# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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/. 
# 
# 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 1029376'
_audit_update_record             
;
2014-10-15 deposited with the CCDC.
2014-12-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H16 Mo N2 O5'
_chemical_formula_weight         376.22

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   7.3971(5)
_cell_length_b                   13.1764(9)
_cell_length_c                   14.2217(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4050(10)
_cell_angle_gamma                90.00
_cell_volume                     1385.73(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5505
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      26.01

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    0.970
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7729
_exptl_absorpt_correction_T_max  0.8925
_exptl_absorpt_process_details   'SADABS (Sheldrick 1997)'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14117
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         26.01
_reflns_number_total             2725
_reflns_number_gt                2597
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker SMART (2003)'
_computing_cell_refinement       'Bruker SMART (2003)'
_computing_data_reduction        'Bruker SAINT-Plus (2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'PLATON (Spek,2002), MERCURY (Macrae et al, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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 > 2σ(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)+(0.0399P)²+0.6374P] 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         2725
_refine_ls_number_parameters     190
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0238
_refine_ls_wR_factor_ref         0.0657
_refine_ls_wR_factor_gt          0.0649
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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
Mo1 Mo 0.42137(2) 0.236573(13) 0.245735(12) 0.02754(8) Uani 1 1 d . . .
O1 O 0.3228(3) 0.29907(14) 0.33575(12) 0.0493(4) Uani 1 1 d . . .
O2 O 0.5139(2) 0.32368(12) 0.17242(11) 0.0410(4) Uani 1 1 d . . .
O3 O 0.2113(2) 0.20484(13) 0.17084(11) 0.0394(4) Uani 1 1 d . . .
O4 O 0.6469(2) 0.19992(11) 0.31895(11) 0.0336(3) Uani 1 1 d . . .
O5 O 0.7587(2) -0.02604(13) 0.51643(10) 0.0417(4) Uani 1 1 d . . .
N1 N 0.5580(2) 0.10809(13) 0.15436(11) 0.0279(4) Uani 1 1 d . . .
N2 N 0.3408(2) 0.07848(12) 0.29805(11) 0.0259(3) Uani 1 1 d . . .
H2A H 0.3101 0.0841 0.3594 0.031 Uiso 1 1 calc R . .
C1 C 0.6301(3) 0.12223(18) 0.06930(14) 0.0348(5) Uani 1 1 d . . .
H1 H 0.6127 0.1842 0.0392 0.042 Uiso 1 1 calc R . .
C2 C 0.7289(3) 0.0481(2) 0.02530(16) 0.0417(5) Uani 1 1 d . . .
H2 H 0.7780 0.0600 -0.0333 0.050 Uiso 1 1 calc R . .
C3 C 0.7534(3) -0.0439(2) 0.06980(17) 0.0464(6) Uani 1 1 d . . .
H3 H 0.8200 -0.0950 0.0417 0.056 Uiso 1 1 calc R . .
C4 C 0.6780(3) -0.05952(17) 0.15683(16) 0.0393(5) Uani 1 1 d . . .
H4 H 0.6923 -0.1214 0.1876 0.047 Uiso 1 1 calc R . .
C5 C 0.5810(3) 0.01839(15) 0.19728(13) 0.0281(4) Uani 1 1 d . . .
C6 C 0.4973(3) 0.00810(14) 0.29300(13) 0.0272(4) Uani 1 1 d . . .
H6 H 0.4539 -0.0616 0.3003 0.033 Uiso 1 1 calc R . .
C7 C 0.1784(3) 0.04452(17) 0.24327(15) 0.0354(5) Uani 1 1 d . . .
H7A H 0.1003 0.0043 0.2825 0.042 Uiso 1 1 calc R . .
