# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_aaa
_database_code_depnum_ccdc_archive 'CCDC 908080'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-10-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C9 H7 Mn N7 O), 4(C2 H6 O), H2 O'
_chemical_formula_sum            'C26 H40 Mn2 N14 O7'
_chemical_formula_weight         770.60
_symmetry_space_group_name_Hall  '-I 4ad '

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I41/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   19.692(9)
_cell_length_b                   19.692(9)
_cell_length_c                   20.101(20)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7795(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      25.50

_exptl_crystal_description       octahedral
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3200
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8164
_exptl_absorpt_correction_T_max  0.8164
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11012
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_av_sigmaI/netI    0.1106
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3585
_reflns_number_gt                1995
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0633P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3585
_refine_ls_number_parameters     238
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1517
_refine_ls_wR_factor_gt          0.1232
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.60456(3) 0.51543(4) 1.02730(3) 0.0319(2) Uani 1 1 d . . .
N1 N 0.8385(2) 0.3695(2) 0.82764(19) 0.0442(11) Uani 1 1 d . . .
N2 N 0.6898(2) 0.4785(2) 0.95706(17) 0.0407(10) Uani 1 1 d . . .
N3 N 0.7588(2) 0.4693(2) 0.95652(19) 0.0461(11) Uani 1 1 d . . .
N4 N 0.71522(18) 0.42061(18) 0.86507(17) 0.0318(9) Uani 1 1 d . . .
N5 N 0.55269(18) 0.47066(18) 0.93824(17) 0.0316(9) Uani 1 1 d . . .
N6 N 0.4879(2) 0.4638(2) 0.91367(18) 0.0395(10) Uani 1 1 d . . .
N7 N 0.5607(2) 0.4267(2) 0.83578(18) 0.0441(11) Uani 1 1 d . . .
C1 C 0.8983(3) 0.3460(3) 0.8060(3) 0.0648(18) Uani 1 1 d . . .
H1 H 0.8986 0.3152 0.7709 0.068(18) Uiso 1 1 calc R . .
C2 C 0.9591(3) 0.3652(4) 0.8330(4) 0.089(2) Uani 1 1 d . . .
H2 H 0.9996 0.3478 0.8163 0.09(2) Uiso 1 1 calc R . .
C3 C 0.9596(3) 0.4099(4) 0.8843(4) 0.099(3) Uani 1 1 d . . .
H3 H 1.0004 0.4240 0.9031 0.15(3) Uiso 1 1 calc R . .
C4 C 0.8981(3) 0.4342(4) 0.9084(3) 0.078(2) Uani 1 1 d . . .
H4 H 0.8971 0.4650 0.9435 0.09(2) Uiso 1 1 calc R . .
C5 C 0.8387(2) 0.4120(3) 0.8795(3) 0.0472(14) Uani 1 1 d . . .
C6 C 0.7715(2) 0.4350(2) 0.9006(2) 0.0379(12) Uani 1 1 d . . .
C7 C 0.6659(2) 0.4490(2) 0.9023(2) 0.0299(11) Uani 1 1 d . . .
C8 C 0.5935(2) 0.4482(2) 0.8903(2) 0.0322(11) Uani 1 1 d . . .
C9 C 0.4953(3) 0.4382(3) 0.8534(2) 0.0490(15) Uani 1 1 d . . .
H9 H 0.4588 0.4289 0.8255 0.035(13) Uiso 1 1 calc R . .
O1 O 0.60862(18) 0.61773(16) 0.98903(16) 0.0491(10) Uani 1 1 d . . .
H1A H 0.6254 0.6203 0.9459 0.067(17) Uiso 1 1 d R . .
H1B H 0.6362 0.6465 1.0138 0.10(2) Uiso 1 1 d R . .
C10 C 0.5334(8) 0.6362(9) 0.8020(10) 0.301(11) Uani 1 1 d DU . .
H10A H 0.5040 0.6071 0.8273 0.452 Uiso 1 1 calc R . .
H10B H 0.5167 0.6398 0.7573 0.452 Uiso 1 1 calc R . .
