#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/22/7032283.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_7032283
loop_
_publ_author_name
'Nagao, Hirotaka'
'Shimura, Naoto'
'Yonezawa, Haruka'
_publ_section_title
;
 Formation of bis(2-pyridylcarbonyl)aminate by oxidation of
 ethylbis(2-pyridylmethyl)amine on the trichloridoruthenium(iii) complex.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15391
_journal_page_last               15397
_journal_paper_doi               10.1039/c4dt01842g
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C12 H9 N3 O2 Ru, 2(H2 O), 5(H1 O0.5)'
_chemical_formula_sum            'C12 H18 Cl3 N3 O6.5 Ru'
_chemical_formula_weight         515.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 96.7949(15)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.139(4)
_cell_length_b                   8.711(4)
_cell_length_c                   21.250(8)
_cell_measurement_reflns_used    5055
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.03
_cell_volume                     1863.6(13)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury70'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14104
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.307
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1032.00
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.020
_refine_diff_density_min         -0.710
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4255
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0242P)²+4.7157P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0794
_reflns_number_gt                3845
_reflns_number_total             4265
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c4dt01842g2.cif
_cod_data_source_block           RuCl3Hbpca
_cod_depositor_comments
'Adding full bibliography for 7032281--7032283.cif.'
_cod_original_cell_volume        1863.6(12)
_cod_original_formula_sum        'C12 H18 Cl3 N3 O6.50 Ru'
_cod_database_code               7032283
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+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
Ru(1) Ru 0.23298(2) 0.22317(3) 0.390204(11) 0.01527(8) Uani 1.0 4 d .
Cl(1) Cl 0.23661(8) 0.23130(9) 0.27790(3) 0.02504(17) Uani 1.0 4 d .
Cl(2) Cl 0.44788(7) 0.11337(8) 0.40146(3) 0.02004(15) Uani 1.0 4 d .
Cl(3) Cl 0.01991(7) 0.33432(9) 0.38096(4) 0.02353(16) Uani 1.0 4 d .
O(1) O 0.2205(3) 0.0434(3) 0.56517(10) 0.0276(6) Uani 1.0 4 d .
O(2) O 0.2798(3) 0.3661(3) 0.57345(10) 0.0256(5) Uani 1.0 4 d .
O(3) O 0.4987(3) 0.0224(4) 0.73408(14) 0.0486(8) Uani 1.0 4 d .
O(4) O 0.3010(4) 0.1885(7) 0.68273(14) 0.0942(18) Uani 1.0 4 d .
O(5) O 0.2182(6) -0.1433(6) 0.6673(3) 0.0334(12) Uani 0.5000 4 d .
O(6) O 0.2157(8) -0.0909(9) 0.7827(3) 0.0562(17) Uani 0.5000 4 d .
O(7) O 0.4241(7) -0.3475(7) 0.7022(3) 0.0514(16) Uani 0.5000 4 d .
O(8) O 0.2961(7) -0.2519(9) 0.6644(3) 0.0577(19) Uani 0.5000 4 d .
O(9) O 0.3577(6) 0.4799(9) 0.7264(4) 0.064(3) Uani 0.5000 4 d .
N(1) N 0.2364(3) 0.2161(3) 0.48332(11) 0.0163(5) Uani 1.0 4 d .
N(2) N 0.1519(3) 0.0078(3) 0.39762(12) 0.0182(5) Uani 1.0 4 d .
N(3) N 0.3092(3) 0.4387(3) 0.41069(12) 0.0176(5) Uani 1.0 4 d .
C(1) C 0.2060(3) 0.0770(4) 0.50888(14) 0.0195(6) Uani 1.0 4 d .
C(2) C 0.2771(3) 0.3472(4) 0.51636(14) 0.0184(6) Uani 1.0 4 d .
C(3) C 0.1500(3) -0.0349(4) 0.45898(15) 0.0193(6) Uani 1.0 4 d .
C(4) C 0.0959(3) -0.1732(4) 0.47505(17) 0.0243(7) Uani 1.0 4 d .
C(5) C 0.0445(3) -0.2718(4) 0.42699(19) 0.0286(8) Uani 1.0 4 d .
C(6) C 0.0481(4) -0.2291(4) 0.36478(18) 0.0284(8) Uani 1.0 4 d .
C(7) C 0.1033(3) -0.0884(4) 0.35150(16) 0.0235(7) Uani 1.0 4 d .
C(8) C 0.3173(3) 0.4716(4) 0.47360(14) 0.0183(6) Uani 1.0 4 d .
