#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:01:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179274 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/94/4319472.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4319472
loop_
_publ_author_name
'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'
_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
_chemical_name_systematic
;

 ?

;
_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/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 1.0000 2.0000 0.5000 0.0183(4) Uani 1 2 d S . .
N1 N 0.9835(3) 2.1553(4) 0.4076(2) 0.0222(8) Uani 1 1 d . . .
N2 N 1.0976(3) 2.2051(4) 0.3830(2) 0.0238(8) Uani 1 1 d . . .
N11 N 1.1345(3) 1.8651(4) 0.4557(2) 0.0237(8) Uani 1 1 d . . .
N12 N 1.2274(3) 1.9549(4) 0.4249(2) 0.0239(8) Uani 1 1 d . . .
N21 N 1.1464(3) 2.1544(4) 0.5509(2) 0.0215(8) Uani 1 1 d . . .
N22 N 1.2397(3) 2.2049(4) 0.5074(2) 0.0225(8) Uani 1 1 d . . .
C1 C 1.0691(4) 2.3182(5) 0.3198(3) 0.0300(10) Uani 1 1 d . . .
H1A H 1.1315 2.3702 0.2922 0.036 Uiso 1 1 calc R . .
C2 C 0.9353(4) 2.3409(5) 0.3047(3) 0.0318(10) Uani 1 1 d . . .
H2A H 0.8860 2.4141 0.2651 0.038 Uiso 1 1 calc R . .
C3 C 0.8829(4) 2.2361(5) 0.3585(3) 0.0297(10) Uani 1 1 d . . .
H3A H 0.7907 2.2239 0.3601 0.036 Uiso 1 1 calc R . .
C11 C 1.3133(4) 1.8479(5) 0.3973(3) 0.0290(10) Uani 1 1 d . . .
H11A H 1.3852 1.8822 0.3726 0.035 Uiso 1 1 calc R . .
C12 C 1.2765(4) 1.6798(5) 0.4117(3) 0.0320(10) Uani 1 1 d . . .
H12A H 1.3187 1.5743 0.4002 0.038 Uiso 1 1 calc R . .
C13 C 1.1635(4) 1.6958(5) 0.4470(3) 0.0285(10) Uani 1 1 d . . .
H13A H 1.1147 1.6000 0.4625 0.034 Uiso 1 1 calc R . .
C21 C 1.3307(4) 2.3151(5) 0.5486(3) 0.0256(9) Uani 1 1 d . . .
H21A H 1.4041 2.3676 0.5306 0.031 Uiso 1 1 calc R . .
C22 C 1.2967(4) 2.3368(5) 0.6215(3) 0.0303(10) Uani 1 1 d . . .
H22A H 1.3415 2.4065 0.6640 0.036 Uiso 1 1 calc R . .
C23 C 1.1817(4) 2.2342(5) 0.6199(3) 0.0249(9) Uani 1 1 d . . .
H23A H 1.1354 2.2234 0.6626 0.030 Uiso 1 1 calc R . .
C30 C 1.2220(4) 2.1462(5) 0.4261(2) 0.0258(10) Uani 1 1 d . . .
H30A H 1.2957 2.1946 0.4014 0.031 Uiso 1 1 calc R . .
F1 F 0.5689(4) 1.1088(5) 0.3524(3) 0.1054(18) Uani 1 1 d . . .
F2 F 0.5552(5) 1.3321(7) 0.2729(3) 0.117(2) Uani 1 1 d . . .
F3 F 0.3700(3) 1.1742(4) 0.28631(19) 0.0608(10) Uani 1 1 d . . .
F4 F 0.4708(3) 1.3517(3) 0.38414(16) 0.0431(8) Uani 1 1 d . . .
B1 B 0.4887(6) 1.2502(7) 0.3212(4) 0.0495(18) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Fe1 N1 180.00(12) 3_796 . ?
