# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

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

data_Mo
_database_code_depnum_ccdc_archive 'CCDC 1518990'
_audit_update_record             
;
2017-01-02 deposited with the CCDC.
2017-01-10 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT601_Mo                  
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        303 Ang3  
RESPONSE: Considering the excellent R-values and the fact that the remaining 
electron densitiy in the last refinement cycle shows only in closest proximity 
of the refined atoms, it can only be concluded that this empty void is an 
inherent feature of the crystal packing. The SQUEEZE routine was NOT applied.
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H45 Mo2 N9 O7'
_chemical_formula_weight         931.71

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           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                   14.506(2)
_cell_length_b                   14.760(2)
_cell_length_c                   20.139(3)
_cell_angle_alpha                90
_cell_angle_beta                 98.609(4)
_cell_angle_gamma                90
_cell_volume                     4263.3(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25081
_cell_measurement_theta_min      1.980
_cell_measurement_theta_max      25.000

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_F_000             1904
_exptl_transmission_factor_min   0.855
_exptl_transmission_factor_max   1
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.118
_exptl_absorpt_coefficient_mu    0.644
_shelx_estimated_absorpt_T_min   0.904
_shelx_estimated_absorpt_T_max   0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  hemisphere
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25081
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.980
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3759
_reflns_number_gt                3332
_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       'SAINT APEX'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    sir92
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ortep
_computing_publication_material  winGX
_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)+(0.0316P)²+4.8781P] 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         3759
_refine_ls_number_parameters     259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0659
_refine_ls_wR_factor_gt          0.0638
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_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
C1 C 1.17278(15) -0.02044(15) 0.16884(11) 0.0153(5) Uani 1 1 d . . . . .
C2 C 1.21508(16) 0.10419(14) 0.26178(13) 0.0164(5) Uani 1 1 d . . . . .
C3 C 1.26235(16) 0.12140(14) 0.13394(12) 0.0162(5) Uani 1 1 d . . . . .
C4 C 0.98700(15) 0.04288(15) 0.19323(11) 0.0134(5) Uani 1 1 d . . . . .
C5 C 0.99098(15) 0.13343(15) 0.21347(11) 0.0137(5) Uani 1 1 d . . . . .
C6 C 0.95108(16) -0.00018(15) 0.12704(11) 0.0155(5) Uani 1 1 d . . . . .
H6A H 0.9850 -0.0575 0.1226 0.019 Uiso 1 1 calc R U . . .
H6B H 0.8841 -0.0147 0.1253 0.019 Uiso 1 1 calc R U . . .
C7 C 0.89901(16) 0.08206(16) 0.01780(12) 0.0184(5) Uani 1 1 d . . . . .
C8 C 0.80422(16) 0.04037(18) 0.00469(13) 0.0248(6) Uani 1 1 d . . . . .
H8A H 0.8101 -0.0250 -0.0022 0.037 Uiso 1 1 calc R U . . .
H8B H 0.7687 0.0677 -0.0356 0.037 Uiso 1 1 calc R U . . .
H8C H 0.7717 0.0511 0.0433 0.037 Uiso 1 1 calc R U . . .
C9 C 0.94051(17) 0.14738(16) -0.01678(12) 0.0210(5) Uani 1 1 d . . . . .
H9 H 0.9137 0.1767 -0.0571 0.025 Uiso 1 1 calc R U . . .
