# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_twin5
_database_code_depnum_ccdc_archive 'CCDC 1850318'
_audit_update_record             
;
2018-06-19 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H22 Mo N6 O3'
_chemical_formula_sum            'C26 H22 Mo N6 O3'
_chemical_formula_weight         562.43

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   7.531(2)
_cell_length_b                   21.121(6)
_cell_length_c                   14.986(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.728(6)
_cell_angle_gamma                90
_cell_volume                     2382.5(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4239
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      25

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_F_000             1144
_exptl_transmission_factor_min   0.833
_exptl_transmission_factor_max   0.906
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.592
_shelx_estimated_absorpt_T_min   0.833
_shelx_estimated_absorpt_T_max   0.906
_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      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  "Bruker APEX II CCD area detector'"
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24283
_diffrn_reflns_av_unetI/netI     0.1076
_diffrn_reflns_v_R_equivalents   0.0742
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.667
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6083
_reflns_number_gt                4587
_reflns_threshold_expression     I>2σ(I)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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       'Bruker APEX II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²+4.6000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6083
_refine_ls_number_parameters     330
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1404
_refine_ls_wR_factor_gt          0.1280
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
Mo1 Mo 0.68005(7) -0.03246(2) 0.23046(3) 0.01700(12) Uani 1 1 d . . . . .
O3 O 0.3122(5) 0.03163(19) 0.2304(3) 0.0304(9) Uani 1 1 d . . . . .
N1S N 0.9325(7) -0.0858(2) 0.2363(3) 0.0222(10) Uani 1 1 d . . . . .
O1 O 0.5985(6) -0.10028(17) 0.3258(2) 0.0210(9) Uani 1 1 d . . . . .
O2 O 0.5884(6) -0.11053(17) 0.1534(2) 0.0212(9) Uani 1 1 d . . . . .
N1 N 0.8213(7) 0.0543(2) 0.2194(3) 0.0214(10) Uani 1 1 d . . . . .
N2 N 0.7474(6) 0.0021(2) 0.3607(3) 0.0194(10) Uani 1 1 d . . . . .
N3 N 0.6965(6) -0.0317(2) 0.4353(3) 0.0199(9) Uani 1 1 d . . . . .
N4 N 0.7192(7) -0.0122(2) 0.0929(3) 0.0196(10) Uani 1 1 d . . . . .
C1 C 0.8833(8) 0.0854(3) 0.2937(4) 0.0220(12) Uani 1 1 d . . . . .
C2 C 0.9782(9) 0.1416(3) 0.2877(4) 0.0272(13) Uani 1 1 d . . . . .
H2A H 1.0178 0.1630 0.3404 0.033 Uiso 1 1 calc R U . . .
C3 C 1.0145(10) 0.1660(3) 0.2054(4) 0.0323(15) Uani 1 1 d . . . . .
H3A H 1.0812 0.2040 0.2006 0.039 Uiso 1 1 calc R U . . .
C4 C 0.9534(9) 0.1349(3) 0.1298(4) 0.0287(14) Uani 1 1 d . . . . .
H4A H 0.9743 0.1521 0.0725 0.034 Uiso 1 1 calc R U . . .
N5 N 0.6668(7) -0.0556(2) 0.0278(3) 0.0206(10) Uani 1 1 d . . . . .
C5 C 0.8609(8) 0.0783(3) 0.1378(4) 0.0224(12) Uani 1 1 d . . . . .
C6 C 0.8392(8) 0.0542(3) 0.3754(4) 0.0214(12) Uani 1 1 d . . . . .
C7 C 0.8918(9) 0.0785(3) 0.4654(4) 0.0263(13) Uani 1 1 d . . . . .
H7A H 0.8217 0.0571 0.5105 0.039 Uiso 1 1 calc R U . . .
H7B H 0.8698 0.1242 0.4679 0.039 Uiso 1 1 calc R U . . .
H7C H 1.0183 0.0702 0.4772 0.039 Uiso 1 1 calc R U . . .
C8 C 0.6215(8) -0.0837(2) 0.4088(3) 0.0187(11) Uani 1 1 d . . . . .
C9 C 0.5548(8) -0.1270(3) 0.4781(4) 0.0202(12) Uani 1 1 d . . . . .
C10 C 0.4803(8) -0.1849(3) 0.4537(4) 0.0220(12) Uani 1 1 d . . . . .
H10A H 0.4741 -0.1972 0.3927 0.026 Uiso 1 1 calc R U . . .
C11 C 0.4145(8) -0.2250(3) 0.5190(4) 0.0240(13) Uani 1 1 d . . . . .
H11A H 0.3604 -0.2641 0.5022 0.029 Uiso 1 1 calc R U . . .
C12 C 0.4279(9) -0.2079(3) 0.6076(4) 0.0270(14) Uani 1 1 d . . . . .
H12A H 0.3843 -0.2353 0.6523 0.032 Uiso 1 1 calc R U . . .
