Study of Neutral Fe(III) Complexes of Pyridoxal-N-Substituted Thiosemicarbazone with Desolvation-Induced Spin-State Transformation above Room Temperature
Eddy W. Yemeli Tido; Gert O. R. Alberda van Ekenstein; Auke Meetsma; Petra J. van Koningsbruggen; Inorganic Chemistry 47 (2008) 143–153; doi:10.1021/ic701695b

data_4304213
_publ_contact_author_address
;
     Crystal Structure Center,
     Chemical Physics,
     Zernike Institute for Advanced Materials,
     University of Groningen,
     Nijenborgh 4,
     NL-9747 AG Groningen,
     The Netherlands.
;
_publ_contact_author_email       A.Meetsma@rug.nl
_publ_contact_author_fax         '+31 50 3634441'
_publ_contact_author_name
;
   Drs. A. Meetsma
;
_publ_contact_author_phone       '+31 50 3634368'
_publ_section_title
;
Study of Neutral Fe(III) Complexes of Pyridoxal-N-Substituted
Thiosemicarbazone with Desolvation-Induced Spin-State Transformation above
Room Temperature
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              143
_journal_page_last               153
_journal_paper_doi               10.1021/ic701695b
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C20 H25 Fe N8 O4 S2, 2(H2 O)'
_chemical_formula_sum            'C20 H29 Fe N8 O6 S2'
_chemical_formula_weight         597.48
_chemical_name_systematic        ?
_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   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2006-05-03  13:37:31'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version :: 280206)
 SHELXL97-2 & Manual Editing 
;
_cell_angle_alpha                90
_cell_angle_beta                 107.589(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.599(1)
_cell_length_b                   24.273(2)
_cell_length_c                   9.0649(9)
_cell_measurement_reflns_used    7811
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.07
_cell_measurement_theta_min      2.49
_cell_volume                     2432.8(4)
_computing_cell_refinement       'SAINTPLUS, Version 6.02A, (Bruker, 2000)'
_computing_data_collection       'SMART, Version 5.624, (Bruker, 2001)'
_computing_data_reduction        'XPREP, Version 5.1/NT, (Bruker, 2000)'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 2006) 
 PLATON (Spek, 2003)
;
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 DIRDIF-99 (Beurskens et al., 1999)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
  Bruker Smart Apex; CCD area detector 
;
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_detector
;
  CCD area-detector
;
_diffrn_radiation_monochromator  'parallel mounted graphite'
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            18107
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization
  effects, decay and absorption and reduced to F~o~^2^
  using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.9751
_exptl_absorpt_correction_T_min  0.8405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, Bruker, 2001))'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         4599
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.652
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+2.4341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                3454
_reflns_number_total             4599
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701695b-file001.cif
_cod_data_source_block           Q1109
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4304213
_vrn_publ_code_frame_time_sec    30.0
_vrn_publ_code_meas_time_hour    18.1