# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_Co(H2mdp)(Ni(CN)4)
_database_code_depnum_ccdc_archive 'CCDC 2327474'
loop_
_audit_author_name
_audit_author_address
'Nathan Harvey-Reid'
;University of Canterbury
New Zealand
;
_audit_update_record             
;
2024-04-05 deposited with the CCDC.	2024-05-15 downloaded from the CCDC.
;
_audit_creation_date             2024-04-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H16 Co N8 Ni, 4(H2 O)'
_chemical_formula_sum            'C15 H24 Co N8 Ni O4'
_chemical_formula_weight         498.06
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_H-M_alt        'P 4/n n c'
_space_group_name_Hall           '-P 4a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y+1/2, x, z'
'y, -x+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y-1/2, -x, -z'
'-y, x-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   14.3689(5)
_cell_length_b                   14.3689(5)
_cell_length_c                   21.6026(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4460.2(4)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1280
_cell_measurement_temperature    120.00(12)
_cell_measurement_theta_max      73.1380
_cell_measurement_theta_min      3.6790
_shelx_estimated_absorpt_T_max   0.782
_shelx_estimated_absorpt_T_min   0.551
_exptl_absorpt_coefficient_mu    7.197
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-7 -6 4 0.0207
7 6 -4 0.0155
7 -7 0 0.0472
-7 6 0 0.0390
4 -8 2 0.0524
-3 -3 -13 0.0085
-2 -2 13 0.0304

_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.036
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0476
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7815
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.409
_diffrn_reflns_theta_min         3.694
_diffrn_ambient_temperature      120.15
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00  -2.00   1.00   37.50    --  -38.50 125.00  90.00   87
  2  ω     33.00 100.00   1.00  117.50    --  103.81 -94.00 -60.00   67
  3  ω     28.00 103.00   1.00  117.50    --  103.81 -94.00-120.00   75
  4  ω     81.00 147.00   1.00  117.50    --  103.81  77.00-120.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1482
_reflns_number_total             2213
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2213
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0552
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0872P)²+1.6064P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1721
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: Ni1(0.2075) O3(0.75) H3A(0.75) H3B(0.75) O2(0.25) H2A(0.25)
 H2B(0.25) Ni1A(0.0425)
3.a Free rotating group:
 O1(H1A,H1B), O3(H3A,H3B), O2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.500000 0.500000 0.500000 0.0101(3) Uani 1 2 d S . P . .
Ni1 Ni 0.750000 0.750000 0.4668(2) 0.0126(8) Uani 0.83 4 d S T P A 1
Ni2 Ni 0.250000 0.750000 0.500000 0.0192(4) Uani 1 4 d S T P . .
N1 N 0.6029(2) 0.6003(2) 0.47467(16) 0.0188(7) Uani 1 1 d . . . . .
N2 N 0.4003(2) 0.6056(2) 0.50299(15) 0.0177(7) Uani 1 1 d . . . . .
N3 N 0.5345(2) 0.5160(2) 0.59616(15) 0.0202(7) Uani 1 1 d . . . . .
N4 N 0.5490(3) 0.4371(2) 0.62977(17) 0.0243(8) Uani 1 1 d . . . . .
O1 O 0.5463(3) 0.2346(3) 0.61676(17) 0.0509(11) Uani 1 1 d G . . . .
H1A H 0.493330 0.230394 0.634077 0.076 Uiso 1 1 d G U . . .
H1B H 0.538773 0.209408 0.581516 0.076 Uiso 1 1 d G U . . .
O3 O 0.3883(3) 0.2392(3) 0.6861(2) 0.0329(10) Uani 0.75 1 d G . P B 4
H3A H 0.354026 0.191045 0.687403 0.049 Uiso 0.75 1 d G U P B 4
H3B H 0.411041 0.243430 0.722313 0.049 Uiso 0.75 1 d G U P B 4
C5 C 0.5536(3) 0.5859(3) 0.63467(19) 0.0213(8) Uani 1 1 d . . . . .
C4 C 0.5801(3) 0.5522(3) 0.69297(19) 0.0247(9) Uani 1 1 d . . . . .
C2 C 0.3433(3) 0.6608(3) 0.50132(19) 0.0206(9) Uani 1 1 d . . . . .
C1 C 0.6593(3) 0.6574(3) 0.47061(19) 0.0206(8) Uani 1 1 d . . . . .
C3 C 0.5770(3) 0.4563(3) 0.68777(18) 0.0235(9) Uani 1 1 d . . . . .
C6 C 0.5467(4) 0.6857(3) 0.6152(2) 0.0342(10) Uani 1 1 d . . . . .
H6A H 0.609358 0.711972 0.611103 0.051 Uiso 1 1 calc R U . . .
H6B H 0.511861 0.720819 0.646427 0.051 Uiso 1 1 calc R U . . .
H6C H 0.514422 0.689643 0.575328 0.051 Uiso 1 1 calc R U . . .
C7 C 0.6067(3) 0.6067(3) 0.750000 0.0316(15) Uani 1 2 d S T P . .
C8 C 0.5966(5) 0.3812(4) 0.7342(2) 0.0436(13) Uani 1 1 d . . . . .
H8A H 0.545992 0.378832 0.764621 0.065 Uiso 1 1 calc R U . . .
H8B H 0.655391 0.394517 0.755445 0.065 Uiso 1 1 calc R U . . .
H8C H 0.601180 0.321073 0.713002 0.065 Uiso 1 1 calc R U . . .
