#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:18:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178621 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/32/4073288.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_4073288
loop_
_publ_author_name
'Albertin, Gabriele'
'Antoniutti, Stefano'
'Castro, Jesús'
'García-Fontán, Soledad'
'Zanardo, Gianluigi'
_publ_section_title
;
 Preparation and Reactivity of Stannyl Complexes of Manganese and Rhenium
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2918
_journal_paper_doi               10.1021/om070220m
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C22 H48 O16 P3 Re Sn'
_chemical_formula_weight         966.40
_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                109.711(2)
_cell_angle_beta                 92.817(2)
_cell_angle_gamma                114.348(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1114(11)
_cell_length_b                   11.9510(13)
_cell_length_c                   16.5529(17)
_cell_measurement_temperature    293(2)
_cell_volume                     1839.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_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  0.0571
_diffrn_reflns_av_sigmaI/netI    0.0863
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11422
_diffrn_reflns_theta_full        28.06
_diffrn_reflns_theta_max         28.06
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    4.158
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3506
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.700
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0459
_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)+(0.0415P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                5588
_reflns_number_total             7968
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070220m-file002.cif
_cod_data_source_block           compound_15b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               4073288
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
H1 H 0.1872 0.1444 0.0100 0.17(5) Uiso 1 1 d .
Re Re 0.00576(3) 0.11558(3) 0.271473(16) 0.04271(9) Uani 1 1 d .
C1 C 0.1949(8) 0.1694(7) 0.3191(4) 0.0565(18) Uani 1 1 d .
O1 O 0.3009(5) 0.1936(6) 0.3495(4) 0.0770(16) Uani 1 1 d .
C2 C -0.0141(7) 0.1828(8) 0.3895(5) 0.063(2) Uani 1 1 d .
O2 O -0.0186(6) 0.2294(6) 0.4625(3) 0.0881(19) Uani 1 1 d .
Sn Sn 0.06765(4) 0.04536(5) 0.10886(3) 0.04300(12) Uani 1 1 d .
O41 O 0.0973(4) 0.0979(4) 0.0036(3) 0.0474(11) Uani 1 1 d .
O42 O 0.1357(5) -0.0981(5) 0.0766(3) 0.0632(13) Uani 1 1 d .
C42 C 0.2182(8) -0.1020(10) 0.1319(6) 0.077(2) Uani 1 1 d .
H42 H 0.2596 -0.0283 0.1850 0.093 Uiso 1 1 calc R
O45 O 0.2463(7) -0.1912(8) 0.1210(4) 0.110(2) Uani 1 1 d .
O43 O 0.2890(5) 0.1897(6) 0.1571(3) 0.0733(16) Uani 1 1 d .
C43 C 0.3683(8) 0.2732(9) 0.1298(5) 0.074(2) Uani 1 1 d .
H43 H 0.4547 0.3290 0.1654 0.089 Uiso 1 1 calc R
O44 O 0.3472(5) 0.2905(6) 0.0636(4) 0.094(2) Uani 1 1 d .
P1 P -0.23315(18) 0.0385(2) 0.22254(12) 0.0498(4) Uani 1 1 d .
O11 O -0.3088(5) -0.1139(5) 0.1599(3) 0.0679(14) Uani 1 1 d .
C11 C -0.4537(7) -0.1903(9) 0.1226(6) 0.081(3) Uani 1 1 d .
H11A H -0.4691 -0.2389 0.0598 0.097 Uiso 1 1 calc R
H11B H -0.4935 -0.1296 0.1314 0.097 Uiso 1 1 calc R
C12 C -0.5202(9) -0.2855(10) 0.1640(8) 0.123(4) Uani 1 1 d .
H12A H -0.4885 -0.3519 0.1495 0.184 Uiso 1 1 calc R
H12B H -0.6165 -0.3281 0.1425 0.184 Uiso 1 1 calc R
H12C H -0.4987 -0.2384 0.2267 0.184 Uiso 1 1 calc R
O12 O -0.3004(5) 0.0560(6) 0.3051(3) 0.0711(15) Uani 1 1 d .
C13 C -0.4204(8) 0.0727(10) 0.3148(6) 0.085(3) Uani 1 1 d .
H13A H -0.4996 -0.0106 0.2796 0.102 Uiso 1 1 calc R
H13B H -0.4181 0.1401 0.2938 0.102 Uiso 1 1 calc R
C14 C -0.4292(10) 0.1129(13) 0.4063(6) 0.126(4) Uani 1 1 d .
H14A H -0.4535 0.0380 0.4228 0.189 Uiso 1 1 calc R
H14B H -0.4967 0.1437 0.4145 0.189 Uiso 1 1 calc R
H14C H -0.3431 0.1835 0.4423 0.189 Uiso 1 1 calc R
O13 O -0.2917(5) 0.1077(5) 0.1774(3) 0.0623(13) Uani 1 1 d .
C15 C -0.2732(8) 0.1098(9) 0.0923(5) 0.065(2) Uani 1 1 d .
