# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

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

data_tj129_a
_database_code_depnum_ccdc_archive 'CCDC 1509812'
_audit_update_record             
;
2016-10-13 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_audit_creation_date             2016-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        
'MoO2(R-AMD)2 (AMD = N,N?-di-R-acetamidinate) R = isopropyl'
_chemical_formula_moiety         'C16 H34 Mo N4 O2'
_chemical_formula_sum            'C16 H34 Mo N4 O2'
_chemical_formula_weight         410.41
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Mo Mo -1.6832 0.6857 '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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   10.3994(4)
_cell_length_b                   10.3994(4)
_cell_length_c                   18.7146(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2023.94(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9673
_cell_measurement_temperature    100
_cell_measurement_theta_max      53.30
_cell_measurement_theta_min      2.98
_shelx_estimated_absorpt_T_max   0.811
_shelx_estimated_absorpt_T_min   0.768
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.6726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0960 before and 0.0607 after correction.
The Ratio of minimum to maximum transmission is 0.8958.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.33
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            71443
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         54.817
_diffrn_reflns_theta_min         2.976
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   microsource
_diffrn_special_details          
;
The Mo atom was found to be disorder over two positions 
with partial occupancy 0.21:0.79.
;
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                10832
_reflns_number_total             12623
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.898
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 
;
 Flack x determined using 4250 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         12623
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0257
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0263P)²+0.0090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0564
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Mo1A)=0.5*(1-FVAR(2))
 Sof(Mo1)=0.5*FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.42330(7) 0.57670(7) 0.7500 0.01386(12) Uani 0.79(2) 2 d S T P A 1
O1 O 0.42447(9) 0.71887(6) 0.70351(5) 0.03375(18) Uani 1 1 d . . . . .
N1 N 0.56680(5) 0.48367(6) 0.67390(3) 0.01577(8) Uani 1 1 d . . . . .
N2 N 0.36219(5) 0.43663(6) 0.67804(3) 0.01605(8) Uani 1 1 d . . . . .
C1 C 0.47462(6) 0.41911(6) 0.64298(3) 0.01440(8) Uani 1 1 d . . . . .
C2 C 0.49039(8) 0.33523(8) 0.57828(4) 0.02230(12) Uani 1 1 d . . . . .
H2A H 0.4055 0.3106 0.5601 0.033 Uiso 1 1 calc GR . . . .
H2B H 0.5388 0.2578 0.5913 0.033 Uiso 1 1 calc GR . . . .
H2C H 0.5372 0.3826 0.5412 0.033 Uiso 1 1 calc GR . . . .
C3 C 0.23651(6) 0.39063(7) 0.65357(4) 0.01677(9) Uani 1 1 d . . . . .
H3 H 0.2515 0.3222 0.6169 0.020 Uiso 1 1 calc R . . . .
C4 C 0.16242(9) 0.49942(9) 0.61788(6) 0.02703(16) Uani 1 1 d . . . . .
H4A H 0.1439 0.5665 0.6532 0.041 Uiso 1 1 calc GR . . . .
H4B H 0.0815 0.4660 0.5985 0.041 Uiso 1 1 calc GR . . . .
H4C H 0.2142 0.5357 0.5791 0.041 Uiso 1 1 calc GR . . . .
C5 C 0.15987(9) 0.33139(10) 0.71437(5) 0.02639(15) Uani 1 1 d . . . . .
H5A H 0.2080 0.2591 0.7347 0.040 Uiso 1 1 calc GR . . . .
H5B H 0.0770 0.3006 0.6962 0.040 Uiso 1 1 calc GR . . . .
H5C H 0.1451 0.3963 0.7515 0.040 Uiso 1 1 calc GR . . . .
C6 C 0.69785(7) 0.49137(8) 0.64687(4) 0.01947(10) Uani 1 1 d . . . . .
H6 H 0.7132 0.4173 0.6139 0.023 Uiso 1 1 calc R . . . .
C7 C 0.71484(11) 0.61620(12) 0.60517(6) 0.0333(2) Uani 1 1 d . . . . .
H7A H 0.6530 0.6188 0.5657 0.050 Uiso 1 1 calc GR . . . .
H7B H 0.8025 0.6205 0.5861 0.050 Uiso 1 1 calc GR . . . .
H7C H 0.7000 0.6895 0.6370 0.050 Uiso 1 1 calc GR . . . .