H7B H 0.2135 0.0036 0.1901 0.042 Uiso 1 1 calc R . .
C8 C 0.0817(3) 0.13906(19) 0.20992(18) 0.0426(5) Uani 1 1 d . . .
H8A H -0.0105 0.1218 0.1629 0.051 Uiso 1 1 calc R . .
H8B H 0.0237 0.1720 0.2622 0.051 Uiso 1 1 calc R . .
C9 C 0.8456(3) 0.16369(19) 0.44599(15) 0.0388(5) Uani 1 1 d . . .
H9A H 0.8693 0.2343 0.4352 0.058 Uiso 1 1 calc R . .
H9B H 0.9542 0.1253 0.4371 0.058 Uiso 1 1 calc R . .
H9C H 0.8058 0.1545 0.5092 0.058 Uiso 1 1 calc R . .
C10 C 0.7012(3) 0.12774(16) 0.37803(13) 0.0287(4) Uani 1 1 d . . .
C11 C 0.6322(3) 0.03147(15) 0.37253(13) 0.0268(4) Uani 1 1 d . . .
C12 C 0.6734(3) -0.04562(16) 0.44371(14) 0.0298(4) Uani 1 1 d . . .
C13 C 0.6020(3) -0.15157(17) 0.43028(16) 0.0400(5) Uani 1 1 d . . .
H13A H 0.4723 -0.1498 0.4262 0.060 Uiso 1 1 calc R . .
H13B H 0.6400 -0.1929 0.4827 0.060 Uiso 1 1 calc R . .
H13C H 0.6482 -0.1796 0.3734 0.060 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.7015(16) . ?
Mo1 O2 1.7055(15) . ?
Mo1 O3 1.9089(15) . ?
Mo1 O4 2.0037(14) . ?
Mo1 N2 2.2955(16) . ?
Mo1 N1 2.3750(17) . ?
O3 C8 1.416(3) . ?
O4 C10 1.325(2) . ?
O5 C12 1.226(2) . ?
N1 C5 1.339(3) . ?
N1 C1 1.347(3) . ?
N2 C7 1.485(2) . ?
N2 C6 1.487(2) . ?
N2 H2A 0.9100 . ?
C1 C2 1.379(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.377(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.385(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.515(3) . ?
C6 C11 1.521(3) . ?
C6 H6 0.9800 . ?
C7 C8 1.507(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.500(3) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.369(3) . ?
C11 C12 1.461(3) . ?
C12 C13 1.503(3) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O2 108.68(9) . . ?
O1 Mo1 O3 99.65(8) . . ?
O2 Mo1 O3 98.04(7) . . ?
O1 Mo1 O4 95.30(8) . . ?
O2 Mo1 O4 97.95(7) . . ?
O3 Mo1 O4 153.29(8) . . ?
O1 Mo1 N2 94.35(7) . . ?
O2 Mo1 N2 156.95(7) . . ?
O3 Mo1 N2 76.58(6) . . ?
O4 Mo1 N2 80.34(6) . . ?
O1 Mo1 N1 162.32(7) . . ?
O2 Mo1 N1 87.85(7) . . ?
O3 Mo1 N1 83.70(7) . . ?
O4 Mo1 N1 75.67(6) . . ?
N2 Mo1 N1 69.38(5) . . ?
C8 O3 Mo1 117.69(13) . . ?
C10 O4 Mo1 137.60(13) . . ?
C5 N1 C1 118.85(18) . . ?
C5 N1 Mo1 115.52(13) . . ?
C1 N1 Mo1 125.18(14) . . ?
C7 N2 C6 114.07(15) . . ?
C7 N2 Mo1 108.45(12) . . ?
C6 N2 Mo1 109.99(11) . . ?
C7 N2 H2A 108.1 . . ?
C6 N2 H2A 108.1 . . ?
Mo1 N2 H2A 108.1 . . ?
N1 C1 C2 122.4(2) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 118.7(2) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 119.4(2) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 119.0(2) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 121.74(19) . . ?
N1 C5 C6 115.99(17) . . ?
C4 C5 C6 122.26(19) . . ?
N2 C6 C5 108.87(15) . . ?
N2 C6 C11 109.59(15) . . ?
C5 C6 C11 112.01(16) . . ?
N2 C6 H6 108.8 . . ?
C5 C6 H6 108.8 . . ?
C11 C6 H6 108.8 . . ?
N2 C7 C8 106.71(17) . . ?
N2 C7 H7A 110.4 . . ?
C8 C7 H7A 110.4 . . ?
N2 C7 H7B 110.4 . . ?
C8 C7 H7B 110.4 . . ?
H7A C7 H7B 108.6 . . ?
O3 C8 C7 108.01(18) . . ?
O3 C8 H8A 110.1 . . ?
C7 C8 H8A 110.1 . . ?
O3 C8 H8B 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O4 C10 C11 121.47(17) . . ?
O4 C10 C9 112.47(18) . . ?
C11 C10 C9 126.03(19) . . ?
C10 C11 C12 122.25(18) . . ?
C10 C11 C6 117.83(17) . . ?
C12 C11 C6 119.75(17) . . ?
O5 C12 C11 122.2(2) . . ?
O5 C12 C13 118.34(19) . . ?
C11 C12 C13 119.41(18) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

