#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/35/7013571.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_7013571
loop_
_publ_author_name
'Jedd Comiskey'
'Etelka Farkas'
'Krystyna A. Krot-Lacina'
'Robin G. Pritchard'
'Charles A. McAuliffe (the late)'
'Kevin B. Nolan'
_publ_section_title
;
 Synthesis, structures and speciation studies of ruthenium(III)
 hydroxamate/hydroximato complexes. Crystal and molecular structure of
 hydrated [Ru(H2edta)(2-methoxyphenylhydroxamate)], the first
 structurally characterised ruthenium(III)--hydroxamate complex
;
_journal_issue                   22
_journal_name_full               'Dalton Trans.'
_journal_page_first              4243
_journal_page_last               4249
_journal_paper_doi               10.1039/b310193m
_journal_year                    2003
_chemical_formula_moiety         'C18 H22 N3 O11 Ru1, 4.91(H2 O1)'
_chemical_formula_sum            'C18 H31.82 N3 O15.91 Ru'
_chemical_formula_weight         645.91
_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                 110.264(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.700(6)
_cell_length_b                   8.5319(9)
_cell_length_c                   15.292(2)
_cell_measurement_reflns_used    19394
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     5226.2(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1962
_diffrn_reflns_av_sigmaI/netI    0.1623
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10672
_diffrn_reflns_theta_full        23.59
_diffrn_reflns_theta_max         23.59
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.68
_exptl_absorpt_correction_T_max  1.056
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
?
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2656.8
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.197
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       0.00093(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         3739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.2074
_refine_ls_R_factor_gt           0.1252
_refine_ls_shift/su_max          0.256
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+329.1807P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2490
_refine_ls_wR_factor_ref         0.3133
_reflns_number_gt                2140
_reflns_number_total             3739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310193m.txt
_cod_data_source_block           new
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7013571
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_assembly
_atom_site_disorder_group
Ru1 Ru 0.146990(11) 0.42968(6) 0.54011(3) 0.04599(12) Uani 1 1 d . . .
C1 C 0.19664(12) 0.3865(8) 0.4644(3) 0.055(2) Uani 1 1 d . . .
C2 C 0.21606(13) 0.3310(7) 0.4070(3) 0.0503(18) Uani 1 1 d . . .
C3 C 0.20333(12) 0.1920(8) 0.3542(3) 0.055(2) Uani 1 1 d . . .
H3 H 0.1846 0.1422 0.3590 0.066 Uiso 1 1 calc R . .
C4 C 0.21915(15) 0.1317(9) 0.2956(4) 0.063(2) Uani 1 1 d . . .
H4 H 0.2098 0.0479 0.2563 0.076 Uiso 1 1 calc R . .
C5 C 0.24857(13) 0.1971(8) 0.2962(3) 0.057(2) Uani 1 1 d . . .
H5 H 0.2596 0.1528 0.2594 0.068 Uiso 1 1 calc R . .
C6 C 0.26236(15) 0.3268(8) 0.3500(4) 0.063(2) Uani 1 1 d . . .
H6 H 0.2823 0.3696 0.3494 0.076 Uiso 1 1 calc R . .
C7 C 0.24554(12) 0.3927(7) 0.4059(3) 0.0497(18) Uani 1 1 d . . .
C8 C 0.29090(11) 0.5769(8) 0.4725(4) 0.0543(18) Uani 1 1 d . . .
H8A H 0.3061 0.4898 0.4874 0.081 Uiso 1 1 calc R . .
H8B H 0.2980 0.6530 0.5217 0.081 Uiso 1 1 calc R . .
H8C H 0.2907 0.6239 0.4152 0.081 Uiso 1 1 calc R . .
C9 C 0.09234(12) 0.5027(7) 0.6023(3) 0.0485(16) Uani 1 1 d . . .
H9A H 0.0805 0.5721 0.5514 0.058 Uiso 1 1 calc R . .
H9B H 0.0841 0.5205 0.6531 0.058 Uiso 1 1 calc R . .
C10 C 0.08632(12) 0.3304(7) 0.5699(4) 0.0506(19) Uani 1 1 d . . .
H10A H 0.0977 0.2604 0.6210 0.061 Uiso 1 1 calc R . .
H10B H 0.0626 0.3066 0.5483 0.061 Uiso 1 1 calc R . .
C11 C 0.14866(14) 0.4646(8) 0.7289(3) 0.055(2) Uani 1 1 d . . .
H11A H 0.1651 0.5403 0.7644 0.066 Uiso 1 1 calc R . .
H11B H 0.1335 0.4456 0.7625 0.066 Uiso 1 1 calc R . .
C12 C 0.16543(13) 0.3208(8) 0.7242(4) 0.0536(19) Uani 1 1 d . . .
C13 C 0.13391(14) 0.7121(7) 0.6354(3) 0.0532(19) Uani 1 1 d . . .
