# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_18101511_sq
_database_code_depnum_ccdc_archive 'CCDC 1892975'
loop_
_audit_author_name
_audit_author_address
Liu
;Sun Yat-sen University
China
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2020-04-14 downloaded from the CCDC.
;
_audit_creation_date             2019-01-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C96 H48 Fe4 N8 Ni2 O20)'
_chemical_formula_sum            'C48 H24 Fe2 N4 Ni O10'
_chemical_formula_weight         987.12
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     20181004-3
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'
Fe Fe 0.3463 0.8444 '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'
Ni Ni 0.3393 1.1124 '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'

_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      orthorhombic
_space_group_IT_number           65
_space_group_name_H-M_alt        'C m m m'
_space_group_name_Hall           '-C 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'

_cell_length_a                   6.8484(3)
_cell_length_b                   32.9205(14)
_cell_length_c                   16.5679(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3735.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4880
_cell_measurement_temperature    200.01(10)
_cell_measurement_theta_max      29.1940
_cell_measurement_theta_min      3.8660
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.936
_exptl_absorpt_coefficient_mu    0.670
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.878
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10245
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.490
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -19.00  28.00   1.00   60.00    --  -12.17 -99.00 -60.00   47
  2  ω     58.00  85.00   1.00   60.00    --   13.26 178.00   0.00   27
  3  ω    -28.00  80.00   1.00   60.00    --   13.26  19.00-120.00  108
  4  ω     20.00  45.00   1.00   60.00    --   13.26 -77.00-180.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0176281000
_diffrn_orient_matrix_UB_12      -0.0178540000
_diffrn_orient_matrix_UB_13      -0.0228068000
_diffrn_orient_matrix_UB_21      -0.0277144000
_diffrn_orient_matrix_UB_22      -0.0120624000
_diffrn_orient_matrix_UB_23      0.0336111000
_diffrn_orient_matrix_UB_31      -0.0981967000
_diffrn_orient_matrix_UB_32      0.0002130000
_diffrn_orient_matrix_UB_33      -0.0135522000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1992
_reflns_number_total             2437
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         2437
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0450
_refine_ls_restrained_S_all      1.080
_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)+(0.0679P)²+2.3175P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1333
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C7(H7), C8(H8)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Ni1 Ni 0.500000 0.500000 1.000000 0.0191(2) Uani 1 8 d S T P . .
Fe1 Fe 0.750000 0.250000 0.500000 0.01517(19) Uani 1 4 d S T P . .
O1 O 0.6617(3) 0.28930(5) 0.58560(11) 0.0370(5) Uani 1 1 d . . . . .
O2 O 1.000000 0.27746(7) 0.500000 0.0095(5) Uani 1 4 d S T P . .
N1 N 0.500000 0.44087(11) 1.000000 0.0227(8) Uani 1 4 d S T P . .
N2 N 0.500000 0.500000 0.8822(2) 0.0237(8) Uani 1 4 d S T P . .
C1 C 0.500000 0.37329(11) 0.9596(2) 0.0446(10) Uani 1 2 d S T P . .
H1 H 0.500000 0.350604 0.926119 0.054 Uiso 1 2 calc RS T P . .
C2 C 0.500000 0.41507(10) 0.9344(2) 0.0300(8) Uani 1 2 d S T P . .
C3 C 0.500000 0.42668(10) 0.8544(2) 0.0264(7) Uani 1 2 d S T P . .
C4 C 0.500000 0.46711(10) 0.8308(2) 0.0275(7) Uani 1 2 d S T P . .
C5 C 0.500000 0.47952(11) 0.7485(2) 0.0400(10) Uani 1 2 d S T P . .
H5 H 0.500000 0.462657 0.703432 0.048 Uiso 1 2 calc RS T P . .
C6 C 0.500000 0.39422(10) 0.7910(2) 0.0295(8) Uani 1 2 d S T P . .
C7 C 0.6722(5) 0.37915(10) 0.7617(2) 0.0554(9) Uani 1 1 d . . . . .
H7 H 0.790236 0.388760 0.781881 0.067 Uiso 1 1 calc R . . . .
C8 C 0.6712(4) 0.34949(10) 0.7019(2) 0.0535(9) Uani 1 1 d . . . . .
H8 H 0.788997 0.339945 0.681403 0.064 Uiso 1 1 calc R . . . .
C9 C 0.500000 0.33422(10) 0.6730(2) 0.0256(7) Uani 1 2 d S T P . .
C10 C 0.500000 0.30153(10) 0.6103(2) 0.0241(7) Uani 1 2 d S T P . .


