#------------------------------------------------------------------------------
#$Date: 2022-03-05 01:49:22 +0200 (Sat, 05 Mar 2022) $
#$Revision: 273443 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/96/7709642.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_7709642
loop_
_publ_author_name
'Shahid, Namrah'
'Burrows, Kay E.'
'Pask, Christopher M.'
'Cespedes, Oscar'
'Howard, Mark J.'
'McGowan, Patrick C.'
'Halcrow, Malcolm A.'
_publ_section_title
;
 Heteroleptic iron(ii) complexes of chiral 2,6-bis(oxazolin-2-yl)-pyridine
 (PyBox) and 2,6-bis(thiazolin-2-yl)pyridine ligands -- the interplay of
 two different ligands on the metal ion spin sate
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00393G
_journal_year                    2022
_chemical_absolute_configuration ab
_chemical_formula_moiety         'C36 H36 Fe N8 O2, 2(Cl O4)'
_chemical_formula_sum            'C36 H36 Cl2 Fe N8 O10'
_chemical_formula_weight         867.48
_chemical_name_systematic
'[2,6-Bis((S)-4-isopropyl-4,5-dihydrooxazol-2-yl)pyridine]-[2,6-bis(1H-benzimidazol-2-yl)pyridine]iron(II) diperchlorate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-09-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2022-01-10 deposited with the CCDC.	2022-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1310(5)
_cell_length_b                   19.1776(10)
_cell_length_c                   19.2647(10)
_cell_measurement_reflns_used    6457
_cell_measurement_temperature    120.02(16)
_cell_measurement_theta_max      72.87
_cell_measurement_theta_min      4.58
_cell_volume                     3742.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.02(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  24.00   1.00    1.00    --  -38.50  37.00 -30.00   77
  2  ω   -107.00 -18.00   1.00    1.00    --  -38.50 -57.00 -30.00   89
  3  ω     82.00 115.00   1.00    4.00    --  104.98 -61.00 -30.00   33
  4  ω     56.00 117.00   1.00    4.00    --  104.98 -65.00 -66.57   61
  5  ω     45.00 128.00   1.00    4.00    --  104.98 -15.00 -60.00   83
  6  ω     98.00 171.00   1.00    4.00    --  104.98  30.00 150.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0122214000
_diffrn_orient_matrix_UB_12      -0.0765764000
_diffrn_orient_matrix_UB_13      0.0374918000
_diffrn_orient_matrix_UB_21      0.0793887000
_diffrn_orient_matrix_UB_22      0.0125203000
_diffrn_orient_matrix_UB_23      -0.0003516000
_diffrn_orient_matrix_UB_31      -0.0030393000
_diffrn_orient_matrix_UB_32      0.0194848000
_diffrn_orient_matrix_UB_33      0.1472406000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9691
_diffrn_reflns_point_group_measured_fraction_full 0.870
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        72.000
_diffrn_reflns_theta_max         73.718
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.147
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1792
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone/diethyl ether'
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 2240 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         6463
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0763P)²+4.5119P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1396
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.591
_reflns_Friedel_fraction_full    0.738
_reflns_Friedel_fraction_max     0.719
_reflns_number_gt                6287
_reflns_number_total             6463
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00393g2.cif
_cod_data_source_block           kb-054
_cod_database_code               7709642
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.644(2)
 0.356(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C18-C21A = C21A-C22A = C21A-C23A = C18-C21B = C21B-C22B = C21B-C23B
 1.53415 with sigma of 0.02
 C18-C22A = C18-C23A = C22A-C23A = C18-C22B = C18-C23B = C22B-C23B
 2.505267 with sigma of 0.02
4. Others
 1(DFIX)=FVAR(1)
 1(DFIX)=1.633*FVAR(2)
 Fixed Sof: H18(0.5) H18A(0.5) C21A(0.5) H21A(0.5) C22A(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C23A(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C21B(0.5)
 H21B(0.5) C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5) C23B(0.5) H23D(0.5)
 H23E(0.5) H23F(0.5)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C18(H18), C18(H18A), C21A(H21A), C21B(H21B)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C19(H19A,H19B)
5.c Me refined with riding coordinates:
 C22A(H22A,H22B,H22C), C23A(H23A,H23B,H23C), C22B(H22D,H22E,H22F), C23B(H23D,
 H23E,H23F)
5.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C26(H26), C27(H27), C28(H28), C33(H33), C34(H34),
 C35(H35), C36(H36), N38(H38), C42(H42), C43(H43), C44(H44), C45(H45), N47(H47)
5.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.348
_oxdiff_exptl_absorpt_empirical_full_min 0.837
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.12836(13) 0.45057(6) 0.71495(7) 0.0269(3) Uani 1 1 d . . . . .
N2 N 0.1262(8) 0.5307(3) 0.7833(4) 0.0307(13) Uani 1 1 d . . . . .
