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_4083891
_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         'C62 H53 Cl P4 Ru'
_chemical_formula_sum            'C62 H53 Cl P4 Ru'
_chemical_formula_weight         1058.44
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-27
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.037(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5037(7)
_cell_length_b                   22.4968(8)
_cell_length_c                   19.4374(10)
_cell_measurement_reflns_used    9682
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.79
_cell_volume                     5017.8(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Rigaku CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Rigaku Saturn 724+ CCD area detector'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           'synchrotron '
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            53556
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.34
_diffrn_source
'undulator, Beamline I19, Diamond Light Source, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.534
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0986 before and 0.0590 after correction.
The Ratio of minimum to maximum transmission is 0.8771.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         13451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0376
_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/[\s^2^(Fo^2^)+(0.0350P)^2^+4.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                11213
_reflns_number_total             13451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500265s_si_002.cif
_cod_data_source_block           2i_smg
_cod_original_cell_volume        5017.9(4)
_cod_database_code               4083891
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H46 of C46, H93 of C93, H56 of C56, H44 of C44, H45 of C45, H85 of C85, H25
  of C25, H53 of C53, H43 of C43, H84 of C84, H86 of C86, H35 of C35, H36 of
  C36, H55 of C55, H75 of C75, H83 of C83, H26 of C26, H32 of C32, H65 of C65,
  H72 of C72, H94 of C94, H62 of C62, H54 of C54, H92 of C92, H34 of C34, H74
  of C74, H82 of C82, H33 of C33, H63 of C63, H52 of C52, H76 of C76, H96 of
  C96, H64 of C64, H73 of C73, H42 of C42, H66 of C66, {H14A,H14B} of C14,
  {H13A,H13B} of C13, {H12A,H12B} of C12, {H11A,H11B} of C11, H24 of C24, H23
  of C23, H22 of C22, H95 of C95, H4 of C4, H10 of C10, H8 of C8, H7 of C7, H5
  of C5
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C22(H22), C23(H23), C24(H24), C25(H25),
 C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55),
 C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73),
  C74(H74), C75(H75), C76(H76), C82(H82), C83(H83), C84(H84), C85(H85),
 C86(H86), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96)
2.c :
 C10(H10)
;