C10 C 1.02977(16) 0.16211(15) 0.01897(12) 0.0177(5) Uani 1 1 d . . . . .
C11 C 1.10305(17) 0.22726(17) 0.00436(12) 0.0228(6) Uani 1 1 d . . . . .
H11A H 1.0930 0.2861 0.0246 0.034 Uiso 1 1 calc R U . . .
H11B H 1.0995 0.2343 -0.0443 0.034 Uiso 1 1 calc R U . . .
H11C H 1.1647 0.2040 0.0232 0.034 Uiso 1 1 calc R U . . .
C12 C 0.95074(15) 0.21385(14) 0.17277(11) 0.0142(5) Uani 1 1 d . . . . .
H12A H 0.9244 0.1935 0.1270 0.017 Uiso 1 1 calc R U . . .
H12B H 0.8994 0.2402 0.1938 0.017 Uiso 1 1 calc R U . . .
C13 C 1.00982(17) 0.37361(15) 0.15984(13) 0.0205(5) Uani 1 1 d . . . . .
C14 C 0.91620(18) 0.41677(16) 0.15440(16) 0.0310(7) Uani 1 1 d . . . . .
H14A H 0.8720 0.3836 0.1216 0.046 Uiso 1 1 calc R U . . .
H14B H 0.9202 0.4798 0.1397 0.046 Uiso 1 1 calc R U . . .
H14C H 0.8948 0.4153 0.1983 0.046 Uiso 1 1 calc R U . . .
C15 C 1.09745(17) 0.40883(15) 0.15838(13) 0.0225(6) Uani 1 1 d . . . . .
H15 H 1.1127 0.4707 0.1530 0.027 Uiso 1 1 calc R U . . .
C16 C 1.15967(16) 0.33580(15) 0.16633(11) 0.0167(5) Uani 1 1 d . . . . .
C17 C 1.26292(16) 0.33722(16) 0.16867(13) 0.0213(5) Uani 1 1 d . . . . .
H17A H 1.2911 0.2892 0.1987 0.032 Uiso 1 1 calc R U . . .
H17B H 1.2874 0.3961 0.1855 0.032 Uiso 1 1 calc R U . . .
H17C H 1.2781 0.3273 0.1234 0.032 Uiso 1 1 calc R U . . .
C18 C 1.47282(19) 0.24516(17) 0.30227(13) 0.0268(6) Uani 1 1 d . . . . .
H18A H 1.4125 0.2657 0.3143 0.032 Uiso 1 1 calc R U . . .
H18B H 1.5205 0.2473 0.3429 0.032 Uiso 1 1 calc R U . . .
C19 C 1.46435(17) 0.15075(17) 0.27376(14) 0.0269(6) Uani 1 1 d . . . . .
H19A H 1.4009 0.1393 0.2495 0.032 Uiso 1 1 calc R U . . .
H19B H 1.4794 0.1047 0.3095 0.032 Uiso 1 1 calc R U . . .
N1 N 1.0000 -0.01029(18) 0.2500 0.0141(6) Uani 1 2 d S T P . .
H1N H 1.0000 -0.060(3) 0.2500 0.017 Uiso 1 2 d S U P . .
N2 N 0.96288(12) 0.05974(12) 0.07149(9) 0.0145(4) Uani 1 1 d . . . . .
N3 N 1.04362(13) 0.10876(12) 0.07345(10) 0.0150(4) Uani 1 1 d . . . . .
N4 N 1.02160(12) 0.28335(12) 0.16828(10) 0.0148(4) Uani 1 1 d . . . . .
N5 N 1.11310(13) 0.25838(12) 0.17141(9) 0.0146(4) Uani 1 1 d . . . . .
O1 O 1.19091(12) -0.09749(10) 0.16890(9) 0.0210(4) Uani 1 1 d . . . . .
O2 O 1.25083(12) 0.09697(11) 0.31756(9) 0.0240(4) Uani 1 1 d . . . . .
O3 O 1.33168(11) 0.12662(11) 0.11065(9) 0.0222(4) Uani 1 1 d . . . . .
O4 O 1.5000 0.30125(15) 0.2500 0.0282(6) Uani 1 2 d S T P . .
Mo Mo 1.14683(2) 0.10851(2) 0.17072(2) 0.01211(8) Uani 1 1 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
C1 O1 1.167(3) . ?
C1 Mo 1.942(2) . ?
C2 O2 1.170(3) . ?
C2 Mo 1.950(3) . ?
C3 O3 1.174(3) . ?
C3 Mo 1.940(2) . ?
C4 N1 1.376(3) . ?
C4 C5 1.396(3) . ?
C4 C6 1.498(3) . ?
C4 Mo 2.614(2) . ?
C5 C5 1.455(5) 2_755 ?
C5 C12 1.509(3) . ?
C5 Mo 2.563(2) . ?
C6 N2 1.456(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N2 1.355(3) . ?
C7 C9 1.379(3) . ?
C7 C8 1.493(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.401(3) . ?
C9 H9 0.9500 . ?
C10 N3 1.341(3) . ?
C10 C11 1.495(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N4 1.465(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N4 1.351(3) . ?
C13 C15 1.378(3) . ?
C13 C14 1.489(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.400(3) . ?
C15 H15 0.9500 . ?
C16 N5 1.339(3) . ?
C16 C17 1.492(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O4 1.440(3) . ?
C18 C19 1.505(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C19 1.511(5) 2_855 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
N1 C4 1.376(3) 2_755 ?
N1 H1N 0.73(4) . ?
N2 N3 1.372(2) . ?
N3 Mo 2.2805(19) . ?
N4 N5 1.370(3) . ?
N5 Mo 2.2659(18) . ?
O4 C18 1.440(3) 2_855 ?

