#------------------------------------------------------------------------------
#$Date: 2017-02-19 20:44:19 +0200 (Sun, 19 Feb 2017) $
#$Revision: 192299 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/58/2005855.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2005855
loop_
_publ_author_name
'Leong, W. K.'
'Einstein, F. W. B.'
'Pomeroy, R. K.'
_publ_contact_author
;
Weng Kee Leong
Department of Chemistry
National University of Singapore
Kent Ridge
Singapore 0511
;
_publ_section_title
;
 Bisphenylbis[tetracarbonyl(hydrido)osmio]germane,
 Ph₂Ge[Os(CO)₄H]₂
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              22
_journal_page_last               24
_journal_paper_doi               10.1107/S0108270196012061
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Os2 (H)2 (C O)8 {Ge (C6 H5)2}]'
_chemical_formula_moiety         'C20 H12 Ge O8 Os2'
_chemical_formula_sum            'C20 H12 Ge O8 Os2'
_chemical_formula_weight         833.30
_chemical_name_systematic
;
Di(hydridotetracarbonylosmium)diphenylgermane
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 105.433(14)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   33.775(6)
_cell_length_b                   9.5143(11)
_cell_length_c                   14.987(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      17.00
_cell_measurement_theta_min      15.00
_cell_volume                     4642.4(14)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'NRCVAX DATRD2 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES'
_computing_structure_refinement
'CRYSTALS (Watkin, Carruthers & Betteridge, 1985)'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Nonius CAD-4'
_diffrn_measurement_method       'ω/2θ scan b/P/b'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3227
_diffrn_reflns_theta_max         22.38
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        50
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    12.24
_exptl_absorpt_correction_T_max  0.2593
_exptl_absorpt_correction_T_min  0.1321
_exptl_absorpt_correction_type   'Gaussian integration (Busing & Levy, 1957)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.385
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.6(2)
_refine_diff_density_min         -1.0(2)
_refine_ls_extinction_coef       0.16(3)
_refine_ls_extinction_method     'Larson (1970)'
_refine_ls_goodness_of_fit_obs   3.0
_refine_ls_hydrogen_treatment    'H atoms: see text'
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2340
_refine_ls_number_restraints     16
_refine_ls_R_factor_obs          0.045
_refine_ls_shift/esd_max         0.11
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[0.0001|Fo|²+σ²(Fo)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.055
_reflns_number_observed          2340
_reflns_number_total             2995
_reflns_observed_criterion       'Inet > 2.5\s(Inet)'
_cod_data_source_file            fg1150.cif
_cod_data_source_block           global
_cod_depositor_comments
;
 Marking atoms 'C(100)' and 'C(200)' as dummy atoms.

 Antanas Vaitkus,
 2017-02-19

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 

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.

'_refine_ls_matrix_type' value 'FULL' changed to 'full'
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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[0.0001|Fo|^2^+\s^2^(Fo)]'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[0.0001|Fo|^2^+\s^2^(Fo)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2005855
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
1/2+x,1/2+y,z
1/2-x,1/2-y,-z
-x,y,1/2-z
x,-y,1/2+z
1/2-x,1/2+y,1/2-z
1/2+x,1/2-y,1/2+z
loop_
_atom_site_label
_atom_site_occupancy
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_type_symbol
_atom_site_calc_flag
Os(1) 1.0000 0.58045(2) 0.04319(6) 0.16885(4) 0.0628 Uani Os ?
Os(2) 1.0000 0.58275(2) 0.43598(7) 0.32288(5) 0.0736 Uani Os ?
Ge(1) 1.0000 0.62469(4) 0.2281(1) 0.27946(9) 0.0584 Uani Ge ?
O(11) 1.0000 0.5489(4) -0.014(2) 0.3394(9) 0.1091 Uani O ?
O(12) 1.0000 0.5988(4) 0.222(1) 0.0145(7) 0.0947 Uani O ?
