# Supplementary Material (ESI) for Chemical Communications

# This journal is © The Royal Society of Chemistry 2002



data_global



_journal_coden_Cambridge      182





loop_

_publ_author_name

'Gerard Parkin'

'Mu-Hyun Baik'

'Brian M. Bridgewater'

'David G. Churchill'

'Richard A. Friesner'

'Tony Hascall'

'Jun Ho Shin'



_publ_contact_author_name     	'Prof Gerard Parkin'  

_publ_contact_author_address 

;

Department of Chemistry

Columbia University

MC3115

3000 Broadway

New York

New York

10027

UNITED STATES OF AMERICA

;



_publ_contact_author_email       'PARKIN@CHEM.COLUMBIA.EDU'



_publ_requested_journal       'Chemical Communications'





_publ_section_title		

;

A Non Classical Hydrogen Bond in the Molybdenum Arene

Complex [h6-C6H5C6H3(Ph)OH]Mo(PMe3)3:  Evidence that Hydrogen Bonding

Facilitates Oxidative Addition of the OH Bond

;



data_ars10 



_database_code_CSD	193307





_audit_creation_method            SHELXL-97 

_chemical_name_systematic 

; 

? 

; 

_chemical_name_common             ? 

_chemical_melting_point           ? 

_chemical_formula_moiety          ? 

_chemical_formula_sum 

'C24 H32 Mo O P2' 

_chemical_formula_weight          494.38 



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' 

'O'  'O'   0.0106   0.0060 

'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

'P'  'P'   0.1023   0.0942 

'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

'Mo'  'Mo'  -1.6832   0.6857 

'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 



_symmetry_cell_setting            Monoclinic 

_symmetry_space_group_name_H-M    P2(1)/n 



loop_ 

_symmetry_equiv_pos_as_xyz 

'x, y, z' 

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

'-x, -y, -z' 

'x-1/2, -y-1/2, z-1/2' 



_cell_length_a                    10.5855(14) 

_cell_length_b                    16.018(2) 

_cell_length_c                    14.007(2) 

_cell_angle_alpha                 90.00 

_cell_angle_beta                  90.515(3) 

_cell_angle_gamma                 90.00 

_cell_volume                      2374.9(6) 

_cell_formula_units_Z             4 

_cell_measurement_temperature     223(2) 

_cell_measurement_reflns_used     ? 

_cell_measurement_theta_min       ? 

_cell_measurement_theta_max       ? 



_exptl_crystal_description        ? 

_exptl_crystal_colour             ? 

_exptl_crystal_size_max           0.30 

_exptl_crystal_size_mid           0.20 

_exptl_crystal_size_min           0.05 

_exptl_crystal_density_meas       ? 

_exptl_crystal_density_diffrn     1.383 

_exptl_crystal_density_method     'not measured' 

_exptl_crystal_F_000              1024 

_exptl_absorpt_coefficient_mu     0.699 

_exptl_absorpt_correction_type    none 

_exptl_absorpt_correction_T_min   0.8178 

_exptl_absorpt_correction_T_max   0.9659 

_exptl_absorpt_process_details    ? 



_exptl_special_details 

; 

? 

; 



_diffrn_ambient_temperature       223(2) 

_diffrn_radiation_wavelength      0.71073 

_diffrn_radiation_type            MoK\a 

_diffrn_radiation_source          'fine-focus sealed tube' 

_diffrn_radiation_monochromator   graphite 

_diffrn_measurement_device_type   'CCD area detector' 

_diffrn_measurement_method        'phi and omega scans' 

_diffrn_detector_area_resol_mean  ? 

_diffrn_standards_number          ? 

_diffrn_standards_interval_count  ? 

_diffrn_standards_interval_time   ? 

_diffrn_standards_decay_%         ? 

_diffrn_reflns_number             17603 

_diffrn_reflns_av_R_equivalents   0.0733 

_diffrn_reflns_av_sigmaI/netI     0.0706 

_diffrn_reflns_limit_h_min        -11 

_diffrn_reflns_limit_h_max        14 

_diffrn_reflns_limit_k_min        -21 

_diffrn_reflns_limit_k_max        20 

_diffrn_reflns_limit_l_min        -17 

_diffrn_reflns_limit_l_max        18 

_diffrn_reflns_theta_min          1.93 

_diffrn_reflns_theta_max          28.27 

_reflns_number_total              5466 

_reflns_number_gt                 3685 

_reflns_threshold_expression      >2sigma(I) 



_computing_data_collection        'Bruker SMART' 

_computing_cell_refinement        'Bruker SMART' 

_computing_data_reduction         'Bruker SHELXTL' 

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 

_computing_molecular_graphics     'Bruker SHELXTL' 

_computing_publication_material   'Bruker SHELXTL' 



_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 

'calc w=1/[σ²(Fo²)+(0.1070P)²+0.0000P] 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      SHELXL 

_refine_ls_extinction_coef        0.0000(5) 

_refine_ls_extinction_expression 

'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 

_refine_ls_number_reflns          5466 

_refine_ls_number_parameters      264 

_refine_ls_number_restraints      0 

_refine_ls_R_factor_all           0.0993 

_refine_ls_R_factor_gt            0.0631 

_refine_ls_wR_factor_ref          0.1716 

_refine_ls_wR_factor_gt           0.1497 

_refine_ls_goodness_of_fit_ref    1.003 

_refine_ls_restrained_S_all       1.003 

_refine_ls_shift/su_max           0.315 

_refine_ls_shift/su_mean          0.001 



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 

Mo Mo 0.31587(3) 0.19599(3) 0.37817(3) 0.03204(16) Uani 1 1 d . . . 

P1 P 0.37137(12) 0.32680(9) 0.45663(11) 0.0408(3) Uani 1 1 d . . . 

P2 P 0.31695(12) 0.25361(9) 0.21665(10) 0.0413(3) Uani 1 1 d . . . 

O O 0.1307(3) 0.25519(19) 0.3796(2) 0.0331(7) Uani 1 1 d . . . 

C11 C 0.3224(8) 0.3290(5) 0.5812(6) 0.085(2) Uani 1 1 d . . . 

H11A H 0.3378 0.3841 0.6075 0.127 Uiso 1 1 calc R . . 

H11B H 0.3704 0.2880 0.6173 0.127 Uiso 1 1 calc R . . 

H11C H 0.2331 0.3161 0.5849 0.127 Uiso 1 1 calc R . . 

C12 C 0.5363(5) 0.3550(5) 0.4667(5) 0.0692(19) Uani 1 1 d . . . 

H12A H 0.5699 0.3654 0.4036 0.104 Uiso 1 1 calc R . . 

H12B H 0.5829 0.3097 0.4966 0.104 Uiso 1 1 calc R . . 

H12C H 0.5447 0.4050 0.5053 0.104 Uiso 1 1 calc R . . 

C13 C 0.3024(6) 0.4230(4) 0.4130(6) 0.072(2) Uani 1 1 d . . . 

H13A H 0.3267 0.4686 0.4548 0.108 Uiso 1 1 calc R . . 

H13B H 0.2111 0.4179 0.4117 0.108 Uiso 1 1 calc R . . 

