# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1421602'
_audit_update_record             
;
2015-09-01 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H15 Cu N4 O4'
_chemical_formula_weight         438.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

loop_
_symmetry_equiv_pos_as_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                   24.513(5)
_cell_length_b                   18.922(4)
_cell_length_c                   17.238(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 119.74(3)
_cell_angle_gamma                90.00
_cell_volume                     6943(2)
_cell_formula_units_Z            16
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    19569
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.59

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3584
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.8001
_exptl_absorpt_correction_T_max  0.8599
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25702
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6116
_reflns_number_gt                4011
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0831P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6116
_refine_ls_number_parameters     527
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1330
_refine_ls_wR_factor_gt          0.1170
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.954
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.48081(4) 0.2500 0.04179(19) Uani 1 2 d S . .
O3 O 0.44257(10) 0.36246(14) 0.70053(15) 0.0468(6) Uani 1 1 d . . .
H3W H 0.4758 0.3834 0.7092 0.056 Uiso 0.50 1 d PR . .
N3 N 0.06970(12) 0.48758(16) 0.36396(17) 0.0362(7) Uani 1 1 d . . .
N4 N 0.16220(12) 0.47849(15) 0.48488(16) 0.0318(6) Uani 1 1 d . . .
O4 O 0.43873(11) 0.42253(16) 0.80842(15) 0.0533(7) Uani 1 1 d . . .
C20 C 0.22464(14) 0.45572(18) 0.5461(2) 0.0326(7) Uani 1 1 d . . .
C19 C 0.41473(15) 0.40051(18) 0.7317(2) 0.0355(8) Uani 1 1 d . . .
C18 C 0.25012(16) 0.4717(2) 0.6359(2) 0.0425(9) Uani 1 1 d . . .
H18A H 0.2262 0.4951 0.6561 0.051 Uiso 1 1 calc R . .
C17 C 0.12359(15) 0.45340(19) 0.4023(2) 0.0349(8) Uani 1 1 d . . .
H17A H 0.1337 0.4167 0.3758 0.042 Uiso 1 1 calc R . .
C16 C 0.34700(15) 0.41746(18) 0.6659(2) 0.0331(7) Uani 1 1 d . . .
C15 C 0.32046(14) 0.40084(18) 0.57611(19) 0.0350(8) Uani 1 1 d . . .
H15A H 0.3441 0.3764 0.5561 0.042 Uiso 1 1 calc R . .
C14 C 0.25953(15) 0.42007(19) 0.5159(2) 0.0370(8) Uani 1 1 d . . .
H14A H 0.2422 0.4091 0.4556 0.044 Uiso 1 1 calc R . .
C13 C 0.07333(16) 0.53734(19) 0.4251(2) 0.0383(8) Uani 1 1 d . . .
H13A H 0.0419 0.5692 0.4163 0.046 Uiso 1 1 calc R . .
C12 C 0.12996(15) 0.53208(19) 0.4995(2) 0.0374(8) Uani 1 1 d . . .
H12A H 0.1446 0.5593 0.5509 0.045 Uiso 1 1 calc R . .
C11 C 0.31110(16) 0.4527(2) 0.6948(2) 0.0430(9) Uani 1 1 d . . .
H11A H 0.3284 0.4639 0.7550 0.052 Uiso 1 1 calc R . .
Cu2 Cu 0.233902(19) 0.21327(3) 0.24972(2) 0.04273(16) Uani 1 1 d . . .
O7 O -0.20898(10) 0.10102(14) -0.19656(15) 0.0432(6) Uani 1 1 d D . .
H7W H -0.2488(6) 0.105(2) -0.230(2) 0.052 Uiso 1 1 d D . .
N7 N 0.16561(13) 0.22208(15) 0.13530(17) 0.0362(7) Uani 1 1 d . . .
O6 O 0.67542(10) 0.09382(13) 0.70811(14) 0.0406(6) Uani 1 1 d . . .
N5 N 0.29997(13) 0.21044(16) 0.36712(18) 0.0376(7) Uani 1 1 d . . .
N8 N 0.07205(12) 0.21496(15) 0.01481(16) 0.0313(6) Uani 1 1 d . . .
O8 O -0.20387(11) 0.15063(15) -0.30976(15) 0.0510(7) Uani 1 1 d . . .
O5 O 0.67242(11) 0.16449(15) 0.80849(15) 0.0513(7) Uani 1 1 d . . .
C40 C -0.18040(15) 0.13428(18) -0.2314(2) 0.0354(8) Uani 1 1 d . . .
