# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_4Mg
_database_code_depnum_ccdc_archive 'CCDC 1475105'
_audit_update_record             
;
2016-08-15 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C74 H66 Mg3 N12 O28'
_chemical_formula_weight         1644.31

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'
Mg Mg 0.0490 0.0360 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.393(2)
_cell_length_b                   14.018(3)
_cell_length_c                   14.240(3)
_cell_angle_alpha                117.59(3)
_cell_angle_beta                 93.18(3)
_cell_angle_gamma                98.27(3)
_cell_volume                     1801.9(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      55.838
_cell_measurement_theta_min      3.258

_exptl_crystal_description       block
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_F_000             854
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.986
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.141
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7108
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30454
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.630
_diffrn_reflns_theta_max         27.922
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measured_fraction_theta_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_point_group_measured_fraction_full 0.929
_reflns_number_total             7830
_reflns_number_gt                6503
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0800P)²+1.5465P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7830
_refine_ls_number_parameters     547
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1422
_refine_ls_wR_factor_gt          0.1332
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
Mg1 Mg 0.5000 0.5000 0.0000 0.01341(19) Uani 1 2 d S . P . .
Mg2 Mg 0.46904(7) 0.54453(5) 0.26553(5) 0.01364(15) Uani 1 1 d . . . . .
O3 O 0.44676(15) 0.29065(11) 0.62403(10) 0.0171(3) Uani 1 1 d . . . . .
O8 O 0.64189(15) 0.49395(12) 0.22424(10) 0.0173(3) Uani 1 1 d . . . . .
O10 O 0.78535(15) 0.36916(12) 0.81514(10) 0.0173(3) Uani 1 1 d . . . . .
O9 O 0.71591(14) 0.42139(12) 0.69684(10) 0.0164(3) Uani 1 1 d . . . . .
O2 O 0.37966(15) 0.37992(11) 0.16563(10) 0.0165(3) Uani 1 1 d . . . . .
O7 O 0.67585(15) 0.50407(13) 0.07445(11) 0.0203(3) Uani 1 1 d . . . . .
O1 O 0.42537(16) 0.35989(12) 0.00612(11) 0.0213(3) Uani 1 1 d . . . . .
O4 O 0.42082(17) 0.21248(12) 0.72982(11) 0.0247(4) Uani 1 1 d . . . . .
O13 O 0.48353(16) 0.51379(13) 0.39382(11) 0.0199(3) Uani 1 1 d D . . . .
O16 O 0.32561(18) 0.61398(13) 0.56387(13) 0.0290(4) Uani 1 1 d . . . . .
N10 N 0.39620(18) 0.70761(13) 0.62532(12) 0.0147(3) Uani 1 1 d . . . . .
N1 N 0.30534(18) -0.01334(14) 0.10770(12) 0.0177(4) Uani 1 1 d . . . . .
O18 O 0.51718(18) 0.71491(15) 0.64104(13) 0.0314(4) Uani 1 1 d . . . . .
N6 N 1.06955(17) 0.34892(14) 0.44950(12) 0.0157(3) Uani 1 1 d . . . . .
N2 N 0.30549(18) -0.04032(14) 0.24595(12) 0.0174(4) Uani 1 1 d . . . . .
N5 N 1.04109(17) 0.35622(14) 0.30142(12) 0.0150(3) Uani 1 1 d . . . . .
O17 O 0.3413(2) 0.78720(17) 0.66512(18) 0.0540(6) Uani 1 1 d . . . . .
C28 C 0.9781(2) 0.34277(17) 0.37534(15) 0.0167(4) Uani 1 1 d . . . . .
H28 H 0.8858 0.3310 0.3753 0.020 Uiso 1 1 calc R U . . .
N8 N 0.9680(2) -0.01168(17) 0.21218(17) 0.0322(5) Uani 1 1 d . . . . .
C27 C 0.8938(2) 0.40937(16) 0.05282(14) 0.0165(4) Uani 1 1 d . . . . .
H27 H 0.8642 0.4257 -0.0015 0.020 Uiso 1 1 calc R U . . .
C1 C 0.3957(2) 0.32396(16) 0.06912(14) 0.0149(4) Uani 1 1 d . . . . .
C23 C 0.8666(2) 0.40446(16) 0.21838(14) 0.0154(4) Uani 1 1 d . . . . .
H23 H 0.8184 0.4159 0.2763 0.019 Uiso 1 1 calc R U . . .
C25 C 1.0535(2) 0.34465(17) 0.12699(15) 0.0180(4) Uani 1 1 d . . . . .
H25 H 1.1311 0.3152 0.1231 0.022 Uiso 1 1 calc R U . . .
C32 C 0.9325(2) 0.36387(16) 0.58838(14) 0.0151(4) Uani 1 1 d . . . . .
H32 H 0.8683 0.3867 0.5573 0.018 Uiso 1 1 calc R U . . .
C30 C 1.1744(2) 0.36963(16) 0.32813(15) 0.0170(4) Uani 1 1 d . . . . .
H30 H 1.2410 0.3802 0.2889 0.020 Uiso 1 1 calc R U . . .
C37 C 0.7961(2) 0.38558(15) 0.73564(14) 0.0144(4) Uani 1 1 d . . . . .
C33 C 0.9156(2) 0.35599(15) 0.68125(14) 0.0148(4) Uani 1 1 d . . . . .
C21 C 0.7030(2) 0.47877(16) 0.14592(14) 0.0160(4) Uani 1 1 d . . . . .
C17 C 0.4167(2) 0.20952(16) 0.64010(15) 0.0167(4) Uani 1 1 d . . . . .
C4 C 0.3305(2) 0.03847(16) 0.04211(15) 0.0177(4) Uani 1 1 d . . . . .
C24 C 0.9823(2) 0.36536(16) 0.21243(14) 0.0150(4) Uani 1 1 d . . . . .
C29 C 1.1927(2) 0.36495(17) 0.42045(15) 0.0174(4) Uani 1 1 d . . . . .
H29 H 1.2745 0.3714 0.4583 0.021 Uiso 1 1 calc R U . . .
C34 C 1.0106(2) 0.32197(16) 0.72555(15) 0.0168(4) Uani 1 1 d . . . . .
H34 H 0.9989 0.3174 0.7891 0.020 Uiso 1 1 calc R U . . .
C36 C 1.1398(2) 0.30207(17) 0.58534(15) 0.0178(4) Uani 1 1 d . . . . .
H36 H 1.2155 0.2831 0.5518 0.021 Uiso 1 1 calc R U . . .
C22 C 0.8217(2) 0.42689(16) 0.13758(14) 0.0151(4) Uani 1 1 d . . . . .
C8 C 0.3404(2) 0.03447(16) 0.21379(15) 0.0178(4) Uani 1 1 d . . . . .
H8 H 0.3827 0.1086 0.2585 0.021 Uiso 1 1 calc R U . . .
C31 C 1.0459(2) 0.33738(16) 0.54262(14) 0.0154(4) Uani 1 1 d . . . . .
C13 C 0.3705(2) 0.09759(16) 0.54416(15) 0.0164(4) Uani 1 1 d . . . . .
C3 C 0.3460(2) 0.15164(16) 0.08708(15) 0.0169(4) Uani 1 1 d . . . . .
H3 H 0.3363 0.1949 0.1600 0.020 Uiso 1 1 calc R U . . .
C10 C 0.2475(2) -0.12140(17) 0.07159(16) 0.0226(5) Uani 1 1 d . . . . .
H10 H 0.2134 -0.1739 -0.0004 0.027 Uiso 1 1 calc R U . . .
C26 C 1.0084(2) 0.36816(17) 0.04783(15) 0.0176(4) Uani 1 1 d . . . . .
H26 H 1.0564 0.3559 -0.0103 0.021 Uiso 1 1 calc R U . . .
C35 C 1.1218(2) 0.29475(17) 0.67784(15) 0.0193(4) Uani 1 1 d . . . . .
H35 H 1.1857 0.2711 0.7083 0.023 Uiso 1 1 calc R U . . .
C7 C 0.3892(2) 0.13601(17) -0.08413(15) 0.0195(4) Uani 1 1 d . . . . .
H7 H 0.4112 0.1697 -0.1271 0.023 Uiso 1 1 calc R U . . .
C9 C 0.2481(2) -0.13913(17) 0.15743(15) 0.0218(4) Uani 1 1 d . . . . .
H9 H 0.2155 -0.2062 0.1571 0.026 Uiso 1 1 calc R U . . .
C12 C 0.3591(2) 0.08426(16) 0.44043(15) 0.0172(4) Uani 1 1 d . . . . .
H12 H 0.3772 0.1458 0.4284 0.021 Uiso 1 1 calc R U . . .
O20 O 1.0261(3) 0.1041(2) 0.1442(2) 0.0646(7) Uani 1 1 d . . . . .
C11 C 0.3204(2) -0.02136(16) 0.35515(14) 0.0168(4) Uani 1 1 d . . . . .
C14 C 0.3420(2) 0.00683(17) 0.56088(15) 0.0207(4) Uani 1 1 d . . . . .
H14 H 0.3477 0.0167 0.6318 0.025 Uiso 1 1 calc R U . . .
C5 C 0.3419(2) -0.02730(17) -0.06497(15) 0.0204(4) Uani 1 1 d . . . . .
H5 H 0.3307 -0.1047 -0.0943 0.025 Uiso 1 1 calc R U . . .
C6 C 0.3701(2) 0.02271(17) -0.12808(15) 0.0213(4) Uani 1 1 d . . . . .
H6 H 0.3763 -0.0210 -0.2017 0.026 Uiso 1 1 calc R U . . .
C2 C 0.3760(2) 0.20057(16) 0.02331(14) 0.0160(4) Uani 1 1 d . . . . .
C15 C 0.3053(3) -0.09772(18) 0.47481(16) 0.0260(5) Uani 1 1 d . . . . .
H15 H 0.2870 -0.1594 0.4866 0.031 Uiso 1 1 calc R U . . .
C16 C 0.2953(2) -0.11213(17) 0.37134(16) 0.0231(5) Uani 1 1 d . . . . .
H16 H 0.2714 -0.1837 0.3120 0.028 Uiso 1 1 calc R U . . .
C41 C 0.9119(3) -0.1202(2) 0.1929(2) 0.0384(6) Uani 1 1 d . . . . .
H41C H 0.8319 -0.1180 0.2266 0.058 Uiso 1 1 calc R U . . .
H41A H 0.9753 -0.1474 0.2234 0.058 Uiso 1 1 calc R U . . .
H41B H 0.8904 -0.1693 0.1157 0.058 Uiso 1 1 calc R U . . .
C42 C 0.9819(3) 0.0129(2) 0.1325(2) 0.0394(6) Uani 1 1 d . . . . .
H42 H 0.9556 -0.0449 0.0614 0.047 Uiso 1 1 calc R U . . .
C40 C 1.0028(4) 0.0731(3) 0.3228(3) 0.0555(9) Uani 1 1 d . . . . .
H40B H 1.0695 0.1326 0.3272 0.083 Uiso 1 1 calc R U . . .
H40A H 1.0379 0.0421 0.3657 0.083 Uiso 1 1 calc R U . . .
H40C H 0.9246 0.1020 0.3503 0.083 Uiso 1 1 calc R U . . .
O12 O 0.44712(15) 0.59403(12) 0.14725(10) 0.0146(3) Uani 1 1 d D . . . .
H12A H 0.503(4) 0.670(3) 0.184(3) 0.065(11) Uiso 1 1 d D . . . .
H12B H 0.361(4) 0.607(3) 0.147(3) 0.069(12) Uiso 1 1 d D . . . .
H13B H 0.494(5) 0.446(2) 0.388(4) 0.099(16) Uiso 1 1 d D . . . .
H13A H 0.432(3) 0.541(3) 0.444(2) 0.045(9) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mg1 O7 2.0411(16) . ?
Mg1 O7 2.0411(16) 2_665 ?
Mg1 O1 2.0480(15) 2_665 ?
Mg1 O1 2.0481(15) . ?
Mg1 O12 2.0524(15) 2_665 ?
Mg1 O12 2.0524(15) . ?
Mg1 Mg2 3.5772(10) . ?
Mg1 Mg2 3.5773(10) 2_665 ?
Mg2 O8 2.0427(17) . ?
Mg2 O13 2.0647(15) . ?
Mg2 O9 2.0861(16) 2_666 ?
Mg2 O2 2.0993(19) . ?
Mg2 O12 2.1108(15) . ?
Mg2 O3 2.1159(19) 2_666 ?
O3 C17 1.261(2) . ?
O3 Mg2 2.1159(19) 2_666 ?
O8 C21 1.261(2) . ?
O10 C37 1.263(2) . ?
O9 C37 1.256(2) . ?
O9 Mg2 2.0860(16) 2_666 ?
O2 C1 1.263(2) . ?
O7 C21 1.254(2) . ?
O1 C1 1.248(2) . ?
O4 C17 1.257(2) . ?
O13 H13B 0.938(19) . ?
O13 H13A 0.894(18) . ?
O16 N10 1.271(2) . ?
N10 O17 1.235(2) . ?
N10 O18 1.246(3) . ?
N1 C8 1.340(2) . ?
N1 C10 1.379(3) . ?
N1 C4 1.438(2) . ?
N6 C28 1.344(3) . ?
N6 C29 1.387(3) . ?
N6 C31 1.438(2) . ?
N2 C8 1.340(3) . ?
N2 C9 1.387(3) . ?
N2 C11 1.446(2) . ?
N5 C28 1.341(2) . ?
N5 C30 1.378(3) . ?
N5 C24 1.443(2) . ?
C28 H28 0.9500 . ?
N8 C42 1.339(3) . ?
N8 C41 1.439(3) . ?
N8 C40 1.450(4) . ?
C27 C26 1.388(3) . ?
C27 C22 1.399(3) . ?
C27 H27 0.9500 . ?
C1 C2 1.516(3) . ?
C23 C24 1.382(3) . ?
C23 C22 1.399(3) . ?
C23 H23 0.9500 . ?
C25 C26 1.389(3) . ?
C25 C24 1.396(3) . ?
C25 H25 0.9500 . ?
C32 C31 1.392(3) . ?
C32 C33 1.395(2) . ?
C32 H32 0.9500 . ?
C30 C29 1.351(3) . ?
C30 H30 0.9500 . ?
C37 C33 1.508(3) . ?
C33 C34 1.394(3) . ?
C21 C22 1.503(3) . ?
C17 C13 1.511(3) . ?
C4 C3 1.388(3) . ?
C4 C5 1.392(3) . ?
C29 H29 0.9500 . ?
C34 C35 1.385(3) . ?
C34 H34 0.9500 . ?
C36 C31 1.386(3) . ?
C36 C35 1.388(3) . ?
C36 H36 0.9500 . ?
C8 H8 0.9500 . ?
C13 C14 1.394(3) . ?
C13 C12 1.396(2) . ?
C3 C2 1.393(3) . ?
C3 H3 0.9500 . ?
C10 C9 1.355(3) . ?
C10 H10 0.9500 . ?
C26 H26 0.9500 . ?
C35 H35 0.9500 . ?
C7 C6 1.389(3) . ?
C7 C2 1.398(3) . ?
C7 H7 0.9500 . ?
C9 H9 0.9500 . ?
C12 C11 1.392(3) . ?
C12 H12 0.9500 . ?
O20 C42 1.224(3) . ?
C11 C16 1.387(3) . ?
C14 C15 1.385(3) . ?
C14 H14 0.9500 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C15 C16 1.387(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C41 H41C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C42 H42 0.9500 . ?
C40 H40B 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40C 0.9800 . ?
O12 H12A 1.01(4) . ?
O12 H12B 0.94(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Mg1 O7 180.0 . 2_665 ?
O7 Mg1 O1 91.15(7) . 2_665 ?
O7 Mg1 O1 88.85(7) 2_665 2_665 ?
O7 Mg1 O1 88.85(7) . . ?
O7 Mg1 O1 91.15(7) 2_665 . ?
O1 Mg1 O1 180.0 2_665 . ?
O7 Mg1 O12 90.94(7) . 2_665 ?
O7 Mg1 O12 89.06(7) 2_665 2_665 ?
O1 Mg1 O12 90.56(6) 2_665 2_665 ?
O1 Mg1 O12 89.44(6) . 2_665 ?
O7 Mg1 O12 89.06(7) . . ?
O7 Mg1 O12 90.94(7) 2_665 . ?
O1 Mg1 O12 89.44(6) 2_665 . ?
O1 Mg1 O12 90.56(6) . . ?
O12 Mg1 O12 180.0 2_665 . ?
O7 Mg1 Mg2 69.78(5) . . ?
O7 Mg1 Mg2 110.22(5) 2_665 . ?
O1 Mg1 Mg2 113.41(5) 2_665 . ?
O1 Mg1 Mg2 66.59(5) . . ?
O12 Mg1 Mg2 148.75(4) 2_665 . ?
O12 Mg1 Mg2 31.25(4) . . ?
O7 Mg1 Mg2 110.22(5) . 2_665 ?
O7 Mg1 Mg2 69.78(5) 2_665 2_665 ?
O1 Mg1 Mg2 66.59(5) 2_665 2_665 ?
O1 Mg1 Mg2 113.41(5) . 2_665 ?
O12 Mg1 Mg2 31.25(4) 2_665 2_665 ?
O12 Mg1 Mg2 148.75(4) . 2_665 ?
Mg2 Mg1 Mg2 180.0 . 2_665 ?
O8 Mg2 O13 90.90(7) . . ?
O8 Mg2 O9 173.80(7) . 2_666 ?
O13 Mg2 O9 86.71(6) . 2_666 ?
O8 Mg2 O2 85.71(7) . . ?
O13 Mg2 O2 89.70(7) . . ?
O9 Mg2 O2 88.56(7) 2_666 . ?
O8 Mg2 O12 94.22(6) . . ?
O13 Mg2 O12 172.96(6) . . ?
O9 Mg2 O12 88.68(6) 2_666 . ?
O2 Mg2 O12 95.49(6) . . ?
O8 Mg2 O3 96.39(7) . 2_666 ?
O13 Mg2 O3 86.45(7) . 2_666 ?
O9 Mg2 O3 89.17(7) 2_666 2_666 ?
O2 Mg2 O3 175.64(6) . 2_666 ?
O12 Mg2 O3 88.18(6) . 2_666 ?
O8 Mg2 Mg1 70.71(5) . . ?
O13 Mg2 Mg1 156.71(5) . . ?
O9 Mg2 Mg1 110.06(5) 2_666 . ?
O2 Mg2 Mg1 75.17(5) . . ?
O12 Mg2 Mg1 30.29(4) . . ?
O3 Mg2 Mg1 109.12(5) 2_666 . ?
C17 O3 Mg2 129.42(12) . 2_666 ?
C21 O8 Mg2 133.57(13) . . ?
C37 O9 Mg2 130.59(12) . 2_666 ?
C1 O2 Mg2 124.90(13) . . ?
C21 O7 Mg1 131.41(14) . . ?
C1 O1 Mg1 142.92(13) . . ?
Mg2 O13 H13B 124(3) . . ?
Mg2 O13 H13A 119(2) . . ?
H13B O13 H13A 106(3) . . ?
O17 N10 O18 123.3(2) . . ?
O17 N10 O16 118.1(2) . . ?
O18 N10 O16 118.56(17) . . ?
C8 N1 C10 108.73(17) . . ?
C8 N1 C4 125.30(17) . . ?
C10 N1 C4 125.89(17) . . ?
C28 N6 C29 108.98(16) . . ?
C28 N6 C31 126.43(17) . . ?
C29 N6 C31 124.56(17) . . ?
C8 N2 C9 108.86(16) . . ?
C8 N2 C11 126.07(17) . . ?
C9 N2 C11 125.04(17) . . ?
C28 N5 C30 109.36(16) . . ?
C28 N5 C24 126.31(18) . . ?
C30 N5 C24 124.12(16) . . ?
N5 C28 N6 107.44(18) . . ?
N5 C28 H28 126.3 . . ?
N6 C28 H28 126.3 . . ?
C42 N8 C41 122.2(2) . . ?
C42 N8 C40 120.4(3) . . ?
C41 N8 C40 117.2(2) . . ?
C26 C27 C22 120.16(18) . . ?
C26 C27 H27 119.9 . . ?
C22 C27 H27 119.9 . . ?
O1 C1 O2 126.51(18) . . ?
O1 C1 C2 115.78(16) . . ?
O2 C1 C2 117.70(16) . . ?
C24 C23 C22 118.81(17) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C26 C25 C24 118.39(19) . . ?
C26 C25 H25 120.8 . . ?
C24 C25 H25 120.8 . . ?
C31 C32 C33 118.14(18) . . ?
C31 C32 H32 120.9 . . ?
C33 C32 H32 120.9 . . ?
C29 C30 N5 107.24(17) . . ?
C29 C30 H30 126.4 . . ?
N5 C30 H30 126.4 . . ?
O9 C37 O10 126.39(18) . . ?
O9 C37 C33 117.65(16) . . ?
O10 C37 C33 115.94(17) . . ?
C34 C33 C32 120.11(18) . . ?
C34 C33 C37 119.30(16) . . ?
C32 C33 C37 120.58(18) . . ?
O7 C21 O8 126.49(19) . . ?
O7 C21 C22 116.24(17) . . ?
O8 C21 C22 117.26(17) . . ?
O4 C17 O3 125.96(19) . . ?
O4 C17 C13 115.79(17) . . ?
O3 C17 C13 118.24(16) . . ?
C3 C4 C5 121.93(18) . . ?
C3 C4 N1 119.72(17) . . ?
C5 C4 N1 118.33(18) . . ?
C23 C24 C25 122.13(17) . . ?
C23 C24 N5 120.19(16) . . ?
C25 C24 N5 117.33(18) . . ?
C30 C29 N6 106.98(18) . . ?
C30 C29 H29 126.5 . . ?
N6 C29 H29 126.5 . . ?
C35 C34 C33 120.71(17) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.6 . . ?
C31 C36 C35 119.15(18) . . ?
C31 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C27 C22 C23 119.82(19) . . ?
C27 C22 C21 119.49(17) . . ?
C23 C22 C21 120.48(17) . . ?
N2 C8 N1 108.16(18) . . ?
N2 C8 H8 125.9 . . ?
N1 C8 H8 125.9 . . ?
C36 C31 C32 122.08(17) . . ?
C36 C31 N6 118.06(17) . . ?
C32 C31 N6 119.85(17) . . ?
C14 C13 C12 120.27(18) . . ?
C14 C13 C17 118.66(17) . . ?
C12 C13 C17 121.06(18) . . ?
C4 C3 C2 118.79(17) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C9 C10 N1 107.54(18) . . ?
C9 C10 H10 126.2 . . ?
N1 C10 H10 126.2 . . ?
C27 C26 C25 120.66(18) . . ?
C27 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C34 C35 C36 119.81(19) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C6 C7 C2 120.09(18) . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
C10 C9 N2 106.70(18) . . ?
C10 C9 H9 126.7 . . ?
N2 C9 H9 126.7 . . ?
C11 C12 C13 118.36(18) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C16 C11 C12 121.54(17) . . ?
C16 C11 N2 117.52(18) . . ?
C12 C11 N2 120.94(17) . . ?
C15 C14 C13 120.42(18) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C4 C5 C6 118.59(19) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C7 C6 C5 120.45(18) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C3 C2 C7 120.12(18) . . ?
C3 C2 C1 120.75(16) . . ?
C7 C2 C1 119.13(17) . . ?
C14 C15 C16 119.82(19) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C11 C16 C15 119.56(19) . . ?
C11 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
N8 C41 H41C 109.5 . . ?
N8 C41 H41A 109.5 . . ?
H41C C41 H41A 109.5 . . ?
N8 C41 H41B 109.5 . . ?
H41C C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O20 C42 N8 125.1(3) . . ?
O20 C42 H42 117.5 . . ?
N8 C42 H42 117.5 . . ?
N8 C40 H40B 109.5 . . ?
N8 C40 H40A 109.5 . . ?
H40B C40 H40A 109.5 . . ?
N8 C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
Mg1 O12 Mg2 118.46(7) . . ?
Mg1 O12 H12A 111(2) . . ?
Mg2 O12 H12A 101(2) . . ?
Mg1 O12 H12B 116(2) . . ?
Mg2 O12 H12B 104(2) . . ?
H12A O12 H12B 104(3) . . ?

