#Copyright The Royal Society of Chemistry, 1998

#TITLE:
#Preparation, characterization and reactivity of a series of classical and
#non-classical rhenium hydride complexes

#AUTHORS:
#G. Albertin, S. Antoniutti, R. Carballo, S. Garcia-Font n, F. Padoan

#===========================

data_[ReH(CO)4(PPh2OMe)]

_audit_creation_method  SHELXL
_chemical_name_systematic
;
cis-tetracarbonyl-hydride-(diphenyl-methyl-phosphinite)rhenium(I) 
;
_chemical_name_common   ?
_chemical_formula_moiety        ?
_chemical_formula_structural    ?
_chemical_formula_analytical    ?
_chemical_formula_sum   'C17 H14 O5 P Re'
_chemical_formula_weight        515.45
_chemical_melting_point ?
_chemical_compound_source       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'Re' 'Re' -1.0185 7.2310
'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' 'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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'

_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  8.498(7)
_cell_length_b  9.706(8)
_cell_length_c  11.5359(10)
_cell_angle_alpha       83.84(6)
_cell_angle_beta        88.46(6)
_cell_angle_gamma       74.28(8)
_cell_volume    910.7(11)
_cell_formula_units_Z   2
_cell_measurement_temperature   203(2)
_cell_measurement_reflns_used   25
_cell_measurement_theta_min     7
_cell_measurement_theta_max     15

_exptl_crystal_description      prismatic
_exptl_crystal_colour   colourless
_exptl_crystal_size_max 0.60
_exptl_crystal_size_mid 0.50
_exptl_crystal_size_min 0.40
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_diffrn   1.880
_exptl_crystal_density_method   ?
_exptl_crystal_F_000    492
_exptl_absorpt_coefficient_mu   6.781
_exptl_absorpt_correction_type Psi-scan
_exptl_absorpt_correction_T_min 0.5656
_exptl_absorpt_correction_T_max 0.992

_exptl_special_details ?



_diffrn_ambient_temperature     203(2)
_diffrn_radiation_wavelength    0.71073
_diffrn_radiation_type  MoKa
_diffrn_radiation_source        'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite 
_diffrn_measurement_device     'CAD4 Enraf Nonius'
_diffrn_measurement_method      '\w scans'
_diffrn_standards_number        3
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time 3600
_diffrn_standards_decay_%       0
_diffrn_reflns_number   4321
_diffrn_reflns_av_R_equivalents 0.0349
_diffrn_reflns_av_sigmaI/netI   0.0290
_diffrn_reflns_limit_h_min      -1
_diffrn_reflns_limit_h_max      10
_diffrn_reflns_limit_k_min      -11
_diffrn_reflns_limit_k_max      11
_diffrn_reflns_limit_l_min      -14
_diffrn_reflns_limit_l_max      14
_diffrn_reflns_theta_min        3.05
_diffrn_reflns_theta_max        25.94
_reflns_number_total    3563
_reflns_number_observed 3235
_reflns_observed_criterion      >2sigma(I)

_computing_data_collection      'CAD4 Enraf Nonius'
_computing_cell_refinement      'CAD4 Enraf Nonius'
_computing_data_reduction       'HELENA (Spek, 1996)'
_computing_structure_solution   'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics   'ZORTEP (Zsolnai, 1994)'
_computing_publication_material 'SHELXL-93 (Sheldrick, 1993)'

