# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-DyvaldienPONa
_database_code_depnum_ccdc_archive 'CCDC 1415417'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H33 Cl Dy N3 Na O8 P'
_chemical_formula_weight         839.52

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.2015(14)
_cell_length_b                   8.3733(5)
_cell_length_c                   36.918(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6863.0(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9995
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      27.57

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.48
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3352
_exptl_absorpt_coefficient_mu    2.368
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.3613
_exptl_absorpt_correction_T_max  0.3961
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43751
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         27.63
_reflns_number_total             7952
_reflns_number_gt                6826
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0219P)²+11.6788P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7952
_refine_ls_number_parameters     430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0823
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_restrained_S_all      1.239
_refine_ls_shift/su_max          0.001
_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
Dy1 Dy 0.481978(8) 0.54323(2) 0.142736(4) 0.03250(6) Uani 1 1 d . . .
O3 O 0.55053(13) 0.3714(3) 0.16364(7) 0.0400(6) Uani 1 1 d . . .
O1 O 0.42686(13) 0.3720(3) 0.17407(7) 0.0430(7) Uani 1 1 d . . .
C7 C 0.3263(2) 0.5591(6) 0.14617(12) 0.0489(10) Uani 1 1 d . . .
H7 H 0.2901 0.6031 0.1383 0.059 Uiso 1 1 calc R . .
O4 O 0.58561(15) 0.1428(4) 0.20697(8) 0.0553(8) Uani 1 1 d . . .
C11 C 0.5795(2) 0.7482(6) 0.08848(14) 0.0612(14) Uani 1 1 d . . .
H11A H 0.6129 0.7377 0.0717 0.073 Uiso 1 1 calc R . .
H11B H 0.5823 0.8519 0.1000 0.073 Uiso 1 1 calc R . .
C9 C 0.4113(2) 0.7492(5) 0.07872(12) 0.0511(11) Uani 1 1 d . . .
H9A H 0.4057 0.6519 0.0649 0.061 Uiso 1 1 calc R . .
H9B H 0.4065 0.8394 0.0625 0.061 Uiso 1 1 calc R . .
C18 C 0.6088(2) 0.3543(5) 0.16780(10) 0.0398(9) Uani 1 1 d . . .
N1 N 0.37374(17) 0.6215(4) 0.13328(9) 0.0453(8) Uani 1 1 d . . .
C10 C 0.5209(2) 0.7350(5) 0.06829(11) 0.0509(11) Uani 1 1 d . . .
H10A H 0.5181 0.8186 0.0502 0.061 Uiso 1 1 calc R . .
H10B H 0.5184 0.6325 0.0562 0.061 Uiso 1 1 calc R . .
C13 C 0.6520(2) 0.4490(5) 0.15035(12) 0.0460(10) Uani 1 1 d . . .
N3 N 0.58279(17) 0.6210(4) 0.11613(10) 0.0467(9) Uani 1 1 d . . .
C6 C 0.3212(2) 0.4267(5) 0.17182(12) 0.0467(10) Uani 1 1 d . . .
C8 C 0.3656(2) 0.7582(6) 0.10880(13) 0.0566(12) Uani 1 1 d . . .
H8A H 0.3707 0.8571 0.1221 0.068 Uiso 1 1 calc R . .
H8B H 0.3253 0.7566 0.0987 0.068 Uiso 1 1 calc R . .
C17 C 0.6303(2) 0.2315(5) 0.19120(11) 0.0454(10) Uani 1 1 d . . .
C12 C 0.6356(2) 0.5734(5) 0.12438(13) 0.0508(11) Uani 1 1 d . . .
H12 H 0.6673 0.6236 0.1125 0.061 Uiso 1 1 calc R . .
C14 C 0.7138(2) 0.4217(6) 0.15632(15) 0.0608(13) Uani 1 1 d . . .
H14 H 0.7420 0.4839 0.1442 0.073 Uiso 1 1 calc R . .
C15 C 0.7328(3) 0.3067(7) 0.17941(16) 0.0710(16) Uani 1 1 d . . .
H15 H 0.7737 0.2925 0.1837 0.085 Uiso 1 1 calc R . .
C19 C 0.4081(3) 0.0364(7) 0.25160(14) 0.0783(18) Uani 1 1 d . . .
H19A H 0.3931 0.0906 0.2727 0.117 Uiso 1 1 calc R . .
H19B H 0.4471 -0.0075 0.2568 0.117 Uiso 1 1 calc R . .
H19C H 0.3810 -0.0481 0.2451 0.117 Uiso 1 1 calc R . .
C20 C 0.6020(3) 0.0303(7) 0.23419(16) 0.087(2) Uani 1 1 d . . .
H20A H 0.6312 -0.0430 0.2246 0.131 Uiso 1 1 calc R . .
H20B H 0.5669 -0.0276 0.2418 0.131 Uiso 1 1 calc R . .
H20C H 0.6191 0.0856 0.2545 0.131 Uiso 1 1 calc R . .
C16 C 0.6908(2) 0.2095(6) 0.19681(14) 0.0606(14) Uani 1 1 d . . .
H16 H 0.7038 0.1293 0.2123 0.073 Uiso 1 1 calc R . .
N2 N 0.47159(17) 0.7512(4) 0.09480(9) 0.0394(8) Uani 1 1 d . . .
Na1 Na 0.49005(8) 0.13662(19) 0.17625(4) 0.0442(4) Uani 1 1 d . . .
O5 O 0.47076(13) 0.3856(3) 0.09236(7) 0.0378(6) Uani 1 1 d . . .
O2 O 0.41285(16) 0.1471(4) 0.22223(8) 0.0566(9) Uani 1 1 d . . .
C1 C 0.3713(2) 0.3448(5) 0.18464(11) 0.0421(10) Uani 1 1 d . . .
C2 C 0.3614(2) 0.2238(5) 0.21177(11) 0.0474(11) Uani 1 1 d . . .
P1 P 0.46294(5) 0.21174(12) 0.08475(3) 0.0360(2) Uani 1 1 d . . .
O7 O 0.39776(14) 0.1831(3) 0.06770(8) 0.0473(7) Uani 1 1 d . . .
C21 C 0.3658(2) 0.3042(5) 0.05008(12) 0.0451(10) Uani 1 1 d . . .
C22 C 0.3126(2) 0.3521(6) 0.06571(15) 0.0617(13) Uani 1 1 d . . .
H22 H 0.2993 0.3057 0.0871 0.074 Uiso 1 1 calc R . .
C3 C 0.3048(3) 0.1962(6) 0.22474(14) 0.0646(15) Uani 1 1 d . . .
H3 H 0.2991 0.1210 0.2430 0.078 Uiso 1 1 calc R . .
C24 C 0.2993(3) 0.5403(8) 0.0181(2) 0.0826(19) Uani 1 1 d . . .
H24 H 0.2772 0.6225 0.0077 0.099 Uiso 1 1 calc R . .
C4 C 0.2555(3) 0.2784(7) 0.21117(16) 0.0740(16) Uani 1 1 d . . .
H4 H 0.2171 0.2565 0.2200 0.089 Uiso 1 1 calc R . .
C5 C 0.2632(2) 0.3920(7) 0.18478(15) 0.0637(14) Uani 1 1 d . . .
H5 H 0.2300 0.4460 0.1755 0.076 Uiso 1 1 calc R . .
C26 C 0.3866(3) 0.3698(6) 0.01826(13) 0.0614(13) Uani 1 1 d . . .
H26 H 0.4224 0.3357 0.0077 0.074 Uiso 1 1 calc R . .
C23 C 0.2796(3) 0.4701(8) 0.0490(2) 0.0848(19) Uani 1 1 d . . .
H23 H 0.2431 0.5022 0.0591 0.102 Uiso 1 1 calc R . .
O6 O 0.47216(14) 0.0946(3) 0.11365(8) 0.0464(7) Uani 1 1 d . . .
O8 O 0.50263(13) 0.1662(4) 0.04960(7) 0.0444(7) Uani 1 1 d . . .
C27 C 0.5648(2) 0.1481(5) 0.05008(11) 0.0405(9) Uani 1 1 d . . .
C28 C 0.6010(2) 0.1970(6) 0.07811(12) 0.0500(11) Uani 1 1 d . . .
H28 H 0.5843 0.2477 0.0982 0.060 Uiso 1 1 calc R . .
C29 C 0.6627(2) 0.1704(7) 0.07636(15) 0.0682(15) Uani 1 1 d . . .
H29 H 0.6875 0.2040 0.0951 0.082 Uiso 1 1 calc R . .
C25 C 0.3514(3) 0.4906(7) 0.00243(16) 0.0791(18) Uani 1 1 d . . .
H25 H 0.3640 0.5373 -0.0191 0.095 Uiso 1 1 calc R . .
C32 C 0.5890(2) 0.0723(5) 0.02025(12) 0.0508(11) Uani 1 1 d . . .
H32 H 0.5643 0.0384 0.0014 0.061 Uiso 1 1 calc R . .
C31 C 0.6503(3) 0.0475(7) 0.01885(15) 0.0724(16) Uani 1 1 d . . .
H31 H 0.6672 -0.0017 -0.0013 0.087 Uiso 1 1 calc R . .
C30 C 0.6867(3) 0.0944(8) 0.04689(17) 0.0771(17) Uani 1 1 d . . .
H30 H 0.7279 0.0746 0.0459 0.093 Uiso 1 1 calc R . .
Cl1 Cl 0.49107(8) 0.79240(14) 0.18616(3) 0.0726(4) Uani 1 1 d . . .
H2 H 0.468(3) 0.848(9) 0.1057(19) 0.13(3) Uiso 1 1 d . . .


