#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:36:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179979 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/73/7027347.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027347
loop_
_publ_author_name
'Kilián, Petr'
'Marek, Jaromír'
'Marek, Radek'
'Tousek, Jaromír'
'Humpa, Otakar'
'Slawin, Alexandra M. Z.'
'Touzín, Jirí'
'Novosad, Josef'
'Woollins, J. Derek'
_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            'C17 H27 N P2 S4 Si2'
_chemical_formula_weight         491.76
_chemical_melting_point          156-8
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_alpha                105.81(2)
_cell_angle_beta                 93.25(2)
_cell_angle_gamma                100.94(2)
_cell_formula_units_Z            2
_cell_length_a                   7.178(2)
_cell_length_b                   10.502(3)
_cell_length_c                   17.184(5)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     1215.6(6)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(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  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4439
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.625
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       needle
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.018
_refine_ls_goodness_of_fit_obs   1.034
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_restrained_S_obs      1.034
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0730P)²+1.3088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1232
_refine_ls_wR_factor_obs         0.1140
_reflns_number_observed          3609
_reflns_number_total             4289
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901698hsup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+1.3088P] 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^)+(0.0730P)^2^+1.3088P] 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      P-1
_cod_database_code               7027347
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
S1 S 0.10083(12) 0.30752(7) 0.35061(5) 0.0304(2) Uani 1 d
S1' S 0.45301(10) 0.14533(7) 0.28074(5) 0.0292(2) Uani 1 d
S19 S -0.02187(10) -0.00422(7) 0.24119(4) 0.02187(18) Uani 1 d
S9 S -0.14619(11) -0.32802(7) 0.17301(5) 0.0312(2) Uani 1 d
P1 P 0.18950(10) 0.13944(7) 0.32467(4) 0.02005(18) Uani 1 d
P9 P 0.06757(10) -0.18656(7) 0.23398(4) 0.01907(18) Uani 1 d
Si1 Si 0.50522(13) 0.32036(8) 0.23318(5) 0.0298(2) Uani 1 d
Si9 Si 0.28288(11) -0.21691(8) 0.08600(5) 0.0250(2) Uani 1 d
N9 N 0.2707(3) -0.1860(2) 0.19343(13) 0.0223(5) Uani 1 d
C1 C 0.2190(4) 0.0721(3) 0.41037(16) 0.0198(5) Uani 1 d
C2 C 0.2798(4) 0.1728(3) 0.48291(19) 0.0272(6) Uani 1 d
C3 C 0.3097(4) 0.1444(3) 0.55651(19) 0.0295(7) Uani 1 d
C4 C 0.2798(4) 0.0143(3) 0.55794(17) 0.0274(6) Uani 1 d
C5 C 0.2185(4) -0.0935(3) 0.48563(17) 0.0226(6) Uani 1 d
C10 C 0.1843(4) -0.0681(3) 0.40845(16) 0.0197(5) Uani 1 d
C9 C 0.1183(4) -0.1839(3) 0.33923(17) 0.0211(6) Uani 1 d
C8 C 0.0891(5) -0.3126(3) 0.3489(2) 0.0322(7) Uani 1 d
C7 C 0.1253(6) -0.3345(3) 0.4243(2) 0.0371(8) Uani 1 d
C6 C 0.1885(5) -0.2269(3) 0.4910(2) 0.0326(7) Uani 1 d
C11 C 0.4403(5) -0.1960(4) 0.2396(2) 0.0302(7) Uani 1 d
C12 C 0.2742(7) -0.3997(4) 0.0415(2) 0.0433(9) Uani 1 d
C13 C 0.5186(5) -0.1189(4) 0.0744(2) 0.0396(8) Uani 1 d