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 C1 Mo 178.0(2) . . ?
O2 C2 Mo 174.77(19) . . ?
O3 C3 Mo 177.9(2) . . ?
N1 C4 C5 108.0(2) . . ?
N1 C4 C6 118.91(19) . . ?
C5 C4 C6 131.3(2) . . ?
N1 C4 Mo 109.92(12) . . ?
C5 C4 Mo 72.35(12) . . ?
C6 C4 Mo 101.67(13) . . ?
C4 C5 C5 106.77(13) . 2_755 ?
C4 C5 C12 126.8(2) . . ?
C5 C5 C12 123.05(14) 2_755 . ?
C4 C5 Mo 76.38(12) . . ?
C5 C5 Mo 107.79(19) 2_755 . ?
C12 C5 Mo 102.67(13) . . ?
N2 C6 C4 111.14(18) . . ?
N2 C6 H6A 109.4 . . ?
C4 C6 H6A 109.4 . . ?
N2 C6 H6B 109.4 . . ?
C4 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N2 C7 C9 105.9(2) . . ?
N2 C7 C8 122.9(2) . . ?
C9 C7 C8 131.2(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 C10 106.8(2) . . ?
C7 C9 H9 126.6 . . ?
C10 C9 H9 126.6 . . ?
N3 C10 C9 110.1(2) . . ?
N3 C10 C11 121.0(2) . . ?
C9 C10 C11 128.9(2) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 C5 111.48(18) . . ?
N4 C12 H12A 109.3 . . ?
C5 C12 H12A 109.3 . . ?
N4 C12 H12B 109.3 . . ?
C5 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
N4 C13 C15 106.0(2) . . ?
N4 C13 C14 121.9(2) . . ?
C15 C13 C14 132.2(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 C16 106.7(2) . . ?
C13 C15 H15 126.6 . . ?
C16 C15 H15 126.6 . . ?
N5 C16 C15 110.0(2) . . ?
N5 C16 C17 121.7(2) . . ?
C15 C16 C17 128.3(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 C18 C19 105.6(2) . . ?
O4 C18 H18A 110.6 . . ?
C19 C18 H18A 110.6 . . ?
O4 C18 H18B 110.6 . . ?
C19 C18 H18B 110.6 . . ?
H18A C18 H18B 108.8 . . ?
C18 C19 C19 102.54(15) . 2_855 ?
C18 C19 H19A 111.3 . . ?
C19 C19 H19A 111.3 2_855 . ?
C18 C19 H19B 111.3 . . ?
C19 C19 H19B 111.3 2_855 . ?
H19A C19 H19B 109.2 . . ?
C4 N1 C4 110.5(3) . 2_755 ?
C4 N1 H1N 124.77(13) . . ?
C4 N1 H1N 124.77(13) 2_755 . ?
C7 N2 N3 111.93(18) . . ?
C7 N2 C6 128.00(19) . . ?
N3 N2 C6 119.74(18) . . ?
C10 N3 N2 105.27(18) . . ?
C10 N3 Mo 134.62(15) . . ?
N2 N3 Mo 118.14(13) . . ?
C13 N4 N5 112.01(18) . . ?
C13 N4 C12 128.45(19) . . ?
N5 N4 C12 119.53(17) . . ?
C16 N5 N4 105.26(17) . . ?
C16 N5 Mo 136.11(15) . . ?
N4 N5 Mo 118.10(13) . . ?
C18 O4 C18 109.8(3) . 2_855 ?
C3 Mo C1 84.70(9) . . ?
C3 Mo C2 90.93(10) . . ?
C1 Mo C2 85.05(9) . . ?
C3 Mo N5 96.10(8) . . ?
C1 Mo N5 178.61(8) . . ?
C2 Mo N5 96.07(8) . . ?
C3 Mo N3 99.52(8) . . ?
C1 Mo N3 95.12(8) . . ?
C2 Mo N3 169.52(8) . . ?
N5 Mo N3 83.63(6) . . ?
C3 Mo C5 165.87(8) . . ?
C1 Mo C5 109.30(8) . . ?
C2 Mo C5 92.17(8) . . ?
N5 Mo C5 69.86(7) . . ?
N3 Mo C5 77.86(7) . . ?
C3 Mo C4 160.32(8) . . ?
C1 Mo C4 79.61(8) . . ?
C2 Mo C4 99.40(8) . . ?
N5 Mo C4 99.37(7) . . ?
N3 Mo C4 70.39(7) . . ?
C5 Mo C4 31.26(7) . . ?

