#------------------------------------------------------------------------------
#$Date: 2019-11-23 08:29:06 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232561 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/78/4347882.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_4347882
loop_
_publ_author_name
'Chakarawet, Khetpakorn'
'Knopf, Ioana'
'Nava, Matthew'
'Jiang, Yanfeng'
'Stauber, Julia M.'
'Cummins, Christopher C.'
_publ_section_title
;
 Crystalline Metaphosphate Acid Salts: Synthesis in Organic Media,
 Structures, Hydrogen-Bonding Capability, and Implication of Superacidity.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6178
_journal_page_last               6185
_journal_paper_doi               10.1021/acs.inorgchem.6b00749
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C144 H126 N4 O20 P14'
_chemical_formula_weight         2666.06
_chemical_name_systematic
'Bis(triphenylphosphine)iminium dihydrogenhexametaphosphate dihydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                97.0320(14)
_cell_angle_beta                 107.0490(13)
_cell_angle_gamma                109.7810(13)
_cell_formula_units_Z            1
_cell_length_a                   14.7633(9)
_cell_length_b                   16.1312(10)
_cell_length_c                   17.2418(11)
_cell_measurement_reflns_used    9683
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.89
_cell_measurement_theta_min      2.47
_cell_volume                     3580.2(4)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2011)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2011)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            132614
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.028
_diffrn_reflns_theta_min         1.275
_diffrn_source
'I\mS micro-focus sealed tube, multilayer optics'
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         22569
_refine_ls_number_restraints     1516
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0469P)²+2.3615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17005
_reflns_number_total             22569
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00749_si_005.cif
_cod_data_source_block           X14137S
_cod_database_code               4347882
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.910
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.85303(3) 0.31091(3) 0.40055(2) 0.01677(8) Uani 1 1 d . U . . .
P2 P 0.81012(3) 0.47054(3) 0.44826(3) 0.01866(8) Uani 1 1 d . U . . .
P3 P 0.95562(3) 0.57698(3) 0.62044(2) 0.01710(8) Uani 1 1 d . U . . .
O1 O 0.84182(10) 0.38750(7) 0.46343(7) 0.0238(2) Uani 1 1 d . U . . .
O2 O 0.84880(8) 0.52916(7) 0.54263(7) 0.0193(2) Uani 1 1 d . U . . .
O3 O 1.02405(9) 0.64361(8) 0.57992(8) 0.0245(2) Uani 1 1 d . U . . .
O11 O 0.79604(9) 0.30650(8) 0.31281(7) 0.0225(2) Uani 1 1 d . U . . .
O12 O 0.83325(9) 0.22974(7) 0.43424(7) 0.0235(2) Uani 1 1 d . U . . .
O21 O 0.87434(11) 0.52545(8) 0.40419(8) 0.0274(3) Uani 1 1 d . U . . .
H1 H 0.9265(15) 0.5131(13) 0.3898(10) 0.033 Uiso 1 1 d . U . . .
O22 O 0.69859(10) 0.44433(10) 0.41257(8) 0.0323(3) Uani 1 1 d . U . . .
O31 O 0.99813(9) 0.50603(7) 0.64057(7) 0.0216(2) Uani 1 1 d . U . . .
O32 O 0.93831(10) 0.62660(8) 0.68830(8) 0.0280(3) Uani 1 1 d . U . . .
O1W O 0.86499(15) 0.23551(11) 0.19567(10) 0.0469(4) Uani 1 1 d D . . . .
H1W H 0.833(2) 0.2587(18) 0.2302(15) 0.056 Uiso 1 1 d D U . . .
H2W H 0.9326(15) 0.2827(16) 0.2291(15) 0.056 Uiso 1 1 d D U . . .
N1 N 0.31943(11) 0.44754(10) 0.09730(9) 0.0249(3) Uani 1 1 d . U . . .
N2 N 0.76309(10) 0.00359(8) 0.54662(8) 0.0179(2) Uani 1 1 d . U . . .
P1C P 0.21925(3) 0.46854(3) 0.06995(3) 0.02013(8) Uani 1 1 d . U . . .
P2C P 0.41801(3) 0.46764(3) 0.17667(3) 0.02074(8) Uani 1 1 d . U . . .
P3C P 0.68911(3) -0.08951(2) 0.47858(2) 0.01594(8) Uani 1 1 d . U . . .
P4C P 0.83286(3) 0.03095(3) 0.64293(2) 0.01674(8) Uani 1 1 d . U . . .
C111 C 0.20739(12) 0.50725(11) -0.02441(10) 0.0211(3) Uani 1 1 d . U . . .
C112 C 0.13933(14) 0.54946(12) -0.05133(11) 0.0267(3) Uani 1 1 d . U . . .
H112 H 0.0981 0.5570 -0.0200 0.032 Uiso 1 1 calc R U . . .
C113 C 0.13185(15) 0.58041(12) -0.12365(12) 0.0302(4) Uani 1 1 d . U . . .
H113 H 0.0851 0.6085 -0.1421 0.036 Uiso 1 1 calc R U . . .
