# 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_2b(trans)
_database_code_depnum_ccdc_archive 'CCDC 888516'
_audit_update_record             
;
2013-09-11 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;\
(bis{2-[bis(1-methylethyl)phosphanyl-κP]ethyl}carbamato-κ²N,\
O)(carbonyl)(nitrosyl)tungsten 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H36 N2 O4 P2 W'
_chemical_formula_sum            'C18 H36 N2 O4 P2 W'
_chemical_formula_weight         590.28

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   7.8847(1)
_cell_length_b                   26.3644(4)
_cell_length_c                   11.5872(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.979(2)
_cell_angle_gamma                90.00
_cell_volume                     2303.70(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    27135
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      32.67

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    5.178
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_T_max  0.432
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Version 1.171.35.11 (Agilent, 2011).
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid (1995).
;

_exptl_special_details           ?

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37089
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         28.28
_reflns_number_total             5720
_reflns_number_gt                5574
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_cell_refinement       
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_data_reduction        
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_structure_solution    
; SHELXS97 (Sheldrick, 2008) 
;
_computing_structure_refinement  
; SHELXL97 (Sheldrick, 2008)
;
_computing_molecular_graphics    
;
DIAMOND (Brandenburg, 2006) 
;
_computing_publication_material  
; 
WinGX (Farrugia, 1999), PLATON for Windows (Spek, 2003) and
publCIF (Westrip, 2010)
;

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

All hydrogen positions were calculated after each cycle of refinement using a
riding model, with C---H = 0.97 Å and Uiso(H) = 1.2Ueq(C)
for methylene H atoms, with C---H = 0.98 Å and Uiso(H) =
1.2Ueq(C) for methine H atoms, and with C---H = 0.96 Å and
Uiso(H) = 1.5Ueq(C) for methyl H atoms. No classic hydrogen
 bonds found.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0093P)²+2.1311P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5720
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0203
_refine_ls_wR_factor_ref         0.0403
_refine_ls_wR_factor_gt          0.0400
_refine_ls_goodness_of_fit_ref   1.294
_refine_ls_restrained_S_all      1.294
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9429(3) 0.15311(10) 0.2801(2) 0.0250(5) Uani 1 1 d . . .
C2 C 0.5948(3) 0.02971(9) 0.2558(2) 0.0214(5) Uani 1 1 d . . .
C3 C 0.4417(3) 0.18271(10) -0.0234(2) 0.0260(5) Uani 1 1 d . . .
H3 H 0.5273 0.2105 -0.0138 0.031 Uiso 1 1 calc R . .
C4 C 0.3014(4) 0.19968(12) 0.0358(3) 0.0350(7) Uani 1 1 d . . .
H4A H 0.2511 0.2314 0.0015 0.052 Uiso 1 1 calc R . .
H4B H 0.3553 0.2038 0.1210 0.052 Uiso 1 1 calc R . .
H4C H 0.2097 0.1745 0.0222 0.052 Uiso 1 1 calc R . .
C5 C 0.3563(4) 0.17531(13) -0.1588(3) 0.0413(8) Uani 1 1 d . . .
H5A H 0.2703 0.1485 -0.1716 0.062 Uiso 1 1 calc R . .
H5B H 0.4460 0.1666 -0.1963 0.062 Uiso 1 1 calc R . .
H5C H 0.2989 0.2062 -0.1934 0.062 Uiso 1 1 calc R . .
C6 C 0.7011(3) 0.10688(11) -0.0462(2) 0.0257(5) Uani 1 1 d . . .
H6 H 0.6223 0.0983 -0.1262 0.031 Uiso 1 1 calc R . .
C7 C 0.8193(4) 0.15142(12) -0.0580(2) 0.0321(6) Uani 1 1 d . . .
H7A H 0.8839 0.1633 0.0209 0.048 Uiso 1 1 calc R . .
H7B H 0.7469 0.1784 -0.1021 0.048 Uiso 1 1 calc R . .
H7C H 0.9011 0.1405 -0.1001 0.048 Uiso 1 1 calc R . .
C8 C 0.8151(4) 0.06071(12) 0.0056(3) 0.0342(6) Uani 1 1 d . . .
H8A H 0.8827 0.0510 -0.0476 0.051 Uiso 1 1 calc R . .
H8B H 0.7399 0.0331 0.0135 0.051 Uiso 1 1 calc R . .
H8C H 0.8942 0.0690 0.0834 0.051 Uiso 1 1 calc R . .
C9 C 0.3947(3) 0.07696(10) 0.0348(2) 0.0238(5) Uani 1 1 d . . .
H9A H 0.2968 0.0840 -0.0365 0.029 Uiso 1 1 calc R . .
H9B H 0.4443 0.0443 0.0238 0.029 Uiso 1 1 calc R . .
C10 C 0.3264(3) 0.07489(10) 0.1451(2) 0.0228(5) Uani 1 1 d . . .
H10A H 0.2512 0.1040 0.1447 0.027 Uiso 1 1 calc R . .
H10B H 0.2555 0.0445 0.1415 0.027 Uiso 1 1 calc R . .
C11 C 0.4092(3) 0.07084(10) 0.3662(2) 0.0231(5) Uani 1 1 d . . .
H11A H 0.3278 0.0425 0.3559 0.028 Uiso 1 1 calc R . .
H11B H 0.3450 0.1015 0.3731 0.028 Uiso 1 1 calc R . .
C12 C 0.5624(3) 0.06339(10) 0.4811(2) 0.0236(5) Uani 1 1 d . . .
H12A H 0.6054 0.0288 0.4838 0.028 Uiso 1 1 calc R . .
H12B H 0.5198 0.0685 0.5507 0.028 Uiso 1 1 calc R . .
C13 C 0.9381(3) 0.06785(11) 0.5705(2) 0.0270(6) Uani 1 1 d . . .
H13 H 0.9212 0.0352 0.5283 0.032 Uiso 1 1 calc R . .
C14 C 0.9452(4) 0.05604(12) 0.7007(2) 0.0338(6) Uani 1 1 d . . .
H14A H 1.0299 0.0295 0.7312 0.051 Uiso 1 1 calc R . .
H14B H 0.8302 0.0452 0.7036 0.051 Uiso 1 1 calc R . .
H14C H 0.9799 0.0859 0.7492 0.051 Uiso 1 1 calc R . .
C15 C 1.1145(4) 0.08829(14) 0.5620(3) 0.0432(8) Uani 1 1 d . . .
H15A H 1.1366 0.1209 0.6003 0.065 Uiso 1 1 calc R . .
H15B H 1.1103 0.0916 0.4787 0.065 Uiso 1 1 calc R . .
H15C H 1.2078 0.0653 0.6016 0.065 Uiso 1 1 calc R . .
C16 C 0.7199(4) 0.15804(10) 0.5927(2) 0.0257(5) Uani 1 1 d . . .
H16 H 0.7403 0.1429 0.6728 0.031 Uiso 1 1 calc R . .
C17 C 0.8547(4) 0.20073(12) 0.6034(3) 0.0403(7) Uani 1 1 d . . .
H17A H 0.8437 0.2145 0.5249 0.060 Uiso 1 1 calc R . .
H17B H 0.9723 0.1876 0.6373 0.060 Uiso 1 1 calc R . .
H17C H 0.8328 0.2269 0.6549 0.060 Uiso 1 1 calc R . .
C18 C 0.5308(4) 0.17906(11) 0.5535(3) 0.0316(6) Uani 1 1 d . . .
H18A H 0.5196 0.2052 0.6084 0.047 Uiso 1 1 calc R . .
H18B H 0.4485 0.1523 0.5539 0.047 Uiso 1 1 calc R . .
H18C H 0.5055 0.1928 0.4736 0.047 Uiso 1 1 calc R . .
N1 N 0.6421(3) 0.19345(8) 0.28873(17) 0.0205(4) Uani 1 1 d . . .
N2 N 0.4771(3) 0.07465(8) 0.25918(17) 0.0181(4) Uani 1 1 d . . .
O1 O 1.0838(3) 0.16676(9) 0.2828(2) 0.0438(6) Uani 1 1 d . . .
O2 O 0.6004(3) 0.23680(7) 0.30062(17) 0.0356(5) Uani 1 1 d . . .
O3 O 0.7506(2) 0.04650(7) 0.26377(16) 0.0237(4) Uani 1 1 d . . .
O4 O 0.5375(3) -0.01304(7) 0.24741(18) 0.0330(4) Uani 1 1 d . . .
P1 P 0.56579(8) 0.12643(2) 0.05210(5) 0.01864(12) Uani 1 1 d . . .
P2 P 0.74744(8) 0.10777(2) 0.48901(5) 0.01853(12) Uani 1 1 d . . .
W1 W 0.704076(12) 0.129037(3) 0.273888(8) 0.01562(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.159(3) . ?
C1 W1 1.969(3) . ?
C2 O4 1.208(3) . ?
C2 O3 1.283(3) . ?
C2 N2 1.512(3) . ?
C3 C5 1.528(4) . ?
C3 C4 1.530(4) . ?
C3 P1 1.851(3) . ?
C3 H3 0.9800 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C8 1.528(4) . ?
C6 C7 1.530(4) . ?
C6 P1 1.847(3) . ?
C6 H6 0.9800 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.526(4) . ?
C9 P1 1.845(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.498(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.491(3) . ?
C11 C12 1.526(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 P2 1.852(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C15 1.521(4) . ?
C13 C14 1.526(4) . ?
C13 P2 1.852(3) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.528(4) . ?
C16 C18 1.530(4) . ?
C16 P2 1.844(3) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
N1 O2 1.208(3) . ?
N1 W1 1.789(2) . ?
N2 W1 2.2603(19) . ?
O3 W1 2.2155(18) . ?
P1 W1 2.4822(6) . ?
P2 W1 2.4793(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 W1 179.1(3) . . ?
O4 C2 O3 130.9(2) . . ?
O4 C2 N2 121.0(2) . . ?
O3 C2 N2 108.0(2) . . ?
C5 C3 C4 109.8(2) . . ?
C5 C3 P1 113.4(2) . . ?
C4 C3 P1 111.96(18) . . ?
C5 C3 H3 107.1 . . ?
C4 C3 H3 107.1 . . ?
P1 C3 H3 107.1 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C8 C6 C7 110.1(2) . . ?
C8 C6 P1 111.07(18) . . ?
C7 C6 P1 108.51(19) . . ?
C8 C6 H6 109.1 . . ?
C7 C6 H6 109.1 . . ?
P1 C6 H6 109.1 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 111.12(17) . . ?
C10 C9 H9A 109.4 . . ?
P1 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
P1 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 C9 110.86(19) . . ?
N2 C10 H10A 109.5 . . ?
C9 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
N2 C11 C12 110.4(2) . . ?
N2 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N2 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
C11 C12 P2 111.93(17) . . ?
C11 C12 H12A 109.2 . . ?
P2 C12 H12A 109.2 . . ?
C11 C12 H12B 109.2 . . ?
P2 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C15 C13 C14 111.5(2) . . ?
C15 C13 P2 112.8(2) . . ?
C14 C13 P2 114.18(19) . . ?
C15 C13 H13 105.9 . . ?
C14 C13 H13 105.9 . . ?
P2 C13 H13 105.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C18 110.6(2) . . ?
C17 C16 P2 111.79(19) . . ?
C18 C16 P2 110.91(18) . . ?
C17 C16 H16 107.8 . . ?
C18 C16 H16 107.8 . . ?
P2 C16 H16 107.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O2 N1 W1 178.97(18) . . ?
C11 N2 C10 110.45(18) . . ?
C11 N2 C2 109.93(18) . . ?
C10 N2 C2 108.37(18) . . ?
C11 N2 W1 116.67(15) . . ?
C10 N2 W1 118.08(14) . . ?
C2 N2 W1 91.18(13) . . ?
C2 O3 W1 99.96(15) . . ?
C9 P1 C6 105.76(12) . . ?
C9 P1 C3 104.28(12) . . ?
C6 P1 C3 104.64(12) . . ?
C9 P1 W1 102.61(8) . . ?
C6 P1 W1 119.21(8) . . ?
C3 P1 W1 118.63(9) . . ?
C16 P2 C12 104.22(12) . . ?
C16 P2 C13 108.00(12) . . ?
C12 P2 C13 100.20(12) . . ?
C16 P2 W1 118.98(9) . . ?
C12 P2 W1 102.57(8) . . ?
C13 P2 W1 119.60(9) . . ?
N1 W1 C1 88.61(10) . . ?
N1 W1 O3 172.47(8) . . ?
C1 W1 O3 98.47(9) . . ?
N1 W1 N2 112.15(8) . . ?
C1 W1 N2 159.24(9) . . ?
O3 W1 N2 60.83(7) . . ?
N1 W1 P2 94.55(6) . . ?
C1 W1 P2 100.76(7) . . ?
O3 W1 P2 81.65(5) . . ?
N2 W1 P2 78.82(5) . . ?
N1 W1 P1 94.37(6) . . ?
C1 W1 P1 99.96(7) . . ?
O3 W1 P1 86.99(5) . . ?
N2 W1 P1 78.79(5) . . ?
P2 W1 P1 157.60(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.657
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.076

