#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:10:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178551 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/58/4065815.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_4065815
loop_
_publ_author_name
'Cabeza, Javier A.'
'del Río, Ignacio'
'Fernández-Colinas, José M.'
'Pérez-Carreño, Enrique'
'Vázquez-García, Digna'
_publ_section_title
;
 From Allenes to Edge-Bridging Allyl Ligands or Face-Capping Alkenyl
 Ligands on a Triruthenium Hydrido Carbonyl Cluster: An Experimental and
 DFT Computational Study†
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4818
_journal_paper_doi               10.1021/om100148z
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         '2(C16 H16 N2 O10 Ru3), C Cl2'
_chemical_formula_sum            'C33 H32 Cl2 N4 O20 Ru6'
_chemical_formula_weight         1481.95
_chemical_name_systematic
;
 ?
;
_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'
_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                 123.9040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.0688(5)
_cell_length_b                   15.2472(4)
_cell_length_c                   17.7538(4)
_cell_measurement_reflns_used    4207
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.407
_cell_volume                     4733.5(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13532
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    2.055
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.079
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [1.00000+-1.00000exp(-100.00(sinθ/λ)²)]/
   [σ²(Fo²)+0.3333+3.3411*P+(0.0505P)²+0.3333sinθ/λ]
 where P = 0.33333Fo² + 0.66667Fc²
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                4035
_reflns_number_total             4328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100148z_si_002.cif
_cod_data_source_block           7_(d252f)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4065815
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_group
C1 C 0.18417(17) 0.70977(18) 0.36609(19) 0.0248(6) Uani 1 1 d . .
H1A H 0.2137 0.7030 0.4309 0.037 Uiso 1 1 calc R .
H1B H 0.1311 0.7155 0.3437 0.037 Uiso 1 1 calc R .
H1C H 0.2007 0.7613 0.3506 0.037 Uiso 1 1 calc R .
C2 C 0.14727(16) 0.64761(18) 0.22475(17) 0.0224(6) Uani 1 1 d . .
H2A H 0.1521 0.5987 0.1942 0.034 Uiso 1 1 calc R .
H2B H 0.1643 0.7000 0.2112 0.034 Uiso 1 1 calc R .
H2C H 0.0947 0.6542 0.2045 0.034 Uiso 1 1 calc R .
C3 C 0.31212(18) 0.35208(19) 0.4213(2) 0.0293(7) Uani 1 1 d . .
H3A H 0.2709 0.3147 0.4096 0.044 Uiso 1 1 calc R .
H3B H 0.3490 0.3565 0.4855 0.044 Uiso 1 1 calc R .
H3C H 0.3360 0.3278 0.3931 0.044 Uiso 1 1 calc R .
C4 C 0.28088(17) 0.44331(17) 0.38221(19) 0.0212(6) Uani 1 1 d . .
C5 C 0.22442(17) 0.44946(18) 0.28530(19) 0.0203(6) Uani 1 1 d . .
C6 C 0.19627(16) 0.37723(18) 0.21835(19) 0.0220(6) Uani 1 1 d . .
C7 C 0.09091(18) 0.3346(2) 0.0717(2) 0.0318(7) Uani 1 1 d . .
H7A H 0.0968 0.2759 0.0960 0.038 Uiso 1 1 calc R .
H7B H 0.1144 0.3362 0.0378 0.038 Uiso 1 1 calc R .
C8 C 0.00797(19) 0.3576(3) 0.0112(2) 0.0434(9) Uani 1 1 d . .
H8A H 0.0028 0.4156 -0.0128 0.065 Uiso 1 1 calc R .
H8B H -0.0147 0.3558 0.0454 0.065 Uiso 1 1 calc R .
H8C H -0.0174 0.3163 -0.0379 0.065 Uiso 1 1 calc R .
C200 C 0.25449(17) 0.55989(18) 0.50982(19) 0.0222(6) Uani 1 1 d . .
