# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_global
_database_code_depnum_ccdc_archive 'CCDC 1555086'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
_audit_creation_date             2016-07-26
_audit_creation_method           CRYSTALS_ver_14.61

_oxford_structure_analysis_title 'kso-a-011 in C 1 2/c 1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.8650(10)
_cell_length_b                   16.262(2)
_cell_length_c                   16.402(2)
_cell_angle_alpha                90
_cell_angle_beta                 92.280(10)
_cell_angle_gamma                90
_cell_volume                     2629.2(5)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1 '
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C25 H37.50 Fe1.25 N10 
# Dc =      1.38 Fooo =   1000.00 Mu =      7.41 M =    273.97
# Found Formula = C20 H48 Fe1 N8 
# Dc =      1.15 FOOO =   1000.00 Mu =      5.94 M =    228.25

_chemical_formula_sum            'C20 H48 Fe1 N8'
_chemical_formula_moiety         'C20 H48 Fe1 N8'
_chemical_compound_source        ?
_chemical_formula_weight         456.50


_cell_measurement_reflns_used    6017
_cell_measurement_theta_min      3.6890
_cell_measurement_theta_max      29.3580
_cell_measurement_temperature    100

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_min          0.226
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_max          0.384

_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1000
_exptl_absorpt_coefficient_mu    0.594

# Sheldrick geometric approximatio 0.87 0.87 
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            18348
_reflns_number_total             3370
_diffrn_reflns_av_R_equivalents  0.056
# Number of reflections without Friedels Law is 5312 
# Number of reflections with Friedels Law is 3370 
# Theoretical number of reflections is about 3689 


_diffrn_reflns_theta_min         2.796
_diffrn_reflns_theta_max         29.574
_diffrn_measured_fraction_theta_max 0.912

_diffrn_reflns_theta_full        25.138
_diffrn_measured_fraction_theta_full 0.987


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.74
_refine_diff_density_max         0.59


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         3366
_refine_ls_number_restraints     0
_refine_ls_number_parameters     133
_oxford_refine_ls_R_factor_ref   0.0572
_refine_ls_wR_factor_ref         0.1013
_refine_ls_goodness_of_fit_ref   0.9633
_refine_ls_shift/su_max          0.0005898
_refine_ls_shift/su_mean         0.0000405


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3366
_refine_ls_R_factor_all          0.0572
_refine_ls_wR_factor_all         0.1013

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2930
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_gt          0.0907

# The Flack parameter was determined before Friedel pairs were merged 
_refine_ls_abs_structure_Flack   .
_refine_ls_abs_structure_details 'Flack (1983), 1942 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.165E+04 0.243E+04 0.135E+04 427. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 1.0000 0.72098(3) 0.7500 0.0150 1.0000 Uani S T . . . .
N1 N 1.09472(18) 0.83001(11) 0.82190(11) 0.0188 1.0000 Uani . . . . . .
C3 C 1.0277(3) 0.84027(16) 0.90003(14) 0.0266 1.0000 Uani . . . . . .
H33 H 1.0439 0.7921 0.9329 0.0408 1.0000 Uiso R . . . . .
H32 H 1.0648 0.8887 0.9286 0.0416 1.0000 Uiso R . . . . .
H31 H 0.9313 0.8475 0.8905 0.0411 1.0000 Uiso R . . . . .
C4 C 1.0707(2) 0.90264(14) 0.76919(14) 0.0242 1.0000 Uani . . . . . .
H42 H 1.0853 0.9535 0.8006 0.0313 1.0000 Uiso R . . . . .
H41 H 1.1361 0.9005 0.7261 0.0308 1.0000 Uiso R . . . . .
C5 C 1.2422(2) 0.82091(15) 0.83936(15) 0.0257 1.0000 Uani . . . . . .
H51 H 1.2864 0.8095 0.7892 0.0394 1.0000 Uiso R . . . . .
H53 H 1.2796 0.8707 0.8642 0.0396 1.0000 Uiso R . . . . .
H52 H 1.2587 0.7761 0.8769 0.0394 1.0000 Uiso R . . . . .
N2 N 0.82154(18) 0.68732(11) 0.81267(11) 0.0184 1.0000 Uani . . . . . .
N3 N 0.77899(19) 0.63306(12) 0.75796(11) 0.0202 1.0000 Uani . . . . . .
N4 N 0.85620(18) 0.63704(11) 0.69485(11) 0.0179 1.0000 Uani . . . . . .
C9 C 0.8254(2) 0.57553(14) 0.63035(13) 0.0210 1.0000 Uani . . . . . .
C10 C 0.6724(2) 0.56333(16) 0.61569(15) 0.0268 1.0000 Uani . . . . . .
H101 H 0.6569 0.5235 0.5718 0.0416 1.0000 Uiso R . . . . .
H103 H 0.6297 0.6156 0.6002 0.0420 1.0000 Uiso R . . . . .
H102 H 0.6322 0.5438 0.6660 0.0420 1.0000 Uiso R . . . . .
C11 C 0.8951(3) 0.49383(15) 0.65335(16) 0.0278 1.0000 Uani . . . . . .
H111 H 0.8799 0.4541 0.6097 0.0421 1.0000 Uiso R . . . . .
H113 H 0.9912 0.5028 0.6614 0.0428 1.0000 Uiso R . . . . .
H112 H 0.8598 0.4731 0.7041 0.0423 1.0000 Uiso R . . . . .
C12 C 0.8856(3) 0.60944(16) 0.55280(14) 0.0271 1.0000 Uani . . . . . .
H121 H 0.8761 0.5693 0.5093 0.0429 1.0000 Uiso R . . . . .
H123 H 0.8388 0.6596 0.5343 0.0431 1.0000 Uiso R . . . . .
H122 H 0.9818 0.6217 0.5630 0.0426 1.0000 Uiso R . . . . .
C13 C 0.7395(2) 0.68907(15) 0.88622(14) 0.0238 1.0000 Uani . . . . . .
C14 C 0.7038(3) 0.60434(16) 0.91795(16) 0.0288 1.0000 Uani . . . . . .
H141 H 0.6640 0.6083 0.9710 0.0438 1.0000 Uiso R . . . . .
H143 H 0.6391 0.5781 0.8800 0.0436 1.0000 Uiso R . . . . .
H142 H 0.7838 0.5700 0.9235 0.0437 1.0000 Uiso R . . . . .
C15 C 0.6128(3) 0.74166(17) 0.87211(17) 0.0334 1.0000 Uani . . . . . .
H151 H 0.5618 0.7446 0.9211 0.0503 1.0000 Uiso R . . . . .
H153 H 0.6376 0.7970 0.8571 0.0510 1.0000 Uiso R . . . . .
H152 H 0.5571 0.7171 0.8274 0.0504 1.0000 Uiso R . . . . .
H131 H 0.7964 0.7175 0.9294 0.0303 1.0000 Uiso R . . . . .

_refine_ls_extinction_coef       37(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          3.72(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 . N2 5_756 2.1447(18) yes
Fe1 . N4 5_756 2.1428(18) yes
Fe1 . N1 5_756 2.3065(19) yes
Fe1 . N1 . 2.3065(19) yes
Fe1 . N2 . 2.1447(18) yes
Fe1 . N4 . 2.1428(18) yes
N1 . C3 . 1.475(3) yes
N1 . C4 . 1.477(3) yes
N1 . C5 . 1.479(3) yes
C3 . H33 . 0.962 no
C3 . H32 . 0.979 no
C3 . H31 . 0.964 no
C4 . C4 5_756 1.508(5) yes
C4 . H42 . 0.981 no
C4 . H41 . 0.976 no
C5 . H51 . 0.964 no
C5 . H53 . 0.972 no
C5 . H52 . 0.963 no
N2 . N3 . 1.315(3) yes
N2 . C13 . 1.479(3) yes
N3 . N4 . 1.311(3) yes
N4 . C9 . 1.479(3) yes
C9 . C10 . 1.531(3) yes
C9 . C11 . 1.536(3) yes
C9 . C12 . 1.528(3) yes
C10 . H101 . 0.975 no
C10 . H103 . 0.978 no
C10 . H102 . 0.982 no
C11 . H111 . 0.972 no
C11 . H113 . 0.963 no
C11 . H112 . 0.974 no
C12 . H121 . 0.969 no
C12 . H123 . 0.981 no
C12 . H122 . 0.978 no
C13 . C14 . 1.519(3) yes
C13 . C15 . 1.525(3) yes
C13 . H131 . 1.000 no
C14 . H141 . 0.971 no
C14 . H143 . 0.973 no
C14 . H142 . 0.968 no
C15 . H151 . 0.965 no
C15 . H153 . 0.967 no
C15 . H152 . 0.984 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 5_756 Fe1 . N4 5_756 59.83(7) yes
N2 5_756 Fe1 . N1 5_756 105.95(7) yes
N4 5_756 Fe1 . N1 5_756 162.45(7) yes
N2 5_756 Fe1 . N1 . 96.76(7) yes
N4 5_756 Fe1 . N1 . 91.49(7) yes
N1 5_756 Fe1 . N1 . 79.52(9) yes
N2 5_756 Fe1 . N2 . 150.42(10) yes
N4 5_756 Fe1 . N2 . 100.21(7) yes
N1 5_756 Fe1 . N2 . 96.76(7) yes
N1 . Fe1 . N2 . 105.95(7) yes
N2 5_756 Fe1 . N4 . 100.21(7) yes
N4 5_756 Fe1 . N4 . 100.86(10) yes
N1 5_756 Fe1 . N4 . 91.49(7) yes
N1 . Fe1 . N4 . 162.45(7) yes
N2 . Fe1 . N4 . 59.83(7) yes
Fe1 . N1 . C3 . 110.16(14) yes
Fe1 . N1 . C4 . 105.26(13) yes
C3 . N1 . C4 . 110.56(18) yes
Fe1 . N1 . C5 . 113.42(14) yes
C3 . N1 . C5 . 108.35(18) yes
C4 . N1 . C5 . 109.07(18) yes
N1 . C3 . H33 . 109.0 no
N1 . C3 . H32 . 109.5 no
H33 . C3 . H32 . 109.6 no
N1 . C3 . H31 . 110.2 no
H33 . C3 . H31 . 109.3 no
H32 . C3 . H31 . 109.1 no
C4 5_756 C4 . N1 . 111.61(16) yes
C4 5_756 C4 . H42 . 109.5 no
N1 . C4 . H42 . 110.4 no
C4 5_756 C4 . H41 . 109.0 no
N1 . C4 . H41 . 107.4 no
H42 . C4 . H41 . 108.8 no
N1 . C5 . H51 . 109.2 no
N1 . C5 . H53 . 110.6 no
H51 . C5 . H53 . 109.9 no
N1 . C5 . H52 . 109.8 no
H51 . C5 . H52 . 109.2 no
H53 . C5 . H52 . 108.1 no
Fe1 . N2 . N3 . 95.16(13) yes
Fe1 . N2 . C13 . 150.69(15) yes
N3 . N2 . C13 . 113.53(18) yes
N2 . N3 . N4 . 109.02(17) yes
Fe1 . N4 . N3 . 95.38(13) yes
Fe1 . N4 . C9 . 147.86(14) yes
N3 . N4 . C9 . 114.97(17) yes
N4 . C9 . C10 . 111.92(19) yes
N4 . C9 . C11 . 109.40(18) yes
C10 . C9 . C11 . 110.78(19) yes
N4 . C9 . C12 . 106.01(18) yes
C10 . C9 . C12 . 109.24(19) yes
C11 . C9 . C12 . 109.4(2) yes
C9 . C10 . H101 . 109.1 no
C9 . C10 . H103 . 109.9 no
H101 . C10 . H103 . 109.4 no
C9 . C10 . H102 . 109.8 no
H101 . C10 . H102 . 110.4 no
H103 . C10 . H102 . 108.4 no
C9 . C11 . H111 . 109.9 no
C9 . C11 . H113 . 109.3 no
H111 . C11 . H113 . 108.8 no
C9 . C11 . H112 . 109.7 no
H111 . C11 . H112 . 110.5 no
H113 . C11 . H112 . 108.6 no
C9 . C12 . H121 . 109.9 no
C9 . C12 . H123 . 111.4 no
H121 . C12 . H123 . 107.6 no
C9 . C12 . H122 . 109.7 no
H121 . C12 . H122 . 109.2 no
H123 . C12 . H122 . 109.1 no
N2 . C13 . C14 . 113.82(19) yes
N2 . C13 . C15 . 111.0(2) yes
C14 . C13 . C15 . 111.1(2) yes
N2 . C13 . H131 . 106.1 no
C14 . C13 . H131 . 108.0 no
C15 . C13 . H131 . 106.3 no
C13 . C14 . H141 . 110.7 no
C13 . C14 . H143 . 109.5 no
H141 . C14 . H143 . 109.0 no
C13 . C14 . H142 . 110.8 no
H141 . C14 . H142 . 108.2 no
H143 . C14 . H142 . 108.6 no
C13 . C15 . H151 . 110.7 no
C13 . C15 . H153 . 110.3 no
H151 . C15 . H153 . 108.1 no
C13 . C15 . H152 . 108.4 no
H151 . C15 . H152 . 110.2 no
H153 . C15 . H152 . 109.1 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_global_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1555087'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
_audit_creation_date             2016-07-26
_audit_creation_method           CRYSTALS_ver_14.61

