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#$Date: 2009-11-21 12:50:34 +0200 (Sat, 21 Nov 2009) $
#$Revision: 900 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1004001.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#

data_1004001

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
octakis(mu!3$-sulfido)-hexakis(tri-n-butylphosphine)
-hexa-tungsten
;
_chemical_name_common             'Tungsten sulfide cluster with tri-n-'
_chemical_melting_point           ?
_chemical_formula_moiety          'W6 S8 (PC12H27)6'
_chemical_formula_sum
 'C72 H162 P6 S8 W6'
_chemical_formula_weight          2573.42

_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_[local]_cod_cif_authors_sg_H-M  'C 2/c'
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'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 '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

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

loop_
_publ_author_name
'Jin, Song.'
'Zhou, Ran.'
'Scheuer, Ellen. M.'
'Adamchuk, Jennifer.'
'Rayburn, Lori. L.'
'DiSalvo, Francis. J.'
_journal_name_full
;
Inorganic Chemistry
;
_journal_volume                    40
_journal_year                      2001
_journal_page_first                2666
_journal_page_last                 2674
_cell_length_a                    24.6648(12)
_cell_length_b                    19.8619(9)
_cell_length_c                    20.1365(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  103.3240(10)
_cell_angle_gamma                 90.00
_cell_volume                      9599.1(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     163(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
_exptl_crystal_description        block
_exptl_crystal_colour             red
_exptl_crystal_size_max           0.4
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.3
_exptl_crystal_density_meas       'NOT MEASURED'
_exptl_crystal_density_diffrn     1.781
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              5024
_exptl_absorpt_coefficient_mu     7.469
_exptl_absorpt_correction_type    empirical
_exptl_absorpt_correction_T_min   0.529617
_exptl_absorpt_correction_T_max   1
_exptl_absorpt_process_details    ?
_exptl_special_details
;
octakis(mu!3$-sulfido)-hexakis(tri-n-butylphosphine)
-hexa-tungsten
;
_diffrn_ambient_temperature       163(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   ?
_diffrn_measurement_method        '\w scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         0
_diffrn_reflns_number             67732
_diffrn_reflns_av_R_equivalents   0.0351
_diffrn_reflns_av_sigmaI/netI     0.0331
_diffrn_reflns_limit_h_min        -37
_diffrn_reflns_limit_h_max        31
_diffrn_reflns_limit_k_min        -30
_diffrn_reflns_limit_k_max        29
_diffrn_reflns_limit_l_min        -30
_diffrn_reflns_limit_l_max        28
_diffrn_reflns_theta_min          1.56
_diffrn_reflns_theta_max          33.22
_reflns_number_total              17073
_reflns_number_gt                 13885
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'BRUKER SMART'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         SHELXTL
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     SHELXTL
_computing_publication_material   SHELXTL

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

 There were some disorder for some butyl groups of the P-n-Bu3 ligands,
 which were all modelled successfully.
 Hydrogen atoms were added based on riding models though some H atoms
 were even visible in Fourier difference maps.

 Anisotropic refinements were performed on all non-hydrogen atoms.

;

_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^)+(0.0273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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          17073
_refine_ls_number_parameters      581
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0396
_refine_ls_R_factor_gt            0.0250
_refine_ls_wR_factor_ref          0.0590
_refine_ls_wR_factor_gt           0.0506
_refine_ls_goodness_of_fit_ref    1.089
_refine_ls_restrained_S_all       1.089
_refine_ls_shift/su_max           0.045
_refine_ls_shift/su_mean          0.002

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
W1 W 0.221998(5) 0.661077(5) 0.487536(5) 0.01761(3) Uani 1 1 d . . .
W2 W 0.318507(5) 0.720290(5) 0.483260(5) 0.01700(3) Uani 1 1 d . . .
W3 W 0.277213(5) 0.732942(5) 0.594292(5) 0.01748(3) Uani 1 1 d . . .
S1 S 0.31176(3) 0.62583(3) 0.55952(4) 0.02175(14) Uani 1 1 d . . .
S2 S 0.26217(3) 0.65700(3) 0.38643(4) 0.02124(14) Uani 1 1 d . . .
