# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_2
_database_code_depnum_ccdc_archive 'CCDC 1828124'
loop_
_audit_author_name
_audit_author_address
'Min Di'
;Northeast Normal University
China
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;
_audit_creation_date             2019-01-17
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.01.14 svn.r3558 for OlexSys, GUI svn.r5646)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.5(C240 H212 Mn24 N36 O128), H8 Mn1 O4, 2(C2 H8 N)+, 36H2O'
_chemical_formula_sum            'C124 H202 Mn13 N20 O104'
_chemical_formula_weight         4351.24
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Mn Mn 0.3368 0.7283 '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'

_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      cubic
_space_group_IT_number           218
_space_group_name_H-M_alt        'P -4 3 n'
_space_group_name_Hall           'P -4n 2 3'
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+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                   22.5444(4)
_cell_length_b                   22.5444(4)
_cell_length_c                   22.5444(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11458.2(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4147
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      29.2539
_cell_measurement_theta_min      2.8514
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4450
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            21484
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.985
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_min         2.857
_diffrn_ambient_temperature      273(2)
_diffrn_detector_area_resol_mean 10.2375
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -32.00   55.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.6627   57.0000  -30.0000 87
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.844
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2803
_reflns_number_total             3364
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3364
_refine_ls_number_restraints     38
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0487
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0643P)²+4.8241P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1230
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.89(5)
 0.11(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
O1W \\sim O1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 O1, N2, C1, C2, C3, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Mn2, O7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O1(0.5) O1W(0.5) N2(0.5) C1(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
 O7(0.3333) H7A(0.3333) H7B(0.3333) O12(0.5)
 Fixed Uiso: C3(0.1) O12(0.1)
6.a Rotating group:
 O7(H7A,H7B)
6.b Ternary CH refined with riding coordinates:
 O2(H2)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Mn1 Mn 0.69078(4) 0.82293(4) 0.24106(4) 0.0244(3) Uani 1 1 d . . . . .
O2 O 0.75810(18) 0.75810(18) 0.24190(18) 0.0215(13) Uani 1 3 d S T P . .
H2 H 0.783199 0.783199 0.216801 0.026 Uiso 1 3 calc RS T P . .
O1 O 0.623(2) 0.8894(19) 0.2372(16) 0.064(3) Uani 0.5 1 d . U . A 1
O1W O 0.6232(19) 0.9010(18) 0.2259(15) 0.063(3) Uani 0.5 1 d . U . A 2
O3 O 0.6774(2) 0.8044(3) 0.3336(2) 0.0567(14) Uani 1 1 d . . . . .
O4 O 0.76060(19) 0.7774(2) 0.37983(19) 0.0388(11) Uani 1 1 d . . . . .
O5 O 0.74976(18) 0.7640(2) 0.60482(18) 0.0388(11) Uani 1 1 d . . . . .
O6 O 0.6631(2) 0.7911(2) 0.64735(18) 0.0461(13) Uani 1 1 d . . . . .
N1 N 0.5146(3) 0.7801(3) 0.4759(2) 0.0578(19) Uani 1 1 d . . . . .
N2 N 0.6101(8) 0.9555(9) 0.1576(8) 0.101(5) Uani 0.5 1 d . U . A 1
C1 C 0.6047(8) 0.9160(10) 0.1842(9) 0.080(4) Uani 0.5 1 d . U . A 1
C2 C 0.5646(10) 0.8779(12) 0.1350(10) 0.106(6) Uani 0.5 1 d . U . A 1
H2A H 0.526587 0.868571 0.151772 0.159 Uiso 0.5 1 calc GR . . A 1
H2B H 0.584917 0.841807 0.125001 0.159 Uiso 0.5 1 calc GR . . A 1
H2C H 0.559230 0.901326 0.099840 0.159 Uiso 0.5 1 calc GR . . A 1
C3 C 0.6495(11) 1.0033(13) 0.1940(11) 0.100 Uiso 0.5 1 d . U . A 1
H3A H 0.637322 1.003581 0.234792 0.150 Uiso 0.5 1 calc GR . . A 1
H3B H 0.643817 1.042080 0.177251 0.150 Uiso 0.5 1 calc GR . . A 1
H3C H 0.690612 0.992652 0.191477 0.150 Uiso 0.5 1 calc GR . . A 1
C4 C 0.5879(8) 0.9751(12) 0.0953(9) 0.113(10) Uani 0.5 1 d . U . A 1
H4A H 0.599267 0.946060 0.066398 0.170 Uiso 0.5 1 calc GR . . A 1
H4B H 0.605157 1.012722 0.085289 0.170 Uiso 0.5 1 calc GR . . A 1
H4C H 0.545432 0.978725 0.095897 0.170 Uiso 0.5 1 calc GR . . A 1
C5 C 0.7066(3) 0.7897(3) 0.3781(3) 0.0397(17) Uani 1 1 d . . . . .
C6 C 0.6727(3) 0.7852(3) 0.4347(3) 0.0387(17) Uani 1 1 d . . . . .
C7 C 0.6095(3) 0.7835(4) 0.4333(3) 0.0459(19) Uani 1 1 d . . . . .
H7 H 0.589598 0.784169 0.397167 0.055 Uiso 1 1 calc R . . . .
C8 C 0.5782(3) 0.7810(4) 0.4850(3) 0.055(2) Uani 1 1 d . . . . .
C9 C 0.6050(3) 0.7791(4) 0.5402(3) 0.0421(18) Uani 1 1 d . . . . .
H9 H 0.582117 0.776481 0.574423 0.051 Uiso 1 1 calc R . . . .
C10 C 0.6657(3) 0.7812(3) 0.5441(3) 0.0387(17) Uani 1 1 d . . . . .
C11 C 0.6997(3) 0.7814(3) 0.4916(3) 0.0338(16) Uani 1 1 d . . . . .
H11 H 0.740795 0.779089 0.494248 0.041 Uiso 1 1 calc R . . . .
C12 C 0.6969(3) 0.7789(3) 0.6034(3) 0.0358(16) Uani 1 1 d . . . . .
Mn2 Mn 0.500000 0.500000 0.500000 0.0711(13) Uani 1 12 d S TU P . .
O7 O 0.4656(12) 0.5900(11) 0.4755(13) 0.124(9) Uani 0.3333 1 d . U . . .
H7A H 0.462782 0.622132 0.496503 0.186 Uiso 0.3333 1 d GR . . . .
H7B H 0.453252 0.600262 0.440562 0.186 Uiso 0.3333 1 d GR . . . .
O12 O 0.6745(7) 0.9816(8) 0.1836(8) 0.100 Uiso 0.5 1 d . . . B 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
Mn1 O2 2.1070(8) . ?
Mn1 O1 2.14(4) . ?
Mn1 O1W 2.35(4) . ?
Mn1 O3 2.148(5) . ?
Mn1 O4 2.164(4) 8_656 ?
Mn1 O5 2.172(4) 19_664 ?
Mn1 O6 2.175(4) 14_664 ?
O2 H2 0.9800 . ?
O1 C1 1.40(3) . ?
O3 C5 1.245(8) . ?
O4 C5 1.249(8) . ?
O5 C12 1.238(8) . ?
O6 C12 1.281(8) . ?
N1 N1 1.269(10) 3_656 ?
N1 C8 1.449(9) . ?
N2 C1 1.08(3) . ?
N2 C3 1.62(3) . ?
N2 C4 1.55(2) . ?
C1 C2 1.67(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.492(9) . ?
C6 C7 1.426(9) . ?
C6 C11 1.422(9) . ?
C7 H7 0.9300 . ?
C7 C8 1.363(9) . ?
C8 C9 1.386(9) . ?
C9 H9 0.9300 . ?
C9 C10 1.372(9) . ?
C10 C11 1.409(9) . ?
C10 C12 1.511(8) . ?
C11 H11 0.9300 . ?
Mn2 O7 2.24(2) 8_656 ?
Mn2 O7 2.24(2) 3_656 ?
Mn2 O7 2.24(3) 11_566 ?
Mn2 O7 2.24(2) . ?
Mn2 O7 2.24(2) 5 ?
Mn2 O7 2.24(2) 12_665 ?
Mn2 O7 2.24(2) 6_566 ?
Mn2 O7 2.24(2) 7_665 ?
Mn2 O7 2.24(2) 9 ?
Mn2 O7 2.24(2) 2_665 ?
Mn2 O7 2.24(2) 10_656 ?
Mn2 O7 2.24(2) 4_566 ?
O7 H7A 0.8680 . ?
O7 H7B 0.8662 . ?

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 Mn1 O1 178.1(9) . . ?
O2 Mn1 O1W 170.6(8) . . ?
O2 Mn1 O3 87.6(2) . . ?
O2 Mn1 O4 94.66(17) . 8_656 ?
O2 Mn1 O5 94.22(17) . 19_664 ?
O2 Mn1 O6 88.5(2) . 14_664 ?
O1 Mn1 O3 94.3(9) . . ?
O1 Mn1 O4 85.5(13) . 8_656 ?
O1 Mn1 O5 85.7(13) . 19_664 ?
O1 Mn1 O6 89.6(9) . 14_664 ?
O3 Mn1 O1W 101.3(9) . . ?
O3 Mn1 O4 87.5(2) . 8_656 ?
O3 Mn1 O5 90.1(2) . 19_664 ?
O3 Mn1 O6 176.07(19) . 14_664 ?
O4 Mn1 O1W 88.9(12) 8_656 . ?
O4 Mn1 O5 170.71(16) 8_656 19_664 ?
