#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:33:24 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179901 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/97/7019779.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_7019779
loop_
_publ_author_name
'Brown, Christopher C.'
'Stephan, Douglas W.'
_publ_section_title
;
 Rearrangements of phosphinoimines to phosphine-imines in ruthenium
 chelate complexes.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9431
_journal_page_last               9438
_journal_paper_doi               10.1039/c2dt30505d
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C66 H62 Cl4 N2 P4 Ru2'
_chemical_formula_weight         1351.00
_chemical_name_systematic
;
?
;
_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-97
_cell_angle_alpha                98.147(2)
_cell_angle_beta                 110.240(2)
_cell_angle_gamma                110.453(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0277(4)
_cell_length_b                   12.3376(5)
_cell_length_c                   14.2100(5)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.96
_cell_measurement_theta_min      2.31
_cell_volume                     1474.93(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42278
_diffrn_reflns_theta_full        33.16
_diffrn_reflns_theta_max         33.16
_diffrn_reflns_theta_min         1.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.9202
_exptl_absorpt_correction_T_min  0.8491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         11200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0319P)²+0.5042P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                9527
_reflns_number_total             11200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30505d.txt
_cod_data_source_block           ccb101_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1474.92(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7019779
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
Ru1 Ru 0.399674(12) 0.397658(9) 0.360829(8) 0.01326(3) Uani 1 1 d
Cl2 Cl 0.54765(4) 0.39670(3) 0.53967(2) 0.01607(6) Uani 1 1 d
Cl1 Cl 0.65344(4) 0.47173(3) 0.35110(3) 0.01798(6) Uani 1 1 d
P1 P 0.33638(4) 0.20292(3) 0.29614(3) 0.01668(7) Uani 1 1 d
P2 P 0.26932(4) 0.42863(3) 0.20762(3) 0.01650(7) Uani 1 1 d
N1 N 0.21758(14) 0.34330(11) 0.40131(9) 0.0165(2) Uani 1 1 d
C1 C -0.0583(3) 0.1567(2) 0.57878(19) 0.0489(6) Uani 1 1 d
C2 C 0.2687(3) 0.76293(19) 0.19315(16) 0.0380(4) Uani 1 1 d
C3 C 0.0131(3) 0.15926(18) 0.51056(16) 0.0369(4) Uani 1 1 d
C4 C 0.4270(3) 0.83847(18) 0.24013(17) 0.0377(4) Uani 1 1 d
C5 C 0.4003(2) 0.15106(15) 0.20031(14) 0.0248(3) Uani 1 1 d
C6 C 0.3206(2) 0.35414(15) -0.10438(12) 0.0265(3) Uani 1 1 d
C7 C -0.1975(2) -0.04125(16) 0.16025(15) 0.0317(4) Uani 1 1 d
C8 C -0.0421(2) 0.25183(16) 0.08264(13) 0.0275(3) Uani 1 1 d
C9 C 0.4844(2) 0.66877(15) 0.26779(12) 0.0241(3) Uani 1 1 d
C10 C -0.1093(2) -0.06465(15) 0.11127(14) 0.0307(4) Uani 1 1 d
C11 C 0.1962(2) 0.37752(16) -0.10128(12) 0.0276(3) Uani 1 1 d
C12 C 0.01280(17) 0.23863(13) 0.44985(11) 0.0206(3) Uani 1 1 d
C13 C -0.12627(19) 0.05854(15) 0.24881(13) 0.0267(3) Uani 1 1 d
