#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:38:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179339 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/36/4323613.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_4323613
loop_
_publ_author_name
'Seth M. Redmore'
'Clifton E. F. Rickard'
'Simon J. Webb'
'L. James Wright'
_publ_section_title
;
 Ruthenium Complexes of a Simple Tridentate Ligand Bearing Two "Distal"
 Pyridine Bases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4743
_journal_page_last               4748
_journal_paper_doi               10.1021/ic961534x
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source        Synthetic
_chemical_formula_moiety         RuCl2(PPh3)(LMe2{H}2)
_chemical_formula_sum            'C37 H32 Cl2 N5 O2 P Ru'
_chemical_formula_weight         781.62
_chemical_name_systematic
; 
Dichloro(triphenylphosphine)[N,N'-bis(6-methyl-1-pyridinium-2-yl)-
2,6-pyridinedicarboximidato-κ³N]ruthenium(II) 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL
_cell_angle_alpha                92.55(3)
_cell_angle_beta                 90.06(3)
_cell_angle_gamma                115.22(3)
_cell_formula_units_Z            2
_cell_length_a                   10.482(5)
_cell_length_b                   11.349(8)
_cell_length_c                   15.710(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      10
_cell_volume                     1688.6(16)
_computing_cell_refinement       'CAD-4 software'
_computing_data_collection       'CAD-4 software'
_computing_data_reduction        'Local software'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       CAD-4
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5536
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   Emperical
_exptl_crystal_colour            Purple
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       Prisms
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.087
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_obs          0.0395
_refine_ls_shift/esd_max         -0.035
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0494P)²+1.5591P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1081
_refine_ls_wR_factor_obs         0.0890
_reflns_number_observed          4013
_reflns_number_total             5298
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961534x_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.5591P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.5591P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1688.6(15)
_cod_database_code               4323613
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ru1 Ru 0.17221(4) 0.21524(3) 0.23845(2) 0.02076(12) Uani 1 d . .
Cl1 Cl -0.08354(11) 0.08197(11) 0.24969(7) 0.0314(3) Uani 1 d . .
Cl2 Cl 0.17002(12) 0.32850(11) 0.37947(7) 0.0287(3) Uani 1 d . .
P1 P 0.40968(12) 0.33988(11) 0.24005(7) 0.0226(3) Uani 1 d . .
O1 O 0.2576(4) -0.1108(3) 0.2082(2) 0.0464(9) Uani 1 d . .
O2 O 0.0559(5) 0.3232(4) 0.0095(2) 0.0531(11) Uani 1 d . .
N1 N 0.1894(4) 0.0782(4) 0.4201(2) 0.0291(9) Uani 1 d . .
H1 H 0.1925(47) 0.1483(45) 0.4129(29) 0.021(9) Uiso 1 d . .
N2 N 0.2001(4) 0.0482(3) 0.2751(2) 0.0268(9) Uani 1 d . .
N3 N 0.1745(4) 0.1312(4) 0.1280(2) 0.0263(9) Uani 1 d . .
N4 N 0.1107(4) 0.3274(4) 0.1540(2) 0.0273(9) Uani 1 d . .
N5 N 0.0041(4) 0.4062(4) 0.2544(3) 0.0314(9) Uani 1 d . .
H5 H 0.0065(46) 0.3471(44) 0.2821(29) 0.021(9) Uiso 1 d . .
C1 C 0.1914(6) 0.1573(5) 0.5671(3) 0.0407(13) Uani 1 d . .
H1A H 0.1416(28) 0.2057(20) 0.5446(9) 0.049 Uiso 1 calc R .
H1B H 0.2910(6) 0.2165(17) 0.5773(15) 0.049 Uiso 1 calc R .
H1C H 0.1492(30) 0.1196(6) 0.6208(7) 0.049 Uiso 1 calc R .
C2 C 0.1798(5) 0.0513(5) 0.5045(3) 0.0343(12) Uani 1 d . .
C3 C 0.1625(5) -0.0699(5) 0.5237(3) 0.0404(13) Uani 1 d . .
H3 H 0.1547(5) -0.0936(5) 0.5814(3) 0.049 Uiso 1 calc R .
C4 C 0.1563(5) -0.1584(5) 0.4591(3) 0.0420(13) Uani 1 d . .
H4 H 0.1404(5) -0.2440(5) 0.4731(3) 0.050 Uiso 1 calc R .
C5 C 0.1724(5) -0.1272(5) 0.3752(3) 0.0341(11) Uani 1 d . .
H5A H 0.1723(5) -0.1886(5) 0.3320(3) 0.041 Uiso 1 calc R .
C6 C 0.1889(5) -0.0023(4) 0.3545(3) 0.0263(10) Uani 1 d . .