O4 Mn1 O6 92.63(19) 8_656 14_664 ?
O5 Mn1 O1W 82.7(12) 19_664 . ?
O5 Mn1 O6 90.34(18) 19_664 14_664 ?
O6 Mn1 O1W 82.6(9) 14_664 . ?
Mn1 O2 Mn1 119.991(7) 8_656 . ?
Mn1 O2 Mn1 119.990(7) 11_566 8_656 ?
Mn1 O2 Mn1 119.989(7) 11_566 . ?
Mn1 O2 H2 90.6 . . ?
Mn1 O2 H2 90.6 8_656 . ?
Mn1 O2 H2 90.6 11_566 . ?
C1 O1 Mn1 123(3) . . ?
C5 O3 Mn1 139.4(5) . . ?
C5 O4 Mn1 130.7(4) . 11_566 ?
C12 O5 Mn1 132.7(4) . 18_656 ?
C12 O6 Mn1 134.9(4) . 14_665 ?
N1 N1 C8 113.0(7) 3_656 . ?
C1 N2 C3 109(2) . . ?
C1 N2 C4 134(3) . . ?
C4 N2 C3 116.4(19) . . ?
O1 C1 C2 121(3) . . ?
N2 C1 O1 142(3) . . ?
N2 C1 C2 96.7(19) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O3 C5 O4 126.9(6) . . ?
O3 C5 C6 115.9(6) . . ?
O4 C5 C6 117.2(6) . . ?
C7 C6 C5 119.6(6) . . ?
C11 C6 C5 123.8(5) . . ?
C11 C6 C7 116.5(5) . . ?
C6 C7 H7 120.0 . . ?
C8 C7 C6 120.0(6) . . ?
C8 C7 H7 120.0 . . ?
C7 C8 N1 113.1(6) . . ?
C7 C8 C9 122.9(6) . . ?
C9 C8 N1 124.0(6) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.5(6) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C11 119.3(6) . . ?
C9 C10 C12 121.2(6) . . ?
C11 C10 C12 119.4(6) . . ?
C6 C11 H11 119.2 . . ?
C10 C11 C6 121.6(5) . . ?
C10 C11 H11 119.2 . . ?
O5 C12 O6 127.7(5) . . ?
O5 C12 C10 118.7(6) . . ?
O6 C12 C10 113.6(6) . . ?
O7 Mn2 O7 100.1(10) 12_665 5 ?
O7 Mn2 O7 89.7(11) 11_566 5 ?
O7 Mn2 O7 116.8(4) 5 . ?
O7 Mn2 O7 51.5(10) 8_656 9 ?
O7 Mn2 O7 89.7(11) 7_665 . ?
O7 Mn2 O7 151.4(15) 6_566 5 ?
O7 Mn2 O7 116.8(4) 9 . ?
O7 Mn2 O7 51.5(10) 2_665 9 ?
O7 Mn2 O7 116.8(4) 3_656 8_656 ?
O7 Mn2 O7 139.5(14) 4_566 . ?
O7 Mn2 O7 151.4(15) 3_656 4_566 ?
O7 Mn2 O7 151.4(15) 11_566 12_665 ?
O7 Mn2 O7 100.1(10) 3_656 12_665 ?
O7 Mn2 O7 116.8(4) 4_566 6_566 ?
O7 Mn2 O7 116.8(4) 11_566 4_566 ?
O7 Mn2 O7 89.7(11) 10_656 . ?
O7 Mn2 O7 116.8(4) 7_665 12_665 ?
O7 Mn2 O7 51.5(10) 4_566 5 ?
O7 Mn2 O7 100.1(10) 3_656 5 ?
O7 Mn2 O7 51.5(10) 7_665 3_656 ?
O7 Mn2 O7 89.7(11) 8_656 12_665 ?
O7 Mn2 O7 139.5(14) 12_665 9 ?
O7 Mn2 O7 100.1(10) 10_656 6_566 ?
O7 Mn2 O7 100.1(10) 11_566 8_656 ?
O7 Mn2 O7 100.1(10) 7_665 4_566 ?
O7 Mn2 O7 50.3(12) 3_656 . ?
O7 Mn2 O7 151.4(15) 2_665 . ?
O7 Mn2 O7 151.4(15) 7_665 8_656 ?
O7 Mn2 O7 89.7(11) 8_656 4_566 ?
O7 Mn2 O7 89.7(11) 6_566 9 ?
O7 Mn2 O7 100.1(10) 7_665 9 ?
O7 Mn2 O7 116.8(4) 3_656 10_656 ?
O7 Mn2 O7 100.1(10) 2_665 6_566 ?
O7 Mn2 O7 116.8(4) 8_656 10_656 ?
O7 Mn2 O7 116.8(4) 5 9 ?
O7 Mn2 O7 50.3(12) 12_665 10_656 ?
O7 Mn2 O7 139.5(14) 8_656 5 ?
O7 Mn2 O7 51.5(10) 4_566 10_656 ?
O7 Mn2 O7 51.5(10) 10_656 5 ?
O7 Mn2 O7 89.7(11) 11_566 2_665 ?
O7 Mn2 O7 89.7(11) 2_665 5 ?
O7 Mn2 O7 116.8(4) 7_665 2_665 ?
O7 Mn2 O7 50.3(12) 7_665 5 ?
O7 Mn2 O7 139.5(14) 3_656 2_665 ?
O7 Mn2 O7 89.7(11) 3_656 9 ?
O7 Mn2 O7 51.5(10) 8_656 2_665 ?
O7 Mn2 O7 100.1(10) 4_566 9 ?
O7 Mn2 O7 116.8(4) 12_665 2_665 ?
O7 Mn2 O7 151.4(15) 10_656 9 ?
O7 Mn2 O7 50.3(12) 4_566 2_665 ?
O7 Mn2 O7 51.5(10) 11_566 7_665 ?
O7 Mn2 O7 100.1(10) 10_656 2_665 ?
O7 Mn2 O7 100.1(10) 11_566 . ?
O7 Mn2 O7 116.8(4) 11_566 6_566 ?
O7 Mn2 O7 100.1(10) 8_656 . ?
O7 Mn2 O7 139.5(14) 7_665 6_566 ?
O7 Mn2 O7 51.5(10) 12_665 . ?
O7 Mn2 O7 89.7(11) 3_656 6_566 ?
O7 Mn2 O7 50.3(12) 11_566 9 ?
O7 Mn2 O7 51.5(10) 12_665 6_566 ?
O7 Mn2 O7 51.5(10) 6_566 . ?
O7 Mn2 O7 89.7(11) 12_665 4_566 ?
O7 Mn2 O7 50.3(12) 8_656 6_566 ?
O7 Mn2 O7 139.5(14) 11_566 10_656 ?
O7 Mn2 O7 51.5(10) 11_566 3_656 ?
O7 Mn2 O7 89.7(11) 7_665 10_656 ?
Mn2 O7 H7A 130.2 . . ?
Mn2 O7 H7B 125.2 . . ?
H7A O7 H7B 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn1 O1 C1 N2 -100(5) . . . . ?
Mn1 O1 C1 C2 72(4) . . . . ?
Mn1 O3 C5 O4 -3.9(14) . . . . ?
Mn1 O3 C5 C6 177.4(5) . . . . ?
Mn1 O4 C5 O3 -13.5(12) 11_566 . . . ?
Mn1 O4 C5 C6 165.1(5) 11_566 . . . ?
Mn1 O5 C12 O6 8.1(12) 18_656 . . . ?
Mn1 O5 C12 C10 -169.2(5) 18_656 . . . ?
Mn1 O6 C12 O5 13.4(12) 14_665 . . . ?
Mn1 O6 C12 C10 -169.2(5) 14_665 . . . ?
O3 C5 C6 C7 14.8(11) . . . . ?
O3 C5 C6 C11 -166.2(7) . . . . ?
O4 C5 C6 C7 -164.0(7) . . . . ?
O4 C5 C6 C11 15.0(11) . . . . ?
N1 N1 C8 C7 -177.4(6) 3_656 . . . ?
N1 N1 C8 C9 3.0(11) 3_656 . . . ?
N1 C8 C9 C10 -178.9(8) . . . . ?
C3 N2 C1 O1 -6(4) . . . . ?
C3 N2 C1 C2 -179.3(15) . . . . ?
C4 N2 C1 O1 175(4) . . . . ?
C4 N2 C1 C2 2(3) . . . . ?
C5 C6 C7 C8 -178.3(8) . . . . ?
C5 C6 C11 C10 175.8(7) . . . . ?
C6 C7 C8 N1 179.5(8) . . . . ?
C6 C7 C8 C9 -0.9(14) . . . . ?
C7 C6 C11 C10 -5.2(11) . . . . ?
C7 C8 C9 C10 1.5(15) . . . . ?
C8 C9 C10 C11 -4.0(13) . . . . ?
C8 C9 C10 C12 -179.6(8) . . . . ?
C9 C10 C11 C6 6.0(11) . . . . ?
C9 C10 C12 O5 159.6(7) . . . . ?
C9 C10 C12 O6 -18.0(10) . . . . ?
C11 C6 C7 C8 2.7(12) . . . . ?
C11 C10 C12 O5 -16.0(10) . . . . ?
C11 C10 C12 O6 166.4(7) . . . . ?
C12 C10 C11 C6 -178.3(7) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 679 electrons were 
found in a volume of 3967Å^3 in 2 voids. 