C14 C 0.12454(18) 0.11157(13) 0.23956(11) 0.0198(3) Uani 1 1 d
C15 C -0.2657(2) 0.2473(2) 0.11139(16) 0.0382(4) Uani 1 1 d
C16 C 0.03387(17) 0.13678(13) 0.28931(11) 0.0200(3) Uani 1 1 d
C17 C 0.28718(17) 0.39078(13) 0.08367(11) 0.0189(3) Uani 1 1 d
C18 C 0.4294(2) 0.35157(14) -0.01394(12) 0.0238(3) Uani 1 1 d
C19 C -0.0601(2) 0.31482(16) 0.45807(13) 0.0273(3) Uani 1 1 d
C20 C -0.1336(3) 0.2311(2) 0.58456(17) 0.0445(5) Uani 1 1 d
C21 C 0.4007(2) 0.12771(15) 0.39323(14) 0.0265(3) Uani 1 1 d
C22 C -0.0095(2) 0.40876(17) 0.22127(13) 0.0279(3) Uani 1 1 d
C23 C 0.09623(17) 0.24428(13) 0.38033(11) 0.0179(2) Uani 1 1 d
C24 C 0.41386(18) 0.37011(13) 0.08047(11) 0.0202(3) Uani 1 1 d
C25 C -0.1347(2) 0.30933(19) 0.52475(15) 0.0351(4) Uani 1 1 d
C26 C -0.2022(2) 0.1958(2) 0.05607(15) 0.0356(4) Uani 1 1 d
C27 C -0.1705(2) 0.3532(2) 0.19374(16) 0.0360(4) Uani 1 1 d
C28 C 0.5356(2) 0.79184(16) 0.27703(15) 0.0321(4) Uani 1 1 d
C29 C 0.05633(18) 0.36010(15) 0.16444(11) 0.0214(3) Uani 1 1 d
C30 C 0.1806(2) 0.39667(15) -0.00795(12) 0.0244(3) Uani 1 1 d
C31 C 0.2163(2) 0.63914(17) 0.18263(13) 0.0292(3) Uani 1 1 d
C32 C 0.32406(19) 0.59126(14) 0.22068(11) 0.0214(3) Uani 1 1 d
C33 C 0.0501(2) 0.01025(14) 0.15073(13) 0.0260(3) Uani 1 1 d
H1 H 0.243(2) 0.3997(18) 0.4594(16) 0.026(5) Uiso 1 1 d
H2 H 0.495(2) 0.3739(17) 0.1465(15) 0.020(4) Uiso 1 1 d
H3 H -0.152(2) -0.1346(19) 0.0535(16) 0.031(5) Uiso 1 1 d
H4 H 0.111(3) -0.0047(19) 0.1203(17) 0.032(5) Uiso 1 1 d
H5 H 0.054(2) 0.4790(18) 0.2787(15) 0.021(5) Uiso 1 1 d
H6 H 0.102(2) 0.5865(17) 0.1485(15) 0.023(5) Uiso 1 1 d
H32 H 0.092(2) 0.4114(18) -0.0051(16) 0.028(5) Uiso 1 1 d
H8 H -0.304(3) -0.094(2) 0.1335(19) 0.045(7) Uiso 1 1 d
H9 H 0.374(2) 0.0634(19) 0.1910(16) 0.029(5) Uiso 1 1 d
H10 H 0.505(3) 0.1939(19) 0.2318(16) 0.028(5) Uiso 1 1 d
H11 H 0.356(2) 0.0403(19) 0.3608(16) 0.030(5) Uiso 1 1 d
H12 H 0.124(2) 0.3822(18) -0.1631(16) 0.027(5) Uiso 1 1 d
H13 H 0.350(3) 0.163(2) 0.1392(18) 0.037(6) Uiso 1 1 d
H14 H 0.368(3) 0.143(2) 0.4467(19) 0.045(7) Uiso 1 1 d
H15 H -0.185(2) 0.0739(19) 0.2823(16) 0.031(5) Uiso 1 1 d
H16 H 0.648(3) 0.844(2) 0.3102(17) 0.035(6) Uiso 1 1 d
H17 H -0.209(3) 0.388(2) 0.2326(19) 0.047(7) Uiso 1 1 d
H18 H 0.330(2) 0.3421(19) -0.1722(16) 0.030(5) Uiso 1 1 d
H19 H 0.559(2) 0.6327(18) 0.2931(16) 0.029(5) Uiso 1 1 d
H20 H 0.502(3) 0.158(2) 0.4243(19) 0.043(6) Uiso 1 1 d
H21 H 0.001(3) 0.2167(19) 0.0434(17) 0.034(6) Uiso 1 1 d
H22 H -0.060(3) 0.370(2) 0.4192(19) 0.041(6) Uiso 1 1 d
H23 H 0.463(3) 0.915(2) 0.2435(19) 0.048(7) Uiso 1 1 d
H24 H 0.521(3) 0.3404(19) -0.0127(17) 0.034(6) Uiso 1 1 d
H25 H -0.182(3) 0.358(2) 0.5268(18) 0.037(6) Uiso 1 1 d
H26 H 0.065(3) 0.102(2) 0.506(2) 0.053(7) Uiso 1 1 d
H27 H -0.383(3) 0.208(2) 0.0916(19) 0.050(7) Uiso 1 1 d
H28 H 0.189(3) 0.791(2) 0.166(2) 0.063(8) Uiso 1 1 d
H29 H -0.058(3) 0.105(2) 0.618(2) 0.061(8) Uiso 1 1 d
H31 H -0.276(3) 0.119(2) -0.001(2) 0.056(7) Uiso 1 1 d
H30 H -0.182(3) 0.224(2) 0.624(2) 0.056(8) Uiso 1 1 d
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'
P P 0.1023 0.0942 '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'
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_3
N1 Ru1 P1 87.27(3) .
