Supplementary Material (ESI) for Dalton Transactions
This journal is © The Royal Society of Chemistry 2002

data_global

#------------------ AUDIT DETAILS-------------------------------------------#

_audit_creation_date            2002-03-08
_audit_creation_method          'WinGX routine CIF_UPDATE'
_audit_conform_dict_name        cif_core.dic
_audit_conform_dict_version     2.2
_audit_conform_dict_location    ftp://ftp.iucr.org/pub/cif_core.dic
_audit_update_record            ?

#------------------ SUBMISSION DETAILS --------------------------------------#

# Name and address of author for correspondence

_journal_coden_Cambridge      186

loop_
_publ_author_name
'Spasojevic-de Bire, Anne'
'Cousson, Alain'
'Hopkins, Michael'
'Kiat, Jean-Michel'
'Manna, Joseph D.'
'Menoret, Carole'
'Quy Dao, Nguyen'

_publ_contact_author_name      'Dr Anne Spasojevic-de Bire'
_publ_contact_author_address
;
Laboratoire SPMS
UMR 8580 du CNRS
Ecole Centrale Paris
92295 Chatenay-Malabry
France
;
_publ_contact_author_email       spaso@spms.ecp.fr
_publ_contact_author_fax         '33 1 41 13 14 37'
_publ_contact_author_phone       '33 1 41 13 15 90'

_publ_requested_journal          'Dalton Transactions'
_publ_requested_coeditor_name    ?
_publ_contact_letter             ?

;
_publ_requested_category        ?


_publ_section_title
;
Chemical Bonding in Methylidyne Complexes:
Neutron diffraction study on a single crystal of BrW.triple.CH(dmpe-d12)2
;

_publ_section_title_footnote
;
?
;



#------------------ TEXT ----------------------------------------------------#

_publ_section_synopsis
;
# Insert blank lines between paragraphs
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;
_publ_section_abstract
;
# Insert blank lines between paragraphs
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;

_publ_section_comment
;
# Insert blank lines between paragraphs
?
;

_publ_section_exptl_prep
;
?
;

_publ_section_exptl_refinement
;
?
;

# Insert blank lines between references

_publ_section_references
;
;
_publ_section_figure_captions
;
?
;
_publ_section_acknowledgements
;
?
;
_publ_section_table_legends
;
?
;

#------------------  SECTION 2. COMPOUND(S) DETAILS -------------------------#

data_1

_database_code_CSD	185256


_audit_creation_date            2002-03-08T19:08:19-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_sum                   'C13 H9 Br D24 P4 W'
_chemical_formula_weight                600.86

#------------------ UNIT CELL INFORMATION -----------------------------------#

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                          8.98(3)
_cell_length_b                          18.23(8)
_cell_length_c                          12.57(7)
_cell_angle_alpha                       90.000(7)
_cell_angle_beta                        100.548(6)
_cell_angle_gamma                       90.000(6)
_cell_volume                            2023(16)
_cell_formula_units_Z                   4
_cell_measurement_temperature           100(2)

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_density_diffrn           1.973
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    980
_exptl_absorpt_coefficient_mu           0.094
_exptl_absorpt_correction_type          none

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength            1.51
_diffrn_reflns_number                   1185
_diffrn_reflns_limit_h_min              -9
_diffrn_reflns_limit_h_max              9
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              20
_diffrn_reflns_limit_l_min              0
_diffrn_reflns_limit_l_max              10
_diffrn_reflns_theta_min                4.23
_diffrn_reflns_theta_max                59.65
_diffrn_reflns_theta_full               59.65
_diffrn_measured_fraction_theta_max	0.375
_diffrn_measured_fraction_theta_full	0.375
_reflns_number_total                    1185
_reflns_number_gt                       1053
_reflns_threshold_expression            >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  fullcycle
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1167P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            SHELXL
_refine_ls_extinction_expression
Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_coef              0.00137(16)
_refine_ls_number_reflns                1185
_refine_ls_number_parameters            470
_refine_ls_number_restraints            0
_refine_ls_R_factor_gt                  0.0537
_refine_ls_wR_factor_ref                0.1376
_refine_ls_goodness_of_fit_ref          1.152
_refine_ls_restrained_S_all             1.152
_refine_ls_shift/su_max                 0.021
_refine_diff_density_max                0.589
_refine_diff_density_min                -0.566

