#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:34:44 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179668 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/21/4512165.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_4512165
loop_
_publ_author_name
'Zaręba, Jan K.'
'Białek, Michał J.'
'Janczak, Jan'
'Zoń, Jerzy'
'Dobosz, Agnieszka'
_publ_section_title
;
 Extending the Family of Tetrahedral Tectons: Phenyl Embraces in
 Supramolecular Polymers of Tetraphenylmethane-based Tetraphosphonic Acid
 Templated by Organic Bases
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              6143
_journal_paper_doi               10.1021/cg501348g
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C25 H17 O12 P4, 2(C6 H18 N2), 2(H2 O)'
_chemical_formula_sum            'C37 H57 N4 O14 P4'
_chemical_formula_weight         905.71
_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                97.820(10)
_cell_angle_beta                 110.20(2)
_cell_angle_gamma                108.590(10)
_cell_formula_units_Z            2
_cell_length_a                   13.597(2)
_cell_length_b                   13.866(2)
_cell_length_c                   15.312(3)
_cell_measurement_reflns_used    2756
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.73
_cell_volume                     2467.7(9)
_computing_cell_refinement
;
Oxofrord Diffraction (2006). CrysAlis CCD, Version 172.32.6
;
_computing_data_collection
;
Oxofrord Diffraction (2006). CrysAlis CCD, Version 172.32.6
;
_computing_data_reduction
;
Oxofrord Diffraction (2006). CrysAlis CCD, Version 172.32.6
;
_computing_molecular_graphics
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       ω-scan
_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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.1287
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33544
_diffrn_reflns_theta_full        27.90
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.9744
_exptl_absorpt_correction_T_min  0.9524
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis Red, Version 172.32.6, Oxford Diffraction 
Poland, 2006
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      1.22
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         11697
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1915
_refine_ls_R_factor_gt           0.0748
_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)+(0.0720P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1647
_reflns_number_gt                5909
_reflns_number_total             11697
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cg501348g_si_002.cif
_cod_data_source_block           Adduct5b
_cod_depositor_comments
'Adding full bibliography for 4512161--4512166.cif.'
_cod_original_cell_volume        2467.7(7)
_cod_database_code               4512165
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
P11 P 0.22128(7) 0.60869(6) 0.14917(6) 0.0418(2) Uani 1 1 d . . .
O11 O 0.1888(2) 0.6439(3) 0.0631(3) 0.0501(10) Uani 0.696(4) 1 d P A -1
O12 O 0.1839(2) 0.4907(2) 0.1361(2) 0.0470(10) Uani 0.696(4) 1 d P A -1
O13 O 0.1735(3) 0.6570(3) 0.2205(3) 0.0652(12) Uani 0.696(4) 1 d P A -1
O14 O 0.1769(5) 0.5475(6) 0.2059(6) 0.049(2) Uani 0.304(4) 1 d P A -2
O15 O 0.1774(5) 0.6950(6) 0.1268(6) 0.046(2) Uani 0.304(4) 1 d P A -2
O16 O 0.2011(5) 0.5342(6) 0.0513(5) 0.046(2) Uani 0.304(4) 1 d P A -2
P21 P 0.87648(9) 0.92900(7) 0.82215(6) 0.0535(3) Uani 1 1 d . . .
O21 O 0.8646(3) 1.0269(2) 0.85865(17) 0.0818(8) Uani 1 1 d . . .
O22 O 0.8137(2) 0.82727(18) 0.83999(15) 0.0619(7) Uani 1 1 d . . .
O23 O 1.01098(19) 0.95793(17) 0.86829(14) 0.0607(7) Uani 1 1 d . . .
P31 P 1.04320(8) 0.58158(7) 0.38135(7) 0.0478(2) Uani 1 1 d . . .