###########################################################


####################################################################### 
# 
# 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_4b(cis)
_database_code_depnum_ccdc_archive 'CCDC 888517'
_audit_update_record             
;
2013-09-11 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;\
(2-[bis(1-methylethyl)phosphanyl-κP]-N-{2-[bis(1-methylethyl)\
phosphanyl-κP]ethyl}ethanamine-κN)(carbonyl)(formato-\
κO)(nitrosyl)tungsten tetrahydrofuran solvate (8/1)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '8(C18 H38 N2 O4 P2 W), C4 H8 O'
_chemical_formula_sum            'C148 H312 N16 O33 P16 W8'
_chemical_formula_weight         4810.46

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'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-y+3/4, x+1/4, z+1/4'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'x, y-1/2, -z'
'y-3/4, -x-1/4, -z-1/4'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   36.3651(6)
_cell_length_b                   36.3651(6)
_cell_length_c                   14.8550(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     19644.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    6283
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      29.40

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9632
_exptl_absorpt_coefficient_mu    4.859
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Version 1.171.35.11 (Agilent Technologies, 2011)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid (1995).
;

_exptl_special_details           ?

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27807
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.1115
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         25.68
_reflns_number_total             9319
_reflns_number_gt                5971
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_cell_refinement       
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_data_reduction        
;
CrysAlisPro, version 1.171.35.11 (Agilent, 2011)
;
_computing_structure_solution    
; SHELXS97 (Sheldrick, 2008) 
;
_computing_structure_refinement  
; SHELXL97 (Sheldrick, 2008)
;
_computing_molecular_graphics    
;
DIAMOND (Brandenburg, 2006).
;
_computing_publication_material  
; 
WinGX (Farrugia, 1999), PLATON for Windows (Spek, 2003) and
publCIF (Westrip, 2010)
;

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based on F,
with F set to zero for negative F². The threshold expression of F² >
2sigma(F²) is used only for calculating R-factors(gt) etc. and is not
relevant to the choice of reflections for refinement. R-factors based on F²
are statistically about twice as large as those based on F, and R- factors
based on ALL data will be even larger.

Disordered solvent molecules of THF are located on 4-fold rotoinversion axes.
All hydrogen positions were calculated after each cycle of refinement using a
riding model, with C---H = 0.93 Å and Uiso(H) = 1.2Ueq(C)
for aromatic H atoms, with C---H = 0.97 Å and Uiso(H) =
1.2Ueq(C) for methylene H atoms, with C---H = 0.98 Å and
Uiso(H) = 1.2Ueq(C) for methine H atoms, with C---H = 0.96
Å and Uiso(H) = 1.5Ueq(C) for methyl H atoms, and with
N---H = 0.91 Å and Uiso(H) = 1.2Ueq(N).

