# Supplementary Information (SI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_mm132
_database_code_depnum_ccdc_archive 'CCDC 2431617'
loop_
_audit_author_name
_audit_author_address
'Navamoney Arulsamy'
;University of Wyoming
United States of America
;
_audit_update_record             
;
2025-03-16 deposited with the CCDC.	2025-06-02 downloaded from the CCDC.
;
_chemical_name_systematic        Mo(CO)3(MeCN)(P2N2)
_chemical_name_common            DS-Mo1
_chemical_formula_moiety         'C29 H39 Mo N3 O3 P2'
_chemical_formula_sum            'C29 H39 Mo N3 O3 P2'
_chemical_formula_iupac          ?
_chemical_formula_weight         635.51
_chemical_absolute_configuration ?

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'
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                   12.2585(15)
_cell_length_b                   21.027(3)
_cell_length_c                   11.8947(14)
_cell_angle_alpha                90
_cell_angle_beta                 102.628(4)
_cell_angle_gamma                90
_cell_volume                     2991.8(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9609
_cell_measurement_theta_min      3.3690
_cell_measurement_theta_max      34.8877
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.686
_exptl_crystal_size_mid          0.423
_exptl_crystal_size_min          0.276
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320

_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.86

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   ?
_diffrn_source_type              ?
_diffrn_source_power             0.07
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            63691
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         33.73
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18

_refine_special_details          
;

Refined as a 2-component inversion twin.
;

_reflns_number_total             11733
_reflns_number_gt                11407
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.966
_reflns_Friedel_fraction_max     0.967
_reflns_Friedel_fraction_full    0.983

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0919
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_number_reflns         11733
_refine_ls_number_parameters     475
_refine_ls_number_restraints     2
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0427P)²+4.5200P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.726
_refine_diff_density_min         -0.918
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(3)

