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

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

data_2
_database_code_depnum_ccdc_archive 'CCDC 1400192'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.041 -0.012 -0.008 7481 1578 ' '
_platon_squeeze_details          
;
The total potential solvent accessible void is 7481 eA3, indicating more
solvent molecules can reside in the crystal structure. Based on the TG
and elemental analysis, 5.4 DMF molecules were included in the final molecules.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46.25 H55.75 N20.38 Ni3 O12.38'
_chemical_formula_weight         1271.24

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      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'

_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, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'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+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, 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+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, 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+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   23.290(3)
_cell_length_b                   23.290(3)
_cell_length_c                   23.290(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12633(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    113.15
_cell_measurement_reflns_used    21843
_cell_measurement_theta_min      2.1409
_cell_measurement_theta_max      27.8744

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_F_000             5271
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.955
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8471
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      113.15
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ω
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58291
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.142
_diffrn_reflns_theta_max         27.925
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2788
_reflns_number_gt                2768
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0425P)²+7.1270P] 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 1238 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2788
_refine_ls_number_parameters     94
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0289
_refine_ls_wR_factor_ref         0.0766
_refine_ls_wR_factor_gt          0.0762
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_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 0.61353(2) 0.28333(2) 0.28333(2) 0.01432(12) Uani 1 2 d S T P . .
O1 O 0.57052(8) 0.27336(9) 0.36068(8) 0.0247(4) Uani 1 1 d . . . . .
O2 O 0.67310(10) 0.32690(10) 0.32690(10) 0.0163(8) Uani 1 6 d S T P . .
N1 N 0.74461(9) 0.25539(9) -0.04350(12) 0.0186(6) Uani 1 2 d S T P . .
N2 N 0.65933(9) 0.30020(9) 0.20834(8) 0.0173(4) Uani 1 1 d . . . . .
N3 N 0.65657(9) 0.27585(9) 0.15692(9) 0.0196(4) Uani 1 1 d . . . . .
C1 C 0.70116(12) 0.22989(13) -0.01713(12) 0.0291(6) Uani 1 1 d . . . . .
H1 H 0.6819 0.2007 -0.0363 0.035 Uiso 1 1 calc R U . . .
C2 C 0.68300(13) 0.24450(14) 0.03755(12) 0.0308(7) Uani 1 1 d . . . . .
H2 H 0.6526 0.2252 0.0549 0.037 Uiso 1 1 calc R U . . .
C3 C 0.71133(10) 0.28867(10) 0.06570(14) 0.0209(6) Uani 1 2 d S T P . .
C4 C 0.69691(11) 0.30309(11) 0.12620(15) 0.0205(7) Uani 1 2 d S T P . .
C5 C 0.58776(11) 0.27184(17) 0.41224(11) 0.0227(7) Uani 1 2 d S T P . .
C6 C 0.54261(11) 0.26953(19) 0.45739(11) 0.0279(8) Uani 1 2 d S T P . .
C7 C 0.48511(14) 0.2682(3) 0.44301(14) 0.0638(15) Uani 1 1 d . . . . .
H7 H 0.4745 0.2672 0.4045 0.077 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01319(19) 0.01488(14) 0.01488(14) -0.00035(16) 0.00068(10) 0.00068(10)
O1 0.0183(8) 0.0377(11) 0.0182(9) -0.0012(8) 0.0053(7) -0.0049(8)
O2 0.0163(8) 0.0163(8) 0.0163(8) 0.0012(9) -0.0012(9) -0.0012(9)
N1 0.0213(9) 0.0213(9) 0.0130(14) -0.0005(8) 0.0005(8) 0.0020(11)
N2 0.0171(9) 0.0202(10) 0.0147(9) -0.0008(8) 0.0011(7) -0.0038(8)
N3 0.0224(10) 0.0209(10) 0.0155(9) -0.0044(8) 0.0025(7) -0.0020(8)
C1 0.0261(13) 0.0408(17) 0.0204(12) -0.0114(11) 0.0042(10) -0.0105(12)
C2 0.0306(15) 0.0411(16) 0.0208(13) -0.0091(11) 0.0088(11) -0.0149(13)
C3 0.0221(10) 0.0221(10) 0.0186(15) 0.0006(9) -0.0006(9) 0.0027(14)
C4 0.0220(10) 0.0220(10) 0.0174(16) -0.0010(9) 0.0010(9) 0.0010(13)
C5 0.0186(10) 0.031(2) 0.0186(10) 0.0011(10) -0.0010(13) -0.0011(10)
C6 0.0176(10) 0.049(3) 0.0176(10) 0.0021(11) 0.0015(13) -0.0021(11)
C7 0.0219(15) 0.150(5) 0.0197(15) -0.008(2) 0.0024(12) -0.007(2)