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
Br Br 0.0215(4) 0.1461(2) 0.0885(3) 0.0275(11) Uani 1 d . . .
P1 P -0.1997(5) 0.0341(2) 0.2201(4) 0.0195(12) Uani 1 d . . .
P2 P 0.1489(6) -0.0063(2) 0.2675(4) 0.0256(14) Uani 1 d . . .
P3 P -0.1041(5) 0.2222(2) 0.3170(4) 0.0206(14) Uani 1 d . . .
P4 P 0.2421(5) 0.1826(2) 0.3525(4) 0.0242(14) Uani 1 d . . .
C2 C -0.3469(5) 0.0660(2) 0.1117(4) 0.0373(13) Uani 1 d . . .
C3 C -0.3114(4) -0.0040(2) 0.3146(4) 0.0284(12) Uani 1 d . . .
C6 C 0.2764(4) -0.0503(2) 0.3759(3) 0.0227(11) Uani 1 d . . .
C8 C -0.2466(5) 0.2609(2) 0.2103(4) 0.0372(14) Uani 1 d . . .
C9 C -0.1928(6) 0.2340(2) 0.4347(4) 0.0402(14) Uani 1 d . . .
C12 C 0.3907(5) 0.1550(2) 0.4624(4) 0.0326(13) Uani 1 d . . .
C13 C 0.3536(5) 0.2130(3) 0.2531(4) 0.0408(14) Uani 1 d . . .
C10 C 0.0363(5) 0.2971(2) 0.3334(5) 0.0434(15) Uani 1 d . . .
C11 C 0.1821(4) 0.2711(2) 0.4018(4) 0.0312(13) Uani 1 d . . .
C4 C -0.1356(5) -0.0491(2) 0.1584(4) 0.0306(12) Uani 1 d . . .
C5 C 0.0052(4) -0.0795(2) 0.2289(4) 0.0273(11) Uani 1 d . . .
W W 0.0192(5) 0.1060(2) 0.2996(5) 0.0180(14) Uani 1 d . . .
C7 C 0.2512(4) -0.0125(2) 0.1556(4) 0.0266(11) Uani 1 d . . .
C1 C 0.0173(4) 0.0818(2) 0.4341(3) 0.0190(11) Uani 1 d . . .
D21 D -0.4194(5) 0.0226(3) 0.0760(4) 0.0489(15) Uani 1 d . . .
D22 D -0.4114(6) 0.1072(3) 0.1416(4) 0.0512(16) Uani 1 d . . .
D23 D -0.2942(5) 0.0909(3) 0.0521(4) 0.0427(15) Uani 1 d . . .
D31 D -0.3992(5) -0.0410(3) 0.2728(4) 0.0467(15) Uani 1 d . . .
D32 D -0.2384(5) -0.0326(3) 0.3783(4) 0.0504(15) Uani 1 d . . .
D33 D -0.3680(5) 0.0417(3) 0.3448(4) 0.0455(15) Uani 1 d . . .
D61 D 0.3120(6) -0.1040(2) 0.3554(4) 0.0485(15) Uani 1 d . . .
D62 D 0.3772(5) -0.0175(3) 0.3945(4) 0.0440(14) Uani 1 d . . .
D63 D 0.2227(5) -0.0532(3) 0.4469(4) 0.0444(15) Uani 1 d . . .
D71 D 0.3022(6) -0.0661(3) 0.1523(4) 0.0496(15) Uani 1 d . . .
D72 D 0.1764(6) -0.0020(4) 0.0797(5) 0.069(2) Uani 1 d . . .
D73 D 0.3371(6) 0.0268(3) 0.1649(5) 0.0597(17) Uani 1 d . . .
D81 D -0.2686(6) 0.3185(3) 0.2248(5) 0.0517(16) Uani 1 d . . .
D82 D -0.2024(6) 0.2591(3) 0.1372(6) 0.0618(19) Uani 1 d . . .
D83 D -0.3467(6) 0.2295(3) 0.1975(5) 0.0597(18) Uani 1 d . . .
D91 D -0.2410(7) 0.2859(3) 0.4367(5) 0.0586(17) Uani 1 d . . .
D92 D -0.2789(6) 0.1932(3) 0.4306(5) 0.0640(18) Uani 1 d . . .
D93 D -0.1086(7) 0.2218(4) 0.5059(5) 0.0661(19) Uani 1 d . . .
D121 D 0.4623(5) 0.2005(2) 0.4921(5) 0.0471(15) Uani 1 d . . .
D122 D 0.3387(6) 0.1342(3) 0.5260(5) 0.0536(17) Uani 1 d . . .
D123 D 0.4556(6) 0.1120(3) 0.4346(5) 0.0603(18) Uani 1 d . . .
D131 D 0.4442(5) 0.2490(3) 0.2903(5) 0.0572(17) Uani 1 d . . .
D132 D 0.4005(6) 0.1651(3) 0.2205(6) 0.078(2) Uani 1 d . . .
D133 D 0.2797(7) 0.2412(4) 0.1899(5) 0.069(2) Uani 1 d . . .
HY01 H -0.0117(9) 0.3466(4) 0.3692(9) 0.052(3) Uani 1 d . . .
HY11 H 0.1645(10) 0.2611(5) 0.4845(8) 0.047(3) Uani 1 d . . .
HY12 H 0.2719(10) 0.3112(5) 0.4100(9) 0.050(3) Uani 1 d . . .
HY41 H -0.2327(10) -0.0908(4) 0.1440(7) 0.044(3) Uani 1 d . . .
HY42 H -0.1068(11) -0.0315(5) 0.0795(9) 0.051(3) Uani 1 d . . .
HY51 H -0.0234(13) -0.1028(4) 0.3076(9) 0.058(3) Uani 1 d . . .
HY52 H 0.0522(8) -0.1253(5) 0.1896(8) 0.047(3) Uani 1 d . . .
HY1 H 0.0163(12) 0.0637(6) 0.5220(8) 0.060(3) Uani 1 d . . .
HY02 H 0.0549(11) 0.3126(5) 0.2558(8) 0.049(3) Uani 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Br 0.0193(18) 0.033(2) 0.028(3) 0.0037(19) -0.0010(18) -0.0015(17)
P1 0.016(2) 0.020(2) 0.023(3) 0.000(2) 0.008(2) 0.000(2)
P2 0.027(2) 0.016(2) 0.032(3) 0.000(2) 0.002(2) -0.002(2)
P3 0.008(2) 0.013(2) 0.038(4) -0.002(2) -0.001(2) 0.0044(18)
P4 0.017(2) 0.018(2) 0.035(4) -0.012(2) -0.001(2) 0.001(2)
C2 0.039(2) 0.033(2) 0.035(3) 0.001(2) -0.008(2) -0.003(2)
C3 0.0103(18) 0.027(2) 0.047(3) -0.012(2) 0.0010(19) -0.0090(16)
C6 0.0036(15) 0.027(2) 0.035(3) 0.0048(19) -0.0025(17) 0.0048(16)
C8 0.030(2) 0.028(2) 0.053(3) 0.005(2) 0.004(2) 0.0043(19)
C9 0.063(3) 0.0187(19) 0.039(3) 0.014(2) 0.008(3) 0.009(2)
C12 0.0197(19) 0.030(2) 0.046(3) -0.008(2) -0.001(2) 0.0022(19)
C13 0.030(2) 0.051(3) 0.044(3) 0.005(2) 0.015(2) -0.014(2)
C10 0.027(2) 0.020(2) 0.084(4) -0.027(2) 0.010(2) -0.0055(18)
C11 0.0178(19) 0.0153(18) 0.054(3) -0.005(2) -0.010(2) -0.0025(17)
C4 0.029(2) 0.033(2) 0.026(3) -0.001(2) -0.003(2) -0.0034(19)
C5 0.0252(19) 0.0228(19) 0.033(3) 0.001(2) 0.004(2) -0.0059(18)
W 0.010(2) 0.016(2) 0.026(4) 0.007(2) -0.001(2) 0.000(2)
C7 0.030(2) 0.021(2) 0.033(3) -0.0071(19) 0.016(2) -0.0049(18)
C1 0.0173(17) 0.035(2) 0.003(2) 0.0011(19) -0.0034(17) 0.0011(17)
D21 0.042(3) 0.043(3) 0.055(3) -0.011(3) -0.009(2) -0.004(2)
D22 0.051(3) 0.049(3) 0.049(4) -0.002(3) -0.003(3) 0.013(2)
D23 0.035(2) 0.052(3) 0.034(3) 0.006(3) -0.014(2) 0.012(2)
D31 0.046(3) 0.052(3) 0.044(3) -0.008(2) 0.014(3) -0.016(2)
D32 0.037(2) 0.062(3) 0.047(4) 0.025(3) -0.006(3) 0.005(3)
D33 0.042(3) 0.051(3) 0.044(3) 0.007(2) 0.010(2) 0.004(2)
D61 0.052(3) 0.034(2) 0.059(4) 0.012(2) 0.008(3) 0.029(2)
D62 0.033(2) 0.044(3) 0.051(3) 0.002(2) -0.002(2) -0.002(2)
D63 0.034(2) 0.060(3) 0.036(3) -0.007(3) -0.003(3) 0.001(2)
D71 0.055(3) 0.036(3) 0.061(4) 0.002(2) 0.017(3) 0.016(2)
D72 0.055(3) 0.115(5) 0.029(3) 0.005(4) -0.011(3) 0.021(3)
D73 0.056(3) 0.039(3) 0.091(4) -0.006(3) 0.034(3) 0.003(3)
D81 0.050(3) 0.045(3) 0.055(4) 0.015(3) -0.003(3) 0.015(2)
D82 0.051(3) 0.053(3) 0.081(5) 0.024(3) 0.012(3) 0.014(3)
D83 0.044(3) 0.043(3) 0.083(4) 0.003(3) -0.011(3) 0.005(3)
D91 0.072(3) 0.051(3) 0.057(4) 0.026(3) 0.024(3) 0.023(3)
D92 0.078(3) 0.036(3) 0.091(5) 0.000(3) 0.050(3) 0.004(3)
D93 0.083(4) 0.080(4) 0.035(4) 0.015(3) 0.009(3) 0.011(3)
D121 0.030(2) 0.032(2) 0.069(4) -0.004(2) -0.019(2) -0.009(2)
D122 0.038(3) 0.067(3) 0.051(4) 0.003(3) -0.005(3) -0.011(3)
D123 0.047(3) 0.056(3) 0.072(4) -0.012(3) -0.006(3) 0.000(3)
D131 0.025(2) 0.066(3) 0.081(4) -0.004(3) 0.010(3) -0.019(2)
D132 0.076(3) 0.066(4) 0.111(5) -0.043(3) 0.065(3) -0.032(3)
D133 0.055(3) 0.092(4) 0.055(4) -0.002(4) -0.001(3) -0.017(3)
HY01 0.043(5) 0.021(4) 0.091(8) -0.018(4) 0.009(5) 0.010(4)
HY11 0.050(5) 0.055(5) 0.034(6) -0.027(5) 0.001(5) 0.007(4)
HY12 0.036(4) 0.038(5) 0.075(7) -0.005(5) 0.008(5) -0.009(4)
HY41 0.047(5) 0.023(4) 0.052(6) 0.001(4) -0.020(4) 0.003(4)
HY42 0.053(5) 0.037(5) 0.052(7) 0.001(5) -0.014(5) 0.009(4)
HY51 0.088(7) 0.031(5) 0.050(7) 0.026(5) 0.004(6) -0.018(5)
HY52 0.017(4) 0.066(6) 0.050(6) -0.001(5) -0.012(4) 0.008(4)
HY1 0.072(6) 0.085(7) 0.029(6) 0.014(5) 0.025(5) -0.004(6)
HY02 0.070(6) 0.040(5) 0.030(6) 0.030(5) -0.010(5) -0.006(5)