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1380)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo1 0.55596(2) 0.25883(2) 0.49873(2) 0.01093(6) Uani d . . . 1 . .
C C1 0.4219(3) 0.20881(15) 0.4389(3) 0.0164(5) Uani d . . . 1 . .
O O1 0.3471(2) 0.17570(14) 0.4010(3) 0.0282(6) Uani d . . . 1 . .
C C2 0.5917(3) 0.18739(15) 0.6097(3) 0.0171(5) Uani d . . . 1 . .
O O2 0.5983(3) 0.14411(13) 0.6712(3) 0.0264(6) Uani d . . . 1 . .
C C3 0.6131(3) 0.21172(14) 0.3792(3) 0.0174(5) Uani d . . . 1 . .
O O3 0.6344(2) 0.18283(13) 0.3033(3) 0.0264(5) Uani d . . . 1 . .
P P1 0.47429(6) 0.35147(3) 0.37474(6) 0.01107(13) Uani d . . . 1 . .
P P2 0.45774(6) 0.32436(3) 0.62407(6) 0.01138(13) Uani d . . . 1 . .
N N1 0.7158(2) 0.31261(13) 0.5514(3) 0.0192(5) Uani d . . . 1 . .
C C4 0.8002(3) 0.33946(17) 0.5684(4) 0.0257(7) Uani d . . . 1 . .
C C5 0.9064(3) 0.3734(2) 0.5871(6) 0.0397(12) Uani d . . . 1 . .
H H5A 0.951781 0.362303 0.663063 0.060000 Uiso calc U . R 1 . .
H H5B 0.892377 0.419279 0.583439 0.060000 Uiso calc U . R 1 . .
H H5C 0.946299 0.361279 0.527411 0.060000 Uiso calc U . R 1 . .
N N2 0.5677(2) 0.43077(13) 0.5581(2) 0.0131(5) Uani d . . . 1 . .
C C6 0.5172(3) 0.43222(16) 0.4358(3) 0.0149(5) Uani d . . . 1 . .
H H6A 0.575(4) 0.444(2) 0.398(4) 0.010(9) Uiso d . . . 1 . .
H H6B 0.452(5) 0.463(3) 0.414(5) 0.032(16) Uiso d . . . 1 . .
N N3 0.2827(2) 0.37365(13) 0.4596(2) 0.0146(4) Uani d . . . 1 . .
C C7 0.3194(2) 0.35254(14) 0.3580(3) 0.0143(5) Uani d . . . 1 . .
H H7A 0.287704 0.308341 0.335281 0.014(10) Uiso d . . R 1 . .
H H7B 0.293227 0.371147 0.302848 0.020(12) Uiso d . . R 1 . .
C C8 0.3046(2) 0.32930(15) 0.5552(3) 0.0150(5) Uani d . . . 1 . .
H H8A 0.280(4) 0.289(3) 0.534(4) 0.016(11) Uiso d . . . 1 . .
H H8B 0.265(5) 0.339(3) 0.614(5) 0.027(13) Uiso d . . . 1 . .
C C9 0.4945(3) 0.41100(14) 0.6328(3) 0.0144(5) Uani d . . . 1 . .
H H9A 0.424(5) 0.437(3) 0.619(5) 0.033(15) Uiso d . . . 1 . .
H H9B 0.528(4) 0.423(3) 0.713(5) 0.021(12) Uiso d . . . 1 . .
C C10 0.4892(3) 0.35828(14) 0.2222(3) 0.0149(5) Uani d . . . 1 . .
C C11 0.6149(3) 0.35591(18) 0.2223(3) 0.0222(6) Uani d . . . 1 . .
H H11A 0.624(7) 0.356(4) 0.148(7) 0.05(2) Uiso d . . . 1 . .
H H11B 0.647(4) 0.320(2) 0.258(4) 0.013(11) Uiso d . . . 1 . .
H H11C 0.651(4) 0.396(3) 0.257(5) 0.019(11) Uiso d . . . 1 . .
C C12 0.4382(4) 0.41964(16) 0.1622(3) 0.0223(6) Uani d . . . 1 . .
H H12A 0.449(5) 0.421(3) 0.079(6) 0.035(15) Uiso d . . . 1 . .
H H12B 0.467(5) 0.454(3) 0.200(5) 0.024(13) Uiso d . . . 1 . .
H H12C 0.365(5) 0.423(3) 0.155(5) 0.028(14) Uiso d . . . 1 . .
C C13 0.4304(3) 0.29982(16) 0.1585(3) 0.0203(6) Uani d . . . 1 . .
