Tris(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')iron(II) bis(1,1,3,3-tetracyano-2-ethoxypropenide) hemihydrate
Setifi, Zouaoui; Setifi, Fatima; Ng, Seik Weng; Oudahmane, Abdelghani; El-Ghozzi, Malika; Avignant, Daniel; Acta Crystallographica Section E 69 (2013) m12–m13; doi:10.1107/S1600536812048611

data_2237151
_publ_section_title
;
 Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)
 bis(1,1,3,3-tetracyano-2-ethoxypropenide) hemihydrate
;
_journal_coeditor_code           HB6994
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m12
_journal_page_last               m13
_journal_paper_doi               10.1107/S1600536812048611
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Fe (C12 H8 N2)3] (C9 H5 N4 O)2, 0.5H2 O'
_chemical_formula_moiety
'C36 H24 Fe1 N6 2+, 2(C9 H5 N4 O -), 0.5(H2 O)'
_chemical_formula_sum            'C54 H35 Fe N14 O2.5'
_chemical_formula_weight         975.81
_chemical_name_systematic
;
Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)
bis(1,1,3,3-tetracyano-2-ethoxypropenide) hemihydrate
;
_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                94.462(2)
_cell_angle_beta                 96.5620(10)
_cell_angle_gamma                101.1290(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3497(3)
_cell_length_b                   14.1736(4)
_cell_length_c                   18.6086(6)
_cell_measurement_reflns_used    7674
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.69
_cell_measurement_theta_min      2.63
_cell_volume                     2391.12(13)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
'X-SEED (Barbour, 2001) and <i>Mercury</i> (Macrae <i>et al.</i>, 2006)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38167
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.9458
_exptl_absorpt_correction_T_min  0.8201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1006
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.426
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         10845
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.6022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                6909
_reflns_number_total             10845
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6994.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C54 H35 Fe N14 O2.50'
_cod_database_code               2237151
_cod_database_fobs_code          2237151