_oxford_structure_analysis_title 'KSO_Fe2 in P2(1)2(1)2'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   19.6470(10)
_cell_length_b                   16.484(2)
_cell_length_c                   8.9926(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2912.4(5)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 2 '
_symmetry_space_group_name_Hall  'P 2 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,-y+1/2,-z
-x+1/2,y+1/2,-z
-x,-y,z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0311 0.0180 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe -1.1336 3.1974 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C24 H20 Fe1 N2 
# Dc =      1.02 Fooo =   1063.99 Mu =     42.86 M =    448.31
# Found Formula = C22 H52.00 Fe1 N877 
# Dc =      1.11 FOOO =   1063.99 Mu =     43.12 M =    484.55

_chemical_formula_sum            'C22 H52 Fe1 N8'
_chemical_formula_moiety         'C22 H52 Fe1 N8'
_chemical_compound_source        ?
_chemical_formula_weight         484.55


_cell_measurement_reflns_used    16768
_cell_measurement_theta_min      3.4420
_cell_measurement_theta_max      66.5330
_cell_measurement_temperature    250

_exptl_crystal_description       block
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_min          0.274
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_max          0.487

_exptl_crystal_density_diffrn    1.105
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1063.990
_exptl_absorpt_coefficient_mu    4.312

# Sheldrick geometric approximatio 0.23 0.31 
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_T_max  0.279
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      250
_diffrn_reflns_number            34851
_reflns_number_total             5157
_diffrn_reflns_av_R_equivalents  0.095
# Number of reflections without Friedels Law is 5157 
# Number of reflections with Friedels Law is 2937 
# Theoretical number of reflections is about 2598 

_diffrn_reflns_theta_min         3.500
_diffrn_reflns_theta_max         67.034
_diffrn_measured_fraction_theta_max 0.981

_diffrn_reflns_theta_full        67.034
_diffrn_measured_fraction_theta_full 0.981


_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_reflns_limit_h_min              -22
_reflns_limit_h_max              23
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              10

_oxford_diffrn_Wilson_B_factor   4.73
_oxford_diffrn_Wilson_scale      0.05

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.74
_refine_diff_density_max         1.03


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         4994
_refine_ls_number_restraints     175
_refine_ls_number_parameters     280
_oxford_refine_ls_R_factor_ref   0.1350
_refine_ls_wR_factor_ref         0.2574
_refine_ls_goodness_of_fit_ref   0.9885
_refine_ls_shift/su_max          0.0009659
_refine_ls_shift/su_mean         0.0001362


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4994
_refine_ls_R_factor_all          0.1350
_refine_ls_wR_factor_all         0.2574

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3806
_refine_ls_R_factor_gt           0.1143
_refine_ls_wR_factor_gt          0.2187

