Oxidative degradation of the organometallic iron(II) complex [Fe{bis[3-(pyridin-2-yl)-1H-imidazol-1-yl]methane}(MeCN)(PMe3)](PF6)2: structure of the ligand decomposition product trapped via coordination to iron(II).
Haslinger, Stefan; Pöthig, Alexander; Cokoja, Mirza; Kühn, Fritz E; Acta crystallographica. Section C, Structural chemistry 71 (2015) 1096–1099; doi:10.1107/S2053229615021968

data_2311849
_publ_section_title
;
 Oxidative degradation of the organometallic iron(II) complex
 [Fe{bis[3-(pyridin-2-yl)-1H-imidazol-1-yl]methane}(MeCN)(PMe3)](PF6)2:
 structure of the ligand decomposition product trapped via coordination to
 iron(II).
;
_journal_coeditor_code           FP3018
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              1096
_journal_page_last               1099
_journal_paper_doi               10.1107/S2053229615021968
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac
'[Fe (C17 H14 N6) (C16 H12 N6) (C3 H9 P)] (P F6)2'
_chemical_formula_moiety         'C36 H35 Fe N12 P 2+, 2(F6 P -)'
_chemical_formula_sum            'C36 H35 F12 Fe N12 P3'
_chemical_formula_weight         1012.52
_chemical_name_systematic
;[1,1'-Bis(pyridin-2-yl)-2,2-bi(1<i>H</i>-imidazole)-\k<i>N</i>^3^][3,3'-bis(pyridin-2-yl-\k<i>N</i>)-1,1'-methanediylbi(1<i>H</i>-imidazol-2-yl-\k<i>C</i>^2^)](trimethylphosphane-\k<i>P</i>)iron(II)
bis(hexafluoridophosphate)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                97.219(2)
_cell_angle_beta                 97.020(2)
_cell_angle_gamma                102.060(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1146(4)
_cell_length_b                   12.1591(5)
_cell_length_c                   17.7002(7)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.3881
_cell_measurement_theta_min      2.3473
_cell_volume                     2087.05(15)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
PLATON (Spek, 2009) and enCIFer (Allen <i>et al.</i>,  2004)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015) and SHELXLE (H\"ubschle <i>et al.</i>,
2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w rotation'
_diffrn_radiation_monochromator  'MONTEL optic'
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_sigmaI/netI    0.0671
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52121
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4143
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.133
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.732
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         7607
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0432P)^2^+3.9609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                5543
_reflns_number_total             7607
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fp3018sup1.cif
_cod_data_source_block           I
_cod_database_code               2311849