#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:16:34 +0100 (vie 25 de mar de 2016) $
#$Revision: 179746 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/42/7004282.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_7004282
loop_
_publ_author_name
'Kabir, Shariff E.'
'Raha, Arun K.'
'Hassan, Mohammad R.'
'Nicholson, Brian K.'
'Rosenberg, Edward'
'Sharmin, Ayesha'
'Salassa, Luca'
_publ_section_title
;
 Ruthenium and osmium carbonyl clusters incorporating stannylene and
 stannyl ligands
;
_journal_issue                   32
_journal_name_full               'Dalton Transactions'
_journal_page_first              4212
_journal_page_last               4219
_journal_paper_doi               10.1039/b805024d
_journal_year                    2008
_chemical_formula_moiety         'C35 H23 N O9 Os3 S Sn'
_chemical_formula_sum            'C35 H23 N O9 Os3 S Sn'
_chemical_formula_weight         1322.89
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.212(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9339(2)
_cell_length_b                   22.8143(2)
_cell_length_c                   14.4812(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    89(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     3597.39(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      89(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER SMART CCD'
_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  0.0235
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21313
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    11.361
_exptl_absorpt_correction_T_max  0.1727
_exptl_absorpt_correction_T_min  0.1074
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.443
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.656
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0204
_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)+(0.0116P)²+10.3200P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0454
_reflns_number_gt                6640
_reflns_number_total             7303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805024d.txt
_cod_data_source_block           akr18g
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7004282
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'
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
Os1 Os 0.903359(14) 0.211645(7) 0.840393(11) 0.01335(4) Uani 1 1 d . . .
Os2 Os 0.948877(14) 0.258587(7) 0.650117(11) 0.01392(4) Uani 1 1 d . . .
Os3 Os 0.985150(14) 0.388139(7) 0.630545(11) 0.01543(4) Uani 1 1 d . . .
Sn1 Sn 0.91296(2) 0.338923(12) 0.790033(19) 0.01372(6) Uani 1 1 d . . .
S1 S 0.92691(9) 0.15952(4) 0.69874(7) 0.01468(19) Uani 1 1 d . . .
C1 C 0.8636(4) 0.25328(18) 0.9473(3) 0.0185(9) Uani 1 1 d . . .
C2 C 1.0713(4) 0.21283(18) 0.8800(3) 0.0170(8) Uani 1 1 d . . .
C3 C 1.1255(4) 0.25416(19) 0.6841(3) 0.0196(9) Uani 1 1 d . . .
C4 C 0.7710(4) 0.26166(17) 0.6212(3) 0.0169(8) Uani 1 1 d . . .
C5 C 0.9724(4) 0.25784(19) 0.5224(3) 0.0207(9) Uani 1 1 d . . .
C6 C 1.1545(4) 0.3826(2) 0.6855(3) 0.0234(10) Uani 1 1 d . . .
C7 C 0.8119(4) 0.38696(18) 0.5826(3) 0.0204(9) Uani 1 1 d . . .
C8 C 0.9763(4) 0.4656(2) 0.6786(3) 0.0217(9) Uani 1 1 d . . .
C9 C 1.0344(4) 0.38996(19) 0.5047(3) 0.0238(10) Uani 1 1 d . . .
O1 O 0.8395(3) 0.27567(14) 1.0147(2) 0.0293(8) Uani 1 1 d . . .
O2 O 1.1744(3) 0.21100(14) 0.9042(2) 0.0240(7) Uani 1 1 d . . .
O3 O 1.2288(3) 0.24918(15) 0.7037(2) 0.0297(8) Uani 1 1 d . . .
O4 O 0.6668(3) 0.26138(14) 0.6050(2) 0.0241(7) Uani 1 1 d . . .
O5 O 0.9841(3) 0.25873(14) 0.4442(2) 0.0267(7) Uani 1 1 d . . .
O6 O 1.2532(3) 0.38046(16) 0.7182(3) 0.0342(8) Uani 1 1 d . . .
O7 O 0.7126(3) 0.38668(14) 0.5536(3) 0.0325(8) Uani 1 1 d . . .
O8 O 0.9724(3) 0.51191(14) 0.7091(2) 0.0301(8) Uani 1 1 d . . .
O9 O 1.0588(3) 0.39367(16) 0.4296(2) 0.0345(8) Uani 1 1 d . . .
C11 C 0.8845(4) 0.13250(18) 0.9165(3) 0.0154(8) Uani 1 1 d . . .
C12 C 0.8308(4) 0.08242(18) 0.8722(3) 0.0195(9) Uani 1 1 d . . .