C3 C 0.0260(8) 0.5372(4) 0.8296(5) 0.0336(18) Uani 1 1 d . . . . .
C4 C 0.0153(8) 0.5951(5) 0.8725(6) 0.041(2) Uani 1 1 d . . . . .
H4 H -0.057161 0.600075 0.903397 0.049 Uiso 1 1 calc R U . . .
C5 C 0.1134(9) 0.6453(4) 0.8690(5) 0.041(2) Uani 1 1 d . . . . .
H5 H 0.108116 0.685294 0.898071 0.050 Uiso 1 1 calc R U . . .
C6 C 0.2183(8) 0.6382(4) 0.8241(5) 0.0338(18) Uani 1 1 d . . . . .
H6 H 0.286639 0.672128 0.822757 0.041 Uiso 1 1 calc R U . . .
C7 C 0.2217(8) 0.5798(4) 0.7805(5) 0.0317(17) Uani 1 1 d . . . . .
C8 C -0.0600(9) 0.4760(5) 0.8226(5) 0.036(2) Uani 1 1 d . . . . .
N9 N -0.0309(7) 0.4277(4) 0.7789(4) 0.0356(17) Uani 1 1 d . . . . .
C10 C -0.1254(10) 0.3695(5) 0.7903(6) 0.049(3) Uani 1 1 d . . . . .
H10 H -0.163212 0.354191 0.744872 0.059 Uiso 1 1 calc R U . . .
C11 C -0.2322(10) 0.4061(5) 0.8333(8) 0.059(3) Uani 1 1 d . . . . .
H11A H -0.307078 0.420623 0.803584 0.071 Uiso 1 1 calc R U . . .
H11B H -0.265649 0.375136 0.870448 0.071 Uiso 1 1 calc R U . . .
O12 O -0.1646(6) 0.4673(3) 0.8629(4) 0.0438(16) Uani 1 1 d . . . . .
C13 C -0.0576(11) 0.3080(5) 0.8259(6) 0.045(2) Uani 1 1 d . . . . .
H13 H 0.015334 0.292055 0.794718 0.055 Uiso 1 1 calc R U . . .
C14 C 0.0037(9) 0.3269(5) 0.8953(6) 0.042(2) Uani 1 1 d . . . . .
H14A H 0.073513 0.361543 0.888162 0.064 Uiso 1 1 calc R U . . .
H14B H 0.041465 0.285005 0.916649 0.064 Uiso 1 1 calc R U . . .
H14C H -0.064208 0.346327 0.925923 0.064 Uiso 1 1 calc R U . . .
C15 C -0.1547(12) 0.2471(6) 0.8335(8) 0.067(4) Uani 1 1 d . . . . .
H15A H -0.108565 0.206653 0.852950 0.101 Uiso 1 1 calc R U . . .
H15B H -0.190805 0.235012 0.787886 0.101 Uiso 1 1 calc R U . . .
H15C H -0.226789 0.260744 0.864609 0.101 Uiso 1 1 calc R U . . .
C16 C 0.3165(8) 0.5616(5) 0.7269(5) 0.0334(18) Uani 1 1 d . . . . .
N17 N 0.2945(7) 0.5093(4) 0.6873(4) 0.0336(16) Uani 1 1 d . . . . .
C18 C 0.4059(9) 0.5044(5) 0.6389(5) 0.043(2) Uani 1 1 d D . . . .
H18 H 0.441130 0.455730 0.639148 0.051 Uiso 0.5 1 calc R U P A 1
H18A H 0.441445 0.455820 0.640496 0.051 Uiso 0.5 1 calc R U P B 2
C19 C 0.5055(11) 0.5525(7) 0.6720(6) 0.055(3) Uani 1 1 d . . . . .
H19A H 0.571886 0.525605 0.698512 0.065 Uiso 1 1 calc R U . . .
H19B H 0.551415 0.580649 0.636302 0.065 Uiso 1 1 calc R U . . .
O20 O 0.4278(6) 0.5973(3) 0.7183(4) 0.0432(15) Uani 1 1 d . . . . .
