#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:51:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179211 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314137.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_4314137
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 N5 O2'
_chemical_formula_weight         688.70
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 112.94(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2961(4)
_cell_length_b                   11.1489(4)
_cell_length_c                   14.1492(4)
_cell_measurement_temperature    295(2)
_cell_volume                     1931.55(18)
_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      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '960 images at 1.0 deg. in ω and 15 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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51050
_diffrn_reflns_theta_full        30.99
_diffrn_reflns_theta_max         30.99
_diffrn_reflns_theta_min         2.69
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.9042
_exptl_absorpt_correction_T_min  0.8479
_exptl_absorpt_correction_type   'Gaussian, face-indexed'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'opaque block'
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.011(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         12239
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0464P)²+0.1837P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                10023
_reflns_number_total             12239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0301526_9.cif
_cod_data_source_block           4@295K
_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^)+(0.0464P)^2^+0.1837P] 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^)+(0.0464P)^2^+0.1837P] 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        1931.55(11)
_cod_database_code               4314137
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.242238(14) 0.10127(2) 0.592898(14) 0.04188(6) Uani 1 d . . .
N11 N 0.28206(14) 0.26874(16) 0.58853(14) 0.0615(4) Uani 1 d . . .
N12 N 0.24413(15) 0.31022(16) 0.50273(16) 0.0649(4) Uani 1 d . . .
N13 N 0.2101(3) 0.3515(2) 0.4231(2) 0.1049(8) Uani 1 d . . .
O1 O 0.08838(7) 0.11769(11) 0.51898(7) 0.0408(2) Uani 1 d . . .
C1 C 0.05730(10) 0.11454(14) 0.41975(9) 0.0359(3) Uani 1 d . . .
C2 C -0.04925(11) 0.14688(13) 0.34875(12) 0.0396(3) Uani 1 d . . .
C3 C -0.06520(12) 0.14225(14) 0.24701(12) 0.0445(3) Uani 1 d . . .
H3 H -0.1342 0.1621 0.1992 0.053 Uiso 1 calc R . .
C4 C 0.01573(11) 0.10932(17) 0.20828(10) 0.0415(3) Uani 1 d . . .
C5 C 0.11625(12) 0.07392(13) 0.27688(11) 0.0401(3) Uani 1 d . . .
H5 H 0.1694 0.0488 0.2538 0.048 Uiso 1 calc R . .
C6 C 0.13856(11) 0.07581(12) 0.38290(10) 0.0355(3) Uani 1 d . . .
N7 N 0.23401(9) 0.04843(11) 0.46034(9) 0.0365(2) Uani 1 d . . .
C8 C 0.31806(12) -0.00722(16) 0.43726(11) 0.0448(3) Uani 1 d . . .
C9 C 0.3005(2) -0.1229(2) 0.39746(16) 0.0660(5) Uani 1 d . . .
H9 H 0.2346 -0.1618 0.3849 0.079 Uiso 1 calc R . .
C10 C 0.3823(3) -0.1791(3) 0.3768(2) 0.1007(11) Uani 1 d . . .
H10 H 0.3714 -0.2564 0.3499 0.121 Uiso 1 calc R . .
C11 C 0.4780(3) -0.1225(5) 0.3954(2) 0.1186(16) Uani 1 d . . .
H11 H 0.5321 -0.1608 0.3805 0.142 Uiso 1 calc R . .
C12 C 0.4960(2) -0.0096(4) 0.4359(2) 0.1037(12) Uani 1 d . . .
H12 H 0.5626 0.0277 0.4490 0.124 Uiso 1 calc R . .
C13 C 0.41513(15) 0.0509(2) 0.45822(16) 0.0682(6) Uani 1 d . . .
H13 H 0.4271 0.1277 0.4862 0.082 Uiso 1 calc R . .
C14 C -0.13699(13) 0.18449(16) 0.38709(14) 0.0503(4) Uani 1 d . . .
C15 C -0.09923(19) 0.2970(2) 0.45399(19) 0.0701(6) Uani 1 d . . .
H15A H -0.0338 0.2792 0.5126 0.105 Uiso 1 calc R . .
H15B H -0.1554 0.3220 0.4765 0.105 Uiso 1 calc R . .
H15C H -0.0849 0.3600 0.4148 0.105 Uiso 1 calc R . .
C16 C -0.24534(16) 0.2121(3) 0.29834(18) 0.0751(6) Uani 1 d . . .
H16A H -0.2354 0.2775 0.2586 0.113 Uiso 1 calc R . .