C114 C 0.19270(14) 0.57030(12) -0.16907(11) 0.0287(4) Uani 1 1 d . U . . .
H114 H 0.1885 0.5926 -0.2180 0.034 Uiso 1 1 calc R U . . .
C115 C 0.25955(15) 0.52773(12) -0.14311(11) 0.0282(4) Uani 1 1 d . U . . .
H115 H 0.3009 0.5207 -0.1745 0.034 Uiso 1 1 calc R U . . .
C116 C 0.26648(13) 0.49516(11) -0.07144(10) 0.0229(3) Uani 1 1 d . U . . .
H116 H 0.3113 0.4648 -0.0546 0.028 Uiso 1 1 calc R U . . .
C121 C 0.21712(13) 0.55529(11) 0.14498(10) 0.0232(3) Uani 1 1 d . U . . .
C122 C 0.27829(14) 0.64586(12) 0.15252(11) 0.0285(4) Uani 1 1 d . U . . .
H122 H 0.3175 0.6601 0.1175 0.034 Uiso 1 1 calc R U . . .
C123 C 0.28158(16) 0.71492(13) 0.21147(12) 0.0333(4) Uani 1 1 d . U . . .
H123 H 0.3229 0.7764 0.2165 0.040 Uiso 1 1 calc R U . . .
C124 C 0.22463(16) 0.69416(14) 0.26304(12) 0.0340(4) Uani 1 1 d . U . . .
H124 H 0.2266 0.7416 0.3029 0.041 Uiso 1 1 calc R U . . .
C125 C 0.16479(15) 0.60424(13) 0.25661(12) 0.0315(4) Uani 1 1 d . U . . .
H125 H 0.1264 0.5903 0.2923 0.038 Uiso 1 1 calc R U . . .
C126 C 0.16113(13) 0.53465(12) 0.19775(11) 0.0258(3) Uani 1 1 d . U . . .
H126 H 0.1206 0.4732 0.1935 0.031 Uiso 1 1 calc R U . . .
C131 C 0.10699(13) 0.36657(11) 0.04932(10) 0.0224(3) Uani 1 1 d . U . . .
C132 C 0.02121(13) 0.33745(12) -0.02421(11) 0.0252(3) Uani 1 1 d . U . . .
H132 H 0.0210 0.3716 -0.0654 0.030 Uiso 1 1 calc R U . . .
C133 C -0.06399(15) 0.25865(13) -0.03747(12) 0.0322(4) Uani 1 1 d . U . . .
H133 H -0.1218 0.2383 -0.0881 0.039 Uiso 1 1 calc R U . . .
C134 C -0.06456(16) 0.20965(13) 0.02338(13) 0.0373(4) Uani 1 1 d . U . . .
H134 H -0.1235 0.1565 0.0148 0.045 Uiso 1 1 calc R U . . .
C135 C 0.02075(17) 0.23824(14) 0.09662(13) 0.0380(5) Uani 1 1 d . U . . .
H135 H 0.0202 0.2045 0.1380 0.046 Uiso 1 1 calc R U . . .
C136 C 0.10641(15) 0.31565(13) 0.10949(12) 0.0319(4) Uani 1 1 d . U . . .
H136 H 0.1651 0.3344 0.1593 0.038 Uiso 1 1 calc R U . . .
C211 C 0.52682(13) 0.56341(11) 0.17812(10) 0.0226(3) Uani 1 1 d . U . . .
C212 C 0.51946(15) 0.59921(13) 0.10813(12) 0.0295(4) Uani 1 1 d . U . . .
H212 H 0.4571 0.5746 0.0609 0.035 Uiso 1 1 calc R U . . .
C213 C 0.60422(16) 0.67149(14) 0.10792(13) 0.0367(4) Uani 1 1 d . U . . .
H213 H 0.5994 0.6964 0.0605 0.044 Uiso 1 1 calc R U . . .
C214 C 0.69515(15) 0.70704(13) 0.17626(13) 0.0347(4) Uani 1 1 d . U . . .
H214 H 0.7528 0.7559 0.1753 0.042 Uiso 1 1 calc R U . . .
C215 C 0.70270(15) 0.67204(13) 0.24583(12) 0.0320(4) Uani 1 1 d . U . . .
H215 H 0.7654 0.6970 0.2928 0.038 Uiso 1 1 calc R U . . .
C216 C 0.61880(14) 0.60026(12) 0.24736(11) 0.0276(4) Uani 1 1 d . U . . .
H216 H 0.6240 0.5763 0.2954 0.033 Uiso 1 1 calc R U . . .
C221 C 0.40441(13) 0.49196(13) 0.27614(10) 0.0276(4) Uani 1 1 d . U . . .
C222 C 0.36752(18) 0.42101(17) 0.31238(13) 0.0433(5) Uani 1 1 d . U . . .
H222 H 0.3544 0.3605 0.2866 0.052 Uiso 1 1 calc R U . . .
C223 C 0.3501(2) 0.4394(2) 0.38638(15) 0.0587(7) Uani 1 1 d . U . . .