_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 O2 1.9960(9) . ?
Ni1 N1 2.070(3) 32_545 ?
Ni1 O1 2.0743(18) . ?
Ni1 O1 2.0744(18) 17 ?
Ni1 N2 2.0839(19) 17 ?
Ni1 N2 2.0839(19) . ?
O1 C5 1.267(2) . ?
O2 Ni1 1.9961(9) 7_665 ?
O2 Ni1 1.9961(9) 10_656 ?
N1 C1 1.324(3) . ?
N1 C1 1.324(3) 14_665 ?
N1 Ni1 2.070(3) 35 ?
N2 N3 1.327(3) . ?
N2 N2 1.333(4) 14_665 ?
N3 C4 1.340(3) . ?
C1 C2 1.384(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.387(3) . ?
C2 H2 0.9300 . ?
C3 C2 1.387(3) 14_665 ?
C3 C4 1.487(5) . ?
C4 N3 1.340(3) 14_665 ?
C5 O1 1.267(2) 23_656 ?
C5 C6 1.488(5) . ?
C6 C7 1.381(4) . ?
C6 C7 1.381(4) 23_656 ?
C7 C7 1.387(6) 21 ?
C7 H7 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 N1 172.05(15) . 32_545 ?
O2 Ni1 O1 87.20(10) . . ?
N1 Ni1 O1 87.08(8) 32_545 . ?
O2 Ni1 O1 87.20(10) . 17 ?
N1 Ni1 O1 87.08(8) 32_545 17 ?
O1 Ni1 O1 87.77(12) . 17 ?
O2 Ni1 N2 88.54(10) . 17 ?
N1 Ni1 N2 96.91(8) 32_545 17 ?
O1 Ni1 N2 89.41(8) . 17 ?
O1 Ni1 N2 174.99(8) 17 17 ?
O2 Ni1 N2 88.54(10) . . ?
N1 Ni1 N2 96.91(8) 32_545 . ?
O1 Ni1 N2 174.99(8) . . ?
O1 Ni1 N2 89.41(8) 17 . ?
N2 Ni1 N2 93.10(11) 17 . ?
C5 O1 Ni1 132.33(19) . . ?
Ni1 O2 Ni1 116.63(7) . 7_665 ?
Ni1 O2 Ni1 116.63(7) . 10_656 ?
Ni1 O2 Ni1 116.63(7) 7_665 10_656 ?
C1 N1 C1 118.1(3) . 14_665 ?
C1 N1 Ni1 120.19(16) . 35 ?
C1 N1 Ni1 120.19(16) 14_665 35 ?
N3 N2 N2 109.67(13) . 14_665 ?
N3 N2 Ni1 130.63(16) . . ?
N2 N2 Ni1 119.68(6) 14_665 . ?
N2 N3 C4 104.2(2) . . ?
N1 C1 C2 123.4(3) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 118.2(3) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C2 C3 C2 118.8(3) . 14_665 ?
C2 C3 C4 120.53(16) . . ?
C2 C3 C4 120.54(16) 14_665 . ?
N3 C4 N3 112.3(3) . 14_665 ?
N3 C4 C3 123.86(15) . . ?
N3 C4 C3 123.85(15) 14_665 . ?
O1 C5 O1 126.9(3) 23_656 . ?
O1 C5 C6 116.55(17) 23_656 . ?
O1 C5 C6 116.55(17) . . ?
C7 C6 C7 118.0(4) . 23_656 ?
C7 C6 C5 120.98(19) . . ?
C7 C6 C5 120.98(19) 23_656 . ?
C6 C7 C7 120.95(19) . 21 ?
C6 C7 H7 119.5 . . ?
C7 C7 H7 119.5 21 . ?