_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed
criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs
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 w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.1029P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary    Patt
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens located
_refine_ls_hydrogen_treatment   ref
_refine_ls_extinction_method    none
_refine_ls_extinction_coef      ?
_refine_ls_number_reflns        3562
_refine_ls_number_parameters    273
_refine_ls_number_restraints    0
_refine_ls_R_factor_all 0.0392
_refine_ls_R_factor_obs 0.0334
_refine_ls_wR_factor_all        0.0862
_refine_ls_wR_factor_obs        0.0828
_refine_ls_goodness_of_fit_all 1.063
_refine_ls_goodness_of_fit_obs 1.077
_refine_ls_restrained_S_all     1.064
_refine_ls_restrained_S_obs     1.077
_refine_ls_shift/esd_max        0.000
_refine_ls_shift/esd_mean       0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re1 Re 0.25383(3) 0.15192(2) 0.12682(2) 0.03608(10) Uani 1 d . . P1 P
0.2625(2) 0.27717(14) 0.29442(12) 0.0310(3) Uani 1 d . . O1 O 0.4588(8)
0.3187(7) -0.0300(5) 0.084(2) Uani 1 d . . O2 O 0.2046(7) -0.0397(5)
-0.0584(5) 0.0656(14) Uani 1 d . . O3 O -0.0828(8) 0.3734(7) 0.0650(6)
0.086(2) Uani 1 d . . O4 O 0.5365(7) -0.0995(6) 0.2370(6) 0.075(2) Uani 1 d
. . O11 O 0.1629(5) 0.2333(4) 0.4072(3) 0.0381(8) Uani 1 d . . C1 C
0.3844(10) 0.2580(8) 0.0285(6) 0.054(2) Uani 1 d . . C2 C 0.2214(8)
0.0343(7) 0.0061(5) 0.0445(13) Uani 1 d . . C3 C 0.0402(8) 0.2958(7)
0.0841(6) 0.053(2) Uani 1 d . . C4 C 0.4370(8) -0.0063(7) 0.1935(6)
0.0475(14) Uani 1 d . . C11 C 0.1640(7) 0.4691(5) 0.2771(5) 0.0348(11) Uani
1 d . . C12 C 0.2461(9) 0.5592(7) 0.2160(6) 0.0489(14) Uani 1 d . . C13 C
0.1715(11) 0.7062(8) 0.2007(7) 0.055(2) Uani 1 d . . C14 C 0.0215(11)
0.7627(7) 0.2401(7) 0.064(2) Uani 1 d . . C15 C -0.0631(10) 0.6748(8)
0.2985(8) 0.071(2) Uani 1 d . . C16 C 0.0096(8) 0.5261(7) 0.3176(7)
0.056(2) Uani 1 d . . C21 C 0.4593(6) 0.2703(6) 0.3568(5) 0.0350(11) Uani 1
d . . C22 C 0.4632(8) 0.3090(7) 0.4686(6) 0.0489(14) Uani 1 d . . C23 C
0.6095(9) 0.3088(8) 0.5172(7) 0.058(2) Uani 1 d . . C24 C 0.7536(9)
0.2712(8) 0.4551(8) 0.059(2) Uani 1 d . . C25 C 0.7513(8) 0.2319(8)
0.3465(7) 0.058(2) Uani 1 d . . C26 C 0.6063(8) 0.2294(8) 0.2960(6)
0.0466(14) Uani 1 d . . C111 C 0.2036(10) 0.0858(7) 0.4577(7) 0.053(2) Uani
1 d . . H1 H 0.1741(95) 0.0450(81) 0.2083(67) 0.060(22) Uiso 1 d . . H12 H
0.3447(91) 0.5169(73) 0.1741(62) 0.051(19) Uiso 1 d . . H13 H 0.2125(112)
0.7443(98) 0.1681(77) 0.068(30) Uiso 1 d . . H14 H -0.0285(99) 0.8690(88)
0.2278(69) 0.072(24) Uiso 1 d . . H15 H -0.1808(100) 0.7002(78) 0.3092(65)
0.059(21) Uiso 1 d . . H16 H -0.0596(94) 0.4717(81) 0.3470(65) 0.057(20)
Uiso 1 d . . H22 H 0.3764(94) 0.3293(74) 0.5156(65) 0.055(20) Uiso 1 d . .
H23 H 0.6176(112) 0.3352(92) 0.5988(83) 0.080(27) Uiso 1 d . . H24 H
0.8213(90) 0.2772(71) 0.4924(60) 0.043(19) Uiso 1 d . . H25 H 0.8331(113)
0.1985(86) 0.3003(76) 0.078(27) Uiso 1 d . . H26 H 0.5897(93) 0.2223(79)
0.2359(66) 0.053(23) Uiso 1 d . . H111 H 0.1795(94) 0.0288(82) 0.4049(67)
0.055(21) Uiso 1 d . . H112 H 0.1437(114) 0.0701(97) 0.5133(84) 0.079(28)
Uiso 1 d . . H113 H 0.3268(118) 0.0428(90) 0.4806(76) 0.078(26) Uiso 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
Re1 0.03434(14) 0.03515(14) 0.03903(15) -0.00668(9) 0.00061(9) -0.00882(9)
P1 0.0260(6) 0.0298(6) 0.0380(7) -0.0030(5) 0.0020(5) -0.0093(5) O1
0.097(5) 0.090(4) 0.074(4) 0.001(3) 0.030(3) -0.049(4) O2 0.080(4) 0.058(3)
0.060(3) -0.020(2) -0.014(3) -0.014(3) O3 0.061(4) 0.089(4) 0.091(4)
-0.024(3) -0.022(3) 0.017(3) O4 0.060(3) 0.059(3) 0.087(4) -0.001(3)
-0.009(3) 0.012(3) O11 0.033(2) 0.035(2) 0.044(2) 0.000(2) 0.009(2)
-0.010(2) C1 0.066(4) 0.048(3) 0.051(4) -0.011(3) 0.004(3) -0.017(3) C2
0.053(4) 0.047(3) 0.034(3) -0.009(2) -0.003(3) -0.011(3) C3 0.048(4)
0.052(4) 0.057(4) -0.012(3) -0.006(3) -0.007(3) C4 0.045(3) 0.047(3)
0.050(3) -0.011(3) 0.004(3) -0.009(3) C11 0.036(3) 0.030(2) 0.038(3)
-0.004(2) -0.004(2) -0.008(2) C12 0.054(4) 0.050(3) 0.044(3) 0.002(3)
0.004(3) -0.020(3) C13 0.080(5) 0.040(3) 0.047(4) 0.006(3) -0.006(4)
-0.023(4) C14 0.089(6) 0.036(3) 0.057(4) -0.001(3) -0.013(4) -0.002(3) C15
0.054(5) 0.054(4) 0.092(6) -0.007(4) 0.011(4) 0.007(3) C16 0.042(3)
0.042(3) 0.079(5) 0.003(3) 0.014(3) -0.006(3) C21 0.026(3) 0.039(3)
0.041(3) -0.002(2) 0.000(2) -0.012(2) C22 0.043(3) 0.057(4) 0.049(4)
-0.008(3) 0.000(3) -0.016(3) C23 0.058(4) 0.061(4) 0.060(4) -0.006(3)
-0.015(3) -0.021(3) C24 0.041(4) 0.062(4) 0.078(5) 0.003(4) -0.018(4)
-0.023(3) C25 0.022(3) 0.072(4) 0.076(5) 0.004(4) 0.005(3) -0.010(3) C26
0.037(3) 0.061(4) 0.045(4) -0.005(3) 0.006(3) -0.020(3) C111 0.054(4)
0.044(3) 0.060(4) 0.011(3) 0.002(3) -0.020(3)

