Preparation and X-ray Structures of Alkali-Metal Derivatives of the Ambidentate Anions [tBuN(E)P(μ-NtBu)2P(E)NtBu]2- (E = S, Se) and [tBuN(Se)P(μ-NtBu)2PN(H)tBu)]-
Tristram Chivers; Mark Krahn; Masood Parvez; Gabriele Schatte; Inorganic Chemistry 40 (2001) 2547–2553; doi:10.1021/ic001093o

data_4319672
_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
;
 Preparation and X-ray Structures of Alkali-Metal Derivatives of the
 Ambidentate Anions [tBuN(E)P(\m-NtBu)2P(E)NtBu]2- (E = S, Se) and
 [tBuN(Se)P(\m-NtBu)2PN(H)tBu)]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2547
_journal_page_last               2553
_journal_paper_doi               10.1021/ic001093o
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '(C24 H53 Li1 N4 O2 P2 Se)2'
_chemical_formula_sum            'C48 H106 Li2 N8 O4 P4 Se2'
_chemical_formula_weight         1155.09
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 95.4216(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.901(2)
_cell_length_b                   10.1486(9)
_cell_length_c                   30.341(3)
_cell_measurement_reflns_used    5560
_cell_measurement_temperature    193(2)
_cell_volume                     6407.0(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  WinGX-1.63.02
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_sigmaI/netI    0.1023
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21397
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.13
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  0.7724
_exptl_absorpt_correction_T_min  0.7129
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; SADABS, V 2.01, Software for Area-Detector Absorption
  Corrections; Bruker AXS Inc., Madison, WI, 2000. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         9121
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0561
_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^+0.8917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                5355
_reflns_number_total             9121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001093o_4.cif
_cod_data_source_block           10
_cod_original_cell_volume        6407.2(10)
_cod_database_code               4319672