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
N1 C4 C5 C5 1.0(3) . . . 2_755 ?
C6 C4 C5 C5 165.0(2) . . . 2_755 ?
Mo C4 C5 C5 -104.8(2) . . . 2_755 ?
N1 C4 C5 C12 -158.40(19) . . . . ?
C6 C4 C5 C12 5.6(4) . . . . ?
Mo C4 C5 C12 95.8(2) . . . . ?
N1 C4 C5 Mo 105.81(13) . . . . ?
C6 C4 C5 Mo -90.2(2) . . . . ?
N1 C4 C6 N2 -166.22(16) . . . . ?
C5 C4 C6 N2 31.2(3) . . . . ?
Mo C4 C6 N2 -45.47(19) . . . . ?
N2 C7 C9 C10 -0.4(3) . . . . ?
C8 C7 C9 C10 178.8(2) . . . . ?
C7 C9 C10 N3 -0.1(3) . . . . ?
C7 C9 C10 C11 -178.5(2) . . . . ?
C4 C5 C12 N4 -125.4(2) . . . . ?
C5 C5 C12 N4 78.2(3) 2_755 . . . ?
Mo C5 C12 N4 -43.08(19) . . . . ?
N4 C13 C15 C16 -0.1(3) . . . . ?
C14 C13 C15 C16 179.6(3) . . . . ?
C13 C15 C16 N5 1.0(3) . . . . ?
C13 C15 C16 C17 -179.6(2) . . . . ?
O4 C18 C19 C19 30.5(3) . . . 2_855 ?
C5 C4 N1 C4 -0.41(11) . . . 2_755 ?
C6 C4 N1 C4 -166.7(2) . . . 2_755 ?
Mo C4 N1 C4 76.81(10) . . . 2_755 ?
C9 C7 N2 N3 0.7(3) . . . . ?
C8 C7 N2 N3 -178.5(2) . . . . ?
C9 C7 N2 C6 174.1(2) . . . . ?
C8 C7 N2 C6 -5.1(4) . . . . ?
C4 C6 N2 C7 -131.8(2) . . . . ?
C4 C6 N2 N3 41.1(3) . . . . ?
C9 C10 N3 N2 0.5(2) . . . . ?
C11 C10 N3 N2 179.1(2) . . . . ?
C9 C10 N3 Mo -162.48(16) . . . . ?
C11 C10 N3 Mo 16.1(3) . . . . ?
C7 N2 N3 C10 -0.8(2) . . . . ?
C6 N2 N3 C10 -174.80(18) . . . . ?
C7 N2 N3 Mo 165.58(14) . . . . ?
C6 N2 N3 Mo -8.4(2) . . . . ?
C15 C13 N4 N5 -0.9(3) . . . . ?
C14 C13 N4 N5 179.4(2) . . . . ?
C15 C13 N4 C12 -179.6(2) . . . . ?
C14 C13 N4 C12 0.7(4) . . . . ?
C5 C12 N4 C13 -152.7(2) . . . . ?
C5 C12 N4 N5 28.7(3) . . . . ?
C15 C16 N5 N4 -1.5(3) . . . . ?
C17 C16 N5 N4 179.1(2) . . . . ?
C15 C16 N5 Mo 169.64(17) . . . . ?
C17 C16 N5 Mo -9.8(4) . . . . ?
C13 N4 N5 C16 1.5(3) . . . . ?
C12 N4 N5 C16 -179.70(19) . . . . ?
C13 N4 N5 Mo -171.55(16) . . . . ?
C12 N4 N5 Mo 7.3(2) . . . . ?
C19 C18 O4 C18 -11.89(12) . . . 2_855 ?

