#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:51:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179211 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314136.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_4314136
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                 112.72(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.2976(5)
_cell_length_b                   10.9599(4)
_cell_length_c                   13.9542(5)
_cell_measurement_temperature    100(2)
_cell_volume                     1875.88(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      100(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       '800 images at 1.0 deg. in ω and 20 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  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45229
_diffrn_reflns_theta_full        33.18
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.442
_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    1.219
_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         0.671
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         14290
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0337
_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)+(0.0480P)²+0.1966P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                13603
_reflns_number_total             14290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0301526_8.cif
_cod_data_source_block           4@100K
_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^)+(0.0480P)^2^+0.1966P] 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^)+(0.0480P)^2^+0.1966P] 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        1875.88(12)
_cod_database_code               4314136
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 0.241103(11) 0.099620(13) 0.594681(10) 0.01175(4) Uani 1 d . . .
N11 N 0.28267(9) 0.27095(9) 0.59459(8) 0.01921(19) Uani 1 d . . .
N12 N 0.24416(9) 0.31258(9) 0.50666(9) 0.0214(2) Uani 1 d . . .
N13 N 0.20941(14) 0.35380(12) 0.42443(11) 0.0366(3) Uani 1 d . . .
O1 O 0.09055(6) 0.12230(7) 0.52197(6) 0.01376(14) Uani 1 d . . .
C1 C 0.05909(8) 0.11965(9) 0.42089(8) 0.01253(17) Uani 1 d . . .
C2 C -0.04785(8) 0.15177(10) 0.34932(8) 0.01313(17) Uani 1 d . . .
C3 C -0.06400(9) 0.14716(10) 0.24537(8) 0.01458(18) Uani 1 d . . .
H3 H -0.1343 0.1679 0.1960 0.017 Uiso 1 calc R . .
C4 C 0.01752(8) 0.11343(10) 0.20648(8) 0.01327(17) Uani 1 d . . .
C5 C 0.11876(9) 0.07803(9) 0.27592(8) 0.01358(18) Uani 1 d . . .
H5 H 0.1734 0.0525 0.2521 0.016 Uiso 1 calc R . .
C6 C 0.14017(8) 0.08029(9) 0.38372(8) 0.01207(17) Uani 1 d . . .
N7 N 0.23532(7) 0.05235(8) 0.46319(7) 0.01218(15) Uani 1 d . . .
C8 C 0.31916(9) -0.00656(11) 0.44055(8) 0.01425(18) Uani 1 d . . .
C9 C 0.30002(11) -0.12488(12) 0.39981(10) 0.0212(2) Uani 1 d . . .
H9 H 0.2317 -0.1633 0.3856 0.025 Uiso 1 calc R . .
C10 C 0.38194(14) -0.18558(15) 0.38036(11) 0.0325(3) Uani 1 d . . .
H10 H 0.3699 -0.2662 0.3533 0.039 Uiso 1 calc R . .
C11 C 0.48128(13) -0.12885(18) 0.40031(11) 0.0369(4) Uani 1 d . . .
H11 H 0.5367 -0.1701 0.3860 0.044 Uiso 1 calc R . .
C12 C 0.49942(11) -0.01222(18) 0.44108(11) 0.0327(3) Uani 1 d . . .
H12 H 0.5677 0.0260 0.4547 0.039 Uiso 1 calc R . .
C13 C 0.41892(9) 0.05044(14) 0.46254(10) 0.0222(2) Uani 1 d . . .
H13 H 0.4321 0.1301 0.4915 0.027 Uiso 1 calc R . .
C14 C -0.13538(9) 0.18933(10) 0.38882(9) 0.01619(19) Uani 1 d . . .
C15 C -0.09736(11) 0.30430(12) 0.45670(10) 0.0225(2) Uani 1 d . . .
H15A H -0.0319 0.2852 0.5181 0.034 Uiso 1 calc R . .
H15B H -0.1553 0.3319 0.4786 0.034 Uiso 1 calc R . .
H15C H -0.0807 0.3690 0.4166 0.034 Uiso 1 calc R . .
C16 C -0.24394(10) 0.21752(13) 0.29895(11) 0.0241(2) Uani 1 d . . .
H16A H -0.2348 0.2881 0.2600 0.036 Uiso 1 calc R . .
H16B H -0.2996 0.2358 0.3268 0.036 Uiso 1 calc R . .
H16C H -0.2668 0.1467 0.2527 0.036 Uiso 1 calc R . .
