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

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

data_Compound-1
_database_code_depnum_ccdc_archive 'CCDC 1057618'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;


#=============================================================================
_audit_creation_method           'SHELXL-2014/6, manual editing plus enCIFer'
_audit_creation_date             '02 April 2015'
#=============================================================================

#=============================================================================
# GENERAL AND CHEMICAL DATA
#=============================================================================

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H22 Cl2 Mo N2 O4'
_chemical_formula_sum            'C18 H22 Cl2 Mo N2 O4'
_chemical_formula_weight         497.21

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'
Cl Cl 0.1484 0.1585 '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'


#=============================================================================
# CRYSTAL DATA
#=============================================================================

_space_group_crystal_system      Orthorhombic
_space_group_IT_number           43
_space_group_name_H-M_alt        'F d d 2'
_space_group_name_Hall           'F 2 -2d'

_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+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'

_cell_length_a                   16.9586(11)
_cell_length_b                   27.5327(19)
_cell_length_c                   8.5225(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3979.3(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    3202
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      28.55

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_F_000             2016
_exptl_transmission_factor_min   0.6652
_exptl_transmission_factor_max   0.7458
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.954
_shelx_estimated_absorpt_T_min   0.832
_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 V2012/1 (Bruker AXS Inc.) 
;

#=============================================================================
# EXPERIMENTAL DATA
#============================================================================= 

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      180(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 X8 Kappa CCD APEX II'
_diffrn_measurement_method       'ω / φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8189
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.813
_diffrn_reflns_theta_max         29.114
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             2605
_reflns_number_gt                2377
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.833
_reflns_Friedel_fraction_max     0.944
_reflns_Friedel_fraction_full    0.979

_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       'APEX2 2012.4 (Bruker AXS Inc., 2012)'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'


#=============================================================================
# REFINEMENT DATA
#=============================================================================

_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)+(0.0227P)²+2.3684P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1007 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2605
_refine_ls_number_parameters     125
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0736
_refine_ls_wR_factor_gt          0.0705
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000


#=============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
#=============================================================================

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 0.5000 0.5000 0.72898(6) 0.02802(13) Uani 1 2 d S T P . .
Cl1 Cl 0.39405(7) 0.55467(4) 0.68059(14) 0.0395(3) Uani 1 1 d . . . . .
O1 O 0.44675(16) 0.46144(11) 0.5264(3) 0.0290(6) Uani 1 1 d . . . . .
O2 O 0.4526(2) 0.46286(15) 0.8540(4) 0.0473(9) Uani 1 1 d . . . . .
N1 N 0.3831(2) 0.43182(13) 0.3187(4) 0.0271(7) Uani 1 1 d . . . . .
C1 C 0.4573(3) 0.43291(19) 0.2314(5) 0.0412(11) Uani 1 1 d . . . . .
H1A H 0.4837 0.4014 0.2410 0.062 Uiso 1 1 calc R U . . .
H1B H 0.4914 0.4584 0.2742 0.062 Uiso 1 1 calc R U . . .
H1C H 0.4465 0.4396 0.1206 0.062 Uiso 1 1 calc R U . . .
C2 C 0.3168(3) 0.40879(18) 0.2380(6) 0.0380(10) Uani 1 1 d . . . . .
H2A H 0.2725 0.4052 0.3110 0.057 Uiso 1 1 calc R U . . .
H2B H 0.3328 0.3767 0.1998 0.057 Uiso 1 1 calc R U . . .
H2C H 0.3005 0.4290 0.1490 0.057 Uiso 1 1 calc R U . . .
C3 C 0.3831(2) 0.44621(13) 0.4679(5) 0.0230(7) Uani 1 1 d . . . . .
C4 C 0.3093(2) 0.44353(14) 0.5622(4) 0.0233(8) Uani 1 1 d . . . . .
C5 C 0.3107(2) 0.41624(14) 0.7006(5) 0.0259(8) Uani 1 1 d . . . . .
H5 H 0.3576 0.4001 0.7316 0.031 Uiso 1 1 calc R U . . .
C6 C 0.2437(2) 0.41283(17) 0.7922(5) 0.0288(9) Uani 1 1 d . . . . .
H6 H 0.2447 0.3939 0.8854 0.035 Uiso 1 1 calc R U . . .
C7 C 0.1749(3) 0.43689(17) 0.7490(5) 0.0336(10) Uani 1 1 d . . . . .
H7 H 0.1293 0.4351 0.8135 0.040 Uiso 1 1 calc R U . . .
C8 C 0.1733(3) 0.46362(17) 0.6104(6) 0.0341(10) Uani 1 1 d . . . . .
H8 H 0.1263 0.4797 0.5794 0.041 Uiso 1 1 calc R U . . .
C9 C 0.2405(2) 0.46693(15) 0.5170(5) 0.0285(10) Uani 1 1 d . . . . .
H9 H 0.2392 0.4852 0.4224 0.034 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.
;

