#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/85/7008515.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_7008515
loop_
_publ_author_name
'Lau, Jasmine Po-Kwan'
'Wong, Wing-Tak'
_publ_section_title
;
 Synthesis and structural characterization of a series of high-hydride
 content osmium-rhodium carbonyl complexes by the hydrogenation of
 arene-coordinated clusters.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2579
_journal_page_last               2587
_journal_paper_doi               10.1039/b503833b
_journal_year                    2005
_chemical_formula_moiety         'C19 H9 O12 Os4 Rh '
_chemical_formula_sum            'C19 H9 O12 Os4 Rh'
_chemical_formula_weight         1292.98
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2005-02-01
_audit_creation_method           'by CrystalStructure v3.5.1'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.24(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.605(2)
_cell_length_b                   16.268(5)
_cell_length_c                   17.416(5)
_cell_measurement_reflns_used    15317
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.2
_cell_volume                     2431.3(12)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction
'SAINT & CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2003)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'CrystalStructure Ver. 3.5.1'
_computing_structure_refinement  'CRYSTALS (Watkin et al., 1996)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.9722
_diffrn_measured_fraction_theta_max 0.9722
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15317
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_exptl_absorpt_coefficient_mu    21.539
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2272.00
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.31
_refine_diff_density_min         -1.37
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     333
_refine_ls_number_reflns         3964
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0002Fo² + 1.0000σ(Fo²) + 0.0001]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0290
_reflns_number_gt                3947
_reflns_number_total             5632
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            b503833b.txt
_cod_data_source_block           wt0912w
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C19 H9 O12 Os4 Rh '
_cod_database_code               7008515
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-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
Os(1) Os 0.09786(4) 0.27242(2) 0.20001(2) 0.02947(10) Uani 1.00 1 d . . .
Os(2) Os 0.31257(5) 0.38529(2) 0.15406(2) 0.03400(11) Uani 1.00 1 d . . .
Os(3) Os 0.41893(4) 0.23140(2) 0.20505(2) 0.02941(10) Uani 1.00 1 d . . .
Os(4) Os 0.19638(4) 0.11751(2) 0.15385(2) 0.03113(11) Uani 1.00 1 d . . .
Rh(1) Rh 0.24568(8) 0.25099(5) 0.06751(4) 0.0284(2) Uani 1.00 1 d . . .
O(1) O -0.1648(9) 0.3305(6) 0.0867(5) 0.070(3) Uani 1.00 1 d . . .
O(2) O -0.1065(10) 0.1540(5) 0.2823(5) 0.069(3) Uani 1.00 1 d . . .
O(3) O 0.0391(10) 0.4118(5) 0.3113(4) 0.057(3) Uani 1.00 1 d . . .
O(4) O 0.3605(10) 0.5008(5) 0.2904(5) 0.069(3) Uani 1.00 1 d . . .
O(5) O 0.0859(11) 0.5045(6) 0.0742(5) 0.081(3) Uani 1.00 1 d . . .
O(6) O 0.5809(10) 0.4492(5) 0.0678(5) 0.061(3) Uani 1.00 1 d . . .
O(7) O 0.6446(11) 0.3525(6) 0.2865(6) 0.091(4) Uani 1.00 1 d . . .
O(8) O 0.6557(10) 0.1690(6) 0.0969(5) 0.069(3) Uani 1.00 1 d . . .
O(9) O 0.5102(10) 0.1079(5) 0.3318(4) 0.061(3) Uani 1.00 1 d . . .
O(10) O 0.3932(10) -0.0028(6) 0.0713(5) 0.075(3) Uani 1.00 1 d . . .
O(11) O -0.0954(9) 0.0459(5) 0.0700(5) 0.055(3) Uani 1.00 1 d . . .
O(12) O 0.1842(10) 0.0095(6) 0.2953(5) 0.072(3) Uani 1.00 1 d . . .
C(1) C -0.0691(13) 0.3063(7) 0.1289(6) 0.046(3) Uani 1.00 1 d . . .
C(2) C -0.0249(13) 0.1936(6) 0.2498(6) 0.044(3) Uani 1.00 1 d . . .
C(3) C 0.0639(12) 0.3615(7) 0.2678(6) 0.040(3) Uani 1.00 1 d . . .
C(4) C 0.3466(13) 0.4586(6) 0.2373(7) 0.045(3) Uani 1.00 1 d . . .
C(5) C 0.1731(13) 0.4592(6) 0.1037(6) 0.042(3) Uani 1.00 1 d . . .
