#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:09:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179233 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/53/4315319.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_4315319
loop_
_publ_author_name
'Joanne Ledger'
'Ramamoorthy Boomishankar'
'Alexander Steiner'
_publ_section_title
;
 Aqueous Chemistry of Chlorocyclophosphazenes: Phosphates {PO2},
 Phosphamides {P(O)NHR}, and the first Phosphites {PHO} and Pyrophosphates
 {(PO)2O} of These Heterocycles
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3896
_journal_page_last               3904
_journal_paper_doi               10.1021/ic100076t
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C28 H57 Cl3 N7 O P3'
_chemical_formula_weight         707.07
_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-97
_cell_angle_alpha                108.653(6)
_cell_angle_beta                 106.908(11)
_cell_angle_gamma                104.696(13)
_cell_formula_units_Z            2
_cell_length_a                   10.224(3)
_cell_length_b                   13.891(4)
_cell_length_c                   15.079(5)
_cell_measurement_temperature    100(2)
_cell_volume                     1793.7(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       ω
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9228
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         6194
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0499P)²+3.2017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1318
_reflns_number_gt                4970
_reflns_number_total             6194
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100076t_si_002_2.cif
_cod_data_source_block           jrl10a
_cod_original_cell_volume        1793.7(9)
_cod_database_code               4315319
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 1.11341(11) 0.75379(8) 1.01557(7) 0.0212(2) Uani 1 1 d . . .
Cl2 Cl 1.11038(11) 0.94227(8) 0.95015(8) 0.0223(2) Uani 1 1 d . . .
Cl3 Cl 0.31886(10) 0.55089(8) 0.57120(7) 0.0175(2) Uani 1 1 d . . .
P1 P 1.04202(10) 0.77699(8) 0.88742(7) 0.0133(2) Uani 1 1 d . . .
P2 P 0.76878(10) 0.65118(8) 0.71794(7) 0.0115(2) Uani 1 1 d . . .
P3 P 1.06300(10) 0.65167(8) 0.70773(7) 0.0119(2) Uani 1 1 d . . .
N1 N 1.1313(3) 0.7449(3) 0.8223(2) 0.0144(7) Uani 1 1 d . . .
N2 N 0.8690(3) 0.7238(3) 0.8378(2) 0.0140(7) Uani 1 1 d . . .
N3 N 0.8804(3) 0.6166(3) 0.6632(2) 0.0132(7) Uani 1 1 d . . .
H3 H 0.839(4) 0.580(3) 0.608(3) 0.012(5) Uiso 1 1 d . . .
N4 N 0.6357(4) 0.5377(3) 0.6844(3) 0.0146(7) Uani 1 1 d . . .
H4 H 0.563(4) 0.542(3) 0.672(3) 0.012(5) Uiso 1 1 d . . .
N5 N 0.6828(4) 0.7198(3) 0.6730(3) 0.0168(7) Uani 1 1 d . . .
H5 H 0.607(4) 0.686(3) 0.632(3) 0.012(5) Uiso 1 1 d . . .
N6 N 1.1150(4) 0.5502(3) 0.7068(3) 0.0153(7) Uani 1 1 d . . .
H6 H 1.151(4) 0.534(3) 0.668(3) 0.012(5) Uiso 1 1 d . . .
N7 N 1.1152(4) 0.6853(3) 0.6268(3) 0.0164(8) Uani 1 1 d . . .
H7 H 1.165(5) 0.668(4) 0.620(3) 0.012(5) Uiso 1 1 d . . .
C41 C 0.6462(4) 0.4376(3) 0.6925(3) 0.0145(8) Uani 1 1 d . . .
H41 H 0.7408 0.4337 0.6886 0.017 Uiso 1 1 calc R . .
C42 C 0.5188(5) 0.3383(3) 0.6025(3) 0.0217(9) Uani 1 1 d . . .
H42A H 0.5270 0.3360 0.5381 0.026 Uiso 1 1 calc R . .