#=============================================================================
# GEOMETRY
#============================================================================= 

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 O2 1.681(3) 2_665 ?
Mo1 O2 1.681(3) . ?
Mo1 O1 2.219(3) . ?
Mo1 O1 2.219(3) 2_665 ?
Mo1 Cl1 2.3800(12) . ?
Mo1 Cl1 2.3800(12) 2_665 ?
O1 C3 1.261(5) . ?
N1 C3 1.332(5) . ?
N1 C1 1.462(6) . ?
N1 C2 1.463(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.489(5) . ?
C4 C9 1.388(6) . ?
C4 C5 1.398(5) . ?
C5 C6 1.381(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.392(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.392(7) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(6) . ?
C8 H8 0.9500 . ?
C9 H9 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
O2 Mo1 O2 101.3(2) 2_665 . ?
O2 Mo1 O1 168.15(16) 2_665 . ?
O2 Mo1 O1 90.45(14) . . ?
O2 Mo1 O1 90.45(14) 2_665 2_665 ?
O2 Mo1 O1 168.15(16) . 2_665 ?
O1 Mo1 O1 77.82(15) . 2_665 ?
O2 Mo1 Cl1 94.92(14) 2_665 . ?
O2 Mo1 Cl1 97.69(14) . . ?
O1 Mo1 Cl1 81.98(8) . . ?
O1 Mo1 Cl1 82.52(8) 2_665 . ?
O2 Mo1 Cl1 97.69(14) 2_665 2_665 ?
O2 Mo1 Cl1 94.93(14) . 2_665 ?
O1 Mo1 Cl1 82.52(8) . 2_665 ?
O1 Mo1 Cl1 81.98(8) 2_665 2_665 ?
Cl1 Mo1 Cl1 160.04(6) . 2_665 ?
C3 O1 Mo1 144.6(3) . . ?
C3 N1 C1 118.6(4) . . ?
C3 N1 C2 125.3(4) . . ?
C1 N1 C2 115.5(4) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O1 C3 N1 118.5(4) . . ?
O1 C3 C4 121.5(3) . . ?
N1 C3 C4 120.0(3) . . ?
C9 C4 C5 119.8(4) . . ?
C9 C4 C3 122.2(3) . . ?
C5 C4 C3 117.9(3) . . ?
C6 C5 C4 120.0(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 120.5(4) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C8 C7 C6 119.5(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C9 120.3(4) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C4 C9 C8 119.9(4) . . ?
C4 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?

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
Mo1 O1 C3 N1 167.4(3) . . . . ?
Mo1 O1 C3 C4 -13.4(7) . . . . ?
C1 N1 C3 O1 1.9(6) . . . . ?
C2 N1 C3 O1 173.5(4) . . . . ?
C1 N1 C3 C4 -177.3(4) . . . . ?
C2 N1 C3 C4 -5.7(6) . . . . ?
O1 C3 C4 C9 123.4(4) . . . . ?
N1 C3 C4 C9 -57.4(5) . . . . ?
O1 C3 C4 C5 -56.7(5) . . . . ?
N1 C3 C4 C5 122.5(4) . . . . ?
C9 C4 C5 C6 -0.3(6) . . . . ?
C3 C4 C5 C6 179.8(4) . . . . ?
C4 C5 C6 C7 -0.8(6) . . . . ?
C5 C6 C7 C8 1.5(6) . . . . ?
C6 C7 C8 C9 -1.0(7) . . . . ?
C5 C4 C9 C8 0.8(6) . . . . ?
C3 C4 C9 C8 -179.4(4) . . . . ?
C7 C8 C9 C4 -0.1(7) . . . . ?

