#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/53/4315367.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_4315367
loop_
_publ_author_name
'Takahiko Kojima'
'Norihisa Hirasa'
'Daisuke Noguchi'
'Tomoya Ishizuka'
'Soushi Miyazaki'
'Yoshihito Shiota'
'Kazunari Yoshizawa'
'Shunichi Fukuzumi'
_publ_section_title
;
 Synthesis and Characterization of Ruthenium(II)-Pyridylamine Complexes
 with Catechol Pendants as Metal Binding Sites
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3737
_journal_page_last               3745
_journal_paper_doi               10.1021/ic902070q
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C32 H28 Cl N6 O6 Ru, H2 O, Cl '
_chemical_formula_sum            'C32 H30 Cl2 N6 O7 Ru'
_chemical_formula_weight         782.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.0165(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.1592(2)
_cell_length_b                   16.1463(3)
_cell_length_c                   18.4551(7)
_cell_measurement_reflns_used    23447
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      3.1
_cell_volume                     3891.83(17)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  MERCURY
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25631
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             1592.00
_exptl_crystal_size_max          0.00
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7156
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.0030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1247P)²+7.4663P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2158
_reflns_number_gt                5351
_reflns_number_total             7156
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic902070q_si_002.cif
_cod_data_source_block           '_RGK1571'
_cod_original_cell_volume        3891.82(18)
_cod_original_formula_sum        'C32 H30 Cl2 N6 O7 Ru '
_cod_database_code               4315367
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,1/2-Y,1/2+Z
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 0.59771(3) 0.50485(3) 0.32292(3) 0.0358(2) Uani 1 1 d . . .
Cl1 Cl 0.63696(11) 0.62452(9) 0.40811(7) 0.0383(4) Uani 1 1 d . . .
O1 O 0.4438(3) 0.5165(2) 0.3383(2) 0.0382(9) Uani 1 1 d . . .
O3 O -0.0021(4) 0.5805(4) 0.4088(3) 0.0779(17) Uani 1 1 d . . .
O4 O 0.3462(4) 0.6796(4) 0.1164(4) 0.097(2) Uani 1 1 d U . .
O5 O -0.0118(4) 0.6211(4) 0.1897(4) 0.095(2) Uani 1 1 d U . .
O6 O -0.0067(4) 0.4631(4) 0.2267(4) 0.0787(16) Uani 1 1 d U . .
N1 N 0.5747(4) 0.4019(3) 0.2597(3) 0.0379(11) Uani 1 1 d . . .
N2 N 0.7473(4) 0.4827(3) 0.3095(3) 0.0412(12) Uani 1 1 d . . .
N3 N 0.6194(4) 0.4265(3) 0.4068(3) 0.0385(11) Uani 1 1 d . . .
N4 N 0.4490(4) 0.4256(3) 0.4361(3) 0.0407(12) Uani 1 1 d . . .
H4N H 0.4107 0.4059 0.4665 0.049 Uiso 1 1 calc R . .
N5 N 0.6129(4) 0.5854(3) 0.2353(3) 0.0413(12) Uani 1 1 d . . .
N6 N 0.4411(4) 0.5936(4) 0.1939(3) 0.0456(12) Uani 1 1 d U . .
H6N H 0.4361 0.5548 0.2252 0.055 Uiso 1 1 calc R . .
C1 C 0.4852(4) 0.3596(4) 0.2472(3) 0.0420(14) Uani 1 1 d . . .
H1 H 0.4272 0.3810 0.2646 0.050 Uiso 1 1 calc R . .
C2 C 0.4779(5) 0.2861(4) 0.2096(4) 0.0486(16) Uani 1 1 d . . .
H2 H 0.4150 0.2593 0.2008 0.058 Uiso 1 1 calc R . .
C3 C 0.5635(5) 0.2514(4) 0.1846(4) 0.0497(16) Uani 1 1 d . . .
H3 H 0.5595 0.2020 0.1585 0.060 Uiso 1 1 calc R . .
C4 C 0.6555(5) 0.2935(4) 0.2002(4) 0.0474(16) Uani 1 1 d . . .
H4 H 0.7152 0.2711 0.1862 0.057 Uiso 1 1 calc R . .
C5 C 0.6588(4) 0.3694(4) 0.2368(3) 0.0377(13) Uani 1 1 d . . .
C6 C 0.7533(5) 0.4205(4) 0.2495(4) 0.0456(15) Uani 1 1 d . . .
H6A H 0.7633 0.4494 0.2048 0.055 Uiso 1 1 calc R . .