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
N1 H1N O4 0.73(4) 2.05(4) 2.782(4) 180.000(0) 3_445

_refine_diff_density_max         0.459
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.069

####################################################################### 
# 
# 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_W
_database_code_depnum_ccdc_archive 'CCDC 1518991'
_audit_update_record             
;
2017-01-02 deposited with the CCDC.
2017-01-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H49 N9 O7.50 W2'
_chemical_formula_weight         1143.58

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'
W W -0.8490 6.8722 '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                   14.4325(9)
_cell_length_b                   14.7737(9)
_cell_length_c                   20.2936(13)
_cell_angle_alpha                90
_cell_angle_beta                 99.005(2)
_cell_angle_gamma                90
_cell_volume                     4273.7(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25049
_cell_measurement_theta_min      1.985
_cell_measurement_theta_max      24.999

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_F_000             2240
_exptl_transmission_factor_min   0.63
_exptl_transmission_factor_max   1.00
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.114
_exptl_absorpt_coefficient_mu    5.439
_shelx_estimated_absorpt_T_min   0.428
_shelx_estimated_absorpt_T_max   0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Brucker CCD APEX 2'
_diffrn_measurement_method       hemisphere
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25049
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.985
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3773
_reflns_number_gt                3531
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          squeeze
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 0.066 0.434 0.500 310 29 ' '
2 -0.089 0.411 1.000 310 29 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 620Å³ and 58 e, respectively. For Z = 4 this gives
14.5 electrons per formula. This number equals about one half of THF molecule
per fromula or 1.45 THF molecules per unit cell.
The fraction of solvent has been treated as a diffuse contribution 
to the overall scattering without specific atom positions.

