#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:05:44 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178884 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/13/4111385.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_4111385
loop_
_publ_author_name
'Richard D. Adams'
'Burjor Captain'
'Mikael Johansson'
'Jack L. Smith'
_publ_section_title
;
 New Rhenium-Tin Cluster Adds Palladium Phosphine Groups across Re-Sn
 Bonds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              488
_journal_page_last               489
_journal_paper_doi               10.1021/ja0443169
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C32 H20 O8 Re2 Sn2'
_chemical_formula_weight         1142.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.3420(10)
_cell_angle_beta                 90.5590(10)
_cell_angle_gamma                105.3800(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5962(5)
_cell_length_b                   12.6495(7)
_cell_length_c                   14.5038(8)
_cell_measurement_reflns_used    7949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.53
_cell_volume                     1639.25(15)
_computing_cell_refinement       'SAINT+  V6.2 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT+  V6.2'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17121
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    8.914
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    2.314
_exptl_crystal_description       Block
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.484
_refine_diff_density_min         -2.635
_refine_diff_density_rms         0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         8069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0522P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                6488
_reflns_number_total             8069
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0443169si20040928_110837_1.cif
_cod_data_source_block           ReSn
_cod_database_code               4111385
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Re1 Re 0.37674(2) 0.058680(18) 0.040235(13) 0.03868(8) Uani 1 1 d .
Sn1 Sn 0.65249(4) 0.17237(3) 0.01238(2) 0.04048(10) Uani 1 1 d .
O11 O 0.2792(5) 0.0532(5) -0.1671(3) 0.0774(14) Uani 1 1 d .
O12 O 0.3466(8) 0.3001(5) 0.1119(4) 0.0972(18) Uani 1 1 d .
O13 O 0.5107(5) 0.0854(4) 0.2453(3) 0.0691(12) Uani 1 1 d .
O14 O 0.0625(5) -0.0386(5) 0.0867(4) 0.0914(17) Uani 1 1 d .
C11 C 0.3159(6) 0.0533(5) -0.0932(4) 0.0502(13) Uani 1 1 d .
C12 C 0.3604(8) 0.2129(6) 0.0852(5) 0.0660(17) Uani 1 1 d .
C13 C 0.4601(6) 0.0744(5) 0.1704(4) 0.0473(12) Uani 1 1 d .
C14 C 0.1802(6) -0.0075(6) 0.0684(4) 0.0558(14) Uani 1 1 d .
C31 C 0.7033(5) 0.2700(5) -0.0901(3) 0.0437(11) Uani 1 1 d .
C32 C 0.7977(7) 0.3788(6) -0.0641(5) 0.0638(17) Uani 1 1 d .
H32 H 0.8353 0.4108 -0.0010 0.077 Uiso 1 1 calc R
C33 C 0.8363(9) 0.4399(7) -0.1316(5) 0.081(2) Uani 1 1 d .
H33 H 0.9001 0.5124 -0.1136 0.098 Uiso 1 1 calc R
C34 C 0.7802(7) 0.3935(6) -0.2254(5) 0.0720(19) Uani 1 1 d .
H34 H 0.8062 0.4348 -0.2705 0.086 Uiso 1 1 calc R
C35 C 0.6867(7) 0.2868(6) -0.2521(4) 0.0614(16) Uani 1 1 d .
H35 H 0.6494 0.2555 -0.3154 0.074 Uiso 1 1 calc R
C36 C 0.6471(6) 0.2252(5) -0.1849(4) 0.0535(14) Uani 1 1 d .
H36 H 0.5822 0.1531 -0.2034 0.064 Uiso 1 1 calc R
C37 C 0.7866(5) 0.2729(5) 0.1390(4) 0.0454(12) Uani 1 1 d .
C38 C 0.7498(7) 0.3657(6) 0.1941(5) 0.0687(17) Uani 1 1 d .
H38 H 0.6688 0.3840 0.1742 0.082 Uiso 1 1 calc R
C39 C 0.8302(8) 0.4330(7) 0.2791(5) 0.080(2) Uani 1 1 d .
H39 H 0.8046 0.4963 0.3141 0.097 Uiso 1 1 calc R
C40 C 0.9479(8) 0.4045(6) 0.3104(5) 0.073(2) Uani 1 1 d .
H40 H 0.9983 0.4450 0.3691 0.087 Uiso 1 1 calc R
C41 C 0.9892(9) 0.3176(7) 0.2552(6) 0.090(3) Uani 1 1 d .
H41 H 1.0728 0.3020 0.2742 0.108 Uiso 1 1 calc R
C42 C 0.9091(7) 0.2497(6) 0.1695(5) 0.0737(19) Uani 1 1 d .
H42 H 0.9387 0.1890 0.1334 0.088 Uiso 1 1 calc R
Re2 Re 0.12563(2) -0.057188(17) 0.513603(13) 0.03862(8) Uani 1 1 d .
Sn2 Sn 0.14937(4) 0.17307(3) 0.56761(2) 0.04144(10) Uani 1 1 d .
