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_4076453
_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         'C34 H31 Fe2 P Se'
_chemical_formula_sum            'C34 H31 Fe2 P Se'
_chemical_formula_weight         661.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 92.184(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.0722(7)
_cell_length_b                   7.4578(5)
_cell_length_c                   15.2042(10)
_cell_measurement_reflns_used    6592
_cell_measurement_temperature    105
_cell_measurement_theta_max      63.8072
_cell_measurement_theta_min      4.5877
_cell_volume                     1367.87(15)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      105
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.980
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9073
_diffrn_reflns_theta_full        63.95
_diffrn_reflns_theta_max         63.95
_diffrn_reflns_theta_min         4.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  5
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    10.740
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4247
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0992P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                4084
_reflns_number_total             4247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201220w_si_001.cif
_cod_data_source_block           manja32
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4076453