H16B H -0.2990 0.2337 0.3252 0.113 Uiso 1 calc R . .
H16C H -0.2697 0.1425 0.2555 0.113 Uiso 1 calc R . .
C17 C -0.15695(16) 0.0817(2) 0.45054(18) 0.0716(6) Uani 1 d . . .
H17A H -0.1763 0.0102 0.4096 0.107 Uiso 1 calc R . .
H17B H -0.2153 0.1034 0.4712 0.107 Uiso 1 calc R . .
H17C H -0.0917 0.0676 0.5104 0.107 Uiso 1 calc R . .
C18 C -0.01174(14) 0.11777(19) 0.09289(11) 0.0535(4) Uani 1 d . . .
C19 C 0.08137(18) 0.0718(2) 0.06501(14) 0.0722(6) Uani 1 d . . .
H19A H 0.1460 0.1180 0.1008 0.108 Uiso 1 calc R . .
H19B H 0.0614 0.0795 -0.0076 0.108 Uiso 1 calc R . .
H19C H 0.0952 -0.0110 0.0843 0.108 Uiso 1 calc R . .
C20 C -0.0310(3) 0.2497(2) 0.06151(18) 0.0875(8) Uani 1 d . . .
H20A H -0.0933 0.2788 0.0730 0.131 Uiso 1 calc R . .
H20B H -0.0441 0.2575 -0.0099 0.131 Uiso 1 calc R . .
H20C H 0.0322 0.2958 0.1017 0.131 Uiso 1 calc R . .
C21 C -0.1138(2) 0.0430(3) 0.03397(17) 0.0863(8) Uani 1 d . . .
H21A H -0.1018 -0.0385 0.0577 0.129 Uiso 1 calc R . .
H21B H -0.1285 0.0453 -0.0380 0.129 Uiso 1 calc R . .
H21C H -0.1750 0.0753 0.0454 0.129 Uiso 1 calc R . .
O31 O 0.37657(9) 0.01813(12) 0.66230(8) 0.0482(3) Uani 1 d . . .
C31 C 0.39716(11) -0.01222(14) 0.75694(11) 0.0389(3) Uani 1 d . . .
C32 C 0.49312(12) -0.07502(14) 0.82024(12) 0.0416(3) Uani 1 d . . .
C33 C 0.50025(14) -0.10157(16) 0.91710(13) 0.0495(4) Uani 1 d . . .
H33 H 0.5619 -0.1430 0.9599 0.059 Uiso 1 calc R . .
C34 C 0.42056(14) -0.07068(15) 0.95786(12) 0.0472(3) Uani 1 d . . .
C35 C 0.32878(13) -0.01108(15) 0.89663(12) 0.0454(3) Uani 1 d . . .
H35 H 0.2757 0.0097 0.9212 0.055 Uiso 1 calc R . .
C36 C 0.31521(12) 0.01883(13) 0.79493(11) 0.0394(3) Uani 1 d . . .
N37 N 0.23027(10) 0.07671(12) 0.72362(9) 0.0419(3) Uani 1 d . . .
C38 C 0.13663(11) 0.11064(19) 0.74391(10) 0.0449(3) Uani 1 d . . .
C39 C 0.1123(2) 0.2311(2) 0.74415(18) 0.0710(6) Uani 1 d . . .
H39 H 0.1583 0.2893 0.7360 0.085 Uiso 1 calc R . .
C40 C 0.0165(3) 0.2633(3) 0.7570(2) 0.0918(9) Uani 1 d . . .
H40 H -0.0002 0.3440 0.7593 0.110 Uiso 1 calc R . .
C41 C -0.0524(2) 0.1776(3) 0.76625(18) 0.0849(9) Uani 1 d . . .
H41 H -0.1162 0.2001 0.7739 0.102 Uiso 1 calc R . .
C42 C -0.02834(19) 0.0614(3) 0.76430(18) 0.0775(7) Uani 1 d . . .
H42 H -0.0762 0.0038 0.7700 0.093 Uiso 1 calc R . .
C43 C 0.06638(16) 0.0251(2) 0.75392(15) 0.0594(5) Uani 1 d . . .
H43 H 0.0825 -0.0560 0.7537 0.071 Uiso 1 calc R . .
C44 C 0.58043(13) -0.10883(16) 0.77984(14) 0.0497(4) Uani 1 d . . .
C45 C 0.53196(17) -0.1916(2) 0.68607(18) 0.0666(5) Uani 1 d . . .
H45A H 0.5869 -0.2100 0.6600 0.100 Uiso 1 calc R . .
