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_4304214
_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         'C18 H21 Fe N8 O4 S2, 0.5(C2 H8 O2), 3(H2 O)'
_chemical_formula_sum            'C19 H31 Fe N8 O8 S2'
_chemical_formula_weight         619.48
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
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_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   direct
_audit_creation_date             '2006-06-08  11:24:48'
_audit_creation_method
;
 PLATON <TABLE ACC> option    (version ::  40506)
 SHELXL97-2 & Manual Editing 
;
_cell_angle_alpha                83.347(3)
_cell_angle_beta                 83.896(3)
_cell_angle_gamma                68.914(3)
_cell_formula_units_Z            2
_cell_length_a                   10.701(2)
_cell_length_b                   10.846(2)
_cell_length_c                   11.910(2)
_cell_measurement_reflns_used    2956
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.54
_cell_volume                     1277.9(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
;
 SIR2002 (Burla et al., 2003)
;
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.971
_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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0748
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9700
_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         26.01
_diffrn_reflns_theta_min         2.58
_diffrn_standards_decay_%        0
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_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.9452
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.612
_refine_diff_density_min         -0.943
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         4874
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          1.169
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^2^+3.20P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1424
_reflns_number_gt                3702
_reflns_number_total             4874
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic701695b-file002.cif
_cod_data_source_block           DATNAM
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        1278.0(4)
_cod_database_code               4304214
_vrn_publ_code_frame_time_sec    20.0
_vrn_publ_code_meas_time_hour    13.5