# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_mo_i06sb178_0m_a_aa
_database_code_depnum_ccdc_archive 'CCDC 1896869'
loop_
_audit_author_name
_audit_author_address
'Merce Font-Bardia'
;Departament de Mineralogia Cristallografia i Diposits Minerals Universitat de Barcelona
Spain
;
_audit_update_record             
;
2019-02-12 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H44 N4 Ni4 O12), 13(H2 O)'
_chemical_formula_sum            'C72 H114 N8 Ni8 O37'
_chemical_formula_weight         2153.39

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

_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.
;

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

_cell_length_a                   13.8143(11)
_cell_length_b                   31.128(3)
_cell_length_c                   11.9196(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5125.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9888
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      24.67

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_F_000             2244
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.095
_exptl_absorpt_coefficient_mu    1.515
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5448
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28130
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_av_R_equivalents  0.0940
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.350
_diffrn_reflns_theta_max         24.661
_diffrn_reflns_theta_full        24.661
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4339
_reflns_number_gt                3649
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_max     0.993
_reflns_Friedel_fraction_full    0.993

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0649P)²+2.9525P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(3)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         4339
_refine_ls_number_parameters     283
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1181
_refine_ls_wR_factor_gt          0.1093
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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_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 0.58421(6) 0.29660(3) 0.34049(7) 0.0186(2) Uani 1 1 d . . . . .
Ni2 Ni 0.40950(7) 0.35972(3) 0.33602(7) 0.0209(3) Uani 1 1 d . . . . .
O1 O 0.4368(3) 0.29536(14) 0.3335(4) 0.0180(10) Uani 1 1 d . . . . .
O2 O 0.5606(3) 0.36179(15) 0.3325(4) 0.0208(10) Uani 1 1 d . . . . .
O3 O 0.7309(3) 0.29671(17) 0.3092(4) 0.0226(11) Uani 1 1 d . . . . .
O4 O 0.7348(4) 0.34889(17) 0.1798(4) 0.0301(13) Uani 1 1 d . . . . .
O5 O 0.3890(4) 0.37441(16) 0.5064(4) 0.0239(12) Uani 1 1 d . . . . .
O6 O 0.3880(4) 0.42386(17) 0.3787(4) 0.0314(13) Uani 1 1 d . . . . .
N1 N 0.5602(4) 0.2321(2) 0.3699(4) 0.0210(14) Uani 1 1 d . . . . .
N2 N 0.6093(5) 0.3130(2) 0.5060(5) 0.0267(16) Uani 1 1 d . . . . .
C1 C 0.6291(6) 0.1998(3) 0.3734(6) 0.0274(18) Uani 1 1 d . . . . .
H1 H 0.692870 0.206127 0.354380 0.033 Uiso 1 1 calc R U . . .
C2 C 0.6051(7) 0.1589(3) 0.4044(7) 0.043(2) Uani 1 1 d . . . . .
H2 H 0.652287 0.137629 0.407757 0.051 Uiso 1 1 calc R U . . .
C3 C 0.5111(8) 0.1496(3) 0.4302(8) 0.047(2) Uani 1 1 d . . . . .
H3 H 0.493915 0.121884 0.451120 0.057 Uiso 1 1 calc R U . . .
C4 C 0.4402(6) 0.1821(3) 0.4253(6) 0.033(2) Uani 1 1 d . . . . .
H4 H 0.375909 0.176009 0.442168 0.039 Uiso 1 1 calc R U . . .
C5 C 0.4677(6) 0.2230(2) 0.3952(6) 0.0243(18) Uani 1 1 d . . . . .
C6 C 0.3944(6) 0.2594(2) 0.3895(5) 0.0233(17) Uani 1 1 d . . . . .
H6 H 0.337674 0.249749 0.347077 0.028 Uiso 1 1 calc R U . . .
C7 C 0.3632(5) 0.2714(3) 0.5071(6) 0.0264(18) Uani 1 1 d . . . . .
H7A H 0.336559 0.246678 0.543882 0.040 Uiso 1 1 calc R U . . .
H7B H 0.315164 0.293659 0.503503 0.040 Uiso 1 1 calc R U . . .
H7C H 0.418241 0.281593 0.548599 0.040 Uiso 1 1 calc R U . . .
