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_7012885
_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            'C45 H46'
_chemical_formula_weight         586.82
_chemical_name_common            penta(3,5-dimethylphenyl)cyclopentadiene
_chemical_name_systematic
; 
penta(3,5-dimethylphenyl)cyclopentadiene

;
_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                92.202(4)
_cell_angle_beta                 93.823(5)
_cell_angle_gamma                104.869(5)
_cell_formula_units_Z            2
_cell_length_a                   8.1689(19)
_cell_length_b                   12.805(3)
_cell_length_c                   17.290(4)
_cell_measurement_temperature    203(2)
_cell_volume                     1741.2(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8242
_diffrn_reflns_theta_full        23.34
_diffrn_reflns_theta_max         23.34
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.9925
_exptl_absorpt_correction_T_min  0.9845
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             632
_exptl_crystal_preparation
; 
crystallized from toluene 
;
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.323
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         4694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.323
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1350P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2286
_reflns_number_gt                3732
_reflns_number_total             4694
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302258g.txt
_cod_data_source_block           ccd5831
_cod_original_cell_volume        1741.3(7)
_cod_database_code               7012885