O2 O 0.7520(9) 0.2901(10) 0.6404(7) 0.029(3) Uani 0.25 1 d G . P C -3
H2A H 0.794544 0.320876 0.622315 0.044 Uiso 0.25 1 d G U P C -3
H2B H 0.761254 0.234107 0.629318 0.044 Uiso 0.25 1 d G U P C -3
Ni1A Ni 0.750000 0.750000 0.4837(13) 0.027(7) Uani 0.17 4 d S T P A 2
H4 H 0.549(4) 0.375(4) 0.610(2) 0.034(14) Uiso 1 1 d . . . . .
H7 H 0.668(4) 0.598(3) 0.756(2) 0.027(13) Uiso 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
Co1 N1 2.136(3) 9_666 ?
Co1 N1 2.136(3) . ?
Co1 N2 2.088(3) . ?
Co1 N2 2.088(3) 9_666 ?
Co1 N3 2.148(3) 9_666 ?
Co1 N3 2.148(3) . ?
Ni1 C1 1.865(4) 2_665 ?
Ni1 C1 1.865(4) 3_655 ?
Ni1 C1 1.865(4) 4_565 ?
Ni1 C1 1.865(4) . ?
Ni2 C2 1.855(4) . ?
Ni2 C2 1.855(5) 11_566 ?
Ni2 C2 1.855(4) 2_565 ?
Ni2 C2 1.855(5) 12_666 ?
N1 C1 1.157(6) . ?
N2 C2 1.141(6) . ?
N3 N4 1.361(5) . ?
N3 C5 1.334(5) . ?
N4 C3 1.344(6) . ?
N4 H4 0.98(6) . ?
O1 H1A 0.8500 . ?
O1 H1B 0.8502 . ?
O3 H3A 0.8496 . ?
O3 H3B 0.8504 . ?
C5 C4 1.402(6) . ?
C5 C6 1.498(6) . ?
C4 C3 1.383(6) . ?
C4 C7 1.509(5) . ?
C1 Ni1A 1.884(6) . ?
C3 C8 1.501(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7 0.90(5) . ?
C7 H7 0.90(5) 7_556 ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
O2 H2A 0.8500 . ?
O2 H2B 0.8504 . ?

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
N1 Co1 N1 180.00(12) . 9_666 ?
N1 Co1 N3 89.07(13) . 9_666 ?
N1 Co1 N3 90.93(13) 9_666 9_666 ?
N1 Co1 N3 90.93(13) . . ?
N1 Co1 N3 89.07(13) 9_666 . ?
N2 Co1 N1 90.43(13) 9_666 . ?
N2 Co1 N1 89.57(13) 9_666 9_666 ?
N2 Co1 N1 90.43(13) . 9_666 ?
N2 Co1 N1 89.57(13) . . ?
N2 Co1 N2 180.00(17) 9_666 . ?
N2 Co1 N3 92.91(13) 9_666 9_666 ?
N2 Co1 N3 92.91(13) . . ?
N2 Co1 N3 87.09(13) . 9_666 ?
N2 Co1 N3 87.09(13) 9_666 . ?
N3 Co1 N3 180.00(18) . 9_666 ?
C1 Ni1 C1 89.886(19) 2_665 4_565 ?
C1 Ni1 C1 89.884(19) 3_655 . ?
C1 Ni1 C1 89.89(2) 4_565 . ?
C1 Ni1 C1 89.886(19) 2_665 3_655 ?
C1 Ni1 C1 174.9(4) 2_665 . ?
C1 Ni1 C1 174.9(4) 4_565 3_655 ?
C2 Ni2 C2 90.014(5) . 12_666 ?
C2 Ni2 C2 90.014(5) 11_566 2_565 ?
C2 Ni2 C2 90.014(4) 12_666 2_565 ?
C2 Ni2 C2 90.013(5) . 11_566 ?
C2 Ni2 C2 178.2(3) 12_666 11_566 ?
C2 Ni2 C2 178.2(3) . 2_565 ?
C1 N1 Co1 169.5(3) . . ?
C2 N2 Co1 175.6(4) . . ?
N4 N3 Co1 117.6(2) . . ?
C5 N3 Co1 137.0(3) . . ?
C5 N3 N4 105.2(3) . . ?
N3 N4 H4 122(3) . . ?
C3 N4 N3 111.9(3) . . ?
C3 N4 H4 126(3) . . ?
H1A O1 H1B 104.5 . . ?
H3A O3 H3B 104.5 . . ?
N3 C5 C4 110.8(4) . . ?
N3 C5 C6 122.2(4) . . ?
C4 C5 C6 127.0(4) . . ?
C5 C4 C7 128.5(4) . . ?
C3 C4 C5 105.2(4) . . ?
C3 C4 C7 126.2(4) . . ?
N2 C2 Ni2 179.0(4) . . ?
N1 C1 Ni1 178.2(4) . . ?
N1 C1 Ni1A 167.0(9) . . ?
N4 C3 C4 106.8(4) . . ?
N4 C3 C8 122.1(4) . . ?
C4 C3 C8 131.0(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 C4 113.8(5) . 7_556 ?
C4 C7 H7 107(3) . . ?
C4 C7 H7 111(3) . 7_556 ?
C4 C7 H7 111(3) 7_556 . ?
C4 C7 H7 107(3) 7_556 7_556 ?
H7 C7 H7 108(6) . 7_556 ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
H2A O2 H2B 104.4 . . ?
C1 Ni1A C1 88.7(3) 3_655 . ?
C1 Ni1A C1 88.7(3) 4_565 . ?
C1 Ni1A C1 88.7(3) 2_665 3_655 ?
C1 Ni1A C1 162.8(17) 2_665 . ?
C1 Ni1A C1 162.8(17) 4_565 3_655 ?
