Supplementary Material (ESI) for Chemical Communications
This journal is (C) The Royal Society of Chemistry 2001

data_global

_journal_coden_Cambridge      182

_publ_requested_journal       'Chemical Communications'

loop_
_publ_author_name
'Wolczanski, P.'
'Lobkovsky, Emil'
'Veige, Adam S.'

_publ_contact_author_name     	'Dr P Wolczanski'  
_publ_contact_author_address 
;
Department of Chemistry and Chemical Biology
Baker Laboratory
Cornell University
Ithaca
New York 14853
UNITED STATES OF AMERICA
;

_publ_contact_author_email       'PTW2@CORNELL.EDU'

_publ_section_title		
;
(silox)3RePMe3 (silox = tBu3SiO) is carbonylated to the double
insertion product (silox)(Me3P){cis-(CO)2}Re{CO2SitBu3)2}
;

data_asv513

_database_code_CSD	173800


_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C43 H90 O7 P Re Si3'
_chemical_formula_weight          1020.59

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'
'Si'  'Si'   0.0817   0.0704
'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'
'Re'  'Re'  -1.0185   7.2310
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                    13.2908(7)
_cell_length_b                    13.4716(8)
_cell_length_c                    17.7266(9)
_cell_angle_alpha                 96.464(2)
_cell_angle_beta                  104.696(2)
_cell_angle_gamma                 116.971(1)
_cell_volume                      2639.1(2)
_cell_formula_units_Z             2
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        block
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.284
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1072
_exptl_absorpt_coefficient_mu     2.442
_exptl_absorpt_correction_type    SADABS
_exptl_absorpt_correction_T_min   0.707013
_exptl_absorpt_correction_T_max   0.7923
_exptl_absorpt_process_details    ?

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       173(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   'Bruker 1K CCD'
_diffrn_measurement_method        '0.3 deg. omega scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             9207
_diffrn_reflns_av_R_equivalents   0.0274
_diffrn_reflns_av_sigmaI/netI     0.0542
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          1.82
_diffrn_reflns_theta_max          21.97
_reflns_number_total              6387
_reflns_number_gt                 5496
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        SMART
_computing_cell_refinement        SAINT+
_computing_data_reduction         SAINT+
_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.

One of the siloxo groups is disordered. We tried two different model:
1. two partitions refined isotropically.
2. one partition refined anisotropically.
The first one converged at sligtly lower R1 = 4/95%, but has some big
(~5 e/A^3) residual peaks and wierd geometry. The second approach produces
very large ellipsoids ( of course ),  R1 = 5.1% with much better overall
geometry and lower residual peaks in the heavy atom vicinity.
We report here results of the second model.
;

_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^)+(0.0642P)^2^+16.2380P] 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          6387
_refine_ls_number_parameters      496
_refine_ls_number_restraints      702
_refine_ls_R_factor_all           0.0632
_refine_ls_R_factor_gt            0.0510
_refine_ls_wR_factor_ref          0.1294
_refine_ls_wR_factor_gt           0.1228
_refine_ls_goodness_of_fit_ref    1.051
_refine_ls_restrained_S_all       1.073
_refine_ls_shift/su_max           1.669
_refine_ls_shift/su_mean          0.125

