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_4327583
_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_moiety         'C32 H44 Fe N12, 2(B F4)'
_chemical_formula_sum            'C32 H44 B2 F8 Fe N12'
_chemical_formula_weight         826.26
_chemical_name_common            00220
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 111.093(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.348(2)
_cell_length_b                   10.3372(7)
_cell_length_c                   19.661(1)
_cell_measurement_reflns_used    7463
_cell_measurement_temperature    220(2)
_cell_volume                     3858.4(5)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SMART Platform CCD, Bruker'
_diffrn_measurement_method       omega-scans
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19114
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.859471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing (1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+1.7958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                3417
_reflns_number_total             4418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0100562B_2.cif
_cod_data_source_block           00220
_cod_original_cell_volume        3858.4(4)
_cod_database_code               4327583