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_4083279
_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         'C54 H44 Cl4 Fe N4 O4 Pd Pt S2, 2(C16 H36 N)'
_chemical_formula_sum            'C86 H116 Cl4 Fe N6 O4 Pd Pt S2'
_chemical_formula_weight         1861.11
_chemical_name_systematic        'compound 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                 103.87(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.279(6)
_cell_length_b                   14.532(4)
_cell_length_c                   34.588(7)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      7
_cell_volume                     8920(4)
_computing_cell_refinement       'Siemens P&#x00A7;/PC data Collection System'
_computing_data_collection       'Siemens P3/PC Data Collection System'
_computing_data_reduction        'SHELXTL-plus, XDISK (Sheldrick, 1991)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nicolet P3'
_diffrn_measurement_method       Wyckoff-Scan
_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  0.1235
_diffrn_reflns_av_sigmaI/netI    0.1934
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            25196
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_max  0.790
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             3824
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.969
_refine_diff_density_min         -1.675
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1174
_refine_ls_number_reflns         24309
_refine_ls_number_restraints     842
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.2547
_refine_ls_R_factor_gt           0.1334
_refine_ls_shift/su_max          0.081
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+7.9500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2657
_refine_ls_wR_factor_ref         0.3097
_reflns_number_gt                10732
_reflns_number_total             24309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300600v_si_003.cif
_cod_data_source_block           s1728rm1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'PSI-Scan' changed to
'psi-scan' according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4083279