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_7114253
_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_compound_source        'synthesized by authors '
_chemical_formula_sum            'C30 H72 Li6 N8 P2 Si2'
_chemical_formula_weight         704.72
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.8927(4)
_cell_length_b                   14.8927(4)
_cell_length_c                   16.0178(6)
_cell_measurement_reflns_used    6543
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.0
_cell_volume                     3076.67(16)
_computing_cell_refinement       'HKL DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'TEXSAN (M. S. C., 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       ' \w & \f '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6937
_diffrn_reflns_theta_full        29.91
_diffrn_reflns_theta_max         29.91
_diffrn_reflns_theta_min         4.37
_diffrn_standards_decay_%        ' < 0.1 '
_exptl_absorpt_coefficient_mu    0.195
_exptl_absorpt_correction_T_max  0.9713
_exptl_absorpt_correction_T_min  0.9529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV: Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0727P)^2^+1.8196P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                1642
_reflns_number_total             1986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b207197e.txt
_cod_data_source_block           Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

2018-10-25
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C15 H36 Li3 N4 P Si'
_cod_original_formula_weight         352.36
_cod_original_formula_units_Z            6
_cod_original_cell_volume        3076.66(16)
_cod_original_sg_symbol_H-M      ' R -3 '
_cod_database_code               7114253