#------------------------------------------------------------------------------
#$Date: 2015-07-08 23:30:10 +0300 (Wed, 08 Jul 2015) $
#$Revision: 141335 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/33/4343315.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_4343315
loop_
_publ_author_name
'Shi, Yan X.'
'Liang, Rong Z.'
'Martin, Katherine A.'
'Weston, Nicholas'
'Gonzalez-Calera, Silvia'
'Ganguly, Rakesh'
'Li, Yongxin'
'Lu, Yunpeng'
'Ribeiro, António J M'
'Ramos, Maria J.'
'Fernandes, Pedro A.'
'García, Felipe'
_publ_section_title
;
 Synthesis and Hydrolytic Studies on the Air-Stable
 [(4-CN-PhO)(E)P(μ-N(t)Bu)]2 (E = O, S, and Se) Cyclodiphosphazanes.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6423
_journal_page_last               6432
_journal_paper_doi               10.1021/acs.inorgchem.5b00735
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C8 H18 Cl2 N2 P2 S2'
_chemical_formula_weight         339.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                105.125(2)
_cell_angle_beta                 97.897(2)
_cell_angle_gamma                102.816(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3283(6)
_cell_length_b                   8.4922(7)
_cell_length_c                   11.9547(10)
_cell_measurement_temperature    103.(2)
_cell_volume                     778.57(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      103.(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16811
_diffrn_reflns_theta_full        31.11
_diffrn_reflns_theta_max         31.11
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
;
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.448
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4982
_refine_ls_number_restraints     526
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0377P)²+0.2815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                3963
_reflns_number_total             4982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00735_si_006.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4343313--4343318.cif.'
_cod_database_code               4343315
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
P P1 0.6172(2) 1.0540(3) -0.04641(18) 0.0225(3) Uani d PD 0.792(4) 1
S S1 0.7730(2) 1.27066(17) -0.01461(13) 0.0406(3) Uani d PD 0.792(4) 1
Cl Cl1 0.6497(3) 0.8865(3) -0.1875(2) 0.0384(3) Uani d PD 0.792(4) 1
N N1 0.5945(6) 0.9675(5) 0.0628(3) 0.0211(6) Uani d PDU 0.792(4) 1
C C1 0.7100(5) 0.8948(4) 0.1299(3) 0.0275(7) Uani d PDU 0.792(4) 1
C C2 0.8892(3) 0.9960(4) 0.1409(3) 0.0405(6) Uani d PDU 0.792(4) 1
H H2A 0.914 0.9838 0.0618 0.061 Uiso calc PR 0.792(4) 1
H H2B 0.9674 0.9539 0.1868 0.061 Uiso calc PR 0.792(4) 1
