#------------------------------------------------------------------------------
#$Date: 2016-03-24 17:15:54 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179683 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/05/7000540.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_7000540
loop_
_publ_author_name
'Gonzalez Calera, Silvia'
'Eisler, Dana J.'
'Goodman, Jonathan M.'
'McPartlin, Mary'
'Singh, Sanjay'
'Wright, Dominic S.'
_publ_section_title
;
 Joining the crown family; the tetrameric, O-bridged macrocycle
 [{P(μ-NtBu)}2(μ-O)]4
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1293
_journal_paper_doi               10.1039/b900268p
_journal_year                    2009
_chemical_formula_moiety         'C32 H72 N8 O4 P8'
_chemical_formula_sum            'C32 H72 N8 O4 P8'
_chemical_formula_weight         880.74
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3176(1)
_cell_length_b                   17.0622(2)
_cell_length_c                   21.4828(3)
_cell_measurement_reflns_used    46296
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     4881.48(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46206
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         11156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0395
_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)+(0.0269P)²+2.0271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0798
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                9798
_reflns_number_total             11156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b900268p.txt
_cod_data_source_block           dw0806
_cod_original_cell_volume        4881.39(10)
_cod_database_code               7000540
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -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
P1 P 0.87181(5) 0.12709(4) 0.90450(3) 0.02853(13) Uani 1 1 d . . .
N1 N 0.96370(14) 0.14130(11) 0.85077(9) 0.0289(4) Uani 1 1 d . . .
N2 N 0.85634(15) 0.04109(11) 0.86307(9) 0.0282(4) Uani 1 1 d . . .
P2 P 0.95241(5) 0.05615(3) 0.81064(3) 0.02840(13) Uani 1 1 d . . .
O1 O 0.89004(12) 0.08295(9) 0.74740(7) 0.0297(4) Uani 1 1 d . . .
P3 P 0.90755(5) 0.04856(4) 0.67623(3) 0.02878(13) Uani 1 1 d . . .
N3 N 0.90654(14) 0.13401(11) 0.63271(9) 0.0276(4) Uani 1 1 d . . .
N4 N 0.78880(15) 0.04106(10) 0.64774(9) 0.0286(4) Uani 1 1 d . . .
P4 P 0.78667(5) 0.12341(4) 0.60321(3) 0.02803(13) Uani 1 1 d . . .
O2 O 0.72127(11) 0.18575(9) 0.64620(7) 0.0289(3) Uani 1 1 d . . .
P5 P 0.63564(5) 0.24709(4) 0.61843(3) 0.03036(14) Uani 1 1 d . . .
N5 N 0.53747(14) 0.23494(11) 0.67001(9) 0.0298(4) Uani 1 1 d . . .
N6 N 0.65503(14) 0.32928(11) 0.66148(10) 0.0318(4) Uani 1 1 d . . .
P6 P 0.55809(5) 0.31935(4) 0.71256(3) 0.03156(14) Uani 1 1 d . . .
O3 O 0.61419(12) 0.28569(9) 0.77587(8) 0.0324(4) Uani 1 1 d . . .
P7 P 0.58543(5) 0.31224(4) 0.84798(3) 0.03138(14) Uani 1 1 d . . .
N7 N 0.59172(14) 0.22680(11) 0.88812(9) 0.0300(4) Uani 1 1 d . . .
N8 N 0.70187(15) 0.32601(11) 0.88117(10) 0.0325(4) Uani 1 1 d . . .
P8 P 0.70573(5) 0.23880(4) 0.92213(3) 0.03086(14) Uani 1 1 d . . .
O4 O 0.77958(11) 0.18313(9) 0.87788(7) 0.0297(3) Uani 1 1 d . . .
C1 C 1.03103(18) 0.20930(14) 0.84159(12) 0.0343(5) Uani 1 1 d . . .
C2 C 1.0479(2) 0.24744(17) 0.90466(13) 0.0481(7) Uani 1 1 d . . .
H2A H 0.9834 0.2653 0.9215 0.072 Uiso 1 1 calc R . .
H2B H 1.0931 0.2924 0.8999 0.072 Uiso 1 1 calc R . .
H2C H 1.0779 0.2093 0.9332 0.072 Uiso 1 1 calc R . .
C3 C 0.9820(2) 0.26621(16) 0.79630(13) 0.0458(7) Uani 1 1 d . . .