_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
Dy1 O1 2.211(3) . ?
Dy1 O3 2.232(3) . ?
Dy1 O5 2.294(3) . ?
Dy1 N2 2.493(3) . ?
Dy1 N1 2.515(4) . ?
Dy1 N3 2.530(4) . ?
Dy1 Cl1 2.6390(12) . ?
Dy1 Na1 3.6270(16) . ?
O3 C18 1.312(5) . ?
O3 Na1 2.426(3) . ?
O1 C1 1.313(5) . ?
O1 Na1 2.421(3) . ?
C7 N1 1.269(6) . ?
C7 C6 1.462(6) . ?
C7 H7 0.9300 . ?
O4 C17 1.369(6) . ?
O4 C20 1.425(5) . ?
O4 Na1 2.406(4) . ?
C11 N3 1.476(5) . ?
C11 C10 1.503(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C9 N2 1.464(6) . ?
C9 C8 1.506(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C18 C13 1.401(6) . ?
C18 C17 1.424(6) . ?
N1 C8 1.469(5) . ?
C10 N2 1.475(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C13 C14 1.408(6) . ?
C13 C12 1.462(6) . ?
N3 C12 1.275(6) . ?
C6 C1 1.391(6) . ?
C6 C5 1.403(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C17 C16 1.371(6) . ?
C12 H12 0.9300 . ?
C14 C15 1.354(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.395(8) . ?
C15 H15 0.9300 . ?
C19 O2 1.431(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C16 H16 0.9300 . ?
N2 H2 0.91(8) . ?
Na1 O6 2.371(3) . ?
Na1 O2 2.414(4) . ?
Na1 Cl1 2.905(2) 1_545 ?
O5 P1 1.493(3) . ?
O2 C2 1.366(6) . ?
C1 C2 1.442(6) . ?
C2 C3 1.365(7) . ?
P1 O6 1.464(3) . ?
P1 O7 1.596(3) . ?
P1 O8 1.614(3) . ?
O7 C21 1.398(5) . ?
C21 C22 1.373(7) . ?
C21 C26 1.377(6) . ?
C22 C23 1.377(8) . ?
C22 H22 0.9300 . ?
C3 C4 1.386(8) . ?
C3 H3 0.9300 . ?
C24 C23 1.356(9) . ?
C24 C25 1.358(9) . ?
C24 H24 0.9300 . ?
C4 C5 1.372(8) . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C26 C25 1.406(8) . ?
C26 H26 0.9300 . ?
C23 H23 0.9300 . ?
O8 C27 1.389(5) . ?
C27 C28 1.372(6) . ?
C27 C32 1.380(6) . ?
C28 C29 1.389(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.368(7) . ?
C29 H29 0.9300 . ?
C25 H25 0.9300 . ?
C32 C31 1.377(7) . ?
C32 H32 0.9300 . ?
C31 C30 1.371(8) . ?
C31 H31 0.9300 . ?
C30 H30 0.9300 . ?
Cl1 Na1 2.905(2) 1_565 ?

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
O1 Dy1 O3 77.21(10) . . ?
O1 Dy1 O5 89.49(10) . . ?
O3 Dy1 O5 89.06(10) . . ?
O1 Dy1 N2 140.60(11) . . ?
O3 Dy1 N2 139.34(11) . . ?
O5 Dy1 N2 79.41(10) . . ?
O1 Dy1 N1 73.31(11) . . ?
O3 Dy1 N1 150.16(11) . . ?
O5 Dy1 N1 86.20(11) . . ?
N2 Dy1 N1 68.36(12) . . ?
O1 Dy1 N3 149.28(11) . . ?
O3 Dy1 N3 72.36(11) . . ?
O5 Dy1 N3 85.95(11) . . ?
N2 Dy1 N3 68.06(12) . . ?
N1 Dy1 N3 136.42(12) . . ?
O1 Dy1 Cl1 103.71(8) . . ?
O3 Dy1 Cl1 104.32(8) . . ?
O5 Dy1 Cl1 162.87(7) . . ?
N2 Dy1 Cl1 83.46(8) . . ?
N1 Dy1 Cl1 87.21(9) . . ?
N3 Dy1 Cl1 87.98(9) . . ?
O1 Dy1 Na1 40.57(8) . . ?
O3 Dy1 Na1 40.83(8) . . ?
O5 Dy1 Na1 75.05(7) . . ?
N2 Dy1 Na1 154.46(8) . . ?
N1 Dy1 Na1 109.82(9) . . ?
N3 Dy1 Na1 109.30(9) . . ?
Cl1 Dy1 Na1 122.08(4) . . ?
C18 O3 Dy1 141.6(3) . . ?
C18 O3 Na1 115.8(2) . . ?
Dy1 O3 Na1 102.20(11) . . ?
C1 O1 Dy1 142.0(3) . . ?
C1 O1 Na1 113.1(3) . . ?
Dy1 O1 Na1 102.98(12) . . ?
N1 C7 C6 128.3(4) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
C17 O4 C20 118.3(4) . . ?
C17 O4 Na1 116.7(2) . . ?
C20 O4 Na1 122.9(3) . . ?
N3 C11 C10 109.4(4) . . ?
N3 C11 H11A 109.8 . . ?
C10 C11 H11A 109.8 . . ?
N3 C11 H11B 109.8 . . ?
C10 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
N2 C9 C8 108.4(4) . . ?
N2 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
N2 C9 H9B 110.0 . . ?
C8 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
O3 C18 C13 124.0(4) . . ?
O3 C18 C17 118.7(4) . . ?
C13 C18 C17 117.3(4) . . ?
C7 N1 C8 116.7(4) . . ?
C7 N1 Dy1 129.4(3) . . ?
C8 N1 Dy1 113.9(3) . . ?
N2 C10 C11 107.9(4) . . ?
N2 C10 H10A 110.1 . . ?
C11 C10 H10A 110.1 . . ?
N2 C10 H10B 110.1 . . ?
C11 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
C18 C13 C14 120.2(4) . . ?
C18 C13 C12 122.3(4) . . ?
C14 C13 C12 117.5(4) . . ?
C12 N3 C11 115.8(4) . . ?
C12 N3 Dy1 129.8(3) . . ?
C11 N3 Dy1 114.2(3) . . ?
C1 C6 C5 121.1(4) . . ?
C1 C6 C7 122.2(4) . . ?
C5 C6 C7 116.7(5) . . ?
N1 C8 C9 109.4(4) . . ?
N1 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
N1 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
O4 C17 C16 124.9(4) . . ?
O4 C17 C18 114.1(4) . . ?
C16 C17 C18 121.0(5) . . ?
N3 C12 C13 127.5(4) . . ?
N3 C12 H12 116.2 . . ?
C13 C12 H12 116.2 . . ?
C15 C14 C13 121.2(5) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 119.8(5) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
O2 C19 H19A 109.5 . . ?
O2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C16 C15 120.5(5) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C9 N2 C10 114.1(3) . . ?
C9 N2 Dy1 111.4(2) . . ?
C10 N2 Dy1 109.8(2) . . ?
C9 N2 H2 96(5) . . ?
C10 N2 H2 117(5) . . ?
Dy1 N2 H2 108(5) . . ?
O6 Na1 O4 127.60(13) . . ?
O6 Na1 O2 124.88(14) . . ?
O4 Na1 O2 107.10(13) . . ?
O6 Na1 O1 89.50(11) . . ?
O4 Na1 O1 120.62(12) . . ?
O2 Na1 O1 65.31(11) . . ?
O6 Na1 O3 91.49(11) . . ?
O4 Na1 O3 65.48(11) . . ?
O2 Na1 O3 119.90(12) . . ?
O1 Na1 O3 69.78(10) . . ?
O6 Na1 Cl1 88.67(8) . 1_545 ?
O4 Na1 Cl1 87.42(9) . 1_545 ?
O2 Na1 Cl1 87.31(10) . 1_545 ?
O1 Na1 Cl1 144.73(11) . 1_545 ?
O3 Na1 Cl1 145.47(11) . 1_545 ?
O6 Na1 Dy1 78.38(7) . . ?
O4 Na1 Dy1 100.62(9) . . ?
O2 Na1 Dy1 99.83(9) . . ?
O1 Na1 Dy1 36.45(7) . . ?
O3 Na1 Dy1 36.98(7) . . ?
Cl1 Na1 Dy1 167.05(6) 1_545 . ?
P1 O5 Dy1 136.58(15) . . ?
C2 O2 C19 117.2(4) . . ?
C2 O2 Na1 114.3(2) . . ?
C19 O2 Na1 124.2(3) . . ?
O1 C1 C6 124.4(4) . . ?
O1 C1 C2 118.2(4) . . ?
C6 C1 C2 117.4(4) . . ?
C3 C2 O2 126.3(4) . . ?
C3 C2 C1 120.2(5) . . ?
O2 C2 C1 113.5(4) . . ?
O6 P1 O5 120.00(16) . . ?
O6 P1 O7 108.28(17) . . ?
O5 P1 O7 109.02(16) . . ?
O6 P1 O8 110.57(17) . . ?
O5 P1 O8 108.56(16) . . ?
O7 P1 O8 98.20(16) . . ?
C21 O7 P1 122.4(3) . . ?
C22 C21 C26 122.1(5) . . ?
C22 C21 O7 116.9(4) . . ?
C26 C21 O7 121.0(4) . . ?
C21 C22 C23 118.7(6) . . ?
C21 C22 H22 120.7 . . ?
C23 C22 H22 120.7 . . ?
C2 C3 C4 121.0(5) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C23 C24 C25 120.1(6) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.0(5) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C21 C26 C25 117.0(5) . . ?
C21 C26 H26 121.5 . . ?
C25 C26 H26 121.5 . . ?
C24 C23 C22 121.0(6) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
P1 O6 Na1 129.37(16) . . ?
C27 O8 P1 123.9(2) . . ?
C28 C27 C32 120.8(4) . . ?
C28 C27 O8 124.0(4) . . ?
C32 C27 O8 115.3(4) . . ?
C27 C28 C29 119.6(4) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C30 C29 C28 119.7(5) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C24 C25 C26 121.1(6) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C31 C32 C27 118.9(5) . . ?
C31 C32 H32 120.5 . . ?
C27 C32 H32 120.5 . . ?
C30 C31 C32 120.7(5) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C29 C30 C31 120.3(5) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
Dy1 Cl1 Na1 135.01(6) . 1_565 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.63
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.391
_refine_diff_density_min         -1.942
_refine_diff_density_rms         0.080
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-DyvaldienPOH
_database_code_depnum_ccdc_archive 'CCDC 1415418'
_audit_update_record             
;
2015-07-28 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H33 Dy N3 O8 P'
_chemical_formula_weight         781.08

