cis-β-Bis(carbonyl) Ruthenium-Salen Complexes: X-ray Crystal Structures and Remarkable Catalytic Properties toward Asymmetric Intramolecular Alkene Cyclopropanation
Zhen-Jiang Xu; Ran Fang; Cunyuan Zhao; Jie-Sheng Huang; Gong-Yong Li; Nianyong Zhu; Chi-Ming Che; Journal of the American Chemical Society 131 (2009) 4405–4417; doi:10.1021/ja8086399

data_4104093
_publ_section_title
;
 cis-\b-Bis(carbonyl) Ruthenium-Salen Complexes: X-ray Crystal Structures
 and Remarkable Catalytic Properties toward Asymmetric Intramolecular
 Alkene Cyclopropanation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4405
_journal_page_last               4417
_journal_paper_doi               10.1021/ja8086399
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C52.50 H55 Cl N2 O4 Ru'
_chemical_formula_sum            'C52.5 H55 Cl N2 O4 Ru'
_chemical_formula_weight         914.51
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                85.14(3)
_cell_angle_beta                 88.56(3)
_cell_angle_gamma                68.73(3)
_cell_formula_units_Z            4
_cell_length_a                   15.678(3)
_cell_length_b                   16.111(3)
_cell_length_c                   20.109(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4716.2(19)
_computing_cell_refinement       scalepack
_computing_data_collection       marcontrol
_computing_data_reduction        denzo
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.651
_diffrn_measured_fraction_theta_max 0.651
_diffrn_measurement_device_type  'marresearch IPDS mar300'
_diffrn_measurement_method       oscillation
_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  0.0475
_diffrn_reflns_av_sigmaI/netI    0.1606
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21678
_diffrn_reflns_theta_full        25.17
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.760
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1084
_refine_ls_number_reflns         11032
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      0.764
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                5425
_reflns_number_total             11032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8086399_si_001_3.cif
_cod_data_source_block           complex_2a
_cod_original_cell_volume        4716.2(16)
_cod_original_formula_sum        'C52.50 H55 Cl N2 O4 Ru'
_cod_database_code               4104093