H13C H 0.3324 0.4340 0.3490 0.108 Uiso 1 1 calc R . . 

C21 C 0.3398(9) 0.1758(5) 0.1240(5) 0.090(3) Uani 1 1 d . . . 

H21A H 0.2858 0.1281 0.1361 0.135 Uiso 1 1 calc R . . 

H21B H 0.4274 0.1581 0.1240 0.135 Uiso 1 1 calc R . . 

H21C H 0.3182 0.1998 0.0623 0.135 Uiso 1 1 calc R . . 

C22 C 0.4366(7) 0.3291(6) 0.1820(6) 0.088(3) Uani 1 1 d . . . 

H22A H 0.5196 0.3038 0.1873 0.131 Uiso 1 1 calc R . . 

H22B H 0.4324 0.3774 0.2237 0.131 Uiso 1 1 calc R . . 

H22C H 0.4215 0.3465 0.1165 0.131 Uiso 1 1 calc R . . 

C23 C 0.1734(6) 0.3056(4) 0.1756(5) 0.0630(18) Uani 1 1 d . . . 

H23A H 0.1840 0.3239 0.1101 0.095 Uiso 1 1 calc R . . 

H23B H 0.1568 0.3536 0.2159 0.095 Uiso 1 1 calc R . . 

H23C H 0.1029 0.2670 0.1789 0.095 Uiso 1 1 calc R . . 

C31 C 0.1772(4) 0.0936(3) 0.4173(4) 0.0345(10) Uani 1 1 d . . . 

C32 C 0.2433(5) 0.0648(3) 0.3384(5) 0.0505(14) Uani 1 1 d . . . 

H32A H 0.1988 0.0555 0.2769 0.061 Uiso 1 1 calc R . . 

C33 C 0.3775(5) 0.0654(4) 0.3424(5) 0.0605(17) Uani 1 1 d . . . 

H33A H 0.4270 0.0547 0.2841 0.073 Uiso 1 1 calc R . . 

C34 C 0.4407(5) 0.0845(4) 0.4304(6) 0.0627(19) Uani 1 1 d . . . 

H34A H 0.5336 0.0912 0.4300 0.075 Uiso 1 1 calc R . . 

C35 C 0.3753(5) 0.1141(4) 0.5080(5) 0.0525(16) Uani 1 1 d . . . 

H35A H 0.4220 0.1396 0.5621 0.063 Uiso 1 1 calc R . . 

C36 C 0.2407(4) 0.1213(3) 0.5027(4) 0.0374(11) Uani 1 1 d . . . 

H36A H 0.1932 0.1490 0.5544 0.045 Uiso 1 1 calc R . . 

C41 C 0.0302(4) 0.2073(3) 0.3869(3) 0.0293(9) Uani 1 1 d . . . 

C42 C 0.0434(4) 0.1213(3) 0.4050(3) 0.0320(10) Uani 1 1 d . . . 

C43 C -0.0617(4) 0.0687(3) 0.4102(4) 0.0389(11) Uani 1 1 d . . . 

H43A H -0.0502 0.0113 0.4211 0.047 Uiso 1 1 calc R . . 

C44 C -0.1818(4) 0.1003(3) 0.3996(4) 0.0425(12) Uani 1 1 d . . . 

H44A H -0.2527 0.0653 0.4051 0.051 Uiso 1 1 calc R . . 

C45 C -0.1962(4) 0.1854(3) 0.3805(4) 0.0392(12) Uani 1 1 d . . . 

H45A H -0.2783 0.2068 0.3727 0.047 Uiso 1 1 calc R . . 

C46 C -0.0953(4) 0.2394(3) 0.3726(3) 0.0301(10) Uani 1 1 d . . . 

C51 C -0.1160(4) 0.3293(3) 0.3497(3) 0.0313(10) Uani 1 1 d . . . 

C52 C -0.0506(4) 0.3929(3) 0.3956(4) 0.0384(11) Uani 1 1 d . . . 

H52A H 0.0097 0.3795 0.4429 0.046 Uiso 1 1 calc R . . 

C53 C -0.0725(5) 0.4754(3) 0.3733(4) 0.0465(13) Uani 1 1 d . . . 

H53A H -0.0266 0.5176 0.4048 0.056 Uiso 1 1 calc R . . 

C54 C -0.1626(5) 0.4965(3) 0.3040(4) 0.0462(13) Uani 1 1 d . . . 

H54A H -0.1777 0.5527 0.2884 0.055 Uiso 1 1 calc R . . 

C55 C -0.2285(5) 0.4342(4) 0.2592(4) 0.0495(14) Uani 1 1 d . . . 

H55A H -0.2896 0.4480 0.2127 0.059 Uiso 1 1 calc R . . 

C56 C -0.2068(4) 0.3513(3) 0.2811(4) 0.0405(12) Uani 1 1 d . . . 

H56A H -0.2533 0.3094 0.2496 0.049 Uiso 1 1 calc R . . 

H H 0.451(5) 0.224(3) 0.345(4) 0.048(15) Uiso 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 

Mo O 2.178(3) . ? 

Mo C33 2.249(6) . ? 

Mo C36 2.265(5) . ? 

Mo C31 2.272(5) . ? 

Mo C32 2.304(5) . ? 

Mo C35 2.324(5) . ? 

Mo C34 2.335(5) . ? 

Mo P1 2.4355(15) . ? 

Mo P2 2.4436(15) . ? 

P1 C12 1.808(5) . ? 

P1 C13 1.809(6) . ? 

P1 C11 1.824(8) . ? 

P2 C21 1.817(7) . ? 

P2 C22 1.820(6) . ? 

P2 C23 1.821(6) . ? 

O C41 1.316(5) . ? 

C31 C32 1.391(8) . ? 

C31 C36 1.437(7) . ? 

C31 C42 1.493(6) . ? 

C32 C33 1.422(8) . ? 

C33 C34 1.430(10) . ? 

C34 C35 1.377(9) . ? 

C35 C36 1.431(6) . ? 

C41 C42 1.407(6) . ? 

C41 C46 1.437(5) . ? 

C42 C43 1.398(6) . ? 

C43 C44 1.374(6) . ? 

C44 C45 1.398(7) . ? 

C45 C46 1.379(6) . ? 

C46 C51 1.491(6) . ? 

C51 C52 1.387(7) . ? 

C51 C56 1.399(6) . ? 

C52 C53 1.376(7) . ? 

C53 C54 1.396(7) . ? 

C54 C55 1.366(8) . ? 

C55 C56 1.382(7) . ? 



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 

O Mo C33 132.07(18) . . ? 

O Mo C36 84.29(14) . . ? 

C33 Mo C36 77.6(2) . . ? 

O Mo C31 74.26(14) . . ? 

C33 Mo C31 64.62(19) . . ? 

C36 Mo C31 36.93(17) . . ? 

O Mo C32 95.80(16) . . ? 

C33 Mo C32 36.4(2) . . ? 

C36 Mo C32 65.5(2) . . ? 

C31 Mo C32 35.39(19) . . ? 

O Mo C35 118.43(18) . . ? 

C33 Mo C35 64.7(3) . . ? 

C36 Mo C35 36.31(16) . . ? 