_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 H1 1.60(8) . y
Re1 C2 1.962(6) . y
Re1 C1 1.970(8) . y
Re1 C4 1.972(7) . y
Re1 C3 2.004(7) . y
Re1 P1 2.405(2) . y
P1 O11 1.614(4) . y
P1 C11 1.815(5) . y
P1 C21 1.820(6) . y
O1 C1 1.137(9) . y
O2 C2 1.125(8) . y
O3 C3 1.122(9) . y
O4 C4 1.139(8) . y
O11 C111 1.440(7) . y
C11 C16 1.369(9) . ?
C11 C12 1.385(8) . ?
C12 C13 1.390(10) . ?
C12 H12 0.97(7) . ?
C13 C14 1.333(12) . ?
C13 H13 0.66(9) . ?
C14 C15 1.372(12) . ?
C14 H14 1.00(8) . ?
C15 C16 1.403(10) . ?
C15 H15 0.97(8) . ?
C16 H16 0.93(8) . ?
C21 C22 1.385(9) . ?
C21 C26 1.398(9) . ?
C22 C23 1.378(10) . ?
C22 H22 0.89(8) . ?
C23 C24 1.383(12) . ?
C23 H23 1.01(9) . ?
C24 C25 1.351(12) . ?
C24 H24 0.75(7) . ?
C25 C26 1.384(10) . ?
C25 H25 0.88(9) . ?
C26 H26 0.73(7) . ?
C111 H111 0.93(8) . ?
C111 H112 0.83(10) . ?
C111 H113 1.05(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1 Re1 C2 82.5(28) . . y
H1 Re1 C1 170.8(27) . . y
C2 Re1 C1 95.5(3) . . y
H1 Re1 C4 73.6(27) . . y
C2 Re1 C4 90.6(3) . . y
C1 Re1 C4 97.5(3) . . y
H1 Re1 C3 94.8(27) . . y
C2 Re1 C3 90.4(3) . . y
C1 Re1 C3 94.2(3) . . y
C4 Re1 C3 168.1(3) . . y
H1 Re1 P1 88.0(28) . . y
C2 Re1 P1 170.2(2) . . y
C1 Re1 P1 94.3(2) . . y
C4 Re1 P1 89.0(2) . . y
C3 Re1 P1 88.0(2) . . y
C2 Re1 H1 82.5(28) . . ?
C1 Re1 H1 170.8(27) . . ?
C4 Re1 H1 73.6(27) . . ?
C3 Re1 H1 94.8(27) . . ?
P1 Re1 H1 88.0(28) . . ?
O11 P1 C11 98.5(2) . . ?
O11 P1 C21 102.3(2) . . ?
C11 P1 C21 102.0(3) . . ?
O11 P1 Re1 115.8(2) . . ?
C11 P1 Re1 115.7(2) . . ?
C21 P1 Re1 119.4(2) . . ?
C111 O11 P1 119.3(4) . . ?
O1 C1 Re1 178.8(7) . . ?
O2 C2 Re1 176.0(6) . . ?
O3 C3 Re1 176.4(7) . . ?
O4 C4 Re1 175.9(6) . . ?
C16 C11 C12 119.4(5) . . ?
C16 C11 P1 122.2(5) . . ?
C12 C11 P1 118.3(5) . . ?
C11 C12 C13 119.0(7) . . ?
C11 C12 H12 118.9(41) . . ?
C13 C12 H12 121.2(40) . . ?
C14 C13 C12 122.0(7) . . ?
C14 C13 H13 122.8(84) . . ?
C12 C13 H13 115.0(84) . . ?
C13 C14 C15 119.8(7) . . ?
C13 C14 H14 120.0(48) . . ?
C15 C14 H14 120.2(48) . . ?
C14 C15 C16 119.8(7) . . ?
C14 C15 H15 124.8(43) . . ?
C16 C15 H15 113.0(45) . . ?
C11 C16 C15 120.0(7) . . ?
C11 C16 H16 124.2(47) . . ?
C15 C16 H16 115.1(47) . . ?
C22 C21 C26 118.7(6) . . ?
C22 C21 P1 118.6(4) . . ?
C26 C21 P1 122.7(5) . . ?
C23 C22 C21 120.1(7) . . ?
C23 C22 H22 115.3(49) . . ?
C21 C22 H22 124.4(49) . . ?
C22 C23 C24 120.6(7) . . ?
C22 C23 H23 122.5(54) . . ?
C24 C23 H23 116.9(54) . . ?
C25 C24 C23 119.7(7) . . ?
C25 C24 H24 132.2(56) . . ?
C23 C24 H24 108.0(56) . . ?
C24 C25 C26 120.9(7) . . ?
C24 C25 H25 129.4(61) . . ?
C26 C25 H25 109.5(61) . . ?
C25 C26 C21 120.0(7) . . ?
C25 C26 H26 129.2(63) . . ?
C21 C26 H26 109.8(62) . . ?
O11 C111 H111 109.4(45) . . ?
O11 C111 H112 114.1(63) . . ?
H111 C111 H112 100.4(75) . . ?
O11 C111 H113 114.3(47) . . ?
H111 C111 H113 107.1(66) . . ?
H112 C111 H113 110.4(77) . . ?