C38 C 0.45288(14) 0.17666(18) 0.55366(19) 0.0310(7) Uani 1 1 d . . .
C39 C 0.57799(15) 0.14678(18) 0.67228(19) 0.0326(7) Uani 1 1 d . . .
N6 N 0.38866(12) 0.19413(15) 0.49271(16) 0.0330(6) Uani 1 1 d . . .
C37 C 0.11082(15) 0.18847(19) 0.0968(2) 0.0352(8) Uani 1 1 d . . .
H37A H 0.1006 0.1516 0.1230 0.042 Uiso 1 1 calc R . .
C36 C 0.64704(15) 0.13460(19) 0.7358(2) 0.0341(8) Uani 1 1 d . . .
C35 C -0.01649(15) 0.20788(19) -0.1366(2) 0.0370(8) Uani 1 1 d . . .
H35A H 0.0071 0.2318 -0.1569 0.044 Uiso 1 1 calc R . .
C34 C 0.35752(14) 0.18382(19) 0.4038(2) 0.0339(8) Uani 1 1 d . . .
H34A H 0.3741 0.1611 0.3723 0.041 Uiso 1 1 calc R . .
C33 C 0.00934(14) 0.19204(17) -0.04611(19) 0.0311(7) Uani 1 1 d . . .
C32 C 0.48568(16) 0.2173(2) 0.6297(2) 0.0395(8) Uani 1 1 d . . .
H32A H 0.4661 0.2548 0.6411 0.047 Uiso 1 1 calc R . .
C31 C -0.11337(14) 0.15214(17) -0.16604(19) 0.0313(7) Uani 1 1 d . . .
C30 C 0.54425(15) 0.1061(2) 0.5961(2) 0.0367(8) Uani 1 1 d . . .
H30A H 0.5638 0.0685 0.5848 0.044 Uiso 1 1 calc R . .
C29 C -0.02552(15) 0.15613(19) -0.0156(2) 0.0358(8) Uani 1 1 d . . .
H29A H -0.0081 0.1452 0.0447 0.043 Uiso 1 1 calc R . .
C28 C -0.07736(16) 0.18771(19) -0.1956(2) 0.0382(8) Uani 1 1 d . . .
H28A H -0.0946 0.1980 -0.2560 0.046 Uiso 1 1 calc R . .
C27 C 0.10392(16) 0.26841(19) -0.0001(2) 0.0394(8) Uani 1 1 d . . .
H27A H 0.0890 0.2964 -0.0510 0.047 Uiso 1 1 calc R . .
C26 C 0.54835(16) 0.2014(2) 0.6888(2) 0.0392(8) Uani 1 1 d . . .
H26A H 0.5705 0.2282 0.7405 0.047 Uiso 1 1 calc R . .
C25 C 0.48143(15) 0.12102(18) 0.5364(2) 0.0360(8) Uani 1 1 d . . .
H25A H 0.4590 0.0937 0.4853 0.043 Uiso 1 1 calc R . .
C24 C -0.08629(15) 0.13674(18) -0.0757(2) 0.0353(8) Uani 1 1 d . . .
H24A H -0.1098 0.1127 -0.0552 0.042 Uiso 1 1 calc R . .
C23 C 0.34853(16) 0.2289(2) 0.5140(2) 0.0417(9) Uani 1 1 d . . .
H23A H 0.3570 0.2429 0.5706 0.050 Uiso 1 1 calc R . .
C22 C 0.16090(16) 0.27208(19) 0.0735(2) 0.0394(8) Uani 1 1 d . . .
H22A H 0.1925 0.3035 0.0818 0.047 Uiso 1 1 calc R . .
C21 C 0.29456(16) 0.2388(2) 0.4367(2) 0.0423(9) Uani 1 1 d . . .
H21A H 0.2591 0.2614 0.4311 0.051 Uiso 1 1 calc R . .
Cu3 Cu 0.0000 0.05268(4) 0.7500 0.0503(2) Uani 1 2 d S . .
O1 O 0.44177(10) 0.16899(13) 1.20447(14) 0.0378(6) Uani 1 1 d . . .
H1W H 0.4744 0.1465 1.2132 0.045 Uiso 0.50 1 d PR . .
N1 N 0.06626(13) 0.05263(16) 0.86814(18) 0.0421(7) Uani 1 1 d . . .
O2 O 0.43807(11) 0.11022(15) 1.31393(15) 0.0501(7) Uani 1 1 d . . .
C10 C 0.41297(15) 0.13328(18) 1.2373(2) 0.0341(8) Uani 1 1 d . . .
N2 N 0.15547(12) 0.06765(15) 0.99414(16) 0.0340(6) Uani 1 1 d . . .
C9 C 0.12416(15) 0.07877(19) 0.9053(2) 0.0375(8) Uani 1 1 d . . .
H9A H 0.1408 0.1017 0.8740 0.045 Uiso 1 1 calc R . .
C8 C 0.21918(14) 0.08677(18) 1.05568(19) 0.0318(7) Uani 1 1 d . . .
C7 C 0.34417(15) 0.12052(18) 1.1746(2) 0.0331(7) Uani 1 1 d . . .
C6 C 0.25228(16) 0.04894(19) 1.1341(2) 0.0393(8) Uani 1 1 d . . .
H6A H 0.2331 0.0118 1.1469 0.047 Uiso 1 1 calc R . .
C5 C 0.31426(16) 0.06659(19) 1.1936(2) 0.0389(8) Uani 1 1 d . . .
H5A H 0.3361 0.0418 1.2470 0.047 Uiso 1 1 calc R . .
C4 C 0.30973(15) 0.15868(19) 1.0963(2) 0.0376(8) Uani 1 1 d . . .
H4A H 0.3287 0.1959 1.0833 0.045 Uiso 1 1 calc R . .
C3 C 0.24745(15) 0.14219(19) 1.0370(2) 0.0383(8) Uani 1 1 d . . .
H3A H 0.2248 0.1684 0.9850 0.046 Uiso 1 1 calc R . .
C2 C 0.06124(17) 0.0228(2) 0.9372(2) 0.0468(9) Uani 1 1 d . . .
H2A H 0.0257 0.0000 0.9312 0.056 Uiso 1 1 calc R . .
C1 C 0.11545(17) 0.0315(2) 1.0148(2) 0.0438(9) Uani 1 1 d . . .
H1A H 0.1241 0.0162 1.0710 0.053 Uiso 1 1 calc R . .


