#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:27:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179920 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/15/7021552.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_7021552
loop_
_publ_author_name
'Sgro, Michael J.'
'Stephan, Douglas W.'
_publ_section_title
;
 Synthesis and reactivity of ruthenium tridentate bis-phosphinite ligand
 complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10460
_journal_page_last               10472
_journal_paper_doi               10.1039/c3dt51065d
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C32 H74 Cl4 N2 O4 P4 Ru2'
_chemical_formula_weight         1018.75
_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                91.428(4)
_cell_angle_beta                 106.792(3)
_cell_angle_gamma                114.206(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7890(8)
_cell_length_b                   10.4080(10)
_cell_length_c                   13.7962(13)
_cell_measurement_reflns_used    9277
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.62
_cell_volume                     1087.02(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0316
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18556
_diffrn_reflns_theta_full        27.65
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.124
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         5020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0221P)²+0.4112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0510
_reflns_number_gt                4575
_reflns_number_total             5020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51065d.txt
_cod_data_source_block           mjs045_0m_Compound_3
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7021552
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
_atom_site_refinement_flags
Ru1 Ru 0.574963(16) 0.985224(14) 0.643222(10) 0.00906(4) Uani 1 1 d .
Cl1 Cl 0.83050(5) 0.97749(5) 0.61297(3) 0.01582(9) Uani 1 1 d .
Cl2 Cl 0.59698(5) 1.17113(4) 0.52863(3) 0.01305(8) Uani 1 1 d .
P1 P 0.73739(6) 1.15114(5) 0.78361(3) 0.01276(9) Uani 1 1 d .
P2 P 0.50098(6) 0.78165(5) 0.71019(3) 0.01174(9) Uani 1 1 d .
O1 O 0.62393(17) 1.19094(15) 0.84452(10) 0.0222(3) Uani 1 1 d .
O2 O 0.28793(15) 0.69284(13) 0.68350(10) 0.0180(3) Uani 1 1 d .
N1 N 0.33540(18) 0.99984(15) 0.63666(11) 0.0138(3) Uani 1 1 d .
H1A H 0.2860 1.0003 0.5674 0.017 Uiso 1 1 calc R
C1 C 0.8643(2) 1.33134(19) 0.75696(14) 0.0189(4) Uani 1 1 d .
H1 H 0.7738 1.3547 0.7083 0.023 Uiso 1 1 calc R
C2 C 0.8902(2) 1.11915(19) 0.89480(13) 0.0171(4) Uani 1 1 d .
H2 H 0.8303 1.0148 0.8970 0.021 Uiso 1 1 calc R
C3 C 0.5586(2) 0.76255(19) 0.84793(13) 0.0169(4) Uani 1 1 d .
H3 H 0.6902 0.8037 0.8775 0.020 Uiso 1 1 calc R
C4 C 0.5574(2) 0.65466(19) 0.64765(14) 0.0180(4) Uani 1 1 d .
H4 H 0.5741 0.6906 0.5832 0.022 Uiso 1 1 calc R
C5 C 0.4451(3) 1.1701(2) 0.80149(15) 0.0244(4) Uani 1 1 d .
H5A H 0.4382 1.2568 0.8267 0.029 Uiso 1 1 calc R
H5B H 0.3712 1.0901 0.8294 0.029 Uiso 1 1 calc R
C6 C 0.3629(2) 1.1393(2) 0.68615(14) 0.0199(4) Uani 1 1 d .
H6A H 0.2473 1.1428 0.6682 0.024 Uiso 1 1 calc R
H6B H 0.4392 1.2160 0.6571 0.024 Uiso 1 1 calc R
C7 C 0.1602(2) 0.7353(2) 0.62170(15) 0.0209(4) Uani 1 1 d .
H7A H 0.0410 0.6663 0.6198 0.025 Uiso 1 1 calc R
H7B H 0.1634 0.7311 0.5506 0.025 Uiso 1 1 calc R
C8 C 0.1891(3) 0.8821(2) 0.65933(17) 0.0260(4) Uani 1 1 d .
H8A H 0.0785 0.8916 0.6280 0.031 Uiso 1 1 calc R
H8B H 0.2140 0.8931 0.7345 0.031 Uiso 1 1 calc R
C9 C 0.9531(3) 1.4507(2) 0.85076(15) 0.0273(4) Uani 1 1 d .