H3A H 0.9202 0.2870 0.8147 0.069 Uiso 1 1 calc R . .
H3B H 0.9661 0.2388 0.7574 0.069 Uiso 1 1 calc R . .
H3C H 1.0283 0.3095 0.7876 0.069 Uiso 1 1 calc R . .
C4 C 1.1309(2) 0.17945(18) 0.81591(15) 0.0504(7) Uani 1 1 d . . .
H4A H 1.1623 0.1445 0.8464 0.076 Uiso 1 1 calc R . .
H4B H 1.1754 0.2240 0.8077 0.076 Uiso 1 1 calc R . .
H4C H 1.1190 0.1507 0.7771 0.076 Uiso 1 1 calc R . .
C5 C 0.84328(18) -0.03612(13) 0.89544(12) 0.0319(5) Uani 1 1 d . . .
C6 C 0.9313(2) -0.05192(16) 0.93997(13) 0.0455(7) Uani 1 1 d . . .
H6A H 0.9940 -0.0544 0.9162 0.068 Uiso 1 1 calc R . .
H6B H 0.9204 -0.1019 0.9615 0.068 Uiso 1 1 calc R . .
H6C H 0.9355 -0.0095 0.9706 0.068 Uiso 1 1 calc R . .
C7 C 0.7448(2) -0.03301(15) 0.93142(13) 0.0389(6) Uani 1 1 d . . .
H7A H 0.6892 -0.0239 0.9024 0.058 Uiso 1 1 calc R . .
H7B H 0.7474 0.0098 0.9618 0.058 Uiso 1 1 calc R . .
H7C H 0.7344 -0.0828 0.9532 0.058 Uiso 1 1 calc R . .
C8 C 0.8382(2) -0.10008(14) 0.84609(12) 0.0416(6) Uani 1 1 d . . .
H8A H 0.7804 -0.0908 0.8189 0.062 Uiso 1 1 calc R . .
H8B H 0.8311 -0.1512 0.8663 0.062 Uiso 1 1 calc R . .
H8C H 0.8999 -0.0994 0.8212 0.062 Uiso 1 1 calc R . .
C9 C 0.99287(18) 0.15644(14) 0.59192(11) 0.0334(5) Uani 1 1 d . . .
C10 C 0.9710(2) 0.23725(15) 0.56515(12) 0.0407(6) Uani 1 1 d . . .
H10A H 0.9647 0.2752 0.5992 0.061 Uiso 1 1 calc R . .
H10B H 0.9082 0.2356 0.5414 0.061 Uiso 1 1 calc R . .
H10C H 1.0261 0.2530 0.5376 0.061 Uiso 1 1 calc R . .
C11 C 1.08711(19) 0.16001(19) 0.63213(13) 0.0491(7) Uani 1 1 d . . .
H11A H 1.0794 0.2012 0.6636 0.074 Uiso 1 1 calc R . .
H11B H 1.1453 0.1718 0.6059 0.074 Uiso 1 1 calc R . .
H11C H 1.0971 0.1094 0.6528 0.074 Uiso 1 1 calc R . .
C12 C 1.0072(2) 0.09707(17) 0.53913(13) 0.0462(7) Uani 1 1 d . . .
H12A H 0.9468 0.0958 0.5131 0.069 Uiso 1 1 calc R . .
H12B H 1.0191 0.0449 0.5568 0.069 Uiso 1 1 calc R . .
H12C H 1.0650 0.1125 0.5137 0.069 Uiso 1 1 calc R . .
C13 C 0.70947(18) -0.01800(13) 0.65969(11) 0.0318(5) Uani 1 1 d . . .
C14 C 0.6439(2) -0.02452(16) 0.60189(13) 0.0459(7) Uani 1 1 d . . .
H14A H 0.6125 0.0263 0.5934 0.069 Uiso 1 1 calc R . .
H14B H 0.5917 -0.0640 0.6088 0.069 Uiso 1 1 calc R . .
H14C H 0.6854 -0.0400 0.5663 0.069 Uiso 1 1 calc R . .
C15 C 0.6480(2) 0.00786(17) 0.71573(13) 0.0456(7) Uani 1 1 d . . .
H15A H 0.6924 0.0141 0.7518 0.068 Uiso 1 1 calc R . .
H15B H 0.5969 -0.0318 0.7249 0.068 Uiso 1 1 calc R . .