H H13A 0.449(5) 0.295(3) 0.083(5) 0.027(13) Uiso d . . . 1 . .
H H13B 0.364(5) 0.301(3) 0.147(5) 0.027(14) Uiso d . . . 1 . .
H H13C 0.453(6) 0.265(3) 0.207(6) 0.031(16) Uiso d . . . 1 . .
C C14 0.2215(2) 0.42978(14) 0.4607(3) 0.0129(5) Uani d . . . 1 . .
C C15 0.2100(3) 0.47400(16) 0.3706(3) 0.0208(6) Uani d . . . 1 . .
H H15 0.256(5) 0.464(3) 0.313(5) 0.033(15) Uiso d . . . 1 . .
C C16 0.1478(4) 0.52920(17) 0.3711(3) 0.0244(7) Uani d . . . 1 . .
H H16 0.146(5) 0.558(3) 0.314(5) 0.027(13) Uiso d . . . 1 . .
C C17 0.0958(3) 0.54352(17) 0.4609(3) 0.0231(6) Uani d . . . 1 . .
H H17 0.057(5) 0.582(3) 0.469(4) 0.022(13) Uiso d . . . 1 . .
C C18 0.1083(3) 0.50071(17) 0.5509(3) 0.0230(6) Uani d . . . 1 . .
H H18 0.071(5) 0.512(3) 0.610(5) 0.029(14) Uiso d . . . 1 . .
C C19 0.1699(3) 0.44464(17) 0.5518(3) 0.0206(6) Uani d . . . 1 . .
H H19 0.171(6) 0.413(3) 0.613(6) 0.049(19) Uiso d . . . 1 . .
C C20 0.4553(3) 0.30415(16) 0.7774(3) 0.0169(5) Uani d . . . 1 . .
C C21 0.3880(4) 0.24218(18) 0.7749(4) 0.0253(7) Uani d . . . 1 . .
H H21A 0.392872 0.227199 0.853860 0.027(14) Uiso calc . . R 1 . .
H H21B 0.418627 0.209750 0.731292 0.049(19) Uiso calc . . R 1 . .
H H21C 0.309582 0.250153 0.737940 0.047(18) Uiso calc . . R 1 . .
C C22 0.4011(3) 0.35737(18) 0.8357(3) 0.0224(6) Uani d . . . 1 . .
H H22A 0.381(5) 0.337(3) 0.909(5) 0.026(13) Uiso d . . . 1 . .
H H22B 0.336(5) 0.368(3) 0.796(5) 0.033(15) Uiso d . . . 1 . .
H H22C 0.445(5) 0.400(3) 0.845(5) 0.032(15) Uiso d . . . 1 . .
C C23 0.5764(3) 0.2933(2) 0.8439(3) 0.0249(7) Uani d . . . 1 . .
H H23A 0.575(6) 0.277(3) 0.917(6) 0.036(16) Uiso d . . . 1 . .
H H23B 0.618(5) 0.327(3) 0.841(5) 0.031(15) Uiso d . . . 1 . .
H H23C 0.608(6) 0.258(3) 0.808(6) 0.026(14) Uiso d . . . 1 . .
C C24 0.6622(2) 0.46808(14) 0.6030(3) 0.0136(5) Uani d . . . 1 . .
C C25 0.7244(3) 0.45744(17) 0.7160(3) 0.0195(6) Uani d . . . 1 . .
H H25 0.703(5) 0.423(3) 0.760(5) 0.034(15) Uiso d . . . 1 . .
C C26 0.8201(3) 0.4930(2) 0.7611(3) 0.0245(7) Uani d . . . 1 . .
H H26 0.865(7) 0.486(4) 0.830(7) 0.05(2) Uiso d . . . 1 . .
C C27 0.8584(3) 0.53982(19) 0.6957(4) 0.0251(7) Uani d . . . 1 . .
H H27 0.919(5) 0.558(3) 0.730(6) 0.033(15) Uiso d . . . 1 . .
C C28 0.7983(3) 0.54992(17) 0.5841(4) 0.0231(7) Uani d . . . 1 . .
H H28 0.824(5) 0.575(3) 0.546(5) 0.028(14) Uiso d . . . 1 . .
C C29 0.7011(3) 0.51529(15) 0.5380(3) 0.0175(5) Uani d . . . 1 . .
H H29 0.659(4) 0.525(2) 0.460(4) 0.014(10) Uiso d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 C1 . 1.949(3) ?
Mo1 C3 . 1.982(3) ?
Mo1 C2 . 1.984(3) ?
Mo1 N1 . 2.230(3) ?
Mo1 P1 . 2.5152(8) ?
Mo1 P2 . 2.5210(8) ?
C1 O1 . 1.162(4) ?
C2 O2 . 1.159(4) ?
