# 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_201412270
_database_code_depnum_ccdc_archive 'CCDC 1045537'
_audit_update_record             
;
2015-01-26 deposited with the CCDC.
2015-12-03 downloaded from the CCDC.
;
_audit_creation_date             2014-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C23 H16 O6 P2 W, C H2 Cl2'
_chemical_formula_sum            'C24 H18 Cl2 O6 P2 W'
_chemical_formula_weight         719.07
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N4O4W1P1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   6.34581(18)
_cell_length_b                   19.8000(6)
_cell_length_c                   21.5196(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.974(3)
_cell_angle_gamma                90.00
_cell_volume                     2677.73(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4059
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.6910
_cell_measurement_theta_min      3.5300
_exptl_absorpt_coefficient_mu    4.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11802
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.05
_diffrn_ambient_temperature      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -11.00   20.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2885  -99.0000 -180.0000 31

#__ type_ start__ end____ width___ exp.time_
  2 omega   -2.00   82.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8666   77.0000   60.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega  -50.00   49.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8666  -77.0000  -60.0000 99

#__ type_ start__ end____ width___ exp.time_
  4 omega   32.00   57.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       19.8666 -178.0000 -180.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0937060000
_diffrn_orient_matrix_UB_12      0.0198367000
_diffrn_orient_matrix_UB_13      -0.0059743000
_diffrn_orient_matrix_UB_21      0.0486219000
_diffrn_orient_matrix_UB_22      0.0202275000
_diffrn_orient_matrix_UB_23      -0.0211978000
_diffrn_orient_matrix_UB_31      -0.0398732000
_diffrn_orient_matrix_UB_32      -0.0219611000
_diffrn_orient_matrix_UB_33      -0.0249367000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4518
_reflns_number_total             5457
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.469
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         5457
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0364
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0267P)²+0.1349P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0720
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
W1 W -0.02446(3) 0.648086(9) 0.516101(9) 0.03201(7) Uani 1 d . . .
P1 P 0.1551(2) 0.72384(6) 0.60052(6) 0.0357(3) Uani 1 d . . .
P2 P 0.0401(2) 0.71027(7) 0.69194(6) 0.0387(3) Uani 1 d . . .
O1 O -0.4584(6) 0.7288(2) 0.5085(2) 0.0689(12) Uani 1 d . . .
O2 O 0.1076(7) 0.7488(2) 0.41373(19) 0.0695(12) Uani 1 d . . .
O3 O -0.2270(7) 0.55334(19) 0.40719(19) 0.0684(12) Uani 1 d . . .
O4 O 0.4031(7) 0.5659(2) 0.5139(3) 0.0861(16) Uani 1 d . . .
O5 O -0.1877(7) 0.5424(2) 0.61025(19) 0.0732(13) Uani 1 d . . .
O6 O -0.1965(6) 0.71398(19) 0.68373(17) 0.0576(10) Uani 1 d . . .
C1 C -0.3017(8) 0.7001(2) 0.5123(2) 0.0407(12) Uani 1 d . . .
C2 C 0.0640(8) 0.7133(2) 0.4512(2) 0.0431(12) Uani 1 d . . .
C3 C -0.1538(8) 0.5882(2) 0.4467(2) 0.0422(12) Uani 1 d . . .
C4 C 0.2532(9) 0.5954(2) 0.5167(3) 0.0475(13) Uani 1 d . . .
C5 C -0.1259(8) 0.5810(3) 0.5784(2) 0.0461(13) Uani 1 d . . .
C6 C 0.1447(9) 0.8155(2) 0.5927(2) 0.0416(12) Uani 1 d . . .
C7 C -0.0401(11) 0.8467(3) 0.5698(3) 0.0629(17) Uani 1 d . . .
H7 H -0.1612 0.8209 0.5574 0.076 Uiso 1 calc . . R
C8 C -0.0510(13) 0.9169(3) 0.5645(3) 0.084(2) Uani 1 d . . .
H8 H -0.1790 0.9378 0.5494 0.100 Uiso 1 calc . . R
C9 C 0.1254(16) 0.9540(3) 0.5816(3) 0.089(3) Uani 1 d . . .
H9 H 0.1196 1.0007 0.5768 0.107 Uiso 1 calc . . R
C10 C 0.3108(14) 0.9243(3) 0.6058(3) 0.085(2) Uani 1 d . . .