C8 C 0.79271(8) 0.48308(11) 0.70852(5) 0.02785(16) Uani 1 1 d . . . . .
H8A H 0.7770 0.5540 0.7419 0.042 Uiso 1 1 calc GR . . . .
H8B H 0.8807 0.4890 0.6900 0.042 Uiso 1 1 calc GR . . . .
H8C H 0.7816 0.4009 0.7334 0.042 Uiso 1 1 calc GR . . . .
Mo1A Mo 0.4186(3) 0.5814(3) 0.7500 0.0247(8) Uani 0.21(2) 2 d S T P A 2


_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 O1 1.7155(9) . ?
Mo1 O1 1.7155(9) 8_666 ?
Mo1 N1 2.2785(10) 8_666 ?
Mo1 N1 2.2784(10) . ?
Mo1 N2 2.0832(6) . ?
Mo1 N2 2.0832(6) 8_666 ?
O1 Mo1A 1.674(3) . ?
N1 C1 1.3056(8) . ?
N1 C6 1.4559(9) . ?
N1 Mo1A 2.332(3) . ?
N2 C1 1.3530(8) . ?
N2 C3 1.4652(8) . ?
N2 Mo1A 2.1036(14) . ?
C1 C2 1.5014(10) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3 1.0000 . ?
C3 C4 1.5231(11) . ?
C3 C5 1.5197(12) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6 1.0000 . ?
C6 C7 1.5249(13) . ?
C6 C8 1.5206(12) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
Mo1A O1 1.674(3) 8_666 ?
Mo1A N1 2.332(3) 8_666 ?
Mo1A N2 2.1036(14) 8_666 ?

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 O1 105.63(9) . 8_666 ?
O1 Mo1 N1 92.54(4) 8_666 8_666 ?
O1 Mo1 N1 92.54(4) . . ?
O1 Mo1 N1 151.46(4) . 8_666 ?
O1 Mo1 N1 151.46(4) 8_666 . ?
O1 Mo1 N2 106.08(3) . . ?
O1 Mo1 N2 106.08(3) 8_666 8_666 ?
O1 Mo1 N2 93.44(3) 8_666 . ?
O1 Mo1 N2 93.44(3) . 8_666 ?
N1 Mo1 N1 80.48(4) . 8_666 ?
N2 Mo1 N1 59.92(3) 8_666 8_666 ?
N2 Mo1 N1 94.34(4) . 8_666 ?
N2 Mo1 N1 94.34(4) 8_666 . ?
N2 Mo1 N1 59.92(3) . . ?
N2 Mo1 N2 147.63(6) . 8_666 ?
C1 N1 Mo1 90.83(4) . . ?
C1 N1 C6 124.16(6) . . ?
C1 N1 Mo1A 90.54(4) . . ?
C6 N1 Mo1 143.80(5) . . ?
C6 N1 Mo1A 143.81(5) . . ?
C1 N2 Mo1 98.28(4) . . ?
C1 N2 C3 125.12(6) . . ?
C1 N2 Mo1A 99.55(9) . . ?
C3 N2 Mo1 134.63(5) . . ?
C3 N2 Mo1A 133.04(11) . . ?
N1 C1 N2 110.51(6) . . ?
N1 C1 C2 125.17(6) . . ?
N2 C1 C2 124.31(6) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 H3 107.9 . . ?
N2 C3 C4 110.23(6) . . ?
N2 C3 C5 111.48(6) . . ?
C4 C3 H3 107.9 . . ?
C5 C3 H3 107.9 . . ?
C5 C3 C4 111.35(7) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 H6 108.7 . . ?
N1 C6 C7 109.45(7) . . ?
N1 C6 C8 109.91(6) . . ?
C7 C6 H6 108.7 . . ?
C8 C6 H6 108.7 . . ?
C8 C6 C7 111.18(8) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 Mo1A O1 109.4(2) . 8_666 ?
O1 Mo1A N1 149.96(10) 8_666 . ?
O1 Mo1A N1 91.75(6) . . ?
O1 Mo1A N1 91.75(6) 8_666 8_666 ?
O1 Mo1A N1 149.96(10) . 8_666 ?
O1 Mo1A N2 93.93(4) 8_666 . ?
O1 Mo1A N2 106.78(5) . . ?
O1 Mo1A N2 106.77(5) 8_666 8_666 ?
O1 Mo1A N2 93.93(4) . 8_666 ?
N1 Mo1A N1 78.27(13) . 8_666 ?