C13 C 0.5055(10) -0.1508(3) 0.6311(4) 0.0294(14) Uani 1 1 d . . . . .
H13A H 0.5163 -0.1395 0.6923 0.035 Uiso 1 1 calc R U . . .
C14 C 0.5673(9) -0.1099(3) 0.5677(4) 0.0237(13) Uani 1 1 d . . . . .
H14A H 0.6180 -0.0704 0.5849 0.028 Uiso 1 1 calc R U . . .
C15 C 0.7989(7) 0.0388(2) 0.0657(4) 0.0202(11) Uani 1 1 d . . . . .
C16 C 0.8318(9) 0.0544(3) -0.0302(3) 0.0234(12) Uani 1 1 d . . . . .
H16A H 0.7892 0.0196 -0.0684 0.035 Uiso 1 1 calc R U . . .
H16B H 0.9594 0.0605 -0.0380 0.035 Uiso 1 1 calc R U . . .
H16C H 0.7681 0.0933 -0.0468 0.035 Uiso 1 1 calc R U . . .
C17 C 0.6018(7) -0.1059(3) 0.0681(4) 0.0179(11) Uani 1 1 d . . . . .
C18 C 0.5407(7) -0.1594(2) 0.0117(4) 0.0186(11) Uani 1 1 d . . . . .
C19 C 0.5538(9) -0.1577(3) -0.0814(4) 0.0263(13) Uani 1 1 d . . . . .
H19A H 0.6050 -0.1222 -0.1099 0.032 Uiso 1 1 calc R U . . .
C20 C 0.4906(11) -0.2087(3) -0.1308(4) 0.0344(17) Uani 1 1 d . . . . .
H20A H 0.5024 -0.2082 -0.1938 0.041 Uiso 1 1 calc R U . . .
C21 C 0.4114(10) -0.2600(3) -0.0919(4) 0.0291(15) Uani 1 1 d . . . . .
H21A H 0.3654 -0.2937 -0.1277 0.035 Uiso 1 1 calc R U . . .
C22 C 0.3997(9) -0.2618(3) 0.0002(4) 0.0252(13) Uani 1 1 d . . . . .
H22A H 0.3470 -0.2973 0.0281 0.030 Uiso 1 1 calc R U . . .
C23 C 0.4650(8) -0.2118(3) 0.0519(4) 0.0194(12) Uani 1 1 d . . . . .
H23A H 0.4579 -0.2135 0.1150 0.023 Uiso 1 1 calc R U . . .
C24 C 0.4521(8) 0.0083(2) 0.2294(4) 0.0197(11) Uani 1 1 d . . . . .
C1S C 1.0587(9) -0.1145(3) 0.2419(4) 0.0261(13) Uani 1 1 d . . . . .
C2S C 1.2164(10) -0.1532(4) 0.2487(5) 0.051(2) Uani 1 1 d . . . . .
H1SC H 1.2250 -0.1727 0.3080 0.061 Uiso 1 1 calc R U . . .
H1SB H 1.3213 -0.1268 0.2395 0.061 Uiso 1 1 calc R U . . .
H1SA H 1.2099 -0.1864 0.2030 0.061 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 C24 1.920(6) . ?
Mo1 O2 2.117(4) . ?
Mo1 N1 2.128(5) . ?
Mo1 O1 2.127(4) . ?
Mo1 N4 2.135(5) . ?
Mo1 N2 2.131(5) . ?
Mo1 N1S 2.209(5) . ?
O3 C24 1.164(7) . ?
N1S C1S 1.128(7) . ?
O1 C8 1.298(6) . ?
O2 C17 1.289(6) . ?
N1 C5 1.365(7) . ?
N1 C1 1.363(7) . ?
N2 C6 1.316(7) . ?
N2 N3 1.389(6) . ?
N3 C8 1.292(7) . ?
N4 C15 1.304(7) . ?
N4 N5 1.386(6) . ?
C1 C2 1.389(8) . ?
C1 C6 1.438(8) . ?
C2 C3 1.373(8) . ?
C2 H2A 0.9500 . ?
C3 C4 1.376(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(8) . ?
C4 H4A 0.9500 . ?
N5 C17 1.322(7) . ?
C5 C15 1.433(8) . ?
C6 C7 1.485(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.483(7) . ?
C9 C10 1.389(8) . ?
C9 C14 1.392(8) . ?
C10 C11 1.396(8) . ?
C10 H10A 0.9500 . ?
C11 C12 1.377(8) . ?
C11 H11A 0.9500 . ?
C12 C13 1.382(9) . ?
C12 H12A 0.9500 . ?
C13 C14 1.374(8) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 C16 1.502(7) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.477(7) . ?
C18 C23 1.391(7) . ?
C18 C19 1.401(8) . ?
C19 C20 1.384(9) . ?
C19 H19A 0.9500 . ?
C20 C21 1.375(9) . ?
C20 H20A 0.9500 . ?
C21 C22 1.387(8) . ?
C21 H21A 0.9500 . ?
C22 C23 1.390(8) . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9500 . ?