H15A H -0.3121 0.0194 0.0480 0.079 Uiso 1 1 calc R
H15B H -0.1775 0.1541 0.0930 0.079 Uiso 1 1 calc R
C16 C -0.3430(11) 0.1844(11) 0.0721(6) 0.108(4) Uani 1 1 d .
H16A H -0.4380 0.1380 0.0696 0.161 Uiso 1 1 calc R
H16B H -0.3302 0.1901 0.0164 0.161 Uiso 1 1 calc R
H16C H -0.3055 0.2727 0.1173 0.161 Uiso 1 1 calc R
P2 P 0.0607(2) 0.3268(2) 0.26676(12) 0.0585(5) Uani 1 1 d .
O21 O 0.1857(7) 0.4545(6) 0.3343(4) 0.103(2) Uani 1 1 d .
C21 C 0.3124(17) 0.4828(15) 0.3575(14) 0.242(12) Uani 1 1 d .
H21A H 0.3096 0.3954 0.3373 0.290 Uiso 1 1 calc R
H21B H 0.3548 0.5218 0.3173 0.290 Uiso 1 1 calc R
C22 C 0.3996(15) 0.5450(18) 0.4240(12) 0.250(11) Uani 1 1 d .
H22A H 0.4569 0.6323 0.4260 0.376 Uiso 1 1 calc R
H22B H 0.4526 0.4990 0.4249 0.376 Uiso 1 1 calc R
H22C H 0.3587 0.5532 0.4741 0.376 Uiso 1 1 calc R
O22 O 0.0806(6) 0.3296(5) 0.1736(3) 0.0794(16) Uani 1 1 d .
C23 C 0.1323(11) 0.4488(10) 0.1534(7) 0.102(3) Uani 1 1 d .
H23A H 0.1575 0.5272 0.2069 0.122 Uiso 1 1 calc R
H23B H 0.2127 0.4580 0.1300 0.122 Uiso 1 1 calc R
C24 C 0.0326(13) 0.4406(11) 0.0908(7) 0.132(4) Uani 1 1 d .
H24A H -0.0058 0.3545 0.0430 0.199 Uiso 1 1 calc R
H24B H 0.0742 0.5089 0.0687 0.199 Uiso 1 1 calc R
H24C H -0.0374 0.4527 0.1185 0.199 Uiso 1 1 calc R
O23 O -0.0435(7) 0.3884(7) 0.2817(5) 0.102(2) Uani 1 1 d .
C25 C -0.0916(11) 0.4203(13) 0.3551(7) 0.116(4) Uani 1 1 d .
H25A H -0.0180 0.4949 0.4023 0.139 Uiso 1 1 calc R
H25B H -0.1250 0.3450 0.3724 0.139 Uiso 1 1 calc R
C26 C -0.2030(11) 0.4567(12) 0.3429(8) 0.129(4) Uani 1 1 d .
H26A H -0.1713 0.5298 0.3243 0.194 Uiso 1 1 calc R
H26B H -0.2304 0.4823 0.3975 0.194 Uiso 1 1 calc R
H26C H -0.2787 0.3812 0.2990 0.194 Uiso 1 1 calc R
P3 P -0.0460(2) -0.0949(2) 0.27804(13) 0.0575(5) Uani 1 1 d .
O31 O 0.0859(5) -0.1022(6) 0.3062(4) 0.0883(19) Uani 1 1 d .
C31 C 0.0905(10) -0.2157(10) 0.3155(8) 0.115(4) Uani 1 1 d .
H31A H 0.0264 -0.2465 0.3503 0.138 Uiso 1 1 calc R
H31B H 0.0618 -0.2872 0.2578 0.138 Uiso 1 1 calc R
C32 C 0.2146(11) -0.1911(11) 0.3541(7) 0.125(4) Uani 1 1 d .
H32A H 0.2742 -0.1796 0.3142 0.188 Uiso 1 1 calc R
H32B H 0.2066 -0.2650 0.3683 0.188 Uiso 1 1 calc R
H32C H 0.2506 -0.1114 0.4068 0.188 Uiso 1 1 calc R
O32 O -0.1346(10) -0.2306(8) 0.2042(8) 0.190(6) Uani 1 1 d .
C33 C -0.1712(16) -0.3102(16) 0.1320(8) 0.147(5) Uani 1 1 d .
H33A H -0.0872 -0.3029 0.1145 0.177 Uiso 1 1 calc R
H33B H -0.2052 -0.2707 0.1000 0.177 Uiso 1 1 calc R
C34 C -0.2545(14) -0.4394(13) 0.0914(9) 0.160(6) Uani 1 1 d .
H34A H -0.2519 -0.4839 0.1296 0.241 Uiso 1 1 calc R
H34B H -0.2270 -0.4760 0.0388 0.241 Uiso 1 1 calc R
H34C H -0.3450 -0.4520 0.0763 0.241 Uiso 1 1 calc R
O33 O -0.1265(12) -0.1303(11) 0.3467(9) 0.210(6) Uani 1 1 d .
C35 C -0.1930(16) -0.1303(17) 0.3931(8) 0.174(7) Uani 1 1 d .