C17 C -0.15559(10) 0.08468(13) 0.45301(11) 0.0242(2) Uani 1 d . . .
H17A H -0.1750 0.0104 0.4107 0.036 Uiso 1 calc R . .
H17B H -0.2154 0.1070 0.4742 0.036 Uiso 1 calc R . .
H17C H -0.0893 0.0702 0.5149 0.036 Uiso 1 calc R . .
C18 C -0.01086(9) 0.12093(10) 0.08932(8) 0.0165(2) Uani 1 d . . .
C19 C 0.08286(10) 0.07591(12) 0.06052(9) 0.0215(2) Uani 1 d . . .
H19A H 0.1480 0.1253 0.0968 0.032 Uiso 1 calc R . .
H19B H 0.0621 0.0834 -0.0147 0.032 Uiso 1 calc R . .
H19C H 0.0984 -0.0098 0.0810 0.032 Uiso 1 calc R . .
C20 C -0.03459(14) 0.25542(13) 0.05524(10) 0.0275(3) Uani 1 d . . .
H20A H -0.0974 0.2841 0.0692 0.041 Uiso 1 calc R . .
H20B H -0.0507 0.2621 -0.0193 0.041 Uiso 1 calc R . .
H20C H 0.0293 0.3054 0.0941 0.041 Uiso 1 calc R . .
C21 C -0.11205(11) 0.04232(14) 0.03060(10) 0.0257(3) Uani 1 d . . .
H21A H -0.0972 -0.0427 0.0536 0.039 Uiso 1 calc R . .
H21B H -0.1292 0.0470 -0.0442 0.039 Uiso 1 calc R . .
H21C H -0.1741 0.0726 0.0450 0.039 Uiso 1 calc R . .
O31 O 0.37376(6) 0.01828(8) 0.66204(6) 0.01473(14) Uani 1 d . . .
C31 C 0.39533(8) -0.01117(10) 0.75899(8) 0.01285(17) Uani 1 d . . .
C32 C 0.49191(8) -0.07370(10) 0.82350(8) 0.01367(17) Uani 1 d . . .
C33 C 0.49971(9) -0.09932(10) 0.92322(9) 0.01565(19) Uani 1 d . . .
H33 H 0.5630 -0.1410 0.9681 0.019 Uiso 1 calc R . .
C34 C 0.41913(9) -0.06747(10) 0.96379(8) 0.01520(18) Uani 1 d . . .
C35 C 0.32630(9) -0.00724(10) 0.90073(8) 0.01468(18) Uani 1 d . . .
H35 H 0.2720 0.0152 0.9259 0.018 Uiso 1 calc R . .
C36 C 0.31342(8) 0.02070(10) 0.79722(8) 0.01314(17) Uani 1 d . . .
N37 N 0.22781(7) 0.07813(8) 0.72347(7) 0.01371(17) Uani 1 d . . .
C38 C 0.13314(8) 0.11098(11) 0.74268(8) 0.01458(18) Uani 1 d . . .
C39 C 0.10683(11) 0.23430(12) 0.74199(10) 0.0230(2) Uani 1 d . . .
H39 H 0.1536 0.2952 0.7336 0.028 Uiso 1 calc R . .
C40 C 0.01080(12) 0.26701(14) 0.75380(11) 0.0289(3) Uani 1 d . . .
H40 H -0.0069 0.3508 0.7551 0.035 Uiso 1 calc R . .
C41 C -0.05903(12) 0.17810(16) 0.76364(10) 0.0282(3) Uani 1 d . . .
H41 H -0.1246 0.2011 0.7708 0.034 Uiso 1 calc R . .
C42 C -0.03301(11) 0.05599(15) 0.76300(10) 0.0249(3) Uani 1 d . . .
H42 H -0.0812 -0.0047 0.7691 0.030 Uiso 1 calc R . .
C43 C 0.06349(10) 0.02165(12) 0.75341(9) 0.0189(2) Uani 1 d . . .
H43 H 0.0818 -0.0622 0.7542 0.023 Uiso 1 calc R . .
C44 C 0.57956(9) -0.10927(10) 0.78300(9) 0.01573(18) Uani 1 d . . .
C45 C 0.53145(10) -0.19670(12) 0.68971(10) 0.0216(2) Uani 1 d . . .
H45A H 0.5875 -0.2166 0.6628 0.032 Uiso 1 calc R . .
H45B H 0.4696 -0.1573 0.6350 0.032 Uiso 1 calc R . .