_refine_diff_density_max         0.253
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.050

_shelx_res_file                  
;

    2.res created by SHELXL-2014/7

TITL 2.res in I-43m
CELL  0.71073  23.2899  23.2899  23.2899   90.000   90.000   90.000
ZERR   8   0.0027   0.0027   0.0027    0.000    0.000    0.000
LATT -2
SYMM  - X, - Y,   Z
SYMM  - X,   Y, - Z
SYMM    X, - Y, - Z
SYMM    Z,   X,   Y
SYMM    Z, - X, - Y
SYMM  - Z, - X,   Y
SYMM  - Z,   X, - Y
SYMM    Y,   Z,   X
SYMM  - Y,   Z, - X
SYMM    Y, - Z, - X
SYMM  - Y, - Z,   X
SYMM    Y,   X,   Z
SYMM  - Y, - X,   Z
SYMM    Y, - X, - Z
SYMM  - Y,   X, - Z
SYMM    X,   Z,   Y
SYMM  - X,   Z, - Y
SYMM  - X, - Z,   Y
SYMM    X, - Z, - Y
SYMM    Z,   Y,   X
SYMM    Z, - Y, - X
SYMM  - Z,   Y, - X
SYMM  - Z, - Y,   X
SFAC C  H  N  O  Ni
UNIT 370 446 163 99 24
MERG 2
L.S. 10
ACTA
BOND   $H
FMAP 2
PLAN 10
LIST 6
WGHT    0.042500    7.127000
FVAR       1.22400
NI1   5    0.613535    0.283328    0.283328    10.50000    0.01319    0.01488 =
         0.01488   -0.00035    0.00068    0.00068
O1    4    0.570516    0.273364    0.360677    11.00000    0.01828    0.03771 =
         0.01825   -0.00115    0.00531   -0.00495
O2    4    0.673103    0.326897    0.326897    10.16667    0.01629    0.01629 =
         0.01629    0.00117   -0.00117   -0.00117
N1    3    0.744610    0.255390   -0.043505    10.50000    0.02134    0.02134 =
         0.01304   -0.00045    0.00045    0.00204
N2    3    0.659331    0.300199    0.208335    11.00000    0.01713    0.02016 =
         0.01470   -0.00076    0.00108   -0.00380
N3    3    0.656573    0.275848    0.156915    11.00000    0.02242    0.02092 =
         0.01546   -0.00440    0.00251   -0.00197
C1    1    0.701158    0.229891   -0.017133    11.00000    0.02606    0.04078 =
         0.02043   -0.01140    0.00425   -0.01052
AFIX  43
H1    2    0.681856    0.200676   -0.036329    11.00000   -1.20000
AFIX   0
C2    1    0.683001    0.244505    0.037552    11.00000    0.03062    0.04107 =
         0.02076   -0.00913    0.00878   -0.01487
AFIX  43
H2    2    0.652645    0.225239    0.054926    11.00000   -1.20000
AFIX   0
C3    1    0.711333    0.288667    0.065703    10.50000    0.02206    0.02206 =
         0.01856    0.00065   -0.00065    0.00268
C4    1    0.696906    0.303094    0.126198    10.50000    0.02204    0.02204 =
         0.01744   -0.00098    0.00098    0.00104
C5    1    0.587756    0.271838    0.412244    10.50000    0.01860    0.03099 =
         0.01860    0.00107   -0.00096   -0.00107
C6    1    0.542609    0.269525    0.457391    10.50000    0.01756    0.04861 =
         0.01756    0.00209    0.00153   -0.00209
C7    1    0.485110    0.268150    0.443011    11.00000    0.02194    0.14969 =
         0.01972   -0.00772    0.00236   -0.00724
AFIX  43
H7    2    0.474466    0.267213    0.404536    11.00000   -1.20000
AFIX   0
HKLF    4

