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_7207255
_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(L1f)(MeOH)~2~] and
Bis(4-pyridylmethyl)sulfide were dissolved in
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. Crystals suitable for X-ray structure analysis
were obtain after recrystallization.
;
_chemical_formula_moiety         'C42 H38 Fe N4 O6 S'
_chemical_formula_sum            'C42 H38 Fe N4 O6 S'
_chemical_formula_weight         782.685
_chemical_name_common            '[FeL4(bpms)]HS'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                Fe_L4_bpms_oo195_Bauer
_audit_creation_date
;
'Wed Oct 27 07:16:47 2010'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             21-Sep-11
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2017(5)
_cell_length_b                   16.2729(8)
_cell_length_c                   25.7799(15)
_cell_measurement_reflns_used    8846
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      26.2496
_cell_measurement_theta_min      4.2358
_cell_volume                     8055.4(6)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
;
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
1 omega 60.00 89.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 21.3869 -138.0000 30.0000 29

2 omega 60.00 101.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 21.3869 179.0000 -180.0000 41

3 omega -7.00 48.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 21.3869 -77.0000 -120.0000 55

4 omega -53.00 64.00 1.0000 30.0000
omega____ theta____ kappa____ phi______ frames
- 21.3869 0.0000 90.0000 117

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0355337322
_diffrn_orient_matrix_UB_12      0.0118613322
_diffrn_orient_matrix_UB_13      0.0132598291
_diffrn_orient_matrix_UB_21      -0.0190924512
_diffrn_orient_matrix_UB_22      0.0074975796
_diffrn_orient_matrix_UB_23      -0.0240981481
_diffrn_orient_matrix_UB_31      -0.0165146097
_diffrn_orient_matrix_UB_32      -0.0341703875
_diffrn_orient_matrix_UB_33      -0.0006792936
_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  0.0376
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            32198
_diffrn_reflns_theta_full        26.27
_diffrn_reflns_theta_max         26.27
_diffrn_reflns_theta_min         4.24
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.2908
_exptl_crystal_density_meas      1.2908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.823
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.823
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                4323
_reflns_number_total             8144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce06253d.txt
_cod_data_source_block           oo195
_cod_database_code               7207255