# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_9b_MeOPAmH
_database_code_depnum_ccdc_archive 'CCDC 1421316'
_audit_update_record             
;
2015-09-29 deposited with the CCDC.
2015-10-02 downloaded from the CCDC.
;
#SHELXTL Code: 0126

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
'(aZ)-N-[2,6-bis(1-methylethyl)phenyl]-a-[[2,6-bis(1-methylethyl)phenyl] phosphinidene]-4-methoxy-benzenemethanamine chromium pentacarbonyl complex'
_chemical_name_common            
; 
 1,3-bis(2,6-diisopropylphenyl)-2-(4-methoxypphenyl)-3-aza-1λ3-phosphapropene 
;
_chemical_melting_point          406
_chemical_formula_moiety         'C32 H42 N O P'
_chemical_formula_sum            'C32 H42 N O P'
_chemical_formula_weight         487.63

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'

_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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   18.1914(16)
_cell_length_b                   10.1898(5)
_cell_length_c                   18.1080(12)
_cell_angle_alpha                90
_cell_angle_beta                 117.319(9)
_cell_angle_gamma                90
_cell_volume                     2982.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5683
_cell_measurement_theta_min      2
_cell_measurement_theta_max      25,5
_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.115
_shelx_estimated_absorpt_T_min   0.901
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  .9008
_exptl_absorpt_correction_T_max  .9879
_exptl_absorpt_process_details   
; 
 STOE/XRED  (Stoe IPDS V2.63)
;
_exptl_special_details           
; 
 A crystal was mounted in epoxy glue on a small glass capilary and data
 collected at RT on an Stoe IPDS image-plate diffractometer. 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       Phi-Oscillation
_diffrn_reflns_number            30504
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.941
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measured_fraction_theta_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_point_group_measured_fraction_full 0.942
_reflns_number_total             5133
_reflns_number_gt                2523
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Stoe IPDS V2.63'
_computing_cell_refinement       'Stoe IPDS V2.63'
_computing_data_reduction        'Stoe IPDS V2.63'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
# Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison
# Wisconsin, USA.
# Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.
# Sheldrick, G. M. (2002). TWINABS, University of Gttingen.
# Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P.,
# Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood,
# P. A. (2008). J. Appl. Cryst. 41, 466-470.
# Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.

_refine_special_details          
;
 RIGU restraints added to improve description of the thermal ellipsoids. See:
 A. Thorn, B. Dittrich and G. M. Sheldrick, Acta Cryst. (2012). A68, 448-451.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0590P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5133
_refine_ls_number_parameters     328
_refine_ls_number_restraints     267
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.1190
_refine_ls_wR_factor_gt          0.1005
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_restrained_S_all      0.859
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P P 0.23355(5) 0.03583(7) 0.38203(5) 0.0574(2) Uani 1 1 d . U . . .
O1 O 0.29450(16) 0.6117(2) 0.54303(15) 0.1004(8) Uani 1 1 d . U . . .
N N 0.25174(13) 0.17354(19) 0.26312(14) 0.0514(5) Uani 1 1 d . U . . .
H1 H 0.2302(15) 0.104(2) 0.2334(16) 0.062 Uiso 1 1 d . U . . .
C1 C 0.25538(13) 0.1723(2) 0.34014(15) 0.0433(6) Uani 1 1 d . U . . .
C2 C 0.27171(14) 0.2942(2) 0.38967(15) 0.0452(6) Uani 1 1 d . U . . .
C3 C 0.23441(15) 0.4120(2) 0.35501(17) 0.0528(6) Uani 1 1 d . U . . .
H3 H 0.2037 0.4185 0.2976 0.063 Uiso 1 1 calc R U . . .
C4 C 0.24166(17) 0.5215(3) 0.40410(19) 0.0629(7) Uani 1 1 d . U . . .
H4 H 0.2164 0.6003 0.3797 0.075 Uiso 1 1 calc R U . . .
C5 C 0.28651(18) 0.5116(3) 0.4890(2) 0.0664(8) Uani 1 1 d . U . . .
C6 C 0.2373(3) 0.7158(3) 0.5133(3) 0.1224(15) Uani 1 1 d . U . . .
H6A H 0.2465 0.7657 0.4733 0.184 Uiso 1 1 calc R U . . .
H6B H 0.2443 0.7715 0.5588 0.184 Uiso 1 1 calc R U . . .
H6C H 0.1821 0.6811 0.4875 0.184 Uiso 1 1 calc R U . . .
C7 C 0.32697(18) 0.3965(3) 0.52474(18) 0.0707(8) Uani 1 1 d . U . . .
H7 H 0.3591 0.3915 0.5821 0.085 Uiso 1 1 calc R U . . .
C8 C 0.32008(16) 0.2891(3) 0.47614(17) 0.0614(7) Uani 1 1 d . U . . .
H8 H 0.3479 0.2121 0.5009 0.074 Uiso 1 1 calc R U . . .
C9 C 0.27404(15) 0.2732(2) 0.22116(16) 0.0473(6) Uani 1 1 d . U . . .
C10 C 0.21475(16) 0.3060(2) 0.14038(16) 0.0553(6) Uani 1 1 d . U . . .
C11 C 0.13075(18) 0.2403(3) 0.10146(19) 0.0740(8) Uani 1 1 d . U . . .
H11 H 0.1159 0.2230 0.1462 0.089 Uiso 1 1 calc R U . . .
C12 C 0.1349(2) 0.1066(4) 0.0636(2) 0.1062(12) Uani 1 1 d . U . . .
H12A H 0.1485 0.1200 0.0188 0.159 Uiso 1 1 calc R U . . .
H12B H 0.0821 0.0636 0.0428 0.159 Uiso 1 1 calc R U . . .
H12C H 0.1765 0.0529 0.1055 0.159 Uiso 1 1 calc R U . . .
C13 C 0.0617(2) 0.3247(4) 0.0365(2) 0.1253(15) Uani 1 1 d . U . . .
H13A H 0.0586 0.4066 0.0611 0.188 Uiso 1 1 calc R U . . .
H13B H 0.0098 0.2793 0.0170 0.188 Uiso 1 1 calc R U . . .
H13C H 0.0732 0.3410 -0.0094 0.188 Uiso 1 1 calc R U . . .
C14 C 0.2366(2) 0.3967(3) 0.09617(19) 0.0719(8) Uani 1 1 d . U . . .
H14 H 0.1982 0.4196 0.0425 0.086 Uiso 1 1 calc R U . . .
C15 C 0.3134(2) 0.4524(3) 0.1304(2) 0.0754(8) Uani 1 1 d . U . . .
H15 H 0.3268 0.5126 0.0999 0.090 Uiso 1 1 calc R U . . .
C16 C 0.37032(19) 0.4200(3) 0.2089(2) 0.0679(8) Uani 1 1 d . U . . .
H16 H 0.4219 0.4603 0.2316 0.082 Uiso 1 1 calc R U . . .
C17 C 0.35378(16) 0.3279(2) 0.25663(16) 0.0525(6) Uani 1 1 d . U . . .
C18 C 0.42301(15) 0.2877(3) 0.34020(18) 0.0642(7) Uani 1 1 d . U . . .
H18 H 0.3995 0.2285 0.3664 0.077 Uiso 1 1 calc R U . . .
C19 C 0.4898(2) 0.2109(4) 0.3284(3) 0.1115(13) Uani 1 1 d . U . . .
H19A H 0.4642 0.1412 0.2892 0.167 Uiso 1 1 calc R U . . .
H19B H 0.5289 0.1748 0.3807 0.167 Uiso 1 1 calc R U . . .
H19C H 0.5178 0.2690 0.3079 0.167 Uiso 1 1 calc R U . . .
C20 C 0.4599(2) 0.4061(3) 0.3982(2) 0.1023(12) Uani 1 1 d . U . . .
H20A H 0.4859 0.4638 0.3753 0.153 Uiso 1 1 calc R U . . .
H20B H 0.5001 0.3762 0.4519 0.153 Uiso 1 1 calc R U . . .
H20C H 0.4166 0.4523 0.4036 0.153 Uiso 1 1 calc R U . . .
C21 C 0.20772(16) -0.0901(2) 0.30030(16) 0.0510(6) Uani 1 1 d . U . . .
C22 C 0.12385(18) -0.1256(3) 0.25312(18) 0.0674(8) Uani 1 1 d . U . . .
C23 C 0.05459(19) -0.0478(3) 0.2578(2) 0.0907(10) Uani 1 1 d . U . . .
H23 H 0.0789 0.0353 0.2856 0.109 Uiso 1 1 calc R U . . .
C24 C -0.0152(2) -0.0127(5) 0.1725(3) 0.1461(17) Uani 1 1 d . U . . .
H24A H -0.0474 -0.0897 0.1474 0.219 Uiso 1 1 calc R U . . .
H24B H 0.0079 0.0204 0.1380 0.219 Uiso 1 1 calc R U . . .
H24C H -0.0498 0.0530 0.1785 0.219 Uiso 1 1 calc R U . . .
C25 C 0.0216(3) -0.1141(5) 0.3092(4) 0.182(3) Uani 1 1 d . U . . .
H25A H -0.0055 -0.1941 0.2825 0.273 Uiso 1 1 calc R U . . .
H25B H -0.0174 -0.0575 0.3155 0.273 Uiso 1 1 calc R U . . .
H25C H 0.0663 -0.1339 0.3629 0.273 Uiso 1 1 calc R U . . .
C26 C 0.1044(2) -0.2326(3) 0.2007(2) 0.0923(10) Uani 1 1 d . U . . .
H26 H 0.0492 -0.2569 0.1699 0.111 Uiso 1 1 calc R U . . .
C27 C 0.1640(3) -0.3033(3) 0.1929(2) 0.0992(11) Uani 1 1 d . U . . .
H27 H 0.1492 -0.3754 0.1575 0.119 Uiso 1 1 calc R U . . .
C28 C 0.2451(3) -0.2690(3) 0.2369(2) 0.0866(10) Uani 1 1 d . U . . .
H28 H 0.2852 -0.3180 0.2308 0.104 Uiso 1 1 calc R U . . .
C29 C 0.26952(18) -0.1613(2) 0.29107(19) 0.0640(7) Uani 1 1 d . U . . .
C30 C 0.3597(2) -0.1249(3) 0.3392(2) 0.0837(9) Uani 1 1 d . U . . .
H30 H 0.3617 -0.0314 0.3528 0.100 Uiso 1 1 calc R U . . .
C31 C 0.4085(3) -0.1416(5) 0.2907(4) 0.174(2) Uani 1 1 d . U . . .
H31A H 0.4100 -0.2328 0.2782 0.261 Uiso 1 1 calc R U . . .
H31B H 0.4639 -0.1102 0.3234 0.261 Uiso 1 1 calc R U . . .
H31C H 0.3824 -0.0924 0.2400 0.261 Uiso 1 1 calc R U . . .
C32 C 0.4009(3) -0.1992(5) 0.4219(3) 0.162(2) Uani 1 1 d . U . . .
H32A H 0.3697 -0.1858 0.4520 0.243 Uiso 1 1 calc R U . . .
H32B H 0.4562 -0.1672 0.4542 0.243 Uiso 1 1 calc R U . . .
H32C H 0.4025 -0.2912 0.4113 0.243 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P C1 1.716(2) . ?
P C21 1.849(2) . ?
O1 C5 1.375(3) . ?
O1 C6 1.408(4) . ?
N C1 1.365(3) . ?
N C9 1.434(3) . ?
N H1 0.87(2) . ?
C1 C2 1.480(3) . ?
C2 C3 1.379(3) . ?
C2 C8 1.401(3) . ?
C3 C4 1.395(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.373(4) . ?
C4 H4 0.9300 . ?
C5 C7 1.379(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.373(4) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.402(3) . ?
C9 C17 1.404(3) . ?
C10 C14 1.394(4) . ?
C10 C11 1.514(4) . ?
C11 C13 1.531(4) . ?
C11 C12 1.543(4) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.365(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.361(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.399(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.515(4) . ?
C18 C20 1.537(4) . ?
C18 C19 1.540(4) . ?
C18 H18 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C29 1.411(3) . ?
C21 C22 1.412(4) . ?
C22 C26 1.381(4) . ?
C22 C23 1.524(4) . ?
C23 C25 1.483(5) . ?
C23 C24 1.524(5) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.362(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.363(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.401(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.509(4) . ?
C30 C31 1.518(5) . ?
C30 C32 1.532(5) . ?
C30 H30 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P C21 103.54(11) . . ?
C5 O1 C6 117.9(3) . . ?
C1 N C9 130.9(2) . . ?
C1 N H1 114.9(17) . . ?
C9 N H1 114.1(18) . . ?
N C1 C2 120.9(2) . . ?
N C1 P 123.11(18) . . ?
C2 C1 P 115.80(18) . . ?
C3 C2 C8 117.8(2) . . ?
C3 C2 C1 122.3(2) . . ?
C8 C2 C1 119.6(2) . . ?
C2 C3 C4 121.5(3) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C5 C4 C3 119.2(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 O1 123.8(3) . . ?
C4 C5 C7 120.2(2) . . ?
O1 C5 C7 116.0(3) . . ?
O1 C6 H6A 109.5 . . ?
O1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C5 120.3(3) . . ?
C8 C7 H7 119.8 . . ?
C5 C7 H7 119.8 . . ?
C7 C8 C2 120.8(3) . . ?
C7 C8 H8 119.6 . . ?
C2 C8 H8 119.6 . . ?
C10 C9 C17 121.4(2) . . ?
C10 C9 N 116.9(2) . . ?
C17 C9 N 121.5(2) . . ?
C14 C10 C9 118.1(3) . . ?
C14 C10 C11 121.2(3) . . ?
C9 C10 C11 120.6(2) . . ?
C10 C11 C13 114.0(3) . . ?
C10 C11 C12 110.7(2) . . ?
C13 C11 C12 110.1(3) . . ?
C10 C11 H11 107.2 . . ?
C13 C11 H11 107.2 . . ?
C12 C11 H11 107.2 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C10 121.1(3) . . ?
C15 C14 H14 119.4 . . ?
C10 C14 H14 119.4 . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 122.1(3) . . ?
C15 C16 H16 118.9 . . ?
C17 C16 H16 118.9 . . ?
C16 C17 C9 117.0(3) . . ?
C16 C17 C18 118.9(2) . . ?
C9 C17 C18 124.1(2) . . ?
C17 C18 C20 111.9(2) . . ?
C17 C18 C19 110.2(3) . . ?
C20 C18 C19 111.7(3) . . ?
C17 C18 H18 107.6 . . ?
C20 C18 H18 107.6 . . ?
C19 C18 H18 107.6 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C29 C21 C22 119.7(2) . . ?
C29 C21 P 121.9(2) . . ?
C22 C21 P 118.02(19) . . ?
C26 C22 C21 118.9(3) . . ?
C26 C22 C23 119.4(3) . . ?
C21 C22 C23 121.6(2) . . ?
C25 C23 C22 112.4(3) . . ?
C25 C23 C24 110.7(4) . . ?
C22 C23 C24 113.0(3) . . ?
C25 C23 H23 106.8 . . ?
C22 C23 H23 106.8 . . ?
C24 C23 H23 106.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C22 121.6(3) . . ?
C27 C26 H26 119.2 . . ?
C22 C26 H26 119.2 . . ?
C26 C27 C28 120.3(3) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C27 C28 C29 121.3(3) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C28 C29 C21 118.2(3) . . ?
C28 C29 C30 120.6(3) . . ?
C21 C29 C30 121.2(3) . . ?
C29 C30 C31 114.0(3) . . ?
C29 C30 C32 111.0(3) . . ?
C31 C30 C32 110.8(4) . . ?
C29 C30 H30 106.9 . . ?
C31 C30 H30 106.9 . . ?
C32 C30 H30 106.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C9 N C1 C2 11.2(4) . . . . ?
C9 N C1 P -174.16(19) . . . . ?
C21 P C1 N 0.2(2) . . . . ?
C21 P C1 C2 175.02(17) . . . . ?
N C1 C2 C3 43.1(3) . . . . ?
P C1 C2 C3 -131.9(2) . . . . ?
N C1 C2 C8 -143.4(2) . . . . ?
P C1 C2 C8 41.6(3) . . . . ?
C8 C2 C3 C4 -2.4(3) . . . . ?
C1 C2 C3 C4 171.3(2) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C3 C4 C5 O1 -177.1(2) . . . . ?
C3 C4 C5 C7 3.0(4) . . . . ?
C6 O1 C5 C4 17.7(4) . . . . ?
C6 O1 C5 C7 -162.4(3) . . . . ?
C4 C5 C7 C8 -2.6(4) . . . . ?
O1 C5 C7 C8 177.4(2) . . . . ?
C5 C7 C8 C2 -0.3(4) . . . . ?
C3 C2 C8 C7 2.7(4) . . . . ?
C1 C2 C8 C7 -171.1(2) . . . . ?
C1 N C9 C10 -129.1(3) . . . . ?
C1 N C9 C17 55.9(3) . . . . ?
C17 C9 C10 C14 -1.0(3) . . . . ?
N C9 C10 C14 -176.1(2) . . . . ?
C17 C9 C10 C11 176.5(2) . . . . ?
N C9 C10 C11 1.5(3) . . . . ?
C14 C10 C11 C13 -30.3(4) . . . . ?
C9 C10 C11 C13 152.2(3) . . . . ?
C14 C10 C11 C12 94.5(3) . . . . ?
C9 C10 C11 C12 -83.0(3) . . . . ?
C9 C10 C14 C15 -0.1(4) . . . . ?
C11 C10 C14 C15 -177.7(3) . . . . ?
C10 C14 C15 C16 0.0(4) . . . . ?
C14 C15 C16 C17 1.4(4) . . . . ?
C15 C16 C17 C9 -2.4(4) . . . . ?
C15 C16 C17 C18 174.3(3) . . . . ?
C10 C9 C17 C16 2.2(3) . . . . ?
N C9 C17 C16 177.1(2) . . . . ?
C10 C9 C17 C18 -174.2(2) . . . . ?
N C9 C17 C18 0.6(4) . . . . ?
C16 C17 C18 C20 57.7(3) . . . . ?
C9 C17 C18 C20 -125.9(3) . . . . ?
C16 C17 C18 C19 -67.2(3) . . . . ?
C9 C17 C18 C19 109.3(3) . . . . ?
C1 P C21 C29 81.8(2) . . . . ?
C1 P C21 C22 -105.9(2) . . . . ?
C29 C21 C22 C26 2.1(4) . . . . ?
P C21 C22 C26 -170.4(2) . . . . ?
C29 C21 C22 C23 -177.0(3) . . . . ?
P C21 C22 C23 10.5(4) . . . . ?
C26 C22 C23 C25 78.1(5) . . . . ?
C21 C22 C23 C25 -102.8(4) . . . . ?
C26 C22 C23 C24 -48.1(5) . . . . ?
C21 C22 C23 C24 131.0(3) . . . . ?
C21 C22 C26 C27 -0.7(5) . . . . ?
C23 C22 C26 C27 178.4(3) . . . . ?
C22 C26 C27 C28 -0.5(6) . . . . ?
C26 C27 C28 C29 0.2(5) . . . . ?
C27 C28 C29 C21 1.1(5) . . . . ?
C27 C28 C29 C30 180.0(3) . . . . ?
C22 C21 C29 C28 -2.3(4) . . . . ?
P C21 C29 C28 169.8(2) . . . . ?
C22 C21 C29 C30 178.9(3) . . . . ?
P C21 C29 C30 -9.0(4) . . . . ?
C28 C29 C30 C31 38.1(4) . . . . ?
C21 C29 C30 C31 -143.1(3) . . . . ?
C28 C29 C30 C32 -87.9(4) . . . . ?
C21 C29 C30 C32 90.9(4) . . . . ?