C21A C 0.391(2) 0.5291(9) 0.5642(9) 0.045(5) Uiso 0.5 1 d D . P C 1
H21A H 0.479119 0.527389 0.541045 0.054 Uiso 0.5 1 calc R U P C 1
C22A C 0.337(2) 0.6030(8) 0.5598(10) 0.040(4) Uiso 0.5 1 d D . P C 1
H22A H 0.329374 0.616640 0.510960 0.061 Uiso 0.5 1 calc R U P C 1
H22B H 0.250535 0.605055 0.582015 0.061 Uiso 0.5 1 calc R U P C 1
H22C H 0.398032 0.634887 0.583536 0.061 Uiso 0.5 1 calc R U P C 1
C23A C 0.298(2) 0.4782(10) 0.5276(11) 0.053(5) Uiso 0.5 1 d D . P C 1
H23A H 0.334068 0.430901 0.530942 0.080 Uiso 0.5 1 calc R U P C 1
H23B H 0.211144 0.479813 0.549682 0.080 Uiso 0.5 1 calc R U P C 1
H23C H 0.289995 0.491401 0.478631 0.080 Uiso 0.5 1 calc R U P C 1
C21B C 0.343(2) 0.5165(10) 0.5665(8) 0.042(5) Uiso 0.5 1 d D . P C 2
H21B H 0.267666 0.483155 0.560494 0.050 Uiso 0.5 1 calc R U P C 2
C22B C 0.288(3) 0.5919(11) 0.5628(12) 0.057(6) Uiso 0.5 1 d D . P C 2
H22D H 0.222690 0.598770 0.599580 0.085 Uiso 0.5 1 calc R U P C 2
H22E H 0.360931 0.625056 0.569070 0.085 Uiso 0.5 1 calc R U P C 2
H22F H 0.246894 0.599557 0.517494 0.085 Uiso 0.5 1 calc R U P C 2
C23B C 0.445(2) 0.5025(11) 0.5109(9) 0.049(5) Uiso 0.5 1 d D . P C 2
H23D H 0.476465 0.454406 0.515133 0.074 Uiso 0.5 1 calc R U P C 2
H23E H 0.404983 0.509255 0.465070 0.074 Uiso 0.5 1 calc R U P C 2
H23F H 0.519020 0.534755 0.516645 0.074 Uiso 0.5 1 calc R U P C 2
N24 N 0.1255(8) 0.3746(3) 0.6416(4) 0.0303(13) Uani 1 1 d . . . D 2
C25 C 0.0502(8) 0.3817(4) 0.5841(5) 0.0309(18) Uani 1 1 d . . . D 2
C26 C 0.0499(10) 0.3344(5) 0.5320(5) 0.040(2) Uani 1 1 d . . . D 2
H26 H -0.005644 0.340327 0.492660 0.048 Uiso 1 1 calc R U . D 2
C27 C 0.1339(11) 0.2764(4) 0.5375(5) 0.0394(19) Uani 1 1 d . . . D 2
H27 H 0.135820 0.242314 0.501742 0.047 Uiso 1 1 calc R U . D 2
C28 C 0.2130(9) 0.2693(5) 0.5948(5) 0.037(2) Uani 1 1 d . . . D 2
H28 H 0.271857 0.230916 0.598779 0.044 Uiso 1 1 calc R U . D 2
C29 C 0.2057(8) 0.3190(4) 0.6466(5) 0.0306(18) Uani 1 1 d . . . D 2
C30 C -0.0222(8) 0.4483(5) 0.5882(5) 0.0323(18) Uani 1 1 d . . . D 2
N31 N -0.0043(8) 0.4909(4) 0.6401(4) 0.0325(16) Uani 1 1 d . . . D 2
C32 C -0.0824(9) 0.5493(5) 0.6272(5) 0.0356(19) Uani 1 1 d . . . D 2
C33 C -0.1010(10) 0.6105(5) 0.6644(6) 0.045(2) Uani 1 1 d . . . D 2
H33 H -0.057992 0.618549 0.707470 0.054 Uiso 1 1 calc R U . D 2
C34 C -0.1856(10) 0.6595(5) 0.6353(6) 0.047(3) Uani 1 1 d . . . D 2
H34 H -0.203060 0.701309 0.660129 0.057 Uiso 1 1 calc R U . D 2
C35 C -0.2453(10) 0.6498(6) 0.5716(7) 0.052(3) Uani 1 1 d . . . D 2
H35 H -0.300557 0.685318 0.553320 0.062 Uiso 1 1 calc R U . D 2
C36 C -0.2266(9) 0.5902(5) 0.5345(6) 0.045(2) Uani 1 1 d . . . D 2
H36 H -0.268076 0.583412 0.490764 0.054 Uiso 1 1 calc R U . D 2
C37 C -0.1436(9) 0.5393(5) 0.5633(5) 0.0365(19) Uani 1 1 d . . . D 2
N38 N -0.1042(8) 0.4744(4) 0.5392(4) 0.0356(16) Uani 1 1 d . . . D 2
H38 H -0.127772 0.454349 0.500029 0.043 Uiso 1 1 calc R U . D 2