H42B H 0.4242 0.3457 0.6001 0.026 Uiso 1 1 calc R . .
C43 C 0.5177(5) 0.2308(3) 0.6100(3) 0.0268(10) Uani 1 1 d . . .
H43A H 0.4300 0.1685 0.5524 0.032 Uiso 1 1 calc R . .
H43B H 0.6072 0.2192 0.6047 0.032 Uiso 1 1 calc R . .
C44 C 0.5139(4) 0.2334(3) 0.7109(3) 0.0215(9) Uani 1 1 d . . .
H44A H 0.5172 0.1643 0.7150 0.026 Uiso 1 1 calc R . .
H44B H 0.4202 0.2386 0.7137 0.026 Uiso 1 1 calc R . .
C45 C 0.6450(4) 0.3315(3) 0.8019(3) 0.0221(9) Uani 1 1 d . . .
H45A H 0.6371 0.3339 0.8664 0.027 Uiso 1 1 calc R . .
H45B H 0.7383 0.3222 0.8031 0.027 Uiso 1 1 calc R . .
C46 C 0.6489(4) 0.4389(3) 0.7951(3) 0.0180(9) Uani 1 1 d . . .
H46A H 0.7396 0.4997 0.8514 0.022 Uiso 1 1 calc R . .
H46B H 0.5626 0.4532 0.8044 0.022 Uiso 1 1 calc R . .
C51 C 0.7245(4) 0.8392(3) 0.7226(3) 0.0145(8) Uani 1 1 d . . .
H51 H 0.7693 0.8642 0.7984 0.017 Uiso 1 1 calc R . .
C52 C 0.8375(4) 0.9010(3) 0.6923(3) 0.0189(9) Uani 1 1 d . . .
H52A H 0.9281 0.8854 0.7132 0.023 Uiso 1 1 calc R . .
H52B H 0.7963 0.8744 0.6169 0.023 Uiso 1 1 calc R . .
C53 C 0.8778(4) 1.0248(3) 0.7420(3) 0.0200(9) Uani 1 1 d . . .
H53A H 0.9472 1.0618 0.7181 0.024 Uiso 1 1 calc R . .
H53B H 0.9278 1.0530 0.8173 0.024 Uiso 1 1 calc R . .
C54 C 0.7385(4) 1.0515(3) 0.7148(3) 0.0188(9) Uani 1 1 d . . .
H54A H 0.7657 1.1316 0.7512 0.023 Uiso 1 1 calc R . .
H54B H 0.6944 1.0306 0.6403 0.023 Uiso 1 1 calc R . .
C55 C 0.6250(4) 0.9893(3) 0.7448(3) 0.0175(8) Uani 1 1 d . . .
H55A H 0.6659 1.0155 0.8202 0.021 Uiso 1 1 calc R . .
H55B H 0.5344 1.0049 0.7239 0.021 Uiso 1 1 calc R . .
C56 C 0.5851(4) 0.8654(3) 0.6943(3) 0.0158(8) Uani 1 1 d . . .
H56A H 0.5363 0.8378 0.6190 0.019 Uiso 1 1 calc R . .
H56B H 0.5147 0.8277 0.7172 0.019 Uiso 1 1 calc R . .
C61 C 1.1667(4) 0.5275(3) 0.7975(3) 0.0153(8) Uani 1 1 d . . .
H61 H 1.2334 0.5990 0.8582 0.018 Uiso 1 1 calc R . .
C62 C 1.2551(4) 0.4554(4) 0.7806(3) 0.0223(9) Uani 1 1 d . . .
H62A H 1.3407 0.4935 0.7696 0.027 Uiso 1 1 calc R . .
H62B H 1.1921 0.3859 0.7183 0.027 Uiso 1 1 calc R . .
C63 C 1.3102(5) 0.4293(4) 0.8721(3) 0.0255(10) Uani 1 1 d . . .
