Palladacycle from Cyclometalation of the Unsubstituted Cyclopentadienyl Ring in Ferrocene: Synthesis, Characterization, Theoretical Studies, and Application to Suzuki‒Miyaura Reaction
Qian, Hengyu; Yin, Zhigang; Zhang, Tongyan; Yan, Shihai; Wang, Quanling; Zhang, Chunxia; Organometallics 33 (2014) 6241–; doi:10.1021/om5008924

data_4084523
_publ_section_title
;
 Palladacycle from Cyclometalation of the Unsubstituted Cyclopentadienyl
 Ring in Ferrocene: Synthesis, Characterization, Theoretical Studies, and
 Application to Suzuki--Miyaura Reaction
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6241
_journal_paper_doi               10.1021/om5008924
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C40 H39 Cl Fe N O P Pd'
_chemical_formula_weight         778.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.738(13)
_cell_angle_beta                 98.035(17)
_cell_angle_gamma                95.052(16)
_cell_formula_units_Z            2
_cell_length_a                   8.1800(19)
_cell_length_b                   10.9180(16)
_cell_length_c                   19.969(4)
_cell_measurement_reflns_used    2344
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3134
_cell_measurement_theta_min      3.0153
_cell_volume                     1753.6(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0925
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14571
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  0.323
_exptl_absorpt_correction_T_min  0.268
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         7162
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1753
_reflns_number_gt                4526
_reflns_number_total             7162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5008924_si_002.cif
_cod_data_source_block           4b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/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 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4084522--4084523.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084523