
_cod_database_fobs_code          2016715