A Synthetic, Structural, Magnetic, and Spectral Study of Several {Fe[tris(pyrazolyl)methane]2}(BF4)2Complexes: Observation of an Unusual Spin-State Crossover
Daniel L. Reger; Christine A. Little; Arnold L. Rheingold; Matthew Lam; Louise M. Liable-Sands; Brian Rhagitan; Tom Concolino; Amitabh Mohan; Gary J. Long; Valérie Briois; Fernande Grandjean; Inorganic Chemistry 40 (2001) 1508–1520; doi:10.1021/ic001102t

data_4319473
_publ_section_title
;
 A Synthetic, Structural, Magnetic, and Spectral Study of Several
 {Fe[tris(pyrazolyl)methane]2}(BF4)2Complexes: Observation of an Unusual
 Spin-State Crossover
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1508
_journal_page_last               1520
_journal_paper_doi               10.1021/ic001102t
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C37.5 H33 B2 F8 Fe N10 O0.5'
_chemical_formula_weight         861.21
_chemical_name_systematic
;

 ?

;
_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                83.0105(8)
_cell_angle_beta                 84.5554(7)
_cell_angle_gamma                62.5797(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4769(2)
_cell_length_b                   12.7449(2)
_cell_length_c                   13.0215(2)
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     1822.57(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14121
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.8847
_exptl_absorpt_correction_T_min  0.8243
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            maroon
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.802
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         7843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.802
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.137
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1988
_refine_ls_wR_factor_ref         0.2061
_reflns_number_gt                7322
_reflns_number_total             7843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001102t_2.cif
_cod_data_source_block           dlr44
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1822.57(4)
_cod_original_formula_sum        'C37.50 H33 B2 F8 Fe N10 O0.50'
_cod_database_code               4319473