H223 H 0.3240 0.3912 0.4108 0.070 Uiso 1 1 calc R U . . .
C224 C 0.37076(17) 0.5281(2) 0.42483(14) 0.0540(7) Uani 1 1 d . U . . .
H224 H 0.3610 0.5407 0.4764 0.065 Uiso 1 1 calc R U . . .
C225 C 0.40529(15) 0.59780(18) 0.38820(13) 0.0442(6) Uani 1 1 d . U . . .
H225 H 0.4172 0.6580 0.4137 0.053 Uiso 1 1 calc R U . . .
C226 C 0.42286(14) 0.58049(14) 0.31395(11) 0.0331(4) Uani 1 1 d . U . . .
H226 H 0.4473 0.6288 0.2892 0.040 Uiso 1 1 calc R U . . .
C231 C 0.4507(3) 0.3668(2) 0.1703(3) 0.0222(11) Uani 0.631(11) 1 d G U P A 1
C232 C 0.3927(3) 0.2925(2) 0.1017(2) 0.0354(10) Uani 0.631(11) 1 d G U P A 1
H232 H 0.3341 0.2924 0.0598 0.043 Uiso 0.631(11) 1 calc R U P A 1
C233 C 0.4204(4) 0.2185(2) 0.0946(2) 0.0487(14) Uani 0.631(11) 1 d G U P A 1
H233 H 0.3808 0.1677 0.0477 0.058 Uiso 0.631(11) 1 calc R U P A 1
C234 C 0.5061(3) 0.2188(2) 0.1560(3) 0.0417(11) Uani 0.631(11) 1 d G U P A 1
H234 H 0.5250 0.1682 0.1511 0.050 Uiso 0.631(11) 1 calc R U P A 1
C235 C 0.5641(3) 0.2930(3) 0.2246(2) 0.0270(10) Uani 0.631(11) 1 d G U P A 1
H235 H 0.6227 0.2932 0.2666 0.032 Uiso 0.631(11) 1 calc R U P A 1
C236 C 0.5364(3) 0.3671(2) 0.2318(3) 0.0223(13) Uani 0.631(11) 1 d G U P A 1
H236 H 0.5760 0.4178 0.2786 0.027 Uiso 0.631(11) 1 calc R U P A 1
C31B C 0.4444(6) 0.3723(3) 0.1730(5) 0.0229(18) Uani 0.369(11) 1 d G U P A 2
C32B C 0.3673(5) 0.2901(4) 0.1221(5) 0.038(2) Uani 0.369(11) 1 d G U P A 2
H32B H 0.3054 0.2891 0.0839 0.046 Uiso 0.369(11) 1 calc R U P A 2
C33B C 0.3806(5) 0.2094(3) 0.1270(5) 0.049(3) Uani 0.369(11) 1 d G U P A 2
H33B H 0.3279 0.1532 0.0922 0.058 Uiso 0.369(11) 1 calc R U P A 2
C34B C 0.4711(5) 0.2109(3) 0.1829(4) 0.0357(18) Uani 0.369(11) 1 d G U P A 2
H34B H 0.4803 0.1557 0.1863 0.043 Uiso 0.369(11) 1 calc R U P A 2
C35B C 0.5483(4) 0.2931(4) 0.2338(4) 0.0282(16) Uani 0.369(11) 1 d G U P A 2
H35B H 0.6102 0.2941 0.2720 0.034 Uiso 0.369(11) 1 calc R U P A 2
C36B C 0.5349(6) 0.3738(3) 0.2289(5) 0.031(3) Uani 0.369(11) 1 d G U P A 2
H36B H 0.5877 0.4299 0.2637 0.038 Uiso 0.369(11) 1 calc R U P A 2
C311 C 0.65528(12) -0.06341(10) 0.37808(10) 0.0181(3) Uani 1 1 d . U . . .
C312 C 0.68733(12) 0.02637(10) 0.37119(10) 0.0194(3) Uani 1 1 d . U . . .
H312 H 0.7236 0.0749 0.4202 0.023 Uiso 1 1 calc R U . . .
C313 C 0.66623(13) 0.04486(11) 0.29249(11) 0.0231(3) Uani 1 1 d . U . . .
H313 H 0.6882 0.1060 0.2878 0.028 Uiso 1 1 calc R U . . .
C314 C 0.61313(14) -0.02616(12) 0.22100(11) 0.0264(3) Uani 1 1 d . U . . .
H314 H 0.5991 -0.0135 0.1674 0.032 Uiso 1 1 calc R U . . .
C315 C 0.58025(15) -0.11614(12) 0.22753(11) 0.0277(4) Uani 1 1 d . U . . .
H315 H 0.5433 -0.1645 0.1784 0.033 Uiso 1 1 calc R U . . .
C316 C 0.60161(14) -0.13477(11) 0.30573(10) 0.0247(3) Uani 1 1 d . U . . .
H316 H 0.5798 -0.1960 0.3102 0.030 Uiso 1 1 calc R U . . .