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
C1 H1C O2 0.98 2.36 3.321(6) 165.9 1_554

_refine_diff_density_max         0.378
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.072
_shelxl_version_number           2014/6


#=============================================================================
#   SHELXL Ins File
#=============================================================================

####################################################################### 
# 
# 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_Compound-2
_database_code_depnum_ccdc_archive 'CCDC 1057619'
_audit_update_record             
;
2015-04-02 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;


#=============================================================================
_audit_creation_method           'SHELXL-2014/6, manual editing plus enCIFer'
_audit_creation_date             '02 April 2015'
#=============================================================================

#=============================================================================
# GENERAL AND CHEMICAL DATA
#=============================================================================

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C6 H12 Cl2 Mo N2 O4), C6 H12 N2 O2, C2 H3 N'
_chemical_formula_sum            'C20 H39 Cl4 Mo2 N7 O10'
_chemical_formula_weight         871.26

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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


#=============================================================================
# CRYSTAL DATA
#=============================================================================

_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                   9.6274(7)
_cell_length_b                   12.3705(9)
_cell_length_c                   16.4500(11)
_cell_angle_alpha                96.854(3)
_cell_angle_beta                 105.901(3)
_cell_angle_gamma                107.175(4)
_cell_volume                     1756.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    9861
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      30.40

_exptl_crystal_description       Plate
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             880
_exptl_transmission_factor_min   0.2298
_exptl_transmission_factor_max   0.2656
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.073
_shelx_estimated_absorpt_T_min   0.847
_shelx_estimated_absorpt_T_max   0.891
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
; 
 SADABS V2012/1 (Bruker AXS Inc.) 
;

#=============================================================================
# EXPERIMENTAL DATA
#============================================================================= 

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      180(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 X8 Kappa CCD APEX II'
_diffrn_measurement_method       'ω / φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43689
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.515
_diffrn_reflns_theta_max         29.129
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9428
_reflns_number_gt                7851
_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       'APEX2 2012.4 (Bruker AXS Inc., 2012)'
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'


#=============================================================================
# REFINEMENT DATA
#=============================================================================

_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)+(0.0270P)²+1.3078P] 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         9428
_refine_ls_number_parameters     442
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0754
_refine_ls_wR_factor_gt          0.0702
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


#=============================================================================
# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
#=============================================================================

