Novel Six- and Eight-Membered Heterocycles. A Trithiadiazaphosphorinane and a Pentathiadiazaphosphocine
Bottle, S. E.; Bott, R. C.; Smith, G.; Wermuth, U. D.; Kennard, C. H. L.; Acta Crystallographica Section C 51 (1995) 2633–2637; doi:10.1107/S0108270195009188

data_2004285
_publ_section_title
;
 Novel Six- and Eight-Membered Heterocycles. A
 Trithiadiazaphosphorinane and a Pentathiadiazaphosphocine
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2633
_journal_page_last               2637
_journal_paper_doi               10.1107/S0108270195009188
_journal_volume                  51
_journal_year                    1995
_chemical_formula_sum            'C14 H23 N2 O P S3'
_chemical_formula_weight         362.5
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 114.24(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.002(3)
_cell_length_b                   9.0989(6)
_cell_length_c                   15.413(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      6
_cell_volume                     1790.5(6)
_computing_cell_refinement       MolEN
_computing_data_collection       'MolEN (Fair, 1990)'
_computing_data_reduction        'Xtal3.2 (Hall, Flack & Stewart, 1992)'
_computing_molecular_graphics    'PLATON92 (Spek, 1990)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.049
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_diffrn_reflns_limit_h_min       0
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_diffrn_reflns_limit_k_min       0
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_diffrn_reflns_limit_l_min       -18
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_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    none
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
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_refine_diff_density_min         -0.36
_refine_ls_extinction_method     none
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_refine_ls_R_factor_obs          0.0367
_refine_ls_shift/esd_max         0.1
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
w = 1/[\s^2^(F~o~^2^) + (0.0738P)^2^ + 0.99P]
where P = [max(F~o~^2^,0) + 2F~c~^2^]/3
;
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