C7 C 0.2247(5) -0.0187(4) 0.2065(3) 0.0312(11) Uani 1 d . .
C8 C 0.2086(5) 0.0305(4) 0.1228(3) 0.0309(11) Uani 1 d . .
C9 C 0.2227(6) -0.0234(5) 0.0450(3) 0.0421(13) Uani 1 d . .
H9 H 0.2501(6) -0.0932(5) 0.0423(3) 0.051 Uiso 1 calc R .
C10 C 0.1967(6) 0.0252(5) -0.0291(3) 0.0442(14) Uani 1 d . .
H10 H 0.2069(6) -0.0103(5) -0.0832(3) 0.053 Uiso 1 calc R .
C11 C 0.1562(5) 0.1252(5) -0.0234(3) 0.0382(12) Uani 1 d . .
H11 H 0.1353(5) 0.1580(5) -0.0736(3) 0.046 Uiso 1 calc R .
C12 C 0.1460(5) 0.1781(4) 0.0560(3) 0.0307(11) Uani 1 d . .
C13 C 0.1028(5) 0.2858(5) 0.0702(3) 0.0332(11) Uani 1 d . .
C14 C 0.0562(4) 0.4146(4) 0.1751(3) 0.0273(10) Uani 1 d . .
C15 C 0.0509(5) 0.5142(5) 0.1270(3) 0.0378(12) Uani 1 d . .
H15 H 0.0811(5) 0.5228(5) 0.0697(3) 0.045 Uiso 1 calc R .
C16 C 0.0021(6) 0.5983(5) 0.1631(3) 0.0422(13) Uani 1 d . .
H16 H 0.0003(6) 0.6662(5) 0.1306(3) 0.051 Uiso 1 calc R .
C17 C -0.0448(5) 0.5871(5) 0.2460(3) 0.0399(13) Uani 1 d . .
H17 H -0.0773(5) 0.6471(5) 0.2704(3) 0.048 Uiso 1 calc R .
C18 C -0.0436(5) 0.4889(5) 0.2919(3) 0.0336(11) Uani 1 d . .
C19 C -0.0931(6) 0.4631(6) 0.3819(3) 0.0503(15) Uani 1 d . .
H19A H -0.0169(13) 0.4626(33) 0.4179(6) 0.060 Uiso 1 calc R .
H19B H -0.1749(22) 0.3782(16) 0.3829(5) 0.060 Uiso 1 calc R .
H19C H -0.1198(34) 0.5316(19) 0.4036(8) 0.060 Uiso 1 calc R .
C21 C 0.4760(5) 0.5189(4) 0.2420(3) 0.0246(10) Uani 1 d . .
C22 C 0.6181(5) 0.5957(5) 0.2252(3) 0.0313(11) Uani 1 d . .
H22 H 0.6799(5) 0.5556(5) 0.2140(3) 0.038 Uiso 1 calc R .
C23 C 0.6686(5) 0.7299(5) 0.2249(3) 0.0351(12) Uani 1 d . .
H23 H 0.7654(5) 0.7818(5) 0.2145(3) 0.042 Uiso 1 calc R .
C24 C 0.5786(5) 0.7887(5) 0.2395(3) 0.0367(12) Uani 1 d . .
H24 H 0.6133(5) 0.8808(5) 0.2388(3) 0.044 Uiso 1 calc R .
C25 C 0.4385(5) 0.7134(4) 0.2552(3) 0.0330(11) Uani 1 d . .
H25 H 0.3764(5) 0.7538(4) 0.2644(3) 0.040 Uiso 1 calc R .
C26 C 0.3871(5) 0.5784(4) 0.2577(3) 0.0280(10) Uani 1 d . .
H26 H 0.2910(5) 0.5273(4) 0.2703(3) 0.034 Uiso 1 calc R .
C31 C 0.4951(4) 0.3112(4) 0.3340(3) 0.0254(10) Uani 1 d . .
C32 C 0.5351(5) 0.3999(5) 0.4037(3) 0.0352(12) Uani 1 d . .
H32 H 0.5338(5) 0.4825(5) 0.3987(3) 0.042 Uiso 1 calc R .
C33 C 0.5775(6) 0.3692(7) 0.4814(3) 0.050(2) Uani 1 d . .
H33 H 0.6042(6) 0.4307(7) 0.5286(3) 0.060 Uiso 1 calc R .
C34 C 0.5801(6) 0.2509(7) 0.4889(3) 0.049(2) Uani 1 d . .
H34 H 0.6065(6) 0.2293(7) 0.5418(3) 0.059 Uiso 1 calc R .
C35 C 0.5448(5) 0.1626(6) 0.4199(4) 0.0485(15) Uani 1 d . .