C321 C 0.57264(12) -0.14522(10) 0.49814(10) 0.0195(3) Uani 1 1 d . U . . .
C322 C 0.48551(13) -0.12857(12) 0.46003(11) 0.0261(3) Uani 1 1 d . U . . .
H322 H 0.4845 -0.0952 0.4183 0.031 Uiso 1 1 calc R U . . .
C323 C 0.39954(14) -0.16121(13) 0.48347(13) 0.0334(4) Uani 1 1 d . U . . .
H323 H 0.3407 -0.1487 0.4585 0.040 Uiso 1 1 calc R U . . .
C324 C 0.39949(15) -0.21168(13) 0.54283(13) 0.0349(4) Uani 1 1 d . U . . .
H324 H 0.3404 -0.2345 0.5578 0.042 Uiso 1 1 calc R U . . .
C325 C 0.48531(15) -0.22883(12) 0.58016(12) 0.0307(4) Uani 1 1 d . U . . .
H325 H 0.4848 -0.2641 0.6204 0.037 Uiso 1 1 calc R U . . .
C326 C 0.57266(14) -0.19488(11) 0.55925(11) 0.0244(3) Uani 1 1 d . U . . .
H326 H 0.6323 -0.2054 0.5864 0.029 Uiso 1 1 calc R U . . .
C331 C 0.75113(12) -0.16715(10) 0.47060(9) 0.0176(3) Uani 1 1 d . U . . .
C332 C 0.70446(13) -0.26042(10) 0.46329(10) 0.0211(3) Uani 1 1 d . U . . .
H332 H 0.6348 -0.2869 0.4597 0.025 Uiso 1 1 calc R U . . .
C333 C 0.76059(14) -0.31425(11) 0.46125(10) 0.0238(3) Uani 1 1 d . U . . .
H333 H 0.7293 -0.3775 0.4568 0.029 Uiso 1 1 calc R U . . .
C334 C 0.86159(14) -0.27612(12) 0.46564(10) 0.0248(3) Uani 1 1 d . U . . .
H334 H 0.8997 -0.3132 0.4650 0.030 Uiso 1 1 calc R U . . .
C335 C 0.90800(13) -0.18341(12) 0.47100(10) 0.0237(3) Uani 1 1 d . U . . .
H335 H 0.9771 -0.1577 0.4731 0.028 Uiso 1 1 calc R U . . .
C336 C 0.85299(12) -0.12903(11) 0.47323(10) 0.0204(3) Uani 1 1 d . U . . .
H336 H 0.8842 -0.0660 0.4765 0.024 Uiso 1 1 calc R U . . .
C411 C 0.91076(12) 0.15017(10) 0.67090(10) 0.0186(3) Uani 1 1 d . U . . .
C412 C 0.90028(12) 0.20106(10) 0.61176(10) 0.0188(3) Uani 1 1 d . U . . .
H412 H 0.8516 0.1727 0.5565 0.023 Uiso 1 1 calc R U . . .
C413 C 0.96154(13) 0.29385(11) 0.63392(11) 0.0223(3) Uani 1 1 d . U . . .
H413 H 0.9541 0.3290 0.5939 0.027 Uiso 1 1 calc R U . . .
C414 C 1.03316(13) 0.33460(11) 0.71409(11) 0.0255(3) Uani 1 1 d . U . . .
H414 H 1.0753 0.3977 0.7288 0.031 Uiso 1 1 calc R U . . .
C415 C 1.04398(14) 0.28408(12) 0.77341(11) 0.0278(4) Uani 1 1 d . U . . .
H415 H 1.0935 0.3125 0.8284 0.033 Uiso 1 1 calc R U . . .
C416 C 0.98219(14) 0.19179(12) 0.75210(11) 0.0265(3) Uani 1 1 d . U . . .
H416 H 0.9886 0.1572 0.7927 0.032 Uiso 1 1 calc R U . . .
C421 C 0.91831(13) -0.02643(11) 0.66812(10) 0.0223(3) Uani 1 1 d . U . . .
C422 C 0.88353(15) -0.11512(12) 0.67822(11) 0.0283(4) Uani 1 1 d . U . . .
H422 H 0.8170 -0.1422 0.6812 0.034 Uiso 1 1 calc R U . . .
C423 C 0.94634(19) -0.16376(14) 0.68384(12) 0.0386(5) Uani 1 1 d . U . . .
H423 H 0.9229 -0.2240 0.6906 0.046 Uiso 1 1 calc R U . . .
C424 C 1.04346(19) -0.12344(17) 0.67949(13) 0.0437(5) Uani 1 1 d . U . . .
H424 H 1.0861 -0.1567 0.6828 0.052 Uiso 1 1 calc R U . . .
C425 C 1.07875(17) -0.03580(16) 0.67036(13) 0.0396(5) Uani 1 1 d . U . . .
H425 H 1.1456 -0.0089 0.6681 0.047 Uiso 1 1 calc R U . . .
C426 C 1.01684(14) 0.01314(13) 0.66455(11) 0.0287(4) Uani 1 1 d . U . . .