_refine_diff_density_max         0.181
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.031

_shelxl_version_number           2014/6

# start Validation Reply Form
_vrf_PLAT029_9b_MeOPAmH          
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.942 Note  
RESPONSE: This is an older dataset collected on an image-plate diffractometer 
at ambient temperature. The instrument was not equipped for LT measurements.
This RT structure is included here specifically for comparison of geometry
details to the metal complexes also obtained at RT. An excellent quality
LT crystal structure of this compound will be published in a different 
context elsewhere.
;

_vrf_PLAT242_9b_MeOPAmH          
;
PROBLEM: Low       Ueq as Compared to Neighbors for .....        C23 Check 
RESPONSE: The two attached atoms to C11, C18, C23 and C30 are iPr Me groups
that undergo significant thermal displacement (typical "rocking" of the 
iPr groups.)
;
# end Validation Reply Form



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol'
_chemical_compound_source        No.
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_10_TolPAmHCrCO5
_database_code_depnum_ccdc_archive 'CCDC 1421317'
_audit_update_record             
;
2015-09-29 deposited with the CCDC.
2015-10-02 downloaded from the CCDC.
;
#  Shelxtl code:0158

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
'(aZ)-N-[2,6-bis(1-methylethyl)phenyl]-a-[[2,6-bis(1-methylethyl)phenyl] phosphinidene]-4-methyl-benzenemethanamine chromium pentacarbonyl complex'
_chemical_name_common            
'1,3-bis(2,6-diisopropylphenyl)-2-(4-methylphenyl)-3-aza-1λ3-phosphapropene chromium pentacarbonyl complex'
_chemical_melting_point          453
_chemical_formula_moiety         'C37 H42 Cr N O5 P'
_chemical_formula_sum            'C37 H42 Cr N O5 P'
_chemical_formula_weight         663.68

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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4722(8)
_cell_length_b                   12.1314(11)
_cell_length_c                   14.7650(13)
_cell_angle_alpha                84.600(11)
_cell_angle_beta                 79.559(10)
_cell_angle_gamma                71.687(10)
_cell_volume                     1749.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6221
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      25.68

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.660
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.414
_shelx_estimated_absorpt_T_min   0.772
_shelx_estimated_absorpt_T_max   0.952
_exptl_absorpt_correction_type   Analytical
_exptl_absorpt_correction_T_min  0.87344
_exptl_absorpt_correction_T_max  0.95354
_exptl_absorpt_process_details   
;
 ABST/PLATON 98
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       Phi-Oscillation
_diffrn_reflns_number            24627
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_av_R_equivalents  0.1285
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.808
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measured_fraction_theta_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_point_group_measured_fraction_full 0.938
_reflns_number_total             6221
_reflns_number_gt                4184
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Stoe IPDS V2.63'
_computing_cell_refinement       'Stoe IPDS V2.63'
_computing_data_reduction        'Stoe IPDS V2.63'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
# Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison
# Wisconsin, USA.
# Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.
# Sheldrick, G. M. (2002). TWINABS, University of Gttingen.
# Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P.,
# Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood,
# P. A. (2008). J. Appl. Cryst. 41, 466-470.
# Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.