This is consistent with the presence of 
2[(CH3)2NH2]+, 30[H2O] per formula unit 
which account for 704 electrons.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.111 -0.805 -0.715 2377.3 209.2 'H2O and 0.33 ((CH3)2NH2)+'
2 0.000 0.000 0.000 795.3 234.7 '2 H2O'
3 0.500 0.500 0.500 795.3 234.7 '2 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.89(5)
2 0.11(5)

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1828125'
loop_
_audit_author_name
_audit_author_address
'Min Di'
;Northeast Normal University
China
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;
_audit_creation_date             2018-11-26
_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         '0.33(C156 H111 N21 O90 Zn18)'
_chemical_formula_sum            'C52 H37 N7 O30 Zn6'
_chemical_formula_weight         1632.10
_chemical_absolute_configuration .
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Zn Zn 0.2839 1.4301 '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      trigonal
_space_group_IT_number           150
_space_group_name_H-M_alt        'P 3 2 1'
_space_group_name_Hall           'P 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'

_cell_length_a                   22.8480(10)
_cell_length_b                   22.8480(10)
_cell_length_c                   20.330(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9191.0(12)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    170.15
_cell_measurement_theta_max      25.862
_cell_measurement_theta_min      2.682
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.9172
_exptl_absorpt_correction_T_min  0.7658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.885
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2454
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            78837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.055
_diffrn_reflns_theta_min         2.252
_diffrn_ambient_temperature      170.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9667
_reflns_number_total             12112
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       SAINT
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2018/3 (Sheldrick, 2015)'
_refine_diff_density_max         0.792
_refine_diff_density_min         -2.530
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         12112
_refine_ls_number_restraints     160
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0644
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0889P)²+20.9271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1749
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.51(3)
 0.49(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C20-N3 = N3A-C30
 1.4 with sigma of 0.02
 N3-N3A
 1.2 with sigma of 0.02
 O6-C9 = C9-O5
 1.2 with sigma of 0.02
 C9-C8
 1.4 with sigma of 0.02
 O6A-C9A = C9A-O5A
 1.2 with sigma of 0.02
 C9A-C8
 1.4 with sigma of 0.02
 C25-C22
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C9A) \\sim
Ueq, Uanis(O6A) \\sim Ueq, Uanis(O5A) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N3, C20, C30, N3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O6, C8, C9, C9A, O6A, O5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C15, C16, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C22, O15, N4, C24, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O5(0.5) O6(0.5) O7(0.5) H7A(0.5) H7B(0.5) H15A(0.5) H15B(0.5)
 N3(0.5) N4(0.5) C9(0.5) C22(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
 N3A(0.5) C9A(0.5) O6A(0.5) O5A(0.5) O7A(0.5) H7AA(0.5) H7AB(0.5)
7.a Riding coordinates:
 O7(H7A,H7B), O13(H13A,H13B), O15(H15A,H15B), O7A(H7AA,H7AB)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C13(H13), C14(H14), C17(H17), C19(H19), C21(H21),
 C28(H28), C29(H29)
7.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.25941(5) 0.11355(5) 0.84842(6) 0.0400(3) Uani 1 1 d . . . . .
Zn2 Zn 0.40760(5) 0.19925(7) 0.81936(7) 0.0593(4) Uani 1 1 d . . . . .
Zn3 Zn 0.07449(4) 0.56232(4) 0.48557(5) 0.0253(2) Uani 1 1 d . . . . .
O1 O 0.3066(4) 0.0791(5) 0.9098(5) 0.075(3) Uani 1 1 d . . . . .
O2 O 0.4166(4) 0.1381(6) 0.8857(5) 0.092(3) Uani 1 1 d . . . . .
O3 O 0.3623(4) 0.2328(5) 0.7574(4) 0.075(3) Uani 1 1 d . . . . .
O4 O 0.2499(4) 0.1746(4) 0.7816(4) 0.064(2) Uani 1 1 d . . . . .
O5 O -0.0354(12) 0.4494(16) 0.5822(18) 0.082(8) Uani 0.5 1 d D U . A 1
O6 O 0.0735(10) 0.4990(9) 0.5531(11) 0.046(4) Uani 0.5 1 d D U . A 1
O7 O 0.1724(14) 0.5964(14) 0.4747(16) 0.108(10) Uani 0.5 1 d . . . A 1
H7A H 0.203086 0.607282 0.504957 0.162 Uiso 0.5 1 d R . . A 1
H7B H 0.194446 0.604222 0.437807 0.162 Uiso 0.5 1 d R . . A 1
O8 O -0.0697(4) 0.2151(4) 0.7740(4) 0.055(2) Uani 1 1 d . . . . .
O9 O -0.1302(5) 0.2648(5) 0.7517(5) 0.079(3) Uani 1 1 d . . . . .
O10 O 0.4355(4) 0.3925(4) 0.5793(4) 0.067(3) Uani 1 1 d . . . . .
O11 O 0.3789(4) 0.4505(5) 0.5581(4) 0.073(3) Uani 1 1 d . . . . .
O12 O 0.7578(5) 0.1405(5) 0.8915(5) 0.092(3) Uani 1 1 d . . . . .
O13 O 0.4999(4) 0.2710(4) 0.8056(5) 0.095(3) Uani 1 1 d . . . . .
H13A H 0.520944 0.311187 0.822684 0.143 Uiso 1 1 d R . . . .
H13B H 0.528084 0.270888 0.780284 0.143 Uiso 1 1 d R . . . .
O14 O 0.8168(4) 0.0894(4) 0.9163(4) 0.064(2) Uani 1 1 d . . . . .
O15 O 0.1638(3) 0.0387(3) 0.8600(4) 0.0452(16) Uani 1 1 d . U . . .
H15A H 0.142305 0.021852 0.896629 0.068 Uiso 0.5 1 d R . . B 2
H15B H 0.134565 0.015792 0.829419 0.068 Uiso 0.5 1 d R . . B 2
N1 N 0.1579(5) 0.3122(5) 0.6845(5) 0.074(3) Uani 1 1 d . . . . .
N2 N 0.1505(6) 0.3549(7) 0.6534(7) 0.108(6) Uani 1 1 d . . . . .
N3 N 0.5167(12) 0.0216(18) 0.9807(18) 0.082(8) Uani 0.5 1 d D U . C -1
N4 N 0.0811(7) -0.0595(8) 0.8934(8) 0.053(4) Uani 0.5 1 d . U . D -1
C1 C 0.3662(5) 0.0917(6) 0.9182(6) 0.059(3) Uani 1 1 d . . . . .
C2 C 0.3030(7) 0.2206(6) 0.7558(5) 0.063(3) Uani 1 1 d . . . . .
C3 C 0.2904(6) 0.2688(7) 0.7131(7) 0.076(4) Uani 1 1 d . . . . .
C4 C 0.2299(6) 0.2700(6) 0.7162(6) 0.061(3) Uani 1 1 d . . . . .
H4 H 0.195065 0.240928 0.745576 0.073 Uiso 1 1 calc R . . . .
C5 C 0.2214(6) 0.3154(7) 0.6749(7) 0.083(5) Uani 1 1 d . . . . .
C6 C 0.0885(6) 0.3533(7) 0.6581(7) 0.072(4) Uani 1 1 d . . . . .
C7 C 0.0800(7) 0.4015(7) 0.6256(6) 0.072(4) Uani 1 1 d . . . . .
H7 H 0.117430 0.435848 0.602147 0.087 Uiso 1 1 calc R . . . .
C8 C 0.0225(8) 0.4027(7) 0.6252(7) 0.073(4) Uani 1 1 d D U . . .
C9 C 0.0226(13) 0.4558(17) 0.582(2) 0.075(8) Uani 0.5 1 d D U . A 1
C10 C -0.0312(7) 0.3540(6) 0.6651(5) 0.067(3) Uani 1 1 d . . . . .
H10 H -0.072874 0.353752 0.667282 0.080 Uiso 1 1 calc R . . . .
C11 C -0.0225(6) 0.3066(6) 0.7011(6) 0.064(3) Uani 1 1 d . . . . .
C12 C -0.0780(6) 0.2558(6) 0.7447(6) 0.063(3) Uani 1 1 d . . . . .
C13 C 0.0373(7) 0.3067(6) 0.7002(6) 0.071(4) Uani 1 1 d . . . . .
H13 H 0.044131 0.276483 0.726902 0.085 Uiso 1 1 calc R . . . .
C14 C 0.2725(6) 0.3607(7) 0.6360(7) 0.078(4) Uani 1 1 d . U . . .
H14 H 0.267864 0.393453 0.611388 0.093 Uiso 1 1 calc R . . . .
C15 C 0.3301(5) 0.3577(6) 0.6333(6) 0.067(3) Uani 1 1 d . U . . .
C16 C 0.3853(6) 0.4008(6) 0.5831(6) 0.068(4) Uani 1 1 d . U . . .
C17 C 0.3398(6) 0.3134(7) 0.6696(6) 0.072(4) Uani 1 1 d . U . . .
H17 H 0.380883 0.312693 0.665231 0.087 Uiso 1 1 calc R . . . .
C18 C 0.3764(6) 0.0458(8) 0.9614(7) 0.075(4) Uani 1 1 d . . . . .
C19 C 0.4382(6) 0.0437(9) 0.9627(7) 0.090(5) Uani 1 1 d . . . . .
H19 H 0.474891 0.074674 0.936074 0.108 Uiso 1 1 calc R . . . .
C20 C 0.4462(7) 0.000000 1.000000 0.118(10) Uani 1 2 d DS TU P . .
C21 C 0.3230(6) 0.000000 1.000000 0.065(5) Uani 1 2 d S T P . .
