#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:40:25 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178576 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/86/4068658.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_4068658
loop_
_publ_author_name
'Albertin, Gabriele'
'Antoniutti, Stefano'
'Castro, Jesús'
'Zanardo, Gianluigi'
_publ_section_title
;
 Reaction of Trihydridostannyl Complexes with SO2: Preparation of
 [Re2{Sn2(μ-S)(μ-SO3)2}(CO)4L2{PPh(OEt)2}4] (L = PPh(OEt)2, (CH3)3CNC)
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1270
_journal_paper_doi               10.1021/om801013s
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C54 H78 N2 O18 P4 Re2 S3 Sn2'
_chemical_formula_weight         1873.02
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.489(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.347(7)
_cell_length_b                   16.615(7)
_cell_length_c                   31.222(14)
_cell_measurement_reflns_used    5089
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.80
_cell_measurement_theta_min      2.28
_cell_volume                     7947(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            25074
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    3.873
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
A. L. Spek, Acta Crystallogr. 1990, A46, C34
;
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         9289
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0497P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                5643
_reflns_number_total             9289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801013s_si_001.cif
_cod_data_source_block           GN470_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        7946(6)
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4068658
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_
_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
Re Re 0.491362(14) 0.246965(13) 0.394245(7) 0.04331(8) Uani 1 1 d .
C1 C 0.5785(4) 0.1649(4) 0.4095(2) 0.0616(16) Uani 1 1 d .
O1 O 0.6305(3) 0.1173(3) 0.41924(18) 0.0932(16) Uani 1 1 d .
C2 C 0.4807(4) 0.2752(4) 0.4541(2) 0.0627(17) Uani 1 1 d .
O2 O 0.4743(4) 0.2910(4) 0.48938(14) 0.1004(18) Uani 1 1 d .
C31 C 0.4007(4) 0.3323(4) 0.37317(18) 0.0529(15) Uani 1 1 d .
N31 N 0.3512(3) 0.3800(3) 0.36043(17) 0.0671(15) Uani 1 1 d .
C32 C 0.2934(5) 0.4411(5) 0.3384(3) 0.080(2) Uani 1 1 d .
C33 C 0.3535(6) 0.5073(6) 0.3238(4) 0.157(5) Uani 1 1 d .
H33A H 0.3618 0.5469 0.3460 0.235 Uiso 1 1 calc R
H33B H 0.3277 0.5322 0.2983 0.235 Uiso 1 1 calc R
H33C H 0.4089 0.4844 0.3177 0.235 Uiso 1 1 calc R
C34 C 0.2493(7) 0.4000(6) 0.2992(4) 0.178(6) Uani 1 1 d .
H34A H 0.2925 0.3727 0.2836 0.267 Uiso 1 1 calc R
H34B H 0.2204 0.4396 0.2810 0.267 Uiso 1 1 calc R
H34C H 0.2073 0.3617 0.3083 0.267 Uiso 1 1 calc R
C35 C 0.2300(9) 0.4695(9) 0.3680(4) 0.232(8) Uani 1 1 d .
H35A H 0.1979 0.4246 0.3782 0.348 Uiso 1 1 calc R
H35B H 0.1904 0.5066 0.3534 0.348 Uiso 1 1 calc R
H35C H 0.2601 0.4962 0.3919 0.348 Uiso 1 1 calc R
Sn Sn 0.49975(3) 0.21959(2) 0.308106(12) 0.04615(11) Uani 1 1 d .
P1 P 0.37836(11) 0.15049(10) 0.40273(5) 0.0532(4) Uani 1 1 d .
O11 O 0.6089(3) 0.4204(3) 0.42266(16) 0.0840(14) Uani 1 1 d .
O12 O 0.6067(3) 0.3823(3) 0.34308(13) 0.0734(13) Uani 1 1 d .
C11 C 0.7143(4) 0.3080(4) 0.4033(2) 0.0587(16) Uani 1 1 d .