N2 Mo1A N1 92.26(13) . 8_666 ?
N2 Mo1A N1 58.75(7) . . ?
N2 Mo1A N1 92.26(13) 8_666 . ?
N2 Mo1A N1 58.75(7) 8_666 8_666 ?
N2 Mo1A N2 144.0(2) . 8_666 ?

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 N1 C1 N2 -6.03(6) . . . . ?
Mo1 N1 C1 C2 174.86(7) . . . . ?
Mo1 N1 C6 C7 -65.09(11) . . . . ?
Mo1 N1 C6 C8 57.28(11) . . . . ?
Mo1 N2 C1 N1 6.67(7) . . . . ?
Mo1 N2 C1 C2 -174.21(6) . . . . ?
Mo1 N2 C3 C4 60.92(10) . . . . ?
Mo1 N2 C3 C5 -63.27(9) . . . . ?
C1 N1 C6 C7 98.04(9) . . . . ?
C1 N1 C6 C8 -139.58(8) . . . . ?
C1 N2 C3 C4 -99.42(9) . . . . ?
C1 N2 C3 C5 136.38(8) . . . . ?
C3 N2 C1 N1 172.67(6) . . . . ?
C3 N2 C1 C2 -8.21(11) . . . . ?
C6 N1 C1 N2 -176.17(6) . . . . ?
C6 N1 C1 C2 4.73(11) . . . . ?
Mo1A N1 C1 N2 -7.10(8) . . . . ?
Mo1A N1 C1 C2 173.79(9) . . . . ?
Mo1A N1 C6 C7 -63.23(15) . . . . ?
Mo1A N1 C6 C8 59.15(15) . . . . ?
Mo1A N2 C1 N1 7.99(10) . . . . ?
Mo1A N2 C1 C2 -172.90(10) . . . . ?
Mo1A N2 C3 C4 59.70(12) . . . . ?
Mo1A N2 C3 C5 -64.49(12) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_date_sample_data_collection 2016-02-06
_olex2_date_sample_submission    2016-02-06
_olex2_exptl_crystal_mounting_method 'Mounted at 100 K on a brass tip.'
_olex2_submission_original_sample_id TJ129
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_sol2
_database_code_depnum_ccdc_archive 'CCDC 1509811'
_audit_update_record             
;
2016-10-13 deposited with the CCDC.
2016-12-22 downloaded from the CCDC.
;
_audit_creation_date             2016-08-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_chemical_name_common            ?
_chemical_name_systematic        
'MoO2(R-AMD)2 (AMD = N,N?-di-R-acetamidinate) R = cyclohexyl '
_chemical_formula_moiety         'C28 H50 Mo N4 O2'
_chemical_formula_sum            'C28 H50 Mo N4 O2'
_chemical_formula_weight         570.66
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
Mo Mo -1.6832 0.6857 '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'

_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.
;
_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'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   11.4715(2)
_cell_length_b                   11.6621(2)
_cell_length_c                   21.5619(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2884.59(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.85
_cell_measurement_theta_min      2.66
_shelx_estimated_absorpt_T_max   0.960
_shelx_estimated_absorpt_T_min   0.900
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.7475
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0676 before and 0.0577 after correction.
The Ratio of minimum to maximum transmission is 0.8852.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.085
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0702
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            44589
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         38.211
_diffrn_reflns_theta_min         2.664
_diffrn_ambient_temperature      100.06
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          None
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                11565
_reflns_number_total             15363
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         2.095
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 
;
 Flack x determined using 4398 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.790
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         15363
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0491
_refine_ls_restrained_S_all      0.790
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1336
_refine_special_details          None
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9), C17(H17), C3(H3), C23(H23)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B), C11(H11A,H11B), C14(H14A,H14B), C12(H12A,
 H12B), C8(H8A,H8B), C21(H21A,H21B), C18(H18A,H18B), C22(H22A,H22B), C4(H4A,
 H4B), C27(H27A,H27B), C5(H5A,H5B), C28(H28A,H28B), C25(H25A,H25B), C6(H6A,H6B),
  C7(H7A,H7B), C20(H20A,H20B), C19(H19A,H19B), C24(H24A,H24B), C26(H26A,H26B)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 -0.07731(2) -0.41162(2) -0.36598(2) 0.01314(6) Uani 1 1 d . . . . .