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
Re1 Re -0.02662(2) -0.17334(2) -0.293092(15) 0.02629(7) Uani 1 1 d . A .
Si1 Si -0.39916(14) -0.18479(15) -0.35214(11) 0.0358(5) Uani 1 1 d . . .
Si2 Si 0.28323(14) 0.19271(14) -0.12863(10) 0.0311(5) Uani 1 1 d . . .
Si3 Si -0.03318(15) -0.41960(15) -0.22871(12) 0.0387(5) Uani 1 1 d . A .
P1 P 0.01318(16) -0.21193(19) -0.41977(11) 0.0500(6) Uani 1 1 d . . .
O1 O -0.0322(4) 0.0335(4) -0.3477(3) 0.0466(14) Uani 1 1 d . A .
O2 O -0.0613(4) -0.1032(4) -0.1333(3) 0.0447(14) Uani 1 1 d . A .
O3 O -0.0227(3) -0.3177(3) -0.2740(3) 0.0370(12) Uani 1 1 d . . .
O4 O -0.2607(4) -0.3218(4) -0.3863(3) 0.0422(14) Uani 1 1 d . A .
O5 O -0.2602(3) -0.1692(3) -0.3162(2) 0.0323(12) Uani 1 1 d . A .
O6 O 0.2216(3) -0.0523(4) -0.2377(3) 0.0419(13) Uani 1 1 d . A .
O7 O 0.1632(3) 0.0638(3) -0.1859(2) 0.0316(11) Uani 1 1 d . A .
C1 C -0.0311(5) -0.0441(6) -0.3271(4) 0.035(2) Uani 1 1 d . . .
C2 C -0.0496(5) -0.1347(5) -0.1913(4) 0.0299(17) Uani 1 1 d . . .
C3 C -0.2087(5) -0.2276(5) -0.3381(4) 0.0316(18) Uani 1 1 d . . .
C4 C -0.5139(5) -0.3261(6) -0.3400(5) 0.085(4) Uani 1 1 d D . .
C5 C -0.4854(14) -0.3222(13) -0.2485(6) 0.209(9) Uani 1 1 d D . .
H5A H -0.5455 -0.3943 -0.2422 0.313 Uiso 1 1 calc R . .
H5B H -0.4874 -0.2569 -0.2198 0.313 Uiso 1 1 calc R . .
H5C H -0.4053 -0.3129 -0.2260 0.313 Uiso 1 1 calc R . .
C6 C -0.5029(8) -0.4309(7) -0.3539(9) 0.136(5) Uani 1 1 d D . .
H6A H -0.5690 -0.4949 -0.3446 0.205 Uiso 1 1 calc R . .
H6B H -0.4260 -0.4155 -0.3165 0.205 Uiso 1 1 calc R . .
H6C H -0.5064 -0.4515 -0.4097 0.205 Uiso 1 1 calc R . .
C7 C -0.6415(5) -0.3462(7) -0.3713(6) 0.075(3) Uani 1 1 d D . .
H7A H -0.6972 -0.4189 -0.3630 0.112 Uiso 1 1 calc R . .
H7B H -0.6642 -0.3502 -0.4291 0.112 Uiso 1 1 calc R . .
H7C H -0.6449 -0.2824 -0.3418 0.112 Uiso 1 1 calc R . .
C8 C -0.3762(5) -0.0565(5) -0.2793(4) 0.052(2) Uani 1 1 d D . .
C9 C -0.2820(10) 0.0535(8) -0.2929(10) 0.242(10) Uani 1 1 d D . .
H9A H -0.2684 0.1216 -0.2558 0.363 Uiso 1 1 calc R . .
H9B H -0.3113 0.0562 -0.3488 0.363 Uiso 1 1 calc R . .
H9C H -0.2064 0.0527 -0.2827 0.363 Uiso 1 1 calc R . .
C10 C -0.3163(12) -0.0421(11) -0.1923(6) 0.179(6) Uani 1 1 d D . .
H10A H -0.3114 0.0245 -0.1593 0.268 Uiso 1 1 calc R . .
H10B H -0.2351 -0.0294 -0.1836 0.268 Uiso 1 1 calc R . .
H10C H -0.3630 -0.1119 -0.1768 0.268 Uiso 1 1 calc R . .
C11 C -0.4843(6) -0.0394(7) -0.2913(6) 0.086(3) Uani 1 1 d D . .
H11A H -0.4633 0.0277 -0.2495 0.129 Uiso 1 1 calc R . .
H11B H -0.5515 -0.1084 -0.2873 0.129 Uiso 1 1 calc R . .
H11C H -0.5076 -0.0266 -0.3448 0.129 Uiso 1 1 calc R . .
C12 C -0.4361(6) -0.1910(7) -0.4607(5) 0.104(4) Uani 1 1 d D . .
C13 C -0.4845(11) -0.3179(8) -0.5137(8) 0.148(5) Uani 1 1 d D . .
H13A H -0.5040 -0.3192 -0.5711 0.222 Uiso 1 1 calc R . .
H13B H -0.5569 -0.3729 -0.5045 0.222 Uiso 1 1 calc R . .
H13C H -0.4225 -0.3394 -0.4979 0.222 Uiso 1 1 calc R . .
C14 C -0.3320(8) -0.1383(11) -0.4888(6) 0.151(6) Uani 1 1 d D . .
H14A H -0.3611 -0.1471 -0.5471 0.226 Uiso 1 1 calc R . .
H14B H -0.2849 -0.1770 -0.4774 0.226 Uiso 1 1 calc R . .
H14C H -0.2814 -0.0561 -0.4604 0.226 Uiso 1 1 calc R . .
C15 C -0.5329(6) -0.1630(7) -0.4972(5) 0.070(3) Uani 1 1 d D . .
H15A H -0.5461 -0.1704 -0.5550 0.104 Uiso 1 1 calc R . .
H15B H -0.5076 -0.0837 -0.4701 0.104 Uiso 1 1 calc R . .
H15C H -0.6078 -0.2166 -0.4901 0.104 Uiso 1 1 calc R . .
C16 C 0.1437(5) -0.0320(5) -0.2307(3) 0.0303(18) Uani 1 1 d . . .
C17 C 0.4027(5) 0.1683(5) -0.0577(4) 0.045(2) Uani 1 1 d D . .
C18 C 0.4827(5) 0.1503(7) -0.0992(5) 0.062(3) Uani 1 1 d D . .
H18A H 0.5408 0.1378 -0.0611 0.093 Uiso 1 1 calc R . .
H18B H 0.5257 0.2188 -0.1172 0.093 Uiso 1 1 calc R . .
H18C H 0.4330 0.0827 -0.1461 0.093 Uiso 1 1 calc R . .
C19 C 0.4855(7) 0.2742(6) 0.0157(4) 0.061(3) Uani 1 1 d D . .
H19A H 0.5455 0.2611 0.0512 0.091 Uiso 1 1 calc R . .
H19B H 0.4374 0.2861 0.0455 0.091 Uiso 1 1 calc R . .
H19C H 0.5263 0.3426 -0.0030 0.091 Uiso 1 1 calc R . .
C20 C 0.3404(7) 0.0612(5) -0.0290(4) 0.056(2) Uani 1 1 d D . .
H20A H 0.4009 0.0488 0.0065 0.084 Uiso 1 1 calc R . .
H20B H 0.2884 -0.0061 -0.0758 0.084 Uiso 1 1 calc R . .
H20C H 0.2916 0.0720 0.0008 0.084 Uiso 1 1 calc R . .
C21 C 0.3386(5) 0.2792(5) -0.2034(4) 0.049(2) Uani 1 1 d D . .
C22 C 0.3575(7) 0.2086(7) -0.2661(4) 0.068(3) Uani 1 1 d D . .
H22A H 0.3852 0.2536 -0.3037 0.101 Uiso 1 1 calc R . .
H22B H 0.2815 0.1371 -0.2961 0.101 Uiso 1 1 calc R . .
H22C H 0.4180 0.1898 -0.2389 0.101 Uiso 1 1 calc R . .
C23 C 0.4594(6) 0.3921(6) -0.1586(5) 0.064(3) Uani 1 1 d D . .
H23A H 0.4857 0.4347 -0.1976 0.096 Uiso 1 1 calc R . .
H23B H 0.5200 0.3736 -0.1311 0.096 Uiso 1 1 calc R . .