_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 N3 1.861(3) 2 ?
Cu1 N3 1.861(3) . ?
O3 C19 1.279(4) . ?
O3 H3W 0.8502 . ?
N3 C17 1.317(4) . ?
N3 C13 1.383(4) . ?
N4 C17 1.346(4) . ?
N4 C12 1.383(4) . ?
N4 C20 1.428(4) . ?
O4 C19 1.223(4) . ?
C20 C14 1.378(4) . ?
C20 C18 1.385(4) . ?
C19 C16 1.509(4) . ?
C18 C11 1.374(5) . ?
C18 H18A 0.9300 . ?
C17 H17A 0.9300 . ?
C16 C11 1.379(5) . ?
C16 C15 1.385(4) . ?
C15 C14 1.379(4) . ?
C15 H15A 0.9300 . ?
C14 H14A 0.9300 . ?
C13 C12 1.347(4) . ?
C13 H13A 0.9300 . ?
C12 H12A 0.9300 . ?
C11 H11A 0.9300 . ?
Cu2 N7 1.856(3) . ?
Cu2 N5 1.863(3) . ?
O7 C40 1.290(4) . ?
O7 H7W 0.856(10) . ?
N7 C37 1.328(4) . ?
N7 C22 1.386(4) . ?
O6 C36 1.280(4) . ?
N5 C34 1.326(4) . ?
N5 C21 1.379(4) . ?
N8 C37 1.349(4) . ?
N8 C27 1.378(4) . ?
N8 C33 1.433(4) . ?
O8 C40 1.217(4) . ?
O5 C36 1.226(4) . ?
C40 C31 1.499(4) . ?
C38 C25 1.376(5) . ?
C38 C32 1.382(4) . ?
C38 N6 1.432(4) . ?
C39 C26 1.373(5) . ?
C39 C30 1.387(4) . ?
C39 C36 1.510(4) . ?
N6 C34 1.345(4) . ?
N6 C23 1.376(4) . ?
C37 H37A 0.9300 . ?
C35 C28 1.379(4) . ?
C35 C33 1.394(4) . ?
C35 H35A 0.9300 . ?
C34 H34A 0.9300 . ?
C33 C29 1.384(5) . ?
C32 C26 1.392(5) . ?
C32 H32A 0.9300 . ?
C31 C24 1.388(4) . ?
C31 C28 1.392(5) . ?
C30 C25 1.392(4) . ?
C30 H30A 0.9300 . ?
C29 C24 1.377(4) . ?
C29 H29A 0.9300 . ?
C28 H28A 0.9300 . ?
C27 C22 1.344(5) . ?
C27 H27A 0.9300 . ?
C26 H26A 0.9300 . ?
C25 H25A 0.9300 . ?
C24 H24A 0.9300 . ?
C23 C21 1.346(5) . ?
C23 H23A 0.9300 . ?
C22 H22A 0.9300 . ?
C21 H21A 0.9300 . ?
Cu3 N1 1.872(3) 2_556 ?
Cu3 N1 1.872(3) . ?
O1 C10 1.293(4) . ?
O1 H1W 0.8501 . ?
N1 C9 1.329(4) . ?
N1 C2 1.377(5) . ?
O2 C10 1.228(4) . ?
C10 C7 1.504(4) . ?
N2 C9 1.346(4) . ?
N2 C1 1.379(4) . ?
N2 C8 1.432(4) . ?
C9 H9A 0.9300 . ?
C8 C3 1.380(5) . ?
C8 C6 1.382(4) . ?
C7 C5 1.387(5) . ?
C7 C4 1.388(4) . ?
C6 C5 1.388(5) . ?
C6 H6A 0.9300 . ?
C5 H5A 0.9300 . ?
C4 C3 1.387(5) . ?
C4 H4A 0.9300 . ?
C3 H3A 0.9300 . ?
C2 C1 1.349(5) . ?
C2 H2A 0.9300 . ?
C1 H1A 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Cu1 N3 172.10(19) 2 . ?
C19 O3 H3W 109.2 . . ?
C17 N3 C13 106.4(3) . . ?
C17 N3 Cu1 131.5(2) . . ?
C13 N3 Cu1 122.0(2) . . ?
C17 N4 C12 106.6(3) . . ?
C17 N4 C20 127.5(3) . . ?
C12 N4 C20 125.9(3) . . ?
C14 C20 C18 120.6(3) . . ?
C14 C20 N4 120.5(3) . . ?
C18 C20 N4 118.9(3) . . ?
O4 C19 O3 125.1(3) . . ?
O4 C19 C16 120.0(3) . . ?
O3 C19 C16 114.9(3) . . ?
C11 C18 C20 119.4(3) . . ?
C11 C18 H18A 120.3 . . ?
C20 C18 H18A 120.3 . . ?
N3 C17 N4 111.2(3) . . ?
N3 C17 H17A 124.4 . . ?
N4 C17 H17A 124.4 . . ?
C11 C16 C15 118.9(3) . . ?
C11 C16 C19 119.5(3) . . ?
C15 C16 C19 121.6(3) . . ?
C14 C15 C16 120.9(3) . . ?
C14 C15 H15A 119.5 . . ?
C16 C15 H15A 119.5 . . ?
C20 C14 C15 119.2(3) . . ?
C20 C14 H14A 120.4 . . ?
C15 C14 H14A 120.4 . . ?
C12 C13 N3 108.7(3) . . ?
C12 C13 H13A 125.6 . . ?
N3 C13 H13A 125.6 . . ?
C13 C12 N4 107.0(3) . . ?
C13 C12 H12A 126.5 . . ?
N4 C12 H12A 126.5 . . ?
C18 C11 C16 121.0(3) . . ?
C18 C11 H11A 119.5 . . ?
C16 C11 H11A 119.5 . . ?
N7 Cu2 N5 175.52(13) . . ?
C40 O7 H7W 110(3) . . ?
C37 N7 C22 105.4(3) . . ?
C37 N7 Cu2 130.0(2) . . ?
C22 N7 Cu2 124.4(2) . . ?
C34 N5 C21 105.8(3) . . ?
C34 N5 Cu2 132.4(2) . . ?
C21 N5 Cu2 121.8(2) . . ?
C37 N8 C27 107.4(3) . . ?
C37 N8 C33 126.7(3) . . ?
C27 N8 C33 126.0(3) . . ?
O8 C40 O7 125.0(3) . . ?
O8 C40 C31 121.0(3) . . ?
O7 C40 C31 114.0(3) . . ?
C25 C38 C32 120.8(3) . . ?
