#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:52:20 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178727 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/38/4083893.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_4083893
loop_
_publ_author_name
'Marqués-González, Santiago'
'Parthey, Matthias'
'Yufit, Dmitry S.'
'Howard, Judith A. K.'
'Kaupp, Martin'
'Low, Paul J.'
_publ_section_title
;
 Combined Spectroscopic and Quantum Chemical Study of [trans-Ru(C≡
 CC6H4R1-4)2(dppe)2]n+and [trans-Ru(C≡CC6H4R1-4)(C≡
 CC6H4R2-4)(dppe)2]n+(n= 0, 1) Complexes: Interpretations beyond the
 Lowest Energy Conformer Paradigm
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4947
_journal_paper_doi               10.1021/om500265s
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C70 H62 P4 Ru'
_chemical_formula_sum            'C70 H62 P4 Ru'
_chemical_formula_weight         1128.15
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2011-09-02
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled 2011.08.21 svn.r1945, GUI svn.r3824)
;
_cell_angle_alpha                117.3140(10)
_cell_angle_beta                 94.8710(10)
_cell_angle_gamma                104.7240(10)
_cell_formula_units_Z            1
_cell_length_a                   9.4458(4)
_cell_length_b                   12.9907(6)
_cell_length_c                   13.5890(6)
_cell_measurement_reflns_used    6595
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.96
_cell_measurement_theta_min      2.43
_cell_volume                     1392.94(11)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16041
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         1.74
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3296
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
"SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0627 before and 0.0284 after correction.
The Ratio of minimum to maximum transmission is 0.3296.
The λ/2 correction factor is 0.00.
{Info from Q:\Struc\11S\11srv172\sad.abs}
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.117
_refine_diff_density_min         -1.580
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         7679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.4000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                6410
_reflns_number_total             7679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500265s_si_002.cif
_cod_data_source_block           3a_11srv172
_cod_database_code               4083893
loop_
_space_group_symop_id
_space_group_symop_operation_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
Ru1 Ru 0.5000 0.5000 0.0000 0.01236(7) Uani 1 2 d S
P1 P 0.28477(6) 0.35497(5) -0.00826(4) 0.01336(10) Uani 1 1 d .
P2 P 0.39903(6) 0.64071(5) 0.12776(4) 0.01364(11) Uani 1 1 d .
C1 C 0.6485(2) 0.51417(18) 0.12982(17) 0.0154(4) Uani 1 1 d .
C2 C 0.7445(2) 0.52267(19) 0.20068(17) 0.0175(4) Uani 1 1 d .
C3 C 0.8673(2) 0.5371(2) 0.28165(18) 0.0185(4) Uani 1 1 d .
C4 C 0.9264(3) 0.6443(2) 0.3878(2) 0.0274(5) Uani 1 1 d .
H4 H 0.8817 0.7068 0.4084 0.033 Uiso 1 1 calc R
C5 C 1.0497(3) 0.6605(2) 0.4635(2) 0.0327(6) Uani 1 1 d .
H5 H 1.0888 0.7345 0.5347 0.039 Uiso 1 1 calc R
C6 C 1.1165(3) 0.5705(2) 0.4371(2) 0.0259(5) Uani 1 1 d .
C7 C 1.0575(3) 0.4643(2) 0.3330(2) 0.0261(5) Uani 1 1 d .
H7 H 1.1021 0.4018 0.3133 0.031 Uiso 1 1 calc R
C8 C 0.9343(2) 0.4463(2) 0.25587(19) 0.0221(4) Uani 1 1 d .
H8 H 0.8954 0.3717 0.1851 0.026 Uiso 1 1 calc R
C9 C 1.2505(3) 0.5892(3) 0.5207(2) 0.0344(6) Uani 1 1 d .
H9A H 1.3059 0.6772 0.5691 0.052 Uiso 1 1 calc R
H9B H 1.3170 0.5478 0.4787 0.052 Uiso 1 1 calc R
H9C H 1.2152 0.5546 0.5684 0.052 Uiso 1 1 calc R
C10 C 0.1424(2) 0.43312(19) 0.02295(17) 0.0166(4) Uani 1 1 d .
H10A H 0.1133 0.4496 -0.0387 0.020 Uiso 1 1 calc R
H10B H 0.0512 0.3815 0.0300 0.020 Uiso 1 1 calc R
C11 C 0.2152(2) 0.55322(19) 0.13521(17) 0.0174(4) Uani 1 1 d .
