#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:51:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179211 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314134.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_4314134
loop_
_publ_author_name
'Hyungphil Chun'
'Eckhard Bill'
'Thomas Weyhermüller'
'Karl Wieghardt'
_publ_section_title
;
 S =3/2 <--> S =1/2 Spin Crossover Behavior in Five-Coordinate Halido- and
 Pseudohalido-bis(o-iminobenzosemiquinonato)iron(III) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5612
_journal_page_last               5620
_journal_paper_doi               10.1021/ic0301526
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C40 H50 Fe I N2 O2'
_chemical_formula_weight         773.57
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.87(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5473(4)
_cell_length_b                   26.4964(8)
_cell_length_c                   11.7437(4)
_cell_measurement_temperature    220(2)
_cell_volume                     3884.1(4)
_computing_cell_refinement       'DENZO, Nonius Collect Software'
_computing_data_collection       'DENZO, Nonius Collect Software'
_computing_data_reduction        'DENZO, Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '1300 images at 0.8 deg. in ω and 16 sec.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            100548
_diffrn_reflns_theta_full        30.98
_diffrn_reflns_theta_max         30.98
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.8481
_exptl_absorpt_correction_T_min  0.7116
_exptl_absorpt_correction_type   'Gaussian, face-indexed'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Opaque Parallelepiped'
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         12353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0258P)²+2.0719P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                10182
_reflns_number_total             12353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0301526_6.cif
_cod_data_source_block           3@220K
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+2.0719P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+2.0719P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3884.1(2)
_cod_database_code               4314134
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.333190(10) 0.628857(4) 0.285569(11) 0.03846(4) Uani 1 d . . .
Fe1 Fe 0.432040(17) 0.605595(8) 0.143113(19) 0.02523(5) Uani 1 d . . .
O1 O 0.48263(8) 0.66770(4) 0.11035(10) 0.0283(2) Uani 1 d . . .
N1 N 0.57633(10) 0.59848(5) 0.25531(11) 0.0248(2) Uani 1 d . . .
O2 O 0.40733(8) 0.53534(4) 0.13082(10) 0.0270(2) Uani 1 d . . .
N2 N 0.31331(10) 0.60601(5) -0.01059(11) 0.0257(2) Uani 1 d . . .
C1 C 0.58208(12) 0.67820(5) 0.17960(13) 0.0249(3) Uani 1 d . . .
C2 C 0.63877(12) 0.63943(5) 0.26430(13) 0.0246(3) Uani 1 d . . .
C3 C 0.74562(12) 0.64687(6) 0.34928(14) 0.0281(3) Uani 1 d . . .
H3 H 0.7821 0.6213 0.4053 0.034 Uiso 1 calc R . .
C4 C 0.79483(12) 0.69190(6) 0.34855(15) 0.0296(3) Uani 1 d . . .
C5 C 0.73832(13) 0.72904(6) 0.25774(15) 0.0300(3) Uani 1 d . . .
H5 H 0.7751 0.7588 0.2554 0.036 Uiso 1 calc R . .
C6 C 0.63436(12) 0.72431(5) 0.17388(14) 0.0262(3) Uani 1 d . . .
C7 C 0.57501(13) 0.76550(6) 0.08084(14) 0.0279(3) Uani 1 d . . .
C8 C 0.64736(15) 0.81064(6) 0.08683(17) 0.0387(4) Uani 1 d . . .
H8A H 0.6066 0.8361 0.0281 0.058 Uiso 1 calc R . .
H8B H 0.7070 0.7997 0.0667 0.058 Uiso 1 calc R . .
H8C H 0.6744 0.8248 0.1695 0.058 Uiso 1 calc R . .
C9 C 0.53496(15) 0.74415(6) -0.05145(15) 0.0359(4) Uani 1 d . . .
H9A H 0.4968 0.7703 -0.1099 0.054 Uiso 1 calc R . .
H9B H 0.4873 0.7159 -0.0587 0.054 Uiso 1 calc R . .
H9C H 0.5956 0.7328 -0.0691 0.054 Uiso 1 calc R . .
C10 C 0.48023(14) 0.78448(7) 0.11055(16) 0.0358(3) Uani 1 d . . .
H10A H 0.4398 0.8092 0.0493 0.054 Uiso 1 calc R . .
H10B H 0.5071 0.7999 0.1918 0.054 Uiso 1 calc R . .
H10C H 0.4341 0.7563 0.1092 0.054 Uiso 1 calc R . .
C11 C 0.90778(13) 0.70461(7) 0.44156(17) 0.0386(4) Uani 1 d . . .