REM  2.res in I-43m
REM R1 =  0.0289 for    2768 Fo > 4sig(Fo)  and  0.0294 for all    2788 data
REM     94 parameters refined using      0 restraints

END

WGHT      0.0424      7.1689

REM Highest difference peak  0.253,  deepest hole -0.303,  1-sigma level  0.050
Q1    1   0.6505  0.3495  0.2211  10.50000  0.05    0.25
Q2    1   0.6484  0.3516  0.3516  10.16667  0.05    0.25
Q3    1   0.6229  0.2821  0.2268  11.00000  0.05    0.25
Q4    1   0.7785  0.2353 -0.0611  11.00000  0.05    0.25
Q5    1   0.7169  0.3599  0.3334  11.00000  0.05    0.25
Q6    1   0.7795  0.2205 -0.0394  10.50000  0.05    0.23
Q7    1   0.7114  0.2886  0.3307  10.50000  0.05    0.22
Q8    1   0.5669  0.2915  0.3072  11.00000  0.05    0.22
Q9    1   0.7484  0.2516  0.0203  10.50000  0.05    0.22
Q10   1   0.5000  0.2691  0.5000  10.25000  0.05    0.21
;
_shelx_res_checksum              97938
####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1400193'
_audit_update_record             
;
2015-09-20 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.044 -0.013 -0.008 7790 3651 ' '
_platon_squeeze_details          
;
The total potential solvent accessible void is 7790 eA3, indicating more
solvent molecules can reside in the crystal structure. Based on the TG
and elemental analysis, two DMF molecules and one dimethylamine cation 
were included in the final molecules.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H40 Co3 N18 O9'
_chemical_formula_weight         1069.67

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           217
_space_group_name_H-M_alt        'I -4 3 m'
_space_group_name_Hall           'I -4 2 3'

_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, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, z'
'-y, -x, z'
'y, -x, -z'
'-y, x, -z'
'x, z, y'
'-x, z, -y'
'-x, -z, y'
'x, -z, -y'
'z, y, x'
'z, -y, -x'
'-z, y, -x'
'-z, -y, x'
'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+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, 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+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, 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+1/2, x+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, z+1/2, y+1/2'
'-x+1/2, z+1/2, -y+1/2'
'-x+1/2, -z+1/2, y+1/2'
'x+1/2, -z+1/2, -y+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'

_cell_length_a                   23.570(3)
_cell_length_b                   23.570(3)
_cell_length_c                   23.570(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13095(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    113.15
_cell_measurement_reflns_used    14621
_cell_measurement_theta_min      1.7270
_cell_measurement_theta_max      27.9143

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_F_000             4376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.803
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.2967
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      113.15
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ω
_diffrn_measurement_method       dtprofit.ref
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60182
_diffrn_reflns_av_unetI/netI     0.1071
_diffrn_reflns_av_R_equivalents  0.3089
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.728
_diffrn_reflns_theta_max         27.975
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2895
_reflns_number_gt                2469
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.867
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    1.000

_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.
;