H11A H 0.2307 0.5354 0.1980 0.021 Uiso 1 1 calc R
H11B H 0.1477 0.6032 0.1514 0.021 Uiso 1 1 calc R
C21 C 0.2679(2) 0.29764(18) 0.09353(17) 0.0153(4) Uani 1 1 d .
C22 C 0.3852(2) 0.33973(19) 0.18689(17) 0.0177(4) Uani 1 1 d .
H22 H 0.4790 0.3969 0.1974 0.021 Uiso 1 1 calc R
C23 C 0.3654(3) 0.2983(2) 0.26469(18) 0.0214(4) Uani 1 1 d .
H23 H 0.4456 0.3278 0.3281 0.026 Uiso 1 1 calc R
C24 C 0.2294(3) 0.2145(2) 0.24995(19) 0.0221(4) Uani 1 1 d .
H24 H 0.2163 0.1862 0.3029 0.026 Uiso 1 1 calc R
C25 C 0.1126(3) 0.1721(2) 0.15728(19) 0.0219(4) Uani 1 1 d .
H25 H 0.0193 0.1145 0.1467 0.026 Uiso 1 1 calc R
C26 C 0.1313(2) 0.2135(2) 0.08023(18) 0.0194(4) Uani 1 1 d .
H26 H 0.0503 0.1844 0.0175 0.023 Uiso 1 1 calc R
C31 C 0.1913(2) 0.21042(19) -0.14200(17) 0.0163(4) Uani 1 1 d .
C32 C 0.2162(2) 0.10255(19) -0.15889(18) 0.0185(4) Uani 1 1 d .
H32 H 0.2821 0.1045 -0.1007 0.022 Uiso 1 1 calc R
C33 C 0.1458(3) -0.0076(2) -0.25980(18) 0.0222(4) Uani 1 1 d .
H33 H 0.1641 -0.0801 -0.2703 0.027 Uiso 1 1 calc R
C34 C 0.0489(3) -0.0118(2) -0.34511(19) 0.0236(4) Uani 1 1 d .
H34 H -0.0005 -0.0873 -0.4136 0.028 Uiso 1 1 calc R
C35 C 0.0242(3) 0.0951(2) -0.32983(18) 0.0226(4) Uani 1 1 d .
H35 H -0.0414 0.0927 -0.3884 0.027 Uiso 1 1 calc R
C36 C 0.0951(2) 0.20509(19) -0.22946(17) 0.0186(4) Uani 1 1 d .
H36 H 0.0781 0.2777 -0.2200 0.022 Uiso 1 1 calc R
C41 C 0.4955(2) 0.73762(19) 0.27932(17) 0.0173(4) Uani 1 1 d .
C42 C 0.5561(2) 0.8647(2) 0.33214(18) 0.0201(4) Uani 1 1 d .
H42 H 0.5466 0.9046 0.2895 0.024 Uiso 1 1 calc R
C43 C 0.6305(3) 0.9343(2) 0.44702(19) 0.0247(5) Uani 1 1 d .
H43 H 0.6723 1.0211 0.4819 0.030 Uiso 1 1 calc R
C44 C 0.6439(3) 0.8776(2) 0.51059(18) 0.0264(5) Uani 1 1 d .
H44 H 0.6923 0.9252 0.5893 0.032 Uiso 1 1 calc R
C45 C 0.5860(3) 0.7507(2) 0.45816(19) 0.0268(5) Uani 1 1 d .
H45 H 0.5967 0.7111 0.5008 0.032 Uiso 1 1 calc R
C46 C 0.5126(3) 0.6814(2) 0.34371(19) 0.0240(4) Uani 1 1 d .
H46 H 0.4734 0.5945 0.3087 0.029 Uiso 1 1 calc R
C51 C 0.3504(2) 0.75264(18) 0.09656(17) 0.0158(4) Uani 1 1 d .
C52 C 0.2628(2) 0.81957(19) 0.15805(18) 0.0186(4) Uani 1 1 d .
H52 H 0.2252 0.8053 0.2149 0.022 Uiso 1 1 calc R
C53 C 0.2302(3) 0.9071(2) 0.13642(19) 0.0217(4) Uani 1 1 d .
H53 H 0.1705 0.9522 0.1784 0.026 Uiso 1 1 calc R
C54 C 0.2850(3) 0.9285(2) 0.0534(2) 0.0233(4) Uani 1 1 d .
