#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/04/4310412.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_4310412
loop_
_publ_author_name
'Pauline Pearson'
'Christopher M. Kepert'
'Glen B. Deacon'
'Leone Spiccia'
'Andrew C. Warden'
'Brian W. Skelton'
'Allan H. White'
_publ_contact_author_address
;
   Department of Chemistry
   University of Western Australia
   35 Stirling Highway
   Crawley
   Western Australia 6009
   Australia
;
_publ_contact_author_email       bws@crystal.uwa.edu.au
_publ_contact_author_fax         (+61)_08_9380_1118
_publ_contact_author_name        'Skelton, B. W.'
_publ_contact_author_phone       (+61)_08-9380_3481
_publ_section_title
;
 Carbonyl-Carboxylato-Ruthenium Complexes Incorporating Diimine Ligands
 and Unexpected Cyclometalation of Carboxylate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              683
_journal_page_last               691
_journal_paper_doi               10.1021/ic0348401
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C19 H14 N2 O5 Ru'
_chemical_formula_weight         451.4
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             01-04-12
_audit_creation_method           Xtal3.6
_cell_angle_alpha                91.27(3)
_cell_angle_beta                 107.50(3)
_cell_angle_gamma                100.31(3)
_cell_formula_units_Z            2
_cell_length_a                   8.001(2)
_cell_length_b                   9.208(2)
_cell_length_c                   12.673(3)
_cell_measurement_temperature    153(2)
_cell_volume                     873.2(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max .99
_diffrn_measurement_device_type
;
 Bruker P4 diffractometer
;
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .057
_diffrn_reflns_av_sigmaI/netI    .084
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10793
_diffrn_reflns_theta_full        27.8
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         3.62
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    .932
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
 ? 
;
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_F_000             452
_refine_diff_density_max         1.173
_refine_diff_density_min         -.664
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3233
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .065
_refine_ls_R_factor_gt           .042
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .048
_refine_ls_wR_factor_ref         .044
_reflns_d_resolution_high        .761
_reflns_d_resolution_low         5.618
_reflns_limit_h_max              10
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              -12
_reflns_limit_l_max              15
_reflns_limit_l_min              -16
_reflns_number_gt                3233
_reflns_number_total             4102
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            ic0348401si20031112_114047_3.cif
_cod_data_source_block           pp70a
_cod_original_sg_symbol_Hall     -p_1
_cod_original_formula_sum        'C19 H14 N2 O5 Ru1'
_cod_database_code               4310412
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ru .66032(4) .72194(3) .26565(2) .01291(13) Uani ? ? 1.00000 ? ?
C10 .8151(5) .9081(4) .2853(3) .0151(15) Uani ? ? 1.00000 ? ?
O10 .9076(4) 1.0193(3) .2943(2) .0214(12) Uani ? ? 1.00000 ? ?
C20 .7900(5) .6496(4) .1839(3) .0163(15) Uani ? ? 1.00000 ? ?
O20 .8618(4) .6068(3) .1275(2) .0265(13) Uani ? ? 1.00000 ? ?
C11 .3451(5) .8357(4) .1511(3) .0147(14) Uani ? ? 1.00000 ? ?
C111 .3475(5) .8393(4) .2696(3) .0139(14) Uani ? ? 1.00000 ? ?
O11 .4870(3) .8002(3) .3392(2) .0143(10) Uani ? ? 1.00000 ? ?
O12 .2279(3) .8770(3) .2998(2) .0206(11) Uani ? ? 1.00000 ? ?
C12 .4889(5) .7903(4) .1276(3) .0148(14) Uani ? ? 1.00000 ? ?
C13 .4896(5) .7890(4) .0171(3) .0182(15) Uani ? ? 1.00000 ? ?
C14 .3513(5) .8296(4) -.0653(3) .0223(16) Uani ? ? 1.00000 ? ?
C15 .2097(5) .8733(4) -.0405(3) .0210(16) Uani ? ? 1.00000 ? ?
C16 .2067(5) .8771(4) .0688(3) .0175(15) Uani ? ? 1.00000 ? ?
N1 .7711(4) .6326(3) .4231(2) .0134(12) Uani ? ? 1.00000 ? ?
C2 .6819(5) .4976(4) .4352(3) .0131(14) Uani ? ? 1.00000 ? ?
