Iron(ii) spin transition coordination polymers with a zigzag structure
Bauer, Wolfgang; Dîrtu, Marinela M.; Garcia, Yann; Weber, Birgit; CrystEngComm 14 (2012) 1223–; doi:10.1039/c2ce06253d

data_7207253
_publ_section_title
;
 Iron(ii) spin transition coordination polymers with a zigzag structure
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              1223
_journal_paper_doi               10.1039/c2ce06253d
_journal_volume                  14
_journal_year                    2012
_chemical_compound_source
;
The synthesis of (I) was carried out under argon using Schlenk tube
techniques. [Fe(L1a)(MeOH)~2~] (0.43 g, 0.85 mmol) and
Bis(4-pyridylmethyl)sulfide (0.92 g, 4.25 mmol) were dissolved in 50 ml
ethanol and heated to reflux for four hours. After 24 hours at room
temperature the product was filtered off and washed two
times with ice-cold ethanol. (I) was obtained as dark purple solid
with a yield of 75%. Crystals suitable for X-ray structure analysis
were obtain after recrystallization from toluene.
;
_chemical_formula_moiety         'C32 H34 Fe N4 O6 S'
_chemical_formula_sum            'C32 H34 Fe N4 O6 S'
_chemical_formula_weight         658.547
_chemical_name_common
;
poly-(E,E)-((diethyl-2,2'-(1,2-
phenylenebis(iminomethylidyne))bis(3-oxobutanato) (2-)-
N,N',O$3,O!3')(bis(4-pyridylmethyl)sulfide)iron(ii)
;
_chemical_name_systematic
;
poly-(E,E)-[{diethyl-2,2'-[1,2-phenylenebis(iminomethylidyne)]bis[3-oxobutanato]
(2-)-N,N',O^3,O^3'}(bis(4-pyridylmethyl)sulfide)iron(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                Fe_L1_bpms_mo231_Bauer
_audit_creation_date
;
'Sat Aug 23 20:54:50 2008'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             26-Aug-08
_cell_angle_alpha                90.00
_cell_angle_beta                 125.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.164(7)
_cell_length_b                   19.0805(11)
_cell_length_c                   16.115(7)
_cell_measurement_reflns_used    6475
_cell_measurement_temperature    225(2)
_cell_measurement_theta_max      26.2499
_cell_measurement_theta_min      3.7719
_cell_volume                     3028(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_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      225(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
1 phi -149.00 -89.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -20.9181 0.0000 - 0.0000 0.0000 60

2 omega -2.00 50.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -20.9181 75.0000 120.0000 0.0000 0.0000 52

3 omega -47.00 3.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -20.9181 45.0000 240.0000 0.0000 0.0000 50

4 omega -52.00 0.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -20.9181 75.0000 0.0000 0.0000 0.0000 52

5 phi 89.00 149.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
-40.0000 -20.9181 0.0000 - 0.0000 0.0000 60

6 omega -52.00 0.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -20.9181 75.0000 120.0000 0.0000 0.0000 52

7 omega 40.00 92.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 75.0000 120.0000 0.0000 0.0000 52

8 phi -61.00 1.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
40.0000 21.0744 0.0000 - 0.0000 0.0000 62

9 phi 59.00 121.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
40.0000 21.0744 0.0000 - 0.0000 0.0000 62

10 omega -10.00 42.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 75.0000 0.0000 0.0000 0.0000 52

11 omega -10.00 42.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 75.0000 240.0000 0.0000 0.0000 52

12 omega 1.00 52.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 -75.0000 120.0000 0.0000 0.0000 51

13 omega 40.00 92.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 75.0000 0.0000 0.0000 0.0000 52

14 omega 40.00 92.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 75.0000 240.0000 0.0000 0.0000 52

15 omega -10.00 42.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 75.0000 120.0000 0.0000 0.0000 52

16 omega -38.00 -5.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 -75.0000 120.0000 0.0000 0.0000 33

17 omega -51.00 -1.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 -45.0000 240.0000 0.0000 0.0000 50

18 omega -27.00 20.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 -97.0000 345.0000 0.0000 0.0000 47

19 omega -5.00 23.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 45.0000 120.0000 0.0000 0.0000 28

20 omega 12.00 53.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 -76.0000 16.0000 0.0000 0.0000 41

21 omega 41.00 82.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 -129.0000 327.0000 0.0000 0.0000 41

22 omega -3.00 47.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 21.0744 -45.0000 240.0000 0.0000 0.0000 50

23 phi -121.00 -93.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
40.0000 21.0744 0.0000 - 0.0000 0.0000 28

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0266964541
_diffrn_orient_matrix_UB_12      0.0076821107
_diffrn_orient_matrix_UB_13      0.0512497265
_diffrn_orient_matrix_UB_21      0.0516478689
_diffrn_orient_matrix_UB_22      0.0050084188
_diffrn_orient_matrix_UB_23      -0.0159386309
_diffrn_orient_matrix_UB_31      -0.0128955095
_diffrn_orient_matrix_UB_32      0.0360252046
_diffrn_orient_matrix_UB_33      -0.0087060680
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57671
_diffrn_reflns_theta_full        26.31
_diffrn_reflns_theta_max         26.31
_diffrn_reflns_theta_min         3.78
_diffrn_source_current           45
_diffrn_source_power             2.50
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           55
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.4446
_exptl_crystal_density_meas      1.4446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         6157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0492P)^2^+2.0115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                4539
_reflns_number_total             6157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce06253d.txt
_cod_data_source_block           mo231
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7207253