#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:40:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179150 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/11/4311106.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_4311106
loop_
_publ_author_name
'Md. Alamgir Hossain'
'Jennifer Ann Liljegren'
'Douglas Powell'
'Kristin Bowman-James'
_publ_contact_author
; 
   Prof. Kristin Bowman-James 
   Department of Chemistry -- University of Kansas
   Malott Hall
   1251 Wescoe Hall Dr, Rm 2010 
   Lawrence, KS  66045-7582  USA 
;
_publ_contact_author_email       kbowman-james@ku.edu
_publ_contact_author_fax         1(785)8645396
_publ_contact_author_phone       1(785)8644278
_publ_section_title
;
 Anion Binding with a Tripodal Amine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3751
_journal_page_last               3755
_journal_paper_doi               10.1021/ic049762b
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '(C27 H36 N4) 3+, (H2 P O4)3 1-, (H3 P O4)'
_chemical_formula_sum            'C27 H48 N4 O16 P4'
_chemical_formula_weight         808.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.783(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1148(17)
_cell_length_b                   27.117(3)
_cell_length_c                   8.9168(10)
_cell_measurement_reflns_used    2483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.45
_cell_measurement_theta_min      2.63
_cell_volume                     3636.1(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       'ω scan frames'
_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  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11104
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.8806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         6294
_refine_ls_number_restraints     932
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2022
_refine_ls_wR_factor_ref         0.2371
_reflns_number_gt                3832
_reflns_number_total             6294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049762bsi20040223_103245_2.cif
_cod_data_source_block           compound_1_
_cod_database_code               4311106
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
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
N1 N 0.5059(4) 0.33982(17) 0.2579(6) 0.0392(12) Uani 1 1 d . . .
C2 C 0.5558(5) 0.3852(2) 0.2206(8) 0.0456(16) Uani 1 1 d . . .
H2A H 0.5790 0.3807 0.1215 0.055 Uiso 1 1 calc R . .
H2B H 0.5145 0.4136 0.2124 0.055 Uiso 1 1 calc R . .
C3 C 0.6312(5) 0.3962(3) 0.3363(8) 0.0461(15) Uani 1 1 d . . .
H3A H 0.6715 0.3673 0.3459 0.055 Uiso 1 1 calc R . .
H3B H 0.6653 0.4244 0.3015 0.055 Uiso 1 1 calc R . .
N4 N 0.6034(4) 0.4077(2) 0.4840(6) 0.0472(13) Uani 1 1 d . . .
H4A H 0.5723 0.3812 0.5157 0.057 Uiso 1 1 calc R . .
H4B H 0.5647 0.4340 0.4734 0.057 Uiso 1 1 calc R . .
C5 C 0.6756(5) 0.4201(3) 0.6052(9) 0.0557(18) Uani 1 1 d . . .
H5A H 0.7148 0.3911 0.6249 0.067 Uiso 1 1 calc R . .
H5B H 0.6489 0.4279 0.6993 0.067 Uiso 1 1 calc R . .
C6 C 0.7315(5) 0.4646(3) 0.5603(8) 0.0495(17) Uani 1 1 d . . .
C7 C 0.8171(6) 0.4569(3) 0.5283(11) 0.066(2) Uani 1 1 d . . .
H7 H 0.8421 0.4248 0.5334 0.079 Uiso 1 1 calc R . .
C8 C 0.8663(6) 0.4967(4) 0.4884(13) 0.078(3) Uani 1 1 d . . .
H8 H 0.9262 0.4919 0.4677 0.094 Uiso 1 1 calc R . .
C9 C 0.8298(6) 0.5432(4) 0.4784(11) 0.074(3) Uani 1 1 d . . .
H9 H 0.8642 0.5702 0.4492 0.089 Uiso 1 1 calc R . .
C10 C 0.7444(5) 0.5506(3) 0.5104(9) 0.0546(18) Uani 1 1 d . . .
H10 H 0.7190 0.5827 0.5038 0.066 Uiso 1 1 calc R . .
