Synthesis and structure of [(ButN)P(μ-NBut)2P(PCy)Li2·thf]2; an unusual cage compound containing an amido/phosphido functionalised [(ButN)P(μ-NBut)2P(PCy)]2− dianion (Cy = C6H11)
Bashall, Alan; McPartlin, Mary; Elvidge, Benjamin R.; Beswick, Michael A.; Kidd, Sara J.; Wright, Dominic S.; Chemical Communications  (2000) 1439–; doi:10.1039/b003468l

data_7110994
_publ_section_title
;
 Synthesis and structure of [(ButN)P(\m-NBut)2P(PCy)Li2&#x00B7;thf]2; an
 unusual cage compound containing an amido/phosphido functionalised
 [(ButN)P(\m-NBut)2P(PCy)]2&#x2212; dianion (Cy = C6H11)
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1439
_journal_paper_doi               10.1039/b003468l
_journal_year                    2000
_chemical_formula_sum            'C24 H50 Li2 N3 O1.5 P3'
_chemical_formula_weight         511.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 95.46(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.679(2)
_cell_length_b                   21.224(8)
_cell_length_c                   13.847(3)
_cell_measurement_temperature    223(2)
_cell_volume                     3124.2(15)
_computing_cell_refinement       'Bruker XSCANS '
_computing_data_collection       'Bruker XSCANS '
_computing_data_reduction        'Bruker XSCANS '
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       theta/2theta
_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  0.0749
_diffrn_reflns_av_sigmaI/netI    0.1161
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4884
_diffrn_reflns_theta_full        22.00
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.92
_diffrn_standards_decay_%        0.2
_diffrn_standards_interval_count 93
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         3836
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1543
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          1.995
_refine_ls_shift/su_mean         0.101
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2419
_reflns_number_gt                1761
_reflns_number_total             3836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003468lsup1.cif
_cod_data_source_block           tx420
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3124.0(15)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C24 H50 Li2 N3 O1.50 P3'
_cod_database_code               7110994