H15C H 0.6153 0.0580 0.7065 0.068 Uiso 1 1 calc R . .
C16 C 0.7602(2) -0.09685(15) 0.67195(14) 0.0462(7) Uani 1 1 d . . .
H16A H 0.8044 -0.0923 0.7082 0.069 Uiso 1 1 calc R . .
H16B H 0.7997 -0.1121 0.6354 0.069 Uiso 1 1 calc R . .
H16C H 0.7088 -0.1367 0.6801 0.069 Uiso 1 1 calc R . .
C17 C 0.43422(18) 0.21349(16) 0.64761(12) 0.0374(6) Uani 1 1 d . . .
C18 C 0.3900(2) 0.27954(18) 0.60817(14) 0.0503(7) Uani 1 1 d . . .
H18A H 0.3850 0.3273 0.6333 0.075 Uiso 1 1 calc R . .
H18B H 0.3230 0.2644 0.5936 0.075 Uiso 1 1 calc R . .
H18C H 0.4336 0.2893 0.5723 0.075 Uiso 1 1 calc R . .
C19 C 0.4422(2) 0.13890(17) 0.60959(15) 0.0513(7) Uani 1 1 d . . .
H19A H 0.4867 0.1478 0.5740 0.077 Uiso 1 1 calc R . .
H19B H 0.3754 0.1239 0.5946 0.077 Uiso 1 1 calc R . .
H19C H 0.4695 0.0968 0.6356 0.077 Uiso 1 1 calc R . .
C20 C 0.3681(2) 0.2000(2) 0.70477(14) 0.0568(8) Uani 1 1 d . . .
H20A H 0.3668 0.2478 0.7302 0.085 Uiso 1 1 calc R . .
H20B H 0.3955 0.1567 0.7294 0.085 Uiso 1 1 calc R . .
H20C H 0.2998 0.1871 0.6914 0.085 Uiso 1 1 calc R . .
C21 C 0.73595(18) 0.38821(14) 0.65838(13) 0.0378(6) Uani 1 1 d . . .
C22 C 0.6941(2) 0.46632(15) 0.68151(18) 0.0589(9) Uani 1 1 d . . .
H22A H 0.6665 0.4596 0.7235 0.088 Uiso 1 1 calc R . .
H22B H 0.6410 0.4841 0.6533 0.088 Uiso 1 1 calc R . .
H22C H 0.7481 0.5054 0.6826 0.088 Uiso 1 1 calc R . .
C23 C 0.82376(19) 0.36146(16) 0.69834(14) 0.0442(7) Uani 1 1 d . . .
H23A H 0.8496 0.3116 0.6824 0.066 Uiso 1 1 calc R . .
H23B H 0.8012 0.3545 0.7414 0.066 Uiso 1 1 calc R . .
H23C H 0.8771 0.4010 0.6970 0.066 Uiso 1 1 calc R . .
C24 C 0.7676(2) 0.39684(19) 0.59005(15) 0.0546(8) Uani 1 1 d . . .
H24A H 0.7905 0.3460 0.5742 0.082 Uiso 1 1 calc R . .
H24B H 0.8224 0.4350 0.5870 0.082 Uiso 1 1 calc R . .
H24C H 0.7103 0.4150 0.5654 0.082 Uiso 1 1 calc R . .
C25 C 0.52401(18) 0.15855(14) 0.88791(12) 0.0343(5) Uani 1 1 d . . .
C26 C 0.5374(2) 0.11439(16) 0.94920(12) 0.0439(6) Uani 1 1 d . . .
H26A H 0.6071 0.0967 0.9530 0.066 Uiso 1 1 calc R . .
H26B H 0.4925 0.0689 0.9499 0.066 Uiso 1 1 calc R . .
H26C H 0.5210 0.1492 0.9840 0.066 Uiso 1 1 calc R . .
C27 C 0.41550(19) 0.18837(17) 0.88249(15) 0.0484(7) Uani 1 1 d . . .
H27A H 0.4086 0.2200 0.8447 0.073 Uiso 1 1 calc R . .
H27B H 0.3992 0.2205 0.9189 0.073 Uiso 1 1 calc R . .
H27C H 0.3695 0.1436 0.8804 0.073 Uiso 1 1 calc R . .
C28 C 0.5510(2) 0.10597(15) 0.83312(12) 0.0424(6) Uani 1 1 d . . .
