#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:41:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179342 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/39/4323993.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_4323993
loop_
_publ_author_name
'Giuseppe Fachinetti'
'Tiziana Funaioli'
'Lorenzo Lecci'
'Fabio Marchetti'
_publ_section_title
;
 Ru3(CO)12 in Acidic Media. Intermediates of the Acid-Cocatalyzed
 Water-Gas Shift Reaction (WGSR)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7217
_journal_page_last               7224
_journal_paper_doi               10.1021/ic960630v
_journal_volume                  35
_journal_year                    1996
_chemical_formula_moiety         '[RuH(CO)2(py)3][BPh4]'
_chemical_formula_sum            'C41 H36 B N3 O2 Ru'
_chemical_formula_weight         714.61
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   9.7604(6)
_cell_length_b                   9.7604(9)
_cell_length_c                   64.244(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      11.0
_cell_volume                     5300.3(9)
_computing_molecular_graphics    'SHELXTL rel. 5.2'
_computing_publication_material  'SHELXTL rel. 5.2'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       '2q/w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0938
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            5129
_diffrn_reflns_theta_max         59.85
_diffrn_reflns_theta_min         5.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 98
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.892
_exptl_absorpt_correction_type   'Psi scanning'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description
'hexagonal prism closed by hexagonal pyramids'
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          '0.21 mm'
_exptl_crystal_size_mid          '0.21 mm'
_exptl_crystal_size_min          '0.48 mm'
_refine_diff_density_max         0.841
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.025(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.108
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5129
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.107
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_obs          0.0343
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0427P)²+0.0858P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0886
_refine_ls_wR_factor_obs         0.0764
_reflns_number_observed          4203
_reflns_number_total             5129
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960630v_3.cif
_cod_data_source_block           coru
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0858P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0858P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323993
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ru Ru 0.33442(4) 0.59164(4) 0.493591(8) 0.04193(11) Uani 1 d . .
H1 H 0.2763(27) 0.7114(28) 0.4999(4) 0.050 Uiso 1 d D .
C1 C 0.4486(7) 0.6525(7) 0.51815(12) 0.052(2) Uani 1 d D .
O1 O 0.5198(5) 0.7015(5) 0.53311(8) 0.0724(13) Uani 1 d . .
C2 C 0.5038(7) 0.7674(7) 0.48130(13) 0.068(2) Uani 1 d D .
O2 O 0.6068(6) 0.8818(6) 0.47480(10) 0.092(2) Uani 1 d . .
N1 N 0.1810(5) 0.5403(5) 0.46719(8) 0.0470(12) Uani 1 d D .
C3P C 0.0881(7) 0.3932(7) 0.45988(11) 0.059(2) Uani 1 d . .
H3P H 0.1037(7) 0.3127(7) 0.46496(11) 0.071 Uiso 1 calc R .
C4P C -0.0275(8) 0.3553(8) 0.44546(13) 0.074(2) Uani 1 d . .
H4P H -0.0894(8) 0.2511(8) 0.44103(13) 0.089 Uiso 1 calc R .
C5P C -0.0522(7) 0.4705(8) 0.43756(12) 0.069(2) Uani 1 d . .
H5P H -0.1322(7) 0.4464(8) 0.42793(12) 0.083 Uiso 1 calc R .
C6P C 0.0435(7) 0.6222(8) 0.44411(12) 0.062(2) Uani 1 d . .
H6P H 0.0306(7) 0.7038(8) 0.43883(12) 0.075 Uiso 1 calc R .
C7P C 0.1581(7) 0.6531(7) 0.45846(10) 0.0524(15) Uani 1 d . .
H7P H 0.2242(7) 0.7576(7) 0.46246(10) 0.063 Uiso 1 calc R .
N2 N 0.1192(5) 0.4092(5) 0.50861(8) 0.0490(12) Uani 1 d D .
C8P C 0.0199(7) 0.4510(7) 0.51699(11) 0.059(2) Uani 1 d . .
H8P H 0.0468(7) 0.5569(7) 0.51670(11) 0.071 Uiso 1 calc R .
C9P C -0.1212(8) 0.3419(8) 0.52603(14) 0.074(2) Uani 1 d . .
H9P H -0.1874(8) 0.3749(8) 0.53172(14) 0.089 Uiso 1 calc R .
C10P C -0.1638(7) 0.1872(8) 0.52668(13) 0.075(2) Uani 1 d . .