H23C H 0.4489 0.4397 -0.1186 0.096 Uiso 1 1 calc R . .
C24 C 0.2500(6) 0.3129(6) -0.2485(5) 0.064(3) Uani 1 1 d D . .
H24A H 0.2817 0.3563 -0.2858 0.097 Uiso 1 1 calc R . .
H24B H 0.2386 0.3610 -0.2097 0.097 Uiso 1 1 calc R . .
H24C H 0.1727 0.2430 -0.2792 0.097 Uiso 1 1 calc R . .
C25 C 0.2042(5) 0.2479(5) -0.0733(3) 0.0393(19) Uani 1 1 d D . .
C26 C 0.1757(7) 0.1870(6) -0.0071(4) 0.059(2) Uani 1 1 d D . .
H26A H 0.1356 0.2170 0.0200 0.088 Uiso 1 1 calc R . .
H26B H 0.2506 0.2014 0.0324 0.088 Uiso 1 1 calc R . .
H26C H 0.1228 0.1037 -0.0315 0.088 Uiso 1 1 calc R . .
C27 C 0.0818(5) 0.2196(6) -0.1314(5) 0.051(2) Uani 1 1 d D . .
H27A H 0.0429 0.2482 -0.1020 0.077 Uiso 1 1 calc R . .
H27B H 0.0310 0.1357 -0.1538 0.077 Uiso 1 1 calc R . .
H27C H 0.0933 0.2566 -0.1754 0.077 Uiso 1 1 calc R . .
C28 C 0.2793(6) 0.3794(5) -0.0346(5) 0.053(2) Uani 1 1 d D . .
H28A H 0.2355 0.4034 -0.0070 0.080 Uiso 1 1 calc R . .
H28B H 0.2935 0.4198 -0.0767 0.080 Uiso 1 1 calc R . .
H28C H 0.3565 0.3986 0.0046 0.080 Uiso 1 1 calc R . .
C29 C 0.1012(5) -0.3526(5) -0.1288(4) 0.052(2) Uani 1 1 d D . .
C30 C 0.0841(7) -0.2797(7) -0.0655(5) 0.074(3) Uani 1 1 d D A .
H30A H 0.1533 -0.2463 -0.0152 0.111 Uiso 1 1 calc R . .
H30B H 0.0106 -0.3287 -0.0549 0.111 Uiso 1 1 calc R . .
H30C H 0.0774 -0.2175 -0.0859 0.111 Uiso 1 1 calc R . .
C31 C 0.2158(6) -0.2681(6) -0.1423(6) 0.068(3) Uani 1 1 d D A .
H31A H 0.2839 -0.2345 -0.0914 0.102 Uiso 1 1 calc R . .
H31B H 0.2057 -0.2064 -0.1610 0.102 Uiso 1 1 calc R . .
H31C H 0.2312 -0.3093 -0.1831 0.102 Uiso 1 1 calc R . .
C32 C 0.1282(8) -0.4371(6) -0.0893(6) 0.088(4) Uani 1 1 d D A .
H32A H 0.1980 -0.3940 -0.0393 0.132 Uiso 1 1 calc R . .
H32B H 0.1456 -0.4815 -0.1265 0.132 Uiso 1 1 calc R . .
H32C H 0.0584 -0.4899 -0.0766 0.132 Uiso 1 1 calc R . .
C33 C -0.0260(5) -0.5334(5) -0.3009(4) 0.055(2) Uani 1 1 d D . .
C34 C -0.1009(8) -0.5504(8) -0.3874(5) 0.086(3) Uani 1 1 d D A .
H34A H -0.0979 -0.6079 -0.4245 0.129 Uiso 1 1 calc R . .
H34B H -0.0685 -0.4769 -0.4020 0.129 Uiso 1 1 calc R . .
H34C H -0.1845 -0.5774 -0.3911 0.129 Uiso 1 1 calc R . .
C35 C 0.1030(6) -0.4913(8) -0.2992(7) 0.095(4) Uani 1 1 d D A .
H35A H 0.1042 -0.5501 -0.3364 0.142 Uiso 1 1 calc R . .
H35B H 0.1547 -0.4776 -0.2443 0.142 Uiso 1 1 calc R . .
H35C H 0.1326 -0.4193 -0.3159 0.142 Uiso 1 1 calc R . .
C36 C -0.0714(8) -0.6513(6) -0.2822(6) 0.091(4) Uani 1 1 d D A .
H36A H -0.0652 -0.7039 -0.3213 0.137 Uiso 1 1 calc R . .
H36B H -0.1555 -0.6831 -0.2858 0.137 Uiso 1 1 calc R . .
H36C H -0.0224 -0.6422 -0.2275 0.137 Uiso 1 1 calc R . .
C37 C -0.1861(5) -0.4894(5) -0.2109(4) 0.046(2) Uani 1 1 d D . .
C38 C -0.2908(6) -0.5632(6) -0.2909(5) 0.059(3) Uani 1 1 d D A .
H38A H -0.3668 -0.5974 -0.2804 0.089 Uiso 1 1 calc R . .
H38B H -0.2799 -0.6247 -0.3157 0.089 Uiso 1 1 calc R . .
H38C H -0.2925 -0.5144 -0.3277 0.089 Uiso 1 1 calc R . .
C39 C -0.1934(7) -0.5654(6) -0.1525(5) 0.070(3) Uani 1 1 d D A .
H39A H -0.2723 -0.5976 -0.1461 0.104 Uiso 1 1 calc R . .
H39B H -0.1304 -0.5190 -0.0998 0.104 Uiso 1 1 calc R . .
H39C H -0.1822 -0.6285 -0.1740 0.104 Uiso 1 1 calc R . .
C40 C -0.2116(5) -0.3956(5) -0.1784(5) 0.051(2) Uani 1 1 d D A .
H40A H -0.2888 -0.4321 -0.1696 0.076 Uiso 1 1 calc R . .
H40B H -0.2148 -0.3506 -0.2178 0.076 Uiso 1 1 calc R . .
H40C H -0.1475 -0.3444 -0.1271 0.076 Uiso 1 1 calc R . .
C41 C 0.0945(14) -0.0686(13) -0.4487(10) 0.057(5) Uiso 0.501(19) 1 d P A 1
H41A H 0.1099 -0.0846 -0.4987 0.086 Uiso 0.501(19) 1 calc PR A 1
H41B H 0.1711 -0.0155 -0.4051 0.086 Uiso 0.501(19) 1 calc PR A 1
H41C H 0.0438 -0.0333 -0.4570 0.086 Uiso 0.501(19) 1 calc PR A 1
C41 C 0.0458(17) -0.1139(16) -0.4724(12) 0.069(6) Uiso 0.499(19) 1 d P A 2
H41D H 0.0580 -0.1431 -0.5204 0.103 Uiso 0.499(19) 1 calc PR A 2
H41E H 0.1193 -0.0423 -0.4387 0.103 Uiso 0.499(19) 1 calc PR A 2
H41F H -0.0208 -0.0985 -0.4890 0.103 Uiso 0.499(19) 1 calc PR A 2
C42 C 0.1272(6) -0.2520(8) -0.4107(5) 0.067(3) Uani 1 1 d . A .
H42A H 0.1365 -0.2653 -0.4634 0.101 Uiso 1 1 calc R . .
H42B H 0.1033 -0.3227 -0.3925 0.101 Uiso 1 1 calc R . .
H42C H 0.2037 -0.1896 -0.3713 0.101 Uiso 1 1 calc R . .
C43 C -0.1086(14) -0.2890(15) -0.5107(10) 0.063(5) Uiso 0.502(16) 1 d P A 1
H43A H -0.0788 -0.2957 -0.5551 0.094 Uiso 0.502(16) 1 calc PR A 1
H43B H -0.1535 -0.2480 -0.5210 0.094 Uiso 0.502(16) 1 calc PR A 1
H43C H -0.1616 -0.3662 -0.5067 0.094 Uiso 0.502(16) 1 calc PR A 1
C43 C -0.1205(13) -0.3456(14) -0.4988(10) 0.054(5) Uiso 0.498(16) 1 d P A 2
H43D H -0.1009 -0.3575 -0.5475 0.080 Uiso 0.498(16) 1 calc PR A 2
H43E H -0.1905 -0.3350 -0.5124 0.080 Uiso 0.498(16) 1 calc PR A 2
H43F H -0.1388 -0.4132 -0.4771 0.080 Uiso 0.498(16) 1 calc PR A 2