_refine_special_details          
;
 RIGU restraints added to improve description of the thermal ellipsoids. See:
 A. Thorn, B. Dittrich and G. M. Sheldrick, Acta Cryst. (2012). A68, 448-451.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6221
_refine_ls_number_parameters     418
_refine_ls_number_restraints     360
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0900
_refine_ls_goodness_of_fit_ref   0.879
_refine_ls_restrained_S_all      0.865
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cr Cr -0.05323(4) 0.84025(3) 0.71076(3) 0.04164(12) Uani 1 1 d . U . . .
P P 0.13914(6) 0.72750(4) 0.78418(4) 0.04226(15) Uani 1 1 d . U . . .
N N 0.3479(2) 0.53778(14) 0.81407(13) 0.0403(4) Uani 1 1 d . U . . .
H1 H 0.366(3) 0.585(2) 0.8459(18) 0.048 Uiso 1 1 d . U . . .
O41 O -0.2834(2) 0.98546(18) 0.61664(17) 0.0870(7) Uani 1 1 d . U . . .
O42 O -0.1427(2) 0.63018(17) 0.69055(18) 0.0794(6) Uani 1 1 d . U . . .
O43 O 0.1231(3) 0.8305(2) 0.52232(15) 0.0819(6) Uani 1 1 d . U . . .
O44 O 0.0005(3) 1.06119(17) 0.74734(18) 0.0916(7) Uani 1 1 d . U . . .
O45 O -0.2687(2) 0.88622(18) 0.88072(15) 0.0765(6) Uani 1 1 d . U . . .
C1 C 0.2335(2) 0.58532(16) 0.77507(14) 0.0344(4) Uani 1 1 d . U . . .
C2 C 0.1899(2) 0.50778(16) 0.72360(14) 0.0368(5) Uani 1 1 d . U . . .
C3 C 0.1503(3) 0.41369(19) 0.76558(16) 0.0477(6) Uani 1 1 d . U . . .
H3 H 0.1473 0.3994 0.8288 0.057 Uiso 1 1 calc R U . . .
C4 C 0.1157(3) 0.3417(2) 0.71485(18) 0.0552(7) Uani 1 1 d . U . . .
H4 H 0.0903 0.2790 0.7446 0.066 Uiso 1 1 calc R U . . .
C5 C 0.1174(3) 0.3592(2) 0.62129(17) 0.0490(6) Uani 1 1 d . U . . .
C6 C 0.0817(4) 0.2791(3) 0.5659(2) 0.0762(9) Uani 1 1 d . U . . .
H6A H 0.1636 0.2233 0.5383 0.114 Uiso 1 1 calc R U . . .
H6B H 0.0334 0.3233 0.5184 0.114 Uiso 1 1 calc R U . . .
H6C H 0.0253 0.2395 0.6054 0.114 Uiso 1 1 calc R U . . .
C7 C 0.1544(3) 0.45387(19) 0.57983(16) 0.0495(6) Uani 1 1 d . U . . .
H7 H 0.1553 0.4686 0.5168 0.059 Uiso 1 1 calc R U . . .
C8 C 0.1901(2) 0.52710(18) 0.62966(16) 0.0436(5) Uani 1 1 d . U . . .
H8 H 0.2147 0.5902 0.5998 0.052 Uiso 1 1 calc R U . . .
C9 C 0.4149(2) 0.41450(16) 0.82556(15) 0.0389(5) Uani 1 1 d . U . . .
C10 C 0.3919(2) 0.36027(17) 0.91212(16) 0.0418(5) Uani 1 1 d . U . . .
C11 C 0.3138(3) 0.42576(19) 0.99706(17) 0.0491(6) Uani 1 1 d . U . . .
H11 H 0.2988 0.5088 0.9817 0.059 Uiso 1 1 calc R U . . .
C12 C 0.3948(4) 0.3938(3) 1.0767(2) 0.0738(8) Uani 1 1 d . U . . .
H12A H 0.3451 0.4406 1.1281 0.111 Uiso 1 1 calc R U . . .
H12B H 0.4813 0.4075 1.0578 0.111 Uiso 1 1 calc R U . . .
H12C H 0.4089 0.3132 1.0944 0.111 Uiso 1 1 calc R U . . .
C13 C 0.1760(3) 0.4077(3) 1.0262(2) 0.0757(8) Uani 1 1 d . U . . .
H13A H 0.1198 0.4416 0.9800 0.113 Uiso 1 1 calc R U . . .
H13B H 0.1338 0.4441 1.0837 0.113 Uiso 1 1 calc R U . . .
H13C H 0.1867 0.3260 1.0336 0.113 Uiso 1 1 calc R U . . .
C14 C 0.4464(3) 0.23985(19) 0.91902(19) 0.0540(6) Uani 1 1 d . U . . .
H14 H 0.4315 0.2008 0.9753 0.065 Uiso 1 1 calc R U . . .
C15 C 0.5213(3) 0.1784(2) 0.8445(2) 0.0606(7) Uani 1 1 d . U . . .
H15 H 0.5535 0.0977 0.8499 0.073 Uiso 1 1 calc R U . . .
C16 C 0.5496(3) 0.2334(2) 0.7626(2) 0.0582(7) Uani 1 1 d . U . . .
H16 H 0.6054 0.1901 0.7136 0.070 Uiso 1 1 calc R U . . .
C17 C 0.4967(2) 0.35316(18) 0.75020(16) 0.0457(5) Uani 1 1 d . U . . .
C18 C 0.5387(3) 0.4116(2) 0.65959(18) 0.0600(7) Uani 1 1 d . U . . .
H18 H 0.4746 0.4902 0.6567 0.072 Uiso 1 1 calc R U . . .
C19 C 0.6791(4) 0.4228(4) 0.6579(3) 0.1008(12) Uani 1 1 d . U . . .
H19A H 0.6805 0.4581 0.7131 0.151 Uiso 1 1 calc R U . . .
H19B H 0.7007 0.4702 0.6052 0.151 Uiso 1 1 calc R U . . .
H19C H 0.7452 0.3471 0.6545 0.151 Uiso 1 1 calc R U . . .
C20 C 0.5347(4) 0.3485(3) 0.5767(2) 0.0872(10) Uani 1 1 d . U . . .
H20A H 0.5512 0.3938 0.5214 0.131 Uiso 1 1 calc R U . . .
H20B H 0.4467 0.3376 0.5818 0.131 Uiso 1 1 calc R U . . .
H20C H 0.6036 0.2743 0.5744 0.131 Uiso 1 1 calc R U . . .
C21 C 0.2362(2) 0.79881(16) 0.83720(16) 0.0408(5) Uani 1 1 d . U . . .
C22 C 0.2107(2) 0.81327(17) 0.93310(16) 0.0431(5) Uani 1 1 d . U . . .
C23 C 0.1189(3) 0.7564(2) 0.99959(17) 0.0520(6) Uani 1 1 d . U . . .
H23 H 0.1098 0.6920 0.9685 0.062 Uiso 1 1 calc R U . . .
C24 C 0.1783(3) 0.7063(2) 1.08767(19) 0.0664(8) Uani 1 1 d . U . . .
H24A H 0.1717 0.7687 1.1254 0.100 Uiso 1 1 calc R U . . .
H24B H 0.2722 0.6617 1.0716 0.100 Uiso 1 1 calc R U . . .
H24C H 0.1281 0.6572 1.1211 0.100 Uiso 1 1 calc R U . . .
C25 C -0.0221(3) 0.8413(2) 1.0243(2) 0.0687(8) Uani 1 1 d . U . . .
H25A H -0.0163 0.9042 1.0566 0.103 Uiso 1 1 calc R U . . .
H25B H -0.0800 0.8022 1.0630 0.103 Uiso 1 1 calc R U . . .
H25C H -0.0595 0.8713 0.9691 0.103 Uiso 1 1 calc R U . . .
C26 C 0.2694(3) 0.8840(2) 0.96802(19) 0.0559(6) Uani 1 1 d . U . . .
H26 H 0.2518 0.8952 1.0311 0.067 Uiso 1 1 calc R U . . .
C27 C 0.3525(3) 0.9379(2) 0.9120(2) 0.0619(7) Uani 1 1 d . U . . .
H27 H 0.3893 0.9864 0.9369 0.074 Uiso 1 1 calc R U . . .
C28 C 0.3817(3) 0.9208(2) 0.8198(2) 0.0596(7) Uani 1 1 d . U . . .
H28 H 0.4402 0.9566 0.7827 0.072 Uiso 1 1 calc R U . . .
C29 C 0.3264(3) 0.8516(2) 0.78000(17) 0.0490(6) Uani 1 1 d . U . . .
C30 C 0.3703(3) 0.8318(3) 0.6780(2) 0.0667(8) Uani 1 1 d . U . . .
H30 H 0.3129 0.7903 0.6599 0.080 Uiso 1 1 calc R U . . .
C31 C 0.5153(4) 0.7552(3) 0.6582(3) 0.0894(10) Uani 1 1 d . U . . .
H31A H 0.5747 0.7935 0.6747 0.134 Uiso 1 1 calc R U . . .
H31B H 0.5390 0.7399 0.5937 0.134 Uiso 1 1 calc R U . . .
H31C H 0.5247 0.6832 0.6934 0.134 Uiso 1 1 calc R U . . .
C32 C 0.3498(4) 0.9450(3) 0.6191(3) 0.1031(13) Uani 1 1 d . U . . .
H32A H 0.4086 0.9860 0.6325 0.155 Uiso 1 1 calc R U . . .
H32B H 0.2567 0.9925 0.6327 0.155 Uiso 1 1 calc R U . . .
H32C H 0.3713 0.9274 0.5550 0.155 Uiso 1 1 calc R U . . .
C41 C -0.1950(3) 0.9292(2) 0.65195(19) 0.0590(7) Uani 1 1 d . U . . .
C42 C -0.1022(3) 0.7050(2) 0.69682(19) 0.0521(6) Uani 1 1 d . U . . .
C43 C 0.0607(3) 0.8301(2) 0.59366(19) 0.0532(6) Uani 1 1 d . U . . .
C44 C -0.0162(3) 0.9765(2) 0.73346(19) 0.0562(6) Uani 1 1 d . U . . .
C45 C -0.1811(3) 0.8647(2) 0.81995(19) 0.0536(6) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr C41 1.845(3) . ?
Cr C45 1.881(3) . ?
Cr C44 1.884(3) . ?
Cr C42 1.905(3) . ?
Cr C43 1.905(3) . ?
Cr P 2.4259(7) . ?
P C1 1.701(2) . ?
P C21 1.834(2) . ?
N C1 1.361(3) . ?
N C9 1.447(3) . ?
N H1 0.86(3) . ?
O41 C41 1.143(3) . ?
O42 C42 1.133(3) . ?
O43 C43 1.135(3) . ?
O44 C44 1.138(3) . ?
O45 C45 1.145(3) . ?
C1 C2 1.484(3) . ?
C2 C8 1.384(3) . ?
C2 C3 1.389(3) . ?
C3 C4 1.369(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(3) . ?
C4 H4 0.9300 . ?
C5 C7 1.380(3) . ?
C5 C6 1.497(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.379(3) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C17 1.391(3) . ?
C9 C10 1.398(3) . ?
C10 C14 1.393(3) . ?
C10 C11 1.510(3) . ?
C11 C13 1.507(4) . ?
C11 C12 1.524(4) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.362(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.357(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.390(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.514(3) . ?
C18 C19 1.514(5) . ?
C18 C20 1.517(4) . ?
C18 H18 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.410(3) . ?
C21 C29 1.416(3) . ?
C22 C26 1.382(3) . ?
C22 C23 1.521(3) . ?
C23 C25 1.515(4) . ?
C23 C24 1.534(4) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.365(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.361(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.381(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.512(4) . ?
C30 C31 1.502(5) . ?
C30 C32 1.532(4) . ?
C30 H30 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C41 Cr C45 86.17(12) . . ?
C41 Cr C44 89.57(11) . . ?
C45 Cr C44 87.68(12) . . ?
C41 Cr C42 89.86(11) . . ?
C45 Cr C42 87.50(12) . . ?
C44 Cr C42 175.17(12) . . ?
C41 Cr C43 87.21(12) . . ?
C45 Cr C43 173.18(10) . . ?
C44 Cr C43 90.60(11) . . ?
C42 Cr C43 94.16(11) . . ?
C41 Cr P 177.63(9) . . ?
C45 Cr P 95.58(8) . . ?
C44 Cr P 88.90(8) . . ?
C42 Cr P 91.81(7) . . ?
C43 Cr P 90.99(8) . . ?
C1 P C21 106.73(10) . . ?
C1 P Cr 130.38(8) . . ?
C21 P Cr 121.09(6) . . ?
C1 N C9 125.02(18) . . ?
C1 N H1 113.7(16) . . ?
C9 N H1 119.1(16) . . ?
N C1 C2 117.61(17) . . ?
N C1 P 122.98(16) . . ?
C2 C1 P 119.41(16) . . ?
C8 C2 C3 117.7(2) . . ?
C8 C2 C1 119.72(18) . . ?
C3 C2 C1 122.61(19) . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 122.1(2) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 H4 118.9 . . ?
C4 C5 C7 117.2(2) . . ?
C4 C5 C6 121.9(2) . . ?
C7 C5 C6 120.9(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C5 121.6(2) . . ?
C8 C7 H7 119.2 . . ?
C5 C7 H7 119.2 . . ?
C7 C8 C2 120.8(2) . . ?
C7 C8 H8 119.6 . . ?
C2 C8 H8 119.6 . . ?
C17 C9 C10 122.09(19) . . ?
C17 C9 N 119.40(19) . . ?
C10 C9 N 118.5(2) . . ?
C14 C10 C9 117.3(2) . . ?
C14 C10 C11 119.4(2) . . ?
C9 C10 C11 123.33(18) . . ?
C13 C11 C10 112.1(2) . . ?
C13 C11 C12 110.3(2) . . ?
C10 C11 C12 111.6(2) . . ?
C13 C11 H11 107.5 . . ?
C10 C11 H11 107.5 . . ?
C12 C11 H11 107.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C10 121.0(2) . . ?
C15 C14 H14 119.5 . . ?
C10 C14 H14 119.5 . . ?
C16 C15 C14 120.7(2) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C15 C16 C17 121.4(3) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 H16 119.3 . . ?
C16 C17 C9 117.3(2) . . ?
C16 C17 C18 119.4(2) . . ?
C9 C17 C18 123.1(2) . . ?
C17 C18 C19 109.0(2) . . ?
C17 C18 C20 112.7(2) . . ?
C19 C18 C20 111.2(3) . . ?
C17 C18 H18 107.9 . . ?
C19 C18 H18 107.9 . . ?
C20 C18 H18 107.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C29 119.5(2) . . ?
C22 C21 P 120.80(17) . . ?
C29 C21 P 119.30(18) . . ?
C26 C22 C21 118.7(2) . . ?
C26 C22 C23 118.5(2) . . ?
C21 C22 C23 122.8(2) . . ?
C25 C23 C22 110.9(2) . . ?
C25 C23 C24 109.8(2) . . ?
C22 C23 C24 112.4(2) . . ?
C25 C23 H23 107.8 . . ?
C22 C23 H23 107.8 . . ?
C24 C23 H23 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C22 121.5(3) . . ?
C27 C26 H26 119.3 . . ?
C22 C26 H26 119.3 . . ?
C28 C27 C26 120.2(2) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 121.6(3) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C28 C29 C21 118.6(2) . . ?
C28 C29 C30 118.1(2) . . ?
C21 C29 C30 123.3(2) . . ?
C31 C30 C29 111.0(2) . . ?
C31 C30 C32 110.9(3) . . ?
C29 C30 C32 113.1(3) . . ?
C31 C30 H30 107.2 . . ?
C29 C30 H30 107.2 . . ?
C32 C30 H30 107.2 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O41 C41 Cr 178.9(3) . . ?
O42 C42 Cr 174.0(2) . . ?
O43 C43 Cr 175.7(3) . . ?
O44 C44 Cr 177.1(3) . . ?
O45 C45 Cr 172.8(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
C9 N C1 C2 -13.1(3) . . . . ?
C9 N C1 P 166.06(17) . . . . ?
C21 P C1 N 8.6(2) . . . . ?
Cr P C1 N 173.08(13) . . . . ?
C21 P C1 C2 -172.19(16) . . . . ?
Cr P C1 C2 -7.7(2) . . . . ?
N C1 C2 C8 -115.4(2) . . . . ?
P C1 C2 C8 65.3(3) . . . . ?
N C1 C2 C3 63.4(3) . . . . ?
P C1 C2 C3 -115.8(2) . . . . ?
C8 C2 C3 C4 1.3(4) . . . . ?
C1 C2 C3 C4 -177.5(2) . . . . ?
C2 C3 C4 C5 -0.5(4) . . . . ?
C3 C4 C5 C7 -0.6(4) . . . . ?
C3 C4 C5 C6 179.0(3) . . . . ?
C4 C5 C7 C8 0.9(4) . . . . ?
C6 C5 C7 C8 -178.7(3) . . . . ?
C5 C7 C8 C2 0.0(4) . . . . ?
C3 C2 C8 C7 -1.1(3) . . . . ?
C1 C2 C8 C7 177.8(2) . . . . ?
C1 N C9 C17 77.8(3) . . . . ?
C1 N C9 C10 -100.5(3) . . . . ?
C17 C9 C10 C14 -4.5(4) . . . . ?
N C9 C10 C14 173.7(2) . . . . ?
C17 C9 C10 C11 174.5(2) . . . . ?
N C9 C10 C11 -7.2(3) . . . . ?
C14 C10 C11 C13 -72.6(3) . . . . ?
C9 C10 C11 C13 108.4(3) . . . . ?
C14 C10 C11 C12 51.7(3) . . . . ?
C9 C10 C11 C12 -127.4(3) . . . . ?
C9 C10 C14 C15 1.3(4) . . . . ?
C11 C10 C14 C15 -177.8(3) . . . . ?
C10 C14 C15 C16 2.8(5) . . . . ?
C14 C15 C16 C17 -3.8(5) . . . . ?
C15 C16 C17 C9 0.7(4) . . . . ?
C15 C16 C17 C18 175.9(3) . . . . ?
C10 C9 C17 C16 3.6(4) . . . . ?
N C9 C17 C16 -174.7(2) . . . . ?
C10 C9 C17 C18 -171.4(2) . . . . ?
N C9 C17 C18 10.3(4) . . . . ?
C16 C17 C18 C19 -78.2(3) . . . . ?
C9 C17 C18 C19 96.6(3) . . . . ?
C16 C17 C18 C20 45.7(4) . . . . ?
C9 C17 C18 C20 -139.4(3) . . . . ?
C1 P C21 C22 -95.12(18) . . . . ?
Cr P C21 C22 98.67(16) . . . . ?
C1 P C21 C29 92.19(19) . . . . ?
Cr P C21 C29 -74.02(19) . . . . ?
C29 C21 C22 C26 3.4(3) . . . . ?
P C21 C22 C26 -169.29(18) . . . . ?
C29 C21 C22 C23 -178.0(2) . . . . ?
P C21 C22 C23 9.3(3) . . . . ?
C26 C22 C23 C25 79.8(3) . . . . ?
C21 C22 C23 C25 -98.9(3) . . . . ?
C26 C22 C23 C24 -43.6(3) . . . . ?
C21 C22 C23 C24 137.8(2) . . . . ?
C21 C22 C26 C27 -1.1(4) . . . . ?
C23 C22 C26 C27 -179.8(2) . . . . ?
C22 C26 C27 C28 -1.3(4) . . . . ?
C26 C27 C28 C29 1.5(4) . . . . ?
C27 C28 C29 C21 0.7(4) . . . . ?
C27 C28 C29 C30 -176.6(3) . . . . ?
C22 C21 C29 C28 -3.2(3) . . . . ?
P C21 C29 C28 169.60(19) . . . . ?
C22 C21 C29 C30 174.0(2) . . . . ?
P C21 C29 C30 -13.2(3) . . . . ?
C28 C29 C30 C31 70.7(3) . . . . ?
C21 C29 C30 C31 -106.5(3) . . . . ?
C28 C29 C30 C32 -54.6(4) . . . . ?
C21 C29 C30 C32 128.2(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N H1 H12B 0.86(3) 2.35(3) 3.071(6) 141(2) 2_667

_refine_diff_density_max         0.234
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.044

_shelxl_version_number           2014/6

# start Validation Reply Form
_vrf_PLAT029_10_TolPAmHCrCO5     
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.938 Note  
RESPONSE: This is an older dataset collected on an image-plate diffractometer 
at ambient temperature. The instrument was not equipped for LT measurements.
Crystals are not available for redetermination on a modern diffractometer. 
The structure is of reasonable quality in most regards and reliable for
the application in this publication.
;
_vrf_PLAT911_10_TolPAmHCrCO5     
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600        385 Report
RESPONSE: This is an older dataset collected on an image-plate diffractometer 
at ambient temperature. The instrument was not equipped for LT measurements.
Crystals are not available for redetermination on a modern diffractometer. 
The structure is of reasonable quality in most regards and reliable for
the application in this publication.
;
# end Validation Reply Form


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl ether'
_chemical_compound_source        No.
_chemical_properties_physical    'Air-sensitive, Light-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_11a_TolPAmHMoCO5
_database_code_depnum_ccdc_archive 'CCDC 1421318'
_audit_update_record             
;
2015-09-29 deposited with the CCDC.
2015-10-02 downloaded from the CCDC.
;
#  Shelxtl code:2026

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
'(aZ)-N-[2,6-bis(1-methylethyl)phenyl]-a-[[2,6-bis(1-methylethyl)phenyl] phosphinidene]-4-methyl-benzenemethanamine molybdenum pentacarbonyl complex'
_chemical_name_common            
'1,3-bis(2,6-diisopropylphenyl)-2-(4-methylphenyl)-3-aza-1λ3-phosphapropene molybdenum pentacarbonyl complex'
_chemical_melting_point          428
_chemical_formula_moiety         'C37 H42 Mo N O5 P'
_chemical_formula_sum            'C37 H42 Mo N O5 P'
_chemical_formula_weight         707.62

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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5913(8)
_cell_length_b                   12.2632(10)
_cell_length_c                   14.8639(13)
_cell_angle_alpha                84.783(10)
_cell_angle_beta                 79.008(10)
_cell_angle_gamma                71.596(9)
_cell_volume                     1797.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      26
_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.450
_shelx_estimated_absorpt_T_min   0.787
_shelx_estimated_absorpt_T_max   0.965
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_process_details   
;
 Stoe IPDS V2.63 FaceIt numerical absorption correction
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0400
0 1 0 0.0400
0 0 1 0.1040
0 0 -1 0.1040
1 1 1 0.2800
-1 -1 -1 0.2800
2 2 -1 0.2800


_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       Phi-Oscillation
_diffrn_reflns_number            25323
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.793
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.250
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measured_fraction_theta_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_point_group_measured_fraction_full 0.938
_reflns_number_total             6402
_reflns_number_gt                5036
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Stoe IPDS V2.63'
_computing_cell_refinement       'Stoe IPDS V2.63'
_computing_data_reduction        'Stoe IPDS V2.63'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
# Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison
# Wisconsin, USA.
# Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.
# Sheldrick, G. M. (2002). TWINABS, University of Gttingen.
# Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P.,
# Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood,
# P. A. (2008). J. Appl. Cryst. 41, 466-470.
# Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.

