Fluorenylidene-Functionalized Lithium Phosphonium Di- and Triylides
Schröder, Fabian G.; Sundermeyer, Jörg; Organometallics 34 (2015) 1017–1020; doi:10.1021/om501325h

data_4085590
_publ_section_title
;
 Fluorenylidene-Functionalized Lithium Phosphonium Di- and Triylides
;
_journal_coden_ASTM              ORGND7
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1017
_journal_page_last               1020
_journal_paper_doi               10.1021/om501325h
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C40 H50 Li4 O2 P2'
_chemical_formula_sum            'C40 H50 Li4 O2 P2'
_chemical_formula_weight         652.50
_chemical_name_common            'compound 4'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.339(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2904(4)
_cell_length_b                   23.4831(15)
_cell_length_c                   9.8369(5)
_cell_measurement_reflns_used    4494
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.375
_cell_measurement_theta_min      25.795
_cell_volume                     1795.69(18)
_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    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_sigmaI/netI    0.1732
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14701
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  0.9908
_exptl_absorpt_correction_T_min  0.9683
_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    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.652
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.652
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0599
_reflns_number_gt                1800
_reflns_number_total             3806
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om501325h_si_002.cif
_cod_data_source_block           cpd4
_cod_depositor_comments
'Adding full bibliography for 4085587--4085590.cif.'
_cod_original_cell_volume        1795.69(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4085590