H54 H 0.2639 0.9890 0.0394 0.028 Uiso 1 1 calc R
C55 C 0.3707(3) 0.8617(2) -0.00896(19) 0.0222(4) Uani 1 1 d .
H55 H 0.4075 0.8756 -0.0662 0.027 Uiso 1 1 calc R
C56 C 0.4025(2) 0.77372(19) 0.01271(17) 0.0178(4) Uani 1 1 d .
H56 H 0.4606 0.7277 -0.0305 0.021 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'
P P 0.1023 0.0942 '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
P1 Ru1 P1 180.00(2) 2_665 .
P1 Ru1 P2 97.014(18) 2_665 .
P1 Ru1 P2 82.985(17) . .
P1 Ru1 P2 82.986(18) 2_665 2_665
P1 Ru1 P2 97.015(18) . 2_665
P2 Ru1 P2 180.0 . 2_665
C1 Ru1 P1 99.23(6) 2_665 2_665
C1 Ru1 P1 80.77(6) . 2_665
C1 Ru1 P1 99.23(6) . .
C1 Ru1 P1 80.77(6) 2_665 .
C1 Ru1 P2 87.21(5) 2_665 .
C1 Ru1 P2 92.79(5) . .
C1 Ru1 P2 92.79(5) 2_665 2_665
C1 Ru1 P2 87.21(5) . 2_665
C1 Ru1 C1 180.0 . 2_665
C10 P1 Ru1 105.15(7) . .
C10 P1 C21 98.50(9) . .
C21 P1 Ru1 125.25(7) . .
C31 P1 Ru1 120.00(6) . .
C31 P1 C10 104.85(9) . .
C31 P1 C21 99.65(9) . .
C11 P2 Ru1 108.30(7) . .
C41 P2 Ru1 120.51(7) . .
C41 P2 C11 101.40(9) . .
C41 P2 C51 101.40(9) . .
C51 P2 Ru1 119.96(7) . .
C51 P2 C11 102.46(9) . .
C2 C1 Ru1 174.54(17) . .
C1 C2 C3 175.6(2) . .
C4 C3 C2 121.04(19) . .
C8 C3 C2 121.3(2) . .
C8 C3 C4 117.65(19) . .
C3 C4 H4 119.6 . .
C5 C4 C3 120.9(2) . .
C5 C4 H4 119.6 . .
C4 C5 H5 119.4 . .
C6 C5 C4 121.2(2) . .
C6 C5 H5 119.4 . .
C5 C6 C9 120.7(2) . .
C7 C6 C5 118.0(2) . .
C7 C6 C9 121.3(2) . .
C6 C7 H7 119.1 . .
C6 C7 C8 121.7(2) . .
C8 C7 H7 119.1 . .
C3 C8 H8 119.7 . .
C7 C8 C3 120.5(2) . .
C7 C8 H8 119.7 . .
C6 C9 H9A 109.5 . .
C6 C9 H9B 109.5 . .
C6 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
P1 C10 H10A 110.4 . .
P1 C10 H10B 110.4 . .
H10A C10 H10B 108.6 . .
C11 C10 P1 106.41(13) . .
C11 C10 H10A 110.4 . .
C11 C10 H10B 110.4 . .
P2 C11 H11A 109.6 . .
P2 C11 H11B 109.6 . .
C10 C11 P2 110.34(13) . .
C10 C11 H11A 109.6 . .
C10 C11 H11B 109.6 . .
H11A C11 H11B 108.1 . .
C22 C21 P1 122.22(15) . .
C22 C21 C26 118.49(18) . .
C26 C21 P1 119.23(15) . .
C21 C22 H22 119.8 . .
C23 C22 C21 120.4(2) . .
C23 C22 H22 119.8 . .
C22 C23 H23 119.8 . .
C24 C23 C22 120.4(2) . .
C24 C23 H23 119.8 . .
C23 C24 H24 120.2 . .
C23 C24 C25 119.5(2) . .
C25 C24 H24 120.2 . .
C24 C25 H25 119.8 . .
C26 C25 C24 120.3(2) . .
C26 C25 H25 119.8 . .
C21 C26 H26 119.6 . .
C25 C26 C21 120.9(2) . .
C25 C26 H26 119.6 . .
C32 C31 P1 120.28(16) . .
C36 C31 P1 121.31(15) . .
C36 C31 C32 118.40(19) . .
C31 C32 H32 119.6 . .
C33 C32 C31 120.8(2) . .
C33 C32 H32 119.6 . .
C32 C33 H33 119.9 . .