_refine_special_details          
;
 RIGU restraints added to improve description of the thermal ellipsoids. See:
 A. Thorn, B. Dittrich and G. M. Sheldrick, Acta Cryst. (2012). A68, 448-451.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0339P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6402
_refine_ls_number_parameters     418
_refine_ls_number_restraints     360
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0675
_refine_ls_wR_factor_gt          0.0649
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_restrained_S_all      0.901
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Mo Mo -0.05770(2) 0.84273(2) 0.70857(2) 0.03965(7) Uani 1 1 d . U . . .
P P 0.14475(6) 0.72657(4) 0.78347(4) 0.04179(13) Uani 1 1 d . U . . .
N N 0.34833(18) 0.53710(14) 0.81610(12) 0.0390(4) Uani 1 1 d . U . . .
H1 H 0.368(2) 0.581(2) 0.8469(15) 0.047 Uiso 1 1 d . U . . .
C1 C 0.2363(2) 0.58489(16) 0.77647(12) 0.0336(4) Uani 1 1 d . U . . .
C2 C 0.1923(2) 0.50849(16) 0.72529(13) 0.0353(4) Uani 1 1 d . U . . .
C3 C 0.1545(2) 0.41532(19) 0.76653(14) 0.0477(5) Uani 1 1 d . U . . .
H3 H 0.1532 0.4005 0.8291 0.057 Uiso 1 1 calc R U . . .
C4 C 0.1186(3) 0.3437(2) 0.71622(16) 0.0550(6) Uani 1 1 d . U . . .
H4 H 0.0932 0.2818 0.7456 0.066 Uiso 1 1 calc R U . . .
C5 C 0.1199(3) 0.36277(19) 0.62264(15) 0.0507(5) Uani 1 1 d . U . . .
C6 C 0.0832(4) 0.2836(3) 0.5675(2) 0.0807(9) Uani 1 1 d . U . . .
H6A H 0.1638 0.2266 0.5407 0.121 Uiso 1 1 calc R U . . .
H6B H 0.0375 0.3273 0.5199 0.121 Uiso 1 1 calc R U . . .
H6C H 0.0249 0.2465 0.6069 0.121 Uiso 1 1 calc R U . . .
C7 C 0.1563(3) 0.4562(2) 0.58199(15) 0.0502(5) Uani 1 1 d . U . . .
H7 H 0.1575 0.4710 0.5194 0.060 Uiso 1 1 calc R U . . .
C8 C 0.1914(2) 0.52867(17) 0.63209(13) 0.0422(5) Uani 1 1 d . U . . .
H8 H 0.2147 0.5917 0.6029 0.051 Uiso 1 1 calc R U . . .
C9 C 0.4146(2) 0.41553(15) 0.82654(13) 0.0370(4) Uani 1 1 d . U . . .
C10 C 0.3925(2) 0.36129(17) 0.91242(14) 0.0427(5) Uani 1 1 d . U . . .
C11 C 0.3138(3) 0.42620(19) 0.99780(15) 0.0503(5) Uani 1 1 d . U . . .
H11 H 0.2991 0.5083 0.9828 0.060 Uiso 1 1 calc R U . . .
C12 C 0.3933(3) 0.3952(3) 1.07652(19) 0.0774(8) Uani 1 1 d . U . . .
H12A H 0.4021 0.3170 1.0968 0.116 Uiso 1 1 calc R U . . .
H12B H 0.3465 0.4453 1.1263 0.116 Uiso 1 1 calc R U . . .
H12C H 0.4814 0.4038 1.0561 0.116 Uiso 1 1 calc R U . . .
C13 C 0.1762(3) 0.4089(3) 1.0270(2) 0.0798(9) Uani 1 1 d . U . . .
H13A H 0.1217 0.4415 0.9808 0.120 Uiso 1 1 calc R U . . .
H13B H 0.1332 0.4460 1.0839 0.120 Uiso 1 1 calc R U . . .
H13C H 0.1866 0.3281 1.0350 0.120 Uiso 1 1 calc R U . . .
C14 C 0.4470(3) 0.24234(19) 0.91876(17) 0.0561(6) Uani 1 1 d . U . . .
H14 H 0.4315 0.2039 0.9746 0.067 Uiso 1 1 calc R U . . .
C15 C 0.5228(3) 0.18094(19) 0.84436(19) 0.0630(7) Uani 1 1 d . U . . .
H15 H 0.5564 0.1012 0.8495 0.076 Uiso 1 1 calc R U . . .
C16 C 0.5496(3) 0.2364(2) 0.76230(18) 0.0579(6) Uani 1 1 d . U . . .
H16 H 0.6042 0.1937 0.7129 0.070 Uiso 1 1 calc R U . . .
C17 C 0.4972(2) 0.35497(18) 0.75082(15) 0.0446(5) Uani 1 1 d . U . . .
C18 C 0.5370(3) 0.4128(2) 0.66037(16) 0.0603(6) Uani 1 1 d . U . . .
H18 H 0.4736 0.4907 0.6585 0.072 Uiso 1 1 calc R U . . .
C19 C 0.6788(4) 0.4230(4) 0.6578(3) 0.1016(12) Uani 1 1 d . U . . .
H19A H 0.6781 0.4646 0.7097 0.152 Uiso 1 1 calc R U . . .
H19B H 0.7042 0.4633 0.6023 0.152 Uiso 1 1 calc R U . . .
H19C H 0.7426 0.3476 0.6598 0.152 Uiso 1 1 calc R U . . .
C20 C 0.5327(4) 0.3506(3) 0.57770(19) 0.0861(10) Uani 1 1 d . U . . .
H20A H 0.6022 0.2777 0.5738 0.129 Uiso 1 1 calc R U . . .
H20B H 0.5470 0.3962 0.5230 0.129 Uiso 1 1 calc R U . . .
H20C H 0.4462 0.3385 0.5840 0.129 Uiso 1 1 calc R U . . .
C21 C 0.2398(2) 0.79818(16) 0.83624(14) 0.0401(5) Uani 1 1 d . U . . .
C22 C 0.2128(2) 0.81298(17) 0.93187(15) 0.0443(5) Uani 1 1 d . U . . .
C23 C 0.1214(3) 0.75640(19) 0.99799(15) 0.0529(6) Uani 1 1 d . U . . .
H23 H 0.1140 0.6920 0.9670 0.063 Uiso 1 1 calc R U . . .
C24 C 0.1779(3) 0.7082(2) 1.08639(18) 0.0699(8) Uani 1 1 d . U . . .
H24A H 0.2717 0.6653 1.0710 0.105 Uiso 1 1 calc R U . . .
H24B H 0.1289 0.6587 1.1189 0.105 Uiso 1 1 calc R U . . .
H24C H 0.1683 0.7706 1.1244 0.105 Uiso 1 1 calc R U . . .
C25 C -0.0200(3) 0.8407(3) 1.0219(2) 0.0742(8) Uani 1 1 d . U . . .
H25A H -0.0161 0.9030 1.0549 0.111 Uiso 1 1 calc R U . . .
H25B H -0.0781 0.8019 1.0593 0.111 Uiso 1 1 calc R U . . .
H25C H -0.0548 0.8704 0.9666 0.111 Uiso 1 1 calc R U . . .
C26 C 0.2704(3) 0.8834(2) 0.96701(17) 0.0573(6) Uani 1 1 d . U . . .
H26 H 0.2524 0.8944 1.0298 0.069 Uiso 1 1 calc R U . . .
C27 C 0.3531(3) 0.9370(2) 0.91134(19) 0.0633(7) Uani 1 1 d . U . . .
H27 H 0.3892 0.9850 0.9362 0.076 Uiso 1 1 calc R U . . .
C28 C 0.3826(3) 0.9199(2) 0.81884(18) 0.0609(6) Uani 1 1 d . U . . .
H28 H 0.4405 0.9555 0.7818 0.073 Uiso 1 1 calc R U . . .
C29 C 0.3282(2) 0.8507(2) 0.77901(16) 0.0502(5) Uani 1 1 d . U . . .
C30 C 0.3708(3) 0.8315(3) 0.67657(17) 0.0682(7) Uani 1 1 d . U . . .
H30 H 0.3134 0.7911 0.6588 0.082 Uiso 1 1 calc R U . . .
C31 C 0.5160(4) 0.7541(3) 0.6558(2) 0.0928(10) Uani 1 1 d . U . . .
H31A H 0.5747 0.7904 0.6744 0.139 Uiso 1 1 calc R U . . .
H31B H 0.5410 0.7412 0.5912 0.139 Uiso 1 1 calc R U . . .
H31C H 0.5241 0.6819 0.6888 0.139 Uiso 1 1 calc R U . . .
C32 C 0.3515(4) 0.9433(4) 0.6195(2) 0.1081(13) Uani 1 1 d . U . . .
H32A H 0.2594 0.9909 0.6340 0.162 Uiso 1 1 calc R U . . .
H32B H 0.3726 0.9266 0.5555 0.162 Uiso 1 1 calc R U . . .
H32C H 0.4104 0.9830 0.6329 0.162 Uiso 1 1 calc R U . . .
O41 O -0.2981(2) 0.99225(19) 0.61407(15) 0.0885(7) Uani 1 1 d . U . . .
C41 C -0.2100(3) 0.9374(2) 0.64814(17) 0.0564(6) Uani 1 1 d . U . . .
O42 O -0.1466(2) 0.62227(17) 0.68829(16) 0.0818(6) Uani 1 1 d . U . . .
C42 C -0.1093(2) 0.6977(2) 0.69372(17) 0.0534(6) Uani 1 1 d . U . . .
O43 O 0.1217(2) 0.8365(2) 0.50967(14) 0.0881(7) Uani 1 1 d . U . . .
C43 C 0.0626(3) 0.8338(2) 0.58100(18) 0.0532(6) Uani 1 1 d . U . . .
O44 O -0.0029(3) 1.07264(17) 0.74485(17) 0.0996(8) Uani 1 1 d . U . . .
C44 C -0.0188(3) 0.9891(2) 0.73173(17) 0.0582(6) Uani 1 1 d . U . . .
O45 O -0.2806(2) 0.89135(17) 0.88783(14) 0.0760(5) Uani 1 1 d . U . . .
C45 C -0.1939(3) 0.86884(19) 0.82648(17) 0.0508(5) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo C41 1.984(3) . ?
Mo C45 2.025(3) . ?
Mo C44 2.036(3) . ?
Mo C42 2.059(3) . ?
Mo C43 2.064(3) . ?
Mo P 2.5612(6) . ?
P C1 1.7031(19) . ?
P C21 1.839(2) . ?
N C1 1.365(3) . ?
N C9 1.442(2) . ?
N H1 0.83(2) . ?
C1 C2 1.488(3) . ?
C2 C3 1.382(3) . ?
C2 C8 1.386(3) . ?
C3 C4 1.383(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(3) . ?
C4 H4 0.9300 . ?
C5 C7 1.375(3) . ?
C5 C6 1.506(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.385(3) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C17 1.396(3) . ?
C9 C10 1.399(3) . ?
C10 C14 1.391(3) . ?
C10 C11 1.517(3) . ?
C11 C13 1.515(4) . ?
C11 C12 1.521(4) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.366(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.367(4) . ?
C15 H15 0.9300 . ?
C16 C17 1.390(3) . ?
C16 H16 0.9300 . ?
C17 C18 1.512(3) . ?
C18 C20 1.519(4) . ?
C18 C19 1.540(4) . ?
C18 H18 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.412(3) . ?
C21 C29 1.412(3) . ?
C22 C26 1.388(3) . ?
C22 C23 1.524(3) . ?
C23 C25 1.524(4) . ?
C23 C24 1.539(4) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.368(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.371(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.390(3) . ?
C28 H28 0.9300 . ?
C29 C30 1.521(3) . ?
C30 C31 1.521(5) . ?
C30 C32 1.524(4) . ?
C30 H30 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
O41 C41 1.141(3) . ?
O42 C42 1.130(3) . ?
O43 C43 1.127(3) . ?
O44 C44 1.128(3) . ?
O45 C45 1.147(3) . ?