H10 H 0.4301 0.9508 0.6185 0.102 Uiso 1 calc . . R
C11 C 0.3240(12) 0.8539(3) 0.6116(3) 0.0662(18) Uani 1 d . . .
H11 H 0.4514 0.8333 0.6279 0.079 Uiso 1 calc . . R
C12 C 0.1660(8) 0.7730(2) 0.7450(2) 0.0381(12) Uani 1 d . . .
C13 C 0.0405(10) 0.8255(3) 0.7622(3) 0.0529(14) Uani 1 d . . .
H13 H -0.1031 0.8273 0.7461 0.063 Uiso 1 calc . . R
C14 C 0.1277(11) 0.8750(3) 0.8030(3) 0.0596(16) Uani 1 d . . .
H14 H 0.0423 0.9098 0.8145 0.071 Uiso 1 calc . . R
C15 C 0.3381(12) 0.8732(3) 0.8267(3) 0.0623(17) Uani 1 d . . .
H15 H 0.3961 0.9065 0.8543 0.075 Uiso 1 calc . . R
C16 C 0.4644(10) 0.8221(3) 0.8097(3) 0.0601(15) Uani 1 d . . .
H16 H 0.6080 0.8210 0.8260 0.072 Uiso 1 calc . . R
C17 C 0.3797(9) 0.7722(3) 0.7683(2) 0.0515(14) Uani 1 d . . .
H17 H 0.4670 0.7382 0.7564 0.062 Uiso 1 calc . . R
C18 C 0.1460(9) 0.6288(2) 0.7193(2) 0.0436(13) Uani 1 d . . .
C19 C 0.0160(10) 0.5899(3) 0.7523(2) 0.0613(17) Uani 1 d . . .
H19 H -0.1152 0.6065 0.7599 0.074 Uiso 1 calc . . R
C20 C 0.0827(14) 0.5268(4) 0.7736(3) 0.080(2) Uani 1 d . . .
H20 H -0.0025 0.5009 0.7962 0.096 Uiso 1 calc . . R
C21 C 0.2745(16) 0.5023(3) 0.7614(3) 0.090(3) Uani 1 d . . .
H21 H 0.3181 0.4594 0.7755 0.107 Uiso 1 calc . . R
C22 C 0.4037(12) 0.5401(3) 0.7286(3) 0.0727(19) Uani 1 d . . .
H22 H 0.5338 0.5231 0.7205 0.087 Uiso 1 calc . . R
C23 C 0.3384(9) 0.6032(3) 0.7079(2) 0.0527(14) Uani 1 d . . .
H23 H 0.4254 0.6290 0.6858 0.063 Uiso 1 calc . . R
Cl1 Cl 0.3786(4) 0.91110(12) 0.44608(11) 0.1233(8) Uani 1 d . . .
Cl2 Cl 0.7125(4) 0.85490(11) 0.38538(13) 0.1167(8) Uani 1 d . . .
C24 C 0.4460(12) 0.8639(3) 0.3860(3) 0.085(2) Uani 1 d . . .
H24A H 0.3843 0.8844 0.3467 0.102 Uiso 1 calc . . R
H24B H 0.3835 0.8194 0.3880 0.102 Uiso 1 calc . . R
H1 H 0.357(7) 0.7145(19) 0.6200(19) 0.039(12) Uiso 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
W1 P1 2.5048(13) . ?
W1 C1 2.031(5) . ?
W1 C2 2.038(5) . ?
W1 C3 1.992(5) . ?
W1 C4 2.047(6) . ?
W1 C5 2.054(5) . ?
P1 P2 2.2078(17) . ?
P1 C6 1.823(5) . ?
P1 H1 1.31(4) . ?
P2 O6 1.489(4) . ?
P2 C12 1.798(5) . ?
P2 C18 1.814(5) . ?
O1 C1 1.138(6) . ?
O2 C2 1.132(5) . ?
O3 C3 1.143(6) . ?
O4 C4 1.124(6) . ?
O5 C5 1.131(5) . ?
C6 C7 1.356(8) . ?
C6 C11 1.381(8) . ?
C7 H7 0.9300 . ?
C7 C8 1.396(7) . ?
C8 H8 0.9300 . ?