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 0.44713(2) 0.54908(2) 0.24515(2) 0.02767(6) Uani 1 1 d . . . . .
Mo2 Mo 0.79371(2) 0.15958(2) 0.20403(2) 0.03503(6) Uani 1 1 d . . . . .
Cl1 Cl 0.19725(7) 0.51943(5) 0.15076(4) 0.03642(13) Uani 1 1 d . . . . .
Cl2 Cl 0.66440(7) 0.51683(6) 0.33599(4) 0.04109(14) Uani 1 1 d . . . . .
Cl3 Cl 0.63747(8) 0.18165(6) 0.28914(5) 0.04484(15) Uani 1 1 d . . . . .
Cl4 Cl 0.97014(7) 0.20893(6) 0.12719(5) 0.04859(17) Uani 1 1 d . . . . .
O1 O 0.5424(2) 0.62081(15) 0.18492(11) 0.0423(4) Uani 1 1 d . . . . .
O2 O 0.4443(2) 0.65385(15) 0.31993(11) 0.0440(4) Uani 1 1 d . . . . .
O3 O 0.8808(2) 0.07963(16) 0.26159(15) 0.0570(6) Uani 1 1 d . . . . .
O4 O 0.6510(2) 0.06298(15) 0.11972(13) 0.0462(5) Uani 1 1 d . . . . .
O5 O 0.41232(18) 0.37983(13) 0.16390(9) 0.0269(3) Uani 1 1 d . . . . .
O6 O 0.32678(18) 0.40628(13) 0.29786(9) 0.0269(3) Uani 1 1 d . . . . .
O7 O 0.95571(18) 0.32397(13) 0.29808(11) 0.0343(4) Uani 1 1 d . . . . .
O8 O 0.74068(18) 0.30823(13) 0.15733(10) 0.0313(3) Uani 1 1 d . . . . .
N1 N 0.3159(2) 0.18431(16) 0.13801(11) 0.0251(4) Uani 1 1 d D . . . .
H1 H 0.266(3) 0.1213(16) 0.1582(15) 0.038 Uiso 1 1 d D U . . .
N2 N 0.2792(2) 0.21972(16) 0.30782(11) 0.0260(4) Uani 1 1 d D . . . .
H2 H 0.269(3) 0.1447(12) 0.2830(15) 0.039 Uiso 1 1 d D U . . .
N3 N 1.0403(2) 0.51927(16) 0.33035(12) 0.0280(4) Uani 1 1 d D . . . .
H3 H 1.031(3) 0.5848(15) 0.3095(16) 0.042 Uiso 1 1 d D U . . .
N4 N 0.8298(2) 0.49861(16) 0.16112(12) 0.0284(4) Uani 1 1 d D . . . .
H4 H 0.904(2) 0.5698(13) 0.1936(15) 0.043 Uiso 1 1 d D U . . .
C1 C 0.1932(3) 0.1106(2) -0.01880(15) 0.0386(6) Uani 1 1 d . . . . .
H1A H 0.1374 0.0338 -0.0120 0.058 Uiso 1 1 calc R U . . .
H1B H 0.2140 0.1031 -0.0739 0.058 Uiso 1 1 calc R U . . .
H1C H 0.1308 0.1604 -0.0183 0.058 Uiso 1 1 calc R U . . .
C2 C 0.3434(3) 0.1638(2) 0.05499(13) 0.0292(5) Uani 1 1 d . . . . .
H2A H 0.4038 0.1113 0.0567 0.035 Uiso 1 1 calc R U . . .
H2B H 0.4040 0.2382 0.0454 0.035 Uiso 1 1 calc R U . . .
C3 C 0.3510(2) 0.28742(18) 0.18410(13) 0.0229(4) Uani 1 1 d . . . . .
C4 C 0.3147(2) 0.30454(18) 0.26885(12) 0.0228(4) Uani 1 1 d . . . . .
C5 C 0.2504(3) 0.2377(2) 0.39098(13) 0.0299(5) Uani 1 1 d . . . . .
H5A H 0.1969 0.1618 0.4015 0.036 Uiso 1 1 calc R U . . .
H5B H 0.1824 0.2846 0.3880 0.036 Uiso 1 1 calc R U . . .
C6 C 0.3983(3) 0.2987(3) 0.46525(16) 0.0480(7) Uani 1 1 d . . . . .
H6A H 0.4635 0.2505 0.4703 0.072 Uiso 1 1 calc R U . . .
H6B H 0.3750 0.3119 0.5192 0.072 Uiso 1 1 calc R U . . .
H6C H 0.4525 0.3733 0.4544 0.072 Uiso 1 1 calc R U . . .
C7 C 1.1695(4) 0.6425(3) 0.47480(18) 0.0535(8) Uani 1 1 d . . . . .
H7A H 1.2154 0.7095 0.4525 0.080 Uiso 1 1 calc R U . . .
H7B H 1.2369 0.6476 0.5329 0.080 Uiso 1 1 calc R U . . .
H7C H 1.0689 0.6418 0.4775 0.080 Uiso 1 1 calc R U . . .
C8 C 1.1503(3) 0.5333(2) 0.41586(14) 0.0347(5) Uani 1 1 d . . . . .
H8A H 1.2509 0.5361 0.4100 0.042 Uiso 1 1 calc R U . . .
H8B H 1.1131 0.4660 0.4410 0.042 Uiso 1 1 calc R U . . .
C9 C 0.9526(2) 0.41870(18) 0.27977(14) 0.0252(4) Uani 1 1 d . . . . .