C25 C38 N6 120.6(3) . . ?
C32 C38 N6 118.6(3) . . ?
C26 C39 C30 119.1(3) . . ?
C26 C39 C36 118.9(3) . . ?
C30 C39 C36 122.0(3) . . ?
C34 N6 C23 107.2(3) . . ?
C34 N6 C38 126.8(3) . . ?
C23 N6 C38 125.9(3) . . ?
N7 C37 N8 110.9(3) . . ?
N7 C37 H37A 124.5 . . ?
N8 C37 H37A 124.5 . . ?
O5 C36 O6 124.4(3) . . ?
O5 C36 C39 119.3(3) . . ?
O6 C36 C39 116.3(3) . . ?
C28 C35 C33 119.4(3) . . ?
C28 C35 H35A 120.3 . . ?
C33 C35 H35A 120.3 . . ?
N5 C34 N6 110.9(3) . . ?
N5 C34 H34A 124.6 . . ?
N6 C34 H34A 124.6 . . ?
C29 C33 C35 120.5(3) . . ?
C29 C33 N8 120.7(3) . . ?
C35 C33 N8 118.8(3) . . ?
C38 C32 C26 119.1(3) . . ?
C38 C32 H32A 120.5 . . ?
C26 C32 H32A 120.5 . . ?
C24 C31 C28 118.4(3) . . ?
C24 C31 C40 122.1(3) . . ?
C28 C31 C40 119.5(3) . . ?
C39 C30 C25 120.6(3) . . ?
C39 C30 H30A 119.7 . . ?
C25 C30 H30A 119.7 . . ?
C24 C29 C33 119.1(3) . . ?
C24 C29 H29A 120.4 . . ?
C33 C29 H29A 120.4 . . ?
C35 C28 C31 120.9(3) . . ?
C35 C28 H28A 119.5 . . ?
C31 C28 H28A 119.5 . . ?
C22 C27 N8 106.4(3) . . ?
C22 C27 H27A 126.8 . . ?
N8 C27 H27A 126.8 . . ?
C39 C26 C32 121.1(3) . . ?
C39 C26 H26A 119.5 . . ?
C32 C26 H26A 119.5 . . ?
C38 C25 C30 119.3(3) . . ?
C38 C25 H25A 120.3 . . ?
C30 C25 H25A 120.3 . . ?
C29 C24 C31 121.7(3) . . ?
C29 C24 H24A 119.2 . . ?
C31 C24 H24A 119.2 . . ?
C21 C23 N6 106.5(3) . . ?
C21 C23 H23A 126.7 . . ?
N6 C23 H23A 126.7 . . ?
C27 C22 N7 110.0(3) . . ?
C27 C22 H22A 125.0 . . ?
N7 C22 H22A 125.0 . . ?
C23 C21 N5 109.6(3) . . ?
C23 C21 H21A 125.2 . . ?
N5 C21 H21A 125.2 . . ?
N1 Cu3 N1 179.94(19) 2_556 . ?
C10 O1 H1W 109.2 . . ?
C9 N1 C2 105.5(3) . . ?
C9 N1 Cu3 131.8(3) . . ?
C2 N1 Cu3 122.6(2) . . ?
O2 C10 O1 124.4(3) . . ?
O2 C10 C7 120.0(3) . . ?
O1 C10 C7 115.5(3) . . ?
C9 N2 C1 107.1(3) . . ?
C9 N2 C8 126.9(3) . . ?
C1 N2 C8 126.0(3) . . ?
N1 C9 N2 111.1(3) . . ?
N1 C9 H9A 124.4 . . ?
N2 C9 H9A 124.4 . . ?
C3 C8 C6 120.2(3) . . ?
C3 C8 N2 120.6(3) . . ?
C6 C8 N2 119.3(3) . . ?
C5 C7 C4 118.3(3) . . ?
C5 C7 C10 119.0(3) . . ?
C4 C7 C10 122.6(3) . . ?
C8 C6 C5 119.6(3) . . ?
C8 C6 H6A 120.2 . . ?
C5 C6 H6A 120.2 . . ?
C7 C5 C6 121.1(3) . . ?
C7 C5 H5A 119.5 . . ?
C6 C5 H5A 119.5 . . ?
C3 C4 C7 121.0(3) . . ?
C3 C4 H4A 119.5 . . ?
C7 C4 H4A 119.5 . . ?
C8 C3 C4 119.7(3) . . ?
C8 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C1 C2 N1 109.9(3) . . ?
C1 C2 H2A 125.1 . . ?
N1 C2 H2A 125.1 . . ?
C2 C1 N2 106.4(3) . . ?
C2 C1 H1A 126.8 . . ?
N2 C1 H1A 126.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3W O3 0.85 1.87 2.464(4) 125.8 2_656
O3 H3W O4 0.85 2.38 3.198(4) 162.0 2_656
C18 H18A O6 0.93 2.64 3.536(4) 163.1 3_455
C17 H17A O5 0.93 2.39 3.308(4) 170.5 8_455
C14 H14A O5 0.93 2.64 3.511(4) 155.3 8_455
C13 H13A O2 0.93 2.40 3.204(4) 145.3 3_454
C12 H12A O6 0.93 2.51 3.401(4) 160.0 3_455
O7 H7W O6 0.856(10) 1.634(14) 2.476(3) 167(4) 1_454
O7 H7W O5 0.856(10) 2.59(3) 3.187(4) 127(3) 1_454
C37 H37A O4 0.93 2.33 3.244(4) 167.7 7_556
C35 H35A O1 0.93 2.60 3.505(4) 163.0 7_556
C34 H34A O2 0.93 2.44 3.357(4) 168.3 1_554
C32 H32A O3 0.93 2.47 3.381(4) 165.1 .
C29 H29A O4 0.93 2.58 3.458(4) 156.8 7_556
C27 H27A O1 0.93 2.45 3.340(4) 159.3 7_556
C22 H22A O8 0.93 2.45 3.250(4) 144.5 8_556
C21 H21A O5 0.93 2.55 3.261(4) 133.7 8_455
O1 H1W O1 0.85 1.88 2.484(4) 126.9 2_657
O1 H1W O2 0.85 2.51 3.308(3) 156.8 2_657
C9 H9A O8 0.93 2.48 3.402(5) 169.1 2
C6 H6A O7 0.93 2.48 3.387(4) 165.3 5_556
C2 H2A O4 0.93 2.59 3.306(4) 134.4 3_445