H10C H 0.5345 0.6805 0.8220 0.452 Uiso 1 1 calc R . .
C11 C 0.5973(8) 0.6096(7) 0.8012(6) 0.209(7) Uani 1 1 d DU . .
H11A H 0.6206 0.6260 0.7619 0.250 Uiso 1 1 calc R . .
H11B H 0.5939 0.5606 0.7975 0.250 Uiso 1 1 calc R . .
O2 O 0.6364(3) 0.6252(3) 0.8570(2) 0.123(2) Uani 1 1 d DU . .
H2A H 0.6757 0.6129 0.8508 0.184 Uiso 1 1 calc R . .
C12 C 0.9278(7) 0.4068(11) 0.1020(10) 0.401(13) Uani 1 1 d DU . .
H12A H 0.9344 0.3585 0.1005 0.601 Uiso 1 1 calc R . .
H12B H 0.9438 0.4240 0.1439 0.601 Uiso 1 1 calc R . .
H12C H 0.9528 0.4277 0.0665 0.601 Uiso 1 1 calc R . .
C13 C 0.8575(7) 0.4218(8) 0.0948(7) 0.274(9) Uani 1 1 d DU . .
H13A H 0.8361 0.4210 0.1383 0.328 Uiso 1 1 calc R . .
H13B H 0.8363 0.3869 0.0678 0.328 Uiso 1 1 calc R . .
O3 O 0.8457(3) 0.4884(4) 0.0640(3) 0.154(3) Uani 1 1 d D . .
H3A H 0.8175 0.4846 0.0342 0.231 Uiso 1 1 calc R . .
O4 O 0.0000 0.2500 0.6697(9) 0.309(10) Uani 1 2 d SD . .
H4A H 0.027(3) 0.258(4) 0.706(2) 0.08(2) Uiso 1 1 d D . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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
Mn1 O1 2.158(3) . ?
Mn1 N6 2.212(4) 9_667 ?
Mn1 N4 2.225(4) 8_454 ?
Mn1 N5 2.242(4) . ?
Mn1 N1 2.302(4) 8_454 ?
Mn1 N2 2.311(4) . ?
N1 C5 1.337(6) . ?
N1 C1 1.339(6) . ?
N1 Mn1 2.302(4) 7_544 ?
N2 C7 1.331(5) . ?
N2 N3 1.370(5) . ?
N3 C6 1.336(6) . ?
N4 C7 1.347(5) . ?
N4 C6 1.348(5) . ?
N4 Mn1 2.225(4) 7_544 ?
N5 C8 1.330(5) . ?
N5 N6 1.374(5) . ?
N6 C9 1.320(5) . ?
N6 Mn1 2.212(4) 9_667 ?
N7 C8 1.342(5) . ?
N7 C9 1.354(6) . ?
C1 C2 1.368(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.356(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.390(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.462(6) . ?
C7 C8 1.447(6) . ?
C9 H9 0.9300 . ?
O1 H1A 0.9284 . ?
O1 H1B 0.9285 . ?
C10 C11 1.362(13) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 O2 1.395(11) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
O2 H2A 0.8200 . ?
C12 C13 1.424(13) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 O3 1.469(12) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
O3 H3A 0.8200 . ?
O4 O4 1.80(4) 15_556 ?
O4 H4A 0.93(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 N6 92.81(14) . 9_667 ?
O1 Mn1 N4 95.81(13) . 8_454 ?
N6 Mn1 N4 91.39(14) 9_667 8_454 ?
O1 Mn1 N5 95.70(14) . . ?
N6 Mn1 N5 97.23(13) 9_667 . ?
N4 Mn1 N5 165.25(13) 8_454 . ?
O1 Mn1 N1 169.11(14) . 8_454 ?
N6 Mn1 N1 91.94(15) 9_667 8_454 ?
N4 Mn1 N1 74.28(14) 8_454 8_454 ?
N5 Mn1 N1 93.42(14) . 8_454 ?
O1 Mn1 N2 92.81(14) . . ?
N6 Mn1 N2 169.78(14) 9_667 . ?
N4 Mn1 N2 96.53(14) 8_454 . ?