C3 O3 . 1.164(4) ?
P1 C7 . 1.866(3) ?
P1 C10 . 1.868(3) ?
P1 C6 . 1.876(3) ?
P2 C9 . 1.874(3) ?
P2 C20 . 1.879(3) ?
P2 C8 . 1.880(3) ?
N1 C4 . 1.157(4) ?
C4 C5 . 1.458(5) ?
N2 C24 . 1.404(4) ?
N2 C6 . 1.452(4) ?
N2 C9 . 1.454(4) ?
N3 C14 . 1.400(4) ?
N3 C7 . 1.448(4) ?
N3 C8 . 1.450(4) ?
C10 C13 . 1.538(5) ?
C10 C12 . 1.540(4) ?
C10 C11 . 1.541(5) ?
C14 C15 . 1.403(4) ?
C14 C19 . 1.404(4) ?
C15 C16 . 1.390(5) ?
C16 C17 . 1.391(5) ?
C17 C18 . 1.381(5) ?
C18 C19 . 1.398(5) ?
C20 C23 . 1.538(5) ?
C20 C21 . 1.539(5) ?
C20 C22 . 1.542(5) ?
C24 C29 . 1.404(4) ?
C24 C25 . 1.411(5) ?
C25 C26 . 1.396(5) ?
C26 C27 . 1.397(6) ?
C27 C28 . 1.387(6) ?
C28 C29 . 1.401(5) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Mo1 C3 . . 82.56(13) ?
C1 Mo1 C2 . . 83.12(13) ?
C3 Mo1 C2 . . 92.14(14) ?
C1 Mo1 N1 . . 174.07(13) ?
C3 Mo1 N1 . . 91.62(12) ?
C2 Mo1 N1 . . 98.30(12) ?
C1 Mo1 P1 . . 90.47(9) ?
C3 Mo1 P1 . . 97.14(10) ?
C2 Mo1 P1 . . 167.97(10) ?
N1 Mo1 P1 . . 89.12(8) ?
C1 Mo1 P2 . . 92.14(10) ?
C3 Mo1 P2 . . 170.64(10) ?
C2 Mo1 P2 . . 94.88(10) ?
N1 Mo1 P2 . . 93.47(8) ?
P1 Mo1 P2 . . 75.12(3) ?
O1 C1 Mo1 . . 175.0(3) ?
O2 C2 Mo1 . . 171.4(3) ?
O3 C3 Mo1 . . 172.5(3) ?
C7 P1 C10 . . 102.08(14) ?
C7 P1 C6 . . 102.89(14) ?
C10 P1 C6 . . 103.15(14) ?
C7 P1 Mo1 . . 109.70(10) ?
C10 P1 Mo1 . . 121.18(10) ?
C6 P1 Mo1 . . 115.60(11) ?
C9 P2 C20 . . 102.74(14) ?
C9 P2 C8 . . 100.11(14) ?
C20 P2 C8 . . 102.07(14) ?
C9 P2 Mo1 . . 115.08(10) ?
C20 P2 Mo1 . . 124.14(11) ?
C8 P2 Mo1 . . 109.47(11) ?
C4 N1 Mo1 . . 173.5(3) ?
N1 C4 C5 . . 178.8(5) ?
C24 N2 C6 . . 120.3(3) ?
C24 N2 C9 . . 119.7(3) ?
C6 N2 C9 . . 115.7(3) ?
N2 C6 P1 . . 113.0(2) ?
C14 N3 C7 . . 122.1(3) ?
C14 N3 C8 . . 122.8(3) ?
C7 N3 C8 . . 114.8(2) ?
N3 C7 P1 . . 114.2(2) ?
N3 C8 P2 . . 111.9(2) ?
N2 C9 P2 . . 114.7(2) ?
C13 C10 C12 . . 110.0(3) ?
C13 C10 C11 . . 109.6(3) ?
C12 C10 C11 . . 109.4(3) ?
C13 C10 P1 . . 106.4(2) ?
C12 C10 P1 . . 113.5(2) ?
C11 C10 P1 . . 107.9(2) ?
N3 C14 C15 . . 121.1(3) ?
N3 C14 C19 . . 121.9(3) ?
C15 C14 C19 . . 117.1(3) ?
C16 C15 C14 . . 120.9(3) ?
C15 C16 C17 . . 121.9(3) ?
C18 C17 C16 . . 117.5(3) ?
C17 C18 C19 . . 121.6(3) ?
C18 C19 C14 . . 121.0(3) ?
C23 C20 C21 . . 109.7(3) ?
C23 C20 C22 . . 109.8(3) ?
C21 C20 C22 . . 109.9(3) ?
C23 C20 P2 . . 108.3(2) ?
C21 C20 P2 . . 107.1(3) ?
C22 C20 P2 . . 111.9(2) ?
C29 C24 N2 . . 122.5(3) ?
C29 C24 C25 . . 117.3(3) ?
N2 C24 C25 . . 120.2(3) ?
C26 C25 C24 . . 121.0(3) ?
C25 C26 C27 . . 121.3(4) ?
C28 C27 C26 . . 117.9(3) ?
C27 C28 C29 . . 121.5(3) ?
C28 C29 C24 . . 121.0(3) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C7 H7B O2 4_454 0.77 2.57 3.107(4) 127.7 ?