H21 H 0.281390 -0.000001 0.999999 0.078 Uiso 1 2 calc RS T P . .
C22 C 0.1358(7) -0.0046(9) 0.8979(8) 0.038(3) Uani 0.5 1 d D U . D -1
C23 C 0.0442(13) -0.1167(17) 0.9274(18) 0.142(17) Uani 0.5 1 d . U . D -1
H23A H -0.003206 -0.128102 0.927500 0.213 Uiso 0.5 1 calc GR . . D -1
H23B H 0.060897 -0.110395 0.972710 0.213 Uiso 0.5 1 calc GR . . D -1
H23C H 0.048065 -0.153396 0.906756 0.213 Uiso 0.5 1 calc GR . . D -1
C24 C 0.0619(14) -0.0739(13) 0.8259(12) 0.093(9) Uani 0.5 1 d . U . D -1
H24A H 0.066347 -0.033377 0.804572 0.139 Uiso 0.5 1 calc GR . . D -1
H24B H 0.014880 -0.110598 0.822984 0.139 Uiso 0.5 1 calc GR . . D -1
H24C H 0.091350 -0.087484 0.803793 0.139 Uiso 0.5 1 calc GR . . D -1
C25 C 0.1595(10) 0.0137(13) 0.9715(9) 0.071(7) Uani 0.5 1 d D U . D -1
H25A H 0.203086 0.055807 0.972820 0.107 Uiso 0.5 1 calc GR . . D -1
H25B H 0.164226 -0.022818 0.991264 0.107 Uiso 0.5 1 calc GR . . D -1
H25C H 0.125877 0.019525 0.996118 0.107 Uiso 0.5 1 calc GR . . D -1
C26 C 0.7675(6) 0.0975(7) 0.9205(7) 0.068(3) Uani 1 1 d . . . . .
C27 C 0.7124(6) 0.0475(7) 0.9603(7) 0.069(4) Uani 1 1 d . . . . .
C28 C 0.7178(6) 0.000000 1.000000 0.067(5) Uani 1 2 d S T P . .
H28 H 0.759339 0.000001 1.000001 0.080 Uiso 1 2 calc RS T P . .
C29 C 0.6504(7) 0.0466(9) 0.9623(10) 0.111(7) Uani 1 1 d . . . . .
H29 H 0.646043 0.079064 0.936849 0.133 Uiso 1 1 calc R . . . .
C30 C 0.5942(8) 0.000000 1.000000 0.107(9) Uani 1 2 d DS TU P . .
N3A N 0.5209(12) -0.020(2) 1.0191(18) 0.090(9) Uani 0.5 1 d D U . C -1
C9A C 0.0010(11) 0.4464(11) 0.5902(12) 0.042(4) Uani 0.5 1 d D U . A 2
O6A O 0.0477(9) 0.4865(13) 0.5538(14) 0.059(6) Uani 0.5 1 d D U . A 2
O5A O -0.0585(9) 0.4370(10) 0.5816(11) 0.040(4) Uani 0.5 1 d D U . A 2
O7A O 0.1714(10) 0.6329(11) 0.4736(11) 0.073(6) Uani 0.5 1 d . . . A 2
H7AA H 0.201136 0.654147 0.504334 0.109 Uiso 0.5 1 d R . . A 2
H7AB H 0.193656 0.648797 0.437074 0.109 Uiso 0.5 1 d R . . A 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
Zn1 Zn2 3.0030(13) . ?
Zn1 O1 2.046(8) . ?
Zn1 O4 2.035(7) . ?
Zn1 O8 2.052(7) 3 ?
Zn1 O14 2.011(8) 3_665 ?
Zn1 O15 2.003(6) . ?
Zn2 O2 2.025(10) . ?
Zn2 O3 2.009(9) . ?
Zn2 O9 2.002(9) 3 ?
Zn2 O12 1.999(9) 3_665 ?
Zn2 O13 1.939(8) . ?
Zn3 Zn3 3.0058(17) 5_556 ?
Zn3 O5 2.06(3) 5_556 ?
Zn3 O6 1.986(19) . ?
Zn3 O7 1.98(3) . ?
Zn3 O10 2.017(7) 6_566 ?
Zn3 O11 2.017(7) 3_565 ?
Zn3 O6A 2.06(2) . ?
Zn3 O5A 1.942(18) 5_556 ?
Zn3 O7A 1.999(19) . ?
O1 C1 1.255(13) . ?
O2 C1 1.290(13) . ?
O3 C2 1.239(15) . ?
O4 C2 1.256(14) . ?
O5 C9 1.26(2) . ?
O6 C9 1.24(2) . ?
O8 C12 1.196(12) . ?
O9 C12 1.317(15) . ?
O10 C16 1.254(17) . ?
O11 C16 1.318(17) . ?
O12 C26 1.258(14) . ?
O14 C26 1.233(14) . ?
O15 C22 1.163(17) . ?
N1 N2 1.245(13) . ?
N1 C5 1.428(15) . ?
N2 C6 1.401(15) . ?
N3 C20 1.483(19) . ?
N3 N3A 1.27(2) . ?
N4 C22 1.26(2) . ?
N4 C23 1.34(3) . ?
N4 C24 1.43(3) . ?
C1 C18 1.474(16) . ?
C2 C3 1.538(15) . ?
C3 C4 1.397(15) . ?
C3 C17 1.394(14) . ?
C4 C5 1.423(15) . ?
C5 C14 1.361(15) . ?
C6 C7 1.380(15) . ?
C6 C13 1.411(15) . ?
C7 C8 1.327(18) . ?
C8 C9 1.49(2) . ?
C8 C10 1.427(17) . ?
C8 C9A 1.496(19) . ?
C10 C11 1.400(13) . ?
C11 C12 1.507(15) . ?
C11 C13 1.366(16) . ?
C14 C15 1.351(17) . ?
C15 C16 1.537(13) . ?
C15 C17 1.359(18) . ?
C18 C19 1.437(14) . ?
C18 C21 1.386(13) . ?
C19 C20 1.337(17) . ?
C22 C25 1.57(2) . ?
C26 C27 1.451(17) . ?
C27 C28 1.406(12) . ?
C27 C29 1.405(15) . ?
C29 C30 1.416(18) . ?
C30 N3A 1.55(2) . ?
C9A O6A 1.24(2) . ?
C9A O5A 1.28(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 Zn2 74.4(2) . . ?
O1 Zn1 O8 85.9(4) . 3 ?
O4 Zn1 Zn2 83.9(2) . . ?
O4 Zn1 O1 158.1(3) . . ?
O4 Zn1 O8 89.8(3) . 3 ?
O8 Zn1 Zn2 70.8(2) 3 . ?
O14 Zn1 Zn2 86.8(2) 3_665 . ?
O14 Zn1 O1 89.3(4) 3_665 . ?
O14 Zn1 O4 86.6(4) 3_665 . ?
O14 Zn1 O8 157.6(3) 3_665 3 ?
O15 Zn1 Zn2 166.4(2) . . ?
O15 Zn1 O1 99.2(3) . . ?
O15 Zn1 O4 102.6(3) . . ?
O15 Zn1 O8 97.1(3) . 3 ?
O15 Zn1 O14 105.3(3) . 3_665 ?
O2 Zn2 Zn1 83.6(2) . . ?
O3 Zn2 Zn1 75.2(3) . . ?
O3 Zn2 O2 158.4(4) . . ?
O9 Zn2 Zn1 87.2(2) 3 . ?
O9 Zn2 O2 86.5(5) 3 . ?
O9 Zn2 O3 88.4(4) 3 . ?
O12 Zn2 Zn1 70.8(2) 3_665 . ?
O12 Zn2 O2 90.1(5) 3_665 . ?
O12 Zn2 O3 86.8(4) 3_665 . ?
O12 Zn2 O9 157.9(3) 3_665 3 ?
O13 Zn2 Zn1 167.2(3) . . ?
O13 Zn2 O2 103.7(4) . . ?
O13 Zn2 O3 97.9(4) . . ?
O13 Zn2 O9 103.5(4) . 3 ?
O13 Zn2 O12 98.5(4) . 3_665 ?
O5 Zn3 Zn3 76.2(7) 5_556 5_556 ?
O6 Zn3 Zn3 81.7(6) . 5_556 ?
O6 Zn3 O5 89.7(12) . 5_556 ?
O6 Zn3 O10 161.4(6) . 6_566 ?
O6 Zn3 O11 89.3(7) . 3_565 ?
O7 Zn3 Zn3 169.1(9) . 5_556 ?
O7 Zn3 O5 100.5(11) . 5_556 ?
O7 Zn3 O6 87.9(11) . . ?
O7 Zn3 O10 110.3(10) . 6_566 ?
O7 Zn3 O11 103.1(9) . 3_565 ?
O10 Zn3 Zn3 79.9(3) 6_566 5_556 ?
O10 Zn3 O5 83.7(10) 6_566 5_556 ?
O10 Zn3 O6A 147.1(6) 6_566 . ?
O11 Zn3 Zn3 80.2(3) 3_565 5_556 ?
O11 Zn3 O5 156.3(8) 3_565 5_556 ?
O11 Zn3 O10 89.9(4) 3_565 6_566 ?
O11 Zn3 O6A 88.5(9) 3_565 . ?
O6A Zn3 O5 84.7(13) . 5_556 ?
O5A Zn3 O5 12.7(10) 5_556 5_556 ?
O5A Zn3 O10 88.1(7) 5_556 6_566 ?
O5A Zn3 O11 168.9(6) 5_556 3_565 ?
O5A Zn3 O6A 87.3(11) 5_556 . ?