N5 Mn1 N2 73.71(14) . . ?
N1 Mn1 N2 84.03(15) 8_454 . ?
C5 N1 C1 117.8(5) . . ?
C5 N1 Mn1 115.2(3) . 7_544 ?
C1 N1 Mn1 126.5(4) . 7_544 ?
C7 N2 N3 106.6(4) . . ?
C7 N2 Mn1 112.7(3) . . ?
N3 N2 Mn1 140.0(3) . . ?
C6 N3 N2 105.0(4) . . ?
C7 N4 C6 102.2(4) . . ?
C7 N4 Mn1 143.8(3) . 7_544 ?
C6 N4 Mn1 113.7(3) . 7_544 ?
C8 N5 N6 105.5(3) . . ?
C8 N5 Mn1 115.7(3) . . ?
N6 N5 Mn1 138.5(3) . . ?
C9 N6 N5 105.4(4) . . ?
C9 N6 Mn1 130.8(3) . 9_667 ?
N5 N6 Mn1 123.6(3) . 9_667 ?
C8 N7 C9 101.0(4) . . ?
N1 C1 C2 123.1(6) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 119.1(6) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 119.0(7) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 118.8(6) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 122.1(5) . . ?
N1 C5 C6 114.6(4) . . ?
C4 C5 C6 123.2(5) . . ?
N3 C6 N4 113.5(4) . . ?
N3 C6 C5 124.8(4) . . ?
N4 C6 C5 121.7(4) . . ?
N2 C7 N4 112.7(4) . . ?
N2 C7 C8 119.4(4) . . ?
N4 C7 C8 127.9(4) . . ?
N5 C8 N7 113.9(4) . . ?
N5 C8 C7 118.2(4) . . ?
N7 C8 C7 127.9(4) . . ?
N6 C9 N7 114.1(4) . . ?
N6 C9 H9 122.9 . . ?
N7 C9 H9 122.9 . . ?
Mn1 O1 H1A 113.3 . . ?
Mn1 O1 H1B 113.5 . . ?
H1A O1 H1B 105.0 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C11 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C10 C11 O2 114.6(15) . . ?
C10 C11 H11A 108.6 . . ?
O2 C11 H11A 108.6 . . ?
C10 C11 H11B 108.6 . . ?
O2 C11 H11B 108.6 . . ?
H11A C11 H11B 107.6 . . ?
C11 O2 H2A 109.5 . . ?
C13 C12 H12A 109.5 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C13 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C12 C13 O3 112.4(14) . . ?
C12 C13 H13A 109.1 . . ?
O3 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
O3 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
C13 O3 H3A 109.5 . . ?
O4 O4 H4A 143(5) 15_556 . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.068
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1408068'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-10-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C10 H6 Fe N7 O2'
_chemical_formula_sum            'C10 H6 Fe N7 O2'
_chemical_formula_weight         312.07
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   p21/n

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.5236(19)
_cell_length_b                   12.240(2)
_cell_length_c                   9.907(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.88(3)
_cell_angle_gamma                90.00
_cell_volume                     1130.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3700
_cell_measurement_theta_min      2.1005
_cell_measurement_theta_max      27.8684

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             628
_exptl_absorpt_coefficient_mu    1.349
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7850
_exptl_absorpt_correction_T_max  0.9885
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7108
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         25.50
_reflns_number_total             2097
_reflns_number_gt                2026
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0296P)²+1.8382P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2097
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0933
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_restrained_S_all      1.178
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -0.00657(5) 0.70480(4) 0.37605(4) 0.02824(16) Uani 1 1 d . . .
N1 N -0.1266(3) 0.8459(2) 0.4414(3) 0.0305(6) Uani 1 1 d . . .
N2 N 0.1523(3) 0.7886(2) 0.5300(3) 0.0275(6) Uani 1 1 d . . .
N3 N 0.3005(3) 0.8316(2) 0.7280(3) 0.0301(6) Uani 1 1 d . . .
N4 N 0.1695(3) 0.8753(2) 0.7337(3) 0.0316(6) Uani 1 1 d . . .
