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_4082915
_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         'C22 H48 O4 P2 Ru'
_chemical_formula_sum            'C22 H48 O4 P2 Ru'
_chemical_formula_weight         539.61
_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             2011-07-19
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.2053(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.81596(13)
_cell_length_b                   17.4581(3)
_cell_length_c                   14.16497(15)
_cell_measurement_reflns_used    10003
_cell_measurement_temperature    109.7
_cell_measurement_theta_max      32.0517
_cell_measurement_theta_min      3.0095
_cell_volume                     2632.40(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      109.7
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_details
;
  1 omega   31.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3892   37.0000  -90.0000 66

  2 omega  -45.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3892  -37.0000   90.0000 72

  3 omega   26.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3892  -77.0000 -180.0000 26

  4 omega    3.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3892  -37.0000  120.0000 49

  5 omega  -33.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3892  -77.0000   30.0000 42
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0343258000
_diffrn_orient_matrix_UB_12      -0.0309238000
_diffrn_orient_matrix_UB_13      0.0151201000
_diffrn_orient_matrix_UB_21      -0.0076493000
_diffrn_orient_matrix_UB_22      -0.0160387000
_diffrn_orient_matrix_UB_23      -0.0466050000
_diffrn_orient_matrix_UB_31      0.0564688000
_diffrn_orient_matrix_UB_32      -0.0208462000
_diffrn_orient_matrix_UB_33      0.0135424000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16355
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         32.19
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
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            '? ? orange'
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_crystal_recrystallization_method Pentane
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.1935
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.498
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         8322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0210P)^2^+0.8788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                7360
_reflns_number_total             8322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500114u_si_005.cif
_cod_data_source_block           Compound3aiPr
_cod_depositor_comments          'Adding full bibliography for 4082915.cif.'
_cod_database_code               4082915
_chemical_oxdiff_formula         'C22H43B N6P Rh Si'
_chemical_oxdiff_usercomment     'Lizzie's ejs35'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01