Cooperative cation and anion coordination by a bifunctional imidophosphorane ligand framework; syntheses and structures of [LiCl{ButNHP(μ-NBut)2PNH(2-py)}3] and [{ButNP(μ-NBut)2PN(2-py)} Li2·{Li(ButN)2P}]
Bond, Andrew D.; Doyle, Emma L.; Kidd, Sara J.; Woods, Anthony D.; Wright, Dominic S.; Chemical Communications  (2001) 777–; doi:10.1039/b010093p

data_7114955
_publ_section_title
;
 Cooperative cation and anion coordination by a bifunctional
 imidophosphorane ligand framework; syntheses and structures of
 [LiCl{ButNHP(\m-NBut)2PNH(2-py)}3] and [{ButNP(\m-NBut)2PN(2-py)}
 Li2&#x00B7;{Li(ButN)2P}]
;
_journal_issue                   8
_journal_name_full               'Chemical Communications'
_journal_page_first              777
_journal_paper_doi               10.1039/b010093p
_journal_year                    2001
_chemical_formula_moiety         'C51 H99 Cl Li N15 P6'
_chemical_formula_sum            'C51 H99 Cl Li N15 P6'
_chemical_formula_weight         1150.66
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   22.563(2)
_cell_length_b                   22.563(2)
_cell_length_c                   23.8030(10)
_cell_measurement_reflns_used    7772
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      1.00
_cell_volume                     10494.4(14)
_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    'SHELXS-97 (Sheldrick 1990)'
_diffrn_ambient_temperature      230(2)
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.1048
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12953
_diffrn_reflns_theta_max         26.70
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.233
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4928
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.1816
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+11.5676P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1763
_reflns_number_gt                2267
_reflns_number_total             4938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b010093p.txt
_cod_data_source_block           dw0048
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7114955