N5 N 0.5323(3) 0.7258(2) 0.6827(3) 0.0311(6) Uani 1 1 d . . .
C9 C 0.6322(3) 0.6813(3) 0.6228(4) 0.0386(8) Uani 1 1 d . . .
H9 H 0.7265 0.6673 0.6666 0.046 Uiso 1 1 calc R . .
N7 N 0.4348(3) 0.6919(3) 0.4580(3) 0.0412(7) Uani 1 1 d . . .
C1 C -0.2605(3) 0.8793(3) 0.3895(4) 0.0390(8) Uani 1 1 d . . .
H1 H -0.3052 0.8557 0.3020 0.047 Uiso 1 1 calc R . .
C2 C -0.3337(4) 0.9462(3) 0.4596(4) 0.0440(9) Uani 1 1 d . . .
H2 H -0.4259 0.9691 0.4195 0.053 Uiso 1 1 calc R . .
C3 C -0.2717(4) 0.9794(3) 0.5881(4) 0.0494(10) Uani 1 1 d . . .
H3 H -0.3221 1.0232 0.6384 0.059 Uiso 1 1 calc R . .
C4 C -0.1343(4) 0.9481(3) 0.6433(4) 0.0431(9) Uani 1 1 d . . .
H4 H -0.0892 0.9712 0.7309 0.052 Uiso 1 1 calc R . .
C5 C -0.0641(3) 0.8819(3) 0.5672(3) 0.0283(7) Uani 1 1 d . . .
C6 C 0.0860(3) 0.8484(3) 0.6129(3) 0.0274(6) Uani 1 1 d . . .
C7 C 0.2863(3) 0.7813(2) 0.6069(3) 0.0260(6) Uani 1 1 d . . .
C8 C 0.4139(3) 0.7300(3) 0.5774(3) 0.0275(6) Uani 1 1 d . . .
N6 N 0.5764(3) 0.6600(3) 0.4913(3) 0.0429(7) Uani 1 1 d . . .
H6 H 0.6224 0.6304 0.4347 0.051 Uiso 1 1 calc R . .
C10 C -0.0478(3) 0.5199(3) 0.5496(3) 0.0284(7) Uani 1 1 d . . .
O1 O -0.0813(3) 0.61916(19) 0.5421(2) 0.0384(6) Uani 1 1 d . . .
O2 O -0.0840(2) 0.45049(19) 0.6287(2) 0.0363(5) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

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 O2 2.092(2) 3_566 ?
Fe1 N3 2.149(3) 4_575 ?
Fe1 N2 2.173(3) . ?
Fe1 O1 2.189(2) . ?
Fe1 N5 2.195(3) 4_575 ?
Fe1 N1 2.239(3) . ?
N1 C1 1.337(4) . ?
N1 C5 1.340(4) . ?
N2 C7 1.347(4) . ?
N2 C6 1.349(4) . ?
N3 C7 1.331(4) . ?
N3 N4 1.369(3) . ?
N3 Fe1 2.149(3) 4_676 ?
N4 C6 1.335(4) . ?
N5 C9 1.337(4) . ?
N5 C8 1.371(4) . ?
N5 Fe1 2.195(3) 4_676 ?
C9 N6 1.327(5) . ?
C9 H9 0.9300 . ?
N7 C8 1.324(4) . ?
N7 N6 1.377(4) . ?
C1 C2 1.355(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.351(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.365(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.466(4) . ?
C7 C8 1.451(4) . ?
N6 H6 0.8600 . ?
C10 O2 1.252(4) . ?
C10 O1 1.254(4) . ?
C10 C10 1.550(6) 3_566 ?
O2 Fe1 2.092(2) 3_566 ?

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
O2 Fe1 N3 95.44(10) 3_566 4_575 ?
O2 Fe1 N2 102.36(10) 3_566 . ?
N3 Fe1 N2 162.09(10) 4_575 . ?
O2 Fe1 O1 77.36(9) 3_566 . ?
N3 Fe1 O1 92.79(10) 4_575 . ?
N2 Fe1 O1 89.18(10) . . ?