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'
Dy Dy -0.1892 4.4098 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.0268(15)
_cell_length_b                   11.6462(16)
_cell_length_c                   27.317(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.808(4)
_cell_angle_gamma                90.00
_cell_volume                     3209.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3693
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      23.46

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1564
_exptl_absorpt_coefficient_mu    2.432
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5929
_exptl_absorpt_correction_T_max  0.6969
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20718
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         27.62
_reflns_number_total             7318
_reflns_number_gt                5247
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0445P)²+0.0000P] where P=(Fo²+2Fc²)/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_number_reflns         7318
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0390
_refine_ls_wR_factor_ref         0.1016
_refine_ls_wR_factor_gt          0.0818
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_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
Dy1 Dy -0.57496(2) -0.056126(18) -0.249896(9) 0.02863(8) Uani 1 1 d . . .
P1 P -0.51342(13) 0.18484(10) -0.32330(5) 0.0320(3) Uani 1 1 d . . .
O1 O -0.4215(3) 0.0256(3) -0.17973(15) 0.0414(9) Uani 1 1 d . . .
O2 O -0.3362(4) 0.1072(3) -0.07673(16) 0.0551(11) Uani 1 1 d . . .
O3 O -0.7060(3) 0.0123(3) -0.21377(15) 0.0411(9) Uani 1 1 d . . .
O4 O -0.7472(4) 0.1315(4) -0.13961(19) 0.0607(12) Uani 1 1 d . . .
O5 O -0.5731(3) 0.0899(3) -0.30416(14) 0.0381(9) Uani 1 1 d . . .
O6 O -0.4235(3) 0.2656(3) -0.28422(14) 0.0364(8) Uani 1 1 d . . .
O7 O -0.6244(4) 0.2615(3) -0.36591(15) 0.0441(9) Uani 1 1 d . . .
O8 O -0.4404(4) 0.1223(3) -0.35584(16) 0.0489(10) Uani 1 1 d . . .
N1 N -0.3517(4) -0.1131(4) -0.24860(18) 0.0385(10) Uani 1 1 d . . .
N2 N -0.5966(4) -0.1725(4) -0.33134(17) 0.0409(11) Uani 1 1 d . . .
H2 H -0.6034 -0.2473 -0.3230 0.049 Uiso 1 1 d R . .
N3 N -0.8131(4) -0.0849(4) -0.31536(18) 0.0399(11) Uani 1 1 d . . .
C1 C -0.2957(6) 0.0197(4) -0.1486(2) 0.0415(13) Uani 1 1 d . . .
C2 C -0.2501(6) 0.0624(4) -0.0956(2) 0.0433(13) Uani 1 1 d . . .
C3 C -0.1175(6) 0.0637(5) -0.0628(3) 0.0615(18) Uani 1 1 d . . .
H3 H -0.0889 0.0924 -0.0282 0.074 Uiso 1 1 calc R . .
C4 C -0.0239(7) 0.0207(6) -0.0820(3) 0.071(2) Uani 1 1 d . . .
H4 H 0.0663 0.0240 -0.0604 0.085 Uiso 1 1 calc R . .
C5 C -0.0661(6) -0.0245(5) -0.1313(3) 0.0549(16) Uani 1 1 d . . .
H5 H -0.0041 -0.0549 -0.1428 0.066 Uiso 1 1 calc R . .
C6 C -0.1998(5) -0.0274(4) -0.1657(2) 0.0406(13) Uani 1 1 d . . .
C7 C -0.2374(6) -0.0863(5) -0.2154(2) 0.0454(14) Uani 1 1 d . . .
H7 H -0.1680 -0.1079 -0.2246 0.054 Uiso 1 1 calc R . .
C8 C -0.3568(6) -0.1869(5) -0.2947(3) 0.0557(17) Uani 1 1 d . . .
H8A H -0.2794 -0.1717 -0.3021 0.067 Uiso 1 1 calc R . .
H8B H -0.3547 -0.2672 -0.2849 0.067 Uiso 1 1 calc R . .
C9 C -0.4762(6) -0.1649(5) -0.3427(2) 0.0539(16) Uani 1 1 d . . .
H9A H -0.4822 -0.2203 -0.3700 0.065 Uiso 1 1 calc R . .
H9B H -0.4709 -0.0889 -0.3562 0.065 Uiso 1 1 calc R . .
C10 C -0.7176(6) -0.1455(5) -0.3764(2) 0.0500(15) Uani 1 1 d . . .
H10A H -0.7281 -0.1963 -0.4060 0.060 Uiso 1 1 calc R . .
H10B H -0.7138 -0.0672 -0.3878 0.060 Uiso 1 1 calc R . .
C11 C -0.8306(6) -0.1583(6) -0.3619(2) 0.0558(16) Uani 1 1 d . . .
H11A H -0.8387 -0.2379 -0.3533 0.067 Uiso 1 1 calc R . .
H11B H -0.9114 -0.1367 -0.3920 0.067 Uiso 1 1 calc R . .
C12 C -0.9169(5) -0.0335(5) -0.3159(2) 0.0461(14) Uani 1 1 d . . .
H12 H -0.9944 -0.0452 -0.3463 0.055 Uiso 1 1 calc R . .
C13 C -0.9289(5) 0.0387(5) -0.2762(3) 0.0475(15) Uani 1 1 d . . .
C14 C -1.0524(6) 0.0927(6) -0.2874(3) 0.075(2) Uani 1 1 d . . .
H14 H -1.1221 0.0812 -0.3205 0.090 Uiso 1 1 calc R . .
C15 C -1.0708(7) 0.1602(7) -0.2510(4) 0.086(3) Uani 1 1 d . . .
H15 H -1.1516 0.1972 -0.2597 0.103 Uiso 1 1 calc R . .
C16 C -0.9704(7) 0.1751(6) -0.2008(3) 0.068(2) Uani 1 1 d . . .
H16 H -0.9845 0.2207 -0.1756 0.082 Uiso 1 1 calc R . .
C17 C -0.8505(6) 0.1229(5) -0.1881(3) 0.0474(15) Uani 1 1 d . . .
C18 C -0.8244(5) 0.0551(4) -0.2261(2) 0.0397(13) Uani 1 1 d . . .
C19 C -0.4342(7) 0.0289(6) -0.0740(3) 0.070(2) Uani 1 1 d . . .
H19A H -0.5086 0.0266 -0.1080 0.104 Uiso 1 1 calc R . .
H19B H -0.4630 0.0543 -0.0470 0.104 Uiso 1 1 calc R . .
H19C H -0.3964 -0.0464 -0.0651 0.104 Uiso 1 1 calc R . .
C20 C -0.7598(8) 0.2071(6) -0.1015(3) 0.084(2) Uani 1 1 d . . .
H20A H -0.7841 0.2821 -0.1170 0.126 Uiso 1 1 calc R . .
H20B H -0.6768 0.2116 -0.0709 0.126 Uiso 1 1 calc R . .
H20C H -0.8271 0.1791 -0.0906 0.126 Uiso 1 1 calc R . .
C21 C -0.7427(6) 0.2178(5) -0.4037(2) 0.0469(15) Uani 1 1 d . . .
C22 C -0.7532(8) 0.2038(7) -0.4550(3) 0.091(3) Uani 1 1 d . . .
H22 H -0.6818 0.2198 -0.4638 0.109 Uiso 1 1 calc R . .
C23 C -0.8719(10) 0.1654(10) -0.4936(3) 0.130(4) Uani 1 1 d . . .
H23 H -0.8807 0.1530 -0.5285 0.156 Uiso 1 1 calc R . .
C24 C -0.9774(9) 0.1454(8) -0.4796(4) 0.106(3) Uani 1 1 d . . .
H24 H -1.0593 0.1245 -0.5058 0.127 Uiso 1 1 calc R . .
C25 C -0.9633(7) 0.1560(6) -0.4287(4) 0.082(2) Uani 1 1 d . . .
H25 H -1.0336 0.1382 -0.4194 0.098 Uiso 1 1 calc R . .
C26 C -0.8438(6) 0.1933(5) -0.3897(3) 0.0573(17) Uani 1 1 d . . .
H26 H -0.8337 0.2013 -0.3544 0.069 Uiso 1 1 calc R . .
C27 C -0.3929(6) 0.1748(5) -0.3904(2) 0.0465(14) Uani 1 1 d . . .
C28 C -0.3446(6) 0.2838(5) -0.3833(3) 0.0562(16) Uani 1 1 d . . .
H28 H -0.3418 0.3279 -0.3545 0.067 Uiso 1 1 calc R . .
C29 C -0.2993(7) 0.3281(7) -0.4206(4) 0.078(2) Uani 1 1 d . . .
H29 H -0.2660 0.4025 -0.4167 0.093 Uiso 1 1 calc R . .
C30 C -0.3041(9) 0.2617(10) -0.4627(4) 0.098(3) Uani 1 1 d . . .
H30 H -0.2763 0.2922 -0.4879 0.118 Uiso 1 1 calc R . .
C31 C -0.3486(9) 0.1522(10) -0.4681(4) 0.104(3) Uani 1 1 d . . .
H31 H -0.3486 0.1072 -0.4962 0.125 Uiso 1 1 calc R . .
C32 C -0.3935(8) 0.1079(7) -0.4321(3) 0.082(2) Uani 1 1 d . . .
H32 H -0.4245 0.0328 -0.4358 0.098 Uiso 1 1 calc R . .