C1 Ni1A C1 88.7(3) 2_665 4_565 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A O3 0.85 1.89 2.721(6) 166.8 . yes
O3 H3A O3 0.85 2.01 2.818(7) 159.8 4 yes
O3 H3B O3 0.85 2.02 2.778(9) 147.9 6_556 yes
O2 H2A O1 0.85 2.43 2.965(14) 122.0 2_655 yes
N4 H4 O1 0.98(6) 2.03(6) 2.924(5) 151(4) . yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 N1 C1 Ni1A 4(3) . . . . ?
Co1 N3 N4 C3 175.2(3) . . . . ?
Co1 N3 C5 C4 -174.4(3) . . . . ?
Co1 N3 C5 C6 5.4(6) . . . . ?
N1 C1 Ni1A C1 99.9(19) . . . 3_655 ?
N1 C1 Ni1A C1 -178.6(17) . . . 2_665 ?
N1 C1 Ni1A C1 -97.1(19) . . . 4_565 ?
N3 N4 C3 C4 0.7(5) . . . . ?
N3 N4 C3 C8 179.3(4) . . . . ?
N3 C5 C4 C3 0.6(5) . . . . ?
N3 C5 C4 C7 -179.4(4) . . . . ?
N4 N3 C5 C4 -0.2(4) . . . . ?
N4 N3 C5 C6 179.6(4) . . . . ?
C5 N3 N4 C3 -0.3(5) . . . . ?
C5 C4 C3 N4 -0.8(4) . . . . ?
C5 C4 C3 C8 -179.2(5) . . . . ?
C5 C4 C7 C4 126.8(5) . . . 7_556 ?
C3 C4 C7 C4 -53.3(3) . . . 7_556 ?
C6 C5 C4 C3 -179.1(4) . . . . ?
C6 C5 C4 C7 0.8(7) . . . . ?
C7 C4 C3 N4 179.3(4) . . . . ?
C7 C4 C3 C8 0.9(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
####################################################################### 
# 
# 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_Fe(H2mdp)(Ni(CN)4)
_database_code_depnum_ccdc_archive 'CCDC 2327475'
loop_
_audit_author_name
_audit_author_address
'Nathan Harvey-Reid'
;University of Canterbury
New Zealand
;
_audit_update_record             
;
2024-04-05 deposited with the CCDC.	2024-05-15 downloaded from the CCDC.
;
_audit_creation_date             2024-01-31
_audit_creation_method           
;
Olex2 1.5-dev
(compiled 2024.01.11 svn.r2f8d729c for OlexSys, GUI svn.r6697)
;
# start Validation Reply Form
_vrf_PLAT088_FeH2mdpNiCN4        
;
PROBLEM: Poor Data / Parameter Ratio ....................       7.68 Note  
RESPONSE:'Obtained crystals were very small and diffracted 
poorly hindering collection of data at higher resolution'
;
# end Validation Reply Form
_chemical_formula_moiety         'C15 H16 Fe N8 Ni, H2 O2, 3(H2 O)'
_chemical_formula_sum            'C15 H24 Fe N8 Ni O5'
_chemical_formula_weight         510.947
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_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01788 0.00908 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Fe -1.13125 3.15233 11.76950 7.35730 3.52220 2.30450 4.76110 0.30720 15.35350
76.88050 1.03690 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
N 0.03110 0.01806 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
Ni -2.97823 0.51071 12.83760 7.29200 4.44380 2.38000 3.87850 0.25650 12.17630
66.34210 1.03410 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'
O 0.04960 0.03234 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 2'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x,z
3 y,-x,z
4 x,-y,-z
5 -x,y,-z
6 -x,-y,z
7 y,x,-z
8 -y,-x,-z
9 -x,-y,-z
10 y,-x,-z
11 -y,x,-z
12 -x,y,z
13 x,-y,z
14 x,y,-z
15 -y,-x,z
16 y,x,z
17 x+1/2,y+1/2,z+1/2
18 -y+1/2,x+1/2,z+1/2
19 y+1/2,-x+1/2,z+1/2
20 x+1/2,-y+1/2,-z+1/2
21 -x+1/2,y+1/2,-z+1/2
22 -x+1/2,-y+1/2,z+1/2
23 y+1/2,x+1/2,-z+1/2
24 -y+1/2,-x+1/2,-z+1/2
25 -x+1/2,-y+1/2,-z+1/2
26 y+1/2,-x+1/2,-z+1/2
27 -y+1/2,x+1/2,-z+1/2
28 -x+1/2,y+1/2,z+1/2
29 x+1/2,-y+1/2,z+1/2
30 x+1/2,y+1/2,-z+1/2
31 -y+1/2,-x+1/2,z+1/2
32 y+1/2,x+1/2,z+1/2

_symmetry_Int_Tables_number      139
_cell_length_a                   14.4482(3)
_cell_length_b                   14.4482(3)
_cell_length_c                   21.7145(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4532.9(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    1852
_cell_measurement_temperature    120.0(4)
_cell_measurement_theta_max      76.0720
_cell_measurement_theta_min      6.0890
_exptl_absorpt_coefficient_mu    6.534
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       plate
_exptl_crystal_F_000             2087.144
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 -7 -1 0.0325
-7 -7 0 0.0468