C11 C 0.6951(5) 0.5106(3) 0.5526(8) 0.0499(17) Uani 1 1 d . . .
H11 H 0.6357 0.5154 0.5761 0.060 Uiso 1 1 calc R . .
C12 C 0.4134(4) 0.3421(3) 0.1846(8) 0.0448(15) Uani 1 1 d . . .
H12A H 0.3887 0.3083 0.1767 0.054 Uiso 1 1 calc R . .
H12B H 0.4144 0.3551 0.0810 0.054 Uiso 1 1 calc R . .
C13 C 0.3536(5) 0.3738(2) 0.2674(8) 0.0471(16) Uani 1 1 d . . .
H13A H 0.3798 0.4071 0.2810 0.057 Uiso 1 1 calc R . .
H13B H 0.2953 0.3771 0.2067 0.057 Uiso 1 1 calc R . .
N14 N 0.3400(4) 0.3528(2) 0.4169(7) 0.0560(16) Uani 1 1 d . . .
H14A H 0.3945 0.3490 0.4714 0.067 Uiso 1 1 calc R . .
H14B H 0.3149 0.3221 0.4032 0.067 Uiso 1 1 calc R . .
C15 C 0.2815(6) 0.3839(4) 0.5079(11) 0.074(2) Uani 1 1 d . . .
H15A H 0.2800 0.3689 0.6088 0.089 Uiso 1 1 calc R . .
H15B H 0.3079 0.4172 0.5221 0.089 Uiso 1 1 calc R . .
C16 C 0.1900(5) 0.3886(3) 0.4355(10) 0.066(2) Uani 1 1 d . . .
C17 C 0.1613(6) 0.4307(4) 0.3589(15) 0.090(3) Uani 1 1 d . . .
H17 H 0.2014 0.4577 0.3564 0.108 Uiso 1 1 calc R . .
C18 C 0.0768(8) 0.4355(4) 0.2860(18) 0.109(4) Uani 1 1 d . . .
H18 H 0.0606 0.4629 0.2230 0.131 Uiso 1 1 calc R . .
C19 C 0.0170(7) 0.3983(6) 0.3089(17) 0.111(5) Uani 1 1 d . . .
H19 H -0.0437 0.4021 0.2716 0.133 Uiso 1 1 calc R . .
C20 C 0.0458(7) 0.3541(5) 0.3885(14) 0.090(3) Uani 1 1 d . . .
H20 H 0.0050 0.3279 0.3980 0.108 Uiso 1 1 calc R . .
C21 C 0.1283(6) 0.3499(4) 0.4479(12) 0.078(3) Uani 1 1 d . . .
H21 H 0.1469 0.3205 0.5000 0.093 Uiso 1 1 calc R . .
C22 C 0.5501(5) 0.2967(2) 0.2021(8) 0.0453(16) Uani 1 1 d . . .
H22A H 0.6152 0.3021 0.2154 0.054 Uiso 1 1 calc R . .
H22B H 0.5321 0.2931 0.0928 0.054 Uiso 1 1 calc R . .
C23 C 0.5290(5) 0.2497(2) 0.2806(8) 0.0457(16) Uani 1 1 d . . .
H23A H 0.4637 0.2452 0.2734 0.055 Uiso 1 1 calc R . .
H23B H 0.5546 0.2214 0.2297 0.055 Uiso 1 1 calc R . .
N24 N 0.5647(5) 0.2504(2) 0.4401(7) 0.0546(15) Uani 1 1 d . . .
H24A H 0.5399 0.2766 0.4868 0.065 Uiso 1 1 calc R . .
H24B H 0.6251 0.2556 0.4459 0.065 Uiso 1 1 calc R . .
C25 C 0.5472(8) 0.2039(3) 0.5238(10) 0.075(3) Uani 1 1 d . . .
H25A H 0.5752 0.2065 0.6288 0.090 Uiso 1 1 calc R . .
