Tris(5,6-dimethyl-1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')iron(II) bis(tricyanomethanide)
Váhovská, Lucia; Potočňák, Ivan; Acta Crystallographica Section E 68 (2012) m1524–m1525; doi:10.1107/S1600536812046880

data_2236832
_publ_section_title
;
 Tris(5,6-dimethyl-1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)
 bis(tricyanomethanide)
;
_journal_coeditor_code           BX2428
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1524
_journal_page_last               m1525
_journal_paper_doi               10.1107/S1600536812046880
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Fe (C14 H12 N2)3] (C4 N3)2'
_chemical_formula_moiety         'C42 H36 Fe N6 2+, 2(C4 N3 -)'
_chemical_formula_sum            'C50 H36 Fe N12'
_chemical_formula_weight         860.76
_chemical_name_systematic
;
Tris(5,6-dimethyl-1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)
bis(tricyanomethanide)
;
_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                75.458(5)
_cell_angle_beta                 89.623(3)
_cell_angle_gamma                82.323(4)
_cell_formula_units_Z            2
_cell_length_a                   9.3676(3)
_cell_length_b                   12.7079(9)
_cell_length_c                   18.1998(9)
_cell_measurement_reflns_used    5036
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.2328
_cell_measurement_theta_min      2.9578
_cell_volume                     2077.5(2)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 8.3438
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Agilent Xcalibur (Sapphire2)'
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15408
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.416
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.874
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2012), based on expressions derived by Clark &
Reid
(1995)]
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.6642
_exptl_crystal_size_mid          0.2531
_exptl_crystal_size_min          0.0338
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         8167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0501
_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^)+(0.0473P)^2^+1.1913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                6309
_reflns_number_total             8167
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bx2428.cif
_cod_data_source_block           I
_cod_original_cell_volume        2077.52(19)
_cod_database_code               2236832
_cod_database_fobs_code          2236832