C2 C 0.2815(3) -0.4169(3) -0.34719(17) 0.0202(6) Uani 1 1 d . . . . .
H2A H 0.3195 -0.4764 -0.3721 0.030 Uiso 1 1 calc GR . . . .
H2B H 0.2992 -0.4293 -0.3032 0.030 Uiso 1 1 calc GR . . . .
H2C H 0.3102 -0.3414 -0.3599 0.030 Uiso 1 1 calc GR . . . .
C1 C 0.1520(3) -0.4226(2) -0.35686(12) 0.0130(5) Uani 1 1 d . . . . .
C10 C 0.0949(3) -0.5970(3) -0.49432(15) 0.0160(5) Uani 1 1 d . . . . .
H10A H 0.0125 -0.5760 -0.5017 0.019 Uiso 1 1 calc R . . . .
H10B H 0.0963 -0.6657 -0.4673 0.019 Uiso 1 1 calc R . . . .
O1 O -0.0897(2) -0.2992(2) -0.41626(12) 0.0208(5) Uani 1 1 d . . . . .
C9 C 0.1572(3) -0.4982(3) -0.46192(13) 0.0142(5) Uani 1 1 d . . . . .
H9 H 0.2389 -0.5223 -0.4523 0.017 Uiso 1 1 calc R . . . .
N4 N 0.0989(2) -0.4687(2) -0.40432(12) 0.0146(4) Uani 1 1 d . . . . .
O2 O -0.1683(2) -0.3812(2) -0.30545(12) 0.0215(5) Uani 1 1 d . . . . .
C13 C 0.2150(4) -0.4188(3) -0.56736(17) 0.0254(7) Uani 1 1 d . . . . .
H13A H 0.2084 -0.3502 -0.5942 0.030 Uiso 1 1 calc R . . . .
H13B H 0.2988 -0.4363 -0.5620 0.030 Uiso 1 1 calc R . . . .
C11 C 0.1538(3) -0.6249(3) -0.55610(15) 0.0216(6) Uani 1 1 d . . . . .
H11A H 0.2349 -0.6503 -0.5484 0.026 Uiso 1 1 calc R . . . .
H11B H 0.1117 -0.6884 -0.5767 0.026 Uiso 1 1 calc R . . . .
C14 C 0.1609(3) -0.3929(3) -0.50416(16) 0.0202(6) Uani 1 1 d . . . . .
H14A H 0.0805 -0.3640 -0.5103 0.024 Uiso 1 1 calc R . . . .
H14B H 0.2065 -0.3317 -0.4836 0.024 Uiso 1 1 calc R . . . .
C12 C 0.1547(3) -0.5200(4) -0.59856(15) 0.0250(7) Uani 1 1 d . . . . .
H12A H 0.1958 -0.5390 -0.6376 0.030 Uiso 1 1 calc R . . . .
H12B H 0.0735 -0.4986 -0.6091 0.030 Uiso 1 1 calc R . . . .
N2 N -0.0798(2) -0.6050(2) -0.34308(13) 0.0136(4) Uani 1 1 d . . . . .
C17 C -0.0378(3) -0.6950(3) -0.30178(13) 0.0148(5) Uani 1 1 d . . . . .
H17 H -0.0941 -0.7603 -0.3036 0.018 Uiso 1 1 calc R . . . .
N1 N -0.1628(2) -0.5273(2) -0.42400(12) 0.0150(5) Uani 1 1 d . . . . .
N3 N 0.0744(2) -0.3808(3) -0.31569(13) 0.0151(4) Uani 1 1 d . . . . .
C8 C 0.0933(3) -0.3661(3) -0.20087(15) 0.0195(6) Uani 1 1 d . . . . .
H8A H 0.1418 -0.4363 -0.2000 0.023 Uiso 1 1 calc R . . . .
H8B H 0.0109 -0.3892 -0.1953 0.023 Uiso 1 1 calc R . . . .
C3 C 0.1074(3) -0.3068(3) -0.26336(14) 0.0158(5) Uani 1 1 d . . . . .
H3 H 0.1914 -0.2860 -0.2684 0.019 Uiso 1 1 calc R . . . .
C21 C 0.1228(3) -0.8338(3) -0.27774(17) 0.0235(7) Uani 1 1 d . . . . .
H21A H 0.0698 -0.9005 -0.2810 0.028 Uiso 1 1 calc R . . . .
H21B H 0.2018 -0.8590 -0.2903 0.028 Uiso 1 1 calc R . . . .