#------------------ MOLECULAR GEOMETRY --------------------------------------#

_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
Br W 2.755(16) . ?
P1 C2 1.811(8) . ?
P1 C3 1.827(9) . ?
P1 C4 1.842(9) . ?
P1 W 2.422(9) . ?
P2 C6 1.800(8) . ?
P2 C7 1.818(10) . ?
P2 C5 1.858(8) . ?
P2 W 2.425(10) . ?
P3 C9 1.816(11) . ?
P3 C8 1.817(8) . ?
P3 C10 1.844(8) . ?
P3 W 2.419(10) . ?
P4 C12 1.808(8) . ?
P4 C13 1.825(10) . ?
P4 C11 1.845(9) . ?
P4 W 2.432(9) . ?
C2 D22 1.059(7) . ?
C2 D23 1.059(7) . ?
C2 D21 1.069(7) . ?
C3 D32 1.073(7) . ?
C3 D33 1.078(7) . ?
C3 D31 1.097(6) . ?
C6 D62 1.074(6) . ?
C6 D61 1.077(7) . ?
C6 D63 1.090(8) . ?
C8 D83 1.053(7) . ?
C8 D82 1.066(9) . ?
C8 D81 1.090(8) . ?
C9 D91 1.042(8) . ?
C9 D92 1.068(7) . ?
C9 D93 1.084(8) . ?
C12 D122 1.067(8) . ?
C12 D121 1.073(6) . ?
C12 D123 1.073(7) . ?
C13 D133 1.069(8) . ?
C13 D132 1.082(8) . ?
C13 D131 1.083(7) . ?
C10 C11 1.506(7) . ?
C4 C5 1.510(7) . ?
W C1 1.750(11) . ?
C7 D73 1.043(7) . ?
C7 D72 1.079(7) . ?
C7 D71 1.083(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
C2 P1 C3 101.4(4) . . ?
C2 P1 C4 100.9(4) . . ?
C3 P1 C4 102.3(4) . . ?
C2 P1 W 124.2(4) . . ?
C3 P1 W 116.0(4) . . ?
C4 P1 W 109.1(4) . . ?
C6 P2 C7 102.4(5) . . ?
C6 P2 C5 101.2(4) . . ?
C7 P2 C5 100.3(4) . . ?
C6 P2 W 120.6(4) . . ?
C7 P2 W 120.5(3) . . ?
C5 P2 W 108.5(4) . . ?
C9 P3 C8 101.5(5) . . ?
C9 P3 C10 102.4(4) . . ?
C8 P3 C10 99.8(4) . . ?
C9 P3 W 117.0(3) . . ?
C8 P3 W 123.0(4) . . ?
C10 P3 W 110.1(4) . . ?
C12 P4 C13 100.8(5) . . ?
C12 P4 C11 101.9(4) . . ?
C13 P4 C11 101.2(4) . . ?
C12 P4 W 120.4(4) . . ?
C13 P4 W 121.0(4) . . ?
C11 P4 W 108.5(4) . . ?
D22 C2 D23 106.9(6) . . ?
D22 C2 D21 110.0(6) . . ?
D23 C2 D21 109.7(6) . . ?
D22 C2 P1 109.5(5) . . ?
D23 C2 P1 108.1(5) . . ?
D21 C2 P1 112.5(5) . . ?
D32 C3 D33 112.1(6) . . ?
D32 C3 D31 110.3(6) . . ?
D33 C3 D31 107.4(5) . . ?
D32 C3 P1 109.6(5) . . ?
D33 C3 P1 106.6(5) . . ?
D31 C3 P1 110.7(5) . . ?
D62 C6 D61 106.4(5) . . ?
D62 C6 D63 109.3(6) . . ?
D61 C6 D63 110.2(5) . . ?
D62 C6 P2 108.2(5) . . ?
D61 C6 P2 113.6(5) . . ?
D63 C6 P2 109.0(5) . . ?
D83 C8 D82 107.1(7) . . ?
D83 C8 D81 111.8(6) . . ?
D82 C8 D81 106.3(6) . . ?
D83 C8 P3 111.7(5) . . ?
D82 C8 P3 107.5(6) . . ?
D81 C8 P3 112.0(5) . . ?
D91 C9 D92 109.5(7) . . ?
D91 C9 D93 113.4(7) . . ?
D92 C9 D93 106.6(6) . . ?
D91 C9 P3 111.9(5) . . ?
D92 C9 P3 107.5(5) . . ?
D93 C9 P3 107.7(6) . . ?
D122 C12 D121 109.3(7) . . ?
D122 C12 D123 108.9(6) . . ?
D121 C12 D123 110.6(6) . . ?
D122 C12 P4 107.9(5) . . ?
D121 C12 P4 111.2(5) . . ?
D123 C12 P4 108.8(5) . . ?
D133 C13 D132 109.8(8) . . ?
D133 C13 D131 110.2(7) . . ?
D132 C13 D131 109.8(6) . . ?
D133 C13 P4 108.1(6) . . ?
D132 C13 P4 108.3(6) . . ?
D131 C13 P4 110.6(6) . . ?
C11 C10 P3 109.7(4) . . ?
C10 C11 P4 111.1(4) . . ?
C5 C4 P1 110.3(4) . . ?
C4 C5 P2 110.9(4) . . ?
C1 W P3 92.7(3) . . ?
C1 W P1 96.4(3) . . ?
P3 W P1 99.3(3) . . ?
C1 W P2 92.2(3) . . ?
P3 W P2 174.9(3) . . ?
P1 W P2 81.5(3) . . ?
C1 W P4 91.9(3) . . ?
P3 W P4 80.8(3) . . ?
P1 W P4 171.7(3) . . ?
P2 W P4 97.7(4) . . ?
C1 W Br 179.2(3) . . ?
P3 W Br 86.5(3) . . ?
P1 W Br 84.0(3) . . ?
P2 W Br 88.6(3) . . ?
P4 W Br 87.7(3) . . ?
D73 C7 D72 107.8(6) . . ?
D73 C7 D71 108.3(6) . . ?
D72 C7 D71 109.0(6) . . ?
D73 C7 P2 109.8(5) . . ?
D72 C7 P2 110.5(6) . . ?
D71 C7 P2 111.3(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 P1 C2 D22 62.3(6) . . . . ?
C4 P1 C2 D22 167.4(5) . . . . ?
W P1 C2 D22 -70.4(6) . . . . ?
C3 P1 C2 D23 178.4(4) . . . . ?
C4 P1 C2 D23 -76.5(6) . . . . ?
W P1 C2 D23 45.7(6) . . . . ?
C3 P1 C2 D21 -60.3(6) . . . . ?
C4 P1 C2 D21 44.8(6) . . . . ?
W P1 C2 D21 167.0(5) . . . . ?
C2 P1 C3 D32 171.4(4) . . . . ?
C4 P1 C3 D32 67.4(5) . . . . ?
W P1 C3 D32 -51.2(5) . . . . ?
C2 P1 C3 D33 -67.0(5) . . . . ?
C4 P1 C3 D33 -171.0(4) . . . . ?
W P1 C3 D33 70.4(5) . . . . ?
C2 P1 C3 D31 49.5(5) . . . . ?
C4 P1 C3 D31 -54.5(5) . . . . ?
W P1 C3 D31 -173.0(4) . . . . ?
C7 P2 C6 D62 65.2(5) . . . . ?