C(6) C 0.484(1) 0.4238(7) 0.1009(6) 0.044(3) Uani 1.00 1 d . . .
C(7) C 0.554(1) 0.3126(7) 0.2534(7) 0.053(4) Uani 1.00 1 d . . .
C(8) C 0.5684(13) 0.1939(7) 0.1379(6) 0.048(3) Uani 1.00 1 d . . .
C(9) C 0.4730(12) 0.1521(6) 0.2831(6) 0.039(3) Uani 1.00 1 d . . .
C(10) C 0.321(1) 0.0431(7) 0.1033(6) 0.045(3) Uani 1.00 1 d . . .
C(11) C 0.0107(13) 0.0749(7) 0.1021(6) 0.040(3) Uani 1.00 1 d . . .
C(12) C 0.1856(12) 0.0486(6) 0.2398(7) 0.043(3) Uani 1.00 1 d . . .
C(13) C 0.1270(13) 0.3103(7) -0.0415(5) 0.044(3) Uani 1.00 1 d . . .
C(14) C 0.285(1) 0.3334(7) -0.0375(6) 0.048(4) Uani 1.00 1 d . . .
C(15) C 0.4005(13) 0.2706(7) -0.0327(6) 0.046(3) Uani 1.00 1 d . . .
C(16) C 0.354(2) 0.1886(8) -0.0337(6) 0.056(4) Uani 1.00 1 d . . .
C(17) C 0.1903(13) 0.1681(7) -0.0397(5) 0.041(3) Uani 1.00 1 d . . .
C(18) C 0.0773(13) 0.2294(7) -0.0439(5) 0.044(3) Uani 1.00 1 d . . .
C(19) C -0.096(1) 0.2087(9) -0.0554(6) 0.068(4) Uani 1.00 1 d . . .
H(1) H 0.0505(13) 0.3524(7) -0.0426(5) 0.053(3) Uiso 1.00 1 c . . .
H(2) H 0.314(1) 0.3898(7) -0.0379(6) 0.058(4) Uiso 1.00 1 c . . .
H(3) H 0.5080(13) 0.2845(7) -0.0289(6) 0.056(4) Uiso 1.00 1 c . . .
H(4) H 0.430(2) 0.1462(8) -0.0305(6) 0.068(4) Uiso 1.00 1 c . . .
H(5) H 0.1595(13) 0.1120(7) -0.0408(5) 0.049(3) Uiso 1.00 1 c . . .
H(6) H -0.149(1) 0.2315(9) -0.0144(6) 0.081(5) Uiso 1.00 1 c . . .
H(7) H -0.138(1) 0.2311(9) -0.1029(6) 0.081(5) Uiso 1.00 1 c . . .
H(8) H -0.109(1) 0.1508(9) -0.0560(6) 0.081(5) Uiso 1.00 1 c . . .
H(9) H 0.2642 0.2523 0.2647 0.0380 Uiso 1.00 1 c . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Os Os -1.216 7.603
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Rh Rh -1.118 0.919
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
Rh(1) Os(4) C(10) 98.0(3) yes . . .
Rh(1) Os(4) C(11) 101.0(3) yes . . .
Rh(1) Os(4) C(12) 161.0(3) yes . . .
Rh(1) Os(4) Os(1) 59.82(2) yes . . .
Rh(1) Os(4) Os(3) 60.38(2) yes . . .
C(10) Os(4) C(11) 91.8(5) yes . . .
C(10) Os(4) C(12) 93.0(5) yes . . .
C(10) Os(4) Os(1) 155.6(3) yes . . .
C(10) Os(4) Os(3) 100.2(3) yes . . .
C(11) Os(4) C(12) 94.0(4) yes . . .
C(11) Os(4) Os(1) 101.7(3) yes . . .
C(11) Os(4) Os(3) 158.9(3) yes . . .
C(12) Os(4) Os(1) 106.0(3) yes . . .
C(12) Os(4) Os(3) 102.5(3) yes . . .
Os(1) Os(4) Os(3) 61.36(1) yes . . .
C(13) Rh(1) C(14) 35.5(4) yes . . .
C(13) Rh(1) C(15) 64.0(4) yes . . .
C(13) Rh(1) C(16) 74.4(4) yes . . .
C(13) Rh(1) C(17) 61.9(4) yes . . .
C(13) Rh(1) C(18) 34.5(4) yes . . .
C(13) Rh(1) Os(1) 115.9(3) yes . . .
