Synthesis, structure and solution dynamics of lithium salts of superbulky cyclopentadienyl ligands
Giesbrecht, Garth R.; Gordon, John C.; Clark, David L.; Scott, Brian L.; Dalton Transactions  (2003) 2658–; doi:10.1039/b302258g

data_7012884
_publ_section_title
;
 Synthesis, structure and solution dynamics of lithium salts of
 superbulky cyclopentadienyl ligands
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              2658
_journal_paper_doi               10.1039/b302258g
_journal_year                    2003
_chemical_formula_sum            'C98 H106 Li2 O2'
_chemical_formula_weight         1329.71
_chemical_name_common
;
((lithium)bis(penta(3,5-dimethylphenyl)cyclopentadienide)
(lithium(tetrahydrofuran))(tetrahydrofuran)
;
_chemical_name_systematic
; 
[(lithium)bis(penta(3,5-dimethylphenyl)cyclopentadienide]
[lithium(tetrahydrofuran)](tetrahydrofuran)
;
_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                97.393(4)
_cell_angle_beta                 102.993(5)
_cell_angle_gamma                96.523(4)
_cell_formula_units_Z            2
_cell_length_a                   13.997(4)
_cell_length_b                   15.486(4)
_cell_length_c                   20.198(5)
_cell_measurement_temperature    203(2)
_cell_volume                     4184.2(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20273
_diffrn_reflns_theta_full        22.46
_diffrn_reflns_theta_max         22.46
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_correction_T_min  0.9804
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1432
_exptl_crystal_preparation
;
crystallized from toluene
;
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.817
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.305
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         10298
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.305
_refine_ls_R_factor_all          0.1380
_refine_ls_R_factor_gt           0.0933
_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^)+(0.1284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2534
_refine_ls_wR_factor_ref         0.2726
_reflns_number_gt                6519
_reflns_number_total             10298
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302258g.txt
_cod_data_source_block           ccd582s
_cod_original_cell_volume        4184.2(18)
_cod_database_code               7012884