H H2C 0.902 1.1158 0.1813 0.061 Uiso calc PR 0.792(4) 1
C C3 0.6680(3) 0.9143(4) 0.2514(2) 0.0414(7) Uani d PDU 0.792(4) 1
H H3A 0.6819 1.0343 0.2916 0.062 Uiso calc PR 0.792(4) 1
H H3B 0.7438 0.8709 0.2982 0.062 Uiso calc PR 0.792(4) 1
H H3C 0.5513 0.8503 0.2429 0.062 Uiso calc PR 0.792(4) 1
C C4 0.6832(5) 0.7087(3) 0.0637(3) 0.0547(8) Uani d PDU 0.792(4) 1
H H4A 0.5656 0.6471 0.0551 0.082 Uiso calc PR 0.792(4) 1
H H4B 0.7571 0.6609 0.1083 0.082 Uiso calc PR 0.792(4) 1
H H4C 0.7098 0.6983 -0.0148 0.082 Uiso calc PR 0.792(4) 1
P P1A 0.5895(10) 1.0213(9) -0.0692(6) 0.0208(10) Uani d PD 0.208(4) 2
S S1A 0.6709(14) 0.9218(11) -0.2002(8) 0.0399(13) Uani d PD 0.208(4) 2
Cl Cl1A 0.7259(6) 1.2755(6) 0.0042(4) 0.0316(7) Uani d PD 0.208(4) 2
N N1A 0.582(2) 0.939(2) 0.0424(12) 0.024(2) Uani d PDU 0.208(4) 2
C C1A 0.7004(19) 0.8751(18) 0.1140(13) 0.032(2) Uani d PDU 0.208(4) 2
C C2A 0.8506(16) 1.0257(14) 0.1863(14) 0.059(3) Uani d PDU 0.208(4) 2
H H2A1 0.9109 1.0724 0.1323 0.088 Uiso calc PR 0.208(4) 2
H H2A2 0.9269 0.9873 0.2366 0.088 Uiso calc PR 0.208(4) 2
H H2A3 0.8098 1.1133 0.2361 0.088 Uiso calc PR 0.208(4) 2
C C3A 0.6101(13) 0.7877(17) 0.1923(10) 0.053(3) Uani d PDU 0.208(4) 2
H H3A1 0.5717 0.8697 0.2491 0.079 Uiso calc PR 0.208(4) 2
H H3A2 0.6874 0.7413 0.2353 0.079 Uiso calc PR 0.208(4) 2
H H3A3 0.513 0.6956 0.1432 0.079 Uiso calc PR 0.208(4) 2
C C4A 0.7681(17) 0.7494(14) 0.0337(10) 0.049(2) Uani d PDU 0.208(4) 2
H H4A1 0.6742 0.66 -0.0219 0.074 Uiso calc PR 0.208(4) 2
H H4A2 0.8352 0.6993 0.0813 0.074 Uiso calc PR 0.208(4) 2
H H4A3 0.839 0.807 -0.0105 0.074 Uiso calc PR 0.208(4) 2
P P2 0.8941(5) 0.5682(6) 0.4656(2) 0.0194(5) Uani d PD 0.694(3) 1
S S2 0.8647(4) 0.7798(3) 0.5444(2) 0.0451(6) Uani d PD 0.694(3) 1
Cl Cl2 0.7447(2) 0.4430(2) 0.30638(13) 0.0407(3) Uani d PD 0.694(3) 1
N N2 0.9111(10) 0.4315(9) 0.5431(6) 0.0200(10) Uani d PDU 0.694(3) 1
C C5 0.7955(8) 0.3655(7) 0.6168(5) 0.0275(9) Uani d PDU 0.694(3) 1
C C6 0.6130(3) 0.3234(4) 0.5504(3) 0.0482(8) Uani d PDU 0.694(3) 1
H H6A 0.5885 0.4267 0.5394 0.072 Uiso calc PR 0.694(3) 1
H H6B 0.5368 0.2766 0.5964 0.072 Uiso calc PR 0.694(3) 1
H H6C 0.5971 0.2399 0.4729 0.072 Uiso calc PR 0.694(3) 1
C C7 0.8342(3) 0.2052(3) 0.6330(3) 0.0359(6) Uani d PDU 0.694(3) 1
H H7A 0.8161 0.1214 0.5553 0.054 Uiso calc PR 0.694(3) 1
H H7B 0.7598 0.1589 0.6802 0.054 Uiso calc PR 0.694(3) 1
H H7C 0.9517 0.2318 0.6739 0.054 Uiso calc PR 0.694(3) 1
C C8 0.8239(4) 0.4966(3) 0.7373(2) 0.0454(8) Uani d PDU 0.694(3) 1
H H8A 0.9418 0.5247 0.7777 0.068 Uiso calc PR 0.694(3) 1
H H8B 0.7509 0.4504 0.7853 0.068 Uiso calc PR 0.694(3) 1
H H8C 0.7972 0.5991 0.7265 0.068 Uiso calc PR 0.694(3) 1