H63A H 1.3816 0.4981 0.9328 0.031 Uiso 1 1 calc R . .
H63B H 1.3625 0.3791 0.8574 0.031 Uiso 1 1 calc R . .
C64 C 1.1821(5) 0.3758(4) 0.8956(3) 0.0244(10) Uani 1 1 d . . .
H64A H 1.1165 0.3031 0.8381 0.029 Uiso 1 1 calc R . .
H64B H 1.2214 0.3644 0.9580 0.029 Uiso 1 1 calc R . .
C65 C 1.0935(4) 0.4484(4) 0.9118(3) 0.0219(9) Uani 1 1 d . . .
H65A H 1.0079 0.4107 0.9231 0.026 Uiso 1 1 calc R . .
H65B H 1.1565 0.5182 0.9737 0.026 Uiso 1 1 calc R . .
C66 C 1.0388(4) 0.4730(3) 0.8194(3) 0.0166(8) Uani 1 1 d . . .
H66A H 0.9694 0.4037 0.7588 0.020 Uiso 1 1 calc R . .
H66B H 0.9846 0.5221 0.8326 0.020 Uiso 1 1 calc R . .
C71 C 1.0870(4) 0.7665(3) 0.5893(3) 0.0151(8) Uani 1 1 d . . .
H71 H 0.9818 0.7580 0.5747 0.018 Uiso 1 1 calc R . .
C72 C 1.1874(4) 0.8844(3) 0.6680(3) 0.0188(9) Uani 1 1 d . . .
H72A H 1.1664 0.9001 0.7300 0.023 Uiso 1 1 calc R . .
H72B H 1.2920 0.8921 0.6880 0.023 Uiso 1 1 calc R . .
C73 C 1.1644(5) 0.9675(3) 0.6255(3) 0.0234(9) Uani 1 1 d . . .
H73A H 1.2352 1.0423 0.6767 0.028 Uiso 1 1 calc R . .
H73B H 1.0630 0.9658 0.6129 0.028 Uiso 1 1 calc R . .
C74 C 1.1864(5) 0.9430(4) 0.5256(3) 0.0270(10) Uani 1 1 d . . .
H74A H 1.1651 0.9957 0.4980 0.032 Uiso 1 1 calc R . .
H74B H 1.2907 0.9522 0.5394 0.032 Uiso 1 1 calc R . .
C75 C 1.0846(5) 0.8259(4) 0.4467(3) 0.0283(10) Uani 1 1 d . . .
H75A H 1.1047 0.8100 0.3843 0.034 Uiso 1 1 calc R . .
H75B H 0.9803 0.8190 0.4275 0.034 Uiso 1 1 calc R . .
C76 C 1.1079(5) 0.7428(3) 0.4894(3) 0.0237(9) Uani 1 1 d . . .
H76A H 1.0370 0.6681 0.4381 0.028 Uiso 1 1 calc R . .
H76B H 1.2091 0.7445 0.5015 0.028 Uiso 1 1 calc R . .