C12 C 0.98338(17) 0.70948(12) 0.3745(2) 0.0670(7) Uani 1 d . . .
H12A H 0.9601 0.7371 0.3158 0.100 Uiso 1 calc R . .
H12B H 0.9829 0.6783 0.3309 0.100 Uiso 1 calc R . .
H12C H 1.0554 0.7161 0.4340 0.100 Uiso 1 calc R . .
C13 C 0.95094(16) 0.66385(8) 0.5409(2) 0.0558(6) Uani 1 d . . .
H13A H 1.0212 0.6736 0.5998 0.084 Uiso 1 calc R . .
H13B H 0.9563 0.6321 0.5025 0.084 Uiso 1 calc R . .
H13C H 0.9027 0.6599 0.5833 0.084 Uiso 1 calc R . .
C14 C 0.90488(19) 0.75483(8) 0.5066(2) 0.0589(6) Uani 1 d . . .
H14A H 0.8833 0.7819 0.4462 0.088 Uiso 1 calc R . .
H14B H 0.9756 0.7620 0.5686 0.088 Uiso 1 calc R . .
H14C H 0.8540 0.7522 0.5460 0.088 Uiso 1 calc R . .
C15 C 0.62247(11) 0.55416(5) 0.32580(13) 0.0242(3) Uani 1 d . . .
C16 C 0.59096(13) 0.53892(6) 0.41932(15) 0.0331(3) Uani 1 d . . .
H16 H 0.5420 0.5584 0.4394 0.040 Uiso 1 calc R . .
C17 C 0.63227(14) 0.49453(7) 0.48346(16) 0.0364(4) Uani 1 d . . .
H17 H 0.6113 0.4841 0.5472 0.044 Uiso 1 calc R . .
C18 C 0.70388(13) 0.46572(6) 0.45389(15) 0.0335(3) Uani 1 d . . .
H18 H 0.7302 0.4353 0.4960 0.040 Uiso 1 calc R . .
C19 C 0.73663(14) 0.48166(6) 0.36240(16) 0.0356(3) Uani 1 d . . .
H19 H 0.7868 0.4625 0.3437 0.043 Uiso 1 calc R . .
C20 C 0.69604(14) 0.52583(6) 0.29770(15) 0.0323(3) Uani 1 d . . .
H20 H 0.7183 0.5365 0.2351 0.039 Uiso 1 calc R . .
C21 C 0.31681(11) 0.52213(5) 0.04327(13) 0.0239(3) Uani 1 d . . .
C22 C 0.25980(11) 0.56162(5) -0.03909(13) 0.0243(3) Uani 1 d . . .
C23 C 0.15752(12) 0.55295(6) -0.13351(14) 0.0274(3) Uani 1 d . . .
H23 H 0.1205 0.5793 -0.1865 0.033 Uiso 1 calc R . .
C24 C 0.11339(12) 0.50587(6) -0.14656(14) 0.0272(3) Uani 1 d . . .
C25 C 0.17487(12) 0.46620(6) -0.06784(14) 0.0279(3) Uani 1 d . . .
H25 H 0.1448 0.4337 -0.0807 0.034 Uiso 1 calc R . .
C26 C 0.27448(12) 0.47203(5) 0.02512(13) 0.0252(3) Uani 1 d . . .
C27 C 0.33880(13) 0.42836(6) 0.10429(15) 0.0315(3) Uani 1 d . . .
C28 C 0.44595(16) 0.42393(8) 0.0887(2) 0.0500(5) Uani 1 d . . .
H28A H 0.4324 0.4196 0.0019 0.075 Uiso 1 calc R . .
H28B H 0.4854 0.3950 0.1350 0.075 Uiso 1 calc R . .
H28C H 0.4877 0.4544 0.1193 0.075 Uiso 1 calc R . .
C29 C 0.27949(18) 0.37802(6) 0.0657(2) 0.0488(5) Uani 1 d . . .
H29A H 0.2664 0.3711 -0.0200 0.073 Uiso 1 calc R . .
H29B H 0.2117 0.3799 0.0755 0.073 Uiso 1 calc R . .
H29C H 0.3228 0.3512 0.1174 0.073 Uiso 1 calc R . .
C30 C 0.35951(18) 0.43797(7) 0.24064(16) 0.0454(4) Uani 1 d . . .
H30A H 0.3967 0.4699 0.2665 0.068 Uiso 1 calc R . .
H30B H 0.4031 0.4109 0.2909 0.068 Uiso 1 calc R . .