H45B H 0.4717 -0.1522 0.6338 0.100 Uiso 1 calc R . .
H45C H 0.5070 -0.2645 0.7058 0.100 Uiso 1 calc R . .
C46 C 0.67639(16) -0.1748(2) 0.86076(19) 0.0741(6) Uani 1 d . . .
H46A H 0.7071 -0.1258 0.9211 0.111 Uiso 1 calc R . .
H46B H 0.7311 -0.1909 0.8339 0.111 Uiso 1 calc R . .
H46C H 0.6512 -0.2490 0.8781 0.111 Uiso 1 calc R . .
C47 C 0.62535(16) 0.0048(2) 0.74926(19) 0.0650(5) Uani 1 d . . .
H47A H 0.6560 0.0565 0.8078 0.098 Uiso 1 calc R . .
H47B H 0.5672 0.0459 0.6959 0.098 Uiso 1 calc R . .
H47C H 0.6809 -0.0167 0.7249 0.098 Uiso 1 calc R . .
C48 C 0.44274(17) -0.1045(2) 1.06909(14) 0.0624(5) Uani 1 d . . .
C49 C 0.3472(2) -0.0705(3) 1.09957(19) 0.0942(9) Uani 1 d . . .
H49A H 0.3336 0.0141 1.0900 0.141 Uiso 1 calc R . .
H49B H 0.3655 -0.0905 1.1703 0.141 Uiso 1 calc R . .
H49C H 0.2830 -0.1138 1.0574 0.141 Uiso 1 calc R . .
C50 C 0.5448(3) -0.0382(5) 1.1402(2) 0.1323(16) Uani 1 d . . .
H50A H 0.6074 -0.0675 1.1294 0.198 Uiso 1 calc R . .
H50B H 0.5546 -0.0516 1.2103 0.198 Uiso 1 calc R . .
H50C H 0.5364 0.0461 1.1255 0.198 Uiso 1 calc R . .
C51 C 0.4589(4) -0.2389(3) 1.0838(3) 0.1335(16) Uani 1 d . . .
H51A H 0.3940 -0.2796 1.0396 0.200 Uiso 1 calc R . .
H51B H 0.4737 -0.2590 1.1540 0.200 Uiso 1 calc R . .
H51C H 0.5194 -0.2633 1.0672 0.200 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'
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 O31 156.36(5) . . ?
O1 Fe1 N7 81.60(5) . . ?
O31 Fe1 N7 92.23(5) . . ?
O1 Fe1 N37 93.87(5) . . ?
O31 Fe1 N37 81.31(5) . . ?
N7 Fe1 N37 153.03(6) . . ?
O1 Fe1 N11 97.88(6) . . ?
O31 Fe1 N11 105.68(7) . . ?
N7 Fe1 N11 100.09(7) . . ?
N37 Fe1 N11 106.87(7) . . ?
N12 N11 Fe1 112.70(13) . . ?
N13 N12 N11 178.4(2) . . ?
C1 O1 Fe1 114.25(8) . . ?
O1 C1 C2 124.32(12) . . ?
O1 C1 C6 115.62(11) . . ?
C2 C1 C6 120.06(12) . . ?
C3 C2 C1 115.73(13) . . ?
C3 C2 C14 123.85(13) . . ?
C1 C2 C14 120.42(13) . . ?
C2 C3 C4 125.38(13) . . ?
C5 C4 C3 118.30(12) . . ?
C5 C4 C18 122.37(13) . . ?
C3 C4 C18 119.32(13) . . ?
C4 C5 C6 119.48(13) . . ?
N7 C6 C5 126.97(13) . . ?
N7 C6 C1 112.05(12) . . ?
C5 C6 C1 120.92(12) . . ?
C6 N7 C8 119.11(12) . . ?
C6 N7 Fe1 113.57(9) . . ?
C8 N7 Fe1 127.20(9) . . ?
C13 C8 C9 121.49(18) . . ?
C13 C8 N7 120.14(18) . . ?
C9 C8 N7 118.31(17) . . ?
C10 C9 C8 119.0(3) . . ?
C11 C10 C9 120.4(3) . . ?
C10 C11 C12 120.7(2) . . ?
C11 C12 C13 120.8(3) . . ?
C8 C13 C12 117.6(3) . . ?
C2 C14 C16 111.72(15) . . ?
C2 C14 C15 109.44(15) . . ?
C16 C14 C15 108.62(17) . . ?
C2 C14 C17 109.40(14) . . ?
