Lithiation of (tBuNH)3PNSiMe3 and Formation of Tetraimidophosphate Complexes Containing M3O3 Rings (M = Li, K): X-ray Structure of the Stable Radical {(Me3SiN)P(μ3-NtBu)3[μ3-Li(THF)]3(OtBu)}
Andrea Armstrong; Tristram Chivers; Masood Parvez; Gabriele Schatte; René T. Boeré; Inorganic Chemistry 43 (2004) 3453–3460; doi:10.1021/ic035377v

data_4311050
_publ_contact_author_address
; Department of Chemistry

   University of Calgary

   Calgary Alberta T2N 1N4

   Canada

;
_publ_contact_author_email       chivers@ucalgary.ca
_publ_contact_author_fax         '001 403 289 9488'
_publ_contact_author_name        'Dr Tristram Chivers'
_publ_contact_author_phone       '001 403 220 5741'
_publ_section_title
;
 Lithiation of (tBuNH)3PNSiMe3 and Formation of Tetraimidophosphate
 Complexes Containing M3O3 Rings (M = Li, K): X-ray Structure of the
 Stable Radical {(Me3SiN)P(\m3-NtBu)3[\m3-Li(THF)]3(OtBu)}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3453
_journal_page_last               3460
_journal_paper_doi               10.1021/ic035377v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C30 H76 Li2 N8 P2 Si2'
_chemical_formula_sum            'C30 H76 Li2 N8 P2 Si2'
_chemical_formula_weight         680.99
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4399(3)
_cell_length_b                   15.7195(5)
_cell_length_c                   20.3644(5)
_cell_measurement_reflns_used    4165
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      1
_cell_volume                     4302.4(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
; HKL Denzo and Scalepack (Otwinowski & Minor 1997)

;
_computing_molecular_graphics    'Diamond 2.1 (Brandenburg, 2000)'
_computing_publication_material  'Diamond 2.1 (Brandenburg, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device_type  'KappaCCD (Nonius, FR540C)'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0713
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7522
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.00
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.9639
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.051
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.55(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0600P)^2^+1.4500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                5818
_reflns_number_total             7522
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035377vsi20031201_030051.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4311050