H12 H 0.8014 0.0845 0.8086 0.023 Uiso 1 1 calc R . .
C13 C 0.8202(4) 0.0300(2) 0.9201(3) 0.0243(10) Uani 1 1 d . . .
H13 H 0.7850 -0.0033 0.8885 0.029 Uiso 1 1 calc R . .
C14 C 0.8606(4) 0.0259(2) 1.0137(3) 0.0236(10) Uani 1 1 d . . .
H14 H 0.8529 -0.0098 1.0463 0.028 Uiso 1 1 calc R . .
C15 C 0.9125(4) 0.0747(2) 1.0589(3) 0.0232(10) Uani 1 1 d . . .
H15 H 0.9403 0.0724 1.1229 0.028 Uiso 1 1 calc R . .
C16 C 0.9239(4) 0.12699(19) 1.0108(3) 0.0197(9) Uani 1 1 d . . .
H16 H 0.9595 0.1600 1.0430 0.024 Uiso 1 1 calc R . .
C21 C 1.0642(4) 0.11774(18) 0.6913(3) 0.0173(9) Uani 1 1 d . . .
C22 C 1.1016(4) 0.1079(2) 0.6026(3) 0.0249(10) Uani 1 1 d . . .
H22 H 1.0619 0.1276 0.5504 0.030 Uiso 1 1 calc R . .
C23 C 1.1972(4) 0.0691(2) 0.5918(4) 0.0326(12) Uani 1 1 d . . .
H23 H 1.2214 0.0617 0.5315 0.039 Uiso 1 1 calc R . .
C24 C 1.2573(4) 0.0412(2) 0.6671(3) 0.0260(10) Uani 1 1 d . . .
H24 H 1.3233 0.0152 0.6588 0.031 Uiso 1 1 calc R . .
C25 C 1.2210(4) 0.0514(2) 0.7555(3) 0.0257(10) Uani 1 1 d . . .
H25 H 1.2629 0.0325 0.8076 0.031 Uiso 1 1 calc R . .
C26 C 1.1237(4) 0.08911(19) 0.7679(3) 0.0202(9) Uani 1 1 d . . .
H26 H 1.0980 0.0953 0.8280 0.024 Uiso 1 1 calc R . .
C31 C 0.7351(4) 0.37578(18) 0.8137(3) 0.0164(8) Uani 1 1 d . . .
C32 C 0.7189(4) 0.43677(18) 0.8068(3) 0.0202(9) Uani 1 1 d . . .
H32 H 0.7861 0.4609 0.7941 0.024 Uiso 1 1 calc R . .
C33 C 0.6055(4) 0.4623(2) 0.8183(3) 0.0255(10) Uani 1 1 d . . .
H33 H 0.5962 0.5036 0.8132 0.031 Uiso 1 1 calc R . .
C34 C 0.5065(4) 0.4280(2) 0.8371(3) 0.0235(10) Uani 1 1 d . . .
H34 H 0.4294 0.4456 0.8450 0.028 Uiso 1 1 calc R . .
C35 C 0.5206(4) 0.3685(2) 0.8440(3) 0.0234(10) Uani 1 1 d . . .
H35 H 0.4527 0.3446 0.8566 0.028 Uiso 1 1 calc R . .
C36 C 0.6343(4) 0.3425(2) 0.8329(3) 0.0212(9) Uani 1 1 d . . .
H36 H 0.6426 0.3011 0.8386 0.025 Uiso 1 1 calc R . .
C41 C 1.0352(4) 0.37031(18) 0.9061(3) 0.0176(9) Uani 1 1 d . . .
C42 C 0.9893(4) 0.4087(2) 0.9697(4) 0.0324(12) Uani 1 1 d . . .
H42 H 0.9049 0.4192 0.9627 0.039 Uiso 1 1 calc R . .
C43 C 1.0655(5) 0.4319(2) 1.0433(4) 0.0395(13) Uani 1 1 d . . .
H43 H 1.0327 0.4576 1.0864 0.047 Uiso 1 1 calc R . .
C44 C 1.1881(4) 0.4174(2) 1.0536(4) 0.0305(11) Uani 1 1 d . . .
H44 H 1.2402 0.4334 1.1032 0.037 Uiso 1 1 calc R . .
C45 C 1.2354(4) 0.3793(2) 0.9913(3) 0.0260(10) Uani 1 1 d . . .
H45 H 1.3199 0.3691 0.9984 0.031 Uiso 1 1 calc R . .
C46 C 1.1593(4) 0.35616(19) 0.9188(3) 0.0207(9) Uani 1 1 d . . .
H46 H 1.1926 0.3300 0.8767 0.025 Uiso 1 1 calc R . .