C5 P2 C6 D62 168.5(4) . . . . ?
W P2 C6 D62 -72.0(6) . . . . ?
C7 P2 C6 D61 -52.7(5) . . . . ?
C5 P2 C6 D61 50.6(6) . . . . ?
W P2 C6 D61 170.1(4) . . . . ?
C7 P2 C6 D63 -176.1(4) . . . . ?
C5 P2 C6 D63 -72.7(5) . . . . ?
W P2 C6 D63 46.7(5) . . . . ?
C9 P3 C8 D83 -65.7(6) . . . . ?
C10 P3 C8 D83 -170.6(5) . . . . ?
W P3 C8 D83 67.6(7) . . . . ?
C9 P3 C8 D82 177.1(5) . . . . ?
C10 P3 C8 D82 72.2(5) . . . . ?
W P3 C8 D82 -49.7(6) . . . . ?
C9 P3 C8 D81 60.7(6) . . . . ?
C10 P3 C8 D81 -44.2(6) . . . . ?
W P3 C8 D81 -166.1(5) . . . . ?
C8 P3 C9 D91 -44.6(6) . . . . ?
C10 P3 C9 D91 58.3(6) . . . . ?
W P3 C9 D91 178.7(5) . . . . ?
C8 P3 C9 D92 75.7(6) . . . . ?
C10 P3 C9 D92 178.6(5) . . . . ?
W P3 C9 D92 -61.0(6) . . . . ?
C8 P3 C9 D93 -169.8(5) . . . . ?
C10 P3 C9 D93 -66.9(6) . . . . ?
W P3 C9 D93 53.5(6) . . . . ?
C13 P4 C12 D122 -178.3(5) . . . . ?
C11 P4 C12 D122 77.6(6) . . . . ?
W P4 C12 D122 -42.3(6) . . . . ?
C13 P4 C12 D121 61.8(6) . . . . ?
C11 P4 C12 D121 -42.3(6) . . . . ?
W P4 C12 D121 -162.3(5) . . . . ?
C13 P4 C12 D123 -60.3(6) . . . . ?
C11 P4 C12 D123 -164.4(5) . . . . ?
W P4 C12 D123 75.7(6) . . . . ?
C12 P4 C13 D133 -168.4(5) . . . . ?
C11 P4 C13 D133 -63.8(6) . . . . ?
W P4 C13 D133 56.0(6) . . . . ?
C12 P4 C13 D132 72.7(5) . . . . ?
C11 P4 C13 D132 177.3(5) . . . . ?
W P4 C13 D132 -62.9(6) . . . . ?
C12 P4 C13 D131 -47.7(5) . . . . ?
C11 P4 C13 D131 56.9(5) . . . . ?
W P4 C13 D131 176.7(4) . . . . ?
C9 P3 C10 C11 87.9(5) . . . . ?
C8 P3 C10 C11 -167.9(4) . . . . ?
W P3 C10 C11 -37.2(5) . . . . ?
P3 C10 C11 P4 49.4(6) . . . . ?
C12 P4 C11 C10 -168.0(4) . . . . ?
C13 P4 C11 C10 88.3(5) . . . . ?
W P4 C11 C10 -40.1(5) . . . . ?
C2 P1 C4 C5 171.5(3) . . . . ?
C3 P1 C4 C5 -84.1(5) . . . . ?
W P1 C4 C5 39.3(4) . . . . ?
P1 C4 C5 P2 -49.5(5) . . . . ?
C6 P2 C5 C4 165.4(4) . . . . ?
C7 P2 C5 C4 -89.6(5) . . . . ?
W P2 C5 C4 37.7(5) . . . . ?
C9 P3 W C1 -14.6(4) . . . . ?
C8 P3 W C1 -141.3(4) . . . . ?
C10 P3 W C1 101.6(4) . . . . ?
C9 P3 W P1 82.3(4) . . . . ?
C8 P3 W P1 -44.4(4) . . . . ?
C10 P3 W P1 -161.4(4) . . . . ?
C9 P3 W P2 -179(3) . . . . ?
C8 P3 W P2 54(3) . . . . ?
C10 P3 W P2 -63(3) . . . . ?
C9 P3 W P4 -106.1(4) . . . . ?
C8 P3 W P4 127.1(4) . . . . ?
C10 P3 W P4 10.1(4) . . . . ?
C9 P3 W Br 165.7(3) . . . . ?
C8 P3 W Br 38.9(4) . . . . ?
C10 P3 W Br -78.1(3) . . . . ?
C2 P1 W C1 137.9(4) . . . . ?
C3 P1 W C1 11.1(4) . . . . ?
C4 P1 W C1 -103.7(4) . . . . ?
C2 P1 W P3 44.0(5) . . . . ?
C3 P1 W P3 -82.7(3) . . . . ?
C4 P1 W P3 162.5(3) . . . . ?
C2 P1 W P2 -130.9(4) . . . . ?
C3 P1 W P2 102.4(3) . . . . ?
C4 P1 W P2 -12.4(3) . . . . ?
C2 P1 W P4 -45.9(19) . . . . ?
C3 P1 W P4 -172.6(17) . . . . ?
C4 P1 W P4 72.6(18) . . . . ?
C2 P1 W Br -41.4(4) . . . . ?
C3 P1 W Br -168.1(3) . . . . ?
C4 P1 W Br 77.1(3) . . . . ?
C6 P2 W C1 -30.0(4) . . . . ?
C7 P2 W C1 -159.6(3) . . . . ?
C5 P2 W C1 85.7(4) . . . . ?
C6 P2 W P3 134(3) . . . . ?
C7 P2 W P3 5(3) . . . . ?
C5 P2 W P3 -110(3) . . . . ?
C6 P2 W P1 -126.1(3) . . . . ?
C7 P2 W P1 104.2(4) . . . . ?
C5 P2 W P1 -10.4(3) . . . . ?
C6 P2 W P4 62.3(4) . . . . ?
C7 P2 W P4 -67.4(4) . . . . ?
C5 P2 W P4 178.0(3) . . . . ?
C6 P2 W Br 149.8(4) . . . . ?
C7 P2 W Br 20.1(3) . . . . ?
C5 P2 W Br -94.5(3) . . . . ?
C12 P4 W C1 37.0(4) . . . . ?
C13 P4 W C1 164.2(3) . . . . ?
C11 P4 W C1 -79.7(4) . . . . ?
C12 P4 W P3 129.4(4) . . . . ?
C13 P4 W P3 -103.4(3) . . . . ?
C11 P4 W P3 12.8(3) . . . . ?
C12 P4 W P1 -139.3(17) . . . . ?
C13 P4 W P1 -12(2) . . . . ?
C11 P4 W P1 104.1(18) . . . . ?
C12 P4 W P2 -55.5(5) . . . . ?
C13 P4 W P2 71.7(4) . . . . ?
C11 P4 W P2 -172.1(3) . . . . ?
C12 P4 W Br -143.7(4) . . . . ?
C13 P4 W Br -16.5(3) . . . . ?
C11 P4 W Br 99.6(4) . . . . ?
C6 P2 C7 D73 -77.0(6) . . . . ?
C5 P2 C7 D73 179.1(4) . . . . ?
W P2 C7 D73 60.3(6) . . . . ?
C6 P2 C7 D72 164.3(5) . . . . ?
C5 P2 C7 D72 60.3(6) . . . . ?
W P2 C7 D72 -58.5(6) . . . . ?
C6 P2 C7 D71 43.0(5) . . . . ?
C5 P2 C7 D71 -61.0(5) . . . . ?
W P2 C7 D71 -179.8(4) . . . . ?

