Narrowly dispersed silica supported osmium nanoparticles prepared by an organometallic approach: H2 and CO adsorption stoichiometry and hydrogenolysis catalytic activity.
Low, Jia En; Foelske-Schmitz, Annette; Krumeich, Frank; Wörle, Michael; Baudouin, David; Rascón, Fernando; Copéret, Christophe; Dalton transactions (Cambridge, England : 2003) 42 (2013) 12620–12625; doi:10.1039/c3dt50980j

data_7021700
_publ_section_title
;
 Narrowly dispersed silica supported osmium nanoparticles prepared by an
 organometallic approach: H2 and CO adsorption stoichiometry and
 hydrogenolysis catalytic activity.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12620
_journal_page_last               12625
_journal_paper_doi               10.1039/c3dt50980j
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C16 H20 Os'
_chemical_formula_sum            'C16 H20 Os'
_chemical_formula_weight         402.52
_chemical_name_systematic
Osmium(0)(eta4-1,5-cyclooctadiene)(eta6-1,3,5,7-cyclooctatetraene)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-05-06
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr  9 2013 14:10:59, GUI svn.r4458)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.750(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.293(2)
_cell_length_b                   8.9556(16)
_cell_length_c                   13.020(2)
_cell_measurement_reflns_used    7529
_cell_measurement_temperature    233(2)
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      2.93
_cell_volume                     1291.0(4)
_computing_data_collection       'SMART V5.629, Bruker AXS, Inc., USA'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
and 
MERCURY 3.1, Cambridge Crystallographic Data Centre (CCDC), 2012
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      233.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19522
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.969
_diffrn_reflns_theta_min         1.839
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    9.851
_exptl_absorpt_correction_T_max  0.2156
_exptl_absorpt_correction_T_min  0.0950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1543 before and 0.0368 after correction.
The Ratio of minimum to maximum transmission is 0.4406.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_recrystallization_method 'crystallized from pentane'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.030
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0188P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0385
_refine_ls_wR_factor_ref         0.0424
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3771
_reflns_number_total             4897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt50980j_2.txt
_cod_data_source_block           cop20m5
_cod_original_cell_volume        1291.1(4)
_cod_database_code               7021700
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
;
_shelx_estimated_absorpt_t_max   0.339
_shelx_estimated_absorpt_t_min   0.130
_shelx_hkl_checksum              35947
_shelx_res_checksum              10650
_shelxl_version_number           2012-9