C1S C2S 1.443(9) . ?
C2S H1SC 0.9800 . ?
C2S H1SB 0.9800 . ?
C2S H1SA 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
C24 Mo1 O2 93.9(2) . . ?
C24 Mo1 N1 93.6(2) . . ?
O2 Mo1 N1 141.62(16) . . ?
C24 Mo1 O1 91.8(2) . . ?
O2 Mo1 O1 75.29(14) . . ?
N1 Mo1 O1 141.93(16) . . ?
C24 Mo1 N4 93.0(2) . . ?
O2 Mo1 N4 71.41(16) . . ?
N1 Mo1 N4 70.64(17) . . ?
O1 Mo1 N4 146.61(16) . . ?
C24 Mo1 N2 92.4(2) . . ?
O2 Mo1 N2 146.23(15) . . ?
N1 Mo1 N2 70.76(17) . . ?
O1 Mo1 N2 71.37(16) . . ?
N4 Mo1 N2 141.28(17) . . ?
C24 Mo1 N1S 175.6(2) . . ?
O2 Mo1 N1S 83.71(17) . . ?
N1 Mo1 N1S 90.59(17) . . ?
O1 Mo1 N1S 84.01(16) . . ?
N4 Mo1 N1S 89.80(18) . . ?
N2 Mo1 N1S 87.57(18) . . ?
C1S N1S Mo1 177.2(5) . . ?
C8 O1 Mo1 115.4(3) . . ?
C17 O2 Mo1 116.6(3) . . ?
C5 N1 C1 118.3(5) . . ?
C5 N1 Mo1 120.8(4) . . ?
C1 N1 Mo1 120.8(4) . . ?
C6 N2 N3 116.9(5) . . ?
C6 N2 Mo1 123.3(4) . . ?
N3 N2 Mo1 119.8(3) . . ?
C8 N3 N2 108.5(4) . . ?
C15 N4 N5 116.7(4) . . ?
C15 N4 Mo1 123.1(4) . . ?
N5 N4 Mo1 120.1(3) . . ?
N1 C1 C2 121.6(5) . . ?
N1 C1 C6 113.1(5) . . ?
C2 C1 C6 125.3(5) . . ?
C3 C2 C1 119.7(6) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 119.3(6) . . ?
C2 C3 H3A 120.3 . . ?
C4 C3 H3A 120.3 . . ?
C3 C4 C5 119.7(6) . . ?
C3 C4 H4A 120.2 . . ?
C5 C4 H4A 120.2 . . ?
C17 N5 N4 108.1(4) . . ?
N1 C5 C4 121.3(5) . . ?
N1 C5 C15 112.6(5) . . ?
C4 C5 C15 126.0(5) . . ?
N2 C6 C1 112.0(5) . . ?
N2 C6 C7 124.3(5) . . ?
C1 C6 C7 123.6(5) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O1 C8 N3 124.7(5) . . ?
O1 C8 C9 117.7(5) . . ?
N3 C8 C9 117.6(5) . . ?
C10 C9 C14 119.8(5) . . ?
C10 C9 C8 120.2(5) . . ?
C14 C9 C8 120.1(5) . . ?
C11 C10 C9 120.0(5) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C12 C11 C10 119.9(5) . . ?
C12 C11 H11A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C11 C12 C13 119.5(5) . . ?
C11 C12 H12A 120.2 . . ?
C13 C12 H12A 120.2 . . ?
C14 C13 C12 121.5(6) . . ?
C14 C13 H13A 119.3 . . ?
C12 C13 H13A 119.3 . . ?
C13 C14 C9 119.3(5) . . ?
C13 C14 H14A 120.3 . . ?
C9 C14 H14A 120.3 . . ?
N4 C15 C5 112.8(5) . . ?
N4 C15 C16 124.8(5) . . ?
C5 C15 C16 122.3(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O2 C17 N5 123.7(5) . . ?
O2 C17 C18 118.5(5) . . ?
N5 C17 C18 117.8(5) . . ?
C23 C18 C19 119.6(5) . . ?
C23 C18 C17 119.1(5) . . ?
C19 C18 C17 121.3(5) . . ?
C20 C19 C18 118.6(6) . . ?
C20 C19 H19A 120.7 . . ?
C18 C19 H19A 120.7 . . ?
C21 C20 C19 122.2(6) . . ?
C21 C20 H20A 118.9 . . ?
C19 C20 H20A 118.9 . . ?
C20 C21 C22 119.0(6) . . ?
C20 C21 H21A 120.5 . . ?
C22 C21 H21A 120.5 . . ?
C21 C22 C23 120.1(5) . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C22 C23 C18 120.4(5) . . ?
C22 C23 H23A 119.8 . . ?
C18 C23 H23A 119.8 . . ?
O3 C24 Mo1 178.1(5) . . ?
N1S C1S C2S 178.0(7) . . ?
C1S C2S H1SC 109.5 . . ?
C1S C2S H1SB 109.5 . . ?