C39 C 0.2784(8) 0.3211(4) 0.7119(5) 0.0321(17) Uani 1 1 d . . . D 2
N40 N 0.2578(7) 0.3741(4) 0.7547(4) 0.0339(16) Uani 1 1 d . . . D 2
C41 C 0.3355(9) 0.3615(5) 0.8126(5) 0.040(2) Uani 1 1 d . . . D 2
C42 C 0.3561(10) 0.3982(7) 0.8732(5) 0.053(3) Uani 1 1 d . . . D 2
H42 H 0.313939 0.441708 0.881458 0.063 Uiso 1 1 calc R U . D 2
C43 C 0.4405(12) 0.3692(9) 0.9213(7) 0.068(4) Uani 1 1 d . . . D 2
H43 H 0.456693 0.393057 0.963686 0.082 Uiso 1 1 calc R U . D 2
C44 C 0.5035(12) 0.3043(8) 0.9090(8) 0.071(4) Uani 1 1 d . . . D 2
H44 H 0.560488 0.286080 0.943642 0.086 Uiso 1 1 calc R U . D 2
C45 C 0.4865(11) 0.2683(7) 0.8514(9) 0.072(5) Uani 1 1 d . . . D 2
H45 H 0.528994 0.224725 0.844485 0.086 Uiso 1 1 calc R U . D 2
C46 C 0.4039(9) 0.2966(6) 0.8013(5) 0.044(2) Uani 1 1 d . . . D 2
N47 N 0.3631(7) 0.2734(4) 0.7366(4) 0.0388(17) Uani 1 1 d . . . D 2
H47 H 0.387912 0.234744 0.715712 0.047 Uiso 1 1 calc R U . D 2
Cl48 Cl 0.6537(2) 0.34206(12) 0.63120(13) 0.0415(5) Uani 1 1 d . . . E 2
O49 O 0.6404(9) 0.2995(5) 0.6937(5) 0.068(2) Uani 1 1 d . . . E 2
O50 O 0.5346(8) 0.3369(5) 0.5929(5) 0.062(2) Uani 1 1 d . . . E 2
O51 O 0.7629(8) 0.3136(5) 0.5939(5) 0.065(2) Uani 1 1 d . . . E 2
O52 O 0.6830(7) 0.4128(4) 0.6511(4) 0.0535(19) Uani 1 1 d . . . E 2
Cl53 Cl 0.3808(2) 0.09813(10) 0.64360(11) 0.0333(4) Uani 1 1 d . . . F 2
O54 O 0.4638(7) 0.0374(3) 0.6447(4) 0.0466(17) Uani 1 1 d . . . F 2
O55 O 0.3074(7) 0.0999(4) 0.5793(3) 0.0408(15) Uani 1 1 d . . . F 2
O56 O 0.2911(6) 0.0981(4) 0.7005(3) 0.0411(15) Uani 1 1 d . . . F 2
O57 O 0.4605(6) 0.1613(3) 0.6470(4) 0.0424(16) Uani 1 1 d . . . F 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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 N9 76.5(3) . . ?
N2 Fe1 N17 76.4(3) . . ?
N2 Fe1 N24 176.2(3) . . ?
N2 Fe1 N31 99.1(3) . . ?
N2 Fe1 N40 107.3(3) . . ?
N9 Fe1 N17 152.7(3) . . ?
N9 Fe1 N31 89.3(3) . . ?
N9 Fe1 N40 97.0(3) . . ?
N17 Fe1 N31 98.1(3) . . ?
N17 Fe1 N40 88.1(3) . . ?
N24 Fe1 N9 104.5(3) . . ?
N24 Fe1 N17 102.7(3) . . ?
N24 Fe1 N31 77.2(3) . . ?
N24 Fe1 N40 76.3(3) . . ?
N40 Fe1 N31 153.5(3) . . ?
C3 N2 Fe1 120.3(6) . . ?
C7 N2 Fe1 119.7(6) . . ?
C7 N2 C3 119.9(7) . . ?
N2 C3 C4 121.5(8) . . ?
N2 C3 C8 108.1(8) . . ?
C4 C3 C8 130.4(8) . . ?
C3 C4 H4 120.9 . . ?
C5 C4 C3 118.1(8) . . ?
C5 C4 H4 120.9 . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.0(8) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 120.8 . . ?
C5 C6 C7 118.4(8) . . ?
C7 C6 H6 120.8 . . ?
N2 C7 C6 121.0(8) . . ?
N2 C7 C16 109.5(7) . . ?
C6 C7 C16 129.4(8) . . ?
N9 C8 C3 120.0(8) . . ?
N9 C8 O12 118.6(8) . . ?
O12 C8 C3 121.4(9) . . ?
C8 N9 Fe1 114.5(6) . . ?
C8 N9 C10 107.2(9) . . ?
C10 N9 Fe1 138.3(7) . . ?
N9 C10 H10 109.7 . . ?
N9 C10 C11 101.0(7) . . ?
N9 C10 C13 110.9(7) . . ?
C11 C10 H10 109.7 . . ?
C13 C10 H10 109.7 . . ?
C13 C10 C11 115.4(10) . . ?
C10 C11 H11A 110.9 . . ?
C10 C11 H11B 110.9 . . ?
H11A C11 H11B 108.9 . . ?