C(9) C 0.3635(3) 0.6112(4) 0.49778(16) 0.0220(7) Uani 1.0 4 d .
C(10) C 0.4013(3) 0.7216(4) 0.45650(17) 0.0243(7) Uani 1.0 4 d .
C(11) C 0.3920(3) 0.6897(4) 0.39233(17) 0.0253(7) Uani 1.0 4 d .
C(12) C 0.3452(3) 0.5462(4) 0.37103(15) 0.0219(7) Uani 1.0 4 d .
H(1) H 0.0940 -0.2002 0.5182 0.0292 Uiso 1.0 4 calc R
H(2) H 0.0073 -0.3676 0.4369 0.0343 Uiso 1.0 4 calc R
H(3) H 0.0132 -0.2952 0.3313 0.0340 Uiso 1.0 4 calc R
H(4) H 0.1065 -0.0598 0.3086 0.0282 Uiso 1.0 4 calc R
H(5) H 0.3692 0.6313 0.5420 0.0264 Uiso 1.0 4 calc R
H(6) H 0.4333 0.8185 0.4721 0.0292 Uiso 1.0 4 calc R
H(7) H 0.4170 0.7643 0.3633 0.0304 Uiso 1.0 4 calc R
H(8) H 0.3386 0.5239 0.3270 0.0262 Uiso 1.0 4 calc R
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 for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ru Ru -1.2594 0.8363
;
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
Cl(1) Ru(1) Cl(2) 89.43(3)
Cl(1) Ru(1) Cl(3) 91.54(3)
Cl(1) Ru(1) N(1) 178.13(8)
Cl(1) Ru(1) N(2) 99.01(8)
Cl(1) Ru(1) N(3) 97.72(8)
Cl(2) Ru(1) Cl(3) 178.92(3)
Cl(2) Ru(1) N(1) 88.83(8)
Cl(2) Ru(1) N(2) 89.72(8)
Cl(2) Ru(1) N(3) 91.67(8)
Cl(3) Ru(1) N(1) 90.20(8)
Cl(3) Ru(1) N(2) 90.60(8)
Cl(3) Ru(1) N(3) 87.73(8)
N(1) Ru(1) N(2) 81.66(10)
N(1) Ru(1) N(3) 81.66(11)
N(2) Ru(1) N(3) 163.23(11)
O(5) O(8) O(7) 145.4(6)
Ru(1) N(1) C(1) 116.36(19)
Ru(1) N(1) C(2) 116.9(2)
C(1) N(1) C(2) 126.5(3)
Ru(1) N(2) C(3) 111.96(19)
Ru(1) N(2) C(7) 129.0(3)
C(3) N(2) C(7) 119.0(3)
Ru(1) N(3) C(8) 112.2(2)
Ru(1) N(3) C(12) 128.9(2)
C(8) N(3) C(12) 118.8(3)
O(1) C(1) N(1) 126.1(3)
O(1) C(1) C(3) 121.8(3)
N(1) C(1) C(3) 112.1(3)
O(2) C(2) N(1) 126.0(3)
O(2) C(2) C(8) 121.9(3)
N(1) C(2) C(8) 112.1(3)
N(2) C(3) C(1) 116.9(3)
N(2) C(3) C(4) 121.8(3)
C(1) C(3) C(4) 121.3(3)
C(3) C(4) C(5) 118.9(4)
C(4) C(5) C(6) 119.3(4)
C(5) C(6) C(7) 119.3(4)
N(2) C(7) C(6) 121.7(4)
N(3) C(8) C(2) 117.0(3)
N(3) C(8) C(9) 122.0(3)
C(2) C(8) C(9) 121.0(3)
C(8) C(9) C(10) 118.9(3)
C(9) C(10) C(11) 119.5(3)
C(10) C(11) C(12) 118.8(3)
N(3) C(12) C(11) 122.0(3)
C(3) C(4) H(1) 120.569
C(5) C(4) H(1) 120.563
C(4) C(5) H(2) 120.379
C(6) C(5) H(2) 120.368
C(5) C(6) H(3) 120.347
C(7) C(6) H(3) 120.344
N(2) C(7) H(4) 119.133
C(6) C(7) H(4) 119.135
C(8) C(9) H(5) 120.567
C(10) C(9) H(5) 120.567
C(9) C(10) H(6) 120.247
