Syntheses and structures of an unsolvated tetrakisimidophosphate {Li3[P(NBut)3(NSiMe3)]}2 and the face-sharing double-cubane {Li2(THF)[P(O)(NBut)2(NHBut)]}2
Armstrong, Andrea; Chivers, Tristram; Krahn, Mark; Parvez, Masood; Schatte, Gabriele; Chemical Communications  (2002) 2332–; doi:10.1039/b207197e

data_7114252
_publ_section_title
;
 Syntheses and structures of an unsolvated tetrakisimidophosphate
 {Li3[P(NBut)3(NSiMe3)]}2 and the face-sharing double-cubane
 {Li2(THF)[P(O)(NBut)2(NHBut)]}2
;
_journal_issue                   20
_journal_name_full               'Chemical Communications'
_journal_page_first              2332
_journal_paper_doi               10.1039/b207197e
_journal_year                    2002
_chemical_formula_moiety         'C32 H72 Li4 N6 O4 P2'
_chemical_formula_sum            'C32 H72 Li4 N6 O4 P2'
_chemical_formula_weight         694.66
_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
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                103.906(2)
_cell_angle_beta                 92.088(2)
_cell_angle_gamma                119.424(2)
_cell_formula_units_Z            1
_cell_length_a                   10.3775(15)
_cell_length_b                   10.5873(16)
_cell_length_c                   11.5111(17)
_cell_measurement_reflns_used    3012
_cell_measurement_temperature    193(2)
_cell_volume                     1051.3(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5177
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  0.9766
_exptl_absorpt_correction_T_min  0.9302
_exptl_absorpt_correction_type   'Gaussian integration'
_exptl_absorpt_process_details
;
(a) Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182.
(b) Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) Acta Cryst.
18, 1035-1038.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.267
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0825P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                2837
_reflns_number_total             4223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207197e.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7114252