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
Re1 0.01969(10) 0.03407(12) 0.02394(12) 0.00599(9) 0.00951(9) 0.01188(8)
Si1 0.0248(7) 0.0422(9) 0.0399(10) 0.0056(8) 0.0100(7) 0.0182(7)
Si2 0.0283(7) 0.0326(8) 0.0326(9) 0.0103(7) 0.0119(7) 0.0142(6)
Si3 0.0301(8) 0.0289(8) 0.0558(11) 0.0064(8) 0.0153(8) 0.0145(7)
P1 0.0408(8) 0.0783(12) 0.0322(9) 0.0072(8) 0.0154(7) 0.0312(8)
O1 0.048(2) 0.036(2) 0.054(3) 0.026(2) 0.013(2) 0.0187(18)
O2 0.053(2) 0.047(2) 0.035(2) 0.0108(19) 0.0264(19) 0.0211(19)
O3 0.0277(18) 0.040(2) 0.042(2) 0.0053(19) 0.0080(18) 0.0189(16)
O4 0.026(2) 0.034(2) 0.046(3) -0.004(2) 0.002(2) 0.0080(17)
O5 0.0204(16) 0.036(2) 0.040(2) 0.0034(18) 0.0112(17) 0.0139(15)
O6 0.0249(19) 0.044(2) 0.050(3) 0.005(2) 0.0132(19) 0.0135(17)
O7 0.0280(17) 0.033(2) 0.034(2) 0.0091(17) 0.0134(16) 0.0140(15)
C1 0.020(3) 0.048(4) 0.025(3) 0.003(3) 0.009(2) 0.008(3)
C2 0.025(3) 0.024(3) 0.040(3) 0.015(3) 0.015(3) 0.008(2)
C3 0.012(3) 0.032(3) 0.039(3) 0.013(3) 0.008(2) 0.001(2)
C4 0.031(3) 0.038(4) 0.179(10) 0.018(5) 0.035(5) 0.016(3)
C5 0.133(13) 0.166(11) 0.221(14) 0.126(10) -0.006(11) 0.009(10)
C6 0.067(5) 0.088(6) 0.265(13) 0.090(7) 0.079(7) 0.026(5)
C7 0.038(3) 0.084(5) 0.111(6) 0.035(5) 0.038(4) 0.029(3)
C8 0.042(3) 0.048(4) 0.060(5) 0.002(3) 0.007(3) 0.027(3)
C9 0.132(7) 0.036(6) 0.55(3) -0.010(10) 0.190(11) 0.021(6)
C10 0.231(9) 0.207(9) 0.097(10) -0.058(8) -0.042(9) 0.181(7)
C11 0.069(4) 0.092(5) 0.101(7) -0.017(5) 0.021(5) 0.057(4)
C12 0.070(4) 0.204(9) 0.050(5) 0.027(6) 0.011(4) 0.086(5)
C13 0.171(9) 0.168(9) 0.095(9) -0.035(8) -0.003(8) 0.117(7)
C14 0.089(8) 0.239(11) 0.091(6) 0.117(6) 0.024(6) 0.043(8)
C15 0.061(4) 0.069(4) 0.070(6) 0.019(4) -0.002(4) 0.039(4)
C16 0.018(3) 0.046(3) 0.022(3) 0.011(3) 0.009(2) 0.010(2)
C17 0.037(3) 0.049(3) 0.040(4) 0.005(3) -0.003(3) 0.025(3)
C18 0.035(3) 0.067(4) 0.073(6) -0.008(4) 0.002(4) 0.031(3)
C19 0.047(4) 0.057(4) 0.051(5) -0.001(4) -0.016(4) 0.026(3)
C20 0.072(4) 0.048(4) 0.051(4) 0.017(3) 0.008(4) 0.037(3)
C21 0.036(3) 0.045(4) 0.050(4) 0.012(3) 0.021(3) 0.005(3)
C22 0.062(4) 0.059(5) 0.047(4) 0.005(4) 0.029(4) 0.000(4)
C23 0.043(4) 0.051(4) 0.065(5) 0.018(4) 0.018(4) -0.002(4)
C24 0.059(5) 0.066(4) 0.050(4) 0.034(4) 0.014(4) 0.015(4)
C25 0.040(3) 0.033(3) 0.044(4) 0.006(3) 0.016(3) 0.019(3)
C26 0.080(4) 0.062(4) 0.056(4) 0.021(3) 0.048(3) 0.039(3)
C27 0.040(3) 0.050(4) 0.066(5) 0.003(3) 0.019(3) 0.026(3)
C28 0.061(4) 0.036(3) 0.063(5) 0.002(3) 0.019(4) 0.028(3)
C29 0.043(3) 0.042(3) 0.069(5) 0.018(3) 0.007(3) 0.026(3)
C30 0.069(5) 0.070(5) 0.059(5) 0.009(4) -0.007(4) 0.033(4)
C31 0.039(4) 0.050(4) 0.104(7) 0.023(4) 0.005(4) 0.024(3)
C32 0.068(5) 0.071(5) 0.095(7) 0.024(5) -0.013(5) 0.033(4)
C33 0.049(3) 0.042(4) 0.079(5) 0.004(3) 0.029(4) 0.026(3)
C34 0.098(5) 0.073(6) 0.077(6) -0.012(5) 0.047(5) 0.032(5)
C35 0.082(5) 0.080(5) 0.139(9) 0.011(6) 0.053(5) 0.050(4)
C36 0.099(5) 0.036(4) 0.148(9) 0.012(5) 0.050(6) 0.040(4)
C37 0.045(3) 0.036(3) 0.062(4) 0.018(3) 0.028(3) 0.019(3)
C38 0.032(3) 0.045(4) 0.078(6) 0.000(4) 0.012(4) 0.008(3)
C39 0.069(4) 0.066(4) 0.088(6) 0.037(4) 0.037(4) 0.037(4)
C40 0.045(3) 0.052(4) 0.061(4) 0.015(3) 0.028(3) 0.024(3)
C42 0.054(4) 0.089(5) 0.066(5) 0.014(4) 0.030(4) 0.039(4)

