#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:19:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178845 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/99/4109987.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_4109987
loop_
_publ_author_name
'Richard D. Adams'
'Burjor Captain'
'Michael B. Hall'
'Eszter Trufan'
'Xinzheng Yang'
_publ_section_title
;
 Synthesis, Characterization, and Electronic Structures of a Series of
 Two-Dimensional Trimetallic Cluster Complexes,
 Ru3(CO)9(μ-SnPh2)3[Pt(PBut3)]x, x = 0-3
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12328
_journal_page_last               12340
_journal_paper_doi               10.1021/ja074527o
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C81 H111 O9 P3 Pt3 Ru3 Sn3'
_chemical_formula_weight         2566.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   18.5176(2)
_cell_length_b                   18.5176(2)
_cell_length_c                   16.4848(3)
_cell_measurement_reflns_used    8596
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.47
_cell_volume                     4895.35(12)
_computing_cell_refinement       'SAINT+  V6.45 (Bruker, 2003)'
_computing_data_collection       'SMART V5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT+  V6.45'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36758
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    5.563
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.424
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       block
_exptl_crystal_F_000             2460
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.190
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         4201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0366
_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)+(0.0790P)²+4.1542P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1428
_reflns_number_gt                3369
_reflns_number_total             4201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja074527osi20070620_051920.cif
_cod_data_source_block           etru3sns
_cod_database_code               4109987
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
Pt1 Pt 0.404992(19) 0.478724(19) 0.2500 0.04942(14) Uani 1 2 d S
Ru1 Ru 0.39695(4) 0.62361(4) 0.2500 0.04519(18) Uani 1 2 d S
Sn1 Sn 0.25540(4) 0.47577(4) 0.2500 0.0623(2) Uani 1 2 d S
P1 P 0.44424(14) 0.37840(14) 0.2500 0.0515(5) Uani 1 2 d S
O11 O 0.4084(5) 0.6310(4) 0.4348(4) 0.108(2) Uani 1 1 d .
O12 O 0.5605(5) 0.6238(5) 0.2500 0.158(6) Uani 1 2 d S
C11 C 0.4025(5) 0.6290(4) 0.3661(5) 0.0675(18) Uani 1 1 d .
C12 C 0.4891(7) 0.5986(7) 0.2500 0.091(4) Uani 1 2 d S
C21 C 0.2081(6) 0.3970(5) 0.3571(9) 0.100(4) Uani 1 1 d .
C22 C 0.1285(8) 0.3320(8) 0.3646(13) 0.194(9) Uani 1 1 d .
H22 H 0.0905 0.3217 0.3231 0.233 Uiso 1 1 calc R
C23 C 0.1021(12) 0.2794(12) 0.4343(17) 0.217(13) Uani 1 1 d .
H23 H 0.0473 0.2363 0.4394 0.261 Uiso 1 1 calc R
C24 C 0.1582(15) 0.2938(11) 0.4920(13) 0.185(10) Uani 1 1 d .
H24 H 0.1429 0.2569 0.5354 0.222 Uiso 1 1 calc R
C25 C 0.2341(12) 0.3580(8) 0.4900(8) 0.150(6) Uani 1 1 d .
H25 H 0.2713 0.3691 0.5325 0.180 Uiso 1 1 calc R
C26 C 0.2570(9) 0.4095(6) 0.4206(8) 0.116(4) Uani 1 1 d .
H26 H 0.3104 0.4557 0.4193 0.139 Uiso 1 1 calc R
C27 C 0.5084(5) 0.3922(5) 0.3448(5) 0.0714(19) Uani 1 1 d .
C28 C 0.4582(10) 0.3857(13) 0.4183(7) 0.196(9) Uani 1 1 d .
H28A H 0.4841 0.3781 0.4655 0.294 Uiso 1 1 calc R
H28B H 0.4029 0.3390 0.4126 0.294 Uiso 1 1 calc R
H28C H 0.4555 0.4359 0.4241 0.294 Uiso 1 1 calc R
C29 C 0.5388(8) 0.3312(7) 0.3554(7) 0.127(4) Uani 1 1 d .
H29A H 0.5611 0.3250 0.3050 0.190 Uiso 1 1 calc R
H29B H 0.4932 0.2782 0.3719 0.190 Uiso 1 1 calc R
H29C H 0.5816 0.3515 0.3962 0.190 Uiso 1 1 calc R
C30 C 0.5798(11) 0.4776(8) 0.3489(13) 0.222(12) Uani 1 1 d .
H30A H 0.5605 0.5168 0.3436 0.333 Uiso 1 1 calc R
H30B H 0.6180 0.4860 0.3057 0.333 Uiso 1 1 calc R
H30C H 0.6076 0.4858 0.4001 0.333 Uiso 1 1 calc R
C31 C 0.3491(7) 0.2689(6) 0.2500 0.066(2) Uani 1 2 d S
C32 C 0.2948(8) 0.2587(7) 0.3225(10) 0.175(8) Uani 1 1 d .
H32A H 0.2834 0.3038 0.3240 0.263 Uiso 1 1 calc R
H32B H 0.3232 0.2589 0.3713 0.263 Uiso 1 1 calc R
H32C H 0.2433 0.2068 0.3183 0.263 Uiso 1 1 calc R
C33 C 0.3699(10) 0.1979(8) 0.2500 0.132(7) Uani 1 2 d S
H33A H 0.4112 0.2087 0.2907 0.197 Uiso 0.50 1 calc PR
H33B H 0.3912 0.1949 0.1978 0.197 Uiso 0.50 1 calc PR
H33C H 0.3204 0.1459 0.2615 0.197 Uiso 0.50 1 calc PR
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'
Ru Ru -1.2594 0.8363 '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'
Pt Pt -1.7033 8.3905 '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
C12 Pt1 P1 121.1(3) . .