C15 C -0.1366(3) -0.6259(3) -0.39402(13) 0.0142(5) Uani 1 1 d . . . . .
C18 C -0.0344(3) -0.6508(3) -0.23523(14) 0.0206(6) Uani 1 1 d . . . . .
H18A H 0.0185 -0.5839 -0.2327 0.025 Uiso 1 1 calc R . . . .
H18B H -0.1134 -0.6254 -0.2228 0.025 Uiso 1 1 calc R . . . .
C23 C -0.2494(3) -0.5215(3) -0.47377(14) 0.0169(5) Uani 1 1 d . . . . .
H23 H -0.2562 -0.6001 -0.4920 0.020 Uiso 1 1 calc R . . . .
C16 C -0.1649(3) -0.7425(3) -0.41997(16) 0.0196(6) Uani 1 1 d . . . . .
H16A H -0.1360 -0.7478 -0.4626 0.029 Uiso 1 1 calc GR . . . .
H16B H -0.2495 -0.7539 -0.4196 0.029 Uiso 1 1 calc GR . . . .
H16C H -0.1275 -0.8016 -0.3945 0.029 Uiso 1 1 calc GR . . . .
C22 C 0.0811(3) -0.7391(3) -0.32153(16) 0.0210(6) Uani 1 1 d . . . . .
H22A H 0.1379 -0.6752 -0.3213 0.025 Uiso 1 1 calc R . . . .
H22B H 0.0764 -0.7695 -0.3643 0.025 Uiso 1 1 calc R . . . .
C4 C 0.0360(3) -0.1961(3) -0.26464(16) 0.0202(6) Uani 1 1 d . . . . .
H4A H -0.0479 -0.2148 -0.2609 0.024 Uiso 1 1 calc R . . . .
H4B H 0.0481 -0.1567 -0.3048 0.024 Uiso 1 1 calc R . . . .
C27 C -0.3077(4) -0.4432(4) -0.57771(16) 0.0262(7) Uani 1 1 d . . . . .
H27A H -0.2863 -0.3870 -0.6102 0.031 Uiso 1 1 calc R . . . .
H27B H -0.3087 -0.5203 -0.5969 0.031 Uiso 1 1 calc R . . . .
C5 C 0.0714(3) -0.1159(3) -0.21167(17) 0.0211(6) Uani 1 1 d . . . . .
H5A H 0.1528 -0.0904 -0.2180 0.025 Uiso 1 1 calc R . . . .
H5B H 0.0208 -0.0471 -0.2122 0.025 Uiso 1 1 calc R . . . .
C28 C -0.2160(3) -0.4405(4) -0.52606(16) 0.0236(7) Uani 1 1 d . . . . .
H28A H -0.1393 -0.4633 -0.5432 0.028 Uiso 1 1 calc R . . . .
H28B H -0.2090 -0.3615 -0.5097 0.028 Uiso 1 1 calc R . . . .
C25 C -0.4617(4) -0.4927(5) -0.4989(2) 0.0362(11) Uani 1 1 d . . . . .
H25A H -0.4712 -0.5723 -0.5139 0.043 Uiso 1 1 calc R . . . .
H25B H -0.5371 -0.4673 -0.4812 0.043 Uiso 1 1 calc R . . . .
C6 C 0.0611(3) -0.1748(3) -0.14923(16) 0.0209(6) Uani 1 1 d . . . . .
H6A H -0.0221 -0.1908 -0.1404 0.025 Uiso 1 1 calc R . . . .
H6B H 0.0906 -0.1229 -0.1164 0.025 Uiso 1 1 calc R . . . .
C7 C 0.1296(4) -0.2866(3) -0.14767(16) 0.0238(7) Uani 1 1 d . . . . .
H7A H 0.1160 -0.3258 -0.1076 0.029 Uiso 1 1 calc R . . . .
H7B H 0.2139 -0.2697 -0.1510 0.029 Uiso 1 1 calc R . . . .
C20 C 0.1261(4) -0.7924(4) -0.21085(18) 0.0258(7) Uani 1 1 d . . . . .
H20A H 0.1864 -0.7323 -0.2065 0.031 Uiso 1 1 calc R . . . .
H20B H 0.1474 -0.8571 -0.1833 0.031 Uiso 1 1 calc R . . . .
C19 C 0.0077(4) -0.7441(3) -0.19107(15) 0.0251(7) Uani 1 1 d . . . . .