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
N2 H2A O5 0.91 2.00 2.842(2) 152.8 3_656

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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/. 
# 
# 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 1029377'
_audit_update_record             
;
2014-10-15 deposited with the CCDC.
2014-12-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H16 Mo N2 O5'
_chemical_formula_weight         424.26

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'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.1423(7)
_cell_length_b                   10.2929(11)
_cell_length_c                   11.0127(12)
_cell_angle_alpha                112.944(10)
_cell_angle_beta                 93.302(8)
_cell_angle_gamma                99.329(8)
_cell_volume                     831.25(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2392
_cell_measurement_theta_min      3.3150
_cell_measurement_theta_max      28.8000

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             428
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8030
_exptl_absorpt_correction_T_max  0.8939
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_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  'Xcalibur, Eos, Gemini'
_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            5724
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0480
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.02
_diffrn_reflns_theta_max         26.36
_reflns_number_total             3368
_reflns_number_gt                2977
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd. 2010)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd. 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd. 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'PLATON (Spek,2002), MERCURY (Macrae et al, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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 > 2σ(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)+(0.0320P)²+0.0329P] 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         3368
_refine_ls_number_parameters     228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0818
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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
Mo1 Mo 0.57799(3) 0.24782(3) 0.81584(3) 0.03381(11) Uani 1 1 d . . .
O1 O 0.7045(3) 0.4101(2) 0.9101(2) 0.0472(6) Uani 1 1 d . . .
O2 O 0.7025(3) 0.1307(2) 0.7442(2) 0.0463(6) Uani 1 1 d . . .
O3 O 0.5183(2) 0.2847(2) 0.6600(2) 0.0375(5) Uani 1 1 d . . .
O4 O 0.5220(2) 0.1951(2) 0.9614(2) 0.0431(5) Uani 1 1 d . . .
O5 O 0.1533(3) 0.2668(4) 1.2150(3) 0.0831(10) Uani 1 1 d . . .
N1 N 0.3441(3) 0.0656(2) 0.7123(2) 0.0323(6) Uani 1 1 d . . .
N2 N 0.3354(3) 0.3396(2) 0.8617(2) 0.0327(6) Uani 1 1 d . . .
H2A H 0.3581 0.4183 0.9405 0.039 Uiso 1 1 calc R . .
C1 C 0.3481(4) -0.0570(3) 0.6073(3) 0.0395(8) Uani 1 1 d . . .
H1 H 0.4509 -0.0741 0.5788 0.047 Uiso 1 1 calc R . .
C2 C 0.2065(4) -0.1564(3) 0.5418(4) 0.0476(9) Uani 1 1 d . . .
H2 H 0.2128 -0.2410 0.4704 0.057 Uiso 1 1 calc R . .
C3 C 0.0546(5) -0.1309(4) 0.5818(4) 0.0561(10) Uani 1 1 d . . .
H3 H -0.0439 -0.1969 0.5369 0.067 Uiso 1 1 calc R . .
C4 C 0.0499(4) -0.0054(4) 0.6900(3) 0.0470(9) Uani 1 1 d . . .
H4 H -0.0519 0.0140 0.7192 0.056 Uiso 1 1 calc R . .
C5 C 0.1969(4) 0.0899(3) 0.7536(3) 0.0330(7) Uani 1 1 d . . .
C6 C 0.2049(4) 0.2277(3) 0.8740(3) 0.0339(7) Uani 1 1 d . . .
H6 H 0.0962 0.2567 0.8732 0.041 Uiso 1 1 calc R . .
C7 C 0.2910(4) 0.3842(3) 0.7563(3) 0.0348(7) Uani 1 1 d . . .
C8 C 0.3911(4) 0.3536(3) 0.6551(3) 0.0347(7) Uani 1 1 d . . .
C9 C 0.3601(4) 0.3925(3) 0.5500(3) 0.0444(8) Uani 1 1 d . . .
H9 H 0.4232 0.3679 0.4795 0.053 Uiso 1 1 calc R . .
C10 C 0.2356(4) 0.4676(4) 0.5512(4) 0.0517(9) Uani 1 1 d . . .