H35A H -0.2612 -0.1223 0.3598 0.209 Uiso 1 1 calc R
H35B H -0.1379 -0.0401 0.4364 0.209 Uiso 1 1 calc R
C36 C -0.2641(16) -0.1778(17) 0.4424(10) 0.204(8) Uani 1 1 d .
H36A H -0.2697 -0.2637 0.4331 0.306 Uiso 1 1 calc R
H36B H -0.3535 -0.1869 0.4284 0.306 Uiso 1 1 calc R
H36C H -0.2229 -0.1186 0.5028 0.306 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'
P P 0.1023 0.0942 '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 88.1(3) . .
C2 Re P2 89.2(2) . .
C1 Re P2 92.1(2) . .
C2 Re P3 90.4(2) . .
C1 Re P3 87.0(2) . .
P2 Re P3 179.03(7) . .
C2 Re P1 88.4(2) . .
C1 Re P1 174.4(2) . .
P2 Re P1 92.10(7) . .
P3 Re P1 88.77(7) . .
C2 Re Sn 172.6(2) . .
C1 Re Sn 85.87(19) . .
P2 Re Sn 86.83(5) . .
P3 Re Sn 93.47(5) . .
P1 Re Sn 97.96(4) . .
O1 C1 Re 174.8(6) . .
O2 C2 Re 176.1(7) . .
O41 Sn O42 99.30(18) . .
O41 Sn O41 69.66(19) . 2
O42 Sn O41 84.65(18) . 2
O41 Sn O43 81.57(17) . .
O42 Sn O43 84.0(2) . .
O41 Sn O43 146.82(17) 2 .
O41 Sn Re 143.44(13) . .
O42 Sn Re 116.65(13) . .
O41 Sn Re 117.84(11) 2 .
O43 Sn Re 95.08(13) . .
Sn O41 Sn 110.34(19) . 2
C42 O42 Sn 123.1(5) . .
O45 C42 O42 125.9(9) . .
C43 O43 Sn 132.2(5) . .
O44 C43 O43 128.8(7) . .
O11 P1 O13 104.5(3) . .
O11 P1 O12 107.0(3) . .
O13 P1 O12 98.4(3) . .
O11 P1 Re 112.40(18) . .
O13 P1 Re 123.6(2) . .
O12 P1 Re 109.3(2) . .
C11 O11 P1 125.3(5) . .
O11 C11 C12 111.2(7) . .
C13 O12 P1 128.8(5) . .
O12 C13 C14 110.0(7) . .
C15 O13 P1 123.1(4) . .
O13 C15 C16 107.3(6) . .
O21 P2 O22 105.2(3) . .
O21 P2 O23 95.9(4) . .
O22 P2 O23 98.5(3) . .
O21 P2 Re 119.8(3) . .
O22 P2 Re 113.0(2) . .
O23 P2 Re 121.0(3) . .
C21 O21 P2 132.8(9) . .
C22 C21 O21 137(2) . .
C23 O22 P2 125.7(6) . .
C24 C23 O22 110.8(9) . .
C25 O23 P2 126.5(7) . .
O23 C25 C26 112.9(9) . .
O32 P3 O33 93.5(7) . .
O32 P3 O31 104.6(4) . .
O33 P3 O31 101.5(5) . .
O32 P3 Re 125.4(4) . .
O33 P3 Re 117.4(4) . .
O31 P3 Re 111.0(2) . .
C31 O31 P3 125.2(5) . .
C32 C31 O31 114.2(9) . .
C33 O32 P3 155.3(16) . .
O32 C33 C34 136.4(18) . .
C35 O33 P3 160.6(12) . .
O33 C35 C36 153.6(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re C2 1.908(8) .
Re C1 1.957(8) .
Re P2 2.370(2) .
Re P3 2.381(2) .
Re P1 2.4127(18) .
Re Sn 2.7489(5) .
C1 O1 1.135(8) .
C2 O2 1.161(8) .
Sn O41 2.040(4) .
Sn O42 2.070(5) .
Sn O41 2.164(4) 2
Sn O43 2.245(5) .
O41 Sn 2.164(4) 2
O42 C42 1.288(8) .
C42 O45 1.190(9) .
O43 C43 1.263(9) .
C43 O44 1.212(9) .
P1 O11 1.574(5) .
P1 O13 1.574(4) .
P1 O12 1.583(5) .
O11 C11 1.455(8) .
C11 C12 1.480(11) .
O12 C13 1.436(8) .
C13 C14 1.449(11) .
O13 C15 1.441(7) .
C15 C16 1.501(10) .
P2 O21 1.568(6) .
P2 O22 1.578(5) .
P2 O23 1.598(6) .
O21 C21 1.308(15) .
C21 C22 1.205(18) .
O22 C23 1.461(9) .
C23 C24 1.429(13) .
O23 C25 1.351(11) .
C25 C26 1.496(13) .
P3 O32 1.524(8) .
P3 O33 1.543(8) .
P3 O31 1.562(5) .
O31 C31 1.437(9) .
C31 C32 1.359(11) .
O32 C33 1.169(13) .
C33 C34 1.324(15) .
O33 C35 1.093(12) .
C35 C36 1.271(14) .