H25B H 0.4824 0.1999 0.5274 0.090 Uiso 1 1 calc R . .
C26 C 0.5827(5) 0.1598(3) 0.4515(9) 0.0558(19) Uani 1 1 d . . .
C27 C 0.5266(6) 0.1270(3) 0.3713(12) 0.071(3) Uani 1 1 d . . .
H27 H 0.4644 0.1331 0.3633 0.085 Uiso 1 1 calc R . .
C28 C 0.5576(6) 0.0855(3) 0.3017(12) 0.074(3) Uani 1 1 d . . .
H28 H 0.5176 0.0640 0.2447 0.089 Uiso 1 1 calc R . .
C29 C 0.6478(6) 0.0763(3) 0.3174(11) 0.067(2) Uani 1 1 d . . .
H29 H 0.6699 0.0473 0.2746 0.080 Uiso 1 1 calc R . .
C30 C 0.7067(6) 0.1088(3) 0.3948(11) 0.071(2) Uani 1 1 d . . .
H30 H 0.7690 0.1031 0.4023 0.086 Uiso 1 1 calc R . .
C31 C 0.6719(6) 0.1500(3) 0.4613(11) 0.070(2) Uani 1 1 d . . .
H31 H 0.7117 0.1722 0.5159 0.084 Uiso 1 1 calc R . .
P1A P 0.4844(7) 0.3242(4) 0.7522(13) 0.064(3) Uani 0.585(14) 1 d PD A 1
O1A O 0.4956(14) 0.3320(10) 0.5942(15) 0.053(5) Uani 0.585(14) 1 d PDU A 1
O2A O 0.5273(11) 0.3655(4) 0.8447(14) 0.106(5) Uani 0.585(14) 1 d PDU A 1
O3A O 0.3921(8) 0.3236(7) 0.7829(17) 0.127(6) Uani 0.585(14) 1 d PDU A 1
O4A O 0.5311(14) 0.2797(5) 0.810(2) 0.098(7) Uani 0.585(14) 1 d PDU A 1
P1A' P 0.5050(9) 0.3280(5) 0.7622(17) 0.060(4) Uani 0.415(14) 1 d PD A 2
O1A' O 0.512(2) 0.3325(13) 0.6003(18) 0.051(7) Uani 0.415(14) 1 d PDU A 2
O2A' O 0.5893(12) 0.3460(8) 0.843(2) 0.104(7) Uani 0.415(14) 1 d PDU A 2
O3A' O 0.4335(11) 0.3589(6) 0.8096(16) 0.075(5) Uani 0.415(14) 1 d PDU A 2
O4A' O 0.493(2) 0.2764(6) 0.802(4) 0.103(9) Uani 0.415(14) 1 d PDU A 2
P1B P 0.4317(10) 0.5140(5) 0.3651(17) 0.063(5) Uani 0.343(11) 1 d PD B 1
O1B O 0.4439(17) 0.4772(6) 0.485(2) 0.068(6) Uani 0.343(11) 1 d PDU B 1
O2B O 0.5061(13) 0.5096(8) 0.272(2) 0.109(7) Uani 0.343(11) 1 d PDU B 1
O3B O 0.4296(12) 0.5636(5) 0.4342(18) 0.069(5) Uani 0.343(11) 1 d PDU B 1
O4B O 0.3487(16) 0.5063(13) 0.267(3) 0.063(8) Uani 0.343(11) 1 d PDU B 1
P1B' P 0.4246(5) 0.5162(2) 0.3901(8) 0.0469(19) Uani 0.657(11) 1 d PD B 2
O1B' O 0.4652(8) 0.4685(3) 0.4276(14) 0.067(4) Uani 0.657(11) 1 d PDU B 2
O2B' O 0.4961(6) 0.5508(3) 0.3527(12) 0.083(3) Uani 0.657(11) 1 d PDU B 2
O3B' O 0.3824(6) 0.5381(3) 0.5181(9) 0.070(3) Uani 0.657(11) 1 d PDU B 2
O4B' O 0.3603(10) 0.5139(7) 0.2535(16) 0.062(4) Uani 0.657(11) 1 d PDU B 2
P1C P 0.2793(8) 0.2138(5) 0.4011(15) 0.117(7) Uani 0.545(11) 1 d PD C 1
O1C O 0.2628(10) 0.2588(5) 0.3126(18) 0.121(5) Uani 0.545(11) 1 d PDU C 1
