#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/22/7032281.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_7032281
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         'C18 H17 N6 O2 Ru, F6 P, H2 O, H0.5 O0.25'
_chemical_formula_sum            'C18 H19.5 F6 N6 O3.25 P Ru'
_chemical_formula_weight         617.92
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                70.735(15)
_cell_angle_beta                 71.344(13)
_cell_angle_gamma                70.709(16)
_cell_formula_units_Z            2
_cell_length_a                   8.838(3)
_cell_length_b                   11.366(4)
_cell_length_c                   13.810(5)
_cell_measurement_reflns_used    3447
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      4.09
_cell_volume                     1200.9(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_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 0.986
_diffrn_measured_fraction_theta_max 0.976
_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  0.0134
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11904
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             617.00
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.560
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5384
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0257P)²+1.1403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0538
_reflns_number_gt                5176
_reflns_number_total             5384
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c4dt01842g2.cif
_cod_data_source_block           RuAN3bpca
_cod_depositor_comments
'Adding full bibliography for 7032281--7032283.cif.'
_cod_original_cell_volume        1201.0(7)
_cod_original_formula_sum        'C18 H19.50 F6 N6 O3.25 P Ru'
_cod_database_code               7032281
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,-Y,-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 0.417189(13) 0.345870(10) 0.315937(8) 0.00940(4) Uani 1.0 2 d .
P(1) P 0.15692(6) 0.12755(4) 0.11782(4) 0.02308(10) Uani 1.0 2 d .
F(1) F 0.33631(14) 0.03461(14) 0.09362(10) 0.0437(4) Uani 1.0 2 d .
F(2) F -0.02709(17) 0.21644(14) 0.14420(12) 0.0499(4) Uani 1.0 2 d .
F(3) F 0.2255(3) 0.22175(17) 0.14499(17) 0.0748(6) Uani 1.0 2 d .
F(4) F 0.08254(15) 0.03323(11) 0.09273(10) 0.0342(3) Uani 1.0 2 d .
F(5) F 0.18251(17) 0.20383(14) -0.00356(11) 0.0466(4) Uani 1.0 2 d .
F(6) F 0.12982(17) 0.04819(16) 0.23979(9) 0.0510(4) Uani 1.0 2 d .
O(1) O 0.26270(17) 0.51778(12) 0.56232(10) 0.0260(3) Uani 1.0 2 d .
O(2) O 0.11940(16) 0.68452(11) 0.38878(10) 0.0248(3) Uani 1.0 2 d .
O(3) O -0.1404(3) -0.08412(18) 0.35677(14) 0.0428(5) Uani 1.0 2 d .
O(4) O 0.5226(10) 0.7413(8) 0.1144(7) 0.062(3) Uani 0.2500 2 d .
N(1) N 0.30402(15) 0.48193(12) 0.39782(10) 0.0117(3) Uani 1.0 2 d .
N(2) N 0.48747(15) 0.24573(12) 0.45610(10) 0.0115(3) Uani 1.0 2 d .
N(3) N 0.31112(15) 0.49114(12) 0.20267(10) 0.0123(3) Uani 1.0 2 d .
N(4) N 0.53434(15) 0.20463(12) 0.23542(10) 0.0133(3) Uani 1.0 2 d .
N(5) N 0.62186(15) 0.41317(12) 0.26050(10) 0.0118(3) Uani 1.0 2 d .
N(6) N 0.20994(15) 0.28242(12) 0.36819(10) 0.0122(3) Uani 1.0 2 d .
C(1) C 0.32207(19) 0.45115(14) 0.49864(12) 0.0144(3) Uani 1.0 2 d .
C(2) C 0.20781(19) 0.59453(14) 0.35054(12) 0.0149(3) Uani 1.0 2 d .
C(3) C 0.43199(18) 0.31728(14) 0.52812(12) 0.0135(3) Uani 1.0 2 d .
C(4) C 0.47320(19) 0.27204(15) 0.62465(12) 0.0171(3) Uani 1.0 2 d .
C(5) C 0.57269(19) 0.14806(15) 0.65036(13) 0.0183(3) Uani 1.0 2 d .
C(6) C 0.62423(19) 0.07361(15) 0.57882(13) 0.0176(3) Uani 1.0 2 d .