O(13) 1.0000 0.6570(4) -0.151(1) 0.2056(8) 0.0949 Uani O ?
O(14) 1.0000 0.5206(4) -0.156(1) 0.0364(9) 0.1070 Uani O ?
O(21) 1.0000 0.6014(4) 0.306(2) 0.5174(9) 0.1203 Uani O ?
O(22) 1.0000 0.5519(4) 0.467(1) 0.1110(9) 0.1121 Uani O ?
O(23) 1.0000 0.6611(4) 0.625(1) 0.364(1) 0.1136 Uani O ?
O(24) 1.0000 0.5225(4) 0.654(1) 0.363(1) 0.1211 Uani O ?
C(11) 1.0000 0.5606(4) -0.006(2) 0.276(1) 0.0782 Uani C ?
C(12) 1.0000 0.5933(5) 0.151(2) 0.071(1) 0.0711 Uani C ?
C(13) 1.0000 0.6295(5) -0.083(2) 0.193(1) 0.0708 Uani C ?
C(14) 1.0000 0.5422(5) -0.086(2) 0.083(1) 0.0852 Uani C ?
C(21) 1.0000 0.5956(5) 0.353(2) 0.447(1) 0.0825 Uani C ?
C(22) 1.0000 0.5642(5) 0.459(2) 0.191(1) 0.0897 Uani C ?
C(23) 1.0000 0.6324(5) 0.557(2) 0.348(1) 0.0857 Uani C ?
C(24) 1.0000 0.5453(6) 0.571(2) 0.349(1) 0.0944 Uani C ?
C(100) . 0.6850(2) 0.0870(7) 0.4775(4) 0.0500 Uiso . dum
C(101) 1.0000 0.6585(2) 0.1391(9) 0.3950(5) 0.0584 Uani C ?
C(102) 1.0000 0.6864(3) 0.2276(7) 0.4548(6) 0.0626 Uani C ?
C(103) 1.0000 0.7129(2) 0.1756(9) 0.5373(5) 0.0657 Uani C ?
C(104) 1.0000 0.7115(3) 0.035(1) 0.5600(5) 0.0773 Uani C ?
C(105) 1.0000 0.6836(3) -0.0536(7) 0.5003(6) 0.0657 Uani C ?
C(106) 1.0000 0.6571(2) -0.0015(8) 0.4178(5) 0.0626 Uani C ?
C(200) . 0.7001(2) 0.3454(6) 0.1864(4) 0.0500 Uiso . dum
C(201) 1.0000 0.6684(2) 0.2987(8) 0.2250(6) 0.0600 Uani C ?
C(202) 1.0000 0.6625(2) 0.4199(8) 0.1695(6) 0.0627 Uani C ?
C(203) 1.0000 0.6941(3) 0.4666(8) 0.1309(6) 0.0679 Uani C ?
C(204) 1.0000 0.7317(2) 0.392(1) 0.1477(7) 0.0935 Uani C ?
C(205) 1.0000 0.7376(2) 0.271(1) 0.2032(7) 0.0679 Uani C ?
C(206) 1.0000 0.7060(3) 0.2242(7) 0.2418(6) 0.0627 Uani C ?
H(1) 1.0000 0.5397 0.1479 0.1492 0.19(6) Uiso H ?
H(2) 1.0000 0.5412 0.3351 0.3027 0.19(6) Uiso H ?
H(102) 1.0000 0.6875(4) 0.3253(7) 0.4395(8) 0.12(2) Uiso H ?
H(103) 1.0000 0.7319(3) 0.238(1) 0.5777(7) 0.12(2) Uiso H ?
H(104) 1.0000 0.7295(3) -0.001(1) 0.6161(6) 0.13(2) Uiso H ?
H(105) 1.0000 0.6825(4) -0.1512(8) 0.5156(9) 0.12(2) Uiso H ?
H(106) 1.0000 0.6381(3) -0.064(1) 0.3773(7) 0.12(2) Uiso H ?