C31 Mo C35 64.83(17) . . ? 

C32 Mo C35 76.2(2) . . ? 

O Mo C34 146.82(17) . . ? 

C33 Mo C34 36.3(2) . . ? 

C36 Mo C34 63.7(2) . . ? 

C31 Mo C34 74.76(18) . . ? 

C32 Mo C34 64.2(2) . . ? 

C35 Mo C34 34.4(2) . . ? 

O Mo P1 80.49(9) . . ? 

C33 Mo P1 146.24(18) . . ? 

C36 Mo P1 101.07(14) . . ? 

C31 Mo P1 131.78(14) . . ? 

C32 Mo P1 166.47(16) . . ? 

C35 Mo P1 94.02(16) . . ? 

C34 Mo P1 112.51(18) . . ? 

O Mo P2 81.70(9) . . ? 

C33 Mo P2 98.13(19) . . ? 

C36 Mo P2 156.48(11) . . ? 

C31 Mo P2 120.30(12) . . ? 

C32 Mo P2 97.19(17) . . ? 

C35 Mo P2 159.06(17) . . ? 

C34 Mo P2 124.88(19) . . ? 

P1 Mo P2 95.15(5) . . ? 

C12 P1 C13 101.6(3) . . ? 

C12 P1 C11 101.7(4) . . ? 

C13 P1 C11 100.9(4) . . ? 

C12 P1 Mo 118.6(2) . . ? 

C13 P1 Mo 119.0(2) . . ? 

C11 P1 Mo 112.3(3) . . ? 

C21 P2 C22 99.7(4) . . ? 

C21 P2 C23 101.8(3) . . ? 

C22 P2 C23 101.1(4) . . ? 

C21 P2 Mo 113.8(3) . . ? 

C22 P2 Mo 120.5(2) . . ? 

C23 P2 Mo 117.0(2) . . ? 

C41 O Mo 118.3(3) . . ? 

C32 C31 C36 121.9(5) . . ? 

C32 C31 C42 119.4(5) . . ? 

C36 C31 C42 116.1(4) . . ? 

C32 C31 Mo 73.6(3) . . ? 

C36 C31 Mo 71.3(3) . . ? 

C42 C31 Mo 111.9(3) . . ? 

C31 C32 C33 118.4(6) . . ? 

C31 C32 Mo 71.0(3) . . ? 

C33 C32 Mo 69.7(3) . . ? 

C32 C33 C34 119.7(6) . . ? 

C32 C33 Mo 74.0(3) . . ? 

C34 C33 Mo 75.1(4) . . ? 

C35 C34 C33 121.3(5) . . ? 

C35 C34 Mo 72.4(3) . . ? 

C33 C34 Mo 68.6(3) . . ? 

C34 C35 C36 119.6(6) . . ? 

C34 C35 Mo 73.3(3) . . ? 

C36 C35 Mo 69.6(3) . . ? 

C35 C36 C31 118.4(5) . . ? 

C35 C36 Mo 74.1(3) . . ? 

C31 C36 Mo 71.8(3) . . ? 

O C41 C42 120.4(4) . . ? 

O C41 C46 121.8(4) . . ? 

C42 C41 C46 117.7(4) . . ? 

C43 C42 C41 121.5(4) . . ? 

C43 C42 C31 124.7(4) . . ? 

C41 C42 C31 113.8(4) . . ? 

C44 C43 C42 120.5(5) . . ? 

C43 C44 C45 118.6(4) . . ? 

C46 C45 C44 122.9(4) . . ? 

C45 C46 C41 118.7(4) . . ? 

C45 C46 C51 120.7(4) . . ? 

C41 C46 C51 120.6(4) . . ? 

C52 C51 C56 118.0(5) . . ? 

C52 C51 C46 122.6(4) . . ? 

C56 C51 C46 119.3(4) . . ? 

C53 C52 C51 121.2(5) . . ? 

C52 C53 C54 120.2(5) . . ? 

C55 C54 C53 119.1(5) . . ? 

C54 C55 C56 121.1(5) . . ? 

C55 C56 C51 120.5(5) . . ? 



_diffrn_measured_fraction_theta_max    0.927 

_diffrn_reflns_theta_full              28.27 

_diffrn_measured_fraction_theta_full   0.927 

_refine_diff_density_max    1.278 

_refine_diff_density_min   -2.267 

_refine_diff_density_rms    0.137 





data_mops10 



_database_code_CSD	193308





_audit_creation_method            SHELXL-97 

_chemical_name_systematic 

; 

? 

; 

_chemical_name_common             ? 

_chemical_melting_point           ? 

_chemical_formula_moiety          ? 

_chemical_formula_sum 

'C27 H41 Mo O P3' 

_chemical_formula_weight          570.45 



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' 

'O'  'O'   0.0106   0.0060 

'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

'P'  'P'   0.1023   0.0942 

'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

'Mo'  'Mo'  -1.6832   0.6857 

'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 



_symmetry_cell_setting            Monoclinic 

_symmetry_space_group_name_H-M    P2(1)/n 



loop_ 

_symmetry_equiv_pos_as_xyz 

'x, y, z' 

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

'-x, -y, -z' 

'x-1/2, -y-1/2, z-1/2' 



_cell_length_a                    8.3296(7) 

_cell_length_b                    20.6245(18) 

_cell_length_c                    16.2550(14) 

_cell_angle_alpha                 90.00 

_cell_angle_beta                  95.106(2) 

_cell_angle_gamma                 90.00 

_cell_volume                      2781.4(4) 

_cell_formula_units_Z             4 

_cell_measurement_temperature     223(2) 

_cell_measurement_reflns_used     ? 

_cell_measurement_theta_min       ? 

_cell_measurement_theta_max       ? 



_exptl_crystal_description        ? 

_exptl_crystal_colour             ? 

_exptl_crystal_size_max           0.20 

_exptl_crystal_size_mid           0.20 

_exptl_crystal_size_min           0.10 

_exptl_crystal_density_meas       ? 

_exptl_crystal_density_diffrn     1.362 

_exptl_crystal_density_method     'not measured' 

_exptl_crystal_F_000              1192 

_exptl_absorpt_coefficient_mu     0.661 

_exptl_absorpt_correction_type    none 

_exptl_absorpt_correction_T_min   0.8791 

_exptl_absorpt_correction_T_max   0.9368 

_exptl_absorpt_process_details    ? 



_exptl_special_details 

; 

? 

; 



_diffrn_ambient_temperature       223(2) 

_diffrn_radiation_wavelength      0.71073 

_diffrn_radiation_type            MoK\a 

_diffrn_radiation_source          'fine-focus sealed tube' 

_diffrn_radiation_monochromator   graphite 

_diffrn_measurement_device_type   'CCD area detector' 

_diffrn_measurement_method        'phi and omega scans' 

_diffrn_detector_area_resol_mean  ? 

_diffrn_standards_number          ? 

_diffrn_standards_interval_count  ? 

_diffrn_standards_interval_time   ? 

_diffrn_standards_decay_%         ? 