O2 Fe1 N5 100.83(9) 3_566 4_575 ?
N3 Fe1 N5 76.06(10) 4_575 4_575 ?
N2 Fe1 N5 102.22(10) . 4_575 ?
O1 Fe1 N5 168.55(10) . 4_575 ?
O2 Fe1 N1 160.88(9) 3_566 . ?
N3 Fe1 N1 86.66(10) 4_575 . ?
N2 Fe1 N1 75.87(9) . . ?
O1 Fe1 N1 83.57(9) . . ?
N5 Fe1 N1 98.12(10) 4_575 . ?
C1 N1 C5 117.6(3) . . ?
C1 N1 Fe1 128.9(2) . . ?
C5 N1 Fe1 111.52(19) . . ?
C7 N2 C6 101.5(2) . . ?
C7 N2 Fe1 143.8(2) . . ?
C6 N2 Fe1 109.73(19) . . ?
C7 N3 N4 107.0(2) . . ?
C7 N3 Fe1 115.7(2) . 4_676 ?
N4 N3 Fe1 135.37(19) . 4_676 ?
C6 N4 N3 104.3(2) . . ?
C9 N5 C8 103.0(3) . . ?
C9 N5 Fe1 144.0(2) . 4_676 ?
C8 N5 Fe1 113.0(2) . 4_676 ?
N6 C9 N5 109.8(3) . . ?
N6 C9 H9 125.1 . . ?
N5 C9 H9 125.1 . . ?
C8 N7 N6 101.8(3) . . ?
N1 C1 C2 122.5(3) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 118.8(3) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 122.1(3) . . ?
N1 C5 C6 114.4(3) . . ?
C4 C5 C6 123.4(3) . . ?
N4 C6 N2 114.3(3) . . ?
N4 C6 C5 124.8(3) . . ?
N2 C6 C5 120.8(3) . . ?
N3 C7 N2 112.8(3) . . ?
N3 C7 C8 116.7(3) . . ?
N2 C7 C8 130.5(3) . . ?
N7 C8 N5 114.6(3) . . ?
N7 C8 C7 128.2(3) . . ?
N5 C8 C7 117.0(3) . . ?
C9 N6 N7 110.8(3) . . ?
C9 N6 H6 124.6 . . ?
N7 N6 H6 124.6 . . ?
O2 C10 O1 126.6(3) . . ?
O2 C10 C10 117.1(3) . 3_566 ?
O1 C10 C10 116.3(3) . 3_566 ?
C10 O1 Fe1 113.0(2) . . ?
C10 O2 Fe1 115.8(2) . 3_566 ?

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
N6 H6 N4 0.86 2.13 2.902(4) 149.0 4_675

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.582
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.062
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1408069'
_audit_update_record             
;
2015-06-22 deposited with the CCDC.
2015-10-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H8 Fe N7 O, 2(H2 O)'
_chemical_formula_sum            'C9 H12 Fe N7 O3'
_chemical_formula_weight         322.11
_symmetry_space_group_name_Hall  '-I 4ad '

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I41/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   19.623(3)
_cell_length_b                   19.623(3)
_cell_length_c                   19.147(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7373(2)
_cell_formula_units_Z            16
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.55
_cell_measurement_theta_max      25.00

_exptl_crystal_description       octahedral
_exptl_crystal_colour            RED
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2640
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8164
_exptl_absorpt_correction_T_max  0.8962
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9371
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3207
_reflns_number_gt                2654
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0936P)²+12.7064P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3207
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1740
_refine_ls_wR_factor_gt          0.1626
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.39624(3) 0.52176(3) 0.02003(3) 0.0346(2) Uani 1 1 d . . .
N1 N 0.38293(19) 0.41754(17) 0.07140(19) 0.0454(9) Uani 1 1 d . . .
N2 N 0.32919(15) 0.53958(15) 0.10716(16) 0.0339(7) Uani 1 1 d . . .
N3 N 0.2705(2) 0.49598(18) 0.1984(2) 0.0535(10) Uani 1 1 d . . .
H3 H 0.2539 0.4671 0.2276 0.064 Uiso 1 1 calc R . .