_refine_diff_density_max 2.048
_refine_diff_density_min -1.492
_refine_diff_density_rms 0.150

#=======END

data_[ReH(CO)3(PPh2OMe)2]

_audit_creation_method  SHELXL
_chemical_name_systematic
;
mer,trans-tricarbonyl-hydride-bis(diphenyl-methyl-phosphinite)rhenium(I) 
;
_chemical_name_common   ?
_chemical_formula_moiety        ?
_chemical_formula_structural    ?
_chemical_formula_analytical    ?
_chemical_formula_sum   'C29 H27 O5 P2 Re'
_chemical_formula_weight        703.65
_chemical_melting_point ?
_chemical_compound_source       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' .0033 .0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .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  monoclinic
_symmetry_space_group_name_H-M P2(1)/c

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

_cell_length_a  8.629(2)
_cell_length_b  30.720(11)
_cell_length_c  10.617(2)
_cell_angle_alpha       90.00
_cell_angle_beta        91.290(10)
_cell_angle_gamma       90.00
_cell_volume    2813.7(13)
_cell_formula_units_Z   4
_cell_measurement_temperature   203(2)
_cell_measurement_reflns_used   25
_cell_measurement_theta_min     9
_cell_measurement_theta_max     13

_exptl_crystal_description      prismatic
_exptl_crystal_colour   colourless
_exptl_crystal_size_max 0.50
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas     'not measured'
_exptl_crystal_density_diffrn   1.661
_exptl_crystal_density_method   ?
_exptl_crystal_F_000    1384
_exptl_absorpt_coefficient_mu   4.469
_exptl_absorpt_correction_type Psi-scans 
_exptl_absorpt_correction_T_min 0.892
_exptl_absorpt_correction_T_max 0.999

_exptl_special_details
;
?
;

_diffrn_ambient_temperature     203(2)
_diffrn_radiation_wavelength    0.71073
_diffrn_radiation_type  MoKa
_diffrn_radiation_source        'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite 
_diffrn_measurement_device     'CAD4 Enraf-Nonius'
_diffrn_measurement_method      '\w scans'
_diffrn_standards_number        3
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time 3600
_diffrn_standards_decay_%       0
_diffrn_reflns_number   7309
_diffrn_reflns_av_R_equivalents 0.0238
_diffrn_reflns_av_sigmaI/netI   0.0501
_diffrn_reflns_limit_h_min      -1
_diffrn_reflns_limit_h_max      10
_diffrn_reflns_limit_k_min      0
_diffrn_reflns_limit_k_max      39
_diffrn_reflns_limit_l_min      -13
_diffrn_reflns_limit_l_max      13
_diffrn_reflns_theta_min        3.08
_diffrn_reflns_theta_max        26.94
_reflns_number_total    6085
_reflns_number_observed 4531
_reflns_observed_criterion      >2sigma(I)

_computing_data_collection      'CAD4 Enraf Nonius'
_computing_cell_refinement      'CAD4 Enraf Nonius'
_computing_data_reduction       'HELENA (Spek, 1996)'
_computing_structure_solution   'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics   'ZORTEP (Zsolnai, 1994)'
_computing_publication_material 'SHELXL-93 (Sheldrick, 1993)'

