Structural and NMR Spectroscopic Investigations of Chair and Twist Conformers of the P2Se82- Anion
Christiane Rotter; Michael Schuster; Mustafa Kidik; Oliver Schön; Thomas M. Klapötke; Konstantin Karaghiosoff; Inorganic Chemistry 47 (2008) 1663–1673; doi:10.1021/ic7015534

data_4304120
_publ_section_title
;
Structural and NMR Spectroscopic Investigations of Chair and Twist
Conformers of the P2Se82- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1663
_journal_page_last               1673
_journal_paper_doi               10.1021/ic7015534
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C8 H12 Li N4, 0.5(p2 Se8)'
_chemical_formula_sum            'C8 H12 Li N4 P Se4'
_chemical_formula_weight         517.97
_chemical_melting_point          292
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           55
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2ab'
_symmetry_space_group_name_H-M   'P b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Schoen, Oliver; Rotter, Christiane'
_audit_block_code                bx300
_audit_creation_date             28-Feb-2007
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.0535(6)
_cell_length_b                   12.1200(5)
_cell_length_c                   15.0831(6)
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.0000
_cell_measurement_theta_min      3.7552
_cell_volume                     3665.9(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega    0.00  100.80   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000   70.0000    0.0000    0.0000    0.0000 144

  2 omega    0.00  100.80   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000   70.0000  120.0000    0.0000    0.0000 144

  3 omega    0.00  100.80   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000   70.0000  240.0000    0.0000    0.0000 144

  4 omega  -42.00   59.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -70.0000    0.0000    0.0000    0.0000 145

  5 omega  -42.00   59.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -70.0000  120.0000    0.0000    0.0000 145

  6 omega  -42.00   59.50   0.7000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       30.0000  -70.0000  240.0000    0.0000    0.0000 145

;
_diffrn_measurement_device_type  'Oxford diffraction X-calibur'
_diffrn_measurement_method       CCD
_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  0.1607
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35613
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    8.081
_exptl_absorpt_correction_T_max  0.1971
_exptl_absorpt_correction_T_min  0.0948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.535
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.364
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.364
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.1075
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+16.8724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1342
_reflns_number_gt                3427
_reflns_number_total             3732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7015534-file001_4.cif
_cod_data_source_block           v1
_cod_database_code               4304120