# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

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

data_compound_1a
_database_code_depnum_ccdc_archive 'CCDC 1911725'
loop_
_audit_author_name
_audit_author_address
'Francisco Molina Gonzalez'
;CIQSO
Spain
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;

_audit_creation_date             2016-12-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C37 H39 Mo N P2'
_chemical_formula_sum            'C37 H39 Mo N P2'
_chemical_properties_physical    
'air-sensitive, moisture-sensitive,Air-sensitive,Moisture-sensitive'
_chemical_formula_weight         655.57
_exptl_crystal_recrystallization_method 
'recrystallised from a mixture of THF and hexane by slow cooling'
_chemical_melting_point          ?
_exptl_crystal_description       prism
_exptl_crystal_colour            'dark red'
_diffrn_ambient_temperature      100
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'
P P 0.1023 0.0942 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
_chemical_absolute_configuration .
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                   10.994(6)
_cell_length_b                   13.807(7)
_cell_length_c                   23.317(10)
_cell_angle_alpha                90
_cell_angle_beta                 97.29(3)
_cell_angle_gamma                90
_cell_volume                     3511(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9304
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.180
_cell_measurement_theta_min      2.303
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1412 before and 0.0669 after correction.
The Ratio of minimum to maximum transmission is 0.8907.
The λ/2 correction factor is Not present.
;

_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1360
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            138971
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.96
_diffrn_reflns_theta_min         2.16
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Fixed Chi Bruker diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest Apex3 Photon 100 Detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9153
_reflns_number_total             11087
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 v8.35A (Bruker, 2016)'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.35A (Bruker, 2016)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         11087
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0310
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0267P)²+1.8823P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0683
_refine_special_details          
;The voids contain disordered solvent at partial occupancy. A
satisfactory disorder model for the solvent was not found, and therefore the 
OLEX2 Solvent Mask routine (similar to PLATON/SQUEEZE) was used to mask out the 
disordered density

All H atoms were refined using a riding model, with a common U restrained
to be 1.2 times the equivalent isotropic displacement
parameter of the parent atom. 

Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.,OLEX2 Solvent Mask routine
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
C1 C 0.77544(13) 0.56036(10) 0.62522(6) 0.0135(3) Uani 1 1 d . . . . .
C2 C 0.74165(14) 0.61724(11) 0.57592(6) 0.0160(3) Uani 1 1 d . . . . .
H2 H 0.7058 0.5871 0.5412 0.019 Uiso 1 1 calc R . . . .
C3 C 0.75962(15) 0.71678(12) 0.57698(7) 0.0204(3) Uani 1 1 d . . . . .
H3 H 0.7365 0.7540 0.5431 0.024 Uiso 1 1 calc R . . . .
C4 C 0.81146(16) 0.76228(12) 0.62763(7) 0.0226(3) Uani 1 1 d . . . . .
H4 H 0.8259 0.8301 0.6282 0.027 Uiso 1 1 calc R . . . .
C5 C 0.84164(15) 0.70732(12) 0.67710(7) 0.0219(3) Uani 1 1 d . . . . .
H5 H 0.8746 0.7382 0.7121 0.026 Uiso 1 1 calc R . . . .
C6 C 0.82420(14) 0.60728(12) 0.67617(7) 0.0172(3) Uani 1 1 d . . . . .
H6 H 0.8456 0.5707 0.7104 0.021 Uiso 1 1 calc R . . . .
P7 P 0.74418(3) 0.42904(3) 0.62021(2) 0.01235(7) Uani 1 1 d . . . . .
C8 C 0.82529(14) 0.40220(11) 0.55740(6) 0.0143(3) Uani 1 1 d . . . . .
C9 C 0.76070(14) 0.39868(11) 0.50180(6) 0.0156(3) Uani 1 1 d . . . . .
H9 H 0.6743 0.4073 0.4965 0.019 Uiso 1 1 calc R . . . .
C10 C 0.82241(14) 0.38256(11) 0.45403(7) 0.0172(3) Uani 1 1 d . . . . .
H10 H 0.7777 0.3809 0.4164 0.021 Uiso 1 1 calc R . . . .
C11 C 0.94905(15) 0.36889(12) 0.46087(7) 0.0196(3) Uani 1 1 d . . . . .
H11 H 0.9905 0.3573 0.4282 0.024 Uiso 1 1 calc R . . . .
C12 C 1.01400(15) 0.37241(12) 0.51602(7) 0.0214(3) Uani 1 1 d . . . . .
H12 H 1.1002 0.3625 0.5213 0.026 Uiso 1 1 calc R . . . .
C13 C 0.95269(14) 0.39039(12) 0.56342(7) 0.0187(3) Uani 1 1 d . . . . .
H13 H 0.9982 0.3948 0.6008 0.022 Uiso 1 1 calc R . . . .
C14 C 0.85160(14) 0.37832(11) 0.68042(6) 0.0161(3) Uani 1 1 d . . . . .
H14A H 0.8968 0.3238 0.6654 0.019 Uiso 1 1 calc R . . . .
H14B H 0.9123 0.4288 0.6942 0.019 Uiso 1 1 calc R . . . .
C15 C 0.79131(14) 0.34271(10) 0.73112(6) 0.0148(3) Uani 1 1 d . . . . .
C16 C 0.86551(15) 0.32724(11) 0.78332(7) 0.0182(3) Uani 1 1 d . . . . .
H16 H 0.9503 0.3428 0.7869 0.022 Uiso 1 1 calc R . . . .
C17 C 0.81564(15) 0.28916(12) 0.82999(7) 0.0205(3) Uani 1 1 d . . . . .
H17 H 0.8653 0.2779 0.8658 0.025 Uiso 1 1 calc R . . . .
C18 C 0.69117(15) 0.26783(11) 0.82324(7) 0.0188(3) Uani 1 1 d . . . . .
H18 H 0.6547 0.2414 0.8546 0.023 Uiso 1 1 calc R . . . .
C19 C 0.61992(14) 0.28529(10) 0.77049(6) 0.0152(3) Uani 1 1 d . . . . .
N20 N 0.66878(11) 0.32288(9) 0.72426(5) 0.0135(2) Uani 1 1 d . . . . .
Mo21 Mo 0.54855(2) 0.35961(2) 0.64012(2) 0.01072(3) Uani 1 1 d . . . . .
C22 C 0.54488(14) 0.49789(11) 0.69242(6) 0.0155(3) Uani 1 1 d . . . . .
H22A H 0.4940 0.4968 0.7245 0.019 Uiso 1 1 calc R . . . .
H22B H 0.6243 0.5314 0.7023 0.019 Uiso 1 1 calc R . . . .
C23 C 0.48237(14) 0.51584(11) 0.63653(7) 0.0161(3) Uani 1 1 d . . . . .
H23A H 0.5230 0.5604 0.6117 0.019 Uiso 1 1 calc R . . . .
H23B H 0.3927 0.5258 0.6339 0.019 Uiso 1 1 calc R . . . .
C24 C 0.48166(14) 0.37010(11) 0.54449(6) 0.0168(3) Uani 1 1 d . . . . .
H24A H 0.4826 0.4355 0.5271 0.020 Uiso 1 1 calc R . . . .
H24B H 0.5095 0.3185 0.5197 0.020 Uiso 1 1 calc R . . . .
C25 C 0.37865(14) 0.34760(12) 0.57346(6) 0.0172(3) Uani 1 1 d . . . . .
H25A H 0.3432 0.2820 0.5668 0.021 Uiso 1 1 calc R . . . .
H25B H 0.3162 0.3991 0.5742 0.021 Uiso 1 1 calc R . . . .
C26 C 0.55119(15) 0.19540(11) 0.62888(7) 0.0183(3) Uani 1 1 d . . . . .
H26A H 0.5631 0.1564 0.6648 0.022 Uiso 1 1 calc R . . . .
H26B H 0.4892 0.1679 0.5988 0.022 Uiso 1 1 calc R . . . .
C27 C 0.65896(15) 0.23390(11) 0.60954(7) 0.0176(3) Uani 1 1 d . . . . .
H27A H 0.6636 0.2302 0.5675 0.021 Uiso 1 1 calc R . . . .
H27B H 0.7376 0.2188 0.6335 0.021 Uiso 1 1 calc R . . . .
C28 C 0.48654(14) 0.25661(12) 0.76430(6) 0.0181(3) Uani 1 1 d . . . . .
H28A H 0.4513 0.2773 0.7993 0.022 Uiso 1 1 calc R . . . .
H28B H 0.4807 0.1851 0.7620 0.022 Uiso 1 1 calc R . . . .
P29 P 0.39451(4) 0.30926(3) 0.70017(2) 0.01314(7) Uani 1 1 d . . . . .
C30 C 0.29874(14) 0.40420(11) 0.72825(6) 0.0155(3) Uani 1 1 d . . . . .
C31 C 0.30588(16) 0.43077(12) 0.78649(7) 0.0226(3) Uani 1 1 d . . . . .
H31 H 0.3591 0.3964 0.8147 0.027 Uiso 1 1 calc R . . . .
C32 C 0.23560(19) 0.50732(13) 0.80370(8) 0.0302(4) Uani 1 1 d . . . . .
H32 H 0.2416 0.5244 0.8434 0.036 Uiso 1 1 calc R . . . .
C33 C 0.15732(18) 0.55859(12) 0.76342(8) 0.0289(4) Uani 1 1 d . . . . .
H33 H 0.1092 0.6101 0.7755 0.035 Uiso 1 1 calc R . . . .
C34 C 0.14967(16) 0.53417(12) 0.70546(8) 0.0237(3) Uani 1 1 d . . . . .
H34 H 0.0964 0.5692 0.6776 0.028 Uiso 1 1 calc R . . . .
C35 C 0.22001(14) 0.45843(11) 0.68802(7) 0.0171(3) Uani 1 1 d . . . . .
H35 H 0.2148 0.4430 0.6481 0.021 Uiso 1 1 calc R . . . .
C36 C 0.28047(14) 0.21247(11) 0.67997(6) 0.0153(3) Uani 1 1 d . . . . .
C37 C 0.31652(16) 0.11537(11) 0.68047(7) 0.0204(3) Uani 1 1 d . . . . .
H37 H 0.3995 0.0991 0.6933 0.024 Uiso 1 1 calc R . . . .
C38 C 0.23351(17) 0.04202(12) 0.66264(8) 0.0250(4) Uani 1 1 d . . . . .
H38 H 0.2602 -0.0235 0.6637 0.030 Uiso 1 1 calc R . . . .
C39 C 0.11224(17) 0.06376(12) 0.64338(8) 0.0256(4) Uani 1 1 d . . . . .
H39 H 0.0556 0.0137 0.6312 0.031 Uiso 1 1 calc R . . . .
C40 C 0.07475(16) 0.15982(13) 0.64219(8) 0.0273(4) Uani 1 1 d . . . . .
H40 H -0.0080 0.1758 0.6286 0.033 Uiso 1 1 calc R . . . .
C41 C 0.15787(15) 0.23299(12) 0.66077(7) 0.0218(3) Uani 1 1 d . . . . .
H41 H 0.1304 0.2982 0.6603 0.026 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
C1 C2 1.403(2) . ?
C1 C6 1.399(2) . ?
C1 P7 1.8465(17) . ?
C2 H2 0.9500 . ?
C2 C3 1.388(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.394(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.385(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(2) . ?
C6 H6 0.9500 . ?
P7 C8 1.8463(17) . ?
P7 C14 1.8534(16) . ?
P7 Mo21 2.4522(12) . ?
C8 C9 1.398(2) . ?
C8 C13 1.399(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.394(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.390(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.388(2) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.509(2) . ?
C15 C16 1.393(2) . ?
C15 N20 1.364(2) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.393(2) . ?
C19 N20 1.367(2) . ?
C19 C28 1.508(2) . ?
N20 Mo21 2.2793(15) . ?
Mo21 C22 2.2685(17) . ?
Mo21 C23 2.2746(18) . ?
Mo21 C24 2.2622(17) . ?
Mo21 C25 2.2795(18) . ?
Mo21 C26 2.2831(19) . ?
Mo21 C27 2.2835(17) . ?
Mo21 P29 2.4319(10) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.416(2) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.425(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.423(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 P29 1.8451(16) . ?
P29 C30 1.8522(17) . ?
P29 C36 1.8520(17) . ?
C30 C31 1.399(2) . ?
C30 C35 1.408(2) . ?
C31 H31 0.9500 . ?
C31 C32 1.398(3) . ?
C32 H32 0.9500 . ?
C32 C33 1.385(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.385(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.392(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.398(2) . ?
C36 C41 1.394(2) . ?
C37 H37 0.9500 . ?
C37 C38 1.391(2) . ?
C38 H38 0.9500 . ?
C38 C39 1.385(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.388(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.394(2) . ?
C41 H41 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 P7 118.04(11) . . ?
C6 C1 C2 118.02(14) . . ?
C6 C1 P7 123.83(12) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.16(14) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.20(15) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.18(15) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 H5 119.6 . . ?
C4 C5 C6 120.78(15) . . ?
C6 C5 H5 119.6 . . ?
C1 C6 H6 119.7 . . ?
C5 C6 C1 120.61(15) . . ?
C5 C6 H6 119.7 . . ?
C1 P7 C14 103.15(7) . . ?
C1 P7 Mo21 122.18(5) . . ?
C8 P7 C1 98.19(7) . . ?
C8 P7 C14 101.51(8) . . ?
C8 P7 Mo21 126.53(5) . . ?
C14 P7 Mo21 101.47(6) . . ?
C9 C8 P7 120.20(12) . . ?
C9 C8 C13 118.24(14) . . ?
C13 C8 P7 121.46(11) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.35(14) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.6 . . ?
C9 C10 C11 120.71(14) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.30(15) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.89(15) . . ?
C13 C12 H12 120.1 . . ?
C8 C13 H13 119.3 . . ?
C12 C13 C8 121.47(14) . . ?
C12 C13 H13 119.3 . . ?
P7 C14 H14A 108.6 . . ?
P7 C14 H14B 108.6 . . ?
H14A C14 H14B 107.6 . . ?
C15 C14 P7 114.54(11) . . ?
C15 C14 H14A 108.6 . . ?
C15 C14 H14B 108.6 . . ?
C16 C15 C14 117.88(14) . . ?
N20 C15 C14 119.92(13) . . ?
N20 C15 C16 122.13(14) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 119.94(15) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 120.8 . . ?
C16 C17 C18 118.34(14) . . ?
C18 C17 H17 120.8 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 119.93(15) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C28 118.04(14) . . ?
N20 C19 C18 121.94(15) . . ?
N20 C19 C28 119.94(13) . . ?
C15 N20 C19 117.70(12) . . ?
C15 N20 Mo21 120.84(10) . . ?
C19 N20 Mo21 121.37(10) . . ?
N20 Mo21 P7 79.81(5) . . ?
N20 Mo21 C25 155.00(5) . . ?
N20 Mo21 C26 82.15(5) . . ?
N20 Mo21 C27 80.01(6) . . ?
N20 Mo21 P29 79.10(5) . . ?
C22 Mo21 P7 81.29(5) . . ?
C22 Mo21 N20 76.85(5) . . ?
C22 Mo21 C23 36.31(6) . . ?
C22 Mo21 C25 111.03(6) . . ?
C22 Mo21 C26 154.01(6) . . ?
C22 Mo21 C27 148.65(6) . . ?
C22 Mo21 P29 82.52(5) . . ?
C23 Mo21 P7 84.64(5) . . ?
C23 Mo21 N20 112.98(5) . . ?
C23 Mo21 C25 79.24(6) . . ?
C23 Mo21 C26 161.13(6) . . ?
C23 Mo21 C27 152.83(6) . . ?
C23 Mo21 P29 92.83(5) . . ?
C24 Mo21 P7 88.38(5) . . ?
C24 Mo21 N20 160.59(5) . . ?
C24 Mo21 C22 116.76(6) . . ?
C24 Mo21 C23 80.83(6) . . ?
C24 Mo21 C25 36.56(6) . . ?
C24 Mo21 C26 87.58(6) . . ?
C24 Mo21 C27 81.96(6) . . ?
C24 Mo21 P29 115.01(5) . . ?
C25 Mo21 P7 124.19(5) . . ?
C25 Mo21 C26 82.57(6) . . ?
C25 Mo21 C27 98.85(6) . . ?
C25 Mo21 P29 78.55(6) . . ?
C26 Mo21 P7 110.01(5) . . ?
C26 Mo21 C27 36.31(6) . . ?
C26 Mo21 P29 78.59(4) . . ?
C27 Mo21 P7 74.00(5) . . ?
C27 Mo21 P29 113.52(5) . . ?
P29 Mo21 P7 155.828(18) . . ?
Mo21 C22 H22A 116.4 . . ?
Mo21 C22 H22B 116.4 . . ?
H22A C22 H22B 113.4 . . ?
C23 C22 Mo21 72.08(9) . . ?
C23 C22 H22A 116.4 . . ?
C23 C22 H22B 116.4 . . ?
Mo21 C23 H23A 116.4 . . ?
Mo21 C23 H23B 116.4 . . ?
C22 C23 Mo21 71.61(8) . . ?
C22 C23 H23A 116.4 . . ?
C22 C23 H23B 116.4 . . ?
H23A C23 H23B 113.4 . . ?
Mo21 C24 H24A 116.3 . . ?
Mo21 C24 H24B 116.3 . . ?
H24A C24 H24B 113.3 . . ?
C25 C24 Mo21 72.38(9) . . ?
C25 C24 H24A 116.3 . . ?
C25 C24 H24B 116.3 . . ?
Mo21 C25 H25A 116.5 . . ?
Mo21 C25 H25B 116.5 . . ?
C24 C25 Mo21 71.06(9) . . ?
C24 C25 H25A 116.5 . . ?
C24 C25 H25B 116.5 . . ?
H25A C25 H25B 113.5 . . ?
Mo21 C26 H26A 116.4 . . ?
Mo21 C26 H26B 116.4 . . ?
H26A C26 H26B 113.4 . . ?
C27 C26 Mo21 71.86(9) . . ?
C27 C26 H26A 116.4 . . ?
C27 C26 H26B 116.4 . . ?
Mo21 C27 H27A 116.4 . . ?
Mo21 C27 H27B 116.4 . . ?
C26 C27 Mo21 71.83(9) . . ?
C26 C27 H27A 116.4 . . ?
C26 C27 H27B 116.4 . . ?
H27A C27 H27B 113.4 . . ?
C19 C28 H28A 108.8 . . ?
C19 C28 H28B 108.8 . . ?
C19 C28 P29 113.62(11) . . ?
H28A C28 H28B 107.7 . . ?
P29 C28 H28A 108.8 . . ?
P29 C28 H28B 108.8 . . ?
C28 P29 Mo21 103.24(6) . . ?
C28 P29 C30 105.68(8) . . ?
C28 P29 C36 101.88(8) . . ?
C30 P29 Mo21 118.03(6) . . ?
C36 P29 Mo21 123.93(5) . . ?
C36 P29 C30 101.75(8) . . ?
C31 C30 P29 124.35(13) . . ?
C31 C30 C35 117.45(15) . . ?
C35 C30 P29 118.01(12) . . ?
C30 C31 H31 119.6 . . ?
C32 C31 C30 120.79(16) . . ?
C32 C31 H31 119.6 . . ?
C31 C32 H32 119.7 . . ?
C33 C32 C31 120.68(17) . . ?
C33 C32 H32 119.7 . . ?
C32 C33 H33 120.2 . . ?
C34 C33 C32 119.53(16) . . ?
C34 C33 H33 120.2 . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 120.05(17) . . ?
C35 C34 H34 120.0 . . ?
C30 C35 H35 119.3 . . ?
C34 C35 C30 121.48(15) . . ?
C34 C35 H35 119.3 . . ?
C37 C36 P29 120.53(12) . . ?
C41 C36 P29 122.05(12) . . ?
C41 C36 C37 117.33(14) . . ?
C36 C37 H37 119.3 . . ?
C38 C37 C36 121.41(16) . . ?
C38 C37 H37 119.3 . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.48(16) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 120.5 . . ?
C38 C39 C40 119.00(16) . . ?
C40 C39 H39 120.5 . . ?
C39 C40 H40 119.8 . . ?
C39 C40 C41 120.33(17) . . ?
C41 C40 H40 119.8 . . ?
C36 C41 H41 119.3 . . ?
C40 C41 C36 121.43(16) . . ?
C40 C41 H41 119.3 . . ?

_smtbx_masks_special_details     
;
The voids contain disordered solvent at partial occupancy. A
satisfactory disorder model for the solvent was not found, and therefore the 
OLEX2 Solvent Mask routine (similar to PLATON/SQUEEZE) was used to mask out the 
disordered density (Dolomanov, O.V., Bourhis, 
L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.(2009), J. Appl.
Cryst. 42, 339-341.).
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.001 0.000 0.500 367.6 88.4 ?
2 -0.041 0.500 0.000 367.6 88.4 ?

_shelx_SHELXL_version_number     2014/7

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a 150 micro/m MITIGEN holder oil'
_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_compound_1b
_database_code_depnum_ccdc_archive 'CCDC 1911727'
loop_
_audit_author_name
_audit_author_address
'Francisco Molina Gonzalez'
;CIQSO
Spain
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2018-05-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C37 H39 N P2 W'
_chemical_formula_sum            'C37 H39 N P2 W'
_chemical_properties_physical    
'air-sensitive, moisture-sensitive,Air-sensitive,Moisture-sensitive'
_chemical_formula_weight         743.48
_exptl_crystal_recrystallization_method 
'Crystallised from a mixture of THF and hexane by cooling'
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_diffrn_ambient_temperature      100.0
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
_chemical_absolute_configuration .
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                   13.5747(4)
_cell_length_b                   14.5270(4)
_cell_length_c                   15.6334(5)
_cell_angle_alpha                90
_cell_angle_beta                 103.040(2)
_cell_angle_gamma                90
_cell_volume                     3003.40(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.66
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.704
_exptl_absorpt_coefficient_mu    3.981
_exptl_absorpt_correction_T_max  0.0699
_exptl_absorpt_correction_T_min  0.0343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1018 before and 0.0837 after correction. 
The Ratio of minimum to maximum transmission is 0.4907. 
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1488
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.015
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0971
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60609
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.256
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_special_details          ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4746
_reflns_number_total             5921
_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       'Bruker Apex3, 2017'
_computing_data_collection       'Bruker Apex3, 2017'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.209
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5921
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0301
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+8.6323P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0642
_refine_special_details          
;
SIMU and DELU restraints were applied to C21, C22 and C23.