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
C30 N5 C28 N6 0.8(2) . . . . ?
C24 N5 C28 N6 -174.05(17) . . . . ?
C29 N6 C28 N5 -0.9(2) . . . . ?
C31 N6 C28 N5 -179.01(17) . . . . ?
Mg1 O1 C1 O2 16.6(4) . . . . ?
Mg1 O1 C1 C2 -164.05(17) . . . . ?
Mg2 O2 C1 O1 -26.7(3) . . . . ?
Mg2 O2 C1 C2 154.04(14) . . . . ?
C28 N5 C30 C29 -0.4(2) . . . . ?
C24 N5 C30 C29 174.61(17) . . . . ?
Mg2 O9 C37 O10 -5.8(3) 2_666 . . . ?
Mg2 O9 C37 C33 172.44(13) 2_666 . . . ?
C31 C32 C33 C34 -0.2(3) . . . . ?
C31 C32 C33 C37 178.87(18) . . . . ?
O9 C37 C33 C34 176.32(18) . . . . ?
O10 C37 C33 C34 -5.2(3) . . . . ?
O9 C37 C33 C32 -2.8(3) . . . . ?
O10 C37 C33 C32 175.64(18) . . . . ?
Mg1 O7 C21 O8 -37.0(3) . . . . ?
Mg1 O7 C21 C22 144.05(15) . . . . ?
Mg2 O8 C21 O7 8.5(3) . . . . ?
Mg2 O8 C21 C22 -172.55(13) . . . . ?
Mg2 O3 C17 O4 6.7(3) 2_666 . . . ?
Mg2 O3 C17 C13 -173.73(14) 2_666 . . . ?
C8 N1 C4 C3 -25.6(3) . . . . ?
C10 N1 C4 C3 157.8(2) . . . . ?
C8 N1 C4 C5 152.7(2) . . . . ?
C10 N1 C4 C5 -23.8(3) . . . . ?
C22 C23 C24 C25 -1.9(3) . . . . ?
C22 C23 C24 N5 171.15(18) . . . . ?
C26 C25 C24 C23 2.4(3) . . . . ?
C26 C25 C24 N5 -170.83(18) . . . . ?
C28 N5 C24 C23 26.3(3) . . . . ?
C30 N5 C24 C23 -147.9(2) . . . . ?
C28 N5 C24 C25 -160.39(19) . . . . ?
C30 N5 C24 C25 25.5(3) . . . . ?
N5 C30 C29 N6 -0.2(2) . . . . ?
C28 N6 C29 C30 0.7(2) . . . . ?
C31 N6 C29 C30 178.81(18) . . . . ?
C32 C33 C34 C35 -0.6(3) . . . . ?
C37 C33 C34 C35 -179.68(19) . . . . ?
C26 C27 C22 C23 1.1(3) . . . . ?
C26 C27 C22 C21 175.81(18) . . . . ?
C24 C23 C22 C27 0.1(3) . . . . ?
C24 C23 C22 C21 -174.59(18) . . . . ?
O7 C21 C22 C27 -0.3(3) . . . . ?
O8 C21 C22 C27 -179.31(19) . . . . ?
O7 C21 C22 C23 174.46(19) . . . . ?
O8 C21 C22 C23 -4.6(3) . . . . ?
C9 N2 C8 N1 0.8(2) . . . . ?
C11 N2 C8 N1 -177.18(19) . . . . ?
C10 N1 C8 N2 -0.4(3) . . . . ?
C4 N1 C8 N2 -177.41(18) . . . . ?
C35 C36 C31 C32 -1.2(3) . . . . ?
C35 C36 C31 N6 177.28(19) . . . . ?
C33 C32 C31 C36 1.2(3) . . . . ?
C33 C32 C31 N6 -177.35(18) . . . . ?
C28 N6 C31 C36 154.3(2) . . . . ?
C29 N6 C31 C36 -23.5(3) . . . . ?
C28 N6 C31 C32 -27.2(3) . . . . ?
C29 N6 C31 C32 155.04(19) . . . . ?
O4 C17 C13 C14 -2.8(3) . . . . ?
O3 C17 C13 C14 177.5(2) . . . . ?
O4 C17 C13 C12 178.6(2) . . . . ?
O3 C17 C13 C12 -1.1(3) . . . . ?
C5 C4 C3 C2 -1.1(3) . . . . ?
N1 C4 C3 C2 177.19(19) . . . . ?
C8 N1 C10 C9 -0.2(3) . . . . ?
C4 N1 C10 C9 176.8(2) . . . . ?
C22 C27 C26 C25 -0.5(3) . . . . ?
C24 C25 C26 C27 -1.1(3) . . . . ?
C33 C34 C35 C36 0.5(3) . . . . ?
C31 C36 C35 C34 0.4(3) . . . . ?
N1 C10 C9 N2 0.7(3) . . . . ?
C8 N2 C9 C10 -0.9(3) . . . . ?
C11 N2 C9 C10 177.1(2) . . . . ?
C14 C13 C12 C11 -0.8(3) . . . . ?
C17 C13 C12 C11 177.8(2) . . . . ?
C13 C12 C11 C16 -0.9(3) . . . . ?
C13 C12 C11 N2 179.36(19) . . . . ?
C8 N2 C11 C16 -171.3(2) . . . . ?
C9 N2 C11 C16 11.0(3) . . . . ?
C8 N2 C11 C12 8.5(3) . . . . ?
C9 N2 C11 C12 -169.2(2) . . . . ?
C12 C13 C14 C15 1.7(3) . . . . ?
C17 C13 C14 C15 -176.9(2) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
N1 C4 C5 C6 -178.1(2) . . . . ?
C2 C7 C6 C5 -2.1(3) . . . . ?
C4 C5 C6 C7 1.4(3) . . . . ?
C4 C3 C2 C7 0.4(3) . . . . ?
C4 C3 C2 C1 -179.18(19) . . . . ?
C6 C7 C2 C3 1.1(3) . . . . ?
C6 C7 C2 C1 -179.3(2) . . . . ?
O1 C1 C2 C3 178.34(19) . . . . ?
O2 C1 C2 C3 -2.3(3) . . . . ?
O1 C1 C2 C7 -1.3(3) . . . . ?
O2 C1 C2 C7 178.10(19) . . . . ?
C13 C14 C15 C16 -0.8(4) . . . . ?
C12 C11 C16 C15 1.8(4) . . . . ?
N2 C11 C16 C15 -178.5(2) . . . . ?
C14 C15 C16 C11 -0.9(4) . . . . ?
C41 N8 C42 O20 178.2(3) . . . . ?
C40 N8 C42 O20 1.7(5) . . . . ?