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.072
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1421603'
_audit_update_record             
;
2015-10-23 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H38 Mo8 N8 O35'
_chemical_formula_sum            'C40 H38 Mo8 N8 O35'
_chemical_formula_weight         1958.30

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   7.3598(15)
_cell_length_b                   14.818(3)
_cell_length_c                   26.434(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.94(3)
_cell_angle_gamma                90
_cell_volume                     2872.1(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.264
_exptl_crystal_F_000             1900
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.795
_shelx_estimated_absorpt_T_min   0.738
_shelx_estimated_absorpt_T_max   0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_T_max  0.813
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26137
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.061
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             6310
_reflns_number_gt                4588
_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       'SMART (Bruker, 1997)'
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 During the refinement, four unusual reflections of (Iobs-Icalc)/
 sigmaw > 10 outlics are omitted.
 OMIT    -8   3  12
 OMIT     2   4  32
 OMIT     8   9   7
 OMIT    -6   4  24

 "ISOR" and "SIMU" were used to  refine the N4 and C1 atoms with 
 unnormal ADP problems.
 ISOR 0.005 N4
 SIMU 0.01 0.02 2.8 N4 C1

 The bond lenghs and angles of H-O of lattice water molecules are 
 defined with  restrained command 'DFIX'.

 DFIX 0.82 0.01 O1W H1WA O1W H1WB
 DFIX 1.32 0.01 H1WA H1WB

 DFIX 0.82 0.01 O2W H2WA O2W H2WB
 DFIX 1.32 0.01 H2WA H2WB

 
 All above restrained refinement led to a restraint value of 24.
 