P P2A 0.8869(12) 0.5546(14) 0.4620(7) 0.0271(16) Uani d PD 0.306(3) 2
S S2A 0.7077(5) 0.4516(7) 0.3278(4) 0.0524(9) Uani d PD 0.306(3) 2
Cl Cl2A 0.8258(7) 0.7718(7) 0.5312(5) 0.0310(8) Uani d PD 0.306(3) 2
N N2A 0.909(2) 0.445(2) 0.5554(15) 0.0189(18) Uani d PDU 0.306(3) 2
C C5A 0.7980(16) 0.3507(16) 0.6193(11) 0.031(2) Uani d PDU 0.306(3) 2
C C6A 0.6900(9) 0.1860(8) 0.5300(7) 0.0530(17) Uani d PDU 0.306(3) 2
H H6A1 0.6206 0.2109 0.4672 0.079 Uiso calc PR 0.306(3) 2
H H6A2 0.617 0.1217 0.5697 0.079 Uiso calc PR 0.306(3) 2
H H6A3 0.7627 0.119 0.4954 0.079 Uiso calc PR 0.306(3) 2
C C7A 0.9098(9) 0.3246(10) 0.7199(6) 0.0514(17) Uani d PDU 0.306(3) 2
H H7A1 0.9833 0.2566 0.6878 0.077 Uiso calc PR 0.306(3) 2
H H7A2 0.8399 0.2655 0.7639 0.077 Uiso calc PR 0.306(3) 2
H H7A3 0.9787 0.4348 0.7731 0.077 Uiso calc PR 0.306(3) 2
C C8A 0.6912(9) 0.4683(9) 0.6649(7) 0.0511(17) Uani d PDU 0.306(3) 2
H H8A1 0.7646 0.5753 0.7195 0.077 Uiso calc PR 0.306(3) 2
H H8A2 0.6125 0.4145 0.7065 0.077 Uiso calc PR 0.306(3) 2
H H8A3 0.628 0.4905 0.598 0.077 Uiso calc PR 0.306(3) 2
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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 P1 N1 . 2_675 84.9(2)
N1 P1 S1 . . 119.87(17)
N1 P1 S1 2_675 . 121.1(2)
N1 P1 Cl1 . . 110.23(18)
N1 P1 Cl1 2_675 . 106.81(19)
S1 P1 Cl1 . . 111.06(12)
N1 P1 P1 . 2_675 43.10(17)
N1 P1 P1 2_675 2_675 41.84(12)
S1 P1 P1 . 2_675 133.44(17)
Cl1 P1 P1 . 2_675 115.47(15)
C1 N1 P1 . . 131.5(3)
C1 N1 P1 . 2_675 131.9(3)
P1 N1 P1 . 2_675 95.1(2)
N1 C1 C3 . . 107.6(3)
N1 C1 C2 . . 107.6(3)
C3 C1 C2 . . 110.3(3)
N1 C1 C4 . . 109.5(3)
C3 C1 C4 . . 110.5(3)
C2 C1 C4 . . 111.1(3)
N1A P1A N1A 2_675 . 84.2(9)
N1A P1A S1A 2_675 . 137.8(8)
N1A P1A S1A . . 120.6(8)
N1A P1A Cl1A 2_675 . 92.6(8)
N1A P1A Cl1A . . 106.6(6)
S1A P1A Cl1A . . 109.5(5)
N1A P1A P1A 2_675 2_675 43.2(5)
N1A P1A P1A . 2_675 41.0(7)
S1A P1A P1A . 2_675 146.9(6)
Cl1A P1A P1A . 2_675 103.1(5)
C1A N1A P1A . 2_675 127.9(11)
C1A N1A P1A . . 135.5(13)
P1A N1A P1A 2_675 . 95.8(9)
N1A C1A C4A . . 110.3(11)
N1A C1A C3A . . 110.5(11)
C4A C1A C3A . . 108.2(11)
N1A C1A C2A . . 108.3(11)
C4A C1A C2A . . 107.5(11)
C3A C1A C2A . . 112.1(12)
C1A C2A H2A1 . . 109.5
C1A C2A H2A2 . . 109.5
H2A1 C2A H2A2 . . 109.5
C1A C2A H2A3 . . 109.5
H2A1 C2A H2A3 . . 109.5
H2A2 C2A H2A3 . . 109.5
C1A C3A H3A1 . . 109.5
C1A C3A H3A2 . . 109.5
H3A1 C3A H3A2 . . 109.5
C1A C3A H3A3 . . 109.5
H3A1 C3A H3A3 . . 109.5
H3A2 C3A H3A3 . . 109.5
C1A C4A H4A1 . . 109.5
C1A C4A H4A2 . . 109.5
H4A1 C4A H4A2 . . 109.5
C1A C4A H4A3 . . 109.5
H4A1 C4A H4A3 . . 109.5
H4A2 C4A H4A3 . . 109.5
N2 P2 N2 2_766 . 83.5(3)
N2 P2 S2 2_766 . 114.9(4)
N2 P2 S2 . . 118.4(3)
N2 P2 Cl2 2_766 . 108.9(3)
