Magnetism and crystal structure of an N~3~O~3~-coordinated iron(II) complex
Bauer, Wolfgang; Weber, Birgit; Acta Crystallographica Section C 64 (2008) m237–m239; doi:10.1107/S0108270108013498

data_2016653
_publ_section_title
;
 Magnetism and crystal structure of an N~3~O~3~-coordinated iron(II)
 complex
;
_journal_coeditor_code           SQ3144
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m237
_journal_page_last               m239
_journal_paper_doi               10.1107/S0108270108013498
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Fe (C20 H22 N2 O6) (C5 H6 N2) (C H4 O)]'
_chemical_formula_moiety         'C26 H32 Fe N4 O7'
_chemical_formula_sum            'C26 H32 Fe N4 O7'
_chemical_formula_weight         568.400
_chemical_name_common            '[FeL1a(3-apy)(MeOH)]'
_chemical_name_systematic
;
(3-aminopyridine-\kN^1^){(<i>E</i>,<i>E</i>)-diethyl
2,2'-[1,2-phenylenebis(nitrilomethylidyne)]bis(3-oxobutanate)(2-)-
\k^2^O^3^,N,N',O^3'^}(methanol-\kO)iron(II)
;
_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
_cell_angle_alpha                72.740(17)
_cell_angle_beta                 75.67(3)
_cell_angle_gamma                68.91(2)
_cell_formula_units_Z            2
_cell_length_a                   11.234(4)
_cell_length_b                   11.5760(11)
_cell_length_c                   11.834(3)
_cell_measurement_reflns_used    8635
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.1925
_cell_measurement_theta_min      3.7303
_cell_volume                     1354.0(6)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2005)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2005)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2005)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and
SCHAKAL99 (Keller, 1999)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23067
_diffrn_reflns_theta_full        25.23
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         3.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.3942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                2998
_reflns_number_total             4708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sq3144.cif
_cod_data_source_block           I
_cod_database_code               2016653
_cod_database_fobs_code          2016653