C90 C -0.0139(5) 0.2377(4) 0.2231(5) 0.046(2) Uani 0.50 1 d P .
C201 C 0.39751(16) 0.6487(2) 0.55259(18) 0.0236(6) Uani 1 1 d . .
C202 C 0.39780(19) 0.4820(2) 0.5826(2) 0.0284(7) Uani 1 1 d . .
C101 C 0.42367(18) 0.5815(2) 0.4065(2) 0.0291(7) Uani 1 1 d . .
C102 C 0.37385(18) 0.4361(2) 0.3007(2) 0.0307(7) Uani 1 1 d . .
C103 C 0.3027(2) 0.5883(2) 0.2106(2) 0.0367(8) Uani 1 1 d . .
C301 C 0.0888(2) 0.5435(2) 0.3614(2) 0.0296(7) Uani 1 1 d . .
C302 C 0.17123(18) 0.4036(2) 0.4303(2) 0.0305(7) Uani 1 1 d . .
N1 N 0.27694(13) 0.62808(15) 0.35924(15) 0.0191(5) Uani 1 1 d . .
N2 N 0.19490(13) 0.63192(15) 0.32459(15) 0.0192(5) Uani 1 1 d . .
O2 O 0.12709(12) 0.39855(13) 0.14521(13) 0.0274(4) Uani 1 1 d . .
O1 O 0.22879(12) 0.30890(13) 0.22469(14) 0.0296(5) Uani 1 1 d . .
O200 O 0.25025(12) 0.57948(14) 0.57057(13) 0.0301(5) Uani 1 1 d . .
O201 O 0.43702(12) 0.70591(15) 0.59633(14) 0.0343(5) Uani 1 1 d . .
O202 O 0.43688(15) 0.44378(17) 0.64818(16) 0.0460(6) Uani 1 1 d . .
O101 O 0.48464(13) 0.60968(16) 0.44984(17) 0.0412(6) Uani 1 1 d . .
O102 O 0.40360(14) 0.38025(16) 0.28894(18) 0.0470(6) Uani 1 1 d . .
O103 O 0.2905(2) 0.6240(2) 0.14823(19) 0.0659(9) Uani 1 1 d . .
O301 O 0.03270(15) 0.56399(19) 0.35371(18) 0.0469(6) Uani 1 1 d . .
O302 O 0.16217(15) 0.34186(16) 0.45899(17) 0.0477(6) Uani 1 1 d . .
Ru2 Ru 0.336018(13) 0.554200(14) 0.479890(14) 0.01968(9) Uani 1 1 d . .
Ru1 Ru 0.325929(13) 0.530727(15) 0.320416(14) 0.01999(9) Uani 1 1 d . .
Ru3 Ru 0.182999(13) 0.507996(14) 0.382717(14) 0.01980(9) Uani 1 1 d . .
Cl1 Cl 0.03904(14) 0.32891(19) 0.22939(14) 0.0746(8) Uani 0.50 1 d P 1
Cl2 Cl 0.07192(15) 0.25119(18) 0.24268(18) 0.0712(7) Uani 0.50 1 d P 2
H10 H 0.292(3) 0.679(4) 0.356(3) 0.085 Uiso 1 1 d . .
H5 H 0.185(3) 0.492(3) 0.261(4) 0.085 Uiso 1 1 d . .
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'
N N 0.0061 0.0033 '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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
N2 C1 H1A 109.5 . .
N2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N2 C2 H2A 109.5 . .
N2 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N2 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C4 C3 H3A 109.5 . .
C4 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C4 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C4 C3 117.2(2) . .
C5 C4 Ru2 126.94(19) . .
C3 C4 Ru2 115.55(19) . .
C5 C4 Ru1 70.87(16) . .
C3 C4 Ru1 124.7(2) . .
Ru2 C4 Ru1 75.58(9) . .
C5 C4 Ru3 80.35(17) . .
C3 C4 Ru3 123.4(2) . .
Ru2 C4 Ru3 75.52(8) . .