C34 C33 C32 120.2(2) . .
C34 C33 H33 119.9 . .
C33 C34 H34 120.2 . .
C33 C34 C35 119.6(2) . .
C35 C34 H34 120.2 . .
C34 C35 H35 119.9 . .
C36 C35 C34 120.2(2) . .
C36 C35 H35 119.9 . .
C31 C36 H36 119.6 . .
C35 C36 C31 120.8(2) . .
C35 C36 H36 119.6 . .
C42 C41 P2 122.77(16) . .
C42 C41 C46 118.39(19) . .
C46 C41 P2 118.81(16) . .
C41 C42 H42 119.6 . .
C41 C42 C43 120.7(2) . .
C43 C42 H42 119.6 . .
C42 C43 H43 119.8 . .
C44 C43 C42 120.3(2) . .
C44 C43 H43 119.8 . .
C43 C44 H44 120.3 . .
C43 C44 C45 119.3(2) . .
C45 C44 H44 120.3 . .
C44 C45 H45 119.8 . .
C44 C45 C46 120.4(2) . .
C46 C45 H45 119.8 . .
C41 C46 H46 119.6 . .
C45 C46 C41 120.8(2) . .
C45 C46 H46 119.6 . .
C52 C51 P2 120.70(15) . .
C56 C51 P2 120.40(15) . .
C56 C51 C52 118.88(18) . .
C51 C52 H52 119.8 . .
C53 C52 C51 120.4(2) . .
C53 C52 H52 119.8 . .
C52 C53 H53 120.0 . .
C54 C53 C52 120.1(2) . .
C54 C53 H53 120.0 . .
C53 C54 H54 120.0 . .
C55 C54 C53 119.97(19) . .
C55 C54 H54 120.0 . .
C54 C55 H55 120.1 . .
C54 C55 C56 119.8(2) . .
C56 C55 H55 120.1 . .
C51 C56 C55 120.88(19) . .
C51 C56 H56 119.6 . .
C55 C56 H56 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ru1 P1 2.3485(5) .
Ru1 P1 2.3485(5) 2_665
Ru1 P2 2.3495(5) .
Ru1 P2 2.3495(5) 2_665
Ru1 C1 2.065(2) .
Ru1 C1 2.065(2) 2_665
P1 C10 1.848(2) .
P1 C21 1.848(2) .
P1 C31 1.833(2) .
P2 C11 1.857(2) .
P2 C41 1.837(2) .
P2 C51 1.838(2) .
C1 C2 1.210(3) .
C2 C3 1.440(3) .
C3 C4 1.398(3) .
C3 C8 1.398(3) .
C4 H4 0.9500 .
C4 C5 1.390(3) .
C5 H5 0.9500 .
C5 C6 1.386(3) .
C6 C7 1.379(3) .
C6 C9 1.516(3) .
C7 H7 0.9500 .
C7 C8 1.392(3) .
C8 H8 0.9500 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C10 C11 1.525(3) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C21 C22 1.397(3) .
C21 C26 1.398(3) .
C22 H22 0.9500 .
C22 C23 1.395(3) .
C23 H23 0.9500 .
C23 C24 1.386(3) .
C24 H24 0.9500 .
C24 C25 1.388(3) .
C25 H25 0.9500 .
C25 C26 1.384(3) .
C26 H26 0.9500 .
C31 C32 1.397(3) .
C31 C36 1.397(3) .
C32 H32 0.9500 .
C32 C33 1.389(3) .
C33 H33 0.9500 .
C33 C34 1.386(3) .
C34 H34 0.9500 .
C34 C35 1.390(3) .
C35 H35 0.9500 .
C35 C36 1.386(3) .
C36 H36 0.9500 .
C41 C42 1.390(3) .
C41 C46 1.396(3) .
C42 H42 0.9500 .
C42 C43 1.394(3) .
C43 H43 0.9500 .
C43 C44 1.385(3) .
C44 H44 0.9500 .
C44 C45 1.386(3) .
C45 H45 0.9500 .
C45 C46 1.387(3) .
C46 H46 0.9500 .
C51 C52 1.399(3) .
C51 C56 1.389(3) .
C52 H52 0.9500 .
C52 C53 1.394(3) .
C53 H53 0.9500 .
C53 C54 1.390(3) .
C54 H54 0.9500 .
C54 C55 1.388(3) .
C55 H55 0.9500 .
C55 C56 1.397(3) .
C56 H56 0.9500 .