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_mm139a
_database_code_depnum_ccdc_archive 'CCDC 2431618'
loop_
_audit_author_name
_audit_author_address
'Navamoney Arulsamy'
;University of Wyoming
United States of America
;
_audit_update_record             
;
2025-03-16 deposited with the CCDC.	2025-06-02 downloaded from the CCDC.
;
_chemical_name_systematic        Mo(CO)3(NH3)(P2N2)
_chemical_name_common            DS-Mo-1
_chemical_formula_moiety         'C27 H39 Mo N3 O3 P2, C6 H5 F'
_chemical_formula_sum            'C33 H44 F Mo N3 O3 P2'
_chemical_formula_iupac          ?
_chemical_formula_weight         707.59

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.868(2)
_cell_length_b                   13.210(2)
_cell_length_c                   18.026(3)
_cell_angle_alpha                90
_cell_angle_beta                 108.924(4)
_cell_angle_gamma                90
_cell_volume                     3349.0(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9963
_cell_measurement_theta_min      2.3579
_cell_measurement_theta_max      27.3614
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'light yellow'
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.063
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472

_exptl_absorpt_coefficient_mu    0.530
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.97

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   ?
_diffrn_source_type              ?
_diffrn_source_power             0.07
_diffrn_source_current           1.4
_diffrn_source_voltage           50

_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  ?