O31 O 1.0421(3) 0.5540(3) 0.2849(3) 0.0456(11) Uani 0.685(7) 1 d P B -3
O32 O 1.1604(4) 0.6520(4) 0.4613(3) 0.0642(14) Uani 0.685(7) 1 d P B -3
O33 O 0.9911(4) 0.4783(3) 0.4096(4) 0.0580(15) Uani 0.685(7) 1 d P B -3
O34 O 1.1142(6) 0.6010(7) 0.4840(6) 0.045(2) Uani 0.315(7) 1 d P B -4
O35 O 0.9583(10) 0.4700(8) 0.3286(10) 0.127(6) Uani 0.315(7) 1 d P B -4
O36 O 1.1241(12) 0.6351(11) 0.3331(8) 0.094(5) Uani 0.315(7) 1 d P B -4
P41 P 0.87509(8) 1.22023(7) 0.22814(7) 0.0549(3) Uani 1 1 d . . .
O41 O 0.7837(2) 1.2615(2) 0.1948(2) 0.0816(8) Uani 1 1 d . . .
O42 O 0.9136(2) 1.18545(18) 0.15326(17) 0.0678(7) Uani 1 1 d . . .
O43 O 0.98334(19) 1.30518(16) 0.31443(18) 0.0624(7) Uani 1 1 d . . .
H431 H 0.9666 1.3510 0.3380 0.094 Uiso 1 1 calc R . .
C1 C 0.7404(2) 0.83295(19) 0.38233(18) 0.0264(6) Uani 1 1 d . . .
C11 C 0.6119(2) 0.7719(2) 0.32183(18) 0.0293(6) Uani 1 1 d . . .
C12 C 0.5414(2) 0.8250(2) 0.3206(2) 0.0378(7) Uani 1 1 d . A .
H12 H 0.5738 0.8959 0.3556 0.045 Uiso 1 1 calc R . .
C13 C 0.4251(3) 0.7772(2) 0.2698(2) 0.0448(8) Uani 1 1 d . . .
H13 H 0.3806 0.8158 0.2708 0.054 Uiso 1 1 calc R A .
C14 C 0.3735(2) 0.6708(2) 0.2165(2) 0.0380(7) Uani 1 1 d . A .
C15 C 0.4437(2) 0.6181(2) 0.2155(2) 0.0377(7) Uani 1 1 d . . .
H15 H 0.4117 0.5477 0.1793 0.045 Uiso 1 1 calc R A .
C16 C 0.5604(2) 0.6672(2) 0.2669(2) 0.0379(7) Uani 1 1 d . A .
H16 H 0.6054 0.6293 0.2646 0.046 Uiso 1 1 calc R . .
C21 C 0.7684(2) 0.85974(19) 0.49175(19) 0.0276(6) Uani 1 1 d . . .
C22 C 0.6899(2) 0.8272(2) 0.5296(2) 0.0346(7) Uani 1 1 d . . .
H22 H 0.6132 0.7912 0.4880 0.042 Uiso 1 1 calc R . .
C23 C 0.7220(3) 0.8468(2) 0.6282(2) 0.0446(8) Uani 1 1 d . . .
H23 H 0.6665 0.8228 0.6515 0.053 Uiso 1 1 calc R . .
C24 C 0.8355(3) 0.9017(2) 0.6938(2) 0.0402(7) Uani 1 1 d . . .
C25 C 0.9143(2) 0.9352(2) 0.6552(2) 0.0395(7) Uani 1 1 d . . .
H25 H 0.9907 0.9734 0.6967 0.047 Uiso 1 1 calc R . .
C26 C 0.8824(2) 0.9135(2) 0.5574(2) 0.0401(7) Uani 1 1 d . . .
H26 H 0.9380 0.9351 0.5339 0.048 Uiso 1 1 calc R . .
C31 C 0.8117(2) 0.7679(2) 0.37160(19) 0.0297(6) Uani 1 1 d . . .
C32 C 0.7997(2) 0.6803(2) 0.4087(2) 0.0399(7) Uani 1 1 d . B .
H32 H 0.7453 0.6603 0.4337 0.048 Uiso 1 1 calc R . .
