Computational Discovery of Stable Transition-Metal Vinylidene Complexes
Pickup, Oliver J. S.; Khazal, Iman; Smith, Elizabeth J.; Whitwood, Adrian C.; Lynam, Jason M.; Bolaky, Keshan; King, Timothy C.; Rawe, Benjamin W.; Fey, Natalie; Organometallics 33 (2014) 1751–; doi:10.1021/om500114u

data_4082917
_publ_section_title
;
 Computational Discovery of Stable Transition-Metal Vinylidene Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1751
_journal_paper_doi               10.1021/om500114u
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C30 H54 O4 P2 Ru'
_chemical_formula_sum            'C30 H54 O4 P2 Ru'
_chemical_formula_weight         641.74
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-06
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.298(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6749(7)
_cell_length_b                   14.7788(6)
_cell_length_c                   17.0117(7)
_cell_measurement_reflns_used    10454
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      32.0012
_cell_measurement_theta_min      2.8713
_cell_volume                     3186.6(3)
_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
;
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      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details
;
  1 omega  -59.00   -1.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.9830   91.0000  119.0000 58

  2 omega  -30.00    8.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.9830   94.0000 -142.0000 38

  3 omega  -46.00   -3.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3892  -37.0000    0.0000 43

  4 omega  -46.00    2.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3892  -37.0000  -90.0000 48

  5 omega   -4.00   88.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3892   77.0000  -30.0000 92

  6 omega  -56.00  -30.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.0110   94.0000   37.0000 26

  7 omega    3.00   30.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4172   37.0000  -30.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0238242000
_diffrn_orient_matrix_UB_12      0.0425671000
_diffrn_orient_matrix_UB_13      -0.0078175000
_diffrn_orient_matrix_UB_21      0.0453107000
_diffrn_orient_matrix_UB_22      0.0134393000
_diffrn_orient_matrix_UB_23      -0.0212585000
_diffrn_orient_matrix_UB_31      -0.0224311000
_diffrn_orient_matrix_UB_32      -0.0176671000
_diffrn_orient_matrix_UB_33      -0.0350513000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0757
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21096
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.01
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.904
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.1995
_exptl_crystal_size_mid          0.1591
_exptl_crystal_size_min          0.0873
_refine_diff_density_max         1.452
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         9364
_refine_ls_number_restraints     428
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+7.0036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1756
_reflns_number_gt                7413
_reflns_number_total             9364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500114u_si_005.cif
_cod_data_source_block           Compound5aiPr
_cod_depositor_comments          'Adding full bibliography for 4082917.cif.'
_cod_database_code               4082917
_chemical_oxdiff_formula         C30H54O2P2Ru
_chemical_oxdiff_usercomment     'Lizzies ejs39-1'
_reflns_odcompleteness_completeness 97.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01