H1SC C2S H1SB 109.5 . . ?
C1S C2S H1SA 109.5 . . ?
H1SC C2S H1SA 109.5 . . ?
H1SB C2S H1SA 109.5 . . ?

_refine_diff_density_max         1.109
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.117

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1850319'
_audit_update_record             
;
2018-06-19 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H19 Cl2 Mo N5 O2, C8 H20 N'
_chemical_formula_sum            'C31 H39 Cl2 Mo N6 O2'
_chemical_formula_weight         694.52

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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'

_cell_length_a                   21.9939(8)
_cell_length_b                   11.0133(4)
_cell_length_c                   12.8402(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3110.22(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    4682
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      28.32

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_F_000             1436
_exptl_transmission_factor_min   0.879
_exptl_transmission_factor_max   0.906
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.633
_shelx_estimated_absorpt_T_min   0.879
_shelx_estimated_absorpt_T_max   0.906
_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      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  "Bruker APEX II CCD area detector'"
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37734
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.068
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8263
_reflns_number_gt                7119
_reflns_threshold_expression     I>2σ(I)
_reflns_Friedel_coverage         0.918
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'Bruker APEX II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0301P)²] 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 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8263
_refine_ls_number_parameters     386
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0327
_refine_ls_wR_factor_ref         0.0679
_refine_ls_wR_factor_gt          0.0636
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.60314(2) 0.65095(2) 0.48501(3) 0.01587(7) Uani 1 1 d . . . . .
Cl1 Cl 0.65401(4) 0.72204(10) 0.64156(8) 0.0270(2) Uani 1 1 d . . . . .
Cl2 Cl 0.54728(4) 0.57081(8) 0.33598(7) 0.02214(19) Uani 1 1 d . . . . .
O1 O 0.58996(11) 0.4844(2) 0.5590(2) 0.0215(6) Uani 1 1 d . . . . .
O2 O 0.52132(11) 0.6676(2) 0.5645(2) 0.0194(6) Uani 1 1 d . . . . .
N1 N 0.66359(14) 0.7464(3) 0.3931(3) 0.0187(7) Uani 1 1 d . . . . .
N2 N 0.67758(14) 0.5371(3) 0.4501(2) 0.0178(6) Uani 1 1 d . . . . .
N3 N 0.67946(11) 0.4181(2) 0.4875(3) 0.0188(5) Uani 1 1 d . . . . .
N4 N 0.56427(14) 0.8215(3) 0.4497(2) 0.0186(7) Uani 1 1 d . . . . .
N5 N 0.50603(11) 0.8516(3) 0.4858(4) 0.0204(5) Uani 1 1 d . . . . .
C1 C 0.71852(17) 0.6960(4) 0.3613(3) 0.0204(8) Uani 1 1 d . . . . .
C2 C 0.75992(18) 0.7605(4) 0.3005(3) 0.0259(9) Uani 1 1 d . . . . .
H2A H 0.7974 0.7241 0.2810 0.031 Uiso 1 1 calc R U . . .
C3 C 0.74657(19) 0.8779(4) 0.2685(3) 0.0312(10) Uani 1 1 d . . . . .
H3A H 0.7746 0.9225 0.2272 0.037 Uiso 1 1 calc R U . . .
C4 C 0.69163(19) 0.9286(4) 0.2981(3) 0.0273(9) Uani 1 1 d . . . . .
H4A H 0.6816 1.0087 0.2766 0.033 Uiso 1 1 calc R U . . .
C5 C 0.65094(18) 0.8630(3) 0.3591(3) 0.0213(8) Uani 1 1 d . . . . .
C6 C 0.72491(16) 0.5738(4) 0.3945(3) 0.0194(8) Uani 1 1 d . . . . .
C7 C 0.63052(17) 0.4010(3) 0.5438(3) 0.0177(7) Uani 1 1 d . . . . .
C8 C 0.62058(17) 0.2813(4) 0.5935(3) 0.0192(8) Uani 1 1 d . . . . .
C9 C 0.58020(17) 0.2726(4) 0.6772(3) 0.0214(8) Uani 1 1 d . . . . .
H9A H 0.5593 0.3427 0.7010 0.026 Uiso 1 1 calc R U . . .
C10 C 0.57062(19) 0.1614(4) 0.7256(3) 0.0278(9) Uani 1 1 d . . . . .
H10A H 0.5440 0.1564 0.7837 0.033 Uiso 1 1 calc R U . . .
C11 C 0.59957(19) 0.0584(4) 0.6899(3) 0.0290(9) Uani 1 1 d . . . . .
H11A H 0.5922 -0.0177 0.7223 0.035 Uiso 1 1 calc R U . . .
C12 C 0.63965(19) 0.0661(4) 0.6061(3) 0.0272(9) Uani 1 1 d . . . . .
H12A H 0.6596 -0.0048 0.5814 0.033 Uiso 1 1 calc R U . . .
C13 C 0.65052(18) 0.1772(3) 0.5587(3) 0.0237(8) Uani 1 1 d . . . . .