All H atoms were refined using a riding model, with a common U restrained
to be 1.2 times the equivalent isotropic displacement
parameter of the parent atom. 

Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C21, C22, C23
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22 \\sim C23: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C19(H19A,H19B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31)
;
_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
W1 W 0.47224(2) 0.73339(2) 0.40496(2) 0.02251(6) Uani 1 1 d . . . . .
P1 P 0.48762(9) 0.68241(7) 0.26018(8) 0.0244(2) Uani 1 1 d . . . . .
P2 P 0.38603(8) 0.75413(7) 0.52437(7) 0.0237(2) Uani 1 1 d . . . . .
N1 N 0.3569(3) 0.6171(2) 0.3817(2) 0.0230(8) Uani 1 1 d . . . . .
C1 C 0.3073(3) 0.5910(3) 0.4435(3) 0.0240(9) Uani 1 1 d . . . . .
C2 C 0.2436(3) 0.5144(3) 0.4323(3) 0.0261(10) Uani 1 1 d . . . . .
H2 H 0.208460 0.498543 0.476319 0.031 Uiso 1 1 calc R . . . .
C3 C 0.2319(3) 0.4620(3) 0.3574(3) 0.0287(10) Uani 1 1 d . . . . .
H3 H 0.191480 0.407931 0.350218 0.034 Uiso 1 1 calc R . . . .
C4 C 0.2799(3) 0.4895(3) 0.2933(3) 0.0280(10) Uani 1 1 d . . . . .
H4 H 0.271869 0.455089 0.240554 0.034 Uiso 1 1 calc R . . . .
C5 C 0.3403(3) 0.5679(3) 0.3057(3) 0.0259(10) Uani 1 1 d . . . . .
C6 C 0.3782(3) 0.6051(3) 0.2298(3) 0.0289(10) Uani 1 1 d . . . . .
H6A H 0.322393 0.638730 0.190495 0.035 Uiso 1 1 calc R . . . .
H6B H 0.396815 0.552655 0.196153 0.035 Uiso 1 1 calc R . . . .
C7 C 0.5980(4) 0.6166(3) 0.2456(3) 0.0291(10) Uani 1 1 d . . . . .
C8 C 0.5948(4) 0.5235(3) 0.2234(3) 0.0352(11) Uani 1 1 d . . . . .
H8 H 0.532493 0.491056 0.213516 0.042 Uiso 1 1 calc R . . . .
C9 C 0.6827(4) 0.4779(4) 0.2156(4) 0.0439(13) Uani 1 1 d . . . . .
H9 H 0.679603 0.414700 0.199723 0.053 Uiso 1 1 calc R . . . .
C10 C 0.7736(4) 0.5234(4) 0.2305(4) 0.0437(13) Uani 1 1 d . . . . .
H10 H 0.833145 0.491741 0.225113 0.052 Uiso 1 1 calc R . . . .
C11 C 0.7781(4) 0.6151(4) 0.2532(3) 0.0394(12) Uani 1 1 d . . . . .
H11 H 0.840867 0.646885 0.263952 0.047 Uiso 1 1 calc R . . . .
C12 C 0.6911(4) 0.6607(3) 0.2605(3) 0.0332(11) Uani 1 1 d . . . . .
H12 H 0.694991 0.724025 0.276024 0.040 Uiso 1 1 calc R . . . .
C13 C 0.4730(3) 0.7574(3) 0.1624(3) 0.0255(9) Uani 1 1 d . . . . .
C14 C 0.4045(3) 0.7411(3) 0.0824(3) 0.0294(10) Uani 1 1 d . . . . .
H14 H 0.358100 0.691370 0.077478 0.035 Uiso 1 1 calc R . . . .
C15 C 0.4037(4) 0.7970(3) 0.0102(3) 0.0335(11) Uani 1 1 d . . . . .
H15 H 0.356366 0.785446 -0.043538 0.040 Uiso 1 1 calc R . . . .
C16 C 0.4713(4) 0.8694(3) 0.0157(3) 0.0335(11) Uani 1 1 d . . . . .
H16 H 0.471761 0.906460 -0.034226 0.040 Uiso 1 1 calc R . . . .
C17 C 0.5383(4) 0.8870(3) 0.0950(3) 0.0324(11) Uani 1 1 d . . . . .
H17 H 0.583935 0.937325 0.099780 0.039 Uiso 1 1 calc R . . . .
C18 C 0.5392(4) 0.8315(3) 0.1674(3) 0.0297(10) Uani 1 1 d . . . . .
H18 H 0.585720 0.844262 0.221254 0.036 Uiso 1 1 calc R . . . .
C19 C 0.3227(3) 0.6425(3) 0.5286(3) 0.0259(10) Uani 1 1 d . . . . .
H19A H 0.363912 0.604453 0.576011 0.031 Uiso 1 1 calc R . . . .
H19B H 0.256207 0.653060 0.543062 0.031 Uiso 1 1 calc R . . . .
C20 C 0.4568(3) 0.7724(3) 0.6380(3) 0.0255(9) Uani 1 1 d . . . . .
C21 C 0.4841(4) 0.7022(3) 0.6979(3) 0.0401(12) Uani 1 1 d . U . . .
H21 H 0.461529 0.641186 0.682919 0.048 Uiso 1 1 calc R . . . .
C22 C 0.5463(5) 0.7213(3) 0.7824(3) 0.0490(14) Uani 1 1 d . U . . .
H22 H 0.569670 0.671974 0.821627 0.059 Uiso 1 1 calc R . . . .
C23 C 0.5722(4) 0.8080(3) 0.8075(3) 0.0401(12) Uani 1 1 d . U . . .
H23 H 0.607300 0.820579 0.866098 0.048 Uiso 1 1 calc R . . . .
C24 C 0.5478(4) 0.8782(3) 0.7480(3) 0.0341(11) Uani 1 1 d . . . . .
H24 H 0.570022 0.939077 0.764226 0.041 Uiso 1 1 calc R . . . .
C25 C 0.4909(3) 0.8610(3) 0.6643(3) 0.0309(11) Uani 1 1 d . . . . .
H25 H 0.474604 0.910420 0.623789 0.037 Uiso 1 1 calc R . . . .
C26 C 0.2835(3) 0.8390(3) 0.5159(3) 0.0254(10) Uani 1 1 d . . . . .
C27 C 0.3054(3) 0.9308(3) 0.5002(3) 0.0279(10) Uani 1 1 d . . . . .
H27 H 0.372447 0.947340 0.497798 0.034 Uiso 1 1 calc R . . . .
C28 C 0.2309(3) 0.9981(3) 0.4881(3) 0.0289(10) Uani 1 1 d . . . . .
H28 H 0.247541 1.060212 0.478671 0.035 Uiso 1 1 calc R . . . .
C29 C 0.1333(3) 0.9749(3) 0.4896(3) 0.0297(10) Uani 1 1 d . . . . .
H29 H 0.081959 1.020631 0.480188 0.036 Uiso 1 1 calc R . . . .
C30 C 0.1102(4) 0.8845(3) 0.5050(3) 0.0355(12) Uani 1 1 d . . . . .
H30 H 0.042895 0.868288 0.506882 0.043 Uiso 1 1 calc R . . . .
C31 C 0.1847(3) 0.8175(3) 0.5178(3) 0.0287(10) Uani 1 1 d . . . . .
H31 H 0.167641 0.755715 0.528028 0.034 Uiso 1 1 calc R . . . .
C32 C 0.5819(3) 0.8308(3) 0.4885(3) 0.0293(10) Uani 1 1 d . . . . .
H32A H 0.559954 0.895688 0.489271 0.035 Uiso 1 1 calc R . . . .
H32B H 0.617698 0.807696 0.546805 0.035 Uiso 1 1 calc R . . . .
C33 C 0.6224(3) 0.8035(3) 0.4154(3) 0.0283(10) Uani 1 1 d . . . . .
H33A H 0.683013 0.763566 0.428708 0.034 Uiso 1 1 calc R . . . .
H33B H 0.625251 0.851586 0.371157 0.034 Uiso 1 1 calc R . . . .
C34 C 0.4212(3) 0.8672(3) 0.3410(3) 0.0306(11) Uani 1 1 d . . . . .
H34A H 0.415323 0.919110 0.380591 0.037 Uiso 1 1 calc R . . . .
H34B H 0.450719 0.885207 0.291010 0.037 Uiso 1 1 calc R . . . .
C35 C 0.3373(3) 0.8041(3) 0.3217(3) 0.0271(10) Uani 1 1 d . . . . .
H35A H 0.315685 0.783061 0.260039 0.033 Uiso 1 1 calc R . . . .
H35B H 0.280253 0.816998 0.349712 0.033 Uiso 1 1 calc R . . . .
C36 C 0.5491(3) 0.6326(3) 0.5098(3) 0.0277(10) Uani 1 1 d . . . . .
H36A H 0.605814 0.657024 0.555477 0.033 Uiso 1 1 calc R . . . .
H36B H 0.504255 0.590436 0.533242 0.033 Uiso 1 1 calc R . . . .
C37 C 0.5719(3) 0.6073(3) 0.4286(3) 0.0267(10) Uani 1 1 d . . . . .
H37A H 0.541368 0.549228 0.401843 0.032 Uiso 1 1 calc R . . . .
H37B H 0.642860 0.615772 0.424064 0.032 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
W1 P1 2.4349(12) . ?
W1 P2 2.4354(11) . ?
W1 N1 2.276(3) . ?
W1 C32 2.246(4) . ?
W1 C33 2.252(4) . ?
W1 C34 2.225(4) . ?
W1 C35 2.243(4) . ?
W1 C36 2.269(4) . ?
W1 C37 2.257(4) . ?
P1 C6 1.838(4) . ?
P1 C7 1.834(5) . ?
P1 C13 1.851(4) . ?
P2 C19 1.844(4) . ?
P2 C20 1.838(4) . ?
P2 C26 1.842(5) . ?
N1 C1 1.350(6) . ?
N1 C5 1.361(6) . ?
C1 C2 1.395(6) . ?
C1 C19 1.499(6) . ?
C2 C3 1.376(6) . ?
C3 C4 1.372(7) . ?
C4 C5 1.391(6) . ?
C5 C6 1.497(6) . ?
C7 C8 1.395(6) . ?
C7 C12 1.388(7) . ?
C8 C9 1.393(7) . ?
C9 C10 1.373(8) . ?
C10 C11 1.376(7) . ?
C11 C12 1.381(7) . ?
C13 C14 1.400(6) . ?
C13 C18 1.393(6) . ?
C14 C15 1.388(6) . ?
C15 C16 1.386(7) . ?
C16 C17 1.385(7) . ?
C17 C18 1.387(6) . ?
C20 C21 1.377(6) . ?
C20 C25 1.397(6) . ?
C21 C22 1.426(7) . ?
C22 C23 1.342(7) . ?
C23 C24 1.370(7) . ?
C24 C25 1.384(6) . ?
C26 C27 1.400(6) . ?
C26 C31 1.384(6) . ?
C27 C28 1.388(6) . ?
C28 C29 1.373(6) . ?
C29 C30 1.384(6) . ?
C30 C31 1.385(6) . ?
C32 C33 1.430(6) . ?
C34 C35 1.440(6) . ?
C36 C37 1.421(6) . ?

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
P1 W1 P2 155.10(4) . . ?
N1 W1 P1 79.99(10) . . ?
N1 W1 P2 77.40(10) . . ?
C32 W1 P1 123.17(12) . . ?
C32 W1 P2 81.19(12) . . ?
C32 W1 N1 154.44(15) . . ?
C32 W1 C33 37.07(16) . . ?
C32 W1 C36 81.37(17) . . ?
C32 W1 C37 96.99(17) . . ?
C33 W1 P1 86.51(12) . . ?
C33 W1 P2 118.16(12) . . ?
C33 W1 N1 157.88(15) . . ?
C33 W1 C36 88.76(17) . . ?
C33 W1 C37 81.73(16) . . ?
C34 W1 P1 86.05(13) . . ?
C34 W1 P2 94.69(13) . . ?
C34 W1 N1 116.33(15) . . ?
C34 W1 C32 79.01(18) . . ?
C34 W1 C33 79.76(17) . . ?
C34 W1 C35 37.60(16) . . ?
C34 W1 C36 159.19(17) . . ?
C34 W1 C37 153.81(18) . . ?
C35 W1 P1 80.19(12) . . ?
C35 W1 P2 85.28(12) . . ?
C35 W1 N1 78.75(15) . . ?
C35 W1 C32 113.36(17) . . ?
C35 W1 C33 116.25(17) . . ?
C35 W1 C36 153.80(17) . . ?
C35 W1 C37 147.94(16) . . ?
C36 W1 P1 110.71(12) . . ?
C36 W1 P2 75.41(12) . . ?
C36 W1 N1 79.86(15) . . ?
C37 W1 P1 74.44(12) . . ?
C37 W1 P2 110.39(12) . . ?
C37 W1 N1 77.82(14) . . ?
C37 W1 C36 36.59(16) . . ?
C6 P1 W1 101.09(15) . . ?
C6 P1 C13 102.5(2) . . ?
C7 P1 W1 121.18(15) . . ?
C7 P1 C6 106.5(2) . . ?
C7 P1 C13 98.2(2) . . ?
C13 P1 W1 124.97(14) . . ?
C19 P2 W1 103.15(15) . . ?
C20 P2 W1 121.45(14) . . ?
C20 P2 C19 103.8(2) . . ?
C20 P2 C26 101.3(2) . . ?
C26 P2 W1 120.90(15) . . ?
C26 P2 C19 103.9(2) . . ?
C1 N1 W1 122.0(3) . . ?
C1 N1 C5 117.8(4) . . ?
C5 N1 W1 120.1(3) . . ?
N1 C1 C2 121.9(4) . . ?
N1 C1 C19 120.2(4) . . ?
C2 C1 C19 117.8(4) . . ?
C3 C2 C1 119.8(4) . . ?
C4 C3 C2 118.5(4) . . ?
C3 C4 C5 119.9(4) . . ?
N1 C5 C4 121.8(4) . . ?
N1 C5 C6 119.0(4) . . ?
C4 C5 C6 118.8(4) . . ?
C5 C6 P1 114.7(3) . . ?
C8 C7 P1 123.8(4) . . ?
C12 C7 P1 118.5(4) . . ?
C12 C7 C8 117.7(4) . . ?
C9 C8 C7 120.2(5) . . ?
C10 C9 C8 120.7(5) . . ?
C9 C10 C11 119.7(5) . . ?
C10 C11 C12 119.8(5) . . ?
C11 C12 C7 121.9(5) . . ?
C14 C13 P1 124.3(3) . . ?
C18 C13 P1 117.4(3) . . ?
C18 C13 C14 118.1(4) . . ?
C15 C14 C13 120.6(4) . . ?
C16 C15 C14 120.6(5) . . ?
C17 C16 C15 119.2(4) . . ?
C16 C17 C18 120.3(4) . . ?
C17 C18 C13 121.1(4) . . ?
C1 C19 P2 112.3(3) . . ?
C21 C20 P2 123.5(4) . . ?
C21 C20 C25 117.5(4) . . ?
C25 C20 P2 118.9(3) . . ?
C20 C21 C22 119.9(5) . . ?
C23 C22 C21 121.0(4) . . ?
C22 C23 C24 119.5(5) . . ?
C23 C24 C25 120.3(5) . . ?
C24 C25 C20 121.5(4) . . ?
C27 C26 P2 117.6(3) . . ?
C31 C26 P2 124.6(3) . . ?
C31 C26 C27 117.6(4) . . ?
C28 C27 C26 121.1(4) . . ?
C29 C28 C27 120.1(4) . . ?
C28 C29 C30 119.6(4) . . ?
C29 C30 C31 120.3(4) . . ?
C26 C31 C30 121.2(4) . . ?
C33 C32 W1 71.7(2) . . ?
C32 C33 W1 71.3(2) . . ?
C35 C34 W1 71.9(2) . . ?
C34 C35 W1 70.5(2) . . ?
C37 C36 W1 71.3(2) . . ?
C36 C37 W1 72.1(2) . . ?

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
W1 P1 C6 C5 -22.3(4) . . . . ?
W1 P1 C7 C8 109.2(4) . . . . ?
W1 P1 C7 C12 -68.4(4) . . . . ?
W1 P1 C13 C14 -124.1(3) . . . . ?
W1 P1 C13 C18 60.2(4) . . . . ?
W1 P2 C19 C1 -22.3(3) . . . . ?
W1 P2 C20 C21 -93.2(4) . . . . ?
W1 P2 C20 C25 82.5(4) . . . . ?
W1 P2 C26 C27 -57.2(4) . . . . ?
W1 P2 C26 C31 118.1(4) . . . . ?
W1 N1 C1 C2 -174.0(3) . . . . ?
W1 N1 C1 C19 3.6(5) . . . . ?
W1 N1 C5 C4 172.1(3) . . . . ?
W1 N1 C5 C6 -15.1(5) . . . . ?
P1 C7 C8 C9 -178.5(4) . . . . ?
P1 C7 C12 C11 178.2(4) . . . . ?
P1 C13 C14 C15 -175.1(3) . . . . ?
P1 C13 C18 C17 175.2(4) . . . . ?
P2 C20 C21 C22 174.7(4) . . . . ?
P2 C20 C25 C24 -177.5(4) . . . . ?
P2 C26 C27 C28 176.4(4) . . . . ?
P2 C26 C31 C30 -175.6(4) . . . . ?
N1 C1 C2 C3 1.5(6) . . . . ?
N1 C1 C19 P2 14.3(5) . . . . ?
N1 C5 C6 P1 26.1(5) . . . . ?
C1 N1 C5 C4 -4.3(6) . . . . ?
C1 N1 C5 C6 168.6(4) . . . . ?
C1 C2 C3 C4 -3.2(6) . . . . ?
C2 C1 C19 P2 -168.0(3) . . . . ?
C2 C3 C4 C5 1.2(6) . . . . ?
C3 C4 C5 N1 2.6(7) . . . . ?
C3 C4 C5 C6 -170.3(4) . . . . ?
C4 C5 C6 P1 -160.9(3) . . . . ?
C5 N1 C1 C2 2.2(6) . . . . ?
C5 N1 C1 C19 179.9(4) . . . . ?
C6 P1 C7 C8 -5.2(5) . . . . ?
C6 P1 C7 C12 177.1(4) . . . . ?
C6 P1 C13 C14 -10.8(4) . . . . ?
C6 P1 C13 C18 173.5(4) . . . . ?
C7 P1 C6 C5 105.2(4) . . . . ?
C7 P1 C13 C14 98.3(4) . . . . ?
C7 P1 C13 C18 -77.5(4) . . . . ?
C7 C8 C9 C10 0.7(8) . . . . ?
C8 C7 C12 C11 0.4(7) . . . . ?
C8 C9 C10 C11 -0.1(8) . . . . ?
C9 C10 C11 C12 -0.3(8) . . . . ?
C10 C11 C12 C7 0.2(8) . . . . ?
C12 C7 C8 C9 -0.8(7) . . . . ?
C13 P1 C6 C5 -152.2(3) . . . . ?
C13 P1 C7 C8 -110.9(4) . . . . ?
C13 P1 C7 C12 71.4(4) . . . . ?
C13 C14 C15 C16 0.6(7) . . . . ?
C14 C13 C18 C17 -0.8(7) . . . . ?
C14 C15 C16 C17 -1.6(7) . . . . ?
C15 C16 C17 C18 1.4(7) . . . . ?
C16 C17 C18 C13 -0.2(7) . . . . ?
C18 C13 C14 C15 0.6(7) . . . . ?
C19 P2 C20 C21 21.9(5) . . . . ?
C19 P2 C20 C25 -162.3(4) . . . . ?
C19 P2 C26 C27 -172.1(4) . . . . ?
C19 P2 C26 C31 3.2(4) . . . . ?
C19 C1 C2 C3 -176.2(4) . . . . ?
C20 P2 C19 C1 -149.8(3) . . . . ?
C20 P2 C26 C27 80.5(4) . . . . ?
C20 P2 C26 C31 -104.2(4) . . . . ?
C20 C21 C22 C23 5.4(9) . . . . ?
C21 C20 C25 C24 -1.6(7) . . . . ?
C21 C22 C23 C24 -7.0(9) . . . . ?
C22 C23 C24 C25 4.3(8) . . . . ?
C23 C24 C25 C20 0.0(8) . . . . ?
C25 C20 C21 C22 -1.1(8) . . . . ?
C26 P2 C19 C1 104.6(3) . . . . ?
C26 P2 C20 C21 129.5(4) . . . . ?
C26 P2 C20 C25 -54.8(4) . . . . ?
C26 C27 C28 C29 -1.3(7) . . . . ?
C27 C26 C31 C30 -0.3(7) . . . . ?
C27 C28 C29 C30 1.2(7) . . . . ?
C28 C29 C30 C31 -0.8(8) . . . . ?
C29 C30 C31 C26 0.3(8) . . . . ?
C31 C26 C27 C28 0.8(7) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a 75 micro/m MITEGEN holder with Parabar oil'
_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_compound_2a
_database_code_depnum_ccdc_archive 'CCDC 1911730'
loop_
_audit_author_name
_audit_author_address
'Francisco Molina Gonzalez'
;CIQSO
Spain
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2016-12-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C35 H31 Mo N O2 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C43 H47 Mo N O4 P2'
_chemical_properties_physical    
'air-sensitive, moisture-sensitive,Air-sensitive,Moisture-sensitive'
_chemical_formula_weight         799.69
_exptl_crystal_recrystallization_method 
'Recrystallised from a mixture of THF and petroleum ether by slow cooling'
_chemical_melting_point          ?
_exptl_crystal_description       Block
_exptl_crystal_colour            'clear light orange'
_diffrn_ambient_temperature      100
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1529(10)
_cell_length_b                   12.0142(12)
_cell_length_c                   14.6450(15)
_cell_angle_alpha                100.120(4)
_cell_angle_beta                 101.056(4)
_cell_angle_gamma                90.987(4)
_cell_volume                     1893.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9717
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.44
_shelx_estimated_absorpt_T_max   0.959
_shelx_estimated_absorpt_T_min   0.915
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.2814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1191 before and 0.0809 after correction.
The Ratio of minimum to maximum transmission is 0.8440.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             832
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            133684
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         2.118
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Fixed Chi'
_diffrn_measurement_device_type  'Bruker D8 Quest CCD Apex3'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6552
_reflns_number_total             7458
_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       'Bruker Apex3, 2016'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.35A (Bruker, 2016)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.579
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7458
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0399
_refine_ls_restrained_S_all      1.036
_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)+(0.0706P)²+1.8863P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1098
_refine_special_details          
;
A THF solvent molecule shows positional disorder and 
was refined in two opposites (180 turn) conformations. 
They showed to be equally divided to 50%
(SOF of main component: 0.501(6)).
Restraints (SADI, SIMU, RIGU) are a applied in order to enhance the THF models. 