_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
Re1 C1 1.926(8) . ?
Re1 C2 1.958(7) . ?
Re1 O3 2.032(5) . ?
Re1 C3 2.077(6) . ?
Re1 C16 2.078(5) . ?
Re1 P1 2.486(2) . ?
Si1 O5 1.698(4) . ?
Si1 C12 1.844(9) . ?
Si1 C8 1.888(7) . ?
Si1 C4 1.902(7) . ?
Si2 O7 1.691(4) . ?
Si2 C25 1.919(7) . ?
Si2 C21 1.928(7) . ?
Si2 C17 1.941(7) . ?
Si3 O3 1.637(5) . ?
Si3 C33 1.937(7) . ?
Si3 C29 1.927(6) . ?
Si3 C37 1.943(7) . ?
P1 C41 1.66(2) . ?
P1 C43 1.752(15) . ?
P1 C42 1.802(9) . ?
P1 C43 1.905(14) . ?
P1 C41 1.943(17) . ?
O1 C1 1.150(9) . ?
O2 C2 1.141(8) . ?
O4 C3 1.215(7) . ?
O5 C3 1.339(9) . ?
O6 C16 1.214(8) . ?
O7 C16 1.314(8) . ?
C4 C7 1.526(8) . ?
C4 C6 1.484(10) . ?
C4 C5 1.559(11) . ?
C8 C10 1.490(10) . ?
C8 C11 1.522(9) . ?
C8 C9 1.540(10) . ?
C12 C14 1.484(10) . ?
C12 C15 1.514(9) . ?
C12 C13 1.597(10) . ?
C17 C18 1.523(9) . ?
C17 C20 1.524(8) . ?
C17 C19 1.539(7) . ?
C21 C24 1.524(9) . ?
C21 C22 1.525(9) . ?
C21 C23 1.545(7) . ?
C25 C27 1.532(8) . ?
C25 C26 1.535(8) . ?
C25 C28 1.543(7) . ?
C29 C32 1.529(9) . ?
C29 C31 1.532(8) . ?
C29 C30 1.537(9) . ?
C33 C34 1.527(9) . ?
C33 C35 1.533(9) . ?
C33 C36 1.532(9) . ?
C37 C39 1.526(9) . ?
C37 C40 1.539(9) . ?
C37 C38 1.537(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
C1 Re1 C2 93.7(3) . . ?
C1 Re1 O3 171.5(2) . . ?
C2 Re1 O3 94.6(2) . . ?
C1 Re1 C3 76.0(2) . . ?
C2 Re1 C3 81.1(3) . . ?
O3 Re1 C3 104.0(2) . . ?
C1 Re1 C16 74.8(3) . . ?
C2 Re1 C16 81.2(2) . . ?
O3 Re1 C16 107.9(2) . . ?
C3 Re1 C16 144.5(3) . . ?
C1 Re1 P1 84.8(2) . . ?
C2 Re1 P1 176.82(15) . . ?
O3 Re1 P1 86.93(14) . . ?
C3 Re1 P1 101.23(19) . . ?
C16 Re1 P1 95.68(18) . . ?
O5 Si1 C12 108.6(3) . . ?
O5 Si1 C8 99.6(2) . . ?
C12 Si1 C8 119.0(4) . . ?
O5 Si1 C4 109.2(3) . . ?
C12 Si1 C4 108.5(3) . . ?
C8 Si1 C4 111.3(3) . . ?
O7 Si2 C25 98.8(2) . . ?
O7 Si2 C21 106.1(2) . . ?
C25 Si2 C21 113.1(3) . . ?
O7 Si2 C17 109.6(2) . . ?
C25 Si2 C17 113.8(3) . . ?
C21 Si2 C17 114.0(3) . . ?
O3 Si3 C33 106.5(3) . . ?
O3 Si3 C29 108.4(2) . . ?
C33 Si3 C29 110.5(3) . . ?
O3 Si3 C37 109.5(3) . . ?
C33 Si3 C37 109.9(3) . . ?
C29 Si3 C37 112.0(3) . . ?
C41 P1 C43 79.5(9) . . ?
C41 P1 C42 104.4(8) . . ?
C43 P1 C42 112.9(7) . . ?
C41 P1 C43 102.2(8) . . ?
C43 P1 C43 23.9(7) . . ?
C42 P1 C43 99.8(6) . . ?
C41 P1 C41 18.6(7) . . ?
C43 P1 C41 98.1(8) . . ?
C42 P1 C41 97.6(6) . . ?
C43 P1 C41 120.7(7) . . ?
C41 P1 Re1 120.1(8) . . ?
C43 P1 Re1 118.9(6) . . ?
C42 P1 Re1 115.4(3) . . ?
C43 P1 Re1 112.3(5) . . ?
C41 P1 Re1 110.1(5) . . ?
Si3 O3 Re1 157.4(3) . . ?
C3 O5 Si1 134.1(3) . . ?
C16 O7 Si2 137.3(4) . . ?
O1 C1 Re1 178.9(6) . . ?
O2 C2 Re1 174.0(6) . . ?
O4 C3 O5 125.9(5) . . ?
O4 C3 Re1 108.8(5) . . ?
O5 C3 Re1 125.4(4) . . ?
C7 C4 C6 115.6(6) . . ?
C7 C4 C5 106.2(9) . . ?
C6 C4 C5 88.9(10) . . ?
C7 C4 Si1 112.2(6) . . ?
C6 C4 Si1 120.7(6) . . ?
C5 C4 Si1 109.5(6) . . ?
C10 C8 C11 111.0(8) . . ?
C10 C8 C9 100.7(9) . . ?
C11 C8 C9 103.6(7) . . ?
C10 C8 Si1 115.5(7) . . ?
C11 C8 Si1 116.3(4) . . ?
C9 C8 Si1 107.8(7) . . ?
C14 C12 C15 112.9(9) . . ?
C14 C12 C13 93.1(9) . . ?
C15 C12 C13 104.2(7) . . ?
C14 C12 Si1 115.8(5) . . ?
C15 C12 Si1 116.5(6) . . ?
C13 C12 Si1 110.9(7) . . ?
O6 C16 O7 125.0(5) . . ?
O6 C16 Re1 111.2(4) . . ?
O7 C16 Re1 123.7(4) . . ?
C18 C17 C20 107.5(6) . . ?
C18 C17 C19 107.2(5) . . ?
C20 C17 C19 109.7(6) . . ?
C18 C17 Si2 112.7(5) . . ?
C20 C17 Si2 109.7(4) . . ?
C19 C17 Si2 110.0(5) . . ?
C24 C21 C22 107.7(6) . . ?
C24 C21 C23 107.1(6) . . ?
C22 C21 C23 108.0(6) . . ?
C24 C21 Si2 112.4(5) . . ?
C22 C21 Si2 110.5(5) . . ?
C23 C21 Si2 110.9(5) . . ?
C27 C25 C26 105.0(5) . . ?
C27 C25 C28 108.4(6) . . ?
C26 C25 C28 108.5(5) . . ?
C27 C25 Si2 110.7(4) . . ?
C26 C25 Si2 111.4(5) . . ?
C28 C25 Si2 112.5(5) . . ?
C32 C29 C31 107.0(6) . . ?
C32 C29 C30 107.0(7) . . ?
C31 C29 C30 105.4(6) . . ?
C32 C29 Si3 116.3(4) . . ?
C31 C29 Si3 109.8(5) . . ?
C30 C29 Si3 110.7(5) . . ?
C34 C33 C35 106.8(7) . . ?
C34 C33 C36 108.4(6) . . ?
C35 C33 C36 107.1(7) . . ?
C34 C33 Si3 108.8(6) . . ?
C35 C33 Si3 111.1(5) . . ?
C36 C33 Si3 114.4(6) . . ?
C39 C37 C40 108.5(6) . . ?
C39 C37 C38 108.0(5) . . ?
C40 C37 C38 104.9(6) . . ?
C39 C37 Si3 113.7(5) . . ?
C40 C37 Si3 110.4(4) . . ?
C38 C37 Si3 111.0(5) . . ?