H13A H 0.6784 0.1824 0.5025 0.028 Uiso 1 1 calc R U . . .
C14 C 0.59218(18) 0.9034(4) 0.3915(3) 0.0216(8) Uani 1 1 d . . . . .
C15 C 0.48826(16) 0.7626(3) 0.5452(3) 0.0190(8) Uani 1 1 d . . . . .
C16 C 0.42754(17) 0.7678(4) 0.5957(3) 0.0193(8) Uani 1 1 d . . . . .
C17 C 0.41656(17) 0.6964(4) 0.6839(3) 0.0210(8) Uani 1 1 d . . . . .
H17A H 0.4481 0.6467 0.7110 0.025 Uiso 1 1 calc R U . . .
C18 C 0.36023(18) 0.6973(4) 0.7321(3) 0.0232(8) Uani 1 1 d . . . . .
H18A H 0.3536 0.6502 0.7930 0.028 Uiso 1 1 calc R U . . .
C19 C 0.31352(18) 0.7674(4) 0.6912(3) 0.0254(9) Uani 1 1 d . . . . .
H19A H 0.2747 0.7676 0.7236 0.031 Uiso 1 1 calc R U . . .
C20 C 0.32364(18) 0.8372(4) 0.6029(3) 0.0256(9) Uani 1 1 d . . . . .
H20A H 0.2914 0.8841 0.5744 0.031 Uiso 1 1 calc R U . . .
C21 C 0.38038(18) 0.8389(4) 0.5559(3) 0.0251(9) Uani 1 1 d . . . . .
H21A H 0.3872 0.8885 0.4965 0.030 Uiso 1 1 calc R U . . .
C22 C 0.77767(17) 0.4933(4) 0.3705(3) 0.0256(9) Uani 1 1 d . . . . .
H22A H 0.7891 0.4478 0.4331 0.038 Uiso 1 1 calc R U . . .
H22B H 0.8122 0.5429 0.3476 0.038 Uiso 1 1 calc R U . . .
H22C H 0.7664 0.4365 0.3151 0.038 Uiso 1 1 calc R U . . .
C23 C 0.56444(19) 1.0222(4) 0.3632(3) 0.0269(9) Uani 1 1 d . . . . .
H23A H 0.5256 1.0083 0.3279 0.040 Uiso 1 1 calc R U . . .
H23B H 0.5919 1.0664 0.3166 0.040 Uiso 1 1 calc R U . . .
H23C H 0.5576 1.0700 0.4265 0.040 Uiso 1 1 calc R U . . .
N1S N 0.39341(13) 0.3416(3) 0.4939(4) 0.0219(7) Uani 1 1 d . . . . .
C1S C 0.4330(2) 0.2829(4) 0.5770(4) 0.0330(10) Uani 1 1 d . . . . .
H1SA H 0.4761 0.2964 0.5584 0.040 Uiso 1 1 calc R U . . .
H1SB H 0.4254 0.3248 0.6440 0.040 Uiso 1 1 calc R U . . .
C2S C 0.4232(3) 0.1479(5) 0.5930(4) 0.0458(13) Uani 1 1 d . . . . .
H2SA H 0.4488 0.1195 0.6505 0.069 Uiso 1 1 calc R U . . .
H2SB H 0.4341 0.1043 0.5291 0.069 Uiso 1 1 calc R U . . .
H2SC H 0.3804 0.1327 0.6096 0.069 Uiso 1 1 calc R U . . .
C3S C 0.32695(19) 0.3425(4) 0.5275(3) 0.0315(10) Uani 1 1 d . . . . .
H3SA H 0.3017 0.3668 0.4672 0.038 Uiso 1 1 calc R U . . .
H3SB H 0.3151 0.2587 0.5468 0.038 Uiso 1 1 calc R U . . .
C4S C 0.3124(2) 0.4252(5) 0.6174(4) 0.0413(12) Uani 1 1 d . . . . .
H4SA H 0.2703 0.4122 0.6394 0.062 Uiso 1 1 calc R U . . .
H4SB H 0.3177 0.5098 0.5957 0.062 Uiso 1 1 calc R U . . .
H4SC H 0.3398 0.4074 0.6756 0.062 Uiso 1 1 calc R U . . .
C5S C 0.41728(17) 0.4701(3) 0.4816(4) 0.0281(8) Uani 1 1 d . . . . .
H5SA H 0.4147 0.5119 0.5497 0.034 Uiso 1 1 calc R U . . .
H5SB H 0.4607 0.4663 0.4616 0.034 Uiso 1 1 calc R U . . .
C6S C 0.3838(2) 0.5441(4) 0.4020(4) 0.0409(12) Uani 1 1 d . . . . .
H6SA H 0.4022 0.6248 0.3970 0.061 Uiso 1 1 calc R U . . .
H6SB H 0.3411 0.5521 0.4229 0.061 Uiso 1 1 calc R U . . .
H6SC H 0.3860 0.5036 0.3342 0.061 Uiso 1 1 calc R U . . .