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0732P)²] 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 904 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2895
_refine_ls_number_parameters     94
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0661
_refine_ls_wR_factor_ref         0.1648
_refine_ls_wR_factor_gt          0.1594
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_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
Co1 Co 0.38784(4) 0.71608(3) 0.71608(3) 0.0124(3) Uani 1 2 d S T P . .
O1 O 0.43055(18) 0.7267(2) 0.63753(18) 0.0244(11) Uani 1 1 d . . . . .
O2 O 0.3279(2) 0.6721(2) 0.6721(2) 0.014(2) Uani 1 6 d S T P . .
N1 N 0.2551(2) 0.7449(2) 1.0414(3) 0.0183(16) Uani 1 2 d S T P . .
N2 N 0.3409(2) 0.6989(2) 0.79270(19) 0.0165(10) Uani 1 1 d . . . . .
N3 N 0.3435(2) 0.7244(2) 0.8437(2) 0.0180(11) Uani 1 1 d . . . . .
C1 C 0.2987(3) 0.7701(3) 1.0152(3) 0.0320(18) Uani 1 1 d . . . . .
H1 H 0.3181 0.7987 1.0343 0.038 Uiso 1 1 calc R U . . .
C2 C 0.3162(3) 0.7555(3) 0.9610(3) 0.0317(18) Uani 1 1 d . . . . .
H2 H 0.3461 0.7746 0.9438 0.038 Uiso 1 1 calc R U . . .
C3 C 0.2882(3) 0.7118(3) 0.9328(3) 0.0209(17) Uani 1 2 d S T P . .
C4 C 0.3036(3) 0.6964(3) 0.8727(4) 0.0188(18) Uani 1 2 d S T P . .
C5 C 0.4130(2) 0.7278(4) 0.5870(2) 0.0211(19) Uani 1 2 d S T P . .
C6 C 0.4579(3) 0.7304(6) 0.5421(3) 0.034(3) Uani 1 2 d S T P . .
C7 C 0.5156(3) 0.7315(5) 0.5571(3) 0.061(3) Uani 1 1 d . . . . .
H7 H 0.5260 0.7322 0.5952 0.073 Uiso 1 1 calc R U . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0106(5) 0.0133(3) 0.0133(3) -0.0003(5) 0.0003(3) 0.0003(3)
O1 0.014(2) 0.040(3) 0.019(2) -0.005(2) 0.0061(17) -0.002(2)
O2 0.014(2) 0.014(2) 0.014(2) -0.002(2) 0.002(2) 0.002(2)
N1 0.025(2) 0.025(2) 0.005(3) -0.002(2) 0.002(2) -0.002(3)
N2 0.019(2) 0.021(3) 0.009(2) -0.0019(19) -0.0016(18) -0.0019(19)
N3 0.022(3) 0.024(3) 0.009(2) -0.004(2) 0.0021(18) -0.003(2)
C1 0.029(4) 0.040(4) 0.027(4) -0.019(3) 0.012(3) -0.018(3)
C2 0.030(4) 0.051(5) 0.014(3) -0.012(3) 0.007(3) -0.011(3)
C3 0.026(3) 0.026(3) 0.011(3) -0.006(2) 0.006(2) -0.007(4)
C4 0.020(3) 0.020(3) 0.015(4) -0.002(2) 0.002(2) 0.000(3)
C5 0.018(3) 0.028(5) 0.018(3) -0.003(2) 0.011(3) 0.003(2)
C6 0.013(3) 0.074(9) 0.013(3) -0.005(3) 0.010(3) 0.005(3)
C7 0.023(4) 0.144(11) 0.016(4) -0.001(5) -0.004(3) -0.008(5)