_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses 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 observed
criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs
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 w=1/[s^2^(Fo^2^)+( 0.0291P)^2^+1.2374P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary    direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens located
_refine_ls_hydrogen_treatment   ref
_refine_ls_extinction_method    none
_refine_ls_extinction_coef      ?
_refine_ls_number_reflns        6081
_refine_ls_number_parameters    442
_refine_ls_number_restraints    0
_refine_ls_R_factor_all 0.0656
_refine_ls_R_factor_obs 0.0329
_refine_ls_wR_factor_all        0.0754
_refine_ls_wR_factor_obs        0.0597
_refine_ls_goodness_of_fit_all 1.075
_refine_ls_goodness_of_fit_obs 1.001
_refine_ls_restrained_S_all     1.078
_refine_ls_restrained_S_obs     1.001
_refine_ls_shift/esd_max        -0.091
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Re Re 0.17094(2) 0.114153(6) 0.09655(2) 0.03186(7) Uani 1 d . . H1 H
0.0959(79) 0.1495(21) 0.2019(60) 0.093(23) Uiso 1 d . . C1 C 0.3225(7)
0.1573(2) 0.0366(5) 0.0427(13) Uani 1 d . . O1 O 0.4074(5) 0.18221(14)
0.0009(4) 0.0652(13) Uani 1 d . . C2 C 0.2337(7) 0.0702(2) -0.0238(5)
0.0455(14) Uani 1 d . . O2 O 0.2664(6) 0.0435(2) -0.0944(4) 0.0732(14) Uani
1 d . . C3 C 0.0160(7) 0.0745(2) 0.1661(6) 0.052(2) Uani 1 d . . O3 O
-0.0729(6) 0.0519(2) 0.2076(5) 0.094(2) Uani 1 d . . P1 P -0.0177(2)
0.14655(4) -0.04059(12) 0.0335(3) Uani 1 d . . O10 O -0.1246(5) 0.18470(11)
0.0171(3) 0.0446(9) Uani 1 d . . C10 C -0.2153(10) 0.1752(3) 0.1238(8)
0.063(2) Uani 1 d . . C11 C -0.1638(6) 0.1121(2) -0.1183(5) 0.0410(12) Uani
1 d . . C12 C -0.1533(8) 0.0672(2) -0.1212(6) 0.0468(15) Uani 1 d . . C13 C
-0.2648(10) 0.0425(2) -0.1798(7) 0.063(2) Uani 1 d . . C14 C -0.3901(8)
0.0612(3) -0.2381(7) 0.062(2) Uani 1 d . . C15 C -0.4032(9) 0.1058(3)
-0.2372(7) 0.073(2) Uani 1 d . . C16 C -0.2907(9) 0.1310(3) -0.1772(7)
0.060(2) Uani 1 d . . C21 C 0.0590(6) 0.1772(2) -0.1718(5) 0.0367(12) Uani
1 d . . C22 C 0.1593(8) 0.1569(2) -0.2529(6) 0.057(2) Uani 1 d . . C23 C
0.2233(10) 0.1794(2) -0.3521(6) 0.069(2) Uani 1 d . . C24 C 0.1848(9)
0.2215(2) -0.3742(7) 0.066(2) Uani 1 d . . C25 C 0.0858(10) 0.2419(3)
-0.2962(8) 0.077(2) Uani 1 d . . C26 C 0.0220(8) 0.2204(2) -0.1939(7)
0.056(2) Uani 1 d . . P2 P 0.3415(2) 0.09519(4) 0.26717(12) 0.0340(3) Uani
1 d . . O20 O 0.4683(4) 0.05703(12) 0.2465(3) 0.0438(9) Uani 1 d . . C20 C
0.5616(9) 0.0568(3) 0.1360(8) 0.060(2) Uani 1 d . . C31 C 0.4615(7)
0.1386(2) 0.3375(5) 0.0400(13) Uani 1 d . . C32 C 0.4199(9) 0.1818(2)
0.3288(6) 0.053(2) Uani 1 d . . C33 C 0.5121(11) 0.2137(2) 0.3854(7)
0.067(2) Uani 1 d . . C34 C 0.6432(10) 0.2030(3) 0.4501(7) 0.073(2) Uani 1
d . . C35 C 0.6853(10) 0.1604(3) 0.4604(7) 0.075(2) Uani 1 d . . C36 C
0.5969(9) 0.1282(2) 0.4049(7) 0.059(2) Uani 1 d . . C41 C 0.2504(7)
0.0719(2) 0.4046(5) 0.0375(12) Uani 1 d . . C42 C 0.1180(8) 0.0902(2)
0.4510(6) 0.055(2) Uani 1 d . . C43 C 0.0449(10) 0.0727(3) 0.5529(7)
0.066(2) Uani 1 d . . C44 C 0.2339(10) 0.0174(2) 0.5659(6) 0.058(2) Uani 1
d . . C45 C 0.1043(9) 0.0359(2) 0.6104(6) 0.058(2) Uani 1 d . . C46 C
0.3089(8) 0.0347(2) 0.4631(6) 0.0488(15) Uani 1 d . . H12 H -0.0778(65)
0.0553(17) -0.0859(50) 0.040(18) Uiso 1 d . . H13 H -0.2524(76) 0.0164(19)
-0.1837(58) 0.060(22) Uiso 1 d . . H14 H -0.4720(91) 0.0406(25) -0.2800(69)
0.104(27) Uiso 1 d . . H15 H -0.4875(76) 0.1189(18) -0.2683(56) 0.053(18)
Uiso 1 d . . H16 H -0.3028(73) 0.1558(19) -0.1770(57) 0.051(21) Uiso 1 d .