N1 N 0.7169(3) 0.19859(15) 0.7953(2) 0.0164(7) Uani 1 1 d . . .
C51 C 0.6185(4) 0.18570(19) 0.7691(3) 0.0192(9) Uani 1 1 d . . .
C52 C 0.4932(4) 0.1702(2) 0.7339(4) 0.0301(11) Uani 1 1 d . . .
H52A H 0.4777 0.1834 0.6695 0.045 Uiso 1 1 calc R . .
H52B H 0.4350 0.1891 0.7719 0.045 Uiso 1 1 calc R . .
H52C H 0.4830 0.1275 0.7366 0.045 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'
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'
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'
Os Os -1.2165 7.6030 '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
_geom_angle_publ_flag
C2 Os1 C1 91.92(18) . . ?
C2 Os1 N1 172.67(15) . . ?
C1 Os1 N1 92.11(16) . . ?
C2 Os1 C11 89.55(17) . . ?
C1 Os1 C11 87.86(17) . . ?
N1 Os1 C11 84.49(14) . . ?
C2 Os1 S1 95.19(13) . . ?
C1 Os1 S1 172.88(13) . . ?
N1 Os1 S1 80.86(10) . . ?
C11 Os1 S1 92.56(11) . . ?
C2 Os1 Sn1 90.32(12) . . ?
C1 Os1 Sn1 74.30(13) . . ?
N1 Os1 Sn1 96.66(9) . . ?
C11 Os1 Sn1 162.15(11) . . ?
S1 Os1 Sn1 105.23(2) . . ?
C2 Os1 Os2 92.06(13) . . ?
C1 Os1 Os2 129.11(13) . . ?
N1 Os1 Os2 90.14(9) . . ?
C11 Os1 Os2 142.88(11) . . ?
S1 Os1 Os2 50.35(2) . . ?
Sn1 Os1 Os2 54.965(7) . . ?
C5 Os2 C3 91.51(18) . . ?
C5 Os2 C4 90.69(18) . . ?
C3 Os2 C4 177.61(17) . . ?
C5 Os2 S1 107.85(13) . . ?
C3 Os2 S1 90.03(13) . . ?
C4 Os2 S1 88.41(12) . . ?
C5 Os2 Sn1 139.30(13) . . ?
C3 Os2 Sn1 93.01(13) . . ?
C4 Os2 Sn1 85.92(12) . . ?
S1 Os2 Sn1 112.57(3) . . ?
C5 Os2 Os3 83.42(13) . . ?
C3 Os2 Os3 86.47(13) . . ?
C4 Os2 Os3 94.71(12) . . ?
S1 Os2 Os3 168.30(3) . . ?
Sn1 Os2 Os3 56.565(7) . . ?
C5 Os2 Os1 158.74(13) . . ?
C3 Os2 Os1 89.61(13) . . ?
C4 Os2 Os1 88.00(12) . . ?
S1 Os2 Os1 50.91(2) . . ?
Sn1 Os2 Os1 61.769(7) . . ?
Os3 Os2 Os1 117.836(7) . . ?
C8 Os3 C9 110.48(19) . . ?
C8 Os3 C6 89.38(19) . . ?
C9 Os3 C6 92.91(19) . . ?
C8 Os3 C7 93.59(18) . . ?
C9 Os3 C7 90.52(19) . . ?
C6 Os3 C7 174.38(18) . . ?
C8 Os3 Sn1 92.51(14) . . ?
C9 Os3 Sn1 156.99(13) . . ?
C6 Os3 Sn1 87.97(13) . . ?
C7 Os3 Sn1 87.14(14) . . ?
C8 Os3 Os2 150.24(14) . . ?
C9 Os3 Os2 99.19(13) . . ?
C6 Os3 Os2 91.48(13) . . ?
C7 Os3 Os2 83.57(12) . . ?
Sn1 Os3 Os2 57.808(7) . . ?
C41 Sn1 C31 104.30(16) . . ?
C41 Sn1 Os3 108.19(11) . . ?
C31 Sn1 Os3 107.68(11) . . ?
C41 Sn1 Os2 131.47(11) . . ?
C31 Sn1 Os2 123.79(11) . . ?
Os3 Sn1 Os2 65.627(8) . . ?
C41 Sn1 Os1 99.43(11) . . ?
C31 Sn1 Os1 106.54(11) . . ?
Os3 Sn1 Os1 128.270(11) . . ?
Os2 Sn1 Os1 63.266(7) . . ?
C21 S1 Os2 112.28(14) . . ?
C21 S1 Os1 118.03(15) . . ?