7 7 0 0.0468
-6 7 1 0.0729
5 -4 -10 0.0356
1 0 14 0.0195
-1 0 -14 0.0266
-8 5 4 0.0553

_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.046
_diffrn_reflns_av_R_equivalents  0.1029
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_Laue_measured_fraction_full 0.9795
_diffrn_reflns_Laue_measured_fraction_max 0.9717
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7180
_diffrn_reflns_point_group_measured_fraction_full 0.9795
_diffrn_reflns_point_group_measured_fraction_max 0.9717
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         77.66
_diffrn_reflns_theta_min         4.33
_diffrn_ambient_temperature      120.15
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9795
_diffrn_measured_fraction_theta_max 0.9717
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00 -22.00   0.50   30.00    --  -47.45 106.00 144.00  120
  2  ω     38.00  81.00   0.50  120.00    --  107.75-128.00 -33.00   86
  3  ω    101.00 163.00   0.50  120.00    --  107.75  19.00 -12.00  124
  4  ω     44.00  98.00   0.50  120.00    --  107.75-106.00  44.00  108
  5  ω      0.00  76.00   0.50   30.00    --   47.45 -99.00 150.00  152
  6  ω     36.00 118.00   0.50  120.00    --  107.75 -15.00 -30.00  164
  7  ω     40.00 104.00   0.50  120.00    --  107.75 -94.00-120.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                1051
_reflns_number_total             1374
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.6105
_refine_diff_density_min         -0.8965
_refine_diff_density_rms         0.1381
_refine_ls_d_res_high            0.7892
_refine_ls_d_res_low             10.2164
_refine_ls_goodness_of_fit_ref   1.0257
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    30
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1374
_refine_ls_number_restraints     218
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0564
_refine_ls_restrained_S_all      0.9434
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1232P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.1746
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H2b-O2 = O2-H2a
 0.85 with sigma of 0.02
 H2b-H2a
 1.349 with sigma of 0.04
 C6-C10 \\sim C6-C5
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(N3) \\sim
Ueq, Uanis(N4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(N5) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C12) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C7, C5, C4, N3, N4, C3, C8, C6, C9, C10, C11, N5, N6, C12, C13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H3(0.5) H2(0.5) H2b(0.5) C7(0.25) C5(0.25) C4(0.25) N3(0.25)
 N4(0.25) H4(0.25) C3(0.25) H3a(0.25) H3b(0.25) H3c(0.25) C8(0.25) H8a(0.25)
 H8b(0.25) H8c(0.25) C6(0.25) H6b(0.25) H6a(0.25) O1(0.25) C9(0.25) C10(0.25)
 C11(0.25) N5(0.25) N6(0.25) H6(0.25) C12(0.25) H12a(0.25) H12b(0.25)
 H12c(0.25) C13(0.25) H13a(0.25) H13b(0.25) H13c(0.25) H1a(0.25) H1b(0.25)
6.a Riding coordinates:
 O3(H3), O1(H1a,H1b), O2(H2b,H2a)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6b,H6a)
6.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6)
6.d Fitted pentagon refined as free rotating group:
 C7(C5,C4,N3,N4)
6.e Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C8(H8a,H8b,H8c), C12(H12a,H12b,H12c), C13(H13a,H13b,H13c)
;
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_group
Fe1 Fe 0.25 0.75 0.25 0.0159(3) Uani 1.000000 4 S T P .
Ni1 Ni 0.5 0.5 0.21552(7) 0.0171(4) Uani 1.000000 8 S T P 1
Ni2 Ni 0.5 1.0 0.25 0.0191(4) Uani 1.000000 8 S T P .
N1 N 0.35254(17) 0.64746(17) 0.22261(17) 0.0228(8) Uani 1.000000 2 S T P .
N2 N 0.35358(19) 0.85358(19) 0.25 0.0270(9) Uani 1.000000 2 S T P .
O3 O 0.1379(3) 1.0 0.43644(18) 0.0461(10) Uani 1.000000 2 S T P .
H3 H 0.1061(3) 1.04974 0.42858(18) 0.0691(15) Uiso 0.500000 1 R . P .
C2 C 0.4095(2) 0.9095(2) 0.25 0.0234(10) Uani 1.000000 2 S T P .
C1 C 0.4081(2) 0.5919(2) 0.21823(19) 0.0211(8) Uani 1.000000 2 S T P .
O2 O 0.2976(4) 1.0 0.3662(2) 0.0624(14) Uani 1.000000 2 DS T P .
