#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:29:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179113 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/75/4307542.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_4307542
loop_
_publ_author_name
'Richard D. Adams'
'Erin M. Boswell'
'Burjor Captain'
'Mitul A. Patel'
_publ_section_title
;
Multiple Additions of Phenylgermanium Ligands to Tetraruthenium and
Tetraosmium Carbonyl Cluster Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              533
_journal_page_last               540
_journal_paper_doi               10.1021/ic062039w
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C46 H30 Ge4 O10 Ru4'
_chemical_formula_weight         1437.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.5700(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.5604(6)
_cell_length_b                   23.3208(14)
_cell_length_c                   11.4639(7)
_cell_measurement_reflns_used    2515
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      23.34
_cell_measurement_theta_min      2.47
_cell_volume                     2360.2(3)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12460
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    3.809
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.578
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0476P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                2892
_reflns_number_total             4117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062039wsi20061024_100643_1.cif
_cod_data_source_block           Compound11
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4307542
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
Ru1 Ru 0.40596(7) 0.05157(2) 0.59493(5) 0.04317(18) Uani 1 1 d . . .
Ru2 Ru 0.64278(7) 0.06284(2) 0.49054(5) 0.04089(17) Uani 1 1 d . . .
Ge1 Ge 0.38024(10) 0.01991(3) 0.37144(6) 0.0431(2) Uani 1 1 d . . .
Ge2 Ge 0.54667(10) 0.14054(3) 0.58921(7) 0.0461(2) Uani 1 1 d . . .
O1 O 0.1537(9) -0.0146(2) 0.6351(7) 0.087(2) Uani 1 1 d . . .
O11 O 0.4758(11) 0.0601(3) 0.8788(6) 0.113(3) Uani 1 1 d . . .
O12 O 0.1340(8) 0.1315(3) 0.5090(6) 0.087(2) Uani 1 1 d . . .
O21 O 0.6320(8) 0.1460(2) 0.2812(6) 0.090(2) Uani 1 1 d . . .
O22 O 0.9608(7) 0.0920(2) 0.6752(6) 0.0734(18) Uani 1 1 d . . .
C1 C 0.2506(11) -0.0105(3) 0.5989(7) 0.057(2) Uani 1 1 d . . .
C11 C 0.4550(12) 0.0590(3) 0.7728(8) 0.068(3) Uani 1 1 d . . .
C12 C 0.2384(12) 0.1021(3) 0.5402(8) 0.065(2) Uani 1 1 d . . .
C21 C 0.6346(10) 0.1173(3) 0.3610(7) 0.054(2) Uani 1 1 d . . .
C22 C 0.8420(10) 0.0823(3) 0.6081(7) 0.052(2) Uani 1 1 d . . .
C40 C 0.2229(10) 0.0452(3) 0.2146(6) 0.050(2) Uani 1 1 d . . .
C41 C 0.0788(11) 0.0557(3) 0.2098(8) 0.068(2) Uani 1 1 d . . .
H41 H 0.0578 0.0504 0.2818 0.081 Uiso 1 1 calc R . .
C42 C -0.0352(12) 0.0741(4) 0.0992(9) 0.082(3) Uani 1 1 d . . .
H42 H -0.1322 0.0809 0.0965 0.098 Uiso 1 1 calc R . .
C43 C -0.0025(13) 0.0823(4) -0.0073(9) 0.078(3) Uani 1 1 d . . .
H43 H -0.0777 0.0960 -0.0808 0.094 Uiso 1 1 calc R . .
C44 C 0.1365(12) 0.0707(4) -0.0066(7) 0.074(3) Uani 1 1 d . . .
H44 H 0.1552 0.0747 -0.0801 0.088 Uiso 1 1 calc R . .
C45 C 0.2516(11) 0.0527(3) 0.1050(7) 0.062(2) Uani 1 1 d . . .
H45 H 0.3479 0.0456 0.1064 0.074 Uiso 1 1 calc R . .
C46 C 0.4287(9) 0.2028(3) 0.4822(6) 0.0488(19) Uani 1 1 d . . .
C47 C 0.3421(10) 0.1953(3) 0.3533(7) 0.059(2) Uani 1 1 d . . .
H47 H 0.3395 0.1596 0.3164 0.071 Uiso 1 1 calc R . .
C48 C 0.2609(11) 0.2400(4) 0.2808(8) 0.077(3) Uani 1 1 d . . .
H48 H 0.2051 0.2344 0.1951 0.092 Uiso 1 1 calc R . .
C49 C 0.2614(12) 0.2927(3) 0.3334(10) 0.081(3) Uani 1 1 d . . .
H49 H 0.2071 0.3230 0.2841 0.098 Uiso 1 1 calc R . .
C50 C 0.3442(12) 0.2999(3) 0.4612(10) 0.084(3) Uani 1 1 d . . .
H50 H 0.3423 0.3351 0.4988 0.101 Uiso 1 1 calc R . .
