Facile, Thermoreversible Cycloaddition of Small Molecules to a Ruthenium(II) Arene β-Diketiminate
Phillips, Andrew D.; Laurenczy, Gábor; Scopelliti, Rosario; Dyson, Paul J.; Organometallics 26 (2007) 1120–; doi:10.1021/om070017r

data_4073018
_publ_section_title
;
 Facile, Thermoreversible Cycloaddition of Small Molecules to a
 Ruthenium(II) Arene \b-Diketiminate
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1120
_journal_paper_doi               10.1021/om070017r
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C32 H41 F3 N2 O4 Ru S'
_chemical_formula_weight         707.80
_chemical_name_common            BzRu(H)NacNacMe(H)OTf.THF
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.091(2)
_cell_length_b                   11.916(2)
_cell_length_c                   21.966(4)
_cell_measurement_reflns_used    79
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      21.042
_cell_measurement_theta_min      9.265
_cell_volume                     3157.5(9)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'PLATON (Spek, 2005)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_detector                 'Apex II CCD'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker-Nonus KappaCCD'
_diffrn_measurement_method       'phi and 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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            66668
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.54
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.8587
_exptl_absorpt_correction_T_min  0.8587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2.03 (Bruker, 2001)
 R.H. Blessing, Acta Cryst. (1995), a51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0085P)^2^+3.6947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0541
_reflns_number_gt                6225
_reflns_number_total             7159
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            om070017rsi20070108_083327.cif
_cod_data_source_block           adp159
_cod_original_cell_volume        3157.5(11)
_cod_original_sg_symbol_H-M      'P 2 1 / n'
_cod_database_code               4073018