Synthesis and Structural Characterization of Monophosphine-Cyclopalladated Ferrocenylpyrimidine Complexes and Reusable Catalytic System for Amination of Hindered Aryl Chlorides in PEG-400
Xu, Chen; Wang, Zhi-Qiang; Fu, Wei-Jun; Lou, Xin-Hua; Li, Ying-Fei; Cen, Fei-Fei; Ma, Hong-Ji; Ji, Bao-Ming; Organometallics 28 (2009) 1909–1916; doi:10.1021/om801149r

data_4068898
_publ_section_title
;
 Synthesis and Structural Characterization of
 Monophosphine-Cyclopalladated Ferrocenylpyrimidine Complexes and Reusable
 Catalytic System for Amination of Hindered Aryl Chlorides in PEG-400
;
_journal_coden_ASTM              ORGND7
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1909
_journal_page_last               1916
_journal_paper_doi               10.1021/om801149r
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C34 H30 Cl Fe N2 P Pd'
_chemical_formula_weight         695.27
_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                 99.682(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7417(18)
_cell_length_b                   18.765(4)
_cell_length_c                   16.601(3)
_cell_measurement_reflns_used    5038
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.38
_cell_volume                     2991.5(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART(Bruker, 2004)'
_computing_data_reduction        'Bruker SAINT(Bruker, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL(Sheldrick, 2008)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18261
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.7724
_exptl_absorpt_correction_T_min  0.5800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+1.6391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0566
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                4937
_reflns_number_total             5542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801149r_si_003.cif
_cod_data_source_block           a
_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_cell_volume        2991.6(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4068898