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_4064827
_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         'C27 H20 Cl O P'
_chemical_formula_sum            'C27 H20 Cl O P'
_chemical_formula_weight         426.85
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 120.266(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   42.332(4)
_cell_length_b                   5.5148(5)
_cell_length_c                   41.938(4)
_cell_measurement_reflns_used    5331
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.05
_cell_measurement_theta_min      2.23
_cell_volume                     8456.0(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            21460
_diffrn_reflns_theta_full        21.15
_diffrn_reflns_theta_max         21.15
_diffrn_reflns_theta_min         1.11
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_T_max  0.9919
_exptl_absorpt_correction_T_min  0.7891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS v.2.10 (Bruker,2003) was used for absorption correction. 
 R(int) for selected reflections was 0.042 before and 0.027 after 
 correction. The Ratio of minimum to maximum transmission is 0.795588. 
 The \l/2 correction factor is 0.0015 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         4616
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0383P)^2^+14.0752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                4015
_reflns_number_total             4616
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om200357v_si_001.cif
_cod_data_source_block           mjm286(24)
_cod_original_cell_volume        8455.9(14)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4064827