H30C H 0.2917 0.4392 0.2506 0.068 Uiso 1 calc R . .
C31 C 0.00110(13) 0.49343(6) -0.24200(16) 0.0343(3) Uani 1 d . . .
C32 C -0.05279(17) 0.53944(8) -0.3189(2) 0.0568(6) Uani 1 d . . .
H32A H -0.1232 0.5301 -0.3784 0.085 Uiso 1 calc R . .
H32B H -0.0096 0.5518 -0.3623 0.085 Uiso 1 calc R . .
H32C H -0.0599 0.5657 -0.2651 0.085 Uiso 1 calc R . .
C33 C -0.06880(16) 0.47399(10) -0.1760(2) 0.0590(6) Uani 1 d . . .
H33A H -0.0373 0.4436 -0.1305 0.088 Uiso 1 calc R . .
H33B H -0.1400 0.4665 -0.2365 0.088 Uiso 1 calc R . .
H33C H -0.0735 0.4995 -0.1192 0.088 Uiso 1 calc R . .
C34 C 0.00994(18) 0.45250(9) -0.3301(2) 0.0560(6) Uani 1 d . . .
H34A H 0.0446 0.4229 -0.2829 0.084 Uiso 1 calc R . .
H34B H 0.0520 0.4652 -0.3745 0.084 Uiso 1 calc R . .
H34C H -0.0612 0.4436 -0.3886 0.084 Uiso 1 calc R . .
C35 C 0.27988(12) 0.64718(6) -0.09564(14) 0.0271(3) Uani 1 d . . .
C36 C 0.25172(14) 0.69303(6) -0.06041(17) 0.0377(4) Uani 1 d . . .
H36 H 0.2491 0.6968 0.0180 0.045 Uiso 1 calc R . .
C37 C 0.22726(16) 0.73350(7) -0.1423(2) 0.0470(5) Uani 1 d . . .
H37 H 0.2078 0.7647 -0.1189 0.056 Uiso 1 calc R . .
C38 C 0.23126(15) 0.72850(7) -0.25633(19) 0.0464(5) Uani 1 d . . .
H38 H 0.2145 0.7561 -0.3108 0.056 Uiso 1 calc R . .
C39 C 0.25987(15) 0.68287(8) -0.29163(17) 0.0433(4) Uani 1 d . . .
H39 H 0.2626 0.6795 -0.3700 0.052 Uiso 1 calc R . .
C40 C 0.28468(14) 0.64199(7) -0.21100(15) 0.0344(3) Uani 1 d . . .
H40 H 0.3046 0.6110 -0.2346 0.041 Uiso 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 '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
O1 Fe1 O2 156.39(5) . . ?
O1 Fe1 N2 92.41(5) . . ?
O2 Fe1 N2 82.71(5) . . ?
O1 Fe1 N1 82.51(5) . . ?
O2 Fe1 N1 93.41(5) . . ?
N2 Fe1 N1 158.06(6) . . ?
O1 Fe1 I1 104.18(4) . . ?
O2 Fe1 I1 99.40(3) . . ?
N2 Fe1 I1 98.82(4) . . ?
N1 Fe1 I1 103.12(4) . . ?
C1 O1 Fe1 115.44(9) . . ?
C2 N1 C15 119.50(12) . . ?
C2 N1 Fe1 114.76(10) . . ?
C15 N1 Fe1 125.72(9) . . ?
C21 O2 Fe1 114.17(9) . . ?
C22 N2 C35 119.79(12) . . ?
C22 N2 Fe1 113.91(10) . . ?
C35 N2 Fe1 126.27(10) . . ?
O1 C1 C6 124.37(13) . . ?
O1 C1 C2 115.22(12) . . ?
C6 C1 C2 120.42(13) . . ?
N1 C2 C3 127.06(13) . . ?
N1 C2 C1 111.80(13) . . ?
C3 C2 C1 121.06(13) . . ?
C4 C3 C2 118.94(14) . . ?
C3 C4 C5 118.83(14) . . ?
C3 C4 C11 122.75(14) . . ?
C5 C4 C11 118.42(14) . . ?
C6 C5 C4 124.90(14) . . ?
C5 C6 C1 115.67(13) . . ?
C5 C6 C7 123.59(13) . . ?
C1 C6 C7 120.72(13) . . ?
C8 C7 C6 112.00(13) . . ?
C8 C7 C10 108.05(13) . . ?
C6 C7 C10 108.88(12) . . ?
C8 C7 C9 107.55(13) . . ?
C6 C7 C9 109.83(12) . . ?
C10 C7 C9 110.52(14) . . ?
