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_4082144
_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, C59 H52 O3 P3 Ru'
_chemical_formula_sum            'C59 H52 B F4 O3 P3 Ru'
_chemical_formula_weight         1089.80
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-07
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                76.741(6)
_cell_angle_beta                 77.713(6)
_cell_angle_gamma                69.227(7)
_cell_formula_units_Z            2
_cell_length_a                   14.0432(11)
_cell_length_b                   14.2540(10)
_cell_length_c                   15.1618(11)
_cell_measurement_reflns_used    5561
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      25.9059
_cell_measurement_theta_min      2.9032
_cell_volume                     2733.1(4)
_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
;
SHELXL, 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      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.772
_diffrn_measurement_details
;
  1 omega  -37.00   57.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       -9.8267   77.0000   60.0000 94

  2 omega   -5.00   81.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2330   77.0000 -180.0000 86

  3 omega  -16.00   78.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       11.2330   77.0000  -30.0000 94
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0048760000
_diffrn_orient_matrix_UB_12      -0.0412252000
_diffrn_orient_matrix_UB_13      0.0351000000
_diffrn_orient_matrix_UB_21      -0.0389174000
_diffrn_orient_matrix_UB_22      0.0344978000
_diffrn_orient_matrix_UB_23      0.0260785000
_diffrn_orient_matrix_UB_31      -0.0379739000
_diffrn_orient_matrix_UB_32      -0.0050973000
_diffrn_orient_matrix_UB_33      -0.0211168000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13675
_diffrn_reflns_theta_full        22.5
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         2.91
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.908
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.2488
_exptl_crystal_size_mid          0.1373
_exptl_crystal_size_min          0.0917
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         8278
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0520P)^2^+1.9199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                6554
_reflns_number_total             8278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4009247_si_001.cif
_cod_data_source_block           '[4]BF4'
_cod_original_cell_volume        2733.0(3)
_cod_database_code               4082144
_chemical_oxdiff_formula         C43H41B1F4O5P2Ru
_chemical_oxdiff_usercomment     'ejs79-2 colourless'
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     22.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{B1, B1A}
{F2, F2A}
3. Restrained distances
 B1-F1 \\sim B1-F2 \\sim B1-F3 \\sim B1-F4 \\sim B1A-F1A \\sim B1A-F2A \\sim B1A-F3A \\sim B1A-F4A
 with sigma of 0.02
 F3A-F4A \\sim F1A-F2A
 with sigma of 0.02
 F2A-F3A \\sim F4A-F1A
 with sigma of 0.02
 F3-F2 \\sim F1-F4
 with sigma of 0.02
 F3-F4 \\sim F1-F2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(B1) = Uanis(B1A)
Uanis(F2) = Uanis(F2A)
Uanis(F4) = Uanis(F4A)
Uanis(F3) = Uanis(F3A)
5. Others
 Sof(B1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=1-FVAR(1)
 Sof(B1)=Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43),
  C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C51(H51),
 C52(H52), C53(H53), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59)
6.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;