H10P H -0.2592(7) 0.1128(8) 0.53266(13) 0.090 Uiso 1 calc R .
C11P C -0.0621(7) 0.1427(7) 0.51823(13) 0.068(2) Uani 1 d . .
H11P H -0.0873(7) 0.0374(7) 0.51842(13) 0.082 Uiso 1 calc R .
C12P C 0.0768(6) 0.2564(6) 0.50957(12) 0.059(2) Uani 1 d . .
H12P H 0.1453(6) 0.2256(6) 0.50405(12) 0.071 Uiso 1 calc R .
N3 N 0.4090(5) 0.4153(5) 0.48292(9) 0.0504(12) Uani 1 d . .
C13P C 0.4497(6) 0.3390(6) 0.49650(12) 0.054(2) Uani 1 d . .
H13P H 0.4330(6) 0.3470(6) 0.51059(12) 0.065 Uiso 1 calc R .
C14P C 0.5159(7) 0.2481(7) 0.49056(13) 0.067(2) Uani 1 d . .
H14P H 0.5429(7) 0.1963(7) 0.50049(13) 0.080 Uiso 1 calc R .
C15P C 0.5407(9) 0.2360(8) 0.47017(15) 0.079(2) Uani 1 d . .
H15P H 0.5840(9) 0.1747(8) 0.46591(15) 0.095 Uiso 1 calc R .
C16P C 0.5015(9) 0.3147(8) 0.45569(13) 0.076(2) Uani 1 d . .
H16P H 0.5187(9) 0.3085(8) 0.44157(13) 0.092 Uiso 1 calc R .
C17P C 0.4361(7) 0.4030(7) 0.46268(11) 0.057(2) Uani 1 d . .
H17P H 0.4095(7) 0.4564(7) 0.45296(11) 0.068 Uiso 1 calc R .
B B 0.2224(6) 0.1075(6) 0.39453(11) 0.0385(14) Uani 1 d . .
C1B C 0.3794(5) 0.1023(5) 0.40276(9) 0.0403(13) Uani 1 d . .
C2B C 0.3748(7) -0.0026(6) 0.41766(10) 0.0496(14) Uani 1 d . .
H2B H 0.2807(7) -0.0654(6) 0.42476(10) 0.059 Uiso 1 calc R .
C3B C 0.5064(7) -0.0173(7) 0.42237(11) 0.059(2) Uani 1 d . .
H3B H 0.4981(7) -0.0902(7) 0.43234(11) 0.071 Uiso 1 calc R .
C4B C 0.6463(7) 0.0735(7) 0.41257(13) 0.066(2) Uani 1 d . .
H4B H 0.7331(7) 0.0617(7) 0.41551(13) 0.079 Uiso 1 calc R .
C5B C 0.6580(6) 0.1830(8) 0.39830(12) 0.063(2) Uani 1 d . .
H5B H 0.7546(6) 0.2495(8) 0.39195(12) 0.075 Uiso 1 calc R .
C6B C 0.5267(6) 0.1950(6) 0.39330(10) 0.0534(15) Uani 1 d . .
H6B H 0.5367(6) 0.2678(6) 0.38321(10) 0.064 Uiso 1 calc R .
C7B C 0.2413(5) 0.2845(5) 0.39598(9) 0.0370(11) Uani 1 d . .
C8B C 0.3731(6) 0.4201(6) 0.40340(11) 0.0518(15) Uani 1 d . .
H8B H 0.4609(6) 0.4137(6) 0.40759(11) 0.062 Uiso 1 calc R .
C9B C 0.3788(7) 0.5661(6) 0.40481(13) 0.067(2) Uani 1 d . .
H9B H 0.4690(7) 0.6535(6) 0.41006(13) 0.081 Uiso 1 calc R .
C10B C 0.2535(6) 0.5815(6) 0.39858(11) 0.055(2) Uani 1 d . .
H10B H 0.2569(6) 0.6782(6) 0.39967(11) 0.066 Uiso 1 calc R .
C11B C 0.1228(6) 0.4520(6) 0.39070(10) 0.0509(15) Uani 1 d . .
H11B H 0.0380(6) 0.4613(6) 0.38587(10) 0.061 Uiso 1 calc R .
C12B C 0.1160(6) 0.3067(6) 0.38988(10) 0.0483(14) Uani 1 d . .