_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
Dy1 O1 2.197(3) . ?
Dy1 O3 2.202(3) . ?
Dy1 O5 2.261(3) . ?
Dy1 O6 2.279(3) 2_444 ?
Dy1 N3 2.532(4) . ?
Dy1 N2 2.533(4) . ?
Dy1 N1 2.536(4) . ?
P1 O6 1.467(3) . ?
P1 O5 1.486(3) . ?
P1 O7 1.581(4) . ?
P1 O8 1.597(4) . ?
O1 C1 1.304(6) . ?
O2 C2 1.354(7) . ?
O2 C19 1.438(7) . ?
O3 C18 1.308(6) . ?
O4 C17 1.357(7) . ?
O4 C20 1.413(7) . ?
O6 Dy1 2.279(3) 2_454 ?
O7 C21 1.393(6) . ?
O8 C27 1.392(6) . ?
N1 C7 1.260(7) . ?
N1 C8 1.507(7) . ?
N2 C10 1.439(7) . ?
N2 C9 1.482(7) . ?
N2 H2 0.9101 . ?
N3 C12 1.287(7) . ?
N3 C11 1.479(7) . ?
C1 C2 1.418(8) . ?
C1 C6 1.427(8) . ?
C2 C3 1.372(8) . ?
C3 C4 1.424(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.342(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.424(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.457(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.459(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.420(8) . ?
C12 H12 0.9300 . ?
C13 C18 1.402(8) . ?
C13 C14 1.418(8) . ?
C14 C15 1.345(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.382(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.367(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.424(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C26 1.346(8) . ?
C21 C22 1.369(9) . ?
C22 C23 1.382(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.383(13) . ?
C23 H23 0.9300 . ?
C24 C25 1.342(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.387(9) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.360(8) . ?
C27 C32 1.379(9) . ?
C28 C29 1.400(9) . ?
C28 H28 0.9300 . ?
C29 C30 1.370(12) . ?
C29 H29 0.9300 . ?
C30 C31 1.352(13) . ?
C30 H30 0.9300 . ?
C31 C32 1.367(11) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?

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
O1 Dy1 O3 82.28(13) . . ?
O1 Dy1 O5 92.21(13) . . ?
O3 Dy1 O5 101.69(13) . . ?
O1 Dy1 O6 99.69(13) . 2_444 ?
O3 Dy1 O6 91.83(13) . 2_444 ?
O5 Dy1 O6 163.10(13) . 2_444 ?
O1 Dy1 N3 152.56(14) . . ?
O3 Dy1 N3 71.56(14) . . ?
O5 Dy1 N3 85.28(13) . . ?
O6 Dy1 N3 89.50(13) 2_444 . ?
O1 Dy1 N2 139.87(14) . . ?
O3 Dy1 N2 137.85(13) . . ?
O5 Dy1 N2 81.33(14) . . ?
O6 Dy1 N2 81.83(13) 2_444 . ?
N3 Dy1 N2 66.78(14) . . ?
O1 Dy1 N1 72.52(14) . . ?
O3 Dy1 N1 153.81(14) . . ?
O5 Dy1 N1 86.58(13) . . ?
O6 Dy1 N1 85.61(13) 2_444 . ?
N3 Dy1 N1 134.35(15) . . ?
N2 Dy1 N1 67.59(14) . . ?
O6 P1 O5 119.1(2) . . ?
O6 P1 O7 105.6(2) . . ?
O5 P1 O7 111.0(2) . . ?
O6 P1 O8 110.7(2) . . ?
O5 P1 O8 104.5(2) . . ?
O7 P1 O8 105.2(2) . . ?
C1 O1 Dy1 142.0(3) . . ?
C2 O2 C19 115.6(4) . . ?
C18 O3 Dy1 142.2(4) . . ?
C17 O4 C20 118.1(5) . . ?
P1 O5 Dy1 155.9(2) . . ?
P1 O6 Dy1 140.1(2) . 2_454 ?
C21 O7 P1 123.6(3) . . ?
C27 O8 P1 126.1(3) . . ?
C7 N1 C8 115.6(4) . . ?
C7 N1 Dy1 129.0(4) . . ?
C8 N1 Dy1 115.4(3) . . ?
C10 N2 C9 114.1(5) . . ?
C10 N2 Dy1 111.1(3) . . ?
C9 N2 Dy1 112.1(3) . . ?
C10 N2 H2 106.3 . . ?
C9 N2 H2 106.3 . . ?
Dy1 N2 H2 106.3 . . ?
C12 N3 C11 116.8(5) . . ?
C12 N3 Dy1 127.6(4) . . ?
C11 N3 Dy1 115.0(3) . . ?
O1 C1 C2 119.5(5) . . ?
O1 C1 C6 122.7(5) . . ?
C2 C1 C6 117.8(5) . . ?
O2 C2 C3 118.3(6) . . ?
O2 C2 C1 120.6(5) . . ?
C3 C2 C1 121.0(6) . . ?
C2 C3 C4 119.7(6) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 119.9(6) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 122.1(7) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C5 C6 C7 118.5(5) . . ?
C5 C6 C1 119.4(6) . . ?
C7 C6 C1 121.9(5) . . ?
N1 C7 C6 128.8(5) . . ?
N1 C7 H7 115.6 . . ?
C6 C7 H7 115.6 . . ?
C9 C8 N1 111.5(4) . . ?
C9 C8 H8A 109.3 . . ?
N1 C8 H8A 109.3 . . ?
C9 C8 H8B 109.3 . . ?
N1 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C8 C9 N2 111.2(5) . . ?
C8 C9 H9A 109.4 . . ?
N2 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
N2 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 C11 110.2(5) . . ?
N2 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
N2 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C10 C11 N3 110.1(5) . . ?
C10 C11 H11A 109.6 . . ?
N3 C11 H11A 109.6 . . ?
C10 C11 H11B 109.6 . . ?
N3 C11 H11B 109.6 . . ?
H11A C11 H11B 108.2 . . ?
N3 C12 C13 128.5(5) . . ?
N3 C12 H12 115.7 . . ?
C13 C12 H12 115.7 . . ?
C18 C13 C14 119.3(6) . . ?
C18 C13 C12 122.3(5) . . ?
C14 C13 C12 118.4(6) . . ?
C15 C14 C13 121.2(7) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 120.5(6) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 120.1(7) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
O4 C17 C16 124.1(6) . . ?
O4 C17 C18 114.5(5) . . ?
C16 C17 C18 121.4(7) . . ?
O3 C18 C13 122.7(5) . . ?
O3 C18 C17 119.9(5) . . ?
C13 C18 C17 117.4(5) . . ?
O2 C19 H19A 109.5 . . ?
O2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 121.8(6) . . ?
C26 C21 O7 120.2(6) . . ?
C22 C21 O7 118.0(6) . . ?
C21 C22 C23 118.8(8) . . ?
C21 C22 H22 120.6 . . ?
C23 C22 H22 120.6 . . ?
C22 C23 C24 119.2(9) . . ?
C22 C23 H23 120.4 . . ?
C24 C23 H23 120.4 . . ?
C25 C24 C23 120.8(8) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 120.0(8) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 119.3(7) . . ?
C21 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C28 C27 C32 121.1(6) . . ?
C28 C27 O8 123.2(5) . . ?
C32 C27 O8 115.7(6) . . ?
C27 C28 C29 118.3(7) . . ?
C27 C28 H28 120.8 . . ?
C29 C28 H28 120.8 . . ?
C30 C29 C28 119.9(8) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C31 C30 C29 120.9(8) . . ?
C31 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C30 C31 C32 119.9(8) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C31 C32 C27 119.9(8) . . ?
C31 C32 H32 120.1 . . ?
C27 C32 H32 120.1 . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.154
###END
#==============================================================================
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-GdvaldienPONa
_database_code_depnum_ccdc_archive 'CCDC 1432155'
_audit_update_record             
;
2015-10-20 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H33 Cl Gd N3 Na O8 P'
_chemical_formula_weight         834.27

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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   'Pbca '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.267(3)
_cell_length_b                   8.4192(13)
_cell_length_c                   36.839(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6906.3(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9716
_cell_measurement_theta_min      2.64
_cell_measurement_theta_max      26.26