Hydrogen bonds were found in the crystal structure, see the list at the end of
the CIF file.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9319
_refine_ls_number_parameters     510
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0488
_refine_ls_wR_factor_ref         0.0744
_refine_ls_wR_factor_gt          0.0619
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.987
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9104(2) 0.1258(2) 0.3796(5) 0.029(2) Uani 1 1 d . . .
C2 C 0.8209(2) 0.1549(2) 0.6277(5) 0.034(2) Uani 1 1 d . . .
H2 H 0.7973 0.1583 0.6503 0.041 Uiso 1 1 calc R . .
C3 C 0.8685(2) 0.0367(2) 0.4231(5) 0.035(2) Uani 1 1 d . . .
H3 H 0.8534 0.0153 0.4386 0.042 Uiso 1 1 calc R . .
C4 C 0.8806(2) 0.0330(2) 0.3247(4) 0.047(3) Uani 1 1 d . . .
H4A H 0.8924 0.0553 0.3057 0.070 Uiso 1 1 calc R . .
H4B H 0.8594 0.0285 0.2877 0.070 Uiso 1 1 calc R . .
H4C H 0.8974 0.0128 0.3192 0.070 Uiso 1 1 calc R . .
C5 C 0.9024(2) 0.0368(2) 0.4847(4) 0.036(2) Uani 1 1 d . . .
H5A H 0.9146 0.0135 0.4809 0.054 Uiso 1 1 calc R . .
H5B H 0.8948 0.0412 0.5457 0.054 Uiso 1 1 calc R . .
H5C H 0.9190 0.0559 0.4661 0.054 Uiso 1 1 calc R . .
C6 C 0.8049(2) 0.0657(2) 0.5240(5) 0.036(2) Uani 1 1 d . . .
H6 H 0.7889 0.0872 0.5307 0.043 Uiso 1 1 calc R . .
C7 C 0.8219(2) 0.0587(2) 0.6169(4) 0.046(3) Uani 1 1 d . . .
H7A H 0.8028 0.0588 0.6617 0.068 Uiso 1 1 calc R . .
H7B H 0.8394 0.0777 0.6301 0.068 Uiso 1 1 calc R . .
H7C H 0.8340 0.0353 0.6171 0.068 Uiso 1 1 calc R . .
C8 C 0.7797(2) 0.0337(3) 0.4968(5) 0.062(3) Uani 1 1 d . . .
H8A H 0.7937 0.0113 0.4953 0.093 Uiso 1 1 calc R . .
H8B H 0.7695 0.0384 0.4383 0.093 Uiso 1 1 calc R . .
H8C H 0.7601 0.0314 0.5398 0.093 Uiso 1 1 calc R . .
C9 C 0.8143(2) 0.0888(2) 0.3403(5) 0.036(2) Uani 1 1 d . . .
H9A H 0.8297 0.0857 0.2875 0.043 Uiso 1 1 calc R . .
H9B H 0.7936 0.0721 0.3357 0.043 Uiso 1 1 calc R . .
C10 C 0.8007(2) 0.1282(2) 0.3456(5) 0.038(2) Uani 1 1 d . . .
H10A H 0.7861 0.1340 0.2926 0.045 Uiso 1 1 calc R . .
H10B H 0.7852 0.1313 0.3982 0.045 Uiso 1 1 calc R . .
C11 C 0.8207(2) 0.1928(2) 0.3546(5) 0.036(2) Uani 1 1 d . . .
H11A H 0.8072 0.1975 0.4097 0.043 Uiso 1 1 calc R . .
H11B H 0.8047 0.1982 0.3040 0.043 Uiso 1 1 calc R . .
C12 C 0.8543(2) 0.2167(2) 0.3508(4) 0.033(2) Uani 1 1 d . . .
H12A H 0.8472 0.2423 0.3564 0.039 Uiso 1 1 calc R . .
H12B H 0.8664 0.2135 0.2931 0.039 Uiso 1 1 calc R . .
C13 C 0.9317(2) 0.2137(2) 0.3898(5) 0.039(2) Uani 1 1 d . . .
H13 H 0.9321 0.1994 0.3339 0.046 Uiso 1 1 calc R . .
C14 C 0.9381(3) 0.2536(2) 0.3626(6) 0.065(3) Uani 1 1 d . . .
H14A H 0.9396 0.2687 0.4156 0.097 Uiso 1 1 calc R . .
H14B H 0.9181 0.2619 0.3255 0.097 Uiso 1 1 calc R . .
H14C H 0.9607 0.2555 0.3294 0.097 Uiso 1 1 calc R . .
C15 C 0.9637(2) 0.1995(2) 0.4472(6) 0.055(3) Uani 1 1 d . . .
H15A H 0.9857 0.1987 0.4113 0.083 Uiso 1 1 calc R . .
H15B H 0.9581 0.1753 0.4688 0.083 Uiso 1 1 calc R . .
H15C H 0.9675 0.2157 0.4974 0.083 Uiso 1 1 calc R . .
C16 C 0.8800(2) 0.2396(2) 0.5300(5) 0.036(2) Uani 1 1 d . . .
H16 H 0.8909 0.2626 0.5081 0.043 Uiso 1 1 calc R . .
C17 C 0.9004(2) 0.2285(2) 0.6166(5) 0.053(3) Uani 1 1 d . . .
H17A H 0.8951 0.2460 0.6633 0.080 Uiso 1 1 calc R . .
H17B H 0.9264 0.2282 0.6053 0.080 Uiso 1 1 calc R . .
H17C H 0.8925 0.2045 0.6352 0.080 Uiso 1 1 calc R . .
C18 C 0.8393(2) 0.2471(2) 0.5499(5) 0.053(3) Uani 1 1 d . . .
H18A H 0.8277 0.2248 0.5696 0.079 Uiso 1 1 calc R . .
H18B H 0.8274 0.2558 0.4963 0.079 Uiso 1 1 calc R . .
H18C H 0.8373 0.2653 0.5963 0.079 Uiso 1 1 calc R . .
C19 C 0.8043(2) 0.1256(2) -0.1091(5) 0.032(2) Uani 1 1 d . . .
C20 C 0.8981(2) 0.1554(2) 0.1287(5) 0.036(2) Uani 1 1 d . . .
H20 H 0.9221 0.1573 0.1498 0.044 Uiso 1 1 calc R . .
C21 C 0.9146(2) 0.0666(2) 0.0107(4) 0.029(2) Uani 1 1 d . . .
H21 H 0.9305 0.0884 0.0134 0.035 Uiso 1 1 calc R . .
C22 C 0.9380(2) 0.0356(2) -0.0298(5) 0.042(2) Uani 1 1 d . . .
H22A H 0.9556 0.0274 0.0139 0.063 Uiso 1 1 calc R . .
H22B H 0.9506 0.0445 -0.0822 0.063 Uiso 1 1 calc R . .
H22C H 0.9223 0.0154 -0.0463 0.063 Uiso 1 1 calc R . .
C23 C 0.9037(2) 0.0579(2) 0.1072(4) 0.043(2) Uani 1 1 d . . .
H23A H 0.8917 0.0344 0.1092 0.065 Uiso 1 1 calc R . .
H23B H 0.8873 0.0765 0.1292 0.065 Uiso 1 1 calc R . .
H23C H 0.9254 0.0572 0.1443 0.065 Uiso 1 1 calc R . .
C24 C 0.8457(2) 0.0375(2) -0.0638(5) 0.033(2) Uani 1 1 d . . .
H24 H 0.8616 0.0164 -0.0507 0.040 Uiso 1 1 calc R . .
C25 C 0.8151(2) 0.0381(2) 0.0073(5) 0.056(3) Uani 1 1 d . . .
H25A H 0.7988 0.0583 -0.0046 0.084 Uiso 1 1 calc R . .
H25B H 0.8258 0.0410 0.0660 0.084 Uiso 1 1 calc R . .
H25C H 0.8016 0.0155 0.0051 0.084 Uiso 1 1 calc R . .
C26 C 0.8291(2) 0.0317(2) -0.1572(5) 0.054(3) Uani 1 1 d . . .
H26A H 0.8127 0.0110 -0.1559 0.081 Uiso 1 1 calc R . .
H26B H 0.8485 0.0272 -0.1998 0.081 Uiso 1 1 calc R . .
H26C H 0.8158 0.0533 -0.1747 0.081 Uiso 1 1 calc R . .
C27 C 0.8943(2) 0.0895(2) -0.1676(4) 0.034(2) Uani 1 1 d . . .
H27A H 0.9137 0.0719 -0.1806 0.040 Uiso 1 1 calc R . .
H27B H 0.8757 0.0875 -0.2140 0.040 Uiso 1 1 calc R . .
C28 C 0.9099(2) 0.1282(2) -0.1662(5) 0.030(2) Uani 1 1 d . . .
H28A H 0.9286 0.1302 -0.1199 0.037 Uiso 1 1 calc R . .
H28B H 0.9211 0.1339 -0.2238 0.037 Uiso 1 1 calc R . .
C29 C 0.8926(2) 0.1932(2) -0.1453(5) 0.034(2) Uani 1 1 d . . .
H29A H 0.9071 0.1984 -0.1984 0.040 Uiso 1 1 calc R . .
H29B H 0.9077 0.1973 -0.0925 0.040 Uiso 1 1 calc R . .
C30 C 0.8585(2) 0.2184(2) -0.1424(4) 0.035(2) Uani 1 1 d . . .
H30A H 0.8454 0.2167 -0.1991 0.042 Uiso 1 1 calc R . .