N4 N 0.26240(18) 0.56483(16) 0.19883(18) 0.0440(9) Uani 1 1 d . . .
N5 N 0.3350(2) 0.69682(18) 0.08489(19) 0.0569(11) Uani 1 1 d . . .
N6 N 0.27632(17) 0.70140(15) 0.18493(16) 0.0377(8) Uani 1 1 d . . .
N7 N 0.29098(19) 0.76686(16) 0.16637(18) 0.0455(9) Uani 1 1 d . . .
C1 C 0.4122(3) 0.3580(2) 0.0532(3) 0.0620(14) Uani 1 1 d . . .
H1 H 0.4456 0.3569 0.0187 0.074 Uiso 1 1 calc R . .
C2 C 0.3925(4) 0.2995(3) 0.0855(4) 0.101(2) Uani 1 1 d . . .
H2 H 0.4124 0.2588 0.0712 0.122 Uiso 1 1 calc R . .
C3 C 0.3473(4) 0.2971(2) 0.1354(4) 0.095(2) Uani 1 1 d . . .
H3A H 0.3363 0.2563 0.1575 0.115 Uiso 1 1 calc R . .
C4 C 0.3176(4) 0.3555(3) 0.1535(4) 0.094(2) Uani 1 1 d . . .
H4 H 0.2835 0.3554 0.1871 0.113 Uiso 1 1 calc R . .
C5 C 0.3369(3) 0.4168(2) 0.1228(2) 0.0522(12) Uani 1 1 d . . .
C6 C 0.3099(2) 0.4827(2) 0.1429(2) 0.0414(10) Uani 1 1 d . . .
C7 C 0.29816(19) 0.58853(19) 0.14440(19) 0.0337(8) Uani 1 1 d . . .
C8 C 0.30315(19) 0.66218(19) 0.13532(19) 0.0343(9) Uani 1 1 d . . .
C9 C 0.3249(3) 0.7612(2) 0.1068(2) 0.0615(15) Uani 1 1 d . . .
H9 H 0.3404 0.7989 0.0820 0.074 Uiso 1 1 calc R . .
O1 O 0.39412(18) 0.62168(15) -0.01873(15) 0.0553(9) Uani 1 1 d . . .
H1A H 0.4338 0.6330 -0.0324 0.083 Uiso 1 1 d R . .
H1B H 0.3813 0.6485 0.0136 0.083 Uiso 1 1 d R . .
O2 O 0.1555(6) 0.4275(5) 0.2519(3) 0.316(8) Uani 1 1 d G . .
H2A H 0.1134 0.4205 0.2592 0.474 Uiso 1 1 d G . .
H2B H 0.1653 0.4162 0.2102 0.474 Uiso 1 1 d G . .
O3 O 0.3368(8) 0.6500(3) 0.8580(4) 0.357(9) Uani 1 1 d G . .
H3B H 0.3655 0.6363 0.8882 0.536 Uiso 1 1 d G . .
H3C H 0.2967 0.6452 0.8740 0.536 Uiso 1 1 d G . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 2.097(3) . ?
Fe1 N7 2.129(3) 12_766 ?
Fe1 N2 2.153(3) . ?
Fe1 N6 2.172(3) 4_454 ?
Fe1 N4 2.205(3) 4_454 ?
Fe1 N1 2.284(4) . ?
N1 C5 1.337(6) . ?
N1 C1 1.348(5) . ?
N2 C7 1.342(4) . ?
N2 C6 1.364(5) . ?
N3 C6 1.339(5) . ?
N3 N4 1.360(5) . ?
N3 H3 0.8600 . ?
N4 C7 1.340(5) . ?
N4 Fe1 2.205(3) 3 ?
N5 C8 1.336(5) . ?
N5 C9 1.346(5) . ?
N6 C8 1.331(5) . ?
N6 N7 1.363(4) . ?
N6 Fe1 2.172(3) 3 ?
N7 C9 1.325(5) . ?
N7 Fe1 2.129(3) 15_565 ?
C1 C2 1.361(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.305(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.331(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.390(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.448(6) . ?