S3 S 0.13662(3) 0.71088(4) 0.41763(4) 0.02330(14) Uani 1 1 d . . .
S4 S 0.18644(3) 0.68070(4) 0.59069(4) 0.02235(14) Uani 1 1 d . . .
P1 P 0.18736(4) 0.54149(4) 0.47100(4) 0.02516(16) Uani 1 1 d . . .
P2 P 0.41114(3) 0.68164(4) 0.46487(4) 0.02415(15) Uani 1 1 d . . .
P3 P 0.31241(4) 0.70392(5) 0.71849(4) 0.03089(19) Uani 1 1 d . . .
C101 C 0.1333(4) 0.5201(4) 0.5175(5) 0.0234(16) Uani 0.533(8) 1 d P A 1
H10A H 0.1237 0.4719 0.5093 0.028 Uiso 0.533(8) 1 calc PR A 1
H10B H 0.1495 0.5255 0.5669 0.028 Uiso 0.533(8) 1 calc PR A 1
C102 C 0.0800(3) 0.5605(3) 0.4994(4) 0.0297(15) Uani 0.533(8) 1 d P A 1
H10C H 0.0610 0.5508 0.4514 0.036 Uiso 0.533(8) 1 calc PR A 1
H10Z H 0.0895 0.6090 0.5026 0.036 Uiso 0.533(8) 1 calc PR A 1
C103 C 0.0396(3) 0.5458(4) 0.5453(4) 0.046(2) Uani 0.533(8) 1 d P A 1
H10D H 0.0044 0.5707 0.5277 0.056 Uiso 0.533(8) 1 calc PR A 1
H10E H 0.0308 0.4971 0.5433 0.056 Uiso 0.533(8) 1 calc PR A 1
C104 C 0.0624(4) 0.5650(6) 0.6156(6) 0.061(3) Uani 0.533(8) 1 d P A 1
H10F H 0.0352 0.5551 0.6429 0.091 Uiso 0.533(8) 1 calc PR A 1
H10G H 0.0708 0.6133 0.6179 0.091 Uiso 0.533(8) 1 calc PR A 1
H10H H 0.0967 0.5395 0.6336 0.091 Uiso 0.533(8) 1 calc PR A 1
C11' C 0.1512(5) 0.5088(7) 0.5335(7) 0.038(3) Uani 0.467(8) 1 d P A 2
H11H H 0.1430 0.4605 0.5240 0.046 Uiso 0.467(8) 1 calc PR A 2
H11I H 0.1763 0.5122 0.5795 0.046 Uiso 0.467(8) 1 calc PR A 2
C12' C 0.0974(5) 0.5450(5) 0.5340(6) 0.050(3) Uani 0.467(8) 1 d P A 2
H12A H 0.0694 0.5362 0.4910 0.060 Uiso 0.467(8) 1 calc PR A 2
H12Z H 0.1039 0.5942 0.5384 0.060 Uiso 0.467(8) 1 calc PR A 2
C13' C 0.0750(5) 0.5158(5) 0.6005(5) 0.090(5) Uani 0.467(8) 1 d P A 2
H13A H 0.0616 0.4689 0.5925 0.03(2) Uiso 0.467(8) 1 calc PR A 2
H13B H 0.1051 0.5172 0.6426 0.25(11) Uiso 0.467(8) 1 calc PR A 2
C14' C 0.0282(5) 0.5624(5) 0.6060(5) 0.082(5) Uani 0.467(8) 1 d PR A 2
H14A H 0.0124 0.5484 0.6443 0.099 Uiso 0.467(8) 1 calc PR A 2
H14B H -0.0008 0.5607 0.5636 0.099 Uiso 0.467(8) 1 calc PR A 2
H14C H 0.0425 0.6085 0.6137 0.099 Uiso 0.467(8) 1 calc PR A 2
C105 C 0.15063(15) 0.51964(15) 0.38377(17) 0.0318(7) Uani 1 1 d . A .
H10I H 0.1173 0.5488 0.3710 0.038 Uiso 1 1 calc R . .
H10Y H 0.1752 0.5310 0.3529 0.038 Uiso 1 1 calc R . .
C106 C 0.13194(17) 0.44700(17) 0.37022(19) 0.0426(9) Uani 1 1 d . . .