C(13) Rh(1) Os(2) 100.7(3) yes . . .
C(13) Rh(1) Os(3) 161.5(3) yes . . .
C(13) Rh(1) Os(4) 136.1(3) yes . . .
C(14) Rh(1) C(15) 36.0(4) yes . . .
C(14) Rh(1) C(16) 63.7(4) yes . . .
C(14) Rh(1) C(17) 74.6(4) yes . . .
C(14) Rh(1) C(18) 63.4(4) yes . . .
C(14) Rh(1) Os(1) 134.1(3) yes . . .
C(14) Rh(1) Os(2) 86.2(3) yes . . .
C(14) Rh(1) Os(3) 131.0(3) yes . . .
C(14) Rh(1) Os(4) 161.4(3) yes . . .
C(15) Rh(1) C(16) 35.4(4) yes . . .
C(15) Rh(1) C(17) 64.3(4) yes . . .
C(15) Rh(1) C(18) 75.6(4) yes . . .
C(15) Rh(1) Os(1) 162.8(3) yes . . .
C(15) Rh(1) Os(2) 101.6(3) yes . . .
C(15) Rh(1) Os(3) 111.8(3) yes . . .
C(15) Rh(1) Os(4) 131.4(3) yes . . .
C(16) Rh(1) C(17) 36.4(4) yes . . .
C(16) Rh(1) C(18) 64.0(4) yes . . .
C(16) Rh(1) Os(1) 161.0(3) yes . . .
C(16) Rh(1) Os(2) 135.1(3) yes . . .
C(16) Rh(1) Os(3) 113.3(3) yes . . .
C(16) Rh(1) Os(4) 99.3(3) yes . . .
C(17) Rh(1) C(18) 34.6(4) yes . . .
C(17) Rh(1) Os(1) 132.1(3) yes . . .
C(17) Rh(1) Os(2) 160.6(3) yes . . .
C(17) Rh(1) Os(3) 134.4(3) yes . . .
C(17) Rh(1) Os(4) 87.1(3) yes . . .
C(18) Rh(1) Os(1) 114.6(3) yes . . .
C(18) Rh(1) Os(2) 132.3(3) yes . . .
C(18) Rh(1) Os(3) 163.9(3) yes . . .
C(18) Rh(1) Os(4) 103.1(3) yes . . .
Os(1) Rh(1) Os(2) 61.20(2) yes . . .
Os(1) Rh(1) Os(3) 62.32(2) yes . . .
Os(2) Rh(1) Os(3) 61.69(2) yes . . .
Os(2) Rh(1) Os(4) 112.19(3) yes . . .
Os(4) Rh(1) Os(1) 61.96(2) yes . . .
Os(4) Rh(1) Os(3) 61.11(2) yes . . .
Os(1) C(1) O(1) 176(1) yes . . .
Os(1) C(2) O(2) 172(1) yes . . .
Os(1) C(3) O(3) 175.8(9) yes . . .
Os(2) C(4) O(4) 175(1) yes . . .
Os(2) C(5) O(5) 178(1) yes . . .
Os(2) C(6) O(6) 176(1) yes . . .
Os(3) C(7) O(7) 171(1) yes . . .
Os(3) C(8) O(8) 177(1) yes . . .
Os(3) C(9) O(9) 176.2(8) yes . . .
Os(4) C(10) O(10) 178.1(9) yes . . .
Os(4) C(11) O(11) 176(1) yes . . .
Os(4) C(12) O(12) 176.0(9) yes . . .
C(14) C(13) C(18) 123(1) yes . . .
C(14) C(13) H(1) 118(1) no . . .
C(18) C(13) H(1) 118(1) no . . .
H(1) C(13) Rh(1) 125.7(9) no . . .
Rh(1) C(13) C(14) 72.7(6) yes . . .
Rh(1) C(13) C(18) 75.2(6) yes . . .
C(15) C(14) H(2) 120(1) no . . .
H(2) C(14) Rh(1) 128(1) no . . .
H(2) C(14) C(13) 120(1) no . . .
Rh(1) C(14) C(15) 71.3(6) yes . . .
Rh(1) C(14) C(13) 71.8(6) yes . . .
C(13) C(14) C(15) 118(1) yes . . .
C(16) C(15) H(3) 120(1) no . . .
H(3) C(15) Rh(1) 126.7(9) no . . .
H(3) C(15) C(14) 120(1) no . . .
Rh(1) C(15) C(16) 72.1(6) yes . . .
Rh(1) C(15) C(14) 72.6(6) yes . . .
