Selenium Imides: 77Se NMR Investigations of the SeCl2-tBuNH2 Reaction and X-ray Structures of Se3(NtBu)3, tBuNSe(μ-NtBu)2SO2, and tBuNSe(μ-NtBu)2SeO
Tiina Maaninen; Tristram Chivers; Risto Laitinen; Gabriele Schatte; Maija Nissinen; Inorganic Chemistry 39 (2000) 5341–5347; doi:10.1021/ic000598b

data_4321566
_publ_section_title
;
 Selenium Imides: 77Se NMR Investigations of the SeCl2-tBuNH2 Reaction and
 X-ray Structures of Se3(NtBu)3, tBuNSe(\m-NtBu)2SO2, and
 tBuNSe(\m-NtBu)2SeO
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5341
_journal_page_last               5347
_journal_paper_doi               10.1021/ic000598b
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         'C8 H18 N2 Se2'
_chemical_formula_sum            'C8 H18 N2 Se2'
_chemical_formula_weight         300.16
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   9.8660(3)
_cell_length_b                   9.8660(3)
_cell_length_c                   20.8427(7)
_cell_measurement_temperature    293(2)
_cell_volume                     1756.98(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.850
_diffrn_measured_fraction_theta_max 0.850
_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  0.0889
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7094
_diffrn_reflns_theta_full        27.84
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    6.271
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_meas      0.3
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       0.0048(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   0.322
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.322
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+106.5361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                1215
_reflns_number_total             1403
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000598b_1.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+106.5361P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1091P)^2^+106.5361P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 3 c 1'
_cod_database_code               4321566