C7 C 0.3344(12) 0.7976(7) 0.4387(5) 0.027(2) Uani 0.250000 1 . U P -1
C5 C 0.3393(11) 0.7001(7) 0.4457(4) 0.0230(16) Uani 0.250000 1 DG U P -1
C4 C 0.3079(13) 0.6589(7) 0.3901(6) 0.024(2) Uani 0.250000 1 G U P -1
N3 N 0.2836(15) 0.7310(11) 0.3488(5) 0.023(2) Uani 0.250000 1 G U P -1
N4 N 0.3000(13) 0.8168(8) 0.3788(6) 0.027(2) Uani 0.250000 1 G U P -1
H4 H 0.2906(13) 0.8721(8) 0.3630(6) 0.032(3) Uiso 0.250000 1 R . P -1
C3 C 0.2904(12) 0.5600(12) 0.3620(8) 0.028(3) Uani 0.250000 1 . U P -1
H3a H 0.3493(16) 0.534(3) 0.348(4) 0.042(4) Uiso 0.250000 1 GR . P -1
H3b H 0.263(6) 0.520(2) 0.3935(15) 0.042(4) Uiso 0.250000 1 GR . P -1
H3c H 0.248(5) 0.5651(15) 0.327(3) 0.042(4) Uiso 0.250000 1 GR . P -1
C8 C 0.3613(11) 0.8704(10) 0.4833(8) 0.030(3) Uani 0.250000 1 . U P -1
H8a H 0.361(7) 0.845(2) 0.5250(10) 0.045(4) Uiso 0.250000 1 GR . P -1
H8b H 0.423(4) 0.893(6) 0.473(3) 0.045(4) Uiso 0.250000 1 GR . P -1
H8c H 0.317(5) 0.922(3) 0.481(4) 0.045(4) Uiso 0.250000 1 GR . P -1
C6 C 0.3479(5) 0.6311(5) 0.5 0.0245(13) Uani 0.25 1 DS TU P -1
H6b H 0.4139(5) 0.6157(5) 0.5066217946680147 0.0294(16) Uiso 0.250000 1 R . P
-1
H6a H 0.3147(5) 0.5732(5) 0.48970729965110366 0.0294(16) Uiso 0.250000 1 R . P
-1
O1 O 0.5 1.0398(7) 0.3887(6) 0.074(3) Uani 0.25 1 S T P -1
C9 C 0.2163(10) 0.6764(13) 0.5603(7) 0.0237(19) Uani 0.250000 1 . U P -1
C10 C 0.3071(9) 0.6727(11) 0.5598(4) 0.0216(16) Uani 0.250000 1 D U P -1
C11 C 0.3346(9) 0.6927(12) 0.6181(6) 0.0199(19) Uani 0.250000 1 . U P -1
N5 N 0.2650(10) 0.7094(14) 0.6547(6) 0.019(2) Uani 0.250000 1 . U P -1
N6 N 0.1942(9) 0.6971(13) 0.6175(7) 0.0213(19) Uani 0.250000 1 . U P -1
H6 H 0.1365(9) 0.7024(13) 0.6299(7) 0.026(2) Uiso 0.250000 1 R . P -1
C12 C 0.4324(10) 0.6910(11) 0.6324(7) 0.0193(19) Uani 0.250000 1 . U P -1
H12a H 0.4564(18) 0.6281(19) 0.627(5) 0.029(3) Uiso 0.250000 1 GR . P -1
H12b H 0.4654(14) 0.734(5) 0.605(3) 0.029(3) Uiso 0.250000 1 GR . P -1
H12c H 0.4418(12) 0.710(7) 0.6752(15) 0.029(3) Uiso 0.250000 1 GR . P -1
C13 C 0.1369(9) 0.6663(10) 0.5128(6) 0.024(2) Uani 0.250000 1 . U P -1
H13a H 0.132(5) 0.724(3) 0.489(3) 0.036(4) Uiso 0.250000 1 GR . P -1
H13b H 0.150(3) 0.615(5) 0.485(3) 0.036(4) Uiso 0.250000 1 GR . P -1
H13c H 0.0786(14) 0.655(7) 0.5345(6) 0.036(4) Uiso 0.250000 1 GR . P -1
H1a H 0.49999999999999994 1.0370(7) 0.4287(6) 0.111(4) Uiso 0.25 1 RS T P -1
H1b H 0.49999999999999994 1.0987(7) 0.3805(6) 0.111(4) Uiso 0.25 1 RS T P -1
H2a H 0.3465(4) 0.9999999999999999 0.3881(2) 0.40(17) Uiso 1.000000 2 DRS T P .
H2b H 0.2495(4) 0.9999999999999999 0.3886(2) 0.10(4) Uiso 1.000000 2 DRS T P .


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 N1 2.178(4) . y
Fe1 N1 2.178(4) 23_455 y
Fe1 N2 2.116(4) . y
Fe1 N2 2.116(4) 15_665 y
Fe1 N3 2.216(8) 25_565 y
Fe1 N3 2.216(8) 15_665 y
Fe1 N3 2.216(8) . y
Fe1 N3 2.216(8) 23_455 y
Fe1 N5 2.162(11) 8_666 y
Fe1 N5 2.162(11) 32_454 y
Fe1 N5 2.162(11) 14_556 y
Fe1 N5 2.162(11) 22_564 y
Ni1 C1 1.879(4) 2_655 y
Ni1 C1 1.879(4) 3_565 y
Ni1 C1 1.879(4) . y
Ni1 C1 1.879(4) 6_665 y
Ni2 C2 1.848(5) . y
Ni2 C2 1.848(5) 12_655 y
Ni2 C2 1.848(5) 6_675 y
Ni2 C2 1.848(5) 13_575 y
N1 C1 1.139(6) . ?
N2 C2 1.143(7) . ?
O3 H3 0.8700 13_575 ?
O3 H3 0.8700 . ?
O2 H2a 0.8524 . ?
O2 H2b 0.8485 . ?
C7 C5 1.4200 . ?
C7 N4 1.4200 . ?
C7 C8 1.481(18) . ?
C5 C4 1.4200 . ?
C5 C6 1.5483(18) . ?
C4 N3 1.4200 . ?
C4 C3 1.57(2) . ?
N3 N4 1.4200 . ?
N4 H4 0.8800 . ?
C3 H3a 0.9800 . ?
C3 H3b 0.9800 . ?
C3 H3c 0.9800 . ?
C8 H8a 0.9800 . ?
C8 H8b 0.9800 . ?
C8 H8c 0.9800 . ?
C6 H6b 0.9900 . ?
C6 H6b 0.9900 14_556 ?
C6 H6a 0.9900 . ?
C6 H6a 0.9900 14_556 ?
C6 C10 1.5476(18) . ?
C6 C10 1.5476(18) 14_556 ?
O1 H1a 0.8700 . ?
O1 H1b 0.8700 . ?
C9 C10 1.313(18) . ?
C9 N6 1.316(17) . ?
C9 C13 1.548(19) . ?
C10 C11 1.357(15) . ?
C11 N5 1.304(14) . ?
C11 C12 1.45(2) . ?
N5 N6 1.316(15) . ?
N6 H6 0.8800 . ?
C12 H12a 0.9800 . ?
C12 H12b 0.9800 . ?
C12 H12c 0.9800 . ?
C13 H13a 0.9800 . ?
C13 H13b 0.9800 . ?
