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_4082143
_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         'B F4, C65 H51 O4 P2 Ru, 1.06(C H2 Cl2)'
_chemical_formula_sum            'C66.06 H53.12 B Cl2.12 F4 O4 P2 Ru'
_chemical_formula_weight         1235.69
_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             2012-09-20
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                89.703(3)
_cell_angle_beta                 81.511(3)
_cell_angle_gamma                63.313(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9840(4)
_cell_length_b                   14.1298(5)
_cell_length_c                   18.1180(6)
_cell_measurement_reflns_used    8072
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      29.0468
_cell_measurement_theta_min      2.8944
_cell_volume                     2930.29(19)
_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 0.993
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_details
;
  1 omega   -7.00   26.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8640   37.0000 -180.0000 33

  2 omega   -3.00   27.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8640   92.0000   -2.0000 30

  3 omega  -11.00   84.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8640   77.0000  -90.0000 95

  4 omega  -48.00   46.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8640  -77.0000  150.0000 94

  5 omega  -49.00   41.00   1.0000  110.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8640  -37.0000    0.0000 90
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0450591000
_diffrn_orient_matrix_UB_12      0.0107656000
_diffrn_orient_matrix_UB_13      -0.0189189000
_diffrn_orient_matrix_UB_21      -0.0065445000
_diffrn_orient_matrix_UB_22      0.0335159000
_diffrn_orient_matrix_UB_23      0.0311812000
_diffrn_orient_matrix_UB_31      0.0420327000
_diffrn_orient_matrix_UB_32      -0.0439617000
_diffrn_orient_matrix_UB_33      0.0156243000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20612
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         2.90
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.985
_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 dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1264.2
_exptl_crystal_size_max          0.1444
_exptl_crystal_size_mid          0.0839
_exptl_crystal_size_min          0.0735
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         13085
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0311P)^2^+3.0629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                10637
_reflns_number_total             13085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4009247_si_001.cif
_cod_data_source_block           '[3aBz]BF4.CH2Cl2'
_cod_original_cell_volume        2930.28(19)
_cod_database_code               4082143
_chemical_oxdiff_formula         C65H51B1F4O4P2Ru1
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_refinement_special_details
;
 The crystal contained dichloromethanes of crystallisation which 
 were readily lost on removal from the mother liquor.  The
 solvent was modelled as follows.  One dichloromethane was
 disordered and modelled over two sites with refined occupancies
 of 0.848:0.152(3).  The other dichloromethane site was found
 to be only partially occupied and modelled with a refined
 occupancy of 0.058(2).
;