Reactions of RuCp and RuCp* Allyl Carbene Complexes: Products Derived from Activation of Phenyl, Cyclohexyl, and Methyl C−H Bonds in PPh3, PCy3, and Cp* Ligands
Rüba, Eva; Mereiter, Kurt; Schmid, Roland; Kirchner, Karl; Bustelo, Emilio; Puerta, M. Carmen; Valerga, Pedro; Organometallics 21 (2002) 2912–; doi:10.1021/om020094g

data_4076827
_publ_section_title
;
 Reactions of RuCp and RuCp* Allyl Carbene Complexes:&#x00A0; Products
 Derived from Activation of Phenyl, Cyclohexyl, and Methyl C&#x2212;H
 Bonds in PPh3, PCy3, and Cp* Ligands
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2912
_journal_paper_doi               10.1021/om020094g
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C39 H58 P Ru  1+,  F6 P 1-'
_chemical_formula_sum            'C39 H58 F6 P2 Ru'
_chemical_formula_weight         803.86
_chemical_name_common
;
           [RuCp(eta4-CH(C6H9)CHC(C6H9)CH-PCy2(eta1-C6H10))]PF6
;
_chemical_name_systematic
; 
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.101(4)
_cell_length_b                   10.857(3)
_cell_length_c                   17.249(4)
_cell_measurement_reflns_used    6147
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      29.9
_cell_measurement_theta_min      2.3
_cell_volume                     3764.4(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'BRUKER SMART 3-circle with CCD area detector'
_diffrn_measurement_method       'omega 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  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52744
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   'multi-scan (program SADABS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1680
_exptl_crystal_preparation
;
 crystallized from dichloromethane / diethyl ether by vapour diffusion method
;
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(17)
_refine_ls_extinction_coef       0.00036(10)
_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   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         10825
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.1608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0713
_reflns_number_gt                9246
_reflns_number_total             10825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020094g.cif
_cod_data_source_block           6a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               4076827