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration unk


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.294E+04 0.459E+04 0.240E+04 659. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 0.37414(6) 0.25024(9) 0.47883(13) 0.0493 1.0000 Uani . U . . . .
N1 N 0.4462(4) 0.3073(7) 0.3052(10) 0.0816 1.0000 Uani . U . . . .
C3 C 0.4952(6) 0.2470(12) 0.2513(13) 0.0998 1.0000 Uani . U . . . .
H31 H 0.5281 0.2355 0.3282 0.1490 1.0000 Uiso R . . . . .
H33 H 0.5184 0.2686 0.1655 0.1490 1.0000 Uiso R . . . . .
H32 H 0.4715 0.1977 0.2246 0.1490 1.0000 Uiso R . . . . .
C4 C 0.4032(7) 0.3306(12) 0.1751(15) 0.1179 1.0000 Uani . U . . . .
C5 C 0.3386(6) 0.3651(10) 0.2254(16) 0.1098 1.0000 Uani . U . . . .
N2 N 0.2981(4) 0.3092(6) 0.3197(11) 0.0772 1.0000 Uani . U . . . .
C7 C 0.2512(6) 0.3650(10) 0.3961(18) 0.1124 1.0000 Uani . U . . . .
H73 H 0.2325 0.3382 0.4815 0.1680 1.0000 Uiso R . . . . .
H72 H 0.2754 0.4129 0.4266 0.1681 1.0000 Uiso R . . . . .
H71 H 0.2153 0.3803 0.3280 0.1679 1.0000 Uiso R . . . . .
C8 C 0.2577(6) 0.2425(12) 0.2467(14) 0.1102 1.0000 Uani . U . . . .
H83 H 0.2312 0.2131 0.3200 0.1649 1.0000 Uiso R . . . . .
H82 H 0.2893 0.2062 0.1996 0.1651 1.0000 Uiso R . . . . .
H81 H 0.2279 0.2659 0.1737 0.1649 1.0000 Uiso R . . . . .
H52 H 0.3482 0.4149 0.2811 0.1320 1.0000 Uiso R . . . . .
H51 H 0.3116 0.3780 0.1368 0.1322 1.0000 Uiso R . . . . .
H42 H 0.4272 0.3701 0.1142 0.1420 1.0000 Uiso R . . . . .
H41 H 0.3933 0.2821 0.1171 0.1421 1.0000 Uiso R . . . . .
C9 C 0.4865(6) 0.3753(9) 0.3733(19) 0.1103 1.0000 Uani . U . . . .
H91 H 0.4566 0.4114 0.4254 0.1661 1.0000 Uiso R . . . . .
H93 H 0.5106 0.4048 0.2982 0.1659 1.0000 Uiso R . . . . .
H92 H 0.5188 0.3536 0.4433 0.1659 1.0000 Uiso R . . . . .
N3 N 0.4544(4) 0.2348(5) 0.6432(10) 0.0681 1.0000 Uani . . . . . .
N4 N 0.4360(5) 0.2984(5) 0.7262(11) 0.0811 1.0000 Uani . . . . . .
N5 N 0.3876(6) 0.3397(5) 0.6507(11) 0.0926 1.0000 Uani . . . . . .
C13 C 0.3655(8) 0.4050(6) 0.7477(15) 0.1044 1.0000 Uani D U . . . .
C14 C 0.3913(8) 0.4854(6) 0.6879(16) 0.1134 1.0000 Uani D U . . . .
C15 C 0.3680(8) 0.5563(7) 0.7880(16) 0.1190 1.0000 Uani D U . . . .
C16 C 0.4029(8) 0.5615(10) 0.9399(16) 0.1290 1.0000 Uani D U . . . .
H161 H 0.3968 0.6157 0.9776 0.1910 1.0000 Uiso R . . . . .
H163 H 0.4502 0.5496 0.9287 0.1911 1.0000 Uiso R . . . . .
H162 H 0.3821 0.5229 1.0058 0.1910 1.0000 Uiso R . . . . .
H151 H 0.3759 0.6073 0.7359 0.1421 1.0000 Uiso R . . . . .
H152 H 0.3195 0.5495 0.8069 0.1421 1.0000 Uiso R . . . . .
H142 H 0.4406 0.4832 0.6842 0.1362 1.0000 Uiso R . . . . .
H141 H 0.3728 0.4927 0.5878 0.1362 1.0000 Uiso R . . . . .
H132 H 0.3840 0.3976 0.8464 0.1243 1.0000 Uiso R . . . . .
H131 H 0.3161 0.4066 0.7517 0.1241 1.0000 Uiso R . . . . .
C17 C 0.5008(5) 0.1821(8) 0.7166(12) 0.0842 1.0000 Uani D U . . . .
C18 C 0.4673(6) 0.1344(10) 0.8431(15) 0.1094 1.0000 Uani D U . . . .
H181 H 0.4727 0.0771 0.8253 0.1631 1.0000 Uiso R . . . . .
H182 H 0.4892 0.1485 0.9351 0.1632 1.0000 Uiso R . . . . .
H183 H 0.4196 0.1478 0.8496 0.1630 1.0000 Uiso R . . . . .
C19 C 0.5375(9) 0.1264(11) 0.6065(19) 0.1460 1.0000 Uani D U . . . .
H191 H 0.5556 0.0793 0.6609 0.2190 1.0000 Uiso R . . . . .
H192 H 0.5747 0.1572 0.5594 0.2190 1.0000 Uiso R . . . . .
H193 H 0.5033 0.1096 0.5316 0.2190 1.0000 Uiso R . . . . .
C20 C 0.5616(8) 0.2283(11) 0.779(2) 0.1447 1.0000 Uani . U . . . .
H201 H 0.5931 0.1906 0.8236 0.2160 1.0000 Uiso R . . . . .
H202 H 0.5837 0.2572 0.6991 0.2160 1.0000 Uiso R . . . . .
H203 H 0.5454 0.2658 0.8535 0.2160 1.0000 Uiso R . . . . .
N8 N 0.2982(5) 0.1735(5) 0.5840(11) 0.0766 1.0000 Uani . . . . . .
N877 N 0.3164(6) 0.1064(6) 0.5120(14) 0.0991 1.0000 Uani . . . . . .
N6 N 0.3664(7) 0.1270(5) 0.4059(11) 0.0975 1.0000 Uani . . . . . .
C24 C 0.3930(9) 0.0552(9) 0.3364(19) 0.1417 1.0000 Uani D U . . . .
C25 C 0.3559(9) 0.0343(9) 0.193(2) 0.1517 1.0000 Uani D U . . . .
C26 C 0.3848(9) -0.0499(10) 0.144(2) 0.1581 1.0000 Uani D U . . . .
C27 C 0.3339(9) -0.0805(12) 0.031(2) 0.1838 1.0000 Uani D U . . . .
H273 H 0.3527 -0.1276 -0.0177 0.2761 1.0000 Uiso R . . . . .
H272 H 0.3260 -0.0381 -0.0413 0.2762 1.0000 Uiso R . . . . .
H271 H 0.2923 -0.0945 0.0817 0.2761 1.0000 Uiso R . . . . .
H262 H 0.4290 -0.0444 0.0993 0.1880 1.0000 Uiso R . . . . .
H261 H 0.3867 -0.0882 0.2257 0.1878 1.0000 Uiso R . . . . .
H252 H 0.3651 0.0758 0.1197 0.1801 1.0000 Uiso R . . . . .
H251 H 0.3073 0.0308 0.2110 0.1800 1.0000 Uiso R . . . . .
H242 H 0.4406 0.0639 0.3135 0.1679 1.0000 Uiso R . . . . .
H241 H 0.3882 0.0090 0.4028 0.1680 1.0000 Uiso R . . . . .
C28 C 0.2494(5) 0.1594(8) 0.6993(13) 0.0919 1.0000 Uani D U . . . .
C29 C 0.2741(8) 0.0863(11) 0.793(2) 0.1444 1.0000 Uani D U . . . .
H292 H 0.2382 0.0693 0.8603 0.2161 1.0000 Uiso R . . . . .
H291 H 0.3140 0.1019 0.8495 0.2160 1.0000 Uiso R . . . . .
H293 H 0.2854 0.0421 0.7267 0.2160 1.0000 Uiso R . . . . .
C30 C 0.1803(6) 0.1373(13) 0.6318(18) 0.1469 1.0000 Uani D U . . . .
H302 H 0.1474 0.1308 0.7109 0.2180 1.0000 Uiso R . . . . .
H301 H 0.1663 0.1806 0.5660 0.2180 1.0000 Uiso R . . . . .
H303 H 0.1849 0.0870 0.5776 0.2181 1.0000 Uiso R . . . . .
C31 C 0.2517(10) 0.2287(10) 0.8131(16) 0.1446 1.0000 Uani D U . . . .
H312 H 0.2358 0.2087 0.9085 0.2159 1.0000 Uiso R . . . . .
H311 H 0.2981 0.2480 0.8225 0.2162 1.0000 Uiso R . . . . .
H313 H 0.2227 0.2724 0.7786 0.2162 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          4.84(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 . N1 . 2.308(9) yes
Fe1 . N2 . 2.285(8) yes
Fe1 . N3 . 2.176(9) yes
Fe1 . N4 . 2.656(10) yes
Fe1 . N5 . 2.152(9) yes
Fe1 . N8 . 2.172(9) yes
Fe1 . N877 . 2.645(10) yes
Fe1 . N6 . 2.141(8) yes
N1 . C3 . 1.467(16) yes
N1 . C4 . 1.492(15) yes
N1 . C9 . 1.502(17) yes
C3 . H31 . 0.965 no
C3 . H33 . 0.965 no
C3 . H32 . 0.967 no
C4 . C5 . 1.464(18) yes
C4 . H42 . 0.972 no
C4 . H41 . 0.974 no
C5 . N2 . 1.484(15) yes
C5 . H52 . 0.981 no
C5 . H51 . 0.979 no
N2 . C7 . 1.472(16) yes
N2 . C8 . 1.506(17) yes
C7 . H73 . 0.959 no
C7 . H72 . 0.962 no
C7 . H71 . 0.968 no
C8 . H83 . 0.970 no
C8 . H82 . 0.960 no
C8 . H81 . 0.962 no
C9 . H91 . 0.959 no
C9 . H93 . 0.958 no
C9 . H92 . 0.963 no
N3 . N4 . 1.336(12) yes
N3 . C17 . 1.422(12) yes
N4 . N5 . 1.352(13) yes
N5 . C13 . 1.453(13) yes
C13 . C14 . 1.516(9) yes
C13 . H132 . 0.967 no
C13 . H131 . 0.971 no
C14 . C15 . 1.544(9) yes
C14 . H142 . 0.970 no
C14 . H141 . 0.979 no
C15 . C16 . 1.531(9) yes
C15 . H151 . 0.974 no
C15 . H152 . 0.975 no
C16 . H161 . 0.963 no
C16 . H163 . 0.957 no
C16 . H162 . 0.960 no
C17 . C18 . 1.532(9) yes
C17 . C19 . 1.531(9) yes
