A Highly Diastereoselective Recognition Process as the Basis for the Resolution of Palladatricyclo[4.1.0.02,4]heptanes
Hashmi, A. Stephen K.; Grundl, Marc A.; Riedel, Dominic; Rudolph, Matthias; Bats, Jan W.; Organometallics 31 (2012) 523–; doi:10.1021/om2009952

data_4068005
_publ_section_title
;
 A Highly Diastereoselective Recognition Process as the Basis for the
 Resolution of Palladatricyclo[4.1.0.02,4]heptanes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              523
_journal_paper_doi               10.1021/om2009952
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C78 H125 N O17 Pd2'
_chemical_formula_sum            'C78 H125 N O17 Pd2'
_chemical_formula_weight         1561.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.203(3)
_cell_length_b                   26.186(2)
_cell_length_c                   13.8835(15)
_cell_measurement_reflns_used    427
_cell_measurement_temperature    146(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     9162.6(16)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      146(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  SIEMENS_SMART_1K_CCD
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            163141
_diffrn_reflns_theta_full        31.90
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  600
_diffrn_standards_number         1742
_exptl_absorpt_coefficient_mu    0.448
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SHELXTL (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.015(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         31035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.04P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                24174
_reflns_number_total             31035
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om2009952_si_002.cif
_cod_data_source_block           compound-5
_cod_original_cell_volume        9162.5(16)
_cod_database_code               4068005