H10J H 0.1652 0.4175 0.3806 0.051 Uiso 1 1 calc R A .
H10K H 0.1080 0.4346 0.4016 0.051 Uiso 1 1 calc R . .
C107 C 0.10028(19) 0.4340(2) 0.2979(2) 0.0516(11) Uani 1 1 d . A .
H10L H 0.0659 0.4615 0.2883 0.062 Uiso 1 1 calc R . .
H10M H 0.1233 0.4487 0.2663 0.062 Uiso 1 1 calc R . .
C108 C 0.0847(2) 0.3611(2) 0.2838(2) 0.0760(18) Uani 1 1 d . . .
H10N H 0.0642 0.3561 0.2362 0.114 Uiso 1 1 calc R A .
H10O H 0.0611 0.3463 0.3141 0.114 Uiso 1 1 calc R . .
H10P H 0.1185 0.3336 0.2919 0.114 Uiso 1 1 calc R . .
C109 C 0.24167(15) 0.47756(15) 0.49410(17) 0.0333(8) Uani 1 1 d . A .
H10Q H 0.2599 0.4831 0.5430 0.040 Uiso 1 1 calc R . .
H10R H 0.2237 0.4327 0.4886 0.040 Uiso 1 1 calc R . .
C110 C 0.28632(15) 0.47870(16) 0.45350(17) 0.0333(8) Uani 1 1 d . . .
H11A H 0.2982 0.5258 0.4491 0.040 Uiso 1 1 calc R A .
H11B H 0.2706 0.4611 0.4071 0.040 Uiso 1 1 calc R . .
C111 C 0.33680(18) 0.4367(2) 0.4873(2) 0.0528(11) Uani 1 1 d . A .
H11C H 0.3520 0.4539 0.5340 0.063 Uiso 1 1 calc R . .
H11D H 0.3248 0.3896 0.4912 0.063 Uiso 1 1 calc R . .
C112 C 0.38193(18) 0.4376(2) 0.4487(3) 0.0576(12) Uani 1 1 d . . .
H11E H 0.4133 0.4099 0.4728 0.086 Uiso 1 1 calc R A .
H11F H 0.3946 0.4839 0.4454 0.086 Uiso 1 1 calc R . .
H11G H 0.3675 0.4194 0.4028 0.086 Uiso 1 1 calc R . .
C201 C 0.4087(5) 0.6477(5) 0.3791(6) 0.0270(17) Uani 0.734(12) 1 d P B 1
H20A H 0.4459 0.6295 0.3784 0.032 Uiso 0.734(12) 1 calc PR B 1
H20B H 0.3820 0.6096 0.3707 0.032 Uiso 0.734(12) 1 calc PR B 1
C202 C 0.3920(3) 0.6979(3) 0.3214(3) 0.0305(12) Uani 0.734(12) 1 d P B 1
H20C H 0.3598 0.7242 0.3289 0.037 Uiso 0.734(12) 1 calc PR B 1
H20D H 0.4232 0.7297 0.3235 0.037 Uiso 0.734(12) 1 calc PR B 1
C203 C 0.3766(3) 0.6683(3) 0.2508(3) 0.0493(19) Uani 0.734(12) 1 d P B 1
H20E H 0.3465 0.6349 0.2490 0.059 Uiso 0.734(12) 1 calc PR B 1
H20F H 0.3617 0.7046 0.2179 0.059 Uiso 0.734(12) 1 calc PR B 1
C204 C 0.4236(6) 0.6351(7) 0.2287(5) 0.174(8) Uani 0.734(12) 1 d P B 1
H20G H 0.4104 0.6172 0.1825 0.261 Uiso 0.734(12) 1 calc PR B 1
H20H H 0.4380 0.5981 0.2601 0.261 Uiso 0.734(12) 1 calc PR B 1
H20I H 0.4532 0.6680 0.2292 0.261 Uiso 0.734(12) 1 calc PR B 1
C21' C 0.4144(14) 0.6309(13) 0.3902(18) 0.027(4) Uani 0.266(12) 1 d P B 2
H21F H 0.4516 0.6094 0.3977 0.032 Uiso 0.266(12) 1 calc PR B 2