C17 . C20 . 1.525(18) yes
C18 . H181 . 0.963 no
C18 . H182 . 0.961 no
C18 . H183 . 0.963 no
C19 . H191 . 0.984 no
C19 . H192 . 0.986 no
C19 . H193 . 0.990 no
C20 . H201 . 0.964 no
C20 . H202 . 0.967 no
C20 . H203 . 0.964 no
N8 . N877 . 1.331(13) yes
N8 . C28 . 1.432(14) yes
N877 . N6 . 1.411(14) yes
N6 . C24 . 1.436(14) yes
C24 . C25 . 1.520(9) yes
C24 . H242 . 0.969 no
C24 . H241 . 0.972 no
C25 . C26 . 1.565(9) yes
C25 . H252 . 0.968 no
C25 . H251 . 0.969 no
C26 . C27 . 1.512(9) yes
C26 . H262 . 0.962 no
C26 . H261 . 0.969 no
C27 . H273 . 0.964 no
C27 . H272 . 0.965 no
C27 . H271 . 0.966 no
C28 . C29 . 1.550(9) yes
C28 . C30 . 1.529(9) yes
C28 . C31 . 1.534(9) yes
C29 . H292 . 0.967 no
C29 . H291 . 0.967 no
C29 . H293 . 0.970 no
C30 . H302 . 0.968 no
C30 . H301 . 0.968 no
C30 . H303 . 0.966 no
C31 . H312 . 0.971 no
C31 . H311 . 0.969 no
C31 . H313 . 0.970 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Fe1 . N2 . 78.7(3) yes
N1 . Fe1 . N3 . 93.6(3) yes
N2 . Fe1 . N3 . 161.5(3) yes
N1 . Fe1 . N4 . 99.5(3) yes
N2 . Fe1 . N4 . 134.1(3) yes
N3 . Fe1 . N4 . 30.1(3) yes
N1 . Fe1 . N5 . 97.5(4) yes
N2 . Fe1 . N5 . 103.8(4) yes
N3 . Fe1 . N5 . 60.2(4) yes
N4 . Fe1 . N5 . 30.4(3) yes
N1 . Fe1 . N8 . 162.4(4) yes
N2 . Fe1 . N8 . 94.1(4) yes
N3 . Fe1 . N8 . 97.7(3) yes
N4 . Fe1 . N8 . 97.1(4) yes
N5 . Fe1 . N8 . 99.8(4) yes
N1 . Fe1 . N877 . 134.8(4) yes
N2 . Fe1 . N877 . 99.9(4) yes
N3 . Fe1 . N877 . 97.4(3) yes
N4 . Fe1 . N877 . 111.7(3) yes
N5 . Fe1 . N877 . 125.9(4) yes
N1 . Fe1 . N6 . 102.9(4) yes
N2 . Fe1 . N6 . 99.5(4) yes
N3 . Fe1 . N6 . 98.5(4) yes
N4 . Fe1 . N6 . 124.9(4) yes
N5 . Fe1 . N6 . 151.5(4) yes
N8 . Fe1 . N877 . 30.1(3) yes
N8 . Fe1 . N6 . 62.1(4) yes
N877 . Fe1 . N6 . 32.1(3) yes
Fe1 . N1 . C3 . 110.5(8) yes
Fe1 . N1 . C4 . 106.8(7) yes
C3 . N1 . C4 . 106.6(10) yes
Fe1 . N1 . C9 . 110.6(8) yes
C3 . N1 . C9 . 107.1(10) yes
C4 . N1 . C9 . 115.2(12) yes
N1 . C3 . H31 . 109.7 no
N1 . C3 . H33 . 109.0 no
H31 . C3 . H33 . 109.2 no
N1 . C3 . H32 . 109.6 no
H31 . C3 . H32 . 109.6 no
H33 . C3 . H32 . 109.8 no
N1 . C4 . C5 . 110.4(11) yes
N1 . C4 . H42 . 109.9 no
C5 . C4 . H42 . 109.4 no
N1 . C4 . H41 . 108.8 no
C5 . C4 . H41 . 108.1 no
H42 . C4 . H41 . 110.2 no
C4 . C5 . N2 . 113.6(12) yes
C4 . C5 . H52 . 108.4 no
N2 . C5 . H52 . 109.4 no
C4 . C5 . H51 . 107.6 no
N2 . C5 . H51 . 108.1 no
H52 . C5 . H51 . 109.8 no
C5 . N2 . Fe1 . 105.8(6) yes
C5 . N2 . C7 . 102.3(10) yes
Fe1 . N2 . C7 . 112.5(8) yes
C5 . N2 . C8 . 119.1(11) yes
Fe1 . N2 . C8 . 107.9(8) yes
C7 . N2 . C8 . 109.3(10) yes
N2 . C7 . H73 . 109.0 no
N2 . C7 . H72 . 109.7 no
H73 . C7 . H72 . 109.8 no
N2 . C7 . H71 . 108.9 no
H73 . C7 . H71 . 110.3 no
H72 . C7 . H71 . 109.0 no
N2 . C8 . H83 . 110.6 no
N2 . C8 . H82 . 107.9 no
H83 . C8 . H82 . 109.6 no
N2 . C8 . H81 . 109.0 no
H83 . C8 . H81 . 109.7 no
H82 . C8 . H81 . 110.0 no
N1 . C9 . H91 . 109.8 no
N1 . C9 . H93 . 110.6 no
H91 . C9 . H93 . 109.4 no
N1 . C9 . H92 . 109.8 no
H91 . C9 . H92 . 108.3 no
H93 . C9 . H92 . 108.8 no
Fe1 . N3 . N4 . 95.3(6) yes
Fe1 . N3 . C17 . 148.3(8) yes
N4 . N3 . C17 . 113.2(9) yes
N3 . N4 . Fe1 . 54.7(5) yes
N3 . N4 . N5 . 107.8(8) yes
Fe1 . N4 . N5 . 53.7(5) yes
Fe1 . N5 . N4 . 95.8(6) yes
Fe1 . N5 . C13 . 154.5(11) yes
N4 . N5 . C13 . 106.4(10) yes
N5 . C13 . C14 . 109.5(10) yes
N5 . C13 . H132 . 110.2 no
C14 . C13 . H132 . 108.1 no
N5 . C13 . H131 . 109.9 no
C14 . C13 . H131 . 108.9 no
H132 . C13 . H131 . 110.3 no
C13 . C14 . C15 . 110.8(10) yes
C13 . C14 . H142 . 108.3 no
C15 . C14 . H142 . 110.1 no
C13 . C14 . H141 . 108.0 no
C15 . C14 . H141 . 109.4 no
H142 . C14 . H141 . 110.1 no
C14 . C15 . C16 . 115.5(12) yes
C14 . C15 . H151 . 109.0 no
C16 . C15 . H151 . 108.0 no
C14 . C15 . H152 . 107.7 no
C16 . C15 . H152 . 106.7 no
H151 . C15 . H152 . 109.8 no
C15 . C16 . H161 . 108.1 no
C15 . C16 . H163 . 109.2 no
H161 . C16 . H163 . 110.4 no
C15 . C16 . H162 . 108.9 no
H161 . C16 . H162 . 110.2 no
H163 . C16 . H162 . 110.0 no
N3 . C17 . C18 . 112.5(8) yes
N3 . C17 . C19 . 111.6(11) yes
C18 . C17 . C19 . 112.0(12) yes
N3 . C17 . C20 . 111.6(11) yes
C18 . C17 . C20 . 108.7(12) yes
C19 . C17 . C20 . 99.8(12) yes
C17 . C18 . H181 . 109.4 no
C17 . C18 . H182 . 108.8 no
H181 . C18 . H182 . 109.3 no
C17 . C18 . H183 . 110.2 no
H181 . C18 . H183 . 110.1 no
H182 . C18 . H183 . 109.1 no
C17 . C19 . H191 . 108.7 no
C17 . C19 . H192 . 108.5 no
H191 . C19 . H192 . 110.6 no
C17 . C19 . H193 . 106.8 no
H191 . C19 . H193 . 111.3 no
H192 . C19 . H193 . 110.7 no
C17 . C20 . H201 . 109.4 no
C17 . C20 . H202 . 108.9 no
H201 . C20 . H202 . 109.8 no
C17 . C20 . H203 . 108.5 no
H201 . C20 . H203 . 109.8 no
H202 . C20 . H203 . 110.4 no
Fe1 . N8 . N877 . 95.1(7) yes
Fe1 . N8 . C28 . 150.5(8) yes
N877 . N8 . C28 . 113.3(9) yes
N8 . N877 . Fe1 . 54.9(5) yes
N8 . N877 . N6 . 108.4(9) yes
Fe1 . N877 . N6 . 53.8(5) yes
Fe1 . N6 . N877 . 94.0(6) yes
Fe1 . N6 . C24 . 152.8(11) yes
N877 . N6 . C24 . 110.5(11) yes
N6 . C24 . C25 . 112.4(12) yes
N6 . C24 . H242 . 108.8 no
C25 . C24 . H242 . 108.5 no
N6 . C24 . H241 . 110.0 no
C25 . C24 . H241 . 107.3 no
H242 . C24 . H241 . 109.8 no
C24 . C25 . C26 . 105.5(11) yes
C24 . C25 . H252 . 109.2 no
C26 . C25 . H252 . 111.5 no
C24 . C25 . H251 . 110.2 no
C26 . C25 . H251 . 110.5 no
H252 . C25 . H251 . 109.8 no
C25 . C26 . C27 . 104.3(13) yes
C25 . C26 . H262 . 111.3 no
C27 . C26 . H262 . 110.4 no
C25 . C26 . H261 . 112.1 no
C27 . C26 . H261 . 108.7 no
H262 . C26 . H261 . 110.0 no
C26 . C27 . H273 . 108.6 no
C26 . C27 . H272 . 108.6 no
H273 . C27 . H272 . 110.0 no
C26 . C27 . H271 . 108.7 no
H273 . C27 . H271 . 110.3 no
H272 . C27 . H271 . 110.7 no
N8 . C28 . C29 . 108.2(10) yes
N8 . C28 . C30 . 110.3(10) yes
C29 . C28 . C30 . 108.0(12) yes
N8 . C28 . C31 . 109.9(9) yes
C29 . C28 . C31 . 101.8(13) yes
C30 . C28 . C31 . 117.9(14) yes
C28 . C29 . H292 . 109.6 no
C28 . C29 . H291 . 109.4 no
H292 . C29 . H291 . 110.1 no
C28 . C29 . H293 . 108.5 no
H292 . C29 . H293 . 109.5 no
H291 . C29 . H293 . 109.6 no
C28 . C30 . H302 . 109.2 no
C28 . C30 . H301 . 108.6 no
H302 . C30 . H301 . 109.8 no
C28 . C30 . H303 . 108.8 no
H302 . C30 . H303 . 109.8 no
H301 . C30 . H303 . 110.5 no
C28 . C31 . H312 . 109.1 no
C28 . C31 . H311 . 109.4 no
H312 . C31 . H311 . 109.7 no
C28 . C31 . H313 . 108.8 no
H312 . C31 . H313 . 110.3 no
H311 . C31 . H313 . 109.6 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_global_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1555088'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
_audit_creation_date             2016-01-19
_audit_creation_method           CRYSTALS_ver_14.61

