# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Dominic S. Wright'
'Silvia Gonzalez Calera'
'Dana Eisler'
'Jonathan Goodman'
'Mary McPartlin'
'Sanjay Singh'

_publ_contact_author_name        'Dominic S. Wright'
_publ_contact_author_email       DSW1000@CAM.AC.UK

_publ_section_title              
;
Joining the crown family; the tetrameric, O-bridged
macrocycle [{P(mu-NtBu)}2(mu-O)]4
;

# Attachment 'dw0806.cif'

data_dw0806
_database_code_depnum_ccdc_archive 'CCDC 706578'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H72 N8 O4 P8'
_chemical_formula_sum            'C32 H72 N8 O4 P8'
_chemical_formula_weight         880.74

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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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'

_cell_length_a                   13.3176(1)
_cell_length_b                   17.0622(2)
_cell_length_c                   21.4828(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4881.39(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    46296
_cell_measurement_theta_min      1.02
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1888
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_standards_number         0

_diffrn_reflns_number            46206
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.24
_diffrn_reflns_theta_max         27.48
_reflns_number_total             11156
_reflns_number_gt                9798
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+2.0271P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(6)
_refine_ls_number_reflns         11156
_refine_ls_number_parameters     493
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.0848
_refine_ls_wR_factor_gt          0.0798
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0289(3) 0.0315(3) 0.0252(3) 0.0005(2) -0.0006(2) 0.0014(3)
N1 0.0251(10) 0.0320(10) 0.0297(10) 0.0003(8) -0.0010(8) -0.0010(8)
N2 0.0320(10) 0.0278(9) 0.0248(10) 0.0040(8) 0.0031(8) 0.0006(8)
P2 0.0278(3) 0.0300(3) 0.0274(3) 0.0026(2) 0.0013(3) 0.0032(3)
O1 0.0304(9) 0.0339(8) 0.0247(8) -0.0004(6) -0.0003(7) 0.0024(7)
P3 0.0297(3) 0.0302(3) 0.0265(3) 0.0002(2) 0.0026(3) 0.0032(3)
N3 0.0248(9) 0.0314(9) 0.0267(10) 0.0023(8) 0.0041(8) 0.0004(8)
N4 0.0325(10) 0.0258(9) 0.0275(10) 0.0001(8) 0.0009(9) -0.0014(8)
P4 0.0289(3) 0.0320(3) 0.0232(3) 0.0002(2) 0.0009(2) -0.0006(3)
O2 0.0263(8) 0.0325(8) 0.0278(8) 0.0025(7) 0.0005(7) 0.0029(7)
P5 0.0261(3) 0.0361(3) 0.0289(3) 0.0064(3) 0.0001(3) 0.0022(3)
N5 0.0218(9) 0.0372(10) 0.0306(11) 0.0012(8) 0.0012(8) -0.0012(8)
N6 0.0283(10) 0.0287(10) 0.0383(12) 0.0066(9) 0.0020(9) 0.0008(8)
P6 0.0257(3) 0.0330(3) 0.0360(4) 0.0030(3) 0.0006(3) 0.0038(3)
O3 0.0309(9) 0.0347(8) 0.0314(9) -0.0016(7) -0.0001(7) 0.0033(7)
