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_4319472
_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            'C20 H20 B2 F8 Fe N12'
_chemical_formula_weight         657.95
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.7733(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1891(2)
_cell_length_b                   7.6223(2)
_cell_length_c                   17.2411(4)
_cell_measurement_temperature    173(2)
_cell_volume                     1315.42(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 0.867
_diffrn_measured_fraction_theta_max 0.867
_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    0.0295
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4723
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.924
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.217
_refine_ls_shift/su_mean         0.042
_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          0.2051
_refine_ls_wR_factor_ref         0.2154
_reflns_number_gt                1848
_reflns_number_total             2007
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001102t_1.cif
_cod_data_source_block           dlr41
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        1315.41(7)
_cod_database_code               4319472