_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?

_diffrn_detector_area_resol_mean 7.3910

_diffrn_reflns_number            78535
_diffrn_reflns_av_R_equivalents  0.1753
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23

_refine_special_details          
;
;

_reflns_number_total             7374
_reflns_number_gt                5363
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0961
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_number_reflns         7374
_refine_ls_number_parameters     564
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    refall
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0080P)²+4.3781P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.519
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1380)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo Mo1 0.58350(2) 0.86794(2) 0.75438(2) 0.01482(8) Uani d . . . 1 . .
N N1 0.6468(3) 1.0071(2) 0.7087(2) 0.0235(7) Uani d . . . 1 . .
H H1A 0.686(3) 1.040(3) 0.742(3) 0.034(13) Uiso d . . . 1 . .
H H1B 0.606(3) 1.049(3) 0.688(3) 0.040(13) Uiso d . . . 1 . .
H H1C 0.677(4) 1.000(4) 0.678(3) 0.062(17) Uiso d . . . 1 . .
P P1 0.57903(6) 0.76054(6) 0.63766(5) 0.01389(17) Uani d . . . 1 . .
P P2 0.74399(6) 0.78336(6) 0.79246(5) 0.01439(17) Uani d . . . 1 . .
C C1 0.5944(2) 0.9365(2) 0.8535(2) 0.0178(7) Uani d . . . 1 . .
O O1 0.59695(17) 0.97305(17) 0.91302(14) 0.0250(5) Uani d . . . 1 . .
C C2 0.4531(2) 0.9211(2) 0.7116(2) 0.0211(7) Uani d . . . 1 . .
O O2 0.37474(17) 0.94819(18) 0.68702(16) 0.0312(6) Uani d . . . 1 . .
C C3 0.5300(2) 0.7561(2) 0.79519(19) 0.0183(7) Uani d . . . 1 . .
O O3 0.49714(18) 0.69036(18) 0.82145(16) 0.0300(6) Uani d . . . 1 . .
C C4 0.6793(2) 0.7806(2) 0.5981(2) 0.0163(7) Uani d . . . 1 . .
H H4A 0.706(2) 0.718(2) 0.5901(18) 0.007(8) Uiso d . . . 1 . .
H H4B 0.655(2) 0.808(2) 0.5510(19) 0.003(7) Uiso d . . . 1 . .
N N2 0.75339(17) 0.84762(18) 0.64805(15) 0.0150(6) Uani d . . . 1 . .
C C5 0.8113(2) 0.8033(3) 0.72247(19) 0.0161(7) Uani d . . . 1 . .
H H5A 0.859(2) 0.850(2) 0.7465(18) 0.006(8) Uiso d . . . 1 . .
H H5B 0.841(2) 0.742(3) 0.716(2) 0.018(9) Uiso d . . . 1 . .
C C6 0.7307(2) 0.6430(2) 0.79053(19) 0.0159(6) Uani d . . . 1 . .
H H6A 0.785(2) 0.613(2) 0.820(2) 0.016(9) Uiso d . . . 1 . .
H H6B 0.684(2) 0.626(2) 0.8170(18) 0.006(7) Uiso d . . . 1 . .
N N3 0.69709(18) 0.60331(18) 0.71100(15) 0.0146(5) Uani d . . . 1 . .
C C7 0.5978(2) 0.6247(2) 0.6682(2) 0.0156(6) Uani d . . . 1 . .
H H7A 0.562(2) 0.613(2) 0.7020(19) 0.009(8) Uiso d . . . 1 . .
H H7B 0.572(3) 0.578(3) 0.623(2) 0.026(10) Uiso d . . . 1 . .
C C8 0.4727(2) 0.7585(2) 0.54685(19) 0.0172(7) Uani d . . . 1 . .
C C9 0.3864(2) 0.7295(3) 0.5715(2) 0.0214(7) Uani d . . . 1 . .
H H9A 0.329(3) 0.733(3) 0.524(2) 0.032(11) Uiso d . . . 1 . .
H H9B 0.381(3) 0.771(3) 0.608(2) 0.027(11) Uiso d . . . 1 . .
H H9C 0.393(2) 0.663(3) 0.592(2) 0.021(9) Uiso d . . . 1 . .
C C10 0.4581(3) 0.8657(3) 0.5125(2) 0.0229(7) Uani d . . . 1 . .
H H10A 0.399(3) 0.868(3) 0.469(2) 0.029(10) Uiso d . . . 1 . .
H H10B 0.507(2) 0.886(2) 0.4937(19) 0.011(8) Uiso d . . . 1 . .
H H10C 0.456(3) 0.911(3) 0.553(2) 0.032(11) Uiso d . . . 1 . .