H10 H 0.2165 0.4966 0.4824 0.062 Uiso 1 1 calc R . .
C11 C 0.1381(4) 0.5008(4) 0.6532(4) 0.0510(9) Uani 1 1 d . . .
H11 H 0.0541 0.5521 0.6530 0.061 Uiso 1 1 calc R . .
C12 C 0.1648(4) 0.4579(3) 0.7554(4) 0.0443(8) Uani 1 1 d . . .
H12 H 0.0978 0.4788 0.8234 0.053 Uiso 1 1 calc R . .
C13 C 0.4627(4) 0.1845(4) 1.1635(4) 0.0544(9) Uani 1 1 d . . .
H13A H 0.5404 0.1204 1.1430 0.082 Uiso 1 1 calc R . .
H13B H 0.3686 0.1454 1.1961 0.082 Uiso 1 1 calc R . .
H13C H 0.5176 0.2767 1.2302 0.082 Uiso 1 1 calc R . .
C14 C 0.4025(4) 0.2015(3) 1.0400(3) 0.0377(7) Uani 1 1 d . . .
C15 C 0.2471(4) 0.2175(3) 1.0051(3) 0.0347(7) Uani 1 1 d . . .
C16 C 0.1182(4) 0.2281(4) 1.0959(4) 0.0457(8) Uani 1 1 d . . .
C17 C -0.0616(4) 0.1878(4) 1.0383(4) 0.0608(11) Uani 1 1 d . . .
H17A H -0.0774 0.1062 0.9544 0.091 Uiso 1 1 calc R . .
H17B H -0.0943 0.2674 1.0253 0.091 Uiso 1 1 calc R . .
H17C H -0.1291 0.1637 1.0981 0.091 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O2 1.688(2) . ?
Mo1 O1 1.702(2) . ?
Mo1 O4 1.938(2) . ?
Mo1 O3 1.948(2) . ?
Mo1 N1 2.317(2) . ?
Mo1 N2 2.323(2) . ?
O3 C8 1.357(3) . ?
O4 C14 1.332(4) . ?
O5 C16 1.213(4) . ?
N1 C5 1.333(4) . ?
N1 C1 1.345(4) . ?
N2 C7 1.452(4) . ?
N2 C6 1.489(4) . ?
N2 H2A 0.9100 . ?
C1 C2 1.357(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.368(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.382(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.369(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.506(4) . ?
C6 C15 1.512(4) . ?
C6 H6 0.9800 . ?
C7 C12 1.375(4) . ?
C7 C8 1.385(4) . ?
C8 C9 1.387(4) . ?
C9 C10 1.369(5) . ?
C9 H9 0.9300 . ?
C10 C11 1.378(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.378(5) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.503(4) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.355(4) . ?
C15 C16 1.478(4) . ?
C16 C17 1.486(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mo1 O1 107.71(11) . . ?
O2 Mo1 O4 100.57(10) . . ?
O1 Mo1 O4 96.80(11) . . ?
O2 Mo1 O3 96.37(10) . . ?
O1 Mo1 O3 98.41(11) . . ?
O4 Mo1 O3 152.56(9) . . ?
O2 Mo1 N1 89.50(9) . . ?
O1 Mo1 N1 162.79(10) . . ?
O4 Mo1 N1 79.35(9) . . ?
O3 Mo1 N1 79.37(9) . . ?
O2 Mo1 N2 159.44(10) . . ?
O1 Mo1 N2 92.59(9) . . ?
O4 Mo1 N2 79.71(9) . . ?
O3 Mo1 N2 76.92(9) . . ?
N1 Mo1 N2 70.25(8) . . ?
C8 O3 Mo1 121.07(19) . . ?
C14 O4 Mo1 139.69(19) . . ?
C5 N1 C1 119.0(3) . . ?
C5 N1 Mo1 117.43(19) . . ?
C1 N1 Mo1 123.3(2) . . ?
C7 N2 C6 114.7(2) . . ?
C7 N2 Mo1 106.87(18) . . ?
C6 N2 Mo1 108.44(16) . . ?
C7 N2 H2A 108.9 . . ?
C6 N2 H2A 108.9 . . ?
Mo1 N2 H2A 108.9 . . ?
N1 C1 C2 121.9(3) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C1 C2 C3 119.4(3) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C2 C3 C4 118.9(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N1 C5 C4 121.5(3) . . ?
N1 C5 C6 115.4(2) . . ?
C4 C5 C6 123.1(3) . . ?
N2 C6 C5 107.3(2) . . ?
N2 C6 C15 109.2(2) . . ?
C5 C6 C15 114.2(2) . . ?
N2 C6 H6 108.7 . . ?
C5 C6 H6 108.7 . . ?
C15 C6 H6 108.7 . . ?
C12 C7 C8 120.1(3) . . ?
C12 C7 N2 124.4(3) . . ?
C8 C7 N2 115.4(2) . . ?
O3 C8 C7 119.2(3) . . ?
O3 C8 C9 120.8(3) . . ?
C7 C8 C9 120.0(3) . . ?
C10 C9 C8 119.2(3) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C11 120.8(3) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C12 120.1(3) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C7 C12 C11 119.6(3) . . ?
C7 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
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 . . ?
O4 C14 C15 121.6(3) . . ?
O4 C14 C13 111.4(3) . . ?
C15 C14 C13 126.9(3) . . ?
C14 C15 C16 120.4(3) . . ?
C14 C15 C6 120.2(3) . . ?
C16 C15 C6 119.3(3) . . ?
O5 C16 C15 122.7(3) . . ?
O5 C16 C17 118.8(3) . . ?
C15 C16 C17 118.4(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 . . ?