O2C O 0.1967(10) 0.1951(7) 0.455(2) 0.154(7) Uani 0.545(11) 1 d PDU C 1
O3C O 0.3135(13) 0.1756(7) 0.305(2) 0.118(7) Uani 0.545(11) 1 d PDU C 1
O4C O 0.3450(12) 0.2225(9) 0.530(2) 0.185(8) Uani 0.545(11) 1 d PDU C 1
P1C' P 0.2707(7) 0.2141(3) 0.3960(10) 0.062(4) Uani 0.455(11) 1 d PD C 2
O1C' O 0.3312(9) 0.2554(4) 0.430(2) 0.108(6) Uani 0.455(11) 1 d PDU C 2
O2C' O 0.1805(8) 0.2346(8) 0.373(3) 0.166(7) Uani 0.455(11) 1 d PDU C 2
O3C' O 0.2784(18) 0.1783(7) 0.520(2) 0.169(8) Uani 0.455(11) 1 d PDU C 2
O4C' O 0.2931(19) 0.1879(8) 0.2604(15) 0.130(8) Uani 0.455(11) 1 d PDU C 2
P1D P 0.8087(2) 0.28195(16) 0.3945(6) 0.1275(16) Uani 1 1 d D . .
O1D O 0.7402(6) 0.2896(4) 0.4967(10) 0.129(3) Uani 1 1 d D . .
O2D O 0.8251(8) 0.3212(4) 0.2874(13) 0.154(4) Uani 1 1 d D . .
O3D O 0.8932(5) 0.2616(4) 0.4641(10) 0.124(3) Uani 1 1 d D . .
O4D O 0.7686(12) 0.2393(6) 0.308(2) 0.293(13) Uani 1 1 d 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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 N1 C12 109.1(5) . . ?
C22 N1 C2 108.9(5) . . ?
C12 N1 C2 109.9(5) . . ?
C3 C2 N1 112.2(5) . . ?
C3 C2 H2A 109.2 . . ?
N1 C2 H2A 109.2 . . ?
C3 C2 H2B 109.2 . . ?
N1 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N4 C3 C2 113.5(5) . . ?
N4 C3 H3A 108.9 . . ?
C2 C3 H3A 108.9 . . ?
N4 C3 H3B 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C3 N4 C5 116.5(6) . . ?
C3 N4 H4A 108.2 . . ?
C5 N4 H4A 108.2 . . ?
C3 N4 H4B 108.2 . . ?
C5 N4 H4B 108.2 . . ?
H4A N4 H4B 107.3 . . ?
N4 C5 C6 111.4(6) . . ?
N4 C5 H5A 109.3 . . ?
C6 C5 H5A 109.3 . . ?
N4 C5 H5B 109.3 . . ?
C6 C5 H5B 109.3 . . ?
H5A C5 H5B 108.0 . . ?
C11 C6 C7 121.0(7) . . ?
C11 C6 C5 119.9(7) . . ?
C7 C6 C5 119.2(7) . . ?
C6 C7 C8 118.8(8) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
C7 C8 C9 120.7(8) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 H8 119.6 . . ?
C10 C9 C8 120.2(8) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 119.1(8) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C6 C11 C10 120.2(7) . . ?
C6 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
N1 C12 C13 113.4(5) . . ?
N1 C12 H12A 108.9 . . ?
C13 C12 H12A 108.9 . . ?
N1 C12 H12B 108.9 . . ?
C13 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
N14 C13 C12 111.7(5) . . ?
N14 C13 H13A 109.3 . . ?
C12 C13 H13A 109.3 . . ?