H12B H 0.0237(6) 0.2196(6) 0.38504(10) 0.058 Uiso 1 calc R .
C13B C 0.0673(6) -0.0083(6) 0.40876(10) 0.0408(12) Uani 1 d . .
C14B C 0.0581(6) 0.0340(6) 0.42936(10) 0.0497(14) Uani 1 d . .
H14B H 0.1419(6) 0.1277(6) 0.43444(10) 0.060 Uiso 1 calc R .
C15B C -0.0674(7) -0.0544(7) 0.44266(11) 0.060(2) Uani 1 d . .
H15B H -0.0668(7) -0.0199(7) 0.45617(11) 0.072 Uiso 1 calc R .
C16B C -0.1927(6) -0.1936(7) 0.43564(13) 0.061(2) Uani 1 d . .
H16B H -0.2781(6) -0.2545(7) 0.44434(13) 0.074 Uiso 1 calc R .
C17B C -0.1905(6) -0.2413(7) 0.41588(13) 0.061(2) Uani 1 d . .
H17B H -0.2746(6) -0.3364(7) 0.41116(13) 0.073 Uiso 1 calc R .
C18B C -0.0633(6) -0.1497(6) 0.40237(11) 0.0488(14) Uani 1 d . .
H18B H -0.0666(6) -0.1847(6) 0.38882(11) 0.059 Uiso 1 calc R .
C19B C 0.2006(5) 0.0492(5) 0.37021(9) 0.0378(12) Uani 1 d . .
C20B C 0.1685(5) -0.1028(6) 0.36474(10) 0.0460(13) Uani 1 d . .
H20B H 0.1574(5) -0.1715(6) 0.37548(10) 0.055 Uiso 1 calc R .
C21B C 0.1522(6) -0.1577(7) 0.34488(12) 0.058(2) Uani 1 d . .
H21B H 0.1295(6) -0.2610(7) 0.34246(12) 0.070 Uiso 1 calc R .
C22B C 0.1698(6) -0.0584(7) 0.32808(11) 0.060(2) Uani 1 d . .
H22B H 0.1586(6) -0.0934(7) 0.31439(11) 0.072 Uiso 1 calc R .
C23B C 0.2047(6) 0.0942(7) 0.33282(12) 0.062(2) Uani 1 d . .
H23B H 0.2183(6) 0.1635(7) 0.32204(12) 0.074 Uiso 1 calc R .
C24B C 0.2194(6) 0.1452(6) 0.35286(10) 0.0464(13) Uani 1 d . .
H24B H 0.2431(6) 0.2488(6) 0.35520(10) 0.056 Uiso 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 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru 0.0552 3.2960 '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
C1 Ru C2 87.2(3) . . ?
C1 Ru N1 170.2(2) . . ?
C2 Ru N1 94.2(3) . . ?
C1 Ru N2 93.7(2) . . ?
C2 Ru N2 171.0(2) . . ?
N1 Ru N2 83.4(2) . . ?
C1 Ru N3 97.5(2) . . ?
C2 Ru N3 95.5(2) . . ?
N1 Ru N3 92.0(2) . . ?
N2 Ru N3 93.3(2) . . ?
O1 C1 Ru 174.5(5) . . ?
O2 C2 Ru 175.2(6) . . ?
C3P N1 C7P 115.4(5) . . ?
C3P N1 Ru 123.0(4) . . ?
C7P N1 Ru 121.2(4) . . ?
N1 C3P C4P 123.6(6) . . ?
C5P C4P C3P 119.6(6) . . ?
C4P C5P C6P 118.4(6) . . ?
C7P C6P C5P 119.3(6) . . ?
N1 C7P C6P 123.6(6) . . ?
C12P N2 C8P 117.1(5) . . ?
C12P N2 Ru 124.5(4) . . ?
C8P N2 Ru 118.5(4) . . ?
N2 C8P C9P 121.9(6) . . ?
C10P C9P C8P 120.5(6) . . ?
C9P C10P C11P 118.1(6) . . ?
C12P C11P C10P 118.8(6) . . ?
N2 C12P C11P 123.6(6) . . ?
C13P N3 C17P 117.3(5) . . ?
C13P N3 Ru 121.4(4) . . ?
C17P N3 Ru 120.6(4) . . ?
N3 C13P C14P 122.8(7) . . ?
C15P C14P C13P 119.0(7) . . ?