 The lattice water molecule O1W is anistropically refined and the 
 H atoms on O1W are assigned from the residual peaks. The H 
 positions are confirmed based on the weak hydrogen-bonding 
 interactions, such as O1W-H1WA...O6 2.873 A, O1W-H1WB...N2 2.674 A,
 O1W-H1WB...O5 2.757 A, and O1W-H1WB...N2 2.783 A.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0634P)²+0.7832P] 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         6310
_refine_ls_number_parameters     433
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1024
_refine_ls_wR_factor_gt          0.0957
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_restrained_S_all      0.954
_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
Mo1 Mo 0.74492(5) 0.21721(3) 0.57199(2) 0.01678(11) Uani 1 1 d . . . . .
Mo2 Mo 0.52534(5) 0.22412(3) 0.67924(2) 0.01822(11) Uani 1 1 d . . . . .
Mo3 Mo 0.24567(5) 0.24569(3) 0.57118(2) 0.01699(11) Uani 1 1 d . . . . .
Mo4 Mo 1.02713(5) 0.25595(2) 0.67897(2) 0.01631(11) Uani 1 1 d . . . . .
O1 O 0.2024(4) 0.1015(2) 0.59336(12) 0.0242(7) Uani 1 1 d . . . . .
O2 O 0.5601(4) 0.3666(2) 0.65728(12) 0.0246(7) Uani 1 1 d . . . . .
O3 O 0.7065(4) 0.3645(2) 0.58686(12) 0.0237(7) Uani 1 1 d . . . . .
O4 O 0.5007(5) 0.1101(2) 0.68657(15) 0.0345(9) Uani 1 1 d . . . . .
O5 O 0.0657(4) 0.1058(2) 0.66576(12) 0.0235(7) Uani 1 1 d . . . . .
O6 O 1.0004(4) 0.3707(2) 0.68089(13) 0.0294(8) Uani 1 1 d . . . . .
O7 O 0.2762(4) 0.3576(2) 0.56134(14) 0.0315(8) Uani 1 1 d . . . . .
O8 O 0.5432(5) 0.2615(3) 0.73978(14) 0.0360(9) Uani 1 1 d . . . . .
O9 O 0.7759(4) 0.1031(2) 0.57064(14) 0.0298(8) Uani 1 1 d . . . . .
O10 O 0.2230(5) 0.2047(3) 0.51128(13) 0.0316(8) Uani 1 1 d . . . . .
O11 O 1.0593(5) 0.2281(2) 0.74123(13) 0.0291(8) Uani 1 1 d . . . . .
O12 O 0.7128(5) 0.2442(2) 0.50994(13) 0.0297(8) Uani 1 1 d . . . . .
O13 O 0.7779(4) 0.2204(2) 0.65975(12) 0.0222(7) Uani 1 1 d . . . . .
O14 O 0.2728(4) 0.2551(2) 0.65691(12) 0.0211(7) Uani 1 1 d . . . . .
O15 O 0.4971(4) 0.2141(2) 0.59369(12) 0.0203(7) Uani 1 1 d . . . . .
O16 O 0.9955(4) 0.2526(2) 0.59205(12) 0.0212(7) Uani 1 1 d . . . . .
N1 N 0.1197(5) -0.3181(3) 0.62306(16) 0.0276(9) Uani 1 1 d D . . . .
N2 N 0.0966(7) -0.4569(3) 0.6437(2) 0.0472(13) Uani 1 1 d D . . . .
H2B H 0.0789 -0.5046 0.6611 0.057 Uiso 1 1 calc R U . . .
N3 N 0.6187(5) 0.7879(3) 0.62334(18) 0.0317(10) Uani 1 1 d . . . . .
N4 N 0.5752(8) 0.9256(5) 0.6021(3) 0.0740(18) Uani 1 1 d D U . . .
H4B H 0.5461 0.9739 0.5852 0.089 Uiso 1 1 calc R U . . .
C1 C 0.6558(9) 0.9223(4) 0.6517(3) 0.0551(17) Uani 1 1 d D U . . .
H1A H 0.693(8) 0.9698(12) 0.6687(12) 0.066 Uiso 1 1 d D U . . .
C2 C 0.6835(8) 0.8401(4) 0.6631(2) 0.0438(15) Uani 1 1 d D . . . .
H2A H 0.7392 0.8190 0.6938 0.053 Uiso 1 1 calc R U . . .
C3 C 0.5511(8) 0.8419(4) 0.5854(3) 0.0434(14) Uani 1 1 d . . . . .
H3A H 0.4981 0.8241 0.5537 0.052 Uiso 1 1 calc R U . . .
C4 C 0.6575(7) 0.6464(4) 0.5783(2) 0.0337(12) Uani 1 1 d . . . . .
H4A H 0.6801 0.6792 0.5495 0.040 Uiso 1 1 calc R U . . .
C5 C 0.6219(6) 0.6901(3) 0.62249(19) 0.0267(10) Uani 1 1 d . . . . .
C6 C 0.5885(7) 0.6439(4) 0.6657(2) 0.0346(12) Uani 1 1 d . . . . .
H6A H 0.5643 0.6747 0.6950 0.042 Uiso 1 1 calc R U . . .
C7 C 0.5914(7) 0.5508(3) 0.66472(19) 0.0310(11) Uani 1 1 d . . . . .
H7A H 0.5690 0.5185 0.6937 0.037 Uiso 1 1 calc R U . . .
C8 C 0.6274(6) 0.5048(3) 0.62116(18) 0.0256(10) Uani 1 1 d . . . . .
C9 C 0.6591(7) 0.5531(3) 0.57750(19) 0.0295(11) Uani 1 1 d . . . . .
H9A H 0.6813 0.5225 0.5479 0.035 Uiso 1 1 calc R U . . .
C10 C 0.6315(6) 0.4040(3) 0.62177(17) 0.0220(9) Uani 1 1 d . . . . .
C11 C 0.0823(8) -0.3745(4) 0.6596(2) 0.0366(12) Uani 1 1 d D . . . .
H11A H 0.054(8) -0.3591(9) 0.6891(8) 0.044 Uiso 1 1 d D U . . .
C12 C 0.1442(8) -0.4557(4) 0.5949(2) 0.0451(15) Uani 1 1 d . . . . .
H12A H 0.1633 -0.5057 0.5748 0.054 Uiso 1 1 calc R U . . .
C13 C 0.1583(8) -0.3690(4) 0.5815(2) 0.0367(13) Uani 1 1 d . . . . .
H13A H 0.1882 -0.3472 0.5503 0.044 Uiso 1 1 calc R U . . .
C14 C 0.1182(6) -0.2212(3) 0.62585(18) 0.0243(10) Uani 1 1 d . . . . .
C15 C 0.1781(7) -0.1786(4) 0.67012(19) 0.0317(11) Uani 1 1 d . . . . .
H15A H 0.2184 -0.2120 0.6987 0.038 Uiso 1 1 calc R U . . .
C16 C 0.1780(7) -0.0849(3) 0.6719(2) 0.0317(11) Uani 1 1 d . . . . .
H16A H 0.2147 -0.0552 0.7021 0.038 Uiso 1 1 calc R U . . .
C17 C 0.1231(6) -0.0360(3) 0.62877(19) 0.0242(10) Uani 1 1 d . . . . .
C18 C 0.0649(6) -0.0797(3) 0.58456(19) 0.0282(10) Uani 1 1 d . . . . .
H18A H 0.0288 -0.0463 0.5556 0.034 Uiso 1 1 calc R U . . .
C19 C 0.0594(6) -0.1728(3) 0.58256(18) 0.0262(10) Uani 1 1 d . . . . .
H19A H 0.0171 -0.2024 0.5528 0.031 Uiso 1 1 calc R U . . .
C20 C 0.1311(6) 0.0656(3) 0.62961(18) 0.0233(10) Uani 1 1 d . . . . .
O1W O 0.8626(11) 0.0189(6) 0.7386(2) 0.104(2) Uani 1 1 d D . . . .
H1WA H 0.788(7) 0.001(6) 0.758(2) 0.104 Uiso 1 1 d D U . . .
H1WB H 0.961(5) 0.025(7) 0.755(2) 0.104 Uiso 1 1 d D U . . .
O2W O 0.3960(15) 0.0132(7) 0.5112(4) 0.063(3) Uani 0.5 1 d D . P A -1
H2WA H 0.409(14) 0.066(3) 0.519(5) 0.063 Uiso 0.5 1 d D U P B -1
H2WB H 0.285(4) 0.005(7) 0.506(5) 0.063 Uiso 0.5 1 d D U P C -1