C8 C 0.6224(5) 0.2851(2) 0.5912(6) 0.0227(17) Uani 1 1 d . . . . .
H8 H 0.620108 0.255739 0.576345 0.027 Uiso 1 1 calc R U . . .
C9 C 0.6394(6) 0.2989(3) 0.7012(6) 0.0285(18) Uani 1 1 d . . . . .
H9 H 0.652788 0.279227 0.757941 0.034 Uiso 1 1 calc R U . . .
C10 C 0.6356(6) 0.3431(3) 0.7238(6) 0.0277(18) Uani 1 1 d . . . . .
H10 H 0.641545 0.353561 0.796567 0.033 Uiso 1 1 calc R U . . .
C11 C 0.6226(6) 0.3706(3) 0.6331(6) 0.0288(19) Uani 1 1 d . . . . .
H11 H 0.621606 0.400055 0.645779 0.035 Uiso 1 1 calc R U . . .
C12 C 0.6114(6) 0.3560(2) 0.5274(6) 0.0253(19) Uani 1 1 d . . . . .
C13 C 0.6061(6) 0.3853(3) 0.4246(6) 0.0285(18) Uani 1 1 d . . . . .
H13 H 0.563977 0.409600 0.443527 0.034 Uiso 1 1 calc R U . . .
C14 C 0.7043(6) 0.4029(3) 0.3986(7) 0.034(2) Uani 1 1 d . . . . .
H14A H 0.720715 0.424652 0.452558 0.051 Uiso 1 1 calc R U . . .
H14B H 0.704101 0.415255 0.324790 0.051 Uiso 1 1 calc R U . . .
H14C H 0.751187 0.380196 0.401844 0.051 Uiso 1 1 calc R U . . .
C15 C 0.7726(6) 0.3223(3) 0.2437(6) 0.0290(18) Uani 1 1 d . . . . .
C16 C 0.8814(6) 0.3196(3) 0.2439(6) 0.033(2) Uani 1 1 d . . . . .
H16A H 0.906484 0.335855 0.305932 0.049 Uiso 1 1 calc R U . . .
H16B H 0.906132 0.331220 0.174970 0.049 Uiso 1 1 calc R U . . .
H16C H 0.900957 0.290173 0.250939 0.049 Uiso 1 1 calc R U . . .
C17 C 0.3810(6) 0.4129(3) 0.4837(6) 0.0269(18) Uani 1 1 d . . . . .
C18 C 0.3664(8) 0.4469(3) 0.5735(8) 0.052(3) Uani 1 1 d . . . . .
H18A H 0.339956 0.433808 0.639688 0.078 Uiso 1 1 calc R U . . .
H18B H 0.322606 0.468447 0.546360 0.078 Uiso 1 1 calc R U . . .
H18C H 0.427525 0.459929 0.591271 0.078 Uiso 1 1 calc R U . . .
O1W O 0.457(2) 0.0797(10) 0.650(3) 0.0691(15) Uani 0.25 1 d . . P . .
H1WA H 0.500422 0.079100 0.679700 0.083 Uiso 0.25 1 d . U P . .
H1WB H 0.446980 0.045206 0.630400 0.083 Uiso 0.25 1 d . U P . .
O2W O 0.3484(11) 0.0756(5) 0.8553(13) 0.0691(15) Uani 0.5 1 d . . P . .
O3W O 0.000000 0.0223(4) 0.750000 0.0691(15) Uani 1 2 d S T P . .
H3WA H 0.000000 0.048800 0.710700 0.083 Uiso 0.5 1 d . U P . .
O4W O 0.1311(6) 0.0172(2) 0.3898(6) 0.0691(15) Uani 1 1 d . . . . .
H4WA H 0.194000 0.007303 0.378206 0.083 Uiso 1 1 d . U . . .
H4WB H 0.098109 0.033303 0.338907 0.083 Uiso 1 1 d . U . . .
O5W O 0.3028(12) 0.0065(5) 0.2686(13) 0.0691(15) Uani 0.5 1 d . . P . .
O6W O 0.399(2) 0.0459(10) 0.066(2) 0.0691(15) Uani 0.25 1 d . . P . .
H6WA H 0.452459 0.046465 0.065400 0.083 Uiso 0.25 1 d . U P . .
H6WB H 0.376565 0.072465 0.026200 0.083 Uiso 0.25 1 d . U P . .
O7W O 0.574(2) 0.0393(9) 0.089(2) 0.0691(15) Uani 0.25 1 d . . 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 O1 2.039(4) . ?
Ni1 O2 2.057(5) . ?
Ni1 O3 2.060(5) . ?
Ni1 N1 2.065(6) . ?
Ni1 N2 2.067(6) . ?
Ni1 O1 2.095(5) 3_655 ?
Ni1 Ni2 2.8799(12) 3_655 ?
Ni2 O4 2.030(5) 3_655 ?
Ni2 O1 2.039(5) . ?
Ni2 O2 2.051(5) 3_655 ?
Ni2 O6 2.082(5) . ?
Ni2 O2 2.089(5) . ?
Ni2 O5 2.101(5) . ?
Ni2 C17 2.448(8) . ?
O1 C6 1.428(8) . ?
O2 C13 1.462(9) . ?
O3 C15 1.256(9) . ?
O4 C15 1.240(9) . ?
O5 C17 1.232(9) . ?
O6 C17 1.301(9) . ?
N1 C5 1.344(10) . ?
N1 C1 1.384(9) . ?
N2 C8 1.350(9) . ?
N2 C12 1.361(10) . ?
C1 C2 1.367(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.366(13) . ?
C2 H2 0.9300 . ?
C3 C4 1.409(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.520(10) . ?
C6 C7 1.513(9) . ?
C6 H6 0.9800 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.400(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.403(11) . ?
C9 H9 0.9300 . ?
C10 C11 1.391(10) . ?
C10 H10 0.9300 . ?
C11 C12 1.348(10) . ?
C11 H11 0.9300 . ?
C12 C13 1.530(10) . ?
C13 C14 1.496(11) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.505(12) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.519(12) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
O1W H1WA 0.70(3) . ?
O1W H1WB 1.11(3) . ?
O3W H3WA 0.949(10) . ?
O4W H4WA 0.932(8) . ?
O4W H4WB 0.910(7) . ?
O6W H6WA 0.74(3) . ?
O6W H6WB 1.00(3) . ?