H19A H -0.0503 -0.8069 -0.1900 0.030 Uiso 1 1 calc R . . . .
H19B H 0.0141 -0.7119 -0.1487 0.030 Uiso 1 1 calc R . . . .
C24 C -0.3681(3) -0.4894(4) -0.44848(18) 0.0295(8) Uani 1 1 d . . . . .
H24A H -0.3645 -0.4113 -0.4306 0.035 Uiso 1 1 calc R . . . .
H24B H -0.3896 -0.5432 -0.4149 0.035 Uiso 1 1 calc R . . . .
C26 C -0.4288(3) -0.4151(3) -0.5530(2) 0.0235(7) Uani 1 1 d . . . . .
H26A H -0.4308 -0.3341 -0.5392 0.028 Uiso 1 1 calc R . . . .
H26B H -0.4867 -0.4244 -0.5867 0.028 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 O1 1.707(3) . ?
Mo1 N4 2.282(3) . ?
Mo1 O2 1.708(3) . ?
Mo1 N2 2.309(3) . ?
Mo1 N1 2.085(3) . ?
Mo1 N3 2.082(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 C1 1.501(5) . ?
C1 N4 1.307(4) . ?
C1 N3 1.349(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C9 1.525(5) . ?
C10 C11 1.529(5) . ?
C9 H9 1.0000 . ?
C9 N4 1.452(4) . ?
C9 C14 1.530(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.527(5) . ?
C13 C12 1.525(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.528(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N2 C17 1.458(4) . ?
N2 C15 1.300(4) . ?
C17 H17 1.0000 . ?
C17 C18 1.525(4) . ?
C17 C22 1.519(5) . ?
N1 C15 1.353(4) . ?
N1 C23 1.464(4) . ?
N3 C3 1.470(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C3 1.523(5) . ?
C8 C7 1.532(5) . ?
C3 H3 1.0000 . ?
C3 C4 1.530(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.530(5) . ?
C21 C20 1.521(5) . ?
C15 C16 1.506(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.524(5) . ?
C23 H23 1.0000 . ?
C23 C28 1.520(5) . ?
C23 C24 1.514(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.531(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.532(5) . ?
C27 C26 1.524(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.516(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C24 1.528(5) . ?
C25 C26 1.524(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.524(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C19 1.532(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?

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 N4 93.87(11) . . ?
O1 Mo1 O2 105.96(14) . . ?
O1 Mo1 N2 152.23(11) . . ?
O1 Mo1 N1 94.39(11) . . ?
O1 Mo1 N3 105.54(13) . . ?
N4 Mo1 N2 78.68(10) . . ?
O2 Mo1 N4 151.41(12) . . ?
O2 Mo1 N2 91.83(12) . . ?
O2 Mo1 N1 107.79(12) . . ?
O2 Mo1 N3 94.41(11) . . ?
N1 Mo1 N4 90.60(10) . . ?
N1 Mo1 N2 59.37(10) . . ?
N3 Mo1 N4 59.92(10) . . ?
N3 Mo1 N2 93.87(11) . . ?
N3 Mo1 N1 144.82(11) . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
N4 C1 C2 126.1(3) . . ?
N4 C1 N3 110.8(3) . . ?
N3 C1 C2 123.1(3) . . ?
H10A C10 H10B 108.1 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 C11 110.7(3) . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C10 C9 H9 108.8 . . ?
C10 C9 C14 110.3(3) . . ?
N4 C9 C10 110.8(3) . . ?
N4 C9 H9 108.8 . . ?
N4 C9 C14 109.4(3) . . ?
C14 C9 H9 108.8 . . ?
C1 N4 Mo1 90.57(19) . . ?
C1 N4 C9 123.5(3) . . ?
C9 N4 Mo1 141.9(2) . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C12 C13 C14 111.2(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
C12 C11 C10 110.8(3) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
C9 C14 H14A 109.1 . . ?
C9 C14 H14B 109.1 . . ?
C13 C14 C9 112.6(3) . . ?
C13 C14 H14A 109.1 . . ?
C13 C14 H14B 109.1 . . ?
H14A C14 H14B 107.8 . . ?
C13 C12 C11 111.0(3) . . ?
C13 C12 H12A 109.4 . . ?
C13 C12 H12B 109.4 . . ?
C11 C12 H12A 109.4 . . ?
C11 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C17 N2 Mo1 146.0(2) . . ?