_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
Mo1 O12 1.685(3) . ?
Mo1 O9 1.707(3) . ?
Mo1 O16 1.946(3) . ?
Mo1 O15 1.959(3) . ?
Mo1 O3 2.240(3) . ?
Mo1 O13 2.312(3) . ?
Mo2 O8 1.688(4) . ?
Mo2 O4 1.712(4) . ?
Mo2 O14 1.956(3) . ?
Mo2 O13 1.972(3) . ?
Mo2 O2 2.210(3) . ?
Mo2 O15 2.258(3) . ?
Mo3 O10 1.691(3) . ?
Mo3 O7 1.696(4) . ?
Mo3 O15 1.952(3) . ?
Mo3 O16 1.970(3) 1_455 ?
Mo3 O1 2.246(3) . ?
Mo3 O14 2.262(3) . ?
Mo4 O11 1.693(3) . ?
Mo4 O6 1.713(3) . ?
Mo4 O13 1.934(3) . ?
Mo4 O14 1.947(3) 1_655 ?
Mo4 O5 2.274(3) 1_655 ?
Mo4 O16 2.290(3) . ?
O1 C20 1.250(5) . ?
O2 C10 1.245(5) . ?
O3 C10 1.260(5) . ?
O5 C20 1.256(5) . ?
O5 Mo4 2.274(3) 1_455 ?
O14 Mo4 1.947(3) 1_455 ?
O16 Mo3 1.970(3) 1_655 ?
N1 C11 1.323(6) . ?
N1 C13 1.381(6) . ?
N1 C14 1.438(6) . ?
N2 C11 1.299(7) . ?
N2 C12 1.365(8) . ?
N2 H2B 0.8600 . ?
N3 C3 1.346(7) . ?
N3 C2 1.359(7) . ?
N3 C5 1.449(7) . ?
N4 C3 1.323(9) . ?
N4 C1 1.392(10) . ?
N4 H4B 0.8600 . ?
C1 C2 1.267(10) . ?
C1 H1A 0.867(9) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
C4 C5 1.382(7) . ?
C4 C9 1.383(7) . ?
C4 H4A 0.9300 . ?
C5 C6 1.371(7) . ?
C6 C7 1.381(7) . ?
C6 H6A 0.9300 . ?
C7 C8 1.383(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.394(7) . ?
C8 C10 1.494(7) . ?
C9 H9A 0.9300 . ?
C11 H11A 0.855(7) . ?
C12 C13 1.339(8) . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9300 . ?
C14 C15 1.369(7) . ?
C14 C19 1.388(6) . ?
C15 C16 1.389(7) . ?
C15 H15A 0.9300 . ?
C16 C17 1.383(7) . ?
C16 H16A 0.9300 . ?
C17 C18 1.372(7) . ?
C17 C20 1.506(7) . ?
C18 C19 1.381(7) . ?
C18 H18A 0.9300 . ?
C19 H19A 0.9300 . ?
O1W H1WA 0.823(10) . ?
O1W H1WB 0.820(10) . ?
O2W H2WA 0.820(10) . ?
O2W H2WB 0.825(10) . ?

