Structural phase transition to disorder low-temperature phase in [Fe(ptz)~6~](BF~4~)~2~ spin-crossover compounds
Kusz, Joachim; Zubko, Maciej; Neder, Reinhard B.; Gütlich, Phillipp; Acta Crystallographica Section B 68 (2012) 40–56; doi:10.1107/S0108768111053298

data_2105064
_publ_section_title
;
 Structural phase transition to disorder low-temperature phase in
 [Fe(ptz)~6~](BF~4~)~2~ spin-crossover compounds
;
_journal_coeditor_code           PC5004
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              40
_journal_page_last               56
_journal_paper_doi               10.1107/S0108768111053298
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C24 H48 Fe N24, 2(B F4)'
_chemical_formula_sum            'C24 H48 B2 F8 Fe N24'
_chemical_formula_weight         902.33
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   10.7023(2)
_cell_length_b                   10.7023(2)
_cell_length_c                   32.0931(15)
_cell_measurement_temperature    84.0(10)
_cell_volume                     3183.44(17)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      84.0(10)
_diffrn_detector_area_resol_mean 16.0328
_diffrn_measured_fraction_theta_full 0.877
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type
;
Oxford Diffraction Diffractometer with Sapphire3 detector
;
_diffrn_measurement_method       '\w - scan'
_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  0.0111
_diffrn_reflns_av_sigmaI/netI    0.0062
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6536
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         3.36
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_T_max  0.9407
_exptl_absorpt_correction_T_min  0.7742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.247
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0368P)^2^+7.1948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                1099
_reflns_number_total             1105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            pc5004.cif
_cod_data_source_block           PTZ_LS-ord_R-3
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2105064