N14 C13 H13B 109.3 . . ?
C12 C13 H13B 109.3 . . ?
H13A C13 H13B 107.9 . . ?
C13 N14 C15 114.2(6) . . ?
C13 N14 H14A 108.7 . . ?
C15 N14 H14A 108.7 . . ?
C13 N14 H14B 108.7 . . ?
C15 N14 H14B 108.7 . . ?
H14A N14 H14B 107.6 . . ?
C16 C15 N14 112.7(7) . . ?
C16 C15 H15A 109.1 . . ?
N14 C15 H15A 109.1 . . ?
C16 C15 H15B 109.0 . . ?
N14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C17 C16 C21 118.4(9) . . ?
C17 C16 C15 121.5(9) . . ?
C21 C16 C15 120.0(9) . . ?
C18 C17 C16 122.7(10) . . ?
C18 C17 H17 118.6 . . ?
C16 C17 H17 118.7 . . ?
C17 C18 C19 116.8(12) . . ?
C17 C18 H18 121.6 . . ?
C19 C18 H18 121.6 . . ?
C18 C19 C20 120.7(10) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.7 . . ?
C21 C20 C19 120.0(10) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C16 120.8(11) . . ?
C20 C21 H21 119.6 . . ?
C16 C21 H21 119.6 . . ?
N1 C22 C23 113.2(6) . . ?
N1 C22 H22A 108.9 . . ?
C23 C22 H22A 108.9 . . ?
N1 C22 H22B 108.9 . . ?
C23 C22 H22B 108.9 . . ?
H22A C22 H22B 107.8 . . ?
N24 C23 C22 111.4(5) . . ?
N24 C23 H23A 109.4 . . ?
C22 C23 H23A 109.4 . . ?
N24 C23 H23B 109.3 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
C23 N24 C25 113.8(6) . . ?
C23 N24 H24A 108.8 . . ?
C25 N24 H24A 108.8 . . ?
C23 N24 H24B 108.8 . . ?
C25 N24 H24B 108.8 . . ?
H24A N24 H24B 107.7 . . ?
C26 C25 N24 111.8(7) . . ?
C26 C25 H25A 109.3 . . ?
N24 C25 H25A 109.3 . . ?
C26 C25 H25B 109.3 . . ?
N24 C25 H25B 109.3 . . ?
H25A C25 H25B 107.9 . . ?
C31 C26 C27 117.2(8) . . ?
C31 C26 C25 121.7(9) . . ?
C27 C26 C25 121.0(8) . . ?
C26 C27 C28 122.6(8) . . ?
C26 C27 H27 118.7 . . ?
C28 C27 H27 118.7 . . ?
C29 C28 C27 118.3(8) . . ?
C29 C28 H28 120.8 . . ?
C27 C28 H28 120.8 . . ?
C28 C29 C30 120.9(7) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
C29 C30 C31 118.1(8) . . ?
C29 C30 H30 121.0 . . ?
C31 C30 H30 121.0 . . ?
C26 C31 C30 122.8(9) . . ?
C26 C31 H31 118.6 . . ?
C30 C31 H31 118.6 . . ?
O3A P1A O1A 113.2(10) . . ?
O3A P1A O4A 111.4(10) . . ?
O1A P1A O4A 111.1(9) . . ?
O3A P1A O2A 106.0(9) . . ?
O1A P1A O2A 109.8(10) . . ?
O4A P1A O2A 104.7(10) . . ?
O4A' P1A' O3A' 111.5(12) . . ?
O4A' P1A' O1A' 110.1(12) . . ?
O3A' P1A' O1A' 111.3(12) . . ?
O4A' P1A' O2A' 108.4(12) . . ?
O3A' P1A' O2A' 107.2(11) . . ?
O1A' P1A' O2A' 108.2(12) . . ?
O1B P1B O2B 108.2(12) . . ?
O1B P1B O4B 112.2(13) . . ?
O2B P1B O4B 107.8(12) . . ?