H13A H 0.1576 0.7334 0.6531 0.064 Uiso 1 1 calc R . .
H13B H 0.1232 0.7520 0.5727 0.064 Uiso 1 1 calc R . .
C14 C 0.12064(14) 0.8009(7) 0.7002(4) 0.0547(19) Uani 1 1 d . . .
C15 C 0.07792(13) 0.3884(8) 0.4052(4) 0.053(2) Uani 1 1 d . . .
H15A H 0.0566 0.4140 0.4112 0.064 Uiso 1 1 calc R . .
H15B H 0.0737 0.3142 0.3544 0.064 Uiso 1 1 calc R . .
C16 C 0.09294(14) 0.5401(10) 0.3794(4) 0.070(2) Uani 1 1 d . . .
C17 C 0.10429(12) 0.1438(7) 0.4794(4) 0.0504(18) Uani 1 1 d . . .
H17A H 0.1141 0.1332 0.4312 0.060 Uiso 1 1 calc R . .
H17B H 0.1200 0.1007 0.5365 0.060 Uiso 1 1 calc R . .
C18 C 0.07347(14) 0.0523(8) 0.4528(3) 0.060(2) Uani 1 1 d . . .
N1 N 0.20721(11) 0.5059(6) 0.5219(3) 0.0537(16) Uani 1 1 d . . .
H1 H 0.2257 0.5524 0.5274 0.064 Uiso 1 1 calc R . .
N2 N 0.12893(9) 0.5361(5) 0.6340(3) 0.0418(13) Uani 1 1 d . . .
N3 N 0.09952(10) 0.3106(5) 0.4937(3) 0.0457(14) Uani 1 1 d . . .
O1 O 0.16756(9) 0.3218(5) 0.4555(2) 0.0539(13) Uani 1 1 d . . .
O2 O 0.18813(8) 0.5541(5) 0.5726(2) 0.0570(13) Uani 1 1 d . . .
O3 O 0.25685(9) 0.5212(5) 0.4618(2) 0.0595(14) Uani 1 1 d . . .
O4 O 0.16591(9) 0.2753(5) 0.6450(2) 0.0519(12) Uani 1 1 d . . .
O5 O 0.17911(9) 0.2491(5) 0.7966(2) 0.0604(14) Uani 1 1 d . . .
O6 O 0.12623(10) 0.9532(5) 0.6945(2) 0.0671(15) Uani 1 1 d . . .
H6A H 0.1097 0.9942 0.6565 0.101 Uiso 1 1 calc R . .
O7 O 0.10921(10) 0.7470(5) 0.7533(2) 0.0638(14) Uani 1 1 d . . .
O8 O 0.12279(8) 0.5768(5) 0.4324(2) 0.0497(11) Uani 1 1 d . . .
O9 O 0.07628(10) 0.6092(5) 0.3088(2) 0.0649(15) Uani 1 1 d . . .
O10 O 0.04528(9) 0.1041(5) 0.4356(3) 0.0598(14) Uani 1 1 d . . .
O11 O 0.07897(10) -0.1044(5) 0.4525(3) 0.0680(16) Uani 1 1 d . . .
H11 H 0.0610 -0.1505 0.4320 0.102 Uiso 1 1 calc R . .
O12 O 0.12704(11) 0.1169(6) 0.8391(3) 0.0865(17) Uani 1 1 d . . .
O13 O -0.02937(13) -0.2820(7) 0.0668(5) 0.089(3) Uani 0.805(10) 1 d P . .
O14A O -0.0160(2) -0.5398(12) -0.2080(5) 0.106(4) Uani 0.637(11) 1 d P . .
O14B O -0.0212(2) -0.4166(15) -0.1819(6) 0.078(4) Uani 0.425(9) 1 d P . .
O14C O -0.0110(3) -0.3025(19) -0.0788(9) 0.138(6) Uani 0.458(11) 1 d P . .
O15A O 0.0373(2) -0.073(2) 0.1943(7) 0.333(9) Uani 1.000(18) 1 d . . .
O15B O 0.0224(3) 0.1031(19) 0.1359(10) 0.040(4) Uiso 0.214(7) 1 d P . .
O15C O 0.0176(5) 0.107(3) 0.1966(13) 0.132(7) Uiso 0.362(12) 1 d P . .
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'
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
O2 Ru1 O4 94.32(15) . . ?
O2 Ru1 O1 81.89(16) . . ?
O4 Ru1 O1 93.93(16) . . ?
O2 Ru1 O8 91.71(15) . . ?
O4 Ru1 O8 173.75(15) . . ?
O1 Ru1 O8 88.54(15) . . ?
O2 Ru1 N2 95.95(16) . . ?
O4 Ru1 N2 82.95(16) . . ?
O1 Ru1 N2 176.08(13) . . ?