O12 C11 C10 104.2(7) . . ?
O12 C11 H11A 110.9 . . ?
O12 C11 H11B 110.9 . . ?
C8 O12 C11 104.1(9) . . ?
C10 C13 H13 107.4 . . ?
C10 C13 C15 110.1(8) . . ?
C14 C13 C10 113.2(8) . . ?
C14 C13 H13 107.4 . . ?
C14 C13 C15 111.1(10) . . ?
C15 C13 H13 107.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N17 C16 C7 119.8(8) . . ?
N17 C16 O20 118.6(9) . . ?
O20 C16 C7 121.7(8) . . ?
C16 N17 Fe1 114.2(6) . . ?
C16 N17 C18 107.1(8) . . ?
C18 N17 Fe1 138.2(6) . . ?
N17 C18 H18 109.3 . . ?
N17 C18 H18A 108.4 . . ?
N17 C18 C19 102.0(8) . . ?
N17 C18 C21A 120.3(11) . . ?
N17 C18 C21B 104.1(10) . . ?
C19 C18 H18 109.3 . . ?
C19 C18 H18A 108.4 . . ?
C19 C18 C21A 106.1(11) . . ?
C19 C18 C21B 124.4(11) . . ?
C21A C18 H18 109.3 . . ?
C21B C18 H18A 108.4 . . ?
C18 C19 H19A 110.8 . . ?
C18 C19 H19B 110.8 . . ?
H19A C19 H19B 108.9 . . ?
O20 C19 C18 104.8(8) . . ?
O20 C19 H19A 110.8 . . ?
O20 C19 H19B 110.8 . . ?
C16 O20 C19 103.2(8) . . ?
C18 C21A H21A 108.8 . . ?
C18 C21A C23A 107.5(15) . . ?
C22A C21A C18 112.2(14) . . ?
C22A C21A H21A 108.8 . . ?
C22A C21A C23A 110.5(16) . . ?
C23A C21A H21A 108.8 . . ?
C21A C22A H22A 109.5 . . ?
C21A C22A H22B 109.5 . . ?
C21A C22A H22C 109.5 . . ?
H22A C22A H22B 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C21A C23A H23A 109.5 . . ?
C21A C23A H23B 109.5 . . ?
C21A C23A H23C 109.5 . . ?
H23A C23A H23B 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C18 C21B H21B 108.8 . . ?
C22B C21B C18 109.2(14) . . ?
C22B C21B H21B 108.8 . . ?
C23B C21B C18 109.0(14) . . ?
C23B C21B H21B 108.8 . . ?
C23B C21B C22B 112.1(16) . . ?
C21B C22B H22D 109.5 . . ?
C21B C22B H22E 109.5 . . ?
C21B C22B H22F 109.5 . . ?
H22D C22B H22E 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C21B C23B H23D 109.5 . . ?
C21B C23B H23E 109.5 . . ?
C21B C23B H23F 109.5 . . ?
H23D C23B H23E 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C25 N24 Fe1 120.5(5) . . ?
C29 N24 Fe1 120.7(6) . . ?
C29 N24 C25 118.6(7) . . ?
N24 C25 C26 122.9(7) . . ?
N24 C25 C30 108.9(8) . . ?
C26 C25 C30 128.2(8) . . ?
C25 C26 H26 120.9 . . ?
C25 C26 C27 118.2(9) . . ?
C27 C26 H26 120.9 . . ?
C26 C27 H27 120.2 . . ?
C28 C27 C26 119.6(8) . . ?
C28 C27 H27 120.2 . . ?
C27 C28 H28 120.6 . . ?
C27 C28 C29 118.8(8) . . ?
C29 C28 H28 120.6 . . ?
N24 C29 C28 121.9(8) . . ?
N24 C29 C39 110.2(8) . . ?
C28 C29 C39 128.0(8) . . ?
N31 C30 C25 120.9(8) . . ?
N31 C30 N38 112.8(8) . . ?
N38 C30 C25 126.1(8) . . ?
C30 N31 Fe1 112.5(5) . . ?
C30 N31 C32 106.7(8) . . ?
C32 N31 Fe1 140.8(7) . . ?
C33 C32 N31 131.7(10) . . ?
C33 C32 C37 120.8(9) . . ?
C37 C32 N31 107.4(8) . . ?
C32 C33 H33 121.7 . . ?
C32 C33 C34 116.6(11) . . ?
C34 C33 H33 121.7 . . ?
C33 C34 H34 118.8 . . ?
C35 C34 C33 122.5(10) . . ?
C35 C34 H34 118.8 . . ?
C34 C35 H35 119.3 . . ?
C36 C35 C34 121.3(10) . . ?
C36 C35 H35 119.3 . . ?
C35 C36 H36 121.3 . . ?
C35 C36 C37 117.4(11) . . ?
C37 C36 H36 121.3 . . ?
