Synthesis and structure of the Li13 cage [[[O-P(mu-NtBu)]2Li2]3(LiCl)6Li(Cl/OnBu)0.5(thf)7], containing a [O-P(mu-NtBu)]2(2-) dianion.
Chan, Wesley Ting Kwok; Eisler, Dana; García, Felipe; Gonzalez-Calera, Silvia; McPartlin, Mary; Morey, James V; Mulvey, Robert E; Singh, Sanjay; Steiner, Alexander; Wright, Dominic S; Chemical communications (Cambridge, England)  (2008) 2251–2253; doi:10.1039/b800051d

data_7103111
_publ_section_title
;
 Synthesis and structure of the Li13 cage
 [[[O-P(mu-NtBu)]2Li2]3(LiCl)6Li(Cl/OnBu)0.5(thf)7], containing a
 [O-P(mu-NtBu)]2(2-) dianion.
;
_journal_issue                   19
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2251
_journal_page_last               2253
_journal_paper_doi               10.1039/b800051d
_journal_year                    2008
_chemical_formula_sum            'C55 H116.5 Cl6.5 Li13 N6 O13.75 P6'
_chemical_formula_weight         1588.51
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.906(4)
_cell_length_b                   21.982(4)
_cell_length_c                   39.230(8)
_cell_measurement_temperature    180(2)
_cell_volume                     17166(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_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  0.0830
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            77200
_diffrn_reflns_theta_full        23.53
_diffrn_reflns_theta_max         23.53
_diffrn_reflns_theta_min         5.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.9243
_exptl_absorpt_correction_T_min  0.8720
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6704
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.00038(12)
_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   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     890
_refine_ls_number_reflns         12471
_refine_ls_number_restraints     2064
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+38.9028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1853
_reflns_number_gt                7875
_reflns_number_total             12471
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b800051d.txt
_cod_data_source_block           dw0760
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C55 H116.50 Cl6.50 Li13 N6 O13.75 P6'
_cod_database_code               7103111