_diffrn_measured_fraction_theta_max    0.992
_diffrn_reflns_theta_full              21.97
_diffrn_measured_fraction_theta_full   0.992
_refine_diff_density_max    3.707
_refine_diff_density_min   -0.901
_refine_diff_density_rms    0.133


data_asv489_3ReCO

_database_code_CSD	173801


_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C37 H81 O4 Re Si3'
_chemical_formula_weight          860.49

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'
'Si'  'Si'   0.0817   0.0704
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Re'  'Re'  -1.0185   7.2310
'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                    8.7010(17)
_cell_length_b                    21.072(4)
_cell_length_c                    24.334(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  93.89(3)
_cell_angle_gamma                 90.00
_cell_volume                      4451.3(15)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        block
_exptl_crystal_colour             green
_exptl_crystal_size_max           0.05
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.284
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1808
_exptl_absorpt_coefficient_mu     2.843
_exptl_absorpt_correction_type    'no correction'
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?

_exptl_special_details
;
due to disorder in the silox group all carbon atoms had to be refined
isotropically.  Attempts to model the disorder failed.
;

_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.94862
_diffrn_radiation_type            ?
_diffrn_radiation_source          'CHESS'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        '10 deg. phi scan'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             9641
_diffrn_reflns_av_R_equivalents   0.0639
_diffrn_reflns_av_sigmaI/netI     0.0605
_diffrn_reflns_limit_h_min        0
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -21
_diffrn_reflns_limit_k_max        21
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          1.62
_diffrn_reflns_theta_max          29.93
_reflns_number_total              5400
_reflns_number_gt                 4992
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        ?
_computing_cell_refinement        DENZO
_computing_data_reduction         DENZO
_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.
;

_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^)+(0.1080P)^2^+166.3736P] 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     riding
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5400
_refine_ls_number_parameters      224
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0956
_refine_ls_R_factor_gt            0.0896
_refine_ls_wR_factor_ref          0.2278
_refine_ls_wR_factor_gt           0.2227
_refine_ls_goodness_of_fit_ref    1.015
_refine_ls_restrained_S_all       1.015
_refine_ls_shift/su_max           0.759
_refine_ls_shift/su_mean          0.066