_refine_diff_density_max         0.352
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.086

_shelxl_version_number           2014/6


# start Validation Reply Form
_vrf_PLAT029_4Mg                 
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.929 Note  
RESPONSE: Data was collected on the MX1 beamline at the Australian
Synchrotron, where only phi rotation was available for data collection.
Due to the low symmetry, removal and remounting was considered but, like
many materials of this type, the crystals do not respond well to abrupt
temperature changes and remounting.
;
# 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_2Cu
_database_code_depnum_ccdc_archive 'CCDC 1475106'
_audit_update_record             
;
2016-08-20 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40.25 H35.15 Br0.10 Cu2.10 N6.65 O14.45'
_chemical_formula_weight         984.62

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   20.7373(16)
_cell_length_b                   17.9433(14)
_cell_length_c                   10.9131(8)
_cell_angle_alpha                90
_cell_angle_beta                 91.475(7)
_cell_angle_gamma                90
_cell_volume                     4059.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3697
_cell_measurement_theta_max      29.1319
_cell_measurement_theta_min      2.6701

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_F_000             2013
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.277
_shelx_estimated_absorpt_T_min   0.701
_shelx_estimated_absorpt_T_max   0.831
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean 16.1695
_diffrn_reflns_number            18655
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.676
_diffrn_reflns_theta_max         29.196
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5081
_reflns_number_gt                3863
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
17 restraints (ISOR, DFIX, CHIV and EADP) were used in the 
refinement. The structure possesses a DMF located on a mirror 
plane and refinement required the use of restraints to achieve 
a chemically sensible structure. In addition there is a small
amount of a C-Cu-Br carbene moiety disordered with the 
imidazolium-NO3 unit (also on a mirror plane) and DFIX and 
CHIV restraints were required to achieve a chemically sensible 
structure.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0848P)²+14.6135P] 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_number_reflns         5081
_refine_ls_number_parameters     284
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1685
_refine_ls_wR_factor_gt          0.1579
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.078
_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
Cu1 Cu 0.75429(2) 0.17623(2) 0.97947(4) 0.01141(15) Uani 1 1 d . . . . .
O1 O 0.75572(14) 0.06129(14) 0.9434(3) 0.0218(6) Uani 1 1 d . . . . .
C1 C 0.84157(19) 0.1915(2) 1.5966(4) 0.0209(8) Uani 1 1 d . . . . .
H1 H 0.8530 0.1804 1.6795 0.025 Uiso 1 1 calc R U . . .
Cu2 Cu 0.9114(4) 0.5000 0.7489(8) 0.040(2) Uiso 0.1 2 d DS . P A 2
Br3 Br 0.8177(9) 0.5000 0.6116(19) 0.133(6) Uiso 0.1 2 d DS . P A 2
O2 O 0.78543(13) 0.18176(14) 1.1505(2) 0.0194(6) Uani 1 1 d . . . . .
N2 N 1.03650(14) 0.43978(17) 0.8306(3) 0.0178(7) Uani 1 1 d . . . . .
C2 C 0.86398(17) 0.2639(2) 0.9244(3) 0.0143(7) Uani 1 1 d . . . . .
O3 O 0.84222(12) 0.19767(15) 0.9200(2) 0.0179(5) Uani 1 1 d . . . . .
C3 C 0.92951(17) 0.2776(2) 0.8741(3) 0.0160(7) Uani 1 1 d . . . . .
O4 O 0.77865(13) 0.30435(15) 1.1898(2) 0.0192(6) Uani 1 1 d . . . . .
C4 C 1.01255(17) 0.3646(2) 0.8277(3) 0.0171(7) Uani 1 1 d . . . . .
O5 O 0.83506(12) 0.31949(14) 0.9661(3) 0.0200(6) Uani 1 1 d . . . . .
C5 C 0.78983(16) 0.2374(2) 1.2205(3) 0.0160(7) Uani 1 1 d . . . . .
C6 C 0.95194(17) 0.3503(2) 0.8722(3) 0.0152(7) Uani 1 1 d . . . . .
H6 H 0.9260 0.3899 0.9011 0.018 Uiso 1 1 calc R U . . .
N7 N 0.81737(16) 0.06004(18) 1.5579(3) 0.0194(7) Uani 1 1 d . . . . .
C7 C 0.9987(2) 0.5000 0.8149(5) 0.0187(11) Uani 1 2 d S T P . .
H7 H 0.9537 0.5000 0.7962 0.022 Uiso 0.9 2 calc R U P A 1
C8 C 0.8317(3) 0.0000 1.4922(5) 0.0180(11) Uani 1 2 d S T P . .
H8 H 0.8490 0.0000 1.4124 0.022 Uiso 1 2 calc R U P . .
C9 C 0.82270(18) 0.1353(2) 1.5153(3) 0.0182(8) Uani 1 1 d . . . . .
C10 C 1.05130(19) 0.3081(2) 0.7842(4) 0.0238(9) Uani 1 1 d . . . . .
H10 H 1.0930 0.3189 0.7547 0.029 Uiso 1 1 calc R U . . .
C11 C 0.80717(17) 0.1496(2) 1.3935(3) 0.0175(8) Uani 1 1 d . . . . .
H11 H 0.7953 0.1102 1.3393 0.021 Uiso 1 1 calc R U . . .
C12 C 0.80932(17) 0.2228(2) 1.3522(3) 0.0168(7) Uani 1 1 d . . . . .
C13 C 1.09971(17) 0.4626(2) 0.8553(4) 0.0204(8) Uani 1 1 d . . . . .
H13 H 1.1360 0.4311 0.8695 0.025 Uiso 1 1 calc R U . . .
C14 C 0.82685(17) 0.2802(2) 1.4328(3) 0.0183(8) Uani 1 1 d . . . . .
H14 H 0.8275 0.3302 1.4045 0.022 Uiso 1 1 calc R U . . .
C15 C 0.7931(2) 0.0379(2) 1.6704(3) 0.0234(8) Uani 1 1 d . . . . .
H15 H 0.7793 0.0696 1.7343 0.028 Uiso 1 1 calc R U . . .
C16 C 0.7537(2) 0.0000 0.9967(5) 0.0155(10) Uani 1 2 d S T P . .
H16 H 0.7504 0.0000 1.0833 0.019 Uiso 1 2 calc R U P . .
C18 C 0.96789(18) 0.2199(2) 0.8309(4) 0.0225(8) Uani 1 1 d . . . . .
H18 H 0.9528 0.1700 0.8330 0.027 Uiso 1 1 calc R U . . .
C19 C 0.84323(19) 0.2645(2) 1.5531(3) 0.0206(8) Uani 1 1 d . . . . .
H19 H 0.8558 0.3038 1.6070 0.025 Uiso 1 1 calc R U . . .
C20 C 1.0282(2) 0.2358(2) 0.7846(4) 0.0284(10) Uani 1 1 d . . . . .
H20 H 1.0537 0.1966 0.7529 0.034 Uiso 1 1 calc R U . . .
N23 N 0.8328(6) 0.5000 0.6872(10) 0.085(3) Uiso 0.9 2 d DS . P B 1
O24 O 0.7785(6) 0.5000 0.6599(12) 0.135(4) Uiso 0.9 2 d DS . P B 1
O25 O 0.8655(6) 0.5575(6) 0.6922(11) 0.186(5) Uiso 0.9 1 d D . P B 1
O30 O 0.8990(4) 0.0475(5) 1.2458(7) 0.054(2) Uani 0.5 1 d D . P C 1
C31 C 0.8991(4) 0.0554(6) 1.1345(8) 0.032(2) Uani 0.5 1 d D U P C 1
H31 H 0.8910 0.1036 1.1015 0.038 Uiso 0.5 1 calc R U P C 1
N32 N 0.9100(3) 0.0000 1.0581(5) 0.0328(12) Uani 1 2 d DS T P . .
C33 C 0.9075(4) 0.0000 0.9246(7) 0.0492(17) Uani 1 2 d S T P C .
H33A H 0.9181 0.0499 0.8944 0.074 Uiso 0.5 1 calc R U P . .
H33B H 0.9388 -0.0360 0.8940 0.074 Uiso 0.5 1 calc R U P . .
H33C H 0.8641 -0.0138 0.8954 0.074 Uiso 0.5 1 calc R U P . .
C34 C 0.9245(6) -0.0756(7) 1.0985(12) 0.0492(17) Uani 0.5 1 d D U P C 2
H34A H 0.9265 -0.0772 1.1883 0.074 Uiso 0.5 1 calc R U P C 2
H34B H 0.8906 -0.1094 1.0679 0.074 Uiso 0.5 1 calc R U P C 2
H34C H 0.9661 -0.0911 1.0665 0.074 Uiso 0.5 1 calc R U P C 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
Cu1 O2 1.961(3) . ?
Cu1 O5 1.962(3) 7_657 ?
Cu1 O4 1.984(3) 7_657 ?
Cu1 O3 1.989(3) . ?
Cu1 O1 2.100(3) . ?
Cu1 Cu1 2.6915(8) 7_657 ?
O1 C16 1.245(3) . ?
C1 C9 1.392(5) . ?
C1 C19 1.394(6) . ?
C1 H1 0.9500 . ?
Cu2 C7 1.931(10) . ?
Cu2 Br3 2.422(16) . ?
O2 C5 1.259(4) . ?
N2 C7 1.343(4) . ?
N2 C13 1.393(5) . ?
N2 C4 1.438(5) . ?
C2 O5 1.255(4) . ?
C2 O3 1.272(4) . ?
C2 C3 1.499(5) . ?
C3 C6 1.385(5) . ?
C3 C18 1.395(5) . ?
O4 C5 1.268(4) . ?
O4 Cu1 1.984(3) 7_657 ?
C4 C6 1.383(5) . ?
C4 C10 1.384(5) . ?
O5 Cu1 1.962(3) 7_657 ?
C5 C12 1.506(5) . ?
C6 H6 0.9500 . ?
N7 C8 1.332(4) . ?
N7 C15 1.395(5) . ?
N7 C9 1.434(5) . ?
C7 N2 1.343(4) 6_565 ?
C7 H7 0.9500 . ?
C8 N7 1.332(4) 6 ?
C8 H8 0.9500 . ?
C9 C11 1.384(5) . ?
C10 C20 1.384(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.390(5) . ?
C11 H11 0.9500 . ?
C12 C14 1.396(5) . ?
C13 C13 1.342(8) 6_565 ?
C13 H13 0.9500 . ?
C14 C19 1.377(5) . ?
C14 H14 0.9500 . ?
C15 C15 1.361(8) 6 ?
C15 H15 0.9500 . ?
C16 O1 1.245(3) 6 ?
C16 H16 0.9500 . ?
C18 C20 1.390(6) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
N23 O24 1.157(12) . ?
N23 O25 1.236(10) 6_565 ?
N23 O25 1.236(10) . ?
O30 C31 1.223(10) . ?
O30 O30 1.703(17) 6 ?
C31 N32 1.321(10) . ?
C31 C31 1.99(2) 6 ?
C31 H31 0.9500 . ?
N32 C31 1.321(10) 6 ?
N32 C33 1.456(9) . ?
N32 C34 1.455(13) 6 ?
N32 C34 1.455(13) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O5 90.01(12) . 7_657 ?
O2 Cu1 O4 166.93(11) . 7_657 ?
O5 Cu1 O4 88.28(11) 7_657 7_657 ?
O2 Cu1 O3 91.06(11) . . ?
O5 Cu1 O3 166.49(11) 7_657 . ?
O4 Cu1 O3 87.63(11) 7_657 . ?
O2 Cu1 O1 102.82(11) . . ?
O5 Cu1 O1 96.50(11) 7_657 . ?
O4 Cu1 O1 90.24(11) 7_657 . ?
O3 Cu1 O1 96.39(11) . . ?
O2 Cu1 Cu1 79.25(8) . 7_657 ?
O5 Cu1 Cu1 81.03(8) 7_657 7_657 ?
O4 Cu1 Cu1 87.69(8) 7_657 7_657 ?
O3 Cu1 Cu1 85.94(8) . 7_657 ?
O1 Cu1 Cu1 176.82(8) . 7_657 ?
C16 O1 Cu1 141.2(3) . . ?
C9 C1 C19 118.2(3) . . ?
C9 C1 H1 120.9 . . ?
C19 C1 H1 120.9 . . ?
C7 Cu2 Br3 163.7(7) . . ?
C5 O2 Cu1 129.4(2) . . ?
C7 N2 C13 109.4(3) . . ?
C7 N2 C4 123.5(3) . . ?
C13 N2 C4 127.1(3) . . ?
O5 C2 O3 125.7(3) . . ?
O5 C2 C3 116.7(3) . . ?
O3 C2 C3 117.6(3) . . ?
C2 O3 Cu1 119.7(2) . . ?
C6 C3 C18 119.9(3) . . ?
C6 C3 C2 117.9(3) . . ?
C18 C3 C2 122.2(3) . . ?
C5 O4 Cu1 118.0(2) . 7_657 ?
C6 C4 C10 121.7(4) . . ?
C6 C4 N2 118.9(3) . . ?
C10 C4 N2 119.4(3) . . ?
C2 O5 Cu1 127.2(2) . 7_657 ?
O2 C5 O4 125.5(3) . . ?
O2 C5 C12 117.1(3) . . ?
O4 C5 C12 117.4(3) . . ?
C4 C6 C3 119.2(3) . . ?
C4 C6 H6 120.4 . . ?
C3 C6 H6 120.4 . . ?
C8 N7 C15 109.5(3) . . ?
C8 N7 C9 124.5(3) . . ?
C15 N7 C9 125.9(3) . . ?
N2 C7 N2 107.1(4) . 6_565 ?
N2 C7 Cu2 125.9(2) . . ?
N2 C7 Cu2 125.9(2) 6_565 . ?
N2 C7 H7 126.5 . . ?
N2 C7 H7 126.5 6_565 . ?
N7 C8 N7 107.9(5) . 6 ?
N7 C8 H8 126.0 . . ?
N7 C8 H8 126.0 6 . ?
C11 C9 C1 122.2(4) . . ?
C11 C9 N7 117.9(3) . . ?
C1 C9 N7 119.8(3) . . ?
C20 C10 C4 118.7(4) . . ?
C20 C10 H10 120.6 . . ?
C4 C10 H10 120.6 . . ?
C9 C11 C12 118.5(4) . . ?
C9 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C11 C12 C14 120.2(3) . . ?
C11 C12 C5 117.6(3) . . ?
C14 C12 C5 122.2(3) . . ?
C13 C13 N2 107.1(2) 6_565 . ?
C13 C13 H13 126.5 6_565 . ?
N2 C13 H13 126.5 . . ?
C19 C14 C12 120.3(4) . . ?
C19 C14 H14 119.9 . . ?
C12 C14 H14 119.9 . . ?
C15 C15 N7 106.5(2) 6 . ?
C15 C15 H15 126.7 6 . ?
N7 C15 H15 126.7 . . ?
O1 C16 O1 124.1(5) 6 . ?
O1 C16 H16 118.0 6 . ?
O1 C16 H16 118.0 . . ?
C20 C18 C3 119.8(4) . . ?
C20 C18 H18 120.1 . . ?
C3 C18 H18 120.1 . . ?
C14 C19 C1 120.6(4) . . ?
C14 C19 H19 119.7 . . ?
C1 C19 H19 119.7 . . ?
C10 C20 C18 120.5(4) . . ?
C10 C20 H20 119.7 . . ?
C18 C20 H20 119.7 . . ?
O24 N23 O25 122.7(8) . 6_565 ?
O24 N23 O25 122.7(8) . . ?
O25 N23 O25 113.3(15) 6_565 . ?
C31 O30 O30 96.7(6) . 6 ?
O30 C31 N32 122.9(9) . . ?
O30 C31 C31 83.3(6) . 6 ?
N32 C31 C31 41.2(5) . 6 ?
O30 C31 H31 118.5 . . ?
N32 C31 H31 118.5 . . ?
C31 C31 H31 155.5 6 . ?
C31 N32 C31 97.7(10) 6 . ?
C31 N32 C33 129.0(5) 6 . ?
C31 N32 C33 129.0(5) . . ?
C33 N32 C34 107.8(6) . 6 ?
C33 N32 C34 107.8(6) . . ?
C34 N32 C34 137.5(11) 6 . ?
N32 C33 H33A 109.5 . . ?
N32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N32 C34 H34A 109.5 . . ?
N32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 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
O5 C2 O3 Cu1 1.4(5) . . . . ?
C3 C2 O3 Cu1 -177.8(2) . . . . ?
O5 C2 C3 C6 -2.8(5) . . . . ?
O3 C2 C3 C6 176.4(3) . . . . ?
O5 C2 C3 C18 176.7(4) . . . . ?
O3 C2 C3 C18 -4.1(5) . . . . ?
C7 N2 C4 C6 -34.0(6) . . . . ?
C13 N2 C4 C6 142.6(4) . . . . ?
C7 N2 C4 C10 148.0(4) . . . . ?
C13 N2 C4 C10 -35.5(6) . . . . ?
O3 C2 O5 Cu1 -6.8(6) . . . 7_657 ?
C3 C2 O5 Cu1 172.4(2) . . . 7_657 ?
Cu1 O2 C5 O4 -5.5(5) . . . . ?
Cu1 O2 C5 C12 173.8(2) . . . . ?
Cu1 O4 C5 O2 4.4(5) 7_657 . . . ?
Cu1 O4 C5 C12 -174.9(2) 7_657 . . . ?
C10 C4 C6 C3 0.4(6) . . . . ?
N2 C4 C6 C3 -177.6(3) . . . . ?
C18 C3 C6 C4 -0.3(5) . . . . ?
C2 C3 C6 C4 179.2(3) . . . . ?
C13 N2 C7 N2 -0.7(6) . . . 6_565 ?
C4 N2 C7 N2 176.4(2) . . . 6_565 ?
C13 N2 C7 Cu2 167.5(5) . . . . ?
C4 N2 C7 Cu2 -15.4(7) . . . . ?
C15 N7 C8 N7 0.2(6) . . . 6 ?
C9 N7 C8 N7 -176.4(2) . . . 6 ?
C19 C1 C9 C11 1.5(6) . . . . ?
C19 C1 C9 N7 -177.0(3) . . . . ?
C8 N7 C9 C11 36.7(6) . . . . ?
C15 N7 C9 C11 -139.3(4) . . . . ?
C8 N7 C9 C1 -144.8(4) . . . . ?
C15 N7 C9 C1 39.2(6) . . . . ?
C6 C4 C10 C20 0.6(6) . . . . ?
N2 C4 C10 C20 178.6(4) . . . . ?
C1 C9 C11 C12 -1.3(6) . . . . ?
N7 C9 C11 C12 177.1(3) . . . . ?
C9 C11 C12 C14 0.0(5) . . . . ?
C9 C11 C12 C5 -177.8(3) . . . . ?
O2 C5 C12 C11 -13.9(5) . . . . ?
O4 C5 C12 C11 165.5(3) . . . . ?
O2 C5 C12 C14 168.4(3) . . . . ?
O4 C5 C12 C14 -12.3(5) . . . . ?
C7 N2 C13 C13 0.4(4) . . . 6_565 ?
C4 N2 C13 C13 -176.5(3) . . . 6_565 ?
C11 C12 C14 C19 1.2(5) . . . . ?
C5 C12 C14 C19 178.8(3) . . . . ?
C8 N7 C15 C15 -0.1(4) . . . 6 ?
C9 N7 C15 C15 176.4(3) . . . 6 ?
Cu1 O1 C16 O1 179.94(15) . . . 6 ?
C6 C3 C18 C20 -0.8(6) . . . . ?
C2 C3 C18 C20 179.6(4) . . . . ?
C12 C14 C19 C1 -1.0(6) . . . . ?
C9 C1 C19 C14 -0.3(6) . . . . ?
C4 C10 C20 C18 -1.8(7) . . . . ?
C3 C18 C20 C10 1.9(7) . . . . ?
O30 O30 C31 N32 -11.7(10) 6 . . . ?
O30 O30 C31 C31 0.000(3) 6 . . 6 ?
O30 C31 N32 C31 17.8(14) . . . 6 ?
O30 C31 N32 C33 175.5(8) . . . . ?
C31 C31 N32 C33 157.8(11) 6 . . . ?

