#------------------------------------------------------------------------------
#$Date: 2025-08-20 17:59:05 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301833 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/67/4116712.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4116712
loop_
_publ_author_name
'Derek P. Gates'
'Mark Edwards'
'Louise M. Liable-Sands'
'Arnold L. Rheingold'
'Ian Manners'
_publ_contact_author
;
     Dr. Ian Manners
     Chemistry Department
     University of Toronto
     80 St. George Street
     Toronto, Ontario M5S 3H6
     Canada
;
_publ_contact_author_email       imanners@alchemy.chem.utoronto.ca
_publ_contact_author_fax         '416 978 6157'
_publ_contact_author_phone       '416 978 3566'
_publ_section_title
;
 Attempted Generation of the Thionylphosphazene Cation [NSO(NPCl2)2]+:
 Novel Reactivity and the Discovery of an Ambient Temperature Ring-Opening
 Polymerization Route to Poly(thionylphosphazenes)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3249
_journal_page_last               3250
_journal_paper_doi               10.1021/ja9740475
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C4 H6 B Cl4 F6 N3 O6 P2 S2'
_chemical_formula_weight         584.79
_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                71.576(10)
_cell_angle_beta                 62.702(5)
_cell_angle_gamma                77.082(8)
_cell_formula_units_Z            4
_cell_length_a                   12.9815(12)
_cell_length_b                   13.6426(12)
_cell_length_c                   14.1406(15)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     2102.2(4)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5228
_diffrn_reflns_theta_max         23.38
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.992
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.848
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.439
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0084(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.977
_refine_ls_goodness_of_fit_obs   1.063
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         4465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_restrained_S_obs      1.063
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_obs          0.0521
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1242P)²+0.3071P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1786
_refine_ls_wR_factor_obs         0.1524
_reflns_number_observed          3321
_reflns_number_total             4472
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9740475.cif
_cod_data_source_block           ianl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1242P)^2^+0.3071P] 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^)+(0.1242P)^2^+0.3071P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2102.2(3)
_cod_database_code               4116712
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
_atom_site_refinement_flags
S1 S 0.3072(2) 0.88433(13) 0.29218(15) 0.0595(5) Uani 1 d .
S2 S 0.7093(2) 0.9081(2) 0.2775(2) 0.0852(7) Uani 1 d .
P1 P 0.47336(14) 0.68402(13) 0.47233(12) 0.0462(5) Uani 1 d .
P2 P 0.58483(13) 0.64489(12) 0.26655(12) 0.0429(5) Uani 1 d .
Cl1 Cl 0.5485(2) 0.6559(2) 0.5729(2) 0.0851(7) Uani 1 d .
Cl2 Cl 0.3135(2) 0.6505(2) 0.57541(15) 0.0758(6) Uani 1 d .
Cl3 Cl 0.74862(14) 0.58586(15) 0.20430(15) 0.0696(6) Uani 1 d .
Cl4 Cl 0.5130(2) 0.57854(14) 0.20828(15) 0.0681(6) Uani 1 d .
N1 N 0.4728(4) 0.8043(4) 0.4100(4) 0.0504(13) Uani 1 d .
N2 N 0.5769(4) 0.7666(4) 0.2188(4) 0.0462(13) Uani 1 d .
N3 N 0.5320(4) 0.6110(4) 0.3935(4) 0.0513(13) Uani 1 d .
B B 0.5221(6) 0.8464(5) 0.2867(6) 0.048(2) Uani 1 d .
C1 C 0.4196(7) 0.8824(6) 0.4801(6) 0.079(2) Uani 1 d .
H1A H 0.3913(7) 0.8463(6) 0.5563(6) 0.118 Uiso 1 calc R
H1B H 0.3563(7) 0.9244(6) 0.4651(6) 0.118 Uiso 1 calc R
H1C H 0.4777(7) 0.9259(6) 0.4631(6) 0.118 Uiso 1 calc R
C2 C 0.6203(7) 0.8071(6) 0.0976(5) 0.070(2) Uani 1 d .