data_2

_database_code_CSD	185257


_audit_creation_date            2002-03-08T16:47:09-00:00
_audit_creation_method         'WinGX routine CIF_UPDATE'

#------------------ CHEMICAL INFORMATION ------------------------------------#

_chemical_formula_sum                   'C13 H9 Br D24 P4 W'
_chemical_formula_weight                600.86

#------------------ UNIT CELL INFORMATION -----------------------------------#

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                          9.12(3)
_cell_length_b                          18.42(6)
_cell_length_c                          12.77(4)
_cell_angle_alpha                       90
_cell_angle_beta                        101.228(4)
_cell_angle_gamma                       90
_cell_volume                            2104(12)
_cell_formula_units_Z                   4
_cell_measurement_temperature           293(2)

#------------------ CRYSTAL INFORMATION -------------------------------------#

_exptl_crystal_density_diffrn           1.897
_exptl_crystal_density_method           'not measured'
_exptl_crystal_F_000                    980
_exptl_absorpt_coefficient_mu           0.09
_exptl_absorpt_correction_type          none

#------------------ DATA COLLECTION INFORMATION -----------------------------#

_diffrn_radiation_wavelength            1.54
_diffrn_reflns_number                   987
_diffrn_reflns_limit_h_min              -10
_diffrn_reflns_limit_h_max              8
_diffrn_reflns_limit_k_min              0
_diffrn_reflns_limit_k_max              18
_diffrn_reflns_limit_l_min              0
_diffrn_reflns_limit_l_max              12
_diffrn_reflns_theta_min                4.26
_diffrn_reflns_theta_max                51.16
_diffrn_reflns_theta_full               51.16
_diffrn_measured_fraction_theta_max
0.431
_diffrn_measured_fraction_theta_full
0.431
_reflns_number_total                    987
_reflns_number_gt                       868
_reflns_threshold_expression            >2sigma(I)

#------------------ COMPUTER PROGRAMS USED ----------------------------------#

_computing_structure_refinement         'SHELXL-97 (Sheldrick, 1997)'

#------------------ REFINEMENT INFORMATION ----------------------------------#

_refine_ls_structure_factor_coef        Fsqd
_refine_ls_matrix_type                  full
_refine_ls_weighting_scheme             calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1607P)^2^+312.4249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment           mixed
_refine_ls_extinction_method            none
_refine_ls_number_reflns                987
_refine_ls_number_parameters            209
_refine_ls_number_restraints            0
_refine_ls_R_factor_gt                  0.1701
_refine_ls_wR_factor_ref                0.3951
_refine_ls_goodness_of_fit_ref          1.114
_refine_ls_restrained_S_all             1.114
_refine_ls_shift/su_max                 0.078
_refine_diff_density_max                1.252
_refine_diff_density_min                -1