C16 C14 C17 107.89(17) . . ?
C15 C14 C17 109.74(18) . . ?
C19 C18 C20 108.0(2) . . ?
C19 C18 C4 111.99(13) . . ?
C20 C18 C4 108.19(17) . . ?
C19 C18 C21 108.18(18) . . ?
C20 C18 C21 110.7(2) . . ?
C4 C18 C21 109.83(16) . . ?
C31 O31 Fe1 115.74(9) . . ?
O31 C31 C32 123.49(14) . . ?
O31 C31 C36 115.92(12) . . ?
C32 C31 C36 120.57(14) . . ?
C33 C32 C31 115.55(15) . . ?
C33 C32 C44 123.72(14) . . ?
C31 C32 C44 120.73(14) . . ?
C32 C33 C34 125.30(14) . . ?
C35 C34 C33 118.76(14) . . ?
C35 C34 C48 122.65(16) . . ?
C33 C34 C48 118.59(15) . . ?
C34 C35 C36 119.20(15) . . ?
N37 C36 C35 127.54(14) . . ?
N37 C36 C31 111.85(13) . . ?
C35 C36 C31 120.61(13) . . ?
C36 N37 C38 121.04(12) . . ?
C36 N37 Fe1 115.17(10) . . ?
C38 N37 Fe1 123.72(9) . . ?
C43 C38 C39 120.15(18) . . ?
C43 C38 N37 120.92(18) . . ?
C39 C38 N37 118.68(18) . . ?
C38 C39 C40 118.4(3) . . ?
C41 C40 C39 120.7(2) . . ?
C42 C41 C40 120.1(2) . . ?
C41 C42 C43 121.4(3) . . ?
C38 C43 C42 119.3(2) . . ?
C32 C44 C46 111.85(16) . . ?
C32 C44 C47 109.76(15) . . ?
C46 C44 C47 107.78(16) . . ?
C32 C44 C45 110.32(14) . . ?
C46 C44 C45 107.71(17) . . ?
C47 C44 C45 109.35(18) . . ?
C51 C48 C50 110.2(3) . . ?
C51 C48 C34 110.2(2) . . ?
C50 C48 C34 108.9(2) . . ?
C51 C48 C49 107.1(3) . . ?
C50 C48 C49 108.3(3) . . ?
C34 C48 C49 112.20(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
Fe1 O1 1.9091(9) . ?
Fe1 O31 1.9096(10) . ?
Fe1 N7 1.9279(12) . ?
Fe1 N37 1.9367(12) . ?
Fe1 N11 1.9482(18) . ?
N11 N12 1.210(3) . ?
N12 N13 1.135(3) . ?
O1 C1 1.3003(15) . ?
C1 C2 1.4272(18) . ?
C1 C6 1.4371(19) . ?
C2 C3 1.372(2) . ?
C2 C14 1.524(2) . ?
C3 C4 1.433(2) . ?
C4 C5 1.3686(19) . ?
C4 C18 1.5307(19) . ?
C5 C6 1.4113(19) . ?
C6 N7 1.3492(17) . ?
N7 C8 1.4231(18) . ?
C8 C13 1.370(3) . ?
C8 C9 1.390(3) . ?
C9 C10 1.382(3) . ?
C10 C11 1.351(6) . ?
C11 C12 1.364(6) . ?
C12 C13 1.405(4) . ?
C14 C16 1.529(3) . ?
C14 C15 1.533(3) . ?
C14 C17 1.541(3) . ?
C18 C19 1.527(3) . ?
C18 C20 1.529(3) . ?
C18 C21 1.533(3) . ?
O31 C31 1.3027(18) . ?
C31 C32 1.4245(19) . ?
C31 C36 1.433(2) . ?
C32 C33 1.369(2) . ?
C32 C44 1.528(2) . ?
C33 C34 1.432(3) . ?
C34 C35 1.363(2) . ?
C34 C48 1.531(2) . ?
C35 C36 1.418(2) . ?
C36 N37 1.3497(18) . ?
N37 C38 1.4332(18) . ?
C38 C43 1.380(3) . ?
C38 C39 1.382(3) . ?
C39 C40 1.401(4) . ?
C40 C41 1.366(5) . ?
C41 C42 1.337(4) . ?
C42 C43 1.384(3) . ?
C44 C46 1.530(2) . ?
C44 C47 1.533(3) . ?
C44 C45 1.537(3) . ?
C48 C51 1.517(4) . ?
C48 C50 1.528(4) . ?
C48 C49 1.540(3) . ?