H45C H 0.5068 -0.2717 0.7121 0.032 Uiso 1 calc R . .
C46 C 0.67593(10) -0.17439(12) 0.86641(11) 0.0229(2) Uani 1 d . . .
H46A H 0.7077 -0.1211 0.9271 0.034 Uiso 1 calc R . .
H46B H 0.7312 -0.1937 0.8384 0.034 Uiso 1 calc R . .
H46C H 0.6504 -0.2500 0.8870 0.034 Uiso 1 calc R . .
C47 C 0.62331(10) 0.00622(12) 0.74914(10) 0.0205(2) Uani 1 d . . .
H47A H 0.6562 0.0604 0.8090 0.031 Uiso 1 calc R . .
H47B H 0.5631 0.0486 0.6949 0.031 Uiso 1 calc R . .
H47C H 0.6784 -0.0169 0.7219 0.031 Uiso 1 calc R . .
C48 C 0.44224(10) -0.09961(12) 1.07708(9) 0.0195(2) Uani 1 d . . .
C49 C 0.34681(12) -0.06584(15) 1.10775(10) 0.0262(3) Uani 1 d . . .
H49A H 0.3342 0.0224 1.1001 0.039 Uiso 1 calc R . .
H49B H 0.3642 -0.0893 1.1802 0.039 Uiso 1 calc R . .
H49C H 0.2810 -0.1090 1.0626 0.039 Uiso 1 calc R . .
C50 C 0.54372(13) -0.02757(19) 1.14783(11) 0.0344(3) Uani 1 d . . .
H50A H 0.6071 -0.0524 1.1330 0.052 Uiso 1 calc R . .
H50B H 0.5576 -0.0447 1.2208 0.052 Uiso 1 calc R . .
H50C H 0.5308 0.0600 1.1345 0.052 Uiso 1 calc R . .
C51 C 0.46343(16) -0.23745(15) 1.09507(13) 0.0352(3) Uani 1 d . . .
H51A H 0.3978 -0.2827 1.0524 0.053 Uiso 1 calc R . .
H51B H 0.4819 -0.2563 1.1686 0.053 Uiso 1 calc R . .
H51C H 0.5241 -0.2611 1.0756 0.053 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
O31 Fe1 O1 159.13(4) . . ?
O31 Fe1 N7 91.96(4) . . ?
O1 Fe1 N7 82.87(4) . . ?
O31 Fe1 N37 83.06(4) . . ?
O1 Fe1 N37 93.36(4) . . ?
N7 Fe1 N37 155.74(4) . . ?
O31 Fe1 N11 104.21(4) . . ?
O1 Fe1 N11 96.60(4) . . ?
N7 Fe1 N11 99.72(4) . . ?
N37 Fe1 N11 104.51(4) . . ?
N12 N11 Fe1 110.50(8) . . ?
N13 N12 N11 178.56(14) . . ?
C1 O1 Fe1 114.19(7) . . ?
O1 C1 C2 124.42(9) . . ?
O1 C1 C6 115.19(9) . . ?
C2 C1 C6 120.39(9) . . ?
C3 C2 C1 115.66(9) . . ?
C3 C2 C14 123.94(9) . . ?
C1 C2 C14 120.40(9) . . ?
C2 C3 C4 124.89(9) . . ?
C5 C4 C3 118.86(9) . . ?
C5 C4 C18 122.51(9) . . ?
C3 C4 C18 118.62(9) . . ?
C4 C5 C6 118.85(9) . . ?
N7 C6 C5 127.18(9) . . ?
N7 C6 C1 111.53(9) . . ?
C5 C6 C1 121.23(9) . . ?
C6 N7 C8 118.91(9) . . ?
C6 N7 Fe1 114.16(7) . . ?
C8 N7 Fe1 126.92(7) . . ?
C13 C8 C9 120.98(11) . . ?
C13 C8 N7 120.62(11) . . ?
C9 C8 N7 118.35(10) . . ?
C10 C9 C8 119.32(13) . . ?
C11 C10 C9 120.24(15) . . ?
C12 C11 C10 119.89(13) . . ?
C11 C12 C13 121.07(14) . . ?
C8 C13 C12 118.47(14) . . ?
C2 C14 C16 111.56(10) . . ?
C2 C14 C15 109.16(9) . . ?
C16 C14 C15 108.65(10) . . ?
C2 C14 C17 109.75(9) . . ?
C16 C14 C17 107.74(10) . . ?
C15 C14 C17 109.94(10) . . ?