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 Ni1 O2 81.88(18) . . ?
O1 Ni1 O3 167.20(17) . . ?
O2 Ni1 O3 98.4(2) . . ?
O1 Ni1 N1 80.1(2) . . ?
O2 Ni1 N1 160.3(2) . . ?
O3 Ni1 N1 101.0(2) . . ?
O1 Ni1 N2 102.2(2) . . ?
O2 Ni1 N2 80.0(2) . . ?
O3 Ni1 N2 90.4(2) . . ?
N1 Ni1 N2 96.1(2) . . ?
O1 Ni1 O1 79.70(19) . 3_655 ?
O2 Ni1 O1 87.16(18) . 3_655 ?
O3 Ni1 O1 87.53(17) . 3_655 ?
N1 Ni1 O1 97.34(18) . 3_655 ?
N2 Ni1 O1 166.6(2) . 3_655 ?
O1 Ni1 Ni2 90.76(13) . 3_655 ?
O2 Ni1 Ni2 45.42(13) . 3_655 ?
O3 Ni1 Ni2 80.62(14) . 3_655 ?
N1 Ni1 Ni2 142.38(14) . 3_655 ?
N2 Ni1 Ni2 121.55(18) . 3_655 ?
O1 Ni1 Ni2 45.04(12) 3_655 3_655 ?
O4 Ni2 O1 91.0(2) 3_655 . ?
O4 Ni2 O2 96.4(2) 3_655 3_655 ?
O1 Ni2 O2 88.81(18) . 3_655 ?
O4 Ni2 O6 92.4(2) 3_655 . ?
O1 Ni2 O6 166.52(18) . . ?
O2 Ni2 O6 103.77(19) 3_655 . ?
O4 Ni2 O2 169.8(2) 3_655 . ?
O1 Ni2 O2 81.11(18) . . ?
O2 Ni2 O2 77.2(2) 3_655 . ?
O6 Ni2 O2 96.8(2) . . ?
O4 Ni2 O5 89.6(2) 3_655 . ?
O1 Ni2 O5 104.65(19) . . ?
O2 Ni2 O5 165.18(19) 3_655 . ?
O6 Ni2 O5 62.34(19) . . ?
O2 Ni2 O5 98.49(19) . . ?
O4 Ni2 C17 91.2(2) 3_655 . ?
O1 Ni2 C17 134.8(2) . . ?
O2 Ni2 C17 135.7(2) 3_655 . ?
O6 Ni2 C17 32.1(2) . . ?
O2 Ni2 C17 98.9(2) . . ?
O5 Ni2 C17 30.2(2) . . ?
O4 Ni2 Ni1 81.27(15) 3_655 3_655 ?
O1 Ni2 Ni1 46.64(13) . 3_655 ?
O2 Ni2 Ni1 45.58(13) 3_655 3_655 ?
O6 Ni2 Ni1 146.84(13) . 3_655 ?
O2 Ni2 Ni1 88.63(13) . 3_655 ?
O5 Ni2 Ni1 149.17(15) . 3_655 ?
C17 Ni2 Ni1 172.48(19) . 3_655 ?
C6 O1 Ni2 133.4(4) . . ?
C6 O1 Ni1 113.9(4) . . ?
Ni2 O1 Ni1 99.51(19) . . ?
C6 O1 Ni1 114.9(4) . 3_655 ?
Ni2 O1 Ni1 88.32(17) . 3_655 ?
Ni1 O1 Ni1 100.27(19) . 3_655 ?
C13 O2 Ni2 131.7(4) . 3_655 ?
C13 O2 Ni1 113.0(4) . . ?
Ni2 O2 Ni1 89.00(18) 3_655 . ?
C13 O2 Ni2 115.5(4) . . ?
Ni2 O2 Ni2 102.7(2) 3_655 . ?
Ni1 O2 Ni2 97.29(19) . . ?
C15 O3 Ni1 124.4(5) . . ?
C15 O4 Ni2 125.6(5) . 3_655 ?
C17 O5 Ni2 90.6(4) . . ?
C17 O6 Ni2 89.6(5) . . ?
C5 N1 C1 119.7(6) . . ?
C5 N1 Ni1 113.3(5) . . ?
C1 N1 Ni1 126.9(5) . . ?
C8 N2 C12 119.3(6) . . ?
C8 N2 Ni1 125.5(5) . . ?
C12 N2 Ni1 115.2(5) . . ?
C2 C1 N1 121.1(8) . . ?
C2 C1 H1 119.4 . . ?
N1 C1 H1 119.4 . . ?
C3 C2 C1 119.2(9) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 120.0(9) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 118.9(8) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 121.0(7) . . ?
N1 C5 C6 117.8(6) . . ?
C4 C5 C6 121.1(7) . . ?
O1 C6 C7 110.8(6) . . ?
O1 C6 C5 109.4(6) . . ?
C7 C6 C5 109.4(6) . . ?
O1 C6 H6 109.1 . . ?
C7 C6 H6 109.1 . . ?
C5 C6 H6 109.1 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 121.9(7) . . ?
N2 C8 H8 119.0 . . ?
C9 C8 H8 119.0 . . ?
C8 C9 C10 118.4(7) . . ?
C8 C9 H9 120.8 . . ?
C10 C9 H9 120.8 . . ?
C11 C10 C9 117.3(6) . . ?
C11 C10 H10 121.3 . . ?
C9 C10 H10 121.3 . . ?
C12 C11 C10 122.3(7) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 C12 N2 120.6(7) . . ?
C11 C12 C13 123.5(7) . . ?
N2 C12 C13 115.8(6) . . ?
O2 C13 C14 114.7(6) . . ?
O2 C13 C12 108.8(6) . . ?
C14 C13 C12 110.0(6) . . ?
O2 C13 H13 107.7 . . ?
C14 C13 H13 107.7 . . ?
C12 C13 H13 107.7 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O4 C15 O3 127.7(8) . . ?
O4 C15 C16 117.3(7) . . ?
O3 C15 C16 115.0(7) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 O6 117.4(7) . . ?
O5 C17 C18 122.3(7) . . ?
O6 C17 C18 120.3(7) . . ?
O5 C17 Ni2 59.1(4) . . ?
O6 C17 Ni2 58.3(4) . . ?
C18 C17 Ni2 177.8(6) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
H1WA O1W H1WB 101(3) . . ?
H4WA O4W H4WB 123.4(9) . . ?
H6WA O6W H6WB 106(3) . . ?