C14P C15P C16P 119.8(6) . . ?
C15P C16P C17P 118.2(8) . . ?
N3 C17P C16P 122.9(6) . . ?
C19B B C13B 112.1(4) . . ?
C19B B C1B 104.9(4) . . ?
C13B B C1B 110.6(5) . . ?
C19B B C7B 110.2(4) . . ?
C13B B C7B 105.8(4) . . ?
C1B B C7B 113.4(4) . . ?
C2B C1B C6B 114.9(5) . . ?
C2B C1B B 123.9(5) . . ?
C6B C1B B 120.8(5) . . ?
C1B C2B C3B 122.3(6) . . ?
C4B C3B C2B 120.6(6) . . ?
C3B C4B C5B 119.1(5) . . ?
C4B C5B C6B 120.2(6) . . ?
C5B C6B C1B 122.8(6) . . ?
C8B C7B C12B 114.4(5) . . ?
C8B C7B B 125.7(4) . . ?
C12B C7B B 119.9(4) . . ?
C7B C8B C9B 122.6(5) . . ?
C10B C9B C8B 120.7(5) . . ?
C9B C10B C11B 118.7(5) . . ?
C10B C11B C12B 120.3(5) . . ?
C11B C12B C7B 123.3(5) . . ?
C18B C13B C14B 114.1(5) . . ?
C18B C13B B 126.2(6) . . ?
C14B C13B B 119.7(5) . . ?
C15B C14B C13B 124.5(5) . . ?
C16B C15B C14B 119.1(6) . . ?
C17B C16B C15B 119.2(6) . . ?
C16B C17B C18B 121.3(6) . . ?
C13B C18B C17B 121.8(7) . . ?
C20B C19B C24B 113.1(5) . . ?
C20B C19B B 121.9(5) . . ?
C24B C19B B 124.9(4) . . ?
C21B C20B C19B 125.0(6) . . ?
C20B C21B C22B 119.9(6) . . ?
C23B C22B C21B 117.0(6) . . ?
C24B C23B C22B 121.7(6) . . ?
C23B C24B C19B 123.4(5) . . ?
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
Ru C1 1.850(7) . ?
Ru C2 1.861(7) . ?
Ru N1 2.149(5) . ?
Ru N2 2.185(5) . ?
Ru N3 2.284(4) . ?
C1 O1 1.141(8) . ?
C2 O2 1.145(7) . ?
N1 C3P 1.343(7) . ?
N1 C7P 1.350(7) . ?
C3P C4P 1.361(9) . ?
C4P C5P 1.361(9) . ?
C5P C6P 1.363(9) . ?
C6P C7P 1.362(9) . ?
N2 C12P 1.334(7) . ?
N2 C8P 1.339(7) . ?
C8P C9P 1.379(9) . ?
C9P C10P 1.351(9) . ?
C10P C11P 1.379(9) . ?
C11P C12P 1.369(8) . ?
N3 C13P 1.330(8) . ?
N3 C17P 1.344(8) . ?
C13P C14P 1.387(7) . ?
C14P C15P 1.347(11) . ?
C15P C16P 1.376(11) . ?
C16P C17P 1.380(8) . ?
B C19B 1.640(8) . ?
B C13B 1.642(8) . ?
B C1B 1.645(7) . ?
B C7B 1.646(7) . ?
C1B C2B 1.386(8) . ?
C1B C6B 1.398(8) . ?
C2B C3B 1.396(8) . ?
C3B C4B 1.354(9) . ?
C4B C5B 1.369(10) . ?
C5B C6B 1.382(7) . ?
C7B C8B 1.389(7) . ?
C7B C12B 1.400(7) . ?
C8B C9B 1.401(7) . ?
C9B C10B 1.365(8) . ?
C10B C11B 1.367(8) . ?
C11B C12B 1.388(7) . ?
C13B C18B 1.393(8) . ?
C13B C14B 1.403(9) . ?
C14B C15B 1.385(8) . ?
C15B C16B 1.372(8) . ?
C16B C17B 1.356(10) . ?
C17B C18B 1.409(8) . ?
C19B C20B 1.399(7) . ?
C19B C24B 1.408(8) . ?
C20B C21B 1.363(9) . ?
C21B C22B 1.403(10) . ?
C22B C23B 1.386(8) . ?
C23B C24B 1.362(9) . ?