 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'SMART APEX'
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    sir92
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ortep
_computing_publication_material  WinGx
_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)+(0.0277P)²+12.7564P] 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         3773
_refine_ls_number_parameters     259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_ref         0.0524
_refine_ls_wR_factor_gt          0.0514
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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
C1 C 0.1708(2) -0.0171(2) 0.17023(16) 0.0159(7) Uani 1 1 d . . . . .
C2 C 0.2132(2) 0.1075(2) 0.26359(18) 0.0169(7) Uani 1 1 d . . . . .
C3 C 0.2614(2) 0.1257(2) 0.13557(18) 0.0181(7) Uani 1 1 d . . . . .
C4 C -0.0113(2) 0.0444(2) 0.19374(16) 0.0152(7) Uani 1 1 d . . . . .
C5 C -0.0082(2) 0.1356(2) 0.21341(17) 0.0148(7) Uani 1 1 d . . . . .
C6 C -0.0499(2) 0.0026(2) 0.12798(16) 0.0182(7) Uani 1 1 d . . . . .
H6A H -0.0181 -0.0559 0.1234 0.022 Uiso 1 1 calc R U . . .
H6B H -0.1177 -0.0095 0.1264 0.022 Uiso 1 1 calc R U . . .
C7 C -0.0984(3) 0.0807(3) 0.01726(18) 0.0232(8) Uani 1 1 d . . . . .
C8 C -0.1926(3) 0.0385(3) 0.0027(2) 0.0310(9) Uani 1 1 d . . . . .
H8A H -0.1859 -0.0273 -0.0007 0.046 Uiso 1 1 calc R U . . .
H8B H -0.2260 0.0622 -0.0395 0.046 Uiso 1 1 calc R U . . .
H8C H -0.2282 0.0526 0.0388 0.046 Uiso 1 1 calc R U . . .
C9 C -0.0556(3) 0.1446(3) -0.01716(18) 0.0244(8) Uani 1 1 d . . . . .
H9 H -0.0810 0.1720 -0.0584 0.029 Uiso 1 1 calc R U . . .
C10 C 0.0326(2) 0.1615(2) 0.02047(17) 0.0209(7) Uani 1 1 d . . . . .
C11 C 0.1067(3) 0.2260(3) 0.00646(19) 0.0288(9) Uani 1 1 d . . . . .
H11A H 0.1034 0.2814 0.0326 0.043 Uiso 1 1 calc R U . . .
H11B H 0.0968 0.2409 -0.0412 0.043 Uiso 1 1 calc R U . . .
H11C H 0.1686 0.1980 0.0188 0.043 Uiso 1 1 calc R U . . .
C12 C -0.0506(2) 0.2154(2) 0.17337(17) 0.0167(7) Uani 1 1 d . . . . .
H12A H -0.0780 0.1951 0.1280 0.020 Uiso 1 1 calc R U . . .
H12B H -0.1017 0.2413 0.1948 0.020 Uiso 1 1 calc R U . . .
C13 C 0.0090(3) 0.3755(2) 0.1612(2) 0.0304(9) Uani 1 1 d . . . . .
C14 C -0.0848(3) 0.4191(3) 0.1563(3) 0.0457(13) Uani 1 1 d . . . . .
H14A H -0.1293 0.3883 0.1222 0.069 Uiso 1 1 calc R U . . .
H14B H -0.0800 0.4829 0.1442 0.069 Uiso 1 1 calc R U . . .
H14C H -0.1070 0.4148 0.1995 0.069 Uiso 1 1 calc R U . . .
C15 C 0.0976(3) 0.4109(3) 0.1606(2) 0.0317(10) Uani 1 1 d . . . . .
H15 H 0.1130 0.4729 0.1563 0.038 Uiso 1 1 calc R U . . .
C16 C 0.1597(2) 0.3381(2) 0.16769(17) 0.0208(7) Uani 1 1 d . . . . .
C17 C 0.2632(3) 0.3395(2) 0.1705(2) 0.0247(8) Uani 1 1 d . . . . .
H17A H 0.2919 0.2937 0.2023 0.037 Uiso 1 1 calc R U . . .
H17B H 0.2874 0.3995 0.1849 0.037 Uiso 1 1 calc R U . . .
H17C H 0.2787 0.3263 0.1262 0.037 Uiso 1 1 calc R U . . .
C18 C -0.0260(3) -0.2527(2) 0.30224(19) 0.0259(8) Uani 1 1 d . . . . .
H18A H -0.0863 -0.2323 0.3146 0.031 Uiso 1 1 calc R U . . .
H18B H 0.0227 -0.2505 0.3424 0.031 Uiso 1 1 calc R U . . .
C19 C -0.0351(3) -0.3474(2) 0.27399(19) 0.0256(8) Uani 1 1 d . . . . .
H19A H -0.0994 -0.3590 0.2505 0.031 Uiso 1 1 calc R U . . .
H19B H -0.0189 -0.3933 0.3094 0.031 Uiso 1 1 calc R U . . .