_diffrn_reflns_number             20599 

_diffrn_reflns_av_R_equivalents   0.0296 

_diffrn_reflns_av_sigmaI/netI     0.0265 

_diffrn_reflns_limit_h_min        -11 

_diffrn_reflns_limit_h_max        10 

_diffrn_reflns_limit_k_min        -26 

_diffrn_reflns_limit_k_max        27 

_diffrn_reflns_limit_l_min        -21 

_diffrn_reflns_limit_l_max        21 

_diffrn_reflns_theta_min          1.60 

_diffrn_reflns_theta_max          28.30 

_reflns_number_total              6451 

_reflns_number_gt                 5150 

_reflns_threshold_expression      >2sigma(I) 



_computing_data_collection        'Bruker SMART' 

_computing_cell_refinement        'Bruker SMART' 

_computing_data_reduction         'Bruker SHELXTL' 

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 

_computing_molecular_graphics     'Bruker SHELXTL' 

_computing_publication_material   'Bruker SHELXTL' 



_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 

'calc w=1/[σ²(Fo²)+(0.0438P)²+1.2120P] 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      SHELXL 

_refine_ls_extinction_coef        0.00000(18) 

_refine_ls_extinction_expression 

'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 

_refine_ls_number_reflns          6451 

_refine_ls_number_parameters      303 

_refine_ls_number_restraints      0 

_refine_ls_R_factor_all           0.0435 

_refine_ls_R_factor_gt            0.0297 

_refine_ls_wR_factor_ref          0.0842 

_refine_ls_wR_factor_gt           0.0748 

_refine_ls_goodness_of_fit_ref    1.060 

_refine_ls_restrained_S_all       1.060 

_refine_ls_shift/su_max           1.642 

_refine_ls_shift/su_mean          0.006 



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 

Mo Mo 0.181193(18) 0.251019(8) 0.501217(10) 0.02275(7) Uani 1 1 d . . . 

P1 P -0.01483(6) 0.28258(3) 0.59821(3) 0.03132(13) Uani 1 1 d . . . 

P2 P 0.01912(7) 0.16584(3) 0.42853(4) 0.03071(13) Uani 1 1 d . . . 

P3 P 0.05961(7) 0.33031(3) 0.40194(3) 0.03050(13) Uani 1 1 d . . . 

O O 0.13957(18) 0.13735(8) 0.66365(10) 0.0351(4) Uani 1 1 d . . . 

H H 0.141(3) 0.1654(14) 0.6283(17) 0.051(9) Uiso 1 1 d . . . 

C11 C -0.1884(3) 0.23125(17) 0.6154(2) 0.0578(8) Uani 1 1 d . . . 

H11A H -0.2416 0.2480 0.6617 0.087 Uiso 1 1 calc R . . 

H11B H -0.1519 0.1873 0.6274 0.087 Uiso 1 1 calc R . . 

H11C H -0.2635 0.2313 0.5662 0.087 Uiso 1 1 calc R . . 

C12 C -0.1234(4) 0.36042(15) 0.59037(17) 0.0582(8) Uani 1 1 d . . . 

H12A H -0.1875 0.3628 0.5376 0.087 Uiso 1 1 calc R . . 

H12B H -0.0464 0.3958 0.5947 0.087 Uiso 1 1 calc R . . 

H12C H -0.1936 0.3637 0.6347 0.087 Uiso 1 1 calc R . . 

C13 C 0.0672(3) 0.29256(16) 0.70680(15) 0.0542(8) Uani 1 1 d . . . 

H13A H -0.0167 0.3085 0.7392 0.081 Uiso 1 1 calc R . . 

H13B H 0.1557 0.3233 0.7096 0.081 Uiso 1 1 calc R . . 

H13C H 0.1059 0.2511 0.7286 0.081 Uiso 1 1 calc R . . 

C21 C -0.2024(3) 0.16059(15) 0.4181(2) 0.0575(8) Uani 1 1 d . . . 

H21A H -0.2473 0.2013 0.3968 0.086 Uiso 1 1 calc R . . 

H21B H -0.2405 0.1519 0.4717 0.086 Uiso 1 1 calc R . . 

H21C H -0.2361 0.1258 0.3803 0.086 Uiso 1 1 calc R . . 

C22 C 0.0578(3) 0.08184(12) 0.46176(17) 0.0482(6) Uani 1 1 d . . . 

H22A H -0.0023 0.0526 0.4238 0.072 Uiso 1 1 calc R . . 

H22B H 0.0242 0.0759 0.5169 0.072 Uiso 1 1 calc R . . 

H22C H 0.1721 0.0726 0.4621 0.072 Uiso 1 1 calc R . . 

C23 C 0.0531(4) 0.15709(14) 0.31876(16) 0.0528(7) Uani 1 1 d . . . 

H23A H 0.1679 0.1547 0.3132 0.079 Uiso 1 1 calc R . . 

H23B H 0.0078 0.1942 0.2882 0.079 Uiso 1 1 calc R . . 

H23C H 0.0014 0.1178 0.2970 0.079 Uiso 1 1 calc R . . 

C31 C -0.1543(3) 0.32864(13) 0.36224(16) 0.0461(6) Uani 1 1 d . . . 

H31A H -0.1802 0.3677 0.3305 0.069 Uiso 1 1 calc R . . 

H31B H -0.2209 0.3264 0.4082 0.069 Uiso 1 1 calc R . . 

H31C H -0.1746 0.2909 0.3272 0.069 Uiso 1 1 calc R . . 

C32 C 0.0808(3) 0.41701(12) 0.42821(17) 0.0451(6) Uani 1 1 d . . . 

H32A H 0.1931 0.4267 0.4443 0.068 Uiso 1 1 calc R . . 

H32B H 0.0168 0.4269 0.4736 0.068 Uiso 1 1 calc R . . 

H32C H 0.0436 0.4430 0.3805 0.068 Uiso 1 1 calc R . . 

C33 C 0.1498(3) 0.33421(14) 0.30291(15) 0.0494(7) Uani 1 1 d . . . 

H33A H 0.0937 0.3665 0.2678 0.074 Uiso 1 1 calc R . . 

H33B H 0.1405 0.2922 0.2760 0.074 Uiso 1 1 calc R . . 

H33C H 0.2626 0.3460 0.3127 0.074 Uiso 1 1 calc R . . 

C41 C 0.3787(2) 0.18106(11) 0.56000(13) 0.0298(4) Uani 1 1 d . . . 

C42 C 0.3724(2) 0.23892(11) 0.60870(15) 0.0324(5) Uani 1 1 d . . . 

H42A H 0.3385 0.2357 0.6654 0.039 Uiso 1 1 calc R . . 

C43 C 0.3959(2) 0.30155(12) 0.57426(15) 0.0360(5) Uani 1 1 d . . . 

H43A H 0.3774 0.3409 0.6070 0.043 Uiso 1 1 calc R . . 

C44 C 0.4122(2) 0.30700(12) 0.48901(16) 0.0391(5) Uani 1 1 d . . . 

H44A H 0.4069 0.3503 0.4627 0.047 Uiso 1 1 calc R . . 

C45 C 0.4164(3) 0.25047(12) 0.43851(17) 0.0396(6) Uani 1 1 d . . . 

H45A H 0.4134 0.2550 0.3778 0.047 Uiso 1 1 calc R . . 