C15 N2 Mo1 90.5(2) . . ?
C15 N2 C17 123.2(3) . . ?
N2 C17 H17 108.1 . . ?
N2 C17 C18 109.9(3) . . ?
N2 C17 C22 111.7(3) . . ?
C18 C17 H17 108.1 . . ?
C22 C17 H17 108.1 . . ?
C22 C17 C18 110.8(3) . . ?
C15 N1 Mo1 99.14(19) . . ?
C15 N1 C23 122.7(3) . . ?
C23 N1 Mo1 136.8(2) . . ?
C1 N3 Mo1 98.45(19) . . ?
C1 N3 C3 123.2(3) . . ?
C3 N3 Mo1 135.7(2) . . ?
H8A C8 H8B 108.0 . . ?
C3 C8 H8A 109.4 . . ?
C3 C8 H8B 109.4 . . ?
C3 C8 C7 111.0(3) . . ?
C7 C8 H8A 109.4 . . ?
C7 C8 H8B 109.4 . . ?
N3 C3 C8 112.7(3) . . ?
N3 C3 H3 108.0 . . ?
N3 C3 C4 110.1(3) . . ?
C8 C3 H3 108.0 . . ?
C8 C3 C4 110.0(3) . . ?
C4 C3 H3 108.0 . . ?
H21A C21 H21B 108.0 . . ?
C22 C21 H21A 109.4 . . ?
C22 C21 H21B 109.4 . . ?
C20 C21 H21A 109.4 . . ?
C20 C21 H21B 109.4 . . ?
C20 C21 C22 111.3(3) . . ?
N2 C15 N1 110.8(3) . . ?
N2 C15 C16 126.2(3) . . ?
N1 C15 C16 122.8(3) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C19 C18 C17 110.8(3) . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
N1 C23 H23 107.4 . . ?
N1 C23 C28 113.6(3) . . ?
N1 C23 C24 111.0(3) . . ?
C28 C23 H23 107.4 . . ?
C24 C23 H23 107.4 . . ?
C24 C23 C28 109.9(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 C22 C21 110.7(3) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
C3 C4 C5 111.1(3) . . ?
H4A C4 H4B 108.0 . . ?
C5 C4 H4A 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H27A C27 H27B 108.0 . . ?
C28 C27 H27A 109.3 . . ?
C28 C27 H27B 109.3 . . ?
C26 C27 H27A 109.3 . . ?
C26 C27 H27B 109.3 . . ?
C26 C27 C28 111.5(3) . . ?
C4 C5 H5A 109.3 . . ?
C4 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C6 C5 C4 111.4(3) . . ?
C6 C5 H5A 109.3 . . ?
C6 C5 H5B 109.3 . . ?
C23 C28 C27 110.7(3) . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
H25A C25 H25B 108.1 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
C26 C25 C24 110.8(3) . . ?
C5 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
C5 C6 C7 111.5(3) . . ?
H6A C6 H6B 108.0 . . ?
C7 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C6 C7 C8 111.2(3) . . ?
C6 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C21 C20 H20A 109.4 . . ?
C21 C20 H20B 109.4 . . ?
C21 C20 C19 111.0(3) . . ?
H20A C20 H20B 108.0 . . ?
C19 C20 H20A 109.4 . . ?
C19 C20 H20B 109.4 . . ?
C18 C19 C20 111.7(3) . . ?
C18 C19 H19A 109.3 . . ?
C18 C19 H19B 109.3 . . ?
C20 C19 H19A 109.3 . . ?
C20 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
C23 C24 C25 111.7(3) . . ?
C23 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
C25 C24 H24A 109.3 . . ?
C25 C24 H24B 109.3 . . ?
H24A C24 H24B 107.9 . . ?
C27 C26 H26A 109.3 . . ?
C27 C26 H26B 109.3 . . ?
C25 C26 C27 111.5(3) . . ?
C25 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?

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 N2 C17 C18 38.6(5) . . . . ?
Mo1 N2 C17 C22 -84.9(4) . . . . ?
Mo1 N2 C15 N1 -3.6(2) . . . . ?
Mo1 N2 C15 C16 172.8(3) . . . . ?
Mo1 N1 C15 N2 4.1(3) . . . . ?
Mo1 N1 C15 C16 -172.5(3) . . . . ?
Mo1 N1 C23 C28 54.0(4) . . . . ?
Mo1 N1 C23 C24 -70.4(4) . . . . ?