C10 C 0.8325(2) 0.40842(19) 0.19401(14) 0.0261(4) Uani 1 1 d . . . . .
C11 C 0.7205(3) 0.4899(2) 0.07643(14) 0.0361(5) Uani 1 1 d . . . . .
H11A H 0.6145 0.4641 0.0790 0.043 Uiso 1 1 calc R U . . .
H11B H 0.7272 0.4316 0.0322 0.043 Uiso 1 1 calc R U . . .
C12 C 0.7559(4) 0.6054(2) 0.05143(16) 0.0452(7) Uani 1 1 d . . . . .
H12A H 0.7433 0.6618 0.0935 0.068 Uiso 1 1 calc R U . . .
H12B H 0.6854 0.5977 -0.0064 0.068 Uiso 1 1 calc R U . . .
H12C H 0.8620 0.6319 0.0509 0.068 Uiso 1 1 calc R U . . .
O9 O 0.1699(2) 0.98579(14) 0.19685(12) 0.0437(4) Uani 1 1 d . . . . .
O10 O 0.05298(19) 0.71989(13) 0.25645(11) 0.0339(4) Uani 1 1 d . . . . .
N5 N 0.2246(7) 0.8295(4) 0.1632(4) 0.0292(11) Uani 0.582(10) 1 d D . P A 1
H5 H 0.201(3) 0.7505(8) 0.1708(15) 0.044 Uiso 0.582(10) 1 d D U P A 1
C13 C 0.4096(9) 0.8068(5) 0.0930(5) 0.0608(19) Uani 0.582(10) 1 d . U P A 1
H13A H 0.4753 0.7957 0.1461 0.091 Uiso 0.582(10) 1 calc R U P A 1
H13B H 0.4733 0.8432 0.0596 0.091 Uiso 0.582(10) 1 calc R U P A 1
H13C H 0.3355 0.7315 0.0582 0.091 Uiso 0.582(10) 1 calc R U P A 1
C14 C 0.3265(7) 0.8819(4) 0.1155(4) 0.0373(14) Uani 0.582(10) 1 d . . P A 1
H14A H 0.2646 0.8964 0.0618 0.056 Uiso 0.582(10) 1 calc R U P A 1
H14B H 0.4017 0.9574 0.1514 0.056 Uiso 0.582(10) 1 calc R U P A 1
N5' N 0.2645(9) 0.8256(7) 0.1957(6) 0.0311(16) Uani 0.418(10) 1 d D . P A 2
H5' H 0.201(3) 0.7505(8) 0.1708(15) 0.047 Uiso 0.418(10) 1 d D U P A 2
C13' C 0.3331(13) 0.8206(8) 0.0635(6) 0.062(3) Uani 0.418(10) 1 d . U P A 2
H13D H 0.3026 0.7359 0.0519 0.093 Uiso 0.418(10) 1 calc R U P A 2
H13E H 0.4164 0.8525 0.0404 0.093 Uiso 0.418(10) 1 calc R U P A 2
H13F H 0.2447 0.8426 0.0357 0.093 Uiso 0.418(10) 1 calc R U P A 2
C14' C 0.3869(9) 0.8674(6) 0.1587(5) 0.036(2) Uani 0.418(10) 1 d . . P A 2
H14C H 0.4748 0.8437 0.1869 0.055 Uiso 0.418(10) 1 calc R U P A 2
H14D H 0.4231 0.9532 0.1705 0.055 Uiso 0.418(10) 1 calc R U P A 2
N6 N -0.0353(2) 0.86978(16) 0.26713(12) 0.0295(4) Uani 1 1 d D . . . .
H6 H -0.016(3) 0.9459(11) 0.2605(17) 0.044 Uiso 1 1 d D U . . .
C15 C 0.1618(3) 0.8858(2) 0.20337(16) 0.0377(6) Uani 1 1 d . . . . .
C16 C 0.0539(3) 0.81746(19) 0.24628(14) 0.0270(4) Uani 1 1 d . . . . .
C17 C -0.1413(3) 0.8228(2) 0.31249(18) 0.0406(6) Uani 1 1 d . . . . .
H17A H -0.1694 0.7374 0.3013 0.049 Uiso 1 1 calc R U . . .
H17B H -0.2365 0.8406 0.2897 0.049 Uiso 1 1 calc R U . . .
C18 C -0.0737(4) 0.8713(3) 0.4079(2) 0.0674(10) Uani 1 1 d . . . . .
H18A H 0.0224 0.8560 0.4304 0.101 Uiso 1 1 calc R U . . .
H18B H -0.1464 0.8345 0.4364 0.101 Uiso 1 1 calc R U . . .
H18C H -0.0526 0.9551 0.4194 0.101 Uiso 1 1 calc R U . . .
N7 N 0.3460(4) -0.0052(3) 0.3957(2) 0.0909(11) Uani 1 1 d . . . . .
C19 C 0.5849(5) -0.0583(3) 0.3908(3) 0.0723(10) Uani 1 1 d . . . . .
H19A H 0.6633 -0.0298 0.4482 0.108 Uiso 1 1 calc R U . . .
H19B H 0.6261 -0.0222 0.3486 0.108 Uiso 1 1 calc R U . . .
H19C H 0.5559 -0.1427 0.3739 0.108 Uiso 1 1 calc R U . . .
C20 C 0.4517(5) -0.0294(3) 0.3932(2) 0.0664(9) 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.
;

