New Lithium Phosphonium Diylides: A Methylene and a Cyclopentadienyl Moiety as Ylidic Coordination Sites
Lichtenberg, Crispin; Hillesheim, Nina S.; Elfferding, Michael; Oelkers, Benjamin; Sundermeyer, Jörg; Organometallics 31 (2012) 4259–; doi:10.1021/om201182y

data_4078415
_publ_section_title
;
 New Lithium Phosphonium Diylides: A Methylene and a Cyclopentadienyl
 Moiety as Ylidic Coordination Sites
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4259
_journal_paper_doi               10.1021/om201182y
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C44 H48 Li2 P2'
_chemical_formula_sum            'C44 H48 Li2 P2'
_chemical_formula_weight         652.64
_chemical_name_common            'compound 9'
_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                91.412(4)
_cell_angle_beta                 90.728(4)
_cell_angle_gamma                100.064(4)
_cell_formula_units_Z            2
_cell_length_a                   8.5472(4)
_cell_length_b                   11.2691(6)
_cell_length_c                   19.6735(9)
_cell_measurement_reflns_used    14377
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.185
_cell_measurement_theta_min      1.835
_cell_volume                     1864.93(16)
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_collection       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-RED'
_computing_molecular_graphics    'Diamond 3.0 (Brandenburg, 2004)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'Sir97 (Giacovazzo et al., 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17563
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0551P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                5818
_reflns_number_total             7887
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om201182y_si_002.cif
_cod_data_source_block           crl84pe-2
_cod_database_code               4078415