All H atoms were refined using a riding model, with a common U restrained
to be 1.2 times the equivalent isotropic displacement
parameter of the parent atom. 

Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C51-C50 \\sim C50-C49 \\sim C49-C48
 with sigma of 0.02
 O47-C51 \\sim O47-C48
 with sigma of 0.02
 O47-C50 \\sim O47-C49
 with sigma of 0.04
 C50-C48 \\sim C51-C49
 with sigma of 0.04
 C51B-C50B \\sim C50B-C49B \\sim C49B-C48B
 with sigma of 0.02
 O47B-C51B \\sim O47B-C48B
 with sigma of 0.02
 O47B-C50B \\sim O47B-C49B
 with sigma of 0.04
 C50B-C48B \\sim C51B-C49B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O47 \\sim C48 \\sim C49 \\sim C50 \\sim C51: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O47B \\sim C48B \\sim C49B \\sim C50B \\sim C51B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O47, C48, C49, C50, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O47B, C48B, C49B, C50B, C51B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O47B)=Sof(C48B)=Sof(H48C)=Sof(H48D)=Sof(C49B)=Sof(H49C)=Sof(H49D)=
 Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=Sof(H51C)=Sof(H51D)=1-FVAR(1)
 Sof(O47)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=
 Sof(H50A)=Sof(H50B)=Sof(C51)=Sof(H51A)=Sof(H51B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C48(H48A,
 H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C48B(H48C,H48D), C49B(H49C,
 H49D), C50B(H50C,H50D), C51B(H51C,H51D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
;
_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
C1 C 0.6355(2) 0.5458(2) 0.19519(19) 0.0171(5) Uani 1 1 d . . . . .
C2 C 0.6178(3) 0.6030(2) 0.11831(19) 0.0193(5) Uani 1 1 d . . . . .
H2 H 0.5385 0.6256 0.0941 0.023 Uiso 1 1 calc R . . . .
C3 C 0.7152(3) 0.6266(2) 0.0775(2) 0.0219(6) Uani 1 1 d . . . . .
H3 H 0.7024 0.6649 0.0253 0.026 Uiso 1 1 calc R . . . .
C4 C 0.8316(3) 0.5946(2) 0.1125(2) 0.0227(6) Uani 1 1 d . . . . .
H4 H 0.8979 0.6099 0.0837 0.027 Uiso 1 1 calc R . . . .
C5 C 0.8509(3) 0.5400(2) 0.1898(2) 0.0228(6) Uani 1 1 d . . . . .
H5 H 0.9307 0.5192 0.2146 0.027 Uiso 1 1 calc R . . . .
C6 C 0.7532(3) 0.5161(2) 0.2309(2) 0.0212(6) Uani 1 1 d . . . . .
H6 H 0.7668 0.4790 0.2838 0.025 Uiso 1 1 calc R . . . .
P7 P 0.50093(6) 0.50508(5) 0.23850(5) 0.01541(15) Uani 1 1 d . . . . .
C8 C 0.4693(2) 0.3577(2) 0.17507(19) 0.0186(5) Uani 1 1 d . . . . .
C9 C 0.5305(3) 0.3099(2) 0.1045(2) 0.0227(6) Uani 1 1 d . . . . .
H9 H 0.5915 0.3538 0.0875 0.027 Uiso 1 1 calc R . . . .
C10 C 0.5026(3) 0.1977(2) 0.0586(2) 0.0285(7) Uani 1 1 d . . . . .
H10 H 0.5442 0.1660 0.0101 0.034 Uiso 1 1 calc R . . . .
C11 C 0.4150(3) 0.1326(2) 0.0831(2) 0.0289(7) Uani 1 1 d . . . . .
H11 H 0.3970 0.0561 0.0522 0.035 Uiso 1 1 calc R . . . .
C12 C 0.3532(3) 0.1795(3) 0.1532(2) 0.0303(7) Uani 1 1 d . . . . .
H12 H 0.2932 0.1349 0.1708 0.036 Uiso 1 1 calc R . . . .
C13 C 0.3795(3) 0.2919(2) 0.1978(2) 0.0256(6) Uani 1 1 d . . . . .
H13 H 0.3353 0.3241 0.2445 0.031 Uiso 1 1 calc R . . . .
C14 C 0.5608(2) 0.4833(2) 0.36058(19) 0.0184(5) Uani 1 1 d . . . . .
H14A H 0.5034 0.4320 0.3794 0.022 Uiso 1 1 calc R . . . .
H14B H 0.6406 0.4478 0.3636 0.022 Uiso 1 1 calc R . . . .
C15 C 0.5761(2) 0.5946(2) 0.42671(18) 0.0166(5) Uani 1 1 d . . . . .
C16 C 0.6707(2) 0.6158(2) 0.50495(19) 0.0205(6) Uani 1 1 d . . . . .
H16 H 0.7293 0.5606 0.5156 0.025 Uiso 1 1 calc R . . . .
C17 C 0.6797(3) 0.7176(2) 0.5678(2) 0.0228(6) Uani 1 1 d . . . . .
H17 H 0.7451 0.7338 0.6211 0.027 Uiso 1 1 calc R . . . .
C18 C 0.5911(3) 0.7955(2) 0.5511(2) 0.0217(6) Uani 1 1 d . . . . .
H18 H 0.5935 0.8647 0.5944 0.026 Uiso 1 1 calc R . . . .
C19 C 0.4994(2) 0.7717(2) 0.47086(19) 0.0173(5) Uani 1 1 d . . . . .
N20 N 0.49049(19) 0.67228(18) 0.40704(15) 0.0156(4) Uani 1 1 d . . . . .
Mo21 Mo 0.34628(2) 0.63898(2) 0.27018(2) 0.01353(9) Uani 1 1 d . . . . .
C22 C 0.4037(2) 0.7587(2) 0.20640(19) 0.0198(6) Uani 1 1 d . . . . .
O23 O 0.4180(2) 0.82440(18) 0.15949(16) 0.0307(5) Uani 1 1 d . . . . .
C24 C 0.2408(2) 0.5222(2) 0.30268(18) 0.0178(5) Uani 1 1 d . . . . .
O25 O 0.16414(17) 0.45781(16) 0.30821(14) 0.0221(4) Uani 1 1 d . . . . .
C26 C 0.2507(3) 0.5572(2) 0.1213(2) 0.0229(6) Uani 1 1 d . . . . .
H26A H 0.2906 0.5709 0.0692 0.027 Uiso 1 1 calc R . . . .
H26B H 0.2176 0.4783 0.1131 0.027 Uiso 1 1 calc R . . . .
C27 C 0.1774(3) 0.6431(2) 0.1555(2) 0.0244(6) Uani 1 1 d . . . . .
H27A H 0.0985 0.6178 0.1687 0.029 Uiso 1 1 calc R . . . .
H27B H 0.1716 0.7105 0.1247 0.029 Uiso 1 1 calc R . . . .
C28 C 0.4073(2) 0.8572(2) 0.44770(19) 0.0177(5) Uani 1 1 d . . . . .
H28A H 0.4411 0.9103 0.4134 0.021 Uiso 1 1 calc R . . . .
H28B H 0.3897 0.9013 0.5070 0.021 Uiso 1 1 calc R . . . .
P29 P 0.26462(6) 0.78611(5) 0.37411(5) 0.01461(15) Uani 1 1 d . . . . .
C30 C 0.1783(2) 0.9081(2) 0.34550(19) 0.0172(5) Uani 1 1 d . . . . .
C31 C 0.1329(2) 0.9797(2) 0.4150(2) 0.0200(6) Uani 1 1 d . . . . .
H31 H 0.1464 0.9652 0.4778 0.024 Uiso 1 1 calc R . . . .
C32 C 0.0676(3) 1.0729(2) 0.3929(2) 0.0232(6) Uani 1 1 d . . . . .
H32 H 0.0375 1.1219 0.4407 0.028 Uiso 1 1 calc R . . . .
C33 C 0.0467(3) 1.0938(2) 0.3010(2) 0.0236(6) Uani 1 1 d . . . . .
H33 H 0.0018 1.1568 0.2858 0.028 Uiso 1 1 calc R . . . .
C34 C 0.0916(3) 1.0224(2) 0.2313(2) 0.0243(6) Uani 1 1 d . . . . .
H34 H 0.0769 1.0364 0.1684 0.029 Uiso 1 1 calc R . . . .
C35 C 0.1580(3) 0.9303(2) 0.2537(2) 0.0227(6) Uani 1 1 d . . . . .
H35 H 0.1896 0.8824 0.2061 0.027 Uiso 1 1 calc R . . . .
C36 C 0.1803(2) 0.7389(2) 0.45727(19) 0.0176(5) Uani 1 1 d . . . . .
C37 C 0.2289(3) 0.7448(2) 0.5526(2) 0.0219(6) Uani 1 1 d . . . . .
H37 H 0.3086 0.7785 0.5788 0.026 Uiso 1 1 calc R . . . .
C38 C 0.1600(3) 0.7010(2) 0.6105(2) 0.0291(7) Uani 1 1 d . . . . .
H38 H 0.1931 0.7055 0.6759 0.035 Uiso 1 1 calc R . . . .
C39 C 0.0450(3) 0.6517(2) 0.5729(2) 0.0319(8) Uani 1 1 d . . . . .
H39 H -0.0010 0.6214 0.6120 0.038 Uiso 1 1 calc R . . . .
C40 C -0.0036(3) 0.6462(2) 0.4781(2) 0.0303(7) Uani 1 1 d . . . . .
H40 H -0.0832 0.6124 0.4522 0.036 Uiso 1 1 calc R . . . .
C41 C 0.0631(3) 0.6897(2) 0.4203(2) 0.0239(6) Uani 1 1 d . . . . .
H41 H 0.0286 0.6859 0.3552 0.029 Uiso 1 1 calc R . . . .
O47 O 0.0637(4) 0.7298(4) -0.1605(3) 0.0321(13) Uani 0.502(6) 1 d D U P A 1
C48 C -0.0198(11) 0.7168(11) -0.1024(8) 0.032(3) Uani 0.502(6) 1 d D U P A 1
H48A H -0.0070 0.6455 -0.0776 0.038 Uiso 0.502(6) 1 calc R . P A 1
H48B H -0.1045 0.7136 -0.1392 0.038 Uiso 0.502(6) 1 calc R . P A 1
C49 C -0.0003(9) 0.8176(9) -0.0204(7) 0.026(2) Uani 0.502(6) 1 d D U P A 1
H49A H 0.0010 0.7927 0.0406 0.031 Uiso 0.502(6) 1 calc R . P A 1
H49B H -0.0651 0.8721 -0.0299 0.031 Uiso 0.502(6) 1 calc R . P A 1
C50 C 0.1270(12) 0.8706(13) -0.0242(14) 0.029(3) Uani 0.502(6) 1 d D U P A 1
H50A H 0.1192 0.9440 -0.0461 0.035 Uiso 0.502(6) 1 calc R . P A 1
H50B H 0.1830 0.8814 0.0383 0.035 Uiso 0.502(6) 1 calc R . P A 1
C51 C 0.1706(7) 0.7798(6) -0.0966(5) 0.0318(17) Uani 0.502(6) 1 d D U P A 1
H51A H 0.2257 0.8146 -0.1306 0.038 Uiso 0.502(6) 1 calc R . P A 1
H51B H 0.2151 0.7223 -0.0647 0.038 Uiso 0.502(6) 1 calc R . P A 1
O42 O 0.6493(3) 0.9698(2) 0.34758(17) 0.0448(6) Uani 1 1 d . . . . .
C43 C 0.6629(5) 1.0092(3) 0.2627(3) 0.0541(11) Uani 1 1 d . . . . .
H43A H 0.7090 1.0834 0.2788 0.065 Uiso 1 1 calc R . . . .
H43B H 0.5816 1.0180 0.2241 0.065 Uiso 1 1 calc R . . . .
C44 C 0.7313(3) 0.9222(3) 0.2084(2) 0.0398(8) Uani 1 1 d . . . . .
H44A H 0.7907 0.9590 0.1792 0.048 Uiso 1 1 calc R . . . .
H44B H 0.6743 0.8702 0.1582 0.048 Uiso 1 1 calc R . . . .
C45 C 0.7964(3) 0.8598(3) 0.2837(2) 0.0366(8) Uani 1 1 d . . . . .
H45A H 0.8119 0.7813 0.2563 0.044 Uiso 1 1 calc R . . . .
H45B H 0.8746 0.8999 0.3183 0.044 Uiso 1 1 calc R . . . .
C46 C 0.7036(3) 0.8623(3) 0.3466(2) 0.0323(7) Uani 1 1 d . . . . .
H46A H 0.6405 0.7998 0.3212 0.039 Uiso 1 1 calc R . . . .
H46B H 0.7438 0.8544 0.4113 0.039 Uiso 1 1 calc R . . . .
O47B O 0.0347(5) 0.9042(4) -0.0144(3) 0.0378(15) Uani 0.498(6) 1 d D U P A 2
C48B C 0.1497(13) 0.8661(13) -0.0322(15) 0.033(3) Uani 0.498(6) 1 d D U P A 2
H48C H 0.2095 0.8724 0.0282 0.040 Uiso 0.498(6) 1 calc R . P A 2
H48D H 0.1818 0.9131 -0.0722 0.040 Uiso 0.498(6) 1 calc R . P A 2
C49B C 0.1309(8) 0.7441(7) -0.0822(6) 0.039(2) Uani 0.498(6) 1 d D U P A 2
H49C H 0.1907 0.6964 -0.0502 0.046 Uiso 0.498(6) 1 calc R . P A 2
H49D H 0.1397 0.7371 -0.1489 0.046 Uiso 0.498(6) 1 calc R . P A 2
C50B C 0.0009(10) 0.7101(11) -0.0761(8) 0.034(3) Uani 0.498(6) 1 d D U P A 2
H50C H -0.0551 0.7039 -0.1382 0.041 Uiso 0.498(6) 1 calc R . P A 2
H50D H -0.0022 0.6370 -0.0540 0.041 Uiso 0.498(6) 1 calc R . P A 2
C51B C -0.0314(11) 0.8064(9) -0.0044(8) 0.032(2) Uani 0.498(6) 1 d D U P A 2
H51C H -0.1205 0.8170 -0.0174 0.038 Uiso 0.498(6) 1 calc R . P A 2
H51D H -0.0072 0.7905 0.0606 0.038 Uiso 0.498(6) 1 calc R . 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
C1 C2 1.404(4) . ?
C1 C6 1.394(4) . ?
C1 P7 1.828(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.384(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.391(4) . ?
C6 H6 0.9500 . ?
P7 C8 1.843(3) . ?
P7 C14 1.850(3) . ?
P7 Mo21 2.4328(7) . ?
C8 C9 1.392(4) . ?
C8 C13 1.391(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.398(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.378(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.388(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.393(4) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.493(4) . ?
C15 C16 1.384(4) . ?
C15 N20 1.374(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.385(4) . ?
C19 N20 1.370(3) . ?
C19 C28 1.500(4) . ?
N20 Mo21 2.285(2) . ?
Mo21 C22 2.005(3) . ?
Mo21 C24 1.993(3) . ?
Mo21 C26 2.275(3) . ?
Mo21 C27 2.279(3) . ?
Mo21 P29 2.4315(7) . ?
C22 O23 1.162(3) . ?
C24 O25 1.166(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.410(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 P29 1.842(3) . ?
P29 C30 1.833(3) . ?
P29 C36 1.831(3) . ?
C30 C31 1.392(4) . ?
C30 C35 1.393(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.397(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.389(4) . ?
C33 H33 0.9500 . ?
C33 C34 1.389(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.394(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.386(4) . ?
C36 C41 1.394(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.407(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.374(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.379(5) . ?
C40 H40 0.9500 . ?
C40 C41 1.388(4) . ?
C41 H41 0.9500 . ?
O47 C48 1.401(12) . ?
O47 C51 1.416(9) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C48 C49 1.528(12) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.561(13) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C50 C51 1.537(12) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
O42 C43 1.439(4) . ?
O42 C46 1.434(4) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 C44 1.508(5) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.520(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.509(5) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
O47B C48B 1.425(12) . ?
O47B C51B 1.420(10) . ?
C48B H48C 0.9900 . ?
C48B H48D 0.9900 . ?
C48B C49B 1.510(14) . ?
C49B H49C 0.9900 . ?
C49B H49D 0.9900 . ?
C49B C50B 1.523(12) . ?
C50B H50C 0.9900 . ?
C50B H50D 0.9900 . ?
C50B C51B 1.518(12) . ?
C51B H51C 0.9900 . ?
C51B H51D 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
C2 C1 P7 118.2(2) . . ?
C6 C1 C2 118.7(2) . . ?
C6 C1 P7 123.0(2) . . ?
C1 C2 H2 119.8 . . ?
C3 C2 C1 120.3(3) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(3) . . ?
C5 C4 H4 120.1 . . ?
C4 C5 H5 120.1 . . ?
C4 C5 C6 119.9(3) . . ?
C6 C5 H5 120.1 . . ?
C1 C6 H6 119.6 . . ?
C5 C6 C1 120.8(3) . . ?
C5 C6 H6 119.6 . . ?
C1 P7 C8 101.13(12) . . ?
C1 P7 C14 104.98(12) . . ?
C1 P7 Mo21 121.53(9) . . ?
C8 P7 C14 101.17(12) . . ?
C8 P7 Mo21 125.18(9) . . ?
C14 P7 Mo21 99.24(9) . . ?
C9 C8 P7 122.8(2) . . ?
C13 C8 P7 118.6(2) . . ?
C13 C8 C9 118.6(3) . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.4(3) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.8 . . ?
C11 C10 C9 120.5(3) . . ?
C11 C10 H10 119.8 . . ?
C10 C11 H11 120.2 . . ?
C10 C11 C12 119.7(3) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.9(3) . . ?
C13 C12 H12 120.1 . . ?
C8 C13 C12 121.0(3) . . ?
C8 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
P7 C14 H14A 109.8 . . ?
P7 C14 H14B 109.8 . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 P7 109.52(18) . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
C16 C15 C14 120.9(2) . . ?
N20 C15 C14 116.7(2) . . ?
N20 C15 C16 122.4(2) . . ?
C15 C16 H16 120.1 . . ?
C15 C16 C17 119.9(3) . . ?
C17 C16 H16 120.1 . . ?
C16 C17 H17 120.7 . . ?
C16 C17 C18 118.5(3) . . ?
C18 C17 H17 120.7 . . ?
C17 C18 H18 120.2 . . ?
C19 C18 C17 119.6(3) . . ?
C19 C18 H18 120.2 . . ?
C18 C19 C28 120.8(2) . . ?
N20 C19 C18 122.5(2) . . ?
N20 C19 C28 116.6(2) . . ?
C15 N20 Mo21 120.90(17) . . ?
C19 N20 C15 116.9(2) . . ?
C19 N20 Mo21 122.10(17) . . ?
N20 Mo21 P7 76.35(6) . . ?
N20 Mo21 P29 75.39(6) . . ?
C22 Mo21 P7 96.84(7) . . ?
C22 Mo21 N20 98.91(9) . . ?
C22 Mo21 C26 84.39(11) . . ?
C22 Mo21 C27 80.15(11) . . ?
C22 Mo21 P29 88.88(8) . . ?
C24 Mo21 P7 92.67(7) . . ?
C24 Mo21 N20 98.67(9) . . ?
C24 Mo21 C22 161.56(11) . . ?
C24 Mo21 C26 81.14(10) . . ?
C24 Mo21 C27 81.42(11) . . ?
C24 Mo21 P29 90.20(7) . . ?
C26 Mo21 P7 82.90(7) . . ?
C26 Mo21 N20 159.23(9) . . ?
C26 Mo21 C27 36.09(10) . . ?
C26 Mo21 P29 125.31(7) . . ?
C27 Mo21 P7 118.98(8) . . ?
C27 Mo21 N20 164.67(9) . . ?
C27 Mo21 P29 89.28(8) . . ?
P29 Mo21 P7 151.71(2) . . ?
O23 C22 Mo21 168.6(2) . . ?
O25 C24 Mo21 167.9(2) . . ?
Mo21 C26 H26A 116.4 . . ?
Mo21 C26 H26B 116.4 . . ?
H26A C26 H26B 113.4 . . ?
C27 C26 Mo21 72.10(16) . . ?
C27 C26 H26A 116.4 . . ?
C27 C26 H26B 116.4 . . ?
Mo21 C27 H27A 116.4 . . ?
Mo21 C27 H27B 116.4 . . ?
C26 C27 Mo21 71.81(16) . . ?
C26 C27 H27A 116.4 . . ?
C26 C27 H27B 116.4 . . ?
H27A C27 H27B 113.4 . . ?
C19 C28 H28A 109.6 . . ?
C19 C28 H28B 109.6 . . ?
C19 C28 P29 110.41(18) . . ?
H28A C28 H28B 108.1 . . ?
P29 C28 H28A 109.6 . . ?
P29 C28 H28B 109.6 . . ?
C28 P29 Mo21 100.64(9) . . ?
C30 P29 Mo21 129.38(9) . . ?
C30 P29 C28 101.02(12) . . ?
C36 P29 Mo21 116.51(8) . . ?
C36 P29 C28 105.31(13) . . ?
C36 P29 C30 100.80(12) . . ?
C31 C30 P29 120.6(2) . . ?
C31 C30 C35 119.2(2) . . ?
C35 C30 P29 120.2(2) . . ?
C30 C31 H31 119.8 . . ?
C30 C31 C32 120.4(3) . . ?
C32 C31 H31 119.8 . . ?
C31 C32 H32 120.0 . . ?
C33 C32 C31 120.0(3) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.9(3) . . ?
C34 C33 H33 120.1 . . ?
C33 C34 H34 120.0 . . ?
C33 C34 C35 120.0(3) . . ?
C35 C34 H34 120.0 . . ?
C30 C35 C34 120.4(3) . . ?
C30 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C37 C36 P29 123.6(2) . . ?
C37 C36 C41 119.2(3) . . ?
C41 C36 P29 117.1(2) . . ?
C36 C37 H37 120.1 . . ?
C36 C37 C38 119.9(3) . . ?
C38 C37 H37 120.1 . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.3(3) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 120.1 . . ?
C38 C39 C40 119.8(3) . . ?
C40 C39 H39 120.1 . . ?
C39 C40 H40 119.7 . . ?
C39 C40 C41 120.5(3) . . ?
C41 C40 H40 119.7 . . ?
C36 C41 H41 119.9 . . ?
C40 C41 C36 120.3(3) . . ?
C40 C41 H41 119.9 . . ?
C48 O47 C51 104.2(7) . . ?
O47 C48 H48A 110.0 . . ?
O47 C48 H48B 110.0 . . ?
O47 C48 C49 108.5(8) . . ?
H48A C48 H48B 108.4 . . ?
C49 C48 H48A 110.0 . . ?
C49 C48 H48B 110.0 . . ?
C48 C49 H49A 111.2 . . ?
C48 C49 H49B 111.2 . . ?
C48 C49 C50 103.0(7) . . ?
H49A C49 H49B 109.1 . . ?
C50 C49 H49A 111.2 . . ?
C50 C49 H49B 111.2 . . ?
C49 C50 H50A 111.5 . . ?
C49 C50 H50B 111.5 . . ?
H50A C50 H50B 109.3 . . ?
C51 C50 C49 101.5(8) . . ?
C51 C50 H50A 111.5 . . ?
C51 C50 H50B 111.5 . . ?
O47 C51 C50 106.2(8) . . ?
O47 C51 H51A 110.5 . . ?
O47 C51 H51B 110.5 . . ?
C50 C51 H51A 110.5 . . ?
C50 C51 H51B 110.5 . . ?
H51A C51 H51B 108.7 . . ?
C46 O42 C43 108.1(3) . . ?
O42 C43 H43A 110.2 . . ?
O42 C43 H43B 110.2 . . ?
O42 C43 C44 107.4(3) . . ?
H43A C43 H43B 108.5 . . ?
C44 C43 H43A 110.2 . . ?
C44 C43 H43B 110.2 . . ?
C43 C44 H44A 111.1 . . ?
C43 C44 H44B 111.1 . . ?
C43 C44 C45 103.4(3) . . ?
H44A C44 H44B 109.1 . . ?
C45 C44 H44A 111.1 . . ?
C45 C44 H44B 111.1 . . ?
C44 C45 H45A 111.6 . . ?
C44 C45 H45B 111.6 . . ?
H45A C45 H45B 109.4 . . ?
C46 C45 C44 100.9(3) . . ?
C46 C45 H45A 111.6 . . ?
C46 C45 H45B 111.6 . . ?
O42 C46 C45 106.2(3) . . ?
O42 C46 H46A 110.5 . . ?
O42 C46 H46B 110.5 . . ?
C45 C46 H46A 110.5 . . ?
C45 C46 H46B 110.5 . . ?
H46A C46 H46B 108.7 . . ?
C51B O47B C48B 105.5(9) . . ?
O47B C48B H48C 110.1 . . ?
O47B C48B H48D 110.1 . . ?
O47B C48B C49B 108.0(9) . . ?
H48C C48B H48D 108.4 . . ?
C49B C48B H48C 110.1 . . ?
C49B C48B H48D 110.1 . . ?
C48B C49B H49C 110.9 . . ?
C48B C49B H49D 110.9 . . ?
C48B C49B C50B 104.4(8) . . ?
H49C C49B H49D 108.9 . . ?
C50B C49B H49C 110.9 . . ?
C50B C49B H49D 110.9 . . ?
C49B C50B H50C 111.1 . . ?
C49B C50B H50D 111.1 . . ?
H50C C50B H50D 109.1 . . ?
C51B C50B C49B 103.1(8) . . ?
C51B C50B H50C 111.1 . . ?
C51B C50B H50D 111.1 . . ?
O47B C51B C50B 105.8(8) . . ?
O47B C51B H51C 110.6 . . ?
O47B C51B H51D 110.6 . . ?
C50B C51B H51C 110.6 . . ?
C50B C51B H51D 110.6 . . ?
H51C C51B H51D 108.7 . . ?