#=============================================================================
# GEOMETRY
#============================================================================= 

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 O1 1.6847(17) . ?
Mo1 O2 1.6888(17) . ?
Mo1 O6 2.2186(14) . ?
Mo1 O5 2.2259(15) . ?
Mo1 Cl1 2.3726(6) . ?
Mo1 Cl2 2.3853(7) . ?
Mo2 O4 1.6823(18) . ?
Mo2 O3 1.6901(18) . ?
Mo2 O8 2.2157(15) . ?
Mo2 O7 2.2394(16) . ?
Mo2 Cl3 2.3669(8) . ?
Mo2 Cl4 2.3673(8) . ?
O5 C3 1.251(2) . ?
O6 C4 1.251(2) . ?
O7 C9 1.251(2) . ?
O8 C10 1.251(3) . ?
N1 C3 1.300(3) . ?
N1 C2 1.468(3) . ?
N1 H1 0.936(10) . ?
N2 C4 1.303(3) . ?
N2 C5 1.472(3) . ?
N2 H2 0.933(10) . ?
N3 C9 1.304(3) . ?
N3 C8 1.465(3) . ?
N3 H3 0.936(10) . ?
N4 C10 1.301(3) . ?
N4 C11 1.467(3) . ?
N4 H4 0.936(10) . ?
C1 C2 1.511(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.533(3) . ?
C5 C6 1.510(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.496(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.523(3) . ?
C11 C12 1.502(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
O9 C15 1.235(3) . ?
O10 C16 1.236(3) . ?
N5 C15 1.283(6) . ?
N5 C14 1.472(7) . ?
N5 H5 0.967(9) . ?
C13 C14 1.469(9) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
N5' C15 1.425(9) . ?
N5' C14' 1.461(10) . ?
N5' H5' 0.918(9) . ?
C13' C14' 1.489(13) . ?
C13' H13D 0.9800 . ?
C13' H13E 0.9800 . ?
C13' H13F 0.9800 . ?
C14' H14C 0.9900 . ?
C14' H14D 0.9900 . ?
N6 C16 1.308(3) . ?
N6 C17 1.451(3) . ?
N6 H6 0.930(10) . ?
C15 C16 1.523(3) . ?
C17 C18 1.494(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N7 C20 1.152(5) . ?
C19 C20 1.438(5) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 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
O1 Mo1 O2 104.89(9) . . ?
O1 Mo1 O6 161.32(8) . . ?
O2 Mo1 O6 93.68(7) . . ?
O1 Mo1 O5 90.72(7) . . ?
O2 Mo1 O5 164.36(7) . . ?
O6 Mo1 O5 70.76(5) . . ?
O1 Mo1 Cl1 95.84(7) . . ?
O2 Mo1 Cl1 94.43(7) . . ?
O6 Mo1 Cl1 84.57(4) . . ?
O5 Mo1 Cl1 82.86(4) . . ?
O1 Mo1 Cl2 95.26(7) . . ?
O2 Mo1 Cl2 95.77(7) . . ?
O6 Mo1 Cl2 80.59(4) . . ?
O5 Mo1 Cl2 83.47(4) . . ?
Cl1 Mo1 Cl2 162.47(2) . . ?
O4 Mo2 O3 105.14(10) . . ?
O4 Mo2 O8 92.35(8) . . ?
O3 Mo2 O8 162.35(8) . . ?
O4 Mo2 O7 163.44(8) . . ?
O3 Mo2 O7 91.42(8) . . ?
O8 Mo2 O7 71.11(6) . . ?
O4 Mo2 Cl3 96.07(7) . . ?
O3 Mo2 Cl3 97.33(8) . . ?
O8 Mo2 Cl3 82.89(5) . . ?
O7 Mo2 Cl3 81.30(5) . . ?
O4 Mo2 Cl4 95.37(7) . . ?
O3 Mo2 Cl4 95.73(8) . . ?
O8 Mo2 Cl4 80.01(5) . . ?
O7 Mo2 Cl4 82.98(5) . . ?
Cl3 Mo2 Cl4 159.76(3) . . ?
C3 O5 Mo1 119.80(13) . . ?
C4 O6 Mo1 119.31(13) . . ?
C9 O7 Mo2 118.75(14) . . ?
C10 O8 Mo2 118.50(14) . . ?
C3 N1 C2 123.07(18) . . ?
C3 N1 H1 117.2(16) . . ?
C2 N1 H1 119.6(16) . . ?
C4 N2 C5 121.62(19) . . ?
C4 N2 H2 120.7(16) . . ?
C5 N2 H2 117.7(16) . . ?
C9 N3 C8 123.52(19) . . ?
C9 N3 H3 116.7(17) . . ?
C8 N3 H3 119.8(17) . . ?
C10 N4 C11 122.27(19) . . ?
C10 N4 H4 116.5(16) . . ?
C11 N4 H4 121.2(16) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C1 110.81(19) . . ?
N1 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O5 C3 N1 124.64(19) . . ?
O5 C3 C4 114.17(18) . . ?
N1 C3 C4 121.17(18) . . ?
O6 C4 N2 123.66(19) . . ?
O6 C4 C3 114.44(17) . . ?
N2 C4 C3 121.87(19) . . ?
N2 C5 C6 111.5(2) . . ?
