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_4321568
_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_sum            'C12 H27 N3 O Se2'
_chemical_formula_weight         387.29
_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                99.320(3)
_cell_angle_beta                 95.764(3)
_cell_angle_gamma                103.876(3)
_cell_formula_units_Z            2
_cell_length_a                   6.3720(10)
_cell_length_b                   9.926(2)
_cell_length_c                   14.034(3)
_cell_measurement_temperature    293(2)
_cell_volume                     841.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15430
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    4.390
_exptl_absorpt_correction_T_max  0.439
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   'Phi scan'
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.886
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       0.014(3)
_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   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2962
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+4.2169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                2834
_reflns_number_total             2962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000598b_3.cif
_cod_data_source_block           8
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+4.2169P] 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^)+(0.0674P)^2^+4.2169P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4321568