H30B H 0.8663 0.2437 -0.1344 0.042 Uiso 1 1 calc R . .
C31 C 0.8345(2) 0.2407(2) 0.0369(5) 0.040(2) Uani 1 1 d . . .
H31 H 0.8249 0.2641 0.0141 0.048 Uiso 1 1 calc R . .
C32 C 0.8129(3) 0.2301(3) 0.1218(5) 0.060(3) Uani 1 1 d . . .
H32A H 0.8191 0.2054 0.1390 0.090 Uiso 1 1 calc R . .
H32B H 0.7870 0.2316 0.1097 0.090 Uiso 1 1 calc R . .
H32C H 0.8191 0.2466 0.1699 0.090 Uiso 1 1 calc R . .
C33 C 0.8751(3) 0.2459(2) 0.0606(5) 0.054(3) Uani 1 1 d . . .
H33A H 0.8774 0.2643 0.1066 0.081 Uiso 1 1 calc R . .
H33B H 0.8883 0.2535 0.0080 0.081 Uiso 1 1 calc R . .
H33C H 0.8849 0.2230 0.0822 0.081 Uiso 1 1 calc R . .
C34 C 0.7816(2) 0.2138(2) -0.0984(5) 0.042(2) Uani 1 1 d . . .
H34 H 0.7808 0.1999 -0.1549 0.051 Uiso 1 1 calc R . .
C35 C 0.7740(3) 0.2541(2) -0.1241(6) 0.070(3) Uani 1 1 d . . .
H35A H 0.7524 0.2553 -0.1610 0.105 Uiso 1 1 calc R . .
H35B H 0.7947 0.2637 -0.1568 0.105 Uiso 1 1 calc R . .
H35C H 0.7703 0.2683 -0.0704 0.105 Uiso 1 1 calc R . .
C36 C 0.7503(2) 0.1981(3) -0.0391(5) 0.056(3) Uani 1 1 d . . .
H36A H 0.7469 0.2135 0.0126 0.084 Uiso 1 1 calc R . .
H36B H 0.7567 0.1737 -0.0198 0.084 Uiso 1 1 calc R . .
H36C H 0.7279 0.1972 -0.0733 0.084 Uiso 1 1 calc R . .
N1 N 0.83250(16) 0.15351(17) 0.3511(4) 0.0267(16) Uani 1 1 d . . .
H1 H 0.8452 0.1507 0.2988 0.032 Uiso 1 1 calc R . .
N2 N 0.90458(17) 0.12756(18) 0.5517(4) 0.0330(17) Uani 1 1 d . . .
N3 N 0.81440(18) 0.12906(18) 0.0663(4) 0.0327(17) Uani 1 1 d . . .
N4 N 0.87908(17) 0.15436(17) -0.1473(4) 0.0276(16) Uani 1 1 d . . .
H4 H 0.8640 0.1530 -0.1961 0.033 Uiso 1 1 calc R . .
O1 O 0.93449(16) 0.11726(17) 0.3317(3) 0.0489(17) Uani 1 1 d . . .
O2 O 0.92690(16) 0.12010(18) 0.6095(3) 0.0555(19) Uani 1 1 d . . .
O3 O 0.82347(13) 0.15328(14) 0.5424(3) 0.0323(14) Uani 1 1 d . . .
O4 O 0.84518(16) 0.15258(17) 0.6833(3) 0.0504(18) Uani 1 1 d . . .
O5 O 0.78034(16) 0.11662(16) -0.1571(4) 0.0471(17) Uani 1 1 d . . .
O6 O 0.79406(16) 0.12278(18) 0.1296(3) 0.059(2) Uani 1 1 d . . .
O7 O 0.89454(13) 0.15303(14) 0.0435(3) 0.0296(13) Uani 1 1 d . . .
O8 O 0.87431(17) 0.15570(17) 0.1859(3) 0.0507(18) Uani 1 1 d . . .
P1 P 0.84080(6) 0.07891(6) 0.44252(12) 0.0289(5) Uani 1 1 d . . .
P2 P 0.88669(6) 0.20449(6) 0.44270(13) 0.0313(5) Uani 1 1 d . . .
P3 P 0.87407(6) 0.07982(6) -0.05667(12) 0.0279(5) Uani 1 1 d . . .
P4 P 0.82779(6) 0.20513(6) -0.04978(13) 0.0305(5) Uani 1 1 d . . .
W1 W 0.872304(9) 0.138597(9) 0.464632(19) 0.02451(9) Uani 1 1 d . . .
W2 W 0.843460(9) 0.139487(9) -0.027544(19) 0.02397(9) Uani 1 1 d . . .
O9 O 0.9666(12) 0.2348(13) 0.129(2) 0.080(6) Uiso 0.25 1 d PG A -1
C37 C 0.9784(10) 0.2673(9) 0.0843(17) 0.080(6) Uiso 0.25 1 d PG A -1
H37A H 0.9680 0.2685 0.0242 0.095 Uiso 0.25 1 calc PR A -1
H37B H 0.9704 0.2888 0.1175 0.095 Uiso 0.25 1 calc PR A -1
C38 C 1.0174(10) 0.2665(10) 0.080(2) 0.080(6) Uiso 0.25 1 d PG A -1
H38A H 1.0277 0.2876 0.1105 0.095 Uiso 0.25 1 calc PR A -1
H38B H 1.0254 0.2673 0.0172 0.095 Uiso 0.25 1 calc PR A -1
C39 C 1.0296(12) 0.2335(14) 0.121(3) 0.080(6) Uiso 0.25 1 d PG A -1
H39A H 1.0433 0.2188 0.0780 0.095 Uiso 0.25 1 calc PR A -1
H39B H 1.0456 0.2391 0.1713 0.095 Uiso 0.25 1 calc PR A -1
C40 C 0.998(2) 0.2139(6) 0.151(3) 0.080(6) Uiso 0.25 1 d PG A -1
H40A H 0.9994 0.2103 0.2158 0.095 Uiso 0.25 1 calc PR A -1
H40B H 0.9971 0.1900 0.1225 0.095 Uiso 0.25 1 calc PR A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.172(8) . ?
C1 W1 1.930(8) . ?
C2 O4 1.213(8) . ?
C2 O3 1.271(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.532(9) . ?
C3 C5 1.535(10) . ?
C3 P1 1.858(8) . ?
C3 H3 0.9800 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.533(9) . ?
C6 C8 1.534(10) . ?
C6 P1 1.845(7) . ?
C6 H6 0.9800 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.518(10) . ?
C9 P1 1.835(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N1 1.480(9) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N1 1.493(9) . ?
C11 C12 1.500(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 P2 1.857(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.525(10) . ?
C13 C15 1.534(10) . ?
C13 P2 1.846(8) . ?
C13 H13 0.9800 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C18 1.533(10) . ?
C16 C17 1.540(10) . ?
C16 P2 1.837(7) . ?
C16 H16 0.9800 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 O5 1.170(8) . ?
C19 W2 1.938(8) . ?
C20 O8 1.212(9) . ?
C20 O7 1.275(8) . ?
C20 H20 0.9300 . ?
C21 C23 1.522(9) . ?
C21 C22 1.536(9) . ?
C21 P3 1.845(7) . ?
C21 H21 0.9800 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C26 1.528(9) . ?
C24 C25 1.533(10) . ?
C24 P3 1.858(8) . ?
C24 H24 0.9800 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.516(10) . ?
C27 P3 1.839(7) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 N4 1.498(9) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 N4 1.496(9) . ?
C29 C30 1.540(10) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 P4 1.837(7) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 C33 1.527(11) . ?
C31 C32 1.536(10) . ?
C31 P4 1.843(8) . ?
C31 H31 0.9800 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C35 1.539(11) . ?
C34 C36 1.550(10) . ?
C34 P4 1.854(8) . ?
C34 H34 0.9800 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
N1 W1 2.287(5) . ?
N1 H1 0.9100 . ?
N2 O2 1.213(7) . ?
N2 W1 1.792(6) . ?
N3 O6 1.217(7) . ?
N3 W2 1.791(6) . ?
N4 W2 2.266(6) . ?
N4 H4 0.9100 . ?
O3 W1 2.185(5) . ?
O7 W2 2.193(5) . ?
P1 W1 2.476(2) . ?
P2 W1 2.474(2) . ?
P3 W2 2.477(2) . ?
P4 W2 2.476(2) . ?
O9 C40 1.4200 . ?