_refine_diff_density_max         1.292
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.099


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile/diethylether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_mo_i06sb173_0m_a_aa
_database_code_depnum_ccdc_archive 'CCDC 1896870'
loop_
_audit_author_name
_audit_author_address
'Merce Font-Bardia'
;Departament de Mineralogia Cristallografia i Diposits Minerals Universitat de Barcelona
Spain
;
_audit_update_record             
;
2019-02-12 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C36 H44 N4 Ni4 O12), H2 O, 5(C H3 O)'
_chemical_formula_sum            'C77 H109 N8 Ni8 O30'
_chemical_formula_weight         2096.40

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'
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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

_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.
;

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

_cell_length_a                   11.9664(10)
_cell_length_b                   13.8139(11)
_cell_length_c                   14.2301(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2352.3(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9482
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      30.59

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_F_000             1091
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.497
_exptl_crystal_size_mid          0.392
_exptl_crystal_size_min          0.263
_exptl_absorpt_coefficient_mu    1.643
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6348
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            57141
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.224
_diffrn_reflns_theta_max         30.690
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             7236
_reflns_number_gt                6981
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_max     0.987
_reflns_Friedel_fraction_full    0.999

_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0290P)²+4.3835P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.07(2)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         7236
_refine_ls_number_parameters     296
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1076
_refine_ls_wR_factor_gt          0.1069
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_restrained_S_all      1.209
_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_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 0.59058(4) 0.58375(3) 0.39565(3) 0.01090(10) Uani 1 1 d . . . . .
Ni2 Ni 0.58475(5) 0.40845(4) 0.25728(4) 0.01619(12) Uani 1 1 d . . . . .
O1 O 0.5808(3) 0.43645(18) 0.39857(19) 0.0134(3) Uani 1 1 d . . . . .
O2 O 0.5854(3) 0.56090(18) 0.25312(19) 0.0134(3) Uani 1 1 d . . . . .
O4 O 0.4307(3) 0.7355(2) 0.2834(2) 0.0201(6) Uani 1 1 d . . . . .
O3 O 0.5627(3) 0.7299(2) 0.3977(2) 0.0193(6) Uani 1 1 d . . . . .
O6 O 0.6296(3) 0.3826(3) 0.1161(3) 0.0310(8) Uani 1 1 d . . . . .
O5 O 0.7554(3) 0.3861(2) 0.2263(2) 0.0231(7) Uani 1 1 d . . . . .
N1 N 0.6199(3) 0.5602(2) 0.5363(2) 0.0120(6) Uani 1 1 d . . . . .
N2 N 0.7565(3) 0.6084(2) 0.3608(2) 0.0145(6) Uani 1 1 d . . . . .
C1 C 0.6260(4) 0.6273(3) 0.6047(3) 0.0203(8) Uani 1 1 d . . . . .
H1 H 0.607081 0.690915 0.590300 0.024 Uiso 1 1 calc R U . . .
C2 C 0.6583(6) 0.6064(4) 0.6937(4) 0.0365(13) Uani 1 1 d . . . . .
H2 H 0.663432 0.654887 0.738788 0.044 Uiso 1 1 calc R U . . .
C3 C 0.6839(6) 0.5101(5) 0.7163(4) 0.0443(16) Uani 1 1 d . . . . .
H3 H 0.706921 0.493634 0.776700 0.053 Uiso 1 1 calc R U . . .
C4 C 0.6742(5) 0.4387(4) 0.6461(3) 0.0288(11) Uani 1 1 d . . . . .
H4 H 0.687660 0.373888 0.659757 0.035 Uiso 1 1 calc R U . . .
C5 C 0.6441(3) 0.4673(3) 0.5561(3) 0.0147(7) Uani 1 1 d . . . . .
C6 C 0.6390(4) 0.3952(3) 0.4760(3) 0.0157(8) Uani 1 1 d . . . . .
H6 H 0.596533 0.338700 0.497613 0.019 Uiso 1 1 calc R U . . .
C7 C 0.7541(4) 0.3616(3) 0.4495(3) 0.0200(8) Uani 1 1 d . . . . .
H7A H 0.749500 0.319174 0.396281 0.030 Uiso 1 1 calc R U . . .
H7B H 0.786999 0.327684 0.501514 0.030 Uiso 1 1 calc R U . . .
H7C H 0.799522 0.416633 0.433914 0.030 Uiso 1 1 calc R U . . .
C8 C 0.8422(4) 0.6217(3) 0.4204(3) 0.0214(9) Uani 1 1 d . . . . .
H8 H 0.827661 0.621788 0.484569 0.026 Uiso 1 1 calc R U . . .
C9 C 0.9500(4) 0.6353(4) 0.3909(4) 0.0250(9) Uani 1 1 d . . . . .
H9 H 1.007105 0.645445 0.434160 0.030 Uiso 1 1 calc R U . . .
C10 C 0.9728(5) 0.6337(4) 0.2934(4) 0.0303(11) Uani 1 1 d . . . . .
H10 H 1.045446 0.639303 0.270810 0.036 Uiso 1 1 calc R U . . .
C11 C 0.8840(4) 0.6235(4) 0.2334(4) 0.0283(10) Uani 1 1 d . . . . .
H11 H 0.895925 0.625967 0.168828 0.034 Uiso 1 1 calc R U . . .
C12 C 0.7771(4) 0.6096(3) 0.2673(3) 0.0183(8) Uani 1 1 d . . . . .
C13 C 0.6762(4) 0.6035(3) 0.2044(3) 0.0206(9) Uani 1 1 d . . . . .
H13 H 0.695481 0.559923 0.152467 0.025 Uiso 1 1 calc R U . . .
C14 C 0.6512(5) 0.7023(4) 0.1615(4) 0.0347(13) Uani 1 1 d . . . . .
H14A H 0.708915 0.718918 0.117481 0.052 Uiso 1 1 calc R U . . .
H14B H 0.648474 0.750182 0.210390 0.052 Uiso 1 1 calc R U . . .
H14C H 0.580527 0.700163 0.129680 0.052 Uiso 1 1 calc R U . . .
C15 C 0.4972(4) 0.7735(3) 0.3424(3) 0.0203(8) Uani 1 1 d . . . . .
C16 C 0.4960(5) 0.8830(3) 0.3467(4) 0.0291(11) Uani 1 1 d . . . . .
H16A H 0.554839 0.908237 0.307918 0.044 Uiso 1 1 calc R U . . .
H16B H 0.507045 0.903623 0.410393 0.044 Uiso 1 1 calc R U . . .
H16C H 0.425313 0.906462 0.324340 0.044 Uiso 1 1 calc R U . . .
C17 C 0.7310(5) 0.3751(4) 0.1411(4) 0.0282(11) Uani 1 1 d . . . . .
C18 C 0.8189(6) 0.3553(6) 0.0688(5) 0.054(2) Uani 1 1 d . . . . .
H18A H 0.786656 0.360114 0.007146 0.081 Uiso 1 1 calc R U . . .
H18B H 0.848266 0.291324 0.077807 0.081 Uiso 1 1 calc R U . . .
H18C H 0.878019 0.401804 0.074940 0.081 Uiso 1 1 calc R U . . .
C1W C 0.550(2) 0.3555(18) -0.1161(17) 0.088(8) Uani 0.5 1 d D . P A 1
H1WA H 0.573386 0.339871 -0.178796 0.132 Uiso 0.5 1 calc R U P A 1
H1WB H 0.478653 0.387417 -0.118297 0.132 Uiso 0.5 1 calc R U P A 1
H1WC H 0.543462 0.297061 -0.079921 0.132 Uiso 0.5 1 calc R U P A 1
O1W O 0.6307(10) 0.4184(11) -0.0731(8) 0.067(2) Uani 0.5 1 d D . P A 1
O1W' O 0.5658(10) 0.2922(10) -0.0421(9) 0.067(2) Uani 0.5 1 d D . P B 2
C1W' C 0.508(2) 0.3727(17) -0.0853(18) 0.088(8) Uani 0.5 1 d D . P B 2
H1WD H 0.492260 0.421097 -0.038608 0.132 Uiso 0.5 1 calc R U P B 2
H1WE H 0.438436 0.350226 -0.111784 0.132 Uiso 0.5 1 calc R U P B 2
H1WF H 0.553198 0.399970 -0.133949 0.132 Uiso 0.5 1 calc R U P B 2
C2W C 0.918(3) 0.619(3) 0.926(3) 0.088(8) Uani 0.25 1 d D . P C 3
H2WA H 0.960(12) 0.664(6) 0.936(14) 0.132 Uiso 0.25 1 d D U P D 3
H2WB H 0.894(5) 0.602(18) 0.976(6) 0.132 Uiso 0.25 1 d D U P E 3
H2WC H 0.955(13) 0.575(12) 0.906(9) 0.132 Uiso 0.25 1 d D U P F 3
O2W O 0.829(2) 0.645(2) 0.8624(17) 0.067(2) Uani 0.25 1 d D . P C 3
O2W' O 0.871(2) 0.623(3) 0.939(2) 0.067(2) Uani 0.25 1 d . . P G 4


