Characterization of Cyclopentyllithium and Cyclopentyllithium Tetrahydrofuran Complex
Chicheung Su; Russell Hopson; Paul G. Williard; Journal of the American Chemical Society 135 (2013) 12400–12406; doi:10.1021/ja4059102

data_4120333
_publ_section_title
;
 Characterization of Cyclopentyllithium and Cyclopentyllithium
 Tetrahydrofuran Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12400
_journal_page_last               12406
_journal_paper_doi               10.1021/ja4059102
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C9 H17 Li O'
_chemical_formula_weight         148.16
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.8947(7)
_cell_length_b                   18.8947(7)
_cell_length_c                   10.2755(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3668.5(2)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.470
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.470
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5040
_diffrn_reflns_point_group_measured_fraction_full 0.470
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         19.367
_diffrn_reflns_theta_min         2.156
_exptl_absorpt_coefficient_mu    0.065
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.152
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1428P)^2^+11.9077P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2360
_refine_ls_wR_factor_ref         0.2431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                699
_reflns_number_total             784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4059102_si_003.cif
_cod_data_source_block           ccs21jun12_0m_a
_cod_original_cell_volume        3668.5(3)
_cod_database_code               4120333
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.987
_shelxl_version_number           2013-2
_shelx_res_checksum              88325