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_4304119
_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 H15 N2, 0.5(P2 Se8 2-)'
_chemical_formula_sum            'C8 H15 N2 P Se4'
_chemical_formula_weight         486.03
_chemical_melting_point          383
_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
_audit_author_name               'Schoen, Oliver; Rotter, Christiane'
_audit_block_code                cx040
_audit_creation_date             02-Mar-2007
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.211(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.66420(10)
_cell_length_b                   10.9948(2)
_cell_length_c                   17.0380(3)
_cell_measurement_reflns_used    7844
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1545
_cell_measurement_theta_min      3.6968
_cell_volume                     1435.41(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15990
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    10.308
_exptl_absorpt_correction_T_max  0.21
_exptl_absorpt_correction_T_min  0.1504
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.176
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0262P)^2^+4.6021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0763
_reflns_number_gt                2547
_reflns_number_total             3287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7015534-file001_3.cif
_cod_data_source_block           v1
_cod_database_code               4304119