_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 O1 2.039(3) . ?
Ni1 O3 2.047(3) . ?
Ni1 O2 2.054(3) . ?
Ni1 N1 2.058(3) . ?
Ni1 O1 2.071(3) 2_665 ?
Ni1 N2 2.075(4) . ?
Ni1 Ni2 2.8794(8) 2_665 ?
Ni2 O4 2.031(3) 2_665 ?
Ni2 O1 2.048(3) . ?
Ni2 O2 2.081(3) 2_665 ?
Ni2 O2 2.107(3) . ?
Ni2 O6 2.110(4) . ?
Ni2 O5 2.111(4) . ?
Ni2 C17 2.451(6) . ?
O1 C6 1.422(5) . ?
O2 C13 1.417(5) . ?
O4 C15 1.270(6) . ?
O3 C15 1.263(6) . ?
O6 C17 1.268(7) . ?
O5 C17 1.257(6) . ?
N1 C5 1.345(5) . ?
N1 C1 1.347(5) . ?
N2 C8 1.343(6) . ?
N2 C12 1.353(6) . ?
C1 C2 1.354(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.403(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.409(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.516(6) . ?
C6 C7 1.502(6) . ?
C6 H6 0.9800 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.369(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.414(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.371(8) . ?
C10 H10 0.9300 . ?
C11 C12 1.381(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.505(7) . ?
C13 C14 1.525(7) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.514(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.496(8) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C1W O1W 1.438(13) . ?
C1W H1WA 0.9600 . ?
C1W H1WB 0.9600 . ?
C1W H1WC 0.9600 . ?
O1W' C1W' 1.449(13) . ?
C1W' H1WD 0.9600 . ?
C1W' H1WE 0.9600 . ?
C1W' H1WF 0.9600 . ?
C2W O2W 1.45(2) . ?
C2W H2WA 0.805(14) . ?
C2W H2WB 0.806(14) . ?
C2W H2WC 0.805(14) . ?

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 Ni1 O3 167.19(12) . . ?
O1 Ni1 O2 82.24(11) . . ?
O3 Ni1 O2 99.27(12) . . ?
O1 Ni1 N1 80.33(12) . . ?
O3 Ni1 N1 99.77(13) . . ?
O2 Ni1 N1 160.29(12) . . ?
O1 Ni1 O1 78.96(13) . 2_665 ?
O3 Ni1 O1 88.35(12) . 2_665 ?
O2 Ni1 O1 88.24(12) . 2_665 ?
N1 Ni1 O1 97.35(12) . 2_665 ?
O1 Ni1 N2 102.89(13) . . ?
O3 Ni1 N2 89.87(13) . . ?
O2 Ni1 N2 79.51(13) . . ?
N1 Ni1 N2 95.47(14) . . ?
O1 Ni1 N2 167.17(13) 2_665 . ?
O1 Ni1 Ni2 90.55(8) . 2_665 ?
O3 Ni1 Ni2 81.62(10) . 2_665 ?
O2 Ni1 Ni2 46.24(9) . 2_665 ?
N1 Ni1 Ni2 142.67(9) . 2_665 ?
O1 Ni1 Ni2 45.32(8) 2_665 2_665 ?
N2 Ni1 Ni2 121.86(10) . 2_665 ?
O4 Ni2 O1 90.18(12) 2_665 . ?
O4 Ni2 O2 96.61(12) 2_665 2_665 ?
O1 Ni2 O2 88.12(12) . 2_665 ?
O4 Ni2 O2 169.72(13) 2_665 . ?
O1 Ni2 O2 80.73(10) . . ?
O2 Ni2 O2 78.43(12) 2_665 . ?
O4 Ni2 O6 91.81(14) 2_665 . ?
O1 Ni2 O6 166.55(14) . . ?
O2 Ni2 O6 104.85(13) 2_665 . ?
O2 Ni2 O6 98.15(14) . . ?
O4 Ni2 O5 89.05(13) 2_665 . ?
O1 Ni2 O5 104.74(13) . . ?
O2 Ni2 O5 165.97(12) 2_665 . ?
O2 Ni2 O5 97.85(13) . . ?
O6 Ni2 O5 62.00(14) . . ?
O4 Ni2 C17 90.25(16) 2_665 . ?
O1 Ni2 C17 135.57(16) . . ?
O2 Ni2 C17 135.86(15) 2_665 . ?
O2 Ni2 C17 99.59(15) . . ?
O6 Ni2 C17 31.15(16) . . ?
O5 Ni2 C17 30.85(15) . . ?
O4 Ni2 Ni1 81.08(10) 2_665 2_665 ?
O1 Ni2 Ni1 45.97(9) . 2_665 ?
O2 Ni2 Ni1 45.47(8) 2_665 2_665 ?
O2 Ni2 Ni1 89.11(9) . 2_665 ?
O6 Ni2 Ni1 147.44(11) . 2_665 ?
O5 Ni2 Ni1 148.51(10) . 2_665 ?
C17 Ni2 Ni1 171.29(13) . 2_665 ?
C6 O1 Ni1 112.8(2) . . ?
C6 O1 Ni2 132.4(2) . . ?
Ni1 O1 Ni2 99.62(12) . . ?
C6 O1 Ni1 116.5(2) . 2_665 ?
Ni1 O1 Ni1 100.99(13) . 2_665 ?
Ni2 O1 Ni1 88.71(11) . 2_665 ?
C13 O2 Ni1 113.4(3) . . ?
C13 O2 Ni2 132.8(3) . 2_665 ?
Ni1 O2 Ni2 88.29(12) . 2_665 ?
C13 O2 Ni2 115.6(3) . . ?
Ni1 O2 Ni2 97.24(11) . . ?
Ni2 O2 Ni2 101.48(12) 2_665 . ?
C15 O4 Ni2 125.6(3) . 2_665 ?
C15 O3 Ni1 124.2(3) . . ?
C17 O6 Ni2 89.4(3) . . ?
C17 O5 Ni2 89.7(3) . . ?
C5 N1 C1 119.6(4) . . ?
C5 N1 Ni1 113.0(3) . . ?
C1 N1 Ni1 127.1(3) . . ?
C8 N2 C12 118.7(4) . . ?
C8 N2 Ni1 127.0(3) . . ?
C12 N2 Ni1 114.3(3) . . ?
N1 C1 C2 122.9(5) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 118.7(5) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C2 C3 C4 118.9(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 118.4(5) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
N1 C5 C4 121.4(4) . . ?
N1 C5 C6 117.5(3) . . ?
C4 C5 C6 121.1(4) . . ?
O1 C6 C7 112.2(4) . . ?
O1 C6 C5 109.8(3) . . ?
C7 C6 C5 110.7(3) . . ?
O1 C6 H6 108.0 . . ?
C7 C6 H6 108.0 . . ?
C5 C6 H6 108.0 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 123.0(5) . . ?
N2 C8 H8 118.5 . . ?
C9 C8 H8 118.5 . . ?
C8 C9 C10 118.7(5) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 117.6(5) . . ?
C11 C10 H10 121.2 . . ?
C9 C10 H10 121.2 . . ?
C10 C11 C12 121.0(5) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 H11 119.5 . . ?
N2 C12 C11 120.9(4) . . ?
N2 C12 C13 116.0(4) . . ?
C11 C12 C13 122.9(4) . . ?
O2 C13 C12 110.3(4) . . ?
O2 C13 C14 114.6(4) . . ?
C12 C13 C14 110.2(4) . . ?
O2 C13 H13 107.1 . . ?
C12 C13 H13 107.1 . . ?
C14 C13 H13 107.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3 C15 O4 127.1(4) . . ?
O3 C15 C16 117.2(4) . . ?
O4 C15 C16 115.7(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C17 O6 118.9(5) . . ?
O5 C17 C18 121.5(5) . . ?
O6 C17 C18 119.6(5) . . ?
O5 C17 Ni2 59.5(3) . . ?
O6 C17 Ni2 59.4(3) . . ?
C18 C17 Ni2 179.0(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1W C1W H1WA 109.5 . . ?
O1W C1W H1WB 109.5 . . ?
H1WA C1W H1WB 109.5 . . ?
O1W C1W H1WC 109.5 . . ?
H1WA C1W H1WC 109.5 . . ?
H1WB C1W H1WC 109.5 . . ?
O1W' C1W' H1WD 109.5 . . ?
O1W' C1W' H1WE 109.5 . . ?
H1WD C1W' H1WE 109.5 . . ?
O1W' C1W' H1WF 109.5 . . ?
H1WD C1W' H1WF 109.5 . . ?
H1WE C1W' H1WF 109.5 . . ?
O2W C2W H2WA 112(2) . . ?
O2W C2W H2WB 112(2) . . ?
H2WA C2W H2WB 107(2) . . ?
O2W C2W H2WC 112(2) . . ?
H2WA C2W H2WC 107(2) . . ?
H2WB C2W H2WC 107(2) . . ?

