#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:51:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179266 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/86/4318684.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_4318684
loop_
_publ_author_name
'Apurba K. Patra'
'Marilyn M. Olmstead'
'Pradip K. Mascharak'
_publ_section_title
;
 Spontaneous Reduction of a Low-Spin Fe(III) Complex of a Neutral
 Pentadentate N5 Schiff Base Ligand to the Corresponding Fe(II) Species in
 Acetonitrile
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5403
_journal_page_last               5409
_journal_paper_doi               10.1021/ic020373w
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C23 H24 B F4 Fe N7'
_chemical_formula_weight         541.15
_chemical_name_common            '[(SBPY3)Fe(CN)](BF₄)^.^CH₃CN'
_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                109.275(4)
_cell_angle_beta                 92.743(4)
_cell_angle_gamma                97.343(7)
_cell_formula_units_Z            2
_cell_length_a                   8.9246(17)
_cell_length_b                   12.091(2)
_cell_length_c                   12.244(2)
_cell_measurement_reflns_used    815
_cell_measurement_temperature    91(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      3.0
_cell_volume                     1231.2(4)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      91(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16145
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        <0.1
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         7060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0401
_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/[σ²(Fo²)+(0.0697P)²+0.5020P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1127
_reflns_number_gt                6110
_reflns_number_total             7060
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic020373w_2.cif
_cod_data_source_block           mn1366
_cod_database_code               4318684
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.82260(2) 0.336283(18) 0.234697(17) 0.01187(7) Uani 1 1 d . . .
N1 N 0.75220(14) 0.47866(11) 0.33592(11) 0.0139(2) Uani 1 1 d . . .
N2 N 0.61032(14) 0.29093(11) 0.19127(11) 0.0135(2) Uani 1 1 d . . .
N3 N 0.84088(14) 0.17465(11) 0.12800(11) 0.0137(2) Uani 1 1 d . . .
N4 N 0.83201(14) 0.37937(12) 0.09346(11) 0.0147(2) Uani 1 1 d . . .
N5 N 0.82706(14) 0.25563(11) 0.35115(11) 0.0142(2) Uani 1 1 d . . .
N6 N 1.16502(16) 0.43769(13) 0.29998(13) 0.0205(3) Uani 1 1 d . . .
C1 C 0.83348(18) 0.57660(14) 0.41437(14) 0.0176(3) Uani 1 1 d . . .
H1 H 0.9410 0.5834 0.4212 0.021 Uiso 1 1 calc R . .
C2 C 0.76602(18) 0.66824(14) 0.48572(14) 0.0187(3) Uani 1 1 d . . .
H2 H 0.8272 0.7355 0.5407 0.022 Uiso 1 1 calc R . .
C3 C 0.60909(18) 0.66133(14) 0.47644(14) 0.0180(3) Uani 1 1 d . . .
H3 H 0.5615 0.7234 0.5243 0.022 Uiso 1 1 calc R . .
C4 C 0.52340(17) 0.56100(14) 0.39512(13) 0.0166(3) Uani 1 1 d . . .
H4 H 0.4159 0.5538 0.3859 0.020 Uiso 1 1 calc R . .
C5 C 0.59713(16) 0.47193(13) 0.32780(13) 0.0144(3) Uani 1 1 d . . .
C6 C 0.51979(16) 0.36249(13) 0.24101(13) 0.0154(3) Uani 1 1 d . . .
H6 H 0.4128 0.3457 0.2230 0.018 Uiso 1 1 calc R . .
C7 C 0.56637(17) 0.18212(13) 0.09179(13) 0.0157(3) Uani 1 1 d . . .
H7A H 0.5660 0.1995 0.0183 0.019 Uiso 1 1 calc R . .
H7B H 0.4638 0.1432 0.0972 0.019 Uiso 1 1 calc R . .
C8 C 0.68412(17) 0.10296(13) 0.09642(13) 0.0160(3) Uani 1 1 d . . .
H8A H 0.6609 0.0645 0.1548 0.019 Uiso 1 1 calc R . .
H8B H 0.6804 0.0400 0.0198 0.019 Uiso 1 1 calc R . .
C9 C 0.91361(18) 0.18743(14) 0.02518(13) 0.0166(3) Uani 1 1 d . . .
H9A H 0.8822 0.1146 -0.0430 0.020 Uiso 1 1 calc R . .
H9B H 1.0254 0.1987 0.0408 0.020 Uiso 1 1 calc R . .
