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_4078417
_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 11'
_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                95.988(3)
_cell_angle_beta                 105.581(3)
_cell_angle_gamma                97.631(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1573(4)
_cell_length_b                   12.5949(5)
_cell_length_c                   15.5090(7)
_cell_measurement_reflns_used    21517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      4.535
_cell_volume                     1873.76(14)
_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 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotaion 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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27843
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         4.60
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  0.9743
_exptl_absorpt_correction_T_min  0.9564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7873
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                5257
_reflns_number_total             7873
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om201182y_si_002.cif
_cod_data_source_block           nh297
_cod_original_cell_volume        1873.76(13)
_cod_database_code               4078417