_refine_diff_density_max         2.579
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.129

_shelxl_version_number           2014/6


# SQUEEZE RESULTS
# 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 0.000 -0.018 0.500 298 61 ' '
2 0.500 0.420 0.500 298 61 ' '
_platon_squeeze_details          
;
In order to subtract the contribution from the disordered 
solvent molecules, the SQUEEZE command was applied, which 
gave a new HKL file. The number of located electrons is 
122, is included in the formula, formula weight, calculated 
density, and F(000). These residual electron density 
were assigned to approx 3 DMF molecules per unit cell. 
This value calculated based upon electrons analysis. 
(One DMF molecules would give 40 e). 
;

# start Validation Reply Form
_vrf_CHEMW03_2Cu                 
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: 
The formula includes 0.75 DMF molecules per formula
unit to account for the electron density removed by SQUEEZE
(an additional DMF molecule was located in the structure 
giving 1.75 DMF molecules per formula unit).
;
# 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_5Mn
_database_code_depnum_ccdc_archive 'CCDC 1475107'
_audit_update_record             
;
2016-08-15 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72.50 H60.50 Mn3 N11.50 O26.50'
_chemical_formula_weight         1681.64

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 0.3370 0.7280 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.014(2)
_cell_length_b                   13.053(3)
_cell_length_c                   14.145(3)
_cell_angle_alpha                63.88(3)
_cell_angle_beta                 79.87(3)
_cell_angle_gamma                89.57(3)
_cell_volume                     1791.8(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7871
_cell_measurement_theta_max      12.46
_cell_measurement_theta_min      0.76

_exptl_crystal_description       block
_exptl_crystal_colour            'light brown/orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_F_000             863
_exptl_transmission_factor_max   0.930
_exptl_transmission_factor_min   0.847
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.615
_shelx_estimated_absorpt_T_min   0.847
_shelx_estimated_absorpt_T_max   0.930
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7108
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30395
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.634
_diffrn_reflns_theta_max         27.917
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measured_fraction_theta_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_point_group_measured_fraction_full 0.925
_reflns_number_total             7854
_reflns_number_gt                5359
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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       'BluIce (McPhillips, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1502P)²+0.2333P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7854
_refine_ls_number_parameters     460
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0788
_refine_ls_wR_factor_ref         0.2330
_refine_ls_wR_factor_gt          0.2133
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 1.0000 0.5000 0.0000 0.0235(2) Uani 1 2 d S . P . .
O1 O 0.8507(3) 0.5722(3) 0.0652(3) 0.0365(7) Uani 1 1 d . . . . .
N1 N 0.4424(4) 0.6443(4) 0.3658(3) 0.0374(9) Uani 1 1 d . . . . .
C1 C 0.8139(4) 0.5895(3) 0.1449(4) 0.0285(8) Uani 1 1 d . . . . .
Mn2 Mn 1.05784(6) 0.52575(6) 0.23641(6) 0.0320(2) Uani 1 1 d . . . . .
O2 O 0.8723(3) 0.5817(3) 0.2163(3) 0.0355(7) Uani 1 1 d . . . . .
N2 N 0.4135(4) 0.6426(4) 0.5223(3) 0.0381(9) Uani 1 1 d . . . . .
C2 C 0.6805(4) 0.6238(3) 0.1573(3) 0.0286(8) Uani 1 1 d . . . . .
O3 O 0.7612(3) 0.5393(3) 0.7315(3) 0.0344(7) Uani 1 1 d . . . . .
N3 N 0.8303(4) -0.0605(3) 0.7555(3) 0.0371(9) Uani 1 1 d . . . . .
C3 C 0.6252(4) 0.6271(4) 0.2517(4) 0.0356(10) Uani 1 1 d . . . . .
H3 H 0.6703 0.6119 0.3073 0.043 Uiso 1 1 calc R U . . .
O4 O 0.6897(3) 0.5677(3) 0.8764(3) 0.0402(8) Uani 1 1 d . . . . .
N4 N 0.8322(4) -0.0380(3) 0.5931(3) 0.0359(9) Uani 1 1 d . . . . .
C4 C 0.5032(4) 0.6529(4) 0.2636(4) 0.0345(9) Uani 1 1 d . . . . .
C5 C 0.4359(4) 0.6805(4) 0.1833(4) 0.0347(10) Uani 1 1 d . . . . .
H5 H 0.3535 0.7018 0.1920 0.042 Uiso 1 1 calc R U . . .
C6 C 0.4924(4) 0.6762(4) 0.0894(4) 0.0339(9) Uani 1 1 d . . . . .
H6 H 0.4478 0.6935 0.0332 0.041 Uiso 1 1 calc R U . . .
O7 O 0.9736(3) 0.3348(3) 0.1390(2) 0.0367(7) Uani 1 1 d . . . . .
C7 C 0.6138(4) 0.6468(4) 0.0768(3) 0.0305(9) Uani 1 1 d . . . . .
H7 H 0.6509 0.6424 0.0129 0.037 Uiso 1 1 calc R U . . .
O8 O 0.9828(3) 0.3528(3) 0.2882(3) 0.0340(7) Uani 1 1 d . . . . .
C8 C 0.4989(4) 0.6639(4) 0.4337(4) 0.0363(10) Uani 1 1 d . . . . .
H8 H 0.5837 0.6883 0.4215 0.044 Uiso 1 1 calc R U . . .
O9 O 0.8741(3) 0.2959(3) 0.8142(3) 0.0348(7) Uani 1 1 d . . . . .
C9 C 0.3000(5) 0.6107(5) 0.5079(4) 0.0469(12) Uani 1 1 d . . . . .
H9 H 0.2237 0.5930 0.5573 0.056 Uiso 1 1 calc R U . . .
O10 O 0.8172(4) 0.2262(3) 0.9924(3) 0.0433(8) Uani 1 1 d . . . . .
C10 C 0.3178(5) 0.6096(5) 0.4119(4) 0.0455(12) Uani 1 1 d . . . . .
H10 H 0.2574 0.5892 0.3814 0.055 Uiso 1 1 calc R U . . .
C11 C 0.4362(4) 0.6487(4) 0.6168(4) 0.0355(10) Uani 1 1 d . . . . .
C12 C 0.5493(4) 0.6192(4) 0.6486(4) 0.0351(10) Uani 1 1 d . . . . .
H12 H 0.6146 0.6035 0.6044 0.042 Uiso 1 1 calc R U . . .
C13 C 0.5645(4) 0.6132(4) 0.7461(4) 0.0304(9) Uani 1 1 d . . . . .
C14 C 0.4681(4) 0.6351(4) 0.8100(4) 0.0359(10) Uani 1 1 d . . . . .
H14 H 0.4778 0.6278 0.8780 0.043 Uiso 1 1 calc R U . . .
C15 C 0.3565(4) 0.6677(4) 0.7754(4) 0.0381(10) Uani 1 1 d . . . . .
H15 H 0.2913 0.6846 0.8187 0.046 Uiso 1 1 calc R U . . .
C16 C 0.3419(5) 0.6750(5) 0.6780(4) 0.0402(11) Uani 1 1 d . . . . .
H16 H 0.2668 0.6982 0.6533 0.048 Uiso 1 1 calc R U . . .
C17 C 0.6807(4) 0.5701(4) 0.7885(4) 0.0319(9) Uani 1 1 d . . . . .
C20 C 0.9593(4) 0.2985(3) 0.2388(3) 0.0258(8) Uani 1 1 d . . . . .
C21 C 0.9080(4) 0.1748(3) 0.3058(3) 0.0283(8) Uani 1 1 d . . . . .
C22 C 0.8941(4) 0.1264(3) 0.4170(3) 0.0280(8) Uani 1 1 d . . . . .
H22 H 0.9169 0.1703 0.4506 0.034 Uiso 1 1 calc R U . . .
C23 C 0.8464(5) 0.0129(4) 0.4784(4) 0.0376(10) Uani 1 1 d . . . . .
C24 C 0.8122(8) -0.0516(5) 0.4305(4) 0.068(2) Uani 1 1 d . . . . .
H24 H 0.7786 -0.1286 0.4729 0.081 Uiso 1 1 calc R U . . .
C25 C 0.8276(8) -0.0023(5) 0.3192(4) 0.068(2) Uani 1 1 d . . . . .
H25 H 0.8066 -0.0469 0.2855 0.082 Uiso 1 1 calc R U . . .
C26 C 0.8732(5) 0.1108(4) 0.2567(4) 0.0417(11) Uani 1 1 d . . . . .
H26 H 0.8806 0.1445 0.1810 0.050 Uiso 1 1 calc R U . . .
C27 C 0.8585(6) 0.0142(4) 0.6511(4) 0.0436(12) Uani 1 1 d . . . . .
H27 H 0.8916 0.0911 0.6230 0.052 Uiso 1 1 calc R U . . .
C28 C 0.7879(5) -0.1639(4) 0.7633(4) 0.0361(10) Uani 1 1 d . . . . .
H28 H 0.7626 -0.2322 0.8278 0.043 Uiso 1 1 calc R U . . .
C29 C 0.7889(5) -0.1505(4) 0.6635(4) 0.0352(10) Uani 1 1 d . . . . .
H29 H 0.7646 -0.2074 0.6445 0.042 Uiso 1 1 calc R U . . .
C30 C 0.8423(5) -0.0372(4) 0.8434(4) 0.0365(10) Uani 1 1 d . . . . .
C31 C 0.8405(5) 0.0743(4) 0.8313(3) 0.0364(10) Uani 1 1 d . . . . .
H31 H 0.8371 0.1360 0.7634 0.044 Uiso 1 1 calc R U . . .
C32 C 0.8438(4) 0.0948(4) 0.9198(4) 0.0323(9) Uani 1 1 d . . . . .
C33 C 0.8483(5) 0.0037(4) 1.0178(4) 0.0384(10) Uani 1 1 d . . . . .
H33 H 0.8465 0.0169 1.0790 0.046 Uiso 1 1 calc R U . . .
C34 C 0.8556(5) -0.1075(4) 1.0281(4) 0.0433(12) Uani 1 1 d . . . . .
H34 H 0.8617 -0.1691 1.0953 0.052 Uiso 1 1 calc R U . . .
C35 C 0.8538(5) -0.1280(4) 0.9398(4) 0.0387(10) Uani 1 1 d . . . . .
H35 H 0.8604 -0.2030 0.9456 0.046 Uiso 1 1 calc R U . . .
C36 C 0.8441(4) 0.2155(4) 0.9086(4) 0.0342(9) Uani 1 1 d . . . . .
O21 O 0.8686(3) 0.4411(3) -0.0667(3) 0.0328(7) Uani 1 1 d D . . . .
H21B H 0.849(5) 0.3644(19) -0.031(4) 0.049 Uiso 1 1 d D U . . .
H21A H 0.802(4) 0.481(4) -0.065(5) 0.049 Uiso 1 1 d D U . . .
O20 O 1.0154(5) 0.4971(6) 0.4011(5) 0.0338(14) Uani 0.5 1 d D . P . .
H20A H 1.013(12) 0.425(3) 0.441(8) 0.051 Uiso 0.5 1 d D U P . .
H20B H 1.034(10) 0.531(9) 0.437(8) 0.051 Uiso 0.5 1 d D U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.157(3) 2_765 ?
Mn1 O1 2.157(3) . ?
Mn1 O7 2.162(3) . ?
Mn1 O7 2.162(3) 2_765 ?
Mn1 O21 2.171(3) 2_765 ?
Mn1 O21 2.171(3) . ?
O1 C1 1.245(5) . ?
N1 C8 1.343(6) . ?
N1 C10 1.396(6) . ?
N1 C4 1.438(6) . ?
C1 O2 1.257(5) . ?
C1 C2 1.536(6) . ?
Mn2 O20 2.153(6) . ?
Mn2 O8 2.162(3) . ?
Mn2 O2 2.188(3) . ?
Mn2 O3 2.203(3) 2_766 ?
Mn2 O9 2.206(3) 2_766 ?
Mn2 O21 2.239(3) 2_765 ?
N2 C8 1.348(6) . ?
N2 C9 1.395(6) . ?
N2 C11 1.438(6) . ?
C2 C7 1.385(6) . ?
C2 C3 1.386(6) . ?
O3 C17 1.275(6) . ?
O3 Mn2 2.203(3) 2_766 ?
N3 C27 1.343(6) . ?
N3 C28 1.383(6) . ?
N3 C30 1.430(6) . ?
C3 C4 1.382(6) . ?
C3 H3 0.9500 . ?
O4 C17 1.250(6) . ?
N4 C27 1.341(6) . ?
N4 C29 1.389(5) . ?
N4 C23 1.436(6) . ?
C4 C5 1.378(6) . ?
C5 C6 1.390(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.391(6) . ?
C6 H6 0.9500 . ?
O7 C20 1.255(5) . ?
C7 H7 0.9500 . ?
O8 C20 1.250(5) . ?
C8 H8 0.9500 . ?
O9 C36 1.268(6) . ?
O9 Mn2 2.206(3) 2_766 ?
C9 C10 1.345(7) . ?
C9 H9 0.9500 . ?
O10 C36 1.240(6) . ?
C10 H10 0.9500 . ?
C11 C16 1.374(7) . ?
C11 C12 1.392(6) . ?
C12 C13 1.387(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(7) . ?
C13 C17 1.510(6) . ?
C14 C15 1.397(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(7) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C20 C21 1.518(6) . ?
C21 C26 1.391(6) . ?
C21 C22 1.392(6) . ?
C22 C23 1.394(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(7) . ?
C24 C25 1.392(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.342(7) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 C35 1.384(6) . ?
C30 C31 1.389(7) . ?
C31 C32 1.397(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.382(6) . ?
C32 C36 1.512(6) . ?
C33 C34 1.397(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.390(7) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
O21 Mn2 2.239(3) 2_765 ?
O21 H21B 0.91(2) . ?
O21 H21A 0.90(2) . ?
O20 H20A 0.86(2) . ?
O20 H20B 0.86(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 Mn1 O1 180.0 2_765 . ?
O1 Mn1 O7 85.16(13) 2_765 . ?
O1 Mn1 O7 94.84(13) . . ?
O1 Mn1 O7 94.84(13) 2_765 2_765 ?
O1 Mn1 O7 85.16(13) . 2_765 ?
O7 Mn1 O7 180.0 . 2_765 ?
O1 Mn1 O21 88.57(13) 2_765 2_765 ?
O1 Mn1 O21 91.43(13) . 2_765 ?
O7 Mn1 O21 90.33(13) . 2_765 ?
O7 Mn1 O21 89.67(13) 2_765 2_765 ?
O1 Mn1 O21 91.43(13) 2_765 . ?
O1 Mn1 O21 88.57(13) . . ?
O7 Mn1 O21 89.67(13) . . ?
O7 Mn1 O21 90.33(13) 2_765 . ?
O21 Mn1 O21 180.0 2_765 . ?
C1 O1 Mn1 140.9(3) . . ?
C8 N1 C10 109.6(4) . . ?
C8 N1 C4 124.8(4) . . ?
C10 N1 C4 125.6(4) . . ?
O1 C1 O2 127.9(4) . . ?
O1 C1 C2 115.7(4) . . ?
O2 C1 C2 116.5(4) . . ?
O20 Mn2 O8 88.6(2) . . ?
O20 Mn2 O2 89.97(18) . . ?
O8 Mn2 O2 88.09(13) . . ?
O20 Mn2 O3 86.69(18) . 2_766 ?
O8 Mn2 O3 89.51(13) . 2_766 ?
O2 Mn2 O3 175.93(12) . 2_766 ?
O20 Mn2 O9 90.4(2) . 2_766 ?
O8 Mn2 O9 177.42(12) . 2_766 ?
O2 Mn2 O9 89.56(12) . 2_766 ?
O3 Mn2 O9 92.78(12) 2_766 2_766 ?
O20 Mn2 O21 171.46(17) . 2_765 ?
O8 Mn2 O21 95.26(12) . 2_765 ?
O2 Mn2 O21 97.76(12) . 2_765 ?
O3 Mn2 O21 85.73(12) 2_766 2_765 ?
O9 Mn2 O21 86.10(13) 2_766 2_765 ?
C1 O2 Mn2 129.0(3) . . ?
C8 N2 C9 108.5(4) . . ?
C8 N2 C11 125.7(4) . . ?
C9 N2 C11 125.8(4) . . ?
C7 C2 C3 119.9(4) . . ?
C7 C2 C1 120.5(4) . . ?
C3 C2 C1 119.6(4) . . ?
C17 O3 Mn2 128.3(3) . 2_766 ?
C27 N3 C28 108.1(4) . . ?
C27 N3 C30 125.9(4) . . ?
C28 N3 C30 126.0(4) . . ?
C4 C3 C2 118.8(4) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C27 N4 C29 108.0(4) . . ?
C27 N4 C23 126.2(4) . . ?
C29 N4 C23 125.8(4) . . ?
C5 C4 C3 122.6(4) . . ?
C5 C4 N1 118.8(4) . . ?
C3 C4 N1 118.5(4) . . ?
C4 C5 C6 117.8(4) . . ?
C4 C5 H5 121.1 . . ?
C6 C5 H5 121.1 . . ?
C5 C6 C7 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C20 O7 Mn1 136.5(3) . . ?
C2 C7 C6 120.1(4) . . ?
C2 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C20 O8 Mn2 133.0(3) . . ?
N1 C8 N2 107.6(4) . . ?
N1 C8 H8 126.2 . . ?
N2 C8 H8 126.2 . . ?
C36 O9 Mn2 128.5(3) . 2_766 ?
C10 C9 N2 108.0(5) . . ?
C10 C9 H9 126.0 . . ?
N2 C9 H9 126.0 . . ?
C9 C10 N1 106.4(4) . . ?
C9 C10 H10 126.8 . . ?
N1 C10 H10 126.8 . . ?
C16 C11 C12 121.6(4) . . ?
C16 C11 N2 118.8(4) . . ?
C12 C11 N2 119.4(4) . . ?
C13 C12 C11 118.6(4) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
C14 C13 C12 120.0(4) . . ?
C14 C13 C17 119.5(4) . . ?
C12 C13 C17 120.1(4) . . ?
C13 C14 C15 120.6(4) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C16 C15 C14 119.4(4) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C11 C16 C15 119.7(5) . . ?
C11 C16 H16 120.1 . . ?
C15 C16 H16 120.1 . . ?
O4 C17 O3 125.8(4) . . ?
O4 C17 C13 117.2(4) . . ?
O3 C17 C13 117.1(4) . . ?
O8 C20 O7 127.2(4) . . ?
O8 C20 C21 117.0(4) . . ?
O7 C20 C21 115.8(4) . . ?
C26 C21 C22 120.3(4) . . ?
C26 C21 C20 120.3(4) . . ?
C22 C21 C20 119.5(4) . . ?
C21 C22 C23 119.3(4) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C24 C23 C22 120.9(4) . . ?
C24 C23 N4 119.3(4) . . ?
C22 C23 N4 119.8(4) . . ?
C23 C24 C25 119.1(5) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C26 C25 C24 120.9(5) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C25 C26 C21 119.4(4) . . ?
C25 C26 H26 120.3 . . ?
C21 C26 H26 120.3 . . ?
N4 C27 N3 108.6(4) . . ?
N4 C27 H27 125.7 . . ?
N3 C27 H27 125.7 . . ?
C29 C28 N3 107.7(4) . . ?
C29 C28 H28 126.1 . . ?
N3 C28 H28 126.1 . . ?
C28 C29 N4 107.5(4) . . ?
C28 C29 H29 126.3 . . ?
N4 C29 H29 126.3 . . ?
C35 C30 C31 121.5(4) . . ?
C35 C30 N3 118.5(4) . . ?
C31 C30 N3 120.0(4) . . ?
C30 C31 C32 119.4(4) . . ?
C30 C31 H31 120.3 . . ?
C32 C31 H31 120.3 . . ?
C33 C32 C31 119.4(4) . . ?
C33 C32 C36 120.1(4) . . ?
C31 C32 C36 120.5(4) . . ?
C32 C33 C34 120.8(4) . . ?
C32 C33 H33 119.6 . . ?
C34 C33 H33 119.6 . . ?
C35 C34 C33 119.9(4) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C30 C35 C34 119.0(4) . . ?
C30 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
O10 C36 O9 126.3(4) . . ?
O10 C36 C32 117.0(4) . . ?
O9 C36 C32 116.6(4) . . ?
Mn1 O21 Mn2 112.50(14) . 2_765 ?
Mn1 O21 H21B 113(4) . . ?
Mn2 O21 H21B 105(4) 2_765 . ?
Mn1 O21 H21A 106(4) . . ?
Mn2 O21 H21A 109(4) 2_765 . ?
H21B O21 H21A 112(5) . . ?
Mn2 O20 H20A 108(8) . . ?
Mn2 O20 H20B 136(8) . . ?
H20A O20 H20B 107(10) . . ?