O9 C37 1.4200 . ?
C37 C38 1.4200 . ?
C37 H37A 0.9700 . ?
C37 H37B 0.9700 . ?
C38 C39 1.4200 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C39 C40 1.4200 . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 W1 176.5(7) . . ?
O4 C2 O3 128.5(8) . . ?
O4 C2 H2 115.8 . . ?
O3 C2 H2 115.8 . . ?
C4 C3 C5 109.9(7) . . ?
C4 C3 P1 112.1(6) . . ?
C5 C3 P1 109.9(5) . . ?
C4 C3 H3 108.3 . . ?
C5 C3 H3 108.3 . . ?
P1 C3 H3 108.3 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 C8 110.6(7) . . ?
C7 C6 P1 110.4(5) . . ?
C8 C6 P1 116.6(5) . . ?
C7 C6 H6 106.2 . . ?
C8 C6 H6 106.2 . . ?
P1 C6 H6 106.2 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 108.3(5) . . ?
C10 C9 H9A 110.0 . . ?
P1 C9 H9A 110.0 . . ?
C10 C9 H9B 110.0 . . ?
P1 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
N1 C10 C9 109.5(7) . . ?
N1 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
N1 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
N1 C11 C12 108.5(6) . . ?
N1 C11 H11A 110.0 . . ?
C12 C11 H11A 110.0 . . ?
N1 C11 H11B 110.0 . . ?
C12 C11 H11B 110.0 . . ?
H11A C11 H11B 108.4 . . ?
C11 C12 P2 110.6(5) . . ?
C11 C12 H12A 109.5 . . ?
P2 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
P2 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C14 C13 C15 110.6(7) . . ?
C14 C13 P2 114.9(6) . . ?
C15 C13 P2 112.0(5) . . ?
C14 C13 H13 106.2 . . ?
C15 C13 H13 106.2 . . ?
P2 C13 H13 106.2 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C16 C17 110.6(6) . . ?
C18 C16 P2 112.8(6) . . ?
C17 C16 P2 110.1(6) . . ?
C18 C16 H16 107.7 . . ?
C17 C16 H16 107.7 . . ?
P2 C16 H16 107.7 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O5 C19 W2 178.6(8) . . ?
O8 C20 O7 128.6(8) . . ?
O8 C20 H20 115.7 . . ?
O7 C20 H20 115.7 . . ?
C23 C21 C22 111.0(6) . . ?
C23 C21 P3 111.0(5) . . ?
C22 C21 P3 114.9(5) . . ?
C23 C21 H21 106.5 . . ?
C22 C21 H21 106.5 . . ?
P3 C21 H21 106.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 C24 C25 110.0(7) . . ?
C26 C24 P3 112.6(5) . . ?
C25 C24 P3 110.5(5) . . ?
C26 C24 H24 107.8 . . ?
C25 C24 H24 107.8 . . ?
P3 C24 H24 107.8 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 P3 108.4(5) . . ?
C28 C27 H27A 110.0 . . ?
P3 C27 H27A 110.0 . . ?
C28 C27 H27B 110.0 . . ?
P3 C27 H27B 110.0 . . ?
H27A C27 H27B 108.4 . . ?
N4 C28 C27 108.2(6) . . ?
N4 C28 H28A 110.1 . . ?
C27 C28 H28A 110.1 . . ?
N4 C28 H28B 110.1 . . ?
C27 C28 H28B 110.1 . . ?
H28A C28 H28B 108.4 . . ?
N4 C29 C30 107.4(6) . . ?
N4 C29 H29A 110.2 . . ?
C30 C29 H29A 110.2 . . ?
N4 C29 H29B 110.2 . . ?
C30 C29 H29B 110.2 . . ?
H29A C29 H29B 108.5 . . ?
C29 C30 P4 110.7(5) . . ?
C29 C30 H30A 109.5 . . ?
P4 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
P4 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C33 C31 C32 109.6(7) . . ?
C33 C31 P4 112.0(6) . . ?
C32 C31 P4 109.2(6) . . ?
C33 C31 H31 108.7 . . ?
C32 C31 H31 108.7 . . ?
P4 C31 H31 108.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C36 111.2(8) . . ?
C35 C34 P4 114.9(6) . . ?
C36 C34 P4 112.4(5) . . ?
C35 C34 H34 105.9 . . ?
C36 C34 H34 105.9 . . ?
P4 C34 H34 105.9 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C10 N1 C11 111.8(6) . . ?
C10 N1 W1 112.9(4) . . ?
C11 N1 W1 112.6(4) . . ?
C10 N1 H1 106.3 . . ?
C11 N1 H1 106.3 . . ?
W1 N1 H1 106.3 . . ?
O2 N2 W1 178.9(6) . . ?
O6 N3 W2 178.2(7) . . ?
C29 N4 C28 111.1(6) . . ?
C29 N4 W2 113.4(4) . . ?
C28 N4 W2 115.0(4) . . ?
C29 N4 H4 105.5 . . ?
C28 N4 H4 105.5 . . ?
W2 N4 H4 105.5 . . ?
C2 O3 W1 126.7(5) . . ?
C20 O7 W2 125.4(5) . . ?
C9 P1 C6 102.9(4) . . ?
C9 P1 C3 108.6(3) . . ?
C6 P1 C3 105.7(4) . . ?
C9 P1 W1 100.4(3) . . ?
C6 P1 W1 118.0(3) . . ?
C3 P1 W1 119.6(3) . . ?
C16 P2 C13 107.0(4) . . ?
C16 P2 C12 105.6(4) . . ?
C13 P2 C12 101.9(4) . . ?
C16 P2 W1 123.6(3) . . ?
C13 P2 W1 114.8(3) . . ?
C12 P2 W1 101.2(3) . . ?
C27 P3 C21 102.5(3) . . ?
C27 P3 C24 109.3(3) . . ?
C21 P3 C24 105.1(3) . . ?
C27 P3 W2 99.7(3) . . ?
C21 P3 W2 119.5(2) . . ?
C24 P3 W2 119.1(3) . . ?
C30 P4 C31 105.0(4) . . ?
C30 P4 C34 102.4(4) . . ?
C31 P4 C34 105.8(4) . . ?
C30 P4 W2 102.3(3) . . ?
C31 P4 W2 123.6(3) . . ?
C34 P4 W2 115.1(3) . . ?
N2 W1 C1 87.1(3) . . ?
N2 W1 O3 101.9(2) . . ?
C1 W1 O3 170.9(2) . . ?
N2 W1 N1 178.3(3) . . ?
C1 W1 N1 91.6(3) . . ?
O3 W1 N1 79.49(19) . . ?
N2 W1 P2 100.0(2) . . ?
C1 W1 P2 89.7(2) . . ?
O3 W1 P2 90.28(15) . . ?
N1 W1 P2 78.88(17) . . ?
N2 W1 P1 101.7(2) . . ?
C1 W1 P1 91.9(2) . . ?
O3 W1 P1 84.74(15) . . ?
N1 W1 P1 79.47(17) . . ?
P2 W1 P1 158.32(7) . . ?
N3 W2 C19 89.9(3) . . ?
N3 W2 O7 99.9(2) . . ?
C19 W2 O7 169.4(2) . . ?
N3 W2 N4 178.1(3) . . ?
C19 W2 N4 89.5(3) . . ?
O7 W2 N4 80.81(19) . . ?
N3 W2 P4 99.9(2) . . ?
C19 W2 P4 89.9(2) . . ?
O7 W2 P4 92.45(14) . . ?
N4 W2 P4 78.27(16) . . ?
N3 W2 P3 102.5(2) . . ?
C19 W2 P3 89.6(2) . . ?
O7 W2 P3 84.27(14) . . ?
N4 W2 P3 79.34(16) . . ?
P4 W2 P3 157.61(7) . . ?
C40 O9 C37 108.0 . . ?
C38 C37 O9 108.0 . . ?
C38 C37 H37A 110.1 . . ?
O9 C37 H37A 110.1 . . ?
C38 C37 H37B 110.1 . . ?
O9 C37 H37B 110.1 . . ?
H37A C37 H37B 108.4 . . ?
C37 C38 C39 108.0 . . ?
C37 C38 H38A 110.1 . . ?
C39 C38 H38A 110.1 . . ?
C37 C38 H38B 110.1 . . ?
C39 C38 H38B 110.1 . . ?
H38A C38 H38B 108.4 . . ?
C40 C39 C38 108.0 . . ?
C40 C39 H39A 110.1 . . ?
C38 C39 H39A 110.1 . . ?
C40 C39 H39B 110.1 . . ?
C38 C39 H39B 110.1 . . ?
H39A C39 H39B 108.4 . . ?
C39 C40 O9 108.0 . . ?
C39 C40 H40A 110.1 . . ?
O9 C40 H40A 110.1 . . ?
C39 C40 H40B 110.1 . . ?
O9 C40 H40B 110.1 . . ?
H40A C40 H40B 108.4 . . ?

