Improving Grubbs' II type ruthenium catalysts by appropriately modifying the N-heterocyclic carbene ligand.
Vieille-Petit, Ludovic; Luan, Xinjun; Gatti, Michele; Blumentritt, Sascha; Linden, Anthony; Clavier, Hervé; Nolan, Steven P; Dorta, Reto; Chemical communications (Cambridge, England) 34 (2009) 3783–3785; doi:10.1039/b904634h

data_7104571
_publ_section_title
;
 Improving Grubbs' II type ruthenium catalysts by appropriately
 modifying the N-heterocyclic carbene ligand.
;
_journal_issue                   25
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3783
_journal_page_last               3785
_journal_paper_doi               10.1039/b904634h
_journal_volume                  34
_journal_year                    2009
_chemical_formula_moiety         'C67 H90 Cl N2 P Ru, C H2 Cl2'
_chemical_formula_sum            'C68 H92 Cl3 N2 P Ru'
_chemical_formula_weight         1175.82
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             08-09-16
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.3964(8)
_cell_angle_beta                 75.4952(8)
_cell_angle_gamma                79.1259(8)
_cell_formula_units_Z            2
_cell_length_a                   12.6367(2)
_cell_length_b                   12.7897(2)
_cell_length_c                   19.6484(2)
_cell_measurement_reflns_used    94065
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     3019.14(7)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO-SMN and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 '65 mm CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
'Nonius KappaCCD area-detector diffractometer'
_diffrn_measurement_method       '\w scans with \k offsets'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'Nonius FR590 sealed tube generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            77597
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
The asymmetric unit contains one molecule of the Rh-complex plus one
disordered molecule of CH~2~Cl~2~. Attempts to model the solvent molecule
were unsatisfactory. Therefore, the SQUEEZE routine of the program PLATON
was employed. This procedure, which allows the disordered solvent molecule
to be omitted entirely from the subsequent refinement model, gave
substantially improved refinement results and there were no significant
peaks of residual electron density to be found in the voids of the structure.
When the solvent molecule is omitted from the model, each unit cell contains
two cavities of 147 \%A^3^. The electron count in each cavity was calculated
to be approximately 40 e. As the crystals grew from a CH~2~Cl~2~ / MeOH
solution and the initial electron density peak distribution looked somewhat
like a CH~2~Cl~2~ molecule, it is assumed the cavities contain CH~2~Cl~2~.
Allowing for one molecule of CH~2~Cl~2~ per cavity yields 42 e and this
estimate was used in the subsequent calculation of the empirical formula,
formula weight, density, linear absorption coefficient and F(000). Thus
the ratio of Rh-complex to CH~2~Cl~2~ is approximately 1:1.
;
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.0043(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   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         13740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+1.2220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                11087
_reflns_number_total             13742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b904634h.txt
_cod_data_source_block           2c
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7104571