#------------------ ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS --------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
D D 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_refinement_flags
_atom_site_disorder_group
_atom_site_disorder_assembly
W W 0.017(3) 0.1042(11) 0.2960(16) 0.019(5) Uiso 1 d . . .
Br Br 0.014(2) 0.1455(10) 0.0903(15) 0.042(5) Uiso 1 d . . .
P1 P -0.205(3) 0.0334(14) 0.2225(19) 0.042(7) Uiso 1 d . . .
P2 P 0.137(3) -0.0071(15) 0.259(2) 0.048(7) Uiso 1 d . . .
P3 P -0.103(3) 0.2202(15) 0.3149(19) 0.044(7) Uiso 1 d . . .
P4 P 0.239(3) 0.1816(14) 0.346(2) 0.043(7) Uiso 1 d . . .
C1 C 0.022(2) 0.0820(11) 0.4326(17) 0.043(5) Uiso 1 d . . .
C2 C -0.354(3) 0.0681(16) 0.113(2) 0.063(7) Uiso 1 d . . .
C3 C -0.311(4) 0.000(2) 0.314(3) 0.089(9) Uiso 1 d . . .
C4 C -0.144(3) -0.0465(14) 0.1626(19) 0.061(7) Uiso 1 d . . .
C5 C -0.002(3) -0.0789(16) 0.228(2) 0.072(7) Uiso 1 d . . .
C6 C 0.262(4) -0.0528(18) 0.372(3) 0.079(8) Uiso 1 d . . .
C7 C 0.239(4) -0.0122(19) 0.152(2) 0.076(8) Uiso 1 d . . .
C8 C -0.227(5) 0.265(2) 0.211(3) 0.106(11) Uiso 1 d . . .
C10 C 0.035(4) 0.2970(19) 0.335(3) 0.086(9) Uiso 1 d . . .
C9 C -0.192(5) 0.231(3) 0.430(3) 0.108(11) Uiso 1 d . . .
C11 C 0.178(4) 0.2692(18) 0.393(3) 0.091(9) Uiso 1 d . . .
C12 C 0.382(4) 0.156(2) 0.460(3) 0.095(9) Uiso 1 d . . .
C13 C 0.354(6) 0.202(3) 0.237(4) 0.123(14) Uiso 1 d . . .
D21 D -0.419(5) 0.024(2) 0.083(3) 0.127(12) Uiso 1 d . . .
D22 D -0.415(4) 0.109(2) 0.143(3) 0.121(12) Uiso 1 d . . .
D23 D -0.294(4) 0.0924(19) 0.053(3) 0.104(10) Uiso 1 d . . .
D31 D -0.395(4) -0.035(2) 0.277(3) 0.108(10) Uiso 1 d . . .
D33 D -0.361(4) 0.041(2) 0.344(3) 0.098(10) Uiso 1 d . . .
D61 D 0.305(4) -0.100(2) 0.346(3) 0.126(13) Uiso 1 d . . .
D62 D 0.367(4) -0.0197(18) 0.385(3) 0.096(9) Uiso 1 d . . .
D63 D 0.227(4) -0.050(2) 0.438(3) 0.117(12) Uiso 1 d . . .
D71 D 0.278(4) -0.066(2) 0.150(3) 0.115(11) Uiso 1 d . . .
D73 D 0.319(5) 0.021(2) 0.163(3) 0.124(13) Uiso 1 d . . .
D81 D -0.267(6) 0.316(3) 0.229(4) 0.163(17) Uiso 1 d . . .
D32 D -0.243(4) -0.029(2) 0.375(3) 0.109(10) Uiso 1 d . . .
D72 D 0.163(4) -0.0058(19) 0.082(3) 0.106(10) Uiso 1 d . . .
D82 D -0.209(5) 0.255(2) 0.132(4) 0.129(13) Uiso 1 d . . .
D92 D -0.272(6) 0.197(3) 0.422(4) 0.155(17) Uiso 1 d . . .
D83 D -0.329(5) 0.234(2) 0.198(3) 0.120(12) Uiso 1 d . . .
D91 D -0.232(6) 0.286(3) 0.435(4) 0.161(17) Uiso 1 d . . .
D93 D -0.116(6) 0.215(3) 0.498(4) 0.149(15) Uiso 1 d . . .
D121 D 0.453(4) 0.202(2) 0.486(3) 0.111(11) Uiso 1 d . . .
D122 D 0.334(4) 0.132(2) 0.519(3) 0.117(11) Uiso 1 d . . .
D123 D 0.443(4) 0.111(2) 0.436(3) 0.121(12) Uiso 1 d . . .
D131 D 0.432(6) 0.245(3) 0.281(4) 0.153(16) Uiso 1 d . . .
D132 D 0.390(7) 0.161(4) 0.226(5) 0.19(3) Uiso 1 d . . .
D133 D 0.283(6) 0.230(3) 0.182(5) 0.163(18) Uiso 1 d . . .
H1 H 0.016(6) 0.068(3) 0.512(5) 0.098(17) Uiso 1 d . . .
H11 H 0.173(7) 0.263(3) 0.476(5) 0.106(18) Uiso 1 d . . .
H01 H 0.002(7) 0.338(4) 0.360(5) 0.101(18) Uiso 1 d . . .
H12 H 0.275(9) 0.306(4) 0.404(5) 0.13(2) Uiso 1 d . . .
H41 H -0.234(6) -0.085(3) 0.146(4) 0.084(14) Uiso 1 d . . .
H42 H -0.124(5) -0.037(3) 0.082(4) 0.081(14) Uiso 1 d . . .
H51 H -0.025(6) -0.105(3) 0.298(4) 0.085(15) Uiso 1 d . . .
H52 H 0.044(6) -0.124(3) 0.189(4) 0.081(14) Uiso 1 d . . .
H02 H 0.054(13) 0.311(7) 0.265(10) 0.21(4) Uiso 1 d . . .