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
N1 H1 O8 0.91 1.99 2.889(8) 168.4 .
N4 H4 O4 0.91 1.92 2.802(8) 163.5 1_554
C10 H10A O6 0.97 2.47 3.223(9) 134.1 .
C24 H24 O6 0.98 2.46 3.236(9) 135.3 8_554
C18 H18C O2 0.96 2.50 3.273(10) 137.1 15_666
C28 H28B O2 0.97 2.53 3.401(9) 148.7 1_554

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.169

#############################################################


####################################################################### 
# 
# 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_6a(anti)
_database_code_depnum_ccdc_archive 'CCDC 960495'
_audit_update_record             
;
2013-09-11 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;\
(2-[bis(1-methylethyl)phosphanyl-κP]-N-{2-[bis(1-methylethyl)\
phosphanyl-κP]ethyl}ethanamine-κN)(dichloro)\
(nitrosyl)molybdenum  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H37 Cl2 Mo N2 O P2'
_chemical_formula_sum            'C16 H37 Cl2 Mo N2 O P2'
_chemical_formula_weight         502.26

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   7.3971(1)
_cell_length_b                   13.2575(2)
_cell_length_c                   23.8535(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2339.24(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    25183
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      34.41

_exptl_crystal_description       'flat needle'
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1044
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_min  0.799
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
; Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            55639
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         32.58
_reflns_number_total             8495
_reflns_number_gt                7529
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_structure_solution    
; SHELXS97. Program for Crystal Structure solution.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.  
;
_computing_structure_refinement  
; SHELXL97. Program for crystal structure refinement.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_computing_molecular_graphics    
; ORTEP-3 for Windows, Version 2.01.
  Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material  
; WinGX -- An integrated system of Windows programs for the solution,
 refinment and analysis of single crystal X-ray diffraction data,
 Version 1.80.00.
 Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 SHELXL97. Program for crystal structure refinement.
 Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
 PLATON for Windows, Version 1.12.
 Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. 
;

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0541P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
'Flack H. D. (1983), Acta Cryst. A39, 876-881. 3733 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_number_reflns         8495
_refine_ls_number_parameters     225
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0872
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7737(5) 0.8051(2) 0.29206(11) 0.0398(7) Uani 1 1 d . . .
H1 H 0.8354 0.8705 0.2919 0.048 Uiso 1 1 calc R . .
C2 C 0.5749(6) 0.8258(3) 0.30617(15) 0.0618(12) Uani 1 1 d . . .
H2A H 0.5122 0.7630 0.3108 0.093 Uiso 1 1 calc R . .
H2B H 0.5203 0.8634 0.2762 0.093 Uiso 1 1 calc R . .
H2C H 0.5678 0.8640 0.3403 0.093 Uiso 1 1 calc R . .
C3 C 0.8599(8) 0.7434(4) 0.33690(14) 0.0791(17) Uani 1 1 d . . .
H3A H 0.8358 0.7733 0.3728 0.119 Uiso 1 1 calc R . .
H3B H 0.9881 0.7408 0.3308 0.119 Uiso 1 1 calc R . .
H3C H 0.8114 0.6762 0.3360 0.119 Uiso 1 1 calc R . .
C4 C 0.7032(4) 0.6226(2) 0.22232(12) 0.0323(5) Uani 1 1 d . . .
H4 H 0.7227 0.5955 0.2601 0.039 Uiso 1 1 calc R . .
C5 C 0.7921(4) 0.5505(2) 0.18097(15) 0.0411(7) Uani 1 1 d . . .
H5A H 0.7425 0.4841 0.1858 0.062 Uiso 1 1 calc R . .
H5B H 0.9200 0.5486 0.1877 0.062 Uiso 1 1 calc R . .
H5C H 0.7697 0.5732 0.1434 0.062 Uiso 1 1 calc R . .
C6 C 0.4996(4) 0.6262(3) 0.21220(16) 0.0457(7) Uani 1 1 d . . .
H6A H 0.4767 0.6378 0.1731 0.068 Uiso 1 1 calc R . .
H6B H 0.4477 0.6800 0.2338 0.068 Uiso 1 1 calc R . .
H6C H 0.4464 0.5633 0.2233 0.068 Uiso 1 1 calc R . .
C7 C 1.0439(4) 0.7355(2) 0.21286(13) 0.0327(6) Uani 1 1 d . . .
H7A H 1.1065 0.7890 0.2327 0.039 Uiso 1 1 calc R . .
H7B H 1.0808 0.6715 0.2289 0.039 Uiso 1 1 calc R . .
C8 C 1.0935(4) 0.7386(2) 0.15114(12) 0.0317(6) Uani 1 1 d . . .
H8A H 1.2236 0.7330 0.1471 0.038 Uiso 1 1 calc R . .
H8B H 1.0384 0.6818 0.1320 0.038 Uiso 1 1 calc R . .
C9 C 1.0880(4) 0.8409(2) 0.06637(11) 0.0296(5) Uani 1 1 d . . .
H9A H 1.0211 0.7927 0.0439 0.036 Uiso 1 1 calc R . .
H9B H 1.2157 0.8253 0.0632 0.036 Uiso 1 1 calc R . .
C10 C 1.0523(4) 0.9481(2) 0.04502(12) 0.0299(6) Uani 1 1 d . . .
H10A H 1.0824 0.9525 0.0055 0.036 Uiso 1 1 calc R . .
H10B H 1.1273 0.9957 0.0653 0.036 Uiso 1 1 calc R . .
C11 C 0.7048(4) 0.9425(2) -0.01113(10) 0.0283(5) Uani 1 1 d . . .
H11 H 0.7311 0.8706 -0.0160 0.034 Uiso 1 1 calc R . .
C12 C 0.5006(5) 0.9503(3) -0.00707(15) 0.0530(10) Uani 1 1 d . . .
H12A H 0.4661 1.0201 -0.0053 0.080 Uiso 1 1 calc R . .
H12B H 0.4598 0.9163 0.0261 0.080 Uiso 1 1 calc R . .
H12C H 0.4467 0.9196 -0.0394 0.080 Uiso 1 1 calc R . .
C13 C 0.7726(5) 0.9941(3) -0.06451(11) 0.0419(7) Uani 1 1 d . . .
H13A H 0.7221 0.9610 -0.0967 0.063 Uiso 1 1 calc R . .
H13B H 0.9021 0.9902 -0.0660 0.063 Uiso 1 1 calc R . .
H13C H 0.7361 1.0636 -0.0643 0.063 Uiso 1 1 calc R . .
C14 C 0.8148(5) 1.1162(2) 0.06653(12) 0.0377(7) Uani 1 1 d . . .
H14 H 0.8836 1.1255 0.1013 0.045 Uiso 1 1 calc R . .
C15 C 0.6235(6) 1.1561(3) 0.0804(2) 0.0664(13) Uani 1 1 d . . .
H15A H 0.6329 1.2214 0.0975 0.100 Uiso 1 1 calc R . .
H15B H 0.5647 1.1104 0.1058 0.100 Uiso 1 1 calc R . .
H15C H 0.5541 1.1613 0.0465 0.100 Uiso 1 1 calc R . .
C16 C 0.9117(7) 1.1810(2) 0.02382(16) 0.0586(11) Uani 1 1 d . . .
H16A H 0.8380 1.1875 -0.0091 0.088 Uiso 1 1 calc R . .
H16B H 1.0247 1.1501 0.0140 0.088 Uiso 1 1 calc R . .
H16C H 0.9338 1.2466 0.0395 0.088 Uiso 1 1 calc R . .
N1 N 0.6593(3) 0.7658(2) 0.09259(12) 0.0377(6) Uani 1 1 d . . .
N2 N 1.0307(3) 0.83366(16) 0.12558(9) 0.0242(4) Uani 1 1 d . . .
H2 H 1.0923 0.8833 0.1437 0.029 Uiso 1 1 calc R . .
O1 O 0.6149(4) 0.7086(2) 0.06573(10) 0.0537(7) Uani 1 1 d . . .
P1 P 0.79908(9) 0.75139(5) 0.22063(3) 0.02372(13) Uani 1 1 d . . .
P2 P 0.81292(9) 0.97906(5) 0.05539(3) 0.02133(12) Uani 1 1 d . . .
Cl1 Cl 0.86967(10) 1.00517(5) 0.19906(3) 0.03299(15) Uani 1 1 d . . .
Cl2 Cl 0.43435(10) 0.92980(6) 0.16081(3) 0.03788(16) Uani 1 1 d . . .
Mo1 Mo 0.73593(2) 0.869353(14) 0.139192(8) 0.01822(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C3 1.490(5) . ?
C1 C2 1.534(6) . ?
C1 P1 1.856(3) . ?
C1 H1 0.9800 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C5 1.523(4) . ?
C4 C6 1.526(4) . ?
C4 P1 1.850(3) . ?
C4 H4 0.9800 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 C8 1.518(4) . ?
C7 P1 1.833(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.475(3) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.477(3) . ?
C9 C10 1.533(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 P2 1.834(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.517(4) . ?
C11 C13 1.530(4) . ?
C11 P2 1.842(3) . ?
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 C16 1.513(5) . ?
C14 C15 1.547(5) . ?
C14 P2 1.838(3) . ?
C14 H14 0.9800 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
N1 O1 1.046(4) . ?
N1 Mo1 1.855(3) . ?
N2 Mo1 2.255(2) . ?
N2 H2 0.9100 . ?
P1 Mo1 2.5372(7) . ?
P2 Mo1 2.5369(6) . ?
Cl1 Mo1 2.5021(7) . ?
Cl2 Mo1 2.4258(8) . ?