Ru1 C4 Ru3 111.91(11) . .
C4 C5 C6 126.9(3) . .
C4 C5 Ru1 71.42(16) . .
C6 C5 Ru1 121.88(19) . .
C4 C5 Ru3 64.74(15) . .
C6 C5 Ru3 133.15(19) . .
Ru1 C5 Ru3 104.95(10) . .
C4 C5 H5 121(3) . .
C6 C5 H5 107(3) . .
Ru1 C5 H5 102(3) . .
Ru3 C5 H5 61(3) . .
O1 C6 O2 123.2(3) . .
O1 C6 C5 127.6(3) . .
O2 C6 C5 109.2(2) . .
O2 C7 C8 107.7(3) . .
O2 C7 H7A 110.2 . .
C8 C7 H7A 110.2 . .
O2 C7 H7B 110.2 . .
C8 C7 H7B 110.2 . .
H7A C7 H7B 108.5 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O200 C200 Ru3 136.6(2) . .
O200 C200 Ru2 138.7(2) . .
Ru3 C200 Ru2 84.62(10) . .
C90 C90 Cl2 76.1(14) 2 2
C90 C90 Cl2 76.1(14) 2 .
Cl2 C90 Cl2 148.6(5) 2 .
C90 C90 Cl1 84.6(9) 2 .
Cl2 C90 Cl1 117.0(4) 2 .
Cl2 C90 Cl1 45.8(3) . .
C90 C90 Cl1 70.1(9) 2 2
Cl2 C90 Cl1 44.0(3) 2 2
Cl2 C90 Cl1 111.6(4) . 2
Cl1 C90 Cl1 73.0(3) . 2
O201 C201 Ru2 177.6(2) . .
O202 C202 Ru2 175.1(3) . .
O101 C101 Ru1 170.9(3) . .
O102 C102 Ru1 178.7(3) . .
O103 C103 Ru1 177.9(4) . .
O301 C301 Ru3 175.8(3) . .
O302 C302 Ru3 177.7(3) . .
N2 N1 Ru2 109.58(15) . .
N2 N1 Ru1 123.94(16) . .
Ru2 N1 Ru1 80.69(8) . .
N2 N1 H10 109(3) . .
Ru2 N1 H10 122(4) . .
Ru1 N1 H10 110(3) . .
N1 N2 C1 107.0(2) . .
N1 N2 C2 110.9(2) . .
C1 N2 C2 106.0(2) . .
N1 N2 Ru3 100.42(14) . .
C1 N2 Ru3 111.17(16) . .
C2 N2 Ru3 120.71(17) . .
C6 O2 C7 116.5(2) . .
C201 Ru2 C202 86.81(13) . .
C201 Ru2 C200 98.30(11) . .
C202 Ru2 C200 90.02(12) . .
C201 Ru2 N1 94.48(11) . .
C202 Ru2 N1 171.84(11) . .
C200 Ru2 N1 97.75(10) . .
C201 Ru2 C4 166.71(11) . .
C202 Ru2 C4 95.06(12) . .
C200 Ru2 C4 94.86(11) . .
N1 Ru2 C4 81.87(10) . .
C201 Ru2 Ru1 115.75(8) . .
C202 Ru2 Ru1 122.30(9) . .
C200 Ru2 Ru1 132.47(8) . .
N1 Ru2 Ru1 50.05(6) . .
C4 Ru2 Ru1 52.49(7) . .
C201 Ru2 Ru3 137.55(8) . .
C202 Ru2 Ru3 112.86(10) . .
C200 Ru2 Ru3 47.45(8) . .
N1 Ru2 Ru3 71.34(7) . .
C4 Ru2 Ru3 53.24(7) . .
Ru1 Ru2 Ru3 86.027(9) . .
C102 Ru1 C101 90.48(13) . .
C102 Ru1 C103 91.20(14) . .
C101 Ru1 C103 100.09(14) . .
C102 Ru1 N1 172.23(11) . .