C33 C 0.8654(3) 0.6224(2) 0.4096(2) 0.0449(8) Uani 1 1 d . . .
H33 H 0.8540 0.5641 0.4343 0.054 Uiso 1 1 calc R B .
C34 C 0.9491(2) 0.6507(2) 0.3737(2) 0.0365(7) Uani 1 1 d . B .
C35 C 0.9600(3) 0.7367(2) 0.3360(2) 0.0465(8) Uani 1 1 d . . .
H35 H 1.0140 0.7570 0.3107 0.056 Uiso 1 1 calc R B .
C36 C 0.8929(2) 0.7928(2) 0.3350(2) 0.0406(7) Uani 1 1 d . B .
H36 H 0.9028 0.8498 0.3085 0.049 Uiso 1 1 calc R . .
C41 C 0.7739(2) 0.9336(2) 0.34749(19) 0.0300(6) Uani 1 1 d . . .
C42 C 0.7478(3) 0.9210(2) 0.2505(2) 0.0401(7) Uani 1 1 d . . .
H42 H 0.7098 0.8532 0.2081 0.048 Uiso 1 1 calc R . .
C43 C 0.7766(3) 1.0068(2) 0.2150(2) 0.0461(8) Uani 1 1 d . . .
H43 H 0.7587 0.9955 0.1491 0.055 Uiso 1 1 calc R . .
C44 C 0.8317(2) 1.1095(2) 0.2745(2) 0.0393(7) Uani 1 1 d . . .
C45 C 0.8511(3) 1.1225(2) 0.3710(2) 0.0433(8) Uani 1 1 d . . .
H45 H 0.8836 1.1905 0.4125 0.052 Uiso 1 1 calc R . .
C46 C 0.8229(2) 1.0356(2) 0.4072(2) 0.0379(7) Uani 1 1 d . . .
H46 H 0.8372 1.0464 0.4724 0.045 Uiso 1 1 calc R . .
N51 N 0.9012(2) 0.8074(2) 0.02405(18) 0.0471(7) Uani 1 1 d . . .
H511 H 0.9224 0.7531 0.0276 0.071 Uiso 1 1 calc R . .
H512 H 0.9587 0.8665 0.0653 0.071 Uiso 1 1 calc R . .
H513 H 0.8820 0.8141 -0.0359 0.071 Uiso 1 1 calc R . .
C52 C 0.8032(3) 0.7885(3) 0.0489(2) 0.0595(10) Uani 1 1 d . . .
H521 H 0.7857 0.8511 0.0516 0.089 Uiso 1 1 calc R . .
H522 H 0.8236 0.7774 0.1129 0.089 Uiso 1 1 calc R . .
C53 C 0.6995(3) 0.6956(3) -0.0211(2) 0.0509(9) Uani 1 1 d . . .
H531 H 0.7120 0.6312 -0.0154 0.076 Uiso 1 1 calc R . .
H532 H 0.6863 0.7004 -0.0864 0.076 Uiso 1 1 calc R . .
C54 C 0.5956(3) 0.6898(3) -0.0033(3) 0.0667(10) Uani 1 1 d . . .
H541 H 0.5891 0.7576 -0.0022 0.100 Uiso 1 1 calc R . .
H542 H 0.6078 0.6796 0.0604 0.100 Uiso 1 1 calc R . .
C55 C 0.4832(3) 0.6038(3) -0.0761(3) 0.0612(10) Uani 1 1 d . . .
H551 H 0.4755 0.6067 -0.1410 0.092 Uiso 1 1 calc R . .
H552 H 0.4839 0.5353 -0.0699 0.092 Uiso 1 1 calc R . .
C56 C 0.3823(3) 0.6136(3) -0.0632(3) 0.0609(10) Uani 1 1 d . . .
H561 H 0.3901 0.6096 0.0015 0.091 Uiso 1 1 calc R . .
H562 H 0.3835 0.6831 -0.0675 0.091 Uiso 1 1 calc R . .