O5A Zn3 O7A 104.2(8) 5_556 . ?
O7A Zn3 O5 116.2(9) . 5_556 ?
O7A Zn3 O10 92.4(8) . 6_566 ?
O7A Zn3 O11 86.8(6) . 3_565 ?
O7A Zn3 O6A 120.3(10) . . ?
C1 O1 Zn1 135.6(8) . . ?
C1 O2 Zn2 123.5(8) . . ?
C2 O3 Zn2 130.1(7) . . ?
C2 O4 Zn1 117.6(8) . . ?
C9 O5 Zn3 128(2) . 5_556 ?
C9 O6 Zn3 125.2(17) . . ?
C12 O8 Zn1 139.5(9) . 2 ?
C12 O9 Zn2 117.2(7) . 2 ?
C16 O10 Zn3 126.0(8) . 6_666 ?
C16 O11 Zn3 124.2(8) . 2_665 ?
C26 O12 Zn2 137.8(9) . 2_655 ?
C26 O14 Zn1 116.3(8) . 2_655 ?
C22 O15 Zn1 134.9(9) . . ?
N2 N1 C5 115.0(10) . . ?
N1 N2 C6 118.5(10) . . ?
N3A N3 C20 93.7(15) . . ?
C22 N4 C23 140(2) . . ?
C22 N4 C24 109.7(17) . . ?
C23 N4 C24 107(2) . . ?
O1 C1 O2 122.6(12) . . ?
O1 C1 C18 117.2(10) . . ?
O2 C1 C18 119.8(10) . . ?
O3 C2 O4 131.8(11) . . ?
O3 C2 C3 115.4(9) . . ?
O4 C2 C3 112.7(11) . . ?
C4 C3 C2 121.9(9) . . ?
C17 C3 C2 120.5(11) . . ?
C17 C3 C4 117.6(11) . . ?
C3 C4 C5 119.0(10) . . ?
C4 C5 N1 112.8(9) . . ?
C14 C5 N1 125.6(12) . . ?
C14 C5 C4 121.2(12) . . ?
N2 C6 C13 120.5(10) . . ?
C7 C6 N2 119.4(11) . . ?
C7 C6 C13 119.9(11) . . ?
C8 C7 C6 123.7(12) . . ?
C7 C8 C9 114.9(15) . . ?
C7 C8 C10 117.1(10) . . ?
C7 C8 C9A 132.5(14) . . ?
C10 C8 C9 128.0(15) . . ?
C10 C8 C9A 110.5(13) . . ?
O5 C9 C8 110(2) . . ?
O6 C9 O5 127(2) . . ?
O6 C9 C8 123(2) . . ?
C11 C10 C8 120.0(12) . . ?
C10 C11 C12 120.9(11) . . ?
C13 C11 C10 121.4(10) . . ?
C13 C11 C12 117.6(9) . . ?
O8 C12 O9 125.1(12) . . ?
O8 C12 C11 119.6(12) . . ?
O9 C12 C11 115.0(9) . . ?
C11 C13 C6 117.4(9) . . ?
C15 C14 C5 118.2(12) . . ?
C14 C15 C16 120.2(12) . . ?
C14 C15 C17 122.8(10) . . ?
C17 C15 C16 116.7(12) . . ?
O10 C16 O11 127.6(10) . . ?
O10 C16 C15 117.6(13) . . ?
O11 C16 C15 113.5(12) . . ?
C15 C17 C3 120.9(12) . . ?
C19 C18 C1 122.8(12) . . ?
C21 C18 C1 118.8(10) . . ?
C21 C18 C19 118.3(13) . . ?
C20 C19 C18 122.5(14) . . ?
C19 C20 N3 143.7(14) 6_557 . ?
C19 C20 N3 97.6(11) . . ?
C19 C20 C19 118.7(16) . 6_557 ?
C18 C21 C18 119.6(15) . 6_557 ?
O15 C22 N4 130.7(17) . . ?
O15 C22 C25 115.7(15) . . ?
N4 C22 C25 111.9(16) . . ?
O12 C26 C27 117.0(11) . . ?
O14 C26 O12 127.9(13) . . ?
O14 C26 C27 114.9(11) . . ?
C28 C27 C26 123.4(10) . . ?
C29 C27 C26 119.9(12) . . ?
C29 C27 C28 116.6(13) . . ?
C27 C28 C27 123.5(14) . 6_557 ?
C27 C29 C30 123.8(15) . . ?
C29 C30 C29 115.7(17) . 6_557 ?
C29 C30 N3A 143.1(14) . . ?
C29 C30 N3A 101.1(12) 6_557 . ?
N3 N3A C30 95.7(16) . . ?
O6A C9A C8 109.1(19) . . ?
O6A C9A O5A 119.5(19) . . ?
O5A C9A C8 129.0(18) . . ?
C9A O6A Zn3 143.6(17) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O1 C1 O2 3(2) . . . . ?
Zn1 O1 C1 C18 -169.7(10) . . . . ?
Zn1 O4 C2 O3 9(2) . . . . ?
Zn1 O4 C2 C3 -172.7(9) . . . . ?
Zn1 O8 C12 O9 -5(2) 2 . . . ?
Zn1 O8 C12 C11 167.5(9) 2 . . . ?
Zn1 O14 C26 O12 -6(2) 2_655 . . . ?
Zn1 O14 C26 C27 168.7(9) 2_655 . . . ?
Zn1 O15 C22 N4 -158.6(15) . . . . ?
Zn1 O15 C22 C25 38(2) . . . . ?
Zn2 O2 C1 O1 2(2) . . . . ?
Zn2 O2 C1 C18 174.9(10) . . . . ?
Zn2 O3 C2 O4 -17(2) . . . . ?
Zn2 O3 C2 C3 164.9(10) . . . . ?
Zn2 O9 C12 O8 2.4(19) 2 . . . ?
Zn2 O9 C12 C11 -170.9(9) 2 . . . ?
Zn2 O12 C26 O14 9(3) 2_655 . . . ?
Zn2 O12 C26 C27 -165.4(12) 2_655 . . . ?
Zn3 O5 C9 O6 19(7) 5_556 . . . ?
Zn3 O5 C9 C8 -161(2) 5_556 . . . ?
Zn3 O6 C9 O5 -10(7) . . . . ?
Zn3 O6 C9 C8 170(2) . . . . ?
Zn3 O10 C16 O11 -17.7(17) 6_666 . . . ?
Zn3 O10 C16 C15 176.0(8) 6_666 . . . ?
Zn3 O11 C16 O10 18.4(17) 2_665 . . . ?
Zn3 O11 C16 C15 -174.8(8) 2_665 . . . ?
O1 C1 C18 C19 164.2(15) . . . . ?
O1 C1 C18 C21 -12(2) . . . . ?
O2 C1 C18 C19 -9(2) . . . . ?
O2 C1 C18 C21 174.7(12) . . . . ?
O3 C2 C3 C4 -167.3(15) . . . . ?
O3 C2 C3 C17 12(2) . . . . ?
O4 C2 C3 C4 14(2) . . . . ?
O4 C2 C3 C17 -165.9(14) . . . . ?
O12 C26 C27 C28 -174.4(12) . . . . ?
O12 C26 C27 C29 3(2) . . . . ?
O14 C26 C27 C28 10(2) . . . . ?
O14 C26 C27 C29 -172.2(16) . . . . ?
N1 N2 C6 C7 178.0(15) . . . . ?
N1 N2 C6 C13 4(3) . . . . ?
N1 C5 C14 C15 178.6(15) . . . . ?
N2 N1 C5 C4 174.3(15) . . . . ?
N2 N1 C5 C14 1(3) . . . . ?
N2 C6 C7 C8 177.5(16) . . . . ?
N2 C6 C13 C11 -178.3(16) . . . . ?
C1 C18 C19 C20 -177.1(12) . . . . ?
C1 C18 C21 C18 176.9(16) . . . 6_557 ?
C2 C3 C4 C5 -179.4(14) . . . . ?
C2 C3 C17 C15 -177.6(14) . . . . ?
C3 C4 C5 N1 -178.6(14) . . . . ?
C3 C4 C5 C14 -5(3) . . . . ?
C4 C3 C17 C15 2(2) . . . . ?
C4 C5 C14 C15 6(3) . . . . ?
C5 N1 N2 C6 177.4(16) . . . . ?
C5 C14 C15 C16 171.4(14) . . . . ?
C5 C14 C15 C17 -3(3) . . . . ?
C6 C7 C8 C9 -175(2) . . . . ?
C6 C7 C8 C10 5(2) . . . . ?
C6 C7 C8 C9A -175.2(19) . . . . ?
C7 C6 C13 C11 7(2) . . . . ?
C7 C8 C9 O5 175(3) . . . . ?
C7 C8 C9 O6 -5(5) . . . . ?
C7 C8 C10 C11 -2(2) . . . . ?
C7 C8 C9A O6A 3(3) . . . . ?
C7 C8 C9A O5A 165(2) . . . . ?
C8 C10 C11 C12 178.7(13) . . . . ?
C8 C10 C11 C13 2(2) . . . . ?
C8 C9A O6A Zn3 178(3) . . . . ?
C8 C9A O5A Zn3 -162.7(19) . . . 5_556 ?
C9 C8 C10 C11 179(3) . . . . ?
C10 C8 C9 O5 -5(5) . . . . ?
C10 C8 C9 O6 175(3) . . . . ?
C10 C8 C9A O6A -177(2) . . . . ?
C10 C8 C9A O5A -15(3) . . . . ?