H35 H 0.5493(5) 0.0814(6) 0.4251(4) 0.058 Uiso 1 calc R .
C36 C 0.5021(5) 0.1921(5) 0.3420(3) 0.0340(11) Uani 1 d . .
H36 H 0.4780(5) 0.1309(5) 0.2948(3) 0.041 Uiso 1 calc R .
C41 C 0.5093(5) 0.3179(4) 0.1485(3) 0.0275(10) Uani 1 d . .
C42 C 0.6146(5) 0.2761(5) 0.1523(3) 0.0352(12) Uani 1 d . .
H42 H 0.6428(5) 0.2572(5) 0.2055(3) 0.042 Uiso 1 calc R .
C43 C 0.6800(6) 0.2617(6) 0.0778(4) 0.0507(15) Uani 1 d . .
H43 H 0.7523(6) 0.2324(6) 0.0808(4) 0.061 Uiso 1 calc R .
C44 C 0.6416(6) 0.2890(5) 0.0002(4) 0.0501(15) Uani 1 d . .
H44 H 0.6852(6) 0.2771(5) -0.0504(4) 0.060 Uiso 1 calc R .
C45 C 0.5380(6) 0.3344(5) -0.0030(3) 0.0410(13) Uani 1 d . .
H45 H 0.5119(6) 0.3554(5) -0.0562(3) 0.049 Uiso 1 calc R .
C46 C 0.4736(5) 0.3491(4) 0.0692(3) 0.0326(11) Uani 1 d . .
H46 H 0.4034(5) 0.3809(4) 0.0658(3) 0.039 Uiso 1 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 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'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 '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
N3 Ru1 N2 78.48(15) . . ?
N3 Ru1 N4 78.5(2) . . ?
N2 Ru1 N4 155.26(14) . . y
N3 Ru1 P1 92.85(11) . . ?
N2 Ru1 P1 91.66(11) . . ?
N4 Ru1 P1 98.36(11) . . ?
N3 Ru1 Cl1 91.39(11) . . y
N2 Ru1 Cl1 87.13(11) . . ?
N4 Ru1 Cl1 84.54(11) . . y
P1 Ru1 Cl1 175.27(4) . . y
N3 Ru1 Cl2 178.68(11) . . y
N2 Ru1 Cl2 102.81(11) . . ?
N4 Ru1 Cl2 100.30(11) . . ?
P1 Ru1 Cl2 86.79(6) . . ?
Cl1 Ru1 Cl2 89.01(6) . . ?
C31 P1 C21 103.8(2) . . ?
C31 P1 C41 104.9(2) . . ?
C21 P1 C41 98.8(2) . . ?
C31 P1 Ru1 111.20(15) . . ?
C21 P1 Ru1 118.8(2) . . ?
C41 P1 Ru1 117.43(15) . . ?
C6 N1 C2 126.2(4) . . ?
C7 N2 C6 118.3(4) . . y
C7 N2 Ru1 112.4(3) . . ?
C6 N2 Ru1 129.2(3) . . ?
C8 N3 C12 119.9(4) . . ?
C8 N3 Ru1 120.2(3) . . ?
C12 N3 Ru1 119.8(3) . . ?
C14 N4 C13 117.8(4) . . y
C14 N4 Ru1 127.9(3) . . ?
C13 N4 Ru1 113.1(3) . . ?
C14 N5 C18 125.6(4) . . ?
C3 C2 N1 116.9(5) . . ?
C3 C2 C1 125.6(4) . . ?
N1 C2 C1 117.4(4) . . ?
C2 C3 C4 119.6(5) . . ?
C5 C4 C3 122.4(5) . . ?
C4 C5 C6 118.5(5) . . ?
N1 C6 N2 115.0(4) . . y
N1 C6 C5 116.3(4) . . ?
N2 C6 C5 128.7(4) . . ?
O1 C7 N2 127.4(4) . . ?
O1 C7 C8 119.1(4) . . ?
N2 C7 C8 113.5(4) . . y
N3 C8 C9 121.2(4) . . ?
N3 C8 C7 114.4(4) . . y
C9 C8 C7 124.3(5) . . ?
C8 C9 C10 119.4(5) . . ?
C11 C10 C9 119.2(5) . . ?
C10 C11 C12 119.5(5) . . ?
N3 C12 C11 120.7(5) . . ?
N3 C12 C13 114.9(4) . . y
C11 C12 C13 124.4(4) . . ?
O2 C13 N4 126.7(5) . . ?
O2 C13 C12 119.8(4) . . ?
N4 C13 C12 113.4(4) . . y
N5 C14 N4 115.1(4) . . y
N5 C14 C15 115.8(4) . . ?