C57 C 0.2686(3) 0.5321(3) -0.1344(3) 0.0601(10) Uani 1 1 d . . .
H571 H 0.2646 0.5263 -0.1995 0.090 Uiso 1 1 calc R . .
H572 H 0.2597 0.4637 -0.1219 0.090 Uiso 1 1 calc R . .
N58 N 0.1754(2) 0.5610(2) -0.1269(2) 0.0579(8) Uani 1 1 d . . .
H581 H 0.1833 0.5726 -0.0657 0.087 Uiso 1 1 calc R . .
H582 H 0.1086 0.5084 -0.1647 0.087 Uiso 1 1 calc R . .
H583 H 0.1784 0.6194 -0.1457 0.087 Uiso 1 1 calc R . .
N61 N 0.1717(2) 0.3592(2) 0.2544(2) 0.0584(8) Uani 1 1 d . . .
H611 H 0.1821 0.4095 0.2241 0.088 Uiso 1 1 calc R . .
H612 H 0.0989 0.3319 0.2452 0.088 Uiso 1 1 calc R . .
H613 H 0.1899 0.3084 0.2308 0.088 Uiso 1 1 calc R . .
C62 C 0.2436(4) 0.4045(3) 0.3574(3) 0.0792(12) Uani 1 1 d . . .
H621 H 0.2278 0.4635 0.3820 0.119 Uiso 1 1 calc R . .
H622 H 0.2258 0.3517 0.3913 0.119 Uiso 1 1 calc R . .
C63 C 0.3618(4) 0.4404(3) 0.3763(3) 0.0807(12) Uani 1 1 d . . .
H631 H 0.3807 0.4972 0.3467 0.121 Uiso 1 1 calc R . .
H632 H 0.3759 0.3827 0.3466 0.121 Uiso 1 1 calc R . .
C64 C 0.4415(3) 0.4811(4) 0.4877(3) 0.0928(15) Uani 1 1 d . . .
H641 H 0.4250 0.5373 0.5168 0.139 Uiso 1 1 calc R . .
H642 H 0.4219 0.4235 0.5164 0.139 Uiso 1 1 calc R . .
N71 N 0.2179(3) 0.8546(2) 0.0489(2) 0.0708(9) Uani 1 1 d D C .
H71A H 0.1927 0.8938 0.0795 0.106 Uiso 1 1 calc R . .
H71B H 0.2105 0.7957 0.0678 0.106 Uiso 1 1 calc R . .
H71C H 0.1775 0.8377 -0.0147 0.106 Uiso 1 1 calc R . .
C72 C 0.3389(4) 0.9150(7) 0.0723(5) 0.176(4) Uani 1 1 d D . .
H72A H 0.3793 0.9218 0.1403 0.264 Uiso 1 1 calc R C .
H72B H 0.3445 0.9857 0.0682 0.264 Uiso 1 1 calc R . .
C73 C 0.4104(11) 0.8899(7) 0.0245(10) 0.158(5) Uani 0.50 1 d PD C -5
H73A H 0.3656 0.8541 -0.0440 0.236 Uiso 0.50 1 calc PR C -5
H73B H 0.4478 0.8469 0.0552 0.236 Uiso 0.50 1 calc PR C -5
C731 C 0.3782(8) 0.9838(9) 0.0340(11) 0.159(6) Uani 0.50 1 d PD C -6
H73C H 0.3805 1.0509 0.0650 0.239 Uiso 0.50 1 calc PR C -6
H73D H 0.3264 0.9638 -0.0337 0.239 Uiso 0.50 1 calc PR C -6
C74 C 0.4949(6) 0.9989(9) 0.0406(7) 0.236(5) Uani 1 1 d D . .
H74A H 0.4677 1.0521 0.0581 0.354 Uiso 1 1 calc R C .
H74B H 0.5678 1.0128 0.0922 0.354 Uiso 1 1 calc R . .
