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_4304117
_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         'C20 H20 Li N4, 0.5(P2 Se8)'
_chemical_formula_sum            'C20 H20 Li N4 P Se4'
_chemical_formula_weight         670.15
_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           SHELXL-97
_cell_angle_alpha                95.271(6)
_cell_angle_beta                 94.847(6)
_cell_angle_gamma                114.219(7)
_cell_formula_units_Z            2
_cell_length_a                   10.1582(8)
_cell_length_b                   10.7716(8)
_cell_length_c                   12.7499(10)
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.9968
_cell_measurement_theta_min      3.9728
_cell_volume                     1255.41(18)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0792
_diffrn_reflns_av_sigmaI/netI    0.1587
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17142
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.98
_exptl_absorpt_coefficient_mu    5.922
_exptl_absorpt_correction_T_max  0.742656
_exptl_absorpt_correction_T_min  0.494912
_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            rod
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         7312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1739
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0083P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0802
_reflns_number_gt                2885
_reflns_number_total             7312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7015534-file001_1.cif
_cod_data_source_block           v1
_cod_original_cell_volume        1255.40(17)
_cod_database_code               4304117