Synthesis and Structures of Aluminum and Magnesium Complexes of Tetraimidophosphates and Trisamidothiophosphates: EPR and DFT Investigations of the Persistent Neutral Radicals {Me2Al[(μ-NR)(μ-NtBu)P(μ-NtBu)2]Li(THF)2}. (R = SiMe3,tBu)
Andrea Armstrong; Tristram Chivers; Heikki M. Tuononen; Masood Parvez; Inorganic Chemistry 44 (2005) 5778–5788; doi:10.1021/ic050689e

data_4309382
_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
;
Synthesis and Structures of Aluminum and Magnesium Complexes of
Tetraimidophosphates and Trisamidothiophosphates: EPR and DFT
Investigations of the Persistent Neutral Radicals
{Me2Al[(\m-NR)(\m-NtBu)P(\m-NtBu)2]Li(THF)2}. (R = SiMe3,tBu)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5778
_journal_page_last               5788
_journal_paper_doi               10.1021/ic050689e
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H100 Mg3 N9 O4 P3 S3'
_chemical_formula_weight         1033.31
_chemical_name_systematic
; 
 ? 
;
_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                96.188(14)
_cell_angle_beta                 102.701(16)
_cell_angle_gamma                117.474(14)
_cell_formula_units_Z            2
_cell_length_a                   14.993(4)
_cell_length_b                   15.285(4)
_cell_length_c                   15.535(4)
_cell_measurement_reflns_used    24468
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.8
_cell_volume                     2989.9(15)
_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_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24468
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  0.9466
_exptl_absorpt_correction_T_min  0.9364
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.661
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         13502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0500P)^2^+2.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                10269
_reflns_number_total             13502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050689esi20050503_114345_3.cif
_cod_data_source_block           Compound18
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_original_cell_volume        2989.9(14)
_cod_database_code               4309382