C10 C11 C12 O8 178.8(13) . . . . ?
C10 C11 C12 O9 -7.5(19) . . . . ?
C10 C11 C13 C6 -4(2) . . . . ?
C12 C11 C13 C6 178.5(13) . . . . ?
C13 C6 C7 C8 -8(3) . . . . ?
C13 C11 C12 O8 -4(2) . . . . ?
C13 C11 C12 O9 169.7(13) . . . . ?
C14 C15 C16 O10 -174.8(13) . . . . ?
C14 C15 C16 O11 17.0(18) . . . . ?
C14 C15 C17 C3 -1(2) . . . . ?
C16 C15 C17 C3 -175.4(13) . . . . ?
C17 C3 C4 C5 1(2) . . . . ?
C17 C15 C16 O10 -0.6(18) . . . . ?
C17 C15 C16 O11 -168.7(12) . . . . ?
C18 C19 C20 N3 180(2) . . . . ?
C18 C19 C20 C19 0.3(12) . . . 6_557 ?
C19 C18 C21 C18 0.3(11) . . . 6_557 ?
C20 N3 N3A C30 179(3) . . . . ?
C21 C18 C19 C20 -1(2) . . . . ?
C23 N4 C22 O15 172(3) . . . . ?
C23 N4 C22 C25 -23(4) . . . . ?
C24 N4 C22 O15 16(3) . . . . ?
C24 N4 C22 C25 -180(2) . . . . ?
C26 C27 C28 C27 178.6(16) . . . 6_557 ?
C26 C27 C29 C30 -179.6(14) . . . . ?
C27 C29 C30 C29 0.9(14) . . . 6_557 ?
C27 C29 C30 N3A 178(3) . . . . ?
C28 C27 C29 C30 -2(3) . . . . ?
C29 C27 C28 C27 0.8(12) . . . 6_557 ?
C29 C30 N3A N3 5(4) . . . . ?
C29 C30 N3A N3 -177(2) 6_557 . . . ?
N3A N3 C20 C19 178.1(19) . . . . ?
N3A N3 C20 C19 -3(4) . . . 6_557 ?
C9A C8 C10 C11 178.4(16) . . . . ?
O6A C9A O5A Zn3 -2(4) . . . 5_556 ?
O5A C9A O6A Zn3 14(5) . . . . ?

_platon_squeeze_details          
;
A solvent mask was calculated and 1724 electrons were 
found in a volume of 5674Å^3 in 3 voids. 
This is consistent with the presence of 
ten N,N-dimethylacetamide and four methanol per formula unit 
which account for 1656 electrons.
;
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 0.000 0.000 0.000 44 23 '0.33 methanol'
2 0.175 0.606 0.011 5630 1701 '1.66 N,N-dimethylacetamide and 0.5 methanol'

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.51(3)
2 0.49(3)

# start Validation Reply Form
_vrf_PLAT341_3                   
;
PROBLEM: Low Bond Precision on C-C Bonds  0.01974 Ang.
RESPONSE: The quality of crystal was not so good and the data were collected under 
low temperature. Therefore thermal vibration of the C atoms was so high that the 
precision of the C-C bonds is low.
;
_vrf_PLAT420_3                   
;
PROBLEM: D-H Without Acceptor       O7A      --H7AB       Please Check 
         D-H Without Acceptor       O7A      --H7AB       Please Check 
         D-H Without Acceptor       O7       --H7A        Please Check
         D-H Without Acceptor       O7       --H7B        Please Check 
         D-H Without Acceptor       O13      --H13A       Please Check 
         D-H Without Acceptor       O13      --H13B       Please Check 
         D-H Without Acceptor       O15      --H15B       Please Check 
RESPONSE: The coordination compound contained so many hydroxyls. The acceptor of 
the hydrogen on the O-H couldn??t be located because there was no proper atom 
such as O or N for the hydroxyl to form hydrogen bond in the radius of 0.36 nm.
;
# end Validation Reply Form
####################################################################### 
# 
# 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 1892888'
loop_
_audit_author_name
_audit_author_address
'Min Di'
;Northeast Normal University
China
;
_audit_update_record             
;
2019-01-23 deposited with the CCDC.	2019-02-19 downloaded from the CCDC.
;
_audit_creation_date             2018-12-21
_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         'C25 H27 Co2 N5 O11.34'
_chemical_formula_sum            'C25 H27 Co2 N5 O11.34'
_chemical_formula_weight         696.88
_chemical_absolute_configuration .
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 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      tetragonal
_space_group_IT_number           96
_space_group_name_H-M_alt        'P 43 21 2'
_space_group_name_Hall           'P 4nw 2abw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'-y, -x, -z+1/2'
'y, x, -z'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'

_cell_length_a                   13.880
_cell_length_b                   13.880
_cell_length_c                   45.438
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8753.8
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2448
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      29.1368
_cell_measurement_theta_min      3.0629
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96159
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.058
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cone-shaped
_exptl_crystal_F_000             2854
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0948
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            18407
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         3.069
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.2375
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -78.00   10.50   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.6627  -38.0000 -120.0000 118
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0263610000
_diffrn_orient_matrix_UB_12      0.0156057000
_diffrn_orient_matrix_UB_13      -0.0124914000
_diffrn_orient_matrix_UB_21      0.0176907000
_diffrn_orient_matrix_UB_22      0.0398892000
_diffrn_orient_matrix_UB_23      0.0081332000
_diffrn_orient_matrix_UB_31      0.0400394000
_diffrn_orient_matrix_UB_32      -0.0278970000
_diffrn_orient_matrix_UB_33      0.0046218000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.729
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5842
_reflns_number_total             8258
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_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    'SHELXT 2018/3 (Sheldrick, 2015)'
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8258
_refine_ls_number_restraints     196
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0684
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0913P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1569
_refine_ls_wR_factor_ref         0.1765
_refine_special_details          ?
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.53(4)
 0.47(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C20-C21
 2.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Co1, O9, O10, O11, N3, N4, N5, C17, C18, C19, C20, C21, C22, C23, C24, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, N1, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, N2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 C22(H22A,H22B,H22C)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C11(H11), C13(H13), C16(H16), C17(H17), C20(H20),
 C23(H23)
6.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.37860(8) 0.92093(8) 0.57418(2) 0.0399(3) Uani 1 1 d . U . . .
Co2 Co 0.51197(6) 1.01062(6) 0.63096(2) 0.0258(2) Uani 1 1 d . . . . .
O1 O 0.4331(4) 1.0503(4) 0.59248(11) 0.0414(14) Uani 1 1 d . . . . .
O2 O 0.4222(4) 0.9242(4) 0.65331(10) 0.0451(15) Uani 1 1 d . . . . .
O3 O 0.3384(5) 0.8687(5) 0.61473(12) 0.070(2) Uani 1 1 d . . . . .
O4 O 0.0135(5) 0.6355(5) 0.67451(15) 0.0603(17) Uani 1 1 d . . . . .
O5 O 0.0998(4) 0.5932(4) 0.63455(11) 0.0490(15) Uani 1 1 d . . . . .
O6 O 0.4012(5) 1.1376(5) 0.63151(12) 0.0596(18) Uani 1 1 d . . . . .
O7 O 0.0866(4) 1.4332(4) 0.58406(12) 0.0492(15) Uani 1 1 d . . . . .
O8 O 0.1293(4) 1.3711(4) 0.62681(12) 0.0550(16) Uani 1 1 d . . . . .
O9 O 0.2397(5) 0.9774(6) 0.56874(16) 0.072(2) Uani 1 1 d . U . . .
O10 O 0.4102(5) 0.9609(5) 0.53127(12) 0.0627(19) Uani 1 1 d . U . . .
O11 O 0.3219(6) 0.7894(6) 0.55868(14) 0.077(2) Uani 1 1 d . U . . .
N1 N 0.2710(7) 0.7776(7) 0.74137(15) 0.072(3) Uani 1 1 d . U . . .
N2 N 0.2841(7) 1.2357(6) 0.50782(16) 0.067(3) Uani 1 1 d . U . . .
N3 N 0.0809(10) 0.9416(12) 0.5603(4) 0.143(5) Uani 1 1 d . U . . .
N4 N 0.3958(10) 0.9382(8) 0.48251(18) 0.104(3) Uani 1 1 d . U . . .
N5 N 0.2914(10) 0.6322(9) 0.5739(3) 0.114(4) Uani 1 1 d . U . . .
C1 C 0.3583(6) 0.8725(6) 0.64133(15) 0.040(2) Uani 1 1 d . . . . .
C2 C 0.2989(6) 0.8085(6) 0.66134(15) 0.036(2) Uani 1 1 d . . . . .
C3 C 0.3132(7) 0.8130(7) 0.69144(16) 0.053(3) Uani 1 1 d . . . . .
H3 H 0.363153 0.850161 0.699034 0.064 Uiso 1 1 calc R . . . .
C4 C 0.2536(7) 0.7626(7) 0.71022(16) 0.053(3) Uani 1 1 d . U . . .
C5 C 0.1788(7) 0.7082(7) 0.69939(17) 0.056(3) Uani 1 1 d . . . . .
H5 H 0.135725 0.678271 0.712119 0.067 Uiso 1 1 calc R . . . .
C6 C 0.1687(6) 0.6988(6) 0.66918(16) 0.041(2) Uani 1 1 d . . . . .
C7 C 0.0874(7) 0.6358(6) 0.65853(18) 0.042(2) Uani 1 1 d . . . . .
C8 C 0.2291(6) 0.7486(6) 0.65032(16) 0.041(2) Uani 1 1 d . . . . .
