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_4082146
_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         'C53 H44 O3 P2 Ru'
_chemical_formula_sum            'C53 H44 O3 P2 Ru'
_chemical_formula_weight         891.89
_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             2012-04-27
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                79.011(5)
_cell_angle_beta                 88.831(4)
_cell_angle_gamma                86.219(4)
_cell_formula_units_Z            2
_cell_length_a                   9.5638(5)
_cell_length_b                   11.9179(7)
_cell_length_c                   18.5356(10)
_cell_measurement_reflns_used    8033
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      29.3513
_cell_measurement_theta_min      2.8348
_cell_volume                     2069.4(2)
_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
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
Palatinus, L. & Chapuis, G. (2007).
SUPERFLIP - a computer program for the solution of crystal structures
 by charge flipping in arbitrary dimensions.
J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_details
;
  1 omega  -21.00   16.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.4882  -89.0000   62.0000 37

  2 omega  -49.00   41.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5820  -57.0000   60.0000 90

  3 omega   48.00   96.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5820 -178.0000   90.0000 48

  4 omega  -20.00   57.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5820  -99.0000  -60.0000 77

  5 omega  -14.00   88.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5820   19.0000 -120.0000 102

  6 omega   13.00   50.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5820  -77.0000 -180.0000 37
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0456607000
_diffrn_orient_matrix_UB_12      -0.0304924000
_diffrn_orient_matrix_UB_13      -0.0177086000
_diffrn_orient_matrix_UB_21      0.0041491000
_diffrn_orient_matrix_UB_22      -0.0459686000
_diffrn_orient_matrix_UB_23      0.0306129000
_diffrn_orient_matrix_UB_31      -0.0585171000
_diffrn_orient_matrix_UB_32      0.0253990000
_diffrn_orient_matrix_UB_33      0.0163834000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17257
_diffrn_reflns_theta_full        26.67
_diffrn_reflns_theta_max         29.42
_diffrn_reflns_theta_min         2.84
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.502
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.947
_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            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.1547
_exptl_crystal_size_mid          0.1146
_exptl_crystal_size_min          0.0112
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+1.7689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0794
_reflns_number_gt                8096
_reflns_number_total             9679
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4009247_si_001.cif
_cod_data_source_block           '[6]'
_cod_original_cell_volume        2069.38(19)
_cod_database_code               4082146
_chemical_oxdiff_formula         C53H44O3P2Ru1
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67