C13 H13c 0.9800 . ?

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
N1 Fe1 N1 180.0 23_455 . y
N2 Fe1 N1 90.0 15_665 23_455 y
N2 Fe1 N1 90.0 15_665 . y
N2 Fe1 N1 90.0 . . y
N2 Fe1 N1 90.0 . 23_455 y
N2 Fe1 N2 180.0 15_665 . y
N3 Fe1 N1 91.8(5) 25_565 23_455 y
N3 Fe1 N1 88.2(5) 15_665 23_455 y
N3 Fe1 N1 91.8(5) 15_665 . y
N3 Fe1 N1 91.8(5) 23_455 23_455 y
N3 Fe1 N1 88.2(5) 25_565 . y
N3 Fe1 N1 88.2(5) . 23_455 y
N3 Fe1 N1 88.2(5) 23_455 . y
N3 Fe1 N1 91.8(5) . . y
N3 Fe1 N2 93.9(5) 23_455 15_665 y
N3 Fe1 N2 86.1(5) . . y
N3 Fe1 N2 93.9(5) . 15_665 y
N3 Fe1 N2 86.1(5) 25_565 15_665 y
N3 Fe1 N2 93.9(5) 25_565 . y
N3 Fe1 N2 86.1(5) 15_665 15_665 y
N3 Fe1 N2 86.1(5) 23_455 . y
N3 Fe1 N2 93.9(5) 15_665 . y
N3 Fe1 N3 172.3(10) . 23_455 y
N3 Fe1 N3 180.0 25_565 . y
N3 Fe1 N3 7.7(10) 25_565 23_455 y
N3 Fe1 N3 180.0 15_665 23_455 y
N3 Fe1 N3 7.7(10) 15_665 . y
N3 Fe1 N3 172.3(10) 25_565 15_665 y
N5 Fe1 N1 90.5(5) 32_454 23_455 y
N5 Fe1 N1 89.5(5) 14_556 23_455 y
N5 Fe1 N1 90.5(5) 14_556 . y
N5 Fe1 N1 90.5(5) 8_666 . y
N5 Fe1 N1 89.5(5) 32_454 . y
N5 Fe1 N1 89.5(5) 8_666 23_455 y
N5 Fe1 N1 89.5(5) 22_564 . y
N5 Fe1 N1 90.5(5) 22_564 23_455 y
N5 Fe1 N2 83.1(4) 22_564 . y
N5 Fe1 N2 96.9(4) 32_454 . y
N5 Fe1 N2 83.1(4) 14_556 15_665 y
N5 Fe1 N2 83.1(4) 8_666 . y
N5 Fe1 N2 96.9(4) 14_556 . y
N5 Fe1 N2 96.9(4) 8_666 15_665 y
N5 Fe1 N2 83.1(4) 32_454 15_665 y
N5 Fe1 N2 96.9(4) 22_564 15_665 y
N5 Fe1 N3 176.7(10) 22_564 15_665 y
N5 Fe1 N3 10.9(3) 14_556 . y
N5 Fe1 N3 169.1(3) 14_556 25_565 y
N5 Fe1 N3 3.3(10) 32_454 25_565 y
N5 Fe1 N3 3.3(10) 14_556 15_665 y
N5 Fe1 N3 176.7(10) 8_666 25_565 y
N5 Fe1 N3 169.1(3) 22_564 . y
N5 Fe1 N3 10.9(3) 22_564 25_565 y
N5 Fe1 N3 169.1(3) 8_666 23_455 y
N5 Fe1 N3 3.3(10) 22_564 23_455 y
N5 Fe1 N3 10.9(3) 32_454 23_455 y
N5 Fe1 N3 176.7(10) 32_454 . y
N5 Fe1 N3 169.1(3) 32_454 15_665 y
N5 Fe1 N3 10.9(3) 8_666 15_665 y
N5 Fe1 N3 176.7(10) 14_556 23_455 y
N5 Fe1 N3 3.3(10) 8_666 . y
N5 Fe1 N5 166.1(9) 8_666 22_564 y
N5 Fe1 N5 180.0 32_454 8_666 y
N5 Fe1 N5 13.9(9) 32_454 22_564 y
N5 Fe1 N5 180.0 14_556 22_564 y
N5 Fe1 N5 13.9(9) 14_556 8_666 y
N5 Fe1 N5 166.1(9) 32_454 14_556 y
C1 Ni1 C1 89.9 . 2_655 y
C1 Ni1 C1 176.4(3) 6_665 . y
C1 Ni1 C1 89.9 6_665 2_655 y
C1 Ni1 C1 176.4(3) 3_565 2_655 y
C1 Ni1 C1 89.9 3_565 . y
C1 Ni1 C1 89.9 6_665 3_565 y
C2 Ni2 C2 180.0 6_675 . y
C2 Ni2 C2 90.00(10) 13_575 6_675 y
C2 Ni2 C2 90.00(10) 13_575 . y
C2 Ni2 C2 90.00(10) 12_655 . y
C2 Ni2 C2 90.00(10) 12_655 6_675 y
C2 Ni2 C2 180.0 13_575 12_655 y
C1 N1 Fe1 168.9(4) . . ?
C2 N2 Fe1 180.0 . . ?
H3 O3 H3 111.4 . 13_575 ?
N2 C2 Ni2 180.0 . . ?
N1 C1 Ni1 177.0(4) . 3_565 ?
H2b O2 H2a 111.1 . . ?
N4 C7 C5 108.0 . . ?
C8 C7 C5 128.4 . . ?
C8 C7 N4 123.5 . . ?
C4 C5 C7 108.0 . . ?
C6 C5 C7 136.4(9) . . ?
C6 C5 C4 113.8(8) . . ?
