Complete and incomplete spin transitions in 1D chain iron(ii) compounds
Pfaffeneder, Toni M.; Thallmair, Sebastian; Bauer, Wolfgang; Weber, Birgit; New Journal of Chemistry 35 (2011) 691–; doi:10.1039/c0nj00750a

data_7052587
_publ_section_title
;
 Complete and incomplete spin transitions in 1D chain iron(ii)
 compounds
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              691
_journal_paper_doi               10.1039/c0nj00750a
_journal_volume                  35
_journal_year                    2011
_chemical_compound_source
;
A mixture of 0.12 g [FeL1(MeOH)~2~] (0.21 mmol) and 0.25 g
bis(1<i>H</i>-imidazol-1-yl)methane (1.66 mmol) in 10 mL methanol was heated
at reflux for 1 h. After cooling, the dark brown precipitate was filtered off,
washed with 3 mL methanol and dried in vacuum. Single crystals of (I) were
slowly formed by diffusion techniques in methanol solution after several weeks.
;
_chemical_formula_moiety         'C35 H30 Fe N6 O4'
_chemical_formula_sum            'C35 H30 Fe N6 O4'
_chemical_formula_weight         654.496
_chemical_name_common
;
(2,2')-(1,2-phenylenebis(iminomethylidyne)bis(1-phenylbutane-
1,3-dione) (2-)-N,N',O$3!,O$3!')(bis(1H-imidazol-1-yl) methane)iron(ii)
;
_chemical_name_systematic
;
[2,2']-[1,2-phenylenebis(iminomethylidyne)bis(1-phenylbutane-1,3-dione)
(2-)-<i>N</i>,<i>N</i>',<i>O</i>^3^,<i>O</i>^3^'](bis(1<i>H</i>-imidazol-1-yl)
methane)iron(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_block_code                Fe_L5e_bimm_250K_ex179_Bauer
_audit_creation_date
;
'Sat Apr 25 21:03:38 2009'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             24-Sep-10
_cell_angle_alpha                75.074(19)
_cell_angle_beta                 81.233(17)
_cell_angle_gamma                64.423(18)
_cell_formula_units_Z            2
_cell_length_a                   10.3530(16)
_cell_length_b                   10.928(2)
_cell_length_c                   15.794(4)
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      27.5447
_cell_measurement_theta_min      3.7592
_cell_volume                     1555.7(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics
;
ORTEP (M. N. Burnett, C. K. Johnson, ORTEP-III: Oak Ridge Thermal Ellipsoid
Plot Program for Crystal Structure Illustrations, Oak Ridge National
Laboratory Report ORNL-6895, 1996). Windows version (L. J. Farrugia, Univ.
Glasgow) used --- SCHAKAL (E. Keller, University of Freiburg (Breisgau),
Germany, 1995).
;
_computing_publication_material
;
PLATON (A. L. Spek, Acta Crystallogr, Sect. A, 1990, 46, C34, 1995 version).
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      250(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
1 omega -50.00 53.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- -17.4513 37.0000 -180.0000 103

2 omega -10.00 90.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 17.6076 77.0000 30.0000 100

3 omega -11.00 81.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 17.6076 77.0000 150.0000 92

4 omega -55.00 46.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 17.6076 -77.0000 -60.0000 101

5 omega -51.00 51.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 17.6076 -77.0000 30.0000 102

6 omega -11.00 88.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 17.6076 77.0000 -90.0000 99

7 omega -4.00 77.00 1.0000 20.0000
omega____ theta____ kappa____ phi______ frames
- 17.6076 -124.0000 -99.0000 81

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0272666731
_diffrn_orient_matrix_UB_12      -0.0477583882
_diffrn_orient_matrix_UB_13      0.0261236481
_diffrn_orient_matrix_UB_21      0.0708943816
_diffrn_orient_matrix_UB_22      -0.0518915340
_diffrn_orient_matrix_UB_23      0.0058225429
_diffrn_orient_matrix_UB_31      0.0034727833
_diffrn_orient_matrix_UB_32      0.0213410900
_diffrn_orient_matrix_UB_33      0.0380614622
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17523
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.76
_diffrn_source_current           40
_diffrn_source_power             2.01
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.535
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       palett
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0527P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                3350
_reflns_number_total             5624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0NJ00750A.TXT
_cod_data_source_block           ex179
_cod_original_cell_volume        1555.7(5)
_cod_database_code               7052587