C3 .7304(5) .4304(4) .5340(3) .0173(15) Uani ? ? 1.00000 ? ?
C4 .8738(5) .5030(4) .6205(3) .0207(16) Uani ? ? 1.00000 ? ?
C5 .9660(5) .6391(4) .6076(3) .0188(15) Uani ? ? 1.00000 ? ?
C6 .9103(5) .7012(4) .5077(3) .0185(15) Uani ? ? 1.00000 ? ?
N1' .4889(4) .5115(3) .2505(2) .0129(12) Uani ? ? 1.00000 ? ?
C2' .5306(5) .4279(4) .3375(3) .0127(14) Uani ? ? 1.00000 ? ?
C3' .4351(5) .2847(4) .3343(3) .0188(16) Uani ? ? 1.00000 ? ?
C4' .2897(5) .2286(4) .2423(3) .0213(16) Uani ? ? 1.00000 ? ?
C5' .2454(5) .3165(4) .1552(3) .0196(16) Uani ? ? 1.00000 ? ?
C6' .3486(5) .4557(4) .1615(3) .0181(15) Uani ? ? 1.00000 ? ?
O01 .7171(4) 1.0590(3) .4740(2) .0300(13) Uani ? ? 1.00000 ? ?
H13 .58733 .76079 -.00105 .02500 Uiso ? ? 1.00000 ? ?
H14 .35466 .82923 -.14126 .02900 Uiso ? ? 1.00000 ? ?
H15 .11404 .89830 -.09777 .02700 Uiso ? ? 1.00000 ? ?
H16 .11127 .90685 .08775 .02200 Uiso ? ? 1.00000 ? ?
H3 .66453 .33406 .54246 .02300 Uiso ? ? 1.00000 ? ?
H4 .91144 .45888 .68998 .02600 Uiso ? ? 1.00000 ? ?
H5 1.06873 .68975 .66609 .02400 Uiso ? ? 1.00000 ? ?
H6 .97476 .79574 .49918 .02400 Uiso ? ? 1.00000 ? ?
H3' .47130 .22373 .39539 .02500 Uiso ? ? 1.00000 ? ?
H4' .22242 .13049 .23917 .02800 Uiso ? ? 1.00000 ? ?
H5' .14236 .28161 .09240 .02500 Uiso ? ? 1.00000 ? ?
H6' .31690 .51546 .09921 .02400 Uiso ? ? 1.00000 ? ?
H01a .62727 .97554 .45751 .04400 Uiso ? ? 1.00000 ? ?
H01b .70639 1.07837 .53135 .04400 Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C ? 0 38 .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H ? 0 28 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N ? 0 4 .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O ? 0 10 .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
Ru ? 0 2 -1.42 .836 'Int Tables Vol IV Tables 2.2B and 2.3.1'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C10 Ru C20 . . . 88.92(17) ?
C10 Ru O11 . . . 93.87(15) ?
C10 Ru C12 . . . 89.36(14) ?
C10 Ru N1 . . . 101.06(13) ?
C10 Ru N1' . . . 177.71(13) ?
C20 Ru O11 . . . 172.77(12) ?
C20 Ru C12 . . . 93.03(16) ?
C20 Ru N1 . . . 99.67(15) ?
C20 Ru N1' . . . 92.21(14) ?
O11 Ru C12 . . . 80.35(14) ?
O11 Ru N1 . . . 86.36(12) ?
O11 Ru N1' . . . 85.24(11) ?
C12 Ru N1 . . . 163.66(14) ?
C12 Ru N1' . . . 92.57(12) ?
N1 Ru N1' . . . 76.79(10) ?
Ru C10 O10 . . . 178.3(3) ?
Ru C20 O20 . . . 175.6(3) ?
C111 C11 C12 . . . 116.9(3) ?
C111 C11 C16 . . . 121.1(4) ?
C12 C11 C16 . . . 121.9(4) ?
C11 C111 O11 . . . 115.1(4) ?
C11 C111 O12 . . . 122.5(3) ?
O11 C111 O12 . . . 122.4(4) ?
Ru O11 C111 . . . 115.1(2) ?
Ru C12 C11 . . . 112.0(3) ?
Ru C12 C13 . . . 130.4(3) ?
C11 C12 C13 . . . 117.4(3) ?
C12 C13 C14 . . . 120.8(4) ?
C12 C13 H13 . . . 119.2 ?
