Palladium Complexes with Metallocene-Bridged Bidentate Diphosphine Ligands: Synthesis, Structure, and Catalytic Activity in Amination and Cross-Coupling Reactions
Gusev, Oleg V.; Peganova, Tat'yana A.; Kalsin, Alexander M.; Vologdin, Nikolai V.; Petrovskii, Pavel V.; Lyssenko, Konstantin A.; Tsvetkov, Aleksey V.; Beletskaya, Irina P.; Organometallics 25 (2006) 2750–; doi:10.1021/om050869w

data_4074770
_publ_section_title
;
 Palladium Complexes with Metallocene-Bridged Bidentate Diphosphine
 Ligands:&#x00A0; Synthesis, Structure, and Catalytic Activity in
 Amination and Cross-Coupling Reactions
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2750
_journal_paper_doi               10.1021/om050869w
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C18 H28 Cl2 Fe P2 Pd'
_chemical_formula_sum            'C18 H28 Cl2 Fe P2 Pd'
_chemical_formula_weight         539.49
_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                 94.6840(50)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4630(6)
_cell_length_b                   16.7987(9)
_cell_length_c                   11.5739(7)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      2.45
_cell_volume                     2027.5(2)
_computing_cell_refinement       'SMART (Bruker, 1998b)'
_computing_data_collection       'SMART (Bruker, 1998b)'
_computing_data_reduction        'SAINTPlus (Bruker, 1998a)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13343
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.022
_exptl_absorpt_correction_T_max  0.8479
_exptl_absorpt_correction_T_min  0.6843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1998a)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.751
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         5784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+9.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                4495
_reflns_number_total             5784
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            om050869wsi20060227_102203.cif
_cod_data_source_block           comp18
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4074770