Os2 S1 Os1 78.74(3) . . ?
O1 C1 Os1 176.2(4) . . ?
O2 C2 Os1 177.1(4) . . ?
O3 C3 Os2 177.3(4) . . ?
O4 C4 Os2 177.6(4) . . ?
O5 C5 Os2 177.9(4) . . ?
O6 C6 Os3 178.6(4) . . ?
O7 C7 Os3 178.8(4) . . ?
O8 C8 Os3 178.6(4) . . ?
O9 C9 Os3 176.1(4) . . ?
C16 C11 C12 116.6(4) . . ?
C16 C11 Os1 122.9(3) . . ?
C12 C11 Os1 120.4(3) . . ?
C13 C12 C11 121.3(4) . . ?
C14 C13 C12 120.5(4) . . ?
C15 C14 C13 119.2(4) . . ?
C14 C15 C16 120.2(4) . . ?
C15 C16 C11 122.1(4) . . ?
C26 C21 C22 120.0(4) . . ?
C26 C21 S1 122.3(3) . . ?
C22 C21 S1 117.2(3) . . ?
C23 C22 C21 119.4(4) . . ?
C24 C23 C22 121.0(5) . . ?
C23 C24 C25 119.6(4) . . ?
C26 C25 C24 120.4(4) . . ?
C25 C26 C21 119.6(4) . . ?
C36 C31 C32 117.3(4) . . ?
C36 C31 Sn1 123.9(3) . . ?
C32 C31 Sn1 118.7(3) . . ?
C33 C32 C31 120.9(4) . . ?
C34 C33 C32 120.5(4) . . ?
C35 C34 C33 119.4(4) . . ?
C34 C35 C36 120.4(4) . . ?
C31 C36 C35 121.4(4) . . ?
C46 C41 C42 117.5(4) . . ?
C46 C41 Sn1 123.4(3) . . ?
C42 C41 Sn1 119.0(3) . . ?
C41 C42 C43 121.1(4) . . ?
C44 C43 C42 119.9(5) . . ?
C43 C44 C45 119.9(4) . . ?
C46 C45 C44 119.9(4) . . ?
C45 C46 C41 121.6(4) . . ?
C51 N1 Os1 173.0(3) . . ?
N1 C51 C52 178.7(5) . . ?
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
Os1 C2 1.873(4) . ?
Os1 C1 1.899(4) . ?
Os1 N1 2.105(4) . ?
Os1 C11 2.135(4) . ?
Os1 S1 2.4050(10) . ?
Os1 Sn1 2.9981(3) . ?
Os1 Os2 3.0391(2) . ?
Os2 C5 1.890(5) . ?
Os2 C3 1.952(4) . ?
Os2 C4 1.953(4) . ?
Os2 S1 2.3860(10) . ?
Os2 Sn1 2.7862(3) . ?
Os2 Os3 2.9990(2) . ?
Os3 C8 1.904(5) . ?
Os3 C9 1.947(5) . ?
Os3 C6 1.952(5) . ?
Os3 C7 1.957(4) . ?
Os3 Sn1 2.7476(3) . ?
Sn1 C41 2.171(4) . ?
Sn1 C31 2.174(4) . ?
S1 C21 1.790(4) . ?
C1 O1 1.154(5) . ?
C2 O2 1.151(5) . ?
C3 O3 1.145(5) . ?
C4 O4 1.141(5) . ?
C5 O5 1.152(5) . ?
C6 O6 1.139(5) . ?
C7 O7 1.128(5) . ?
C8 O8 1.148(5) . ?
C9 O9 1.145(6) . ?
C11 C16 1.401(6) . ?
C11 C12 1.411(6) . ?
C12 C13 1.393(6) . ?
C13 C14 1.390(7) . ?
C14 C15 1.385(7) . ?
C15 C16 1.393(6) . ?
C21 C26 1.396(6) . ?
C21 C22 1.401(6) . ?
C22 C23 1.389(7) . ?
C23 C24 1.377(7) . ?
C24 C25 1.394(7) . ?
C25 C26 1.393(6) . ?
C31 C36 1.388(6) . ?
C31 C32 1.405(6) . ?
C32 C33 1.393(6) . ?
C33 C34 1.383(6) . ?
C34 C35 1.370(6) . ?
C35 C36 1.400(6) . ?
C41 C46 1.391(6) . ?
C41 C42 1.396(6) . ?
C42 C43 1.397(7) . ?
C43 C44 1.375(7) . ?
C44 C45 1.385(7) . ?
C45 C46 1.384(6) . ?
N1 C51 1.145(5) . ?
C51 C52 1.461(6) . ?