C46 C 0.3973(2) 0.18878(12) 0.47388(14) 0.0341(5) Uani 1 1 d . . . 

H46A H 0.3793 0.1508 0.4369 0.041 Uiso 1 1 calc R . . 

C51 C 0.2656(2) 0.09714(11) 0.65225(13) 0.0308(5) Uani 1 1 d . . . 

C52 C 0.3824(2) 0.11635(11) 0.59959(13) 0.0307(4) Uani 1 1 d . . . 

C53 C 0.5051(3) 0.07215(12) 0.58665(16) 0.0402(5) Uani 1 1 d . . . 

H53A H 0.5817 0.0828 0.5498 0.048 Uiso 1 1 calc R . . 

C54 C 0.5160(3) 0.01306(13) 0.62700(18) 0.0463(6) Uani 1 1 d . . . 

H54A H 0.5996 -0.0159 0.6177 0.056 Uiso 1 1 calc R . . 

C55 C 0.4035(3) -0.00332(12) 0.68099(16) 0.0415(6) Uani 1 1 d . . . 

H55A H 0.4138 -0.0429 0.7096 0.050 Uiso 1 1 calc R . . 

C56 C 0.2742(3) 0.03788(11) 0.69404(14) 0.0336(5) Uani 1 1 d . . . 

C61 C 0.1548(3) 0.01912(11) 0.75262(14) 0.0343(5) Uani 1 1 d . . . 

C62 C 0.2059(3) -0.00855(12) 0.82869(16) 0.0454(6) Uani 1 1 d . . . 

H62A H 0.3166 -0.0156 0.8423 0.055 Uiso 1 1 calc R . . 

C63 C 0.0977(4) -0.02586(13) 0.88462(17) 0.0544(7) Uani 1 1 d . . . 

H63A H 0.1356 -0.0438 0.9359 0.065 Uiso 1 1 calc R . . 

C64 C -0.0657(4) -0.01688(13) 0.86560(17) 0.0508(7) Uani 1 1 d . . . 

H64A H -0.1394 -0.0285 0.9036 0.061 Uiso 1 1 calc R . . 

C65 C -0.1190(3) 0.00930(13) 0.79049(17) 0.0468(6) Uani 1 1 d . . . 

H65A H -0.2301 0.0148 0.7768 0.056 Uiso 1 1 calc R . . 

C66 C -0.0110(3) 0.02773(12) 0.73446(15) 0.0382(5) Uani 1 1 d . . . 

H66A H -0.0499 0.0462 0.6837 0.046 Uiso 1 1 calc R . . 






_geom_special_details 

; 

All esds (except the esd in the dihedral angle between two l.s. planes) 

are estimated using the full covariance matrix.  The cell esds are taken 

into account individually in the estimation of esds in distances, angles 

and torsion angles; correlations between esds in cell parameters are only 

used when they are defined by crystal symmetry.  An approximate (isotropic) 

treatment of cell esds is used for estimating esds involving l.s. planes. 

; 



loop_ 

_geom_bond_atom_site_label_1 

_geom_bond_atom_site_label_2 

_geom_bond_distance 

_geom_bond_site_symmetry_2 

_geom_bond_publ_flag 

Mo C44 2.268(2) . ? 

Mo C42 2.271(2) . ? 

Mo C46 2.287(2) . ? 

Mo C45 2.288(2) . ? 

Mo C43 2.306(2) . ? 

Mo C41 2.328(2) . ? 

Mo P3 2.4522(6) . ? 

Mo P2 2.4538(6) . ? 

Mo P1 2.4564(6) . ? 

P1 C11 1.833(3) . ? 

P1 C12 1.842(3) . ? 

P1 C13 1.847(3) . ? 

P2 C22 1.835(3) . ? 

P2 C23 1.840(3) . ? 

P2 C21 1.841(3) . ? 

P3 C33 1.838(2) . ? 

P3 C31 1.841(2) . ? 

P3 C32 1.843(3) . ? 

O C51 1.363(2) . ? 

C41 C46 1.431(3) . ? 

C41 C42 1.435(3) . ? 

C41 C52 1.481(3) . ? 

C42 C43 1.428(3) . ? 

C43 C44 1.409(3) . ? 

C44 C45 1.428(4) . ? 

C45 C46 1.411(3) . ? 

C51 C56 1.397(3) . ? 

C51 C52 1.409(3) . ? 

C52 C53 1.400(3) . ? 

C53 C54 1.383(4) . ? 

C54 C55 1.381(4) . ? 

C55 C56 1.402(3) . ? 

C56 C61 1.488(3) . ? 

C61 C62 1.394(3) . ? 

C61 C66 1.398(3) . ? 

C62 C63 1.383(4) . ? 

C63 C64 1.381(4) . ? 

C64 C65 1.372(4) . ? 

C65 C66 1.389(3) . ? 



loop_ 

_geom_angle_atom_site_label_1 

_geom_angle_atom_site_label_2 

_geom_angle_atom_site_label_3 

_geom_angle 

_geom_angle_site_symmetry_1 

_geom_angle_site_symmetry_3 

_geom_angle_publ_flag 

C44 Mo C42 65.22(9) . . ? 

C44 Mo C46 65.16(9) . . ? 

C42 Mo C46 65.00(8) . . ? 

C44 Mo C45 36.54(9) . . ? 

C42 Mo C45 76.85(9) . . ? 

C46 Mo C45 35.93(8) . . ? 

C44 Mo C43 35.87(9) . . ? 

C42 Mo C43 36.36(8) . . ? 

C46 Mo C43 76.46(8) . . ? 

C45 Mo C43 64.91(9) . . ? 

C44 Mo C41 77.14(8) . . ? 

C42 Mo C41 36.35(8) . . ? 

C46 Mo C41 36.11(8) . . ? 

C45 Mo C41 65.03(8) . . ? 

C43 Mo C41 65.26(8) . . ? 

C44 Mo P3 84.66(6) . . ? 

C42 Mo P3 143.13(6) . . ? 

C46 Mo P3 122.19(6) . . ? 

C45 Mo P3 91.72(7) . . ? 

C43 Mo P3 107.06(6) . . ? 

C41 Mo P3 156.73(5) . . ? 

C44 Mo P2 139.21(7) . . ? 

C42 Mo P2 127.59(6) . . ? 

C46 Mo P2 85.03(6) . . ? 

C45 Mo P2 103.78(7) . . ? 

C43 Mo P2 160.03(6) . . ? 

C41 Mo P2 95.29(6) . . ? 

P3 Mo P2 89.04(2) . . ? 

C44 Mo P1 122.61(7) . . ? 

C42 Mo P1 89.77(6) . . ? 

C46 Mo P1 148.57(6) . . ? 

C45 Mo P1 158.73(7) . . ? 

C43 Mo P1 94.54(6) . . ? 

C41 Mo P1 112.74(5) . . ? 

P3 Mo P1 89.23(2) . . ? 

P2 Mo P1 97.48(2) . . ? 

C11 P1 C12 97.17(15) . . ? 

C11 P1 C13 98.54(15) . . ? 

C12 P1 C13 96.12(14) . . ? 