O1B P1B O3B 108.8(11) . . ?
O2B P1B O3B 111.0(11) . . ?
O4B P1B O3B 108.9(13) . . ?
O1B' P1B' O4B' 112.3(8) . . ?
O1B' P1B' O3B' 112.5(7) . . ?
O4B' P1B' O3B' 110.5(8) . . ?
O1B' P1B' O2B' 108.2(7) . . ?
O4B' P1B' O2B' 105.7(8) . . ?
O3B' P1B' O2B' 107.2(7) . . ?
O4C P1C O1C 110.8(11) . . ?
O4C P1C O3C 108.7(11) . . ?
O1C P1C O3C 109.0(11) . . ?
O4C P1C O2C 109.4(12) . . ?
O1C P1C O2C 111.0(11) . . ?
O3C P1C O2C 107.9(11) . . ?
O1C' P1C' O2C' 107.0(10) . . ?
O1C' P1C' O3C' 110.5(11) . . ?
O2C' P1C' O3C' 110.9(12) . . ?
O1C' P1C' O4C' 110.5(12) . . ?
O2C' P1C' O4C' 111.0(12) . . ?
O3C' P1C' O4C' 107.0(11) . . ?
O1D P1D O2D 118.7(7) . . ?
O1D P1D O3D 115.5(6) . . ?
O2D P1D O3D 110.5(7) . . ?
O1D P1D O4D 98.9(9) . . ?
O2D P1D O4D 108.4(11) . . ?
O3D P1D O4D 102.6(10) . . ?
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
N1 C22 1.459(8) . ?
N1 C12 1.484(8) . ?
N1 C2 1.497(8) . ?
C2 C3 1.488(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N4 1.457(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N4 C5 1.494(9) . ?
N4 H4A 0.9200 . ?
N4 H4B 0.9200 . ?
C5 C6 1.550(10) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C11 1.363(11) . ?
C6 C7 1.368(12) . ?
C7 C8 1.376(13) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.365(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(10) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.495(10) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N14 1.482(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
N14 C15 1.514(10) . ?
N14 H14A 0.9200 . ?
N14 H14B 0.9200 . ?
C15 C16 1.472(13) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.380(14) . ?
C16 C21 1.415(13) . ?
C17 C18 1.379(16) . ?
C17 H17 0.9500 . ?
C18 C19 1.382(18) . ?
C18 H18 0.9500 . ?
C19 C20 1.44(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.309(15) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.504(9) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 N24 1.469(9) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
N24 C25 1.504(10) . ?
N24 H24A 0.9200 . ?
N24 H24B 0.9200 . ?
C25 C26 1.483(11) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C31 1.368(12) . ?
C26 C27 1.377(12) . ?
C27 C28 1.390(12) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(12) . ?
C28 H28 0.9500 . ?
C29 C30 1.386(13) . ?
C29 H29 0.9500 . ?
C30 C31 1.392(13) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
P1A O3A 1.448(7) . ?
P1A O1A 1.451(7) . ?
P1A O4A 1.465(7) . ?
P1A O2A 1.499(7) . ?
P1A' O4A' 1.460(8) . ?
P1A' O3A' 1.462(8) . ?
P1A' O1A' 1.462(7) . ?
P1A' O2A' 1.481(8) . ?
P1B O1B 1.459(8) . ?
P1B O2B 1.470(8) . ?
P1B O4B 1.472(8) . ?
P1B O3B 1.482(8) . ?
P1B' O1B' 1.455(7) . ?
P1B' O4B' 1.482(7) . ?
P1B' O3B' 1.486(7) . ?
P1B' O2B' 1.495(7) . ?
P1C O4C 1.458(8) . ?
P1C O1C 1.462(8) . ?
P1C O3C 1.472(8) . ?
P1C O2C 1.472(8) . ?
P1C' O1C' 1.459(8) . ?
P1C' O2C' 1.467(8) . ?
P1C' O3C' 1.467(8) . ?