_oxford_structure_analysis_title 'kso_a_046 in C 1 c 1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.6188(2)
_cell_length_b                   16.6011(2)
_cell_length_c                   18.2778(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.1363(18)
_cell_angle_gamma                90
_cell_volume                     2889.27(9)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C100 H100 Cl20 Fe10 N20 O20 
# Dc =      3.64 Fooo =   1064.00 Mu =     35.11 M =    792.39
# Found Formula = C44 H104 Fe2 N16 
# Dc =      1.11 FOOO =   1064.00 Mu =      5.44 M =    242.28

_chemical_formula_sum            'C22 H52 Fe N8'
_chemical_formula_moiety         'C22 H52 Fe N8'
_chemical_compound_source        ?
_chemical_formula_weight         484.57


_cell_measurement_reflns_used    8382
_cell_measurement_theta_min      3.9050
_cell_measurement_theta_max      28.6580
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_min          0.317
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_max          0.445

_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1064
_exptl_absorpt_coefficient_mu    0.544

# Sheldrick geometric approximatio 0.84 0.84 
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.810
_oxdiff_exptl_absorpt_empirical_full_max 1.174
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 15.9897
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            19548
_reflns_number_total             3556
_diffrn_reflns_av_R_equivalents  0.027
# Number of reflections without Friedels Law is 6740 
# Number of reflections with Friedels Law is 3556 
# Theoretical number of reflections is about 3890 


_diffrn_reflns_theta_min         3.129
_diffrn_reflns_theta_max         29.132
_diffrn_measured_fraction_theta_max 0.913

_diffrn_reflns_theta_full        25.053
_diffrn_measured_fraction_theta_full 0.982


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   2.55
_oxford_diffrn_Wilson_scale      0.85

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.45
_refine_diff_density_max         0.66


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3552
_refine_ls_number_restraints     0
_refine_ls_number_parameters     141
_oxford_refine_ls_R_factor_ref   0.0445
_refine_ls_wR_factor_ref         0.0652
_refine_ls_goodness_of_fit_ref   0.9754
_refine_ls_shift/su_max          0.0011502
_refine_ls_shift/su_mean         0.0000408


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3552
_refine_ls_R_factor_all          0.0445
_refine_ls_wR_factor_all         0.0652

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                3164
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_gt          0.0624