C7S C 0.3964(2) 0.2718(4) 0.3930(3) 0.0301(10) Uani 1 1 d . . . . .
H7SA H 0.3669 0.3076 0.3435 0.036 Uiso 1 1 calc R U . . .
H7SB H 0.3838 0.1869 0.4063 0.036 Uiso 1 1 calc R U . . .
C8S C 0.4587(2) 0.2710(4) 0.3425(4) 0.0329(10) Uani 1 1 d . . . . .
H8SA H 0.4575 0.2214 0.2792 0.049 Uiso 1 1 calc R U . . .
H8SB H 0.4884 0.2369 0.3912 0.049 Uiso 1 1 calc R U . . .
H8SC H 0.4704 0.3542 0.3245 0.049 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 N1 2.066(3) . ?
Mo1 O2 2.077(2) . ?
Mo1 O1 2.086(3) . ?
Mo1 N2 2.110(3) . ?
Mo1 N4 2.113(3) . ?
Mo1 Cl1 2.4301(10) . ?
Mo1 Cl2 2.4392(10) . ?
O1 C7 1.295(4) . ?
O2 C15 1.298(4) . ?
N1 C5 1.384(5) . ?
N1 C1 1.391(5) . ?
N2 C6 1.325(5) . ?
N2 N3 1.396(4) . ?
N3 C7 1.310(5) . ?
N4 C14 1.322(5) . ?
N4 N5 1.402(4) . ?
N5 C15 1.302(5) . ?
C1 C2 1.393(5) . ?
C1 C6 1.419(6) . ?
C2 C3 1.387(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.384(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(5) . ?
C4 H4A 0.9500 . ?
C5 C14 1.429(5) . ?
C6 C22 1.492(5) . ?
C7 C8 1.481(5) . ?
C8 C13 1.396(5) . ?
C8 C9 1.397(5) . ?
C9 C10 1.389(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.380(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.393(6) . ?
C11 H11A 0.9500 . ?
C12 C13 1.387(6) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C23 1.488(5) . ?
C15 C16 1.485(5) . ?
C16 C21 1.396(5) . ?
C16 C17 1.400(5) . ?
C17 C18 1.385(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.388(6) . ?
C18 H18A 0.9500 . ?
C19 C20 1.388(6) . ?
C19 H19A 0.9500 . ?
C20 C21 1.386(6) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
N1S C7S 1.509(6) . ?
N1S C3S 1.524(5) . ?
N1S C1S 1.520(6) . ?
N1S C5S 1.517(4) . ?
C1S C2S 1.516(6) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C3S C4S 1.504(6) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
C5S C6S 1.500(7) . ?
C5S H5SA 0.9900 . ?
C5S H5SB 0.9900 . ?
C6S H6SA 0.9800 . ?
C6S H6SB 0.9800 . ?
C6S H6SC 0.9800 . ?
C7S C8S 1.516(6) . ?
C7S H7SA 0.9900 . ?
C7S H7SB 0.9900 . ?
C8S H8SA 0.9800 . ?
C8S H8SB 0.9800 . ?
C8S H8SC 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
N1 Mo1 O2 142.53(11) . . ?
N1 Mo1 O1 142.88(11) . . ?
O2 Mo1 O1 74.53(10) . . ?
N1 Mo1 N2 71.44(12) . . ?
O2 Mo1 N2 145.99(10) . . ?
O1 Mo1 N2 71.47(11) . . ?
N1 Mo1 N4 71.66(12) . . ?
O2 Mo1 N4 71.12(11) . . ?
O1 Mo1 N4 145.40(11) . . ?
N2 Mo1 N4 142.80(12) . . ?
N1 Mo1 Cl1 90.71(9) . . ?
O2 Mo1 Cl1 87.95(8) . . ?
O1 Mo1 Cl1 88.30(8) . . ?
N2 Mo1 Cl1 90.56(9) . . ?
N4 Mo1 Cl1 94.44(9) . . ?
N1 Mo1 Cl2 93.45(9) . . ?
O2 Mo1 Cl2 88.90(8) . . ?
O1 Mo1 Cl2 88.24(8) . . ?
N2 Mo1 Cl2 90.54(9) . . ?
N4 Mo1 Cl2 87.10(9) . . ?
Cl1 Mo1 Cl2 175.84(4) . . ?
C7 O1 Mo1 117.3(2) . . ?
C15 O2 Mo1 117.6(2) . . ?
C5 N1 C1 116.9(3) . . ?
C5 N1 Mo1 121.5(2) . . ?
C1 N1 Mo1 121.6(2) . . ?
C6 N2 N3 116.6(3) . . ?
C6 N2 Mo1 122.9(2) . . ?
N3 N2 Mo1 120.5(2) . . ?
C7 N3 N2 107.5(3) . . ?
C14 N4 N5 116.7(3) . . ?
C14 N4 Mo1 122.7(3) . . ?
N5 N4 Mo1 120.6(2) . . ?