H426 H 1.0413 0.0735 0.6582 0.034 Uiso 1 1 calc R U . . .
C431 C 0.75725(13) 0.01440(11) 0.70938(10) 0.0216(3) Uani 1 1 d . U . . .
C432 C 0.66117(14) 0.01903(11) 0.68008(12) 0.0263(3) Uani 1 1 d . U . . .
H432 H 0.6350 0.0250 0.6247 0.032 Uiso 1 1 calc R U . . .
C433 C 0.60320(17) 0.01495(14) 0.73101(14) 0.0384(5) Uani 1 1 d . U . . .
H433 H 0.5373 0.0175 0.7105 0.046 Uiso 1 1 calc R U . . .
C434 C 0.6419(2) 0.00712(19) 0.81160(16) 0.0562(7) Uani 1 1 d . U . . .
H434 H 0.6024 0.0043 0.8466 0.067 Uiso 1 1 calc R U . . .
C435 C 0.7374(2) 0.0033(2) 0.84189(16) 0.0600(7) Uani 1 1 d . U . . .
H435 H 0.7637 -0.0013 0.8978 0.072 Uiso 1 1 calc R U . . .
C436 C 0.79609(17) 0.00609(16) 0.79062(12) 0.0391(5) Uani 1 1 d . U . . .
H436 H 0.8614 0.0024 0.8110 0.047 Uiso 1 1 calc R U . . .
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'
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
O12 P1 O11 121.69(7) . .
O12 P1 O3 107.00(7) . 2_766
O11 P1 O3 109.74(7) . 2_766
O12 P1 O1 106.61(6) . .
O11 P1 O1 109.65(7) . .
O3 P1 O1 99.95(7) 2_766 .
O22 P2 O21 117.13(8) . .
O22 P2 O1 113.38(8) . .
O21 P2 O1 108.84(7) . .
O22 P2 O2 107.04(7) . .
O21 P2 O2 107.89(7) . .
O1 P2 O2 101.20(6) . .
O32 P3 O31 116.75(7) . .
O32 P3 O3 112.14(7) . .
O31 P3 O3 109.31(7) . .
O32 P3 O2 108.35(7) . .
O31 P3 O2 108.50(6) . .
O3 P3 O2 100.47(6) . .
P2 O1 P1 131.69(8) . .
P3 O2 P2 136.73(7) . .
P3 O3 P1 133.29(8) . 2_766
P2 O21 H1 125.1(13) . .
H1W O1W H2W 91(2) . .
P1C N1 P2C 140.84(10) . .
P4C N2 P3C 135.24(9) . .
N1 P1C C111 109.45(8) . .
N1 P1C C121 114.92(8) . .
C111 P1C C121 106.25(8) . .
N1 P1C C131 109.82(8) . .
C111 P1C C131 108.29(8) . .
C121 P1C C131 107.88(8) . .
N1 P2C C31B 107.8(3) . .
N1 P2C C221 115.57(8) . .
C31B P2C C221 105.5(3) . .
N1 P2C C211 110.97(8) . .
C31B P2C C211 110.4(3) . .
C221 P2C C211 106.38(8) . .
N1 P2C C231 108.03(14) . .
C221 P2C C231 107.54(16) . .
C211 P2C C231 108.10(15) . .
N2 P3C C331 112.84(7) . .
N2 P3C C311 107.53(7) . .
C331 P3C C311 106.17(7) . .
N2 P3C C321 112.03(7) . .
C331 P3C C321 109.26(7) . .
C311 P3C C321 108.75(7) . .
N2 P4C C411 107.80(7) . .
N2 P4C C421 114.20(7) . .
C411 P4C C421 107.30(8) . .
N2 P4C C431 112.25(7) . .
C411 P4C C431 106.13(7) . .
C421 P4C C431 108.73(8) . .
C116 C111 C112 119.60(15) . .
C116 C111 P1C 119.83(13) . .
C112 C111 P1C 120.57(12) . .
C113 C112 C111 120.16(16) . .
C113 C112 H112 119.9 . .
C111 C112 H112 119.9 . .
C112 C113 C114 120.03(18) . .
C112 C113 H113 120.0 . .
C114 C113 H113 120.0 . .
C115 C114 C113 120.03(16) . .
C115 C114 H114 120.0 . .
C113 C114 H114 120.0 . .
C114 C115 C116 120.42(16) . .
C114 C115 H115 119.8 . .
C116 C115 H115 119.8 . .
C115 C116 C111 119.73(16) . .
C115 C116 H116 120.1 . .
C111 C116 H116 120.1 . .
C126 C121 C122 119.78(16) . .
C126 C121 P1C 122.29(13) . .
C122 C121 P1C 117.85(12) . .
C123 C122 C121 119.86(16) . .
C123 C122 H122 120.1 . .
C121 C122 H122 120.1 . .
C124 C123 C122 120.16(18) . .
C124 C123 H123 119.9 . .
C122 C123 H123 119.9 . .
C123 C124 C125 120.26(17) . .
C123 C124 H124 119.9 . .
