Lithiation of the diaminopyridine protio-ligand MeC(2-C~5~H~4~N){CH~2~N(H)Mes}~2~ (Mes = 2,4,6-C~6~H~2~Me~3~)
Ward, Benjamin D.; Gade, Lutz H.; Mountford, Philip; Acta Crystallographica Section E 62 (2006) m472–m474; doi:10.1107/S1600536806004041

data_2208321
_publ_section_title
;
 Lithiation of the diaminopyridine protio-ligand
 MeC(2-C~5~H~4~N){CH~2~N(H)Mes}~2~ (Mes = 2,4,6-C~6~H~2~Me~3~)
;
_journal_coeditor_code           FL6217
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m472
_journal_page_last               m474
_journal_paper_doi               10.1107/S1600536806004041
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Li4 (C55 H64 N6) (C4 H10 O1)]'
_chemical_formula_moiety         'C59 H74 Li4 N6 O1'
_chemical_formula_sum            'C59 H74 Li4 N6 O'
_chemical_formula_weight         911.04
_chemical_name_systematic
;
(diethyl ether)(\m~4~-2-{6-[1,3-dimethyl-3-(2-pyridyl)-1,4-bis(2,4,6-
trimethylanilinio)butyl]-2-pyridyl}-2-methyl-1,3-bis(2,4,6-
trimethylanilinio)propane)tetralithium(I) diethyl ether solvate
;
_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
_cell_angle_alpha                78.18(3)
_cell_angle_beta                 72.68(3)
_cell_angle_gamma                80.31(3)
_cell_formula_units_Z            2
_cell_length_a                   11.607(2)
_cell_length_b                   14.302(3)
_cell_length_c                   17.477(4)
_cell_measurement_reflns_used    22654
_cell_measurement_temperature    173
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     2693.0(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>,  1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22654
_diffrn_reflns_theta_full        25.256
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         5.098
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         4760
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1479
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000236
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;w =
 [1-(F~o~-F~c~)^2^/36\s^2^(F)]^2^/[0.516T~o~(x)+0.342T~1~(x)+0.252T~2~(x)],
where
 T~i~ are the Chebychev polynomials and x = F~c~/F~max~
(Prince, 1982; Watkin,
 1994)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1378
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0537
_reflns_number_gt                4760
_reflns_number_total             12141
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            fl6217.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C59 H74 Li4 N6 O1'
_cod_database_code               2208321
_cod_database_fobs_code          2208321