H21G H 0.3862 0.5946 0.3849 0.032 Uiso 0.266(12) 1 calc PR B 2
C22' C 0.4042(8) 0.6725(11) 0.3247(9) 0.037(4) Uani 0.266(12) 1 d P B 2
H22A H 0.3672 0.6942 0.3176 0.044 Uiso 0.266(12) 1 calc PR B 2
H22B H 0.4325 0.7087 0.3303 0.044 Uiso 0.266(12) 1 calc PR B 2
C23' C 0.4065(8) 0.6313(9) 0.2611(9) 0.050(5) Uani 0.266(12) 1 d P B 2
H23A H 0.4412 0.6045 0.2713 0.060 Uiso 0.266(12) 1 calc PR B 2
H23B H 0.3749 0.5992 0.2525 0.060 Uiso 0.266(12) 1 calc PR B 2
C24' C 0.4045(10) 0.6679(14) 0.2005(10) 0.083(8) Uani 0.266(12) 1 d P B 2
H24A H 0.4035 0.6365 0.1627 0.099 Uiso 0.266(12) 1 calc PR B 2
H24B H 0.4376 0.6965 0.2063 0.099 Uiso 0.266(12) 1 calc PR B 2
H24C H 0.3710 0.6962 0.1904 0.099 Uiso 0.266(12) 1 calc PR B 2
C205 C 0.44569(15) 0.61636(17) 0.52372(18) 0.0344(7) Uani 1 1 d . B .
H20J H 0.4201 0.5776 0.5208 0.041 Uiso 1 1 calc R . .
H20K H 0.4790 0.6007 0.5085 0.041 Uiso 1 1 calc R . .
C206 C 0.46383(18) 0.6381(2) 0.59829(19) 0.0463(10) Uani 1 1 d . . .
H20L H 0.4302 0.6485 0.6153 0.056 Uiso 0.52(2) 1 calc PR B 1
H20M H 0.4858 0.6801 0.6007 0.056 Uiso 0.52(2) 1 calc PR B 1
H20R H 0.5004 0.6610 0.6056 0.056 Uiso 0.48(2) 1 calc PR B 2
H20S H 0.4366 0.6709 0.6083 0.056 Uiso 0.48(2) 1 calc PR B 2
C207 C 0.4992(5) 0.5848(7) 0.6465(6) 0.057(3) Uani 0.52(2) 1 d P B 1
H20N H 0.5321 0.5718 0.6290 0.068 Uiso 0.52(2) 1 calc PR B 1
H20X H 0.5126 0.6040 0.6928 0.068 Uiso 0.52(2) 1 calc PR B 1
C208 C 0.4622(7) 0.5219(6) 0.6497(6) 0.068(4) Uani 0.52(2) 1 d P B 1
H20P H 0.4834 0.4890 0.6817 0.102 Uiso 0.52(2) 1 calc PR B 1
H20Q H 0.4510 0.5016 0.6042 0.102 Uiso 0.52(2) 1 calc PR B 1
H20R H 0.4289 0.5355 0.6651 0.102 Uiso 0.52(2) 1 calc PR B 1
C27' C 0.4685(12) 0.5791(9) 0.6475(7) 0.090(7) Uani 0.48(2) 1 d P B 2
H27A H 0.4817 0.5976 0.6941 0.108 Uiso 0.48(2) 1 calc PR B 2
H27B H 0.4302 0.5623 0.6443 0.108 Uiso 0.48(2) 1 calc PR B 2
C28' C 0.5010(12) 0.5240(8) 0.6425(8) 0.117(9) Uani 0.48(2) 1 d P B 2
H28A H 0.4951 0.4893 0.6747 0.175 Uiso 0.48(2) 1 calc PR B 2
H28B H 0.5404 0.5374 0.6534 0.175 Uiso 0.48(2) 1 calc PR B 2
H28C H 0.4909 0.5061 0.5960 0.175 Uiso 0.48(2) 1 calc PR B 2
C209 C 0.46358(13) 0.74862(16) 0.47293(18) 0.0300(7) Uani 1 1 d . B .
H20O H 0.4489 0.7834 0.4382 0.036 Uiso 1 1 calc R . .
