Tris(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')iron(II) bis(1,1-dicyano-2-ethoxy-2-oxoethanide)
Cai, Zhan-Mao; Zhan, Shu-Zhong; Acta Crystallographica Section E 68 (2012) m956–; doi:10.1107/S1600536812026967

data_2235387
_publ_section_title
;
 Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)
 bis(1,1-dicyano-2-ethoxy-2-oxoethanide)
;
_journal_coeditor_code           BX2413
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m956
_journal_paper_doi               10.1107/S1600536812026967
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Fe (C12 H8 N2)3] (C6 H5 N2 O2)2'
_chemical_formula_sum            'C48 H34 Fe N10 O4'
_chemical_formula_weight         870.70
_chemical_name_systematic
;
Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)
bis(1,1-dicyano-2-ethoxy-2-oxoethanide)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.0680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5855(5)
_cell_length_b                   13.0261(4)
_cell_length_c                   21.4979(6)
_cell_measurement_reflns_used    36630
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.5
_cell_measurement_theta_min      1.86
_cell_volume                     4125.0(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       '\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  0.0813
_diffrn_reflns_av_sigmaI/netI    0.0801
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36630
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.9587
_exptl_absorpt_correction_T_min  0.9197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         8551
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1277
_refine_ls_wR_factor_ref         0.1558
_reflns_number_gt                4862
_reflns_number_total             8551
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bx2413.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2235387
_cod_database_fobs_code          2235387