C(14) C(15) C(16) 119(1) yes . . .
C(17) C(16) H(4) 119(1) no . . .
H(4) C(16) Rh(1) 126(1) no . . .
H(4) C(16) C(15) 119(1) no . . .
Rh(1) C(16) C(17) 73.1(6) yes . . .
Rh(1) C(16) C(15) 72.5(6) yes . . .
C(15) C(16) C(17) 120(1) yes . . .
C(18) C(17) H(5) 119(1) no . . .
H(5) C(17) Rh(1) 127.9(9) no . . .
H(5) C(17) C(16) 119(1) no . . .
Rh(1) C(17) C(18) 74.2(6) yes . . .
Rh(1) C(17) C(16) 70.5(6) yes . . .
C(16) C(17) C(18) 120(1) yes . . .
C(19) C(18) Rh(1) 132.4(7) yes . . .
C(19) C(18) C(13) 120(1) yes . . .
C(19) C(18) C(17) 121(1) yes . . .
Rh(1) C(18) C(13) 70.3(6) yes . . .
Rh(1) C(18) C(17) 71.3(6) yes . . .
C(13) C(18) C(17) 117(1) yes . . .
H(6) C(19) H(7) 109(1) no . . .
H(6) C(19) H(8) 109(1) no . . .
H(6) C(19) C(18) 109(1) no . . .
H(7) C(19) H(8) 109(1) no . . .
H(7) C(19) C(18) 109(1) no . . .
H(8) C(19) C(18) 109(1) no . . .
Os(1) H(9) Os(3) 105 no . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Os(1) Os(2) 2.7648(5) yes . .
Os(1) Os(3) 2.8373(5) yes . .
Os(1) Os(4) 2.7958(5) yes . .
Os(1) Rh(1) 2.7384(8) yes . .
Os(1) C(1) 1.91(1) yes . .
Os(1) C(2) 1.91(1) yes . .
Os(1) C(3) 1.91(1) yes . .
Os(1) H(9) 1.79 no . .
Os(2) Os(3) 2.7881(5) yes . .
Os(2) Rh(1) 2.6923(8) yes . .
Os(2) C(4) 1.88(1) yes . .
Os(2) C(5) 1.87(1) yes . .
Os(2) C(6) 1.90(1) yes . .
Os(3) Os(4) 2.7646(5) yes . .
Os(3) Rh(1) 2.7448(8) yes . .
Os(3) C(7) 1.91(1) yes . .
Os(3) C(8) 1.90(1) yes . .
Os(3) C(9) 1.91(1) yes . .
Os(3) H(9) 1.78 no . .
Os(4) Rh(1) 2.6927(8) yes . .
Os(4) C(10) 1.88(1) yes . .
Os(4) C(11) 1.91(1) yes . .
Os(4) C(12) 1.88(1) yes . .
Rh(1) C(13) 2.30(1) yes . .
Rh(1) C(14) 2.31(1) yes . .
Rh(1) C(15) 2.29(1) yes . .
Rh(1) C(16) 2.29(1) yes . .
Rh(1) C(17) 2.32(1) yes . .
Rh(1) C(18) 2.36(1) yes . .
O(1) C(1) 1.13(1) yes . .
O(2) C(2) 1.13(1) yes . .
O(3) C(3) 1.15(1) yes . .
O(4) C(4) 1.15(1) yes . .
O(5) C(5) 1.15(1) yes . .
O(6) C(6) 1.13(1) yes . .
O(7) C(7) 1.14(1) yes . .
O(8) C(8) 1.15(1) yes . .
O(9) C(9) 1.14(1) yes . .
O(10) C(10) 1.14(1) yes . .
O(11) C(11) 1.14(1) yes . .
O(12) C(12) 1.16(1) yes . .
C(13) C(14) 1.40(2) yes . .
C(13) C(18) 1.38(2) yes . .
C(13) H(1) 0.95(2) no . .
C(14) C(15) 1.43(2) yes . .
C(14) H(2) 0.95(2) no . .
C(15) C(16) 1.39(2) yes . .
C(15) H(3) 0.95(2) no . .
C(16) C(17) 1.44(2) yes . .
C(16) H(4) 0.95(2) no . .
C(17) C(18) 1.39(2) yes . .
C(17) H(5) 0.95(2) no . .
C(18) C(19) 1.53(2) yes . .
C(19) H(6) 0.95(2) no . .
C(19) H(7) 0.95(2) no . .
C(19) H(8) 0.95(2) no . .