H20W H 0.4675 0.7699 0.5182 0.036 Uiso 1 1 calc R . .
C210 C 0.52155(15) 0.72880(19) 0.4654(2) 0.0405(8) Uani 1 1 d . . .
H20S H 0.5375 0.6958 0.5014 0.049 Uiso 1 1 calc R B .
H20T H 0.5181 0.7063 0.4207 0.049 Uiso 1 1 calc R . .
C211 C 0.56111(17) 0.7870(2) 0.4700(2) 0.0517(11) Uani 1 1 d . B .
H21A H 0.5650 0.8093 0.5149 0.062 Uiso 1 1 calc R . .
H21B H 0.5452 0.8203 0.4342 0.062 Uiso 1 1 calc R . .
C212 C 0.61794(18) 0.7662(3) 0.4618(3) 0.0619(13) Uani 1 1 d . . .
H21C H 0.6419 0.8060 0.4652 0.093 Uiso 1 1 calc R B .
H21D H 0.6145 0.7450 0.4170 0.093 Uiso 1 1 calc R . .
H21E H 0.6343 0.7341 0.4977 0.093 Uiso 1 1 calc R . .
C301 C 0.3311(6) 0.6203(6) 0.7393(5) 0.033(2) Uani 0.64(3) 1 d P C 1
H30A H 0.3577 0.6049 0.7123 0.040 Uiso 0.64(3) 1 calc PR C 1
H30B H 0.3500 0.6173 0.7883 0.040 Uiso 0.64(3) 1 calc PR C 1
C302 C 0.2795(7) 0.5741(5) 0.7247(6) 0.039(3) Uani 0.64(3) 1 d P C 1
H30C H 0.2536 0.5894 0.7526 0.047 Uiso 0.64(3) 1 calc PR C 1
H30D H 0.2601 0.5788 0.6761 0.047 Uiso 0.64(3) 1 calc PR C 1
C303 C 0.2925(9) 0.5014(5) 0.7395(5) 0.051(4) Uani 0.64(3) 1 d P C 1
H30E H 0.3132 0.4967 0.7876 0.062 Uiso 0.64(3) 1 calc PR C 1
H30F H 0.3171 0.4854 0.7102 0.062 Uiso 0.64(3) 1 calc PR C 1
C304 C 0.2418(9) 0.4574(5) 0.7277(7) 0.062(4) Uani 0.64(3) 1 d P C 1
H30G H 0.2530 0.4105 0.7383 0.093 Uiso 0.64(3) 1 calc PR C 1
H30H H 0.2215 0.4607 0.6799 0.093 Uiso 0.64(3) 1 calc PR C 1
H30I H 0.2176 0.4721 0.7573 0.093 Uiso 0.64(3) 1 calc PR C 1
C31' C 0.3148(7) 0.6045(8) 0.7326(7) 0.016(2) Uani 0.36(3) 1 d P C 2
H31H H 0.3410 0.5852 0.7071 0.019 Uiso 0.36(3) 1 calc PR C 2
H31Z H 0.3304 0.5955 0.7816 0.019 Uiso 0.36(3) 1 calc PR C 2
C32' C 0.2585(8) 0.5665(9) 0.7105(9) 0.026(3) Uani 0.36(3) 1 d P C 2
H32A H 0.2437 0.5714 0.6607 0.031 Uiso 0.36(3) 1 calc PR C 2
H32B H 0.2311 0.5861 0.7340 0.031 Uiso 0.36(3) 1 calc PR C 2
C33' C 0.2674(8) 0.4899(7) 0.7294(9) 0.032(3) Uani 0.36(3) 1 d P C 2
H33A H 0.2948 0.4707 0.7057 0.038 Uiso 0.36(3) 1 calc PR C 2
H33B H 0.2827 0.4854 0.7791 0.038 Uiso 0.36(3) 1 calc PR C 2
C34' C 0.2131(9) 0.4505(7) 0.7093(8) 0.039(4) Uani 0.36(3) 1 d P C 2
H34A H 0.2202 0.4030 0.7214 0.058 Uiso 0.36(3) 1 calc PR C 2
H34B H 0.1980 0.4544 0.6600 0.058 Uiso 0.36(3) 1 calc PR C 2