H6B H 0.8119 0.3847 0.2623 0.055 Uiso 1 1 calc R . .
C7 C 0.7952(4) 0.4495(4) 0.3818(4) 0.0454(15) Uani 1 1 d . . .
H7A H 0.8196 0.4953 0.4132 0.055 Uiso 1 1 calc R . .
H7B H 0.8536 0.4152 0.3744 0.055 Uiso 1 1 calc R . .
C8 C 0.7193(4) 0.3990(4) 0.4184(3) 0.0406(14) Uani 1 1 d . . .
C9 C 0.7452(5) 0.3343(4) 0.4657(3) 0.0450(15) Uani 1 1 d . . .
H9 H 0.8123 0.3150 0.4727 0.054 Uiso 1 1 calc R . .
C10 C 0.6720(5) 0.2984(4) 0.5023(4) 0.0503(16) Uani 1 1 d . . .
H10 H 0.6892 0.2540 0.5335 0.060 Uiso 1 1 calc R . .
C11 C 0.5729(5) 0.3280(4) 0.4930(3) 0.0439(15) Uani 1 1 d . . .
H11 H 0.5229 0.3047 0.5183 0.053 Uiso 1 1 calc R . .
C12 C 0.5498(5) 0.3938(4) 0.4447(3) 0.0403(14) Uani 1 1 d . . .
C13 C 0.4008(5) 0.4822(4) 0.3880(3) 0.0410(14) Uani 1 1 d . . .
C14 C 0.2940(5) 0.5020(4) 0.3937(3) 0.0402(14) Uani 1 1 d . . .
C15 C 0.2276(5) 0.4523(5) 0.4271(4) 0.0497(16) Uani 1 1 d . . .
H15 H 0.2496 0.4015 0.4470 0.060 Uiso 1 1 calc R . .
C16 C 0.1277(5) 0.4791(5) 0.4305(4) 0.0528(18) Uani 1 1 d . . .
H16 H 0.0832 0.4455 0.4527 0.063 Uiso 0.465(10) 1 calc PR A 2
O2 O 0.0605(8) 0.4259(9) 0.4596(6) 0.090(4) Uani 0.535(10) 1 d P A 1
C17 C 0.0937(5) 0.5529(5) 0.4023(4) 0.0541(18) Uani 1 1 d . A .
C18 C 0.1576(5) 0.6028(5) 0.3672(4) 0.0551(18) Uani 1 1 d . . .
H18 H 0.1338 0.6530 0.3472 0.066 Uiso 0.535(10) 1 calc PR A 1
O2A O 0.1338(7) 0.6829(6) 0.3462(6) 0.052(3) Uani 0.465(10) 1 d P A 2
C19 C 0.2574(5) 0.5779(4) 0.3618(4) 0.0475(16) Uani 1 1 d . . .
H19 H 0.3001 0.6109 0.3373 0.057 Uiso 1 1 calc R . .
C20 C 0.7908(4) 0.5638(4) 0.2881(4) 0.0444(15) Uani 1 1 d . . .
H20A H 0.8540 0.5545 0.2674 0.053 Uiso 1 1 calc R . .
H20B H 0.8054 0.5990 0.3307 0.053 Uiso 1 1 calc R . .
C21 C 0.7125(5) 0.6055(4) 0.2321(4) 0.0440(15) Uani 1 1 d . . .
C22 C 0.7409(5) 0.6598(5) 0.1826(4) 0.061(2) Uani 1 1 d . . .
H22 H 0.8097 0.6712 0.1802 0.074 Uiso 1 1 calc R . .
C23 C 0.6642(5) 0.6985(5) 0.1347(4) 0.061(2) Uani 1 1 d . . .
H23 H 0.6820 0.7388 0.1025 0.073 Uiso 1 1 calc R . .
C24 C 0.5646(5) 0.6777(5) 0.1352(4) 0.0588(19) Uani 1 1 d . . .
H24 H 0.5137 0.7010 0.1020 0.071 Uiso 1 1 calc R . .
C25 C 0.5405(5) 0.6197(4) 0.1874(3) 0.0429(14) Uani 1 1 d . . .
C26 C 0.3504(5) 0.6211(5) 0.1579(4) 0.0625(17) Uani 1 1 d U . .
C27 C 0.2580(5) 0.5749(5) 0.1732(4) 0.0551(15) Uani 1 1 d U . .
C28 C 0.1668(5) 0.6192(5) 0.1703(4) 0.0610(17) Uani 1 1 d U . .