C125 C124 H124 119.9 . .
C124 C125 C126 119.93(16) . .
C124 C125 H125 120.0 . .
C126 C125 H125 120.0 . .
C125 C126 C121 120.00(16) . .
C125 C126 H126 120.0 . .
C121 C126 H126 120.0 . .
C132 C131 C136 119.40(16) . .
C132 C131 P1C 121.99(13) . .
C136 C131 P1C 118.60(13) . .
C133 C132 C131 120.16(16) . .
C133 C132 H132 119.9 . .
C131 C132 H132 119.9 . .
C132 C133 C134 119.94(18) . .
C132 C133 H133 120.0 . .
C134 C133 H133 120.0 . .
C135 C134 C133 120.10(18) . .
C135 C134 H134 119.9 . .
C133 C134 H134 119.9 . .
C136 C135 C134 120.19(18) . .
C136 C135 H135 119.9 . .
C134 C135 H135 119.9 . .
C135 C136 C131 120.17(18) . .
C135 C136 H136 119.9 . .
C131 C136 H136 119.9 . .
C212 C211 C216 119.80(16) . .
C212 C211 P2C 119.22(13) . .
C216 C211 P2C 120.96(13) . .
C211 C212 C213 119.50(18) . .
C211 C212 H212 120.3 . .
C213 C212 H212 120.3 . .
C214 C213 C212 120.40(18) . .
C214 C213 H213 119.8 . .
C212 C213 H213 119.8 . .
C215 C214 C213 120.32(17) . .
C215 C214 H214 119.8 . .
C213 C214 H214 119.8 . .
C214 C215 C216 120.10(18) . .
C214 C215 H215 119.9 . .
C216 C215 H215 119.9 . .
C215 C216 C211 119.88(17) . .
C215 C216 H216 120.1 . .
C211 C216 H216 120.1 . .
C226 C221 C222 119.91(17) . .
C226 C221 P2C 120.07(14) . .
C222 C221 P2C 119.83(16) . .
C223 C222 C221 119.6(2) . .
C223 C222 H222 120.2 . .
C221 C222 H222 120.2 . .
C222 C223 C224 120.2(2) . .
C222 C223 H223 119.9 . .
C224 C223 H223 119.9 . .
C225 C224 C223 120.06(19) . .
C225 C224 H224 120.0 . .
C223 C224 H224 120.0 . .
C224 C225 C226 120.4(2) . .
C224 C225 H225 119.8 . .
C226 C225 H225 119.8 . .
C225 C226 C221 119.7(2) . .
C225 C226 H226 120.1 . .
C221 C226 H226 120.1 . .
C232 C231 C236 120.0 . .
C232 C231 P2C 119.9(2) . .
C236 C231 P2C 120.1(2) . .
C231 C232 C233 120.0 . .
C231 C232 H232 120.0 . .
C233 C232 H232 120.0 . .
C234 C233 C232 120.0 . .
C234 C233 H233 120.0 . .
C232 C233 H233 120.0 . .
C233 C234 C235 120.0 . .
C233 C234 H234 120.0 . .
C235 C234 H234 120.0 . .
C234 C235 C236 120.0 . .
C234 C235 H235 120.0 . .
C236 C235 H235 120.0 . .
C235 C236 C231 120.0 . .
C235 C236 H236 120.0 . .
C231 C236 H236 120.0 . .
C32B C31B C36B 120.0 . .
C32B C31B P2C 118.6(4) . .
C36B C31B P2C 120.7(4) . .
C33B C32B C31B 120.0 . .
C33B C32B H32B 120.0 . .
C31B C32B H32B 120.0 . .
C32B C33B C34B 120.0 . .
C32B C33B H33B 120.0 . .
C34B C33B H33B 120.0 . .
C33B C34B C35B 120.0 . .
C33B C34B H34B 120.0 . .
C35B C34B H34B 120.0 . .
C36B C35B C34B 120.0 . .
C36B C35B H35B 120.0 . .
C34B C35B H35B 120.0 . .
C35B C36B C31B 120.0 . .
C35B C36B H36B 120.0 . .
C31B C36B H36B 120.0 . .
C312 C311 C316 119.81(15) . .
C312 C311 P3C 120.98(12) . .
C316 C311 P3C 119.09(12) . .
C313 C312 C311 120.04(15) . .
C313 C312 H312 120.0 . .
C311 C312 H312 120.0 . .
C314 C313 C312 119.89(15) . .
C314 C313 H313 120.1 . .
C312 C313 H313 120.1 . .
C313 C314 C315 120.32(16) . .
C313 C314 H314 119.8 . .
C315 C314 H314 119.8 . .
C316 C315 C314 119.92(16) . .
C316 C315 H315 120.0 . .
C314 C315 H315 120.0 . .
C315 C316 C311 120.01(15) . .
C315 C316 H316 120.0 . .
C311 C316 H316 120.0 . .
C322 C321 C326 119.45(15) . .
C322 C321 P3C 119.25(12) . .
C326 C321 P3C 120.74(13) . .