H9A H 1.0558 1.4431 0.8973 0.041 Uiso 1 1 calc R
H9B H 0.8687 1.4412 0.8867 0.041 Uiso 1 1 calc R
H9C H 0.9913 1.5439 0.8280 0.041 Uiso 1 1 calc R
C10 C 0.9953(3) 1.3419(2) 0.70083(15) 0.0238(4) Uani 1 1 d .
H10A H 1.0271 1.4304 0.6717 0.036 Uiso 1 1 calc R
H10B H 0.9407 1.2599 0.6455 0.036 Uiso 1 1 calc R
H10C H 1.1018 1.3421 0.7493 0.036 Uiso 1 1 calc R
C11 C 0.9229(3) 1.1945(2) 1.00061(15) 0.0289(5) Uani 1 1 d .
H11A H 0.9827 1.1547 1.0540 0.043 Uiso 1 1 calc R
H11B H 0.8098 1.1800 1.0082 0.043 Uiso 1 1 calc R
H11C H 0.9972 1.2969 1.0073 0.043 Uiso 1 1 calc R
C12 C 1.0646(3) 1.1433(2) 0.87936(16) 0.0267(4) Uani 1 1 d .
H12A H 1.1385 1.2461 0.8873 0.040 Uiso 1 1 calc R
H12B H 1.0410 1.0974 0.8103 0.040 Uiso 1 1 calc R
H12C H 1.1261 1.1021 0.9305 0.040 Uiso 1 1 calc R
C13 C 0.4968(3) 0.8488(2) 0.90572(14) 0.0234(4) Uani 1 1 d .
H13A H 0.3675 0.8051 0.8827 0.035 Uiso 1 1 calc R
H13B H 0.5413 0.9471 0.8919 0.035 Uiso 1 1 calc R
H13C H 0.5422 0.8493 0.9796 0.035 Uiso 1 1 calc R
C14 C 0.4824(3) 0.6084(2) 0.86841(16) 0.0264(4) Uani 1 1 d .
H14A H 0.5139 0.6085 0.9426 0.040 Uiso 1 1 calc R
H14B H 0.5311 0.5542 0.8385 0.040 Uiso 1 1 calc R
H14C H 0.3536 0.5641 0.8372 0.040 Uiso 1 1 calc R
C15 C 0.7349(3) 0.6594(2) 0.71023(17) 0.0277(5) Uani 1 1 d .
H15A H 0.7232 0.6140 0.7707 0.042 Uiso 1 1 calc R
H15B H 0.8239 0.7590 0.7322 0.042 Uiso 1 1 calc R
H15C H 0.7714 0.6083 0.6679 0.042 Uiso 1 1 calc R
C16 C 0.4100(3) 0.5018(2) 0.61279(17) 0.0293(5) Uani 1 1 d .
H16A H 0.4483 0.4433 0.5780 0.044 Uiso 1 1 calc R
H16B H 0.3036 0.5031 0.5654 0.044 Uiso 1 1 calc R
H16C H 0.3840 0.4614 0.6727 0.044 Uiso 1 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'
N N 0.0061 0.0033 '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'
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_1
_geom_angle_site_symmetry_3
N1 Ru1 P1 93.64(4) . .
N1 Ru1 P2 93.42(4) . .
P1 Ru1 P2 102.065(18) . .
N1 Ru1 Cl1 167.76(4) . .
P1 Ru1 Cl1 93.663(17) . .
P2 Ru1 Cl1 94.645(16) . .
N1 Ru1 Cl2 86.15(4) . 2_676
P1 Ru1 Cl2 171.623(16) . 2_676
P2 Ru1 Cl2 86.304(17) . 2_676
Cl1 Ru1 Cl2 85.201(15) . 2_676
N1 Ru1 Cl2 82.09(4) . .
P1 Ru1 Cl2 91.999(17) . .
P2 Ru1 Cl2 165.508(16) . .
Cl1 Ru1 Cl2 87.848(15) . .
Cl2 Ru1 Cl2 79.671(16) 2_676 .
Ru1 Cl2 Ru1 100.330(16) 2_676 .
O1 P1 C1 99.07(8) . .
O1 P1 C2 98.40(8) . .
C1 P1 C2 106.75(8) . .
O1 P1 Ru1 114.90(5) . .
C1 P1 Ru1 113.95(6) . .
C2 P1 Ru1 120.70(6) . .
O2 P2 C3 95.71(7) . .