C12 C 0.7525(5) 0.3202(5) 0.4459(3) 0.091(2) Uani 1 1 d .
H12 H 0.7238 0.3507 0.4656 0.110 Uiso 1 1 calc R
C13 C 0.8336(6) 0.2852(6) 0.4571(3) 0.111(3) Uani 1 1 d .
H13 H 0.8587 0.2916 0.4848 0.133 Uiso 1 1 calc R
C14 C 0.8766(7) 0.2414(6) 0.4274(4) 0.109(3) Uani 1 1 d .
H14 H 0.9313 0.2196 0.4348 0.130 Uiso 1 1 calc R
C15 C 0.8390(6) 0.2298(5) 0.3868(4) 0.097(3) Uani 1 1 d .
H15 H 0.8684 0.1994 0.3673 0.117 Uiso 1 1 calc R
C16 C 0.7559(5) 0.2631(4) 0.3739(3) 0.086(2) Uani 1 1 d .
H16 H 0.7308 0.2546 0.3464 0.103 Uiso 1 1 calc R
C17 C 0.5367(7) 0.4745(5) 0.4259(3) 0.122(3) Uani 1 1 d .
H17A H 0.5139 0.4893 0.3973 0.147 Uiso 1 1 calc R
H17B H 0.4905 0.4473 0.4401 0.147 Uiso 1 1 calc R
C18 C 0.5611(8) 0.5453(6) 0.4491(4) 0.190(6) Uani 1 1 d .
H18A H 0.6124 0.5347 0.4674 0.285 Uiso 1 1 calc R
H18B H 0.5144 0.5614 0.4663 0.285 Uiso 1 1 calc R
H18C H 0.5731 0.5876 0.4294 0.285 Uiso 1 1 calc R
C19 C 0.6722(6) 0.4403(6) 0.3306(3) 0.117(3) Uani 1 1 d .
H19A H 0.6978 0.4670 0.3560 0.141 Uiso 1 1 calc R
H19B H 0.7184 0.4122 0.3169 0.141 Uiso 1 1 calc R
C110 C 0.6345(8) 0.4977(6) 0.3024(3) 0.163(5) Uani 1 1 d .
H11A H 0.5942 0.4717 0.2821 0.244 Uiso 1 1 calc R
H11B H 0.6794 0.5237 0.2874 0.244 Uiso 1 1 calc R
H11C H 0.6041 0.5371 0.3183 0.244 Uiso 1 1 calc R
P2 P 0.60522(10) 0.34378(9) 0.38974(5) 0.0526(4) Uani 1 1 d .
O21 O 0.3673(3) 0.0715(3) 0.37328(14) 0.0694(12) Uani 1 1 d .
O22 O 0.3872(3) 0.1155(3) 0.45107(13) 0.0786(14) Uani 1 1 d .
C21 C 0.2665(4) 0.1871(4) 0.3966(2) 0.0604(16) Uani 1 1 d .
C22 C 0.2197(5) 0.1799(5) 0.3577(2) 0.078(2) Uani 1 1 d .
H22 H 0.2436 0.1538 0.3348 0.094 Uiso 1 1 calc R
C23 C 0.1349(6) 0.2130(7) 0.3532(4) 0.122(4) Uani 1 1 d .
H23 H 0.1019 0.2067 0.3274 0.146 Uiso 1 1 calc R
C24 C 0.1015(8) 0.2528(7) 0.3852(5) 0.131(5) Uani 1 1 d .
H24 H 0.0464 0.2759 0.3810 0.157 Uiso 1 1 calc R
C25 C 0.1466(7) 0.2609(6) 0.4245(5) 0.122(4) Uani 1 1 d .
H25 H 0.1210 0.2867 0.4470 0.147 Uiso 1 1 calc R
C26 C 0.2324(6) 0.2295(5) 0.4303(3) 0.094(3) Uani 1 1 d .