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
Re1 Re 0.91054(7) 0.72957(2) 0.19554(2) 0.0233(3) Uani 1 1 d . . .
Si1 Si 1.0202(4) 0.71534(17) 0.33633(15) 0.0177(8) Uani 1 1 d . . .
Si2 Si 0.8056(4) 0.59247(16) 0.12177(15) 0.0177(8) Uani 1 1 d . . .
Si3 Si 1.0075(4) 0.86712(16) 0.12564(15) 0.0158(8) Uani 1 1 d . . .
O1 O 0.9681(14) 0.7273(4) 0.2699(4) 0.032(3) Uani 1 1 d . . .
O2 O 0.8808(10) 0.6520(4) 0.1613(3) 0.021(2) Uani 1 1 d . . .
O3 O 0.9839(10) 0.7953(4) 0.1530(3) 0.016(2) Uani 1 1 d . . .
O4 O 0.5806(14) 0.7736(6) 0.2083(6) 0.054(4) Uani 1 1 d . . .
C1 C 0.7115(19) 0.7567(8) 0.2024(7) 0.034(4) Uiso 1 1 d . . .
C2 C 0.9552(17) 0.6305(7) 0.3508(6) 0.029(3) Uiso 1 1 d . . .
C3 C 0.788(3) 0.6196(15) 0.3311(13) 0.112(10) Uiso 1 1 d . . .
H3A H 0.7591 0.5769 0.3396 0.168 Uiso 1 1 calc R . .
H3B H 0.7755 0.6260 0.2920 0.168 Uiso 1 1 calc R . .
H3C H 0.7236 0.6489 0.3491 0.168 Uiso 1 1 calc R . .
C4 C 1.039(3) 0.5832(12) 0.3158(10) 0.075(7) Uiso 1 1 d . . .
H4A H 1.0053 0.5409 0.3234 0.112 Uiso 1 1 calc R . .
H4B H 1.1482 0.5864 0.3245 0.112 Uiso 1 1 calc R . .
H4C H 1.0167 0.5926 0.2775 0.112 Uiso 1 1 calc R . .
C5 C 0.975(3) 0.6094(12) 0.4105(10) 0.084(7) Uiso 1 1 d . . .
H5A H 0.9402 0.5665 0.4135 0.125 Uiso 1 1 calc R . .
H5B H 0.9166 0.6366 0.4328 0.125 Uiso 1 1 calc R . .
H5C H 1.0824 0.6118 0.4229 0.125 Uiso 1 1 calc R . .
C6 C 0.9157(19) 0.7763(7) 0.3780(7) 0.033(4) Uiso 1 1 d . . .
C7 C 0.912(4) 0.8401(15) 0.3582(14) 0.124(11) Uiso 1 1 d . . .
H7A H 0.8591 0.8664 0.3829 0.185 Uiso 1 1 calc R . .
H7B H 0.8597 0.8414 0.3223 0.185 Uiso 1 1 calc R . .
H7C H 1.0157 0.8552 0.3562 0.185 Uiso 1 1 calc R . .
C8 C 0.947(2) 0.7710(9) 0.4397(8) 0.054(5) Uiso 1 1 d . . .
H8A H 0.8909 0.8036 0.4575 0.081 Uiso 1 1 calc R . .
H8B H 1.0550 0.7760 0.4491 0.081 Uiso 1 1 calc R . .
H8C H 0.9137 0.7302 0.4518 0.081 Uiso 1 1 calc R . .
C9 C 0.724(4) 0.7583(16) 0.3762(14) 0.116(11) Uiso 1 1 d . . .
H9A H 0.6712 0.7892 0.3972 0.174 Uiso 1 1 calc R . .
H9B H 0.7104 0.7169 0.3917 0.174 Uiso 1 1 calc R . .
H9C H 0.6812 0.7588 0.3387 0.174 Uiso 1 1 calc R . .
C10 C 1.2378(19) 0.7257(7) 0.3431(7) 0.035(4) Uiso 1 1 d . . .
C11 C 1.321(4) 0.6926(15) 0.3000(13) 0.113(10) Uiso 1 1 d . . .
H11A H 1.4298 0.6999 0.3064 0.169 Uiso 1 1 calc R . .
H11B H 1.2868 0.7088 0.2644 0.169 Uiso 1 1 calc R . .
H11C H 1.3006 0.6479 0.3015 0.169 Uiso 1 1 calc R . .
C12 C 1.282(4) 0.7952(17) 0.3391(16) 0.134(12) Uiso 1 1 d . . .
H12A H 1.3917 0.7992 0.3428 0.202 Uiso 1 1 calc R . .
H12B H 1.2373 0.8185 0.3680 0.202 Uiso 1 1 calc R . .
H12C H 1.2434 0.8117 0.3041 0.202 Uiso 1 1 calc R . .
C13 C 1.303(3) 0.7100(13) 0.3993(10) 0.081(7) Uiso 1 1 d . . .
H13A H 1.4126 0.7159 0.4013 0.122 Uiso 1 1 calc R . .
H13B H 1.2801 0.6666 0.4075 0.122 Uiso 1 1 calc R . .
H13C H 1.2585 0.7372 0.4256 0.122 Uiso 1 1 calc R . .
C14 C 0.9178(15) 0.5172(6) 0.1462(6) 0.022(3) Uiso 1 1 d . . .
C15 C 0.9140(18) 0.4658(7) 0.1006(6) 0.033(4) Uiso 1 1 d . . .
H15A H 0.9703 0.4292 0.1140 0.050 Uiso 1 1 calc R . .
H15B H 0.9601 0.4824 0.0688 0.050 Uiso 1 1 calc R . .
H15C H 0.8091 0.4541 0.0906 0.050 Uiso 1 1 calc R . .
C16 C 0.8560(19) 0.4863(8) 0.1968(6) 0.035(4) Uiso 1 1 d . . .
H16A H 0.9163 0.4494 0.2067 0.052 Uiso 1 1 calc R . .
H16B H 0.7506 0.4741 0.1887 0.052 Uiso 1 1 calc R . .
H16C H 0.8622 0.5159 0.2268 0.052 Uiso 1 1 calc R . .
C17 C 1.0868(17) 0.5330(7) 0.1615(6) 0.030(4) Uiso 1 1 d . . .
H17A H 1.1405 0.4952 0.1736 0.045 Uiso 1 1 calc R . .
H17B H 1.0932 0.5638 0.1906 0.045 Uiso 1 1 calc R . .
H17C H 1.1330 0.5500 0.1299 0.045 Uiso 1 1 calc R . .
C18 C 0.5860(19) 0.5866(8) 0.1299(7) 0.037(4) Uiso 1 1 d . . .
C19 C 0.495(2) 0.6411(8) 0.1011(7) 0.045(4) Uiso 1 1 d . . .
H19A H 0.3868 0.6358 0.1063 0.068 Uiso 1 1 calc R . .
H19B H 0.5105 0.6406 0.0625 0.068 Uiso 1 1 calc R . .
H19C H 0.5292 0.6809 0.1167 0.068 Uiso 1 1 calc R . .
C20 C 0.5548(19) 0.5907(8) 0.1912(7) 0.037(4) Uiso 1 1 d . . .
H20A H 0.4460 0.5879 0.1951 0.055 Uiso 1 1 calc R . .
H20B H 0.5928 0.6304 0.2059 0.055 Uiso 1 1 calc R . .
H20C H 0.6062 0.5564 0.2108 0.055 Uiso 1 1 calc R . .
C21 C 0.523(2) 0.5239(8) 0.1069(7) 0.041(4) Uiso 1 1 d . . .
H21A H 0.4140 0.5219 0.1110 0.062 Uiso 1 1 calc R . .
H21B H 0.5730 0.4894 0.1266 0.062 Uiso 1 1 calc R . .
H21C H 0.5418 0.5209 0.0686 0.062 Uiso 1 1 calc R . .
C22 C 0.8530(15) 0.6165(6) 0.0485(5) 0.020(3) Uiso 1 1 d . . .
C23 C 1.0277(18) 0.6127(8) 0.0409(7) 0.039(4) Uiso 1 1 d . . .
H23A H 1.0471 0.6251 0.0041 0.059 Uiso 1 1 calc R . .
H23B H 1.0627 0.5700 0.0473 0.059 Uiso 1 1 calc R . .
H23C H 1.0818 0.6406 0.0667 0.059 Uiso 1 1 calc R . .
C24 C 0.812(2) 0.6873(8) 0.0392(7) 0.043(4) Uiso 1 1 d . . .
H24A H 0.8341 0.6996 0.0026 0.065 Uiso 1 1 calc R . .
H24B H 0.8710 0.7128 0.0656 0.065 Uiso 1 1 calc R . .
H24C H 0.7038 0.6935 0.0438 0.065 Uiso 1 1 calc R . .
C25 C 0.7655(18) 0.5774(8) 0.0032(7) 0.036(4) Uiso 1 1 d . . .
H25A H 0.7928 0.5918 -0.0322 0.054 Uiso 1 1 calc R . .
H25B H 0.6567 0.5824 0.0060 0.054 Uiso 1 1 calc R . .
H25C H 0.7925 0.5334 0.0076 0.054 Uiso 1 1 calc R . .
C26 C 0.8103(16) 0.8978(7) 0.0973(6) 0.024(3) Uiso 1 1 d . . .
C27 C 0.7176(18) 0.8457(7) 0.0657(7) 0.033(4) Uiso 1 1 d . . .
H27A H 0.6203 0.8626 0.0516 0.050 Uiso 1 1 calc R . .
H27B H 0.7004 0.8109 0.0900 0.050 Uiso 1 1 calc R . .
H27C H 0.7741 0.8310 0.0356 0.050 Uiso 1 1 calc R . .
C28 C 0.7093(19) 0.9207(8) 0.1436(7) 0.038(4) Uiso 1 1 d . . .
H28A H 0.6119 0.9354 0.1275 0.058 Uiso 1 1 calc R . .
H28B H 0.7608 0.9547 0.1636 0.058 Uiso 1 1 calc R . .
H28C H 0.6929 0.8861 0.1682 0.058 Uiso 1 1 calc R . .
C29 C 0.826(2) 0.9550(8) 0.0578(7) 0.044(4) Uiso 1 1 d . . .
H29A H 0.7254 0.9686 0.0439 0.066 Uiso 1 1 calc R . .
H29B H 0.8847 0.9424 0.0276 0.066 Uiso 1 1 calc R . .
H29C H 0.8775 0.9892 0.0775 0.066 Uiso 1 1 calc R . .
C30 C 1.1512(16) 0.8541(6) 0.0697(6) 0.023(3) Uiso 1 1 d . . .
C31 C 1.2758(18) 0.8044(7) 0.0892(7) 0.034(4) Uiso 1 1 d . . .
H31A H 1.3463 0.7986 0.0610 0.051 Uiso 1 1 calc R . .
H31B H 1.2269 0.7648 0.0965 0.051 Uiso 1 1 calc R . .
H31C H 1.3311 0.8193 0.1222 0.051 Uiso 1 1 calc R . .
C32 C 1.0735(19) 0.8283(8) 0.0154(7) 0.039(4) Uiso 1 1 d . . .
H32A H 1.1498 0.8223 -0.0108 0.058 Uiso 1 1 calc R . .
H32B H 0.9976 0.8581 0.0010 0.058 Uiso 1 1 calc R . .
H32C H 1.0248 0.7885 0.0223 0.058 Uiso 1 1 calc R . .
C33 C 1.2328(18) 0.9155(7) 0.0546(7) 0.034(4) Uiso 1 1 d . . .
H33A H 1.3035 0.9067 0.0270 0.051 Uiso 1 1 calc R . .
H33B H 1.2881 0.9325 0.0868 0.051 Uiso 1 1 calc R . .
H33C H 1.1578 0.9459 0.0406 0.051 Uiso 1 1 calc R . .
C34 C 1.0992(16) 0.9177(7) 0.1854(6) 0.027(3) Uiso 1 1 d . . .
C35 C 1.0108(17) 0.9060(7) 0.2370(6) 0.031(4) Uiso 1 1 d . . .
H35A H 1.0561 0.9308 0.2670 0.046 Uiso 1 1 calc R . .
H35B H 1.0162 0.8619 0.2465 0.046 Uiso 1 1 calc R . .
H35C H 0.9051 0.9182 0.2298 0.046 Uiso 1 1 calc R . .
C36 C 1.2660(19) 0.8999(8) 0.2010(7) 0.042(4) Uiso 1 1 d . . .
H36A H 1.3062 0.9268 0.2303 0.063 Uiso 1 1 calc R . .
H36B H 1.3260 0.9052 0.1696 0.063 Uiso 1 1 calc R . .
H36C H 1.2711 0.8564 0.2128 0.063 Uiso 1 1 calc R . .
C37 C 1.090(2) 0.9895(9) 0.1727(8) 0.049(5) Uiso 1 1 d . . .
H37A H 1.1387 1.0127 0.2031 0.073 Uiso 1 1 calc R . .
H37B H 0.9839 1.0020 0.1674 0.073 Uiso 1 1 calc R . .
H37C H 1.1415 0.9983 0.1399 0.073 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
Re1 0.0446(5) 0.0135(4) 0.0112(4) 0.0027(2) -0.0033(3) -0.0098(2)
Si1 0.028(2) 0.0157(19) 0.009(2) 0.0013(14) -0.0034(16) 0.0048(16)
Si2 0.028(2) 0.0088(18) 0.016(2) -0.0039(14) -0.0026(16) -0.0032(15)
Si3 0.024(2) 0.0094(18) 0.014(2) 0.0044(14) 0.0049(16) -0.0047(15)
O1 0.066(8) 0.023(6) 0.006(5) 0.007(4) 0.010(5) -0.002(5)
O2 0.027(5) 0.025(5) 0.010(5) -0.005(4) -0.006(4) -0.013(4)
O3 0.031(5) 0.013(5) 0.007(5) 0.001(4) 0.006(4) -0.010(4)
O4 0.034(7) 0.069(9) 0.059(9) 0.005(6) 0.006(6) 0.004(6)