_refine_diff_density_max         0.772
_refine_diff_density_min         -1.434
_refine_diff_density_rms         0.104


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile/diethylether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_api266c_0m_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1896872'
loop_
_audit_author_name
_audit_author_address
'Melanie Pilkington'
;Brock University
Canada
;
_audit_update_record             
;
2019-02-12 deposited with the CCDC.	2019-05-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H68 N4 Ni4 O12'
_chemical_formula_sum            'C48 H68 N4 Ni4 O12'
_chemical_formula_weight         1127.90

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_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.
;

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

_cell_length_a                   12.548(3)
_cell_length_b                   20.583(6)
_cell_length_c                   12.063(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.276(10)
_cell_angle_gamma                90
_cell_volume                     2840.1(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9735
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      28.31

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.362
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
Solvent Accessible Volume =     374.6
Electrons Found in S.A.V. =      39.2
Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.376 0.236 0.702 !       2.22 eA-3
C102 0.410 0.236 0.647 !       1.97 eA-3
C103 0.468 0.234 0.562 !       1.96 eA-3
Q104 0.047 0.161 0.652 !       0.68 eA-3
Q105 0.581 0.500 0.470 !       0.58 eA-3
Q106 0.392 0.486 0.323 !       0.57 eA-3
Q107 0.505 0.030 0.179 !       0.56 eA-3
Q108 0.077 0.092 0.425 !       0.55 eA-3
Q109 0.846 0.029 0.820 !       0.53 eA-3
Q110 0.376 0.405 0.320 !       0.52 eA-3
C111 0.018 0.170 0.108 !       0.51 eA-3
The unit cell contains void content and count electrons
conistent with 2 water molecules which have been treated as 
a diffuse contrubution to the overall 
scattering without specific atom positions by SQUEEZE/PLATON
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20232
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.206
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_point_group_measured_fraction_full 0.861
_reflns_number_total             4437
_reflns_number_gt                4202
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_max     0.764
_reflns_Friedel_fraction_full    0.744