H2A H 0.6532(7) 0.7503(6) 0.0631(5) 0.105 Uiso 1 calc R
H2B H 0.6789(7) 0.8532(6) 0.0720(5) 0.105 Uiso 1 calc R
H2C H 0.5569(7) 0.8440(6) 0.0796(5) 0.105 Uiso 1 calc R
C3 C 0.2840(9) 0.9499(8) 0.1679(8) 0.092(3) Uani 1 d .
C4 C 0.8188(9) 0.9610(10) 0.1421(12) 0.123(4) Uani 1 d .
O1 O 0.4272(4) 0.9166(3) 0.2552(3) 0.0536(11) Uani 1 d .
O2 O 0.2199(4) 0.9324(4) 0.3743(4) 0.086(2) Uani 1 d .
O3 O 0.3105(4) 0.7768(3) 0.3060(5) 0.078(2) Uani 1 d .
O4 O 0.6057(4) 0.9257(3) 0.2494(4) 0.0589(12) Uani 1 d .
O5 O 0.6954(6) 0.9756(8) 0.3406(7) 0.168(4) Uani 1 d .
O6 O 0.7469(6) 0.8003(5) 0.3043(7) 0.125(2) Uani 1 d .
F1 F 0.3641(6) 0.9193(6) 0.0846(5) 0.145(3) Uani 1 d .
F2 F 0.1816(6) 0.9286(5) 0.1851(6) 0.148(2) Uani 1 d .
F3 F 0.2833(5) 1.0507(4) 0.1497(4) 0.116(2) Uani 1 d .
F4 F 0.7889(7) 1.0574(8) 0.1052(8) 0.207(4) Uani 1 d .
F5 F 0.9153(5) 0.9588(6) 0.1525(7) 0.177(3) Uani 1 d .
F6 F 0.8358(7) 0.9094(10) 0.0766(7) 0.214(5) Uani 1 d .
S1' S -0.0129(2) 0.6707(2) 0.8508(2) 0.0720(6) Uani 1 d .
S2' S -0.4150(2) 0.6690(2) 0.8523(2) 0.0694(6) Uani 1 d .
P1' P -0.07322(14) 0.63116(14) 0.58755(13) 0.0495(5) Uani 1 d .
P2' P -0.12396(14) 0.46075(13) 0.76525(14) 0.0473(5) Uani 1 d .
Cl1' Cl -0.1492(2) 0.6715(2) 0.4861(2) 0.0830(7) Uani 1 d .
Cl2' Cl 0.0865(2) 0.6685(2) 0.4872(2) 0.0801(6) Uani 1 d .
Cl3' Cl -0.2400(2) 0.3667(2) 0.8032(2) 0.0769(6) Uani 1 d .
Cl4' Cl -0.0040(2) 0.3625(2) 0.8033(2) 0.0802(6) Uani 1 d .
N1' N -0.1332(5) 0.6991(4) 0.6753(4) 0.0525(14) Uani 1 d .
N2' N -0.1784(4) 0.5413(4) 0.8401(4) 0.0479(13) Uani 1 d .
N3' N -0.0744(4) 0.5138(4) 0.6402(4) 0.0534(14) Uani 1 d .
B' B -0.1842(6) 0.6570(6) 0.7984(6) 0.050(2) Uani 1 d .
C1' C -0.1394(8) 0.8144(5) 0.6321(7) 0.092(3) Uani 1 d .
H1'A H -0.1047(8) 0.8314(5) 0.5533(7) 0.138 Uiso 1 calc R
H1'B H -0.0982(8) 0.8433(5) 0.6570(7) 0.138 Uiso 1 calc R
H1'C H -0.2194(8) 0.8427(5) 0.6582(7) 0.138 Uiso 1 calc R
C2' C -0.2289(7) 0.4964(6) 0.9626(5) 0.074(2) Uani 1 d .