C(7) C 0.58110(18) 0.12504(14) 0.48205(12) 0.0143(3) Uani 1.0 2 d .
C(8) C 0.22172(18) 0.59868(14) 0.23722(12) 0.0142(3) Uani 1.0 2 d .
C(9) C 0.1463(2) 0.70970(16) 0.17216(13) 0.0187(3) Uani 1.0 2 d .
C(10) C 0.1617(2) 0.71107(16) 0.06830(13) 0.0206(4) Uani 1.0 2 d .
C(11) C 0.2504(2) 0.60126(17) 0.03368(12) 0.0202(4) Uani 1.0 2 d .
C(12) C 0.32320(19) 0.49276(16) 0.10259(12) 0.0161(3) Uani 1.0 2 d .
C(13) C 0.60190(18) 0.12361(15) 0.19365(12) 0.0153(3) Uani 1.0 2 d .
C(14) C 0.6879(2) 0.01917(16) 0.14086(14) 0.0216(4) Uani 1.0 2 d .
C(15) C 0.73560(19) 0.45300(14) 0.22945(12) 0.0138(3) Uani 1.0 2 d .
C(16) C 0.8822(2) 0.50353(17) 0.18912(14) 0.0220(4) Uani 1.0 2 d .
C(17) C 0.09211(18) 0.24856(14) 0.39316(12) 0.0137(3) Uani 1.0 2 d .
C(18) C -0.05601(19) 0.20172(15) 0.42398(14) 0.0180(3) Uani 1.0 2 d .
H(1) H 0.4341 0.3249 0.6728 0.0205 Uiso 1.0 2 calc R
H(2) H 0.6045 0.1153 0.7157 0.0219 Uiso 1.0 2 calc R
H(3) H 0.6889 -0.0124 0.5956 0.0211 Uiso 1.0 2 calc R
H(4) H 0.6188 0.0735 0.4330 0.0171 Uiso 1.0 2 calc R
H(5) H 0.0851 0.7837 0.1981 0.0225 Uiso 1.0 2 calc R
H(6) H 0.1121 0.7863 0.0220 0.0247 Uiso 1.0 2 calc R
H(7) H 0.2615 0.5999 -0.0367 0.0242 Uiso 1.0 2 calc R
H(8) H 0.3834 0.4175 0.0783 0.0193 Uiso 1.0 2 calc R
H(9) H 0.7971 0.0311 0.0991 0.0259 Uiso 1.0 2 calc R
H(10) H 0.6239 0.0200 0.0943 0.0259 Uiso 1.0 2 calc R
H(11) H 0.7005 -0.0635 0.1939 0.0259 Uiso 1.0 2 calc R
H(12) H 0.8638 0.5818 0.1322 0.0263 Uiso 1.0 2 calc R
H(13) H 0.9772 0.4388 0.1619 0.0263 Uiso 1.0 2 calc R
H(14) H 0.9039 0.5239 0.2463 0.0263 Uiso 1.0 2 calc R
H(15) H -0.1516 0.2655 0.4521 0.0216 Uiso 1.0 2 calc R
H(16) H -0.0426 0.1203 0.4783 0.0216 Uiso 1.0 2 calc R
H(17) H -0.0732 0.1880 0.3622 0.0216 Uiso 1.0 2 calc R
H(18) H -0.0775 -0.0438 0.3229 0.0437 Uiso 1.0 2 calc R
H(19) H -0.0848 -0.1507 0.3683 0.0469 Uiso 1.0 2 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)
;
F F 0.0171 0.0103
;
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)
;
P P 0.1023 0.0942
;
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
N(1) Ru(1) N(2) 80.78(6)
N(1) Ru(1) N(3) 80.65(6)
N(1) Ru(1) N(4) 178.73(5)
N(1) Ru(1) N(5) 90.37(6)
N(1) Ru(1) N(6) 89.43(6)
N(2) Ru(1) N(3) 161.43(6)
N(2) Ru(1) N(4) 97.95(6)
N(2) Ru(1) N(5) 90.11(6)