. H22 H 0.1957(74) 0.1273(20) -0.2403(58) 0.066(20) Uiso 1 d . . H23 H
0.2841(78) 0.1662(21) -0.4074(60) 0.071(22) Uiso 1 d . . H24 H 0.2296(78)
0.2376(21) -0.4425(61) 0.077(22) Uiso 1 d . . H25 H 0.0662(100) 0.2695(27)
-0.3026(77) 0.116(32) Uiso 1 d . . H26 H -0.0515(83) 0.2335(21) -0.1480(63)
0.077(23) Uiso 1 d . . H32 H 0.3385(68) 0.1900(18) 0.2859(51) 0.042(18)
Uiso 1 d . . H33 H 0.4771(67) 0.2412(19) 0.3726(51) 0.047(17) Uiso 1 d . .
H34 H 0.6940(90) 0.2240(23) 0.4891(68) 0.091(26) Uiso 1 d . . H35 H
0.7930(98) 0.1546(25) 0.5049(74) 0.111(29) Uiso 1 d . . H36 H 0.6239(72)
0.0982(20) 0.4084(57) 0.061(19) Uiso 1 d . . H42 H 0.0840(82) 0.1162(20)
0.4112(66) 0.078(22) Uiso 1 d . . H43 H -0.0365(74) 0.0829(20) 0.5742(60)
0.056(21) Uiso 1 d . . H44 H 0.2742(87) -0.0043(23) 0.5996(66) 0.082(25)
Uiso 1 d . . H45 H 0.0533(64) 0.0237(17) 0.6751(52) 0.047(16) Uiso 1 d . .
H46 H 0.4116(61) 0.0231(15) 0.4347(45) 0.037(14) Uiso 1 d . . H10A H
-0.2651(74) 0.2012(20) 0.1468(58) 0.061(19) Uiso 1 d . . H10B H -0.1636(75)
0.1724(20) 0.1951(60) 0.058(22) Uiso 1 d . . H10C H -0.3092(101) 0.1524(29)
0.1055(72) 0.121(32) Uiso 1 d . . H20A H 0.6258(80) 0.0368(22) 0.1504(61)
0.065(22) Uiso 1 d . . H20B H 0.5055(114) 0.0691(31) 0.0577(91) 0.147(39)
Uiso 1 d . . H20C H 0.6199(129) 0.0842(38) 0.1383(103) 0.167(48) Uiso 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
Re 0.03710(12) 0.02816(10) 0.03034(10) 0.00511(9) 0.00145(7) -0.00083(11)
C1 0.043(3) 0.043(3) 0.042(3) 0.009(3) -0.001(3) 0.003(3) O1 0.057(3)
0.064(3) 0.075(3) 0.022(2) 0.009(2) -0.021(2) C2 0.048(4) 0.041(3) 0.047(3)
0.002(3) -0.004(3) 0.007(3) O2 0.080(3) 0.065(3) 0.075(3) -0.029(3)
-0.008(3) 0.018(3) C3 0.045(4) 0.058(4) 0.053(4) 0.026(3) -0.014(3)
-0.006(3) O3 0.072(4) 0.113(4) 0.098(4) 0.070(3) -0.019(3) -0.048(3) P1
0.0390(8) 0.0299(6) 0.0316(7) 0.0040(5) 0.0021(6) 0.0031(6) O10 0.052(2)
0.039(2) 0.043(2) 0.000(2) 0.013(2) 0.013(2) C10 0.053(5) 0.078(5) 0.059(5)
-0.006(4) 0.021(4) 0.010(4) C11 0.042(3) 0.046(3) 0.036(3) 0.001(3)
0.001(2) 0.004(3) C12 0.053(4) 0.041(3) 0.046(4) -0.005(3) -0.006(3)
-0.003(3) C13 0.075(5) 0.053(4) 0.061(4) -0.009(4) 0.004(4) -0.013(4) C14
0.052(4) 0.073(5) 0.059(4) -0.009(4) -0.005(3) -0.014(4) C15 0.047(4)
0.100(6) 0.070(5) 0.002(4) -0.021(4) 0.004(4) C16 0.056(4) 0.058(4)
0.065(5) 0.004(4) -0.012(4) 0.004(4) C21 0.042(3) 0.034(3) 0.034(3)
0.010(2) -0.002(2) -0.005(2) C22 0.083(5) 0.043(3) 0.046(3) 0.012(3)
0.021(3) 0.013(3) C23 0.094(6) 0.067(5) 0.047(4) 0.010(3) 0.031(4) 0.000(4)
C24 0.081(5) 0.063(4) 0.054(4) 0.025(3) 0.009(4) -0.011(4) C25 0.089(6)
0.051(4) 0.092(6) 0.034(4) 0.016(5) 0.008(4) C26 0.059(4) 0.041(3) 0.069(4)
0.015(3) 0.015(4) 0.009(3) P2 0.0401(8) 0.0307(6) 0.0312(7) 0.0023(5)
0.0024(6) 0.0023(6) O20 0.045(2) 0.044(2) 0.042(2) 0.002(2) 0.003(2)
0.011(2) C20 0.056(5) 0.066(5) 0.059(4) 0.007(4) 0.016(4) 0.022(4) C31
0.041(3) 0.043(3) 0.036(3) -0.001(2) 0.003(3) -0.008(3) C32 0.058(4)
0.049(4) 0.051(4) -0.011(3) 0.008(3) -0.005(3) C33 0.087(6) 0.047(4)
0.068(5) -0.016(3) 0.024(4) -0.015(4) C34 0.071(6) 0.086(6) 0.063(5)
-0.031(4) 0.008(4) -0.039(5) C35 0.068(5) 0.087(6) 0.070(5) -0.009(4)
-0.016(4) -0.023(5) C36 0.062(5) 0.056(4) 0.059(4) -0.002(3) -0.006(4)
-0.003(3) C41 0.045(3) 0.038(3) 0.030(3) -0.001(2) 0.002(2) -0.002(2) C42
0.066(5) 0.053(4) 0.046(4) 0.014(3) 0.007(3) 0.014(3) C43 0.068(5) 0.077(5)
0.056(4) 0.006(4) 0.023(4) 0.003(4) C44 0.073(5) 0.054(4) 0.047(4) 0.017(3)
-0.004(4) -0.009(4) C45 0.074(5) 0.066(4) 0.033(3) 0.015(3) 0.009(3)
-0.009(4) C46 0.055(4) 0.048(3) 0.044(3) 0.011(3) 0.001(3) 0.002(3)