C C11 0.4835(3) 0.6835(3) 0.4855(2) 0.0216(7) Uani d . . . 1 . .
H H11A 0.433(3) 0.692(3) 0.442(2) 0.028(10) Uiso d . . . 1 . .
H H11B 0.488(3) 0.613(3) 0.503(2) 0.034(11) Uiso d . . . 1 . .
H H11C 0.538(2) 0.695(2) 0.4688(19) 0.009(8) Uiso d . . . 1 . .
C C12 0.8034(2) 0.9049(2) 0.60707(19) 0.0163(7) Uani d . . . 1 . .
C C13 0.7518(3) 0.9695(2) 0.5468(2) 0.0212(7) Uani d . . . 1 . .
H H13 0.686(2) 0.966(2) 0.531(2) 0.015(9) Uiso d . . . 1 . .
C C14 0.7981(3) 1.0312(3) 0.5086(2) 0.0257(8) Uani d . . . 1 . .
H H14 0.758(3) 1.071(3) 0.469(2) 0.022(9) Uiso d . . . 1 . .
C C15 0.8956(3) 1.0308(3) 0.5300(2) 0.0316(9) Uani d . . . 1 . .
H H15 0.926(2) 1.068(3) 0.506(2) 0.022(10) Uiso d . . . 1 . .
C C16 0.9472(3) 0.9662(3) 0.5879(2) 0.0301(9) Uani d . . . 1 . .
H H16 1.019(3) 0.962(3) 0.600(2) 0.040(11) Uiso d . . . 1 . .
C C17 0.9026(2) 0.9029(3) 0.6262(2) 0.0217(7) Uani d . . . 1 . .
H H17 0.935(2) 0.855(2) 0.663(2) 0.014(9) Uiso d . . . 1 . .
C C18 0.7554(2) 0.5496(2) 0.67823(19) 0.0154(7) Uani d . . . 1 . .
C C19 0.7223(2) 0.5171(2) 0.5995(2) 0.0178(7) Uani d . . . 1 . .
H H19 0.662(2) 0.531(2) 0.567(2) 0.015(9) Uiso d . . . 1 . .
C C20 0.7805(2) 0.4658(2) 0.5663(2) 0.0203(7) Uani d . . . 1 . .
H H20 0.756(2) 0.446(2) 0.516(2) 0.019(9) Uiso d . . . 1 . .
C C21 0.8737(3) 0.4441(3) 0.6086(2) 0.0264(8) Uani d . . . 1 . .
H H21 0.914(2) 0.409(3) 0.588(2) 0.018(9) Uiso d . . . 1 . .
C C22 0.9072(3) 0.4749(3) 0.6857(2) 0.0295(9) Uani d . . . 1 . .
H H22 0.969(3) 0.466(3) 0.715(2) 0.028(10) Uiso d . . . 1 . .
C C23 0.8501(2) 0.5271(3) 0.7200(2) 0.0229(8) Uani d . . . 1 . .
H H23 0.876(2) 0.547(2) 0.772(2) 0.012(8) Uiso d . . . 1 . .
C C24 0.8374(2) 0.8071(2) 0.88960(19) 0.0172(7) Uani d . . . 1 . .
C C25 0.9306(3) 0.7510(3) 0.8982(2) 0.0255(8) Uani d . . . 1 . .
H H25A 0.977(3) 0.767(3) 0.947(3) 0.040(12) Uiso d . . . 1 . .
H H25B 0.959(3) 0.765(3) 0.857(3) 0.036(11) Uiso d . . . 1 . .
H H25C 0.919(3) 0.680(3) 0.898(2) 0.025(10) Uiso d . . . 1 . .
C C26 0.7967(3) 0.7729(3) 0.9529(2) 0.0273(8) Uani d . . . 1 . .
H H26A 0.836(3) 0.790(3) 0.998(3) 0.031(11) Uiso d . . . 1 . .
H H26B 0.786(3) 0.701(3) 0.955(2) 0.034(11) Uiso d . . . 1 . .
H H26C 0.741(3) 0.804(3) 0.948(2) 0.027(10) Uiso d . . . 1 . .
C C27 0.8561(3) 0.9218(3) 0.8969(2) 0.0227(8) Uani d . . . 1 . .
H H27A 0.902(3) 0.935(3) 0.947(2) 0.025(10) Uiso d . . . 1 . .
H H27B 0.799(3) 0.960(3) 0.892(2) 0.026(10) Uiso d . . . 1 . .
H H27C 0.885(3) 0.946(3) 0.861(2) 0.025(10) Uiso d . . . 1 . .
F F1 0.8922(3) 0.2256(3) 0.92290(18) 0.1087(15) Uani d . . . 1 . .
C C28 0.8654(3) 0.2223(4) 0.8438(3) 0.0491(12) Uani d . . . 1 . .
C C29 0.7868(3) 0.2737(4) 0.8024(3) 0.0464(11) Uani d . . . 1 . .
H H29 0.751(3) 0.312(3) 0.827(3) 0.056(14) Uiso d . . . 1 . .
C C30 0.7574(4) 0.2694(4) 0.7222(3) 0.0489(12) Uani d . . . 1 . .
H H30 0.698(5) 0.303(5) 0.689(4) 0.11(2) Uiso d . . . 1 . .
C C31 0.8092(5) 0.2144(4) 0.6856(3) 0.0600(16) Uani d . . . 1 . .
H H31 0.788(3) 0.211(4) 0.631(3) 0.060(15) Uiso d . . . 1 . .
C C32 0.8887(4) 0.1636(4) 0.7287(4) 0.0560(15) Uani d . . . 1 . .
H H32 0.926(4) 0.126(4) 0.703(3) 0.072(16) Uiso d . . . 1 . .
C C33 0.9185(4) 0.1674(4) 0.8089(4) 0.0528(14) Uani d . . . 1 . .
