Synthesis, Electrochemistry, Spectroelectrochemistry, and Solid-State Structures of Palladium Biferrocenylphosphines and Their Use in C,C Cross-Coupling Reactions
Lohan, Manja; Milde, Bianca; Heider, Silvio; Speck, J. Matthäus; Krauße, Sabrina; Schaarschmidt, Dieter; Rüffer, Tobias; Lang, Heinrich; Organometallics 31 (2012) 2310–; doi:10.1021/om201220w

data_4076452
_publ_section_title
;
 Synthesis, Electrochemistry, Spectroelectrochemistry, and Solid-State
 Structures of Palladium Biferrocenylphosphines and Their Use in C,C
 Cross-Coupling Reactions
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              2310
_journal_paper_doi               10.1021/om201220w
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C44 H60 Fe2 P2 Se2'
_chemical_formula_sum            'C44 H60 Fe2 P2 Se2'
_chemical_formula_weight         920.48
_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                91.239(3)
_cell_angle_beta                 92.001(4)
_cell_angle_gamma                108.578(4)
_cell_formula_units_Z            1
_cell_length_a                   8.1138(4)
_cell_length_b                   9.2620(3)
_cell_length_c                   13.9761(6)
_cell_measurement_reflns_used    6027
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.6428
_cell_measurement_theta_min      2.9067
_cell_volume                     994.37(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Oxford Gemini S'
_diffrn_measurement_method       '\w 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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9605
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.671
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.37 (release 24-10-2008 CrysAlis171 .NET)
(compiled Oct 24 2008,09:44:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.947
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0587
_reflns_number_gt                3162
_reflns_number_total             3880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201220w_si_001.cif
_cod_data_source_block           exp_023
_cod_original_cell_volume        994.37(7)
_cod_database_code               4076452