H34C H 0.1862 0.4687 0.7335 0.058 Uiso 0.36(3) 1 calc PR C 2
C305 C 0.3817(3) 0.7501(4) 0.7583(4) 0.0340(18) Uani 0.610(10) 1 d P C 1
H30J H 0.3969 0.7315 0.8045 0.041 Uiso 0.610(10) 1 calc PR C 1
H30K H 0.4089 0.7402 0.7303 0.041 Uiso 0.610(10) 1 calc PR C 1
C306 C 0.3768(3) 0.8273(4) 0.7643(4) 0.0363(16) Uani 0.610(10) 1 d P C 1
H30L H 0.3510 0.8444 0.7225 0.044 Uiso 0.610(10) 1 calc PR C 1
H30Z H 0.3602 0.8376 0.8035 0.044 Uiso 0.610(10) 1 calc PR C 1
C307 C 0.4315(3) 0.8638(4) 0.7736(4) 0.058(2) Uani 0.610(10) 1 d P C 1
H30M H 0.4474 0.8546 0.7337 0.069 Uiso 0.610(10) 1 calc PR C 1
H30N H 0.4246 0.9128 0.7748 0.069 Uiso 0.610(10) 1 calc PR C 1
C308 C 0.4733(4) 0.8442(6) 0.8373(5) 0.092(4) Uani 0.610(10) 1 d P C 1
H30O H 0.5075 0.8704 0.8408 0.138 Uiso 0.610(10) 1 calc PR C 1
H30P H 0.4818 0.7961 0.8356 0.138 Uiso 0.610(10) 1 calc PR C 1
H30Q H 0.4579 0.8532 0.8772 0.138 Uiso 0.610(10) 1 calc PR C 1
C35' C 0.3787(5) 0.7217(5) 0.7626(6) 0.025(2) Uani 0.390(10) 1 d P C 2
H35A H 0.3867 0.6972 0.8066 0.030 Uiso 0.390(10) 1 calc PR C 2
H35B H 0.4055 0.7063 0.7361 0.030 Uiso 0.390(10) 1 calc PR C 2
C36' C 0.3862(4) 0.7979(5) 0.7763(5) 0.0246(19) Uani 0.390(10) 1 d P C 2
H36A H 0.3767 0.8222 0.7322 0.030 Uiso 0.390(10) 1 calc PR C 2
H36B H 0.3598 0.8127 0.8037 0.030 Uiso 0.390(10) 1 calc PR C 2
C37' C 0.4451(4) 0.8163(5) 0.8137(6) 0.046(3) Uani 0.390(10) 1 d P C 2
H37A H 0.4554 0.7898 0.8564 0.055 Uiso 0.390(10) 1 calc PR C 2
H37B H 0.4712 0.8041 0.7849 0.055 Uiso 0.390(10) 1 calc PR C 2
C38' C 0.4515(6) 0.8908(6) 0.8310(8) 0.067(4) Uani 0.390(10) 1 d P C 2
H38A H 0.4901 0.9000 0.8552 0.100 Uiso 0.390(10) 1 calc PR C 2
H38B H 0.4263 0.9032 0.8601 0.100 Uiso 0.390(10) 1 calc PR C 2
H38C H 0.4424 0.9173 0.7888 0.100 Uiso 0.390(10) 1 calc PR C 2
C309 C 0.26647(14) 0.72969(16) 0.77369(15) 0.0286(7) Uani 1 1 d . C .
H30R H 0.2629 0.7793 0.7715 0.034 Uiso 1 1 calc R . .
H30S H 0.2290 0.7106 0.7547 0.034 Uiso 1 1 calc R . .
C310 C 0.28445(17) 0.70919(19) 0.84890(17) 0.0401(9) Uani 1 1 d . . .
H31A H 0.2864 0.6595 0.8518 0.048 Uiso 1 1 calc R C .
H31B H 0.3223 0.7269 0.8681 0.048 Uiso 1 1 calc R . .
C311 C 0.24542(17) 0.73457(19) 0.89221(18) 0.0403(9) Uani 1 1 d . C .
H31C H 0.2070 0.7199 0.8709 0.048 Uiso 1 1 calc R . .
