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_4076451
_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         'C56 H46 Cl2 Fe4 O4 P2 Pd, 2/3(C H Cl3)'
_chemical_formula_sum            'C57.33333 H47.33333 Cl5.33333 Fe4 O4 P2 Pd'
_chemical_formula_weight         1381.09
_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                103.956(3)
_cell_angle_beta                 92.056(3)
_cell_angle_gamma                103.990(3)
_cell_formula_units_Z            3
_cell_length_a                   10.7582(4)
_cell_length_b                   15.1506(5)
_cell_length_c                   26.4251(9)
_cell_measurement_reflns_used    15096
_cell_measurement_temperature    105
_cell_measurement_theta_max      28.7082
_cell_measurement_theta_min      2.9833
_cell_volume                     4035.6(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      105
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33156
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.752
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2082
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.463
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     997
_refine_ls_number_reflns         15792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0914P)^2^+35.2423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1981
_refine_ls_wR_factor_ref         0.2079
_reflns_number_gt                10531
_reflns_number_total             15792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201220w_si_001.cif
_cod_data_source_block           exp_072
_cod_depositor_comments
;

2021-04-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        4035.6(2)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_moiety     '3(C56 H46 Cl2 Fe4 O4 P2 Pd), 2(C H Cl3)'
_cod_original_formula_sum        'C172 H142 Cl16 Fe12 O12 P6 Pd3'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     4143.28
_cod_database_code               4076451