C11 P1 Mo 121.54(11) . . ? 

C12 P1 Mo 122.48(9) . . ? 

C13 P1 Mo 115.62(9) . . ? 

C22 P2 C23 98.91(13) . . ? 

C22 P2 C21 96.89(14) . . ? 

C23 P2 C21 98.29(15) . . ? 

C22 P2 Mo 117.36(9) . . ? 

C23 P2 Mo 114.31(9) . . ? 

C21 P2 Mo 126.18(10) . . ? 

C33 P3 C31 98.74(13) . . ? 

C33 P3 C32 97.03(13) . . ? 

C31 P3 C32 99.74(12) . . ? 

C33 P3 Mo 115.38(10) . . ? 

C31 P3 Mo 123.26(9) . . ? 

C32 P3 Mo 117.98(9) . . ? 

C46 C41 C42 117.4(2) . . ? 

C46 C41 C52 121.7(2) . . ? 

C42 C41 C52 120.65(19) . . ? 

C46 C41 Mo 70.36(12) . . ? 

C42 C41 Mo 69.64(12) . . ? 

C52 C41 Mo 136.35(14) . . ? 

C43 C42 C41 121.5(2) . . ? 

C43 C42 Mo 73.15(13) . . ? 

C41 C42 Mo 74.01(12) . . ? 

C44 C43 C42 119.1(2) . . ? 

C44 C43 Mo 70.61(13) . . ? 

C42 C43 Mo 70.48(12) . . ? 

C43 C44 C45 120.6(2) . . ? 

C43 C44 Mo 73.52(12) . . ? 

C45 C44 Mo 72.48(13) . . ? 

C46 C45 C44 119.5(2) . . ? 

C46 C45 Mo 71.99(12) . . ? 

C44 C45 Mo 70.98(12) . . ? 

C45 C46 C41 121.7(2) . . ? 

C45 C46 Mo 72.08(13) . . ? 

C41 C46 Mo 73.53(12) . . ? 

O C51 C56 118.2(2) . . ? 

O C51 C52 119.6(2) . . ? 

C56 C51 C52 122.2(2) . . ? 

C53 C52 C51 117.5(2) . . ? 

C53 C52 C41 120.6(2) . . ? 

C51 C52 C41 121.92(19) . . ? 

C54 C53 C52 121.4(2) . . ? 

C55 C54 C53 119.8(2) . . ? 

C54 C55 C56 121.4(2) . . ? 

C51 C56 C55 117.6(2) . . ? 

C51 C56 C61 122.0(2) . . ? 

C55 C56 C61 120.3(2) . . ? 

C62 C61 C66 117.2(2) . . ? 

C62 C61 C56 120.4(2) . . ? 

C66 C61 C56 122.4(2) . . ? 

C63 C62 C61 121.6(3) . . ? 

C64 C63 C62 120.3(3) . . ? 

C65 C64 C63 119.1(3) . . ? 

C64 C65 C66 121.0(3) . . ? 

C65 C66 C61 120.8(2) . . ? 



_diffrn_measured_fraction_theta_max    0.932 

_diffrn_reflns_theta_full              28.30 

_diffrn_measured_fraction_theta_full   0.932 

_refine_diff_density_max    0.529 

_refine_diff_density_min   -0.886 

_refine_diff_density_rms    0.071 







data_woars10 



_database_code_CSD	193309





_audit_creation_method            SHELXL-97 

_chemical_name_systematic 

; 

? 

; 

_chemical_name_common             ? 

_chemical_melting_point           ? 

_chemical_formula_moiety          ? 

_chemical_formula_sum 

'C24 H32 O P2 W' 

_chemical_formula_weight          582.29 



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' 

'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    P2(1)/n 



loop_ 

_symmetry_equiv_pos_as_xyz 

'x, y, z' 

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

'-x, -y, -z' 

'x-1/2, -y-1/2, z-1/2' 



_cell_length_a                    10.5899(5) 

_cell_length_b                    15.9694(7) 

_cell_length_c                    14.0653(6) 

_cell_angle_alpha                 90.00 

_cell_angle_beta                  90.5850(10) 

_cell_angle_gamma                 90.00 

_cell_volume                      2378.52(18) 

_cell_formula_units_Z             4 

_cell_measurement_temperature     223(2) 

_cell_measurement_reflns_used     ? 

_cell_measurement_theta_min       ? 

_cell_measurement_theta_max       ? 



_exptl_crystal_description        ? 

_exptl_crystal_colour             ? 

_exptl_crystal_size_max           0.30 

_exptl_crystal_size_mid           0.30 

_exptl_crystal_size_min           0.10 

_exptl_crystal_density_meas       ? 

_exptl_crystal_density_diffrn     1.626 

_exptl_crystal_density_method     'not measured' 

_exptl_crystal_F_000              1152 

_exptl_absorpt_coefficient_mu     5.003 

_exptl_absorpt_correction_type    none 

_exptl_absorpt_correction_T_min   0.3153 

_exptl_absorpt_correction_T_max   0.6346 

_exptl_absorpt_process_details    ? 



_exptl_special_details 

; 

? 

; 



_diffrn_ambient_temperature       223(2) 

_diffrn_radiation_wavelength      0.71073 

_diffrn_radiation_type            MoK\a 

_diffrn_radiation_source          'fine-focus sealed tube' 

_diffrn_radiation_monochromator   graphite 

_diffrn_measurement_device_type   'CCD area detector' 

_diffrn_measurement_method        'phi and omega scans' 

_diffrn_detector_area_resol_mean  ? 

_diffrn_standards_number          ? 

_diffrn_standards_interval_count  ? 

_diffrn_standards_interval_time   ? 

_diffrn_standards_decay_%         ? 

_diffrn_reflns_number             17646 

_diffrn_reflns_av_R_equivalents   0.0306 

_diffrn_reflns_av_sigmaI/netI     0.0322 

_diffrn_reflns_limit_h_min        -13 

_diffrn_reflns_limit_h_max        13 

_diffrn_reflns_limit_k_min        -20 

_diffrn_reflns_limit_k_max        17 

_diffrn_reflns_limit_l_min        -14 

_diffrn_reflns_limit_l_max        18 

_diffrn_reflns_theta_min          1.93 

_diffrn_reflns_theta_max          28.31 

_reflns_number_total              5511 

_reflns_number_gt                 4488 

_reflns_threshold_expression      >2sigma(I) 



_computing_data_collection        'Bruker SMART' 

_computing_cell_refinement        'Bruker SMART' 

_computing_data_reduction         'Bruker SHELXTL' 

_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 

_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 

_computing_molecular_graphics     'Bruker SHELXTL' 

_computing_publication_material   'Bruker SHELXTL' 



_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 

'calc w=1/[σ²(Fo²)+(0.0218P)²+0.6641P] 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_number_reflns          5511 

_refine_ls_number_parameters      263 

_refine_ls_number_restraints      0 

_refine_ls_R_factor_all           0.0359 

_refine_ls_R_factor_gt            0.0233 

_refine_ls_wR_factor_ref          0.0506 

_refine_ls_wR_factor_gt           0.0475 

_refine_ls_goodness_of_fit_ref    1.005 

_refine_ls_restrained_S_all       1.005 

_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 

W W 0.311971(11) 0.195090(7) 0.874695(9) 0.03132(5) Uani 1 1 d . . . 