O21 O 0.4402(4) 0.0383(5) 0.6040(4) 0.0811(14) Uani 1 1 d .
O22 O 0.2311(5) -0.0297(4) 0.3157(3) 0.0707(13) Uani 1 1 d .
O23 O 0.1545(7) -0.3007(4) 0.4724(4) 0.0889(17) Uani 1 1 d .
O24 O 0.0051(5) -0.0768(4) 0.7103(3) 0.0695(12) Uani 1 1 d .
C21 C 0.3224(6) 0.0065(6) 0.5717(4) 0.0552(14) Uani 1 1 d .
C22 C 0.1902(6) -0.0403(5) 0.3855(4) 0.0469(12) Uani 1 1 d .
C23 C 0.1420(7) -0.2109(6) 0.4864(5) 0.0623(16) Uani 1 1 d .
C24 C 0.0492(6) -0.0689(5) 0.6390(4) 0.0457(12) Uani 1 1 d .
C43 C 0.2847(6) 0.2762(5) 0.4880(4) 0.0477(12) Uani 1 1 d .
C44 C 0.4086(8) 0.2525(6) 0.4506(6) 0.084(2) Uani 1 1 d .
H44 H 0.4374 0.1921 0.4623 0.100 Uiso 1 1 calc R
C45 C 0.4906(10) 0.3185(7) 0.3954(7) 0.109(4) Uani 1 1 d .
H45 H 0.5739 0.3023 0.3709 0.131 Uiso 1 1 calc R
C46 C 0.4481(10) 0.4066(8) 0.3778(5) 0.092(3) Uani 1 1 d .
H46 H 0.5010 0.4495 0.3397 0.111 Uiso 1 1 calc R
C47 C 0.3278(8) 0.4320(7) 0.4161(6) 0.082(2) Uani 1 1 d .
H47 H 0.2998 0.4930 0.4048 0.099 Uiso 1 1 calc R
C48 C 0.2481(7) 0.3680(6) 0.4709(5) 0.0676(18) Uani 1 1 d .
H48 H 0.1673 0.3871 0.4972 0.081 Uiso 1 1 calc R
C49 C 0.2044(6) 0.2637(5) 0.7145(4) 0.0459(12) Uani 1 1 d .
C50 C 0.3429(7) 0.3324(6) 0.7397(4) 0.0628(16) Uani 1 1 d .
H50 H 0.4067 0.3409 0.6925 0.075 Uiso 1 1 calc R
C51 C 0.3902(8) 0.3899(7) 0.8343(5) 0.080(2) Uani 1 1 d .
H51 H 0.4847 0.4362 0.8500 0.096 Uiso 1 1 calc R
C52 C 0.2960(9) 0.3778(7) 0.9044(5) 0.079(2) Uani 1 1 d .
H52 H 0.3263 0.4159 0.9679 0.095 Uiso 1 1 calc R
C53 C 0.1588(9) 0.3099(7) 0.8801(5) 0.084(2) Uani 1 1 d .
H53 H 0.0948 0.3009 0.9272 0.100 Uiso 1 1 calc R
C54 C 0.1133(8) 0.2538(7) 0.7856(5) 0.074(2) Uani 1 1 d .
H54 H 0.0184 0.2082 0.7701 0.089 Uiso 1 1 calc R
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'
Sn Sn -0.6537 1.4246 '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'
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
C14 Re1 C12 92.7(3) . .
C14 Re1 C13 93.3(2) . .
C12 Re1 C13 87.9(3) . .
C14 Re1 C11 93.3(2) . .
C12 Re1 C11 90.8(3) . .
C13 Re1 C11 173.3(2) . .
C14 Re1 Sn1 174.23(19) . .
C12 Re1 Sn1 81.8(2) . .
C13 Re1 Sn1 84.77(15) . .
C11 Re1 Sn1 88.54(16) . .
C14 Re1 Sn1 76.4(2) . 2_655
C12 Re1 Sn1 169.1(2) . 2_655
C13 Re1 Sn1 92.03(17) . 2_655
C11 Re1 Sn1 90.45(17) . 2_655
Sn1 Re1 Sn1 109.074(11) . 2_655
C14 Re1 Re1 130.5(2) . 2_655
C12 Re1 Re1 136.7(2) . 2_655
C13 Re1 Re1 87.27(15) . 2_655
C11 Re1 Re1 89.13(16) . 2_655
Sn1 Re1 Re1 54.895(10) . 2_655
Sn1 Re1 Re1 54.179(9) 2_655 2_655
C37 Sn1 C31 105.2(2) . .
C37 Sn1 Re1 115.65(14) . .
C31 Sn1 Re1 124.31(14) . .
C37 Sn1 Re1 118.26(15) . 2_655
C31 Sn1 Re1 120.29(14) . 2_655
Re1 Sn1 Re1 70.926(11) . 2_655
O11 C11 Re1 177.6(6) . .
O12 C12 Re1 177.7(7) . .
O13 C13 Re1 178.5(5) . .
O14 C14 Re1 174.9(6) . .
C32 C31 C36 118.3(5) . .
C32 C31 Sn1 120.5(4) . .
