Asymmetric Synthesis of Heterobimetallic Planar Chiral Ferrocene Pallada-/Platinacycles and Their Application to Enantioselective Aza-Claisen Rearrangements
Weiss, Marcel; Frey, Wolfgang; Peters, René; Organometallics 31 (2012) 6365–; doi:10.1021/om300600v

data_4083278
_publ_section_title
;
 Asymmetric Synthesis of Heterobimetallic Planar Chiral Ferrocene
 Pallada-/Platinacycles and Their Application to Enantioselective
 Aza-Claisen Rearrangements
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6365
_journal_paper_doi               10.1021/om300600v
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration rd
_chemical_formula_moiety
' C108 H88 Cl4 Fe2 N8 O8 Pd2 Pt2 S4, 7(C H Cl3)'
_chemical_formula_sum            'C115 H95 Cl25 Fe2 N8 O8 Pd2 Pt2 S4'
_chemical_formula_weight         3446.16
_chemical_name_systematic        'Compound [FBIP-CL]~2~'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 118.643(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.2401(5)
_cell_length_b                   30.2619(12)
_cell_length_c                   15.5994(6)
_cell_measurement_reflns_used    33804
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.62
_cell_measurement_theta_min      1.35
_cell_volume                     6313.9(4)
_computing_cell_refinement       'Bruker APEX II Software Suite, 2008'
_computing_data_collection       'Bruker APEX II Software Suite, 2008'
_computing_data_reduction        'Bruker APEX II Software Suite, 2008'
_computing_molecular_graphics    'SHELXTL-plus, XP (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            129233
_diffrn_reflns_theta_full        30.62
_diffrn_reflns_theta_max         30.62
_diffrn_reflns_theta_min         1.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.363
_exptl_absorpt_correction_T_max  0.6503
_exptl_absorpt_correction_T_min  0.4220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.813
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3388
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.744
_refine_diff_density_min         -4.833
_refine_diff_density_rms         0.193
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1499
_refine_ls_number_reflns         37781
_refine_ls_number_restraints     217
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0492
_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^)+(0.0210P)^2^+59.3176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1231
_reflns_number_gt                33804
_reflns_number_total             37781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300600v_si_002.cif
_cod_data_source_block           s1806lm1
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4083278