H1 H 0.457(3) 0.211(2) 0.848(2) 0.055(10) Uiso 1 1 d . . . 

O O 0.12912(18) 0.25475(12) 0.87520(14) 0.0321(4) Uani 1 1 d . . . 

P1 P 0.36483(8) 0.32598(5) 0.95456(6) 0.0394(2) Uani 1 1 d . . . 

P2 P 0.31437(8) 0.25544(6) 0.71505(6) 0.0399(2) Uani 1 1 d . . . 

C11 C 0.3171(5) 0.3275(3) 1.0781(3) 0.0797(15) Uani 1 1 d . . . 

H11A H 0.3590 0.2824 1.1123 0.120 Uiso 1 1 calc R . . 

H11B H 0.2263 0.3202 1.0817 0.120 Uiso 1 1 calc R . . 

H11C H 0.3404 0.3807 1.1065 0.120 Uiso 1 1 calc R . . 

C12 C 0.5309(4) 0.3537(3) 0.9661(3) 0.0704(13) Uani 1 1 d . . . 

H12A H 0.5397 0.4017 1.0079 0.106 Uiso 1 1 calc R . . 

H12B H 0.5641 0.3674 0.9040 0.106 Uiso 1 1 calc R . . 

H12C H 0.5775 0.3067 0.9926 0.106 Uiso 1 1 calc R . . 

C13 C 0.2956(4) 0.4247(2) 0.9139(3) 0.0664(11) Uani 1 1 d . . . 

H13A H 0.2068 0.4163 0.8991 0.100 Uiso 1 1 calc R . . 

H13B H 0.3390 0.4436 0.8574 0.100 Uiso 1 1 calc R . . 

H13C H 0.3043 0.4665 0.9635 0.100 Uiso 1 1 calc R . . 

C21 C 0.4358(4) 0.3316(3) 0.6827(3) 0.0872(16) Uani 1 1 d . . . 

H21A H 0.5186 0.3063 0.6901 0.131 Uiso 1 1 calc R . . 

H21B H 0.4299 0.3802 0.7238 0.131 Uiso 1 1 calc R . . 

H21C H 0.4233 0.3486 0.6171 0.131 Uiso 1 1 calc R . . 

C22 C 0.3348(6) 0.1786(3) 0.6209(3) 0.0873(17) Uani 1 1 d . . . 

H22A H 0.2686 0.1368 0.6247 0.131 Uiso 1 1 calc R . . 

H22B H 0.4164 0.1518 0.6282 0.131 Uiso 1 1 calc R . . 

H22C H 0.3301 0.2064 0.5596 0.131 Uiso 1 1 calc R . . 

C23 C 0.1727(4) 0.3098(2) 0.6744(3) 0.0596(11) Uani 1 1 d . . . 

H23A H 0.1814 0.3247 0.6079 0.089 Uiso 1 1 calc R . . 

H23B H 0.1611 0.3602 0.7118 0.089 Uiso 1 1 calc R . . 

H23C H 0.1000 0.2734 0.6817 0.089 Uiso 1 1 calc R . . 

C31 C 0.1710(3) 0.09258(18) 0.9153(2) 0.0341(7) Uani 1 1 d . . . 

C32 C 0.2340(3) 0.06623(19) 0.8335(3) 0.0457(8) Uani 1 1 d . . . 

H32A H 0.1868 0.0590 0.7730 0.055 Uiso 1 1 calc R . . 

C33 C 0.3685(4) 0.0642(2) 0.8342(3) 0.0617(11) Uani 1 1 d . . . 

H33A H 0.4150 0.0540 0.7746 0.074 Uiso 1 1 calc R . . 

C34 C 0.4354(4) 0.0796(2) 0.9205(4) 0.0661(13) Uani 1 1 d . . . 

H34A H 0.5284 0.0852 0.9176 0.079 Uiso 1 1 calc R . . 

C35 C 0.3747(3) 0.1114(2) 0.9996(3) 0.0543(10) Uani 1 1 d . . . 

H35A H 0.4248 0.1356 1.0527 0.065 Uiso 1 1 calc R . . 

C36 C 0.2399(3) 0.12044(19) 0.9982(2) 0.0369(7) Uani 1 1 d . . . 

H36A H 0.1959 0.1483 1.0512 0.044 Uiso 1 1 calc R . . 

C41 C 0.0260(3) 0.20799(17) 0.88506(19) 0.0293(6) Uani 1 1 d . . . 

C42 C 0.0383(3) 0.12155(18) 0.9059(2) 0.0297(6) Uani 1 1 d . . . 

C43 C -0.0663(3) 0.07031(19) 0.9141(2) 0.0375(7) Uani 1 1 d . . . 

H43A H -0.0559 0.0129 0.9266 0.045 Uiso 1 1 calc R . . 

C44 C -0.1864(3) 0.1037(2) 0.9038(2) 0.0423(8) Uani 1 1 d . . . 

H44A H -0.2578 0.0694 0.9111 0.051 Uiso 1 1 calc R . . 

C45 C -0.2005(3) 0.18749(19) 0.8826(2) 0.0386(7) Uani 1 1 d . . . 

H45A H -0.2824 0.2093 0.8748 0.046 Uiso 1 1 calc R . . 

C46 C -0.0975(3) 0.24114(18) 0.87255(19) 0.0292(6) Uani 1 1 d . . . 

C51 C -0.1180(3) 0.33081(19) 0.8478(2) 0.0306(6) Uani 1 1 d . . . 

C52 C -0.0528(3) 0.39488(19) 0.8946(2) 0.0382(7) Uani 1 1 d . . . 

H52A H 0.0066 0.3815 0.9424 0.046 Uiso 1 1 calc R . . 

C53 C -0.0746(3) 0.4774(2) 0.8716(2) 0.0432(8) Uani 1 1 d . . . 

H53A H -0.0300 0.5197 0.9041 0.052 Uiso 1 1 calc R . . 

C54 C -0.1609(4) 0.4989(2) 0.8016(2) 0.0474(9) Uani 1 1 d . . . 

H54A H -0.1741 0.5553 0.7854 0.057 Uiso 1 1 calc R . . 

C55 C -0.2273(3) 0.4363(2) 0.7561(2) 0.0495(9) Uani 1 1 d . . . 

H55A H -0.2881 0.4502 0.7095 0.059 Uiso 1 1 calc R . . 

C56 C -0.2054(3) 0.3536(2) 0.7781(2) 0.0401(8) Uani 1 1 d . . . 

H56A H -0.2504 0.3117 0.7454 0.048 Uiso 1 1 calc R . . 






_geom_special_details 

; 

All esds (except the esd in the dihedral angle between two l.s. planes) 

are estimated using the full covariance matrix.  The cell esds are taken 

into account individually in the estimation of esds in distances, angles 

and torsion angles; correlations between esds in cell parameters are only 

used when they are defined by crystal symmetry.  An approximate (isotropic) 

treatment of cell esds is used for estimating esds involving l.s. planes. 