N(2) Ru(1) N(6) 91.40(6)
N(3) Ru(1) N(4) 100.61(6)
N(3) Ru(1) N(5) 89.63(6)
N(3) Ru(1) N(6) 88.80(6)
N(4) Ru(1) N(5) 89.64(6)
N(4) Ru(1) N(6) 90.60(6)
N(5) Ru(1) N(6) 178.43(5)
F(1) P(1) F(2) 177.73(9)
F(1) P(1) F(3) 91.59(10)
F(1) P(1) F(4) 89.83(9)
F(1) P(1) F(5) 90.17(7)
F(1) P(1) F(6) 89.70(7)
F(2) P(1) F(3) 90.24(11)
F(2) P(1) F(4) 88.31(9)
F(2) P(1) F(5) 91.10(8)
F(2) P(1) F(6) 88.99(8)
F(3) P(1) F(4) 178.33(9)
F(3) P(1) F(5) 92.11(11)
F(3) P(1) F(6) 89.17(11)
F(4) P(1) F(5) 88.75(9)
F(4) P(1) F(6) 89.97(9)
F(5) P(1) F(6) 178.72(11)
Ru(1) N(1) C(1) 117.21(10)
Ru(1) N(1) C(2) 117.59(13)
C(1) N(1) C(2) 125.08(14)
Ru(1) N(2) C(3) 112.72(9)
Ru(1) N(2) C(7) 128.96(13)
C(3) N(2) C(7) 118.30(15)
Ru(1) N(3) C(8) 112.71(12)
Ru(1) N(3) C(12) 128.85(11)
C(8) N(3) C(12) 118.42(13)
Ru(1) N(4) C(13) 177.56(13)
Ru(1) N(5) C(15) 178.89(12)
Ru(1) N(6) C(17) 176.93(14)
O(1) C(1) N(1) 128.06(14)
O(1) C(1) C(3) 120.13(16)
N(1) C(1) C(3) 111.81(14)
O(2) C(2) N(1) 128.07(17)
O(2) C(2) C(8) 120.88(14)
N(1) C(2) C(8) 111.06(14)
N(2) C(3) C(1) 117.36(15)
N(2) C(3) C(4) 122.37(13)
C(1) C(3) C(4) 120.27(16)
C(3) C(4) C(5) 119.12(17)
C(4) C(5) C(6) 118.54(17)
C(5) C(6) C(7) 119.78(14)
N(2) C(7) C(6) 121.82(17)
N(3) C(8) C(2) 117.68(12)
N(3) C(8) C(9) 122.13(17)
C(2) C(8) C(9) 120.19(15)
C(8) C(9) C(10) 119.00(16)
C(9) C(10) C(11) 118.88(15)
C(10) C(11) C(12) 119.53(17)
N(3) C(12) C(11) 122.03(16)
N(4) C(13) C(14) 179.57(15)
N(5) C(15) C(16) 179.61(19)
N(6) C(17) C(18) 178.27(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ru(1) N(1) 2.0197(16)
Ru(1) N(2) 2.0679(15)
Ru(1) N(3) 2.0647(14)
Ru(1) N(4) 2.0564(16)
Ru(1) N(5) 2.0212(16)
Ru(1) N(6) 2.0199(16)
P(1) F(1) 1.5902(13)
P(1) F(2) 1.6052(15)
P(1) F(3) 1.579(3)
P(1) F(4) 1.5994(18)
P(1) F(5) 1.5939(15)
P(1) F(6) 1.6094(14)
O(1) C(1) 1.226(3)
O(2) C(2) 1.225(2)
N(1) C(1) 1.368(3)
N(1) C(2) 1.3683(18)
N(2) C(3) 1.360(3)
N(2) C(7) 1.3455(18)
N(3) C(8) 1.361(2)
N(3) C(12) 1.346(3)
N(4) C(13) 1.142(3)
N(5) C(15) 1.139(3)
N(6) C(17) 1.140(3)
C(1) C(3) 1.514(2)
C(2) C(8) 1.516(3)
C(3) C(4) 1.382(3)
C(4) C(5) 1.391(2)
C(5) C(6) 1.382(3)
C(6) C(7) 1.391(3)
C(8) C(9) 1.387(2)
C(9) C(10) 1.392(3)
C(10) C(11) 1.381(3)
C(11) C(12) 1.391(3)
C(13) C(14) 1.462(3)
C(15) C(16) 1.462(3)
C(17) C(18) 1.460(3)