N2 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
N2 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C8 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C7 110.4(2) . . ?
N3 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
N3 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
O7 C9 N3 123.7(2) . . ?
O7 C9 C10 114.65(19) . . ?
N3 C9 C10 121.56(19) . . ?
O8 C10 N4 123.0(2) . . ?
O8 C10 C9 115.65(18) . . ?
N4 C10 C9 121.32(19) . . ?
N4 C11 C12 110.1(2) . . ?
N4 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N4 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C15 N5 C14 123.4(4) . . ?
C15 N5 H5 111.5(18) . . ?
C14 N5 H5 125.0(18) . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C13 C14 N5 111.8(5) . . ?
C13 C14 H14A 109.3 . . ?
N5 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
N5 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
C15 N5' C14' 122.7(6) . . ?
C15 N5' H5' 103.7(18) . . ?
C14' N5' H5' 114.3(19) . . ?
C14' C13' H13D 109.5 . . ?
C14' C13' H13E 109.5 . . ?
H13D C13' H13E 109.5 . . ?
C14' C13' H13F 109.5 . . ?
H13D C13' H13F 109.5 . . ?
H13E C13' H13F 109.5 . . ?
N5' C14' C13' 111.5(6) . . ?
N5' C14' H14C 109.3 . . ?
C13' C14' H14C 109.3 . . ?
N5' C14' H14D 109.3 . . ?
C13' C14' H14D 109.3 . . ?
H14C C14' H14D 108.0 . . ?
C16 N6 C17 123.3(2) . . ?
C16 N6 H6 116.2(18) . . ?
C17 N6 H6 119.6(18) . . ?
O9 C15 N5 121.5(3) . . ?
O9 C15 N5' 130.1(4) . . ?
O9 C15 C16 120.9(2) . . ?
N5 C15 C16 116.8(3) . . ?
N5' C15 C16 107.3(4) . . ?
O10 C16 N6 125.7(2) . . ?
O10 C16 C15 120.1(2) . . ?
N6 C16 C15 114.1(2) . . ?
N6 C17 C18 112.0(2) . . ?
N6 C17 H17A 109.2 . . ?
C18 C17 H17A 109.2 . . ?
N6 C17 H17B 109.2 . . ?
C18 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N7 C20 C19 179.3(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
C3 N1 C2 C1 -113.0(2) . . . . ?
Mo1 O5 C3 N1 175.04(16) . . . . ?
Mo1 O5 C3 C4 -3.4(2) . . . . ?
C2 N1 C3 O5 -0.5(3) . . . . ?
C2 N1 C3 C4 177.75(19) . . . . ?
Mo1 O6 C4 N2 163.59(16) . . . . ?
Mo1 O6 C4 C3 -14.3(2) . . . . ?
C5 N2 C4 O6 -0.2(3) . . . . ?
C5 N2 C4 C3 177.53(19) . . . . ?
O5 C3 C4 O6 11.6(3) . . . . ?
N1 C3 C4 O6 -166.89(19) . . . . ?
O5 C3 C4 N2 -166.4(2) . . . . ?
N1 C3 C4 N2 15.2(3) . . . . ?
C4 N2 C5 C6 -75.2(3) . . . . ?
C9 N3 C8 C7 -149.9(2) . . . . ?
Mo2 O7 C9 N3 179.00(17) . . . . ?
Mo2 O7 C9 C10 1.3(3) . . . . ?
C8 N3 C9 O7 -1.6(4) . . . . ?
C8 N3 C9 C10 175.9(2) . . . . ?
Mo2 O8 C10 N4 165.26(17) . . . . ?
Mo2 O8 C10 C9 -13.2(3) . . . . ?
C11 N4 C10 O8 -1.7(4) . . . . ?
C11 N4 C10 C9 176.6(2) . . . . ?
O7 C9 C10 O8 7.8(3) . . . . ?
N3 C9 C10 O8 -169.9(2) . . . . ?
O7 C9 C10 N4 -170.7(2) . . . . ?
N3 C9 C10 N4 11.6(3) . . . . ?
C10 N4 C11 C12 -173.9(2) . . . . ?
C15 N5 C14 C13 166.9(7) . . . . ?
C15 N5' C14' C13' -90.3(10) . . . . ?
C14 N5 C15 O9 8.0(7) . . . . ?
C14 N5 C15 C16 177.5(4) . . . . ?
C14' N5' C15 O9 -14.1(9) . . . . ?
C14' N5' C15 C16 -178.8(5) . . . . ?
C17 N6 C16 O10 5.3(4) . . . . ?
C17 N6 C16 C15 -176.8(2) . . . . ?
O9 C15 C16 O10 -176.2(2) . . . . ?
N5 C15 C16 O10 14.3(5) . . . . ?
N5' C15 C16 O10 -9.8(4) . . . . ?
O9 C15 C16 N6 5.8(3) . . . . ?
N5 C15 C16 N6 -163.8(4) . . . . ?
N5' C15 C16 N6 172.2(4) . . . . ?
C16 N6 C17 C18 95.9(3) . . . . ?

