Synthesis of Novel Dimeric Allylpalladium(II) Complexes from PdCl2-Promoted Ring-Opening Reactions of Vinylidenecyclopropanes
Gu, Xingxing; Wang, Feijun; Qi, Ming-hui; Shao, Li-xiong; Shi, Min; Organometallics 28 (2009) 1569–; doi:10.1021/om801117g

data_4068820
_publ_section_title
;
 Synthesis of Novel Dimeric Allylpalladium(II) Complexes from
 PdCl2-Promoted Ring-Opening Reactions of Vinylidenecyclopropanes
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1569
_journal_paper_doi               10.1021/om801117g
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C64 H54 Cl2 Pd2'
_chemical_formula_weight         1106.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.3370(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1405(11)
_cell_length_b                   16.7692(11)
_cell_length_c                   22.9735(16)
_cell_measurement_reflns_used    6056
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.536
_cell_measurement_theta_min      4.393
_cell_volume                     6024.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1113
_diffrn_reflns_av_sigmaI/netI    0.1099
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34758
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6514
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.081
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       0.0023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         13083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0630
_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^)+(0.1092P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2140
_reflns_number_gt                7843
_reflns_number_total             13083
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801117g_si_002.cif
_cod_data_source_block           cd27457
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4068820