Crystal structure of methyl 2-[2,4-bis(4-fluorophenyl)-3-azabicyclo[3.3.1]nonan-9-ylidene]hydrazinecarboxylate
Kamaraj, A.; Rajkumar, R.; Krishnasamy, K.; Murugavel, S.; Acta Crystallographica Section E 70 (2014) 145–147; doi:10.1107/S1600536814018935

data_2239933
_publ_section_title
;
 Crystal structure of methyl
 2-[2,4-bis(4-fluorophenyl)-3-azabicyclo[3.3.1]nonan-9-ylidene]hydrazinecarboxylate
;
_journal_coeditor_code           SU2773
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              145
_journal_page_last               147
_journal_paper_doi               10.1107/S1600536814018935
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C22 H23 F2 N3 O2'
_chemical_formula_moiety         'C22 H23 F2 N3 O2'
_chemical_formula_sum            'C22 H23 F2 N3 O2'
_chemical_formula_weight         399.43
_chemical_name_systematic
2-[2,4-Bis(4-fluorophenyl)-3-azabicyclo[3.3.1]nonan-9-ylidene]hydrazinecarboxylate
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.997(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.751(6)
_cell_length_b                   7.087(2)
_cell_length_c                   28.492(9)
_cell_measurement_reflns_used    3821
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      1.5
_cell_volume                     3886(2)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia (2012)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and  PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            18613
_diffrn_reflns_theta_full        26.06
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         1.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0752P)^2^+2.7221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1472
_reflns_number_gt                2872
_reflns_number_total             3793
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2773sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2239933
_cod_database_fobs_code          2239933