New P–S–N containing ring systems. Reaction of 2,4-(naphthalene-1,8-diyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide and its 4-methoxynaphthalene derivative with hexamethyldisilazane
Kilián, Petr; Marek, Jaromír; Marek, Radek; Tou·ín, Jiøí; Humpa, Otakar; Novosad, Josef; Woollins, J. Derek; Journal of the Chemical Society, Dalton Transactions  (1998) 1175–; doi:10.1039/a708348c

data_7027961
_publ_section_title
;
 New P--S--N containing ring systems. Reaction of
 2,4-(naphthalene-1,8-diyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide and
 its 4-methoxynaphthalene derivative with hexamethyldisilazane
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1175
_journal_paper_doi               10.1039/a708348c
_journal_year                    1998
_chemical_formula_sum            'C13 H15 N P2 S3 Si'
_chemical_formula_weight         371.47
_chemical_melting_point          441.0(10)
_chemical_name_systematic
;
2,4-(naphthalene-1,8-diyl)-3-trimethyl
silyl-1,3,2,4-thiazadiphosphetidine-2,4-
disulfide
;
_space_group_IT_number           2
_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
_cell_angle_alpha                76.08(2)
_cell_angle_beta                 89.74(2)
_cell_angle_gamma                87.545(15)
_cell_formula_units_Z            4
_cell_length_a                   8.9437(15)
_cell_length_b                   11.490(2)
_cell_length_c                   17.165(4)
_cell_measurement_temperature    150.0(1)
_cell_volume                     1710.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(1)
_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  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6226
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.9050
_exptl_absorpt_correction_T_min  0.5499
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             768
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          1.00
_exptl_crystal_size_min          0.15
_refine_diff_density_max         .538
_refine_diff_density_min         -.544
_refine_diff_density_rms         .085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         6008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.884
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0939P)^2^+2.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                5112
_reflns_number_total             6008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c708348sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '440-442 K' was changed to
'441.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+2.4000P] 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^)+(0.0939P)^2^+2.4000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7027961