C8 C9 1.348(10) . ?
C9 H9 0.9300 . ?
C9 C10 1.353(10) . ?
C10 H10 0.9300 . ?
C10 C11 1.402(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.390(7) . ?
C12 C17 1.380(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.380(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.362(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.370(8) . ?
C16 H16 0.9300 . ?
C16 C17 1.387(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.392(7) . ?
C18 C23 1.375(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.378(8) . ?
C20 H20 0.9300 . ?
C20 C21 1.369(10) . ?
C21 H21 0.9300 . ?
C21 C22 1.375(9) . ?
C22 H22 0.9300 . ?
C22 C23 1.371(7) . ?
C23 H23 0.9300 . ?
Cl1 C24 1.698(7) . ?
Cl2 C24 1.702(8) . ?
C24 H24A 0.9700 . ?
C24 H24B 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
C1 W1 P1 91.70(14) . . ?
C1 W1 C2 88.32(19) . . ?
C1 W1 C4 178.1(2) . . ?
C1 W1 C5 90.3(2) . . ?
C2 W1 P1 88.67(15) . . ?
C2 W1 C4 90.5(2) . . ?
C2 W1 C5 177.2(2) . . ?
C3 W1 P1 177.02(15) . . ?
C3 W1 C1 90.4(2) . . ?
C3 W1 C2 89.3(2) . . ?
C3 W1 C4 88.0(2) . . ?
C3 W1 C5 88.3(2) . . ?
C4 W1 P1 89.79(15) . . ?
C4 W1 C5 90.8(2) . . ?
C5 W1 P1 93.78(14) . . ?
W1 P1 H1 118.4(17) . . ?
P2 P1 W1 113.58(6) . . ?
P2 P1 H1 97.3(17) . . ?
C6 P1 W1 121.51(17) . . ?
C6 P1 P2 101.01(15) . . ?
C6 P1 H1 101.1(17) . . ?
O6 P2 P1 109.92(16) . . ?
O6 P2 C12 113.2(2) . . ?
O6 P2 C18 113.9(2) . . ?
C12 P2 P1 107.99(16) . . ?
C12 P2 C18 107.2(2) . . ?
C18 P2 P1 104.14(17) . . ?
O1 C1 W1 178.1(5) . . ?
O2 C2 W1 177.7(5) . . ?
O3 C3 W1 179.4(5) . . ?
O4 C4 W1 176.6(5) . . ?
O5 C5 W1 176.5(5) . . ?
C7 C6 P1 120.3(4) . . ?
C7 C6 C11 119.5(5) . . ?
C11 C6 P1 120.2(5) . . ?
C6 C7 H7 119.6 . . ?
C6 C7 C8 120.9(6) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.5(7) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 H9 119.6 . . ?
C8 C9 C10 120.8(7) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 119.9 . . ?
C9 C10 C11 120.3(7) . . ?
C11 C10 H10 119.9 . . ?
C6 C11 C10 119.0(7) . . ?
C6 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C13 C12 P2 117.7(4) . . ?
C17 C12 P2 123.4(4) . . ?
C17 C12 C13 118.8(5) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.5(6) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.9 . . ?
C15 C14 C13 120.3(6) . . ?
C15 C14 H14 119.9 . . ?
C14 C15 H15 120.0 . . ?
C14 C15 C16 120.0(6) . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 119.7 . . ?
C15 C16 C17 120.5(6) . . ?
C17 C16 H16 119.7 . . ?
C12 C17 C16 119.9(5) . . ?
C12 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C19 C18 P2 116.0(4) . . ?
C23 C18 P2 124.6(4) . . ?
C23 C18 C19 119.4(5) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.6(6) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.9(6) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.5 . . ?
C20 C21 C22 120.9(6) . . ?
C22 C21 H21 119.5 . . ?
C21 C22 H22 120.4 . . ?
C23 C22 C21 119.2(7) . . ?
C23 C22 H22 120.4 . . ?
C18 C23 H23 119.5 . . ?
C22 C23 C18 120.9(6) . . ?
C22 C23 H23 119.5 . . ?
Cl1 C24 Cl2 114.8(4) . . ?
Cl1 C24 H24A 108.6 . . ?
Cl1 C24 H24B 108.6 . . ?
Cl2 C24 H24A 108.6 . . ?
Cl2 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
