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_4319669
_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         'C28 H60 K2 N4 O3 P2 Se2'
_chemical_formula_sum            'C28 H60 K2 N4 O3 P2 Se2'
_chemical_formula_weight         798.86
_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                 90.99(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.733(11)
_cell_length_b                   14.085(10)
_cell_length_c                   26.138(9)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      21.05
_cell_measurement_theta_min      18.20
_cell_volume                     3951(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_molecular_graphics    'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_detector       'scintillation counter'
_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  0.120
_diffrn_reflns_av_sigmaI/netI    0.336
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            6958
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        3.2
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.194
_exptl_absorpt_correction_T_max  0.6680
_exptl_absorpt_correction_T_min  0.4067
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
 North,Phillips & Matthews, 1968
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       0.0025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.2959
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0744P)^2^+9.9743P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.2380
_reflns_number_gt                2135
_reflns_number_total             6958
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001093o_1.cif
_cod_data_source_block           12b
_cod_database_code               4319669