C14 C13 H13 . . . 120.0 ?
C13 C14 C15 . . . 120.9(4) ?
C13 C14 H14 . . . 119.8 ?
C15 C14 H14 . . . 119.3 ?
C14 C15 C16 . . . 119.4(3) ?
C14 C15 H15 . . . 120.3 ?
C16 C15 H15 . . . 120.2 ?
C11 C16 C15 . . . 119.5(4) ?
C11 C16 H16 . . . 119.6 ?
C15 C16 H16 . . . 120.9 ?
Ru N1 C2 . . . 114.8(2) ?
Ru N1 C6 . . . 126.1(2) ?
C2 N1 C6 . . . 119.1(3) ?
N1 C2 C3 . . . 121.4(3) ?
N1 C2 C2' . . . 116.0(3) ?
C3 C2 C2' . . . 122.6(3) ?
C2 C3 C4 . . . 118.7(3) ?
C2 C3 H3 . . . 120.9 ?
C4 C3 H3 . . . 120.4 ?
C3 C4 C5 . . . 119.9(4) ?
C3 C4 H4 . . . 120.7 ?
C5 C4 H4 . . . 119.4 ?
C4 C5 C6 . . . 118.7(3) ?
C4 C5 H5 . . . 121.0 ?
C6 C5 H5 . . . 120.2 ?
N1 C6 C5 . . . 122.2(3) ?
N1 C6 H6 . . . 119.4 ?
C5 C6 H6 . . . 118.4 ?
Ru N1' C2' . . . 116.1(2) ?
Ru N1' C6' . . . 125.3(3) ?
C2' N1' C6' . . . 118.6(3) ?
C2 C2' N1' . . . 116.1(3) ?
C2 C2' C3' . . . 122.6(3) ?
N1' C2' C3' . . . 121.3(3) ?
C2' C3' C4' . . . 119.6(4) ?
C2' C3' H3' . . . 120.3 ?
C4' C3' H3' . . . 120.0 ?
C3' C4' C5' . . . 118.5(3) ?
C3' C4' H4' . . . 120.5 ?
C5' C4' H4' . . . 121.0 ?
C4' C5' C6' . . . 119.3(3) ?
C4' C5' H5' . . . 119.8 ?
C6' C5' H5' . . . 120.9 ?
N1' C6' C5' . . . 122.7(3) ?
N1' C6' H6' . . . 119.1 ?
C5' C6' H6' . . . 118.2 ?
H01a O01 H01b . . . 94.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ru C10 . . 1.890(4) ?
Ru C20 . . 1.860(5) ?
Ru O11 . . 2.102(3) ?
Ru C12 . . 2.062(3) ?
Ru N1 . . 2.171(3) ?
Ru N1' . . 2.133(3) ?
C10 O10 . . 1.132(4) ?
C20 O20 . . 1.145(6) ?
C11 C111 . . 1.496(6) ?
C11 C12 . . 1.400(6) ?
C11 C16 . . 1.390(5) ?
C111 O11 . . 1.311(4) ?
C111 O12 . . 1.231(5) ?
C12 C13 . . 1.402(6) ?
C13 C14 . . 1.387(5) ?
C13 H13 . . .954 ?
C14 C15 . . 1.385(7) ?
C14 H14 . . .970 ?
C15 C16 . . 1.393(6) ?
C15 H15 . . .950 ?
C16 H16 . . .948 ?
N1 C2 . . 1.355(4) ?
N1 C6 . . 1.338(4) ?
C2 C3 . . 1.389(5) ?
C2 C2' . . 1.482(4) ?
C3 C4 . . 1.379(5) ?
C3 H3 . . .973 ?
C4 C5 . . 1.376(5) ?
C4 H4 . . .965 ?
C5 C6 . . 1.383(5) ?
C5 H5 . . .961 ?
C6 H6 . . .956 ?
N1' C2' . . 1.352(5) ?
N1' C6' . . 1.343(4) ?
C2' C3' . . 1.393(5) ?
C3' C4' . . 1.387(5) ?
C3' H3' . . .970 ?
C4' C5' . . 1.380(6) ?
C4' H4' . . .959 ?
C5' C6' . . 1.381(5) ?
C5' H5' . . .957 ?
C6' H6' . . .969 ?
O01 H01a . . .925 ?
O01 H01b . . .778 ?