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3336
_exptl_absorpt_coefficient_mu    2.110
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5517
_exptl_absorpt_correction_T_max  0.5896
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42211
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         27.47
_reflns_number_total             7834
_reflns_number_gt                6370
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0153P)²+11.8957P] where P=(Fo²+2Fc²)/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_number_reflns         7834
_refine_ls_number_parameters     426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_ref         0.0778
_refine_ls_wR_factor_gt          0.0738
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_restrained_S_all      1.173
_refine_ls_shift/su_max          0.001
_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
Gd1 Gd 0.518237(9) 1.04488(2) 0.143472(5) 0.03196(6) Uani 1 1 d . . .
C13 C 0.6798(2) 0.9264(5) 0.17140(12) 0.0471(11) Uani 1 1 d . . .
C17 C 0.6404(2) 0.7242(5) 0.21180(11) 0.0458(11) Uani 1 1 d . . .
C18 C 0.6300(2) 0.8438(5) 0.18463(11) 0.0408(10) Uani 1 1 d . . .
C15 C 0.7461(3) 0.7791(7) 0.21078(16) 0.0750(17) Uani 1 1 d . . .
H15 H 0.7845 0.7582 0.2195 0.090 Uiso 1 1 calc R . .
C14 C 0.7379(2) 0.8911(6) 0.18426(15) 0.0624(14) Uani 1 1 d . . .
H14 H 0.7709 0.9442 0.1747 0.075 Uiso 1 1 calc R . .
C16 C 0.6975(3) 0.6968(6) 0.22469(14) 0.0659(15) Uani 1 1 d . . .
H16 H 0.7035 0.6221 0.2429 0.079 Uiso 1 1 calc R . .
O1 O 0.41346(15) 0.6416(4) 0.20676(8) 0.0550(8) Uani 1 1 d . . .
O2 O 0.58941(16) 0.6471(4) 0.22252(8) 0.0577(9) Uani 1 1 d . . .
N3 N 0.62711(17) 1.1222(4) 0.13335(9) 0.0454(9) Uani 1 1 d . . .
C12 C 0.6749(2) 1.0582(5) 0.14579(13) 0.0496(11) Uani 1 1 d . . .
H12 H 0.7110 1.1006 0.1375 0.060 Uiso 1 1 calc R . .
C10 C 0.5890(2) 1.2499(5) 0.07885(12) 0.0512(12) Uani 1 1 d . . .
H10A H 0.5939 1.3400 0.0627 0.061 Uiso 1 1 calc R . .
H10B H 0.5944 1.1535 0.0648 0.061 Uiso 1 1 calc R . .
C11 C 0.6349(2) 1.2572(6) 0.10871(13) 0.0560(12) Uani 1 1 d . . .
H11A H 0.6750 1.2547 0.0983 0.067 Uiso 1 1 calc R . .
H11B H 0.6305 1.3557 0.1221 0.067 Uiso 1 1 calc R . .
N2 N 0.52874(16) 1.2524(4) 0.09479(9) 0.0396(8) Uani 1 1 d . . .
H2 H 0.5243 1.3485 0.1058 0.048 Uiso 1 1 calc R . .
C9 C 0.4794(2) 1.2367(5) 0.06860(12) 0.0509(11) Uani 1 1 d . . .
H9A H 0.4821 1.1352 0.0562 0.061 Uiso 1 1 calc R . .
H9B H 0.4820 1.3204 0.0506 0.061 Uiso 1 1 calc R . .
C8 C 0.4207(2) 1.2482(6) 0.08859(14) 0.0621(14) Uani 1 1 d . . .
H8A H 0.4176 1.3512 0.1002 0.075 Uiso 1 1 calc R . .
H8B H 0.3877 1.2380 0.0716 0.075 Uiso 1 1 calc R . .
N1 N 0.41683(17) 1.1215(4) 0.11619(10) 0.0454(9) Uani 1 1 d . . .
C7 C 0.3643(2) 1.0718(5) 0.12408(12) 0.0504(11) Uani 1 1 d . . .
H7 H 0.3326 1.1203 0.1119 0.060 Uiso 1 1 calc R . .
C1 C 0.3907(2) 0.8530(5) 0.16796(11) 0.0392(9) Uani 1 1 d . . .
C6 C 0.3480(2) 0.9481(5) 0.14993(12) 0.0458(10) Uani 1 1 d . . .
C5 C 0.2858(2) 0.9199(6) 0.15565(15) 0.0602(13) Uani 1 1 d . . .
H5 H 0.2577 0.9814 0.1434 0.072 Uiso 1 1 calc R . .
C2 C 0.3689(2) 0.7306(5) 0.19098(12) 0.0445(10) Uani 1 1 d . . .
C4 C 0.2667(2) 0.8046(7) 0.17879(16) 0.0698(16) Uani 1 1 d . . .
H4 H 0.2258 0.7902 0.1829 0.084 Uiso 1 1 calc R . .
C3 C 0.3083(2) 0.7083(6) 0.19628(14) 0.0607(14) Uani 1 1 d . . .
H3 H 0.2951 0.6281 0.2117 0.073 Uiso 1 1 calc R . .
Cl1 Cl 0.50966(8) 1.29646(14) 0.18728(3) 0.0745(4) Uani 1 1 d . . .
O4 O 0.44896(13) 0.8710(3) 0.16391(7) 0.0412(7) Uani 1 1 d . . .
O3 O 0.57456(13) 0.8716(3) 0.17445(7) 0.0434(7) Uani 1 1 d . . .
P1 P 0.53733(5) 0.71263(12) 0.08485(3) 0.0356(2) Uani 1 1 d . . .
O6 O 0.52807(14) 0.5959(3) 0.11401(7) 0.0452(7) Uani 1 1 d . . .
O5 O 0.52924(13) 0.8864(3) 0.09216(7) 0.0379(6) Uani 1 1 d . . .
O8 O 0.60246(13) 0.6845(3) 0.06752(8) 0.0458(7) Uani 1 1 d . . .
O7 O 0.49761(13) 0.6659(3) 0.04961(8) 0.0446(7) Uani 1 1 d . . .
C21 C 0.4355(2) 0.6467(5) 0.05010(11) 0.0406(10) Uani 1 1 d . . .
C22 C 0.3993(2) 0.6963(5) 0.07816(12) 0.0495(11) Uani 1 1 d . . .
H22 H 0.4157 0.7481 0.0981 0.059 Uiso 1 1 calc R . .
C26 C 0.4115(2) 0.5714(5) 0.02025(11) 0.0489(11) Uani 1 1 d . . .
H26 H 0.4362 0.5381 0.0014 0.059 Uiso 1 1 calc R . .
C25 C 0.3507(2) 0.5463(7) 0.01878(15) 0.0694(15) Uani 1 1 d . . .
H25 H 0.3340 0.4970 -0.0014 0.083 Uiso 1 1 calc R . .
C24 C 0.3142(2) 0.5934(7) 0.04696(17) 0.0748(17) Uani 1 1 d . . .
H24 H 0.2731 0.5739 0.0460 0.090 Uiso 1 1 calc R . .
C23 C 0.3382(2) 0.6685(6) 0.07632(15) 0.0652(14) Uani 1 1 d . . .
H23 H 0.3134 0.7012 0.0952 0.078 Uiso 1 1 calc R . .
C28 C 0.6876(2) 0.8531(6) 0.06518(15) 0.0602(13) Uani 1 1 d . . .
H28 H 0.7013 0.8068 0.0866 0.072 Uiso 1 1 calc R . .
C30 C 0.7002(3) 1.0398(7) 0.0177(2) 0.0816(19) Uani 1 1 d . . .
H30 H 0.7223 1.1210 0.0070 0.098 Uiso 1 1 calc R . .
C29 C 0.7204(3) 0.9705(7) 0.04857(19) 0.0790(17) Uani 1 1 d . . .
H29 H 0.7568 1.0027 0.0586 0.095 Uiso 1 1 calc R . .
C27 C 0.6341(2) 0.8047(5) 0.04986(12) 0.0433(10) Uani 1 1 d . . .
C31 C 0.6470(3) 0.9909(7) 0.00204(16) 0.0766(18) Uani 1 1 d . . .
H31 H 0.6336 1.0378 -0.0193 0.092 Uiso 1 1 calc R . .
C32 C 0.6135(2) 0.8710(6) 0.01835(13) 0.0595(13) Uani 1 1 d . . .
H32 H 0.5777 0.8365 0.0080 0.071 Uiso 1 1 calc R . .
C20 C 0.5944(3) 0.5369(6) 0.25186(14) 0.0772(17) Uani 1 1 d . . .
H20A H 0.6208 0.4519 0.2450 0.116 Uiso 1 1 calc R . .
H20B H 0.5554 0.4947 0.2575 0.116 Uiso 1 1 calc R . .
H20C H 0.6103 0.5902 0.2728 0.116 Uiso 1 1 calc R . .
C19 C 0.3964(3) 0.5294(7) 0.23406(16) 0.085(2) Uani 1 1 d . . .
H19A H 0.3744 0.5827 0.2528 0.128 Uiso 1 1 calc R . .
H19B H 0.4318 0.4817 0.2442 0.128 Uiso 1 1 calc R . .
H19C H 0.3717 0.4484 0.2234 0.128 Uiso 1 1 calc R . .
Na1 Na 0.51056(8) 0.63796(19) 0.17695(4) 0.0450(4) Uani 1 1 d . . .