N1 Ru1 P2 96.68(4) .
P1 Ru1 P2 97.771(14) .
N1 Ru1 Cl1 167.94(3) .
P1 Ru1 Cl1 95.217(13) .
P2 Ru1 Cl1 94.673(13) .
N1 Ru1 Cl2 82.47(3) .
P1 Ru1 Cl2 91.181(13) .
P2 Ru1 Cl2 170.966(12) .
Cl1 Ru1 Cl2 85.673(12) .
N1 Ru1 Cl2 83.12(3) 2_666
P1 Ru1 Cl2 168.481(13) 2_666
P2 Ru1 Cl2 89.672(12) 2_666
Cl1 Ru1 Cl2 92.911(12) 2_666
Cl2 Ru1 Cl2 81.295(12) 2_666
Ru1 Cl2 Ru1 98.704(12) 2_666
C14 P1 C5 105.40(7) .
C14 P1 C21 99.68(8) .
C5 P1 C21 99.95(8) .
C14 P1 Ru1 111.62(5) .
C5 P1 Ru1 121.90(6) .
C21 P1 Ru1 115.45(5) .
C29 P2 C17 102.31(7) .
C29 P2 C32 104.98(7) .
C17 P2 C32 96.16(6) .
C29 P2 Ru1 112.41(5) .
C17 P2 Ru1 126.04(5) .
C32 P2 Ru1 112.21(5) .
C23 N1 Ru1 137.59(10) .
C23 N1 H1 113.4(13) .
Ru1 N1 H1 107.1(13) .
C20 C1 C3 119.9(2) .
C20 C1 H29 120.4(18) .
C3 C1 H29 119.7(18) .
C4 C2 C31 120.37(18) .
C4 C2 H28 122.9(17) .
C31 C2 H28 116.7(17) .
C1 C3 C12 120.12(19) .
C1 C3 H26 118.8(15) .
C12 C3 H26 121.1(15) .
C2 C4 C28 120.00(17) .
C2 C4 H23 122.2(17) .
C28 C4 H23 117.6(17) .
P1 C5 H9 108.2(12) .
P1 C5 H10 103.5(13) .
H9 C5 H10 109.4(17) .
P1 C5 H13 108.7(14) .
H9 C5 H13 110.8(18) .
H10 C5 H13 115.7(19) .
C18 C6 C11 119.76(14) .
C18 C6 H18 121.9(12) .
C11 C6 H18 118.3(12) .
C10 C7 C13 119.66(16) .
C10 C7 H8 118.9(15) .
C13 C7 H8 121.4(15) .
C26 C8 C29 120.96(16) .
C26 C8 H21 119.4(13) .
C29 C8 H21 119.6(13) .
C28 C9 C32 120.53(16) .
C28 C9 H19 121.9(12) .
C32 C9 H19 117.5(12) .
C7 C10 C33 120.14(15) .
C7 C10 H3 122.3(13) .
C33 C10 H3 117.4(13) .
C30 C11 C6 119.93(15) .
C30 C11 H12 120.5(12) .
C6 C11 H12 119.6(12) .
C19 C12 C3 119.44(15) .
C19 C12 C23 121.00(14) .
C3 C12 C23 119.51(14) .
C7 C13 C16 121.38(15) .
C7 C13 H15 119.8(13) .
C16 C13 H15 118.8(13) .
C33 C14 C16 118.69(14) .
C33 C14 P1 120.87(12) .
C16 C14 P1 120.29(10) .
C27 C15 C26 120.44(18) .
C27 C15 H27 119.1(14) .
C26 C15 H27 120.4(14) .
C13 C16 C14 118.79(13) .
C13 C16 C23 117.09(13) .
C14 C16 C23 124.08(13) .
C24 C17 C30 118.64(13) .
C24 C17 P2 121.96(11) .
C30 C17 P2 118.98(11) .
C6 C18 C24 120.62(15) .
C6 C18 H24 121.6(13) .
C24 C18 H24 117.7(13) .
C25 C19 C12 119.93(17) .
C25 C19 H22 119.2(14) .
C12 C19 H22 120.8(14) .
C25 C20 C1 120.27(18) .
C25 C20 H30 121.7(18) .
C1 C20 H30 117.9(18) .
P1 C21 H11 111.0(12) .