H8 H 0.222284 0.741425 0.630074 0.049 Uiso 1 1 calc R . . . .
C9 C 0.3900(6) 1.1220(6) 0.60504(17) 0.042(2) Uani 1 1 d . . . . .
C10 C 0.3280(6) 1.1848(6) 0.58617(18) 0.043(2) Uani 1 1 d . . . . .
C11 C 0.3323(6) 1.1834(6) 0.55611(17) 0.042(2) Uani 1 1 d . . . . .
H11 H 0.374534 1.141414 0.546734 0.050 Uiso 1 1 calc R . . . .
C12 C 0.2736(7) 1.2446(6) 0.53921(18) 0.049(2) Uani 1 1 d . . . . .
C13 C 0.2130(7) 1.3092(6) 0.55327(17) 0.045(2) Uani 1 1 d . . . . .
H13 H 0.176604 1.352426 0.542282 0.054 Uiso 1 1 calc R . . . .
C14 C 0.2067(6) 1.3094(6) 0.58373(16) 0.039(2) Uani 1 1 d . . . . .
C15 C 0.1365(6) 1.3756(6) 0.59958(17) 0.0385(18) Uani 1 1 d . . . . .
C16 C 0.2652(6) 1.2501(6) 0.60077(18) 0.042(2) Uani 1 1 d . . . . .
H16 H 0.263297 1.253149 0.621213 0.050 Uiso 1 1 calc R . . . .
C17 C 0.1680(12) 0.9180(13) 0.5714(4) 0.118(5) Uani 1 1 d . U . . .
H17 H 0.176633 0.859250 0.580901 0.142 Uiso 1 1 calc R . . . .
C18 C 0.0663(18) 1.0373(19) 0.5435(5) 0.210(10) Uani 1 1 d . U . . .
H18A H 0.089894 1.089877 0.555165 0.315 Uiso 1 1 calc GR . . . .
H18B H -0.000988 1.046533 0.539534 0.315 Uiso 1 1 calc GR . . . .
H18C H 0.101110 1.034976 0.525209 0.315 Uiso 1 1 calc GR . . . .
C19 C 0.0008(15) 0.8654(18) 0.5686(5) 0.213(10) Uani 1 1 d . U . . .
H19A H -0.040695 0.855277 0.551996 0.320 Uiso 1 1 calc GR . . . .
H19B H -0.036404 0.889055 0.584892 0.320 Uiso 1 1 calc GR . . . .
H19C H 0.030857 0.805662 0.573971 0.320 Uiso 1 1 calc GR . . . .
C20 C 0.3658(11) 0.9348(10) 0.5106(2) 0.095(4) Uani 1 1 d D U . . .
H20 H 0.304695 0.909685 0.514125 0.113 Uiso 1 1 calc R . . . .
C21 C 0.4888(12) 0.9787(14) 0.4772(4) 0.156(7) Uani 1 1 d D U . . .
H21A H 0.482017 1.037587 0.466274 0.234 Uiso 1 1 calc GR . . . .
H21B H 0.527027 0.934000 0.466063 0.234 Uiso 1 1 calc GR . . . .
H21C H 0.519969 0.991863 0.495615 0.234 Uiso 1 1 calc GR . . . .
C22 C 0.3298(18) 0.9130(17) 0.4578(4) 0.203(10) Uani 1 1 d . U . . .
H22A H 0.350228 0.854544 0.448368 0.305 Uiso 1 1 d R . . . .
H22B H 0.330868 0.964764 0.443768 0.305 Uiso 1 1 d R . . . .
H22C H 0.265528 0.905094 0.465188 0.305 Uiso 1 1 d R . . . .
C23 C 0.3469(10) 0.7115(10) 0.5721(3) 0.089(4) Uani 1 1 d . U . . .
H23 H 0.407076 0.710015 0.581086 0.107 Uiso 1 1 calc R . . . .
C24 C 0.3179(16) 0.5560(15) 0.5946(4) 0.168(8) Uani 1 1 d . U . . .
H24A H 0.323000 0.495818 0.584322 0.251 Uiso 1 1 calc GR . . . .
H24B H 0.269354 0.550928 0.609589 0.251 Uiso 1 1 calc GR . . . .
H24C H 0.378662 0.571323 0.603538 0.251 Uiso 1 1 calc GR . . . .
C25 C 0.2021(17) 0.6347(16) 0.5581(5) 0.211(11) Uani 1 1 d . U . . .
H25A H 0.213410 0.656321 0.538356 0.317 Uiso 1 1 calc GR . . . .
H25B H 0.158502 0.678186 0.567757 0.317 Uiso 1 1 calc GR . . . .
H25C H 0.174437 0.571321 0.557706 0.317 Uiso 1 1 calc GR . . . .
O12 O 0.362(4) 0.808(4) 0.7464(8) 0.072(15) Uani 0.150(18) 1 d . U . . .
O13 O 0.372(3) 1.206(3) 0.5006(6) 0.068(13) Uani 0.193(19) 1 d . 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
Co1 O1 2.118(6) . ?
Co1 O3 2.057(5) . ?
Co1 O4 2.030(6) 3_566 ?
Co1 O9 2.095(7) . ?
Co1 O10 2.074(6) . ?
Co1 O11 2.109(7) . ?
Co2 O1 2.135(5) . ?
Co2 O2 2.005(5) . ?
Co2 O5 2.015(5) 3_566 ?
Co2 O6 2.339(6) . ?
Co2 O7 2.052(5) 3_576 ?
Co2 O8 2.339(6) 3_576 ?
O1 C9 1.294(9) . ?
O2 C1 1.264(9) . ?
O3 C1 1.241(9) . ?
O4 C7 1.257(10) . ?
O5 C7 1.251(9) . ?
O6 C9 1.232(9) . ?
O7 C15 1.271(9) . ?
O8 C15 1.243(9) . ?
O9 C17 1.298(16) . ?
O10 C20 1.179(12) . ?
O11 C23 1.288(14) . ?
N1 N1 1.235(14) 5_666 ?
N1 C4 1.451(10) . ?
N1 O12 1.35(5) . ?
N2 N2 1.187(14) 6_466 ?
N2 C12 1.439(10) . ?
N2 O13 1.32(3) . ?
N3 C17 1.35(2) . ?
N3 C18 1.55(2) . ?
N3 C19 1.58(2) . ?
N4 C20 1.345(13) . ?
N4 C21 1.430(18) . ?
N4 C22 1.49(2) . ?
N5 C23 1.347(16) . ?
N5 C24 1.46(2) . ?
N5 C25 1.43(2) . ?
C1 C2 1.516(10) . ?
C2 C3 1.384(10) . ?
C2 C8 1.371(10) . ?
C3 H3 0.9300 . ?
C3 C4 1.380(11) . ?
C4 C5 1.374(11) . ?
C5 H5 0.9300 . ?
C5 C6 1.386(10) . ?
C6 C7 1.507(11) . ?
C6 C8 1.384(11) . ?
C8 H8 0.9300 . ?
C9 C10 1.495(11) . ?
C10 C11 1.367(11) . ?
C10 C16 1.422(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.405(11) . ?
C12 C13 1.385(11) . ?
C13 H13 0.9300 . ?
C13 C14 1.387(10) . ?
C14 C15 1.521(10) . ?
C14 C16 1.391(11) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9601 . ?
C22 H22B 0.9590 . ?
C22 H22C 0.9602 . ?
C23 H23 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?

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
O3 Co1 O1 92.5(2) . . ?
O3 Co1 O9 89.3(3) . . ?
O3 Co1 O10 173.5(3) . . ?
O3 Co1 O11 83.9(3) . . ?
O4 Co1 O1 89.2(2) 3_566 . ?
O4 Co1 O3 95.0(3) 3_566 . ?
O4 Co1 O9 174.9(3) 3_566 . ?
O4 Co1 O10 86.3(3) 3_566 . ?
O4 Co1 O11 91.2(3) 3_566 . ?
O9 Co1 O1 93.3(3) . . ?
O9 Co1 O11 86.6(3) . . ?
O10 Co1 O1 93.8(2) . . ?
O10 Co1 O9 89.1(3) . . ?
O10 Co1 O11 89.8(3) . . ?
O11 Co1 O1 176.4(2) . . ?
O1 Co2 O6 58.50(19) . . ?
O1 Co2 O8 93.0(2) . 3_576 ?
O2 Co2 O1 104.5(2) . . ?
O2 Co2 O5 97.2(3) . 3_566 ?
O2 Co2 O6 92.1(3) . . ?
O2 Co2 O7 98.5(2) . 3_576 ?
O2 Co2 O8 158.21(19) . 3_576 ?
O5 Co2 O1 102.0(2) 3_566 . ?
O5 Co2 O6 160.1(2) 3_566 . ?
O5 Co2 O7 103.7(2) 3_566 3_576 ?
O5 Co2 O8 91.6(2) 3_566 3_576 ?
O6 Co2 O8 86.0(2) . 3_576 ?
O7 Co2 O1 142.7(2) 3_576 . ?
O7 Co2 O6 92.1(2) 3_576 . ?
O7 Co2 O8 59.9(2) 3_576 3_576 ?
Co1 O1 Co2 106.6(2) . . ?
C9 O1 Co1 131.3(5) . . ?
C9 O1 Co2 94.3(5) . . ?
C1 O2 Co2 123.9(4) . . ?
C1 O3 Co1 142.8(5) . . ?
C7 O4 Co1 140.5(6) . 3_466 ?
C7 O5 Co2 124.0(5) . 3_466 ?