#------------------ MOLECULAR GEOMETRY --------------------------------------#

_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 C1 1.78(3) . ?
W P2 2.41(3) . ?
W P3 2.43(4) . ?
W P1 2.44(3) . ?
W P4 2.46(3) . ?
W Br 2.73(3) . ?
P1 C3 1.76(4) . ?
P1 C4 1.80(4) . ?
P1 C2 1.86(4) . ?
P2 C7 1.80(4) . ?
P2 C5 1.82(4) . ?
P2 C6 1.86(4) . ?
P3 C8 1.77(5) . ?
P3 C9 1.82(5) . ?
P3 C10 1.88(4) . ?
P4 C12 1.82(4) . ?
P4 C11 1.84(4) . ?
P4 C13 1.94(5) . ?
C2 D21 1.03(4) . ?
C2 D22 1.05(4) . ?
C2 D23 1.12(4) . ?
C3 D33 1.01(4) . ?
C3 D31 1.04(4) . ?
C3 D32 1.04(4) . ?
C4 C5 1.52(4) . ?
C6 D63 0.97(4) . ?
C6 D61 1.03(4) . ?
C6 D62 1.12(4) . ?
C7 D73 0.95(4) . ?
C7 D72 1.02(3) . ?
C7 D71 1.06(4) . ?
C8 D82 1.06(4) . ?
C8 D81 1.06(5) . ?
C8 D83 1.07(4) . ?
C10 C11 1.46(4) . ?
C9 D92 0.95(5) . ?
C9 D93 1.04(5) . ?
C9 D91 1.08(5) . ?
C12 D122 1.03(4) . ?
C12 D121 1.08(4) . ?
C12 D123 1.08(4) . ?
C13 D132 0.84(7) . ?
C13 D133 1.00(6) . ?
C13 D131 1.14(5) . ?