C32 C37 C36 121.4(9) . . ?
N38 C37 C32 107.0(8) . . ?
N38 C37 C36 131.7(10) . . ?
C30 N38 C37 106.0(8) . . ?
C30 N38 H38 127.0 . . ?
C37 N38 H38 127.0 . . ?
N40 C39 C29 118.6(8) . . ?
N40 C39 N47 113.8(8) . . ?
N47 C39 C29 127.6(8) . . ?
C39 N40 Fe1 113.9(6) . . ?
C39 N40 C41 106.0(8) . . ?
C41 N40 Fe1 140.0(7) . . ?
N40 C41 C46 107.7(9) . . ?
C42 C41 N40 132.6(10) . . ?
C42 C41 C46 119.7(9) . . ?
C41 C42 H42 121.4 . . ?
C43 C42 C41 117.1(13) . . ?
C43 C42 H42 121.4 . . ?
C42 C43 H43 119.3 . . ?
C42 C43 C44 121.4(13) . . ?
C44 C43 H43 119.3 . . ?
C43 C44 H44 118.6 . . ?
C45 C44 C43 122.8(11) . . ?
C45 C44 H44 118.6 . . ?
C44 C45 H45 121.3 . . ?
C44 C45 C46 117.3(14) . . ?
C46 C45 H45 121.3 . . ?
C45 C46 C41 121.6(12) . . ?
C45 C46 N47 132.8(12) . . ?
N47 C46 C41 105.6(8) . . ?
C39 N47 C46 106.9(8) . . ?
C39 N47 H47 126.6 . . ?
C46 N47 H47 126.6 . . ?
O50 Cl48 O49 108.2(6) . . ?
O50 Cl48 O51 111.7(5) . . ?
O50 Cl48 O52 112.3(5) . . ?
O51 Cl48 O49 105.8(6) . . ?
O51 Cl48 O52 109.5(5) . . ?
O52 Cl48 O49 109.1(5) . . ?
O54 Cl53 O55 109.4(4) . . ?
O54 Cl53 O57 110.4(4) . . ?
O55 Cl53 O57 107.7(4) . . ?
O56 Cl53 O54 111.2(4) . . ?
O56 Cl53 O55 109.4(4) . . ?
O56 Cl53 O57 108.7(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 N2 2.024(6) . ?
Fe1 N9 2.076(8) . ?
Fe1 N17 2.094(8) . ?
Fe1 N24 2.029(7) . ?
Fe1 N31 2.118(7) . ?
Fe1 N40 2.110(7) . ?
N2 C3 1.357(11) . ?
N2 C7 1.351(11) . ?
C3 C4 1.389(13) . ?
C3 C8 1.468(12) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(13) . ?
C5 H5 0.9500 . ?
C5 C6 1.378(13) . ?
C6 H6 0.9500 . ?
C6 C7 1.401(12) . ?
C7 C16 1.453(13) . ?
C8 N9 1.285(13) . ?
C8 O12 1.325(12) . ?
N9 C10 1.487(11) . ?
C10 H10 1.0000 . ?
C10 C11 1.533(18) . ?
C10 C13 1.528(13) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 O12 1.474(13) . ?
C13 H13 1.0000 . ?
C13 C14 1.519(15) . ?
C13 C15 1.534(14) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N17 1.280(13) . ?
C16 O20 1.329(10) . ?
N17 C18 1.467(11) . ?
C18 H18 1.0000 . ?
C18 H18A 1.0000 . ?
C18 C19 1.507(16) . ?
C18 C21A 1.521(18) . ?
C18 C21B 1.552(18) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 O20 1.469(13) . ?
C21A H21A 1.0000 . ?
C21A C22A 1.520(19) . ?
C21A C23A 1.53(2) . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C21B H21B 1.0000 . ?
C21B C22B 1.55(2) . ?
C21B C23B 1.51(2) . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
N24 C25 1.352(11) . ?
N24 C29 1.345(10) . ?
C25 C26 1.353(14) . ?
C25 C30 1.475(12) . ?
C26 H26 0.9500 . ?
C26 C27 1.405(13) . ?
C27 H27 0.9500 . ?
C27 C28 1.371(13) . ?
C28 H28 0.9500 . ?
C28 C29 1.383(13) . ?
C29 C39 1.458(12) . ?
C30 N31 1.304(13) . ?
C30 N38 1.354(11) . ?
N31 C32 1.393(10) . ?
C32 C33 1.388(14) . ?
C32 C37 1.393(14) . ?
C33 H33 0.9500 . ?
C33 C34 1.391(14) . ?
C34 H34 0.9500 . ?
C34 C35 1.380(18) . ?
C35 H35 0.9500 . ?
C35 C36 1.360(17) . ?
C36 H36 0.9500 . ?
C36 C37 1.403(13) . ?
C37 N38 1.386(12) . ?