# The Flack parameter was determined before Friedel pairs were merged 
_refine_ls_abs_structure_Flack   .
_refine_ls_abs_structure_details 'Flack (1983), 3184 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 582. 842. 415. 104. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 0.5000 0.564927(19) 0.2500 0.0285 1.0000 Uani S T . . . .
N2 N 0.47016(16) 0.64315(8) 0.33587(7) 0.0330 1.0000 Uani . . . . . .
N3 N 0.59513(17) 0.64386(8) 0.37567(7) 0.0358 1.0000 Uani . . . . . .
N4 N 0.68014(15) 0.59461(8) 0.34959(7) 0.0304 1.0000 Uani . . . . . .
C5 C 0.8205(2) 0.59576(11) 0.39683(9) 0.0377 1.0000 Uani . . . . . .
C6 C 0.8822(3) 0.68092(13) 0.40181(12) 0.0604 1.0000 Uani . . . . . .
H61 H 0.9767 0.6803 0.4321 0.0890 1.0000 Uiso R . . . . .
H63 H 0.8231 0.7183 0.4234 0.0910 1.0000 Uiso R . . . . .
H62 H 0.8944 0.6992 0.3520 0.0902 1.0000 Uiso R . . . . .
C7 C 0.8079(2) 0.56597(15) 0.47484(10) 0.0522 1.0000 Uani . . . . . .
H71 H 0.9004 0.5677 0.5060 0.0763 1.0000 Uiso R . . . . .
H73 H 0.7416 0.5981 0.4970 0.0772 1.0000 Uiso R . . . . .
H72 H 0.7765 0.5108 0.4729 0.0765 1.0000 Uiso R . . . . .
C8 C 0.9156(2) 0.54015(14) 0.36095(11) 0.0510 1.0000 Uani . . . . . .
H81 H 1.0099 0.5391 0.3901 0.0756 1.0000 Uiso R . . . . .
H83 H 0.9268 0.5592 0.3113 0.0741 1.0000 Uiso R . . . . .
H82 H 0.8786 0.4864 0.3572 0.0751 1.0000 Uiso R . . . . .
C9 C 0.3726(3) 0.70091(12) 0.36336(11) 0.0522 1.0000 Uani . . . . . .
C10 C 0.3418(3) 0.67416(19) 0.44081(12) 0.0917 1.0000 Uani . . . . . .
H101 H 0.2687 0.7071 0.4578 0.1366 1.0000 Uiso R . . . . .
H103 H 0.4309 0.6833 0.4757 0.1362 1.0000 Uiso R . . . . .
H102 H 0.3200 0.6165 0.4404 0.1373 1.0000 Uiso R . . . . .
C11 C 0.4319(3) 0.78502(14) 0.36754(19) 0.0975 1.0000 Uani . . . . . .
H111 H 0.3659 0.8202 0.3844 0.1456 1.0000 Uiso R . . . . .
H112 H 0.5173 0.7838 0.4040 0.1447 1.0000 Uiso R . . . . .
H113 H 0.4487 0.7987 0.3141 0.1429 1.0000 Uiso R . . . . .
C12 C 0.2367(2) 0.69781(13) 0.31065(11) 0.0504 1.0000 Uani . . . . . .
H121 H 0.1706 0.7351 0.3272 0.0746 1.0000 Uiso R . . . . .
H122 H 0.2566 0.7128 0.2610 0.0746 1.0000 Uiso R . . . . .
H123 H 0.1954 0.6442 0.3085 0.0759 1.0000 Uiso R . . . . .
N1 N 0.58261(15) 0.45639(8) 0.18867(8) 0.0313 1.0000 Uani . . . . . .
C14 C 0.5688(2) 0.38526(10) 0.23536(11) 0.0423 1.0000 Uani . . . . . .
H141 H 0.5773 0.3364 0.2063 0.0504 1.0000 Uiso R . . . . .
H142 H 0.6464 0.3871 0.2768 0.0506 1.0000 Uiso R . . . . .
C15 C 0.7316(2) 0.46545(14) 0.17905(11) 0.0503 1.0000 Uani . . . . . .
H152 H 0.7459 0.5116 0.1478 0.0743 1.0000 Uiso R . . . . .
H151 H 0.7662 0.4172 0.1566 0.0740 1.0000 Uiso R . . . . .
H153 H 0.7867 0.4737 0.2273 0.0730 1.0000 Uiso R . . . . .
C16 C 0.5021(2) 0.44457(12) 0.11467(10) 0.0430 1.0000 Uani . . . . . .
H162 H 0.5093 0.4935 0.0849 0.0627 1.0000 Uiso R . . . . .
H161 H 0.4036 0.4346 0.1191 0.0634 1.0000 Uiso R . . . . .
H163 H 0.5375 0.4003 0.0884 0.0637 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          2.822(14)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 . N2 6_655 2.0880(13) yes
Fe1 . N1 6_655 2.3209(14) yes
Fe1 . N4 6_655 2.3803(13) yes
Fe1 . N2 . 2.0880(13) yes
Fe1 . N4 . 2.3803(13) yes
Fe1 . N1 . 2.3209(14) yes
N2 . N3 . 1.314(2) yes
N2 . C9 . 1.478(2) yes
N3 . N4 . 1.294(2) yes
N4 . C5 . 1.496(2) yes
C5 . C6 . 1.531(3) yes
C5 . C7 . 1.530(2) yes
C5 . C8 . 1.513(3) yes
C6 . H61 . 0.995 no
C6 . H63 . 0.963 no
C6 . H62 . 0.982 no
C7 . H71 . 0.987 no
C7 . H73 . 0.964 no
C7 . H72 . 0.963 no
C8 . H81 . 0.984 no
C8 . H83 . 0.982 no
C8 . H82 . 0.960 no
C9 . C10 . 1.552(3) yes
C9 . C11 . 1.506(3) yes
C9 . C12 . 1.511(3) yes
C10 . H101 . 0.977 no
C10 . H103 . 1.005 no
C10 . H102 . 0.981 no
C11 . H111 . 0.945 no
C11 . H112 . 0.983 no
C11 . H113 . 1.037 no
C12 . H121 . 0.966 no
C12 . H122 . 0.986 no
C12 . H123 . 0.973 no
N1 . C14 . 1.474(2) yes
N1 . C15 . 1.476(2) yes
N1 . C16 . 1.474(2) yes
C14 . C14 6_655 1.496(4) yes
C14 . H141 . 0.980 no
C14 . H142 . 0.986 no
C15 . H152 . 0.977 no
C15 . H151 . 0.979 no
C15 . H153 . 0.972 no
C16 . H162 . 0.985 no
C16 . H161 . 0.976 no
C16 . H163 . 0.966 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 6_655 Fe1 . N1 6_655 159.85(5) yes
N2 6_655 Fe1 . N4 6_655 57.25(5) yes
N1 6_655 Fe1 . N4 6_655 105.56(5) yes
N2 6_655 Fe1 . N2 . 103.09(8) yes
N1 6_655 Fe1 . N2 . 91.54(5) yes
N4 6_655 Fe1 . N2 . 106.47(5) yes
N2 6_655 Fe1 . N4 . 106.47(5) yes
N1 6_655 Fe1 . N4 . 93.05(5) yes
N4 6_655 Fe1 . N4 . 156.10(7) yes
N2 . Fe1 . N4 . 57.25(5) yes
N2 6_655 Fe1 . N1 . 91.54(5) yes
N1 6_655 Fe1 . N1 . 78.15(7) yes
N4 6_655 Fe1 . N1 . 93.05(5) yes
N2 . Fe1 . N1 . 159.85(5) yes
N4 . Fe1 . N1 . 105.56(5) yes
Fe1 . N2 . N3 . 102.08(11) yes
Fe1 . N2 . C9 . 145.11(12) yes
N3 . N2 . C9 . 112.39(14) yes
N2 . N3 . N4 . 111.51(13) yes
Fe1 . N4 . N3 . 89.02(10) yes
Fe1 . N4 . C5 . 160.67(12) yes
N3 . N4 . C5 . 110.19(13) yes
N4 . C5 . C6 . 110.88(16) yes
N4 . C5 . C7 . 110.46(15) yes
C6 . C5 . C7 . 108.91(17) yes
N4 . C5 . C8 . 107.10(14) yes
C6 . C5 . C8 . 109.64(18) yes
C7 . C5 . C8 . 109.82(17) yes
C5 . C6 . H61 . 109.8 no
C5 . C6 . H63 . 112.0 no
H61 . C6 . H63 . 108.9 no
C5 . C6 . H62 . 109.1 no
H61 . C6 . H62 . 107.4 no
H63 . C6 . H62 . 109.5 no
C5 . C7 . H71 . 110.2 no
C5 . C7 . H73 . 110.9 no
H71 . C7 . H73 . 109.7 no
C5 . C7 . H72 . 109.7 no
H71 . C7 . H72 . 107.5 no
H73 . C7 . H72 . 108.7 no
C5 . C8 . H81 . 110.1 no
C5 . C8 . H83 . 110.9 no
H81 . C8 . H83 . 107.0 no
C5 . C8 . H82 . 110.9 no
H81 . C8 . H82 . 109.1 no
H83 . C8 . H82 . 108.7 no
N2 . C9 . C10 . 109.67(16) yes
N2 . C9 . C11 . 111.4(2) yes
C10 . C9 . C11 . 109.8(2) yes
N2 . C9 . C12 . 107.13(15) yes
C10 . C9 . C12 . 108.2(2) yes
C11 . C9 . C12 . 110.54(19) yes
C9 . C10 . H101 . 111.7 no
C9 . C10 . H103 . 106.3 no
H101 . C10 . H103 . 107.5 no
C9 . C10 . H102 . 110.0 no
H101 . C10 . H102 . 112.7 no
H103 . C10 . H102 . 108.4 no
C9 . C11 . H111 . 108.8 no
C9 . C11 . H112 . 106.8 no
H111 . C11 . H112 . 109.1 no
C9 . C11 . H113 . 105.3 no
H111 . C11 . H113 . 111.9 no
H112 . C11 . H113 . 114.6 no
C9 . C12 . H121 . 109.1 no
C9 . C12 . H122 . 108.4 no
H121 . C12 . H122 . 110.4 no
C9 . C12 . H123 . 111.6 no
H121 . C12 . H123 . 108.3 no
H122 . C12 . H123 . 109.0 no
Fe1 . N1 . C14 . 106.09(10) yes
Fe1 . N1 . C15 . 112.52(11) yes
C14 . N1 . C15 . 108.62(15) yes
Fe1 . N1 . C16 . 112.04(10) yes
C14 . N1 . C16 . 110.25(14) yes
C15 . N1 . C16 . 107.30(14) yes
C14 6_655 C14 . N1 . 111.34(14) yes
C14 6_655 C14 . H141 . 109.8 no
N1 . C14 . H141 . 109.2 no
C14 6_655 C14 . H142 . 109.7 no
N1 . C14 . H142 . 107.4 no
H141 . C14 . H142 . 109.2 no
N1 . C15 . H152 . 111.7 no
N1 . C15 . H151 . 111.1 no
H152 . C15 . H151 . 108.2 no
N1 . C15 . H153 . 108.7 no
H152 . C15 . H153 . 108.5 no
H151 . C15 . H153 . 108.7 no
N1 . C16 . H162 . 109.2 no
N1 . C16 . H161 . 109.7 no
H162 . C16 . H161 . 109.3 no
N1 . C16 . H163 . 112.4 no
H162 . C16 . H163 . 107.1 no
H161 . C16 . H163 . 109.1 no


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_global_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1555085'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
_audit_creation_date             2016-10-12
_audit_creation_method           CRYSTALS_ver_14.61

_oxford_structure_analysis_title 'SIR2014 run in space group P n a 21'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   17.6602(3)
_cell_length_b                   8.9362(2)
_cell_length_c                   15.8756(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2505.41(8)

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21 '
_symmetry_space_group_name_Hall  'P 2c -2n'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,z
-x,-y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C12.50 H12.50 Fe1.25 N20 O5 
# Dc =      1.57 Fooo =    936.00 Mu =      8.09 M =    592.68
# Found Formula = C18 H44 Fe1 N8 
# Dc =      1.14 FOOO =    936.00 Mu =      6.20 M =    428.45

_chemical_formula_sum            'C18 H44 Fe1 N8'
_chemical_formula_moiety         'C18 H44 Fe1 N8'
_chemical_compound_source        ?
_chemical_formula_weight         428.45


_cell_measurement_reflns_used    10493
_cell_measurement_theta_min      4.1090
_cell_measurement_theta_max      27.3970
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_min          0.233
_exptl_crystal_size_mid          0.392
_exptl_crystal_size_max          0.574

_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             936.000
_exptl_absorpt_coefficient_mu    0.620

# Sheldrick geometric approximatio 0.78 0.87 
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.700
_oxdiff_exptl_absorpt_empirical_full_max 1.432
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 15.9897
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            33283
_reflns_number_total             6225
_diffrn_reflns_av_R_equivalents  0.041
# Number of reflections without Friedels Law is 6225 
# Number of reflections with Friedels Law is 3366 
# Theoretical number of reflections is about 3538 


_diffrn_reflns_theta_min         2.859
_diffrn_reflns_theta_max         29.647
_diffrn_measured_fraction_theta_max 0.919

_diffrn_reflns_theta_full        26.720
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              0
_reflns_limit_h_max              24
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              -21
_reflns_limit_l_max              21