C(11) C(10) H(6) 120.240
C(10) C(11) H(7) 120.626
C(12) C(11) H(7) 120.623
N(3) C(12) H(8) 118.985
C(11) C(12) H(8) 118.989
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru(1) Cl(1) 2.3921(12)
Ru(1) Cl(2) 2.3656(11)
Ru(1) Cl(3) 2.3543(11)
Ru(1) N(1) 1.976(3)
Ru(1) N(2) 2.061(3)
Ru(1) N(3) 2.058(3)
O(1) C(1) 1.223(4)
O(2) C(2) 1.221(4)
O(5) O(8) 1.238(9)
O(7) O(8) 1.666(9)
N(1) C(1) 1.377(4)
N(1) C(2) 1.378(4)
N(2) C(3) 1.358(5)
N(2) C(7) 1.339(4)
N(3) C(8) 1.360(4)
N(3) C(12) 1.338(5)
C(1) C(3) 1.502(5)
C(2) C(8) 1.501(5)
C(3) C(4) 1.383(5)
C(4) C(5) 1.388(5)
C(5) C(6) 1.378(6)
C(6) C(7) 1.390(5)
C(8) C(9) 1.380(5)
C(9) C(10) 1.386(5)
C(10) C(11) 1.384(5)
C(11) C(12) 1.394(5)
C(4) H(1) 0.950
C(5) H(2) 0.950
C(6) H(3) 0.950
C(7) H(4) 0.950
C(9) H(5) 0.950
C(10) H(6) 0.950
C(11) H(7) 0.950
C(12) H(8) 0.950
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Cl1 Ru1 N2 C3 173.90(14)
Cl1 Ru1 N2 C7 -6.5(2)
Cl1 Ru1 N3 C8 178.68(13)
Cl1 Ru1 N3 C12 1.2(2)
Cl2 Ru1 N1 C1 -81.00(15)
Cl2 Ru1 N1 C2 94.90(16)
Cl2 Ru1 N2 C3 84.52(15)
Cl2 Ru1 N2 C7 -95.9(2)
Cl2 Ru1 N3 C8 -91.67(14)
Cl2 Ru1 N3 C12 90.86(19)
Cl3 Ru1 N1 C1 99.47(15)
Cl3 Ru1 N1 C2 -84.64(16)
Cl3 Ru1 N2 C3 -94.44(15)
Cl3 Ru1 N2 C7 85.2(2)
Cl3 Ru1 N3 C8 87.43(14)
Cl3 Ru1 N3 C12 -90.04(19)
N1 Ru1 N2 C3 -4.33(16)
N1 Ru1 N2 C7 175.3(3)
N2 Ru1 N1 C1 8.89(16)
N2 Ru1 N1 C2 -175.22(18)
N1 Ru1 N3 C8 -3.10(15)
N1 Ru1 N3 C12 179.4(2)
N3 Ru1 N1 C1 -172.86(18)
N3 Ru1 N1 C2 3.04(16)
Ru1 N1 C1 O1 169.1(2)
Ru1 N1 C1 C3 -11.2(3)
Ru1 N1 C2 O2 176.6(2)
Ru1 N1 C2 C8 -2.4(3)
C1 N1 C2 O2 -8.0(5)
C1 N1 C2 C8 173.1(3)
C2 N1 C1 O1 -6.4(5)
C2 N1 C1 C3 173.3(3)
Ru1 N2 C3 C1 -0.4(3)
Ru1 N2 C3 C4 177.85(18)
Ru1 N2 C7 C6 -178.06(17)
C3 N2 C7 C6 1.5(5)
C7 N2 C3 C1 179.9(3)
C7 N2 C3 C4 -1.8(4)
Ru1 N3 C8 C2 2.8(3)
Ru1 N3 C8 C9 -178.84(18)
Ru1 N3 C12 C11 178.05(17)
C8 N3 C12 C11 0.7(4)
C12 N3 C8 C2 -179.5(3)
C12 N3 C8 C9 -1.1(4)
O1 C1 C3 N2 -172.8(3)
O1 C1 C3 C4 8.9(5)
N1 C1 C3 N2 7.5(4)
N1 C1 C3 C4 -170.8(3)
O2 C2 C8 N3 -179.4(3)
O2 C2 C8 C9 2.2(5)
N1 C2 C8 N3 -0.4(4)
N1 C2 C8 C9 -178.8(3)
N2 C3 C4 C5 1.2(5)
C1 C3 C4 C5 179.4(3)
C3 C4 C5 C6 -0.3(5)
C4 C5 C6 C7 0.1(5)
C5 C6 C7 N2 -0.7(5)
N3 C8 C9 C10 0.7(5)
C2 C8 C9 C10 179.1(3)
C8 C9 C10 C11 0.0(5)
C9 C10 C11 C12 -0.3(5)
C10 C11 C12 N3 -0.0(5)