H28A H 0.6209 0.0887 0.8372 0.064 Uiso 1 1 calc R . .
H28B H 0.5430 0.1352 0.7942 0.064 Uiso 1 1 calc R . .
H28C H 0.5066 0.0602 0.8327 0.064 Uiso 1 1 calc R . .
C29 C 0.7303(2) 0.40282(15) 0.90967(14) 0.0426(6) Uani 1 1 d . . .
C30 C 0.6580(3) 0.42587(18) 0.96224(15) 0.0620(9) Uani 1 1 d . . .
H30A H 0.5894 0.4284 0.9459 0.093 Uiso 1 1 calc R . .
H30B H 0.6771 0.4772 0.9788 0.093 Uiso 1 1 calc R . .
H30C H 0.6613 0.3867 0.9955 0.093 Uiso 1 1 calc R . .
C31 C 0.7289(3) 0.46457(16) 0.85910(16) 0.0573(8) Uani 1 1 d . . .
H31A H 0.7758 0.4497 0.8260 0.086 Uiso 1 1 calc R . .
H31B H 0.7491 0.5152 0.8767 0.086 Uiso 1 1 calc R . .
H31C H 0.6610 0.4688 0.8419 0.086 Uiso 1 1 calc R . .
C32 C 0.8369(2) 0.39454(19) 0.93559(19) 0.0672(10) Uani 1 1 d . . .
H32A H 0.8828 0.3800 0.9019 0.101 Uiso 1 1 calc R . .
H32B H 0.8378 0.3538 0.9677 0.101 Uiso 1 1 calc R . .
H32C H 0.8582 0.4445 0.9537 0.101 Uiso 1 1 calc R . .
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
O4 P1 N1 102.53(9) . . ?
O4 P1 N2 102.92(9) . . ?
N1 P1 N2 81.79(9) . . ?
C1 N1 P2 131.13(16) . . ?
C1 N1 P1 129.69(16) . . ?
P2 N1 P1 99.16(10) . . ?
C5 N2 P2 121.33(15) . . ?
C5 N2 P1 121.38(15) . . ?
P2 N2 P1 96.97(10) . . ?
O1 P2 N1 102.99(9) . . ?
O1 P2 N2 101.82(9) . . ?
N1 P2 N2 82.04(9) . . ?
P3 O1 P2 126.11(10) . . ?
O1 P3 N4 103.20(9) . . ?
O1 P3 N3 101.49(9) . . ?
N4 P3 N3 82.06(9) . . ?
C9 N3 P4 121.49(15) . . ?
C9 N3 P3 121.72(15) . . ?
P4 N3 P3 96.73(9) . . ?
C13 N4 P4 130.34(16) . . ?
C13 N4 P3 130.66(15) . . ?
P4 N4 P3 98.97(10) . . ?
O2 P4 N4 103.06(9) . . ?
O2 P4 N3 102.37(9) . . ?
N4 P4 N3 82.22(9) . . ?
P4 O2 P5 124.49(10) . . ?
O2 P5 N6 102.73(9) . . ?
O2 P5 N5 102.35(9) . . ?
N6 P5 N5 82.23(10) . . ?
C17 N5 P5 121.12(16) . . ?
C17 N5 P6 121.20(16) . . ?
P5 N5 P6 96.85(10) . . ?
C21 N6 P5 130.45(17) . . ?
C21 N6 P6 130.59(18) . . ?
P5 N6 P6 98.82(10) . . ?
O3 P6 N6 102.82(10) . . ?
O3 P6 N5 102.55(9) . . ?
N6 P6 N5 82.10(9) . . ?
P6 O3 P7 124.65(10) . . ?
O3 P7 N7 103.22(9) . . ?
O3 P7 N8 102.47(9) . . ?
N7 P7 N8 82.08(10) . . ?
C25 N7 P7 130.38(16) . . ?
C25 N7 P8 130.12(16) . . ?
P7 N7 P8 99.17(10) . . ?
C29 N8 P7 121.13(16) . . ?
C29 N8 P8 122.56(17) . . ?
P7 N8 P8 96.90(10) . . ?
O4 P8 N7 102.34(9) . . ?
O4 P8 N8 102.58(9) . . ?
N7 P8 N8 81.85(9) . . ?
P1 O4 P8 124.71(10) . . ?
N1 C1 C2 107.8(2) . . ?
N1 C1 C3 109.0(2) . . ?