O2 P2 C4 102.58(8) . .
C3 P2 C4 105.05(8) . .
O2 P2 Ru1 112.30(5) . .
C3 P2 Ru1 127.70(6) . .
C4 P2 Ru1 110.22(6) . .
C5 O1 P1 126.09(11) . .
C7 O2 P2 124.51(11) . .
C6 N1 C8 109.82(14) . .
C6 N1 Ru1 114.30(11) . .
C8 N1 Ru1 121.44(11) . .
C6 N1 H1A 102.8 . .
C8 N1 H1A 102.8 . .
Ru1 N1 H1A 102.8 . .
C10 C1 C9 110.45(16) . .
C10 C1 P1 115.98(13) . .
C9 C1 P1 114.21(14) . .
C10 C1 H1 105.0 . .
C9 C1 H1 105.0 . .
P1 C1 H1 105.0 . .
C12 C2 C11 110.76(16) . .
C12 C2 P1 112.97(13) . .
C11 C2 P1 116.23(13) . .
C12 C2 H2 105.3 . .
C11 C2 H2 105.3 . .
P1 C2 H2 105.3 . .
C13 C3 C14 108.27(15) . .
C13 C3 P2 109.98(12) . .
C14 C3 P2 114.88(13) . .
C13 C3 H3 107.8 . .
C14 C3 H3 107.8 . .
P2 C3 H3 107.8 . .
C15 C4 C16 112.46(16) . .
C15 C4 P2 112.58(13) . .
C16 C4 P2 114.71(13) . .
C15 C4 H4 105.4 . .
C16 C4 H4 105.4 . .
P2 C4 H4 105.4 . .
O1 C5 C6 118.19(16) . .
O1 C5 H5A 107.8 . .
C6 C5 H5A 107.8 . .
O1 C5 H5B 107.8 . .
C6 C5 H5B 107.8 . .
H5A C5 H5B 107.1 . .
N1 C6 C5 115.06(15) . .
N1 C6 H6A 108.5 . .
C5 C6 H6A 108.5 . .
N1 C6 H6B 108.5 . .
C5 C6 H6B 108.5 . .
H6A C6 H6B 107.5 . .
O2 C7 C8 113.72(16) . .
O2 C7 H7A 108.8 . .
C8 C7 H7A 108.8 . .
O2 C7 H7B 108.8 . .
C8 C7 H7B 108.8 . .
H7A C7 H7B 107.7 . .
N1 C8 C7 114.73(15) . .
N1 C8 H8A 108.6 . .
C7 C8 H8A 108.6 . .
N1 C8 H8B 108.6 . .
C7 C8 H8B 108.6 . .
H8A C8 H8B 107.6 . .
C1 C9 H9A 109.5 . .
C1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C1 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C1 C10 H10A 109.5 . .
C1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C2 C11 H11A 109.5 . .
C2 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C2 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C2 C12 H12A 109.5 . .
C2 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C2 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C3 C13 H13A 109.5 . .
C3 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C3 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C3 C14 H14A 109.5 . .
C3 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C3 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C4 C15 H15A 109.5 . .
C4 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C4 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C4 C16 H16A 109.5 . .
C4 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C4 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 N1 2.1489(14) .
Ru1 P1 2.2328(5) .
Ru1 P2 2.2540(5) .
Ru1 Cl1 2.4316(5) .
Ru1 Cl2 2.5048(5) 2_676
Ru1 Cl2 2.5106(5) .
Cl2 Ru1 2.5047(5) 2_676
P1 O1 1.6364(13) .
P1 C1 1.8582(19) .
P1 C2 1.8627(18) .
P2 O2 1.6315(13) .
P2 C3 1.8581(18) .
P2 C4 1.8613(18) .
O1 C5 1.430(2) .
O2 C7 1.434(2) .
N1 C6 1.483(2) .
N1 C8 1.488(2) .
N1 H1A 0.9300 .
C1 C10 1.534(3) .
C1 C9 1.539(3) .
C1 H1 1.0000 .
C2 C12 1.527(3) .
C2 C11 1.531(3) .
C2 H2 1.0000 .
C3 C13 1.533(3) .
C3 C14 1.534(3) .
C3 H3 1.0000 .
C4 C15 1.529(3) .
C4 C16 1.534(3) .
C4 H4 1.0000 .
C5 C6 1.509(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.494(3) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