_oxford_diffrn_Wilson_B_factor   2.56
_oxford_diffrn_Wilson_scale      0.04

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.59
_refine_diff_density_max         0.65


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     521
_refine_ls_number_parameters     381
_oxford_refine_ls_R_factor_ref   0.0688
_refine_ls_wR_factor_ref         0.1271
_refine_ls_goodness_of_fit_ref   0.9578
_refine_ls_shift/su_max          0.0004046
_refine_ls_shift/su_mean         0.0000227


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        6216
_refine_ls_R_factor_all          0.0688
_refine_ls_wR_factor_all         0.1271

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5274
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_gt          0.1162

_refine_ls_abs_structure_Flack   0.32(3)
_refine_ls_abs_structure_details 'Flack (1983), 2859 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.207E+04 0.316E+04 0.174E+04 624. 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 0.39573(3) 0.41979(5) 0.49935(13) 0.0312 1.0000 Uani . U . . . .
N2 N 0.2958(2) 0.2582(5) 0.4944(4) 0.0649 1.0000 Uani D U . . . .
C3 C 0.2884(6) 0.1774(10) 0.5736(5) 0.1161 1.0000 Uani D U . . . .
C4 C 0.2238(3) 0.3402(9) 0.4784(5) 0.0979 1.0000 Uani D U . . . .
C5 C 0.3060(3) 0.1640(9) 0.4211(5) 0.0870 1.0000 Uani D U . . . .
C6 C 0.3873(3) 0.1177(7) 0.4113(5) 0.0853 1.0000 Uani D U . . . .
N1 N 0.4361(2) 0.2513(5) 0.4022(3) 0.0500 1.0000 Uani . U . . . .
C8 C 0.5149(3) 0.2053(6) 0.4203(5) 0.0690 1.0000 Uani . U . . . .
C9 C 0.4347(4) 0.3187(9) 0.3176(4) 0.0742 1.0000 Uani . U . . . .
N8 N 0.4754(3) 0.5884(6) 0.4622(4) 0.0408 0.644(3) Uani D U P 1 1 .
N12 N 0.5017(5) 0.5312(10) 0.5111(6) 0.0417 0.356(3) Uani D U P 1 2 .
C12 C 0.5473(2) 0.6668(5) 0.4810(3) 0.0612 1.0000 Uani D U . . . .
C13 C 0.6030(5) 0.5642(10) 0.5266(8) 0.1251 0.644(3) Uani D U P 1 1 .
C14 C 0.6213(8) 0.6092(16) 0.4407(13) 0.0978 0.356(3) Uani D U P 1 2 .
C15 C 0.5797(8) 0.7409(18) 0.4015(7) 0.1562 0.644(3) Uani D U P 1 1 .
N13 N 0.5270(6) 0.4589(13) 0.5771(7) 0.0600 0.356(3) Uani D U P 1 2 .
N14 N 0.4781(7) 0.3541(14) 0.5964(8) 0.0577 0.356(3) Uani D U P 1 2 .
N3 N 0.4392(5) 0.3341(9) 0.6149(4) 0.0637 0.644(3) Uani D U P 1 1 .
C19 C 0.5016(5) 0.2751(9) 0.6684(5) 0.0928 1.0000 Uani D U . . . .
C20 C 0.4751(10) 0.1163(14) 0.6904(11) 0.0883 0.356(3) Uani D U P 1 2 .
C21 C 0.5503(9) 0.1393(15) 0.6622(10) 0.1486 0.644(3) Uani D U P 1 1 .
N4 N 0.4068(4) 0.4355(8) 0.6623(4) 0.0693 0.644(3) Uani D U P 1 1 .
N5 N 0.3612(3) 0.5159(7) 0.6156(3) 0.0447 0.644(3) Uani D U P 1 1 .
N9 N 0.3290(7) 0.5661(13) 0.5720(7) 0.0457 0.356(3) Uani D U P 1 2 .
C25 C 0.3158(3) 0.6307(6) 0.6598(3) 0.0598 1.0000 Uani D U . . . .
C26 C 0.2870(6) 0.7420(11) 0.5984(6) 0.0870 0.644(3) Uani D U P 1 1 .
C27 C 0.2291(5) 0.646(3) 0.6706(11) 0.1058 0.356(3) Uani D U P 1 2 .
C28 C 0.2483(6) 0.5511(14) 0.7025(9) 0.1127 0.644(3) Uani D U P 1 1 .
C29 C 0.3497(10) 0.5327(17) 0.7291(7) 0.0801 0.356(3) Uani D U P 1 2 .
C30 C 0.3654(6) 0.7072(13) 0.7267(6) 0.0938 0.644(3) Uani D U P 1 1 .
C31 C 0.3526(11) 0.7886(13) 0.6623(11) 0.1032 0.356(3) Uani D U P 1 2 .
N10 N 0.3069(5) 0.6465(10) 0.5076(6) 0.0494 0.356(3) Uani D U P 1 2 .
N11 N 0.3299(8) 0.5802(14) 0.4386(6) 0.0421 0.356(3) Uani D U P 1 2 .
N7 N 0.4276(3) 0.6696(6) 0.4187(4) 0.0433 0.644(3) Uani D U P 1 1 .
N6 N 0.3646(3) 0.5935(6) 0.4114(4) 0.0385 0.644(3) Uani D U P 1 1 .
C36 C 0.3115(7) 0.6811(15) 0.3608(8) 0.0564 0.644(3) Uani D U P 1 1 .
C37 C 0.2959(12) 0.669(3) 0.3695(11) 0.0512 0.356(3) Uani D U P 1 2 .
C38 C 0.2982(11) 0.613(3) 0.2785(12) 0.0705 0.356(3) Uani D U P 1 2 .
C39 C 0.2613(9) 0.601(2) 0.2976(9) 0.1051 0.644(3) Uani D U P 1 1 .
C40 C 0.5628(10) 0.7767(19) 0.5534(10) 0.0943 0.356(3) Uani D U P 1 2 .
C41 C 0.5302(6) 0.7989(11) 0.5383(7) 0.0900 0.644(3) Uani D U P 1 1 .
C42 C 0.5010(9) 0.747(2) 0.4144(11) 0.1036 0.356(3) Uani D U P 1 2 .
H31 H 0.3331 0.1188 0.5844 0.1741 1.0000 Uiso R . . . . .
H32 H 0.2814 0.2518 0.6179 0.1740 1.0000 Uiso R . . . . .
H33 H 0.2447 0.1125 0.5699 0.1739 1.0000 Uiso R . . . . .
H41 H 0.2295 0.4072 0.4310 0.1519 1.0000 Uiso R . . . . .
H42 H 0.2103 0.3990 0.5265 0.1519 1.0000 Uiso R . . . . .
H43 H 0.1838 0.2701 0.4669 0.1521 1.0000 Uiso R . . . . .
H51 H 0.2752 0.0740 0.4269 0.0998 1.0000 Uiso R . . . . .
H52 H 0.2916 0.2187 0.3703 0.1004 1.0000 Uiso R . . . . .
H61 H 0.4019 0.0649 0.4639 0.0996 1.0000 Uiso R . . . . .
H62 H 0.3930 0.0513 0.3634 0.1002 1.0000 Uiso R . . . . .
H81 H 0.5496 0.2873 0.4138 0.1037 1.0000 Uiso R . . . . .
H82 H 0.5163 0.1646 0.4761 0.1039 1.0000 Uiso R . . . . .
H83 H 0.5270 0.1296 0.3807 0.1039 1.0000 Uiso R . . . . .
H91 H 0.4688 0.4036 0.3153 0.1088 1.0000 Uiso R . . . . .
H92 H 0.4491 0.2422 0.2766 0.1091 1.0000 Uiso R . . . . .
H93 H 0.3838 0.3542 0.3076 0.1091 1.0000 Uiso R . . . . .
H141 H 0.6549 0.6907 0.4273 0.1701 0.356(3) Uiso R . P 1 2 .
H142 H 0.6437 0.5483 0.4837 0.1700 0.356(3) Uiso R . P 1 2 .
H143 H 0.6123 0.5491 0.3909 0.1698 0.356(3) Uiso R . P 1 2 .
H151 H 0.6203 0.8104 0.4174 0.2079 0.644(3) Uiso R . P 1 1 .
H152 H 0.5423 0.7932 0.3675 0.2081 0.644(3) Uiso R . P 1 1 .
H153 H 0.6003 0.6544 0.3707 0.2080 0.644(3) Uiso R . P 1 1 .
H201 H 0.5100 0.0788 0.7368 0.1570 0.356(3) Uiso R . P 1 2 .
H202 H 0.4205 0.1215 0.7108 0.1569 0.356(3) Uiso R . P 1 2 .
H203 H 0.4798 0.0535 0.6376 0.1571 0.356(3) Uiso R . P 1 2 .
H211 H 0.5796 0.1312 0.7132 0.1561 0.644(3) Uiso R . P 1 1 .
H212 H 0.5834 0.1556 0.6148 0.1561 0.644(3) Uiso R . P 1 1 .
H213 H 0.5200 0.0502 0.6545 0.1562 0.644(3) Uiso R . P 1 1 .
H271 H 0.2199 0.7195 0.7153 0.1879 0.356(3) Uiso R . P 1 2 .
H272 H 0.2076 0.6811 0.6174 0.1881 0.356(3) Uiso R . P 1 2 .
H273 H 0.2082 0.5493 0.6861 0.1880 0.356(3) Uiso R . P 1 2 .
H281 H 0.2327 0.6053 0.7515 0.1359 0.644(3) Uiso R . P 1 1 .
H282 H 0.2634 0.4520 0.7184 0.1358 0.644(3) Uiso R . P 1 1 .
H283 H 0.2066 0.5446 0.6640 0.1359 0.644(3) Uiso R . P 1 1 .
H291 H 0.3884 0.5950 0.7626 0.1700 0.356(3) Uiso R . P 1 2 .
H292 H 0.3747 0.4410 0.6987 0.1701 0.356(3) Uiso R . P 1 2 .
H293 H 0.3039 0.5015 0.7662 0.1700 0.356(3) Uiso R . P 1 2 .
H301 H 0.3348 0.7806 0.7558 0.1099 0.644(3) Uiso R . P 1 1 .
H302 H 0.3827 0.6320 0.7659 0.1101 0.644(3) Uiso R . P 1 1 .
H303 H 0.4087 0.7554 0.7001 0.1099 0.644(3) Uiso R . P 1 1 .
H311 H 0.3355 0.8363 0.7145 0.2030 0.356(3) Uiso R . P 1 2 .
H312 H 0.4080 0.7755 0.6629 0.2029 0.356(3) Uiso R . P 1 2 .
H313 H 0.3373 0.8485 0.6139 0.2030 0.356(3) Uiso R . P 1 2 .
H361 H 0.3350 0.7670 0.3355 0.0634 0.644(3) Uiso R . P 1 1 .
H362 H 0.2784 0.7137 0.4047 0.0633 0.644(3) Uiso R . P 1 1 .
H371 H 0.3217 0.7621 0.3608 0.0842 0.356(3) Uiso R . P 1 2 .
H372 H 0.2450 0.6881 0.3880 0.0841 0.356(3) Uiso R . P 1 2 .
H381 H 0.2530 0.6518 0.2509 0.1230 0.356(3) Uiso R . P 1 2 .
H382 H 0.3425 0.6359 0.2440 0.1230 0.356(3) Uiso R . P 1 2 .
H383 H 0.2932 0.5042 0.2873 0.1228 0.356(3) Uiso R . P 1 2 .
H391 H 0.2353 0.6795 0.2675 0.1310 0.644(3) Uiso R . P 1 1 .
H392 H 0.2923 0.5456 0.2588 0.1311 0.644(3) Uiso R . P 1 1 .
H393 H 0.2250 0.5349 0.3234 0.1308 0.644(3) Uiso R . P 1 1 .
H411 H 0.5527 0.8844 0.5120 0.1111 0.644(3) Uiso R . P 1 1 .
H412 H 0.5506 0.7871 0.5937 0.1111 0.644(3) Uiso R . P 1 1 .
H413 H 0.4761 0.8121 0.5409 0.1109 0.644(3) Uiso R . P 1 1 .
H421 H 0.5137 0.8521 0.4158 0.1890 0.356(3) Uiso R . P 1 2 .
H422 H 0.4466 0.7315 0.4218 0.1889 0.356(3) Uiso R . P 1 2 .
H423 H 0.5171 0.7023 0.3621 0.1891 0.356(3) Uiso R . P 1 2 .
H191 H 0.4933 0.3353 0.7184 0.1041 0.356(3) Uiso R . P 1 2 .
H192 H 0.5555 0.2700 0.6568 0.1037 0.356(3) Uiso R . P 1 2 .
H193 H 0.5358 0.3604 0.6721 0.1041 0.644(3) Uiso R . P 1 1 .
H194 H 0.4785 0.2573 0.7230 0.1041 0.644(3) Uiso R . P 1 1 .
H131 H 0.6484 0.6162 0.5396 0.1311 0.644(3) Uiso R . P 1 1 .
H132 H 0.5808 0.5274 0.5770 0.1311 0.644(3) Uiso R . P 1 1 .
H133 H 0.6141 0.4829 0.4901 0.1311 0.644(3) Uiso R . P 1 1 .
H401 H 0.5936 0.8565 0.5337 0.1219 0.356(3) Uiso R . P 1 2 .
H402 H 0.5870 0.7291 0.5996 0.1219 0.356(3) Uiso R . P 1 2 .
H403 H 0.5152 0.8149 0.5710 0.1219 0.356(3) Uiso R . P 1 2 .
H261 H 0.2580 0.8162 0.6267 0.0825 0.644(3) Uiso R . P 1 1 .
H262 H 0.3286 0.7879 0.5708 0.0825 0.644(3) Uiso R . P 1 1 .
H263 H 0.2561 0.6926 0.5581 0.0825 0.644(3) Uiso R . P 1 1 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          6.41(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 . N2 . 2.281(3) yes
Fe1 . N1 . 2.270(4) yes
Fe1 . N8 . 2.144(5) yes
Fe1 . N3 . 2.131(7) yes
Fe1 . N5 . 2.125(6) yes
Fe1 . N6 . 2.159(6) yes
Fe1 . N2 . 2.281(3) yes
Fe1 . N1 . 2.270(4) yes
Fe1 . N12 . 2.128(9) yes
Fe1 . N14 . 2.199(12) yes
Fe1 . N9 . 2.104(12) yes
Fe1 . N11 . 2.083(12) yes
N2 . C3 . 1.457(7) yes
N2 . C4 . 1.490(6) yes
N2 . C5 . 1.447(6) yes
C3 . H31 . 0.963 no
C3 . H32 . 0.975 no
C3 . H33 . 0.967 no
C4 . H41 . 0.967 no
C4 . H42 . 0.956 no
C4 . H43 . 0.961 no
C5 . C6 . 1.503(5) yes
C5 . H51 . 0.975 no
C5 . H52 . 0.976 no
C6 . N1 . 1.479(7) yes
C6 . H61 . 0.992 no
C6 . H62 . 0.970 no
N1 . C8 . 1.479(7) yes
N1 . C9 . 1.472(8) yes
C8 . H81 . 0.961 no
C8 . H82 . 0.957 no
C8 . H83 . 0.948 no
C9 . H91 . 0.969 no
C9 . H92 . 0.978 no
C9 . H93 . 0.967 no
N8 . C12 . 1.482(6) yes
N8 . N7 . 1.3094(11) yes
N12 . C12 . 1.532(10) yes
N12 . N13 . 1.3100(11) yes
C12 . C13 . 1.527(5) yes
C12 . C15 . 1.536(9) yes
C12 . C41 . 1.520(8) yes
C12 . C14 . 1.543(9) yes
C12 . C40 . 1.537(10) yes
C12 . C42 . 1.516(10) yes
C13 . H131 . 0.950 no
C13 . H132 . 0.950 no
C13 . H133 . 0.950 no