_shelx_SHELXL_version_number     2014/7

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a 100 micro/m MITIGEN holder oil'
_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_compound_3b
_database_code_depnum_ccdc_archive 'CCDC 1911736'
loop_
_audit_author_name
_audit_author_address
'Francisco Molina Gonzalez'
;CIQSO
Spain
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;

_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C36 H35 N O2 P2 W, 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H39 Cl4 N O2 P2 W'
_chemical_properties_physical    
'air-sensitive, moisture-sensitive,Air-sensitive,Moisture-sensitive'
_chemical_formula_weight         929.29
_exptl_crystal_recrystallization_method 'Crystallised from dichloromethane'
_chemical_melting_point          ?
_exptl_crystal_description       prism
_exptl_crystal_colour            'light yellow'
_diffrn_ambient_temperature      100.0
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'
Cl Cl 0.1484 0.1585 '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'
W W -0.8490 6.8722 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yn'
_chemical_absolute_configuration .
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'
'-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                   35.714(3)
_cell_length_b                   16.0980(13)
_cell_length_c                   15.0574(12)
_cell_angle_alpha                90
_cell_angle_beta                 111.571(2)
_cell_angle_gamma                90
_cell_volume                     8050.5(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.14
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.247
_exptl_absorpt_correction_T_max  0.0183
_exptl_absorpt_correction_T_min  0.0046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1099 before and 0.0732 after correction. 
The Ratio of minimum to maximum transmission is 0.2514. 
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             3696
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            127331
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.178
_diffrn_reflns_theta_max         25.178
_diffrn_reflns_theta_min         2.179
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6058
_reflns_number_total             7184
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Bruker Apex3, 2017'
_computing_data_collection       'Bruker Apex3, 2017'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.909
_refine_diff_density_min         -1.871
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7184
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0677
_refine_ls_restrained_S_all      1.194
_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)+(0.0134P)²+268.4964P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1560
_refine_special_details          
;A disordered dicholoromethane solvent molecule was refined 
using DFIX contraints and SIMU and RIGU restraints
in order to enhance the model.

All H atoms were refined using a riding model, with a common U restrained
to be 1.2 (1.5 for methyl groups) times the equivalent isotropic displacement
parameter of the parent atom. 

Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.,Olex2 solvent mask tool
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl4-C37 = Cl3-C37
 1.771 with sigma of 0.01
 Cl4-Cl3
 2.916 with sigma of 0.03
3. Uiso/Uaniso restraints and constraints
Cl3 \\sim Cl4 \\sim C37: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl3, Cl4, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C12(H12A,
 H12B), C38(H38A,H38B), C37(H37A,H37B)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_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
W1 W 0.36394(2) 0.35583(3) 0.44082(3) 0.04135(14) Uani 1 1 d . . . . .
P1 P 0.31575(8) 0.27155(18) 0.3169(2) 0.0448(6) Uani 1 1 d . . . . .
P2 P 0.39310(8) 0.42682(19) 0.5946(2) 0.0430(6) Uani 1 1 d . . . . .
O1 O 0.3478(2) 0.2154(5) 0.5740(6) 0.0525(19) Uani 1 1 d . . . . .
O2 O 0.3947(2) 0.2400(5) 0.5082(5) 0.0477(17) Uani 1 1 d . . . . .
N1 N 0.3078(2) 0.3774(5) 0.4753(6) 0.044(2) Uani 1 1 d . . . . .
C1 C 0.3637(3) 0.2537(7) 0.5249(8) 0.049(3) Uani 1 1 d . . . . .
C2 C 0.3524(3) 0.4905(7) 0.4065(8) 0.049(3) Uani 1 1 d . . . . .
H2A H 0.337662 0.520663 0.440880 0.058 Uiso 1 1 calc R . . . .
H2B H 0.374884 0.522771 0.400317 0.058 Uiso 1 1 calc R . . . .
C3 C 0.3286(3) 0.4440(6) 0.3252(7) 0.043(2) Uani 1 1 d . . . . .
H3A H 0.336349 0.447278 0.268608 0.052 Uiso 1 1 calc R . . . .
H3B H 0.299105 0.445169 0.309194 0.052 Uiso 1 1 calc R . . . .
C4 C 0.4250(3) 0.3770(7) 0.4387(8) 0.048(3) Uani 1 1 d . . . . .
H4A H 0.431857 0.435089 0.429281 0.058 Uiso 1 1 calc R . . . .
H4B H 0.447345 0.346717 0.487269 0.058 Uiso 1 1 calc R . . . .
C5 C 0.4024(3) 0.3319(8) 0.3550(8) 0.051(3) Uani 1 1 d . . . . .
H5A H 0.410602 0.273625 0.351659 0.061 Uiso 1 1 calc R . . . .
H5B H 0.395095 0.362103 0.293602 0.061 Uiso 1 1 calc R . . . .
C6 C 0.3478(3) 0.4613(7) 0.6163(7) 0.046(3) Uani 1 1 d . . . . .
H6A H 0.351939 0.450319 0.683961 0.055 Uiso 1 1 calc R . . . .
H6B H 0.344901 0.522078 0.606248 0.055 Uiso 1 1 calc R . . . .
C7 C 0.3093(3) 0.4206(7) 0.5546(7) 0.046(2) Uani 1 1 d . . . . .
C8 C 0.2763(3) 0.4302(7) 0.5789(8) 0.048(3) Uani 1 1 d . . . . .
H8 H 0.278173 0.461843 0.633679 0.058 Uiso 1 1 calc R . . . .
C9 C 0.2396(3) 0.3934(8) 0.5233(8) 0.053(3) Uani 1 1 d . . . . .
H9 H 0.216560 0.398913 0.539955 0.064 Uiso 1 1 calc R . . . .
C10 C 0.2380(3) 0.3496(7) 0.4449(8) 0.048(3) Uani 1 1 d . . . . .
H10 H 0.213372 0.324395 0.405697 0.057 Uiso 1 1 calc R . . . .
C11 C 0.2721(3) 0.3413(7) 0.4214(7) 0.044(2) Uani 1 1 d . . . . .
C12 C 0.2682(3) 0.2902(8) 0.3359(8) 0.052(3) Uani 1 1 d . . . . .
H12A H 0.249063 0.318118 0.278570 0.063 Uiso 1 1 calc R . . . .
H12B H 0.256369 0.235793 0.341879 0.063 Uiso 1 1 calc R . . . .
C13 C 0.3047(3) 0.2928(7) 0.1890(8) 0.053(3) Uani 1 1 d . . . . .
C14 C 0.2742(4) 0.3438(8) 0.1328(9) 0.062(3) Uani 1 1 d . . . . .
H14 H 0.256859 0.369866 0.159471 0.075 Uiso 1 1 calc R . . . .
C15 C 0.2684(4) 0.3573(9) 0.0382(9) 0.071(4) Uani 1 1 d . . . . .
H15 H 0.247025 0.391872 -0.000005 0.085 Uiso 1 1 calc R . . . .
C16 C 0.2933(5) 0.3213(10) -0.0006(9) 0.072(4) Uani 1 1 d . . . . .
H16 H 0.289669 0.331980 -0.065265 0.087 Uiso 1 1 calc R . . . .
C17 C 0.3232(4) 0.2704(10) 0.0527(9) 0.071(4) Uani 1 1 d . . . . .
H17 H 0.340060 0.244741 0.024471 0.085 Uiso 1 1 calc R . . . .
C18 C 0.3298(4) 0.2547(9) 0.1488(9) 0.062(3) Uani 1 1 d . . . . .
H18 H 0.350878 0.218778 0.185781 0.074 Uiso 1 1 calc R . . . .
C19 C 0.3169(3) 0.1566(7) 0.3090(8) 0.051(3) Uani 1 1 d . . . . .
C20 C 0.2823(4) 0.1140(8) 0.2520(9) 0.057(3) Uani 1 1 d . . . . .
H20 H 0.257966 0.143941 0.221968 0.068 Uiso 1 1 calc R . . . .
C21 C 0.2828(4) 0.0314(10) 0.2391(10) 0.072(4) Uani 1 1 d . . . . .
H21 H 0.259170 0.004100 0.198405 0.086 Uiso 1 1 calc R . . . .
C22 C 0.3174(5) -0.0142(10) 0.2845(13) 0.096(5) Uani 1 1 d . . . . .
H22 H 0.317805 -0.072710 0.276461 0.116 Uiso 1 1 calc R . . . .
C23 C 0.3514(5) 0.0278(10) 0.3418(12) 0.094(5) Uani 1 1 d . . . . .
H23 H 0.375399 -0.002779 0.373504 0.113 Uiso 1 1 calc R . . . .
C24 C 0.3517(4) 0.1120(8) 0.3546(10) 0.069(4) Uani 1 1 d . . . . .
H24 H 0.375582 0.139345 0.394348 0.083 Uiso 1 1 calc R . . . .
C25 C 0.4244(3) 0.5197(7) 0.6067(7) 0.043(2) Uani 1 1 d . . . . .
C26 C 0.4647(3) 0.5080(7) 0.6252(7) 0.045(2) Uani 1 1 d . . . . .
H26 H 0.475268 0.453270 0.631732 0.054 Uiso 1 1 calc R . . . .
C27 C 0.4900(3) 0.5759(8) 0.6347(8) 0.053(3) Uani 1 1 d . . . . .
H27 H 0.517753 0.567057 0.646277 0.064 Uiso 1 1 calc R . . . .
C28 C 0.4755(3) 0.6544(8) 0.6273(7) 0.052(3) Uani 1 1 d . . . . .
H28 H 0.493221 0.700151 0.634839 0.063 Uiso 1 1 calc R . . . .
C29 C 0.4351(4) 0.6689(7) 0.6090(8) 0.055(3) Uani 1 1 d . . . . .
H29 H 0.425012 0.723990 0.603605 0.066 Uiso 1 1 calc R . . . .
C30 C 0.4091(3) 0.5998(7) 0.5986(7) 0.047(3) Uani 1 1 d . . . . .
H30 H 0.381287 0.608344 0.586042 0.056 Uiso 1 1 calc R . . . .
C31 C 0.4230(3) 0.3772(7) 0.7078(7) 0.045(2) Uani 1 1 d . . . . .
C32 C 0.4277(4) 0.4181(8) 0.7949(8) 0.057(3) Uani 1 1 d . . . . .
H32 H 0.414869 0.470109 0.793169 0.068 Uiso 1 1 calc R . . . .
C33 C 0.4505(4) 0.3840(8) 0.8816(8) 0.058(3) Uani 1 1 d . . . . .
H33 H 0.453701 0.412859 0.938999 0.069 Uiso 1 1 calc R . . . .
C34 C 0.4688(3) 0.3076(8) 0.8855(8) 0.054(3) Uani 1 1 d . . . . .
H34 H 0.483759 0.283294 0.945631 0.064 Uiso 1 1 calc R . . . .
C35 C 0.4655(3) 0.2674(9) 0.8042(9) 0.059(3) Uani 1 1 d . . . . .
H35 H 0.478463 0.215225 0.808314 0.071 Uiso 1 1 calc R . . . .
C36 C 0.4430(3) 0.3013(8) 0.7118(8) 0.055(3) Uani 1 1 d . . . . .
H36 H 0.441627 0.273295 0.655114 0.066 Uiso 1 1 calc R . . . .
Cl1 Cl 0.32916(12) -0.3023(3) 0.2911(3) 0.1028(15) Uani 1 1 d . . . . .
Cl2 Cl 0.38715(16) -0.1798(3) 0.4066(3) 0.0983(13) Uani 1 1 d . . . . .
C38 C 0.3691(4) -0.2366(10) 0.3005(11) 0.084(5) Uani 1 1 d . . . . .
H38A H 0.360343 -0.197312 0.246070 0.100 Uiso 1 1 calc R . . . .
H38B H 0.391419 -0.270227 0.295295 0.100 Uiso 1 1 calc R . . . .
Cl3 Cl 0.3586(3) -0.0460(4) 0.5939(5) 0.189(3) Uani 1 1 d D U . . .
Cl4 Cl 0.4229(2) 0.0559(5) 0.7165(5) 0.167(3) Uani 1 1 d D U . . .
C37 C 0.3909(6) 0.0382(12) 0.5986(9) 0.159(6) Uani 1 1 d D U . . .
H37A H 0.406992 0.025858 0.558913 0.191 Uiso 1 1 calc R . . . .
H37B H 0.374692 0.088696 0.572643 0.191 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
W1 P1 2.434(3) . ?
W1 P2 2.446(3) . ?
W1 O2 2.212(8) . ?
W1 N1 2.275(8) . ?
W1 C1 2.077(12) . ?
W1 C2 2.231(11) . ?
W1 C3 2.241(10) . ?
W1 C4 2.218(10) . ?
W1 C5 2.239(10) . ?
P1 C12 1.848(10) . ?
P1 C13 1.850(12) . ?
P1 C19 1.856(12) . ?
P2 C6 1.850(10) . ?
P2 C25 1.836(11) . ?
P2 C31 1.829(11) . ?
O1 C1 1.248(13) . ?
O2 C1 1.243(12) . ?
N1 C7 1.364(13) . ?
N1 C11 1.364(13) . ?
C2 C3 1.420(14) . ?
C4 C5 1.421(15) . ?
C6 C7 1.496(14) . ?
C7 C8 1.369(14) . ?
C8 C9 1.399(16) . ?
C9 C10 1.358(16) . ?
C10 C11 1.396(14) . ?
C11 C12 1.490(15) . ?
C13 C14 1.379(17) . ?
C13 C18 1.394(17) . ?
C14 C15 1.380(17) . ?
C15 C16 1.36(2) . ?
C16 C17 1.35(2) . ?
C17 C18 1.401(17) . ?
C19 C20 1.399(16) . ?
C19 C24 1.380(17) . ?
C20 C21 1.345(18) . ?
C21 C22 1.38(2) . ?
C22 C23 1.38(2) . ?
C23 C24 1.368(19) . ?
C25 C26 1.374(14) . ?
C25 C30 1.387(15) . ?
C26 C27 1.393(15) . ?
C27 C28 1.357(17) . ?
C28 C29 1.384(16) . ?
C29 C30 1.421(15) . ?
C31 C32 1.421(15) . ?
C31 C36 1.406(16) . ?
C32 C33 1.374(16) . ?
C33 C34 1.384(17) . ?
C34 C35 1.351(16) . ?
C35 C36 1.434(16) . ?
Cl1 C38 1.739(16) . ?
Cl2 C38 1.746(14) . ?
Cl3 C37 1.764(9) . ?
Cl4 C37 1.746(9) . ?

