Neutral Ruthenium Carbene Complexes bearing N,N,O Heteroscorpionate Ligands: Syntheses and Activity in Metathesis Reactions
Kopf, Henning; Holzberger, Bastian; Pietraszuk, Cezary; Hübner, Eike; Burzlaff, Nicolai; Organometallics 27 (2008) 5894–; doi:10.1021/om8006129

data_4072147
_publ_section_title
;
 Neutral Ruthenium Carbene Complexes bearing N,N,O Heteroscorpionate
 Ligands: Syntheses and Activity in Metathesis Reactions
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5894
_journal_paper_doi               10.1021/om8006129
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H46 Cl N4 O2 P Ru, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C34.5 H49 Cl4 N4 O2 P Ru'
_chemical_formula_weight         825.62
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-06-23T21:44:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.78(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.350(3)
_cell_length_b                   10.613(2)
_cell_length_c                   25.671(5)
_cell_measurement_reflns_used    24491
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.12
_cell_measurement_theta_min      1.66
_cell_volume                     4133.0(14)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1077
_diffrn_reflns_av_unetI/netI     0.1054
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26071
_diffrn_reflns_theta_full        23.77
_diffrn_reflns_theta_max         23.77
_diffrn_reflns_theta_min         3.3
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.71
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.283
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.815
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0011(4)
_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   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         5757
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1188P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1719
_refine_ls_wR_factor_ref         0.1955
_reflns_number_gt                3540
_reflns_number_total             5757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8006129_si_001.cif
_cod_data_source_block           compound6
_cod_original_cell_volume        4133.1(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C34.50 H49 Cl4 N4 O2 P Ru'
_cod_database_code               4072147