Bis[tris(pyridin-2-yl)amine]iron(II) tris(dicyanomethylidene)methanediide
Setifi, Zouaoui; Setifi, Fatima; Dege, Necmi; Al-Douh, Mohammed Hadi; Glidewell, Christopher; IUCrData 5 (2020) x201278–; doi:10.1107/S241431462001278X

data_1559209
_publ_section_title
;
 Bis[tris(pyridin-2-yl)amine]iron(II) tris(dicyanomethylidene)methanediide
;
_journal_coeditor_code           IM4010
_journal_issue                   9
_journal_name_full               IUCrData
_journal_page_first              x201278
_journal_paper_doi               10.1107/S241431462001278X
_journal_volume                  5
_journal_year                    2020
_chemical_formula_iupac          '[Fe (C15 H12 N4)2] (C10 N6)'
_chemical_formula_moiety         'C30 H24 Fe N8 2+, C10 N6 2-'
_chemical_formula_sum            'C40 H24 Fe N14'
_chemical_formula_weight         756.58
_chemical_name_systematic
;
Bis[tris(pyridin-2-yl)amine]iron(II) tris(dicyanomethylidene)methanediide
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                98.825(7)
_cell_angle_beta                 90.900(7)
_cell_angle_gamma                117.747(6)
_cell_formula_units_Z            1
_cell_length_a                   9.8291(8)
_cell_length_b                   10.0499(8)
_cell_length_c                   11.0308(9)
_cell_measurement_reflns_used    4139
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.070
_cell_measurement_theta_min      1.878
_cell_volume                     948.19(15)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-RED32 (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020) and Mercury (Macrae <i>et al.</i>,  2020)
;
_computing_publication_material
;
SHELXL-2014 (Sheldrick, 2015) and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL-2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS86 (Sheldrick, 2015)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9558
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.547
_diffrn_reflns_theta_min         1.878
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.447
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.899
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED32; Stoe & Cie, 2002)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       needle
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_refine_diff_density_max         1.008
_refine_diff_density_min         -0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3955
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0793P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1641
_reflns_number_gt                2609
_reflns_number_total             3955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            im4010sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        948.18(14)
_cod_database_code               1559209
_shelx_estimated_absorpt_t_min   0.845
_shelx_estimated_absorpt_t_max   0.952
_shelx_hkl_checksum              75606
_shelx_res_checksum              660
_shelx_fab_checksum              47093
_shelxl_version_number           2.014
_cod_database_fobs_code 1559209