C10 C 0.86685(17) 0.29245(14) -0.00019(13) 0.0160(3) Uani 1 1 d . . .
C11 C 0.8647(2) 0.30237(15) -0.10999(14) 0.0212(3) Uani 1 1 d . . .
H11 H 0.8886 0.2399 -0.1745 0.025 Uiso 1 1 calc R . .
C12 C 0.8271(2) 0.40501(16) -0.12398(15) 0.0248(3) Uani 1 1 d . . .
H12 H 0.8251 0.4137 -0.1983 0.030 Uiso 1 1 calc R . .
C13 C 0.7925(2) 0.49459(16) -0.02876(15) 0.0234(3) Uani 1 1 d . . .
H13 H 0.7673 0.5658 -0.0366 0.028 Uiso 1 1 calc R . .
C14 C 0.79536(18) 0.47854(14) 0.07853(14) 0.0188(3) Uani 1 1 d . . .
H14 H 0.7706 0.5397 0.1438 0.023 Uiso 1 1 calc R . .
C15 C 0.93389(17) 0.12010(14) 0.19422(13) 0.0161(3) Uani 1 1 d . . .
H15A H 1.0428 0.1519 0.1990 0.019 Uiso 1 1 calc R . .
H15B H 0.9202 0.0330 0.1555 0.019 Uiso 1 1 calc R . .
C16 C 0.88042(17) 0.15061(14) 0.31397(13) 0.0160(3) Uani 1 1 d . . .
C17 C 0.88468(19) 0.07887(16) 0.38200(15) 0.0211(3) Uani 1 1 d . . .
H17 H 0.9228 0.0058 0.3539 0.025 Uiso 1 1 calc R . .
C18 C 0.8326(2) 0.11523(17) 0.49159(15) 0.0239(3) Uani 1 1 d . . .
H18 H 0.8330 0.0669 0.5390 0.029 Uiso 1 1 calc R . .
C19 C 0.78015(19) 0.22324(17) 0.53025(14) 0.0229(3) Uani 1 1 d . . .
H19 H 0.7451 0.2506 0.6052 0.027 Uiso 1 1 calc R . .
C20 C 0.77935(17) 0.29108(15) 0.45845(13) 0.0180(3) Uani 1 1 d . . .
H20 H 0.7439 0.3653 0.4859 0.022 Uiso 1 1 calc R . .
C21 C 1.03834(17) 0.39568(13) 0.27515(13) 0.0146(3) Uani 1 1 d . . .
B1 B 0.3194(2) 0.03531(17) 0.27163(16) 0.0212(3) Uani 1 1 d . . .
F1 F 0.38674(13) -0.03647(10) 0.17894(10) 0.0287(2) Uani 1 1 d . . .
F2 F 0.29919(14) 0.14030(10) 0.25434(11) 0.0324(3) Uani 1 1 d . . .
F3 F 0.17619(14) -0.02556(11) 0.27744(11) 0.0343(3) Uani 1 1 d . . .
F4 F 0.40726(18) 0.05824(12) 0.37552(11) 0.0469(4) Uani 1 1 d . . .
N7 N 0.7543(3) -0.19675(19) 0.1096(2) 0.0486(5) Uani 1 1 d . . .
C22 C 0.6792(2) -0.19122(19) 0.1829(2) 0.0364(5) Uani 1 1 d . . .
C23 C 0.5843(3) -0.1823(3) 0.2790(3) 0.0533(7) Uani 1 1 d . . .
H23A H 0.6396 -0.1998 0.3409 0.080 Uiso 1 1 calc R . .
H23B H 0.4906 -0.2392 0.2508 0.080 Uiso 1 1 calc R . .
H23C H 0.5591 -0.1018 0.3094 0.080 Uiso 1 1 calc R . .
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
N2 Fe1 C21 174.67(6) . . ?
N2 Fe1 N1 81.00(5) . . ?
C21 Fe1 N1 96.02(6) . . ?
N2 Fe1 N4 86.47(5) . . ?
C21 Fe1 N4 89.62(6) . . ?
N1 Fe1 N4 98.41(6) . . ?
N2 Fe1 N5 94.80(5) . . ?
C21 Fe1 N5 89.88(6) . . ?
N1 Fe1 N5 95.85(5) . . ?
N4 Fe1 N5 165.71(6) . . ?
N2 Fe1 N3 85.43(5) . . ?
C21 Fe1 N3 97.78(6) . . ?
N1 Fe1 N3 165.97(5) . . ?