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
N2 H2A O1 0.91 2.05 2.894(3) 153.4 2_667

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.075
####################################################################### 
# 
# 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/. 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1029378'
_audit_update_record             
;
2014-10-15 deposited with the CCDC.
2014-12-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H15 Cl Mo N2 O5'
_chemical_formula_weight         458.70

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.8674(5)
_cell_length_b                   8.4723(5)
_cell_length_c                   13.9072(8)
_cell_angle_alpha                76.8190(10)
_cell_angle_beta                 84.3280(10)
_cell_angle_gamma                77.5580(10)
_cell_volume                     880.16(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    7291
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      25.92

_exptl_crystal_description       Block
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             460
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8219
_exptl_absorpt_correction_T_max  0.8657
_exptl_absorpt_process_details   'SADABS (Sheldrick 1997)'

_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8471
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3093
_reflns_number_gt                2916
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'Bruker SMART (2003)'
_computing_cell_refinement       'Bruker SMART (2003)'
_computing_data_reduction        'Bruker SAINT-Plus (2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'PLATON (Spek,2002), MERCURY (Macrae et al, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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 > 2σ(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)+(0.0410P)²+0.5006P] 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         3093
_refine_ls_number_parameters     235
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0724
_refine_ls_wR_factor_gt          0.0711
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.98830(3) 0.37566(3) 0.274050(15) 0.03484(10) Uani 1 1 d . . .
Cl1 Cl 0.21236(11) 0.78537(13) 0.03925(6) 0.0759(3) Uani 1 1 d . . .
O1 O 1.0267(3) 0.5434(3) 0.30881(16) 0.0554(5) Uani 1 1 d . . .
O2 O 1.1846(2) 0.2594(3) 0.24744(15) 0.0539(5) Uani 1 1 d . . .
O3 O 0.9284(2) 0.4744(2) 0.13839(13) 0.0416(4) Uani 1 1 d . . .
O4 O 0.9404(2) 0.2519(2) 0.40889(12) 0.0383(4) Uani 1 1 d . . .
O5 O 0.5064(3) 0.3095(2) 0.60035(13) 0.0449(4) Uani 1 1 d . . .
N1 N 0.8481(3) 0.1741(3) 0.24765(15) 0.0344(5) Uani 1 1 d . . .
N2 N 0.6878(3) 0.4654(2) 0.28578(13) 0.0283(4) Uani 1 1 d . . .
H2A H 0.6623 0.5423 0.3240 0.034 Uiso 1 1 calc R . .
C1 C 0.9253(4) 0.0486(3) 0.20366(19) 0.0428(6) Uani 1 1 d . . .
H1 H 1.0401 0.0434 0.1789 0.051 Uiso 1 1 calc R . .
C2 C 0.8405(4) -0.0706(3) 0.1943(2) 0.0502(7) Uani 1 1 d . . .
H2 H 0.8976 -0.1572 0.1650 0.060 Uiso 1 1 calc R . .
C3 C 0.6690(4) -0.0616(3) 0.2288(2) 0.0514(7) Uani 1 1 d . . .
H3 H 0.6079 -0.1403 0.2215 0.062 Uiso 1 1 calc R . .
C4 C 0.5895(4) 0.0657(3) 0.2743(2) 0.0412(6) Uani 1 1 d . . .
H4 H 0.4743 0.0737 0.2986 0.049 Uiso 1 1 calc R . .
C5 C 0.6828(3) 0.1806(3) 0.28325(17) 0.0315(5) Uani 1 1 d . . .
C6 C 0.6064(3) 0.3206(3) 0.33472(16) 0.0285(5) Uani 1 1 d . . .
H6 H 0.4806 0.3512 0.3262 0.034 Uiso 1 1 calc R . .
C7 C 0.6314(3) 0.5430(3) 0.18687(17) 0.0300(5) Uani 1 1 d . . .
C8 C 0.7642(3) 0.5481(3) 0.11308(18) 0.0353(5) Uani 1 1 d . . .
C9 C 0.7268(4) 0.6269(4) 0.01694(19) 0.0474(7) Uani 1 1 d . . .
H9 H 0.8155 0.6310 -0.0325 0.057 Uiso 1 1 calc R . .
C10 C 0.5572(4) 0.6994(4) -0.0050(2) 0.0526(7) Uani 1 1 d . . .