C15 N5 N4 106.9(3) . . ?
C2 C1 N1 121.9(4) . . ?
C2 C1 C6 126.0(4) . . ?
N1 C1 C6 112.1(3) . . ?
C1 C2 C3 120.2(4) . . ?
C1 C2 H2A 119.9 . . ?
C3 C2 H2A 119.9 . . ?
C4 C3 C2 118.7(4) . . ?
C4 C3 H3A 120.7 . . ?
C2 C3 H3A 120.7 . . ?
C3 C4 C5 120.4(4) . . ?
C3 C4 H4A 119.8 . . ?
C5 C4 H4A 119.8 . . ?
N1 C5 C4 122.0(4) . . ?
N1 C5 C14 112.3(3) . . ?
C4 C5 C14 125.7(4) . . ?
N2 C6 C1 111.9(3) . . ?
N2 C6 C22 122.8(3) . . ?
C1 C6 C22 125.3(3) . . ?
O1 C7 N3 123.2(3) . . ?
O1 C7 C8 117.7(3) . . ?
N3 C7 C8 119.2(3) . . ?
C13 C8 C9 119.3(4) . . ?
C13 C8 C7 121.6(3) . . ?
C9 C8 C7 119.1(3) . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 H9A 119.9 . . ?
C8 C9 H9A 119.9 . . ?
C9 C10 C11 120.4(4) . . ?
C9 C10 H10A 119.8 . . ?
C11 C10 H10A 119.8 . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C13 C12 C11 120.1(4) . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C12 C13 C8 120.2(4) . . ?
C12 C13 H13A 119.9 . . ?
C8 C13 H13A 119.9 . . ?
N4 C14 C5 111.8(3) . . ?
N4 C14 C23 123.2(4) . . ?
C5 C14 C23 125.0(4) . . ?
N5 C15 O2 123.4(3) . . ?
N5 C15 C16 119.7(3) . . ?
O2 C15 C16 116.9(3) . . ?
C21 C16 C17 118.9(4) . . ?
C21 C16 C15 122.0(3) . . ?
C17 C16 C15 119.1(3) . . ?
C18 C17 C16 120.8(4) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C17 C18 C19 119.8(4) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C18 C19 C20 119.9(4) . . ?
C18 C19 H19A 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C21 C20 C19 120.5(4) . . ?
C21 C20 H20A 119.8 . . ?
C19 C20 H20A 119.8 . . ?
C20 C21 C16 120.2(4) . . ?
C20 C21 H21A 119.9 . . ?
C16 C21 H21A 119.9 . . ?
C6 C22 H22A 109.5 . . ?
C6 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C6 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C14 C23 H23A 109.5 . . ?
C14 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C14 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C7S N1S C3S 106.7(3) . . ?
C7S N1S C1S 111.2(3) . . ?
C3S N1S C1S 110.7(4) . . ?
C7S N1S C5S 111.7(4) . . ?
C3S N1S C5S 110.8(3) . . ?
C1S N1S C5S 105.8(3) . . ?
C2S C1S N1S 115.5(4) . . ?
C2S C1S H1SA 108.4 . . ?
N1S C1S H1SA 108.4 . . ?
C2S C1S H1SB 108.4 . . ?
N1S C1S H1SB 108.4 . . ?
H1SA C1S H1SB 107.5 . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
C4S C3S N1S 115.1(4) . . ?
C4S C3S H3SA 108.5 . . ?
N1S C3S H3SA 108.5 . . ?
C4S C3S H3SB 108.5 . . ?
N1S C3S H3SB 108.5 . . ?
H3SA C3S H3SB 107.5 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
C6S C5S N1S 114.0(4) . . ?
C6S C5S H5SA 108.7 . . ?
N1S C5S H5SA 108.7 . . ?
C6S C5S H5SB 108.7 . . ?
N1S C5S H5SB 108.7 . . ?
H5SA C5S H5SB 107.6 . . ?
C5S C6S H6SA 109.5 . . ?
C5S C6S H6SB 109.5 . . ?
H6SA C6S H6SB 109.5 . . ?
C5S C6S H6SC 109.5 . . ?
H6SA C6S H6SC 109.5 . . ?
H6SB C6S H6SC 109.5 . . ?
N1S C7S C8S 114.2(3) . . ?
N1S C7S H7SA 108.7 . . ?
C8S C7S H7SA 108.7 . . ?
N1S C7S H7SB 108.7 . . ?
C8S C7S H7SB 108.7 . . ?
H7SA C7S H7SB 107.6 . . ?
C7S C8S H8SA 109.5 . . ?
C7S C8S H8SB 109.5 . . ?
H8SA C8S H8SB 109.5 . . ?
C7S C8S H8SC 109.5 . . ?
H8SA C8S H8SC 109.5 . . ?
H8SB C8S H8SC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 N2 N3 C7 177.2(3) . . . . ?
Mo1 N2 N3 C7 -1.5(4) . . . . ?
C14 N4 N5 C15 -176.7(3) . . . . ?