N4 Fe1 N3 84.25(5) . . ?
N5 Fe1 N3 81.67(5) . . ?
C1 N1 C5 117.27(13) . . ?
C1 N1 Fe1 129.12(11) . . ?
C5 N1 Fe1 113.52(10) . . ?
C6 N2 C7 125.11(13) . . ?
C6 N2 Fe1 118.93(10) . . ?
C7 N2 Fe1 115.46(10) . . ?
C15 N3 C9 112.22(12) . . ?
C15 N3 C8 108.50(12) . . ?
C9 N3 C8 112.78(12) . . ?
C15 N3 Fe1 107.09(9) . . ?
C9 N3 Fe1 107.94(9) . . ?
C8 N3 Fe1 108.07(9) . . ?
C14 N4 C10 118.38(14) . . ?
C14 N4 Fe1 127.45(11) . . ?
C10 N4 Fe1 113.89(11) . . ?
C20 N5 C16 118.19(14) . . ?
C20 N5 Fe1 127.70(11) . . ?
C16 N5 Fe1 114.07(10) . . ?
N1 C1 C2 122.53(14) . . ?
C3 C2 C1 119.93(14) . . ?
C2 C3 C4 118.26(14) . . ?
C5 C4 C3 119.08(14) . . ?
N1 C5 C4 122.92(14) . . ?
N1 C5 C6 113.00(13) . . ?
C4 C5 C6 124.08(13) . . ?
N2 C6 C5 113.49(13) . . ?
N2 C7 C8 105.92(12) . . ?
N3 C8 C7 110.42(12) . . ?
N3 C9 C10 109.50(12) . . ?
N4 C10 C11 122.11(15) . . ?
N4 C10 C9 114.92(13) . . ?
C11 C10 C9 122.93(14) . . ?
C12 C11 C10 118.87(16) . . ?
C13 C12 C11 119.45(16) . . ?
C12 C13 C14 118.78(16) . . ?
N4 C14 C13 122.41(15) . . ?
N3 C15 C16 106.90(12) . . ?
N5 C16 C17 122.05(15) . . ?
N5 C16 C15 114.18(13) . . ?
C17 C16 C15 123.77(14) . . ?
C16 C17 C18 119.27(16) . . ?
C19 C18 C17 118.69(16) . . ?
C18 C19 C20 119.31(16) . . ?
N5 C20 C19 122.47(16) . . ?
N6 C21 Fe1 175.97(14) . . ?
F2 B1 F4 110.53(15) . . ?
F2 B1 F1 110.45(15) . . ?
F4 B1 F1 110.34(15) . . ?
F2 B1 F3 108.56(15) . . ?
F4 B1 F3 108.46(16) . . ?
F1 B1 F3 108.43(14) . . ?
N7 C22 C23 179.0(3) . . ?
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 N2 1.9022(13) . ?
Fe1 C21 1.9465(16) . ?
Fe1 N1 1.9588(13) . ?
Fe1 N4 1.9664(13) . ?
Fe1 N5 1.9769(13) . ?
Fe1 N3 1.9922(13) . ?
N1 C1 1.3468(19) . ?
N1 C5 1.3728(19) . ?
N2 C6 1.2846(19) . ?
N2 C7 1.4604(18) . ?
N3 C15 1.4866(19) . ?
N3 C9 1.4869(19) . ?
N3 C8 1.5083(19) . ?
N4 C14 1.348(2) . ?
N4 C10 1.356(2) . ?
N5 C20 1.3489(19) . ?
N5 C16 1.356(2) . ?
N6 C21 1.161(2) . ?
C1 C2 1.391(2) . ?
C2 C3 1.389(2) . ?
C3 C4 1.393(2) . ?
C4 C5 1.385(2) . ?
C5 C6 1.458(2) . ?
C7 C8 1.520(2) . ?
C9 C10 1.506(2) . ?
C10 C11 1.388(2) . ?
C11 C12 1.387(2) . ?
C12 C13 1.383(3) . ?
C13 C14 1.389(2) . ?
C15 C16 1.506(2) . ?
C16 C17 1.389(2) . ?
C17 C18 1.390(2) . ?
C18 C19 1.385(3) . ?
C19 C20 1.387(2) . ?
B1 F2 1.386(2) . ?
B1 F4 1.388(2) . ?
B1 F1 1.396(2) . ?
B1 F3 1.409(2) . ?
N7 C22 1.135(3) . ?
C22 C23 1.466(3) . ?