C7 C8 1.459(5) . ?
C9 H9 0.9300 . ?
O1 H1A 0.8503 . ?
O1 H1B 0.8504 . ?
O2 H2A 0.8501 . ?
O2 H2B 0.8502 . ?
O3 H3B 0.8499 . ?
O3 H3C 0.8499 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 N7 93.03(14) . 12_766 ?
O1 Fe1 N2 96.33(12) . . ?
N7 Fe1 N2 91.01(12) 12_766 . ?
O1 Fe1 N6 98.66(12) . 4_454 ?
N7 Fe1 N6 96.13(12) 12_766 4_454 ?
N2 Fe1 N6 163.01(12) . 4_454 ?
O1 Fe1 N4 92.92(14) . 4_454 ?
N7 Fe1 N4 171.09(13) 12_766 4_454 ?
N2 Fe1 N4 94.91(12) . 4_454 ?
N6 Fe1 N4 76.42(12) 4_454 4_454 ?
O1 Fe1 N1 170.85(13) . . ?
N7 Fe1 N1 90.22(14) 12_766 . ?
N2 Fe1 N1 75.04(12) . . ?
N6 Fe1 N1 89.49(13) 4_454 . ?
N4 Fe1 N1 84.90(14) 4_454 . ?
C5 N1 C1 118.0(4) . . ?
C5 N1 Fe1 113.8(3) . . ?
C1 N1 Fe1 128.0(3) . . ?
C7 N2 C6 101.1(3) . . ?
C7 N2 Fe1 143.6(3) . . ?
C6 N2 Fe1 115.2(2) . . ?
C6 N3 N4 105.4(3) . . ?
C6 N3 H3 127.3 . . ?
N4 N3 H3 127.3 . . ?
C7 N4 N3 106.2(3) . . ?
C7 N4 Fe1 112.9(2) . 3 ?
N3 N4 Fe1 139.4(3) . 3 ?
C8 N5 C9 100.5(3) . . ?
C8 N6 N7 106.0(3) . . ?
C8 N6 Fe1 114.8(2) . 3 ?
N7 N6 Fe1 139.2(2) . 3 ?
C9 N7 N6 104.6(3) . . ?
C9 N7 Fe1 130.4(3) . 15_565 ?
N6 N7 Fe1 124.6(2) . 15_565 ?
N1 C1 C2 119.5(5) . . ?
N1 C1 H1 120.2 . . ?
C2 C1 H1 120.2 . . ?
C3 C2 C1 123.8(5) . . ?
C3 C2 H2 118.1 . . ?
C1 C2 H2 118.1 . . ?
C2 C3 C4 117.2(5) . . ?
C2 C3 H3A 121.4 . . ?
C4 C3 H3A 121.4 . . ?
C3 C4 C5 121.1(6) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
N1 C5 C4 120.2(4) . . ?
N1 C5 C6 115.7(4) . . ?
C4 C5 C6 124.1(4) . . ?
N3 C6 N2 113.5(3) . . ?
N3 C6 C5 126.6(4) . . ?
N2 C6 C5 119.7(4) . . ?
N4 C7 N2 113.7(3) . . ?
N4 C7 C8 118.2(3) . . ?
N2 C7 C8 128.0(3) . . ?
N6 C8 N5 114.0(3) . . ?
N6 C8 C7 117.5(3) . . ?
N5 C8 C7 128.4(3) . . ?
N7 C9 N5 114.9(4) . . ?
N7 C9 H9 122.5 . . ?
N5 C9 H9 122.5 . . ?
Fe1 O1 H1A 109.5 . . ?
Fe1 O1 H1B 109.1 . . ?
H1A O1 H1B 109.4 . . ?
H2A O2 H2B 109.5 . . ?
H3B O3 H3C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.069
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.016 -0.001 -0.001 2393 201 ' '
2 0.500 0.750 0.125 53 4 ' '
3 0.000 0.750 0.375 53 4 ' '
4 0.000 0.250 0.625 53 4 ' '
5 0.500 0.250 0.875 53 4 ' '
_platon_squeeze_details          
;
;