H26 H 0.2652 0.2371 0.4560 0.113 Uiso 1 1 calc R
C27 C 0.4399(6) 0.0234(4) 0.3634(3) 0.107(3) Uani 1 1 d .
H27A H 0.4483 0.0298 0.3330 0.129 Uiso 1 1 calc R
H27B H 0.4912 0.0455 0.3788 0.129 Uiso 1 1 calc R
C28 C 0.4379(8) -0.0544(7) 0.3715(6) 0.269(10) Uani 1 1 d .
H28A H 0.4758 -0.0821 0.3531 0.404 Uiso 1 1 calc R
H28B H 0.3794 -0.0740 0.3664 0.404 Uiso 1 1 calc R
H28C H 0.4571 -0.0637 0.4009 0.404 Uiso 1 1 calc R
C29 C 0.3271(6) 0.0538(6) 0.4647(3) 0.122(4) Uani 1 1 d .
H29A H 0.2684 0.0755 0.4642 0.146 Uiso 1 1 calc R
H29B H 0.3269 0.0086 0.4450 0.146 Uiso 1 1 calc R
C210 C 0.3519(13) 0.0284(9) 0.5050(4) 0.314(12) Uani 1 1 d .
H21A H 0.4048 -0.0022 0.5043 0.471 Uiso 1 1 calc R
H21B H 0.3068 -0.0046 0.5157 0.471 Uiso 1 1 calc R
H21C H 0.3615 0.0743 0.5234 0.471 Uiso 1 1 calc R
S1 S 0.5000 0.31565(14) 0.2500 0.0698(7) Uani 1 2 d S
S2 S 0.65420(19) 0.1339(2) 0.25688(8) 0.1458(14) Uani 1 1 d D
O5 O 0.7158(7) 0.1852(13) 0.2605(4) 0.471(16) Uani 1 1 d D
O3 O 0.5970(4) 0.1400(4) 0.29414(16) 0.127(2) Uani 1 1 d .
O4 O 0.4009(4) 0.1461(4) 0.28275(15) 0.129(3) Uani 1 1 d .
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'
N N 0.0061 0.0033 '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'
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'
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
C2 Re C1 91.8(3) . .
C2 Re C31 92.7(2) . .
C1 Re C31 175.6(2) . .
C2 Re P2 89.9(2) . .
C1 Re P2 89.5(2) . .
C31 Re P2 90.01(17) . .
C2 Re P1 87.2(2) . .
C1 Re P1 89.7(2) . .
C31 Re P1 90.93(17) . .
P2 Re P1 177.02(5) . .
C2 Re Sn 175.1(2) . .
C1 Re Sn 92.91(18) . .
C31 Re Sn 82.65(16) . .
P2 Re Sn 88.61(4) . .
P1 Re Sn 94.32(4) . .
O1 C1 Re 178.6(7) . .
O2 C2 Re 179.3(7) . .
N31 C31 Re 178.2(5) . .
C31 N31 C32 172.2(6) . .
C35 C32 N31 109.2(7) . .
C35 C32 C33 113.3(10) . .
N31 C32 C33 106.0(6) . .
C35 C32 C34 111.9(10) . .
N31 C32 C34 106.7(7) . .
C33 C32 C34 109.2(8) . .
O3 Sn O4 93.7(3) . .
O3 Sn S1 103.35(15) . .
O4 Sn S1 97.89(15) . .
O3 Sn Re 113.11(14) . .
O4 Sn Re 113.40(14) . .
S1 Sn Re 129.04(5) . .
O21 P1 O22 103.9(3) . .
O21 P1 C21 98.4(3) . .
O22 P1 C21 104.1(3) . .
O21 P1 Re 122.52(17) . .
O22 P1 Re 108.97(18) . .
C21 P1 Re 116.8(2) . .
C17 O11 P2 122.3(5) . .
C19 O12 P2 123.8(4) . .
