Crystal structure of <i>fac</i>-bis[bis(pyridin-2-yl)methanamine]iron(II) 1,1,3,3-tetracyano-2-(dicyanomethylidene)propane-1,3-diide, [Fe(dipa)~2~](tcpd)
Setifi, Zouaoui; Corfield, Peter W. R.; Setifi, Fatima; Morgenstern, Bernd; Hegetschweiler, Kaspar; Kaddouri, Yassine; Acta Crystallographica Section E 74 (2018) 1227–1230; doi:10.1107/S2056989018011143

data_2242590
_publ_section_title
;
 Crystal structure of <i>fac</i>-bis[bis(pyridin-2-yl)methanamine]iron(II)
 1,1,3,3-tetracyano-2-(dicyanomethylidene)propane-1,3-diide,
 [Fe(dipa)~2~](tcpd)
;
_journal_coeditor_code           HB7760
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1227
_journal_page_last               1230
_journal_paper_doi               10.1107/S2056989018011143
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '[Fe (C11 H11 N3)2] (C10 N6)'
_chemical_formula_moiety         'C22 H22 Fe N6 2+, C10 N6 2-'
_chemical_formula_sum            'C32 H22 Fe N12'
_chemical_formula_weight         630.46
_chemical_name_systematic
;
<i>fac</i>-Bis[bis(pyridin-2-yl)methanamine]iron(II)
1,1,3,3-tetracyano-2-(dicyanomethylene)propane-1,3-diide, [Fe(dipa)~2~](tcpd)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 117.006(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5394(7)
_cell_length_b                   13.5094(7)
_cell_length_c                   13.7913(6)
_cell_measurement_reflns_used    3760
_cell_measurement_temperature    162(2)
_cell_measurement_theta_max      27.05
_cell_measurement_theta_min      2.18
_cell_volume                     2911.5(2)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      162(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11328
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.144
_diffrn_reflns_theta_min         1.993
_exptl_absorpt_coefficient_mu    0.564
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2015)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.422
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3227
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0355P)^2^+2.4992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                2623
_reflns_number_total             3227
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7760sup1.cif
_cod_data_source_block           I
_cod_database_code               2242590
_shelx_estimated_absorpt_t_min   0.809
_shelx_estimated_absorpt_t_max   0.988
_shelx_hkl_checksum              46187
_shelx_res_checksum              34306
_cod_database_fobs_code 2242590