N3 C4 C5 108.000000000(15) . . ?
C3 C4 C5 139.6(11) . . ?
C3 C4 N3 112.4(11) . . ?
C4 N3 Fe1 139.2(8) . 23_455 ?
N4 N3 Fe1 111.9(8) . 23_455 ?
N4 N3 C4 108.0 . . ?
N3 N4 C7 108.0 . . ?
H4 N4 C7 126.0(5) . . ?
H4 N4 N3 126.0(5) . . ?
H3a C3 C4 109.5 . . ?
H3b C3 C4 109.5 . . ?
H3b C3 H3a 109.5 . . ?
H3c C3 C4 109.5 . . ?
H3c C3 H3a 109.5 . . ?
H3c C3 H3b 109.5 . . ?
H8a C8 C7 109.5 . . ?
H8b C8 C7 109.5 . . ?
H8b C8 H8a 109.5 . . ?
H8c C8 C7 109.5 . . ?
H8c C8 H8a 109.5 . . ?
H8c C8 H8b 109.5 . . ?
C5 C6 C5 99.2(10) 14_556 . ?
H6b C6 C5 109.4(7) 14_556 14_556 ?
H6b C6 C5 96.4(7) . 14_556 ?
H6b C6 C5 109.4(7) . . ?
H6b C6 C5 96.4(7) 14_556 . ?
H6b C6 H6b 16.70(3) 14_556 . ?
H6a C6 C5 109.4(5) . . ?
H6a C6 C5 132.6(6) . 14_556 ?
H6a C6 C5 132.6(6) 14_556 . ?
H6a C6 C5 109.4(5) 14_556 14_556 ?
H6a C6 H6b 104.1 . 14_556 ?
H6a C6 H6b 108.0 . . ?
H6a C6 H6b 104.1 14_556 . ?
H6a C6 H6b 108.0 14_556 14_556 ?
H6a C6 H6a 26.1 . 14_556 ?
C10 C6 C5 111.0(6) . . ?
C10 C6 C5 23.2(5) 14_556 . ?
C10 C6 C5 23.2(5) . 14_556 ?
C10 C6 C5 111.0(6) 14_556 14_556 ?
C10 C6 H6b 125.2(6) 14_556 . ?
C10 C6 H6b 109.4(6) . . ?
C10 C6 H6b 125.2(6) . 14_556 ?
C10 C6 H6b 109.4(6) 14_556 14_556 ?
C10 C6 H6a 87.4(6) . 14_556 ?
C10 C6 H6a 109.4(6) . . ?
C10 C6 H6a 109.4(6) 14_556 14_556 ?
C10 C6 H6a 87.4(6) 14_556 . ?
C10 C6 C10 114.1(12) 14_556 . ?
H1b O1 H1a 104.5 . . ?
N6 C9 C10 105.0(10) . . ?
C13 C9 C10 136.9(13) . . ?
C13 C9 N6 118.0(13) . . ?
C9 C10 C6 113.8(11) . . ?
C11 C10 C6 138.8(11) . . ?
C11 C10 C9 106.1(9) . . ?
N5 C11 C10 112.4(9) . . ?
C12 C11 C10 118.8(13) . . ?
C12 C11 N5 128.7(13) . . ?
C11 N5 Fe1 135.3(10) . 22_565 ?
N6 N5 Fe1 123.1(10) . 22_565 ?
N6 N5 C11 101.5(9) . . ?
N5 N6 C9 115.0(11) . . ?
H6 N6 C9 122.5(8) . . ?
H6 N6 N5 122.5(8) . . ?
H12a C12 C11 109.5 . . ?
H12b C12 C11 109.5 . . ?
H12b C12 H12a 109.5 . . ?
H12c C12 C11 109.5 . . ?
H12c C12 H12a 109.5 . . ?
H12c C12 H12b 109.5 . . ?
H13a C13 C9 109.5 . . ?
H13b C13 C9 109.5 . . ?
H13b C13 H13a 109.5 . . ?
H13c C13 C9 109.5 . . ?
H13c C13 H13a 109.5 . . ?
H13c C13 H13b 109.5 . . ?

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
N4 H4 O2 0.8800 1.852(12) 2.661(10) 152.0(4) .
N6 H6 O2 0.8800 1.974(15) 2.829(13) 163.9(5) 8_666

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N3 C4 C5 167.6(9) 23_455 . . . ?
Fe1 N3 C4 C5 167.6(9) 15_665 . . . ?
Fe1 N3 C4 C5 167.6(9) . . . . ?
Fe1 N3 C4 C5 167.6(9) 25_565 . . . ?
Fe1 N3 C4 C3 -14(2) 25_565 . . . ?
Fe1 N3 C4 C3 -14(2) 15_665 . . . ?
Fe1 N3 C4 C3 -14(2) 23_455 . . . ?
Fe1 N3 C4 C3 -14(2) . . . . ?
Fe1 N3 N4 C7 -171.3(4) 15_665 . . . ?
Fe1 N3 N4 C7 -171.3(4) 23_455 . . . ?
Fe1 N3 N4 C7 -171.3(4) . . . . ?
Fe1 N3 N4 C7 -171.3(4) 25_565 . . . ?
Fe1 N5 C11 C10 -177.4(13) 22_565 . . . ?
Fe1 N5 C11 C10 -177.4(13) 14_556 . . . ?
Fe1 N5 C11 C10 -177.4(13) 8_666 . . . ?
Fe1 N5 C11 C10 -177.4(13) 32_455 . . . ?
Fe1 N5 C11 C12 4(2) 32_455 . . . ?
Fe1 N5 C11 C12 4(2) 14_556 . . . ?