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
P1 W1 P2 157.13(9) . . ?
O2 W1 P1 88.5(2) . . ?
O2 W1 P2 89.6(2) . . ?
O2 W1 N1 110.8(3) . . ?
O2 W1 C2 160.6(3) . . ?
O2 W1 C3 158.9(3) . . ?
O2 W1 C4 79.1(4) . . ?
O2 W1 C5 79.2(4) . . ?
N1 W1 P1 80.0(2) . . ?
N1 W1 P2 79.4(2) . . ?
C1 W1 P1 82.3(3) . . ?
C1 W1 P2 83.6(3) . . ?
C1 W1 O2 33.5(3) . . ?
C1 W1 N1 77.3(4) . . ?
C1 W1 C2 150.2(4) . . ?
C1 W1 C3 147.9(4) . . ?
C1 W1 C4 110.8(4) . . ?
C1 W1 C5 110.9(4) . . ?
C2 W1 P1 110.2(3) . . ?
C2 W1 P2 75.1(3) . . ?
C2 W1 N1 78.5(4) . . ?
C2 W1 C3 37.0(4) . . ?
C2 W1 C5 97.7(4) . . ?
C3 W1 P1 73.7(3) . . ?
C3 W1 P2 111.2(3) . . ?
C3 W1 N1 77.8(4) . . ?
C4 W1 P1 119.8(3) . . ?
C4 W1 P2 82.1(3) . . ?
C4 W1 N1 158.9(4) . . ?
C4 W1 C2 86.9(4) . . ?
C4 W1 C3 99.7(4) . . ?
C4 W1 C5 37.2(4) . . ?
C5 W1 P1 82.7(3) . . ?
C5 W1 P2 119.3(3) . . ?
C5 W1 N1 159.6(4) . . ?
C5 W1 C3 87.2(4) . . ?
C12 P1 W1 102.9(4) . . ?
C12 P1 C13 106.0(5) . . ?
C12 P1 C19 102.5(5) . . ?
C13 P1 W1 121.0(4) . . ?
C13 P1 C19 96.8(5) . . ?
C19 P1 W1 125.4(4) . . ?
C6 P2 W1 102.2(3) . . ?
C25 P2 W1 120.4(3) . . ?
C25 P2 C6 106.2(5) . . ?
C31 P2 W1 125.3(4) . . ?
C31 P2 C6 102.5(5) . . ?
C31 P2 C25 97.9(5) . . ?
C1 O2 W1 67.3(7) . . ?
C7 N1 W1 121.4(7) . . ?
C7 N1 C11 117.8(9) . . ?
C11 N1 W1 120.5(7) . . ?
O1 C1 W1 149.0(9) . . ?
O2 C1 W1 79.2(7) . . ?
O2 C1 O1 131.8(11) . . ?
C3 C2 W1 71.9(6) . . ?
C2 C3 W1 71.1(6) . . ?
C5 C4 W1 72.2(6) . . ?
C4 C5 W1 70.6(6) . . ?
C7 C6 P2 114.9(7) . . ?
N1 C7 C6 120.0(9) . . ?
N1 C7 C8 122.0(10) . . ?
C8 C7 C6 118.0(10) . . ?
C7 C8 C9 120.1(10) . . ?
C10 C9 C8 118.2(10) . . ?
C9 C10 C11 120.5(11) . . ?
N1 C11 C10 121.3(10) . . ?
N1 C11 C12 121.4(9) . . ?
C10 C11 C12 117.3(10) . . ?
C11 C12 P1 115.0(8) . . ?
C14 C13 P1 124.5(10) . . ?
C14 C13 C18 119.0(12) . . ?
C18 C13 P1 116.4(10) . . ?
C13 C14 C15 120.7(14) . . ?
C16 C15 C14 120.3(14) . . ?
C17 C16 C15 120.1(13) . . ?
C16 C17 C18 121.3(14) . . ?
C13 C18 C17 118.5(13) . . ?
C20 C19 P1 119.5(9) . . ?
C24 C19 P1 121.7(9) . . ?
C24 C19 C20 118.8(11) . . ?
C21 C20 C19 121.1(13) . . ?
C20 C21 C22 120.8(14) . . ?
C23 C22 C21 118.0(15) . . ?
C24 C23 C22 122.2(15) . . ?
C23 C24 C19 119.1(12) . . ?
C26 C25 P2 117.5(9) . . ?
C26 C25 C30 119.7(10) . . ?
C30 C25 P2 122.8(8) . . ?
C25 C26 C27 120.4(11) . . ?
C28 C27 C26 120.5(11) . . ?
C27 C28 C29 120.8(11) . . ?
C28 C29 C30 118.8(11) . . ?
C25 C30 C29 119.8(10) . . ?
C32 C31 P2 119.2(9) . . ?
C36 C31 P2 122.2(8) . . ?
C36 C31 C32 118.5(10) . . ?
C33 C32 C31 121.3(12) . . ?
C32 C33 C34 120.1(12) . . ?
C35 C34 C33 120.3(12) . . ?
C34 C35 C36 121.9(12) . . ?
C31 C36 C35 117.8(11) . . ?
Cl1 C38 Cl2 114.1(9) . . ?
Cl4 C37 Cl3 109.8(8) . . ?

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
W1 P1 C12 C11 -5.3(9) . . . . ?
W1 P1 C13 C14 -92.0(10) . . . . ?
W1 P1 C13 C18 87.2(9) . . . . ?
W1 P1 C19 C20 162.0(8) . . . . ?
W1 P1 C19 C24 -20.8(13) . . . . ?
W1 P2 C6 C7 15.0(9) . . . . ?
W1 P2 C25 C26 -85.8(8) . . . . ?
W1 P2 C25 C30 94.7(9) . . . . ?
W1 P2 C31 C32 -160.9(7) . . . . ?
W1 P2 C31 C36 21.8(10) . . . . ?
W1 O2 C1 O1 -177.9(14) . . . . ?
W1 N1 C7 C6 5.4(14) . . . . ?
W1 N1 C7 C8 -176.4(8) . . . . ?
W1 N1 C11 C10 176.0(8) . . . . ?
W1 N1 C11 C12 -2.9(13) . . . . ?
P1 C13 C14 C15 178.9(9) . . . . ?
P1 C13 C18 C17 -178.6(9) . . . . ?
P1 C19 C20 C21 175.2(10) . . . . ?
P1 C19 C24 C23 -176.3(13) . . . . ?
P2 C6 C7 N1 -14.5(14) . . . . ?
P2 C6 C7 C8 167.2(9) . . . . ?
P2 C25 C26 C27 179.6(8) . . . . ?
P2 C25 C30 C29 179.8(8) . . . . ?
P2 C31 C32 C33 -178.8(9) . . . . ?
P2 C31 C36 C35 -179.7(8) . . . . ?
N1 C7 C8 C9 1.6(17) . . . . ?
N1 C11 C12 P1 5.8(14) . . . . ?
C6 P2 C25 C26 159.0(8) . . . . ?
C6 P2 C25 C30 -20.5(10) . . . . ?
C6 P2 C31 C32 -46.0(9) . . . . ?
C6 P2 C31 C36 136.7(9) . . . . ?
C6 C7 C8 C9 179.9(10) . . . . ?
C7 N1 C11 C10 1.4(15) . . . . ?
C7 N1 C11 C12 -177.5(10) . . . . ?
C7 C8 C9 C10 -0.9(17) . . . . ?
C8 C9 C10 C11 0.5(17) . . . . ?
C9 C10 C11 N1 -0.8(16) . . . . ?
C9 C10 C11 C12 178.2(10) . . . . ?
C10 C11 C12 P1 -173.2(8) . . . . ?
C11 N1 C7 C6 179.9(10) . . . . ?
C11 N1 C7 C8 -1.9(16) . . . . ?
C12 P1 C13 C14 24.2(11) . . . . ?
C12 P1 C13 C18 -156.6(9) . . . . ?
C12 P1 C19 C20 46.2(11) . . . . ?
C12 P1 C19 C24 -136.7(11) . . . . ?
C13 P1 C12 C11 -133.2(9) . . . . ?
C13 P1 C19 C20 -61.9(10) . . . . ?
C13 P1 C19 C24 115.3(11) . . . . ?
C13 C14 C15 C16 -0.9(19) . . . . ?
C14 C13 C18 C17 0.7(17) . . . . ?
C14 C15 C16 C17 2(2) . . . . ?
C15 C16 C17 C18 -1(2) . . . . ?
C16 C17 C18 C13 0.0(19) . . . . ?
C18 C13 C14 C15 -0.2(18) . . . . ?
C19 P1 C12 C11 125.8(9) . . . . ?
C19 P1 C13 C14 129.3(10) . . . . ?
C19 P1 C13 C18 -51.5(10) . . . . ?
C19 C20 C21 C22 2(2) . . . . ?
C20 C19 C24 C23 1(2) . . . . ?
C20 C21 C22 C23 -1(3) . . . . ?
C21 C22 C23 C24 0(3) . . . . ?
C22 C23 C24 C19 0(3) . . . . ?
C24 C19 C20 C21 -2.0(19) . . . . ?
C25 P2 C6 C7 142.0(8) . . . . ?
C25 P2 C31 C32 62.6(9) . . . . ?
C25 P2 C31 C36 -114.7(9) . . . . ?
C25 C26 C27 C28 1.2(16) . . . . ?
C26 C25 C30 C29 0.3(15) . . . . ?
C26 C27 C28 C29 -0.9(17) . . . . ?
C27 C28 C29 C30 0.4(17) . . . . ?
C28 C29 C30 C25 -0.1(16) . . . . ?
C30 C25 C26 C27 -0.9(15) . . . . ?
C31 P2 C6 C7 -115.8(9) . . . . ?
C31 P2 C25 C26 53.5(9) . . . . ?
C31 P2 C25 C30 -126.0(9) . . . . ?
C31 C32 C33 C34 -1.2(18) . . . . ?
C32 C31 C36 C35 3.0(16) . . . . ?
C32 C33 C34 C35 2.2(18) . . . . ?
C33 C34 C35 C36 -0.5(18) . . . . ?
C34 C35 C36 C31 -2.1(17) . . . . ?
C36 C31 C32 C33 -1.4(16) . . . . ?

_smtbx_masks_special_details     
;
During the structure refinement, regions of electron density 
were identified as a highly disordered dichloromethane solvent molecules. 
Attempts to model these electron densities as dichloromethane 
were not successful due to the extent of the disorder. 
In the final structure model, this electron density contribution
has been removed from the intensity data
using the solvent mask tool in Olex2 (Dolomanov, O.V., Bourhis, 
L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.(2009), J. Appl.
Cryst. 42, 339-341.)
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 -0.773 535.1 135.0 ?
2 0.500 0.000 -0.902 535.1 135.0 ?


_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a 200 micro/m MITEGEN holder in perfluoroether oil'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound_3a
_database_code_depnum_ccdc_archive 'CCDC 1911735'
loop_
_audit_author_name
_audit_author_address
'Francisco Molina Gonzalez'
;CIQSO
Spain
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2018-06-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C36 H35 Mo N O2 P2, C7 H8'
_chemical_formula_sum            'C43 H43 Mo N O2 P2'
_chemical_properties_physical    
'moisture-sensitive, air-sensitive,Air-sensitive,Moisture-sensitive'
_chemical_formula_weight         763.66
_exptl_crystal_recrystallization_method 
'Crystallised from toluene at room temperature'
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_diffrn_ambient_temperature      100
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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.1562(7)
_cell_length_b                   14.2402(7)
_cell_length_c                   21.7973(12)
_cell_angle_alpha                74.258(2)
_cell_angle_beta                 74.580(2)
_cell_angle_gamma                65.252(2)
_cell_volume                     3514.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9480
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      2.30
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.0329
_exptl_absorpt_correction_T_min  0.0160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1045 before and 0.0654 after correction. 
The Ratio of minimum to maximum transmission is 0.4863. 
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            153539
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.102
_diffrn_reflns_theta_max         25.102
_diffrn_reflns_theta_min         2.244
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10036
_reflns_number_total             12480
_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       'Bruker Apex3, 2017'
_computing_data_collection       'Bruker Apex3, 2017'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.718
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     885
_refine_ls_number_reflns         12480
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0566P)²+6.3387P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1160
_refine_special_details          
;
Restraints (DELU, ISOR) are applied in order 
to enhance one toluene solvent model. 

All H atoms were refined using a riding model, with a common U restrained
to be 1.2 (1.5 for methyl groups) times the equivalent isotropic displacement
parameter of the parent atom. 

Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_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. Rigid bond restraints
 C80, C81, C82, C83, C84, C85, C86
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C80) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C11(H11A,H11B), C24(H24A,
 H24B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C47(H47A,H47B), C60(H60A,H60B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
 C43(H43), C44(H44), C45(H45), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
  C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C62(H62), C63(H63),
 C64(H64), C65(H65), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72),
  C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C82(H82), C83(H83),
 C84(H84), C85(H85), C86(H86)
4.c Idealised Me refined as rotating group:
 C73(H73A,H73B,H73C), C80(H80A,H80B,H80C)
;
_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 0.56855(3) 0.51398(2) 0.23037(2) 0.02709(9) Uani 1 1 d . . . . .
P1 P 0.65137(8) 0.60330(8) 0.13013(5) 0.0307(2) Uani 1 1 d . . . . .
P2 P 0.41397(8) 0.48773(7) 0.31655(4) 0.0281(2) Uani 1 1 d . . . . .
O1 O 0.3753(2) 0.5919(2) 0.14510(13) 0.0399(6) Uani 1 1 d . . . . .
O2 O 0.5202(2) 0.4371(2) 0.17313(12) 0.0343(6) Uani 1 1 d . . . . .
N1 N 0.4398(2) 0.6830(2) 0.22975(14) 0.0279(6) Uani 1 1 d . . . . .
C1 C 0.4553(3) 0.5323(3) 0.17155(17) 0.0314(8) Uani 1 1 d . . . . .
C2 C 0.7325(3) 0.3787(3) 0.20920(19) 0.0351(8) Uani 1 1 d . . . . .
H2A H 0.743467 0.350281 0.170207 0.042 Uiso 1 1 calc R . . . .
H2B H 0.802070 0.383614 0.215146 0.042 Uiso 1 1 calc R . . . .
C3 C 0.6658(3) 0.3433(3) 0.26567(19) 0.0337(8) Uani 1 1 d . . . . .
H3A H 0.693805 0.326047 0.306792 0.040 Uiso 1 1 calc R . . . .
H3B H 0.635209 0.292718 0.261858 0.040 Uiso 1 1 calc R . . . .
C4 C 0.6716(3) 0.5794(3) 0.26202(18) 0.0350(8) Uani 1 1 d . . . . .
H4A H 0.754093 0.537148 0.258987 0.042 Uiso 1 1 calc R . . . .
H4B H 0.653820 0.655954 0.248161 0.042 Uiso 1 1 calc R . . . .
C5 C 0.5994(3) 0.5477(3) 0.31800(17) 0.0323(8) Uani 1 1 d . . . . .
H5A H 0.536843 0.604743 0.338633 0.039 Uiso 1 1 calc R . . . .
H5B H 0.637155 0.485889 0.349464 0.039 Uiso 1 1 calc R . . . .
C6 C 0.4513(3) 0.7612(3) 0.17946(17) 0.0309(8) Uani 1 1 d . . . . .
C7 C 0.3630(3) 0.8581(3) 0.16935(18) 0.0326(8) Uani 1 1 d . . . . .
H7 H 0.373302 0.911170 0.133823 0.039 Uiso 1 1 calc R . . . .
C8 C 0.2605(3) 0.8768(3) 0.21103(18) 0.0342(8) Uani 1 1 d . . . . .
H8 H 0.198993 0.942226 0.204273 0.041 Uiso 1 1 calc R . . . .
C9 C 0.2487(3) 0.7988(3) 0.26277(18) 0.0310(8) Uani 1 1 d . . . . .
H9 H 0.178932 0.810341 0.292389 0.037 Uiso 1 1 calc R . . . .
C10 C 0.3386(3) 0.7040(3) 0.27132(17) 0.0288(8) Uani 1 1 d . . . . .
C11 C 0.3271(3) 0.6220(3) 0.33076(17) 0.0300(8) Uani 1 1 d . . . . .
H11A H 0.246383 0.629727 0.344143 0.036 Uiso 1 1 calc R . . . .
H11B H 0.350309 0.634262 0.366634 0.036 Uiso 1 1 calc R . . . .
C12 C 0.3159(3) 0.4399(3) 0.29964(16) 0.0281(7) Uani 1 1 d . . . . .
C13 C 0.1986(3) 0.4915(3) 0.30966(17) 0.0308(8) Uani 1 1 d . . . . .
H13 H 0.164983 0.552580 0.328750 0.037 Uiso 1 1 calc R . . . .
C14 C 0.1296(3) 0.4547(3) 0.29206(19) 0.0349(8) Uani 1 1 d . . . . .
H14 H 0.049442 0.490811 0.299115 0.042 Uiso 1 1 calc R . . . .
C15 C 0.1773(3) 0.3656(3) 0.26435(18) 0.0341(8) Uani 1 1 d . . . . .
H15 H 0.130188 0.341529 0.251504 0.041 Uiso 1 1 calc R . . . .
C16 C 0.2936(3) 0.3120(3) 0.25543(18) 0.0338(8) Uani 1 1 d . . . . .
H16 H 0.326362 0.249565 0.237683 0.041 Uiso 1 1 calc R . . . .
C17 C 0.3624(3) 0.3489(3) 0.27229(18) 0.0334(8) Uani 1 1 d . . . . .
H17 H 0.442446 0.312119 0.265255 0.040 Uiso 1 1 calc R . . . .
C18 C 0.4393(3) 0.4102(3) 0.39709(18) 0.0325(8) Uani 1 1 d . . . . .
C19 C 0.4193(3) 0.4540(3) 0.45113(19) 0.0382(9) Uani 1 1 d . . . . .
H19 H 0.387521 0.528308 0.447684 0.046 Uiso 1 1 calc R . . . .
C20 C 0.4455(3) 0.3900(4) 0.51015(19) 0.0405(9) Uani 1 1 d . . . . .
H20 H 0.431247 0.421253 0.546502 0.049 Uiso 1 1 calc R . . . .
C21 C 0.4919(3) 0.2820(3) 0.5165(2) 0.0419(10) Uani 1 1 d . . . . .
H21 H 0.509650 0.238713 0.556846 0.050 Uiso 1 1 calc R . . . .
C22 C 0.5121(3) 0.2377(3) 0.4629(2) 0.0393(9) Uani 1 1 d . . . . .
H22 H 0.543862 0.163422 0.466631 0.047 Uiso 1 1 calc R . . . .
C23 C 0.4866(3) 0.3007(3) 0.40424(19) 0.0358(9) Uani 1 1 d . . . . .
H23 H 0.501494 0.268942 0.368051 0.043 Uiso 1 1 calc R . . . .
C24 C 0.5641(3) 0.7428(3) 0.1350(2) 0.0373(9) Uani 1 1 d . . . . .
H24A H 0.607790 0.772011 0.149885 0.045 Uiso 1 1 calc R . . . .
H24B H 0.550662 0.782102 0.091060 0.045 Uiso 1 1 calc R . . . .
C25 C 0.6498(3) 0.5946(3) 0.04761(19) 0.0371(9) Uani 1 1 d . . . . .
C26 C 0.6289(4) 0.5140(4) 0.0350(2) 0.0445(10) Uani 1 1 d . . . . .
H26 H 0.613041 0.462122 0.069719 0.053 Uiso 1 1 calc R . . . .
C27 C 0.6313(4) 0.5093(4) -0.0287(2) 0.0507(11) Uani 1 1 d . . . . .
H27 H 0.615275 0.455237 -0.037025 0.061 Uiso 1 1 calc R . . . .
C28 C 0.6563(4) 0.5818(4) -0.0786(2) 0.0476(11) Uani 1 1 d . . . . .
H28 H 0.656329 0.578677 -0.121626 0.057 Uiso 1 1 calc R . . . .
C29 C 0.6815(4) 0.6593(4) -0.0678(2) 0.0502(11) Uani 1 1 d . . . . .
H29 H 0.701165 0.708347 -0.103121 0.060 Uiso 1 1 calc R . . . .
C30 C 0.6783(4) 0.6658(4) -0.0047(2) 0.0476(10) Uani 1 1 d . . . . .
H30 H 0.695863 0.719620 0.002719 0.057 Uiso 1 1 calc R . . . .
C31 C 0.7983(3) 0.5950(3) 0.11682(18) 0.0371(9) Uani 1 1 d . . . . .
C32 C 0.8837(4) 0.5064(4) 0.0952(2) 0.0497(11) Uani 1 1 d . . . . .
H32 H 0.863782 0.454915 0.086650 0.060 Uiso 1 1 calc R . . . .
C33 C 0.9968(4) 0.4918(5) 0.0859(3) 0.0641(14) Uani 1 1 d . . . . .
H33 H 1.053814 0.430429 0.071273 0.077 Uiso 1 1 calc R . . . .
C34 C 1.0272(4) 0.5652(5) 0.0976(3) 0.0685(16) Uani 1 1 d . . . . .
H34 H 1.105088 0.555442 0.090502 0.082 Uiso 1 1 calc R . . . .
C35 C 0.9458(5) 0.6520(5) 0.1193(3) 0.0684(15) Uani 1 1 d . . . . .
H35 H 0.966868 0.702906 0.127671 0.082 Uiso 1 1 calc R . . . .
C36 C 0.8311(4) 0.6667(4) 0.1295(2) 0.0553(12) Uani 1 1 d . . . . .
H36 H 0.774939 0.727289 0.145415 0.066 Uiso 1 1 calc R . . . .
Mo2 Mo -0.17955(2) 0.88700(2) 0.40753(2) 0.02493(9) Uani 1 1 d . . . . .
P3 P -0.19483(8) 0.86842(7) 0.30222(4) 0.0270(2) Uani 1 1 d . . . . .
P4 P -0.13643(8) 0.82804(7) 0.51721(4) 0.02604(19) Uani 1 1 d . . . . .
O3 O 0.0496(2) 0.6866(2) 0.38828(12) 0.0328(6) Uani 1 1 d . . . . .
O4 O 0.0007(2) 0.86528(19) 0.36306(11) 0.0294(5) Uani 1 1 d . . . . .
N2 N -0.1924(2) 0.7238(2) 0.43421(14) 0.0269(6) Uani 1 1 d . . . . .
C37 C -0.0140(3) 0.7784(3) 0.38444(16) 0.0261(7) Uani 1 1 d . . . . .
C38 C -0.1982(3) 1.0540(3) 0.36147(18) 0.0320(8) Uani 1 1 d . . . . .
H38A H -0.139991 1.063376 0.323397 0.038 Uiso 1 1 calc R . . . .
H38B H -0.276142 1.104514 0.356621 0.038 Uiso 1 1 calc R . . . .
C39 C -0.1683(3) 1.0327(3) 0.42252(17) 0.0304(8) Uani 1 1 d . . . . .
H39A H -0.227603 1.069911 0.455919 0.037 Uiso 1 1 calc R . . . .
H39B H -0.091420 1.028763 0.422687 0.037 Uiso 1 1 calc R . . . .
C40 C -0.3680(3) 0.9383(3) 0.40993(17) 0.0309(8) Uani 1 1 d . . . . .
H40A H -0.406881 1.010872 0.387791 0.037 Uiso 1 1 calc R . . . .
H40B H -0.393285 0.886213 0.402854 0.037 Uiso 1 1 calc R . . . .
C41 C -0.3504(3) 0.9271(3) 0.47339(17) 0.0294(8) Uani 1 1 d . . . . .
H41A H -0.364809 0.868113 0.505743 0.035 Uiso 1 1 calc R . . . .
H41B H -0.378400 0.992724 0.490686 0.035 Uiso 1 1 calc R . . . .
C42 C -0.1959(3) 0.6791(3) 0.38701(17) 0.0281(8) Uani 1 1 d . . . . .
C43 C -0.1739(3) 0.5730(3) 0.39649(18) 0.0310(8) Uani 1 1 d . . . . .
H43 H -0.177244 0.544106 0.362912 0.037 Uiso 1 1 calc R . . . .
C44 C -0.1469(3) 0.5086(3) 0.45461(18) 0.0327(8) Uani 1 1 d . . . . .
H44 H -0.130067 0.435242 0.461380 0.039 Uiso 1 1 calc R . . . .
C45 C -0.1451(3) 0.5540(3) 0.50257(18) 0.0302(8) Uani 1 1 d . . . . .
H45 H -0.127458 0.511930 0.543210 0.036 Uiso 1 1 calc R . . . .
C46 C -0.1690(3) 0.6612(3) 0.49139(16) 0.0259(7) Uani 1 1 d . . . . .
C47 C -0.1705(3) 0.7087(3) 0.54583(17) 0.0291(8) Uani 1 1 d . . . . .
H47A H -0.114835 0.655772 0.572970 0.035 Uiso 1 1 calc R . . . .
H47B H -0.246753 0.726274 0.573334 0.035 Uiso 1 1 calc R . . . .
C48 C 0.0058(3) 0.7816(3) 0.53811(17) 0.0272(7) Uani 1 1 d . . . . .
C49 C 0.0216(3) 0.7363(3) 0.60233(17) 0.0299(8) Uani 1 1 d . . . . .
H49 H -0.041527 0.731897 0.634866 0.036 Uiso 1 1 calc R . . . .
C50 C 0.1288(3) 0.6978(3) 0.61862(19) 0.0326(8) Uani 1 1 d . . . . .
H50 H 0.138987 0.667015 0.662130 0.039 Uiso 1 1 calc R . . . .
C51 C 0.2208(3) 0.7045(3) 0.57134(18) 0.0323(8) Uani 1 1 d . . . . .
H51 H 0.294277 0.677669 0.582329 0.039 Uiso 1 1 calc R . . . .
C52 C 0.2059(3) 0.7499(3) 0.50844(18) 0.0307(8) Uani 1 1 d . . . . .
H52 H 0.269327 0.754309 0.476177 0.037 Uiso 1 1 calc R . . . .
C53 C 0.0996(3) 0.7892(3) 0.49179(17) 0.0284(8) Uani 1 1 d . . . . .
H53 H 0.090266 0.821725 0.448346 0.034 Uiso 1 1 calc R . . . .
C54 C -0.2189(3) 0.9102(3) 0.57911(16) 0.0279(7) Uani 1 1 d . . . . .
C55 C -0.3214(3) 0.9075(3) 0.61745(17) 0.0307(8) Uani 1 1 d . . . . .
H55 H -0.348927 0.857099 0.614657 0.037 Uiso 1 1 calc R . . . .
C56 C -0.3839(3) 0.9778(3) 0.65971(18) 0.0347(9) Uani 1 1 d . . . . .
H56 H -0.453395 0.974922 0.685709 0.042 Uiso 1 1 calc R . . . .
C57 C -0.3448(3) 1.0519(3) 0.66397(19) 0.0383(9) Uani 1 1 d . . . . .
H57 H -0.388211 1.100933 0.692158 0.046 Uiso 1 1 calc R . . . .
C58 C -0.2427(3) 1.0542(3) 0.62709(19) 0.0385(9) Uani 1 1 d . . . . .
H58 H -0.214932 1.103920 0.630676 0.046 Uiso 1 1 calc R . . . .
C59 C -0.1805(3) 0.9845(3) 0.58483(17) 0.0318(8) Uani 1 1 d . . . . .
H59 H -0.110569 0.987426 0.559393 0.038 Uiso 1 1 calc R . . . .
C60 C -0.2302(3) 0.7495(3) 0.32471(17) 0.0292(8) Uani 1 1 d . . . . .
H60A H -0.313332 0.771598 0.328319 0.035 Uiso 1 1 calc R . . . .
H60B H -0.192692 0.708445 0.289364 0.035 Uiso 1 1 calc R . . . .
C61 C -0.0690(3) 0.8374(3) 0.23838(17) 0.0290(8) Uani 1 1 d . . . . .
C62 C 0.0123(3) 0.7359(3) 0.24083(18) 0.0333(8) Uani 1 1 d . . . . .
H62 H 0.001407 0.681574 0.275252 0.040 Uiso 1 1 calc R . . . .
C63 C 0.1096(3) 0.7126(3) 0.19354(18) 0.0341(8) Uani 1 1 d . . . . .
H63 H 0.164478 0.642810 0.195858 0.041 Uiso 1 1 calc R . . . .
C64 C 0.1264(3) 0.7906(3) 0.14348(19) 0.0386(9) Uani 1 1 d . . . . .
H64 H 0.192324 0.774505 0.110947 0.046 Uiso 1 1 calc R . . . .
C65 C 0.0475(3) 0.8919(3) 0.1406(2) 0.0432(10) Uani 1 1 d . . . . .
H65 H 0.059397 0.945742 0.106090 0.052 Uiso 1 1 calc R . . . .
C66 C -0.0495(3) 0.9159(3) 0.18771(19) 0.0384(9) Uani 1 1 d . . . . .
H66 H -0.103016 0.986219 0.185518 0.046 Uiso 1 1 calc R . . . .
C67 C -0.3023(3) 0.9601(3) 0.25233(17) 0.0297(8) Uani 1 1 d . . . . .
C68 C -0.3230(3) 1.0675(3) 0.23890(17) 0.0326(8) Uani 1 1 d . . . . .
H68 H -0.284869 1.093076 0.258002 0.039 Uiso 1 1 calc R . . . .
C69 C -0.3981(3) 1.1375(3) 0.19823(18) 0.0349(9) Uani 1 1 d . . . . .
H69 H -0.411154 1.210294 0.189567 0.042 Uiso 1 1 calc R . . . .
C70 C -0.4542(3) 1.1011(3) 0.17018(18) 0.0376(9) Uani 1 1 d . . . . .
H70 H -0.505523 1.148767 0.142085 0.045 Uiso 1 1 calc R . . . .
C71 C -0.4352(3) 0.9953(3) 0.18324(18) 0.0369(9) Uani 1 1 d . . . . .
H71 H -0.474618 0.970418 0.164613 0.044 Uiso 1 1 calc R . . . .
C72 C -0.3592(3) 0.9251(3) 0.22329(17) 0.0328(8) Uani 1 1 d . . . . .
H72 H -0.345589 0.852221 0.231097 0.039 Uiso 1 1 calc R . . . .
C73 C 0.9731(6) 0.2020(5) 0.0854(3) 0.0858(19) Uani 1 1 d . . . . .
H73A H 0.895045 0.205936 0.103334 0.129 Uiso 1 1 calc GR . . . .
H73B H 1.011956 0.145980 0.059742 0.129 Uiso 1 1 calc GR . . . .
H73C H 0.971694 0.269345 0.057804 0.129 Uiso 1 1 calc GR . . . .
C74 C 1.0351(5) 0.1787(4) 0.1396(3) 0.0606(13) Uani 1 1 d . . . . .
C75 C 0.9831(4) 0.1648(4) 0.2026(3) 0.0558(12) Uani 1 1 d . . . . .
H75 H 0.906750 0.168795 0.212001 0.067 Uiso 1 1 calc R . . . .
C76 C 1.0380(4) 0.1453(4) 0.2525(3) 0.0598(13) Uani 1 1 d . . . . .
H76 H 0.998277 0.136872 0.295702 0.072 Uiso 1 1 calc R . . . .
C77 C 1.1470(4) 0.1377(4) 0.2426(3) 0.0584(13) Uani 1 1 d . . . . .
H77 H 1.182725 0.126526 0.277911 0.070 Uiso 1 1 calc R . . . .
C78 C 1.2029(4) 0.1464(4) 0.1817(3) 0.0576(12) Uani 1 1 d . . . . .
H78 H 1.280146 0.138917 0.174420 0.069 Uiso 1 1 calc R . . . .
C79 C 1.1523(5) 0.1660(4) 0.1286(3) 0.0682(15) Uani 1 1 d . . . . .
H79 H 1.194609 0.170894 0.085901 0.082 Uiso 1 1 calc R . . . .
C80 C -0.3350(8) 1.2413(6) 0.0169(4) 0.119(2) Uani 1 1 d . U . . .
H80A H -0.403390 1.267819 0.048743 0.179 Uiso 1 1 calc GR . . . .
H80B H -0.349928 1.278607 -0.026704 0.179 Uiso 1 1 calc GR . . . .
H80C H -0.272342 1.252941 0.025694 0.179 Uiso 1 1 calc GR . . . .
C81 C -0.3041(6) 1.1283(6) 0.0211(3) 0.0861(14) Uani 1 1 d . U . . .
C82 C -0.3798(6) 1.0921(6) 0.0058(3) 0.0936(17) Uani 1 1 d . U . . .
H82 H -0.450094 1.139949 -0.006900 0.112 Uiso 1 1 calc R . . . .
C83 C -0.3461(6) 0.9839(6) 0.0105(3) 0.0959(17) Uani 1 1 d . U . . .
H83 H -0.393245 0.959218 -0.001880 0.115 Uiso 1 1 calc R . . . .
C84 C -0.2510(6) 0.9131(6) 0.0313(3) 0.0899(17) Uani 1 1 d . U . . .
H84 H -0.231672 0.840070 0.034183 0.108 Uiso 1 1 calc R . . . .
C85 C -0.1824(6) 0.9481(6) 0.0484(3) 0.0872(16) Uani 1 1 d . U . . .
H85 H -0.116105 0.898503 0.064828 0.105 Uiso 1 1 calc R . . . .
C86 C -0.2071(6) 1.0536(5) 0.0423(3) 0.0832(15) Uani 1 1 d . U . . .
H86 H -0.155792 1.075321 0.052930 0.100 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 P1 2.4423(10) . ?
Mo1 P2 2.4553(10) . ?
Mo1 O2 2.215(3) . ?
Mo1 N1 2.290(3) . ?
Mo1 C1 2.107(4) . ?
Mo1 C2 2.247(4) . ?
Mo1 C3 2.246(4) . ?
Mo1 C4 2.255(4) . ?
Mo1 C5 2.262(3) . ?
P1 C24 1.848(4) . ?
P1 C25 1.842(4) . ?
P1 C31 1.834(4) . ?
P2 C11 1.834(4) . ?
P2 C12 1.841(4) . ?
P2 C18 1.834(4) . ?
O1 C1 1.213(4) . ?
O2 C1 1.261(4) . ?
N1 C6 1.361(5) . ?
N1 C10 1.363(5) . ?
C2 C3 1.414(5) . ?
C4 C5 1.428(5) . ?
C6 C7 1.390(5) . ?
C6 C24 1.503(5) . ?
C7 C8 1.376(5) . ?
C8 C9 1.379(5) . ?
C9 C10 1.378(5) . ?
C10 C11 1.512(5) . ?
C12 C13 1.389(5) . ?
C12 C17 1.404(5) . ?
C13 C14 1.392(5) . ?
C14 C15 1.383(5) . ?
C15 C16 1.381(5) . ?
C16 C17 1.383(5) . ?
C18 C19 1.394(5) . ?
C18 C23 1.397(5) . ?
C19 C20 1.393(6) . ?
C20 C21 1.379(6) . ?
C21 C22 1.389(6) . ?
C22 C23 1.381(5) . ?
C25 C26 1.395(6) . ?
C25 C30 1.390(6) . ?
C26 C27 1.400(6) . ?
C27 C28 1.357(6) . ?
C28 C29 1.369(6) . ?
C29 C30 1.391(6) . ?
C31 C32 1.390(6) . ?
C31 C36 1.375(6) . ?
C32 C33 1.379(6) . ?
C33 C34 1.366(8) . ?
C34 C35 1.356(8) . ?
C35 C36 1.397(7) . ?
Mo2 P3 2.4493(9) . ?
Mo2 P4 2.4445(9) . ?
Mo2 O4 2.233(2) . ?
Mo2 N2 2.304(3) . ?
Mo2 C37 2.100(3) . ?
Mo2 C38 2.251(4) . ?
Mo2 C39 2.255(3) . ?
Mo2 C40 2.263(3) . ?
Mo2 C41 2.257(3) . ?
P3 C60 1.847(4) . ?
P3 C61 1.836(4) . ?
P3 C67 1.840(4) . ?
P4 C47 1.842(4) . ?
P4 C48 1.844(4) . ?
P4 C54 1.839(3) . ?
O3 C37 1.216(4) . ?
O4 C37 1.274(4) . ?
N2 C42 1.368(4) . ?
N2 C46 1.347(4) . ?
C38 C39 1.406(5) . ?
C40 C41 1.419(5) . ?
C42 C43 1.381(5) . ?
C42 C60 1.504(5) . ?
C43 C44 1.381(5) . ?
C44 C45 1.380(5) . ?
C45 C46 1.387(5) . ?
C46 C47 1.509(5) . ?
C48 C49 1.404(5) . ?
C48 C53 1.394(5) . ?
C49 C50 1.389(5) . ?
C50 C51 1.384(5) . ?
C51 C52 1.375(5) . ?
C52 C53 1.380(5) . ?
C54 C55 1.396(5) . ?
C54 C59 1.394(5) . ?
C55 C56 1.391(5) . ?
C56 C57 1.386(6) . ?
C57 C58 1.378(6) . ?
C58 C59 1.385(5) . ?
C61 C62 1.389(5) . ?
C61 C66 1.398(5) . ?
C62 C63 1.393(5) . ?
C63 C64 1.375(6) . ?
C64 C65 1.377(6) . ?
C65 C66 1.389(6) . ?
C67 C68 1.396(5) . ?
C67 C72 1.395(5) . ?
C68 C69 1.385(5) . ?
C69 C70 1.385(6) . ?
C70 C71 1.380(6) . ?
C71 C72 1.384(5) . ?
C73 C74 1.497(8) . ?
C74 C75 1.364(7) . ?
C74 C79 1.436(8) . ?
C75 C76 1.368(7) . ?
C76 C77 1.353(7) . ?
C77 C78 1.335(7) . ?
C78 C79 1.393(8) . ?
C80 C81 1.467(10) . ?
C81 C82 1.439(10) . ?
C81 C86 1.373(9) . ?
C82 C83 1.396(10) . ?
C83 C84 1.336(9) . ?
C84 C85 1.363(9) . ?
C85 C86 1.373(9) . ?

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
P1 Mo1 P2 155.42(3) . . ?
O2 Mo1 P1 89.70(7) . . ?
O2 Mo1 P2 86.66(7) . . ?
O2 Mo1 N1 109.01(10) . . ?
O2 Mo1 C2 78.56(12) . . ?
O2 Mo1 C3 78.55(12) . . ?
O2 Mo1 C4 160.18(12) . . ?
O2 Mo1 C5 158.71(12) . . ?
N1 Mo1 P1 79.80(8) . . ?
N1 Mo1 P2 78.46(8) . . ?
C1 Mo1 P1 81.81(10) . . ?
C1 Mo1 P2 81.71(10) . . ?
C1 Mo1 O2 33.80(12) . . ?
C1 Mo1 N1 75.27(12) . . ?
C1 Mo1 C2 109.80(14) . . ?
C1 Mo1 C3 111.22(14) . . ?
C1 Mo1 C4 149.74(14) . . ?
C1 Mo1 C5 149.56(14) . . ?
C2 Mo1 P1 81.89(10) . . ?
C2 Mo1 P2 120.97(10) . . ?
C2 Mo1 N1 160.08(13) . . ?
C2 Mo1 C4 86.46(14) . . ?
C2 Mo1 C5 99.49(14) . . ?
C3 Mo1 P1 118.54(10) . . ?
C3 Mo1 P2 84.51(10) . . ?
C3 Mo1 N1 160.78(12) . . ?
C3 Mo1 C2 36.69(14) . . ?
C3 Mo1 C4 97.12(14) . . ?
C3 Mo1 C5 87.31(14) . . ?
C4 Mo1 P1 75.28(10) . . ?
C4 Mo1 P2 112.36(10) . . ?
C4 Mo1 N1 81.38(12) . . ?
C4 Mo1 C5 36.86(14) . . ?
C5 Mo1 P1 111.15(10) . . ?
C5 Mo1 P2 76.12(10) . . ?
C5 Mo1 N1 80.03(12) . . ?
C24 P1 Mo1 101.42(13) . . ?
C25 P1 Mo1 125.71(13) . . ?
C25 P1 C24 103.52(19) . . ?
C31 P1 Mo1 121.32(13) . . ?
C31 P1 C24 104.28(19) . . ?
C31 P1 C25 97.80(17) . . ?
C11 P2 Mo1 102.14(12) . . ?
C11 P2 C12 105.31(17) . . ?
C12 P2 Mo1 119.31(12) . . ?
C18 P2 Mo1 122.16(12) . . ?
C18 P2 C11 104.48(17) . . ?
C18 P2 C12 101.52(16) . . ?
C1 O2 Mo1 68.4(2) . . ?
C6 N1 Mo1 120.3(2) . . ?
C6 N1 C10 117.4(3) . . ?
C10 N1 Mo1 120.8(2) . . ?
O1 C1 Mo1 146.7(3) . . ?
O1 C1 O2 135.4(4) . . ?
O2 C1 Mo1 77.8(2) . . ?
C3 C2 Mo1 71.6(2) . . ?
C2 C3 Mo1 71.7(2) . . ?
C5 C4 Mo1 71.8(2) . . ?
C4 C5 Mo1 71.3(2) . . ?
N1 C6 C7 122.0(3) . . ?
N1 C6 C24 118.7(3) . . ?
C7 C6 C24 119.3(3) . . ?
C8 C7 C6 119.7(4) . . ?
C7 C8 C9 118.8(3) . . ?
C10 C9 C8 119.7(3) . . ?
N1 C10 C9 122.4(3) . . ?
N1 C10 C11 118.4(3) . . ?
C9 C10 C11 119.1(3) . . ?
C10 C11 P2 112.3(2) . . ?
C13 C12 P2 123.7(3) . . ?
C13 C12 C17 118.0(3) . . ?
C17 C12 P2 118.2(3) . . ?
C12 C13 C14 120.8(3) . . ?
C15 C14 C13 120.2(4) . . ?
C16 C15 C14 119.7(4) . . ?
C15 C16 C17 120.1(3) . . ?
C16 C17 C12 121.1(3) . . ?
C19 C18 P2 123.9(3) . . ?
C19 C18 C23 117.8(4) . . ?
C23 C18 P2 118.2(3) . . ?
C20 C19 C18 120.7(4) . . ?
C21 C20 C19 120.9(4) . . ?
C20 C21 C22 118.8(4) . . ?
C23 C22 C21 120.6(4) . . ?
C22 C23 C18 121.2(4) . . ?
C6 C24 P1 114.7(3) . . ?
C26 C25 P1 122.2(3) . . ?
C30 C25 P1 119.5(3) . . ?
C30 C25 C26 118.2(4) . . ?
C25 C26 C27 120.1(4) . . ?
C28 C27 C26 120.3(4) . . ?
C27 C28 C29 120.8(4) . . ?
C28 C29 C30 119.7(4) . . ?
C25 C30 C29 120.9(4) . . ?
C32 C31 P1 117.2(3) . . ?
C36 C31 P1 125.3(3) . . ?
C36 C31 C32 117.4(4) . . ?
C33 C32 C31 121.3(5) . . ?
C34 C33 C32 120.2(5) . . ?
C35 C34 C33 119.8(5) . . ?
C34 C35 C36 120.2(5) . . ?
C31 C36 C35 121.0(5) . . ?
P4 Mo2 P3 156.60(3) . . ?
O4 Mo2 P3 85.18(6) . . ?
O4 Mo2 P4 92.50(7) . . ?
O4 Mo2 N2 107.63(10) . . ?
O4 Mo2 C38 79.24(12) . . ?
O4 Mo2 C39 78.22(11) . . ?
O4 Mo2 C40 156.56(11) . . ?
O4 Mo2 C41 163.30(11) . . ?
N2 Mo2 P3 79.73(7) . . ?
N2 Mo2 P4 78.81(7) . . ?
C37 Mo2 P3 82.05(9) . . ?
C37 Mo2 P4 83.08(9) . . ?
C37 Mo2 O4 34.03(11) . . ?
C37 Mo2 N2 73.74(12) . . ?
C37 Mo2 C38 112.77(14) . . ?
C37 Mo2 C39 108.53(13) . . ?
C37 Mo2 C40 148.39(13) . . ?
C37 Mo2 C41 149.30(13) . . ?
C38 Mo2 P3 86.40(10) . . ?
C38 Mo2 P4 116.10(10) . . ?
C38 Mo2 N2 163.80(12) . . ?
C38 Mo2 C39 36.36(13) . . ?
C38 Mo2 C40 87.28(14) . . ?
C38 Mo2 C41 96.23(14) . . ?
C39 Mo2 P3 122.20(10) . . ?
C39 Mo2 P4 79.78(9) . . ?
C39 Mo2 N2 158.00(12) . . ?
C39 Mo2 C40 102.01(13) . . ?
C39 Mo2 C41 88.60(13) . . ?
C40 Mo2 P3 74.83(9) . . ?
C40 Mo2 P4 110.71(9) . . ?
C40 Mo2 N2 81.08(12) . . ?
C41 Mo2 P3 110.74(9) . . ?
C41 Mo2 P4 74.93(9) . . ?
C41 Mo2 N2 81.08(12) . . ?
C41 Mo2 C40 36.59(13) . . ?
C60 P3 Mo2 101.32(11) . . ?
C61 P3 Mo2 120.34(12) . . ?
C61 P3 C60 104.06(16) . . ?
C61 P3 C67 99.47(16) . . ?
C67 P3 Mo2 126.28(11) . . ?
C67 P3 C60 102.14(17) . . ?
C47 P4 Mo2 102.61(12) . . ?
C47 P4 C48 101.97(16) . . ?
C48 P4 Mo2 125.48(12) . . ?
C54 P4 Mo2 120.07(11) . . ?
C54 P4 C47 104.97(16) . . ?
C54 P4 C48 98.98(16) . . ?
C37 O4 Mo2 67.24(18) . . ?
C42 N2 Mo2 119.8(2) . . ?
C46 N2 Mo2 120.5(2) . . ?
C46 N2 C42 117.8(3) . . ?
O3 C37 Mo2 147.2(3) . . ?
O3 C37 O4 133.9(3) . . ?
O4 C37 Mo2 78.73(19) . . ?
C39 C38 Mo2 72.0(2) . . ?
C38 C39 Mo2 71.7(2) . . ?
C41 C40 Mo2 71.45(19) . . ?
C40 C41 Mo2 71.95(19) . . ?
N2 C42 C43 121.7(3) . . ?
N2 C42 C60 118.3(3) . . ?
C43 C42 C60 119.9(3) . . ?
C42 C43 C44 120.2(3) . . ?
C45 C44 C43 118.0(3) . . ?
C44 C45 C46 120.0(3) . . ?
N2 C46 C45 122.2(3) . . ?
N2 C46 C47 119.4(3) . . ?
C45 C46 C47 118.4(3) . . ?
C46 C47 P4 113.1(2) . . ?
C49 C48 P4 119.6(3) . . ?
C53 C48 P4 122.0(3) . . ?
C53 C48 C49 118.4(3) . . ?
C50 C49 C48 120.4(3) . . ?
C51 C50 C49 119.9(4) . . ?
C52 C51 C50 120.1(3) . . ?
C51 C52 C53 120.6(3) . . ?
C52 C53 C48 120.6(3) . . ?
C55 C54 P4 123.8(3) . . ?
C59 C54 P4 117.9(3) . . ?
C59 C54 C55 118.2(3) . . ?
C56 C55 C54 120.7(3) . . ?
C57 C56 C55 120.1(4) . . ?
C58 C57 C56 119.6(3) . . ?
C57 C58 C59 120.4(4) . . ?
C58 C59 C54 120.9(3) . . ?
C42 C60 P3 114.7(2) . . ?
C62 C61 P3 120.7(3) . . ?
C62 C61 C66 118.2(3) . . ?
C66 C61 P3 121.0(3) . . ?
C61 C62 C63 120.9(4) . . ?
C64 C63 C62 120.0(4) . . ?
C63 C64 C65 119.9(4) . . ?
C64 C65 C66 120.4(4) . . ?
C65 C66 C61 120.5(4) . . ?
C68 C67 P3 119.9(3) . . ?
C72 C67 P3 121.9(3) . . ?
C72 C67 C68 118.0(3) . . ?
C69 C68 C67 121.1(4) . . ?
C68 C69 C70 119.9(4) . . ?
C71 C70 C69 119.7(4) . . ?
C70 C71 C72 120.5(4) . . ?
C71 C72 C67 120.7(4) . . ?
C75 C74 C73 121.0(5) . . ?
C75 C74 C79 116.4(5) . . ?
C79 C74 C73 122.5(5) . . ?
C74 C75 C76 121.7(5) . . ?
C77 C76 C75 122.3(6) . . ?
C78 C77 C76 118.2(5) . . ?
C77 C78 C79 122.6(5) . . ?
C78 C79 C74 118.8(5) . . ?
C82 C81 C80 119.8(7) . . ?
C86 C81 C80 122.6(8) . . ?
C86 C81 C82 117.5(7) . . ?
C83 C82 C81 117.5(7) . . ?
C84 C83 C82 123.5(8) . . ?
C83 C84 C85 118.5(8) . . ?
C84 C85 C86 121.4(7) . . ?
C85 C86 C81 121.5(7) . . ?

