New P–S–N containing ring systems. Reaction of 2,4-(naphthalene-1,8-diyl)-1,3,2,4-dithiadiphosphetane 2,4-disulfide with methylbis(trimethylsilyl)amine
Kilián, Petr; Marek, Jaromír; Marek, Radek; Tousek, Jaromír; Humpa, Otakar; Slawin, Alexandra M. Z.; Touzín, Jirí; Novosad, Josef; Woollins, J. Derek; Journal of the Chemical Society, Dalton Transactions  (1999) 2231–; doi:10.1039/a901698h

data_7027349
_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 with
 methylbis(trimethylsilyl)amine
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2231
_journal_paper_doi               10.1039/a901698h
_journal_year                    1999
_chemical_formula_sum            'C13 H12 N2 P2 S3'
_chemical_formula_weight         354.37
_chemical_melting_point          219.0(10)
_chemical_name_systematic
; 
 2,6-(naphthalene-1,8-diyl)-3,4-dimethyl-1,3,5,2,6-
 thiadiazadiphosphinine-2,6-disulfide 
;
_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_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.038(3)
_cell_length_b                   27.939(3)
_cell_length_c                   7.891(2)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      9
_cell_volume                     1506.8(8)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2888
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.693
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       needle
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.75
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_obs          0.0347
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0934
_refine_ls_wR_factor_obs         0.0874
_reflns_number_observed          2271
_reflns_number_total             2668
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901698hsup1.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '218-220' was changed to '219.0(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^)+(0.0400P)^2^+1.5000P] 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^)+(0.0400P)^2^+1.5000P] 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      P21/n
_cod_database_code               7027349