H31D H 0.2562 0.7135 0.9379 0.048 Uiso 1 1 calc R . .
C312 C 0.24594(19) 0.8098(2) 0.9005(2) 0.0477(10) Uani 1 1 d . . .
H31E H 0.2202 0.8227 0.9288 0.072 Uiso 1 1 calc R C .
H31F H 0.2343 0.8311 0.8556 0.072 Uiso 1 1 calc R . .
H31G H 0.2837 0.8247 0.9225 0.072 Uiso 1 1 calc R . .

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
W1 0.01963(6) 0.01538(5) 0.01926(5) -0.00059(4) 0.00741(4) -0.00143(4)
W2 0.01750(6) 0.01722(5) 0.01737(5) -0.00004(4) 0.00626(4) 0.00013(4)
W3 0.01970(6) 0.01794(5) 0.01551(5) 0.00054(4) 0.00549(4) 0.00091(4)
S1 0.0252(4) 0.0197(3) 0.0216(3) 0.0028(2) 0.0080(3) 0.0040(3)
S2 0.0242(4) 0.0207(3) 0.0198(3) -0.0031(2) 0.0072(3) -0.0006(2)
S3 0.0191(4) 0.0270(3) 0.0234(3) -0.0045(3) 0.0041(3) -0.0019(3)
S4 0.0260(4) 0.0206(3) 0.0233(3) 0.0013(2) 0.0114(3) -0.0020(3)
P1 0.0318(5) 0.0181(3) 0.0286(4) -0.0015(3) 0.0133(3) -0.0041(3)
P2 0.0211(4) 0.0261(4) 0.0270(4) -0.0009(3) 0.0091(3) 0.0022(3)
P3 0.0338(5) 0.0426(5) 0.0170(4) 0.0040(3) 0.0075(3) 0.0157(4)
C101 0.017(5) 0.019(3) 0.039(5) 0.003(3) 0.016(3) 0.001(3)
C102 0.028(4) 0.031(3) 0.034(4) 0.000(3) 0.014(3) -0.003(3)
C103 0.044(5) 0.042(4) 0.063(5) 0.006(4) 0.032(4) 0.000(3)
C104 0.048(6) 0.069(6) 0.075(7) -0.005(5) 0.035(6) -0.007(5)
C11' 0.028(7) 0.038(6) 0.050(7) 0.000(4) 0.011(5) -0.005(4)
C12' 0.045(6) 0.042(5) 0.057(7) 0.001(4) 0.000(5) -0.019(4)
C13' 0.087(10) 0.124(13) 0.062(8) -0.050(8) 0.025(7) -0.003(9)
C14' 0.136(15) 0.066(8) 0.061(8) -0.006(6) 0.054(10) -0.011(10)
C105 0.034(2) 0.0225(14) 0.0368(18) -0.0027(12) 0.0032(14) -0.0031(12)
C106 0.052(2) 0.0265(16) 0.043(2) -0.0046(14) -0.0026(17) -0.0082(15)
C107 0.062(3) 0.042(2) 0.044(2) -0.0078(17) -0.0041(19) -0.0134(19)
C108 0.111(5) 0.046(3) 0.052(3) -0.016(2) -0.019(3) -0.012(3)
C109 0.046(2) 0.0196(14) 0.0322(17) 0.0040(12) 0.0040(14) -0.0018(13)
C110 0.037(2) 0.0243(15) 0.0360(18) -0.0045(13) 0.0030(14) 0.0078(13)
C111 0.044(3) 0.043(2) 0.069(3) 0.015(2) 0.006(2) 0.0122(18)
C112 0.042(3) 0.047(2) 0.081(3) -0.011(2) 0.007(2) 0.0113(19)
C201 0.030(3) 0.025(5) 0.029(4) 0.001(3) 0.012(3) 0.007(3)
C202 0.033(3) 0.033(3) 0.027(2) 0.000(2) 0.011(2) 0.005(2)
C203 0.069(5) 0.046(3) 0.029(3) -0.004(2) 0.004(3) 0.015(3)
C204 0.228(16) 0.261(17) 0.042(6) 0.027(8) 0.049(8) 0.182(14)
C21' 0.033(12) 0.014(10) 0.036(13) 0.001(7) 0.014(9) -0.001(7)