N2 P2 Cl2 . . 109.4(4)
S2 P2 Cl2 . . 116.95(18)
N2 P2 P2 2_766 2_766 42.4(2)
N2 P2 P2 . 2_766 41.1(3)
S2 P2 P2 . 2_766 127.0(3)
Cl2 P2 P2 . 2_766 116.1(3)
C5 N2 P2 . 2_766 132.8(5)
C5 N2 P2 . . 129.4(6)
P2 N2 P2 2_766 . 96.5(3)
N2 C5 C7 . . 107.8(5)
N2 C5 C8 . . 110.4(5)
C7 C5 C8 . . 109.8(4)
N2 C5 C6 . . 108.8(5)
C7 C5 C6 . . 109.5(4)
C8 C5 C6 . . 110.4(4)
N2A P2A N2A . 2_766 87.5(8)
N2A P2A S2A . . 116.4(9)
N2A P2A S2A 2_766 . 118.8(8)
N2A P2A Cl2A . . 114.0(8)
N2A P2A Cl2A 2_766 . 121.4(9)
S2A P2A Cl2A . . 99.8(4)
N2A P2A P2A . 2_766 45.2(6)
N2A P2A P2A 2_766 2_766 42.3(4)
S2A P2A P2A . 2_766 130.0(7)
Cl2A P2A P2A . 2_766 130.1(7)
C5A N2A P2A . . 136.7(12)
C5A N2A P2A . 2_766 130.1(11)
P2A N2A P2A . 2_766 92.5(8)
N2A C5A C7A . . 107.9(10)
N2A C5A C6A . . 107.9(11)
C7A C5A C6A . . 113.2(9)
N2A C5A C8A . . 104.4(11)
C7A C5A C8A . . 111.6(9)
C6A C5A C8A . . 111.3(9)
C5A C6A H6A1 . . 109.5
C5A C6A H6A2 . . 109.5
H6A1 C6A H6A2 . . 109.5
C5A C6A H6A3 . . 109.5
H6A1 C6A H6A3 . . 109.5
H6A2 C6A H6A3 . . 109.5
C5A C7A H7A1 . . 109.5
C5A C7A H7A2 . . 109.5
H7A1 C7A H7A2 . . 109.5
C5A C7A H7A3 . . 109.5
H7A1 C7A H7A3 . . 109.5
H7A2 C7A H7A3 . . 109.5
C5A C8A H8A1 . . 109.5
C5A C8A H8A2 . . 109.5
H8A1 C8A H8A2 . . 109.5
C5A C8A H8A3 . . 109.5
H8A1 C8A H8A3 . . 109.5
H8A2 C8A H8A3 . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
P1 N1 . 1.670(3)
P1 N1 2_675 1.710(5)
P1 S1 . 1.911(2)
P1 Cl1 . 1.996(3)
P1 P1 2_675 2.493(4)
N1 C1 . 1.503(4)
N1 P1 2_675 1.710(5)
C1 C3 . 1.515(4)
C1 C2 . 1.517(4)
C1 C4 . 1.521(4)
C2 H2A . 0.98
C2 H2B . 0.98
C2 H2C . 0.98
C3 H3A . 0.98
C3 H3B . 0.98
C3 H3C . 0.98
C4 H4A . 0.98
C4 H4B . 0.98
C4 H4C . 0.98
P1A N1A 2_675 1.59(2)
P1A N1A . 1.662(12)
P1A S1A . 1.866(10)
P1A Cl1A . 2.090(7)
P1A P1A 2_675 2.417(17)
N1A C1A . 1.499(13)
N1A P1A 2_675 1.59(2)
C1A C4A . 1.503(14)
C1A C3A . 1.518(13)
C1A C2A . 1.537(14)
C2A H2A1 . 0.98
C2A H2A2 . 0.98
C2A H2A3 . 0.98
C3A H3A1 . 0.98
C3A H3A2 . 0.98
C3A H3A3 . 0.98
C4A H4A1 . 0.98
C4A H4A2 . 0.98
C4A H4A3 . 0.98
P2 N2 2_766 1.639(9)
P2 N2 . 1.680(5)
P2 S2 . 1.885(5)
P2 Cl2 . 2.002(4)
P2 P2 2_766 2.477(6)
N2 C5 . 1.507(6)
N2 P2 2_766 1.639(9)
C5 C7 . 1.520(5)
C5 C8 . 1.524(6)
C5 C6 . 1.532(6)
C6 H6A . 0.98
C6 H6B . 0.98
C6 H6C . 0.98
C7 H7A . 0.98
C7 H7B . 0.98
C7 H7C . 0.98
C8 H8A . 0.98
C8 H8B . 0.98
C8 H8C . 0.98
P2A N2A . 1.649(11)
P2A N2A 2_766 1.736(19)
P2A S2A . 1.897(9)
P2A Cl2A . 2.020(10)
P2A P2A 2_766 2.446(15)
N2A C5A . 1.505(12)
N2A P2A 2_766 1.736(19)
C5A C7A . 1.511(12)
C5A C6A . 1.518(12)
C5A C8A . 1.525(12)
C6A H6A1 . 0.98
C6A H6A2 . 0.98
C6A H6A3 . 0.98
C7A H7A1 . 0.98
C7A H7A2 . 0.98
C7A H7A3 . 0.98
C8A H8A1 . 0.98
C8A H8A2 . 0.98
C8A H8A3 . 0.98
