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#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/37/7013784.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_7013784
loop_
_publ_author_name
'Matthews, Craig J.'
'Elsegood, Mark R. J.'
'Bernardinelli, Gérald'
'Clegg, William'
'Williams, Alan F.'
_publ_section_title
;
 Crystal structures of dicarboxy-2,2'-bipyridyl complexes: the role of
 hydrogen bonding and stacking interactions.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              492
_journal_page_last               497
_journal_paper_doi               10.1039/b314539e
_journal_year                    2004
_chemical_formula_moiety         'C36 H22 N6 O12 Ru,2.5 H2 O'
_chemical_formula_sum            'C36 H27 N6 O14.5 Ru'
_chemical_formula_weight         876.71
_chemical_name_common
;Ruthenium(iii) tris(2,2'-bipyridine-5,5'-dicarboxylic acid)
2.6-hydrate
;
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 97.147(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.605(2)
_cell_length_b                   12.503(2)
_cell_length_c                   19.601(3)
_cell_measurement_reflns_used    3170
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.94
_cell_volume                     3551.5(9)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'thin-slice ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_sigmaI/netI    0.1353
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9139
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00044(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3128
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0582
_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/[σ²(Fo²)+(0.0382P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                2073
_reflns_number_total             3128
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b314539e.txt
_cod_data_source_block           cjm2a
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'C36 H27 N6 O14.50 Ru'
_cod_database_code               7013784
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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 0.2500 0.22038(5) 0.5000 0.0158(2) Uani 1 2 d S . .
N1 N 0.3367(3) 0.0920(3) 0.48883(18) 0.0159(9) Uani 1 1 d . . .
N2 N 0.3246(2) 0.2118(3) 0.59660(17) 0.0172(9) Uani 1 1 d . . .
C1 C 0.3321(3) 0.0296(3) 0.4321(2) 0.0175(11) Uani 1 1 d . . .
H1 H 0.3050 0.0579 0.3894 0.021 Uiso 1 1 calc R . .
C2 C 0.3655(3) -0.0740(4) 0.4342(2) 0.0207(12) Uani 1 1 d . . .
C3 C 0.4071(3) -0.1147(4) 0.4962(2) 0.0250(12) Uani 1 1 d . . .
H3 H 0.4289 -0.1864 0.4988 0.030 Uiso 1 1 calc R . .
C4 C 0.4167(3) -0.0512(4) 0.5538(2) 0.0241(12) Uani 1 1 d . . .
H4 H 0.4466 -0.0775 0.5963 0.029 Uiso 1 1 calc R . .
C5 C 0.3814(3) 0.0530(4) 0.5488(2) 0.0191(11) Uani 1 1 d . . .
C6 C 0.3816(3) 0.1263(4) 0.6083(2) 0.0180(11) Uani 1 1 d . . .
C7 C 0.4385(3) 0.1128(4) 0.6695(2) 0.0295(13) Uani 1 1 d . . .
H7 H 0.4783 0.0526 0.6759 0.035 Uiso 1 1 calc R . .
C8 C 0.4369(4) 0.1875(4) 0.7211(3) 0.0340(14) Uani 1 1 d . . .
H8 H 0.4761 0.1800 0.7633 0.041 Uiso 1 1 calc R . .
C9 C 0.3775(3) 0.2732(4) 0.7105(2) 0.0239(11) Uani 1 1 d . . .
C10 C 0.3231(3) 0.2819(4) 0.6481(2) 0.0190(10) Uani 1 1 d . . .
H10 H 0.2821 0.3410 0.6412 0.023 Uiso 1 1 calc R . .
C11 C 0.3495(3) -0.1427(4) 0.3700(3) 0.0255(12) Uani 1 1 d . . .
C12 C 0.3749(4) 0.3571(4) 0.7644(3) 0.0281(13) Uani 1 1 d . . .
O1 O 0.3217(2) -0.0988(3) 0.31389(16) 0.0344(10) Uani 1 1 d . . .
O2 O 0.3613(3) -0.2410(3) 0.37833(18) 0.0435(11) Uani 1 1 d . . .
O3 O 0.3030(2) 0.4196(3) 0.75306(17) 0.0314(9) Uani 1 1 d . . .
H3O H 0.3148 0.4786 0.7727 0.047 Uiso 1 1 calc R . .
O4 O 0.4346(3) 0.3657(3) 0.81279(19) 0.0580(13) Uani 1 1 d . . .
N3 N 0.3287(3) 0.3475(3) 0.47488(18) 0.0164(9) Uani 1 1 d . . .
C13 C 0.2923(3) 0.4466(4) 0.4828(2) 0.0183(12) Uani 1 1 d . . .
C14 C 0.3301(4) 0.5386(4) 0.4593(3) 0.0265(13) Uani 1 1 d . . .
H14 H 0.3022 0.6061 0.4648 0.032 Uiso 1 1 calc R . .
C15 C 0.4093(4) 0.5309(4) 0.4276(3) 0.0330(14) Uani 1 1 d . . .
H15 H 0.4361 0.5931 0.4105 0.040 Uiso 1 1 calc R . .
C16 C 0.4492(3) 0.4309(4) 0.4209(2) 0.0223(12) Uani 1 1 d . . .
C17 C 0.4063(3) 0.3420(4) 0.4444(2) 0.0193(12) Uani 1 1 d . . .
H17 H 0.4328 0.2737 0.4388 0.023 Uiso 1 1 calc R . .
C18 C 0.5351(4) 0.4237(4) 0.3880(3) 0.0317(14) Uani 1 1 d . . .
O5 O 0.5712(2) 0.3282(3) 0.39039(18) 0.0331(9) Uani 1 1 d . . .