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
C41 Mo C45 85.73(10) . . ?
C41 Mo C44 89.14(11) . . ?
C45 Mo C44 87.96(10) . . ?
C41 Mo C42 89.95(10) . . ?
C45 Mo C42 87.60(10) . . ?
C44 Mo C42 175.52(10) . . ?
C41 Mo C43 86.94(10) . . ?
C45 Mo C43 172.40(9) . . ?
C44 Mo C43 89.93(10) . . ?
C42 Mo C43 94.40(9) . . ?
C41 Mo P 177.48(8) . . ?
C45 Mo P 95.72(7) . . ?
C44 Mo P 88.86(8) . . ?
C42 Mo P 92.16(7) . . ?
C43 Mo P 91.53(7) . . ?
C1 P C21 107.11(9) . . ?
C1 P Mo 130.41(7) . . ?
C21 P Mo 121.25(6) . . ?
C1 N C9 125.25(17) . . ?
C1 N H1 115.5(16) . . ?
C9 N H1 117.6(16) . . ?
N C1 C2 117.92(17) . . ?
N C1 P 123.28(15) . . ?
C2 C1 P 118.80(15) . . ?
C3 C2 C8 117.83(19) . . ?
C3 C2 C1 122.59(17) . . ?
C8 C2 C1 119.56(17) . . ?
C2 C3 C4 121.06(19) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C3 C4 C5 121.2(2) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C7 C5 C4 117.6(2) . . ?
C7 C5 C6 121.2(2) . . ?
C4 C5 C6 121.2(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 C8 121.5(2) . . ?
C5 C7 H7 119.2 . . ?
C8 C7 H7 119.2 . . ?
C7 C8 C2 120.81(19) . . ?
C7 C8 H8 119.6 . . ?
C2 C8 H8 119.6 . . ?
C17 C9 C10 121.88(18) . . ?
C17 C9 N 119.38(17) . . ?
C10 C9 N 118.74(17) . . ?
C14 C10 C9 117.7(2) . . ?
C14 C10 C11 119.25(19) . . ?
C9 C10 C11 123.08(18) . . ?
C13 C11 C10 112.3(2) . . ?
C13 C11 C12 110.6(2) . . ?
C10 C11 C12 111.7(2) . . ?
C13 C11 H11 107.3 . . ?
C10 C11 H11 107.3 . . ?
C12 C11 H11 107.3 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C10 121.2(2) . . ?
C15 C14 H14 119.4 . . ?
C10 C14 H14 119.4 . . ?
C14 C15 C16 120.1(2) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C15 C16 C17 121.7(2) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C16 C17 C9 117.2(2) . . ?
C16 C17 C18 119.5(2) . . ?
C9 C17 C18 123.18(19) . . ?
C17 C18 C20 113.2(2) . . ?
C17 C18 C19 108.0(2) . . ?
C20 C18 C19 111.1(3) . . ?
C17 C18 H18 108.1 . . ?
C20 C18 H18 108.1 . . ?
C19 C18 H18 108.1 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C29 119.92(19) . . ?
C22 C21 P 120.57(16) . . ?
C29 C21 P 119.05(16) . . ?
C26 C22 C21 118.6(2) . . ?
C26 C22 C23 118.6(2) . . ?
C21 C22 C23 122.80(19) . . ?
C22 C23 C25 110.6(2) . . ?
C22 C23 C24 112.7(2) . . ?
C25 C23 C24 109.8(2) . . ?
C22 C23 H23 107.8 . . ?
C25 C23 H23 107.8 . . ?
C24 C23 H23 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C22 121.5(2) . . ?
C27 C26 H26 119.2 . . ?
C22 C26 H26 119.2 . . ?
C26 C27 C28 119.9(2) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C27 C28 C29 121.6(2) . . ?
C27 C28 H28 119.2 . . ?
C29 C28 H28 119.2 . . ?
C28 C29 C21 118.4(2) . . ?
C28 C29 C30 118.6(2) . . ?
C21 C29 C30 123.0(2) . . ?
C31 C30 C29 110.3(2) . . ?
C31 C30 C32 111.0(3) . . ?
C29 C30 C32 112.9(3) . . ?
C31 C30 H30 107.5 . . ?
C29 C30 H30 107.5 . . ?
C32 C30 H30 107.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O41 C41 Mo 179.4(3) . . ?
O42 C42 Mo 175.1(2) . . ?
O43 C43 Mo 174.9(2) . . ?
O44 C44 Mo 177.1(3) . . ?
O45 C45 Mo 172.7(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
C9 N C1 C2 -11.4(3) . . . . ?
C9 N C1 P 168.11(15) . . . . ?
C21 P C1 N 8.32(19) . . . . ?
Mo P C1 N 175.40(12) . . . . ?
C21 P C1 C2 -172.13(14) . . . . ?
Mo P C1 C2 -5.05(19) . . . . ?
N C1 C2 C3 61.1(3) . . . . ?
P C1 C2 C3 -118.4(2) . . . . ?
N C1 C2 C8 -117.3(2) . . . . ?
P C1 C2 C8 63.1(2) . . . . ?
C8 C2 C3 C4 0.8(4) . . . . ?
C1 C2 C3 C4 -177.7(2) . . . . ?
C2 C3 C4 C5 0.3(4) . . . . ?
C3 C4 C5 C7 -0.8(4) . . . . ?
C3 C4 C5 C6 178.9(3) . . . . ?
C4 C5 C7 C8 0.3(4) . . . . ?
C6 C5 C7 C8 -179.4(3) . . . . ?
C5 C7 C8 C2 0.7(4) . . . . ?
C3 C2 C8 C7 -1.2(3) . . . . ?
C1 C2 C8 C7 177.3(2) . . . . ?
C1 N C9 C17 77.0(3) . . . . ?
C1 N C9 C10 -102.1(2) . . . . ?
C17 C9 C10 C14 -5.1(3) . . . . ?
N C9 C10 C14 174.0(2) . . . . ?
C17 C9 C10 C11 174.3(2) . . . . ?
N C9 C10 C11 -6.6(3) . . . . ?
C14 C10 C11 C13 -73.1(3) . . . . ?
C9 C10 C11 C13 107.6(3) . . . . ?
C14 C10 C11 C12 51.8(3) . . . . ?
C9 C10 C11 C12 -127.5(2) . . . . ?
C9 C10 C14 C15 1.9(4) . . . . ?
C11 C10 C14 C15 -177.5(2) . . . . ?
C10 C14 C15 C16 1.7(4) . . . . ?
C14 C15 C16 C17 -2.4(4) . . . . ?
C15 C16 C17 C9 -0.7(4) . . . . ?
C15 C16 C17 C18 176.2(2) . . . . ?
C10 C9 C17 C16 4.5(3) . . . . ?
N C9 C17 C16 -174.6(2) . . . . ?
C10 C9 C17 C18 -172.3(2) . . . . ?
N C9 C17 C18 8.7(3) . . . . ?
C16 C17 C18 C20 45.1(3) . . . . ?
C9 C17 C18 C20 -138.3(3) . . . . ?
C16 C17 C18 C19 -78.4(3) . . . . ?
C9 C17 C18 C19 98.2(3) . . . . ?
C1 P C21 C22 -93.65(17) . . . . ?
Mo P C21 C22 97.83(16) . . . . ?
C1 P C21 C29 94.09(18) . . . . ?
Mo P C21 C29 -74.43(19) . . . . ?
C29 C21 C22 C26 2.6(3) . . . . ?
P C21 C22 C26 -169.62(17) . . . . ?
C29 C21 C22 C23 -178.4(2) . . . . ?
P C21 C22 C23 9.4(3) . . . . ?
C26 C22 C23 C25 80.7(3) . . . . ?
C21 C22 C23 C25 -98.4(2) . . . . ?
C26 C22 C23 C24 -42.7(3) . . . . ?
C21 C22 C23 C24 138.3(2) . . . . ?
C21 C22 C26 C27 -0.7(4) . . . . ?
C23 C22 C26 C27 -179.8(2) . . . . ?
C22 C26 C27 C28 -1.2(4) . . . . ?
C26 C27 C28 C29 1.4(4) . . . . ?
C27 C28 C29 C21 0.5(4) . . . . ?
C27 C28 C29 C30 -177.2(3) . . . . ?
C22 C21 C29 C28 -2.4(3) . . . . ?
P C21 C29 C28 169.86(19) . . . . ?
C22 C21 C29 C30 175.2(2) . . . . ?
P C21 C29 C30 -12.5(3) . . . . ?
C28 C29 C30 C31 71.5(3) . . . . ?
C21 C29 C30 C31 -106.1(3) . . . . ?
C28 C29 C30 C32 -53.3(4) . . . . ?
C21 C29 C30 C32 129.1(3) . . . . ?

_refine_diff_density_max         0.238
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.043

_shelxl_version_number           2014/6

# start Validation Reply Form
_vrf_PLAT029_11a_TolPAmHMoCO5    
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.938 Note  
RESPONSE: This is an older dataset collected on an image-plate diffractometer 
at ambient temperature. The instrument was not equipped for LT measurements.
Crystals are not available for redetermination on a modern diffractometer. 
The structure is of reasonable quality in most regards and reliable for
the application in this publication.
;
# end Validation Reply Form


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Heptane'
_chemical_compound_source        No.
_chemical_properties_physical    'Air-sensitive, Light-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_11b_MeOPAmHMoCO5
_database_code_depnum_ccdc_archive 'CCDC 1421319'
_audit_update_record             
;
2015-09-29 deposited with the CCDC.
2015-10-02 downloaded from the CCDC.
;
#  Shelxtl code: 0125

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
'(aZ)-N-[2,6-bis(1-methylethyl)phenyl]-a-[[2,6-bis(1-methylethyl)phenyl] phosphinidene]-4-methoxy-benzenemethanamine chromium pentacarbonyl complex'
_chemical_name_common            
'1,3-bis(2,6-diisopropylphenyl)-2-(4-methoxyphenyl)-3-aza-1λ3-phosphapropene molybdenum pentacarbonyl complex'
_chemical_melting_point          423
_chemical_formula_moiety         'C37 H42 Mo N O6 P'
_chemical_formula_sum            'C37 H42 Mo N O6 P'
_chemical_formula_weight         723.62
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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7566(8)
_cell_length_b                   13.4617(11)
_cell_length_c                   14.2564(12)
_cell_angle_alpha                104.733(10)
_cell_angle_beta                 108.862(9)
_cell_angle_gamma                92.700(9)
_cell_volume                     1870.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2
_cell_measurement_theta_max      25,5

_exptl_crystal_description       'transparent block'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.436
_shelx_estimated_absorpt_T_min   0.845
_shelx_estimated_absorpt_T_max   0.941
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   
;
 Stoe IPDS V2.63 FaceIt numerical absorption correction
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 2 0.0600
0 0 -1 0.0800
0 -1 -2 0.0800
0 2 -1 0.1400
2 0 -1 0.2000
-2 0 1 0.2000
0 -2 1 0.0800

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       Phi-Oscillation
_diffrn_reflns_number            26266
_diffrn_reflns_av_unetI/netI     0.0500
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.992
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 0.938
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 0.938
_reflns_number_total             6658
_reflns_number_gt                4889
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


_computing_data_collection       'Stoe IPDS V2.63'
_computing_cell_refinement       'Stoe IPDS V2.63'
_computing_data_reduction        'Stoe IPDS V2.63'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
# Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison
# Wisconsin, USA.
# Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.
# Sheldrick, G. M. (2002). TWINABS, University of Gttingen.
# Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P.,
# Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood,
# P. A. (2008). J. Appl. Cryst. 41, 466-470.
# Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.


_refine_special_details          
;
 RIGU restraints added to improve description of the thermal ellipsoids. See:
 A. Thorn, B. Dittrich and G. M. Sheldrick, Acta Cryst. (2012). A68, 448-451.
 The N-H bond refines unusually short, so a distance restraint was 
 added to try and improve this parameter.

 Especially large displacement ellipsoids for the C42/O42 carbonyl group 
 indicated possible disorder. A two-part disorder model was refined
 anisotropically toan occupancy ratio of 65major:35minor, which was then fixed.
 The refinementwas made anisotropic and refined to convergence to result in an 
 excellent two-part disorder model. Whilst this might imply further disorder 
 in the rotation of the Mo(CO)4 equatorial plane, such is not obvious from the
 final displacement ellipsoids, so major feature seems to be the angle that 
 the CO group projects from the metal. 

 The displacement ellipsoids of tolyl ring C3 and C4 atoms were elongated 
 perpendicular to the plane suggesting a possible correlation of the rotation
 of this aryl ring in conjunction with the C42/O42 carbonyl disorder. A two-
 position disorder model for these two atoms was added in with the same
 occupancies as the carbonyl groups. The combined disorder makes chemical 
 sense and the model refined adequately.