_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
Gd1 O3 2.237(3) . ?
Gd1 O4 2.256(3) . ?
Gd1 O5 2.327(3) . ?
Gd1 N2 2.515(3) . ?
Gd1 N3 2.538(4) . ?
Gd1 N1 2.554(4) . ?
Gd1 Cl1 2.6698(12) . ?
Gd1 Na1 3.6452(16) . ?
C13 C18 1.396(6) . ?
C13 C14 1.410(6) . ?
C13 C12 1.460(6) . ?
C17 O2 1.366(6) . ?
C17 C16 1.376(7) . ?
C17 C18 1.439(6) . ?
C18 O3 1.312(5) . ?
C15 C14 1.370(7) . ?
C15 C16 1.384(8) . ?
O1 C2 1.372(5) . ?
O1 C19 1.431(5) . ?
O1 Na1 2.425(4) . ?
O2 C20 1.429(5) . ?
O2 Na1 2.430(4) . ?
N3 C12 1.279(5) . ?
N3 C11 1.465(5) . ?
C10 N2 1.464(5) . ?
C10 C11 1.504(6) . ?
N2 C9 1.468(5) . ?
C9 C8 1.502(7) . ?
C8 N1 1.476(5) . ?
N1 C7 1.277(6) . ?
C7 C6 1.457(6) . ?
C1 O4 1.315(5) . ?
C1 C6 1.409(6) . ?
C1 C2 1.420(6) . ?
C6 C5 1.420(6) . ?
C5 C4 1.361(7) . ?
C2 C3 1.376(6) . ?
C4 C3 1.390(7) . ?
Cl1 Na1 2.900(2) 1_565 ?
O4 Na1 2.442(3) . ?
O3 Na1 2.431(3) . ?
P1 O6 1.471(3) . ?
P1 O5 1.498(3) . ?
P1 O8 1.602(3) . ?
P1 O7 1.619(3) . ?
O6 Na1 2.378(3) . ?
O8 C27 1.395(5) . ?
O7 C21 1.392(5) . ?
C21 C22 1.376(6) . ?
C21 C26 1.377(6) . ?
C22 C23 1.381(6) . ?
C26 C25 1.372(7) . ?
C25 C24 1.377(7) . ?
C24 C23 1.362(7) . ?
C28 C29 1.373(7) . ?
C28 C27 1.379(6) . ?
C30 C29 1.356(9) . ?
C30 C31 1.380(9) . ?
C27 C32 1.367(6) . ?
C31 C32 1.392(7) . ?
Na1 Cl1 2.900(2) 1_545 ?

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
O3 Gd1 O4 77.88(10) . . ?
O3 Gd1 O5 88.94(10) . . ?
O4 Gd1 O5 88.34(10) . . ?
O3 Gd1 N2 139.89(11) . . ?
O4 Gd1 N2 138.80(11) . . ?
O5 Gd1 N2 79.00(10) . . ?
O3 Gd1 N3 72.94(11) . . ?
O4 Gd1 N3 150.32(11) . . ?
O5 Gd1 N3 85.83(11) . . ?
N2 Gd1 N3 68.17(11) . . ?
O3 Gd1 N1 149.44(11) . . ?
O4 Gd1 N1 71.99(11) . . ?
O5 Gd1 N1 85.32(11) . . ?
N2 Gd1 N1 68.04(12) . . ?
N3 Gd1 N1 136.20(12) . . ?
O3 Gd1 Cl1 104.42(8) . . ?
O4 Gd1 Cl1 105.31(8) . . ?
O5 Gd1 Cl1 162.49(7) . . ?
N2 Gd1 Cl1 83.49(8) . . ?
N3 Gd1 Cl1 87.34(9) . . ?
N1 Gd1 Cl1 88.52(9) . . ?
O3 Gd1 Na1 40.60(8) . . ?
O4 Gd1 Na1 40.99(8) . . ?
O5 Gd1 Na1 74.97(7) . . ?
N2 Gd1 Na1 153.98(8) . . ?
N3 Gd1 Na1 109.61(9) . . ?
N1 Gd1 Na1 109.22(9) . . ?
Cl1 Gd1 Na1 122.53(4) . . ?
C18 C13 C14 120.4(4) . . ?
C18 C13 C12 123.1(4) . . ?
C14 C13 C12 116.4(4) . . ?
O2 C17 C16 126.1(4) . . ?
O2 C17 C18 113.6(4) . . ?
C16 C17 C18 120.4(5) . . ?
O3 C18 C13 123.9(4) . . ?
O3 C18 C17 118.4(4) . . ?
C13 C18 C17 117.7(4) . . ?
C14 C15 C16 120.3(5) . . ?
C15 C14 C13 120.5(5) . . ?
C17 C16 C15 120.7(5) . . ?
C2 O1 C19 117.8(4) . . ?
C2 O1 Na1 117.4(2) . . ?
C19 O1 Na1 123.1(3) . . ?
C17 O2 C20 117.6(4) . . ?
C17 O2 Na1 114.6(2) . . ?
C20 O2 Na1 123.9(3) . . ?
C12 N3 C11 116.8(4) . . ?
C12 N3 Gd1 129.4(3) . . ?
C11 N3 Gd1 113.8(3) . . ?
N3 C12 C13 127.8(4) . . ?
N2 C10 C11 109.2(4) . . ?
N3 C11 C10 109.9(4) . . ?
C10 N2 C9 114.9(3) . . ?
C10 N2 Gd1 111.2(2) . . ?
C9 N2 Gd1 109.7(2) . . ?
N2 C9 C8 108.8(4) . . ?
N1 C8 C9 110.0(4) . . ?
C7 N1 C8 116.6(4) . . ?
C7 N1 Gd1 129.6(3) . . ?
C8 N1 Gd1 113.7(3) . . ?
N1 C7 C6 127.7(4) . . ?
O4 C1 C6 123.2(4) . . ?
O4 C1 C2 119.2(4) . . ?
C6 C1 C2 117.6(4) . . ?
C1 C6 C5 119.5(4) . . ?
C1 C6 C7 123.1(4) . . ?
C5 C6 C7 117.3(4) . . ?
C4 C5 C6 121.2(5) . . ?
O1 C2 C3 125.1(4) . . ?
O1 C2 C1 113.7(4) . . ?
C3 C2 C1 121.2(5) . . ?
C5 C4 C3 119.8(5) . . ?
C2 C3 C4 120.6(5) . . ?
Gd1 Cl1 Na1 134.96(6) . 1_565 ?
C1 O4 Gd1 141.9(3) . . ?
C1 O4 Na1 116.1(2) . . ?
Gd1 O4 Na1 101.71(12) . . ?
C18 O3 Gd1 142.2(3) . . ?
C18 O3 Na1 113.4(2) . . ?
Gd1 O3 Na1 102.61(12) . . ?
O6 P1 O5 120.28(16) . . ?
O6 P1 O8 108.60(17) . . ?
O5 P1 O8 108.97(16) . . ?
O6 P1 O7 110.27(16) . . ?
O5 P1 O7 108.41(16) . . ?
O8 P1 O7 98.00(16) . . ?
P1 O6 Na1 129.47(16) . . ?
P1 O5 Gd1 135.96(15) . . ?
C27 O8 P1 122.4(2) . . ?
C21 O7 P1 124.1(2) . . ?
C22 C21 C26 120.8(4) . . ?
C22 C21 O7 123.8(4) . . ?
C26 C21 O7 115.4(4) . . ?
C21 C22 C23 119.3(4) . . ?
C25 C26 C21 119.1(4) . . ?
C26 C25 C24 120.6(5) . . ?
C23 C24 C25 120.0(5) . . ?
C24 C23 C22 120.3(5) . . ?
C29 C28 C27 119.3(5) . . ?
C29 C30 C31 120.5(6) . . ?
C30 C29 C28 120.4(6) . . ?
C32 C27 C28 121.1(5) . . ?
C32 C27 O8 121.5(4) . . ?
C28 C27 O8 117.4(4) . . ?
C30 C31 C32 119.8(6) . . ?
C27 C32 C31 118.8(5) . . ?
O6 Na1 O1 126.13(13) . . ?
O6 Na1 O2 124.04(13) . . ?
O1 Na1 O2 109.33(13) . . ?
O6 Na1 O3 89.29(11) . . ?
O1 Na1 O3 121.97(12) . . ?
O2 Na1 O3 64.97(11) . . ?
O6 Na1 O4 91.15(11) . . ?
O1 Na1 O4 65.04(10) . . ?
O2 Na1 O4 121.08(12) . . ?
O3 Na1 O4 70.83(10) . . ?
O6 Na1 Cl1 88.93(8) . 1_545 ?
O1 Na1 Cl1 86.97(9) . 1_545 ?
O2 Na1 Cl1 86.89(9) . 1_545 ?
O3 Na1 Cl1 144.21(10) . 1_545 ?
O4 Na1 Cl1 144.94(11) . 1_545 ?
O6 Na1 Gd1 78.61(7) . . ?
O1 Na1 Gd1 100.55(9) . . ?
O2 Na1 Gd1 99.79(9) . . ?
O3 Na1 Gd1 36.79(7) . . ?
O4 Na1 Gd1 37.30(7) . . ?
Cl1 Na1 Gd1 167.54(6) 1_545 . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.821
_refine_diff_density_min         -2.064
_refine_diff_density_rms         0.078
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4-TbvaldienPONa
_database_code_depnum_ccdc_archive 'CCDC 1432156'
_audit_update_record             
;
2015-10-20 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H33 Cl N3 Na O8 P Tb'
_chemical_formula_weight         835.94

