Crystal structure of 1-ferrocenyl-2-(4-methylbenzoyl)spiro[11<i>H</i>-pyrrolidizine-3,11'-indeno[1,2-<i>b</i>]quinoxaline]
Chandralekha, Kuppan; Gavaskar, Deivasigamani; Sureshbabu, Adukamparai Rajukrishnan; Lakshmi, Srinivasakannan; Acta Crystallographica Section E 70 (2014) 124–126; doi:10.1107/S1600536814017644

data_2239834
_publ_section_title
;
 Crystal structure of
 1-ferrocenyl-2-(4-methylbenzoyl)spiro[11<i>H</i>-pyrrolidizine-3,11'-indeno[1,2-<i>b</i>]quinoxaline]
;
_journal_coeditor_code           RZ5131
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              124
_journal_page_last               126
_journal_paper_doi               10.1107/S1600536814017644
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Fe (C5 H5) (C34 H28 N3 O)]'
_chemical_formula_moiety         'C39 H33 Fe N3 O'
_chemical_formula_sum            'C39 H33 Fe N3 O'
_chemical_formula_weight         615.53
_chemical_name_systematic
;
1-Ferrocenyl-2-(4-methylbenzoyl)spiro[11<i>H</i>-pyrrolidizine-3,11'-\
indeno[1,2-<i>b</i>]quinoxaline]
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 116.1790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0017(4)
_cell_length_b                   30.2487(10)
_cell_length_c                   9.3597(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.359
_cell_measurement_theta_min      4.843
_cell_volume                     3049.35(18)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 2004)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 2012) and SCHAKAL99 (Keller, 1999)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'Bruker axs kappa apex2 CCD Diffractometer'
_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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17682
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.8786
_exptl_absorpt_correction_T_min  0.8359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.153
_refine_ls_abs_structure_details 'Flack (1983), 2669 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.007(9)
_refine_ls_extinction_coef       0.00070(15)
_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   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         5362
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.3631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0624
_reflns_number_gt                5128
_reflns_number_total             5362
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz5131sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        3049.35(17)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2239834
_cod_database_fobs_code          2239834