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 O2 12.5(8) . . . . ?
Mn1 O1 C1 C2 -167.2(3) . . . . ?
O1 C1 O2 Mn2 -3.8(7) . . . . ?
C2 C1 O2 Mn2 175.8(3) . . . . ?
O1 C1 C2 C7 -7.4(6) . . . . ?
O2 C1 C2 C7 172.9(4) . . . . ?
O1 C1 C2 C3 169.9(4) . . . . ?
O2 C1 C2 C3 -9.9(6) . . . . ?
C7 C2 C3 C4 0.3(7) . . . . ?
C1 C2 C3 C4 -176.9(4) . . . . ?
C2 C3 C4 C5 -3.0(8) . . . . ?
C2 C3 C4 N1 173.5(4) . . . . ?
C8 N1 C4 C5 -151.9(5) . . . . ?
C10 N1 C4 C5 31.2(7) . . . . ?
C8 N1 C4 C3 31.5(7) . . . . ?
C10 N1 C4 C3 -145.4(5) . . . . ?
C3 C4 C5 C6 3.3(7) . . . . ?
N1 C4 C5 C6 -173.2(4) . . . . ?
C4 C5 C6 C7 -1.1(7) . . . . ?
C3 C2 C7 C6 1.8(7) . . . . ?
C1 C2 C7 C6 179.0(4) . . . . ?
C5 C6 C7 C2 -1.4(7) . . . . ?
C10 N1 C8 N2 0.0(6) . . . . ?
C4 N1 C8 N2 -177.3(4) . . . . ?
C9 N2 C8 N1 -1.1(6) . . . . ?
C11 N2 C8 N1 177.4(4) . . . . ?
C8 N2 C9 C10 1.8(6) . . . . ?
C11 N2 C9 C10 -176.7(5) . . . . ?
N2 C9 C10 N1 -1.7(6) . . . . ?
C8 N1 C10 C9 1.1(6) . . . . ?
C4 N1 C10 C9 178.4(5) . . . . ?
C8 N2 C11 C16 151.5(5) . . . . ?
C9 N2 C11 C16 -30.2(8) . . . . ?
C8 N2 C11 C12 -33.5(7) . . . . ?
C9 N2 C11 C12 144.7(5) . . . . ?
C16 C11 C12 C13 2.0(8) . . . . ?
N2 C11 C12 C13 -172.9(4) . . . . ?
C11 C12 C13 C14 0.7(7) . . . . ?
C11 C12 C13 C17 173.8(4) . . . . ?
C12 C13 C14 C15 -2.5(7) . . . . ?
C17 C13 C14 C15 -175.7(4) . . . . ?
C13 C14 C15 C16 1.7(8) . . . . ?
C12 C11 C16 C15 -2.8(8) . . . . ?
N2 C11 C16 C15 172.1(5) . . . . ?
C14 C15 C16 C11 0.9(8) . . . . ?
Mn2 O3 C17 O4 -0.9(7) 2_766 . . . ?
Mn2 O3 C17 C13 179.1(3) 2_766 . . . ?
C14 C13 C17 O4 -7.5(6) . . . . ?
C12 C13 C17 O4 179.3(4) . . . . ?
C14 C13 C17 O3 172.5(4) . . . . ?
C12 C13 C17 O3 -0.7(6) . . . . ?
Mn2 O8 C20 O7 -0.8(7) . . . . ?
Mn2 O8 C20 C21 179.0(3) . . . . ?
Mn1 O7 C20 O8 -17.1(7) . . . . ?
Mn1 O7 C20 C21 163.2(3) . . . . ?
O8 C20 C21 C26 176.5(4) . . . . ?
O7 C20 C21 C26 -3.7(6) . . . . ?
O8 C20 C21 C22 -2.5(6) . . . . ?
O7 C20 C21 C22 177.4(4) . . . . ?
C26 C21 C22 C23 0.7(7) . . . . ?
C20 C21 C22 C23 179.7(4) . . . . ?
C21 C22 C23 C24 -0.4(8) . . . . ?
C21 C22 C23 N4 179.7(4) . . . . ?
C27 N4 C23 C24 -178.4(6) . . . . ?
C29 N4 C23 C24 1.8(8) . . . . ?
C27 N4 C23 C22 1.5(8) . . . . ?
C29 N4 C23 C22 -178.3(4) . . . . ?
C22 C23 C24 C25 0.9(11) . . . . ?
N4 C23 C24 C25 -179.2(6) . . . . ?
C23 C24 C25 C26 -1.8(12) . . . . ?
C24 C25 C26 C21 2.2(11) . . . . ?
C22 C21 C26 C25 -1.7(8) . . . . ?
C20 C21 C26 C25 179.4(5) . . . . ?
C29 N4 C27 N3 -1.6(6) . . . . ?
C23 N4 C27 N3 178.6(5) . . . . ?
C28 N3 C27 N4 1.6(6) . . . . ?
C30 N3 C27 N4 -178.5(5) . . . . ?
C27 N3 C28 C29 -0.9(6) . . . . ?
C30 N3 C28 C29 179.1(5) . . . . ?
N3 C28 C29 N4 -0.1(6) . . . . ?
C27 N4 C29 C28 1.0(6) . . . . ?
C23 N4 C29 C28 -179.2(5) . . . . ?
C27 N3 C30 C35 -156.6(5) . . . . ?
C28 N3 C30 C35 23.3(8) . . . . ?
C27 N3 C30 C31 24.2(8) . . . . ?
C28 N3 C30 C31 -155.9(5) . . . . ?
C35 C30 C31 C32 -3.4(8) . . . . ?
N3 C30 C31 C32 175.7(5) . . . . ?
C30 C31 C32 C33 -0.3(7) . . . . ?
C30 C31 C32 C36 179.0(5) . . . . ?
C31 C32 C33 C34 3.1(8) . . . . ?
C36 C32 C33 C34 -176.2(5) . . . . ?
C32 C33 C34 C35 -2.3(8) . . . . ?
C31 C30 C35 C34 4.2(8) . . . . ?
N3 C30 C35 C34 -174.9(5) . . . . ?
C33 C34 C35 C30 -1.3(8) . . . . ?
Mn2 O9 C36 O10 19.5(7) 2_766 . . . ?
Mn2 O9 C36 C32 -159.2(3) 2_766 . . . ?
C33 C32 C36 O10 -17.7(7) . . . . ?
C31 C32 C36 O10 163.0(5) . . . . ?
C33 C32 C36 O9 161.1(4) . . . . ?
C31 C32 C36 O9 -18.2(7) . . . . ?