O1 O 0.5437(6) 0.7094(4) -0.0233(4) 0.0463(16) Uiso 0.748(10) 1 d PDU A 1
C11 C 0.6039(8) 0.8093(6) 0.0694(5) 0.0409(19) Uiso 0.748(10) 1 d PDU A 1
H11A H 0.7132 0.8419 0.0963 0.049 Uiso 0.748(10) 1 calc PR A 1
H11B H 0.5753 0.7951 0.1227 0.049 Uiso 0.748(10) 1 calc PR A 1
C12 C 0.5364(9) 0.8849(6) 0.0369(6) 0.033(2) Uiso 0.748(10) 1 d PDU A 1
H12A H 0.6028 0.9631 0.0798 0.040 Uiso 0.748(10) 1 calc PR A 1
H12B H 0.4393 0.8733 0.0414 0.040 Uiso 0.748(10) 1 calc PR A 1
C13 C 0.5191(9) 0.8504(6) -0.0746(5) 0.0335(19) Uiso 0.748(10) 1 d PDU A 1
H13A H 0.4171 0.8348 -0.1202 0.040 Uiso 0.748(10) 1 calc PR A 1
H13B H 0.5894 0.9088 -0.0811 0.040 Uiso 0.748(10) 1 calc PR A 1
C14 C 0.5535(9) 0.7463(6) -0.1009(6) 0.043(2) Uiso 0.748(10) 1 d PDU A 1
H14A H 0.4810 0.6894 -0.1696 0.051 Uiso 0.748(10) 1 calc PR A 1
H14B H 0.6540 0.7629 -0.1002 0.051 Uiso 0.748(10) 1 calc PR A 1
O1' O 0.532(3) 0.8182(19) -0.0835(14) 0.081(8) Uiso 0.252(10) 1 d PDU A 2
C11' C 0.606(3) 0.7503(18) -0.0489(18) 0.050(6) Uiso 0.252(10) 1 d PDU A 2
H11C H 0.7151 0.7899 -0.0159 0.060 Uiso 0.252(10) 1 calc PR A 2
H11D H 0.5808 0.6799 -0.1069 0.060 Uiso 0.252(10) 1 calc PR A 2
C12' C 0.546(2) 0.7315(15) 0.0268(16) 0.033(5) Uiso 0.252(10) 1 d PDU A 2
H12C H 0.4430 0.6771 -0.0083 0.039 Uiso 0.252(10) 1 calc PR A 2
H12D H 0.6080 0.7060 0.0706 0.039 Uiso 0.252(10) 1 calc PR A 2
C13' C 0.555(2) 0.8435(15) 0.0879(12) 0.037(5) Uiso 0.252(10) 1 d PDU A 2
H13C H 0.6559 0.8908 0.1412 0.045 Uiso 0.252(10) 1 calc PR A 2
H13D H 0.4839 0.8392 0.1207 0.045 Uiso 0.252(10) 1 calc PR A 2
C14' C 0.514(3) 0.8849(18) 0.0068(17) 0.040(7) Uiso 0.252(10) 1 d PDU A 2
H14C H 0.4096 0.8789 -0.0125 0.048 Uiso 0.252(10) 1 calc PR A 2
H14D H 0.5779 0.9631 0.0335 0.048 Uiso 0.252(10) 1 calc PR A 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'
O O 0.0106 0.0060 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 P1 N2 120.03(17) . . ?
N1 P1 Cl2 107.79(13) . . ?
N2 P1 Cl2 109.77(13) . . ?
N1 P1 Cl1 109.64(12) . . ?
N2 P1 Cl1 108.00(12) . . ?
Cl2 P1 Cl1 99.70(6) . . ?
N2 P2 N4 117.73(17) . . ?
N2 P2 N5 109.19(17) . . ?
N4 P2 N5 102.62(17) . . ?
N2 P2 N3 107.04(16) . . ?
N4 P2 N3 106.00(17) . . ?
N5 P2 N3 114.51(17) . . ?
N1 P3 N7 116.74(18) . . ?
N1 P3 N6 109.84(17) . . ?
N7 P3 N6 102.96(18) . . ?
N1 P3 N3 106.87(16) . . ?
N7 P3 N3 106.50(17) . . ?
N6 P3 N3 114.15(17) . . ?
P1 N1 P3 125.8(2) . . ?
P1 N2 P2 125.22(19) . . ?
P3 N3 P2 132.7(2) . . ?
C41 N4 P2 128.0(3) . . ?
C51 N5 P2 125.2(3) . . ?
C61 N6 P3 124.0(3) . . ?
C71 N7 P3 127.9(3) . . ?
N4 C41 C42 109.2(3) . . ?
N4 C41 C46 111.3(3) . . ?
C42 C41 C46 111.6(3) . . ?
C41 C42 C43 111.8(3) . . ?
C44 C43 C42 111.1(3) . . ?