H H33 0.967(4) 0.142(4) 0.844(3) 0.060(16) Uiso d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mo1 C3 . 1.934(3) ?
Mo1 C1 . 1.963(4) ?
Mo1 C2 . 1.969(4) ?
Mo1 N1 . 2.333(3) ?
Mo1 P2 . 2.5202(9) ?
Mo1 P1 . 2.5205(9) ?
P1 C4 . 1.868(3) ?
P1 C8 . 1.871(3) ?
P1 C7 . 1.871(3) ?
P2 C6 . 1.864(3) ?
P2 C5 . 1.865(3) ?
P2 C24 . 1.875(3) ?
C1 O1 . 1.166(4) ?
C2 O2 . 1.161(4) ?
C3 O3 . 1.168(4) ?
C4 N2 . 1.471(4) ?
N2 C12 . 1.424(4) ?
N2 C5 . 1.461(4) ?
C6 N3 . 1.454(4) ?
N3 C18 . 1.391(4) ?
N3 C7 . 1.455(4) ?
C8 C11 . 1.531(5) ?
C8 C10 . 1.533(5) ?
C8 C9 . 1.536(5) ?
C12 C13 . 1.399(5) ?
C12 C17 . 1.401(5) ?
C13 C14 . 1.386(5) ?
C14 C15 . 1.374(5) ?
C15 C16 . 1.373(6) ?
C16 C17 . 1.383(5) ?
C18 C23 . 1.396(4) ?
C18 C19 . 1.410(5) ?
C19 C20 . 1.379(5) ?
C20 C21 . 1.378(5) ?
C21 C22 . 1.377(5) ?
C22 C23 . 1.385(5) ?
C24 C26 . 1.523(5) ?
C24 C25 . 1.534(5) ?
C24 C27 . 1.539(4) ?
F1 C28 . 1.351(5) ?
C28 C29 . 1.349(6) ?
C28 C33 . 1.366(7) ?
C29 C30 . 1.368(7) ?
C30 C31 . 1.373(8) ?
C31 C32 . 1.363(8) ?
C32 C33 . 1.369(8) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3 Mo1 C1 . . 85.94(13) ?
C3 Mo1 C2 . . 86.98(14) ?
C1 Mo1 C2 . . 88.40(13) ?
C3 Mo1 N1 . . 177.77(13) ?
C1 Mo1 N1 . . 91.96(13) ?
C2 Mo1 N1 . . 92.25(13) ?
C3 Mo1 P2 . . 91.59(10) ?
C1 Mo1 P2 . . 99.52(9) ?
C2 Mo1 P2 . . 171.84(10) ?
N1 Mo1 P2 . . 89.47(9) ?
C3 Mo1 P1 . . 89.12(10) ?
C1 Mo1 P1 . . 172.66(9) ?
C2 Mo1 P1 . . 96.76(10) ?
N1 Mo1 P1 . . 93.05(9) ?
P2 Mo1 P1 . . 75.17(3) ?
C4 P1 C8 . . 102.72(15) ?
C4 P1 C7 . . 100.79(15) ?
C8 P1 C7 . . 104.24(14) ?
C4 P1 Mo1 . . 115.50(11) ?
C8 P1 Mo1 . . 121.66(11) ?
C7 P1 Mo1 . . 109.47(11) ?
C6 P2 C5 . . 101.82(15) ?
C6 P2 C24 . . 103.06(14) ?
C5 P2 C24 . . 102.18(15) ?
C6 P2 Mo1 . . 110.52(11) ?
C5 P2 Mo1 . . 114.91(11) ?
C24 P2 Mo1 . . 121.95(11) ?
O1 C1 Mo1 . . 175.9(3) ?
O2 C2 Mo1 . . 176.9(3) ?
O3 C3 Mo1 . . 178.0(3) ?
N2 C4 P1 . . 112.5(2) ?
C12 N2 C5 . . 116.0(2) ?
C12 N2 C4 . . 114.6(3) ?
C5 N2 C4 . . 115.0(2) ?
N2 C5 P2 . . 113.1(2) ?
N3 C6 P2 . . 112.2(2) ?
C18 N3 C6 . . 122.7(3) ?
C18 N3 C7 . . 122.6(3) ?
C6 N3 C7 . . 114.7(3) ?
N3 C7 P1 . . 111.8(2) ?
C11 C8 C10 . . 109.9(3) ?
C11 C8 C9 . . 109.9(3) ?
C10 C8 C9 . . 108.9(3) ?
C11 C8 P1 . . 112.6(2) ?
C10 C8 P1 . . 108.0(2) ?
C9 C8 P1 . . 107.4(2) ?
C13 C12 C17 . . 118.1(3) ?
C13 C12 N2 . . 118.7(3) ?
C17 C12 N2 . . 123.2(3) ?
C14 C13 C12 . . 120.6(3) ?
C15 C14 C13 . . 120.4(4) ?
C16 C15 C14 . . 119.6(3) ?
C15 C16 C17 . . 121.0(4) ?
C16 C17 C12 . . 120.1(3) ?
N3 C18 C23 . . 122.5(3) ?
N3 C18 C19 . . 121.4(3) ?
C23 C18 C19 . . 116.1(3) ?
C20 C19 C18 . . 121.5(3) ?
C21 C20 C19 . . 121.5(3) ?
C22 C21 C20 . . 117.8(3) ?
C21 C22 C23 . . 121.6(3) ?
C22 C23 C18 . . 121.5(3) ?
C26 C24 C25 . . 110.3(3) ?
C26 C24 C27 . . 109.5(3) ?
C25 C24 C27 . . 109.6(3) ?
C26 C24 P2 . . 107.2(2) ?
C25 C24 P2 . . 112.6(2) ?
C27 C24 P2 . . 107.7(2) ?
C29 C28 F1 . . 118.3(5) ?
C29 C28 C33 . . 122.6(5) ?
F1 C28 C33 . . 119.1(5) ?
C28 C29 C30 . . 119.2(5) ?
C29 C30 C31 . . 119.5(5) ?
C32 C31 C30 . . 120.3(5) ?
C31 C32 C33 . . 120.5(5) ?
C28 C33 C32 . . 117.9(5) ?



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane, fluorobenzene'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Hygroscopic,Oxygen-sensitive