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 P1 C24 C6 -21.0(3) . . . . ?
Mo1 P1 C25 C26 -18.3(4) . . . . ?
Mo1 P1 C25 C30 166.6(3) . . . . ?
Mo1 P1 C31 C32 82.4(3) . . . . ?
Mo1 P1 C31 C36 -94.2(4) . . . . ?
Mo1 P2 C11 C10 27.1(3) . . . . ?
Mo1 P2 C12 C13 -125.3(3) . . . . ?
Mo1 P2 C12 C17 51.7(3) . . . . ?
Mo1 P2 C18 C19 100.5(3) . . . . ?
Mo1 P2 C18 C23 -76.3(3) . . . . ?
Mo1 O2 C1 O1 177.8(5) . . . . ?
Mo1 N1 C6 C7 164.6(3) . . . . ?
Mo1 N1 C6 C24 -17.4(4) . . . . ?
Mo1 N1 C10 C9 -164.1(3) . . . . ?
Mo1 N1 C10 C11 19.1(4) . . . . ?
P1 C25 C26 C27 -178.5(3) . . . . ?
P1 C25 C30 C29 177.9(4) . . . . ?
P1 C31 C32 C33 -177.9(4) . . . . ?
P1 C31 C36 C35 178.2(4) . . . . ?
P2 C12 C13 C14 175.9(3) . . . . ?
P2 C12 C17 C16 -176.7(3) . . . . ?
P2 C18 C19 C20 -177.0(3) . . . . ?
P2 C18 C23 C22 177.4(3) . . . . ?
N1 C6 C7 C8 0.1(6) . . . . ?
N1 C6 C24 P1 26.4(5) . . . . ?
N1 C10 C11 P2 -31.8(4) . . . . ?
C6 N1 C10 C9 2.0(5) . . . . ?
C6 N1 C10 C11 -174.8(3) . . . . ?
C6 C7 C8 C9 1.1(5) . . . . ?
C7 C6 C24 P1 -155.5(3) . . . . ?
C7 C8 C9 C10 -0.7(5) . . . . ?
C8 C9 C10 N1 -0.9(5) . . . . ?
C8 C9 C10 C11 175.8(3) . . . . ?
C9 C10 C11 P2 151.3(3) . . . . ?
C10 N1 C6 C7 -1.6(5) . . . . ?
C10 N1 C6 C24 176.4(3) . . . . ?
C11 P2 C12 C13 -11.5(3) . . . . ?
C11 P2 C12 C17 165.5(3) . . . . ?
C11 P2 C18 C19 -14.3(4) . . . . ?
C11 P2 C18 C23 169.0(3) . . . . ?
C12 P2 C11 C10 -98.2(3) . . . . ?
C12 P2 C18 C19 -123.6(3) . . . . ?
C12 P2 C18 C23 59.6(3) . . . . ?
C12 C13 C14 C15 0.1(6) . . . . ?
C13 C12 C17 C16 0.4(5) . . . . ?
C13 C14 C15 C16 1.4(6) . . . . ?
C14 C15 C16 C17 -2.0(6) . . . . ?
C15 C16 C17 C12 1.1(6) . . . . ?
C17 C12 C13 C14 -1.0(5) . . . . ?
C18 P2 C11 C10 155.3(3) . . . . ?
C18 P2 C12 C13 97.2(3) . . . . ?
C18 P2 C12 C17 -85.8(3) . . . . ?
C18 C19 C20 C21 0.1(6) . . . . ?
C19 C18 C23 C22 0.4(6) . . . . ?
C19 C20 C21 C22 0.0(6) . . . . ?
C20 C21 C22 C23 0.2(6) . . . . ?
C21 C22 C23 C18 -0.4(6) . . . . ?
C23 C18 C19 C20 -0.3(6) . . . . ?
C24 P1 C25 C26 -133.4(4) . . . . ?
C24 P1 C25 C30 51.5(4) . . . . ?
C24 P1 C31 C32 -164.3(3) . . . . ?
C24 P1 C31 C36 19.0(4) . . . . ?
C24 C6 C7 C8 -177.9(3) . . . . ?
C25 P1 C24 C6 110.4(3) . . . . ?
C25 P1 C31 C32 -58.2(4) . . . . ?
C25 P1 C31 C36 125.2(4) . . . . ?
C25 C26 C27 C28 1.5(7) . . . . ?
C26 C25 C30 C29 2.5(7) . . . . ?
C26 C27 C28 C29 1.1(7) . . . . ?
C27 C28 C29 C30 -1.9(7) . . . . ?
C28 C29 C30 C25 0.0(7) . . . . ?
C30 C25 C26 C27 -3.2(6) . . . . ?
C31 P1 C24 C6 -147.7(3) . . . . ?
C31 P1 C25 C26 119.8(4) . . . . ?
C31 P1 C25 C30 -55.3(4) . . . . ?
C31 C32 C33 C34 -0.3(8) . . . . ?
C32 C31 C36 C35 1.6(7) . . . . ?
C32 C33 C34 C35 1.0(9) . . . . ?
C33 C34 C35 C36 -0.3(9) . . . . ?
C34 C35 C36 C31 -1.0(8) . . . . ?
C36 C31 C32 C33 -0.9(7) . . . . ?
Mo2 P3 C60 C42 -22.5(3) . . . . ?
Mo2 P3 C61 C62 76.5(3) . . . . ?
Mo2 P3 C61 C66 -100.4(3) . . . . ?
Mo2 P3 C67 C68 50.0(3) . . . . ?
Mo2 P3 C67 C72 -134.5(3) . . . . ?
Mo2 P4 C47 C46 21.7(3) . . . . ?
Mo2 P4 C48 C49 -171.2(2) . . . . ?
Mo2 P4 C48 C53 8.3(3) . . . . ?
Mo2 P4 C54 C55 86.1(3) . . . . ?
Mo2 P4 C54 C59 -89.3(3) . . . . ?
Mo2 O4 C37 O3 -176.3(5) . . . . ?
Mo2 N2 C42 C43 162.8(3) . . . . ?
Mo2 N2 C42 C60 -20.1(4) . . . . ?
Mo2 N2 C46 C45 -161.9(3) . . . . ?
Mo2 N2 C46 C47 19.1(4) . . . . ?
P3 C61 C62 C63 -178.1(3) . . . . ?
P3 C61 C66 C65 178.4(3) . . . . ?
P3 C67 C68 C69 175.9(3) . . . . ?
P3 C67 C72 C71 -176.6(3) . . . . ?
P4 C48 C49 C50 177.9(3) . . . . ?
P4 C48 C53 C52 -177.4(3) . . . . ?
P4 C54 C55 C56 -174.8(3) . . . . ?
P4 C54 C59 C58 175.3(3) . . . . ?
N2 C42 C43 C44 -0.3(5) . . . . ?
N2 C42 C60 P3 29.3(4) . . . . ?
N2 C46 C47 P4 -27.9(4) . . . . ?
C42 N2 C46 C45 2.2(5) . . . . ?
C42 N2 C46 C47 -176.8(3) . . . . ?
C42 C43 C44 C45 1.3(5) . . . . ?
C43 C42 C60 P3 -153.6(3) . . . . ?
C43 C44 C45 C46 -0.5(5) . . . . ?
C44 C45 C46 N2 -1.2(5) . . . . ?
C44 C45 C46 C47 177.7(3) . . . . ?
C45 C46 C47 P4 153.1(3) . . . . ?
C46 N2 C42 C43 -1.4(5) . . . . ?
C46 N2 C42 C60 175.6(3) . . . . ?
C47 P4 C48 C49 -56.0(3) . . . . ?
C47 P4 C48 C53 123.4(3) . . . . ?
C47 P4 C54 C55 -28.5(3) . . . . ?
C47 P4 C54 C59 156.1(3) . . . . ?
C48 P4 C47 C46 -109.2(3) . . . . ?
C48 P4 C54 C55 -133.5(3) . . . . ?
C48 P4 C54 C59 51.0(3) . . . . ?
C48 C49 C50 C51 0.2(5) . . . . ?
C49 C48 C53 C52 2.1(5) . . . . ?
C49 C50 C51 C52 0.6(5) . . . . ?
C50 C51 C52 C53 0.0(5) . . . . ?
C51 C52 C53 C48 -1.3(5) . . . . ?
C53 C48 C49 C50 -1.5(5) . . . . ?
C54 P4 C47 C46 148.0(2) . . . . ?
C54 P4 C48 C49 51.5(3) . . . . ?
C54 P4 C48 C53 -129.1(3) . . . . ?
C54 C55 C56 C57 0.3(6) . . . . ?
C55 C54 C59 C58 -0.4(5) . . . . ?
C55 C56 C57 C58 -1.3(6) . . . . ?
C56 C57 C58 C59 1.5(6) . . . . ?
C57 C58 C59 C54 -0.6(6) . . . . ?
C59 C54 C55 C56 0.6(5) . . . . ?
C60 P3 C61 C62 -35.9(3) . . . . ?
C60 P3 C61 C66 147.2(3) . . . . ?
C60 P3 C67 C68 164.1(3) . . . . ?
C60 P3 C67 C72 -20.5(3) . . . . ?
C60 C42 C43 C44 -177.3(3) . . . . ?
C61 P3 C60 C42 103.1(3) . . . . ?
C61 P3 C67 C68 -89.2(3) . . . . ?
C61 P3 C67 C72 86.3(3) . . . . ?
C61 C62 C63 C64 0.0(6) . . . . ?
C62 C61 C66 C65 1.4(6) . . . . ?
C62 C63 C64 C65 0.7(6) . . . . ?
C63 C64 C65 C66 -0.4(6) . . . . ?
C64 C65 C66 C61 -0.7(6) . . . . ?
C66 C61 C62 C63 -1.1(5) . . . . ?
C67 P3 C60 C42 -153.8(3) . . . . ?
C67 P3 C61 C62 -141.1(3) . . . . ?
C67 P3 C61 C66 42.0(3) . . . . ?
C67 C68 C69 C70 0.1(5) . . . . ?
C68 C67 C72 C71 -1.0(5) . . . . ?
C68 C69 C70 C71 0.3(6) . . . . ?
C69 C70 C71 C72 -1.1(6) . . . . ?
C70 C71 C72 C67 1.4(6) . . . . ?
C72 C67 C68 C69 0.3(5) . . . . ?
C73 C74 C75 C76 -178.8(5) . . . . ?
C73 C74 C79 C78 178.8(5) . . . . ?
C74 C75 C76 C77 -0.6(8) . . . . ?
C75 C74 C79 C78 -3.4(7) . . . . ?
C75 C76 C77 C78 -2.1(8) . . . . ?
C76 C77 C78 C79 2.0(8) . . . . ?
C77 C78 C79 C74 0.8(8) . . . . ?
C79 C74 C75 C76 3.4(7) . . . . ?
C80 C81 C82 C83 179.8(6) . . . . ?
C80 C81 C86 C85 177.3(6) . . . . ?
C81 C82 C83 C84 3.6(10) . . . . ?
C82 C81 C86 C85 0.4(9) . . . . ?
C82 C83 C84 C85 -0.7(11) . . . . ?
C83 C84 C85 C86 -2.4(11) . . . . ?
C84 C85 C86 C81 2.6(11) . . . . ?
C86 C81 C82 C83 -3.2(9) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a 100 micro/m MITEGEN holder in perfluoroether oil'
_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_compound_2b
_database_code_depnum_ccdc_archive 'CCDC 1911733'
loop_
_audit_author_name
_audit_author_address
'Francisco Molina Gonzalez'
;CIQSO
Spain
;
_audit_update_record             
;
2019-04-23 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2018-04-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C35 H31 N O2 P2 W, 2(C4 H8 O)'
_chemical_formula_sum            'C43 H47 N O4 P2 W'
_chemical_properties_physical    
'air-sensitive, moisture-sensitive,Air-sensitive,Moisture-sensitive'
_chemical_formula_weight         887.60
_exptl_crystal_recrystallization_method 
'Crystallised from a mixture of THF and hexane by cooling'
_chemical_melting_point          ?
_exptl_crystal_description       plate
_exptl_crystal_colour            red
_diffrn_ambient_temperature      100.0
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration .
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1247(5)
_cell_length_b                   11.9967(6)
_cell_length_c                   14.6407(7)
_cell_angle_alpha                100.370(2)
_cell_angle_beta                 100.905(2)
_cell_angle_gamma                90.773(2)
_cell_volume                     1885.03(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      33.06
_cell_measurement_theta_min      2.45
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.193
_exptl_absorpt_correction_T_max  0.0432
_exptl_absorpt_correction_T_min  0.0090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1115 before and 0.0798 after correction. 
The Ratio of minimum to maximum transmission is 0.2083. 
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             896
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            180254
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.448
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Quest'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed x-ray tube'
_diffrn_source_type              'Incoatec I/mS high brilliance'
_diffrn_special_details          ?
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7970
_reflns_number_total             8652
_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       'Bruker Apex3, 2017'
_computing_data_collection       'Bruker Apex3, 2017'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.988
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8652
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0238
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0222P)²+2.0782P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0577
_refine_special_details          
;
A THF solvent molecule shows positional disorder and 
was refined in two opposites (180 turn) conformations. 
They showed to be equally divided to 50% (SOF of main component: 0.500(2)).
Restraints (SADI, SIMU, RIGU) are a applied in order to enhance the THF models.

All H atoms were refined using a riding model, with a common U restrained
to be 1.2  times the equivalent isotropic displacement
parameter of the parent atom. 