P1C' O4C' 1.471(8) . ?
P1D O1D 1.462(7) . ?
P1D O2D 1.467(7) . ?
P1D O3D 1.470(6) . ?
P1D O4D 1.484(8) . ?
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
N4 H4A O1A 0.92 1.94 2.86(2) 171.9 .
N4 H4A O1A' 0.92 1.81 2.73(3) 173.0 .
N4 H4B O1B 0.92 2.18 3.06(2) 159.6 .
N4 H4B O1B' 0.92 1.78 2.669(10) 160.5 .
N14 H14A O1A 0.92 1.85 2.76(2) 170.4 .
N14 H14A O1A' 0.92 2.06 2.97(3) 173.5 .
N14 H14B O1C 0.92 2.02 2.916(16) 164.1 .
N14 H14B O1C' 0.92 1.84 2.648(14) 145.8 .
N24 H24A O1A 0.92 1.94 2.85(2) 176.0 .
N24 H24A O1A' 0.92 1.90 2.81(3) 169.0 .
N24 H24B O1D 0.92 1.98 2.855(12) 158.1 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C22 N1 C2 C3 -85.4(7) . . . . ?
C12 N1 C2 C3 155.2(6) . . . . ?
N1 C2 C3 N4 -64.0(8) . . . . ?
C2 C3 N4 C5 -178.9(6) . . . . ?
C3 N4 C5 C6 57.8(8) . . . . ?
N4 C5 C6 C11 70.0(9) . . . . ?
N4 C5 C6 C7 -109.6(8) . . . . ?
C11 C6 C7 C8 0.3(13) . . . . ?
C5 C6 C7 C8 180.0(8) . . . . ?
C6 C7 C8 C9 -1.1(15) . . . . ?
C7 C8 C9 C10 1.1(15) . . . . ?
C8 C9 C10 C11 -0.2(13) . . . . ?
C7 C6 C11 C10 0.6(11) . . . . ?
C5 C6 C11 C10 -179.1(7) . . . . ?
C9 C10 C11 C6 -0.6(11) . . . . ?
C22 N1 C12 C13 160.9(5) . . . . ?
C2 N1 C12 C13 -79.8(7) . . . . ?
N1 C12 C13 N14 -65.8(7) . . . . ?
C12 C13 N14 C15 178.7(6) . . . . ?
C13 N14 C15 C16 63.5(10) . . . . ?
N14 C15 C16 C17 -102.1(10) . . . . ?
N14 C15 C16 C21 80.0(11) . . . . ?
C21 C16 C17 C18 -4.3(16) . . . . ?
C15 C16 C17 C18 177.8(11) . . . . ?
C16 C17 C18 C19 8.3(19) . . . . ?
C17 C18 C19 C20 -8.1(19) . . . . ?
C18 C19 C20 C21 4.1(18) . . . . ?
C19 C20 C21 C16 0.2(16) . . . . ?
C17 C16 C21 C20 -0.2(14) . . . . ?
C15 C16 C21 C20 177.7(9) . . . . ?
C12 N1 C22 C23 -81.9(7) . . . . ?
C2 N1 C22 C23 158.2(6) . . . . ?
N1 C22 C23 N24 -66.0(7) . . . . ?
C22 C23 N24 C25 -178.7(7) . . . . ?
C23 N24 C25 C26 56.6(10) . . . . ?
N24 C25 C26 C31 73.8(11) . . . . ?
N24 C25 C26 C27 -106.2(10) . . . . ?
C31 C26 C27 C28 -0.2(13) . . . . ?
C25 C26 C27 C28 179.8(8) . . . . ?
C26 C27 C28 C29 1.8(14) . . . . ?
C27 C28 C29 C30 -2.9(14) . . . . ?
C28 C29 C30 C31 2.5(14) . . . . ?
C27 C26 C31 C30 -0.2(13) . . . . ?
C25 C26 C31 C30 179.8(8) . . . . ?
C29 C30 C31 C26 -0.9(14) . . . . ?