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
C3 C1 C2 110.6(3) . . ?
C3 C1 P1 113.9(2) . . ?
C2 C1 P1 111.5(2) . . ?
C3 C1 H1 106.8 . . ?
C2 C1 H1 106.8 . . ?
P1 C1 H1 106.8 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C6 110.1(3) . . ?
C5 C4 P1 113.58(19) . . ?
C6 C4 P1 110.2(2) . . ?
C5 C4 H4 107.6 . . ?
C6 C4 H4 107.6 . . ?
P1 C4 H4 107.6 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P1 109.50(19) . . ?
C8 C7 H7A 109.8 . . ?
P1 C7 H7A 109.8 . . ?
C8 C7 H7B 109.8 . . ?
P1 C7 H7B 109.8 . . ?
H7A C7 H7B 108.2 . . ?
N2 C8 C7 110.4(2) . . ?
N2 C8 H8A 109.6 . . ?
C7 C8 H8A 109.6 . . ?
N2 C8 H8B 109.6 . . ?
C7 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
N2 C9 C10 109.2(2) . . ?
N2 C9 H9A 109.8 . . ?
C10 C9 H9A 109.8 . . ?
N2 C9 H9B 109.8 . . ?
C10 C9 H9B 109.8 . . ?
H9A C9 H9B 108.3 . . ?
C9 C10 P2 109.21(18) . . ?
C9 C10 H10A 109.8 . . ?
P2 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
P2 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
C12 C11 C13 110.4(3) . . ?
C12 C11 P2 111.1(2) . . ?
C13 C11 P2 117.20(19) . . ?
C12 C11 H11 105.8 . . ?
C13 C11 H11 105.8 . . ?
P2 C11 H11 105.8 . . ?
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 . . ?
C16 C14 C15 112.5(3) . . ?
C16 C14 P2 117.9(2) . . ?
C15 C14 P2 111.3(2) . . ?
C16 C14 H14 104.5 . . ?
C15 C14 H14 104.5 . . ?
P2 C14 H14 104.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O1 N1 Mo1 178.7(3) . . ?
C8 N2 C9 111.1(2) . . ?
C8 N2 Mo1 115.10(16) . . ?
C9 N2 Mo1 113.66(16) . . ?
C8 N2 H2 105.3 . . ?
C9 N2 H2 105.3 . . ?
Mo1 N2 H2 105.3 . . ?
C7 P1 C4 105.96(13) . . ?
C7 P1 C1 103.70(15) . . ?
C4 P1 C1 107.17(14) . . ?
C7 P1 Mo1 100.10(9) . . ?
C4 P1 Mo1 121.02(9) . . ?
C1 P1 Mo1 116.62(9) . . ?
C10 P2 C14 103.51(15) . . ?
C10 P2 C11 104.14(13) . . ?
C14 P2 C11 112.84(14) . . ?
C10 P2 Mo1 101.22(9) . . ?
C14 P2 Mo1 117.06(10) . . ?
C11 P2 Mo1 115.51(9) . . ?
N1 Mo1 N2 93.09(10) . . ?
N1 Mo1 Cl2 95.21(8) . . ?
N2 Mo1 Cl2 171.60(6) . . ?
N1 Mo1 Cl1 174.48(8) . . ?
N2 Mo1 Cl1 81.42(6) . . ?
Cl2 Mo1 Cl1 90.26(3) . . ?
N1 Mo1 P2 91.19(7) . . ?
N2 Mo1 P2 77.86(5) . . ?
Cl2 Mo1 P2 100.64(2) . . ?
Cl1 Mo1 P2 87.04(2) . . ?
N1 Mo1 P1 93.38(7) . . ?
N2 Mo1 P1 78.63(6) . . ?
Cl2 Mo1 P1 102.13(2) . . ?
Cl1 Mo1 P1 86.20(2) . . ?
P2 Mo1 P1 156.25(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        32.58
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.107
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.091


####################################################################### 
# 
# 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_6b(syn)
_database_code_depnum_ccdc_archive 'CCDC 960496'
_audit_update_record             
;
2013-09-11 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;\
(2-[bis(1-methylethyl)phosphanyl-κP]-N-{2-[bis(1-methylethyl)\
phosphanyl-κP]ethyl}ethanamine-κN)(dichloro)(nitrosyl)tungsten  
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H37 Cl2 N2 O P2 W'
_chemical_formula_sum            'C16 H37 Cl2 N2 O P2 W'
_chemical_formula_weight         590.16

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   7.4129(1)
_cell_length_b                   13.2003(2)
_cell_length_c                   23.8800(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2336.72(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    7811
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      30.77

_exptl_crystal_description       'small block'
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1172
_exptl_absorpt_coefficient_mu    5.316
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
; Goniometer Xcalibur, detector: Ruby
Oxford Diffraction (2007). Oxford Diffraction Ltd.,
Xcalibur CCD system
;
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            16728
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.88
_diffrn_reflns_theta_max         28.28
_reflns_number_total             5804
_reflns_number_gt                4644
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_solution    
; SHELXS97. Program for Crystal Structure solution.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.  
;
_computing_structure_refinement  
; SHELXL97. Program for crystal structure refinement.
  Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_computing_molecular_graphics    
; ORTEP-3 for Windows, Version 2.01.
  Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565.
;
_computing_publication_material  
; WinGX -- An integrated system of Windows programs for the solution,
 refinment and analysis of single crystal X-ray diffraction data,
 Version 1.80.00.
 Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838.
 SHELXL97. Program for crystal structure refinement.
 Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
 PLATON for Windows, Version 1.12.
 Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. 
;