H(202) 1.0000 0.6371(3) 0.471(1) 0.1579(9) 0.12(2) Uiso H ?
H(203) 1.0000 0.6901(4) 0.549(1) 0.0930(9) 0.13(2) Uiso H ?
H(204) 1.0000 0.7530(3) 0.424(1) 0.1213(9) 0.14(2) Uiso H ?
H(205) 1.0000 0.7630(3) 0.220(1) 0.215(1) 0.13(2) Uiso H ?
H(206) 1.0000 0.7100(4) 0.141(1) 0.2797(8) 0.12(2) Uiso H ?
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Os -1.816 7.605 'International Tables Vol. IV Table 2.2B'
Ge 0.081 1.801 'International Tables Vol. IV Table 2.2B'
O 0.008 0.006 'International Tables Vol. IV Table 2.2B'
C 0.002 0.002 'International Tables Vol. IV Table 2.2B'
H 0.000 0.000 'International Tables Vol. IV Table 2.2B'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
3 1 -2
4 -2 -3
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
Ge(1) Os(1) C(11) 84.4(5) no
Ge(1) Os(1) C(12) 85.3(4) no
C(11) Os(1) C(12) 161.1(7) no
Ge(1) Os(1) C(13) 89.1(4) no
C(11) Os(1) C(13) 99.1(6) no
C(12) Os(1) C(13) 96.6(7) no
Ge(1) Os(1) C(14) 174.6(5) no
C(11) Os(1) C(14) 94.3(7) no
C(12) Os(1) C(14) 94.5(7) no
C(13) Os(1) C(14) 96.3(6) no
Ge(1) Os(2) C(21) 86.3(5) no
Ge(1) Os(2) C(22) 83.1(5) no
C(21) Os(2) C(22) 162.3(7) no
Ge(1) Os(2) C(23) 90.0(5) no
C(21) Os(2) C(23) 95.4(7) no
C(22) Os(2) C(23) 98.7(8) no
Ge(1) Os(2) C(24) 171.8(6) no
C(21) Os(2) C(24) 93.9(8) no
C(22) Os(2) C(24) 94.6(8) no
C(23) Os(2) C(24) 98.2(8) no
Os(1) Ge(1) Os(2) 114.41(6) yes
Os(1) Ge(1) C(101) 111.5(3) no
Os(2) Ge(1) C(101) 109.2(3) no
Os(1) Ge(1) C(201) 109.3(3) no
Os(2) Ge(1) C(201) 111.0(2) no
C(101) Ge(1) C(201) 100.6(4) no
Os(1) C(11) O(11) 170.2(17) yes
Os(1) C(12) O(12) 174.9(14) yes
Os(1) C(13) O(13) 178.7(15) yes
Os(1) C(14) O(14) 178.8(16) yes
Os(2) C(21) O(21) 177.5(16) yes
Os(2) C(22) O(22) 176.1(18) yes
Os(2) C(23) O(23) 178.2(17) yes
Os(2) C(24) O(24) 178.5(19) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Os(1) Ge(1) 2.599(2) yes
Os(1) C(11) 1.95(2) yes
Os(1) C(12) 1.94(2) yes
Os(1) C(13) 2.00(2) yes
Os(1) C(14) 1.98(2) yes
Os(2) Ge(1) 2.614(2) yes
Os(2) C(21) 1.97(2) yes
Os(2) C(22) 1.93(2) yes
Os(2) C(23) 1.99(2) yes
Os(2) C(24) 1.92(2) yes
Ge(1) C(101) 1.992(6) yes
Ge(1) C(201) 1.986(6) yes
O(11) C(11) 1.13(2) yes
O(12) C(12) 1.130(10) yes
O(13) C(13) 1.11(2) yes
O(14) C(14) 1.10(2) yes
O(21) C(21) 1.11(2) yes
O(22) C(22) 1.16(2) yes
O(23) C(23) 1.14(2) yes
O(24) C(24) 1.16(2) yes