C51 C 0.4290(10) 0.2560(3) 0.5334(8) 0.059(2) Uani 1 1 d . . .
H51 H 0.4875 0.2623 0.6184 0.071 Uiso 1 1 calc R . .
C52 C 0.6853(10) 0.1787(3) 0.7436(6) 0.051(2) Uani 1 1 d . . .
C53 C 0.8095(11) 0.2065(3) 0.7435(8) 0.065(2) Uani 1 1 d . . .
H53 H 0.8317 0.2054 0.6713 0.078 Uiso 1 1 calc R . .
C54 C 0.9039(11) 0.2366(4) 0.8474(9) 0.081(3) Uani 1 1 d . . .
H54 H 0.9874 0.2559 0.8440 0.097 Uiso 1 1 calc R . .
C55 C 0.8760(12) 0.2382(4) 0.9529(9) 0.083(3) Uani 1 1 d . . .
H55 H 0.9408 0.2582 1.0230 0.100 Uiso 1 1 calc R . .
C56 C 0.7528(13) 0.2106(4) 0.9584(9) 0.086(3) Uani 1 1 d . . .
H56 H 0.7336 0.2114 1.0320 0.103 Uiso 1 1 calc R . .
C57 C 0.6569(11) 0.1813(4) 0.8530(7) 0.072(3) Uani 1 1 d . . .
H57 H 0.5718 0.1631 0.8558 0.087 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'
Ge Ge 0.1547 1.8001 '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'
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
C12 Ru1 C11 97.3(4) . . ?
C12 Ru1 C1 85.5(4) . . ?
C11 Ru1 C1 85.7(3) . . ?
C12 Ru1 Ge2 82.5(3) . . ?
C11 Ru1 Ge2 92.2(3) . . ?
C1 Ru1 Ge2 167.4(2) . . ?
C12 Ru1 Ge1 170.2(2) . 3_656 ?
C11 Ru1 Ge1 92.5(3) . 3_656 ?
C1 Ru1 Ge1 94.5(2) . 3_656 ?
Ge2 Ru1 Ge1 98.00(3) . 3_656 ?
C12 Ru1 Ge1 95.9(3) . . ?
C11 Ru1 Ge1 166.2(2) . . ?
C1 Ru1 Ge1 91.5(2) . . ?
Ge2 Ru1 Ge1 93.37(3) . . ?
Ge1 Ru1 Ge1 74.27(3) 3_656 . ?
C12 Ru1 Ru2 118.0(3) . 3_656 ?
C11 Ru1 Ru2 113.3(2) . 3_656 ?
C1 Ru1 Ru2 47.7(2) . 3_656 ?
Ge2 Ru1 Ru2 143.07(3) . 3_656 ?
Ge1 Ru1 Ru2 56.61(2) 3_656 3_656 ?
Ge1 Ru1 Ru2 56.30(2) . 3_656 ?
C12 Ru1 Ru2 119.6(3) . . ?
C11 Ru1 Ru2 120.7(3) . . ?
C1 Ru1 Ru2 137.2(2) . . ?
Ge2 Ru1 Ru2 53.71(2) . . ?
Ge1 Ru1 Ru2 54.84(2) 3_656 . ?
Ge1 Ru1 Ru2 54.52(2) . . ?
Ru2 Ru1 Ru2 89.63(2) 3_656 . ?
C22 Ru2 C21 96.9(3) . . ?
C22 Ru2 C1 86.8(3) . 3_656 ?
C21 Ru2 C1 83.7(3) . 3_656 ?
C22 Ru2 Ge2 87.0(2) . . ?
C21 Ru2 Ge2 87.6(2) . . ?
C1 Ru2 Ge2 168.6(2) 3_656 . ?
C22 Ru2 Ge1 167.0(2) . . ?
C21 Ru2 Ge1 96.0(2) . . ?
C1 Ru2 Ge1 94.2(2) 3_656 . ?
Ge2 Ru2 Ge1 93.99(3) . . ?
C22 Ru2 Ge1 92.4(2) . 3_656 ?
C21 Ru2 Ge1 169.5(2) . 3_656 ?
C1 Ru2 Ge1 92.1(2) 3_656 3_656 ?
Ge2 Ru2 Ge1 97.68(3) . 3_656 ?
Ge1 Ru2 Ge1 74.63(3) . 3_656 ?
C22 Ru2 Ru1 117.1(2) . 3_656 ?
C21 Ru2 Ru1 113.7(2) . 3_656 ?
C1 Ru2 Ru1 47.5(2) 3_656 3_656 ?
Ge2 Ru2 Ru1 143.69(3) . 3_656 ?
Ge1 Ru2 Ru1 56.38(2) . 3_656 ?
Ge1 Ru2 Ru1 57.24(2) 3_656 3_656 ?
C22 Ru2 Ru1 116.4(2) . . ?
C21 Ru2 Ru1 124.0(3) . . ?
C1 Ru2 Ru1 137.8(2) 3_656 . ?
Ge2 Ru2 Ru1 53.59(2) . . ?