_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 O2 2.036(2) . ?
Co1 N1 2.115(7) 32_656 ?
Co1 O1 2.122(4) . ?
Co1 O1 2.122(4) 17 ?
Co1 N2 2.157(5) 17 ?
Co1 N2 2.157(5) . ?
O1 C5 1.261(6) . ?
O2 Co1 2.036(2) 7_665 ?
O2 Co1 2.036(2) 10_656 ?
N1 C1 1.337(7) 14_665 ?
N1 C1 1.337(7) . ?
N1 Co1 2.116(7) 35_466 ?
N2 N2 1.324(10) 14_665 ?
N2 N3 1.346(6) . ?
N3 C4 1.336(7) . ?
C1 C2 1.386(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.392(8) . ?
C2 H2 0.9300 . ?
C3 C2 1.392(8) 14_665 ?
C3 C4 1.508(11) . ?
C4 N3 1.336(7) 14_665 ?
C5 O1 1.261(6) 23_656 ?
C5 C6 1.500(12) . ?
C6 C7 1.406(9) 23_656 ?
C6 C7 1.406(9) . ?
C7 C7 1.382(16) 21 ?
C7 H7 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 N1 171.9(3) . 32_656 ?
O2 Co1 O1 86.8(2) . . ?
N1 Co1 O1 87.36(19) 32_656 . ?
O2 Co1 O1 86.8(2) . 17 ?
N1 Co1 O1 87.36(19) 32_656 17 ?
O1 Co1 O1 88.9(3) . 17 ?
O2 Co1 N2 88.5(2) . 17 ?
N1 Co1 N2 97.04(19) 32_656 17 ?
O1 Co1 N2 88.89(19) . 17 ?
O1 Co1 N2 175.0(2) 17 17 ?
O2 Co1 N2 88.5(2) . . ?
N1 Co1 N2 97.04(19) 32_656 . ?
O1 Co1 N2 175.0(2) . . ?
O1 Co1 N2 88.89(19) 17 . ?
N2 Co1 N2 93.0(3) 17 . ?
C5 O1 Co1 132.1(5) . . ?
Co1 O2 Co1 116.57(16) 7_665 10_656 ?
Co1 O2 Co1 116.57(16) 7_665 . ?
Co1 O2 Co1 116.57(16) 10_656 . ?
C1 N1 C1 118.0(8) 14_665 . ?
C1 N1 Co1 120.3(4) 14_665 35_466 ?
C1 N1 Co1 120.3(4) . 35_466 ?
N2 N2 N3 110.4(3) 14_665 . ?
N2 N2 Co1 119.73(13) 14_665 . ?
N3 N2 Co1 129.8(4) . . ?
C4 N3 N2 101.7(5) . . ?
N1 C1 C2 123.0(6) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 118.8(6) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C2 C3 C2 118.3(8) 14_665 . ?
C2 C3 C4 120.8(4) 14_665 . ?
C2 C3 C4 120.8(4) . . ?
N3 C4 N3 115.8(7) 14_665 . ?
N3 C4 C3 122.0(4) 14_665 . ?
N3 C4 C3 122.0(4) . . ?
O1 C5 O1 128.3(8) . 23_656 ?
O1 C5 C6 115.8(4) . . ?
O1 C5 C6 115.8(4) 23_656 . ?
C7 C6 C7 119.2(9) 23_656 . ?
C7 C6 C5 120.4(5) 23_656 . ?
C7 C6 C5 120.4(4) . . ?
C7 C7 C6 120.4(4) 21 . ?
C7 C7 H7 119.8 21 . ?
C6 C7 H7 119.8 . . ?

_refine_diff_density_max         1.221
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.130

_shelx_res_file                  
;