C14 C 0.0917(6) -0.1583(6) 0.0378(2) 0.0486(10) Uani 1 d
C15 C 0.7178(5) 0.2895(4) 0.1801(2) 0.0366(8) Uani 1 d
C17 C 0.5689(8) 0.4779(4) 0.3176(3) 0.0600(14) Uani 1 d
C16 C 0.3021(8) 0.3133(8) 0.1598(4) 0.0675(16) Uani 1 d
H2 H 0.2978(49) 0.2499(37) 0.4841(21) 0.028(9) Uiso 1 d
H3 H 0.3556(54) 0.2161(40) 0.6055(24) 0.041(10) Uiso 1 d
H4 H 0.2936(46) -0.0163(33) 0.6056(20) 0.026(8) Uiso 1 d
H8 H 0.0322(54) -0.3928(40) 0.2987(24) 0.043(10) Uiso 1 d
H9 H 0.1133(63) -0.4183(46) 0.4297(27) 0.059(13) Uiso 1 d
H10 H 0.2225(53) -0.2400(37) 0.5455(23) 0.040(10) Uiso 1 d
H11A H 0.4588(66) -0.1461(48) 0.2918(31) 0.061(13) Uiso 1 d
H11B H 0.5424(84) -0.1671(56) 0.2199(34) 0.085(17) Uiso 1 d
H11C H 0.4447(80) -0.2876(62) 0.2305(34) 0.088(18) Uiso 1 d
H12A H 0.2502(80) -0.4177(56) -0.0105(38) 0.083(17) Uiso 1 d
H12B H 0.3876(69) -0.4294(45) 0.0614(27) 0.058(13) Uiso 1 d
H12C H 0.1527(96) -0.4411(62) 0.0470(37) 0.102(21) Uiso 1 d
H13A H 0.6053(70) -0.1553(49) 0.0921(29) 0.065(15) Uiso 1 d
H13B H 0.5213(62) -0.1237(44) 0.0239(29) 0.053(12) Uiso 1 d
H13C H 0.5465(93) -0.0114(71) 0.1067(40) 0.119(23) Uiso 1 d
H14A H 0.0882(72) -0.0793(53) 0.0666(32) 0.066(16) Uiso 1 d
H14B H 0.0937(68) -0.1684(49) -0.0141(33) 0.067(14) Uiso 1 d
H14C H -0.0300(89) -0.2083(57) 0.0352(34) 0.086(18) Uiso 1 d
H15A H 0.7647(76) 0.3716(56) 0.1658(32) 0.082(16) Uiso 1 d
H15B H 0.6878(66) 0.2152(50) 0.1316(30) 0.064(13) Uiso 1 d
H15C H 0.8182(59) 0.2718(41) 0.2172(25) 0.048(11) Uiso 1 d
H16A H 0.6380(103) 0.5462(74) 0.2994(43) 0.126(24) Uiso 1 d
H16B H 0.4658(74) 0.4963(47) 0.3428(30) 0.066(14) Uiso 1 d
H16C H 0.6599(71) 0.4707(49) 0.3547(31) 0.061(16) Uiso 1 d
H17A H 0.3491(88) 0.3769(64) 0.1303(39) 0.100(19) Uiso 1 d
H17B H 0.2284(126) 0.3397(85) 0.1865(52) 0.138(32) Uiso 1 d
H17C H 0.2522(135) 0.2350(96) 0.1261(57) 0.165(43) Uiso 1 d
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
P1 S1' Si1 106.29(5)
P1 S19 P9 102.73(4)
C1 P1 S1 114.48(10)
C1 P1 S1' 102.61(9)
S1 P1 S1' 116.28(5)
C1 P1 S19 105.89(9)
S1 P1 S19 106.58(5)
S1' P1 S19 110.59(5)
N9 P9 C9 106.88(12)
N9 P9 S9 115.08(9)
C9 P9 S9 114.57(10)
N9 P9 S19 110.38(9)
C9 P9 S19 104.63(9)
S9 P9 S19 104.79(5)
C17 Si1 C16 114.4(3)
C17 Si1 C15 110.1(2)
C16 Si1 C15 110.7(2)
C17 Si1 S1' 110.12(18)
C16 Si1 S1' 110.8(2)
C15 Si1 S1' 99.76(12)
N9 Si9 C14 111.41(15)
N9 Si9 C12 107.90(16)
C14 Si9 C12 112.8(2)
N9 Si9 C13 106.52(15)
C14 Si9 C13 109.1(2)
C12 Si9 C13 109.0(2)
C11 N9 P9 120.32(19)
C11 N9 Si9 115.12(19)
P9 N9 Si9 122.67(14)
C2 C1 C10 120.5(3)
C2 C1 P1 112.5(2)
C10 C1 P1 127.0(2)
C1 C2 C3 122.3(3)
C4 C3 C2 119.5(3)
C3 C4 C5 120.9(3)
C6 C5 C4 118.3(3)
C6 C5 C10 120.5(3)
C4 C5 C10 121.2(3)
C9 C10 C1 127.5(2)
C9 C10 C5 116.9(2)
C1 C10 C5 115.6(2)
C8 C9 C10 119.8(3)
C8 C9 P9 112.5(2)
C10 C9 P9 127.7(2)
C9 C8 C7 122.2(3)
C6 C7 C8 119.5(3)
C7 C6 C5 121.2(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 P1 1.9363(11)
S1' P1 2.0722(11)
S1' Si1 2.1862(12)
S19 P1 2.0835(12)
S19 P9 2.1073(11)
S9 P9 1.9399(12)
P1 C1 1.8175(27)
P9 N9 1.6508(24)
P9 C9 1.8162(29)
Si1 C17 1.8384(44)
Si1 C16 1.8500(51)
Si1 C15 1.8572(35)
Si9 N9 1.7953(23)
Si9 C14 1.8487(38)
Si9 C12 1.8506(38)
Si9 C13 1.8579(36)
N9 C11 1.4521(40)
C1 C2 1.3809(41)
C1 C10 1.4363(37)
C2 C3 1.3903(45)
C3 C4 1.3499(45)
C4 C5 1.4147(42)
C5 C6 1.4060(42)
C5 C10 1.4394(38)
C10 C9 1.4313(39)
C9 C8 1.3841(40)
C8 C7 1.3948(47)
C7 C6 1.3561(49)