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0194P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881. 2507 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.007(7)
_refine_ls_number_reflns         5804
_refine_ls_number_parameters     257
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0505
_refine_ls_wR_factor_gt          0.0488
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_restrained_S_all      0.895
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4537(6) 0.9474(4) 0.0424(2) 0.0401(14) Uani 1 1 d . . .
H1A H 0.3758 0.9952 0.0616 0.048 Uiso 1 1 calc R . .
H1B H 0.4273 0.9507 0.0027 0.048 Uiso 1 1 calc R . .
C2 C 0.4201(6) 0.8414(4) 0.0640(2) 0.0424(15) Uani 1 1 d . . .
H2A H 0.2930 0.8253 0.0603 0.051 Uiso 1 1 calc R . .
H2B H 0.4879 0.7933 0.0416 0.051 Uiso 1 1 calc R . .
C3 C 0.4114(6) 0.7374(4) 0.1478(3) 0.0469(16) Uani 1 1 d . . .
H3A H 0.4687 0.6807 0.1290 0.056 Uiso 1 1 calc R . .
H3B H 0.2821 0.7313 0.1426 0.056 Uiso 1 1 calc R . .
C4 C 0.4553(6) 0.7336(5) 0.2102(2) 0.0467(16) Uani 1 1 d . . .
H4A H 0.4206 0.6684 0.2255 0.056 Uiso 1 1 calc R . .
H4B H 0.3889 0.7860 0.2298 0.056 Uiso 1 1 calc R . .
C5 C 0.8060(6) 0.9461(4) -0.0108(2) 0.0392(14) Uani 1 1 d . . .
H5 H 0.7836 0.8735 -0.0160 0.047 Uiso 1 1 calc R . .
C6 C 1.0058(7) 0.9564(6) -0.0056(3) 0.068(2) Uani 1 1 d . . .
H6A H 1.0632 0.9227 -0.0365 0.102 Uiso 1 1 calc R . .
H6B H 1.0449 0.9263 0.0289 0.102 Uiso 1 1 calc R . .
H6C H 1.0379 1.0269 -0.0059 0.102 Uiso 1 1 calc R . .
C7 C 0.7390(10) 0.9964(4) -0.06402(19) 0.0570(14) Uani 1 1 d . . .
H7A H 0.7840 1.0645 -0.0658 0.085 Uiso 1 1 calc R . .
H7B H 0.6095 0.9976 -0.0640 0.085 Uiso 1 1 calc R . .
H7C H 0.7811 0.9591 -0.0959 0.085 Uiso 1 1 calc R . .
C8 C 0.6886(7) 1.1182(4) 0.0659(2) 0.0505(16) Uani 1 1 d . . .
H8 H 0.6167 1.1259 0.1001 0.061 Uiso 1 1 calc R . .
C9 C 0.5907(9) 1.1803(5) 0.0249(3) 0.075(2) Uani 1 1 d . . .
H9A H 0.5675 1.2460 0.0405 0.113 Uiso 1 1 calc R . .
H9B H 0.4785 1.1481 0.0157 0.113 Uiso 1 1 calc R . .
H9C H 0.6623 1.1874 -0.0084 0.113 Uiso 1 1 calc R . .
C10 C 0.8736(10) 1.1584(4) 0.0830(3) 0.083(3) Uani 1 1 d . . .
H10A H 0.9559 1.1516 0.0522 0.125 Uiso 1 1 calc R . .
H10B H 0.9177 1.1204 0.1144 0.125 Uiso 1 1 calc R . .
H10C H 0.8634 1.2286 0.0931 0.125 Uiso 1 1 calc R . .
C11 C 0.8014(5) 0.6260(4) 0.2226(2) 0.0430(13) Uani 1 1 d . . .
H11 H 0.7817 0.6000 0.2606 0.052 Uiso 1 1 calc R . .
C12 C 0.7174(8) 0.5504(4) 0.1817(3) 0.0592(17) Uani 1 1 d . . .
H12A H 0.7439 0.5707 0.1440 0.089 Uiso 1 1 calc R . .
H12B H 0.5891 0.5487 0.1871 0.089 Uiso 1 1 calc R . .
H12C H 0.7667 0.4842 0.1884 0.089 Uiso 1 1 calc R . .
C13 C 1.0035(6) 0.6312(5) 0.2131(3) 0.0621(18) Uani 1 1 d . . .
H13A H 1.0549 0.5650 0.2179 0.093 Uiso 1 1 calc R . .
H13B H 1.0565 0.6771 0.2396 0.093 Uiso 1 1 calc R . .
H13C H 1.0271 0.6547 0.1758 0.093 Uiso 1 1 calc R . .
C14 C 0.7197(9) 0.8089(4) 0.2901(2) 0.0617(16) Uani 1 1 d U . .
H14 H 0.6571 0.8743 0.2887 0.074 Uiso 1 1 calc R . .
C15 C 0.6272(10) 0.7474(6) 0.3351(3) 0.094(3) Uani 1 1 d U . .
H15A H 0.6881 0.6837 0.3394 0.142 Uiso 1 1 calc R . .
H15B H 0.5039 0.7356 0.3246 0.142 Uiso 1 1 calc R . .
H15C H 0.6308 0.7839 0.3699 0.142 Uiso 1 1 calc R . .
C16 C 0.9145(9) 0.8320(5) 0.3051(3) 0.081(2) Uani 1 1 d U . .
H16A H 0.9183 0.8682 0.3400 0.121 Uiso 1 1 calc R . .
H16B H 0.9679 0.8727 0.2762 0.121 Uiso 1 1 calc R . .
H16C H 0.9805 0.7698 0.3087 0.121 Uiso 1 1 calc R . .
N1A N 0.8382(19) 0.7726(9) 0.0941(5) 0.0356(19) Uani 0.698(8) 1 d PU A 1
O1A O 0.8941(14) 0.7047(7) 0.0643(5) 0.053(2) Uani 0.698(8) 1 d PU A 1
Cl2A Cl 0.6327(4) 1.0060(2) 0.19796(13) 0.0384(8) Uani 0.698(8) 1 d PU A 1
N1B N 0.660(3) 0.9710(16) 0.1806(10) 0.045(4) Uani 0.302(8) 1 d PU A 2
O1B O 0.595(3) 1.0420(15) 0.2094(10) 0.054(4) Uani 0.302(8) 1 d PU A 2
Cl2B Cl 0.8568(12) 0.7399(6) 0.0775(4) 0.0412(18) Uani 0.302(8) 1 d PU A 2
N2 N 0.4736(5) 0.8318(4) 0.1230(2) 0.0377(13) Uani 1 1 d . A .
H H 0.412(6) 0.875(4) 0.136(2) 0.031(14) Uiso 1 1 d . . .
P1 P 0.69160(15) 0.98009(10) 0.05492(6) 0.0299(3) Uani 1 1 d . A .
P2 P 0.69962(16) 0.75335(10) 0.21911(6) 0.0353(3) Uani 1 1 d . A .
Cl1 Cl 1.06362(16) 0.92974(11) 0.16052(6) 0.0432(4) Uani 1 1 d . A .
W1 W 0.76172(2) 0.871944(14) 0.138714(8) 0.02690(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
C1 C2 1.512(7) . ?
C1 P1 1.840(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.467(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.455(6) . ?
C3 C4 1.525(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 P2 1.842(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.493(7) . ?
C5 C7 1.517(6) . ?
C5 P1 1.840(5) . ?
C5 H5 0.9800 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.468(7) . ?
C8 C10 1.527(8) . ?
C8 P1 1.842(6) . ?
C8 H8 0.9800 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C13 1.517(6) . ?
C11 C12 1.530(7) . ?
C11 P2 1.844(5) . ?
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 1.512(8) . ?
C14 C16 1.519(8) . ?
C14 P2 1.852(6) . ?
C14 H14 0.9800 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
N1A O1A 1.216(13) . ?
N1A W1 1.783(9) . ?
Cl2A W1 2.460(2) . ?
N1B O1B 1.26(3) . ?
N1B W1 1.811(19) . ?
Cl2B W1 2.381(6) . ?
N2 W1 2.232(4) . ?
N2 H 0.79(4) . ?
P1 W1 2.5123(13) . ?
P2 W1 2.5197(14) . ?
Cl1 W1 2.4211(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 P1 108.6(3) . . ?
C2 C1 H1A 110.0 . . ?
P1 C1 H1A 110.0 . . ?
C2 C1 H1B 110.0 . . ?
P1 C1 H1B 110.0 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 111.3(4) . . ?
N2 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
N2 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
N2 C3 C4 111.0(5) . . ?
N2 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
N2 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C3 C4 P2 108.6(3) . . ?
C3 C4 H4A 110.0 . . ?
P2 C4 H4A 110.0 . . ?
C3 C4 H4B 110.0 . . ?
P2 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
C6 C5 C7 110.8(5) . . ?
C6 C5 P1 111.4(4) . . ?
C7 C5 P1 117.2(4) . . ?
C6 C5 H5 105.5 . . ?
C7 C5 H5 105.5 . . ?
P1 C5 H5 105.5 . . ?
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 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C10 115.3(6) . . ?
C9 C8 P1 117.6(4) . . ?
C10 C8 P1 111.8(4) . . ?
C9 C8 H8 103.2 . . ?
C10 C8 H8 103.2 . . ?
P1 C8 H8 103.2 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C12 109.6(5) . . ?
C13 C11 P2 110.9(4) . . ?
C12 C11 P2 113.6(3) . . ?
C13 C11 H11 107.5 . . ?
C12 C11 H11 107.5 . . ?
P2 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 C16 111.7(6) . . ?
C15 C14 P2 113.7(4) . . ?
C16 C14 P2 111.9(4) . . ?
C15 C14 H14 106.3 . . ?
C16 C14 H14 106.3 . . ?
P2 C14 H14 106.3 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O1A N1A W1 178.5(15) . . ?
O1B N1B W1 178(3) . . ?
C3 N2 C2 112.3(4) . . ?
C3 N2 W1 116.0(3) . . ?
C2 N2 W1 113.6(3) . . ?
C3 N2 H 105(4) . . ?
C2 N2 H 99(4) . . ?
W1 N2 H 109(3) . . ?
C5 P1 C1 104.2(2) . . ?
C5 P1 C8 111.6(3) . . ?
C1 P1 C8 104.1(2) . . ?
C5 P1 W1 116.47(16) . . ?
C1 P1 W1 101.22(17) . . ?
C8 P1 W1 116.86(19) . . ?
C4 P2 C11 106.2(2) . . ?
C4 P2 C14 104.0(3) . . ?
C11 P2 C14 106.6(3) . . ?
C4 P2 W1 100.31(18) . . ?
C11 P2 W1 121.75(17) . . ?
C14 P2 W1 115.87(18) . . ?
N1A W1 N1B 173.7(9) . . ?
N1A W1 N2 91.6(5) . . ?
N1B W1 N2 82.3(8) . . ?
N1A W1 Cl2B 1.5(6) . . ?
N1B W1 Cl2B 172.2(8) . . ?
N2 W1 Cl2B 90.3(3) . . ?
N1A W1 Cl1 93.8(5) . . ?
N1B W1 Cl1 92.3(8) . . ?
N2 W1 Cl1 174.50(13) . . ?
Cl2B W1 Cl1 95.1(2) . . ?
N1A W1 Cl2A 175.6(5) . . ?
N1B W1 Cl2A 2.1(8) . . ?
N2 W1 Cl2A 84.02(14) . . ?
Cl2B W1 Cl2A 174.2(2) . . ?
Cl1 W1 Cl2A 90.52(8) . . ?
N1A W1 P1 90.4(5) . . ?
N1B W1 P1 86.8(8) . . ?
N2 W1 P1 78.62(13) . . ?
Cl2B W1 P1 89.4(2) . . ?
Cl1 W1 P1 100.57(4) . . ?
Cl2A W1 P1 88.21(8) . . ?
N1A W1 P2 93.3(5) . . ?
N1B W1 P2 87.2(8) . . ?
N2 W1 P2 78.82(13) . . ?
Cl2B W1 P2 93.8(2) . . ?
Cl1 W1 P2 101.58(5) . . ?
Cl2A W1 P2 86.43(8) . . ?
P1 W1 P2 157.23(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.044
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.110