N1 N 0.0000 -0.0084(3) 0.2500 0.0169(8) Uani 1 2 d S T P . .
H1N H 0.0000 -0.065(4) 0.2500 0.020 Uiso 1 2 d S U P . .
N2 N -0.03669(19) 0.06154(19) 0.07280(14) 0.0174(6) Uani 1 1 d . . . . .
N3 N 0.0441(2) 0.11129(17) 0.07645(15) 0.0173(6) Uani 1 1 d . . . . .
N4 N 0.02005(19) 0.28511(19) 0.16852(15) 0.0179(6) Uani 1 1 d . . . . .
N5 N 0.11195(19) 0.25997(18) 0.17183(14) 0.0165(6) Uani 1 1 d . . . . .
O1 O 0.18774(18) -0.09527(16) 0.16936(13) 0.0229(6) Uani 1 1 d . . . . .
O2 O 0.24945(18) 0.10006(17) 0.31923(13) 0.0262(6) Uani 1 1 d . . . . .
O3 O 0.33056(17) 0.13112(17) 0.11261(13) 0.0233(6) Uani 1 1 d . . . . .
O4 O 0.0000 -0.1966(2) 0.2500 0.0283(8) Uani 1 2 d S T P . .
W W 0.14551(2) 0.11144(2) 0.17259(2) 0.01334(6) Uani 1 1 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
C1 O1 1.181(4) . ?
C1 W 1.936(3) . ?
C2 O2 1.173(4) . ?
C2 W 1.950(4) . ?
C3 O3 1.169(4) . ?
C3 W 1.949(4) . ?
C4 N1 1.372(4) . ?
C4 C5 1.404(5) . ?
C4 C6 1.497(5) . ?
C4 W 2.567(3) . ?
C5 C5 1.467(7) 2 ?
C5 C12 1.507(5) . ?
C5 W 2.511(3) . ?
C6 N2 1.454(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N2 1.352(5) . ?
C7 C9 1.377(5) . ?
C7 C8 1.484(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.400(5) . ?
C9 H9 0.9500 . ?
C10 N3 1.345(4) . ?
C10 C11 1.493(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N4 1.462(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N4 1.350(4) . ?
C13 C15 1.382(6) . ?
C13 C14 1.489(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.394(5) . ?
C15 H15 0.9500 . ?
C16 N5 1.353(4) . ?
C16 C17 1.486(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O4 1.442(4) . ?
C18 C19 1.509(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C19 1.511(7) 2 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
N1 C4 1.372(4) 2 ?
N1 H1N 0.83(6) . ?
N2 N3 1.371(4) . ?
N3 W 2.248(3) . ?
N4 N5 1.369(4) . ?
N5 W 2.247(3) . ?
O4 C18 1.442(4) 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 C1 W 178.9(3) . . ?
O2 C2 W 175.0(3) . . ?
O3 C3 W 177.6(3) . . ?
N1 C4 C5 108.4(3) . . ?
N1 C4 C6 119.1(3) . . ?
C5 C4 C6 129.8(3) . . ?
N1 C4 W 111.45(17) . . ?
C5 C4 W 71.78(18) . . ?
C6 C4 W 103.0(2) . . ?
C4 C5 C5 106.31(19) . 2 ?
C4 C5 C12 127.3(3) . . ?
C5 C5 C12 122.2(2) 2 . ?
C4 C5 W 76.15(18) . . ?
C5 C5 W 108.9(3) 2 . ?
C12 C5 W 103.8(2) . . ?
N2 C6 C4 111.4(3) . . ?
N2 C6 H6A 109.4 . . ?
C4 C6 H6A 109.4 . . ?
N2 C6 H6B 109.4 . . ?
C4 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
N2 C7 C9 106.1(3) . . ?
N2 C7 C8 122.8(3) . . ?
C9 C7 C8 131.1(4) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 C10 106.6(3) . . ?
C7 C9 H9 126.7 . . ?
C10 C9 H9 126.7 . . ?
N3 C10 C9 110.2(3) . . ?
N3 C10 C11 121.0(3) . . ?
C9 C10 C11 128.8(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N4 C12 C5 111.0(3) . . ?
N4 C12 H12A 109.4 . . ?
C5 C12 H12A 109.4 . . ?
N4 C12 H12B 109.4 . . ?
C5 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
N4 C13 C15 106.4(3) . . ?
N4 C13 C14 121.7(3) . . ?
C15 C13 C14 131.9(3) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 C16 106.8(3) . . ?
C13 C15 H15 126.6 . . ?
C16 C15 H15 126.6 . . ?
N5 C16 C15 109.8(3) . . ?
N5 C16 C17 121.9(3) . . ?
C15 C16 C17 128.3(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O4 C18 C19 105.7(3) . . ?