_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
Ni1 N1 1.946(3) 9_667 ?
Ni1 N1 1.947(3) . ?
Ni1 N2 1.951(4) 9_667 ?
Ni1 N2 1.951(4) . ?
Fe1 O1 2.0125(16) 10_556 ?
Fe1 O1 2.0125(16) . ?
Fe1 O1 2.0125(16) 6_655 ?
Fe1 O1 2.0125(16) 13_656 ?
Fe1 O2 1.9361(11) . ?
Fe1 O2 1.9361(11) 13_656 ?
O1 C10 1.248(2) . ?
N1 C2 1.379(4) 10_557 ?
N1 C2 1.379(4) . ?
N2 C4 1.378(4) 2_665 ?
N2 C4 1.378(4) . ?
C1 C1 1.340(8) 10_557 ?
C1 C2 1.437(5) . ?
C2 C3 1.379(5) . ?
C3 C4 1.388(4) . ?
C3 C6 1.499(4) . ?
C4 C5 1.423(5) . ?
C5 C5 1.348(7) 2_665 ?
C6 C7 1.368(3) 11_655 ?
C6 C7 1.368(3) . ?
C7 C8 1.391(4) . ?
C8 C9 1.363(3) . ?
C9 C10 1.496(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 180.0 9_667 . ?
N1 Ni1 N2 90.0 . . ?
N1 Ni1 N2 90.0 9_667 . ?
N1 Ni1 N2 90.0 9_667 9_667 ?
N1 Ni1 N2 90.0 . 9_667 ?
N2 Ni1 N2 180.0 9_667 . ?
O1 Fe1 O1 89.62(12) 13_656 6_655 ?
O1 Fe1 O1 90.39(12) 6_655 . ?
O1 Fe1 O1 89.61(12) 10_556 . ?
O1 Fe1 O1 180.00(9) 10_556 6_655 ?
O1 Fe1 O1 180.00(9) 13_656 . ?
O1 Fe1 O1 90.38(12) 13_656 10_556 ?
O2 Fe1 O1 88.02(7) 13_656 6_655 ?
O2 Fe1 O1 91.98(7) . 13_656 ?
O2 Fe1 O1 88.02(7) . 10_556 ?
O2 Fe1 O1 91.98(7) . 6_655 ?
O2 Fe1 O1 91.98(7) 13_656 10_556 ?
O2 Fe1 O1 88.02(7) 13_656 13_656 ?
O2 Fe1 O1 91.98(7) 13_656 . ?
O2 Fe1 O1 88.02(7) . . ?
O2 Fe1 O2 180.0 13_656 . ?
C10 O1 Fe1 134.87(17) . . ?
Fe1 O2 Fe1 124.33(13) . 7_556 ?
C2 N1 Ni1 128.01(18) 10_557 . ?
C2 N1 Ni1 128.01(18) . . ?
C2 N1 C2 104.0(4) 10_557 . ?
C4 N2 Ni1 128.23(19) 2_665 . ?
C4 N2 Ni1 128.23(19) . . ?
C4 N2 C4 103.5(4) . 2_665 ?
C1 C1 C2 106.9(2) 10_557 . ?
N1 C2 C1 111.1(3) . . ?
C3 C2 N1 125.9(3) . . ?
C3 C2 C1 122.9(3) . . ?
C2 C3 C4 122.5(3) . . ?
C2 C3 C6 118.4(3) . . ?
C4 C3 C6 119.1(3) . . ?
N2 C4 C3 125.4(3) . . ?
N2 C4 C5 111.5(3) . . ?
C3 C4 C5 123.1(3) . . ?
C5 C5 C4 106.69(19) 2_665 . ?
C7 C6 C3 120.44(17) 11_655 . ?
C7 C6 C3 120.45(17) . . ?
C7 C6 C7 119.1(3) 11_655 . ?
C6 C7 C8 120.2(3) . . ?
C9 C8 C7 120.9(3) . . ?
C8 C9 C8 118.7(3) 11_655 . ?
C8 C9 C10 120.63(16) 11_655 . ?
C8 C9 C10 120.63(16) . . ?
O1 C10 O1 125.2(3) . 11_655 ?
O1 C10 C9 117.40(15) 11_655 . ?
O1 C10 C9 117.40(15) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.119
_oxdiff_exptl_absorpt_empirical_full_min 0.587