_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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²+14.0735P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1737 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.123(10)
_chemical_absolute_configuration syn
_refine_ls_number_reflns         4437
_refine_ls_number_parameters     256
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1183
_refine_ls_wR_factor_gt          0.1148
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.018
_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_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
N1 N 0.4344(8) 0.6387(3) 0.5969(6) 0.068(3) Uani 1 1 d G . . . .
C1 C 0.3511(6) 0.6875(4) 0.5723(6) 0.110(3) Uani 1 1 d G . . . .
H1 H 0.2706 0.6777 0.5283 0.132 Uiso 1 1 calc R U . . .
C2 C 0.3858(9) 0.7505(3) 0.6121(7) 0.110(3) Uani 1 1 d G . . . .
H2 H 0.3289 0.7839 0.5953 0.132 Uiso 1 1 calc R U . . .
C3 C 0.5036(9) 0.7648(3) 0.6765(7) 0.110(3) Uani 1 1 d G . . . .
H3 H 0.5273 0.8079 0.7037 0.132 Uiso 1 1 calc R U . . .
C4 C 0.5869(7) 0.7160(4) 0.7010(6) 0.110(3) Uani 1 1 d G . . . .
H4 H 0.6674 0.7258 0.7450 0.132 Uiso 1 1 calc R U . . .
C5 C 0.5522(7) 0.6530(4) 0.6612(6) 0.110(3) Uani 1 1 d G . . . .
Ni1 Ni 0.40149(9) 0.54255(5) 0.55206(7) 0.0436(3) Uani 1 1 d . . . . .
Ni2 Ni 0.38505(8) 0.44545(5) 0.37172(8) 0.0413(3) Uani 1 1 d . . . . .
O1 O 0.5806(5) 0.5438(4) 0.6140(4) 0.0431(13) Uani 1 1 d . . . . .
O2 O 0.4311(4) 0.4439(4) 0.5585(4) 0.0375(12) Uani 1 1 d . . . . .
O3 O 0.2230(5) 0.5460(5) 0.4527(4) 0.068(2) Uani 1 1 d . . . . .
O4 O 0.2122(5) 0.4647(4) 0.3187(5) 0.068(2) Uani 1 1 d . . . . .
O5 O 0.3488(5) 0.4172(3) 0.1879(5) 0.0474(15) Uani 1 1 d . . . . .
O6 O 0.3440(6) 0.3474(3) 0.3237(5) 0.0592(17) Uani 1 1 d . . . . .
N2 N 0.3793(5) 0.5204(4) 0.7087(5) 0.0437(17) Uani 1 1 d . . . . .
C6 C 0.6346(9) 0.5959(5) 0.6898(7) 0.059(3) Uani 1 1 d . . . . .
H6 H 0.7038 0.6092 0.6740 0.070 Uiso 1 1 calc R U . . .
C7 C 0.6782(8) 0.5780(5) 0.8260(6) 0.060(3) Uani 1 1 d . . . . .
H7A H 0.6130 0.5606 0.8417 0.091 Uiso 1 1 calc R U . . .
H7B H 0.7092 0.6169 0.8758 0.091 Uiso 1 1 calc R U . . .
H7C H 0.7399 0.5452 0.8468 0.091 Uiso 1 1 calc R U . . .
C8 C 0.3661(6) 0.5614(5) 0.7891(7) 0.0509(10) Uani 1 1 d . . . . .
H8 H 0.3651 0.6068 0.7748 0.061 Uiso 1 1 calc R U . . .
C9 C 0.3539(6) 0.5397(5) 0.8913(6) 0.0509(10) Uani 1 1 d . . . . .
H9 H 0.3447 0.5700 0.9462 0.061 Uiso 1 1 calc R U . . .
C10 C 0.3551(7) 0.4752(5) 0.9132(7) 0.0509(10) Uani 1 1 d . . . . .
H10 H 0.3485 0.4598 0.9843 0.061 Uiso 1 1 calc R U . . .
C11 C 0.3661(6) 0.4319(5) 0.8304(6) 0.0509(10) Uani 1 1 d . . . . .
H11 H 0.3648 0.3864 0.8438 0.061 Uiso 1 1 calc R U . . .
C12 C 0.3788(6) 0.4544(6) 0.7285(6) 0.0509(10) Uani 1 1 d . . . . .
C13 C 0.3806(8) 0.4106(5) 0.6294(8) 0.057(2) Uani 1 1 d . . . . .
H13 H 0.4310 0.3723 0.6686 0.068 Uiso 1 1 calc R U . . .
C14 C 0.2598(11) 0.3866(8) 0.5564(10) 0.102(5) Uani 1 1 d . . . . .
H14A H 0.2072 0.4236 0.5230 0.153 Uiso 1 1 calc R U . . .
H14B H 0.2330 0.3609 0.6085 0.153 Uiso 1 1 calc R U . . .
H14C H 0.2596 0.3594 0.4896 0.153 Uiso 1 1 calc R U . . .
C15 C 0.1684(8) 0.5094(7) 0.3601(7) 0.072(4) Uani 1 1 d . . . . .
C16 C 0.0336(9) 0.5182(7) 0.2878(9) 0.080(4) Uani 1 1 d . . . . .
C17 C -0.0269(12) 0.4635(10) 0.3168(18) 0.146(8) Uani 1 1 d . . . . .
H17A H -0.1094 0.4746 0.2922 0.218 Uiso 1 1 calc R U . . .
H17B H 0.0095 0.4552 0.4045 0.218 Uiso 1 1 calc R U . . .
H17C H -0.0208 0.4246 0.2730 0.218 Uiso 1 1 calc R U . . .
C18 C 0.0058(10) 0.5287(14) 0.1565(10) 0.204(14) Uani 1 1 d . . . . .
H18A H -0.0792 0.5297 0.1103 0.306 Uiso 1 1 calc R U . . .
H18B H 0.0388 0.4931 0.1266 0.306 Uiso 1 1 calc R U . . .
H18C H 0.0394 0.5700 0.1464 0.306 Uiso 1 1 calc R U . . .
C19 C -0.0025(12) 0.5772(11) 0.3362(18) 0.164(9) Uani 1 1 d . . . . .
H19A H 0.0384 0.6154 0.3245 0.247 Uiso 1 1 calc R U . . .
H19B H 0.0175 0.5714 0.4232 0.247 Uiso 1 1 calc R U . . .
H19C H -0.0871 0.5835 0.2928 0.247 Uiso 1 1 calc R U . . .
C20 C 0.3259(8) 0.3612(5) 0.2143(8) 0.055(2) Uani 1 1 d . . . . .
C21 C 0.2731(12) 0.3095(6) 0.1122(10) 0.083(4) Uani 1 1 d . . . . .
C22 C 0.255(2) 0.2460(7) 0.1612(15) 0.168(10) Uani 1 1 d . . . . .
H22A H 0.1832 0.2478 0.1748 0.252 Uiso 1 1 calc R U . . .
H22B H 0.3216 0.2369 0.2383 0.252 Uiso 1 1 calc R U . . .
H22C H 0.2480 0.2115 0.1027 0.252 Uiso 1 1 calc R U . . .
C23 C 0.3668(18) 0.2997(9) 0.0601(15) 0.150(8) Uani 1 1 d . . . . .
H23A H 0.4440 0.2947 0.1273 0.225 Uiso 1 1 calc R U . . .
H23B H 0.3672 0.3375 0.0110 0.225 Uiso 1 1 calc R U . . .
H23C H 0.3480 0.2606 0.0093 0.225 Uiso 1 1 calc R U . . .
C24 C 0.1738(16) 0.3377(11) 0.0115(15) 0.166(9) Uani 1 1 d . . . . .
H24A H 0.1461 0.3072 -0.0569 0.249 Uiso 1 1 calc R U . . .
H24B H 0.1978 0.3784 -0.0139 0.249 Uiso 1 1 calc R U . . .
H24C H 0.1108 0.3465 0.0374 0.249 Uiso 1 1 calc R U . . .