Refinement of F² against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C43-C42 \\sim C42-C41 \\sim C41-C40
 with sigma of 0.02
 O4-C43 \\sim O4-C40
 with sigma of 0.02
 O4-C42 \\sim O4-C41
 with sigma of 0.04
 C42-C40 \\sim C43-C41
 with sigma of 0.04
 C44-C45 \\sim C45-C46 \\sim C46-C47
 with sigma of 0.02
 O5-C44 \\sim O5-C47
 with sigma of 0.02
 O5-C45 \\sim O5-C46
 with sigma of 0.04
 C45-C47 \\sim C44-C46
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O4 \\sim C40 \\sim C41 \\sim C42 \\sim C43: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O5 \\sim C44 \\sim C45 \\sim C46 \\sim C47: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O4, C40, C41, C42, C43
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, C44, C45, C46, C47
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O5)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=1-FVAR(1)
 Sof(O4)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C23(H23A,H23B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
  C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
W1 W 0.34594(2) 0.63778(2) 0.27018(2) 0.03104(4) Uani 1 1 d . . . . .
P1 P 0.50111(6) 0.50380(6) 0.23853(5) 0.03291(14) Uani 1 1 d . . . . .
P2 P 0.26475(6) 0.78545(6) 0.37468(5) 0.03143(13) Uani 1 1 d . . . . .
O1 O 0.16491(19) 0.45689(17) 0.30932(15) 0.0400(4) Uani 1 1 d . . . . .
O2 O 0.4186(2) 0.8219(2) 0.15937(17) 0.0516(5) Uani 1 1 d . . . . .
N1 N 0.4902(2) 0.67126(19) 0.40632(16) 0.0326(5) Uani 1 1 d . . . . .
C1 C 0.1782(3) 0.6425(3) 0.1569(2) 0.0464(7) Uani 1 1 d . . . . .
H1A H 0.099074 0.618162 0.170516 0.056 Uiso 1 1 calc R . . . .
H1B H 0.172895 0.709548 0.125911 0.056 Uiso 1 1 calc R . . . .
C2 C 0.2509(3) 0.5557(3) 0.1230(2) 0.0460(7) Uani 1 1 d . . . . .
H2A H 0.291014 0.568395 0.070608 0.055 Uiso 1 1 calc R . . . .
H2B H 0.217216 0.477036 0.115200 0.055 Uiso 1 1 calc R . . . .
C3 C 0.2402(3) 0.5209(2) 0.30330(19) 0.0347(6) Uani 1 1 d . . . . .
C4 C 0.4033(3) 0.7560(2) 0.2064(2) 0.0375(6) Uani 1 1 d . . . . .
C5 C 0.4989(2) 0.7707(2) 0.47001(19) 0.0347(5) Uani 1 1 d . . . . .
C6 C 0.5912(3) 0.7946(3) 0.5502(2) 0.0394(6) Uani 1 1 d . . . . .
H6 H 0.594097 0.864407 0.593341 0.047 Uiso 1 1 calc R . . . .
C7 C 0.6790(3) 0.7162(3) 0.5670(2) 0.0423(6) Uani 1 1 d . . . . .
H7 H 0.744292 0.732285 0.620405 0.051 Uiso 1 1 calc R . . . .
C8 C 0.6696(3) 0.6143(3) 0.5044(2) 0.0395(6) Uani 1 1 d . . . . .
H8 H 0.728015 0.558694 0.515141 0.047 Uiso 1 1 calc R . . . .
C9 C 0.5754(2) 0.5929(2) 0.42598(19) 0.0347(5) Uani 1 1 d . . . . .
C10 C 0.5613(3) 0.4818(2) 0.35970(19) 0.0371(6) Uani 1 1 d . . . . .
H10A H 0.504329 0.429949 0.378367 0.045 Uiso 1 1 calc R . . . .
H10B H 0.641674 0.446772 0.362380 0.045 Uiso 1 1 calc R . . . .
C11 C 0.6351(3) 0.5449(2) 0.1948(2) 0.0360(6) Uani 1 1 d . . . . .
C12 C 0.7533(3) 0.5160(3) 0.2308(2) 0.0401(6) Uani 1 1 d . . . . .
H12 H 0.767126 0.479385 0.283955 0.048 Uiso 1 1 calc R . . . .
C13 C 0.8512(3) 0.5402(3) 0.1898(2) 0.0435(7) Uani 1 1 d . . . . .
H13 H 0.931275 0.519715 0.214652 0.052 Uiso 1 1 calc R . . . .
C14 C 0.8318(3) 0.5940(3) 0.1128(2) 0.0441(7) Uani 1 1 d . . . . .
H14 H 0.898444 0.609442 0.084055 0.053 Uiso 1 1 calc R . . . .
C15 C 0.7150(3) 0.6256(3) 0.0773(2) 0.0422(6) Uani 1 1 d . . . . .
H15 H 0.702007 0.664105 0.025182 0.051 Uiso 1 1 calc R . . . .
C16 C 0.6175(3) 0.6009(3) 0.1181(2) 0.0389(6) Uani 1 1 d . . . . .
H16 H 0.537743 0.622441 0.093454 0.047 Uiso 1 1 calc R . . . .
C17 C 0.4682(3) 0.3570(2) 0.1746(2) 0.0356(6) Uani 1 1 d . . . . .
C18 C 0.5295(3) 0.3086(3) 0.1037(2) 0.0426(6) Uani 1 1 d . . . . .
H18 H 0.590938 0.352088 0.086744 0.051 Uiso 1 1 calc R . . . .
C19 C 0.5010(3) 0.1967(3) 0.0575(2) 0.0493(7) Uani 1 1 d . . . . .
H19 H 0.542396 0.164835 0.008553 0.059 Uiso 1 1 calc R . . . .
C20 C 0.4132(3) 0.1318(3) 0.0820(2) 0.0506(8) Uani 1 1 d . . . . .
H20 H 0.395230 0.055090 0.051177 0.061 Uiso 1 1 calc R . . . .
C21 C 0.3518(3) 0.1794(3) 0.1519(3) 0.0503(8) Uani 1 1 d . . . . .
H21 H 0.291486 0.135115 0.169319 0.060 Uiso 1 1 calc R . . . .
C22 C 0.3775(3) 0.2913(3) 0.1968(2) 0.0454(7) Uani 1 1 d . . . . .
H22 H 0.332747 0.323680 0.243413 0.055 Uiso 1 1 calc R . . . .
C23 C 0.4066(3) 0.8564(2) 0.44782(19) 0.0352(5) Uani 1 1 d . . . . .
H23A H 0.440238 0.909823 0.413682 0.042 Uiso 1 1 calc R . . . .
H23B H 0.389026 0.900398 0.507412 0.042 Uiso 1 1 calc R . . . .
C24 C 0.1799(3) 0.7387(2) 0.4572(2) 0.0342(5) Uani 1 1 d . . . . .
C25 C 0.0627(3) 0.6891(2) 0.4205(2) 0.0423(6) Uani 1 1 d . . . . .
H25 H 0.028519 0.684613 0.355320 0.051 Uiso 1 1 calc R . . . .
C26 C -0.0045(3) 0.6461(3) 0.4781(3) 0.0509(8) Uani 1 1 d . . . . .
H26 H -0.084374 0.612561 0.452240 0.061 Uiso 1 1 calc R . . . .
C27 C 0.0441(3) 0.6518(3) 0.5728(3) 0.0530(9) Uani 1 1 d . . . . .
H27 H -0.001705 0.621472 0.612064 0.064 Uiso 1 1 calc R . . . .
C28 C 0.1594(3) 0.7017(3) 0.6103(3) 0.0498(8) Uani 1 1 d . . . . .
H28 H 0.192491 0.706659 0.675737 0.060 Uiso 1 1 calc R . . . .
C29 C 0.2281(3) 0.7450(2) 0.5529(2) 0.0409(6) Uani 1 1 d . . . . .
H29 H 0.307780 0.778656 0.579183 0.049 Uiso 1 1 calc R . . . .
C30 C 0.1782(2) 0.9064(2) 0.3445(2) 0.0344(5) Uani 1 1 d . . . . .
C31 C 0.1583(3) 0.9283(3) 0.2529(2) 0.0435(7) Uani 1 1 d . . . . .
H31 H 0.189883 0.879621 0.205190 0.052 Uiso 1 1 calc R . . . .
C32 C 0.0930(3) 1.0202(3) 0.2306(2) 0.0446(7) Uani 1 1 d . . . . .
H32 H 0.079035 1.033961 0.167590 0.054 Uiso 1 1 calc R . . . .
C33 C 0.0481(3) 1.0920(3) 0.2995(2) 0.0433(7) Uani 1 1 d . . . . .
H33 H 0.003592 1.155271 0.284071 0.052 Uiso 1 1 calc R . . . .
C34 C 0.0678(3) 1.0722(2) 0.3909(2) 0.0432(7) Uani 1 1 d . . . . .
H34 H 0.037272 1.122082 0.438471 0.052 Uiso 1 1 calc R . . . .
C35 C 0.1323(3) 0.9792(2) 0.4136(2) 0.0389(6) Uani 1 1 d . . . . .
H35 H 0.145072 0.965284 0.476479 0.047 Uiso 1 1 calc R . . . .
O3 O 0.6479(3) 0.9702(2) 0.34806(19) 0.0706(8) Uani 1 1 d . . . . .
C36 C 0.6596(6) 1.0088(4) 0.2625(3) 0.0882(16) Uani 1 1 d . . . . .
H36A H 0.703481 1.084155 0.277782 0.106 Uiso 1 1 calc R . . . .
H36B H 0.577580 1.015267 0.223903 0.106 Uiso 1 1 calc R . . . .
C37 C 0.7301(4) 0.9234(4) 0.2093(3) 0.0653(10) Uani 1 1 d . . . . .
H37A H 0.789348 0.961265 0.180691 0.078 Uiso 1 1 calc R . . . .
H37B H 0.674383 0.870855 0.158617 0.078 Uiso 1 1 calc R . . . .
C38 C 0.7956(4) 0.8613(4) 0.2833(3) 0.0637(10) Uani 1 1 d . . . . .
H38A H 0.811032 0.782538 0.255430 0.076 Uiso 1 1 calc R . . . .
H38B H 0.874065 0.901287 0.317456 0.076 Uiso 1 1 calc R . . . .
C39 C 0.7033(4) 0.8642(3) 0.3464(3) 0.0567(9) Uani 1 1 d . . . . .
H39A H 0.640794 0.801146 0.321339 0.068 Uiso 1 1 calc R . . . .
H39B H 0.744190 0.856692 0.411044 0.068 Uiso 1 1 calc R . . . .
O4 O 0.0323(5) 0.9036(4) -0.0144(4) 0.0594(16) Uani 0.500(6) 1 d D U P A 1
C40 C 0.1480(15) 0.8672(14) -0.0328(17) 0.059(4) Uani 0.500(6) 1 d D U P A 1
H40A H 0.208472 0.875152 0.027289 0.071 Uiso 0.500(6) 1 calc R . P A 1
H40B H 0.178235 0.914083 -0.073636 0.071 Uiso 0.500(6) 1 calc R . P A 1
C41 C 0.1318(8) 0.7444(7) -0.0818(7) 0.058(2) Uani 0.500(6) 1 d D U P A 1
H41A H 0.192123 0.697709 -0.048976 0.070 Uiso 0.500(6) 1 calc R . P A 1
H41B H 0.141381 0.736445 -0.148498 0.070 Uiso 0.500(6) 1 calc R . P A 1
C42 C 0.0022(12) 0.7099(13) -0.0760(9) 0.056(3) Uani 0.500(6) 1 d D U P A 1
H42A H -0.053574 0.703389 -0.138224 0.068 Uiso 0.500(6) 1 calc R . P A 1
H42B H -0.000353 0.636688 -0.054093 0.068 Uiso 0.500(6) 1 calc R . P A 1
C43 C -0.0317(10) 0.8051(10) -0.0049(9) 0.050(2) Uani 0.500(6) 1 d D U P A 1
H43A H -0.121257 0.814502 -0.018077 0.060 Uiso 0.500(6) 1 calc R . P A 1
H43B H -0.007360 0.789414 0.059979 0.060 Uiso 0.500(6) 1 calc R . P A 1
O5 O 0.0659(5) 0.7296(4) -0.1610(3) 0.0544(15) Uani 0.500(6) 1 d D U P A 2
C44 C -0.0192(12) 0.7158(13) -0.1024(9) 0.055(3) Uani 0.500(6) 1 d D U P A 2
H44A H -0.006419 0.644148 -0.078020 0.065 Uiso 0.500(6) 1 calc R . P A 2
H44B H -0.104170 0.713276 -0.138721 0.065 Uiso 0.500(6) 1 calc R . P A 2
C45 C 0.0025(10) 0.8170(9) -0.0207(8) 0.047(2) Uani 0.500(6) 1 d D U P A 2
H45A H 0.002984 0.792587 0.040394 0.056 Uiso 0.500(6) 1 calc R . P A 2
H45B H -0.061373 0.872813 -0.030020 0.056 Uiso 0.500(6) 1 calc R . P A 2
C46 C 0.1291(11) 0.8676(13) -0.0240(12) 0.047(3) Uani 0.500(6) 1 d D U P A 2
H46A H 0.122488 0.942291 -0.043710 0.056 Uiso 0.500(6) 1 calc R . P A 2
H46B H 0.185123 0.875888 0.038301 0.056 Uiso 0.500(6) 1 calc R . P A 2
C47 C 0.1722(8) 0.7790(8) -0.0982(6) 0.0553(19) Uani 0.500(6) 1 d D U P A 2
H47A H 0.226218 0.815205 -0.132068 0.066 Uiso 0.500(6) 1 calc R . P A 2
H47B H 0.218126 0.720779 -0.067854 0.066 Uiso 0.500(6) 1 calc R . 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
W1 P1 2.4264(7) . ?
W1 P2 2.4260(7) . ?
W1 N1 2.279(2) . ?
W1 C1 2.258(3) . ?
W1 C2 2.253(3) . ?
W1 C3 2.000(3) . ?
W1 C4 1.992(3) . ?
P1 C10 1.841(3) . ?
P1 C11 1.825(3) . ?
P1 C17 1.836(3) . ?
P2 C23 1.833(3) . ?
P2 C24 1.825(3) . ?
P2 C30 1.827(3) . ?
O1 C3 1.155(3) . ?
O2 C4 1.169(4) . ?
N1 C5 1.366(4) . ?
N1 C9 1.371(4) . ?
C1 C2 1.404(5) . ?
C5 C6 1.390(4) . ?
C5 C23 1.496(4) . ?
C6 C7 1.384(4) . ?
C7 C8 1.379(4) . ?
C8 C9 1.384(4) . ?
C9 C10 1.488(4) . ?
C11 C12 1.394(4) . ?
C11 C16 1.394(4) . ?
C12 C13 1.390(4) . ?
C13 C14 1.381(4) . ?
C14 C15 1.390(4) . ?
C15 C16 1.386(4) . ?
C17 C18 1.394(4) . ?
C17 C22 1.392(4) . ?
C18 C19 1.392(4) . ?
C19 C20 1.379(5) . ?
C20 C21 1.380(5) . ?
C21 C22 1.384(4) . ?
C24 C25 1.393(4) . ?
C24 C29 1.390(4) . ?
C25 C26 1.386(4) . ?
C26 C27 1.379(5) . ?
C27 C28 1.379(5) . ?
C28 C29 1.396(4) . ?
C30 C31 1.390(4) . ?
C30 C35 1.391(4) . ?
C31 C32 1.384(4) . ?
C32 C33 1.378(4) . ?
C33 C34 1.378(4) . ?
C34 C35 1.391(4) . ?
O3 C36 1.439(5) . ?
O3 C39 1.419(5) . ?
C36 C37 1.496(6) . ?
C37 C38 1.505(6) . ?
C38 C39 1.502(5) . ?
O4 C40 1.422(14) . ?
O4 C43 1.414(11) . ?
C40 C41 1.509(15) . ?
C41 C42 1.517(13) . ?
C42 C43 1.503(13) . ?
O5 C44 1.420(13) . ?
O5 C47 1.403(9) . ?
C44 C45 1.525(13) . ?
C45 C46 1.537(13) . ?
C46 C47 1.528(13) . ?

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
P2 W1 P1 151.33(2) . . ?
N1 W1 P1 76.11(6) . . ?
N1 W1 P2 75.25(6) . . ?
C1 W1 P1 119.30(9) . . ?
C1 W1 P2 89.34(9) . . ?
C1 W1 N1 164.59(10) . . ?
C2 W1 P1 83.05(9) . . ?
C2 W1 P2 125.53(9) . . ?
C2 W1 N1 159.13(11) . . ?
C2 W1 C1 36.27(12) . . ?
C3 W1 P1 92.74(8) . . ?
C3 W1 P2 90.16(8) . . ?
C3 W1 N1 98.63(9) . . ?
C3 W1 C1 81.65(12) . . ?
C3 W1 C2 81.03(12) . . ?
C4 W1 P1 96.60(8) . . ?
C4 W1 P2 89.14(8) . . ?
C4 W1 N1 98.85(10) . . ?
C4 W1 C1 80.08(12) . . ?
C4 W1 C2 84.54(12) . . ?
C4 W1 C3 161.72(11) . . ?
C10 P1 W1 99.66(9) . . ?
C11 P1 W1 121.18(9) . . ?
C11 P1 C10 105.09(13) . . ?
C11 P1 C17 101.67(13) . . ?
C17 P1 W1 124.48(9) . . ?
C17 P1 C10 101.36(13) . . ?
C23 P2 W1 100.93(9) . . ?
C24 P2 W1 116.48(9) . . ?
C24 P2 C23 105.57(13) . . ?
C24 P2 C30 101.20(12) . . ?
C30 P2 W1 128.34(9) . . ?
C30 P2 C23 101.43(13) . . ?
C5 N1 W1 122.03(18) . . ?
C5 N1 C9 117.1(2) . . ?
C9 N1 W1 120.87(18) . . ?
C2 C1 W1 71.67(18) . . ?
C1 C2 W1 72.06(18) . . ?
O1 C3 W1 168.3(2) . . ?
O2 C4 W1 169.0(3) . . ?
N1 C5 C6 122.4(3) . . ?
N1 C5 C23 116.9(2) . . ?
C6 C5 C23 120.7(3) . . ?
C7 C6 C5 119.7(3) . . ?
C8 C7 C6 118.5(3) . . ?
C7 C8 C9 120.1(3) . . ?
N1 C9 C8 122.2(3) . . ?
N1 C9 C10 117.0(2) . . ?
C8 C9 C10 120.8(3) . . ?
C9 C10 P1 109.36(19) . . ?
C12 C11 P1 122.7(2) . . ?
C16 C11 P1 118.6(2) . . ?
C16 C11 C12 118.6(3) . . ?
C13 C12 C11 120.7(3) . . ?
C14 C13 C12 119.9(3) . . ?
C13 C14 C15 120.1(3) . . ?
C16 C15 C14 119.9(3) . . ?
C15 C16 C11 120.8(3) . . ?
C18 C17 P1 122.6(2) . . ?
C22 C17 P1 119.0(2) . . ?
C22 C17 C18 118.4(3) . . ?
C19 C18 C17 120.3(3) . . ?
C20 C19 C18 120.6(3) . . ?
C19 C20 C21 119.3(3) . . ?
C20 C21 C22 120.5(3) . . ?
C21 C22 C17 120.8(3) . . ?
C5 C23 P2 110.21(19) . . ?
C25 C24 P2 117.5(2) . . ?
C29 C24 P2 123.5(2) . . ?
C29 C24 C25 118.8(3) . . ?
C26 C25 C24 120.7(3) . . ?
C27 C26 C25 120.2(3) . . ?
C26 C27 C28 119.7(3) . . ?
C27 C28 C29 120.6(3) . . ?
C24 C29 C28 120.0(3) . . ?
C31 C30 P2 120.8(2) . . ?
C31 C30 C35 119.0(3) . . ?
C35 C30 P2 120.2(2) . . ?
C32 C31 C30 120.5(3) . . ?
C33 C32 C31 120.1(3) . . ?
C32 C33 C34 120.1(3) . . ?
C33 C34 C35 120.0(3) . . ?
C34 C35 C30 120.2(3) . . ?
C39 O3 C36 107.6(3) . . ?
O3 C36 C37 107.3(4) . . ?
C36 C37 C38 104.2(3) . . ?
C39 C38 C37 100.6(3) . . ?
O3 C39 C38 106.9(3) . . ?
C43 O4 C40 105.5(10) . . ?
O4 C40 C41 108.1(10) . . ?
C40 C41 C42 104.0(8) . . ?
C43 C42 C41 103.5(9) . . ?
O4 C43 C42 106.1(8) . . ?
C47 O5 C44 104.8(8) . . ?
O5 C44 C45 107.0(9) . . ?
C44 C45 C46 103.8(8) . . ?
C47 C46 C45 102.3(9) . . ?
O5 C47 C46 106.2(8) . . ?

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
W1 P1 C10 C9 -42.8(2) . . . . ?
W1 P1 C11 C12 135.6(2) . . . . ?
W1 P1 C11 C16 -48.8(3) . . . . ?
W1 P1 C17 C18 134.2(2) . . . . ?
W1 P1 C17 C22 -45.0(3) . . . . ?
W1 P2 C23 C5 -39.30(19) . . . . ?
W1 P2 C24 C25 -73.7(2) . . . . ?
W1 P2 C24 C29 103.0(2) . . . . ?
W1 P2 C30 C31 -4.8(3) . . . . ?
W1 P2 C30 C35 176.05(18) . . . . ?
W1 N1 C5 C6 -175.9(2) . . . . ?
W1 N1 C5 C23 1.7(3) . . . . ?
W1 N1 C9 C8 175.0(2) . . . . ?
W1 N1 C9 C10 -5.9(3) . . . . ?
P1 C11 C12 C13 174.2(2) . . . . ?
P1 C11 C16 C15 -174.7(2) . . . . ?
P1 C17 C18 C19 180.0(2) . . . . ?
P1 C17 C22 C21 -178.5(3) . . . . ?
P2 C24 C25 C26 176.5(2) . . . . ?
P2 C24 C29 C28 -176.5(2) . . . . ?
P2 C30 C31 C32 -179.8(2) . . . . ?
P2 C30 C35 C34 179.1(2) . . . . ?
N1 C5 C6 C7 0.5(4) . . . . ?
N1 C5 C23 P2 27.4(3) . . . . ?
N1 C9 C10 P1 34.7(3) . . . . ?
C5 N1 C9 C8 -2.8(4) . . . . ?
C5 N1 C9 C10 176.3(2) . . . . ?
C5 C6 C7 C8 -2.1(4) . . . . ?
C6 C5 C23 P2 -155.0(2) . . . . ?
C6 C7 C8 C9 1.2(4) . . . . ?
C7 C8 C9 N1 1.3(4) . . . . ?
C7 C8 C9 C10 -177.8(3) . . . . ?
C8 C9 C10 P1 -146.2(2) . . . . ?
C9 N1 C5 C6 1.8(4) . . . . ?
C9 N1 C5 C23 179.4(2) . . . . ?
C10 P1 C11 C12 24.1(3) . . . . ?
C10 P1 C11 C16 -160.2(2) . . . . ?
C10 P1 C17 C18 -115.6(3) . . . . ?
C10 P1 C17 C22 65.2(3) . . . . ?
C11 P1 C10 C9 83.3(2) . . . . ?
C11 P1 C17 C18 -7.4(3) . . . . ?
C11 P1 C17 C22 173.4(2) . . . . ?
C11 C12 C13 C14 0.4(5) . . . . ?
C12 C11 C16 C15 1.1(4) . . . . ?
C12 C13 C14 C15 1.0(5) . . . . ?
C13 C14 C15 C16 -1.3(5) . . . . ?
C14 C15 C16 C11 0.2(5) . . . . ?
C16 C11 C12 C13 -1.4(4) . . . . ?
C17 P1 C10 C9 -171.15(19) . . . . ?
C17 P1 C11 C12 -81.2(3) . . . . ?
C17 P1 C11 C16 94.4(2) . . . . ?
C17 C18 C19 C20 -0.9(5) . . . . ?
C18 C17 C22 C21 2.3(5) . . . . ?
C18 C19 C20 C21 1.2(5) . . . . ?
C19 C20 C21 C22 0.2(5) . . . . ?
C20 C21 C22 C17 -2.0(5) . . . . ?
C22 C17 C18 C19 -0.8(5) . . . . ?
C23 P2 C24 C25 175.3(2) . . . . ?
C23 P2 C24 C29 -8.0(3) . . . . ?
C23 P2 C30 C31 109.2(3) . . . . ?
C23 P2 C30 C35 -70.0(2) . . . . ?
C23 C5 C6 C7 -176.9(3) . . . . ?
C24 P2 C23 C5 82.4(2) . . . . ?
C24 P2 C30 C31 -142.2(2) . . . . ?
C24 P2 C30 C35 38.7(3) . . . . ?
C24 C25 C26 C27 -0.1(5) . . . . ?
C25 C24 C29 C28 0.1(4) . . . . ?
C25 C26 C27 C28 0.8(5) . . . . ?
C26 C27 C28 C29 -0.9(5) . . . . ?
C27 C28 C29 C24 0.5(4) . . . . ?
C29 C24 C25 C26 -0.3(4) . . . . ?
C30 P2 C23 C5 -172.43(19) . . . . ?
C30 P2 C24 C25 69.9(2) . . . . ?
C30 P2 C24 C29 -113.4(2) . . . . ?
C30 C31 C32 C33 0.8(5) . . . . ?
C31 C30 C35 C34 -0.1(4) . . . . ?
C31 C32 C33 C34 -0.2(5) . . . . ?
C32 C33 C34 C35 -0.4(5) . . . . ?
C33 C34 C35 C30 0.6(5) . . . . ?
C35 C30 C31 C32 -0.6(5) . . . . ?
O3 C36 C37 C38 -20.3(5) . . . . ?
C36 O3 C39 C38 24.5(4) . . . . ?
C36 C37 C38 C39 33.3(4) . . . . ?
C37 C38 C39 O3 -36.0(4) . . . . ?
C39 O3 C36 C37 -2.4(5) . . . . ?
O4 C40 C41 C42 -8.3(19) . . . . ?
C40 O4 C43 C42 -37.0(15) . . . . ?
C40 C41 C42 C43 -13.3(16) . . . . ?
C41 C42 C43 O4 31.0(13) . . . . ?
C43 O4 C40 C41 28.2(19) . . . . ?
O5 C44 C45 C46 -16.0(15) . . . . ?
C44 O5 C47 C46 -41.1(12) . . . . ?
C44 C45 C46 C47 -7.8(15) . . . . ?
C45 C46 C47 O5 29.7(14) . . . . ?
C47 O5 C44 C45 35.7(12) . . . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a 200 micro/m MITEGEN holder in perfluoroether oil'
_olex2_submission_special_instructions 'No special instructions were received'