C43 C44 C45 110.8(3) . . ?
C46 C45 C44 111.1(3) . . ?
C45 C46 C41 112.6(3) . . ?
N5 C51 C52 112.0(3) . . ?
N5 C51 C56 109.1(3) . . ?
C52 C51 C56 110.3(3) . . ?
C53 C52 C51 111.7(3) . . ?
C52 C53 C54 110.6(3) . . ?
C55 C54 C53 110.5(3) . . ?
C56 C55 C54 111.5(3) . . ?
C55 C56 C51 110.4(3) . . ?
N6 C61 C66 111.7(3) . . ?
N6 C61 C62 109.3(3) . . ?
C66 C61 C62 110.4(3) . . ?
C61 C62 C63 111.2(3) . . ?
C62 C63 C64 111.2(3) . . ?
C65 C64 C63 110.5(3) . . ?
C66 C65 C64 110.9(3) . . ?
C61 C66 C65 111.1(3) . . ?
N7 C71 C76 109.0(3) . . ?
N7 C71 C72 112.0(3) . . ?
C76 C71 C72 110.5(3) . . ?
C73 C72 C71 111.6(3) . . ?
C72 C73 C74 111.5(3) . . ?
C75 C74 C73 110.6(3) . . ?
C74 C75 C76 110.9(4) . . ?
C71 C76 C75 112.2(3) . . ?
C14 O1 C11 104.5(5) . . ?
O1 C11 C12 104.3(5) . . ?
C11 C12 C13 103.1(6) . . ?
C14 C13 C12 104.6(5) . . ?
O1 C14 C13 105.7(5) . . ?
C14' O1' C11' 104.5(14) . . ?
O1' C11' C12' 103.2(13) . . ?
C13' C12' C11' 102.4(12) . . ?
C12' C13' C14' 102.0(11) . . ?
O1' C14' C13' 108.7(13) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 P1 2.0169(15) . ?
Cl2 P1 2.0166(15) . ?
P1 N1 1.563(3) . ?
P1 N2 1.565(3) . ?
P2 N2 1.602(3) . ?
P2 N4 1.610(3) . ?
P2 N5 1.623(3) . ?
P2 N3 1.669(3) . ?
P3 N1 1.600(3) . ?
P3 N7 1.616(4) . ?
P3 N6 1.626(3) . ?
P3 N3 1.665(3) . ?
N4 C41 1.462(5) . ?
N5 C51 1.467(5) . ?
N6 C61 1.478(5) . ?
N7 C71 1.466(5) . ?
C41 C42 1.518(5) . ?
C41 C46 1.533(5) . ?
C42 C43 1.531(5) . ?
C43 C44 1.521(6) . ?
C44 C45 1.531(6) . ?
C45 C46 1.519(5) . ?
C51 C52 1.528(5) . ?
C51 C56 1.535(5) . ?
C52 C53 1.525(5) . ?
C53 C54 1.536(5) . ?
C54 C55 1.532(5) . ?
C55 C56 1.528(5) . ?
C61 C66 1.518(5) . ?
C61 C62 1.523(5) . ?
C62 C63 1.524(5) . ?
C63 C64 1.530(6) . ?
C64 C65 1.526(5) . ?
C65 C66 1.523(5) . ?
C71 C76 1.525(5) . ?
C71 C72 1.530(5) . ?
C72 C73 1.524(5) . ?
C73 C74 1.530(6) . ?
C74 C75 1.525(6) . ?
C75 C76 1.526(6) . ?
O1 C14 1.438(8) . ?
O1 C11 1.444(8) . ?
C11 C12 1.523(9) . ?
C12 C13 1.535(9) . ?
C13 C14 1.530(9) . ?
O1' C14' 1.474(15) . ?
O1' C11' 1.480(15) . ?
C11' C12' 1.506(15) . ?
C12' C13' 1.498(18) . ?
C13' C14' 1.509(15) . ?