O8 Ru1 N2 94.80(15) . . ?
O2 Ru1 N3 174.16(16) . . ?
O4 Ru1 N3 91.50(15) . . ?
O1 Ru1 N3 98.16(17) . . ?
O8 Ru1 N3 82.46(15) . . ?
N2 Ru1 N3 84.33(17) . . ?
O1 C1 N1 118.9(5) . . ?
O1 C1 C2 120.4(5) . . ?
N1 C1 C2 120.7(5) . . ?
C7 C2 C3 118.8(5) . . ?
C7 C2 C1 126.2(5) . . ?
C3 C2 C1 114.7(5) . . ?
C4 C3 C2 119.6(6) . . ?
C5 C4 C3 119.5(6) . . ?
C4 C5 C6 122.0(6) . . ?
C5 C6 C7 118.6(6) . . ?
C2 C7 O3 115.2(5) . . ?
C2 C7 C6 121.2(5) . . ?
O3 C7 C6 123.6(5) . . ?
N2 C9 C10 108.9(4) . . ?
N3 C10 C9 107.3(5) . . ?
C12 C11 N2 114.4(4) . . ?
O5 C12 O4 123.2(6) . . ?
O5 C12 C11 118.2(5) . . ?
O4 C12 C11 118.6(5) . . ?
C14 C13 N2 115.2(5) . . ?
O7 C14 O6 123.7(6) . . ?
O7 C14 C13 126.7(6) . . ?
O6 C14 C13 109.4(5) . . ?
N3 C15 C16 114.7(4) . . ?
O9 C16 O8 125.8(7) . . ?
O9 C16 C15 117.5(5) . . ?
O8 C16 C15 116.6(5) . . ?
C18 C17 N3 113.7(5) . . ?
O10 C18 O11 120.9(6) . . ?
O10 C18 C17 126.3(6) . . ?
O11 C18 C17 112.7(5) . . ?
C1 N1 O2 118.5(5) . . ?
C9 N2 C13 108.6(4) . . ?
C9 N2 C11 113.7(4) . . ?
C13 N2 C11 110.6(4) . . ?
C9 N2 Ru1 107.0(3) . . ?
C13 N2 Ru1 111.3(3) . . ?
C11 N2 Ru1 105.6(3) . . ?
C17 N3 C10 109.9(5) . . ?
C17 N3 C15 111.6(4) . . ?
C10 N3 C15 112.2(4) . . ?
C17 N3 Ru1 110.1(3) . . ?
C10 N3 Ru1 105.1(3) . . ?
C15 N3 Ru1 107.6(3) . . ?
C1 O1 Ru1 110.2(3) . . ?
N1 O2 Ru1 110.5(3) . . ?
C7 O3 C8 116.4(5) . . ?
C12 O4 Ru1 115.0(4) . . ?
C16 O8 Ru1 118.1(4) . . ?
O14A O14B O14C 141.0(9) . . ?
O15B O15A O15C 33.8(9) . . ?
O15C O15B O15A 73.3(15) . . ?
O15B O15C O15A 73.0(16) . . ?
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
Ru1 O2 1.964(4) . ?
Ru1 O4 2.016(4) . ?
Ru1 O1 2.019(4) . ?
Ru1 O8 2.044(3) . ?
Ru1 N2 2.060(4) . ?
Ru1 N3 2.156(4) . ?
C1 O1 1.323(7) . ?
C1 N1 1.319(8) . ?
C1 C2 1.479(8) . ?
C2 C7 1.370(8) . ?
C2 C3 1.432(8) . ?
C3 C4 1.394(9) . ?
C4 C5 1.371(9) . ?
C5 C6 1.383(9) . ?
C6 C7 1.409(9) . ?
C7 O3 1.372(7) . ?
C8 O3 1.484(7) . ?
C9 N2 1.494(6) . ?
C9 C10 1.544(8) . ?
C10 N3 1.470(8) . ?
C11 C12 1.435(9) . ?
C11 N2 1.530(6) . ?
C12 O5 1.222(6) . ?
C12 O4 1.278(7) . ?
C13 C14 1.505(9) . ?
C13 N2 1.516(8) . ?
C14 O7 1.177(8) . ?
C14 O6 1.329(7) . ?
C15 N3 1.502(6) . ?
C15 C16 1.555(10) . ?
C16 O9 1.220(7) . ?
C16 O8 1.290(6) . ?
C17 C18 1.462(8) . ?
C17 N3 1.465(7) . ?
C18 O10 1.222(7) . ?
C18 O11 1.358(8) . ?
N1 O2 1.368(7) . ?
O14A O14B 1.174(16) . ?
O14B O14C 1.773(18) . ?
O15A O15B 1.75(2) . ?
O15A O15C 1.75(3) . ?
O15B O15C 1.02(3) . ?