H10 H 0.5307 0.7524 -0.0696 0.063 Uiso 1 1 calc R . .
C11 C 0.4260(4) 0.6933(3) 0.0690(2) 0.0453(7) Uani 1 1 d . . .
C12 C 0.4604(3) 0.6154(3) 0.16540(18) 0.0360(5) Uani 1 1 d . . .
H12 H 0.3713 0.6115 0.2146 0.043 Uiso 1 1 calc R . .
C13 C 0.8631(4) 0.1762(3) 0.57722(19) 0.0427(6) Uani 1 1 d . . .
H13A H 0.9877 0.1600 0.5771 0.064 Uiso 1 1 calc R . .
H13B H 0.8275 0.0727 0.6037 0.064 Uiso 1 1 calc R . .
H13C H 0.8107 0.2542 0.6173 0.064 Uiso 1 1 calc R . .
C14 C 0.8060(3) 0.2413(3) 0.47360(17) 0.0319(5) Uani 1 1 d . . .
C15 C 0.6382(3) 0.2797(3) 0.44455(17) 0.0304(5) Uani 1 1 d . . .
C16 C 0.4906(3) 0.2944(3) 0.51663(18) 0.0349(5) Uani 1 1 d . . .
C17 C 0.3115(4) 0.2975(5) 0.4876(2) 0.0648(10) Uani 1 1 d . . .
H17A H 0.2301 0.3073 0.5431 0.097 Uiso 1 1 calc R . .
H17B H 0.3106 0.1969 0.4671 0.097 Uiso 1 1 calc R . .
H17C H 0.2790 0.3901 0.4340 0.097 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.695(2) . ?
Mo1 O2 1.7001(19) . ?
Mo1 O3 1.9410(18) . ?
Mo1 O4 1.9729(17) . ?
Mo1 N2 2.323(2) . ?
Mo1 N1 2.333(2) . ?
Cl1 C11 1.741(3) . ?
O3 C8 1.351(3) . ?
O4 C14 1.323(3) . ?
O5 C16 1.221(3) . ?
N1 C5 1.339(3) . ?
N1 C1 1.349(3) . ?
N2 C7 1.451(3) . ?
N2 C6 1.500(3) . ?
N2 H2A 0.9100 . ?
C1 C2 1.359(4) . ?
C1 H1 0.9300 . ?
C2 C3 1.379(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.508(3) . ?
C6 C15 1.521(3) . ?
C6 H6 0.9800 . ?
C7 C12 1.384(3) . ?
C7 C8 1.391(3) . ?
C8 C9 1.381(4) . ?
C9 C10 1.376(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.384(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.378(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.497(3) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.368(3) . ?
C15 C16 1.461(3) . ?
C16 C17 1.497(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O2 107.54(11) . . ?
O1 Mo1 O3 99.67(9) . . ?
O2 Mo1 O3 96.84(9) . . ?
O1 Mo1 O4 96.04(9) . . ?
O2 Mo1 O4 99.36(9) . . ?
O3 Mo1 O4 152.84(8) . . ?
O1 Mo1 N2 92.93(9) . . ?
O2 Mo1 N2 159.30(9) . . ?
O3 Mo1 N2 76.19(7) . . ?
O4 Mo1 N2 81.03(7) . . ?
O1 Mo1 N1 161.84(9) . . ?
O2 Mo1 N1 90.14(9) . . ?
O3 Mo1 N1 81.81(8) . . ?
O4 Mo1 N1 76.52(7) . . ?
N2 Mo1 N1 69.72(7) . . ?
C8 O3 Mo1 122.81(15) . . ?
C14 O4 Mo1 138.11(16) . . ?
C5 N1 C1 118.6(2) . . ?
C5 N1 Mo1 117.02(15) . . ?
C1 N1 Mo1 124.29(19) . . ?
C7 N2 C6 114.10(18) . . ?
C7 N2 Mo1 107.58(14) . . ?
C6 N2 Mo1 108.67(13) . . ?
C7 N2 H2A 108.8 . . ?
C6 N2 H2A 108.8 . . ?
Mo1 N2 H2A 108.8 . . ?
N1 C1 C2 122.1(3) . . ?
N1 C1 H1 119.0 . . ?
C2 C1 H1 119.0 . . ?
C1 C2 C3 119.3(3) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C4 C3 C2 119.0(3) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C5 C4 C3 119.1(3) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
N1 C5 C4 121.9(2) . . ?
N1 C5 C6 115.9(2) . . ?
C4 C5 C6 122.1(2) . . ?
N2 C6 C5 107.74(18) . . ?
N2 C6 C15 108.56(18) . . ?
C5 C6 C15 113.75(19) . . ?
N2 C6 H6 108.9 . . ?
C5 C6 H6 108.9 . . ?
C15 C6 H6 108.9 . . ?
C12 C7 C8 120.9(2) . . ?
C12 C7 N2 123.9(2) . . ?
C8 C7 N2 115.1(2) . . ?
O3 C8 C9 121.7(2) . . ?
O3 C8 C7 118.2(2) . . ?
C9 C8 C7 120.1(2) . . ?
C10 C9 C8 119.4(3) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 120.0(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 121.6(3) . . ?
C12 C11 Cl1 119.2(2) . . ?
C10 C11 Cl1 119.2(2) . . ?
C11 C12 C7 118.0(2) . . ?
C11 C12 H12 121.0 . . ?
C7 C12 H12 121.0 . . ?
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 . . ?
O4 C14 C15 121.8(2) . . ?
O4 C14 C13 111.8(2) . . ?
C15 C14 C13 126.4(2) . . ?
C14 C15 C16 121.0(2) . . ?
C14 C15 C6 119.0(2) . . ?
C16 C15 C6 119.8(2) . . ?
O5 C16 C15 122.2(2) . . ?
O5 C16 C17 117.8(2) . . ?
C15 C16 C17 120.0(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 . . ?