H28 H 0.1647 0.6746 0.1565 0.073 Uiso 1 1 calc R . .
C29 C 0.0796(5) 0.5807(5) 0.1879(5) 0.0679(18) Uani 1 1 d U . .
C30 C 0.0814(5) 0.4966(5) 0.2093(5) 0.0630(17) Uani 1 1 d U . .
C31 C 0.1721(5) 0.4529(5) 0.2107(4) 0.0581(17) Uani 1 1 d U . .
H31 H 0.1748 0.3972 0.2234 0.070 Uiso 1 1 calc R . .
C32 C 0.2599(5) 0.4932(5) 0.1927(4) 0.0561(16) Uani 1 1 d U . .
H32 H 0.3208 0.4638 0.1941 0.067 Uiso 1 1 calc R . .
Cl2 Cl -0.0056(3) 0.8077(2) 0.1730(3) 0.0636(15) Uiso 0.535(10) 1 d P A 1
Cl2A Cl 0.0077(7) 0.8011(5) 0.2126(7) 0.127(3) Uiso 0.465(10) 1 d P A 2
O8 O -0.0591(13) 0.7348(11) 0.3342(11) 0.130(6) Uiso 0.535(10) 1 d P A 1
O8A O -0.034(3) 0.747(3) 0.402(3) 0.284(18) Uiso 0.465(10) 1 d P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
Cl Cl 0.148 0.159
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ru Ru -1.259 0.836
;
International Tables for Crystallography
(1992, 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
Cl1 Ru1 O1 88.51(11) yes . . .
Cl1 Ru1 N1 175.03(13) yes . . .
Cl1 Ru1 N2 94.78(14) yes . . .
Cl1 Ru1 N3 90.18(14) yes . . .
Cl1 Ru1 N5 88.48(14) yes . . .
O1 Ru1 N1 94.17(17) yes . . .
O1 Ru1 N2 175.02(18) yes . . .
O1 Ru1 N3 90.05(18) yes . . .
O1 Ru1 N5 103.51(17) yes . . .
N1 Ru1 N2 82.28(19) yes . . .
N1 Ru1 N3 85.63(19) yes . . .
N1 Ru1 N5 94.9(2) yes . . .
N2 Ru1 N3 86.2(2) yes . . .
N2 Ru1 N5 80.36(19) yes . . .
N3 Ru1 N5 166.33(18) yes . . .
Ru1 O1 C13 126.0(3) yes . . .
Ru1 N1 C1 125.2(4) yes . . .
Ru1 N1 C5 115.5(3) yes . . .
C1 N1 C5 118.8(5) yes . . .
Ru1 N2 C6 110.1(3) yes . . .
Ru1 N2 C7 105.1(3) yes . . .
Ru1 N2 C20 106.4(3) yes . . .
C6 N2 C7 111.3(4) yes . . .
C6 N2 C20 109.4(5) yes . . .
C7 N2 C20 114.3(4) yes . . .
Ru1 N3 C8 111.6(3) yes . . .
Ru1 N3 C12 128.2(3) yes . . .
C8 N3 C12 119.8(5) yes . . .
C12 N4 C13 131.8(5) yes . . .
Ru1 N5 C21 111.4(3) yes . . .
Ru1 N5 C25 129.6(4) yes . . .
C21 N5 C25 119.0(5) yes . . .
C25 N6 C26 129.3(6) yes . . .
N1 C1 C2 121.9(5) yes . . .
C1 C2 C3 120.5(5) yes . . .
C2 C3 C4 117.2(6) yes . . .
C3 C4 C5 120.3(6) yes . . .
N1 C5 C4 121.2(5) yes . . .
N1 C5 C6 116.1(5) yes . . .
C4 C5 C6 122.6(5) yes . . .
N2 C6 C5 111.6(5) yes . . .
N2 C7 C8 111.1(4) yes . . .
N3 C8 C7 115.3(5) yes . . .
N3 C8 C9 120.0(5) yes . . .
C7 C8 C9 124.5(5) yes . . .
C8 C9 C10 119.9(5) yes . . .
C9 C10 C11 120.2(6) yes . . .
C10 C11 C12 118.1(6) yes . . .
N3 C12 N4 119.7(5) yes . . .
N3 C12 C11 121.9(5) yes . . .
N4 C12 C11 118.4(5) yes . . .
O1 C13 N4 123.3(5) yes . . .
O1 C13 C14 118.5(5) yes . . .
