Preparation of hydrido(vinylidene)ruthenium(II) complexes and a one-pot synthesis of Grubbs-type ruthenium carbenes.
Stüer, Wolfram; Weberndörfer, Birgit; Wolf, Justin; Werner, Helmut; Dalton transactions (Cambridge, England : 2003)  (2005) 1796–1803; doi:10.1039/b502440d

data_7008413
_publ_section_title
;
 Preparation of hydrido(vinylidene)ruthenium(II) complexes and a
 one-pot synthesis of Grubbs-type ruthenium carbenes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1796
_journal_page_last               1803
_journal_paper_doi               10.1039/b502440d
_journal_year                    2005
_chemical_formula_sum            'C44 H79 Cl N P2 Ru'
_chemical_formula_weight         820.54
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.43(3)
_cell_angle_beta                 76.10(3)
_cell_angle_gamma                74.81(3)
_cell_formula_units_Z            2
_cell_length_a                   10.672(2)
_cell_length_b                   11.352(2)
_cell_length_c                   19.703(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      2.41
_cell_volume                     2236.1(8)
_computing_cell_refinement       'IPDS (STOE)'
_computing_data_collection       'IPDS (STOE)'
_computing_data_reduction        'IPDS (STOE)'
_computing_molecular_graphics    'ZORTEP (Zsolnai)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'IPDS (STOE)'
_diffrn_measurement_method       Psi-Scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_sigmaI/netI    0.1174
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26086
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.511
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0099(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7178
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                4230
_reflns_number_total             7178
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b502440d.txt
_cod_data_source_block           ws5wb
_cod_database_code               7008413