O4 C18 H18A 110.6 . . ?
C19 C18 H18A 110.6 . . ?
O4 C18 H18B 110.6 . . ?
C19 C18 H18B 110.6 . . ?
H18A C18 H18B 108.7 . . ?
C18 C19 C19 102.6(2) . 2 ?
C18 C19 H19A 111.3 . . ?
C19 C19 H19A 111.3 2 . ?
C18 C19 H19B 111.3 . . ?
C19 C19 H19B 111.3 2 . ?
H19A C19 H19B 109.2 . . ?
C4 N1 C4 110.6(4) 2 . ?
C4 N1 H1N 124.7(2) 2 . ?
C4 N1 H1N 124.7(2) . . ?
C7 N2 N3 112.1(3) . . ?
C7 N2 C6 128.2(3) . . ?
N3 N2 C6 119.5(3) . . ?
C10 N3 N2 105.0(3) . . ?
C10 N3 W 135.3(2) . . ?
N2 N3 W 118.7(2) . . ?
C13 N4 N5 111.7(3) . . ?
C13 N4 C12 129.2(3) . . ?
N5 N4 C12 119.1(3) . . ?
C16 N5 N4 105.3(3) . . ?
C16 N5 W 136.2(2) . . ?
N4 N5 W 118.1(2) . . ?
C18 O4 C18 109.7(4) . 2 ?
C1 W C3 85.39(13) . . ?
C1 W C2 85.72(13) . . ?
C3 W C2 92.02(14) . . ?
C1 W N5 177.80(12) . . ?
C3 W N5 95.11(12) . . ?
C2 W N5 96.40(12) . . ?
C1 W N3 94.44(11) . . ?
C3 W N3 98.44(13) . . ?
C2 W N3 169.52(12) . . ?
N5 W N3 83.37(10) . . ?
C1 W C5 109.12(12) . . ?
C3 W C5 165.25(12) . . ?
C2 W C5 91.69(13) . . ?
N5 W C5 70.29(10) . . ?
N3 W C5 78.34(11) . . ?
C1 W C4 78.50(12) . . ?
C3 W C4 159.74(12) . . ?
C2 W C4 98.88(12) . . ?
N5 W C4 100.55(10) . . ?
N3 W C4 70.95(10) . . ?
C5 W C4 32.07(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
N1 C4 C5 C5 1.2(4) . . . 2 ?
C6 C4 C5 C5 162.1(3) . . . 2 ?
W C4 C5 C5 -106.0(3) . . . 2 ?
N1 C4 C5 C12 -155.8(3) . . . . ?
C6 C4 C5 C12 5.0(6) . . . . ?
W C4 C5 C12 97.0(3) . . . . ?
N1 C4 C5 W 107.2(2) . . . . ?
C6 C4 C5 W -91.9(3) . . . . ?
N1 C4 C6 N2 -166.6(2) . . . . ?
C5 C4 C6 N2 34.3(5) . . . . ?
W C4 C6 N2 -42.7(3) . . . . ?
N2 C7 C9 C10 0.0(4) . . . . ?
C8 C7 C9 C10 178.3(4) . . . . ?
C7 C9 C10 N3 -0.8(4) . . . . ?
C7 C9 C10 C11 -178.9(4) . . . . ?
C4 C5 C12 N4 -125.5(3) . . . . ?
C5 C5 C12 N4 80.8(4) 2 . . . ?
W C5 C12 N4 -42.5(3) . . . . ?
N4 C13 C15 C16 0.1(5) . . . . ?
C14 C13 C15 C16 179.2(5) . . . . ?
C13 C15 C16 N5 0.6(5) . . . . ?
C13 C15 C16 C17 -179.6(4) . . . . ?
O4 C18 C19 C19 30.3(4) . . . 2 ?
C5 C4 N1 C4 -0.50(16) . . . 2 ?
C6 C4 N1 C4 -163.7(3) . . . 2 ?
W C4 N1 C4 76.59(15) . . . 2 ?
C9 C7 N2 N3 0.8(4) . . . . ?
C8 C7 N2 N3 -177.7(3) . . . . ?
C9 C7 N2 C6 175.7(3) . . . . ?
C8 C7 N2 C6 -2.8(6) . . . . ?
C4 C6 N2 C7 -137.1(3) . . . . ?
C4 C6 N2 N3 37.4(4) . . . . ?
C9 C10 N3 N2 1.3(4) . . . . ?
C11 C10 N3 N2 179.6(3) . . . . ?
C9 C10 N3 W -166.1(3) . . . . ?
C11 C10 N3 W 12.2(5) . . . . ?
C7 N2 N3 C10 -1.3(4) . . . . ?
C6 N2 N3 C10 -176.7(3) . . . . ?
C7 N2 N3 W 168.6(2) . . . . ?
C6 N2 N3 W -6.8(4) . . . . ?
C15 C13 N4 N5 -0.8(5) . . . . ?
C14 C13 N4 N5 179.9(4) . . . . ?
C15 C13 N4 C12 178.8(4) . . . . ?
C14 C13 N4 C12 -0.4(7) . . . . ?
C5 C12 N4 C13 -151.8(4) . . . . ?
C5 C12 N4 N5 27.8(4) . . . . ?
C15 C16 N5 N4 -1.1(4) . . . . ?
C17 C16 N5 N4 179.1(3) . . . . ?
C15 C16 N5 W 172.0(3) . . . . ?
C17 C16 N5 W -7.9(5) . . . . ?
C13 N4 N5 C16 1.2(4) . . . . ?
C12 N4 N5 C16 -178.5(3) . . . . ?
C13 N4 N5 W -173.4(3) . . . . ?
C12 N4 N5 W 7.0(4) . . . . ?
C19 C18 O4 C18 -11.78(17) . . . 2 ?

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
N1 H1N O4 0.83(6) 1.95(6) 2.779(5) 180.000(0) .

_refine_diff_density_max         1.091
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.102



#===========================================================================END