_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
Re H1 1.70(6) . y
Re C2 1.943(6) . y
Re C3 1.966(6) . y
Re C1 1.977(6) . y
Re P1 2.3775(14) . y
Re P2 2.3804(14) . y
C1 O1 1.131(6) . y
C2 O2 1.152(6) . y
C3 O3 1.131(7) . y
P1 O10 1.620(4) . y
P1 C21 1.818(5) . y
P1 C11 1.828(6) . y
O10 C10 1.422(8) . y
C10 H10A 0.94(6) . ?
C10 H10B 0.87(6) . ?
C10 H10C 1.08(9) . ?
C11 C16 1.376(9) . ?
C11 C12 1.383(8) . ?
C12 C13 1.365(9) . ?
C12 H12 0.83(5) . ?
C13 C14 1.362(10) . ?
C13 H13 0.81(6) . ?
C14 C15 1.374(10) . ?
C14 H14 1.04(8) . ?
C15 C16 1.386(10) . ?
C15 H15 0.89(6) . ?
C16 H16 0.77(6) . ?
C21 C22 1.384(8) . ?
C21 C26 1.385(7) . ?
C22 C23 1.386(8) . ?
C22 H22 0.97(6) . ?
C23 C24 1.354(10) . ?
C23 H23 0.89(6) . ?
C24 C25 1.356(10) . ?
C24 H24 0.97(6) . ?
C25 C26 1.395(9) . ?
C25 H25 0.87(8) . ?
C26 H26 0.90(7) . ?
P2 O20 1.622(4) . y
P2 C41 1.820(5) . y
P2 C31 1.837(6) . y
O20 C20 1.438(8) . y
C20 H20A 0.84(7) . ?
C20 H20B 1.02(10) . ?
C20 H20C 0.98(12) . ?
C31 C32 1.379(8) . ?
C31 C36 1.393(9) . ?
C32 C33 1.391(9) . ?
C32 H32 0.87(5) . ?
C33 C34 1.351(11) . ?
C33 H33 0.91(5) . ?
C34 C35 1.361(11) . ?
C34 H34 0.88(7) . ?
C35 C36 1.375(9) . ?
C35 H35 1.05(8) . ?
C36 H36 0.95(6) . ?
C41 C42 1.375(8) . ?
C41 C46 1.390(7) . ?
C42 C43 1.374(9) . ?
C42 H42 0.95(6) . ?
C43 C45 1.380(10) . ?
C43 H43 0.81(6) . ?
C44 C45 1.348(10) . ?
C44 C46 1.386(9) . ?
C44 H44 0.83(7) . ?
C45 H45 0.91(6) . ?
C46 H46 1.01(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
H1 Re C2 173.3(23) . . y
H1 Re C3 82.9(23) . . y
C2 Re C3 91.0(3) . . y
H1 Re C1 92.8(23) . . y
C2 Re C1 93.3(2) . . y
C3 Re C1 175.6(3) . . y
H1 Re P1 82.5(22) . . y
C2 Re P1 94.9(2) . . y
C3 Re P1 91.6(2) . . y
C1 Re P1 88.3(2) . . y
H1 Re P2 83.9(22) . . y
C2 Re P2 98.8(2) . . y
C3 Re P2 88.6(2) . . y
C1 Re P2 90.4(2) . . y
P1 Re P2 166.27(5) . . y
H1 Re H1 0.0(63) . . ?
C2 Re H1 173.3(23) . . ?
C3 Re H1 82.9(23) . . ?
C1 Re H1 92.8(23) . . ?
P1 Re H1 82.5(22) . . ?
P2 Re H1 83.9(22) . . ?
O1 C1 Re 178.9(5) . . ?
O2 C2 Re 177.8(6) . . ?
O3 C3 Re 179.1(6) . . ?
O10 P1 C21 97.8(2) . . ?
O10 P1 C11 101.3(2) . . ?
C21 P1 C11 102.3(2) . . ?
O10 P1 Re 117.3(2) . . ?
C21 P1 Re 115.5(2) . . ?
C11 P1 Re 119.3(2) . . ?
C10 O10 P1 118.8(4) . . ?
O10 C10 H10A 107.2(38) . . ?
O10 C10 H10B 115.5(43) . . ?
H10A C10 H10B 94.9(53) . . ?
O10 C10 H10C 114.3(42) . . ?
H10A C10 H10C 104.4(57) . . ?
H10B C10 H10C 117.2(61) . . ?
C16 C11 C12 117.5(6) . . ?