C321 C322 C323 119.70(17) . .
C321 C322 H322 120.2 . .
C323 C322 H322 120.2 . .
C324 C323 C322 120.48(19) . .
C324 C323 H323 119.8 . .
C322 C323 H323 119.8 . .
C325 C324 C323 119.92(16) . .
C325 C324 H324 120.0 . .
C323 C324 H324 120.0 . .
C324 C325 C326 120.44(17) . .
C324 C325 H325 119.8 . .
C326 C325 H325 119.8 . .
C325 C326 C321 119.98(17) . .
C325 C326 H326 120.0 . .
C321 C326 H326 120.0 . .
C332 C331 C336 119.80(14) . .
C332 C331 P3C 124.01(12) . .
C336 C331 P3C 116.18(11) . .
C333 C332 C331 119.65(15) . .
C333 C332 H332 120.2 . .
C331 C332 H332 120.2 . .
C334 C333 C332 120.36(15) . .
C334 C333 H333 119.8 . .
C332 C333 H333 119.8 . .
C333 C334 C335 120.35(15) . .
C333 C334 H334 119.8 . .
C335 C334 H334 119.8 . .
C336 C335 C334 119.85(15) . .
C336 C335 H335 120.1 . .
C334 C335 H335 120.1 . .
C335 C336 C331 119.95(14) . .
C335 C336 H336 120.0 . .
C331 C336 H336 120.0 . .
C412 C411 C416 120.15(14) . .
C412 C411 P4C 120.06(12) . .
C416 C411 P4C 119.79(12) . .
C411 C412 C413 119.73(15) . .
C411 C412 H412 120.1 . .
C413 C412 H412 120.1 . .
C414 C413 C412 119.95(15) . .
C414 C413 H413 120.0 . .
C412 C413 H413 120.0 . .
C413 C414 C415 120.56(15) . .
C413 C414 H414 119.7 . .
C415 C414 H414 119.7 . .
C414 C415 C416 119.82(16) . .
C414 C415 H415 120.1 . .
C416 C415 H415 120.1 . .
C415 C416 C411 119.78(16) . .
C415 C416 H416 120.1 . .
C411 C416 H416 120.1 . .
C422 C421 C426 119.46(16) . .
C422 C421 P4C 121.24(13) . .
C426 C421 P4C 118.54(13) . .
C423 C422 C421 120.06(19) . .
C423 C422 H422 120.0 . .
C421 C422 H422 120.0 . .
C424 C423 C422 119.5(2) . .
C424 C423 H423 120.3 . .
C422 C423 H423 120.3 . .
C425 C424 C423 120.84(19) . .
C425 C424 H424 119.6 . .
C423 C424 H424 119.6 . .
C424 C425 C426 120.1(2) . .
C424 C425 H425 119.9 . .
C426 C425 H425 119.9 . .
C425 C426 C421 120.00(19) . .
C425 C426 H426 120.0 . .
C421 C426 H426 120.0 . .
C432 C431 C436 119.87(16) . .
C432 C431 P4C 117.77(13) . .
C436 C431 P4C 122.06(14) . .
C433 C432 C431 120.59(19) . .
C433 C432 H432 119.7 . .
C431 C432 H432 119.7 . .
C434 C433 C432 119.5(2) . .
C434 C433 H433 120.3 . .
C432 C433 H433 120.3 . .
C433 C434 C435 120.66(19) . .
C433 C434 H434 119.7 . .
C435 C434 H434 119.7 . .
C434 C435 C436 120.3(2) . .
C434 C435 H435 119.8 . .
C436 C435 H435 119.8 . .
C431 C436 C435 119.0(2) . .
C431 C436 H436 120.5 . .
C435 C436 H436 120.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O12 1.4712(11) .
P1 O11 1.4791(12) .
P1 O3 1.6200(12) 2_766
P1 O1 1.6264(12) .
P2 O22 1.4627(13) .
P2 O21 1.5098(12) .
P2 O1 1.5874(12) .
P2 O2 1.6064(12) .
P3 O32 1.4695(12) .
P3 O31 1.5099(12) .
P3 O3 1.5896(12) .
P3 O2 1.6015(12) .
O3 P1 1.6201(12) 2_766
O21 H1 0.95(2) .
O1W H1W 0.970(17) .
O1W H2W 0.974(17) .
N1 P1C 1.5792(15) .
N1 P2C 1.5811(15) .
N2 P4C 1.5885(14) .
N2 P3C 1.5911(13) .
P1C C111 1.7953(16) .
P1C C121 1.8009(17) .
P1C C131 1.8014(17) .
P2C C31B 1.708(4) .
P2C C221 1.7961(17) .
P2C C211 1.8042(17) .
P2C C231 1.846(3) .
P3C C331 1.7982(15) .
P3C C311 1.8007(16) .
P3C C321 1.8018(15) .
P4C C411 1.7900(15) .
P4C C421 1.7901(17) .
P4C C431 1.8036(16) .
C111 C116 1.396(2) .
C111 C112 1.398(2) .
C112 C113 1.388(2) .