O1W O 0.9472(3) 0.6312(2) 0.0491(3) 0.1167(12) Uani 1 1 d . . .
O2W O 0.6955(4) 1.3273(4) 0.3329(4) 0.1789(18) Uani 1 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'
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
O14 P11 O11 143.5(3) .
O14 P11 O12 51.7(3) .
O11 P11 O12 117.40(19) .
O14 P11 O15 115.8(4) .
O11 P11 O15 48.0(3) .
O12 P11 O15 143.2(3) .
O14 P11 O16 110.9(4) .
O11 P11 O16 62.6(3) .
O12 P11 O16 60.6(3) .
O15 P11 O16 109.3(4) .
O14 P11 O13 59.2(3) .
O11 P11 O13 107.7(2) .
O12 P11 O13 109.17(19) .
O15 P11 O13 61.2(3) .
O16 P11 O13 151.2(2) .
O14 P11 C14 106.7(3) .
O11 P11 C14 109.58(16) .
O12 P11 C14 108.71(15) .
O15 P11 C14 108.1(3) .
O16 P11 C14 105.4(2) .
O13 P11 C14 103.39(16) .
O21 P21 O22 119.23(16) .
O21 P21 O23 104.74(15) .
O22 P21 O23 110.41(14) .
O21 P21 C24 110.09(14) .
O22 P21 C24 106.49(13) .
O23 P21 C24 105.05(14) .
O34 P31 O31 141.5(3) .
O34 P31 O35 116.2(6) .
O31 P31 O35 71.3(7) .
O34 P31 O32 38.0(3) .
O31 P31 O32 114.4(2) .
O35 P31 O32 145.9(4) .
O34 P31 O33 73.8(4) .
O31 P31 O33 110.23(19) .
O35 P31 O33 43.4(5) .
O32 P31 O33 109.7(2) .
O34 P31 O36 107.7(5) .
O31 P31 O36 46.5(5) .
O35 P31 O36 116.7(7) .
O32 P31 O36 71.4(5) .
O33 P31 O36 144.6(4) .
O34 P31 C34 107.9(3) .
O31 P31 C34 107.37(16) .
O35 P31 C34 100.8(4) .
O32 P31 C34 108.47(17) .
O33 P31 C34 106.32(16) .
O36 P31 C34 106.6(3) .
O41 P41 O42 115.76(16) .
O41 P41 O43 110.79(15) .
O42 P41 O43 106.63(15) .
O41 P41 C44 111.24(14) .
O42 P41 C44 106.70(14) .
O43 P41 C44 105.06(14) .
P41 O43 H431 109.5 .
C11 C1 C21 111.0(2) .
C11 C1 C31 113.3(2) .
C21 C1 C31 103.8(2) .
C11 C1 C41 105.7(2) .
C21 C1 C41 112.3(2) .
C31 C1 C41 110.9(2) .
C12 C11 C16 116.9(2) .
C12 C11 C1 118.0(2) .
C16 C11 C1 125.1(2) .
C13 C12 C11 122.5(3) .
C13 C12 H12 118.7 .
C11 C12 H12 118.7 .
C12 C13 C14 120.3(3) .
C12 C13 H13 119.8 .
C14 C13 H13 119.8 .
C15 C14 C13 117.4(3) .
C15 C14 P11 122.3(2) .
C13 C14 P11 120.2(2) .
C14 C15 C16 121.6(3) .
C14 C15 H15 119.2 .
C16 C15 H15 119.2 .
C15 C16 C11 121.2(3) .
C15 C16 H16 119.4 .
C11 C16 H16 119.4 .
C22 C21 C26 117.0(3) .
C22 C21 C1 124.4(2) .
C26 C21 C1 118.4(2) .
C21 C22 C23 121.4(3) .
C21 C22 H22 119.3 .
C23 C22 H22 119.3 .
C22 C23 C24 121.6(3) .
C22 C23 H23 119.2 .
C24 C23 H23 119.2 .
C25 C24 C23 116.8(3) .