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
N2 H2A O5 0.91 2.01 2.850(3) 152.3 2_666

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.064
####################################################################### 
# 
# 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/. 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1029379'
_audit_update_record             
;
2014-10-15 deposited with the CCDC.
2014-12-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 Mo N2 O5'
_chemical_formula_weight         438.28

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.9031(5)
_cell_length_b                   8.4137(7)
_cell_length_c                   14.0404(9)
_cell_angle_alpha                75.991(6)
_cell_angle_beta                 83.346(5)
_cell_angle_gamma                78.967(6)
_cell_volume                     886.72(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2170
_cell_measurement_theta_min      2.6299
_cell_measurement_theta_max      28.9810

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            'Light Brown'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             444
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8486
_exptl_absorpt_correction_T_max  0.8997
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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  'Xcalibur, Eos, Gemini'
_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            6338
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.64
_diffrn_reflns_theta_max         26.37
_reflns_number_total             3621
_reflns_number_gt                2933
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlisPro (Oxford Diffraction Ltd. 2010)'
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction Ltd. 2010)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction Ltd. 2010)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'PLATON (Spek,2002), MERCURY (Macrae et al, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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 > 2σ(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)+(0.0344P)²+0.0965P] 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         3621
_refine_ls_number_parameters     238
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0847
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo -0.01068(4) 0.38174(4) 0.77555(2) 0.03382(13) Uani 1 1 d . . .
O1 O 0.0318(4) 0.5494(4) 0.8091(2) 0.0544(8) Uani 1 1 d . . .
O2 O 0.1815(3) 0.2655(4) 0.7493(2) 0.0528(8) Uani 1 1 d . . .
O3 O -0.0646(3) 0.4830(3) 0.64052(18) 0.0405(7) Uani 1 1 d . . .
O4 O -0.0646(3) 0.2548(3) 0.90964(17) 0.0362(6) Uani 1 1 d . . .
O5 O -0.5007(3) 0.3087(3) 1.09960(18) 0.0433(7) Uani 1 1 d . . .
N1 N -0.1536(4) 0.1787(4) 0.7497(2) 0.0304(7) Uani 1 1 d . . .
N2 N -0.3071(3) 0.4688(3) 0.78696(19) 0.0255(7) Uani 1 1 d . . .
H2A H -0.3319 0.5453 0.8248 0.031 Uiso 1 1 calc R . .
C1 C -0.0796(5) 0.0551(5) 0.7055(3) 0.0418(10) Uani 1 1 d . . .
H1 H 0.0360 0.0493 0.6822 0.050 Uiso 1 1 calc R . .
C2 C -0.1676(6) -0.0616(5) 0.6935(3) 0.0494(12) Uani 1 1 d . . .
H2 H -0.1123 -0.1464 0.6633 0.059 Uiso 1 1 calc R . .
C3 C -0.3378(6) -0.0536(5) 0.7261(3) 0.0497(11) Uani 1 1 d . . .
H3 H -0.4007 -0.1312 0.7174 0.060 Uiso 1 1 calc R . .
C4 C -0.4143(5) 0.0715(5) 0.7721(3) 0.0382(10) Uani 1 1 d . . .
H4 H -0.5302 0.0798 0.7949 0.046 Uiso 1 1 calc R . .
C5 C -0.3186(5) 0.1840(4) 0.7842(2) 0.0272(8) Uani 1 1 d . . .
C6 C -0.3925(4) 0.3235(4) 0.8361(2) 0.0258(8) Uani 1 1 d . . .
H6 H -0.5168 0.3542 0.8277 0.031 Uiso 1 1 calc R . .
C7 C -0.3604(4) 0.5477(4) 0.6890(2) 0.0257(8) Uani 1 1 d . . .
C8 C -0.2271(5) 0.5546(4) 0.6156(3) 0.0325(9) Uani 1 1 d . . .
C9 C -0.2629(6) 0.6325(5) 0.5198(3) 0.0461(11) Uani 1 1 d . . .
H9 H -0.1747 0.6394 0.4698 0.055 Uiso 1 1 calc R . .
C10 C -0.4321(6) 0.7000(5) 0.4994(3) 0.0502(12) Uani 1 1 d . . .
H10 H -0.4562 0.7514 0.4348 0.060 Uiso 1 1 calc R . .
C11 C -0.5671(5) 0.6938(5) 0.5721(3) 0.0390(10) Uani 1 1 d . . .
C12 C -0.5285(5) 0.6158(4) 0.6669(3) 0.0326(9) Uani 1 1 d . . .