C22' 0.029(9) 0.042(11) 0.040(9) 0.001(8) 0.010(6) 0.015(7)
C23' 0.043(11) 0.056(11) 0.054(11) 0.019(8) 0.018(8) -0.004(8)
C24' 0.072(16) 0.14(2) 0.035(11) -0.016(12) 0.013(10) 0.008(14)
C205 0.0283(19) 0.0326(17) 0.044(2) 0.0031(14) 0.0112(14) 0.0087(13)
C206 0.046(3) 0.048(2) 0.040(2) 0.0087(17) 0.0001(17) 0.0079(18)
C207 0.018(5) 0.090(8) 0.063(6) 0.035(5) 0.010(4) 0.015(5)
C208 0.071(9) 0.061(7) 0.077(7) 0.042(5) 0.027(6) 0.030(6)
C27' 0.117(18) 0.095(12) 0.054(7) 0.026(7) 0.012(9) 0.053(12)
C28' 0.15(2) 0.101(12) 0.108(12) 0.051(9) 0.047(12) 0.087(13)
C209 0.0201(16) 0.0326(16) 0.0385(18) -0.0018(13) 0.0093(13) -0.0007(12)
C210 0.0266(19) 0.049(2) 0.049(2) 0.0014(17) 0.0169(16) 0.0019(15)
C211 0.028(2) 0.061(3) 0.070(3) 0.010(2) 0.0203(19) -0.0047(18)
C212 0.028(2) 0.091(4) 0.069(3) 0.023(3) 0.015(2) -0.001(2)
C301 0.042(6) 0.030(5) 0.029(3) 0.004(3) 0.011(4) 0.005(4)
C302 0.062(9) 0.031(4) 0.025(4) 0.009(3) 0.014(5) 0.019(5)
C303 0.091(11) 0.027(4) 0.036(4) 0.007(3) 0.015(5) 0.007(5)
C304 0.109(13) 0.032(4) 0.055(6) 0.006(4) 0.035(7) 0.004(6)
C31' 0.017(6) 0.011(5) 0.017(4) 0.003(3) 0.001(4) -0.003(4)
C32' 0.031(8) 0.024(5) 0.021(6) 0.002(4) 0.002(5) 0.002(5)
C33' 0.037(9) 0.015(5) 0.041(7) 0.007(4) 0.004(6) -0.006(5)
C34' 0.052(10) 0.030(5) 0.035(7) 0.004(4) 0.012(6) -0.016(6)
C305 0.030(4) 0.049(5) 0.022(3) 0.008(4) 0.003(2) 0.007(4)
C306 0.034(4) 0.039(4) 0.034(3) -0.004(3) 0.004(3) 0.000(3)
C307 0.046(5) 0.064(5) 0.056(5) 0.001(4) -0.004(3) -0.009(4)
C308 0.069(7) 0.116(10) 0.071(7) 0.003(6) -0.026(5) -0.023(6)
C35' 0.029(5) 0.026(5) 0.021(4) 0.007(4) 0.007(3) 0.002(4)
C36' 0.028(5) 0.016(4) 0.028(4) -0.005(4) 0.003(3) 0.002(3)
C37' 0.019(5) 0.047(6) 0.070(8) -0.022(5) 0.006(5) -0.007(4)
C38' 0.050(8) 0.044(7) 0.104(12) -0.030(7) 0.013(7) -0.019(6)
C309 0.0320(18) 0.0340(16) 0.0211(14) 0.0019(12) 0.0085(12) 0.0095(13)
C310 0.051(2) 0.051(2) 0.0215(16) 0.0055(14) 0.0145(15) 0.0200(18)
C311 0.048(2) 0.053(2) 0.0233(16) 0.0026(15) 0.0155(15) 0.0113(17)
C312 0.058(3) 0.053(2) 0.035(2) -0.0089(17) 0.0165(18) 0.006(2)

_diffrn_measured_fraction_theta_max    0.927
_diffrn_reflns_theta_full              33.22
_diffrn_measured_fraction_theta_full   0.927
_refine_diff_density_max    0.983
_refine_diff_density_min   -1.718
_refine_diff_density_rms    0.396