Ge1 Ru2 Ru1 55.45(2) . . ?
Ge1 Ru2 Ru1 54.58(2) 3_656 . ?
Ru1 Ru2 Ru1 90.37(2) 3_656 . ?
C40 Ge1 Ru1 129.0(2) . 3_656 ?
C40 Ge1 Ru2 129.0(2) . . ?
Ru1 Ge1 Ru2 67.01(3) 3_656 . ?
C40 Ge1 Ru2 125.6(2) . 3_656 ?
Ru1 Ge1 Ru2 70.58(3) 3_656 3_656 ?
Ru2 Ge1 Ru2 105.37(3) . 3_656 ?
C40 Ge1 Ru1 125.2(2) . . ?
Ru1 Ge1 Ru1 105.73(3) 3_656 . ?
Ru2 Ge1 Ru1 70.03(3) . . ?
Ru2 Ge1 Ru1 66.46(2) 3_656 . ?
C46 Ge2 C52 104.8(3) . . ?
C46 Ge2 Ru1 116.6(2) . . ?
C52 Ge2 Ru1 122.5(2) . . ?
C46 Ge2 Ru2 118.6(2) . . ?
C52 Ge2 Ru2 119.9(2) . . ?
Ru1 Ge2 Ru2 72.70(3) . . ?
O1 C1 Ru1 137.8(6) . . ?
O1 C1 Ru2 137.4(6) . 3_656 ?
Ru1 C1 Ru2 84.8(3) . 3_656 ?
O11 C11 Ru1 174.5(9) . . ?
O12 C12 Ru1 177.4(8) . . ?
O21 C21 Ru2 175.2(7) . . ?
O22 C22 Ru2 177.3(8) . . ?
C41 C40 C45 118.6(7) . . ?
C41 C40 Ge1 119.9(6) . . ?
C45 C40 Ge1 121.5(7) . . ?
C40 C41 C42 121.0(9) . . ?
C43 C42 C41 119.0(10) . . ?
C44 C43 C42 121.4(8) . . ?
C43 C44 C45 119.5(9) . . ?
C44 C45 C40 120.4(9) . . ?
C51 C46 C47 117.9(6) . . ?
C51 C46 Ge2 119.8(5) . . ?
C47 C46 Ge2 122.3(5) . . ?
C48 C47 C46 120.8(7) . . ?
C49 C48 C47 120.6(8) . . ?
C48 C49 C50 118.7(8) . . ?
C51 C50 C49 120.9(8) . . ?
C50 C51 C46 121.0(8) . . ?
C53 C52 C57 117.2(8) . . ?
C53 C52 Ge2 120.3(6) . . ?
C57 C52 Ge2 122.4(7) . . ?
C52 C53 C54 121.8(9) . . ?
C55 C54 C53 120.2(10) . . ?
C54 C55 C56 120.3(9) . . ?
C55 C56 C57 119.1(9) . . ?
C52 C57 C56 121.2(10) . . ?
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
Ru1 C12 1.892(9) . ?
Ru1 C11 1.917(8) . ?
Ru1 C1 2.087(8) . ?
Ru1 Ge2 2.4871(9) . ?
Ru1 Ge1 2.5497(10) 3_656 ?
Ru1 Ge1 2.5857(9) . ?
Ru1 Ru2 2.8188(7) 3_656 ?
Ru1 Ru2 2.9508(9) . ?
Ru2 C22 1.918(9) . ?
Ru2 C21 1.933(7) . ?
Ru2 C1 2.093(8) 3_656 ?
Ru2 Ge2 2.4910(9) . ?
Ru2 Ge1 2.5565(10) . ?
Ru2 Ge1 2.5580(8) 3_656 ?
Ru2 Ru1 2.8188(7) 3_656 ?
Ge1 C40 1.940(7) . ?
Ge1 Ru1 2.5497(10) 3_656 ?
Ge1 Ru2 2.5580(8) 3_656 ?
Ge2 C46 1.955(6) . ?
Ge2 C52 1.969(7) . ?
O1 C1 1.155(10) . ?
O11 C11 1.153(9) . ?
O12 C12 1.148(10) . ?
O21 C21 1.125(8) . ?
O22 C22 1.123(9) . ?
C1 Ru2 2.093(8) 3_656 ?
C40 C41 1.380(12) . ?
C40 C45 1.396(11) . ?
C41 C42 1.385(11) . ?
C42 C43 1.384(14) . ?
C43 C44 1.353(13) . ?
C44 C45 1.394(11) . ?
C46 C51 1.372(9) . ?
C46 C47 1.400(9) . ?
C47 C48 1.373(10) . ?
C48 C49 1.368(12) . ?
C49 C50 1.383(12) . ?
C50 C51 1.370(11) . ?
C52 C53 1.354(12) . ?
C52 C57 1.383(11) . ?
C53 C54 1.378(11) . ?
C54 C55 1.337(13) . ?
C55 C56 1.364(14) . ?
C56 C57 1.384(11) . ?