N38 H38 0.8800 . ?
C39 N40 1.326(12) . ?
C39 N47 1.342(11) . ?
N40 C41 1.387(11) . ?
C41 C42 1.380(15) . ?
C41 C46 1.440(16) . ?
C42 H42 0.9500 . ?
C42 C43 1.379(17) . ?
C43 H43 0.9500 . ?
C43 C44 1.42(2) . ?
C44 H44 0.9500 . ?
C44 C45 1.32(2) . ?
C45 H45 0.9500 . ?
C45 C46 1.387(14) . ?
C46 N47 1.388(13) . ?
N47 H47 0.8800 . ?
Cl48 O49 1.461(9) . ?
Cl48 O50 1.418(8) . ?
Cl48 O51 1.428(8) . ?
Cl48 O52 1.440(7) . ?
Cl53 O54 1.437(6) . ?
Cl53 O55 1.446(7) . ?
Cl53 O56 1.423(6) . ?
Cl53 O57 1.458(7) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N38 H38 O55 0.88 1.96 2.835(10) 172.2 3_456 yes
N47 H47 O57 0.88 2.07 2.928(11) 165.4 . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N2 C3 C4 -173.8(7) . . . . ?
Fe1 N2 C3 C8 5.0(10) . . . . ?
Fe1 N2 C7 C6 175.9(7) . . . . ?
Fe1 N2 C7 C16 -2.7(10) . . . . ?
Fe1 N9 C10 C11 -164.7(8) . . . . ?
Fe1 N9 C10 C13 72.5(13) . . . . ?
Fe1 N17 C18 C19 -158.1(8) . . . . ?
Fe1 N17 C18 C21A 85.0(13) . . . . ?
Fe1 N17 C18 C21B 71.4(12) . . . . ?
Fe1 N24 C25 C26 176.5(8) . . . . ?
Fe1 N24 C25 C30 -1.4(9) . . . . ?
Fe1 N24 C29 C28 -174.9(7) . . . . ?
Fe1 N24 C29 C39 4.7(9) . . . . ?
Fe1 N31 C32 C33 1.2(16) . . . . ?
Fe1 N31 C32 C37 178.5(7) . . . . ?
Fe1 N40 C41 C42 2.0(17) . . . . ?
Fe1 N40 C41 C46 -177.4(7) . . . . ?
N2 C3 C4 C5 -2.6(15) . . . . ?
N2 C3 C8 N9 1.4(12) . . . . ?
N2 C3 C8 O12 178.1(8) . . . . ?
N2 C7 C16 N17 6.0(11) . . . . ?
N2 C7 C16 O20 -172.7(8) . . . . ?
C3 N2 C7 C6 -0.9(13) . . . . ?
C3 N2 C7 C16 -179.6(7) . . . . ?
C3 C4 C5 C6 0.2(15) . . . . ?
C3 C8 N9 Fe1 -6.7(11) . . . . ?
C3 C8 N9 C10 172.8(8) . . . . ?
C3 C8 O12 C11 172.6(9) . . . . ?
C4 C3 C8 N9 -180.0(10) . . . . ?
C4 C3 C8 O12 -3.3(16) . . . . ?
C4 C5 C6 C7 1.8(14) . . . . ?
C5 C6 C7 N2 -1.4(14) . . . . ?
C5 C6 C7 C16 176.9(9) . . . . ?
C6 C7 C16 N17 -172.5(9) . . . . ?
C6 C7 C16 O20 8.8(14) . . . . ?
C7 N2 C3 C4 3.0(14) . . . . ?
C7 N2 C3 C8 -178.3(8) . . . . ?
C7 C16 N17 Fe1 -6.3(10) . . . . ?
C7 C16 N17 C18 179.7(8) . . . . ?
C7 C16 O20 C19 167.0(9) . . . . ?
C8 C3 C4 C5 178.9(10) . . . . ?
C8 N9 C10 C11 15.9(10) . . . . ?
C8 N9 C10 C13 -106.9(10) . . . . ?
N9 C8 O12 C11 -10.7(11) . . . . ?
N9 C10 C11 O12 -21.3(10) . . . . ?
N9 C10 C13 C14 58.2(13) . . . . ?
N9 C10 C13 C15 -176.8(10) . . . . ?
C10 C11 O12 C8 19.8(10) . . . . ?
C11 C10 C13 C14 -55.9(11) . . . . ?
C11 C10 C13 C15 69.1(12) . . . . ?
O12 C8 N9 Fe1 176.5(6) . . . . ?
O12 C8 N9 C10 -3.9(11) . . . . ?
C13 C10 C11 O12 98.3(9) . . . . ?
C16 N17 C18 C19 13.7(10) . . . . ?
C16 N17 C18 C21A -103.2(12) . . . . ?
C16 N17 C18 C21B -116.8(11) . . . . ?