C16 C11 C12 121.1(7) . .
C16 C11 P2 119.1(6) . .
C12 C11 P2 119.4(5) . .
C13 C12 C11 118.8(8) . .
C14 C13 C12 120.3(9) . .
C15 C14 C13 120.2(9) . .
C14 C15 C16 121.7(9) . .
C11 C16 C15 117.8(9) . .
C18 C17 O11 111.9(9) . .
C110 C19 O12 110.6(7) . .
O12 P2 O11 105.1(3) . .
O12 P2 C11 106.4(3) . .
O11 P2 C11 96.5(3) . .
O12 P2 Re 112.11(17) . .
O11 P2 Re 119.05(19) . .
C11 P2 Re 115.9(2) . .
C27 O21 P1 121.8(5) . .
C29 O22 P1 120.4(5) . .
C22 C21 C26 120.6(7) . .
C22 C21 P1 120.2(5) . .
C26 C21 P1 118.9(6) . .
C21 C22 C23 118.9(8) . .
C24 C23 C22 120.9(11) . .
C23 C24 C25 121.6(12) . .
C24 C25 C26 119.3(10) . .
C21 C26 C25 118.6(10) . .
C28 C27 O21 118.8(8) . .
C210 C29 O22 109.9(9) . .
Sn S1 Sn 97.32(9) 2_655 .
O5 S2 O4 111.7(8) . 2_655
O5 S2 O3 110.6(8) . .
O4 S2 O3 108.0(4) 2_655 .
S2 O3 Sn 132.2(3) . .
S2 O4 Sn 140.9(3) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re C2 1.944(6) .
Re C1 1.948(7) .
Re C31 2.065(6) .
Re P2 2.3856(17) .
Re P1 2.3881(17) .
Re Sn 2.7383(12) .
C1 O1 1.152(7) .
C2 O2 1.141(7) .
C31 N31 1.152(7) .
N31 C32 1.489(8) .
C32 C35 1.461(11) .
C32 C33 1.523(11) .
C32 C34 1.525(12) .
Sn O3 2.060(5) .
Sn O4 2.067(5) .
Sn S1 2.4165(17) .
P1 O21 1.606(5) .
P1 O22 1.615(4) .
P1 C21 1.821(7) .
O11 C17 1.435(9) .
O11 P2 1.635(5) .
O12 C19 1.462(8) .
O12 P2 1.593(4) .
C11 C16 1.370(10) .
C11 C12 1.435(9) .
C11 P2 1.802(6) .
C12 C13 1.400(10) .
C13 C14 1.380(13) .
C14 C15 1.373(13) .
C15 C16 1.426(11) .
C17 C18 1.420(12) .
C19 C110 1.400(12) .
O21 C27 1.421(8) .
O22 C29 1.459(8) .
C21 C22 1.377(9) .
C21 C26 1.395(9) .
C22 C23 1.412(11) .
C23 C24 1.328(15) .
C24 C25 1.377(15) .
C25 C26 1.417(13) .
C27 C28 1.317(12) .
C29 C210 1.360(12) .
S1 Sn 2.4165(17) 2_655
S2 O5 1.274(14) .
S2 O4 1.470(5) 2_655
S2 O3 1.503(5) .
O4 S2 1.470(5) 2_655
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.301 0.250 184.8 30.1
2 0.000 0.699 0.750 184.8 29.6
3 0.164 -0.008 0.038 37.2 2.7
4 0.164 1.008 0.538 37.2 1.5
5 0.335 0.492 0.462 37.2 2.3
6 0.335 0.508 0.962 37.2 2.0
7 0.500 0.801 0.250 184.7 30.1
8 0.500 0.199 0.750 184.8 29.6
9 0.664 0.492 0.038 37.2 2.7
10 0.664 0.508 0.538 37.2 1.5
11 0.835 0.992 0.462 37.2 2.3
12 0.835 0.008 0.962 37.2 2.0