H5O H 0.6150 0.3267 0.3663 0.050 Uiso 1 1 calc R . .
O6 O 0.5668(3) 0.5001(3) 0.3619(3) 0.0655(14) Uani 1 1 d . . .
O1W O 0.6957(3) 0.3095(5) 0.3136(2) 0.0734(16) Uani 1 1 d D . .
H1WA H 0.685(5) 0.345(5) 0.277(2) 0.110 Uiso 1 1 d D . .
H1WB H 0.7503(19) 0.304(6) 0.333(4) 0.110 Uiso 1 1 d D . .
O2W O 0.8893(16) 0.3990(18) 0.2505(12) 0.114(8) Uiso 0.25 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
N1 Ru1 N1 78.5(2) . 2_556 ?
N1 Ru1 N2 78.29(14) . . ?
N1 Ru1 N2 78.29(14) 2_556 2_556 ?
N1 Ru1 N2 97.02(14) 2_556 . ?
N1 Ru1 N2 97.02(14) . 2_556 ?
N1 Ru1 N3 101.89(14) . . ?
N1 Ru1 N3 172.13(14) 2_556 . ?
N1 Ru1 N3 101.89(14) 2_556 2_556 ?
N1 Ru1 N3 172.13(14) . 2_556 ?
N2 Ru1 N2 174.0(2) . 2_556 ?
N2 Ru1 N3 90.74(14) . . ?
N2 Ru1 N3 93.88(14) 2_556 . ?
N2 Ru1 N3 90.74(14) 2_556 2_556 ?
N2 Ru1 N3 93.88(14) . 2_556 ?
N3 Ru1 N3 78.8(2) . 2_556 ?
Ru1 N1 C1 124.4(3) . . ?
Ru1 N1 C5 114.8(3) . . ?
C1 N1 C5 118.2(4) . . ?
Ru1 N2 C6 116.0(3) . . ?
Ru1 N2 C10 126.9(3) . . ?
C6 N2 C10 117.1(4) . . ?
N1 C1 C2 122.4(4) . . ?
C1 C2 C3 119.0(4) . . ?
C1 C2 C11 119.2(4) . . ?
C3 C2 C11 121.6(4) . . ?
C2 C3 C4 119.8(4) . . ?
C3 C4 C5 118.8(4) . . ?
N1 C5 C4 121.7(4) . . ?
N1 C5 C6 114.3(4) . . ?
C4 C5 C6 123.8(4) . . ?
N2 C6 C5 114.4(4) . . ?
N2 C6 C7 122.2(4) . . ?
C5 C6 C7 123.3(4) . . ?
C6 C7 C8 119.4(5) . . ?
C7 C8 C9 118.9(5) . . ?
C8 C9 C10 118.6(4) . . ?
C8 C9 C12 120.7(4) . . ?
C10 C9 C12 120.7(5) . . ?
N2 C10 C9 123.7(4) . . ?
C2 C11 O1 118.7(4) . . ?
C2 C11 O2 116.3(4) . . ?
O1 C11 O2 124.9(5) . . ?
C9 C12 O3 113.0(4) . . ?
C9 C12 O4 122.5(5) . . ?
O3 C12 O4 124.5(5) . . ?
Ru1 N3 C13 115.9(3) . . ?
Ru1 N3 C17 126.4(3) . . ?
C13 N3 C17 117.3(4) . . ?
N3 C13 C13 114.3(3) . 2_556 ?
N3 C13 C14 122.8(4) . . ?
C13 C13 C14 122.9(3) 2_556 . ?
C13 C14 C15 118.9(5) . . ?
C14 C15 C16 119.2(5) . . ?
C15 C16 C17 118.5(5) . . ?
C15 C16 C18 118.8(5) . . ?
C17 C16 C18 122.7(5) . . ?
N3 C17 C16 123.3(5) . . ?
C16 C18 O5 113.6(5) . . ?
C16 C18 O6 121.9(5) . . ?
O5 C18 O6 124.5(6) . . ?
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 N1 2.073(4) . ?
Ru1 N1 2.073(4) 2_556 ?
Ru1 N2 2.066(3) . ?
Ru1 N2 2.066(3) 2_556 ?
Ru1 N3 2.057(4) . ?
Ru1 N3 2.057(4) 2_556 ?
N1 C1 1.353(5) . ?
N1 C5 1.362(5) . ?
N2 C6 1.357(5) . ?
N2 C10 1.340(5) . ?
C1 C2 1.382(6) . ?
C2 C3 1.386(6) . ?
C2 C11 1.518(6) . ?
C3 C4 1.374(6) . ?
C4 C5 1.399(6) . ?
C5 C6 1.482(6) . ?
C6 C7 1.382(6) . ?
C7 C8 1.380(6) . ?
C8 C9 1.378(6) . ?
C9 C10 1.378(6) . ?
C9 C12 1.493(6) . ?
C11 O1 1.251(5) . ?
C11 O2 1.249(5) . ?
C12 O3 1.305(6) . ?
C12 O4 1.209(6) . ?
N3 C13 1.365(5) . ?
N3 C17 1.346(5) . ?
C13 C13 1.480(9) 2_556 ?
C13 C14 1.379(6) . ?
C14 C15 1.383(7) . ?
C15 C16 1.393(6) . ?
C16 C17 1.383(6) . ?
C16 C18 1.483(7) . ?
C18 O5 1.303(6) . ?
C18 O6 1.203(6) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3O O1 0.84 1.70 2.536(4) 171.5 8
O5 H5O O1W 0.84 1.68 2.512(6) 172.6 .
O1W H1WA O1 0.839(10) 1.91(2) 2.732(5) 167(7) 4
O1W H1WB O2 0.840(10) 1.92(3) 2.726(6) 160(8) 6_655
