High Pressure Study of Ru3(CO)12 by X-ray Diffraction, Raman, and Infrared Spectroscopy
Carla Slebodnick; Jing Zhao; Ross Angel; Brian E. Hanson; Yang Song; Zhenxian Liu; Russell J. Hemley; Inorganic Chemistry 43 (2004) 5245–5252; doi:10.1021/ic049617y

data_4311838
_publ_contact_author_address
;
Department Of Chemistry, Virginia Tech, Blacksburg, VA 24061
;
_publ_contact_author_email       hanson@vt.edu
_publ_contact_author_fax         '540 231-3255'
_publ_contact_author_name        'Brian E. Hanson'
_publ_contact_author_phone       '540 231 7206'
_publ_section_title
;
 High Pressure Study of Ru3(CO)12 by X-ray Diffraction, Raman, and
 Infrared Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5245
_journal_page_last               5252
_journal_paper_doi               10.1021/ic049617y
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C12 O12 Ru3'
_chemical_formula_sum            'C12 O12 Ru3'
_chemical_formula_weight         639.33
_chemical_name_common            'triruthenium dodecacarbonyl'
_chemical_name_systematic        'triruthenium dodecacarbonyl'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.195(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7435(10)
_cell_length_b                   14.141(2)
_cell_length_c                   13.830(2)
_cell_measurement_pressure       1800000
_cell_measurement_reflns_used    719
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      2.82
_cell_volume                     1490.5(4)
_computing_cell_refinement       'Crysalis (Oxford Diffraction)'
_computing_data_collection       'Crysalis (Oxford Diffraction)'
_computing_data_reduction
;
 WinIntergrStp 3.3 (Angel, J. Appl. Cryst. 2003)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
;
 Bruker SHELXTL (Sheldrick, 2001) and PLATON (Spek, A. L., J Appl. 
 Cryst., 2003)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
 coordinates obtained from CCDC (Allan, Acta Cryst B., 2002 and Bruno et al. 
 Acta Cryst. B, 2002) from the structure by 
 Churchill, et al. (Inorg Chem, 1977).
;
_diffrn_ambient_pressure         1800000
_diffrn_ambient_temperature      293(2)
_diffrn_detector_type            'point detector'
_diffrn_measured_fraction_theta_full 0.263
_diffrn_measured_fraction_theta_max 0.264
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 1'
_diffrn_measurement_method       'constant precision omega scans at phi=0'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0475
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            719
_diffrn_reflns_theta_full        22.52
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.072
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.761
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 Correction for absorption affects of the diamond anvil cell
 and the sample were made using ABSORB 5.3.  Reference: 
  Absorb (Angel, J. Appl. Cryst. 2004) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.339
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         518
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.305
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0507
_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/[\s^2^(Fo^2^)+(0.0000P)^2^+71.3452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1256
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                514
_reflns_number_total             518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049617ysi20040322_044432_5.cif
_cod_data_source_block           18kbar
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
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_original_cell_volume        1490.4(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4311838