The LIESST state of [Fe(pic)~3~]Cl~2~.EtOH – the superstructure under continuous irradiation
Kusz, Joachim; Schollmeyer, Dieter; Spiering, Hartmunt; Gütlich, Philipp; Journal of Applied Crystallography 38 (2005) 528–536; doi:10.1107/S0021889805009891

data_2300096
_publ_section_title
;
 The LIESST state of [Fe(pic)~3~]Cl~2~.EtOH -- the superstructure under
 continuous irradiation
;
_journal_coden_ASTM              JACGAR
_journal_issue                   3
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              528
_journal_page_last               536
_journal_paper_doi               10.1107/S0021889805009891
_journal_volume                  38
_journal_year                    2005
_chemical_formula_moiety         'C18 H24 Fe N6, C2 H6 O, 2(Cl)'
_chemical_formula_sum            'C20 H30 Cl2 Fe N6 O'
_chemical_formula_weight         497.25
_chemical_name_common
;
 tris(2-Picolylamine)-iron(ii) chloride ethanol solvate
;
_chemical_name_systematic
;
 tris(2-Picolylamine)-iron(ii) chloride ethanol solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.184(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7322(14)
_cell_length_b                   21.5055(7)
_cell_length_c                   11.323(2)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    10(2)
_cell_measurement_theta_max      40
_cell_measurement_theta_min      30
_cell_volume                     2324.7(6)
_computing_cell_refinement       'STADI4 (Stoe, 1995)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      10.0(10)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'CCD Oxford Diffraction'
_diffrn_measurement_method       \f-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1049
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20473
_diffrn_reflns_theta_full        27.85
_diffrn_reflns_theta_max         27.85
_diffrn_reflns_theta_min         3.91
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.569
_refine_ls_extinction_coef       0.0044(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+5.8012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1301
_reflns_number_gt                4302
_reflns_number_total             5154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ks5056.cif
_cod_data_source_block           fpic10k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+5.8012P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+5.8012P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2324.7(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2300096