Triethylammonium [2-ethoxycarbonyl-2-(2-methylbenzyl)-6,9-dinitro-3-oxobicyclo[3.3.1]non-6-en-8-ylidene]azinate
Manickkam, Vaduganathan; Kalaivani, Doraisamyraja; Rajeswari, S.; Acta Crystallographica Section E 67 (2011) o1469–; doi:10.1107/S1600536811018095

data_2230446
_publ_section_title
;
 Triethylammonium
 [2-ethoxycarbonyl-2-(2-methylbenzyl)-6,9-dinitro-3-oxobicyclo[3.3.1]non-6-en-8-ylidene]azinate
;
_journal_coeditor_code           PV2406
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1469
_journal_paper_doi               10.1107/S1600536811018095
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C6 H16 N +, C20 H20 N3 O9 -'
_chemical_formula_moiety         'C6 H16 N +, C20 H20 N3 O9 -'
_chemical_formula_sum            'C26 H36 N4 O9'
_chemical_formula_weight         548.59
_chemical_name_systematic
;
Triethylammonium [2-ethoxycarbonyl-2-(2-methylbenzyl)-6,9-dinitro-
3-oxobicyclo[3.3.1]non-6-en-8-ylidene]azinate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.103(2)
_cell_angle_beta                 100.991(5)
_cell_angle_gamma                93.283(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2820(3)
_cell_length_b                   10.9776(4)
_cell_length_c                   15.9881(6)
_cell_measurement_reflns_used    7927
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.75
_cell_measurement_theta_min      2.14
_cell_volume                     1411.08(9)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w and \f'
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25290
_diffrn_reflns_theta_full        24.63
_diffrn_reflns_theta_max         24.63
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_correction_T_min  0.9712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0542
_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^)+(0.1121P)^2^+0.3791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1965
_reflns_number_gt                3459
_reflns_number_total             4754
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pv2406.cif
_cod_data_source_block           I
_cod_database_code               2230446
_cod_database_fobs_code          2230446