Mo1 N3 C3 C8 91.6(4) . . . . ?
Mo1 N3 C3 C4 -31.7(4) . . . . ?
C2 C1 N4 Mo1 -176.7(3) . . . . ?
C2 C1 N4 C9 -14.8(5) . . . . ?
C2 C1 N3 Mo1 176.2(3) . . . . ?
C2 C1 N3 C3 12.0(5) . . . . ?
C1 N3 C3 C8 -111.1(4) . . . . ?
C1 N3 C3 C4 125.7(3) . . . . ?
C10 C9 N4 Mo1 -57.7(4) . . . . ?
C10 C9 N4 C1 152.6(3) . . . . ?
C10 C9 C14 C13 -54.7(4) . . . . ?
C10 C11 C12 C13 57.0(4) . . . . ?
C9 C10 C11 C12 -58.4(4) . . . . ?
N4 C1 N3 Mo1 -4.8(3) . . . . ?
N4 C1 N3 C3 -169.0(3) . . . . ?
N4 C9 C14 C13 -176.8(3) . . . . ?
C11 C10 C9 N4 177.8(3) . . . . ?
C11 C10 C9 C14 56.6(4) . . . . ?
C14 C9 N4 Mo1 64.0(4) . . . . ?
C14 C9 N4 C1 -85.6(4) . . . . ?
C14 C13 C12 C11 -54.2(4) . . . . ?
C12 C13 C14 C9 53.6(4) . . . . ?
N2 C17 C18 C19 179.2(3) . . . . ?
N2 C17 C22 C21 -179.7(3) . . . . ?
C17 N2 C15 N1 -178.6(3) . . . . ?
C17 N2 C15 C16 -2.2(5) . . . . ?
C17 C18 C19 C20 55.2(4) . . . . ?
N1 C23 C28 C27 177.4(3) . . . . ?
N1 C23 C24 C25 -175.3(3) . . . . ?
N3 C1 N4 Mo1 4.3(2) . . . . ?
N3 C1 N4 C9 166.2(3) . . . . ?
N3 C3 C4 C5 -178.3(3) . . . . ?
C8 C3 C4 C5 56.9(4) . . . . ?
C3 C8 C7 C6 56.3(4) . . . . ?
C3 C4 C5 C6 -55.8(4) . . . . ?
C21 C20 C19 C18 -54.3(4) . . . . ?
C15 N2 C17 C18 -150.4(3) . . . . ?
C15 N2 C17 C22 86.1(4) . . . . ?
C15 N1 C23 C28 -142.3(3) . . . . ?
C15 N1 C23 C24 93.3(4) . . . . ?
C18 C17 C22 C21 57.5(4) . . . . ?
C23 N1 C15 N2 -164.7(3) . . . . ?
C23 N1 C15 C16 18.7(5) . . . . ?
C22 C17 C18 C19 -56.9(4) . . . . ?
C22 C21 C20 C19 54.7(4) . . . . ?
C4 C5 C6 C7 54.4(4) . . . . ?
C5 C6 C7 C8 -54.6(4) . . . . ?
C28 C23 C24 C25 58.2(5) . . . . ?
C28 C27 C26 C25 -54.0(5) . . . . ?
C7 C8 C3 N3 179.4(3) . . . . ?
C7 C8 C3 C4 -57.2(4) . . . . ?
C20 C21 C22 C17 -56.6(4) . . . . ?
C24 C23 C28 C27 -57.6(4) . . . . ?
C24 C25 C26 C27 53.6(5) . . . . ?
C26 C27 C28 C23 56.1(5) . . . . ?
C26 C25 C24 C23 -56.2(5) . . . . ?

_shelx_SHELXL_version_number     2014/7

_olex2_date_sample_completion    2016-01-11
_olex2_date_sample_data_collection 2016-01-10
_olex2_date_sample_submission    2016-01-10
_olex2_exptl_crystal_mounting_method 
'Mounted on a brass tip in Paratone-N under air free conditions.'
_olex2_submission_original_sample_id TJ109
_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT973_sol2                
;
PROBLEM: Check Calcd Positive Residual Density on     Mo1       2.51 eA-3  
RESPONSE: The residual electron density is an artifact of the absorption
correction. The highest Q-peak is < 0.05 Angstroms from the Mo center;
no other significant Q-peaks are observable, suggesting no further
electron disorder in the solution.
;
# end Validation Reply Form