N1 Fe1 N21 93.17(13) 3_796 . ?
N1 Fe1 N21 86.83(13) . . ?
N1 Fe1 N21 86.83(13) 3_796 3_796 ?
N1 Fe1 N21 93.17(13) . 3_796 ?
N21 Fe1 N21 179.999(1) . 3_796 ?
N1 Fe1 N11 87.74(13) 3_796 3_796 ?
N1 Fe1 N11 92.26(13) . 3_796 ?
N21 Fe1 N11 92.22(12) . 3_796 ?
N21 Fe1 N11 87.78(12) 3_796 3_796 ?
N1 Fe1 N11 92.26(13) 3_796 . ?
N1 Fe1 N11 87.74(13) . . ?
N21 Fe1 N11 87.78(12) . . ?
N21 Fe1 N11 92.22(12) 3_796 . ?
N11 Fe1 N11 180.00(17) 3_796 . ?
C3 N1 N2 105.6(3) . . ?
C3 N1 Fe1 136.3(3) . . ?
N2 N1 Fe1 118.1(2) . . ?
N1 N2 C1 110.8(3) . . ?
N1 N2 C30 118.7(3) . . ?
C1 N2 C30 130.5(3) . . ?
C13 N11 N12 104.9(3) . . ?
C13 N11 Fe1 136.8(3) . . ?
N12 N11 Fe1 118.3(2) . . ?
C11 N12 N11 112.4(3) . . ?
C11 N12 C30 129.7(3) . . ?
N11 N12 C30 117.9(3) . . ?
C23 N21 N22 105.2(3) . . ?
C23 N21 Fe1 136.9(3) . . ?
N22 N21 Fe1 117.9(2) . . ?
C21 N22 N21 111.4(3) . . ?
C21 N22 C30 130.4(3) . . ?
N21 N22 C30 118.0(3) . . ?
C2 C1 N2 106.8(4) . . ?
C1 C2 C3 107.1(4) . . ?
N1 C3 C2 109.7(4) . . ?
N12 C11 C12 106.5(3) . . ?
C11 C12 C13 105.8(3) . . ?
N11 C13 C12 110.4(4) . . ?
N22 C21 C22 106.9(3) . . ?
C21 C22 C23 105.5(4) . . ?
N21 C23 C22 111.1(4) . . ?
N2 C30 N22 110.3(3) . . ?
N2 C30 N12 110.0(3) . . ?
N22 C30 N12 108.8(3) . . ?
F2 B1 F4 113.0(4) . . ?
F2 B1 F3 115.8(6) . . ?
F4 B1 F3 110.4(4) . . ?
F2 B1 F1 105.9(5) . . ?
F4 B1 F1 106.6(5) . . ?
F3 B1 F1 104.3(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N1 1.966(3) 3_796 ?
Fe1 N1 1.966(3) . ?
Fe1 N21 1.972(3) . ?
Fe1 N21 1.972(3) 3_796 ?
Fe1 N11 1.977(3) 3_796 ?
Fe1 N11 1.977(3) . ?
N1 C3 1.349(5) . ?
N1 N2 1.364(4) . ?
N2 C1 1.377(5) . ?
N2 C30 1.417(5) . ?
N11 C13 1.339(5) . ?
N11 N12 1.354(4) . ?
N12 C11 1.347(5) . ?
N12 C30 1.460(4) . ?
N21 C23 1.324(5) . ?
N21 N22 1.372(4) . ?
N22 C21 1.351(5) . ?
N22 C30 1.450(5) . ?
C1 C2 1.350(6) . ?
C2 C3 1.403(6) . ?
C11 C12 1.371(6) . ?
C12 C13 1.404(6) . ?
C21 C22 1.376(6) . ?
C22 C23 1.405(5) . ?
F1 B1 1.398(8) . ?
F2 B1 1.325(6) . ?
F3 B1 1.374(6) . ?
F4 B1 1.372(5) . ?
