Mapping the Elimination of Water from Hydroxyvinylidene Complexes of Ruthenium(II): Access to Allenylidene and Vinylvinylidene Complexes in a Stepwise Fashion
Smith, Elizabeth J.; Johnson, David G.; Thatcher, Robert J.; Whitwood, Adrian C.; Lynam, Jason M.; Organometallics 32 (2013) 7407–; doi:10.1021/om4009247

data_4082145
_publ_section_title
;
 Mapping the Elimination of Water from Hydroxyvinylidene Complexes of
 Ruthenium(II): Access to Allenylidene and Vinylvinylidene Complexes in a
 Stepwise Fashion
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7407
_journal_paper_doi               10.1021/om4009247
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C55 H46 O4 P2 Ru, 0.5(C4 H10 O)'
_chemical_formula_sum            'C57 H51 O4.5 P2 Ru'
_chemical_formula_weight         970.99
_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             2012-08-23
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                105.546(2)
_cell_angle_beta                 105.975(3)
_cell_angle_gamma                100.147(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1443(3)
_cell_length_b                   13.0096(3)
_cell_length_c                   18.0739(6)
_cell_measurement_reflns_used    21961
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      32.1999
_cell_measurement_theta_min      2.9174
_cell_volume                     2337.01(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_details
;
  1 omega  -94.00  -64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1672 -178.0000   30.0000 30

  2 omega  -44.00  -13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1672  -79.0000  170.0000 31

  3 omega   -3.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172   79.0000    9.0000 47

  4 omega  -37.00   36.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172  -57.0000   30.0000 73

  5 omega    0.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172   79.0000  114.0000 33

  6 omega  -20.00   66.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172  -99.0000  -90.0000 86

  7 omega  -38.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172    0.0000 -120.0000 130

  8 omega    1.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172   37.0000  120.0000 98

  9 omega   -4.00   97.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172   77.0000 -150.0000 101

 10 omega  -18.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172   19.0000   30.0000 117
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0449883000
_diffrn_orient_matrix_UB_12      -0.0526527000
_diffrn_orient_matrix_UB_13      -0.0224005000
_diffrn_orient_matrix_UB_21      0.0316037000
_diffrn_orient_matrix_UB_22      -0.0079670000
_diffrn_orient_matrix_UB_23      -0.0293819000
_diffrn_orient_matrix_UB_31      0.0412840000
_diffrn_orient_matrix_UB_32      -0.0248667000
_diffrn_orient_matrix_UB_33      0.0226073000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43066
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.27
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1006
_exptl_crystal_recrystallization_method ether
_exptl_crystal_size_max          0.2586
_exptl_crystal_size_mid          0.1761
_exptl_crystal_size_min          0.137
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         15076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0261P)^2^+1.3875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                13255
_reflns_number_total             15076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4009247_si_001.cif
_cod_data_source_block           '[5].Et2O'
_cod_original_cell_volume        2337.02(11)
_cod_original_formula_sum        'C57 H51 O4.5 P2 Ru1'
_cod_database_code               4082145
_chemical_oxdiff_formula         'C55 H46 O4 P2 Ru1'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01