Synthesis and structure of a new macrotricyclic ligand that encapsulates lithium and transition metal ions
Barclay, Tosha M.; McAuley, Alex; Subramanian, S.; Chemical Communications  (2002) 170–; doi:10.1039/b109793h

data_7114088
_publ_section_title
;
 Synthesis and structure of a new macrotricyclic ligand that encapsulates
 lithium and transition metal ions
;
_journal_issue                   2
_journal_name_full               'Chemical Communications'
_journal_page_first              170
_journal_paper_doi               10.1039/b109793h
_journal_year                    2002
_chemical_formula_sum            'C18 H38 Cl2 N4 O8 S2'
_chemical_formula_weight         573.54
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.364(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.408(2)
_cell_length_b                   16.534(5)
_cell_length_c                   10.412(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1264.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6459
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.473
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0680P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                1284
_reflns_number_total             2230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109793h.txt
_cod_data_source_block           for_[H2L3](ClO4)2
_cod_original_cell_volume        1264.8(7)
_cod_database_code               7114088