 In addition, there are indications from  displacement ellipsoids that the iPr
 groups undergo positional disorder.
 Attempts to model this disorder were not satisfactory as often found for such
 groups and these have been left with anisotropic refinement to encompass the
 likely positional disorder, behaviour we often see for "dipp" groups.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6658
_refine_ls_number_parameters     464
_refine_ls_number_restraints     418
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0911
_refine_ls_wR_factor_gt          0.0849
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_restrained_S_all      0.934
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Mo Mo 0.83434(3) 0.54130(2) 0.73309(2) 0.04831(10) Uani 1 1 d . U . . .
P P 0.69482(8) 0.67434(5) 0.79453(5) 0.04530(18) Uani 1 1 d . U . . .
N N 0.5861(3) 0.85281(18) 0.8049(2) 0.0596(7) Uani 1 1 d D U . . .
H1 H 0.559(3) 0.836(2) 0.850(2) 0.072 Uiso 1 1 d D U . . .
O1 O 0.9038(3) 0.91805(18) 0.51354(18) 0.0819(8) Uani 1 1 d . U . . .
C1 C 0.6624(3) 0.78771(18) 0.76651(18) 0.0375(5) Uani 1 1 d . U . . .
C2 C 0.7238(3) 0.82057(18) 0.69776(18) 0.0384(6) Uani 1 1 d . U . . .
C3A C 0.8320(16) 0.8929(10) 0.7364(13) 0.082(5) Uani 0.65 1 d . U P A 1
H3A H 0.8690 0.9215 0.8077 0.098 Uiso 0.65 1 calc R U P A 1
C4A C 0.8901(19) 0.9262(12) 0.6752(11) 0.091(6) Uani 0.65 1 d . U P A 1
H4A H 0.9625 0.9785 0.7046 0.109 Uiso 0.65 1 calc R U P A 1
C3B C 0.814(3) 0.9143(16) 0.735(2) 0.046(3) Uani 0.35 1 d . U P A 2
H3B H 0.8374 0.9553 0.8033 0.055 Uiso 0.35 1 calc R U P A 2
C4B C 0.866(3) 0.9425(19) 0.6662(19) 0.059(4) Uani 0.35 1 d . U P A 2
H4B H 0.9204 1.0058 0.6878 0.070 Uiso 0.35 1 calc R U P A 2
C5 C 0.8403(3) 0.8813(2) 0.5692(2) 0.0537(7) Uani 1 1 d . U . . .
C6 C 0.8892(5) 0.8567(3) 0.4142(3) 0.0790(11) Uani 1 1 d . U . . .
H6A H 0.9521 0.8856 0.3901 0.118 Uiso 1 1 calc R U . . .
H6B H 0.8008 0.8549 0.3680 0.118 Uiso 1 1 calc R U . . .
H6C H 0.9045 0.7875 0.4163 0.118 Uiso 1 1 calc R U . . .
C7 C 0.7393(3) 0.8022(2) 0.5295(2) 0.0547(7) Uani 1 1 d . U . . .
H7 H 0.7082 0.7683 0.4591 0.066 Uiso 1 1 calc R U . . .
C8 C 0.6817(3) 0.7713(2) 0.5939(2) 0.0526(7) Uani 1 1 d . U . . .
H8 H 0.6131 0.7160 0.5658 0.063 Uiso 1 1 calc R U . . .
C9 C 0.5614(3) 0.9510(2) 0.7839(3) 0.0586(8) Uani 1 1 d . U . . .
C10 C 0.6343(4) 1.0426(3) 0.8597(3) 0.0772(10) Uani 1 1 d . U . . .
C11 C 0.7292(6) 1.0429(4) 0.9643(4) 0.1174(17) Uani 1 1 d . U . . .
H11 H 0.7399 0.9709 0.9639 0.141 Uiso 1 1 calc R U . . .
C12 C 0.6741(9) 1.0907(7) 1.0495(5) 0.209(4) Uani 1 1 d . U . . .
H12A H 0.7422 1.1029 1.1159 0.313 Uiso 1 1 calc R U . . .
H12B H 0.6006 1.0440 1.0447 0.313 Uiso 1 1 calc R U . . .
H12C H 0.6448 1.1552 1.0413 0.313 Uiso 1 1 calc R U . . .
C13 C 0.8667(7) 1.1034(5) 0.9914(6) 0.174(3) Uani 1 1 d . U . . .
H13A H 0.9257 1.0950 1.0549 0.261 Uiso 1 1 calc R U . . .
H13B H 0.8594 1.1756 0.9994 0.261 Uiso 1 1 calc R U . . .
H13C H 0.9010 1.0774 0.9369 0.261 Uiso 1 1 calc R U . . .
C14 C 0.6136(5) 1.1362(3) 0.8345(4) 0.0970(13) Uani 1 1 d . U . . .
H14 H 0.6600 1.1983 0.8825 0.116 Uiso 1 1 calc R U . . .
C15 C 0.5274(5) 1.1382(3) 0.7415(4) 0.1009(14) Uani 1 1 d . U . . .
H15 H 0.5174 1.2011 0.7260 0.121 Uiso 1 1 calc R U . . .
C16 C 0.4559(4) 1.0493(3) 0.6710(3) 0.0874(11) Uani 1 1 d . U . . .
H16 H 0.3968 1.0526 0.6080 0.105 Uiso 1 1 calc R U . . .
C17 C 0.4684(4) 0.9525(2) 0.6903(3) 0.0657(8) Uani 1 1 d . U . . .
C18 C 0.3782(4) 0.8579(3) 0.6127(3) 0.0765(10) Uani 1 1 d . U . . .
H18 H 0.4157 0.7966 0.6282 0.092 Uiso 1 1 calc R U . . .
C19 C 0.2420(5) 0.8556(4) 0.6252(4) 0.1138(15) Uani 1 1 d . U . . .
H19A H 0.1847 0.7944 0.5771 0.171 Uiso 1 1 calc R U . . .
H19B H 0.2041 0.9160 0.6121 0.171 Uiso 1 1 calc R U . . .
H19C H 0.2519 0.8550 0.6945 0.171 Uiso 1 1 calc R U . . .
C20 C 0.3633(6) 0.8516(4) 0.5009(3) 0.1141(16) Uani 1 1 d . U . . .
H20A H 0.3218 0.7835 0.4571 0.171 Uiso 1 1 calc R U . . .
H20B H 0.4493 0.8655 0.4965 0.171 Uiso 1 1 calc R U . . .
H20C H 0.3095 0.9021 0.4790 0.171 Uiso 1 1 calc R U . . .
C21 C 0.6010(3) 0.65796(19) 0.8780(2) 0.0472(6) Uani 1 1 d . U . . .
C22 C 0.6635(4) 0.6906(2) 0.9858(2) 0.0669(9) Uani 1 1 d . U . . .
C23 C 0.8071(5) 0.7380(4) 1.0391(3) 0.1030(14) Uani 1 1 d . U . . .
H23 H 0.8397 0.7527 0.9866 0.124 Uiso 1 1 calc R U . . .
C24 C 0.8224(9) 0.8418(5) 1.1215(4) 0.174(3) Uani 1 1 d . U . . .
H24A H 0.7565 0.8824 1.0938 0.262 Uiso 1 1 calc R U . . .
H24B H 0.9092 0.8792 1.1405 0.262 Uiso 1 1 calc R U . . .
H24C H 0.8109 0.8285 1.1814 0.262 Uiso 1 1 calc R U . . .
C25 C 0.8902(7) 0.6620(6) 1.0845(5) 0.164(3) Uani 1 1 d . U . . .
H25A H 0.9817 0.6924 1.1150 0.246 Uiso 1 1 calc R U . . .
H25B H 0.8806 0.5994 1.0307 0.246 Uiso 1 1 calc R U . . .
H25C H 0.8605 0.6462 1.1365 0.246 Uiso 1 1 calc R U . . .
C26 C 0.5904(6) 0.6733(3) 1.0473(3) 0.0927(13) Uani 1 1 d . U . . .
H26 H 0.6299 0.6951 1.1190 0.111 Uiso 1 1 calc R U . . .
C27 C 0.4629(6) 0.6252(4) 1.0039(4) 0.1024(14) Uani 1 1 d . U . . .
H27 H 0.4163 0.6148 1.0461 0.123 Uiso 1 1 calc R U . . .
C28 C 0.4023(5) 0.5920(3) 0.8985(4) 0.0840(11) Uani 1 1 d . U . . .
H28 H 0.3153 0.5586 0.8701 0.101 Uiso 1 1 calc R U . . .
C29 C 0.4696(3) 0.6077(2) 0.8334(3) 0.0588(8) Uani 1 1 d . U . . .
C30 C 0.3983(4) 0.5670(3) 0.7185(3) 0.0716(9) Uani 1 1 d . U . . .
H30 H 0.4530 0.5940 0.6848 0.086 Uiso 1 1 calc R U . . .
C31 C 0.2634(5) 0.6034(4) 0.6834(5) 0.1198(17) Uani 1 1 d . U . . .
H31A H 0.2718 0.6767 0.7148 0.180 Uiso 1 1 calc R U . . .
H31B H 0.2020 0.5673 0.7037 0.180 Uiso 1 1 calc R U . . .
H31C H 0.2313 0.5892 0.6095 0.180 Uiso 1 1 calc R U . . .
C32 C 0.3836(5) 0.4490(3) 0.6824(4) 0.1088(15) Uani 1 1 d . U . . .
H32A H 0.3497 0.4258 0.6082 0.163 Uiso 1 1 calc R U . . .
H32B H 0.3231 0.4201 0.7086 0.163 Uiso 1 1 calc R U . . .
H32C H 0.4685 0.4269 0.7075 0.163 Uiso 1 1 calc R U . . .
C41 C 0.9356(4) 0.4334(3) 0.6861(3) 0.0738(9) Uani 1 1 d . U . . .
O41 O 0.9944(4) 0.3708(3) 0.6585(3) 0.1212(12) Uani 1 1 d . U . . .
C42A C 0.9042(11) 0.6202(7) 0.6502(6) 0.067(2) Uani 0.65 1 d . U P B 1
O42A O 0.9516(8) 0.6588(6) 0.6056(5) 0.105(2) Uani 0.65 1 d . U P B 1
C42B C 0.9306(19) 0.6518(13) 0.6911(13) 0.069(4) Uani 0.35 1 d . U P B 2
O42B O 0.9911(14) 0.7082(10) 0.6711(12) 0.116(5) Uani 0.35 1 d . U P B 2
C43 C 0.6819(4) 0.4739(3) 0.5986(3) 0.0712(9) Uani 1 1 d . U . . .
O43 O 0.5998(4) 0.4295(3) 0.5233(2) 0.1188(11) Uani 1 1 d . U . . .
C44 C 0.7669(4) 0.4464(2) 0.8003(3) 0.0648(8) Uani 1 1 d . U . . .
O44 O 0.7306(3) 0.3896(2) 0.8359(3) 0.1113(10) Uani 1 1 d . U . . .
C45 C 0.9963(4) 0.5991(3) 0.8627(3) 0.0749(10) Uani 1 1 d . U . . .
O45 O 1.0916(3) 0.6261(3) 0.9332(3) 0.1275(13) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo C41 1.967(4) . ?
Mo C44 2.016(3) . ?
Mo C45 2.028(4) . ?
Mo C43 2.033(4) . ?
Mo C42A 2.056(9) . ?
Mo C42B 2.086(18) . ?
Mo P 2.5559(8) . ?
P C1 1.697(2) . ?
P C21 1.837(3) . ?
N C1 1.362(3) . ?
N C9 1.446(3) . ?
N H1 0.856(18) . ?
O1 C5 1.363(3) . ?
O1 C6 1.401(4) . ?
C1 C2 1.485(3) . ?
C2 C3A 1.347(15) . ?
C2 C8 1.370(4) . ?
C2 C3B 1.42(2) . ?
C3A C4A 1.370(19) . ?
C3A H3A 0.9300 . ?
C4A C5 1.384(15) . ?
C4A H4A 0.9300 . ?
C3B C4B 1.40(3) . ?
C3B H3B 0.9300 . ?
C4B C5 1.35(3) . ?
C4B H4B 0.9300 . ?
C5 C7 1.349(4) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.392(4) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C17 1.390(5) . ?
C9 C10 1.410(5) . ?
C10 C14 1.405(5) . ?
C10 C11 1.509(6) . ?
C11 C12 1.532(8) . ?
C11 C13 1.535(9) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.357(6) . ?
C14 H14 0.9300 . ?
C15 C16 1.355(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.403(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.503(5) . ?
C18 C20 1.529(6) . ?
C18 C19 1.532(6) . ?
C18 H18 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.403(4) . ?
C21 C29 1.404(4) . ?
C22 C26 1.406(5) . ?
C22 C23 1.507(6) . ?
C23 C25 1.521(8) . ?
C23 C24 1.542(7) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.358(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.370(6) . ?
C27 H27 0.9300 . ?
C28 C29 1.397(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.505(5) . ?
C30 C31 1.522(6) . ?
C30 C32 1.524(5) . ?
C30 H30 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C41 O41 1.144(4) . ?
C42A O42A 1.134(9) . ?
C42B O42B 1.125(17) . ?
C43 O43 1.140(4) . ?
C44 O44 1.137(4) . ?
C45 O45 1.143(4) . ?

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
C41 Mo C44 88.85(15) . . ?
C41 Mo C45 87.85(15) . . ?
C44 Mo C45 90.71(15) . . ?
C41 Mo C43 87.01(15) . . ?
C44 Mo C43 89.48(15) . . ?
C45 Mo C43 174.85(14) . . ?
C41 Mo C42A 84.5(3) . . ?
C44 Mo C42A 172.3(3) . . ?
C45 Mo C42A 92.9(3) . . ?
C43 Mo C42A 86.3(3) . . ?
C41 Mo C42B 92.4(5) . . ?
C44 Mo C42B 169.2(5) . . ?
C45 Mo C42B 78.6(5) . . ?
C43 Mo C42B 101.3(5) . . ?
C41 Mo P 177.13(12) . . ?
C44 Mo P 88.54(10) . . ?
C45 Mo P 93.37(10) . . ?
C43 Mo P 91.78(10) . . ?
C42A Mo P 98.0(3) . . ?
C42B Mo P 90.4(5) . . ?
C1 P C21 106.23(12) . . ?
C1 P Mo 130.05(9) . . ?
C21 P Mo 123.66(8) . . ?
C1 N C9 124.8(2) . . ?
C1 N H1 116(2) . . ?
C9 N H1 119(2) . . ?
C5 O1 C6 118.9(3) . . ?
N C1 C2 117.1(2) . . ?
N C1 P 124.53(19) . . ?
C2 C1 P 118.33(18) . . ?
C3A C2 C8 116.9(7) . . ?
C8 C2 C3B 117.6(11) . . ?
C3A C2 C1 121.3(7) . . ?
C8 C2 C1 121.5(2) . . ?
C3B C2 C1 120.2(11) . . ?
C2 C3A C4A 122.8(14) . . ?
C2 C3A H3A 118.6 . . ?
C4A C3A H3A 118.6 . . ?
C3A C4A C5 119.5(14) . . ?
C3A C4A H4A 120.2 . . ?
C5 C4A H4A 120.2 . . ?
C4B C3B C2 118(2) . . ?
C4B C3B H3B 121.2 . . ?
C2 C3B H3B 121.2 . . ?
C5 C4B C3B 122(2) . . ?
C5 C4B H4B 118.8 . . ?
C3B C4B H4B 118.8 . . ?
C4B C5 C7 118.8(13) . . ?
C4B C5 O1 114.9(12) . . ?
C7 C5 O1 125.1(3) . . ?
C7 C5 C4A 118.7(7) . . ?
O1 C5 C4A 116.1(7) . . ?
O1 C6 H6A 109.5 . . ?
O1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
O1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 C8 120.1(3) . . ?
C5 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C2 C8 C7 121.5(3) . . ?
C2 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C17 C9 C10 122.2(3) . . ?
C17 C9 N 119.6(3) . . ?
C10 C9 N 118.2(3) . . ?
C14 C10 C9 116.8(4) . . ?
C14 C10 C11 120.4(4) . . ?
C9 C10 C11 122.8(3) . . ?
C10 C11 C12 110.7(5) . . ?
C10 C11 C13 112.9(5) . . ?
C12 C11 C13 108.0(5) . . ?
C10 C11 H11 108.4 . . ?
C12 C11 H11 108.4 . . ?
C13 C11 H11 108.4 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C10 121.5(4) . . ?
C15 C14 H14 119.2 . . ?
C10 C14 H14 119.2 . . ?
C16 C15 C14 120.6(4) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 121.8(4) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C9 C17 C16 117.0(3) . . ?
C9 C17 C18 123.7(3) . . ?
C16 C17 C18 119.2(3) . . ?
C17 C18 C20 113.5(3) . . ?
C17 C18 C19 109.2(3) . . ?
C20 C18 C19 110.2(4) . . ?
C17 C18 H18 107.9 . . ?
C20 C18 H18 107.9 . . ?
C19 C18 H18 107.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C29 120.5(3) . . ?
C22 C21 P 119.7(2) . . ?
C29 C21 P 119.7(2) . . ?
C21 C22 C26 118.2(4) . . ?
C21 C22 C23 123.5(3) . . ?
C26 C22 C23 118.2(4) . . ?
C22 C23 C25 110.8(4) . . ?
C22 C23 C24 111.3(5) . . ?
C25 C23 C24 111.8(5) . . ?
C22 C23 H23 107.6 . . ?
C25 C23 H23 107.6 . . ?
C24 C23 H23 107.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C22 121.1(4) . . ?
C27 C26 H26 119.4 . . ?
C22 C26 H26 119.4 . . ?
C26 C27 C28 120.7(4) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C27 C28 C29 120.8(4) . . ?
C27 C28 H28 119.6 . . ?
C29 C28 H28 119.6 . . ?
C28 C29 C21 118.7(3) . . ?
C28 C29 C30 118.0(3) . . ?
C21 C29 C30 123.3(3) . . ?
C29 C30 C31 112.8(4) . . ?
C29 C30 C32 111.2(3) . . ?
C31 C30 C32 110.2(4) . . ?
C29 C30 H30 107.5 . . ?
C31 C30 H30 107.5 . . ?
C32 C30 H30 107.5 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O41 C41 Mo 179.8(3) . . ?
O42A C42A Mo 174.0(10) . . ?
O42B C42B Mo 174.7(17) . . ?
O43 C43 Mo 175.1(3) . . ?
O44 C44 Mo 177.2(3) . . ?
O45 C45 Mo 175.3(3) . . ?

