Intramolecular Amine-Induced [1,3]-Sigmatropic Rearrangement in the Reactions of Aminophosphinites or Phosphites with Elemental Sulfur or Selenium
Chandrasekaran, P.; Mague, Joel T.; Balakrishna, Maravanji S.; Inorganic Chemistry 45 (2006) 5893–5897; doi:10.1021/ic060413m

data_4332467
_publ_section_title
;
 Intramolecular Amine-Induced [1,3]-Sigmatropic Rearrangement in the
 Reactions of Aminophosphinites or Phosphites with Elemental Sulfur or
 Selenium
;
_journal_issue                   15
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5893
_journal_page_last               5897
_journal_paper_doi               10.1021/ic060413m
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C16 H38 N4 O2 P2 Se2'
_chemical_formula_sum            'C16 H38 N4 O2 P2 Se2'
_chemical_formula_weight         538.36
_chemical_name_systematic
; 
 {2-[1.3-di-tert-butyl-4-(2-dimethylaminoethylselanyl)
-2,4-dioxo-2\l^5^,4\l^5^-[1,2,3,4]diazphosphetidin-2-
ylselanyl]ethyl}dimethylamine 
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.505(2)
_cell_angle_beta                 93.929(2)
_cell_angle_gamma                104.507(2)
_cell_formula_units_Z            1
_cell_length_a                   6.7992(8)
_cell_length_b                   9.691(1)
_cell_length_c                   9.166(1)
_cell_measurement_reflns_used    4167
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.19
_cell_volume                     579.31(11)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0135
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5127
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    3.347
_exptl_absorpt_correction_T_max  0.7549
_exptl_absorpt_correction_T_min  0.6004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2671
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.3042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0630
_reflns_number_gt                2514
_reflns_number_total             2671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060413msup1.cif
_cod_data_source_block           msb171a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        579.3(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4332467