C25 C24 P21 121.8(2) .
C23 C24 P21 121.4(2) .
C26 C25 C24 121.4(3) .
C26 C25 H25 119.3 .
C24 C25 H25 119.3 .
C25 C26 C21 121.8(3) .
C25 C26 H26 119.1 .
C21 C26 H26 119.1 .
C36 C31 C32 115.9(3) .
C36 C31 C1 125.9(2) .
C32 C31 C1 118.0(2) .
C33 C32 C31 122.5(3) .
C33 C32 H32 118.8 .
C31 C32 H32 118.8 .
C32 C33 C34 120.5(3) .
C32 C33 H33 119.7 .
C34 C33 H33 119.7 .
C35 C34 C33 116.9(3) .
C35 C34 P31 121.5(2) .
C33 C34 P31 121.5(2) .
C36 C35 C34 121.6(3) .
C36 C35 H35 119.2 .
C34 C35 H35 119.2 .
C35 C36 C31 122.5(3) .
C35 C36 H36 118.7 .
C31 C36 H36 118.7 .
C42 C41 C46 117.7(3) .
C42 C41 C1 118.2(2) .
C46 C41 C1 124.0(2) .
C43 C42 C41 121.2(3) .
C43 C42 H42 119.4 .
C41 C42 H42 119.4 .
C42 C43 C44 121.9(3) .
C42 C43 H43 119.1 .
C44 C43 H43 119.1 .
C45 C44 C43 116.8(3) .
C45 C44 P41 121.8(2) .
C43 C44 P41 121.3(2) .
C44 C45 C46 121.2(3) .
C44 C45 H45 119.4 .
C46 C45 H45 119.4 .
C41 C46 C45 120.9(3) .
C41 C46 H46 119.5 .
C45 C46 H46 119.5 .
C52 N51 H511 109.5 .
C52 N51 H512 109.5 .
H511 N51 H512 109.5 .
C52 N51 H513 109.5 .
H511 N51 H513 109.5 .
H512 N51 H513 109.5 .
N51 C52 C53 113.3(3) .
N51 C52 H521 108.9 .
C53 C52 H521 108.9 .
N51 C52 H522 108.9 .
C53 C52 H522 108.9 .
H521 C52 H522 107.7 .
C52 C53 C54 111.8(3) .
C52 C53 H531 109.3 .
C54 C53 H531 109.3 .
C52 C53 H532 109.3 .
C54 C53 H532 109.3 .
H531 C53 H532 107.9 .
C53 C54 C55 116.1(3) .
C53 C54 H541 108.3 .
C55 C54 H541 108.3 .
C53 C54 H542 108.3 .
C55 C54 H542 108.3 .
H541 C54 H542 107.4 .
C56 C55 C54 113.0(3) .
C56 C55 H551 109.0 .
C54 C55 H551 109.0 .
C56 C55 H552 109.0 .
C54 C55 H552 109.0 .
H551 C55 H552 107.8 .
C57 C56 C55 115.5(3) .
C57 C56 H561 108.4 .
C55 C56 H561 108.4 .
C57 C56 H562 108.4 .
C55 C56 H562 108.4 .
H561 C56 H562 107.5 .
N58 C57 C56 110.6(3) .
N58 C57 H571 109.5 .
C56 C57 H571 109.5 .
N58 C57 H572 109.5 .
C56 C57 H572 109.5 .
H571 C57 H572 108.1 .
C57 N58 H581 109.5 .
C57 N58 H582 109.5 .
H581 N58 H582 109.5 .
C57 N58 H583 109.5 .
H581 N58 H583 109.5 .
H582 N58 H583 109.5 .
C62 N61 H611 109.5 .
C62 N61 H612 109.5 .
H611 N61 H612 109.5 .
C62 N61 H613 109.5 .
H611 N61 H613 109.5 .
H612 N61 H613 109.5 .
C63 C62 N61 111.4(4) .
C63 C62 H621 109.4 .
N61 C62 H621 109.4 .