C101 Ru1 N1 87.70(11) . .
C103 Ru1 N1 96.55(11) . .
C102 Ru1 C5 92.94(12) . .
C101 Ru1 C5 151.82(12) . .
C103 Ru1 C5 107.78(13) . .
N1 Ru1 C5 85.17(9) . .
C102 Ru1 C4 92.95(12) . .
C101 Ru1 C4 114.19(12) . .
C103 Ru1 C4 145.41(13) . .
N1 Ru1 C4 80.93(9) . .
C5 Ru1 C4 37.72(10) . .
C102 Ru1 Ru2 123.04(10) . .
C101 Ru1 Ru2 72.17(9) . .
C103 Ru1 Ru2 144.22(10) . .
N1 Ru1 Ru2 49.26(6) . .
C5 Ru1 Ru2 82.62(7) . .
C4 Ru1 Ru2 51.93(7) . .
C301 Ru3 C302 86.88(14) . .
C301 Ru3 C200 98.94(12) . .
C302 Ru3 C200 91.84(12) . .
C301 Ru3 N2 92.36(11) . .
C302 Ru3 N2 179.06(12) . .
C200 Ru3 N2 88.81(10) . .
C301 Ru3 C4 167.04(12) . .
C302 Ru3 C4 88.97(12) . .
C200 Ru3 C4 93.46(11) . .
N2 Ru3 C4 91.67(9) . .
C301 Ru3 C5 134.50(12) . .
C302 Ru3 C5 101.14(11) . .
C200 Ru3 C5 125.10(11) . .
N2 Ru3 C5 79.02(8) . .
C4 Ru3 C5 34.91(10) . .
C301 Ru3 Ru2 141.59(9) . .
C302 Ru3 Ru2 109.56(10) . .
C200 Ru3 Ru2 47.93(8) . .
N2 Ru3 Ru2 71.38(6) . .
C4 Ru3 Ru2 51.23(7) . .
C5 Ru3 Ru2 77.71(7) . .
C90 Cl1 C90 25.3(4) . 2
C90 Cl1 Cl1 55.7(3) . 2
C90 Cl1 Cl1 51.3(3) 2 2
C90 Cl2 C90 27.8(4) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.479(3) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 N2 1.491(3) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 C4 1.530(4) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 C5 1.449(4) .
C4 Ru2 2.229(3) .
C4 Ru1 2.246(3) .
C4 Ru3 2.290(3) .
C5 C6 1.480(4) .
C5 Ru1 2.238(3) .
C5 Ru3 2.497(3) .
C5 H5 0.94(5) .
C6 O1 1.217(3) .
C6 O2 1.343(3) .
C7 O2 1.458(3) .
C7 C8 1.496(5) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C200 O200 1.169(3) .
C200 Ru3 2.048(3) .
C200 Ru2 2.064(3) .
C90 C90 0.794(13) 2
C90 Cl2 1.653(10) 2
C90 Cl2 1.653(11) .
C90 Cl1 1.747(9) .
C90 Cl1 1.850(8) 2
C201 O201 1.155(4) .
C201 Ru2 1.886(3) .
C202 O202 1.142(4) .
C202 Ru2 1.893(3) .
C101 O101 1.151(4) .
C101 Ru1 1.914(3) .
C102 O102 1.143(4) .
C102 Ru1 1.902(3) .
C103 O103 1.127(4) .
C103 Ru1 1.936(3) .
C301 O301 1.154(4) .
C301 Ru3 1.881(3) .
C302 O302 1.136(4) .
C302 Ru3 1.882(3) .
N1 N2 1.478(3) .
N1 Ru2 2.105(2) .
N1 Ru1 2.130(2) .
N1 H10 0.86(5) .
N2 Ru3 2.233(2) .
Ru2 Ru1 2.7419(3) .
Ru2 Ru3 2.7679(3) .
Cl1 C90 1.850(8) 2
Cl1 Cl1 2.141(5) 2
Cl2 C90 1.653(11) 2