C112 H112 0.9500 .
C113 C114 1.388(3) .
C113 H113 0.9500 .
C114 C115 1.386(3) .
C114 H114 0.9500 .
C115 C116 1.391(2) .
C115 H115 0.9500 .
C116 H116 0.9500 .
C121 C126 1.397(2) .
C121 C122 1.399(2) .
C122 C123 1.391(2) .
C122 H122 0.9500 .
C123 C124 1.389(3) .
C123 H123 0.9500 .
C124 C125 1.390(3) .
C124 H124 0.9500 .
C125 C126 1.393(2) .
C125 H125 0.9500 .
C126 H126 0.9500 .
C131 C132 1.394(2) .
C131 C136 1.400(2) .
C132 C133 1.389(2) .
C132 H132 0.9500 .
C133 C134 1.389(3) .
C133 H133 0.9500 .
C134 C135 1.388(3) .
C134 H134 0.9500 .
C135 C136 1.381(3) .
C135 H135 0.9500 .
C136 H136 0.9500 .
C211 C212 1.392(2) .
C211 C216 1.397(2) .
C212 C213 1.393(3) .
C212 H212 0.9500 .
C213 C214 1.380(3) .
C213 H213 0.9500 .
C214 C215 1.378(3) .
C214 H214 0.9500 .
C215 C216 1.390(2) .
C215 H215 0.9500 .
C216 H216 0.9500 .
C221 C226 1.394(3) .
C221 C222 1.396(3) .
C222 C223 1.390(3) .
C222 H222 0.9500 .
C223 C224 1.391(4) .
C223 H223 0.9500 .
C224 C225 1.377(4) .
C224 H224 0.9500 .
C225 C226 1.393(3) .
C225 H225 0.9500 .
C226 H226 0.9500 .
C231 C232 1.3900 .
C231 C236 1.3900 .
C232 C233 1.3900 .
C232 H232 0.9500 .
C233 C234 1.3900 .
C233 H233 0.9500 .
C234 C235 1.3900 .
C234 H234 0.9500 .
C235 C236 1.3900 .
C235 H235 0.9500 .
C236 H236 0.9500 .
C31B C32B 1.3900 .
C31B C36B 1.3900 .
C32B C33B 1.3900 .
C32B H32B 0.9500 .
C33B C34B 1.3900 .
C33B H33B 0.9500 .
C34B C35B 1.3900 .
C34B H34B 0.9500 .
C35B C36B 1.3900 .
C35B H35B 0.9500 .
C36B H36B 0.9500 .
C311 C312 1.395(2) .
C311 C316 1.400(2) .
C312 C313 1.393(2) .
C312 H312 0.9500 .
C313 C314 1.388(2) .
C313 H313 0.9500 .
C314 C315 1.397(2) .
C314 H314 0.9500 .
C315 C316 1.386(2) .
C315 H315 0.9500 .
C316 H316 0.9500 .
C321 C322 1.393(2) .
C321 C326 1.399(2) .
C322 C323 1.397(2) .
C322 H322 0.9500 .
C323 C324 1.384(3) .
C323 H323 0.9500 .
C324 C325 1.378(3) .
C324 H324 0.9500 .
C325 C326 1.391(2) .
C325 H325 0.9500 .
C326 H326 0.9500 .
C331 C332 1.398(2) .
C331 C336 1.403(2) .
C332 C333 1.392(2) .
C332 H332 0.9500 .
C333 C334 1.382(2) .
C333 H333 0.9500 .
C334 C335 1.396(2) .
C334 H334 0.9500 .
C335 C336 1.387(2) .
C335 H335 0.9500 .
C336 H336 0.9500 .
C411 C412 1.391(2) .
C411 C416 1.396(2) .
C412 C413 1.395(2) .
C412 H412 0.9500 .
C413 C414 1.382(2) .
C413 H413 0.9500 .
C414 C415 1.390(2) .
C414 H414 0.9500 .
C415 C416 1.391(2) .
C415 H415 0.9500 .
C416 H416 0.9500 .
C421 C422 1.399(2) .
C421 C426 1.400(2) .
C422 C423 1.394(3) .
C422 H422 0.9500 .
C423 C424 1.389(3) .
C423 H423 0.9500 .
C424 C425 1.378(3) .
C424 H424 0.9500 .
C425 C426 1.387(3) .
C425 H425 0.9500 .
C426 H426 0.9500 .
C431 C432 1.391(3) .
C431 C436 1.391(3) .
C432 C433 1.387(2) .
C432 H432 0.9500 .
C433 C434 1.378(4) .
C433 H433 0.9500 .
C434 C435 1.378(4) .
C434 H434 0.9500 .
C435 C436 1.402(3) .
C435 H435 0.9500 .
C436 H436 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O21 H1 O31 0.95(2) 1.46(2) 2.4087(17) 174.6(17) 2_766
O1W H2W O32 0.974(17) 1.953(17) 2.918(2) 171(2) 2_766
O1W H1W O11 0.970(17) 1.845(18) 2.803(2) 169(2) .