C12 C11 C13 108.68(18) . . ?
C12 C11 C4 109.66(16) . . ?
C13 C11 C4 111.61(14) . . ?
C12 C11 C14 109.58(18) . . ?
C13 C11 C14 107.90(18) . . ?
C4 C11 C14 109.38(15) . . ?
C16 C15 C20 120.19(14) . . ?
C16 C15 N1 119.84(14) . . ?
C20 C15 N1 119.94(13) . . ?
C15 C16 C17 119.53(15) . . ?
C18 C17 C16 120.35(15) . . ?
C19 C18 C17 119.82(15) . . ?
C18 C19 C20 120.41(16) . . ?
C15 C20 C19 119.68(15) . . ?
O2 C21 C26 124.51(13) . . ?
O2 C21 C22 115.55(12) . . ?
C26 C21 C22 119.93(13) . . ?
N2 C22 C23 126.96(13) . . ?
N2 C22 C21 111.84(12) . . ?
C23 C22 C21 121.14(13) . . ?
C24 C23 C22 119.22(14) . . ?
C23 C24 C25 118.55(13) . . ?
C23 C24 C31 123.01(14) . . ?
C25 C24 C31 118.44(13) . . ?
C26 C25 C24 125.06(14) . . ?
C25 C26 C21 115.85(13) . . ?
C25 C26 C27 123.35(13) . . ?
C21 C26 C27 120.80(13) . . ?
C26 C27 C29 111.72(14) . . ?
C26 C27 C30 109.81(13) . . ?
C29 C27 C30 108.35(15) . . ?
C26 C27 C28 109.10(14) . . ?
C29 C27 C28 108.03(16) . . ?
C30 C27 C28 109.80(16) . . ?
C32 C31 C33 108.78(18) . . ?
C32 C31 C24 111.82(14) . . ?
C33 C31 C24 109.64(15) . . ?
C32 C31 C34 108.07(17) . . ?
C33 C31 C34 109.27(18) . . ?
C24 C31 C34 109.22(14) . . ?
C36 C35 C40 120.11(15) . . ?
C36 C35 N2 120.70(15) . . ?
C40 C35 N2 118.96(14) . . ?
C35 C36 C37 119.29(18) . . ?
C38 C37 C36 120.83(18) . . ?
C37 C38 C39 120.08(17) . . ?
C38 C39 C40 119.93(18) . . ?
C35 C40 C39 119.77(17) . . ?
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
I1 Fe1 2.5910(3) . ?
Fe1 O1 1.8790(10) . ?
Fe1 O2 1.8868(10) . ?
Fe1 N2 1.8944(12) . ?
Fe1 N1 1.8949(12) . ?
O1 C1 1.3048(17) . ?
N1 C2 1.3544(18) . ?
N1 C15 1.4328(18) . ?
O2 C21 1.3052(17) . ?
N2 C22 1.3536(18) . ?
N2 C35 1.4287(19) . ?
C1 C6 1.427(2) . ?
C1 C2 1.429(2) . ?
C2 C3 1.417(2) . ?
C3 C4 1.368(2) . ?
C4 C5 1.434(2) . ?
C4 C11 1.533(2) . ?
C5 C6 1.375(2) . ?
C6 C7 1.532(2) . ?
C7 C8 1.531(2) . ?
C7 C10 1.540(2) . ?
C7 C9 1.540(2) . ?
C11 C12 1.521(3) . ?
C11 C13 1.529(3) . ?
C11 C14 1.542(3) . ?
C15 C16 1.384(2) . ?
C15 C20 1.386(2) . ?
C16 C17 1.392(2) . ?
C17 C18 1.381(2) . ?
C18 C19 1.378(2) . ?
C19 C20 1.387(2) . ?
C21 C26 1.429(2) . ?
C21 C22 1.431(2) . ?
C22 C23 1.417(2) . ?
C23 C24 1.366(2) . ?
C24 C25 1.434(2) . ?
C24 C31 1.534(2) . ?
C25 C26 1.375(2) . ?
C26 C27 1.527(2) . ?
C27 C29 1.532(2) . ?
C27 C30 1.536(2) . ?
C27 C28 1.537(3) . ?
C31 C32 1.524(3) . ?
C31 C33 1.527(3) . ?
C31 C34 1.535(3) . ?
C35 C36 1.384(2) . ?
C35 C40 1.388(2) . ?
C36 C37 1.392(3) . ?
C37 C38 1.368(3) . ?
C38 C39 1.381(3) . ?
C39 C40 1.391(2) . ?