_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
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
N1 Ni1 2.048(6) . ?
C1 C2 1.3900 . ?
C1 H1 0.9500 . ?
C2 C3 1.3900 . ?
C2 H2 0.9500 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.508(13) . ?
Ni1 O1 2.056(6) . ?
Ni1 O2 2.061(8) . ?
Ni1 O3 2.062(6) . ?
Ni1 N2 2.072(6) . ?
Ni1 O1 2.106(4) 2_656 ?
Ni1 Ni2 2.8984(14) . ?
Ni2 O4 2.032(6) . ?
Ni2 O1 2.063(8) 2_656 ?
Ni2 O2 2.083(4) . ?
Ni2 O6 2.105(7) . ?
Ni2 O2 2.106(5) 2_656 ?
Ni2 O5 2.152(5) . ?
Ni2 C20 2.450(9) . ?
O1 C6 1.391(11) . ?
O1 Ni2 2.063(8) 2_656 ?
O1 Ni1 2.106(4) 2_656 ?
O2 C13 1.431(10) . ?
O2 Ni2 2.106(5) 2_656 ?
O3 C15 1.287(12) . ?
O4 C15 1.273(12) . ?
O5 C20 1.259(11) . ?
O6 C20 1.277(10) . ?
N2 C8 1.346(10) . ?
N2 C12 1.379(13) . ?
C6 C7 1.548(10) . ?
C6 H6 1.0000 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.377(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.352(14) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(11) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.505(12) . ?
C13 C14 1.491(14) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.562(13) . ?
C16 C17 1.478(19) . ?
C16 C18 1.490(16) . ?
C16 C19 1.50(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.554(14) . ?
C21 C24 1.46(2) . ?
C21 C22 1.491(19) . ?
C21 C23 1.557(19) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 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
C1 N1 C5 120.0 . . ?
C1 N1 Ni1 126.1(4) . . ?
C5 N1 Ni1 113.8(4) . . ?
N1 C1 C2 120.0 . . ?
N1 C1 H1 120.0 . . ?
C2 C1 H1 120.0 . . ?
C3 C2 C1 120.0 . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 C6 124.1(6) . . ?
N1 C5 C6 115.8(6) . . ?
N1 Ni1 O1 79.6(3) . . ?
N1 Ni1 O2 158.2(3) . . ?
O1 Ni1 O2 81.1(3) . . ?
N1 Ni1 O3 100.0(4) . . ?
O1 Ni1 O3 167.1(2) . . ?
O2 Ni1 O3 101.1(3) . . ?
N1 Ni1 N2 93.5(3) . . ?
O1 Ni1 N2 102.0(2) . . ?
O2 Ni1 N2 80.7(2) . . ?
O3 Ni1 N2 90.9(2) . . ?
N1 Ni1 O1 98.6(3) . 2_656 ?
O1 Ni1 O1 79.5(2) . 2_656 ?
O2 Ni1 O1 87.7(2) . 2_656 ?
O3 Ni1 O1 87.8(2) . 2_656 ?
N2 Ni1 O1 167.9(3) . 2_656 ?
N1 Ni1 Ni2 143.98(17) . . ?
O1 Ni1 Ni2 90.68(19) . . ?
O2 Ni1 Ni2 45.94(12) . . ?
O3 Ni1 Ni2 82.1(2) . . ?
N2 Ni1 Ni2 122.5(2) . . ?
O1 Ni1 Ni2 45.4(2) 2_656 . ?
O4 Ni2 O1 89.7(3) . 2_656 ?
O4 Ni2 O2 97.4(2) . . ?
O1 Ni2 O2 88.3(2) 2_656 . ?
O4 Ni2 O6 89.5(3) . . ?
O1 Ni2 O6 169.6(2) 2_656 . ?
O2 Ni2 O6 102.1(3) . . ?
O4 Ni2 O2 168.8(3) . 2_656 ?
O1 Ni2 O2 79.9(3) 2_656 2_656 ?
O2 Ni2 O2 78.24(19) . 2_656 ?
O6 Ni2 O2 101.5(3) . 2_656 ?
O4 Ni2 O5 89.0(2) . . ?
O1 Ni2 O5 107.4(2) 2_656 . ?
O2 Ni2 O5 163.1(3) . . ?
O6 Ni2 O5 62.2(2) . . ?
O2 Ni2 O5 98.1(2) 2_656 . ?
O4 Ni2 C20 87.1(3) . . ?
O1 Ni2 C20 138.2(3) 2_656 . ?
O2 Ni2 C20 133.5(3) . . ?
O6 Ni2 C20 31.4(3) . . ?
O2 Ni2 C20 103.4(3) 2_656 . ?
O5 Ni2 C20 30.9(3) . . ?
O4 Ni2 Ni1 80.76(19) . . ?
O1 Ni2 Ni1 46.57(12) 2_656 . ?
O2 Ni2 Ni1 45.3(2) . . ?
O6 Ni2 Ni1 143.28(16) . . ?
O2 Ni2 Ni1 88.99(18) 2_656 . ?
O5 Ni2 Ni1 151.55(18) . . ?
C20 Ni2 Ni1 167.2(2) . . ?
C6 O1 Ni1 114.4(6) . . ?
C6 O1 Ni2 132.3(6) . 2_656 ?
Ni1 O1 Ni2 100.2(3) . 2_656 ?
C6 O1 Ni1 114.9(5) . 2_656 ?
Ni1 O1 Ni1 100.5(2) . 2_656 ?
Ni2 O1 Ni1 88.1(3) 2_656 2_656 ?
C13 O2 Ni1 112.1(5) . . ?
C13 O2 Ni2 131.3(5) . . ?
Ni1 O2 Ni2 88.8(3) . . ?
C13 O2 Ni2 116.8(5) . 2_656 ?
Ni1 O2 Ni2 98.7(3) . 2_656 ?
Ni2 O2 Ni2 101.73(19) . 2_656 ?
C15 O3 Ni1 123.2(6) . . ?
C15 O4 Ni2 126.4(6) . . ?
C20 O5 Ni2 87.7(5) . . ?
C20 O6 Ni2 89.4(6) . . ?
C8 N2 C12 118.8(7) . . ?
C8 N2 Ni1 128.4(6) . . ?
C12 N2 Ni1 112.8(5) . . ?
O1 C6 C5 110.3(8) . . ?
O1 C6 C7 112.2(7) . . ?
C5 C6 C7 109.7(8) . . ?
O1 C6 H6 108.2 . . ?
C5 C6 H6 108.2 . . ?
C7 C6 H6 108.2 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 122.3(9) . . ?
N2 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C10 C9 C8 119.7(8) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 119.2(8) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C12 C11 C10 120.4(10) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
N2 C12 C11 119.6(8) . . ?
N2 C12 C13 116.7(7) . . ?
C11 C12 C13 123.4(10) . . ?
O2 C13 C14 113.5(8) . . ?
O2 C13 C12 110.1(8) . . ?
C14 C13 C12 109.0(8) . . ?
O2 C13 H13 108.0 . . ?
C14 C13 H13 108.0 . . ?
C12 C13 H13 108.0 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O4 C15 O3 127.0(8) . . ?
O4 C15 C16 114.0(9) . . ?
O3 C15 C16 118.9(9) . . ?
C17 C16 C18 116.3(15) . . ?
C17 C16 C19 104.9(13) . . ?
C18 C16 C19 108.7(16) . . ?
C17 C16 C15 108.8(11) . . ?
C18 C16 C15 109.7(8) . . ?
C19 C16 C15 108.0(10) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O5 C20 O6 120.2(8) . . ?
O5 C20 C21 119.5(8) . . ?
O6 C20 C21 120.2(9) . . ?
O5 C20 Ni2 61.4(4) . . ?
O6 C20 Ni2 59.2(5) . . ?
C21 C20 Ni2 173.1(8) . . ?
C24 C21 C22 117.5(15) . . ?
C24 C21 C20 109.2(12) . . ?
C22 C21 C20 111.8(9) . . ?
C24 C21 C23 104.1(13) . . ?
C22 C21 C23 108.0(14) . . ?
C20 C21 C23 105.2(11) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_refine_diff_density_max         0.642
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.085

_shelxl_version_number           2014-3



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_preparation       'Magnetic properties'