    1.res created by SHELXL-2014/7

TITL 1 in I-43m
CELL 0.71073  23.5702  23.5702  23.5702  90.000  90.000  90.000
ZERR  8   0.0027   0.0027   0.0027   0.000   0.000   0.000
LATT -2
SYMM -X, -Y, Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM Z, X, Y
SYMM Z, -X, -Y
SYMM -Z, -X, Y
SYMM -Z, X, -Y
SYMM Y, Z, X
SYMM -Y, Z, -X
SYMM Y, -Z, -X
SYMM -Y, -Z, X
SYMM Y, X, Z
SYMM -Y, -X, Z
SYMM Y, -X, -Z
SYMM -Y, X, -Z
SYMM X, Z, Y
SYMM -X, Z, -Y
SYMM -X, -Z, Y
SYMM X, -Z, -Y
SYMM Z, Y, X
SYMM Z, -Y, -X
SYMM -Z, Y, -X
SYMM -Z, -Y, X
SFAC C  H  N  O  Co
UNIT 304 320 144 72 24
MERG 2
L.S. 10
ACTA
BOND   $H
FMAP 2
PLAN 10
LIST 6
WGHT    0.073200
FVAR       0.61350
CO1   5    0.387836    0.716080    0.716080    10.50000    0.01064    0.01328 =
         0.01328   -0.00032    0.00031    0.00031
O1    4    0.430547    0.726687    0.637534    11.00000    0.01429    0.03976 =
         0.01910   -0.00477    0.00608   -0.00178
O2    4    0.327902    0.672098    0.672098    10.16667    0.01352    0.01352 =
         0.01352   -0.00156    0.00156    0.00156
N1    3    0.255098    0.744902    1.041372    10.50000    0.02504    0.02504 =
         0.00477   -0.00167    0.00167   -0.00232
N2    3    0.340871    0.698860    0.792698    11.00000    0.01913    0.02134 =
         0.00890   -0.00190   -0.00160   -0.00194
N3    3    0.343515    0.724381    0.843739    11.00000    0.02162    0.02356 =
         0.00896   -0.00389    0.00209   -0.00331
C1    1    0.298669    0.770080    1.015220    11.00000    0.02896    0.04000 =
         0.02696   -0.01923    0.01206   -0.01769
AFIX  43
H1    2    0.318108    0.798655    1.034257    11.00000   -1.20000
AFIX   0
C2    1    0.316182    0.755512    0.960998    11.00000    0.03009    0.05115 =
         0.01387   -0.01216    0.00722   -0.01104
AFIX  43
H2    2    0.346104    0.774597    0.943756    11.00000   -1.20000
AFIX   0
C3    1    0.288187    0.711813    0.932818    10.50000    0.02585    0.02585 =
         0.01086   -0.00599    0.00599   -0.00694
C4    1    0.303641    0.696359    0.872687    10.50000    0.02047    0.02047 =
         0.01541   -0.00245    0.00245   -0.00046
C5    1    0.412978    0.727776    0.587022    10.50000    0.01763    0.02808 =
         0.01763   -0.00284    0.01052    0.00284
C6    1    0.457934    0.730400    0.542066    10.50000    0.01322    0.07445 =
         0.01322   -0.00535    0.01003    0.00535
C7    1    0.515635    0.731501    0.557104    11.00000    0.02271    0.14437 =
         0.01649   -0.00073   -0.00401   -0.00758
AFIX  43
H7    2    0.525970    0.732236    0.595176    11.00000   -1.20000
AFIX   0
HKLF    4

REM  1 in I-43m
REM R1 =  0.0661 for    2469 Fo > 4sig(Fo)  and  0.0762 for all    2895 data
REM     94 parameters refined using      0 restraints

END

WGHT      0.0731      0.0000

REM Highest difference peak  1.221,  deepest hole -0.850,  1-sigma level  0.130
Q1    1   0.5000  0.5000  0.5000  10.04167  0.05    1.22
Q2    1   0.5000  0.9305  0.5000  10.25000  0.05    0.73
Q3    1   0.5000  1.0000  1.0000  10.12500  0.05    0.52
Q4    1   0.4297  0.5703  1.0060  10.50000  0.05    0.51
Q5    1   0.4198  0.5802  0.5802  10.16667  0.05    0.50
Q6    1   0.5420  0.6809  0.5420  10.50000  0.05    0.50
Q7    1   0.3985  0.7067  0.7773  11.00000  0.05    0.43
Q8    1   0.4804  0.6894  0.6003  11.00000  0.05    0.42
Q9    1   0.3631  0.7306  0.6369  10.50000  0.05    0.40
Q10   1   0.5280  0.8587  0.5280  10.50000  0.05    0.40
;
_shelx_res_checksum              91311