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
C9 N C1 C2 -0.2(4) . . . . ?
C9 N C1 P 178.0(2) . . . . ?
C21 P C1 N 2.9(3) . . . . ?
Mo P C1 N -179.7(2) . . . . ?
C21 P C1 C2 -178.93(19) . . . . ?
Mo P C1 C2 -1.5(2) . . . . ?
N C1 C2 C3A 77.4(8) . . . . ?
P C1 C2 C3A -100.9(8) . . . . ?
N C1 C2 C8 -109.5(3) . . . . ?
P C1 C2 C8 72.1(3) . . . . ?
N C1 C2 C3B 60.7(12) . . . . ?
P C1 C2 C3B -117.7(12) . . . . ?
C8 C2 C3A C4A 7.6(17) . . . . ?
C1 C2 C3A C4A -179.0(12) . . . . ?
C2 C3A C4A C5 -3(2) . . . . ?
C8 C2 C3B C4B -8(3) . . . . ?
C1 C2 C3B C4B -178.4(18) . . . . ?
C2 C3B C4B C5 -4(4) . . . . ?
C3B C4B C5 C7 15(3) . . . . ?
C3B C4B C5 O1 -177(2) . . . . ?
C6 O1 C5 C4B 176.2(15) . . . . ?
C6 O1 C5 C7 -16.7(5) . . . . ?
C6 O1 C5 C4A 159.5(9) . . . . ?
C3A C4A C5 C7 -3.2(19) . . . . ?
C3A C4A C5 O1 -179.6(12) . . . . ?
C4B C5 C7 C8 -13.2(15) . . . . ?
O1 C5 C7 C8 -179.9(3) . . . . ?
C4A C5 C7 C8 4.0(10) . . . . ?
C3A C2 C8 C7 -6.6(8) . . . . ?
C3B C2 C8 C7 9.6(12) . . . . ?
C1 C2 C8 C7 180.0(3) . . . . ?
C5 C7 C8 C2 0.9(5) . . . . ?
C1 N C9 C17 78.6(4) . . . . ?
C1 N C9 C10 -100.9(4) . . . . ?
C17 C9 C10 C14 -3.1(5) . . . . ?
N C9 C10 C14 176.4(3) . . . . ?
C17 C9 C10 C11 176.1(4) . . . . ?
N C9 C10 C11 -4.4(6) . . . . ?
C14 C10 C11 C12 69.1(7) . . . . ?
C9 C10 C11 C12 -110.0(6) . . . . ?
C14 C10 C11 C13 -52.1(6) . . . . ?
C9 C10 C11 C13 128.8(5) . . . . ?
C9 C10 C14 C15 0.1(7) . . . . ?
C11 C10 C14 C15 -179.1(5) . . . . ?
C10 C14 C15 C16 1.8(8) . . . . ?
C14 C15 C16 C17 -0.6(7) . . . . ?
C10 C9 C17 C16 4.2(5) . . . . ?
N C9 C17 C16 -175.4(3) . . . . ?
C10 C9 C17 C18 -172.9(3) . . . . ?
N C9 C17 C18 7.6(5) . . . . ?
C15 C16 C17 C9 -2.3(6) . . . . ?
C15 C16 C17 C18 174.9(4) . . . . ?
C9 C17 C18 C20 -138.0(4) . . . . ?
C16 C17 C18 C20 45.0(5) . . . . ?
C9 C17 C18 C19 98.7(4) . . . . ?
C16 C17 C18 C19 -78.3(4) . . . . ?
C1 P C21 C22 -95.2(2) . . . . ?
Mo P C21 C22 87.1(2) . . . . ?
C1 P C21 C29 88.3(2) . . . . ?
Mo P C21 C29 -89.3(2) . . . . ?
C29 C21 C22 C26 -1.2(4) . . . . ?
P C21 C22 C26 -177.6(2) . . . . ?
C29 C21 C22 C23 175.5(3) . . . . ?
P C21 C22 C23 -1.0(4) . . . . ?
C21 C22 C23 C25 -107.0(4) . . . . ?
C26 C22 C23 C25 69.7(5) . . . . ?
C21 C22 C23 C24 127.9(4) . . . . ?
C26 C22 C23 C24 -55.4(5) . . . . ?
C21 C22 C26 C27 0.7(5) . . . . ?
C23 C22 C26 C27 -176.1(4) . . . . ?
C22 C26 C27 C28 0.2(7) . . . . ?
C26 C27 C28 C29 -0.7(6) . . . . ?
C27 C28 C29 C21 0.2(5) . . . . ?
C27 C28 C29 C30 178.6(3) . . . . ?
C22 C21 C29 C28 0.7(4) . . . . ?
P C21 C29 C28 177.2(2) . . . . ?
C22 C21 C29 C30 -177.6(3) . . . . ?
P C21 C29 C30 -1.2(4) . . . . ?
C28 C29 C30 C31 52.7(4) . . . . ?
C21 C29 C30 C31 -128.9(4) . . . . ?
C28 C29 C30 C32 -71.7(4) . . . . ?
C21 C29 C30 C32 106.7(4) . . . . ?

_refine_diff_density_max         0.403
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.048

_shelxl_version_number           2014/6


# start Validation Reply Form
_vrf_PLAT029_11b_MeOPAmHMoCO5    
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.938 Note  
RESPONSE: This is an older dataset collected on an image-plate diffractometer 
at ambient temperature. The instrument was not equipped for LT measurements.
Crystals are not available for redetermination on a modern diffractometer. 
The structure is of reasonable quality in most regards and reliable for
the application in this publication.
;
_vrf_PLAT910_11b_MeOPAmHMoCO5    
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ... 11 Report
RESPONSE: One low-angle rfl was omitted due to very poor agreement.
;
_vrf_PLAT911_11b_MeOPAmHMoCO5    
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 411 Report
RESPONSE: Also caused by it being an older dataset on an image-plate
diffractometer. Images are not available for a re-assessment.
;
# end Validation Reply Form




_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Heptane'
_chemical_compound_source        No
_chemical_properties_physical    'Air-sensitive, Light-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_12_TolPAmHWCO5
_database_code_depnum_ccdc_archive 'CCDC 1421320'
_audit_update_record             
;
2015-09-29 deposited with the CCDC.
2015-10-02 downloaded from the CCDC.
;
#  Shelxtl code: 0145

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        
'(aZ)-N-[2,6-bis(1-methylethyl)phenyl]-a-[[2,6-bis(1-methylethyl)phenyl] phosphinidene]-4-methyl-benzenemethanamine tungsten pentacarbonyl complex'
_chemical_name_common            
'1,3-bis(2,6-diisopropylphenyl)-2-(4-methylphenyl)-3-aza-1λ3-phosphapropene tungsten pentacarbonyl complex'
_chemical_melting_point          443
_chemical_formula_moiety         'C37 H42 N O5 P W'
_chemical_formula_sum            'C37 H42 N O5 P W'
_chemical_formula_weight         795.53

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.5413(9)
_cell_length_b                   12.2130(11)
_cell_length_c                   14.8135(14)
_cell_angle_alpha                84.662(11)
_cell_angle_beta                 79.167(11)
_cell_angle_gamma                71.661(10)
_cell_volume                     1776.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      26

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    3.337
_shelx_estimated_absorpt_T_min   0.380
_shelx_estimated_absorpt_T_max   0.501
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_T_max  0.704
_exptl_absorpt_process_details   
;
 SHELXA
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       Phi-Oscillation
_diffrn_reflns_number            25048
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_av_R_equivalents  0.1372
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.802
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_full        25.250
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measured_fraction_theta_full 0.939
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_Laue_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 0.939
_reflns_number_total             6327
_reflns_number_gt                5641
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Stoe IPDS V2.63'
_computing_cell_refinement       'Stoe IPDS V2.63'
_computing_data_reduction        'Stoe IPDS V2.63'
_computing_structure_solution    'SIR97 (Giacovazzo et al., 1997)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
# Bruker (2008). APEX2, SAINT-Plus and SADABS. Bruker AXS Inc., Madison
# Wisconsin, USA.
# Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8.
# Sheldrick, G. M. (2002). TWINABS, University of Gttingen.
# Macrae, C. F., Bruno, I. J., Chisholm, J. A., Edgington, P. R., McCabe, P.,
# Pidcock, E., Rodriguez-Monge, L., Taylor, R., van de Streek, J. & Wood,
# P. A. (2008). J. Appl. Cryst. 41, 466-470.
# Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.