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'
Na Na 0.0362 0.0249 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.2076(17)
_cell_length_b                   8.4021(7)
_cell_length_c                   36.877(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6880.9(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6972
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      25.97

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.35
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3344
_exptl_absorpt_coefficient_mu    2.245
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.3769
_exptl_absorpt_correction_T_max  0.5071
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41969
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         27.45
_reflns_number_total             7836
_reflns_number_gt                5936
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0257P)²+8.8185P] where P=(Fo²+2Fc²)/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_number_reflns         7836
_refine_ls_number_parameters     426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.0842
_refine_ls_wR_factor_gt          0.0777
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_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
Tb1 Tb 0.518004(9) -0.04421(2) 0.143214(5) 0.03081(7) Uani 1 1 d . . .
C2 C 0.6397(2) 0.2765(5) 0.21155(12) 0.0455(12) Uani 1 1 d . . .
C6 C 0.6793(2) 0.0732(5) 0.17180(13) 0.0446(11) Uani 1 1 d . . .
C4 C 0.7456(3) 0.2206(7) 0.21103(16) 0.0685(16) Uani 1 1 d . . .
H4 H 0.7840 0.2413 0.2199 0.082 Uiso 1 1 calc R . .
C3 C 0.6966(3) 0.3033(6) 0.22438(15) 0.0649(16) Uani 1 1 d . . .
H3 H 0.7024 0.3788 0.2425 0.078 Uiso 1 1 calc R . .
C19 C 0.5931(3) 0.4641(7) 0.25188(15) 0.0774(18) Uani 1 1 d . . .
H19A H 0.6106 0.4117 0.2725 0.116 Uiso 1 1 calc R . .
H19B H 0.5539 0.5036 0.2582 0.116 Uiso 1 1 calc R . .
H19C H 0.6184 0.5513 0.2447 0.116 Uiso 1 1 calc R . .
C5 C 0.7374(2) 0.1076(6) 0.18456(15) 0.0595(14) Uani 1 1 d . . .
H5 H 0.7704 0.0538 0.1751 0.071 Uiso 1 1 calc R . .
O2 O 0.58785(16) 0.3534(4) 0.22249(9) 0.0556(9) Uani 1 1 d . . .
O1 O 0.57373(13) 0.1283(3) 0.17424(8) 0.0414(7) Uani 1 1 d . . .
C1 C 0.6293(2) 0.1556(5) 0.18477(11) 0.0383(10) Uani 1 1 d . . .
C7 C 0.6746(2) -0.0583(6) 0.14596(13) 0.0464(11) Uani 1 1 d . . .
H7 H 0.7108 -0.1008 0.1378 0.056 Uiso 1 1 calc R . .
N1 N 0.62678(17) -0.1217(4) 0.13322(10) 0.0417(9) Uani 1 1 d . . .
C21 C 0.6340(2) 0.1952(5) 0.05013(13) 0.0412(11) Uani 1 1 d . . .
C24 C 0.7006(3) -0.0389(7) 0.0182(2) 0.079(2) Uani 1 1 d . . .
H24 H 0.7231 -0.1194 0.0074 0.094 Uiso 1 1 calc R . .
C23 C 0.7207(3) 0.0279(8) 0.0490(2) 0.0750(18) Uani 1 1 d . . .
H23 H 0.7566 -0.0063 0.0593 0.090 Uiso 1 1 calc R . .
C25 C 0.6477(3) 0.0090(7) 0.00233(16) 0.0737(18) Uani 1 1 d . . .
H25 H 0.6347 -0.0386 -0.0191 0.088 Uiso 1 1 calc R . .
C26 C 0.6136(2) 0.1288(6) 0.01826(14) 0.0567(13) Uani 1 1 d . . .
H26 H 0.5779 0.1633 0.0077 0.068 Uiso 1 1 calc R . .
C22 C 0.6879(2) 0.1471(6) 0.06534(15) 0.0569(14) Uani 1 1 d . . .
H22 H 0.7019 0.1949 0.0865 0.068 Uiso 1 1 calc R . .
O6 O 0.52800(15) 0.4042(3) 0.11387(8) 0.0453(8) Uani 1 1 d . . .
P1 P 0.53720(5) 0.28796(13) 0.08479(3) 0.0335(2) Uani 1 1 d . . .
O5 O 0.52904(13) 0.1147(3) 0.09236(7) 0.0356(7) Uani 1 1 d . . .
O7 O 0.60249(13) 0.3165(3) 0.06769(9) 0.0425(7) Uani 1 1 d . . .
O8 O 0.49767(13) 0.3344(4) 0.04955(8) 0.0418(8) Uani 1 1 d . . .
C8 C 0.6344(2) -0.2584(6) 0.10888(14) 0.0538(13) Uani 1 1 d . . .
H8A H 0.6293 -0.3565 0.1224 0.065 Uiso 1 1 calc R . .
H8B H 0.6747 -0.2576 0.0987 0.065 Uiso 1 1 calc R . .
C9 C 0.5890(2) -0.2501(6) 0.07903(13) 0.0499(12) Uani 1 1 d . . .
H9A H 0.5949 -0.1534 0.0651 0.060 Uiso 1 1 calc R . .
H9B H 0.5940 -0.3403 0.0629 0.060 Uiso 1 1 calc R . .
C11 C 0.4202(2) -0.2480(6) 0.08850(15) 0.0581(14) Uani 1 1 d . . .
H11A H 0.3870 -0.2374 0.0716 0.070 Uiso 1 1 calc R . .
H11B H 0.4171 -0.3513 0.1001 0.070 Uiso 1 1 calc R . .
C10 C 0.4792(2) -0.2360(6) 0.06841(13) 0.0502(12) Uani 1 1 d . . .
H10A H 0.4819 -0.3196 0.0504 0.060 Uiso 1 1 calc R . .
H10B H 0.4818 -0.1341 0.0561 0.060 Uiso 1 1 calc R . .
N3 N 0.41672(17) -0.1211(4) 0.11612(10) 0.0435(9) Uani 1 1 d . . .
C12 C 0.3645(2) -0.0718(6) 0.12413(13) 0.0482(12) Uani 1 1 d . . .
H12 H 0.3327 -0.1202 0.1119 0.058 Uiso 1 1 calc R . .
N2 N 0.52838(17) -0.2516(4) 0.09456(10) 0.0390(9) Uani 1 1 d . . .
H2 H 0.5237 -0.3478 0.1055 0.047 Uiso 1 1 calc R . .
Na1 Na 0.51036(8) 0.3624(2) 0.17673(5) 0.0432(4) Uani 1 1 d . . .
O3 O 0.44896(13) 0.1288(3) 0.16376(8) 0.0389(7) Uani 1 1 d . . .
C18 C 0.3906(2) 0.1464(5) 0.16767(11) 0.0349(10) Uani 1 1 d . . .
C13 C 0.3479(2) 0.0519(5) 0.15020(12) 0.0410(10) Uani 1 1 d . . .
C17 C 0.3690(2) 0.2682(5) 0.19102(12) 0.0425(11) Uani 1 1 d . . .
C16 C 0.3082(2) 0.2899(6) 0.19623(15) 0.0579(14) Uani 1 1 d . . .
H16 H 0.2949 0.3699 0.2117 0.069 Uiso 1 1 calc R . .
C14 C 0.2857(2) 0.0791(6) 0.15570(15) 0.0573(14) Uani 1 1 d . . .
H14 H 0.2576 0.0173 0.1434 0.069 Uiso 1 1 calc R . .
C15 C 0.2665(2) 0.1940(7) 0.17871(16) 0.0661(16) Uani 1 1 d . . .
H15 H 0.2255 0.2086 0.1827 0.079 Uiso 1 1 calc R . .
O4 O 0.41345(15) 0.3574(4) 0.20671(9) 0.0522(9) Uani 1 1 d . . .
C27 C 0.4351(2) 0.3530(5) 0.05019(11) 0.0377(10) Uani 1 1 d . . .
C32 C 0.4110(2) 0.4288(5) 0.02030(12) 0.0484(12) Uani 1 1 d . . .
H32 H 0.4359 0.4620 0.0014 0.058 Uiso 1 1 calc R . .
C28 C 0.3992(2) 0.3034(6) 0.07833(13) 0.0493(12) Uani 1 1 d . . .
H28 H 0.4160 0.2519 0.0983 0.059 Uiso 1 1 calc R . .
C31 C 0.3502(2) 0.4545(7) 0.01872(15) 0.0666(16) Uani 1 1 d . . .
H31 H 0.3335 0.5041 -0.0014 0.080 Uiso 1 1 calc R . .
C29 C 0.3383(2) 0.3309(7) 0.07667(15) 0.0622(15) Uani 1 1 d . . .
H29 H 0.3134 0.2982 0.0956 0.075 Uiso 1 1 calc R . .
Cl1 Cl 0.50924(8) -0.29463(15) 0.18686(4) 0.0705(4) Uani 1 1 d . . .
C30 C 0.3140(3) 0.4071(7) 0.04691(17) 0.0724(18) Uani 1 1 d . . .
H30 H 0.2728 0.4265 0.0459 0.087 Uiso 1 1 calc R . .
C20 C 0.3968(3) 0.4701(7) 0.23408(16) 0.081(2) Uani 1 1 d . . .
H20A H 0.3729 0.5529 0.2234 0.121 Uiso 1 1 calc R . .
H20B H 0.4325 0.5155 0.2445 0.121 Uiso 1 1 calc R . .
H20C H 0.3739 0.4174 0.2526 0.121 Uiso 1 1 calc R . .