_refine_diff_density_max         2.915
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.125

_shelxl_version_number           2014/6


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 0.130 0.281 0.622 42 20 ' '
2 0.500 0.000 0.828 300 90 ' '
3 0.870 0.719 0.379 42 19 ' '

_platon_squeeze_details          
;
In order to subtract the contribution from the disordered 
solvent molecules and anions not located in the 
difference map, the SQUEEZE command was applied, which 
gave a new HKL file. The number of located electrons is 
129, is included in the formula, formula weight, calculated 
density, and F(000). These residual electron density 
were assigned to the 2 NO3 anions and approx 1.5 DMF 
molecules per unit cell. 
This value calculated based upon electrons analysis. 
(One DMF molecules would give 40 e; one NO3- anion would
give 32 e). 
;

# start Validation Reply Form
_vrf_DIFMX01_5Mn                 
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: The electron density maxima is likely due to unresolvale
solvent or anion electron density corresponding to hydrogen bonded solvate
water molecules or possibly an unresolved anion position.  While the
SQUEEZE routine of Platon was applied to the data this region of electon
density could not be accounted for due to its proximity to the 
imidazolium group.
;
_vrf_CHEMW03_5Mn                 
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: The nitrate anions could not be located in the structure
but are included in the formula. Also, the formula contains 1.5
DMF molecules per formula unit to account for electron density
removed by the SQUEEZE routine.
;
_vrf_PLAT029_5Mn                 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.925 Note  
RESPONSE: Data was collected on the MX1 beamline at the
Australian Synchrotron, where only phi rotation was available for data
collection. Due to the low symmetry, removal and remounting was
considered but, like many materials of this type, the crystals do not 
respond well to abrupt temperature changes and remounting.
;
_vrf_PLAT097_5Mn                 
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       2.91 eA-3  
RESPONSE: As above.
;
_vrf_PLAT420_5Mn                 
;
PROBLEM: D-H Without Acceptor      *O20    -- *H20A   ...     Please Check 
RESPONSE: This was a partially occupied coordinated water molecule.  There
is electron density adjacent this hydrogen but it could not be refined to 
give a chemically sensible model.
;
# 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-Cu
_database_code_depnum_ccdc_archive 'CCDC 1475108'
_audit_update_record             
;
2016-08-15 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72.25 H50.25 Br1.20 Cu1.20 N10.55 O26.15 Zn4'
_chemical_formula_weight         1918.20

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'
Br Br -0.3820 2.4670 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3280 1.2650 '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 0.2910 1.4480 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   20.889(4)
_cell_length_b                   18.004(4)
_cell_length_c                   10.913(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.36(3)
_cell_angle_gamma                90
_cell_volume                     4103.1(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5725
_cell_measurement_theta_min      0.71
_cell_measurement_theta_max      13.64

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_F_000             1927
_exptl_transmission_factor_min   0.619
_exptl_transmission_factor_max   0.676
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.124
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7108
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41452
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.493
_diffrn_reflns_theta_max         30.085
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measured_fraction_theta_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_point_group_measured_fraction_full 0.938
_reflns_number_total             5725
_reflns_number_gt                5509
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1053P)²+54.0311P] 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_number_reflns         5725
_refine_ls_number_parameters     275
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0760
_refine_ls_wR_factor_ref         0.2127
_refine_ls_wR_factor_gt          0.2121
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.057
_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
Br1 Br 0.68714(9) 0.5000 0.3356(3) 0.0610(6) Uani 0.5 2 d S T P A 1
Zn01 Zn 0.75490(2) 0.66837(2) -0.02248(4) 0.01067(15) Uani 1 1 d . . . . .
Cu1 Cu 0.58943(7) 0.5000 0.24437(19) 0.0295(4) Uani 0.5 2 d S T P A 1
N1 N 0.46493(15) 0.55980(18) 0.1669(4) 0.0184(6) Uani 1 1 d . . . . .
C2 C 0.5035(3) 0.5000 0.1834(6) 0.0202(11) Uani 0.5 2 d S T P A 1
C2B C 0.5035(3) 0.5000 0.1834(6) 0.0202(11) Uani 0.5 2 d S T P A 2
H2B H 0.5481 0.5000 0.2024 0.024 Uiso 0.5 2 calc R U P A 2
C5 C 0.40193(18) 0.5373(2) 0.1418(5) 0.0229(8) Uani 1 1 d . . . . .
H5 H 0.3660 0.5688 0.1274 0.027 Uiso 1 1 calc R U . . .
C11 C 0.48735(18) 0.6349(2) 0.1707(4) 0.0173(7) Uani 1 1 d . . . . .
C12 C 0.54754(17) 0.6505(2) 0.1267(4) 0.0168(7) Uani 1 1 d . . . . .
H12 H 0.5735 0.6118 0.0960 0.020 Uiso 1 1 calc R U . . .
C13 C 0.56969(17) 0.7234(2) 0.1278(4) 0.0156(7) Uani 1 1 d . . . . .
C14 C 0.53152(18) 0.7800(2) 0.1736(4) 0.0202(8) Uani 1 1 d . . . . .
H14 H 0.5464 0.8298 0.1739 0.024 Uiso 1 1 calc R U . . .
C15 C 0.4714(2) 0.7629(2) 0.2188(5) 0.0234(8) Uani 1 1 d . . . . .
H15 H 0.4456 0.8014 0.2510 0.028 Uiso 1 1 calc R U . . .
C16 C 0.44877(18) 0.6903(2) 0.2174(4) 0.0207(8) Uani 1 1 d . . . . .
H16 H 0.4077 0.6789 0.2478 0.025 Uiso 1 1 calc R U . . .
C17 C 0.63506(17) 0.7386(2) 0.0779(4) 0.0151(6) Uani 1 1 d . . . . .
O18 O 0.66353(13) 0.68352(17) 0.0335(3) 0.0198(6) Uani 1 1 d . . . . .
O19 O 0.65608(13) 0.80402(16) 0.0845(3) 0.0190(6) Uani 1 1 d . . . . .
N21 N 0.81694(18) 0.56004(19) 0.5558(3) 0.0197(7) Uani 1 1 d . . . . .
C22 C 0.8319(3) 0.5000 0.4894(6) 0.0200(10) Uani 1 2 d S T P . .
H22 H 0.8498 0.5000 0.4101 0.024 Uiso 1 2 calc R U P B 1
C25 C 0.7915(2) 0.5376(2) 0.6670(4) 0.0260(9) Uani 1 1 d . . . . .
H25 H 0.7769 0.5690 0.7305 0.031 Uiso 1 1 calc R U . . .
C31 C 0.82276(19) 0.6350(2) 0.5148(4) 0.0180(7) Uani 1 1 d . . . . .
C32 C 0.80785(18) 0.6512(2) 0.3936(4) 0.0178(7) Uani 1 1 d . . . . .
H32 H 0.7962 0.6126 0.3380 0.021 Uiso 1 1 calc R U . . .
C33 C 0.81011(17) 0.7247(2) 0.3542(4) 0.0159(7) Uani 1 1 d . . . . .
C34 C 0.82722(18) 0.7810(2) 0.4371(4) 0.0177(7) Uani 1 1 d . . . . .
H34 H 0.8276 0.8313 0.4107 0.021 Uiso 1 1 calc R U . . .
C35 C 0.8436(2) 0.7635(2) 0.5579(4) 0.0203(7) Uani 1 1 d . . . . .
H35 H 0.8563 0.8018 0.6132 0.024 Uiso 1 1 calc R U . . .
C36 C 0.84146(19) 0.6901(2) 0.5984(4) 0.0188(7) Uani 1 1 d . . . . .
H36 H 0.8525 0.6778 0.6809 0.023 Uiso 1 1 calc R U . . .
C37 C 0.79044(17) 0.7417(2) 0.2239(3) 0.0155(6) Uani 1 1 d . . . . .
O38 O 0.78581(15) 0.68706(18) 0.1521(3) 0.0214(6) Uani 1 1 d . . . . .
O39 O 0.77950(14) 0.80885(17) 0.1965(3) 0.0199(6) Uani 1 1 d . . . . .
O40 O 0.75675(15) 0.56070(15) -0.0522(3) 0.0203(6) Uani 1 1 d . . . . .
C41 C 0.7549(3) 0.5000 0.0001(6) 0.0191(10) Uani 1 2 d S T P . .
H41 H 0.7518 0.5000 0.0868 0.023 Uiso 1 2 calc R U P . .
N50 N 0.9092(3) 0.5000 0.0542(6) 0.0240(11) Uani 0.9 2 d DS T P C 1
O51 O 0.9085(4) 0.5000 -0.0717(9) 0.080(3) Uani 0.9 2 d DS T P C 1
O52 O 0.9101(6) 0.5663(5) 0.1175(11) 0.135(5) Uani 0.9 1 d D U P C 1
Cu2 Cu 0.8577(6) 0.5000 0.3154(12) 0.048(3) Uani 0.1 2 d S T P D 2
Br2 Br 0.8816 0.5000 0.1217 0.070 Uani 0.1 2 d S T P D 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
Br1 Cu1 2.249(2) . ?
Zn01 O40 1.966(3) . ?
Zn01 O38 2.025(3) . ?
Zn01 O18 2.036(3) . ?
Zn01 O19 2.055(3) 7_665 ?
Zn01 O39 2.056(3) 7_665 ?
Zn01 Zn01 2.9876(10) 7_665 ?
Cu1 C2 1.900(6) . ?
N1 C2B 1.354(5) . ?
N1 C2 1.354(5) . ?
N1 C5 1.398(5) . ?
N1 C11 1.431(5) . ?
C2 N1 1.354(5) 6_565 ?
C2B N1 1.354(5) 6_565 ?
C2B H2B 0.9500 . ?
C5 C5 1.344(8) 6_565 ?
C5 H5 0.9500 . ?
C11 C12 1.385(5) . ?
C11 C16 1.387(5) . ?
C12 C13 1.391(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.393(5) . ?
C13 C17 1.507(5) . ?
C14 C15 1.395(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(6) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 O19 1.258(5) . ?
C17 O18 1.259(5) . ?
O19 Zn01 2.055(3) 7_665 ?
N21 C22 1.343(5) . ?
N21 C25 1.396(6) . ?
N21 C31 1.429(5) . ?
C22 N21 1.343(5) 6_565 ?
C22 Cu2 1.986(14) . ?
C22 H22 0.9500 . ?
C25 C25 1.353(9) 6_565 ?
C25 H25 0.9500 . ?
C31 C32 1.382(6) . ?
C31 C36 1.396(5) . ?
C32 C33 1.393(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.400(5) . ?
C33 C37 1.502(5) . ?
C34 C35 1.390(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.395(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 O38 1.260(5) . ?
C37 O39 1.264(5) . ?
O39 Zn01 2.056(3) 7_665 ?
O40 C41 1.234(4) . ?
C41 O40 1.234(4) 6_565 ?
C41 H41 0.9500 . ?
N50 O51 1.373(11) . ?
N50 O52 1.379(8) . ?
N50 O52 1.379(8) 6_565 ?
Cu2 Br2 2.183(13) . ?

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
O40 Zn01 O38 108.18(14) . . ?
O40 Zn01 O18 101.76(13) . . ?
O38 Zn01 O18 88.62(13) . . ?
O40 Zn01 O19 99.36(12) . 7_665 ?
O38 Zn01 O19 89.92(13) . 7_665 ?
O18 Zn01 O19 158.19(12) . 7_665 ?
O40 Zn01 O39 92.98(13) . 7_665 ?
O38 Zn01 O39 158.83(13) . 7_665 ?
O18 Zn01 O39 86.59(13) . 7_665 ?
O19 Zn01 O39 86.95(12) 7_665 7_665 ?
O40 Zn01 Zn01 177.20(10) . 7_665 ?
O38 Zn01 Zn01 72.76(9) . 7_665 ?
O18 Zn01 Zn01 75.56(9) . 7_665 ?
O19 Zn01 Zn01 83.23(8) 7_665 7_665 ?
O39 Zn01 Zn01 86.08(9) 7_665 7_665 ?
C2 Cu1 Br1 174.3(2) . . ?
C2B N1 C5 110.5(3) . . ?
C2 N1 C5 110.5(3) . . ?
C2B N1 C11 123.7(3) . . ?
C2 N1 C11 123.7(3) . . ?
C5 N1 C11 125.8(3) . . ?
N1 C2 N1 105.4(5) . 6_565 ?
N1 C2 Cu1 126.9(2) . . ?
N1 C2 Cu1 126.9(2) 6_565 . ?
N1 C2B N1 105.4(5) . 6_565 ?
N1 C2B H2B 127.3 . . ?
N1 C2B H2B 127.3 6_565 . ?
C5 C5 N1 106.8(2) 6_565 . ?
C5 C5 H5 126.6 6_565 . ?
N1 C5 H5 126.6 . . ?
C12 C11 C16 121.4(4) . . ?
C12 C11 N1 118.8(3) . . ?
C16 C11 N1 119.9(3) . . ?
C11 C12 C13 119.6(4) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C14 119.9(3) . . ?
C12 C13 C17 118.2(3) . . ?
C14 C13 C17 121.9(3) . . ?
C13 C14 C15 119.6(4) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C16 C15 C14 120.8(4) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C11 C16 C15 118.7(4) . . ?
C11 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
O19 C17 O18 126.3(4) . . ?
O19 C17 C13 117.8(3) . . ?
O18 C17 C13 115.9(3) . . ?
C17 O18 Zn01 132.5(3) . . ?
C17 O19 Zn01 121.7(3) . 7_665 ?
C22 N21 C25 109.5(4) . . ?
C22 N21 C31 124.7(4) . . ?
C25 N21 C31 125.7(4) . . ?
N21 C22 N21 107.3(5) . 6_565 ?
N21 C22 Cu2 126.0(3) . . ?
N21 C22 Cu2 126.0(3) 6_565 . ?
N21 C22 H22 126.4 . . ?
N21 C22 H22 126.4 6_565 . ?
C25 C25 N21 106.8(2) 6_565 . ?
C25 C25 H25 126.6 6_565 . ?
N21 C25 H25 126.6 . . ?
C32 C31 C36 121.9(4) . . ?
C32 C31 N21 118.6(4) . . ?
C36 C31 N21 119.4(4) . . ?
C31 C32 C33 119.1(4) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C32 C33 C34 119.9(4) . . ?
C32 C33 C37 118.4(3) . . ?
C34 C33 C37 121.6(3) . . ?
C35 C34 C33 120.1(4) . . ?
C35 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C34 C35 C36 120.4(4) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C35 C36 C31 118.4(4) . . ?
C35 C36 H36 120.8 . . ?
C31 C36 H36 120.8 . . ?
O38 C37 O39 126.1(4) . . ?
O38 C37 C33 116.4(3) . . ?
O39 C37 C33 117.6(3) . . ?
C37 O38 Zn01 137.1(3) . . ?
C37 O39 Zn01 117.8(3) . 7_665 ?
C41 O40 Zn01 142.8(4) . . ?
O40 C41 O40 124.7(6) 6_565 . ?
O40 C41 H41 117.7 6_565 . ?
O40 C41 H41 117.7 . . ?
O51 N50 O52 120.1(6) . . ?
O51 N50 O52 120.0(6) . 6_565 ?
O52 N50 O52 119.9(12) . 6_565 ?
C22 Cu2 Br2 177.4(8) . . ?

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
C5 N1 C2 N1 0.8(7) . . . 6_565 ?
C11 N1 C2 N1 -177.0(3) . . . 6_565 ?
C5 N1 C2 Cu1 -169.3(4) . . . . ?
C11 N1 C2 Cu1 12.8(8) . . . . ?
C5 N1 C2B N1 0.8(7) . . . 6_565 ?
C11 N1 C2B N1 -177.0(3) . . . 6_565 ?
C2B N1 C5 C5 -0.5(4) . . . 6_565 ?
C2 N1 C5 C5 -0.5(4) . . . 6_565 ?
C11 N1 C5 C5 177.3(3) . . . 6_565 ?
C2B N1 C11 C12 34.6(7) . . . . ?
C2 N1 C11 C12 34.6(7) . . . . ?
C5 N1 C11 C12 -142.9(4) . . . . ?
C2B N1 C11 C16 -145.7(5) . . . . ?
C2 N1 C11 C16 -145.7(5) . . . . ?
C5 N1 C11 C16 36.7(6) . . . . ?
C16 C11 C12 C13 -0.8(6) . . . . ?
N1 C11 C12 C13 178.9(4) . . . . ?
C11 C12 C13 C14 0.3(6) . . . . ?
C11 C12 C13 C17 -179.3(4) . . . . ?
C12 C13 C14 C15 0.4(7) . . . . ?
C17 C13 C14 C15 -179.9(4) . . . . ?
C13 C14 C15 C16 -0.8(7) . . . . ?
C12 C11 C16 C15 0.4(7) . . . . ?
N1 C11 C16 C15 -179.3(4) . . . . ?
C14 C15 C16 C11 0.4(7) . . . . ?
C12 C13 C17 O19 -176.7(4) . . . . ?
C14 C13 C17 O19 3.6(6) . . . . ?
C12 C13 C17 O18 3.2(5) . . . . ?
C14 C13 C17 O18 -176.5(4) . . . . ?
O19 C17 O18 Zn01 10.0(7) . . . . ?
C13 C17 O18 Zn01 -169.9(3) . . . . ?
O18 C17 O19 Zn01 -0.9(6) . . . 7_665 ?
C13 C17 O19 Zn01 178.9(3) . . . 7_665 ?
C25 N21 C22 N21 -0.3(7) . . . 6_565 ?
C31 N21 C22 N21 -176.8(3) . . . 6_565 ?
C25 N21 C22 Cu2 170.5(6) . . . . ?
C31 N21 C22 Cu2 -5.9(9) . . . . ?
C22 N21 C25 C25 0.2(4) . . . 6_565 ?
C31 N21 C25 C25 176.7(3) . . . 6_565 ?
C22 N21 C31 C32 37.8(6) . . . . ?
C25 N21 C31 C32 -138.1(4) . . . . ?
C22 N21 C31 C36 -144.0(5) . . . . ?
C25 N21 C31 C36 40.1(6) . . . . ?
C36 C31 C32 C33 -1.5(6) . . . . ?
N21 C31 C32 C33 176.7(4) . . . . ?
C31 C32 C33 C34 -0.1(6) . . . . ?
C31 C32 C33 C37 -176.8(3) . . . . ?
C32 C33 C34 C35 1.7(6) . . . . ?
C37 C33 C34 C35 178.3(3) . . . . ?
C33 C34 C35 C36 -1.8(6) . . . . ?
C34 C35 C36 C31 0.2(6) . . . . ?
C32 C31 C36 C35 1.4(6) . . . . ?
N21 C31 C36 C35 -176.7(4) . . . . ?
C32 C33 C37 O38 -14.2(5) . . . . ?
C34 C33 C37 O38 169.2(4) . . . . ?
C32 C33 C37 O39 165.2(4) . . . . ?
C34 C33 C37 O39 -11.5(5) . . . . ?
O39 C37 O38 Zn01 -6.5(7) . . . . ?
C33 C37 O38 Zn01 172.8(3) . . . . ?
O38 C37 O39 Zn01 4.4(5) . . . 7_665 ?
C33 C37 O39 Zn01 -174.8(2) . . . 7_665 ?
Zn01 O40 C41 O40 179.21(17) . . . 6_565 ?