_refine_special_details          
;
 RIGU restraints added to improve description of the thermal ellipsoids. See:
 A. Thorn, B. Dittrich and G. M. Sheldrick, Acta Cryst. (2012). A68, 448-451.
 The N-H bond refines unusually short, so a distance restraint was 
 added to try and improve this parameter.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0857P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6327
_refine_ls_number_parameters     418
_refine_ls_number_restraints     361
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1302
_refine_ls_wR_factor_gt          0.1279
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
W W -0.05767(2) 0.84250(2) 0.70925(2) 0.04558(11) Uani 1 1 d . U . . .
P P 0.14349(17) 0.72663(12) 0.78431(11) 0.0480(3) Uani 1 1 d . U . . .
N N 0.3481(5) 0.5371(4) 0.8149(3) 0.0469(10) Uani 1 1 d D U . . .
H1 H 0.389(7) 0.577(5) 0.839(5) 0.056 Uiso 1 1 d D U . . .
C1 C 0.2368(6) 0.5846(4) 0.7759(3) 0.0425(10) Uani 1 1 d . U . . .
C2 C 0.1924(6) 0.5087(4) 0.7251(3) 0.0427(11) Uani 1 1 d . U . . .
C3 C 0.1527(7) 0.4146(5) 0.7666(4) 0.0531(14) Uani 1 1 d . U . . .
H3 H 0.1495 0.4001 0.8296 0.064 Uiso 1 1 calc R U . . .
C4 C 0.1179(8) 0.3424(6) 0.7154(5) 0.0605(16) Uani 1 1 d . U . . .
H4 H 0.0932 0.2795 0.7445 0.073 Uiso 1 1 calc R U . . .
C5 C 0.1191(8) 0.3621(6) 0.6224(5) 0.0589(15) Uani 1 1 d . U . . .
C6 C 0.0837(11) 0.2824(7) 0.5668(6) 0.082(2) Uani 1 1 d . U . . .
H6A H 0.1646 0.2367 0.5297 0.124 Uiso 1 1 calc R U . . .
H6B H 0.0214 0.3270 0.5278 0.124 Uiso 1 1 calc R U . . .
H6C H 0.0426 0.2325 0.6074 0.124 Uiso 1 1 calc R U . . .
C7 C 0.1554(8) 0.4572(5) 0.5808(4) 0.0557(14) Uani 1 1 d . U . . .
H7 H 0.1555 0.4724 0.5181 0.067 Uiso 1 1 calc R U . . .
C8 C 0.1913(7) 0.5295(5) 0.6307(4) 0.0496(12) Uani 1 1 d . U . . .
H8 H 0.2150 0.5926 0.6012 0.059 Uiso 1 1 calc R U . . .
C9 C 0.4152(6) 0.4153(4) 0.8264(4) 0.0436(11) Uani 1 1 d . U . . .
C10 C 0.3926(7) 0.3599(5) 0.9127(4) 0.0505(13) Uani 1 1 d . U . . .
C11 C 0.3140(7) 0.4261(5) 0.9981(4) 0.0561(14) Uani 1 1 d . U . . .
H11 H 0.3005 0.5082 0.9825 0.067 Uiso 1 1 calc R U . . .
C12 C 0.3939(10) 0.3949(8) 1.0762(6) 0.081(2) Uani 1 1 d . U . . .
H12A H 0.3502 0.4478 1.1248 0.121 Uiso 1 1 calc R U . . .
H12B H 0.4840 0.3994 1.0546 0.121 Uiso 1 1 calc R U . . .
H12C H 0.3985 0.3178 1.0989 0.121 Uiso 1 1 calc R U . . .
C13 C 0.1759(9) 0.4105(9) 1.0265(6) 0.084(2) Uani 1 1 d . U . . .
H13A H 0.1847 0.3296 1.0333 0.126 Uiso 1 1 calc R U . . .
H13B H 0.1212 0.4453 0.9803 0.126 Uiso 1 1 calc R U . . .
H13C H 0.1337 0.4465 1.0840 0.126 Uiso 1 1 calc R U . . .
C14 C 0.4476(8) 0.2426(5) 0.9190(5) 0.0601(15) Uani 1 1 d . U . . .
H14 H 0.4338 0.2046 0.9756 0.072 Uiso 1 1 calc R U . . .
C15 C 0.5226(9) 0.1789(5) 0.8445(5) 0.0678(18) Uani 1 1 d . U . . .
H15 H 0.5544 0.0988 0.8500 0.081 Uiso 1 1 calc R U . . .
C16 C 0.5498(8) 0.2349(5) 0.7624(5) 0.0645(17) Uani 1 1 d . U . . .
H16 H 0.6047 0.1922 0.7130 0.077 Uiso 1 1 calc R U . . .
C17 C 0.4976(7) 0.3536(5) 0.7508(4) 0.0505(12) Uani 1 1 d . U . . .
C18 C 0.5374(8) 0.4127(6) 0.6598(5) 0.0670(17) Uani 1 1 d . U . . .
H18 H 0.4734 0.4906 0.6578 0.080 Uiso 1 1 calc R U . . .
C19 C 0.6785(12) 0.4235(11) 0.6566(7) 0.104(3) Uani 1 1 d . U . . .
H19A H 0.7433 0.3479 0.6565 0.157 Uiso 1 1 calc R U . . .
H19B H 0.6791 0.4630 0.7095 0.157 Uiso 1 1 calc R U . . .
H19C H 0.7019 0.4663 0.6017 0.157 Uiso 1 1 calc R U . . .
C20 C 0.5333(11) 0.3500(8) 0.5773(6) 0.089(2) Uani 1 1 d . U . . .
H20A H 0.6064 0.2790 0.5718 0.134 Uiso 1 1 calc R U . . .
H20B H 0.5423 0.3977 0.5227 0.134 Uiso 1 1 calc R U . . .
H20C H 0.4484 0.3336 0.5853 0.134 Uiso 1 1 calc R U . . .
C21 C 0.2391(6) 0.7984(4) 0.8367(4) 0.0464(11) Uani 1 1 d . U . . .
C22 C 0.2110(6) 0.8133(5) 0.9324(4) 0.0501(12) Uani 1 1 d . U . . .
C23 C 0.1211(8) 0.7567(5) 0.9986(5) 0.0589(15) Uani 1 1 d . U . . .
H23 H 0.1129 0.6924 0.9676 0.071 Uiso 1 1 calc R U . . .
C24 C 0.1778(10) 0.7080(7) 1.0870(5) 0.075(2) Uani 1 1 d . U . . .
H24A H 0.2731 0.6687 1.0719 0.112 Uiso 1 1 calc R U . . .
H24B H 0.1321 0.6547 1.1178 0.112 Uiso 1 1 calc R U . . .
H24C H 0.1638 0.7700 1.1268 0.112 Uiso 1 1 calc R U . . .
C25 C -0.0203(9) 0.8413(8) 1.0230(6) 0.076(2) Uani 1 1 d . U . . .
H25A H -0.0161 0.9021 1.0579 0.114 Uiso 1 1 calc R U . . .
H25B H -0.0793 0.8016 1.0589 0.114 Uiso 1 1 calc R U . . .
H25C H -0.0547 0.8735 0.9676 0.114 Uiso 1 1 calc R U . . .
C26 C 0.2710(8) 0.8834(6) 0.9679(5) 0.0628(15) Uani 1 1 d . U . . .
H26 H 0.2549 0.8932 1.0310 0.075 Uiso 1 1 calc R U . . .
C27 C 0.3530(9) 0.9378(6) 0.9111(5) 0.0668(17) Uani 1 1 d . U . . .
H27 H 0.3884 0.9870 0.9356 0.080 Uiso 1 1 calc R U . . .
C28 C 0.3830(8) 0.9199(6) 0.8189(5) 0.0651(16) Uani 1 1 d . U . . .
H28 H 0.4416 0.9552 0.7820 0.078 Uiso 1 1 calc R U . . .
C29 C 0.3287(7) 0.8505(6) 0.7782(5) 0.0572(14) Uani 1 1 d . U . . .
C30 C 0.3707(9) 0.8312(8) 0.6771(5) 0.0722(18) Uani 1 1 d . U . . .
H30 H 0.3137 0.7898 0.6594 0.087 Uiso 1 1 calc R U . . .
C31 C 0.5158(12) 0.7556(10) 0.6572(7) 0.095(3) Uani 1 1 d . U . . .
H31A H 0.5398 0.7393 0.5930 0.143 Uiso 1 1 calc R U . . .
H31B H 0.5257 0.6845 0.6929 0.143 Uiso 1 1 calc R U . . .
H31C H 0.5742 0.7946 0.6730 0.143 Uiso 1 1 calc R U . . .
C32 C 0.3518(13) 0.9414(10) 0.6194(7) 0.107(3) Uani 1 1 d . U . . .
H32A H 0.2594 0.9891 0.6332 0.160 Uiso 1 1 calc R U . . .
H32B H 0.3735 0.9237 0.5555 0.160 Uiso 1 1 calc R U . . .
H32C H 0.4107 0.9817 0.6327 0.160 Uiso 1 1 calc R U . . .
C41 C -0.2101(8) 0.9382(6) 0.6484(5) 0.0605(15) Uani 1 1 d . U . . .
O41 O -0.2980(7) 0.9916(5) 0.6128(5) 0.0920(19) Uani 1 1 d . U . . .
O42 O -0.1460(7) 0.6213(5) 0.6894(5) 0.0843(18) Uani 1 1 d . U . . .
C42 C -0.1084(7) 0.6983(5) 0.6949(5) 0.0560(14) Uani 1 1 d . U . . .
O43 O 0.1236(7) 0.8351(6) 0.5109(4) 0.092(2) Uani 1 1 d . U . . .
C43 C 0.0648(8) 0.8339(6) 0.5822(5) 0.0604(15) Uani 1 1 d . U . . .
C44 C -0.0184(8) 0.9874(5) 0.7330(5) 0.0604(15) Uani 1 1 d . U . . .
O44 O 0.0018(9) 1.0706(5) 0.7468(6) 0.100(2) Uani 1 1 d . U . . .
O45 O -0.2818(6) 0.8906(5) 0.8886(4) 0.0780(15) Uani 1 1 d . U . . .
C45 C -0.1968(7) 0.8686(5) 0.8271(5) 0.0574(14) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W C41 1.982(7) . ?
W C44 2.015(7) . ?
W C42 2.034(7) . ?
W C45 2.036(7) . ?
W C43 2.063(8) . ?
W P 2.5378(16) . ?
P C1 1.706(5) . ?
P C21 1.834(6) . ?
N C1 1.346(8) . ?
N C9 1.441(7) . ?
N H1 0.88(2) . ?
C1 C2 1.477(8) . ?
C2 C3 1.396(7) . ?
C2 C8 1.400(7) . ?
C3 C4 1.385(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(9) . ?
C4 H4 0.9300 . ?
C5 C7 1.391(9) . ?
C5 C6 1.503(9) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.380(9) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C17 1.398(8) . ?
C9 C10 1.406(8) . ?
C10 C14 1.367(8) . ?
C10 C11 1.521(8) . ?
C11 C13 1.504(11) . ?
C11 C12 1.508(11) . ?
C11 H11 0.9800 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.376(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.366(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.386(9) . ?
C16 H16 0.9300 . ?
C17 C18 1.520(9) . ?
C18 C20 1.515(12) . ?
C18 C19 1.526(14) . ?
C18 H18 0.9800 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.410(8) . ?
C21 C29 1.419(9) . ?
C22 C26 1.399(9) . ?
C22 C23 1.508(9) . ?
C23 C25 1.522(11) . ?
C23 C24 1.535(11) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.371(11) . ?
C26 H26 0.9300 . ?
C27 C28 1.365(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.392(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.499(10) . ?
C30 C32 1.504(12) . ?
C30 C31 1.507(14) . ?
C30 H30 0.9800 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C41 O41 1.141(9) . ?
O42 C42 1.144(9) . ?
O43 C43 1.121(10) . ?
C44 O44 1.145(9) . ?
O45 C45 1.138(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
C41 W C44 89.2(3) . . ?
C41 W C42 90.5(3) . . ?
C44 W C42 175.4(3) . . ?
C41 W C45 85.2(3) . . ?
C44 W C45 88.1(3) . . ?
C42 W C45 87.2(3) . . ?
C41 W C43 87.5(3) . . ?
C44 W C43 89.8(3) . . ?
C42 W C43 94.8(3) . . ?
C45 W C43 172.4(3) . . ?
C41 W P 177.3(2) . . ?
C44 W P 88.6(2) . . ?
C42 W P 91.8(2) . . ?
C45 W P 96.2(2) . . ?
C43 W P 91.0(2) . . ?
C1 P C21 107.1(3) . . ?
C1 P W 130.3(2) . . ?
C21 P W 121.09(18) . . ?
C1 N C9 125.9(5) . . ?
C1 N H1 124(5) . . ?
C9 N H1 110(5) . . ?
N C1 C2 117.9(5) . . ?
N C1 P 123.3(4) . . ?
C2 C1 P 118.8(4) . . ?
C3 C2 C8 117.5(5) . . ?
C3 C2 C1 123.0(5) . . ?
C8 C2 C1 119.4(5) . . ?
C4 C3 C2 121.1(5) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 121.2(6) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C7 118.2(6) . . ?
C4 C5 C6 121.1(6) . . ?
C7 C5 C6 120.8(6) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C5 121.4(6) . . ?
C8 C7 H7 119.3 . . ?
C5 C7 H7 119.3 . . ?
C7 C8 C2 120.6(5) . . ?
C7 C8 H8 119.7 . . ?
C2 C8 H8 119.7 . . ?
C17 C9 C10 121.2(5) . . ?
C17 C9 N 119.6(5) . . ?
C10 C9 N 119.2(5) . . ?
C14 C10 C9 117.7(6) . . ?
C14 C10 C11 119.9(6) . . ?
C9 C10 C11 122.4(5) . . ?
C13 C11 C12 111.5(7) . . ?
C13 C11 C10 112.1(6) . . ?
C12 C11 C10 111.3(6) . . ?
C13 C11 H11 107.2 . . ?
C12 C11 H11 107.2 . . ?
C10 C11 H11 107.2 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 C15 122.3(6) . . ?
C10 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C16 C15 C14 119.1(6) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
C15 C16 C17 121.8(6) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C16 C17 C9 117.8(6) . . ?
C16 C17 C18 119.7(6) . . ?
C9 C17 C18 122.4(5) . . ?
C20 C18 C17 112.9(7) . . ?
C20 C18 C19 110.8(7) . . ?
C17 C18 C19 108.6(7) . . ?
C20 C18 H18 108.2 . . ?
C17 C18 H18 108.2 . . ?
C19 C18 H18 108.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C29 120.9(5) . . ?
C22 C21 P 120.0(5) . . ?
C29 C21 P 118.7(5) . . ?
C26 C22 C21 118.2(6) . . ?
C26 C22 C23 118.3(6) . . ?
C21 C22 C23 123.5(5) . . ?
C22 C23 C25 110.4(6) . . ?
C22 C23 C24 113.3(7) . . ?
C25 C23 C24 109.5(6) . . ?
C22 C23 H23 107.8 . . ?
C25 C23 H23 107.8 . . ?
C24 C23 H23 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C22 121.0(7) . . ?
C27 C26 H26 119.5 . . ?
C22 C26 H26 119.5 . . ?
C28 C27 C26 120.3(6) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 122.3(7) . . ?
C27 C28 H28 118.9 . . ?
C29 C28 H28 118.9 . . ?
C28 C29 C21 117.3(6) . . ?
C28 C29 C30 119.2(6) . . ?
C21 C29 C30 123.5(6) . . ?
C29 C30 C32 113.4(8) . . ?
C29 C30 C31 110.0(7) . . ?
C32 C30 C31 110.3(8) . . ?
C29 C30 H30 107.6 . . ?
C32 C30 H30 107.6 . . ?
C31 C30 H30 107.6 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O41 C41 W 178.9(7) . . ?
O42 C42 W 175.2(6) . . ?
O43 C43 W 174.9(8) . . ?
O44 C44 W 178.9(8) . . ?
O45 C45 W 173.9(6) . . ?

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
C9 N C1 C2 -11.8(8) . . . . ?
C9 N C1 P 166.8(4) . . . . ?
C21 P C1 N 9.2(5) . . . . ?
W P C1 N 174.8(3) . . . . ?
C21 P C1 C2 -172.2(4) . . . . ?
W P C1 C2 -6.6(5) . . . . ?
N C1 C2 C3 61.8(8) . . . . ?
P C1 C2 C3 -116.8(6) . . . . ?
N C1 C2 C8 -117.1(6) . . . . ?
P C1 C2 C8 64.2(7) . . . . ?
C8 C2 C3 C4 2.1(10) . . . . ?
C1 C2 C3 C4 -176.9(6) . . . . ?
C2 C3 C4 C5 -1.1(12) . . . . ?
C3 C4 C5 C7 -0.5(12) . . . . ?
C3 C4 C5 C6 178.9(8) . . . . ?
C4 C5 C7 C8 0.9(11) . . . . ?
C6 C5 C7 C8 -178.4(8) . . . . ?
C5 C7 C8 C2 0.1(11) . . . . ?
C3 C2 C8 C7 -1.6(10) . . . . ?
C1 C2 C8 C7 177.4(6) . . . . ?
C1 N C9 C17 76.7(8) . . . . ?
C1 N C9 C10 -101.0(7) . . . . ?
C17 C9 C10 C14 -3.6(10) . . . . ?
N C9 C10 C14 174.0(6) . . . . ?
C17 C9 C10 C11 174.3(6) . . . . ?
N C9 C10 C11 -8.0(9) . . . . ?
C14 C10 C11 C13 -74.7(9) . . . . ?
C9 C10 C11 C13 107.4(8) . . . . ?
C14 C10 C11 C12 50.9(9) . . . . ?
C9 C10 C11 C12 -127.0(7) . . . . ?
C9 C10 C14 C15 -0.2(11) . . . . ?
C11 C10 C14 C15 -178.2(7) . . . . ?
C10 C14 C15 C16 3.7(13) . . . . ?
C14 C15 C16 C17 -3.5(13) . . . . ?
C15 C16 C17 C9 -0.1(11) . . . . ?
C15 C16 C17 C18 176.4(8) . . . . ?
C10 C9 C17 C16 3.8(10) . . . . ?
N C9 C17 C16 -173.9(6) . . . . ?
C10 C9 C17 C18 -172.7(6) . . . . ?
N C9 C17 C18 9.6(9) . . . . ?
C16 C17 C18 C20 44.7(10) . . . . ?
C9 C17 C18 C20 -138.9(7) . . . . ?
C16 C17 C18 C19 -78.5(9) . . . . ?
C9 C17 C18 C19 97.9(9) . . . . ?
C1 P C21 C22 -95.0(5) . . . . ?
W P C21 C22 97.7(5) . . . . ?
C1 P C21 C29 92.6(5) . . . . ?
W P C21 C29 -74.6(5) . . . . ?
C29 C21 C22 C26 1.7(9) . . . . ?
P C21 C22 C26 -170.5(5) . . . . ?
C29 C21 C22 C23 -177.6(6) . . . . ?
P C21 C22 C23 10.2(8) . . . . ?
C26 C22 C23 C25 81.3(8) . . . . ?
C21 C22 C23 C25 -99.3(7) . . . . ?
C26 C22 C23 C24 -41.9(8) . . . . ?
C21 C22 C23 C24 137.4(6) . . . . ?
C21 C22 C26 C27 1.1(11) . . . . ?
C23 C22 C26 C27 -179.6(7) . . . . ?
C22 C26 C27 C28 -3.2(13) . . . . ?
C26 C27 C28 C29 2.5(13) . . . . ?
C27 C28 C29 C21 0.3(12) . . . . ?
C27 C28 C29 C30 -177.6(8) . . . . ?
C22 C21 C29 C28 -2.4(10) . . . . ?
P C21 C29 C28 169.9(6) . . . . ?
C22 C21 C29 C30 175.4(7) . . . . ?
P C21 C29 C30 -12.3(10) . . . . ?
C28 C29 C30 C32 -53.5(11) . . . . ?
C21 C29 C30 C32 128.7(8) . . . . ?
C28 C29 C30 C31 70.6(10) . . . . ?
C21 C29 C30 C31 -107.2(9) . . . . ?

_refine_diff_density_max         2.494
_refine_diff_density_min         -2.814
_refine_diff_density_rms         0.172

_shelxl_version_number           2014/6

# start Validation Reply Form
_vrf_PLAT029_12_TolPAmHWCO5      
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.938 Note  
RESPONSE: This is an older dataset collected on an image-plate diffractometer 
at ambient temperature. The instrument was not equipped for LT measurements.
Crystals are not available for redetermination on a modern diffractometer. 
The structure is of reasonable quality in most regards and reliable for
the application in this publication.
;
# end Validation Reply Form



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Tetrahydrofuran'
_chemical_compound_source        No
_chemical_properties_physical    'Air-sensitive, Light-sensitive'