_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
Re1 O1 1.844(10) . ?
Re1 C1 1.842(17) . ?
Re1 O2 1.844(9) . ?
Re1 O3 1.868(8) . ?
Si1 O1 1.669(10) . ?
Si1 C10 1.902(17) . ?
Si1 C6 1.906(16) . ?
Si1 C2 1.914(15) . ?
Si2 O2 1.687(9) . ?
Si2 C14 1.934(14) . ?
Si2 C22 1.926(14) . ?
Si2 C18 1.939(17) . ?
Si3 O3 1.671(9) . ?
Si3 C26 1.918(14) . ?
Si3 C34 1.930(15) . ?
Si3 C30 1.928(14) . ?
O4 C1 1.21(2) . ?
C2 C5 1.52(3) . ?
C2 C3 1.52(3) . ?
C2 C4 1.53(3) . ?
C6 C7 1.43(3) . ?
C6 C8 1.51(3) . ?
C6 C9 1.71(4) . ?
C10 C12 1.52(4) . ?
C10 C13 1.48(3) . ?
C10 C11 1.49(3) . ?
C14 C16 1.52(2) . ?
C14 C17 1.53(2) . ?
C14 C15 1.55(2) . ?
C18 C20 1.53(2) . ?
C18 C19 1.54(2) . ?
C18 C21 1.52(2) . ?
C22 C24 1.55(2) . ?
C22 C23 1.55(2) . ?
C22 C25 1.54(2) . ?
C26 C27 1.54(2) . ?
C26 C28 1.55(2) . ?
C26 C29 1.55(2) . ?
C30 C33 1.53(2) . ?
C30 C31 1.56(2) . ?
C30 C32 1.54(2) . ?
C34 C36 1.52(2) . ?
C34 C35 1.54(2) . ?
C34 C37 1.54(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Re1 C1 96.5(6) . . ?
O1 Re1 O2 116.1(4) . . ?
C1 Re1 O2 102.2(6) . . ?
O1 Re1 O3 118.9(4) . . ?
C1 Re1 O3 100.3(6) . . ?
O2 Re1 O3 116.7(4) . . ?
O1 Si1 C10 105.6(7) . . ?
O1 Si1 C6 107.8(6) . . ?
C10 Si1 C6 112.6(7) . . ?
O1 Si1 C2 104.8(6) . . ?
C10 Si1 C2 113.4(7) . . ?
C6 Si1 C2 111.9(7) . . ?
O2 Si2 C14 105.4(5) . . ?
O2 Si2 C22 103.5(5) . . ?
C14 Si2 C22 111.4(6) . . ?
O2 Si2 C18 109.6(6) . . ?
C14 Si2 C18 113.4(7) . . ?
C22 Si2 C18 112.7(6) . . ?
O3 Si3 C26 108.5(6) . . ?
O3 Si3 C34 104.8(5) . . ?
C26 Si3 C34 113.5(6) . . ?
O3 Si3 C30 104.8(5) . . ?
C26 Si3 C30 113.6(6) . . ?
C34 Si3 C30 110.8(6) . . ?
Si1 O1 Re1 172.8(6) . . ?
Si2 O2 Re1 162.6(6) . . ?
Si3 O3 Re1 161.4(6) . . ?
O4 C1 Re1 178.1(15) . . ?
C5 C2 C3 107.7(18) . . ?
C5 C2 C4 108.2(16) . . ?
C3 C2 C4 102.0(18) . . ?
C5 C2 Si1 115.7(13) . . ?
C3 C2 Si1 111.9(15) . . ?
C4 C2 Si1 110.3(12) . . ?
C7 C6 C8 113.7(19) . . ?
C7 C6 C9 102(2) . . ?
C8 C6 C9 96.7(17) . . ?
C7 C6 Si1 117.1(18) . . ?
C8 C6 Si1 114.8(12) . . ?
C9 C6 Si1 109.7(14) . . ?
C12 C10 C13 101(2) . . ?
C12 C10 C11 106(2) . . ?
C13 C10 C11 111.8(19) . . ?
C12 C10 Si1 111.0(17) . . ?
C13 C10 Si1 111.7(14) . . ?
C11 C10 Si1 114.6(16) . . ?
C16 C14 C17 106.4(12) . . ?
C16 C14 C15 106.8(12) . . ?
C17 C14 C15 107.5(12) . . ?
C16 C14 Si2 113.6(10) . . ?
C17 C14 Si2 110.7(10) . . ?
C15 C14 Si2 111.5(10) . . ?
C20 C18 C19 106.3(13) . . ?
C20 C18 C21 108.9(14) . . ?
C19 C18 C21 108.5(13) . . ?
C20 C18 Si2 109.7(11) . . ?
C19 C18 Si2 112.9(11) . . ?
C21 C18 Si2 110.5(11) . . ?
C24 C22 C23 104.7(12) . . ?
C24 C22 C25 108.4(12) . . ?
C23 C22 C25 109.3(12) . . ?
C24 C22 Si2 109.0(10) . . ?
C23 C22 Si2 111.7(10) . . ?
C25 C22 Si2 113.3(10) . . ?
C27 C26 C28 106.4(12) . . ?
C27 C26 C29 108.1(12) . . ?
C28 C26 C29 106.6(12) . . ?
C27 C26 Si3 111.5(10) . . ?
C28 C26 Si3 112.4(10) . . ?
C29 C26 Si3 111.7(10) . . ?
C33 C30 C31 108.4(12) . . ?
C33 C30 C32 106.0(12) . . ?
C31 C30 C32 106.2(12) . . ?
C33 C30 Si3 112.5(10) . . ?
C31 C30 Si3 110.6(10) . . ?
C32 C30 Si3 112.8(10) . . ?
C36 C34 C35 106.1(12) . . ?
C36 C34 C37 109.1(13) . . ?
C35 C34 C37 107.2(13) . . ?
C36 C34 Si3 113.0(11) . . ?
C35 C34 Si3 108.9(10) . . ?
C37 C34 Si3 112.2(11) . . ?

_diffrn_measured_fraction_theta_max    0.849
_diffrn_reflns_theta_full              29.93
_diffrn_measured_fraction_theta_full   0.849
_refine_diff_density_max    5.087
_refine_diff_density_min   -3.827
_refine_diff_density_rms    0.235