_refine_diff_density_max         4.567
_refine_diff_density_min         -4.015
_refine_diff_density_rms         0.179

_shelxl_version_number           2014/6


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 0.500 -0.014 0.500 342 30 ' '
2 0.000 0.448 0.500 342 30 ' '
_platon_squeeze_details          
;
In order to subtract the contribution from the disordered 
solvent molecules, the SQUEEZE command was applied, which 
gave a new HKL file. The number of located electrons is 60, 
is included in the formula, formula weight, calculated 
density, and F(000). These residual electron density 
were assigned to approx 1.5 DMF molecules per unit cell. 
This value calculated based upon electrons analysis. 
(One DMF molecules would give 40 e). 
;

# start Validation Reply Form
_vrf_CHEMW03_1-Cu                
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The formula includes 0.75 DMF molecules per formula
unit to account for the electron density removed by SQUEEZE.
;
_vrf_DIFMN02_1-Cu                
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*1.00
RESPONSE: Based on EDX/ICP-MS analysis Cu(I) metalation of the 
parent MOF structure is around 50% overall.  In the structure the 
prominent metalation site is at C2 but a minor site also occurs
at the C22 position.  Metalation of the C22 imidazolium position 
was observed with low occupancy of the Cu and Br positions, 
approximately 10%. Also seen present in this position is a 
nitrate anion that exists, based on chemical sensibility, 
only when there is no metalation in the structure. 
We suspect that when C22 is not metalated, but 
C2 is, a DMF molecule also exists in the same area. However, this
was unable to be modeled and refined due to the existance of a
number of molecules in this site. The unacounted electron density 
arises from this DMF and some disorder of the CuBr moiety.
;
_vrf_DIFMX01_1-Cu                
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00
RESPONSE: As above for minimum difference density.
;
_vrf_PLAT029_1-Cu                
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.938 Note  
RESPONSE: Data was collected on the MX1 beamline at the
Australian Synchrotron, where only phi rotation was available for data
collection. Due to the low symmetry, removal and remounting was
considered but, like many materials of this type, the crystals do not respond
well to abrupt temperature changes and remounting.
;
_vrf_PLAT097_1-Cu                
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       4.57 eA-3  
RESPONSE: As above for minimum difference density.
;
_vrf_PLAT098_1-Cu                
;
PROBLEM: Large Reported Min.  (Negative) Residual Density      -4.01 eA-3  
RESPONSE: As above for minimum difference density.
;
# 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_3Co
_database_code_depnum_ccdc_archive 'CCDC 1475109'
_audit_update_record             
;
2016-08-15 deposited with the CCDC.
2016-08-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C75.50 H69.50 Co3 N12.50 O28.50'
_chemical_formula_weight         1784.72

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 0.3490 0.9720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   23.128(5)
_cell_length_b                   14.043(3)
_cell_length_c                   23.412(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.37(3)
_cell_angle_gamma                90
_cell_volume                     7571(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9394
_cell_measurement_theta_max      23.31
_cell_measurement_theta_min      0.76

_exptl_crystal_description       'thin rod'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_F_000             3676
_exptl_transmission_factor_max   0.929
_exptl_transmission_factor_min   0.818
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.746
_shelx_estimated_absorpt_T_min   0.818
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.7108
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62700
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.699
_diffrn_reflns_theta_max         27.923
_diffrn_reflns_theta_full        27.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9027
_reflns_number_gt                8310
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0590P)²+21.1187P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9027
_refine_ls_number_parameters     500
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1199
_refine_ls_wR_factor_gt          0.1181
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.002
_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 0.7500 0.7500 0.5000 0.01619(9) Uani 1 2 d S . P . .
Co2 Co 0.77263(2) 0.49991(2) 0.51507(2) 0.01746(8) Uani 1 1 d . . . . .
O12 O 0.80350(6) 0.63941(10) 0.53006(6) 0.0204(3) Uani 1 1 d D . . . .
H12A H 0.8127(16) 0.634(3) 0.5689(16) 0.054(10) Uiso 1 1 d . . . . .
H12B H 0.8370(12) 0.635(3) 0.5103(16) 0.071(12) Uiso 1 1 d D . . . .
O8 O 0.69274(6) 0.52773(10) 0.54502(6) 0.0213(3) Uani 1 1 d . . . . .
O2 O 0.73873(7) 0.52942(10) 0.43105(6) 0.0229(3) Uani 1 1 d . . . . .
O13 O 0.74776(7) 0.36027(11) 0.50167(7) 0.0249(3) Uani 1 1 d D . . . .
H13A H 0.7499(17) 0.334(3) 0.4705(18) 0.067(12) Uiso 1 1 d . . . . .
H13B H 0.7182(15) 0.335(3) 0.5219(17) 0.085(14) Uiso 1 1 d D . . . .
O3 O 0.69632(7) 0.03939(11) 0.39856(6) 0.0269(3) Uani 1 1 d . . . . .
O9 O 0.64609(7) 0.03752(10) 0.51475(7) 0.0247(3) Uani 1 1 d . . . . .
O1 O 0.74135(9) 0.68861(11) 0.42048(6) 0.0355(4) Uani 1 1 d . . . . .
O4 O 0.67119(7) -0.10486(11) 0.36281(7) 0.0251(3) Uani 1 1 d . . . . .
O7 O 0.67613(7) 0.68158(11) 0.52315(8) 0.0321(4) Uani 1 1 d . . . . .
O10 O 0.61404(8) -0.11014(11) 0.52985(8) 0.0344(4) Uani 1 1 d . . . . .
O21 O 0.72518(9) 0.20753(14) 0.60658(8) 0.0397(4) Uani 1 1 d . . . . .
O22 O 0.65484(8) 0.28182(13) 0.55402(8) 0.0371(4) Uani 1 1 d . . . . .
N2 N 0.67509(11) 0.25413(13) 0.22123(8) 0.0319(5) Uani 1 1 d . . . . .
N6 N 0.48412(8) 0.24744(13) 0.58340(11) 0.0329(5) Uani 1 1 d . . . . .
N1 N 0.69032(11) 0.40566(14) 0.23112(8) 0.0336(5) Uani 1 1 d . . . . .
N10 N 0.67436(10) 0.23747(15) 0.59985(9) 0.0327(4) Uani 1 1 d . . . . .
C32 C 0.55704(9) 0.01758(15) 0.55679(9) 0.0214(4) Uani 1 1 d . . . . .
C20 C 0.66148(9) 0.60071(14) 0.53866(9) 0.0214(4) Uani 1 1 d . . . . .
C21 C 0.59906(10) 0.59096(15) 0.55204(11) 0.0280(5) Uani 1 1 d . . . . .
C1 C 0.73264(10) 0.60515(15) 0.40267(8) 0.0232(4) Uani 1 1 d . . . . .
C36 C 0.61007(9) -0.02066(15) 0.53170(9) 0.0226(4) Uani 1 1 d . . . . .
C12 C 0.67645(11) 0.12102(15) 0.28853(9) 0.0266(4) Uani 1 1 d . . . . .
H12 H 0.6927 0.1614 0.3184 0.032 Uiso 1 1 calc R U . . .
N5 N 0.49425(9) 0.40067(14) 0.58123(12) 0.0383(5) Uani 1 1 d . . . . .
C33 C 0.51906(10) -0.04548(15) 0.57968(10) 0.0256(4) Uani 1 1 d . . . . .
H33 H 0.5263 -0.1120 0.5785 0.031 Uiso 1 1 calc R U . . .
C31 C 0.54569(9) 0.11491(15) 0.55711(9) 0.0233(4) Uani 1 1 d . . . . .
H31 H 0.5707 0.1584 0.5405 0.028 Uiso 1 1 calc R U . . .
O20 O 0.63851(11) 0.2231(2) 0.63616(9) 0.0599(6) Uani 1 1 d . . . . .
C30 C 0.49725(9) 0.14742(15) 0.58210(11) 0.0269(4) Uani 1 1 d . . . . .
C17 C 0.67877(9) -0.01689(15) 0.35846(9) 0.0226(4) Uani 1 1 d . . . . .
C13 C 0.66535(11) 0.02566(16) 0.29922(9) 0.0284(5) Uani 1 1 d . . . . .
C22 C 0.57687(10) 0.50115(15) 0.56220(11) 0.0290(5) Uani 1 1 d . . . . .
H22 H 0.6008 0.4462 0.5615 0.035 Uiso 1 1 calc R U . . .
C3 C 0.71444(12) 0.50690(16) 0.31369(9) 0.0302(5) Uani 1 1 d . . . . .
H3 H 0.7287 0.4527 0.3348 0.036 Uiso 1 1 calc R U . . .
C2 C 0.71340(11) 0.59522(16) 0.33971(9) 0.0291(5) Uani 1 1 d . . . . .
C9 C 0.68551(12) 0.29018(17) 0.16794(9) 0.0321(5) Uani 1 1 d . . . . .
H9 H 0.6860 0.2548 0.1334 0.038 Uiso 1 1 calc R U . . .
C11 C 0.66336(12) 0.15602(16) 0.23338(9) 0.0305(5) Uani 1 1 d . . . . .
C4 C 0.69435(14) 0.49867(16) 0.25640(10) 0.0352(6) Uani 1 1 d . . . . .
C10 C 0.69478(12) 0.38421(17) 0.17409(9) 0.0323(5) Uani 1 1 d . . . . .
H10 H 0.7029 0.4277 0.1448 0.039 Uiso 1 1 calc R U . . .
C7 C 0.69491(13) 0.67504(17) 0.30761(10) 0.0362(6) Uani 1 1 d . . . . .
H7 H 0.6938 0.7356 0.3255 0.043 Uiso 1 1 calc R U . . .
C34 C 0.47083(11) -0.01217(17) 0.60424(13) 0.0348(5) Uani 1 1 d . . . . .
H34 H 0.4451 -0.0559 0.6198 0.042 Uiso 1 1 calc R U . . .
C27 C 0.52191(10) 0.31769(16) 0.57741(13) 0.0350(6) Uani 1 1 d . . . . .
H27 H 0.5617 0.3100 0.5715 0.042 Uiso 1 1 calc R U . . .
C8 C 0.67801(13) 0.32620(17) 0.25895(9) 0.0345(5) Uani 1 1 d . . . . .
H8 H 0.6723 0.3216 0.2985 0.041 Uiso 1 1 calc R U . . .
C26 C 0.56376(12) 0.67136(17) 0.55292(14) 0.0396(6) Uani 1 1 d . . . . .
H26 H 0.5791 0.7326 0.5461 0.048 Uiso 1 1 calc R U . . .
C35 C 0.45983(10) 0.08498(17) 0.60622(13) 0.0349(5) Uani 1 1 d . . . . .
H35 H 0.4273 0.1083 0.6238 0.042 Uiso 1 1 calc R U . . .
C23 C 0.51907(11) 0.49309(16) 0.57347(15) 0.0393(6) Uani 1 1 d . . . . .
C16 C 0.63993(15) 0.09842(18) 0.18872(10) 0.0426(7) Uani 1 1 d . . . . .
H16 H 0.6307 0.1240 0.1514 0.051 Uiso 1 1 calc R U . . .
C5 C 0.67664(15) 0.57681(18) 0.22337(11) 0.0450(7) Uani 1 1 d . . . . .
H5 H 0.6638 0.5697 0.1839 0.054 Uiso 1 1 calc R U . . .
C14 C 0.64307(14) -0.03317(18) 0.25456(11) 0.0429(7) Uani 1 1 d . . . . .
H14 H 0.6365 -0.0987 0.2617 0.052 Uiso 1 1 calc R U . . .
C28 C 0.43061(11) 0.28723(19) 0.59128(15) 0.0437(7) Uani 1 1 d . . . . .
H28 H 0.3958 0.2535 0.5963 0.052 Uiso 1 1 calc R U . . .
C6 C 0.67802(16) 0.66573(18) 0.24917(11) 0.0464(7) Uani 1 1 d . . . . .
H6 H 0.6674 0.7206 0.2269 0.056 Uiso 1 1 calc R U . . .
C25 C 0.50597(13) 0.66150(19) 0.56380(17) 0.0508(8) Uani 1 1 d . . . . .
H25 H 0.4818 0.7162 0.5639 0.061 Uiso 1 1 calc R U . . .
C29 C 0.43694(11) 0.38275(18) 0.59059(16) 0.0462(7) Uani 1 1 d . . . . .
H29 H 0.4078 0.4288 0.5955 0.055 Uiso 1 1 calc R U . . .
C15 C 0.63035(18) 0.00327(19) 0.19967(12) 0.0533(9) Uani 1 1 d . . . . .
H15 H 0.6150 -0.0374 0.1695 0.064 Uiso 1 1 calc R U . . .
C24 C 0.48326(12) 0.57256(19) 0.57445(18) 0.0530(9) Uani 1 1 d . . . . .
H24 H 0.4439 0.5660 0.5823 0.064 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.0444(16) . ?
Co1 O1 2.0444(16) 7_666 ?
Co1 O12 2.0676(15) . ?
Co1 O12 2.0676(15) 7_666 ?
Co1 O7 2.0758(16) . ?
Co1 O7 2.0759(16) 7_666 ?
Co2 O13 2.0594(16) . ?
Co2 O8 2.0738(16) . ?
Co2 O2 2.0897(15) . ?
Co2 O12 2.1032(15) . ?
Co2 O9 2.1315(16) 7_656 ?
Co2 O3 2.1535(16) 7_656 ?
O12 H12A 0.92(4) . ?
O12 H12B 0.942(19) . ?
O8 C20 1.255(3) . ?
O2 C1 1.255(3) . ?
O13 H13A 0.83(4) . ?
O13 H13B 0.937(19) . ?
O3 C17 1.265(3) . ?
O3 Co2 2.1535(16) 7_656 ?
O9 C36 1.257(3) . ?
O9 Co2 2.1315(16) 7_656 ?
O1 C1 1.254(3) . ?
O4 C17 1.253(3) . ?
O7 C20 1.249(2) . ?
O10 C36 1.261(3) . ?
O21 N10 1.244(3) . ?
O22 N10 1.285(3) . ?
N2 C8 1.341(3) . ?
N2 C9 1.388(3) . ?
N2 C11 1.438(3) . ?
N6 C27 1.334(3) . ?
N6 C28 1.386(3) . ?
N6 C30 1.438(3) . ?
N1 C8 1.336(3) . ?
N1 C10 1.382(3) . ?
N1 C4 1.433(3) . ?
N10 O20 1.258(3) . ?
C32 C33 1.390(3) . ?
C32 C31 1.392(3) . ?
C32 C36 1.508(3) . ?
C20 C21 1.512(3) . ?
C21 C22 1.391(3) . ?
C21 C26 1.395(3) . ?
C1 C2 1.506(3) . ?
C12 C11 1.388(3) . ?
C12 C13 1.391(3) . ?
C12 H12 0.9500 . ?
N5 C27 1.336(3) . ?
N5 C29 1.387(3) . ?
N5 C23 1.438(3) . ?
C33 C34 1.384(3) . ?
C33 H33 0.9500 . ?
C31 C30 1.389(3) . ?
C31 H31 0.9500 . ?
C30 C35 1.389(3) . ?
C17 C13 1.515(3) . ?
C13 C14 1.393(3) . ?
C22 C23 1.391(3) . ?
C22 H22 0.9500 . ?
C3 C4 1.382(3) . ?
C3 C2 1.383(3) . ?
C3 H3 0.9500 . ?
C2 C7 1.394(3) . ?
C9 C10 1.343(3) . ?
C9 H9 0.9500 . ?
C11 C16 1.391(3) . ?
C4 C5 1.382(3) . ?
C10 H10 0.9500 . ?
C7 C6 1.393(3) . ?
C7 H7 0.9500 . ?
C34 C35 1.389(3) . ?
C34 H34 0.9500 . ?
C27 H27 0.9500 . ?
C8 H8 0.9500 . ?
C26 C25 1.391(4) . ?
C26 H26 0.9500 . ?
C35 H35 0.9500 . ?
C23 C24 1.391(3) . ?
C16 C15 1.382(4) . ?
C16 H16 0.9500 . ?
C5 C6 1.386(4) . ?
C5 H5 0.9500 . ?
C14 C15 1.389(4) . ?
C14 H14 0.9500 . ?
C28 C29 1.350(4) . ?
C28 H28 0.9500 . ?
C6 H6 0.9500 . ?
C25 C24 1.387(4) . ?
C25 H25 0.9500 . ?
C29 H29 0.9500 . ?
C15 H15 0.9500 . ?
C24 H24 0.9500 . ?

