Variable-Temperature X-ray Structural Investigation of {Fe[HC(3,5-Me2pz)3]2}(BF4)2 (pz = Pyrazolyl Ring): Observation of a Thermally Induced Spin State Change from All High Spin to an Equal High Spin-Low Spin Mixture, Concomitant with the Onset of Nonmerohedral Twinning
Daniel L. Reger; Christine A. Little; Victor G. Young; Maren Pink; Inorganic Chemistry 40 (2001) 2870–2874; doi:10.1021/ic010056+

data_4327585
_publ_section_title
;
 Variable-Temperature X-ray Structural Investigation of
 {Fe[HC(3,5-Me2pz)3]2}(BF4)2 (pz = Pyrazolyl Ring): Observation of a
 Thermally Induced Spin State Change from All High Spin to an Equal High
 Spin-Low Spin Mixture, Concomitant with the Onset of Nonmerohedral
 Twinning
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2870
_journal_page_last               2874
_journal_paper_doi               10.1021/ic010056+
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C32 H44 B2 F8 Fe N12'
_chemical_formula_weight         826.25
_chemical_name_common            00110aaa
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.852(4)
_cell_angle_beta                 105.245(4)
_cell_angle_gamma                116.304(4)
_cell_formula_units_Z            2
_cell_length_a                   10.287(2)
_cell_length_b                   11.355(3)
_cell_length_c                   18.949(4)
_cell_measurement_temperature    173(1)
_cell_volume                     1892.2(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11367
_diffrn_reflns_theta_full        25.22
_diffrn_reflns_theta_max         25.22
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       Euhedral
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         6622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1048
_reflns_number_gt                4322
_reflns_number_total             6622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0100562B_4.cif
_cod_data_source_block           00110aaa
_cod_original_cell_volume        1892.3(8)
_cod_database_code               4327585