Fe1 N5 C11 C12 4(2) 22_565 . . . ?
Fe1 N5 C11 C12 4(2) 8_666 . . . ?
Fe1 N5 N6 C9 177.2(10) 14_556 . . . ?
Fe1 N5 N6 C9 177.2(10) 22_565 . . . ?
Fe1 N5 N6 C9 177.2(10) 8_666 . . . ?
Fe1 N5 N6 C9 177.2(10) 32_455 . . . ?
C7 C5 C4 N3 -0.0(15) . . . . ?
C7 C5 C4 C3 -178.3(12) . . . . ?
C7 C5 C6 C5 6.2(11) . . . 14_556 ?
C7 C5 C6 C10 26.9(15) . . . . ?
C7 C5 C6 C10 129(2) . . . 14_556 ?
C7 N4 N3 C4 -0.0(15) . . . . ?
C5 C4 N3 N4 0.0(15) . . . . ?
C5 C6 C5 C4 156.2(11) . . 14_556 14_556 ?
C5 C6 C10 C9 -136(3) . . 14_556 14_556 ?
C5 C6 C10 C9 73.3(11) . . . . ?
C5 C6 C10 C11 -122.1(12) . . . . ?
C5 C6 C10 C11 60(3) . . 14_556 14_556 ?
C6 C10 C9 N6 169.0(12) . . . . ?
C6 C10 C9 N6 169.0(12) 14_556 . . . ?
C6 C10 C9 C13 -13.6(19) . . . . ?
C6 C10 C9 C13 -13.6(19) 14_556 . . . ?
C6 C10 C11 N5 -165.9(16) . . . . ?
C6 C10 C11 N5 -165.9(16) 14_556 . . . ?
C6 C10 C11 C12 13(2) . . . . ?
C6 C10 C11 C12 13(2) 14_556 . . . ?
C9 C10 C11 N5 -0.6(18) . . . . ?
C9 C10 C11 C12 178.1(12) . . . . ?
C9 N6 N5 C11 -1.7(17) . . . . ?
C10 C11 N5 N6 1.4(16) . . . . ?


_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O2 H2a 1 0.8500 0.0200 -0.0024
H2b O2 1 0.8500 0.0200 0.0015
H2b H2a 1 1.3490 0.0400 -0.0535

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_site_symmetry_2
_restr_equal_distance_class_id
C6 C5 1 1
C6 C10 1 1

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
1 0.0010 1.5479 0.0003 0.0003

loop_
_restr_RIGU_atom_site_label_1
_restr_RIGU_atom_site_label_2
_restr_RIGU_target_weight_param
_restr_RIGU_U13_diff
_restr_RIGU_U23_diff
_restr_RIGU_U33_diff
C7 C5 0.001000 0.000496 0.000260 0.000093
C7 C4 0.001000 0.000450 0.000297 0.001304
C7 N3 0.001000 -0.000062 -0.000258 0.001843
C7 N4 0.001000 0.000109 -0.000299 0.000379
C7 C8 0.001000 0.000155 0.000161 -0.000360
C7 C6 0.001000 -0.000830 0.000826 0.000188
C5 C4 0.001000 0.000356 0.000194 -0.000443
C5 N3 0.001000 -0.000339 -0.000813 0.000188
C5 N4 0.001000 -0.000450 -0.002247 0.000137
C5 C3 0.001000 0.001308 0.002166 -0.000567
C5 C8 0.001000 0.001251 -0.001347 -0.001690
C5 C6 0.001000 0.000171 0.000365 -0.000476
C5 C10 0.001000 0.001791 0.000199 0.001092
C4 N3 0.001000 0.000015 -0.000113 -0.000078
C4 N4 0.001000 0.000376 -0.001348 0.000245
C4 C3 0.001000 -0.000066 0.000494 -0.000185
C4 C6 0.001000 -0.001151 0.001137 -0.000099
N3 N4 0.001000 -0.000354 0.000231 0.000414
N3 C3 0.001000 -0.000112 -0.000871 -0.001032
N4 C8 0.001000 -0.000719 0.001736 -0.002512
C6 C9 0.001000 0.000751 -0.001332 0.000421
C6 C10 0.001000 0.000199 0.000361 0.000973
C6 C11 0.001000 -0.000329 0.000061 0.001547
C9 C10 0.001000 -0.000063 0.000206 0.000366
C9 C11 0.001000 0.000903 0.000787 0.001161
C9 N5 0.001000 0.000128 -0.000219 0.001341
C9 N6 0.001000 0.000082 -0.000484 0.000473
C9 C13 0.001000 0.000417 -0.000394 -0.000175
C10 C11 0.001000 0.000202 -0.000281 -0.000145
C10 N5 0.001000 -0.000439 -0.000821 0.001153
C10 N6 0.001000 -0.000423 -0.001423 0.000909
C10 C12 0.001000 -0.000253 0.000433 0.001555
C10 C13 0.001000 0.001556 -0.001263 -0.001358
C11 N5 0.001000 0.000016 0.000122 0.000056
C11 N6 0.001000 0.000413 -0.001247 0.000024
C11 C12 0.001000 -0.000501 -0.000295 0.000023
N5 N6 0.001000 -0.000172 0.000146 0.000328
N5 C12 0.001000 0.000057 0.000689 -0.000135
N6 C13 0.001000 -0.000769 0.000173 -0.001722

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
C7 0.0050
C5 0.0050
C4 0.0050
N3 0.0050
N4 0.0050
C3 0.0050
C8 0.0050
C6 0.0050
C9 0.0050
C10 0.0050
C11 0.0050
N5 0.0050
N6 0.0050
C12 0.0010
C12 0.0050
C13 0.0050