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 H1 O9 0.936(10) 1.932(10) 2.867(2) 176(2) 1_545
N2 H2 O9 0.933(10) 2.067(13) 2.950(3) 157(2) 1_545
N3 H3 O10 0.936(10) 1.960(12) 2.877(2) 166(2) 1_655
N4 H4 O10 0.936(10) 1.932(10) 2.868(2) 178(2) 1_655
C2 H2A O4 0.99 2.59 3.497(3) 151.6 .
C5 H5B O7 0.99 2.49 3.365(3) 146.6 1_455
C6 H6B O2 0.98 2.64 3.343(3) 128.5 2_666
C12 H12B O5 0.98 2.58 3.520(3) 160.2 2_665
N5 H5 Cl1 0.967(9) 2.828(13) 3.743(5) 158(2) .
N5 H5 O10 0.967(9) 2.25(3) 2.736(6) 110(2) .
C13 H13A O1 0.98 2.54 3.275(8) 132.1 .
C13 H13B O4 0.98 2.64 3.224(7) 118.3 1_565
C14 H14B O4 0.99 2.60 3.239(5) 122.7 1_565
N5' H5' Cl1 0.918(9) 2.828(13) 3.596(8) 142(2) .
C13' H13F Cl4 0.98 2.76 3.546(11) 137.2 2_665
C14' H14D O4 0.99 2.62 3.219(6) 118.9 1_565
N6 H6 O3 0.930(10) 2.17(2) 2.941(3) 140(2) 1_465
C17 H17A Cl2 0.99 2.94 3.813(3) 148.0 1_455
C19 H19A N7 0.98 2.58 3.339(5) 134.0 2_656
C19 H19B Cl3 0.98 2.79 3.553(4) 134.8 .
C19 H19C O2 0.98 2.37 3.342(4) 170.3 1_545

_refine_diff_density_max         0.870
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.073
_shelxl_version_number           2014/6

#=============================================================================
#   SHELXL Ins File
#=============================================================================