P7 0.0279(3) 0.0308(3) 0.0355(3) -0.0055(3) -0.0001(3) 0.0036(3)
N7 0.0259(9) 0.0336(10) 0.0305(11) -0.0031(8) 0.0021(9) 0.0006(8)
N8 0.0322(10) 0.0258(10) 0.0396(12) -0.0070(9) -0.0061(9) -0.0003(8)
P8 0.0307(3) 0.0330(3) 0.0289(3) -0.0059(3) -0.0010(3) 0.0015(3)
O4 0.0291(8) 0.0304(8) 0.0296(9) -0.0019(7) -0.0010(7) 0.0031(7)
C1 0.0280(12) 0.0375(13) 0.0374(14) 0.0034(11) -0.0035(11) -0.0052(10)
C2 0.0453(15) 0.0536(16) 0.0455(16) -0.0080(13) -0.0056(13) -0.0181(14)
C3 0.0503(17) 0.0401(14) 0.0470(17) 0.0104(12) -0.0014(13) -0.0049(13)
C4 0.0323(14) 0.0574(17) 0.0615(19) 0.0007(15) 0.0065(14) -0.0087(13)
C5 0.0366(13) 0.0280(11) 0.0310(13) 0.0071(10) 0.0018(11) 0.0038(10)
C6 0.0499(17) 0.0433(14) 0.0434(16) 0.0129(12) -0.0021(13) 0.0115(13)
C7 0.0415(15) 0.0376(14) 0.0376(15) 0.0065(11) 0.0060(12) -0.0019(11)
C8 0.0567(17) 0.0289(12) 0.0391(15) 0.0027(11) 0.0095(13) -0.0007(12)
C9 0.0277(12) 0.0414(13) 0.0311(13) 0.0003(11) 0.0090(10) -0.0027(11)
C10 0.0429(15) 0.0418(14) 0.0375(15) 0.0049(11) 0.0098(12) -0.0065(12)
C11 0.0307(14) 0.0707(19) 0.0459(17) 0.0061(14) 0.0048(12) -0.0037(14)
C12 0.0464(16) 0.0520(16) 0.0400(15) -0.0055(13) 0.0179(13) 0.0030(13)
C13 0.0338(13) 0.0295(11) 0.0320(13) -0.0012(10) 0.0049(11) -0.0034(10)
C14 0.0478(16) 0.0476(15) 0.0423(16) -0.0018(12) -0.0072(13) -0.0140(13)
C15 0.0458(16) 0.0504(16) 0.0407(15) 0.0010(13) 0.0119(13) -0.0031(14)
C16 0.0569(18) 0.0295(13) 0.0523(18) -0.0020(12) 0.0058(14) -0.0020(12)
C17 0.0248(12) 0.0535(15) 0.0339(13) 0.0031(11) -0.0027(11) -0.0046(11)
C18 0.0365(15) 0.0683(19) 0.0460(17) 0.0073(14) -0.0080(13) 0.0094(14)
C19 0.0381(15) 0.0566(17) 0.0591(19) -0.0047(15) -0.0064(14) -0.0087(14)
C20 0.0292(14) 0.098(2) 0.0437(17) 0.0039(16) 0.0018(13) -0.0144(16)
C21 0.0288(12) 0.0329(13) 0.0516(17) 0.0129(11) -0.0021(12) -0.0010(10)
C22 0.0504(18) 0.0292(14) 0.097(3) 0.0095(15) 0.0001(18) -0.0001(12)
C23 0.0343(14) 0.0438(15) 0.0545(18) 0.0024(13) -0.0041(12) -0.0006(12)
C24 0.0413(16) 0.0633(19) 0.059(2) 0.0315(16) -0.0001(14) -0.0086(14)
C25 0.0300(12) 0.0383(13) 0.0346(14) -0.0036(11) 0.0062(11) -0.0041(10)
C26 0.0441(16) 0.0457(15) 0.0420(15) 0.0036(12) 0.0108(13) -0.0015(13)
C27 0.0303(13) 0.0572(17) 0.0577(18) -0.0024(14) 0.0052(13) -0.0039(13)
C28 0.0464(15) 0.0406(14) 0.0402(15) -0.0105(11) 0.0038(13) -0.0090(12)
C29 0.0423(15) 0.0317(12) 0.0537(17) -0.0136(12) -0.0080(13) -0.0016(11)
C30 0.076(2) 0.0521(18) 0.058(2) -0.0265(15) 0.0039(18) -0.0021(16)
C31 0.068(2) 0.0310(14) 0.073(2) -0.0065(14) -0.0019(18) -0.0033(14)
C32 0.055(2) 0.0477(17) 0.099(3) -0.0176(18) -0.0282(19) -0.0071(15)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 . ?

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 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.073