C9 O6 Co2 86.6(5) . . ?
C15 O7 Co2 94.8(4) . 3_476 ?
C15 O8 Co2 82.6(5) . 3_476 ?
C17 O9 Co1 117.2(9) . . ?
C20 O10 Co1 123.7(7) . . ?
C23 O11 Co1 117.9(8) . . ?
N1 N1 C4 116.7(9) 5_666 . ?
N1 N1 O12 124.9(19) 5_666 . ?
O12 N1 C4 111.5(17) . . ?
N2 N2 C12 119.2(9) 6_466 . ?
N2 N2 O13 123.1(16) 6_466 . ?
O13 N2 C12 111.5(14) . . ?
C17 N3 C18 120.7(17) . . ?
C17 N3 C19 112.2(17) . . ?
C18 N3 C19 126.9(17) . . ?
C20 N4 C21 117.0(12) . . ?
C20 N4 C22 121.2(15) . . ?
C21 N4 C22 121.2(14) . . ?
C23 N5 C24 119.0(14) . . ?
C23 N5 C25 116.5(15) . . ?
C25 N5 C24 123.9(16) . . ?
O2 C1 C2 117.2(6) . . ?
O3 C1 O2 126.9(7) . . ?
O3 C1 C2 115.9(7) . . ?
C3 C2 C1 119.2(7) . . ?
C8 C2 C1 121.4(6) . . ?
C8 C2 C3 119.4(7) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.1(7) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 N1 115.5(7) . . ?
C5 C4 N1 123.7(7) . . ?
C5 C4 C3 120.7(7) . . ?
C4 C5 H5 120.6 . . ?
C4 C5 C6 118.9(7) . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C7 116.7(7) . . ?
C8 C6 C5 120.3(7) . . ?
C8 C6 C7 123.0(7) . . ?
O4 C7 C6 115.3(7) . . ?
O5 C7 O4 127.8(8) . . ?
O5 C7 C6 116.8(8) . . ?
C2 C8 C6 120.3(7) . . ?
C2 C8 H8 119.8 . . ?
C6 C8 H8 119.8 . . ?
O1 C9 C10 117.5(7) . . ?
O6 C9 O1 120.5(7) . . ?
O6 C9 C10 122.0(7) . . ?
C11 C10 C9 122.6(7) . . ?
C11 C10 C16 120.1(7) . . ?
C16 C10 C9 117.2(7) . . ?
C10 C11 H11 119.6 . . ?
C10 C11 C12 120.8(7) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 N2 115.5(7) . . ?
C13 C12 N2 125.0(7) . . ?
C13 C12 C11 119.4(8) . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0(7) . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C15 120.9(7) . . ?
C13 C14 C16 121.2(7) . . ?
C16 C14 C15 117.9(7) . . ?
O7 C15 C14 117.8(7) . . ?
O8 C15 O7 122.7(7) . . ?
O8 C15 C14 119.5(7) . . ?
C10 C16 H16 120.8 . . ?
C14 C16 C10 118.4(7) . . ?
C14 C16 H16 120.8 . . ?
O9 C17 N3 119.8(16) . . ?
O9 C17 H17 120.1 . . ?
N3 C17 H17 120.1 . . ?
N3 C18 H18A 109.5 . . ?
N3 C18 H18B 109.5 . . ?
N3 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 H19A 109.5 . . ?
N3 C19 H19B 109.5 . . ?
N3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O10 C20 N4 125.6(12) . . ?
O10 C20 H20 117.2 . . ?
N4 C20 H20 117.2 . . ?
N4 C21 H21A 109.5 . . ?
N4 C21 H21B 109.5 . . ?
N4 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C22 H22A 110.6 . . ?
N4 C22 H22B 108.4 . . ?
N4 C22 H22C 109.4 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O11 C23 N5 124.0(13) . . ?
O11 C23 H23 118.0 . . ?
N5 C23 H23 118.0 . . ?
N5 C24 H24A 109.5 . . ?
N5 C24 H24B 109.5 . . ?
N5 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C25 H25A 109.5 . . ?
N5 C25 H25B 109.5 . . ?
N5 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O1 C9 O6 112.0(8) . . . . ?
Co1 O1 C9 C10 -68.7(9) . . . . ?
Co1 O3 C1 O2 3(2) . . . . ?
Co1 O3 C1 C2 -177.4(8) . . . . ?
Co1 O4 C7 O5 0.1(16) 3_466 . . . ?
Co1 O4 C7 C6 177.2(6) 3_466 . . . ?
Co1 O9 C17 N3 -161.4(13) . . . . ?
Co1 O10 C20 N4 -162.5(10) . . . . ?
Co1 O11 C23 N5 150.8(12) . . . . ?
Co2 O1 C9 O6 -4.6(9) . . . . ?
Co2 O1 C9 C10 174.7(7) . . . . ?
Co2 O2 C1 O3 -2.6(14) . . . . ?
Co2 O2 C1 C2 177.8(6) . . . . ?
Co2 O5 C7 O4 -13.2(13) 3_466 . . . ?
Co2 O5 C7 C6 169.7(5) 3_466 . . . ?
Co2 O6 C9 O1 4.2(8) . . . . ?
Co2 O6 C9 C10 -175.1(8) . . . . ?
Co2 O7 C15 O8 -1.3(9) 3_476 . . . ?
Co2 O7 C15 C14 178.1(7) 3_476 . . . ?
Co2 O8 C15 O7 1.2(8) 3_476 . . . ?
Co2 O8 C15 C14 -178.3(8) 3_476 . . . ?
O1 C9 C10 C11 -15.3(13) . . . . ?
O1 C9 C10 C16 167.0(8) . . . . ?
O2 C1 C2 C3 3.4(13) . . . . ?
O2 C1 C2 C8 -178.8(9) . . . . ?
O3 C1 C2 C3 -176.3(10) . . . . ?
O3 C1 C2 C8 1.5(14) . . . . ?
O6 C9 C10 C11 164.0(9) . . . . ?
O6 C9 C10 C16 -13.8(13) . . . . ?
N1 N1 C4 C3 -175.9(7) 5_666 . . . ?
N1 N1 C4 C5 9.0(13) 5_666 . . . ?
N1 C4 C5 C6 179.8(10) . . . . ?
N2 N2 C12 C11 178.8(6) 6_466 . . . ?
N2 N2 C12 C13 -2.7(13) 6_466 . . . ?
N2 C12 C13 C14 178.1(10) . . . . ?
C1 C2 C3 C4 173.6(9) . . . . ?
C1 C2 C8 C6 -172.9(9) . . . . ?
C2 C3 C4 N1 -176.0(10) . . . . ?
C2 C3 C4 C5 -0.7(17) . . . . ?
C3 C2 C8 C6 4.9(14) . . . . ?
C3 C4 C5 C6 5.0(17) . . . . ?
C4 C5 C6 C7 178.1(10) . . . . ?
C4 C5 C6 C8 -4.3(16) . . . . ?
C5 C6 C7 O4 32.6(12) . . . . ?
C5 C6 C7 O5 -150.0(9) . . . . ?
C5 C6 C8 C2 -0.6(15) . . . . ?
C7 C6 C8 C2 176.8(8) . . . . ?
C8 C2 C3 C4 -4.2(15) . . . . ?
C8 C6 C7 O4 -145.0(9) . . . . ?
C8 C6 C7 O5 32.5(13) . . . . ?
C9 C10 C11 C12 -179.1(9) . . . . ?
C9 C10 C16 C14 180.0(8) . . . . ?
C10 C11 C12 N2 -179.4(9) . . . . ?
C10 C11 C12 C13 2.0(15) . . . . ?
C11 C10 C16 C14 2.2(14) . . . . ?
C11 C12 C13 C14 -3.5(15) . . . . ?
C12 C13 C14 C15 -176.5(9) . . . . ?
C12 C13 C14 C16 4.5(15) . . . . ?
C13 C14 C15 O7 -2.6(13) . . . . ?
C13 C14 C15 O8 176.8(9) . . . . ?
C13 C14 C16 C10 -3.7(14) . . . . ?
C15 C14 C16 C10 177.2(8) . . . . ?
C16 C10 C11 C12 -1.4(14) . . . . ?
C16 C14 C15 O7 176.5(8) . . . . ?
C16 C14 C15 O8 -4.1(13) . . . . ?
C18 N3 C17 O9 2(3) . . . . ?
C19 N3 C17 O9 -174.0(15) . . . . ?
C21 N4 C20 O10 -1(2) . . . . ?
C22 N4 C20 O10 -173.4(17) . . . . ?
C24 N5 C23 O11 -167.3(15) . . . . ?
C25 N5 C23 O11 4(2) . . . . ?
O12 N1 C4 C3 -23(3) . . . . ?
O12 N1 C4 C5 161(3) . . . . ?
O13 N2 C12 C11 -28(2) . . . . ?
O13 N2 C12 C13 150(2) . . . . ?

_platon_squeeze_details          
;
A solvent mask was calculated and 948 electrons were 
found in a volume of 3575Å^3 in 1 voids. 
This is consistent with the presence of 
three N,N-dimethyformamide per formula unit 
which account for 960 electrons.
;
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 0.020 0.092 -0.016 3575 948 '3 N,N-dimethyformamide'

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.53(4)
2 0.47(4)

# start Validation Reply Form 
_vrf_PLAT910_1                   
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         15 Note 
RESPONSE: Some reflections with high intensities, which made the 
detector overflow were automatically omitted by the diffractometer. 
So some reflections were missing.
;
# end Validation Reply Form