H12 H -0.6168 0.6089 0.7169 0.039 Uiso 1 1 calc R . .
C13 C -0.1470(5) 0.1739(5) 1.0768(3) 0.0430(10) Uani 1 1 d . . .
H13A H -0.0432 0.0933 1.0762 0.065 Uiso 1 1 calc R . .
H13B H -0.2372 0.1219 1.1167 0.065 Uiso 1 1 calc R . .
H13C H -0.1263 0.2626 1.1035 0.065 Uiso 1 1 calc R . .
C14 C -0.2003(5) 0.2419(4) 0.9743(3) 0.0310(9) Uani 1 1 d . . .
C15 C -0.3650(4) 0.2793(4) 0.9448(2) 0.0273(8) Uani 1 1 d . . .
C16 C -0.5141(5) 0.2922(4) 1.0172(3) 0.0329(9) Uani 1 1 d . . .
C17 C -0.6896(5) 0.2905(7) 0.9882(3) 0.0664(15) Uani 1 1 d . . .
H17A H -0.6845 0.1989 0.9578 0.100 Uiso 1 1 calc R . .
H17B H -0.7280 0.3927 0.9425 0.100 Uiso 1 1 calc R . .
H17C H -0.7690 0.2789 1.0456 0.100 Uiso 1 1 calc R . .
C18 C -0.7500(6) 0.7682(6) 0.5467(3) 0.0666(15) Uani 1 1 d . . .
H18A H -0.7678 0.7505 0.4838 0.100 Uiso 1 1 calc R . .
H18B H -0.7693 0.8854 0.5440 0.100 Uiso 1 1 calc R . .
H18C H -0.8292 0.7162 0.5960 0.100 Uiso 1 1 calc R . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.693(3) . ?
Mo1 O2 1.696(3) . ?
Mo1 O3 1.941(2) . ?
Mo1 O4 1.970(2) . ?
Mo1 N2 2.315(3) . ?
Mo1 N1 2.336(3) . ?
O3 C8 1.357(4) . ?
O4 C14 1.325(4) . ?
O5 C16 1.217(4) . ?
N1 C5 1.334(4) . ?
N1 C1 1.343(5) . ?
N2 C7 1.448(4) . ?
N2 C6 1.491(4) . ?
N2 H2A 0.9100 . ?
C1 C2 1.359(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.364(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.373(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.518(5) . ?
C6 C15 1.512(5) . ?
C6 H6 0.9800 . ?
C7 C12 1.381(5) . ?
C7 C8 1.386(5) . ?
C8 C9 1.382(5) . ?
C9 C10 1.382(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.388(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.375(5) . ?
C11 C18 1.508(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.492(5) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.368(5) . ?
C15 C16 1.470(5) . ?
C16 C17 1.493(5) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mo1 O2 107.56(15) . . ?
O1 Mo1 O3 99.52(13) . . ?
O2 Mo1 O3 96.91(12) . . ?
O1 Mo1 O4 96.44(13) . . ?
O2 Mo1 O4 99.12(12) . . ?
O3 Mo1 O4 152.77(11) . . ?
O1 Mo1 N2 93.60(12) . . ?
O2 Mo1 N2 158.63(13) . . ?
O3 Mo1 N2 76.09(10) . . ?
O4 Mo1 N2 81.04(9) . . ?
O1 Mo1 N1 162.39(12) . . ?
O2 Mo1 N1 89.60(13) . . ?
O3 Mo1 N1 81.83(11) . . ?
O4 Mo1 N1 76.44(10) . . ?
N2 Mo1 N1 69.55(10) . . ?
C8 O3 Mo1 122.6(2) . . ?
C14 O4 Mo1 138.2(2) . . ?
C5 N1 C1 118.2(3) . . ?
C5 N1 Mo1 117.2(2) . . ?
C1 N1 Mo1 124.5(3) . . ?
C7 N2 C6 113.8(3) . . ?
C7 N2 Mo1 108.16(19) . . ?
C6 N2 Mo1 109.01(19) . . ?
C7 N2 H2A 108.6 . . ?
C6 N2 H2A 108.6 . . ?
Mo1 N2 H2A 108.6 . . ?
N1 C1 C2 122.3(4) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C1 C2 C3 119.6(4) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C2 C3 C4 118.6(4) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
N1 C5 C4 121.8(3) . . ?
N1 C5 C6 115.5(3) . . ?
C4 C5 C6 122.8(3) . . ?
N2 C6 C15 109.2(3) . . ?
N2 C6 C5 107.4(3) . . ?
C15 C6 C5 113.7(3) . . ?
N2 C6 H6 108.8 . . ?
C15 C6 H6 108.8 . . ?
C5 C6 H6 108.8 . . ?
C12 C7 C8 120.6(3) . . ?
C12 C7 N2 124.7(3) . . ?
C8 C7 N2 114.7(3) . . ?
O3 C8 C9 122.1(3) . . ?
O3 C8 C7 118.4(3) . . ?
C9 C8 C7 119.5(3) . . ?
C8 C9 C10 119.0(4) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C9 C10 C11 122.2(4) . . ?
C9 C10 H10 118.9 . . ?
C11 C10 H10 118.9 . . ?
C12 C11 C10 117.8(4) . . ?
C12 C11 C18 121.6(4) . . ?
C10 C11 C18 120.6(4) . . ?
C11 C12 C7 120.9(3) . . ?
C11 C12 H12 119.5 . . ?
C7 C12 H12 119.5 . . ?
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 . . ?
O4 C14 C15 121.3(3) . . ?
O4 C14 C13 111.6(3) . . ?
C15 C14 C13 126.9(3) . . ?
C14 C15 C16 120.5(3) . . ?
C14 C15 C6 119.3(3) . . ?
C16 C15 C6 120.0(3) . . ?
O5 C16 C15 122.3(4) . . ?
O5 C16 C17 118.5(3) . . ?
C15 C16 C17 119.2(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 . . ?
C11 C18 H18A 109.5 . . ?
C11 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C11 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

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
N2 H2A O5 0.91 2.02 2.854(4) 152.1 2_467

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.090

#===End