P1 C21 H14 109.2(14) .
H11 C21 H14 109.0(19) .
P1 C21 H20 110.9(16) .
H11 C21 H20 110.8(19) .
H14 C21 H20 106(2) .
C27 C22 C29 120.59(17) .
C27 C22 H5 118.6(12) .
C29 C22 H5 120.8(12) .
N1 C23 C16 123.14(13) .
N1 C23 C12 118.46(12) .
C16 C23 C12 118.39(12) .
C17 C24 C18 119.97(14) .
C17 C24 H2 119.0(11) .
C18 C24 H2 120.9(11) .
C20 C25 C19 120.33(18) .
C20 C25 H25 122.3(15) .
C19 C25 H25 117.3(15) .
C15 C26 C8 119.74(19) .
C15 C26 H31 116.6(15) .
C8 C26 H31 123.6(15) .
C15 C27 C22 119.88(17) .
C15 C27 H17 122.3(16) .
C22 C27 H17 117.8(16) .
C4 C28 C9 120.02(19) .
C4 C28 H16 120.9(13) .
C9 C28 H16 119.1(13) .
C8 C29 C22 118.33(15) .
C8 C29 P2 121.60(12) .
C22 C29 P2 119.69(12) .
C11 C30 C17 121.02(15) .
C11 C30 H32 120.7(12) .
C17 C30 H32 118.2(12) .
C32 C31 C2 120.25(18) .
C32 C31 H6 120.7(11) .
C2 C31 H6 119.0(11) .
C31 C32 C9 118.82(15) .
C31 C32 P2 124.17(13) .
C9 C32 P2 116.96(11) .
C10 C33 C14 121.33(15) .
C10 C33 H4 121.4(14) .
C14 C33 H4 117.2(14) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 2.0236(12) .
Ru1 P1 2.2192(4) .
Ru1 P2 2.2825(4) .
Ru1 Cl1 2.4462(4) .
Ru1 Cl2 2.4642(3) .
Ru1 Cl2 2.4991(3) 2_666
Cl2 Ru1 2.4990(3) 2_666
P1 C14 1.8214(15) .
P1 C5 1.8215(15) .
P1 C21 1.8291(17) .
P2 C29 1.8268(16) .
P2 C17 1.8429(14) .
P2 C32 1.8482(15) .
N1 C23 1.2919(18) .
N1 H1 0.89(2) .
C1 C20 1.388(3) .
C1 C3 1.389(3) .
C1 H29 0.90(3) .
C2 C4 1.375(3) .
C2 C31 1.397(3) .
C2 H28 0.96(3) .
C3 C12 1.394(2) .
C3 H26 1.02(3) .
C4 C28 1.386(3) .
C4 H23 0.87(2) .
C5 H9 1.00(2) .
C5 H10 0.90(2) .
C5 H13 0.90(2) .
C6 C18 1.382(2) .
C6 C11 1.388(2) .
C6 H18 1.00(2) .
C7 C10 1.378(3) .
C7 C13 1.391(2) .
C7 H8 0.93(2) .
C8 C26 1.389(2) .
C8 C29 1.398(2) .
C8 H21 0.96(2) .
C9 C28 1.392(2) .
C9 C32 1.395(2) .
C9 H19 0.99(2) .
C10 C33 1.387(2) .
C10 H3 0.95(2) .
C11 C30 1.386(2) .
C11 H12 0.95(2) .
C12 C19 1.393(2) .
C12 C23 1.494(2) .
C13 C16 1.401(2) .
C13 H15 0.93(2) .
C14 C33 1.401(2) .
C14 C16 1.415(2) .
C15 C27 1.382(3) .
C15 C26 1.383(3) .
C15 H27 1.01(3) .
C16 C23 1.4823(19) .
C17 C24 1.394(2) .
C17 C30 1.400(2) .
C18 C24 1.400(2) .
C18 H24 0.97(2) .
C19 C25 1.391(2) .
C19 H22 0.93(2) .
C20 C25 1.373(3) .
C20 H30 0.85(3) .
C21 H11 0.98(2) .
C21 H14 0.95(2) .
C21 H20 0.86(2) .
C22 C27 1.394(3) .
C22 C29 1.399(2) .
C22 H5 0.94(2) .
C24 H2 0.989(18) .
C25 H25 0.89(2) .
C26 H31 0.98(3) .
C27 H17 0.92(2) .
C28 H16 0.97(2) .
C30 H32 0.98(2) .
C31 C32 1.394(2) .
C31 H6 0.989(19) .
C33 H4 0.91(2) .