H2'A H -0.2195(7) 0.4220(6) 0.9779(5) 0.111 Uiso 1 calc R
H2'B H -0.3103(7) 0.5196(6) 0.9941(5) 0.111 Uiso 1 calc R
H2'C H -0.1893(7) 0.5190(6) 0.9938(5) 0.111 Uiso 1 calc R
C3' C 0.0423(12) 0.7978(12) 0.8041(15) 0.140(5) Uani 1 d .
C4' C -0.4904(9) 0.7958(9) 0.8156(10) 0.108(3) Uani 1 d .
O1' O -0.1327(3) 0.7043(3) 0.8500(4) 0.0596(12) Uani 1 d .
O2' O 0.0605(4) 0.6187(4) 0.7688(5) 0.090(2) Uani 1 d .
O3' O -0.0223(6) 0.6327(8) 0.9586(5) 0.159(4) Uani 1 d .
O4' O -0.3101(3) 0.7047(3) 0.8496(4) 0.0576(12) Uani 1 d .
O5' O -0.4952(5) 0.6282(5) 0.9631(4) 0.108(2) Uani 1 d .
O6' O -0.3822(5) 0.6209(4) 0.7665(4) 0.081(2) Uani 1 d .
F1' F -0.0273(7) 0.8557(7) 0.8648(10) 0.241(6) Uani 1 d .
F2' F 0.1428(6) 0.7833(6) 0.8086(8) 0.192(4) Uani 1 d .
F3' F 0.0554(9) 0.8381(7) 0.7023(11) 0.219(5) Uani 1 d .
F4' F -0.5860(6) 0.7775(5) 0.8185(7) 0.159(3) Uani 1 d .
F5' F -0.4177(7) 0.8439(5) 0.7095(6) 0.155(3) Uani 1 d .
F6' F -0.5120(6) 0.8499(5) 0.8828(6) 0.143(2) Uani 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'
B B 0.0013 0.0007 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 '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
O3 S1 O2 119.5(3)
O3 S1 O1 111.6(3)
O2 S1 O1 112.2(3)
O3 S1 C3 107.0(4)
O2 S1 C3 104.9(4)
O1 S1 C3 99.3(4)
O5 S2 O6 122.5(6)
O5 S2 O4 110.4(4)
O6 S2 O4 111.7(3)
O5 S2 C4 104.7(5)
O6 S2 C4 105.4(5)
O4 S2 C4 99.0(5)
N3 P1 N1 113.3(2)
N3 P1 Cl2 111.0(2)
N1 P1 Cl2 109.8(2)
N3 P1 Cl1 110.3(2)
N1 P1 Cl1 110.2(2)
Cl2 P1 Cl1 101.62(11)
N3 P2 N2 113.7(3)
N3 P2 Cl3 110.3(2)
N2 P2 Cl3 109.8(2)
N3 P2 Cl4 110.8(2)
N2 P2 Cl4 110.3(2)
Cl3 P2 Cl4 101.13(10)
B N1 C1 117.4(5)
B N1 P1 125.2(4)
C1 N1 P1 117.4(4)
C2 N2 B 116.6(5)
C2 N2 P2 118.0(4)
B N2 P2 125.4(4)
P2 N3 P1 126.1(3)
O4 B N2 110.2(5)
O4 B N1 111.0(5)
N2 B N1 116.3(5)
O4 B O1 99.1(5)
N2 B O1 109.6(5)
N1 B O1 109.3(5)
F1 C3 F3 109.3(9)
F1 C3 F2 110.0(9)
F3 C3 F2 109.2(8)
F1 C3 S1 111.1(7)
F3 C3 S1 109.4(7)
F2 C3 S1 107.7(7)
F6 C4 F4 110.2(15)
F6 C4 F5 110.5(10)
F4 C4 F5 106.8(9)
F6 C4 S2 110.9(8)
F4 C4 S2 110.9(8)
F5 C4 S2 107.5(11)
S1 O1 B 123.9(4)
B O4 S2 124.8(4)
O2' S1' O3' 121.6(5)