C2 C1 C3 111.1(2) . . ?
N1 C1 C4 108.3(2) . . ?
C2 C1 C4 109.7(2) . . ?
C3 C1 C4 110.8(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C8 108.16(19) . . ?
N2 C5 C7 107.72(18) . . ?
C8 C5 C7 109.9(2) . . ?
N2 C5 C6 110.8(2) . . ?
C8 C5 C6 110.0(2) . . ?
C7 C5 C6 110.3(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 107.84(19) . . ?
N3 C9 C11 108.13(19) . . ?
C10 C9 C11 109.6(2) . . ?
N3 C9 C12 111.1(2) . . ?
C10 C9 C12 110.1(2) . . ?
C11 C9 C12 110.0(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C15 108.9(2) . . ?
N4 C13 C14 108.48(19) . . ?
C15 C13 C14 111.0(2) . . ?
N4 C13 C16 108.3(2) . . ?
C15 C13 C16 110.9(2) . . ?
C14 C13 C16 109.2(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N5 C17 C19 108.3(2) . . ?
N5 C17 C18 110.5(2) . . ?
C19 C17 C18 110.3(2) . . ?
N5 C17 C20 107.8(2) . . ?
C19 C17 C20 110.3(2) . . ?
C18 C17 C20 109.5(2) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N6 C21 C23 109.4(2) . . ?
N6 C21 C22 108.3(2) . . ?
C23 C21 C22 111.0(2) . . ?
N6 C21 C24 108.0(2) . . ?
C23 C21 C24 110.9(2) . . ?
C22 C21 C24 109.1(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N7 C25 C28 108.87(19) . . ?
N7 C25 C26 108.4(2) . . ?
C28 C25 C26 110.4(2) . . ?
N7 C25 C27 108.3(2) . . ?
C28 C25 C27 111.0(2) . . ?
C26 C25 C27 109.8(2) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C25 C28 H28A 109.5 . . ?
C25 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C25 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N8 C29 C31 108.2(2) . . ?
N8 C29 C32 107.6(2) . . ?
C31 C29 C32 109.7(3) . . ?
N8 C29 C30 111.5(2) . . ?
C31 C29 C30 110.0(2) . . ?
C32 C29 C30 109.7(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
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
P1 O4 1.6583(16) . ?
P1 N1 1.700(2) . ?
P1 N2 1.729(2) . ?
N1 C1 1.479(3) . ?
N1 P2 1.696(2) . ?
N2 C5 1.500(3) . ?
N2 P2 1.724(2) . ?
P2 O1 1.6567(16) . ?
O1 P3 1.6542(17) . ?
P3 N4 1.701(2) . ?
P3 N3 1.7319(19) . ?
N3 C9 1.496(3) . ?
N3 P4 1.7271(19) . ?
N4 C13 1.483(3) . ?
N4 P4 1.6999(19) . ?
P4 O2 1.6562(16) . ?
O2 P5 1.6588(16) . ?
P5 N6 1.700(2) . ?
P5 N5 1.7263(19) . ?
N5 C17 1.502(3) . ?
N5 P6 1.728(2) . ?
N6 C21 1.475(3) . ?
N6 P6 1.703(2) . ?
P6 O3 1.6545(17) . ?
O3 P7 1.6588(17) . ?
P7 N7 1.696(2) . ?
P7 N8 1.723(2) . ?
N7 C25 1.473(3) . ?
N7 P8 1.697(2) . ?
N8 C29 1.495(3) . ?
N8 P8 1.729(2) . ?
P8 O4 1.6653(16) . ?
C1 C2 1.520(4) . ?
C1 C3 1.522(4) . ?
C1 C4 1.527(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C8 1.523(3) . ?
C5 C7 1.524(3) . ?
C5 C6 1.536(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.522(3) . ?
C9 C11 1.525(4) . ?
C9 C12 1.533(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C15 1.521(3) . ?
C13 C14 1.522(4) . ?
C13 C16 1.528(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.516(4) . ?
C17 C18 1.528(4) . ?
C17 C20 1.528(4) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C23 1.521(3) . ?
C21 C22 1.527(4) . ?
C21 C24 1.534(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C28 1.523(3) . ?
C25 C26 1.528(4) . ?
C25 C27 1.537(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C31 1.513(4) . ?
C29 C32 1.531(4) . ?
C29 C30 1.536(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