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
O12 Mo1 O9 102.84(18) . . ?
O12 Mo1 O16 104.57(16) . . ?
O9 Mo1 O16 98.47(14) . . ?
O12 Mo1 O15 103.58(15) . . ?
O9 Mo1 O15 96.43(14) . . ?
O16 Mo1 O15 144.17(14) . . ?
O12 Mo1 O3 86.02(15) . . ?
O9 Mo1 O3 171.11(15) . . ?
O16 Mo1 O3 79.69(12) . . ?
O15 Mo1 O3 80.61(12) . . ?
O12 Mo1 O13 164.95(15) . . ?
O9 Mo1 O13 92.21(14) . . ?
O16 Mo1 O13 72.90(12) . . ?
O15 Mo1 O13 74.13(12) . . ?
O3 Mo1 O13 78.93(12) . . ?
O8 Mo2 O4 102.53(19) . . ?
O8 Mo2 O14 101.75(17) . . ?
O4 Mo2 O14 99.12(15) . . ?
O8 Mo2 O13 104.99(17) . . ?
O4 Mo2 O13 96.52(15) . . ?
O14 Mo2 O13 145.12(14) . . ?
O8 Mo2 O2 86.22(16) . . ?
O4 Mo2 O2 171.17(16) . . ?
O14 Mo2 O2 79.92(12) . . ?
O13 Mo2 O2 79.92(12) . . ?
O8 Mo2 O15 164.60(16) . . ?
O4 Mo2 O15 92.68(15) . . ?
O14 Mo2 O15 73.15(12) . . ?
O13 Mo2 O15 75.16(12) . . ?
O2 Mo2 O15 78.62(12) . . ?
O10 Mo3 O7 102.20(18) . . ?
O10 Mo3 O15 102.34(15) . . ?
O7 Mo3 O15 98.44(15) . . ?
O10 Mo3 O16 105.17(15) . 1_455 ?
O7 Mo3 O16 97.57(14) . 1_455 ?
O15 Mo3 O16 144.27(14) . 1_455 ?
O10 Mo3 O1 84.13(15) . . ?
O7 Mo3 O1 173.59(15) . . ?
O15 Mo3 O1 81.03(12) . . ?
O16 Mo3 O1 79.57(12) 1_455 . ?
O10 Mo3 O14 162.44(15) . . ?
O7 Mo3 O14 95.28(15) . . ?
O15 Mo3 O14 73.13(12) . . ?
O16 Mo3 O14 73.75(13) 1_455 . ?
O1 Mo3 O14 78.42(12) . . ?
O11 Mo4 O6 102.71(17) . . ?
O11 Mo4 O13 103.83(16) . . ?
O6 Mo4 O13 99.76(15) . . ?
O11 Mo4 O14 103.51(16) . 1_655 ?
O6 Mo4 O14 97.31(14) . 1_655 ?
O13 Mo4 O14 143.50(14) . 1_655 ?
O11 Mo4 O5 84.37(15) . 1_655 ?
O6 Mo4 O5 172.77(14) . 1_655 ?
O13 Mo4 O5 79.71(13) . 1_655 ?
O14 Mo4 O5 79.40(12) 1_655 1_655 ?
O11 Mo4 O16 164.44(15) . . ?
O6 Mo4 O16 92.83(14) . . ?
O13 Mo4 O16 73.64(13) . . ?
O14 Mo4 O16 73.51(13) 1_655 . ?
O5 Mo4 O16 80.08(11) 1_655 . ?
C20 O1 Mo3 133.1(3) . . ?
C10 O2 Mo2 133.6(3) . . ?
C10 O3 Mo1 130.7(3) . . ?
C20 O5 Mo4 129.9(3) . 1_455 ?
Mo4 O13 Mo2 144.87(18) . . ?
Mo4 O13 Mo1 106.53(13) . . ?
Mo2 O13 Mo1 104.05(14) . . ?
Mo4 O14 Mo2 142.57(18) 1_455 . ?
Mo4 O14 Mo3 107.23(14) 1_455 . ?
Mo2 O14 Mo3 106.71(13) . . ?
Mo3 O15 Mo1 141.93(17) . . ?
Mo3 O15 Mo2 107.01(13) . . ?
Mo1 O15 Mo2 106.51(14) . . ?
Mo1 O16 Mo3 142.79(18) . 1_655 ?
Mo1 O16 Mo4 106.94(13) . . ?
Mo3 O16 Mo4 105.40(14) 1_655 . ?
C11 N1 C13 107.8(5) . . ?
C11 N1 C14 126.1(4) . . ?
C13 N1 C14 126.1(4) . . ?
C11 N2 C12 109.1(5) . . ?
C11 N2 H2B 125.4 . . ?
C12 N2 H2B 125.4 . . ?
C3 N3 C2 108.7(5) . . ?
C3 N3 C5 126.1(5) . . ?
C2 N3 C5 125.2(5) . . ?
C3 N4 C1 108.4(6) . . ?
C3 N4 H4B 125.8 . . ?
C1 N4 H4B 125.8 . . ?
C2 C1 N4 107.8(6) . . ?
C2 C1 H1A 128(2) . . ?
N4 C1 H1A 123(2) . . ?
C1 C2 N3 108.9(6) . . ?
C1 C2 H2A 125.5 . . ?
N3 C2 H2A 125.5 . . ?
N4 C3 N3 106.2(6) . . ?
N4 C3 H3A 126.9 . . ?
N3 C3 H3A 126.9 . . ?
C5 C4 C9 118.9(5) . . ?
C5 C4 H4A 120.5 . . ?
C9 C4 H4A 120.5 . . ?
C6 C5 C4 122.1(5) . . ?
C6 C5 N3 118.8(4) . . ?
C4 C5 N3 119.1(5) . . ?
C5 C6 C7 118.7(5) . . ?
C5 C6 H6A 120.7 . . ?
C7 C6 H6A 120.7 . . ?
C6 C7 C8 120.8(5) . . ?
C6 C7 H7A 119.6 . . ?
C8 C7 H7A 119.6 . . ?
C7 C8 C9 119.6(5) . . ?
C7 C8 C10 119.2(4) . . ?
C9 C8 C10 121.1(4) . . ?
C4 C9 C8 119.9(5) . . ?
C4 C9 H9A 120.1 . . ?
C8 C9 H9A 120.1 . . ?
O2 C10 O3 125.8(4) . . ?
O2 C10 C8 116.3(4) . . ?
O3 C10 C8 117.8(4) . . ?
N2 C11 N1 109.2(5) . . ?
N2 C11 H11A 125.3(11) . . ?
N1 C11 H11A 125.5(11) . . ?
C13 C12 N2 107.1(5) . . ?
C13 C12 H12A 126.5 . . ?
N2 C12 H12A 126.5 . . ?
C12 C13 N1 106.7(5) . . ?
C12 C13 H13A 126.6 . . ?
N1 C13 H13A 126.6 . . ?
C15 C14 C19 121.4(5) . . ?
C15 C14 N1 120.1(4) . . ?
C19 C14 N1 118.5(4) . . ?
C14 C15 C16 119.4(5) . . ?
C14 C15 H15A 120.3 . . ?
C16 C15 H15A 120.3 . . ?
C17 C16 C15 119.8(5) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C18 C17 C16 120.2(5) . . ?
C18 C17 C20 119.6(4) . . ?
C16 C17 C20 120.2(4) . . ?
C17 C18 C19 120.7(5) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C18 C19 C14 118.6(4) . . ?
C18 C19 H19A 120.7 . . ?
C14 C19 H19A 120.7 . . ?
O1 C20 O5 126.5(4) . . ?
O1 C20 C17 115.6(4) . . ?
O5 C20 C17 117.9(4) . . ?
H1WA O1W H1WB 107.6(18) . . ?
H2WA O2W H2WB 106.6(18) . . ?

_refine_diff_density_max         1.674
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.166

_shelxl_version_number           2014-3

