Synthesis and structure of the novel mixed anion‒dianion lithium cage compound [(6-LiCH2Py-2-OLi)4(6-CH3Py-2-OLi)2(THF)9]
Liddle, Stephen T.; Clegg, William; Chemical Communications  (2001) 1584–; doi:10.1039/b104680m

data_7115047
_publ_section_title
;
 Synthesis and structure of the novel mixed anion--dianion lithium cage
 compound [(6-LiCH2Py-2-OLi)4(6-CH3Py-2-OLi)2(THF)9]
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1584
_journal_paper_doi               10.1039/b104680m
_journal_year                    2001
_chemical_formula_sum            'C80 H120 Li10 N6 O17'
_chemical_formula_weight         1507.22
_chemical_name_systematic
;
?
;
_space_group_IT_number           1
_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                106.1560(10)
_cell_angle_beta                 99.760(2)
_cell_angle_gamma                104.4510(10)
_cell_formula_units_Z            1
_cell_length_a                   12.1861(12)
_cell_length_b                   13.4120(12)
_cell_length_c                   14.5875(14)
_cell_measurement_reflns_used    6323
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.58
_cell_volume                     2143.1(4)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.1062
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13722
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7272
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_coef       0.0000(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         12522
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.576
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0930
_refine_ls_shift/su_max          7.800
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2103
_reflns_number_gt                9624
_reflns_number_total             12522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104680m.txt
_cod_data_source_block           stl36
_cod_original_sg_symbol_H-M      P1
_cod_database_code               7115047