C36 C31 Sn1 121.1(4) . .
C33 C32 C31 120.6(6) . .
C34 C33 C32 120.2(7) . .
C35 C34 C33 120.0(6) . .
C34 C35 C36 120.1(6) . .
C35 C36 C31 120.8(6) . .
C38 C37 C42 117.4(5) . .
C38 C37 Sn1 119.1(4) . .
C42 C37 Sn1 123.4(5) . .
C37 C38 C39 122.1(7) . .
C40 C39 C38 119.2(7) . .
C41 C40 C39 119.3(6) . .
C40 C41 C42 121.6(7) . .
C37 C42 C41 120.1(7) . .
C23 Re2 C21 92.6(3) . .
C23 Re2 C24 90.9(2) . .
C21 Re2 C24 91.5(2) . .
C23 Re2 C22 92.1(2) . .
C21 Re2 C22 91.6(2) . .
C24 Re2 C22 175.6(2) . .
C23 Re2 Sn2 80.5(2) . 2_556
C21 Re2 Sn2 172.92(19) . 2_556
C24 Re2 Sn2 87.10(15) . 2_556
C22 Re2 Sn2 90.24(15) . 2_556
C23 Re2 Sn2 170.2(2) . .
C21 Re2 Sn2 77.61(19) . .
C24 Re2 Sn2 88.77(16) . .
C22 Re2 Sn2 88.83(16) . .
Sn2 Re2 Sn2 109.285(11) 2_556 .
C23 Re2 Re2 135.4(2) . 2_556
C21 Re2 Re2 131.87(19) . 2_556
C24 Re2 Re2 86.44(15) . 2_556
C22 Re2 Re2 89.19(15) . 2_556
Sn2 Re2 Re2 54.990(10) 2_556 2_556
Sn2 Re2 Re2 54.295(10) . 2_556
C49 Sn2 C43 105.7(2) . .
C49 Sn2 Re2 125.47(15) . 2_556
C43 Sn2 Re2 116.37(14) . 2_556
C49 Sn2 Re2 119.12(15) . .
C43 Sn2 Re2 116.84(15) . .
Re2 Sn2 Re2 70.715(11) 2_556 .
O21 C21 Re2 176.0(6) . .
O22 C22 Re2 177.5(5) . .
O23 C23 Re2 178.2(7) . .
O24 C24 Re2 179.3(6) . .
C48 C43 C44 117.8(6) . .
C48 C43 Sn2 120.1(4) . .
C44 C43 Sn2 122.2(5) . .
C43 C44 C45 120.6(8) . .
C46 C45 C44 119.8(8) . .
C45 C46 C47 119.9(7) . .
C46 C47 C48 120.3(8) . .
C47 C48 C43 121.6(7) . .
C54 C49 C50 117.6(5) . .
C54 C49 Sn2 124.6(4) . .
C50 C49 Sn2 117.7(4) . .
C49 C50 C51 121.5(6) . .
C52 C51 C50 119.5(7) . .
C53 C52 C51 119.4(6) . .
C52 C53 C54 120.3(7) . .
C49 C54 C53 121.6(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C14 1.942(5) .
Re1 C12 1.946(7) .
Re1 C13 1.986(5) .
Re1 C11 1.995(6) .
Re1 Sn1 2.7429(4) .
Re1 Sn1 2.7675(5) 2_655
Re1 Re1 3.1971(4) 2_655
Sn1 C37 2.139(5) .
Sn1 C31 2.139(5) .
Sn1 Re1 2.7675(5) 2_655
O11 C11 1.125(7) .
O12 C12 1.120(8) .
O13 C13 1.146(6) .
O14 C14 1.150(6) .
C31 C32 1.390(8) .
C31 C36 1.393(7) .
C32 C33 1.386(9) .
C33 C34 1.382(10) .
C34 C35 1.367(9) .
C35 C36 1.390(8) .
C37 C38 1.379(9) .
C37 C42 1.379(8) .
C38 C39 1.397(9) .
C39 C40 1.378(10) .
C40 C41 1.344(11) .
C41 C42 1.405(9) .
Re2 C23 1.935(7) .
Re2 C21 1.936(6) .
Re2 C24 1.993(5) .
Re2 C22 2.008(6) .
Re2 Sn2 2.7445(4) 2_556
Re2 Sn2 2.7682(5) .
Re2 Re2 3.1902(4) 2_556
Sn2 C49 2.139(5) .
Sn2 C43 2.145(5) .
Sn2 Re2 2.7445(4) 2_556
O21 C21 1.147(6) .
O22 C22 1.116(6) .
O23 C23 1.142(7) .
O24 C24 1.138(6) .
C43 C48 1.375(9) .
C43 C44 1.385(8) .
C44 C45 1.397(10) .
C45 C46 1.362(12) .
C46 C47 1.365(12) .
C47 C48 1.369(9) .
C49 C54 1.367(8) .
C49 C50 1.369(8) .
C50 C51 1.391(9) .
C51 C52 1.377(10) .
C52 C53 1.356(10) .
C53 C54 1.384(10) .