C19 C18 C4 111.89(9) . . ?
C19 C18 C21 108.21(10) . . ?
C4 C18 C21 110.02(10) . . ?
C19 C18 C20 108.48(11) . . ?
C4 C18 C20 108.48(9) . . ?
C21 C18 C20 109.73(11) . . ?
C31 O31 Fe1 115.06(7) . . ?
O31 C31 C32 123.68(10) . . ?
O31 C31 C36 115.51(9) . . ?
C32 C31 C36 120.79(10) . . ?
C33 C32 C31 115.57(10) . . ?
C33 C32 C44 123.24(9) . . ?
C31 C32 C44 121.19(9) . . ?
C32 C33 C34 124.75(10) . . ?
C35 C34 C33 119.10(10) . . ?
C35 C34 C48 122.91(10) . . ?
C33 C34 C48 117.96(10) . . ?
C34 C35 C36 118.65(10) . . ?
N37 C36 C35 127.35(10) . . ?
N37 C36 C31 111.53(9) . . ?
C35 C36 C31 121.12(9) . . ?
C36 N37 C38 121.00(9) . . ?
C36 N37 Fe1 114.82(7) . . ?
C38 N37 Fe1 124.04(7) . . ?
C43 C38 C39 120.37(11) . . ?
C43 C38 N37 120.81(10) . . ?
C39 C38 N37 118.62(11) . . ?
C38 C39 C40 119.10(13) . . ?
C41 C40 C39 120.56(13) . . ?
C42 C41 C40 119.98(12) . . ?
C41 C42 C43 120.28(13) . . ?
C42 C43 C38 119.69(12) . . ?
C32 C44 C46 111.75(10) . . ?
C32 C44 C47 109.62(9) . . ?
C46 C44 C47 108.12(9) . . ?
C32 C44 C45 110.09(9) . . ?
C46 C44 C45 107.69(10) . . ?
C47 C44 C45 109.52(10) . . ?
C34 C48 C49 112.03(10) . . ?
C34 C48 C51 110.20(11) . . ?
C49 C48 C51 108.09(12) . . ?
C34 C48 C50 108.63(11) . . ?
C49 C48 C50 108.12(12) . . ?
C51 C48 C50 109.72(13) . . ?
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 O31 1.8732(8) . ?
Fe1 O1 1.8788(8) . ?
Fe1 N7 1.8793(9) . ?
Fe1 N37 1.8873(9) . ?
Fe1 N11 1.9576(10) . ?
N11 N12 1.2209(15) . ?
N12 N13 1.1511(17) . ?
O1 C1 1.3075(12) . ?
C1 C2 1.4306(14) . ?
C1 C6 1.4314(14) . ?
C2 C3 1.3827(15) . ?
C2 C14 1.5245(16) . ?
C3 C4 1.4355(15) . ?
C4 C5 1.3763(14) . ?
C4 C18 1.5315(15) . ?
C5 C6 1.4191(14) . ?
C6 N7 1.3567(13) . ?
N7 C8 1.4253(14) . ?
C8 C13 1.3892(16) . ?
C8 C9 1.3993(17) . ?
C9 C10 1.3897(18) . ?
C10 C11 1.387(3) . ?
C11 C12 1.382(3) . ?
C12 C13 1.3982(19) . ?
C14 C16 1.5341(17) . ?
C14 C15 1.5397(18) . ?
C14 C17 1.5413(17) . ?
C18 C19 1.5314(16) . ?
C18 C21 1.5403(17) . ?
C18 C20 1.5436(17) . ?
O31 C31 1.3103(13) . ?
C31 C32 1.4269(14) . ?
C31 C36 1.4290(15) . ?
C32 C33 1.3836(16) . ?
C32 C44 1.5293(16) . ?
C33 C34 1.4350(16) . ?
C34 C35 1.3765(15) . ?
C34 C48 1.5305(16) . ?
C35 C36 1.4208(15) . ?
C36 N37 1.3587(13) . ?
N37 C38 1.4307(13) . ?
C38 C43 1.3950(17) . ?
C38 C39 1.3952(17) . ?
C39 C40 1.3961(19) . ?
C40 C41 1.389(3) . ?
C41 C42 1.383(2) . ?
C42 C43 1.3925(17) . ?
C44 C46 1.5344(16) . ?
C44 C47 1.5415(17) . ?
C44 C45 1.5424(17) . ?
C48 C49 1.5330(19) . ?
C48 C51 1.539(2) . ?
C48 C50 1.546(2) . ?