C12 Pt1 Sn1 104.1(3) . .
P1 Pt1 Sn1 134.83(6) . .
C12 Pt1 Ru1 45.8(3) . .
P1 Pt1 Ru1 166.86(6) . .
Sn1 Pt1 Ru1 58.312(17) . .
C11 Ru1 C11 173.9(5) 10_556 .
C11 Ru1 C12 89.0(2) 10_556 .
C11 Ru1 C12 89.0(2) . .
C11 Ru1 Sn1 87.0(2) 10_556 2_665
C11 Ru1 Sn1 87.0(2) . 2_665
C12 Ru1 Sn1 81.6(3) . 2_665
C11 Ru1 Sn1 93.0(2) 10_556 .
C11 Ru1 Sn1 93.0(2) . .
C12 Ru1 Sn1 106.2(3) . .
Sn1 Ru1 Sn1 172.20(3) 2_665 .
C11 Ru1 Pt1 91.30(19) 10_556 .
C11 Ru1 Pt1 91.30(19) . .
C12 Ru1 Pt1 45.6(3) . .
Sn1 Ru1 Pt1 127.28(3) 2_665 .
Sn1 Ru1 Pt1 60.522(18) . .
C11 Ru1 Ru1 91.9(2) 10_556 3_565
C11 Ru1 Ru1 91.9(2) . 3_565
C12 Ru1 Ru1 162.0(3) . 3_565
Sn1 Ru1 Ru1 116.39(3) 2_665 3_565
Sn1 Ru1 Ru1 55.81(3) . 3_565
Pt1 Ru1 Ru1 116.33(3) . 3_565
C11 Ru1 Ru1 88.88(19) 10_556 2_665
C11 Ru1 Ru1 88.88(19) . 2_665
C12 Ru1 Ru1 138.0(3) . 2_665
Sn1 Ru1 Ru1 56.39(3) 2_665 2_665
Sn1 Ru1 Ru1 115.81(3) . 2_665
Pt1 Ru1 Ru1 176.33(3) . 2_665
Ru1 Ru1 Ru1 60.002(1) 3_565 2_665
C21 Sn1 C21 108.5(7) . 10_556
C21 Sn1 Ru1 113.7(2) . 3_565
C21 Sn1 Ru1 113.7(2) 10_556 3_565
C21 Sn1 Ru1 123.0(3) . .
C21 Sn1 Ru1 123.0(3) 10_556 .
Ru1 Sn1 Ru1 67.81(3) 3_565 .
C21 Sn1 Pt1 94.5(2) . .
C21 Sn1 Pt1 94.5(2) 10_556 .
Ru1 Sn1 Pt1 128.97(3) 3_565 .
Ru1 Sn1 Pt1 61.166(17) . .
C27 P1 C27 110.5(5) . 10_556
C27 P1 C31 109.0(3) . .
C27 P1 C31 109.0(3) 10_556 .
C27 P1 Pt1 108.6(2) . .
C27 P1 Pt1 108.6(2) 10_556 .
C31 P1 Pt1 111.1(3) . .
O11 C11 Ru1 176.9(7) . .
O12 C12 Pt1 123.5(9) . .
O12 C12 Ru1 147.9(10) . .
Pt1 C12 Ru1 88.6(4) . .
C26 C21 C22 115.1(13) . .
C26 C21 Sn1 120.8(7) . .
C22 C21 Sn1 124.1(12) . .
C21 C22 C23 121.7(18) . .
C24 C23 C22 118.1(17) . .
C25 C24 C23 122.6(18) . .
C24 C25 C26 117.1(19) . .
C21 C26 C25 125.0(14) . .
C30 C27 C28 103.8(13) . .
C30 C27 C29 109.2(10) . .
C28 C27 C29 107.2(10) . .
C30 C27 P1 110.4(7) . .
C28 C27 P1 109.5(6) . .
C29 C27 P1 116.0(6) . .
C32 C31 C32 104.5(15) . 10_556
C32 C31 C33 109.1(8) . .
C32 C31 C33 109.1(8) 10_556 .
C32 C31 P1 109.6(6) . .
C32 C31 P1 109.6(6) 10_556 .
C33 C31 P1 114.5(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pt1 C12 1.974(11) .
Pt1 P1 2.308(2) .
Pt1 Sn1 2.7432(7) .
Pt1 Ru1 2.7605(6) .
Ru1 C11 1.916(8) 10_556
Ru1 C11 1.916(8) .
Ru1 C12 1.979(10) .
Ru1 Sn1 2.6632(9) 2_665
Ru1 Sn1 2.6814(8) .
Ru1 Ru1 2.9812(10) 3_565
Ru1 Ru1 2.9812(10) 2_665
Sn1 C21 2.176(11) .
Sn1 C21 2.176(11) 10_556
Sn1 Ru1 2.6632(9) 3_565
P1 C27 1.901(7) .
P1 C27 1.901(7) 10_556
P1 C31 1.909(10) .
O11 C11 1.137(10) .
O12 C12 1.161(13) .
C21 C26 1.326(17) .
C21 C22 1.364(14) .
C22 C23 1.43(2) .
C23 C24 1.33(3) .
C24 C25 1.31(2) .
C25 C26 1.413(15) .
C27 C30 1.471(14) .
C27 C28 1.496(15) .
C27 C29 1.503(11) .
C31 C32 1.512(13) .
C31 C32 1.512(13) 10_556
C31 C33 1.544(15) .