C14 . H141 . 0.964 no
C14 . H142 . 0.958 no
C14 . H143 . 0.969 no
C15 . H151 . 0.982 no
C15 . H152 . 0.972 no
C15 . H153 . 0.984 no
N13 . N14 . 1.3100(11) yes
N14 . C19 . 1.406(13) yes
N3 . C19 . 1.488(9) yes
N3 . N4 . 1.3099(11) yes
C19 . C21 . 1.491(7) yes
C19 . H193 . 0.974 no
C19 . H194 . 0.971 no
C19 . C20 . 1.535(10) yes
C19 . H191 . 0.970 no
C19 . H192 . 0.971 no
C20 . H201 . 1.017 no
C20 . H202 . 1.018 no
C20 . H203 . 1.012 no
C21 . H211 . 0.963 no
C21 . H212 . 0.965 no
C21 . H213 . 0.967 no
N4 . N5 . 1.3096(11) yes
N5 . C25 . 1.479(7) yes
N9 . C25 . 1.527(12) yes
N9 . N10 . 1.3100(11) yes
C25 . C26 . 1.482(8) yes
C25 . C28 . 1.546(6) yes
C25 . C30 . 1.536(6) yes
C25 . C27 . 1.547(7) yes
C25 . C29 . 1.528(7) yes
C25 . C31 . 1.554(7) yes
C26 . H261 . 0.950 no
C26 . H262 . 0.950 no
C26 . H263 . 0.950 no
C27 . H271 . 0.978 no
C27 . H272 . 0.978 no
C27 . H273 . 0.974 no
C28 . H281 . 0.956 no
C28 . H282 . 0.959 no
C28 . H283 . 0.958 no
C29 . H291 . 1.030 no
C29 . H292 . 1.049 no
C29 . H293 . 1.038 no
C30 . H301 . 0.969 no
C30 . H302 . 0.965 no
C30 . H303 . 0.973 no
C31 . H311 . 0.980 no
C31 . H312 . 0.984 no
C31 . H313 . 0.975 no
N10 . N11 . 1.3099(11) yes
N11 . C37 . 1.480(10) yes
N7 . N6 . 1.3097(11) yes
N6 . C36 . 1.462(8) yes
C36 . C39 . 1.516(9) yes
C36 . H361 . 0.961 no
C36 . H362 . 0.955 no
C37 . C38 . 1.529(10) yes
C37 . H371 . 0.960 no
C37 . H372 . 0.960 no
C38 . H381 . 0.975 no
C38 . H382 . 0.978 no
C38 . H383 . 0.984 no
C39 . H391 . 0.963 no
C39 . H392 . 0.963 no
C39 . H393 . 0.964 no
C40 . H401 . 0.950 no
C40 . H402 . 0.950 no
C40 . H403 . 0.950 no
C41 . H411 . 0.957 no
C41 . H412 . 0.957 no
C41 . H413 . 0.963 no
C42 . H421 . 0.968 no
C42 . H422 . 0.977 no
C42 . H423 . 0.963 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 . Fe1 . N1 . 78.43(17) yes
N2 . Fe1 . N8 . 160.5(2) yes
N1 . Fe1 . N8 . 94.19(18) yes
N2 . Fe1 . N3 . 94.7(3) yes
N1 . Fe1 . N3 . 103.5(2) yes
N8 . Fe1 . N3 . 104.7(3) yes
N2 . Fe1 . N5 . 93.7(2) yes
N1 . Fe1 . N5 . 161.5(2) yes
N8 . Fe1 . N5 . 98.3(2) yes
N3 . Fe1 . N5 . 60.07(18) yes
N2 . Fe1 . N6 . 103.61(18) yes
N1 . Fe1 . N6 . 96.7(2) yes
N8 . Fe1 . N6 . 58.94(16) yes
N3 . Fe1 . N6 . 155.1(3) yes
N5 . Fe1 . N6 . 101.4(3) yes
N2 . Fe1 . N1 . 78.43(17) yes
N2 . Fe1 . N12 . 168.3(3) yes
N1 . Fe1 . N12 . 95.4(3) yes
N2 . Fe1 . N14 . 111.5(3) yes
N1 . Fe1 . N14 . 95.2(4) yes
N12 . Fe1 . N14 . 58.8(3) yes
N2 . Fe1 . N9 . 88.8(4) yes
N1 . Fe1 . N9 . 163.8(4) yes
N12 . Fe1 . N9 . 98.8(4) yes
N14 . Fe1 . N9 . 98.8(5) yes
N2 . Fe1 . N11 . 89.3(4) yes
N1 . Fe1 . N11 . 108.5(3) yes
N12 . Fe1 . N11 . 102.1(5) yes
N14 . Fe1 . N11 . 151.4(5) yes
N9 . Fe1 . N11 . 60.9(2) yes
Fe1 . N2 . C3 . 110.7(5) yes
Fe1 . N2 . C4 . 110.8(3) yes
C3 . N2 . C4 . 108.2(6) yes
Fe1 . N2 . C5 . 107.5(3) yes
C3 . N2 . C5 . 114.6(5) yes
C4 . N2 . C5 . 104.8(6) yes
N2 . C3 . H31 . 110.5 no
N2 . C3 . H32 . 107.2 no
H31 . C3 . H32 . 110.2 no
N2 . C3 . H33 . 108.5 no
H31 . C3 . H33 . 109.8 no
H32 . C3 . H33 . 110.6 no
N2 . C4 . H41 . 110.2 no
N2 . C4 . H42 . 110.3 no
H41 . C4 . H42 . 107.9 no
N2 . C4 . H43 . 109.8 no
H41 . C4 . H43 . 109.5 no
H42 . C4 . H43 . 109.1 no
N2 . C5 . C6 . 111.2(5) yes
N2 . C5 . H51 . 109.5 no
C6 . C5 . H51 . 108.4 no
N2 . C5 . H52 . 109.9 no
C6 . C5 . H52 . 107.6 no
H51 . C5 . H52 . 110.2 no
C5 . C6 . N1 . 110.1(5) yes
C5 . C6 . H61 . 107.0 no
N1 . C6 . H61 . 108.4 no
C5 . C6 . H62 . 110.3 no
N1 . C6 . H62 . 110.9 no
H61 . C6 . H62 . 110.0 no
C6 . N1 . Fe1 . 106.6(3) yes
C6 . N1 . C8 . 107.7(5) yes
Fe1 . N1 . C8 . 110.3(3) yes
C6 . N1 . C9 . 114.2(5) yes
Fe1 . N1 . C9 . 110.1(4) yes
C8 . N1 . C9 . 107.8(5) yes
N1 . C8 . H81 . 111.6 no
N1 . C8 . H82 . 108.1 no
H81 . C8 . H82 . 111.8 no
N1 . C8 . H83 . 106.3 no
H81 . C8 . H83 . 109.1 no
H82 . C8 . H83 . 109.6 no
N1 . C9 . H91 . 110.2 no
N1 . C9 . H92 . 108.5 no
H91 . C9 . H92 . 111.1 no
N1 . C9 . H93 . 107.4 no
H91 . C9 . H93 . 108.3 no
H92 . C9 . H93 . 111.3 no
Fe1 . N8 . C12 . 147.1(4) yes
Fe1 . N8 . N7 . 96.4(3) yes
C12 . N8 . N7 . 113.4(4) yes
Fe1 . N12 . C12 . 143.6(5) yes
Fe1 . N12 . N13 . 98.0(7) yes
C12 . N12 . N13 . 117.4(8) yes
N8 . C12 . C13 . 111.3(5) yes
N8 . C12 . C15 . 110.9(6) yes
C13 . C12 . C15 . 114.1(7) yes
N8 . C12 . C41 . 108.5(5) yes
C13 . C12 . C41 . 108.1(6) yes
C15 . C12 . C41 . 103.4(7) yes
N12 . C12 . C14 . 108.1(6) yes
N12 . C12 . C40 . 111.4(8) yes
C14 . C12 . C40 . 111.8(8) yes
N12 . C12 . C42 . 107.9(7) yes
C14 . C12 . C42 . 109.0(8) yes
C40 . C12 . C42 . 108.5(8) yes
C12 . C13 . H131 . 110.7 no
C12 . C13 . H132 . 110.0 no
H131 . C13 . H132 . 109.5 no
C12 . C13 . H133 . 107.7 no
H131 . C13 . H133 . 109.5 no
H132 . C13 . H133 . 109.5 no
C12 . C14 . H141 . 111.2 no
C12 . C14 . H142 . 104.2 no
H141 . C14 . H142 . 109.4 no
C12 . C14 . H143 . 112.6 no
H141 . C14 . H143 . 109.8 no
H142 . C14 . H143 . 109.5 no
C12 . C15 . H151 . 109.4 no
C12 . C15 . H152 . 114.3 no
H151 . C15 . H152 . 109.5 no
C12 . C15 . H153 . 101.9 no
H151 . C15 . H153 . 110.7 no
H152 . C15 . H153 . 110.8 no
N12 . N13 . N14 . 108.3(10) yes
Fe1 . N14 . N13 . 94.7(7) yes
Fe1 . N14 . C19 . 154.0(9) yes
N13 . N14 . C19 . 110.7(10) yes
Fe1 . N3 . C19 . 152.3(6) yes
Fe1 . N3 . N4 . 95.1(4) yes
C19 . N3 . N4 . 104.0(6) yes
N3 . C19 . C21 . 132.7(8) yes
N3 . C19 . H193 . 102.4 no
C21 . C19 . H193 . 106.5 no
N3 . C19 . H194 . 104.8 no
C21 . C19 . H194 . 99.7 no
H193 . C19 . H194 . 109.7 no
N14 . C19 . C20 . 124.0(9) yes
N14 . C19 . H191 . 110.0 no
C20 . C19 . H191 . 106.3 no
N14 . C19 . H192 . 99.1 no
C20 . C19 . H192 . 107.4 no
H191 . C19 . H192 . 109.3 no
C19 . C20 . H201 . 106.5 no
C19 . C20 . H202 . 108.6 no
H201 . C20 . H202 . 111.1 no
C19 . C20 . H203 . 107.4 no
H201 . C20 . H203 . 111.5 no
H202 . C20 . H203 . 111.5 no
C19 . C21 . H211 . 108.4 no
C19 . C21 . H212 . 106.1 no
H211 . C21 . H212 . 110.0 no
C19 . C21 . H213 . 111.1 no
H211 . C21 . H213 . 110.0 no
H212 . C21 . H213 . 111.1 no
N3 . N4 . N5 . 108.8(6) yes
Fe1 . N5 . N4 . 95.4(4) yes
Fe1 . N5 . C25 . 148.0(4) yes
N4 . N5 . C25 . 116.4(5) yes
Fe1 . N9 . C25 . 145.2(6) yes
Fe1 . N9 . N10 . 94.6(7) yes
C25 . N9 . N10 . 117.4(9) yes
N5 . C25 . C26 . 109.8(5) yes
N5 . C25 . C28 . 107.9(5) yes
C26 . C25 . C28 . 109.4(7) yes
N5 . C25 . C30 . 109.1(5) yes
C26 . C25 . C30 . 110.6(6) yes
C28 . C25 . C30 . 110.0(7) yes
N9 . C25 . C27 . 106.6(7) yes
N9 . C25 . C29 . 112.4(6) yes
C27 . C25 . C29 . 111.1(8) yes
N9 . C25 . C31 . 107.6(7) yes
C27 . C25 . C31 . 109.2(8) yes
C29 . C25 . C31 . 109.8(8) yes
C25 . C26 . H261 . 110.0 no
C25 . C26 . H262 . 109.1 no
H261 . C26 . H262 . 109.5 no
C25 . C26 . H263 . 109.2 no
H261 . C26 . H263 . 109.5 no
H262 . C26 . H263 . 109.5 no
C25 . C27 . H271 . 107.9 no
C25 . C27 . H272 . 108.5 no
H271 . C27 . H272 . 110.5 no
C25 . C27 . H273 . 108.8 no
H271 . C27 . H273 . 110.4 no
H272 . C27 . H273 . 110.7 no
C25 . C28 . H281 . 110.2 no
C25 . C28 . H282 . 109.0 no
H281 . C28 . H282 . 109.5 no
C25 . C28 . H283 . 109.9 no
H281 . C28 . H283 . 109.3 no
H282 . C28 . H283 . 109.0 no
C25 . C29 . H291 . 108.8 no
C25 . C29 . H292 . 106.4 no
H291 . C29 . H292 . 112.4 no
C25 . C29 . H293 . 104.9 no
H291 . C29 . H293 . 111.6 no
H292 . C29 . H293 . 112.3 no
C25 . C30 . H301 . 108.3 no
C25 . C30 . H302 . 108.4 no
H301 . C30 . H302 . 109.9 no
C25 . C30 . H303 . 110.2 no
H301 . C30 . H303 . 110.2 no
H302 . C30 . H303 . 109.8 no
C25 . C31 . H311 . 106.7 no
C25 . C31 . H312 . 107.9 no
H311 . C31 . H312 . 110.6 no
C25 . C31 . H313 . 111.2 no
H311 . C31 . H313 . 110.0 no
H312 . C31 . H313 . 110.4 no
N9 . N10 . N11 . 108.2(8) yes
Fe1 . N11 . N10 . 95.6(7) yes
Fe1 . N11 . C37 . 159.7(10) yes
N10 . N11 . C37 . 104.6(12) yes
N8 . N7 . N6 . 107.9(5) yes
Fe1 . N6 . N7 . 95.7(3) yes
Fe1 . N6 . C36 . 154.6(6) yes
N7 . N6 . C36 . 108.4(7) yes
N6 . C36 . C39 . 119.1(11) yes
N6 . C36 . H361 . 112.3 no
C39 . C36 . H361 . 110.6 no
N6 . C36 . H362 . 98.9 no
C39 . C36 . H362 . 105.6 no
H361 . C36 . H362 . 109.1 no
N11 . C37 . C38 . 120.9(17) yes
N11 . C37 . H371 . 112.2 no
C38 . C37 . H371 . 97.8 no
N11 . C37 . H372 . 104.4 no
C38 . C37 . H372 . 111.9 no
H371 . C37 . H372 . 109.4 no
C37 . C38 . H381 . 106.6 no
C37 . C38 . H382 . 118.8 no
H381 . C38 . H382 . 109.1 no
C37 . C38 . H383 . 100.8 no
H381 . C38 . H383 . 110.1 no
H382 . C38 . H383 . 111.1 no
C36 . C39 . H391 . 105.5 no
C36 . C39 . H392 . 109.6 no
H391 . C39 . H392 . 109.1 no
C36 . C39 . H393 . 113.4 no
H391 . C39 . H393 . 109.9 no
H392 . C39 . H393 . 109.2 no
C12 . C40 . H401 . 109.6 no
C12 . C40 . H402 . 111.8 no
H401 . C40 . H402 . 109.5 no
C12 . C40 . H403 . 106.9 no
H401 . C40 . H403 . 109.5 no
H402 . C40 . H403 . 109.5 no
C12 . C41 . H411 . 106.0 no
C12 . C41 . H412 . 112.9 no
H411 . C41 . H412 . 109.5 no
C12 . C41 . H413 . 108.6 no
H411 . C41 . H413 . 109.4 no
H412 . C41 . H413 . 110.3 no
C12 . C42 . H421 . 108.5 no
C12 . C42 . H422 . 112.5 no
H421 . C42 . H422 . 111.1 no
C12 . C42 . H423 . 104.3 no
H421 . C42 . H423 . 110.6 no
H422 . C42 . H423 . 109.7 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N4 . H292 . C28 . 133.0(8) 0.810 2.441 3.051(17) yes
C29 . H292 . N14 . 145.9(5) 1.049 2.564 3.483(17) yes
C29 . H292 . N3 . 157.2(5) 1.049 1.995 2.989(17) yes
N4 . H292 . C29 . 132.1(12) 0.810 1.049 1.701(17) yes
C42 . H422 . N11 . 155.0(5) 0.977 2.480 3.390(17) yes
C42 . H422 . N6 . 145.6(6) 0.977 1.910 2.771(17) yes
C21 . H192 . N13 . 143.0(10) 1.175 2.168 3.186(17) yes
C13 . H132 . N13 . 122.4(9) 0.950 1.130 1.825(17) yes
C13 . H132 . N14 . 130.0(4) 0.950 2.405 3.101(17) yes