C63 C62 H622 109.4 .
N61 C62 H622 109.4 .
H621 C62 H622 108.0 .
C62 C63 C64 112.5(4) .
C62 C63 H631 109.1 .
C64 C63 H631 109.1 .
C62 C63 H632 109.1 .
C64 C63 H632 109.1 .
H631 C63 H632 107.8 .
C64 C64 C63 116.0(5) 2_666
C64 C64 H641 108.3 2_666
C63 C64 H641 108.3 .
C64 C64 H642 108.3 2_666
C63 C64 H642 108.3 .
H641 C64 H642 107.4 .
C72 N71 H71A 109.5 .
C72 N71 H71B 109.5 .
H71A N71 H71B 109.5 .
C72 N71 H71C 109.5 .
H71A N71 H71C 109.5 .
H71B N71 H71C 109.5 .
C731 C72 N71 126.9(7) .
C731 C72 C73 65.6(3) .
N71 C72 C73 128.2(7) .
C731 C72 H72A 120.5 .
N71 C72 H72A 105.2 .
C73 C72 H72A 105.2 .
C731 C72 H72B 40.0 .
N71 C72 H72B 105.2 .
C73 C72 H72B 105.2 .
H72A C72 H72B 106.0 .
C72 C73 C74 101.2(5) .
C72 C73 H73A 111.5 .
C74 C73 H73A 111.5 .
C72 C73 H73B 111.5 .
C74 C73 H73B 111.5 .
H73A C73 H73B 109.3 .
C72 C731 C74 114.4(7) .
C72 C731 H73C 108.7 .
C74 C731 H73C 108.7 .
C72 C731 H73D 108.7 .
C74 C731 H73D 108.7 .
H73C C731 H73D 107.6 .
C74 C74 C731 113.9(11) 2_675
C74 C74 C73 106.5(13) 2_675
C731 C74 C73 60.2(3) .
C74 C74 H74A 110.4 2_675
C731 C74 H74A 51.5 .
C73 C74 H74A 110.4 .
C74 C74 H74B 110.4 2_675
C731 C74 H74B 135.5 .
C73 C74 H74B 110.4 .
H74A C74 H74B 108.6 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P11 O14 1.440(6) .
P11 O11 1.442(3) .
P11 O12 1.512(3) .
P11 O15 1.528(7) .
P11 O16 1.583(6) .
P11 O13 1.623(3) .
P11 C14 1.799(3) .
P21 O21 1.476(3) .
P21 O22 1.514(2) .
P21 O23 1.602(3) .
P21 C24 1.796(3) .
P31 O34 1.466(7) .
P31 O31 1.468(3) .
P31 O35 1.502(10) .
P31 O32 1.525(4) .
P31 O33 1.573(3) .
P31 O36 1.580(11) .
P31 C34 1.810(3) .
P41 O41 1.493(2) .
P41 O42 1.499(3) .
P41 O43 1.558(2) .
P41 C44 1.793(3) .
O43 H431 0.8200 .
C1 C11 1.534(4) .
C1 C21 1.546(4) .
C1 C31 1.552(4) .
C1 C41 1.551(4) .
C11 C12 1.380(4) .
C11 C16 1.385(4) .
C12 C13 1.373(4) .
C12 H12 0.9300 .
C13 C14 1.396(4) .
C13 H13 0.9300 .
C14 C15 1.379(4) .
C15 C16 1.380(4) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C21 C22 1.368(4) .
C21 C26 1.397(4) .
C22 C23 1.379(4) .
C22 H22 0.9300 .
C23 C24 1.394(4) .
C23 H23 0.9300 .
C24 C25 1.381(4) .
C25 C26 1.367(4) .
C25 H25 0.9300 .
C26 H26 0.9300 .
C31 C36 1.374(4) .
C31 C32 1.397(4) .
C32 C33 1.375(4) .
C32 H32 0.9300 .
C33 C34 1.399(4) .
C33 H33 0.9300 .