N4 C13 C14 118.2(5) yes . . .
C13 C14 C15 124.8(5) yes . . .
C13 C14 C19 116.2(5) yes . . .
C15 C14 C19 119.0(5) yes . . .
C14 C15 C16 119.3(6) yes . . .
O2 C16 C15 118.4(7) yes . . .
O2 C16 C17 119.8(7) yes . . .
C15 C16 C17 121.7(6) yes . . .
O3 C17 C16 121.6(6) yes . . .
O3 C17 C18 118.3(6) yes . . .
C16 C17 C18 120.1(6) yes . . .
O2A C18 C17 123.4(7) yes . . .
O2A C18 C19 115.9(7) yes . . .
C17 C18 C19 120.0(6) yes . . .
C14 C19 C18 119.8(6) yes . . .
N2 C20 C21 108.5(4) yes . . .
N5 C21 C20 116.1(5) yes . . .
N5 C21 C22 122.2(5) yes . . .
C20 C21 C22 121.7(5) yes . . .
C21 C22 C23 118.5(6) yes . . .
C22 C23 C24 120.5(7) yes . . .
C23 C24 C25 118.0(6) yes . . .
N5 C25 N6 114.7(5) yes . . .
N5 C25 C24 121.8(5) yes . . .
N6 C25 C24 123.6(5) yes . . .
O4 C26 N6 121.9(6) yes . . .
O4 C26 C27 122.5(6) yes . . .
N6 C26 C27 115.6(6) yes . . .
C26 C27 C28 117.3(7) yes . . .
C26 C27 C32 123.2(6) yes . . .
C28 C27 C32 119.5(6) yes . . .
C27 C28 C29 119.9(7) yes . . .
O5 C29 C28 123.3(7) yes . . .
O5 C29 C30 115.8(6) yes . . .
C28 C29 C30 120.9(6) yes . . .
O6 C30 C29 117.7(6) yes . . .
O6 C30 C31 123.6(6) yes . . .
C29 C30 C31 118.7(6) yes . . .
C30 C31 C32 119.5(6) yes . . .
C27 C32 C31 121.5(6) yes . . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ru1 Cl1 2.5047(14) yes . .
Ru1 O1 2.088(4) yes . .
Ru1 N1 2.032(4) yes . .
Ru1 N2 2.045(5) yes . .
Ru1 N3 1.993(4) yes . .
Ru1 N5 2.103(5) yes . .
O1 C13 1.262(7) yes . .
O2 C16 1.387(14) yes . .
O2A C18 1.377(12) yes . .
O3 C17 1.356(8) yes . .
O4 C26 1.213(11) yes . .
O5 C29 1.373(9) yes . .
O6 C30 1.353(9) yes . .
N1 C1 1.356(7) yes . .
N1 C5 1.339(7) yes . .
N2 C6 1.504(8) yes . .
N2 C7 1.502(8) yes . .
N2 C20 1.502(8) yes . .
N3 C8 1.378(7) yes . .
N3 C12 1.327(8) yes . .
N4 C12 1.413(7) yes . .
N4 C13 1.374(7) yes . .
N5 C21 1.359(7) yes . .
N5 C25 1.338(7) yes . .
N6 C25 1.393(7) yes . .
N6 C26 1.368(8) yes . .
C1 C2 1.371(9) yes . .
C2 C3 1.387(9) yes . .
C3 C4 1.387(9) yes . .
C4 C5 1.398(9) yes . .
C5 C6 1.488(8) yes . .
C7 C8 1.511(9) yes . .
C8 C9 1.377(8) yes . .
C9 C10 1.371(9) yes . .
C10 C11 1.379(9) yes . .
C11 C12 1.398(8) yes . .
C13 C14 1.458(8) yes . .
C14 C15 1.386(9) yes . .
C14 C19 1.417(8) yes . .
C15 C16 1.393(9) yes . .
C16 C17 1.353(10) yes . .
C17 C18 1.382(10) yes . .
C18 C19 1.389(9) yes . .
C20 C21 1.524(8) yes . .
C21 C22 1.351(10) yes . .
C22 C23 1.404(10) yes . .
C23 C24 1.354(10) yes . .
C24 C25 1.407(10) yes . .
C26 C27 1.482(10) yes . .
C27 C28 1.393(9) yes . .
C27 C32 1.366(10) yes . .
C28 C29 1.378(10) yes . .
C29 C30 1.412(11) yes . .
C30 C31 1.385(10) yes . .
C31 C32 1.400(10) yes . .
