Combined Spectroscopic and Quantum Chemical Study of [trans-Ru(C\τb CC6H4R1-4)2(dppe)2]n+and [trans-Ru(C≡CC6H4R1-4)(C\τb CC6H4R2-4)(dppe)2]n+(n= 0, 1) Complexes: Interpretations beyond the Lowest Energy Conformer Paradigm
Marqués-González, Santiago; Parthey, Matthias; Yufit, Dmitry S.; Howard, Judith A. K.; Kaupp, Martin; Low, Paul J.; Organometallics 33 (2014) 4947–; doi:10.1021/om500265s

data_4083892
_publ_section_title
;
 Combined Spectroscopic and Quantum Chemical Study of [trans-Ru(C\\tb
 CC6H4R1-4)2(dppe)2]n+and [trans-Ru(C\\tb CC6H4R1-4)(C\\tb
 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         'C59 H57 Cl P4 Ru Si'
_chemical_formula_sum            'C59 H57 Cl P4 Ru Si'
_chemical_formula_weight         1054.54
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-03-09
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled 2012.01.17 svn.r2163, GUI svn.r4036)
;
_cell_angle_alpha                77.540(5)
_cell_angle_beta                 78.486(6)
_cell_angle_gamma                68.888(5)
_cell_formula_units_Z            2
_cell_length_a                   9.8038(7)
_cell_length_b                   12.5100(5)
_cell_length_c                   23.4636(16)
_cell_measurement_reflns_used    3815
_cell_measurement_temperature    150
_cell_measurement_theta_max      32.6661
_cell_measurement_theta_min      2.5799
_cell_volume                     2597.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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      150
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -94.00  -10.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -57.0000    0.0000 84

  2 omega  -46.00   40.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867   57.0000 -120.0000 86

  3 omega  -98.00    8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867  -19.0000   60.0000 106

  4 omega  -69.00  -43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.1867 -179.0000  120.0000 26

  5 omega   62.00   88.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000  150.0000 26

  6 omega   26.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -114.0000  -11.0000 51

  7 omega   29.00   77.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -114.0000  168.0000 48

  8 omega  -33.00   45.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  -19.0000  -90.0000 78

  9 omega   66.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000    0.0000 32
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0403862000
_diffrn_orient_matrix_UB_12      -0.0217197000
_diffrn_orient_matrix_UB_13      0.0255808000
_diffrn_orient_matrix_UB_21      -0.0541944000
_diffrn_orient_matrix_UB_22      0.0038149000
_diffrn_orient_matrix_UB_23      -0.0170561000
_diffrn_orient_matrix_UB_31      0.0394521000
_diffrn_orient_matrix_UB_32      -0.0574590000
_diffrn_orient_matrix_UB_33      -0.0055361000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.1284
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26759
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.59
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.4587
_exptl_crystal_size_mid          0.1581
_exptl_crystal_size_min          0.0361
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         11934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0558
_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/[\s^2^(Fo^2^)+(0.0050P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                7644
_reflns_number_total             11934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500265s_si_002.cif
_cod_data_source_block           2j_12srv072
_cod_database_code               4083892
_chemical_oxdiff_formula         C59H57Cl1P4Ru1Si1
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44