C34 C35 1.383(4) .
C35 C36 1.372(4) .
C35 H35 0.9300 .
C36 H36 0.9300 .
C41 C42 1.374(4) .
C41 C46 1.381(4) .
C42 C43 1.376(4) .
C42 H42 0.9300 .
C43 C44 1.384(4) .
C43 H43 0.9300 .
C44 C45 1.383(4) .
C45 C46 1.393(4) .
C45 H45 0.9300 .
C46 H46 0.9300 .
N51 C52 1.464(4) .
N51 H511 0.8900 .
N51 H512 0.8900 .
N51 H513 0.8900 .
C52 C53 1.490(4) .
C52 H521 0.9700 .
C52 H522 0.9700 .
C53 C54 1.509(5) .
C53 H531 0.9700 .
C53 H532 0.9700 .
C54 C55 1.517(5) .
C54 H541 0.9700 .
C54 H542 0.9700 .
C55 C56 1.496(5) .
C55 H551 0.9700 .
C55 H552 0.9700 .
C56 C57 1.497(4) .
C56 H561 0.9700 .
C56 H562 0.9700 .
C57 N58 1.481(4) .
C57 H571 0.9700 .
C57 H572 0.9700 .
N58 H581 0.8900 .
N58 H582 0.8900 .
N58 H583 0.8900 .
N61 C62 1.454(4) .
N61 H611 0.8900 .
N61 H612 0.8900 .
N61 H613 0.8900 .
C62 C63 1.430(5) .
C62 H621 0.9700 .
C62 H622 0.9700 .
C63 C64 1.573(5) .
C63 H631 0.9700 .
C63 H632 0.9700 .
C64 C64 1.397(7) 2_666
C64 H641 0.9700 .
C64 H642 0.9700 .
N71 C72 1.473(4) .
N71 H71A 0.8900 .
N71 H71B 0.8900 .
N71 H71C 0.8900 .
C72 C731 1.257(11) .
C72 C73 1.497(5) .
C72 H72A 0.9700 .
C72 H72B 0.9700 .
C73 C74 1.503(5) .
C73 H73A 0.9700 .
C73 H73B 0.9700 .
C731 C74 1.498(5) .
C731 H73C 0.9700 .
C731 H73D 0.9700 .
C74 C74 1.301(15) 2_675
C74 H74A 0.9700 .
C74 H74B 0.9700 .
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
O43 H431 O35 0.82 1.71 2.408(9) 141.5 1_565
O43 H431 O33 0.82 1.81 2.584(4) 156.9 1_565
N51 H511 O1W 0.89 1.87 2.751(4) 167.8 .
N51 H512 O21 0.89 2.16 2.985(4) 154.7 2_776
N51 H512 O23 0.89 2.35 3.072(3) 138.1 2_776
N51 H513 O22 0.89 1.87 2.746(3) 168.1 1_554
N58 H581 O16 0.89 1.90 2.720(7) 153.3 .
N58 H581 O11 0.89 2.05 2.900(5) 159.7 .
N58 H582 O31 0.89 2.04 2.855(5) 151.3 2_665
N58 H583 O41 0.89 1.90 2.769(4) 164.3 2_675
N61 H611 O12 0.89 1.87 2.746(4) 167.5 .
N61 H611 O14 0.89 1.99 2.796(7) 149.9 .
N61 H612 O43 0.89 2.15 2.925(4) 145.3 1_445
N61 H612 O42 0.89 2.44 3.218(4) 145.9 1_445
N61 H613 O22 0.89 2.02 2.885(4) 164.9 2_666
N71 H71A O21 0.89 1.87 2.758(4) 178.3 2_676
N71 H71B O15 0.89 1.79 2.649(7) 162.4 .
N71 H71B O11 0.89 2.02 2.870(4) 159.7 .
N71 H71C O42 0.89 1.97 2.857(4) 174.1 2_675
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 1.000 0.500 342 57 'disordered solvnt molecules '