; 



loop_ 

_geom_bond_atom_site_label_1 

_geom_bond_atom_site_label_2 

_geom_bond_distance 

_geom_bond_site_symmetry_2 

_geom_bond_publ_flag 

W H1 1.60(4) . ? 

W O 2.158(2) . ? 

W C36 2.246(3) . ? 

W C33 2.249(4) . ? 

W C32 2.289(3) . ? 

W C31 2.292(3) . ? 

W C35 2.300(3) . ? 

W C34 2.347(3) . ? 

W P1 2.4354(9) . ? 

W P2 2.4439(8) . ? 

O C41 1.331(3) . ? 

P1 C11 1.815(4) . ? 

P1 C12 1.819(4) . ? 

P1 C13 1.828(4) . ? 

P2 C22 1.819(4) . ? 

P2 C23 1.820(4) . ? 

P2 C21 1.831(4) . ? 

C31 C32 1.400(4) . ? 

C31 C36 1.440(4) . ? 

C31 C42 1.484(4) . ? 

C32 C33 1.424(5) . ? 

C33 C34 1.420(6) . ? 

C34 C35 1.388(6) . ? 

C35 C36 1.434(5) . ? 

C41 C42 1.417(4) . ? 

C41 C46 1.421(4) . ? 

C42 C43 1.383(4) . ? 

C43 C44 1.385(4) . ? 

C44 C45 1.379(4) . ? 

C45 C46 1.395(4) . ? 

C46 C51 1.489(4) . ? 

C51 C56 1.389(4) . ? 

C51 C52 1.396(4) . ? 

C52 C53 1.376(4) . ? 

C53 C54 1.380(5) . ? 

C54 C55 1.376(5) . ? 

C55 C56 1.376(4) . ? 



loop_ 

_geom_angle_atom_site_label_1 

_geom_angle_atom_site_label_2 

_geom_angle_atom_site_label_3 

_geom_angle 

_geom_angle_site_symmetry_1 

_geom_angle_site_symmetry_3 

_geom_angle_publ_flag 

H1 W O 142.5(12) . . ? 

H1 W C36 126.8(12) . . ? 

O W C36 85.41(10) . . ? 

H1 W C33 79.9(12) . . ? 

O W C33 130.72(12) . . ? 

C36 W C33 78.23(14) . . ? 

H1 W C32 114.9(12) . . ? 

O W C32 94.39(10) . . ? 

C36 W C32 66.05(12) . . ? 

C33 W C32 36.57(13) . . ? 

H1 W C31 142.8(12) . . ? 

O W C31 74.20(9) . . ? 

C36 W C31 36.98(11) . . ? 

C33 W C31 64.86(12) . . ? 

C32 W C31 35.59(11) . . ? 

H1 W C35 90.1(12) . . ? 

O W C35 120.39(12) . . ? 

C36 W C35 36.74(12) . . ? 

C33 W C35 65.04(16) . . ? 

C32 W C35 76.79(13) . . ? 

C31 W C35 65.06(12) . . ? 

H1 W C34 69.8(12) . . ? 

O W C34 147.49(11) . . ? 

C36 W C34 64.11(13) . . ? 

C33 W C34 35.92(16) . . ? 

C32 W C34 63.98(15) . . ? 

C31 W C34 74.50(12) . . ? 

C35 W C34 34.73(14) . . ? 

H1 W P1 76.2(12) . . ? 

O W P1 79.72(6) . . ? 

C36 W P1 100.20(9) . . ? 

C33 W P1 148.63(12) . . ? 

C32 W P1 165.62(9) . . ? 

C31 W P1 130.20(8) . . ? 

C35 W P1 94.76(11) . . ? 

C34 W P1 115.03(13) . . ? 

H1 W P2 72.7(12) . . ? 

O W P2 81.18(6) . . ? 

C36 W P2 157.88(8) . . ? 

C33 W P2 97.39(12) . . ? 

C32 W P2 97.43(10) . . ? 

C31 W P2 121.56(8) . . ? 

C35 W P2 157.73(11) . . ? 

C34 W P2 123.44(12) . . ? 

P1 W P2 94.64(3) . . ? 

C41 O W 119.31(17) . . ? 

C11 P1 C12 100.9(2) . . ? 

C11 P1 C13 100.0(2) . . ? 

C12 P1 C13 101.7(2) . . ? 

C11 P1 W 112.84(16) . . ? 

C12 P1 W 117.87(14) . . ? 

C13 P1 W 120.41(14) . . ? 

C22 P2 C23 101.3(2) . . ? 

C22 P2 C21 100.3(3) . . ? 

C23 P2 C21 100.6(2) . . ? 

C22 P2 W 113.90(15) . . ? 

C23 P2 W 117.42(14) . . ? 

C21 P2 W 120.26(15) . . ? 

C32 C31 C36 121.0(3) . . ? 

C32 C31 C42 118.7(3) . . ? 

C36 C31 C42 116.6(3) . . ? 

C32 C31 W 72.11(18) . . ? 

C36 C31 W 69.80(16) . . ? 

C42 C31 W 111.96(19) . . ? 

C31 C32 C33 119.1(3) . . ? 

C31 C32 W 72.30(18) . . ? 

C33 C32 W 70.2(2) . . ? 

C34 C33 C32 119.5(4) . . ? 

C34 C33 W 75.8(2) . . ? 

C32 C33 W 73.26(19) . . ? 

C35 C34 C33 121.2(3) . . ? 

C35 C34 W 70.8(2) . . ? 

C33 C34 W 68.3(2) . . ? 

C34 C35 C36 119.6(4) . . ? 

C34 C35 W 74.5(2) . . ? 

C36 C35 W 69.58(17) . . ? 

C35 C36 C31 118.5(3) . . ? 

C35 C36 W 73.68(19) . . ? 

C31 C36 W 73.22(17) . . ? 

O C41 C42 119.6(3) . . ? 

O C41 C46 122.2(2) . . ? 

C42 C41 C46 118.1(3) . . ? 

C43 C42 C41 121.5(3) . . ? 

C43 C42 C31 124.5(3) . . ? 

C41 C42 C31 114.0(2) . . ? 

C42 C43 C44 119.9(3) . . ? 

C45 C44 C43 119.6(3) . . ? 

C44 C45 C46 122.4(3) . . ? 

C45 C46 C41 118.6(3) . . ? 

C45 C46 C51 120.2(3) . . ? 

C41 C46 C51 121.3(3) . . ? 

C56 C51 C52 117.6(3) . . ? 

C56 C51 C46 120.7(3) . . ? 

C52 C51 C46 121.6(3) . . ? 

C53 C52 C51 120.7(3) . . ? 

C52 C53 C54 121.0(3) . . ? 

C55 C54 C53 118.9(3) . . ? 

C54 C55 C56 120.5(3) . . ? 

C55 C56 C51 121.3(3) . . ? 



_diffrn_measured_fraction_theta_max    0.930 

_diffrn_reflns_theta_full              28.31 

_diffrn_measured_fraction_theta_full   0.930 

_refine_diff_density_max    0.700 

_refine_diff_density_min   -0.627 

_refine_diff_density_rms    0.081 

#===END 











