Chiral Osmium Complexes with Sterically Bulky Schiff-Base Ligands. Crystal Structures of Os(IV) Derivatives and the Reactivity and Catalytic Cyclopropanation of Alkenes with EDA
Jing Zhang; Jiang-Lin Liang; Xian-Ru Sun; Hai-Bing Zhou; Nian-Yong Zhu; Zhong-Yuan Zhou; Philip Wai Hong Chan; Chi-Ming Che; Inorganic Chemistry 44 (2005) 3942–3954; doi:10.1021/ic0481935

data_4308867
_publ_section_title
;
Chiral Osmium Complexes with Sterically Bulky Schiff-Base Ligands. Crystal
Structures of Os(IV) Derivatives and the Reactivity and Catalytic
Cyclopropanation of Alkenes with EDA
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3942
_journal_page_last               3954
_journal_paper_doi               10.1021/ic0481935
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C33.50 H28 Br4 Cl4.50 N6 O6 Os'
_chemical_formula_sum            'C33.5 H28 Br4 Cl4.5 N6 O6 Os'
_chemical_formula_weight         1279.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 104.25(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.574(3)
_cell_length_b                   17.400(4)
_cell_length_c                   19.254(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     4082.9(17)
_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      253(2)
_diffrn_measured_fraction_theta_full 0.796
_diffrn_measured_fraction_theta_max 0.796
_diffrn_measurement_device_type  'Marresearch imaging Plate'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_sigmaI/netI    0.1336
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19063
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    7.384
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2446
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.346
_refine_diff_density_min         -1.879
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5921
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.941
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                3442
_reflns_number_total             5921
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0481935si20041222_032309.cif
_cod_data_source_block           mar376
_cod_original_cell_volume        4082.9(16)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C33.50 H28 Br4 Cl4.50 N6 O6 Os'
_cod_database_code               4308867