N17 C16 O20 C19 -11.8(11) . . . . ?
N17 C18 C19 O20 -19.9(10) . . . . ?
N17 C18 C21A C22A 52(2) . . . . ?
N17 C18 C21A C23A -69.4(17) . . . . ?
N17 C18 C21B C22B 65.3(18) . . . . ?
N17 C18 C21B C23B -171.9(14) . . . . ?
C18 C19 O20 C16 19.2(10) . . . . ?
C19 C18 C21A C22A -62.3(18) . . . . ?
C19 C18 C21A C23A 175.9(14) . . . . ?
C19 C18 C21B C22B -50(2) . . . . ?
C19 C18 C21B C23B 72.5(17) . . . . ?
O20 C16 N17 Fe1 172.5(6) . . . . ?
O20 C16 N17 C18 -1.5(11) . . . . ?
C21A C18 C19 O20 106.8(12) . . . . ?
C21B C18 C19 O20 96.7(13) . . . . ?
N24 C25 C26 C27 -1.5(15) . . . . ?
N24 C25 C30 N31 2.6(11) . . . . ?
N24 C25 C30 N38 177.8(8) . . . . ?
N24 C29 C39 N40 -0.2(11) . . . . ?
N24 C29 C39 N47 176.9(8) . . . . ?
C25 N24 C29 C28 0.0(13) . . . . ?
C25 N24 C29 C39 179.7(7) . . . . ?
C25 C26 C27 C28 0.0(16) . . . . ?
C25 C30 N31 Fe1 -2.6(10) . . . . ?
C25 C30 N31 C32 177.8(8) . . . . ?
C25 C30 N38 C37 -176.7(8) . . . . ?
C26 C25 C30 N31 -175.0(10) . . . . ?
C26 C25 C30 N38 0.2(15) . . . . ?
C26 C27 C28 C29 1.5(16) . . . . ?
C27 C28 C29 N24 -1.5(14) . . . . ?
C27 C28 C29 C39 178.9(9) . . . . ?
C28 C29 C39 N40 179.4(9) . . . . ?
C28 C29 C39 N47 -3.5(15) . . . . ?
C29 N24 C25 C26 1.5(13) . . . . ?
C29 N24 C25 C30 -176.3(7) . . . . ?
C29 C39 N40 Fe1 -3.9(10) . . . . ?
C29 C39 N40 C41 178.1(7) . . . . ?
C29 C39 N47 C46 -177.9(8) . . . . ?
C30 C25 C26 C27 175.9(9) . . . . ?
C30 N31 C32 C33 -179.3(9) . . . . ?
C30 N31 C32 C37 -2.1(10) . . . . ?
N31 C30 N38 C37 -1.1(10) . . . . ?
N31 C32 C33 C34 178.7(9) . . . . ?
N31 C32 C37 C36 -178.2(8) . . . . ?
N31 C32 C37 N38 1.4(10) . . . . ?
C32 C33 C34 C35 -2.3(15) . . . . ?
C32 C37 N38 C30 -0.2(10) . . . . ?
C33 C32 C37 C36 -0.5(14) . . . . ?
C33 C32 C37 N38 179.0(8) . . . . ?
C33 C34 C35 C36 1.7(15) . . . . ?
C34 C35 C36 C37 -0.4(14) . . . . ?
C35 C36 C37 C32 -0.2(13) . . . . ?
C35 C36 C37 N38 -179.6(9) . . . . ?
C36 C37 N38 C30 179.3(9) . . . . ?
C37 C32 C33 C34 1.7(14) . . . . ?
N38 C30 N31 Fe1 -178.4(6) . . . . ?
N38 C30 N31 C32 2.0(10) . . . . ?
C39 N40 C41 C42 179.2(10) . . . . ?
C39 N40 C41 C46 -0.2(9) . . . . ?
N40 C39 N47 C46 -0.6(10) . . . . ?
N40 C41 C42 C43 179.0(10) . . . . ?
N40 C41 C46 C45 -177.7(9) . . . . ?
N40 C41 C46 N47 -0.1(9) . . . . ?
C41 C42 C43 C44 0.1(16) . . . . ?
C41 C46 N47 C39 0.4(9) . . . . ?
C42 C41 C46 C45 2.8(14) . . . . ?
C42 C41 C46 N47 -179.7(8) . . . . ?
C42 C43 C44 C45 0.4(19) . . . . ?
C43 C44 C45 C46 0.7(18) . . . . ?
C44 C45 C46 C41 -2.3(16) . . . . ?
C44 C45 C46 N47 -179.1(11) . . . . ?
C45 C46 N47 C39 177.6(11) . . . . ?
C46 C41 C42 C43 -1.6(14) . . . . ?
N47 C39 N40 Fe1 178.6(6) . . . . ?
N47 C39 N40 C41 0.5(10) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.644(2)
2 0.356(2)