N4 C14 C15 129.1(4) . . ?
C16 C15 C14 119.6(5) . . ?
C15 C16 C17 121.6(5) . . ?
C18 C17 C16 119.0(5) . . ?
N5 C18 C17 118.3(5) . . ?
N5 C18 C19 116.6(4) . . ?
C17 C18 C19 125.1(5) . . ?
C26 C21 C22 119.3(4) . . ?
C26 C21 P1 121.1(3) . . ?
C22 C21 P1 119.6(4) . . ?
C23 C22 C21 120.2(5) . . ?
C24 C23 C22 120.2(4) . . ?
C25 C24 C23 119.8(4) . . ?
C24 C25 C26 120.5(5) . . ?
C21 C26 C25 119.9(4) . . ?
C32 C31 C36 118.4(4) . . ?
C32 C31 P1 120.3(4) . . ?
C36 C31 P1 120.7(4) . . ?
C31 C32 C33 121.0(5) . . ?
C34 C33 C32 119.9(6) . . ?
C33 C34 C35 120.2(5) . . ?
C34 C35 C36 120.4(5) . . ?
C31 C36 C35 120.1(5) . . ?
C42 C41 C46 118.5(4) . . ?
C42 C41 P1 125.8(4) . . ?
C46 C41 P1 115.7(4) . . ?
C41 C42 C43 119.9(5) . . ?
C44 C43 C42 121.1(5) . . ?
C43 C44 C45 118.8(5) . . ?
C46 C45 C44 120.6(5) . . ?
C45 C46 C41 120.9(5) . . ?
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 N3 1.947(4) . y
Ru1 N2 2.140(4) . y
Ru1 N4 2.155(4) . y
Ru1 P1 2.279(2) . y
Ru1 Cl1 2.465(2) . y
Ru1 Cl2 2.5165(14) . y
P1 C31 1.837(4) . ?
P1 C21 1.844(5) . ?
P1 C41 1.847(4) . ?
O1 C7 1.234(6) . y
O2 C13 1.242(6) . y
N1 C6 1.345(6) . ?
N1 C2 1.369(6) . ?
N2 C7 1.378(6) . y
N2 C6 1.380(6) . y
N3 C8 1.335(6) . ?
N3 C12 1.356(6) . ?
N4 C14 1.367(6) . y
N4 C13 1.370(6) . y
N5 C14 1.351(6) . ?
N5 C18 1.354(6) . ?
C1 C2 1.482(7) . ?
C2 C3 1.356(7) . ?
C3 C4 1.378(8) . ?
C4 C5 1.372(7) . ?
/C5 C6 1.406(6) . ?
C7 C8 1.488(7) . y
C8 C9 1.378(7) . ?
C9 C10 1.386(7) . ?
C10 C11 1.370(8) . ?
C11 C12 1.385(7) . ?
C12 C13 1.482(7) . y
C14 C15 1.407(6) . ?
C15 C16 1.366(7) . ?
C16 C17 1.384(7) . ?
C17 C18 1.358(7) . ?
C18 C19 1.505(7) . ?
C21 C26 1.382(6) . ?
C21 C22 1.401(6) . ?
C22 C23 1.383(6) . ?
C23 C24 1.382(7) . ?
C24 C25 1.378(7) . ?
C25 C26 1.393(6) . ?
C31 C32 1.388(7) . ?
C31 C36 1.396(7) . ?
C32 C33 1.407(7) . ?
C33 C34 1.366(8) . ?
C34 C35 1.378(8) . ?
C35 C36 1.404(7) . ?
C41 C42 1.376(6) . ?
C41 C46 1.404(7) . ?
C42 C43 1.396(7) . ?
C43 C44 1.372(8) . ?
C44 C45 1.387(8) . ?
C45 C46 1.361(7) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N2 C6 N1 169.0(4) . . . . ?
C13 N4 C14 N5 149.5(4) . . . . ?
C12 C13 N4 C14 -171.8(4) . . . . ?
C13 N4 C14 C15 -32.8(7) . . . . ?
N4 C14 C15 N5 -177.7(7) . . . . ?
C8 C7 N2 C6 169.4(4) . . . . ?
C7 N2 C6 C5 -13.4(7) . . . . ?
N2 C6 C5 N1 -177.6(8) . . . . ?
C8 C7 N2 C6 169.4(4) . . . . ?
Ru1 N2 C7 O1 172.7(4) . . . . ?
C6 N2 C7 O1 -10.8(7) . . . . ?
C12 C13 N4 C14 -171.8(4) . . . . ?
Ru1 N4 C13 O2 171.8(4) . . . . ?
C14 N4 C13 O2 3.2(7) . . . . ?
