κ1- and κ2-Complexes of Fluorenylidene‒Allenyl Phosphines and Phosphine Oxides with Palladium Chloride and Iron Carbonyl: Displacement of Trimethylsilyl by Diphenylphosphino via a Stabilized Carbanion
Milosevic, Sandra; Banide, Emilie V.; Müller-Bunz, Helge; Gilheany, Declan G.; McGlinchey, Michael J.; Organometallics 30 (2011) 3804–; doi:10.1021/om200357v

data_4064832
_publ_section_title
;
 \k1- and \k2-Complexes of Fluorenylidene--Allenyl Phosphines and
 Phosphine Oxides with Palladium Chloride and Iron Carbonyl: Displacement
 of Trimethylsilyl by Diphenylphosphino via a Stabilized Carbanion
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3804
_journal_paper_doi               10.1021/om200357v
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         '2 (C78 H56 Cl4 O2 P4 Pd2), 5 (C H Cl3)'
_chemical_formula_sum            'C161 H117 Cl23 O4 P8 Pd4'
_chemical_formula_weight         3604.26
_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                84.129(2)
_cell_angle_beta                 87.199(2)
_cell_angle_gamma                81.094(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4539(3)
_cell_length_b                   12.5942(3)
_cell_length_c                   29.1459(7)
_cell_measurement_reflns_used    34358
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.7626
_cell_measurement_theta_min      3.5658
_cell_volume                     3769.03(17)
_computing_cell_refinement
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_collection
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_reduction
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3196
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            75669
_diffrn_reflns_theta_full        62.00
_diffrn_reflns_theta_max         76.97
_diffrn_reflns_theta_min         3.57
_exptl_absorpt_coefficient_mu    8.785
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1810
_exptl_crystal_size_max          0.1519
_exptl_crystal_size_mid          0.0668
_exptl_crystal_size_min          0.0474
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         15282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+1.0121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                12940
_reflns_number_total             15282
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200357v_si_001.cif
_cod_data_source_block           mjm359(34)
_cod_database_code               4064832