Mo1 N4 N5 C15 4.7(4) . . . . ?
C5 N1 C1 C2 1.8(5) . . . . ?
Mo1 N1 C1 C2 -179.0(3) . . . . ?
C5 N1 C1 C6 -175.9(3) . . . . ?
Mo1 N1 C1 C6 3.2(4) . . . . ?
N1 C1 C2 C3 -1.0(6) . . . . ?
C6 C1 C2 C3 176.4(4) . . . . ?
C1 C2 C3 C4 -0.1(6) . . . . ?
C2 C3 C4 C5 0.3(6) . . . . ?
C1 N1 C5 C4 -1.6(5) . . . . ?
Mo1 N1 C5 C4 179.3(3) . . . . ?
C1 N1 C5 C14 176.9(3) . . . . ?
Mo1 N1 C5 C14 -2.2(4) . . . . ?
C3 C4 C5 N1 0.6(6) . . . . ?
C3 C4 C5 C14 -177.7(4) . . . . ?
N3 N2 C6 C1 -179.5(3) . . . . ?
Mo1 N2 C6 C1 -0.8(4) . . . . ?
N3 N2 C6 C22 0.9(5) . . . . ?
Mo1 N2 C6 C22 179.6(3) . . . . ?
C2 C1 C6 N2 -179.1(4) . . . . ?
N1 C1 C6 N2 -1.4(5) . . . . ?
C2 C1 C6 C22 0.5(6) . . . . ?
N1 C1 C6 C22 178.1(3) . . . . ?
Mo1 O1 C7 N3 2.2(5) . . . . ?
Mo1 O1 C7 C8 -178.2(2) . . . . ?
N2 N3 C7 O1 -0.5(5) . . . . ?
N2 N3 C7 C8 179.9(3) . . . . ?
O1 C7 C8 C13 160.8(4) . . . . ?
N3 C7 C8 C13 -19.6(5) . . . . ?
O1 C7 C8 C9 -19.1(5) . . . . ?
N3 C7 C8 C9 160.5(4) . . . . ?
C13 C8 C9 C10 0.7(6) . . . . ?
C7 C8 C9 C10 -179.4(3) . . . . ?
C8 C9 C10 C11 -1.8(6) . . . . ?
C9 C10 C11 C12 1.4(6) . . . . ?
C10 C11 C12 C13 0.1(6) . . . . ?
C11 C12 C13 C8 -1.1(6) . . . . ?
C9 C8 C13 C12 0.7(6) . . . . ?
C7 C8 C13 C12 -179.2(3) . . . . ?
N5 N4 C14 C5 -179.9(3) . . . . ?
Mo1 N4 C14 C5 -1.4(4) . . . . ?
N5 N4 C14 C23 -0.6(5) . . . . ?
Mo1 N4 C14 C23 177.9(3) . . . . ?
N1 C5 C14 N4 2.2(5) . . . . ?
C4 C5 C14 N4 -179.4(4) . . . . ?
N1 C5 C14 C23 -177.1(4) . . . . ?
C4 C5 C14 C23 1.3(6) . . . . ?
N4 N5 C15 O2 0.7(5) . . . . ?
N4 N5 C15 C16 -180.0(3) . . . . ?
Mo1 O2 C15 N5 -5.8(5) . . . . ?
Mo1 O2 C15 C16 174.9(2) . . . . ?
N5 C15 C16 C21 23.3(6) . . . . ?
O2 C15 C16 C21 -157.3(4) . . . . ?
N5 C15 C16 C17 -158.9(4) . . . . ?
O2 C15 C16 C17 20.5(5) . . . . ?
C21 C16 C17 C18 -1.0(6) . . . . ?
C15 C16 C17 C18 -179.0(4) . . . . ?
C16 C17 C18 C19 1.7(6) . . . . ?
C17 C18 C19 C20 -0.7(6) . . . . ?
C18 C19 C20 C21 -0.9(6) . . . . ?
C19 C20 C21 C16 1.6(6) . . . . ?
C17 C16 C21 C20 -0.6(6) . . . . ?
C15 C16 C21 C20 177.3(4) . . . . ?
C7S N1S C1S C2S -50.7(5) . . . . ?
C3S N1S C1S C2S 67.7(5) . . . . ?
C5S N1S C1S C2S -172.2(4) . . . . ?
C7S N1S C3S C4S -170.3(4) . . . . ?
C1S N1S C3S C4S 68.6(5) . . . . ?
C5S N1S C3S C4S -48.4(6) . . . . ?
C7S N1S C5S C6S 58.9(4) . . . . ?
C3S N1S C5S C6S -60.0(6) . . . . ?
C1S N1S C5S C6S -180.0(4) . . . . ?
C3S N1S C7S C8S 174.9(4) . . . . ?
C1S N1S C7S C8S -64.4(5) . . . . ?
C5S N1S C7S C8S 53.6(5) . . . . ?

_refine_diff_density_max         0.377
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.068

_shelxl_version_number           2014/6