C16 C11 P1 119.7(5) . . ?
C12 C11 P1 122.8(5) . . ?
C13 C12 C11 121.3(7) . . ?
C13 C12 H12 120.0(39) . . ?
C11 C12 H12 118.7(39) . . ?
C14 C13 C12 121.0(7) . . ?
C14 C13 H13 120.0(49) . . ?
C12 C13 H13 118.8(49) . . ?
C13 C14 C15 118.9(7) . . ?
C13 C14 H14 117.5(42) . . ?
C15 C14 H14 123.6(42) . . ?
C14 C15 C16 120.2(7) . . ?
C14 C15 H15 121.1(40) . . ?
C16 C15 H15 118.5(41) . . ?
C11 C16 C15 121.0(7) . . ?
C11 C16 H16 121.5(50) . . ?
C15 C16 H16 117.4(50) . . ?
C22 C21 C26 118.2(5) . . ?
C22 C21 P1 119.1(4) . . ?
C26 C21 P1 122.7(5) . . ?
C21 C22 C23 120.9(6) . . ?
C21 C22 H22 122.8(38) . . ?
C23 C22 H22 116.1(38) . . ?
C24 C23 C22 120.5(7) . . ?
C24 C23 H23 117.6(42) . . ?
C22 C23 H23 121.6(43) . . ?
C23 C24 C25 119.5(6) . . ?
C23 C24 H24 121.2(41) . . ?
C25 C24 H24 119.3(41) . . ?
C24 C25 C26 121.4(7) . . ?
C24 C25 H25 122.0(57) . . ?
C26 C25 H25 116.3(58) . . ?
C21 C26 C25 119.5(7) . . ?
C21 C26 H26 119.8(44) . . ?
C25 C26 H26 120.4(44) . . ?
O20 P2 C41 97.4(2) . . ?
O20 P2 C31 101.7(2) . . ?
C41 P2 C31 102.1(2) . . ?
O20 P2 Re 118.79(15) . . ?
C41 P2 Re 115.8(2) . . ?
C31 P2 Re 117.7(2) . . ?
C20 O20 P2 120.4(4) . . ?
O20 C20 H20A 103.5(47) . . ?
O20 C20 H20B 113.4(53) . . ?
H20A C20 H20B 135.7(68) . . ?
O20 C20 H20C 105.8(64) . . ?
H20A C20 H20C 106.7(75) . . ?
H20B C20 H20C 86.3(71) . . ?
C32 C31 C36 118.0(6) . . ?
C32 C31 P2 121.9(5) . . ?
C36 C31 P2 120.1(5) . . ?
C31 C32 C33 120.3(7) . . ?
C31 C32 H32 121.4(38) . . ?
C33 C32 H32 118.3(39) . . ?
C34 C33 C32 120.8(7) . . ?
C34 C33 H33 125.2(39) . . ?
C32 C33 H33 114.0(39) . . ?
C33 C34 C35 119.6(7) . . ?
C33 C34 H34 117.7(51) . . ?
C35 C34 H34 122.6(51) . . ?
C34 C35 C36 120.9(8) . . ?
C34 C35 H35 115.7(44) . . ?
C36 C35 H35 123.1(45) . . ?
C35 C36 C31 120.4(7) . . ?
C35 C36 H36 123.2(40) . . ?
C31 C36 H36 116.4(40) . . ?
C42 C41 C46 118.3(5) . . ?
C42 C41 P2 120.2(4) . . ?
C46 C41 P2 121.5(4) . . ?
C43 C42 C41 121.4(6) . . ?
C43 C42 H42 122.6(44) . . ?
C41 C42 H42 115.9(43) . . ?
C42 C43 C45 119.8(7) . . ?
C42 C43 H43 119.2(48) . . ?
C45 C43 H43 120.8(47) . . ?
C45 C44 C46 121.4(7) . . ?
C45 C44 H44 122.0(52) . . ?
C46 C44 H44 116.6(53) . . ?
C44 C45 C43 119.5(6) . . ?
C44 C45 H45 120.9(36) . . ?
C43 C45 H45 119.6(36) . . ?
C44 C46 C41 119.6(6) . . ?
C44 C46 H46 122.0(28) . . ?
C41 C46 H46 118.0(28) . . ?

_refine_diff_density_max        .588
_refine_diff_density_min -.527
_refine_diff_density_rms        .121