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 W P2 94.0(12) . . ?
C1 W P3 91.8(12) . . ?
P2 W P3 174.2(13) . . ?
C1 W P1 96.7(13) . . ?
P2 W P1 81.1(11) . . ?
P3 W P1 98.7(12) . . ?
C1 W P4 90.7(12) . . ?
P2 W P4 99.3(12) . . ?
P3 W P4 80.1(11) . . ?
P1 W P4 172.5(13) . . ?
C1 W Br 176.9(14) . . ?
P2 W Br 88.2(10) . . ?
P3 W Br 86.1(9) . . ?
P1 W Br 85.8(9) . . ?
P4 W Br 86.7(10) . . ?
C3 P1 C4 104.3(19) . . ?
C3 P1 C2 102(2) . . ?
C4 P1 C2 101.8(17) . . ?
C3 P1 W 116.9(18) . . ?
C4 P1 W 107.3(15) . . ?
C2 P1 W 122.3(16) . . ?
C7 P2 C5 104(2) . . ?
C7 P2 C6 104(2) . . ?
C5 P2 C6 97.8(18) . . ?
C7 P2 W 120.9(18) . . ?
C5 P2 W 109.5(16) . . ?
C6 P2 W 117.9(17) . . ?
C8 P3 C9 104(2) . . ?
C8 P3 C10 94(2) . . ?
C9 P3 C10 102(2) . . ?
C8 P3 W 124(2) . . ?
C9 P3 W 117(2) . . ?
C10 P3 W 111.8(17) . . ?
C12 P4 C11 101(2) . . ?
C12 P4 C13 103(2) . . ?
C11 P4 C13 108(2) . . ?
C12 P4 W 118.9(18) . . ?
C11 P4 W 107.9(17) . . ?
C13 P4 W 117(2) . . ?
D21 C2 D22 113(4) . . ?
D21 C2 D23 112(4) . . ?
D22 C2 D23 109(4) . . ?
D21 C2 P1 108(3) . . ?
D22 C2 P1 110(3) . . ?
D23 C2 P1 106(3) . . ?
D33 C3 D31 107(5) . . ?
D33 C3 D32 111(4) . . ?
D31 C3 D32 108(4) . . ?
D33 C3 P1 109(3) . . ?
D31 C3 P1 111(3) . . ?
D32 C3 P1 111(4) . . ?
C5 C4 P1 113(2) . . ?
C4 C5 P2 108(2) . . ?
D63 C6 D61 123(5) . . ?
D63 C6 D62 104(4) . . ?
D61 C6 D62 98(4) . . ?
D63 C6 P2 113(4) . . ?
D61 C6 P2 110(4) . . ?
D62 C6 P2 105(3) . . ?
D73 C7 D72 115(5) . . ?
D73 C7 D71 111(5) . . ?
D72 C7 D71 105(4) . . ?
D73 C7 P2 111(4) . . ?
D72 C7 P2 108(3) . . ?
D71 C7 P2 107(3) . . ?
D82 C8 D81 119(6) . . ?
D82 C8 D83 93(5) . . ?
D81 C8 D83 101(5) . . ?
D82 C8 P3 116(4) . . ?
D81 C8 P3 116(5) . . ?
D83 C8 P3 107(4) . . ?
C11 C10 P3 108(3) . . ?
D92 C9 D93 107(7) . . ?
D92 C9 D91 110(6) . . ?
D93 C9 D91 112(6) . . ?
D92 C9 P3 107(5) . . ?
D93 C9 P3 108(4) . . ?
D91 C9 P3 111(4) . . ?
C10 C11 P4 116(3) . . ?
D122 C12 D121 115(5) . . ?
D122 C12 D123 102(5) . . ?
D121 C12 D123 112(5) . . ?
D122 C12 P4 110(4) . . ?
D121 C12 P4 109(3) . . ?
D123 C12 P4 108(3) . . ?
D132 C13 D133 125(9) . . ?
D132 C13 D131 118(9) . . ?
D133 C13 D131 104(7) . . ?
D132 C13 P4 103(7) . . ?
D133 C13 P4 104(5) . . ?
D131 C13 P4 99(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 W P1 C3 12(2) . . . . ?
P2 W P1 C3 105(2) . . . . ?
P3 W P1 C3 -81(2) . . . . ?
P4 W P1 C3 -162(10) . . . . ?
Br W P1 C3 -166.4(19) . . . . ?
C1 W P1 C4 -104.8(16) . . . . ?
P2 W P1 C4 -11.8(15) . . . . ?
P3 W P1 C4 162.4(14) . . . . ?
P4 W P1 C4 82(10) . . . . ?
Br W P1 C4 77.0(15) . . . . ?
C1 W P1 C2 138.4(18) . . . . ?
P2 W P1 C2 -128.6(18) . . . . ?
P3 W P1 C2 45.6(19) . . . . ?
P4 W P1 C2 -35(11) . . . . ?
Br W P1 C2 -39.8(18) . . . . ?
C1 W P2 C7 -155(2) . . . . ?
P3 W P2 C7 20(14) . . . . ?
P1 W P2 C7 109(2) . . . . ?
P4 W P2 C7 -64(2) . . . . ?
Br W P2 C7 23(2) . . . . ?
C1 W P2 C5 84.3(17) . . . . ?
P3 W P2 C5 -100(14) . . . . ?
P1 W P2 C5 -11.9(16) . . . . ?
P4 W P2 C5 175.7(16) . . . . ?
Br W P2 C5 -98.0(16) . . . . ?
C1 W P2 C6 -26(2) . . . . ?
P3 W P2 C6 149(13) . . . . ?
P1 W P2 C6 -122.4(19) . . . . ?
P4 W P2 C6 65(2) . . . . ?
Br W P2 C6 151.5(18) . . . . ?
C1 W P3 C8 -150(2) . . . . ?
P2 W P3 C8 34(14) . . . . ?
P1 W P3 C8 -53(2) . . . . ?
P4 W P3 C8 119(2) . . . . ?
Br W P3 C8 32(2) . . . . ?
C1 W P3 C9 -18(2) . . . . ?
P2 W P3 C9 167(13) . . . . ?
P1 W P3 C9 79(2) . . . . ?
P4 W P3 C9 -108(2) . . . . ?
Br W P3 C9 164(2) . . . . ?
C1 W P3 C10 98.7(18) . . . . ?
P2 W P3 C10 -77(14) . . . . ?
P1 W P3 C10 -164.3(16) . . . . ?
P4 W P3 C10 8.2(17) . . . . ?
Br W P3 C10 -79.1(17) . . . . ?
C1 W P4 C12 34(2) . . . . ?
P2 W P4 C12 -60(2) . . . . ?
P3 W P4 C12 126(2) . . . . ?
P1 W P4 C12 -153(10) . . . . ?
Br W P4 C12 -147.9(19) . . . . ?
C1 W P4 C11 -80.0(18) . . . . ?
P2 W P4 C11 -174.1(16) . . . . ?
P3 W P4 C11 11.7(16) . . . . ?
P1 W P4 C11 94(10) . . . . ?
Br W P4 C11 98.3(16) . . . . ?
C1 W P4 C13 159(2) . . . . ?
P2 W P4 C13 64(2) . . . . ?
P3 W P4 C13 -110(2) . . . . ?
P1 W P4 C13 -28(11) . . . . ?
Br W P4 C13 -23(2) . . . . ?
C3 P1 C2 D21 -62(4) . . . . ?
C4 P1 C2 D21 45(4) . . . . ?
W P1 C2 D21 165(3) . . . . ?
C3 P1 C2 D22 61(4) . . . . ?
C4 P1 C2 D22 169(3) . . . . ?
W P1 C2 D22 -72(4) . . . . ?
C3 P1 C2 D23 178(3) . . . . ?
C4 P1 C2 D23 -74(3) . . . . ?
W P1 C2 D23 45(3) . . . . ?
C4 P1 C3 D33 -172(4) . . . . ?
C2 P1 C3 D33 -67(4) . . . . ?
W P1 C3 D33 69(4) . . . . ?
C4 P1 C3 D31 -55(4) . . . . ?
C2 P1 C3 D31 51(4) . . . . ?
W P1 C3 D31 -173(3) . . . . ?
C4 P1 C3 D32 66(4) . . . . ?
C2 P1 C3 D32 171(3) . . . . ?
W P1 C3 D32 -53(4) . . . . ?
C3 P1 C4 C5 -84(3) . . . . ?
C2 P1 C4 C5 170(2) . . . . ?
W P1 C4 C5 40(2) . . . . ?
P1 C4 C5 P2 -51(3) . . . . ?
C7 P2 C5 C4 -92(2) . . . . ?
C6 P2 C5 C4 162(2) . . . . ?
W P2 C5 C4 38(2) . . . . ?
C7 P2 C6 D63 173(4) . . . . ?
C5 P2 C6 D63 -80(4) . . . . ?
W P2 C6 D63 37(5) . . . . ?
C7 P2 C6 D61 -44(4) . . . . ?
C5 P2 C6 D61 62(4) . . . . ?
W P2 C6 D61 179(3) . . . . ?
C7 P2 C6 D62 60(4) . . . . ?
C5 P2 C6 D62 167(3) . . . . ?
W P2 C6 D62 -76(4) . . . . ?
C5 P2 C7 D73 -176(4) . . . . ?
C6 P2 C7 D73 -75(4) . . . . ?
W P2 C7 D73 60(4) . . . . ?
C5 P2 C7 D72 57(4) . . . . ?
C6 P2 C7 D72 159(4) . . . . ?
W P2 C7 D72 -66(4) . . . . ?
C5 P2 C7 D71 -55(4) . . . . ?
C6 P2 C7 D71 47(4) . . . . ?
W P2 C7 D71 -178(3) . . . . ?
C9 P3 C8 D82 -167(5) . . . . ?
C10 P3 C8 D82 90(5) . . . . ?
W P3 C8 D82 -29(5) . . . . ?
C9 P3 C8 D81 46(5) . . . . ?
C10 P3 C8 D81 -57(5) . . . . ?
W P3 C8 D81 -177(4) . . . . ?
C9 P3 C8 D83 -65(4) . . . . ?
C10 P3 C8 D83 -168(4) . . . . ?
W P3 C8 D83 72(5) . . . . ?
C8 P3 C10 C11 -161(3) . . . . ?
C9 P3 C10 C11 93(3) . . . . ?
W P3 C10 C11 -32(3) . . . . ?
C8 P3 C9 D92 76(5) . . . . ?
C10 P3 C9 D92 173(5) . . . . ?
W P3 C9 D92 -65(6) . . . . ?
C8 P3 C9 D93 -168(5) . . . . ?
C10 P3 C9 D93 -72(5) . . . . ?
W P3 C9 D93 50(5) . . . . ?
C8 P3 C9 D91 -45(5) . . . . ?
C10 P3 C9 D91 52(5) . . . . ?
W P3 C9 D91 174(4) . . . . ?
P3 C10 C11 P4 45(3) . . . . ?
C12 P4 C11 C10 -163(3) . . . . ?
C13 P4 C11 C10 89(3) . . . . ?
W P4 C11 C10 -38(3) . . . . ?
C11 P4 C12 D122 81(4) . . . . ?
C13 P4 C12 D122 -168(4) . . . . ?
W P4 C12 D122 -36(5) . . . . ?
C11 P4 C12 D121 -46(4) . . . . ?
C13 P4 C12 D121 65(4) . . . . ?
W P4 C12 D121 -163(3) . . . . ?
C11 P4 C12 D123 -168(4) . . . . ?
C13 P4 C12 D123 -57(4) . . . . ?
W P4 C12 D123 75(4) . . . . ?
C12 P4 C13 D132 65(7) . . . . ?
C11 P4 C13 D132 171(7) . . . . ?
W P4 C13 D132 -67(8) . . . . ?
C12 P4 C13 D133 -163(5) . . . . ?
C11 P4 C13 D133 -57(6) . . . . ?
W P4 C13 D133 64(6) . . . . ?
C12 P4 C13 D131 -57(5) . . . . ?
C11 P4 C13 D131 49(5) . . . . ?
W P4 C13 D131 171(4) . . . . ?