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 Co1 O1 180.00(4) . 7_666 ?
O1 Co1 O12 89.86(7) . . ?
O1 Co1 O12 90.14(7) 7_666 . ?
O1 Co1 O12 90.14(7) . 7_666 ?
O1 Co1 O12 89.86(7) 7_666 7_666 ?
O12 Co1 O12 180.0 . 7_666 ?
O1 Co1 O7 91.71(8) . . ?
O1 Co1 O7 88.29(8) 7_666 . ?
O12 Co1 O7 92.55(6) . . ?
O12 Co1 O7 87.45(6) 7_666 . ?
O1 Co1 O7 88.29(8) . 7_666 ?
O1 Co1 O7 91.71(8) 7_666 7_666 ?
O12 Co1 O7 87.46(6) . 7_666 ?
O12 Co1 O7 92.55(6) 7_666 7_666 ?
O7 Co1 O7 180.00(7) . 7_666 ?
O13 Co2 O8 89.19(6) . . ?
O13 Co2 O2 88.32(6) . . ?
O8 Co2 O2 90.76(6) . . ?
O13 Co2 O12 176.33(6) . . ?
O8 Co2 O12 93.86(6) . . ?
O2 Co2 O12 93.67(6) . . ?
O13 Co2 O9 87.57(6) . 7_656 ?
O8 Co2 O9 176.56(6) . 7_656 ?
O2 Co2 O9 90.30(7) . 7_656 ?
O12 Co2 O9 89.33(6) . 7_656 ?
O13 Co2 O3 87.87(6) . 7_656 ?
O8 Co2 O3 87.72(7) . 7_656 ?
O2 Co2 O3 175.91(6) . 7_656 ?
O12 Co2 O3 90.22(6) . 7_656 ?
O9 Co2 O3 91.00(7) 7_656 7_656 ?
Co1 O12 Co2 117.38(7) . . ?
Co1 O12 H12A 119(2) . . ?
Co2 O12 H12A 97(2) . . ?
Co1 O12 H12B 112(2) . . ?
Co2 O12 H12B 98(2) . . ?
H12A O12 H12B 111(3) . . ?
C20 O8 Co2 129.45(13) . . ?
C1 O2 Co2 132.84(14) . . ?
Co2 O13 H13A 122(3) . . ?
Co2 O13 H13B 119(3) . . ?
H13A O13 H13B 112(4) . . ?
C17 O3 Co2 126.34(14) . 7_656 ?
C36 O9 Co2 125.02(14) . 7_656 ?
C1 O1 Co1 134.10(14) . . ?
C20 O7 Co1 138.51(15) . . ?
C8 N2 C9 108.33(19) . . ?
C8 N2 C11 126.28(19) . . ?
C9 N2 C11 125.39(18) . . ?
C27 N6 C28 108.5(2) . . ?
C27 N6 C30 125.3(2) . . ?
C28 N6 C30 126.13(19) . . ?
C8 N1 C10 109.13(19) . . ?
C8 N1 C4 124.62(19) . . ?
C10 N1 C4 126.1(2) . . ?
O21 N10 O20 122.3(2) . . ?
O21 N10 O22 121.5(2) . . ?
O20 N10 O22 116.1(2) . . ?
C33 C32 C31 119.8(2) . . ?
C33 C32 C36 119.33(19) . . ?
C31 C32 C36 120.84(18) . . ?
O7 C20 O8 127.5(2) . . ?
O7 C20 C21 115.65(19) . . ?
O8 C20 C21 116.88(18) . . ?
C22 C21 C26 120.4(2) . . ?
C22 C21 C20 119.5(2) . . ?
C26 C21 C20 120.1(2) . . ?
O1 C1 O2 127.56(19) . . ?
O1 C1 C2 115.82(18) . . ?
O2 C1 C2 116.61(18) . . ?
O9 C36 O10 125.7(2) . . ?
O9 C36 C32 118.60(18) . . ?
O10 C36 C32 115.65(18) . . ?
C11 C12 C13 118.7(2) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C27 N5 C29 108.8(2) . . ?
C27 N5 C23 125.4(2) . . ?
C29 N5 C23 125.6(2) . . ?
C34 C33 C32 120.5(2) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C30 C31 C32 119.02(19) . . ?
C30 C31 H31 120.5 . . ?
C32 C31 H31 120.5 . . ?
C31 C30 C35 121.4(2) . . ?
C31 C30 N6 120.69(19) . . ?
C35 C30 N6 117.9(2) . . ?
O4 C17 O3 126.4(2) . . ?
O4 C17 C13 116.42(19) . . ?
O3 C17 C13 117.19(19) . . ?
C12 C13 C14 119.8(2) . . ?
C12 C13 C17 121.27(19) . . ?
C14 C13 C17 118.9(2) . . ?
C23 C22 C21 118.9(2) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C4 C3 C2 119.0(2) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C2 C7 120.0(2) . . ?
C3 C2 C1 119.9(2) . . ?
C7 C2 C1 120.0(2) . . ?
C10 C9 N2 107.54(19) . . ?
C10 C9 H9 126.2 . . ?
N2 C9 H9 126.2 . . ?
C12 C11 C16 121.9(2) . . ?
C12 C11 N2 119.6(2) . . ?
C16 C11 N2 118.4(2) . . ?
C5 C4 C3 122.1(2) . . ?
C5 C4 N1 119.2(2) . . ?
C3 C4 N1 118.7(2) . . ?
C9 C10 N1 107.0(2) . . ?
C9 C10 H10 126.5 . . ?
N1 C10 H10 126.5 . . ?
C6 C7 C2 119.8(2) . . ?
C6 C7 H7 120.1 . . ?
C2 C7 H7 120.1 . . ?
C33 C34 C35 120.2(2) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 H34 119.9 . . ?
N6 C27 N5 108.4(2) . . ?
N6 C27 H27 125.8 . . ?
N5 C27 H27 125.8 . . ?
N1 C8 N2 108.00(19) . . ?
N1 C8 H8 126.0 . . ?
N2 C8 H8 126.0 . . ?
C25 C26 C21 119.7(2) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
C30 C35 C34 118.9(2) . . ?
C30 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C22 C23 C24 121.5(2) . . ?
C22 C23 N5 120.0(2) . . ?
C24 C23 N5 118.5(2) . . ?
C15 C16 C11 118.7(2) . . ?
C15 C16 H16 120.6 . . ?
C11 C16 H16 120.6 . . ?
C4 C5 C6 118.5(2) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C15 C14 C13 120.5(2) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C29 C28 N6 107.5(2) . . ?
C29 C28 H28 126.3 . . ?
N6 C28 H28 126.3 . . ?
C5 C6 C7 120.4(2) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C24 C25 C26 120.6(2) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C28 C29 N5 106.8(2) . . ?
C28 C29 H29 126.6 . . ?
N5 C29 H29 126.6 . . ?
C16 C15 C14 120.3(2) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C25 C24 C23 118.9(2) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.5 . . ?

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 O7 C20 O8 -0.5(4) . . . . ?
Co1 O7 C20 C21 178.51(17) . . . . ?
Co2 O8 C20 O7 -16.4(3) . . . . ?
Co2 O8 C20 C21 164.58(15) . . . . ?
O7 C20 C21 C22 171.5(2) . . . . ?
O8 C20 C21 C22 -9.4(3) . . . . ?
O7 C20 C21 C26 -7.1(3) . . . . ?
O8 C20 C21 C26 172.0(2) . . . . ?
Co1 O1 C1 O2 -16.6(4) . . . . ?
Co1 O1 C1 C2 164.24(18) . . . . ?
Co2 O2 C1 O1 -7.3(4) . . . . ?
Co2 O2 C1 C2 171.85(15) . . . . ?
Co2 O9 C36 O10 -5.6(3) 7_656 . . . ?
Co2 O9 C36 C32 174.25(13) 7_656 . . . ?
C33 C32 C36 O9 -175.2(2) . . . . ?
C31 C32 C36 O9 5.0(3) . . . . ?
C33 C32 C36 O10 4.7(3) . . . . ?
C31 C32 C36 O10 -175.1(2) . . . . ?
C31 C32 C33 C34 -1.8(3) . . . . ?
C36 C32 C33 C34 178.4(2) . . . . ?
C33 C32 C31 C30 2.0(3) . . . . ?
C36 C32 C31 C30 -178.2(2) . . . . ?
C32 C31 C30 C35 -0.5(4) . . . . ?
C32 C31 C30 N6 179.9(2) . . . . ?
C27 N6 C30 C31 -20.1(4) . . . . ?
C28 N6 C30 C31 160.2(3) . . . . ?
C27 N6 C30 C35 160.2(3) . . . . ?
C28 N6 C30 C35 -19.4(4) . . . . ?
Co2 O3 C17 O4 7.0(3) 7_656 . . . ?
Co2 O3 C17 C13 -173.16(15) 7_656 . . . ?
C11 C12 C13 C14 1.8(4) . . . . ?
C11 C12 C13 C17 179.9(2) . . . . ?
O4 C17 C13 C12 -175.0(2) . . . . ?
O3 C17 C13 C12 5.2(3) . . . . ?
O4 C17 C13 C14 3.1(4) . . . . ?
O3 C17 C13 C14 -176.7(2) . . . . ?
C26 C21 C22 C23 -0.3(4) . . . . ?
C20 C21 C22 C23 -178.9(2) . . . . ?
C4 C3 C2 C7 -3.0(4) . . . . ?
C4 C3 C2 C1 177.4(2) . . . . ?
O1 C1 C2 C3 166.5(2) . . . . ?
O2 C1 C2 C3 -12.8(3) . . . . ?
O1 C1 C2 C7 -13.1(4) . . . . ?
O2 C1 C2 C7 167.6(2) . . . . ?
C8 N2 C9 C10 0.1(3) . . . . ?
C11 N2 C9 C10 -179.7(3) . . . . ?
C13 C12 C11 C16 -0.4(4) . . . . ?
C13 C12 C11 N2 -179.3(2) . . . . ?
C8 N2 C11 C12 -25.7(4) . . . . ?
C9 N2 C11 C12 154.1(3) . . . . ?
C8 N2 C11 C16 155.4(3) . . . . ?
C9 N2 C11 C16 -24.8(4) . . . . ?
C2 C3 C4 C5 4.1(5) . . . . ?
C2 C3 C4 N1 -174.1(3) . . . . ?
C8 N1 C4 C5 -145.6(3) . . . . ?
C10 N1 C4 C5 30.0(5) . . . . ?
C8 N1 C4 C3 32.6(4) . . . . ?
C10 N1 C4 C3 -151.7(3) . . . . ?
N2 C9 C10 N1 0.3(3) . . . . ?
C8 N1 C10 C9 -0.6(3) . . . . ?
C4 N1 C10 C9 -176.8(3) . . . . ?
C3 C2 C7 C6 -0.6(4) . . . . ?
C1 C2 C7 C6 179.0(3) . . . . ?
C32 C33 C34 C35 0.1(4) . . . . ?
C28 N6 C27 N5 0.0(4) . . . . ?
C30 N6 C27 N5 -179.7(3) . . . . ?
C29 N5 C27 N6 0.6(4) . . . . ?
C23 N5 C27 N6 -176.0(3) . . . . ?
C10 N1 C8 N2 0.7(3) . . . . ?
C4 N1 C8 N2 177.0(3) . . . . ?
C9 N2 C8 N1 -0.5(3) . . . . ?
C11 N2 C8 N1 179.4(3) . . . . ?
C22 C21 C26 C25 -0.2(5) . . . . ?
C20 C21 C26 C25 178.3(3) . . . . ?
C31 C30 C35 C34 -1.2(4) . . . . ?
N6 C30 C35 C34 178.5(3) . . . . ?
C33 C34 C35 C30 1.4(4) . . . . ?
C21 C22 C23 C24 0.3(5) . . . . ?
C21 C22 C23 N5 176.9(3) . . . . ?
C27 N5 C23 C22 -1.5(5) . . . . ?
C29 N5 C23 C22 -177.6(3) . . . . ?
C27 N5 C23 C24 175.1(3) . . . . ?
C29 N5 C23 C24 -0.9(5) . . . . ?
C12 C11 C16 C15 -1.0(5) . . . . ?
N2 C11 C16 C15 177.9(3) . . . . ?
C3 C4 C5 C6 -1.4(5) . . . . ?
N1 C4 C5 C6 176.8(3) . . . . ?
C12 C13 C14 C15 -1.7(5) . . . . ?
C17 C13 C14 C15 -179.9(3) . . . . ?
C27 N6 C28 C29 -0.7(4) . . . . ?
C30 N6 C28 C29 179.1(3) . . . . ?
C4 C5 C6 C7 -2.3(5) . . . . ?
C2 C7 C6 C5 3.3(5) . . . . ?
C21 C26 C25 C24 0.7(5) . . . . ?
N6 C28 C29 N5 1.0(4) . . . . ?
C27 N5 C29 C28 -1.1(4) . . . . ?
C23 N5 C29 C28 175.5(3) . . . . ?
C11 C16 C15 C14 1.1(6) . . . . ?
C13 C14 C15 C16 0.3(6) . . . . ?
C26 C25 C24 C23 -0.7(6) . . . . ?
C22 C23 C24 C25 0.1(6) . . . . ?
N5 C23 C24 C25 -176.4(3) . . . . ?

_refine_diff_density_max         0.864
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.081

_shelxl_version_number           2014/6


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 -0.073 0.250 400 103 ' '
2 0.000 0.066 0.750 400 103 ' '
3 0.500 0.079 0.250 400 103 ' '
4 0.500 -0.106 0.750 400 103 ' '

_platon_squeeze_details          
;
In order to subtract the contribution from the disordered 
solvent molecules, the SQUEEZE command was applied, which 
gave a new HKL file. The number of located electrons is 
412, is included in the formula, formula weight, calculated 
density, and F(000). These residual electron density 
were assigned to approx 10 DMF molecules per unit cell. 
This value calculated based upon electrons analysis. 
(One DMF molecules would give 40 e). 
;

# start Validation Reply Form
_vrf_CHEMW03_3Co                 
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: 
The formula includes 2.5 DMF molecules per formula
unit to account for the electron density removed by SQUEEZE.
;
# end Validation Reply Form