O2' S1' O1' 111.8(3)
O3' S1' O1' 110.9(3)
O2' S1' C3' 105.5(5)
O3' S1' C3' 104.5(7)
O1' S1' C3' 99.8(5)
O6' S2' O5' 123.1(4)
O6' S2' O4' 111.5(3)
O5' S2' O4' 111.0(3)
O6' S2' C4' 106.3(4)
O5' S2' C4' 102.0(5)
O4' S2' C4' 99.4(4)
N3' P1' N1' 113.0(3)
N3' P1' Cl1' 110.4(2)
N1' P1' Cl1' 109.7(2)
N3' P1' Cl2' 111.1(2)
N1' P1' Cl2' 110.4(2)
Cl1' P1' Cl2' 101.64(11)
N3' P2' N2' 113.2(3)
N3' P2' Cl3' 110.1(2)
N2' P2' Cl3' 110.4(2)
N3' P2' Cl4' 110.9(2)
N2' P2' Cl4' 110.3(2)
Cl3' P2' Cl4' 101.36(12)
C1' N1' B' 117.4(5)
C1' N1' P1' 117.1(4)
B' N1' P1' 125.5(4)
B' N2' C2' 118.1(5)
B' N2' P2' 125.2(4)
C2' N2' P2' 116.7(4)
P1' N3' P2' 126.5(3)
N2' B' N1' 116.6(5)
N2' B' O1' 110.4(6)
N1' B' O1' 110.6(5)
N2' B' O4' 110.2(5)
N1' B' O4' 109.8(6)
O1' B' O4' 97.6(4)
F1' C3' F2' 110.0(11)
F1' C3' F3' 110.7(15)
F2' C3' F3' 109.9(14)
F1' C3' S1' 110.2(11)
F2' C3' S1' 107.7(11)
F3' C3' S1' 108.3(9)
F6' C4' F4' 111.1(9)
F6' C4' F5' 111.1(10)
F4' C4' F5' 110.6(10)
F6' C4' S2' 110.6(8)
F4' C4' S2' 106.5(8)
F5' C4' S2' 106.7(6)
S1' O1' B' 124.8(4)
S2' O4' B' 124.6(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 O3 1.410(5)
S1 O2 1.417(5)
S1 O1 1.519(4)
S1 C3 1.830(10)
S2 O5 1.405(6)
S2 O6 1.428(7)
S2 O4 1.520(5)
S2 C4 1.816(12)
P1 N3 1.549(5)
P1 N1 1.598(5)
P1 Cl2 1.967(2)
P1 Cl1 1.970(2)
P2 N3 1.548(5)
P2 N2 1.582(5)
P2 Cl3 1.977(2)
P2 Cl4 1.980(2)
N1 B 1.512(9)
N1 C1 1.519(8)
N2 C2 1.488(7)
N2 B 1.517(9)
B O4 1.505(8)
B O1 1.530(8)
C3 F1 1.280(10)
C3 F3 1.315(10)
C3 F2 1.321(10)
C4 F6 1.247(12)
C4 F4 1.295(13)
C4 F5 1.319(13)
S1' O2' 1.400(5)
S1' O3' 1.402(6)
S1' O1' 1.524(4)
S1' C3' 1.831(15)
S2' O6' 1.410(5)
S2' O5' 1.435(5)
S2' O4' 1.527(4)
S2' C4' 1.834(10)
P1' N3' 1.538(5)
P1' N1' 1.588(5)
P1' Cl1' 1.973(2)
P1' Cl2' 1.972(2)
P2' N3' 1.555(5)
P2' N2' 1.590(5)
P2' Cl3' 1.972(2)
P2' Cl4' 1.973(2)
N1' C1' 1.496(9)
N1' B' 1.509(9)
N2' B' 1.499(9)
N2' C2' 1.507(8)
B' O1' 1.528(8)
B' O4' 1.534(8)
C3' F1' 1.255(13)
C3' F2' 1.303(14)
C3' F3' 1.31(2)
C4' F6' 1.278(11)
C4' F4' 1.299(11)
C4' F5' 1.389(12)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139120609