_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
Tb1 O1 2.223(3) . ?
Tb1 O3 2.245(3) . ?
Tb1 O5 2.315(3) . ?
Tb1 N2 2.512(3) . ?
Tb1 N1 2.529(4) . ?
Tb1 N3 2.545(4) . ?
Tb1 Cl1 2.6561(12) . ?
Tb1 Na1 3.6374(17) . ?
C2 C3 1.368(7) . ?
C2 O2 1.380(6) . ?
C2 C1 1.436(6) . ?
C6 C1 1.393(6) . ?
C6 C5 1.403(7) . ?
C6 C7 1.462(7) . ?
C4 C5 1.374(8) . ?
C4 C3 1.382(8) . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C19 O2 1.433(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C5 H5 0.9300 . ?
O2 Na1 2.412(4) . ?
O1 C1 1.313(5) . ?
O1 Na1 2.420(3) . ?
C7 N1 1.278(6) . ?
C7 H7 0.9300 . ?
N1 C8 1.467(6) . ?
C21 C26 1.378(7) . ?
C21 C22 1.382(7) . ?
C21 O7 1.396(5) . ?
C24 C23 1.343(9) . ?
C24 C25 1.373(9) . ?
C24 H24 0.9300 . ?
C23 C22 1.376(8) . ?
C23 H23 0.9300 . ?
C25 C26 1.390(7) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C22 H22 0.9300 . ?
O6 P1 1.465(3) . ?
O6 Na1 2.377(3) . ?
P1 O5 1.493(3) . ?
P1 O7 1.599(3) . ?
P1 O8 1.616(3) . ?
O8 C27 1.398(5) . ?
C8 C9 1.495(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.463(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 N3 1.477(6) . ?
C11 C10 1.509(7) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C10 N2 1.463(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
N3 C12 1.267(6) . ?
C12 C13 1.463(7) . ?
C12 H12 0.9300 . ?
N2 H2 0.9100 . ?
Na1 O4 2.420(4) . ?
Na1 O3 2.437(3) . ?
Na1 Cl1 2.906(2) 1_565 ?
O3 C18 1.312(5) . ?
C18 C13 1.394(6) . ?
C18 C17 1.421(6) . ?
C13 C14 1.416(7) . ?
C17 O4 1.367(6) . ?
C17 C16 1.377(6) . ?
C16 C15 1.387(8) . ?
C16 H16 0.9300 . ?
C14 C15 1.355(7) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
O4 C20 1.432(5) . ?
C27 C28 1.373(6) . ?
C27 C32 1.381(6) . ?
C32 C31 1.368(7) . ?
C32 H32 0.9300 . ?
C28 C29 1.375(7) . ?
C28 H28 0.9300 . ?
C31 C30 1.373(8) . ?
C31 H31 0.9300 . ?
C29 C30 1.380(7) . ?
C29 H29 0.9300 . ?
Cl1 Na1 2.905(2) 1_545 ?
C30 H30 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?

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
O1 Tb1 O3 77.53(11) . . ?
O1 Tb1 O5 88.95(10) . . ?
O3 Tb1 O5 88.40(10) . . ?
O1 Tb1 N2 140.26(11) . . ?
O3 Tb1 N2 138.86(11) . . ?
O5 Tb1 N2 79.15(10) . . ?
O1 Tb1 N1 73.22(11) . . ?
O3 Tb1 N1 150.28(11) . . ?
O5 Tb1 N1 85.95(11) . . ?
N2 Tb1 N1 68.26(12) . . ?
O1 Tb1 N3 149.28(12) . . ?
O3 Tb1 N3 72.13(11) . . ?
O5 Tb1 N3 85.52(11) . . ?
N2 Tb1 N3 67.95(12) . . ?
N1 Tb1 N3 136.20(12) . . ?
O1 Tb1 Cl1 104.22(9) . . ?
O3 Tb1 Cl1 104.98(8) . . ?
O5 Tb1 Cl1 162.84(7) . . ?
N2 Tb1 Cl1 83.69(9) . . ?
N1 Tb1 Cl1 87.38(9) . . ?
N3 Tb1 Cl1 88.40(9) . . ?
O1 Tb1 Na1 40.40(8) . . ?
O3 Tb1 Na1 40.98(8) . . ?
O5 Tb1 Na1 74.83(7) . . ?
N2 Tb1 Na1 153.98(8) . . ?
N1 Tb1 Na1 109.63(9) . . ?
N3 Tb1 Na1 109.30(9) . . ?
Cl1 Tb1 Na1 122.33(4) . . ?
C3 C2 O2 126.3(5) . . ?
C3 C2 C1 120.2(5) . . ?
O2 C2 C1 113.5(4) . . ?
C1 C6 C5 121.0(5) . . ?
C1 C6 C7 122.8(4) . . ?
C5 C6 C7 116.1(5) . . ?
C5 C4 C3 119.7(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C2 C3 C4 121.4(5) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
O2 C19 H19A 109.5 . . ?
O2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C4 C5 C6 120.2(5) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C2 O2 C19 117.2(4) . . ?
C2 O2 Na1 113.9(3) . . ?
C19 O2 Na1 124.5(3) . . ?
C1 O1 Tb1 142.1(3) . . ?
C1 O1 Na1 113.2(3) . . ?
Tb1 O1 Na1 103.06(12) . . ?
O1 C1 C6 124.1(4) . . ?
O1 C1 C2 118.5(4) . . ?
C6 C1 C2 117.4(4) . . ?
N1 C7 C6 127.9(4) . . ?
N1 C7 H7 116.1 . . ?
C6 C7 H7 116.1 . . ?
C7 N1 C8 117.1(4) . . ?
C7 N1 Tb1 129.3(3) . . ?
C8 N1 Tb1 113.7(3) . . ?
C26 C21 C22 120.9(5) . . ?
C26 C21 O7 121.7(4) . . ?
C22 C21 O7 117.4(4) . . ?
C23 C24 C25 121.4(6) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 H24 119.3 . . ?
C24 C23 C22 120.0(6) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C24 C25 C26 119.9(6) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 118.3(5) . . ?
C21 C26 H26 120.9 . . ?
C25 C26 H26 120.9 . . ?
C23 C22 C21 119.5(6) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
P1 O6 Na1 129.66(17) . . ?
O6 P1 O5 119.76(17) . . ?
O6 P1 O7 108.37(18) . . ?
O5 P1 O7 109.26(16) . . ?
O6 P1 O8 110.61(17) . . ?
O5 P1 O8 108.65(17) . . ?
O7 P1 O8 98.00(16) . . ?
P1 O5 Tb1 136.60(16) . . ?
C21 O7 P1 121.9(3) . . ?
C27 O8 P1 123.6(3) . . ?
N1 C8 C9 109.6(4) . . ?
N1 C8 H8A 109.7 . . ?
C9 C8 H8A 109.7 . . ?
N1 C8 H8B 109.7 . . ?
C9 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
N2 C9 C8 109.4(4) . . ?
N2 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
N2 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
N3 C11 C10 109.6(4) . . ?
N3 C11 H11A 109.8 . . ?
C10 C11 H11A 109.8 . . ?
N3 C11 H11B 109.8 . . ?
C10 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
N2 C10 C11 108.6(4) . . ?
N2 C10 H10A 110.0 . . ?
C11 C10 H10A 110.0 . . ?
N2 C10 H10B 110.0 . . ?
C11 C10 H10B 110.0 . . ?
H10A C10 H10B 108.3 . . ?
C12 N3 C11 116.4(4) . . ?
C12 N3 Tb1 129.4(3) . . ?
C11 N3 Tb1 114.1(3) . . ?
N3 C12 C13 128.0(4) . . ?
N3 C12 H12 116.0 . . ?
C13 C12 H12 116.0 . . ?
C9 N2 C10 115.3(4) . . ?
C9 N2 Tb1 111.0(3) . . ?
C10 N2 Tb1 109.9(3) . . ?
C9 N2 H2 106.7 . . ?
C10 N2 H2 106.7 . . ?
Tb1 N2 H2 106.7 . . ?
O6 Na1 O2 124.71(14) . . ?
O6 Na1 O4 126.49(14) . . ?
O2 Na1 O4 108.33(14) . . ?
O6 Na1 O1 89.27(11) . . ?
O2 Na1 O1 65.55(11) . . ?
O4 Na1 O1 121.35(13) . . ?
O6 Na1 O3 91.13(11) . . ?
O2 Na1 O3 120.74(13) . . ?
O4 Na1 O3 65.04(11) . . ?
O1 Na1 O3 70.32(11) . . ?
O6 Na1 Cl1 88.87(9) . 1_565 ?
O2 Na1 Cl1 86.98(10) . 1_565 ?
O4 Na1 Cl1 87.20(10) . 1_565 ?
O1 Na1 Cl1 144.66(11) . 1_565 ?
O3 Na1 Cl1 144.99(11) . 1_565 ?
O6 Na1 Tb1 78.44(8) . . ?
O2 Na1 Tb1 100.07(9) . . ?
O4 Na1 Tb1 100.39(9) . . ?
O1 Na1 Tb1 36.54(7) . . ?
O3 Na1 Tb1 37.15(7) . . ?
Cl1 Na1 Tb1 167.31(6) 1_565 . ?
C18 O3 Tb1 141.7(3) . . ?
C18 O3 Na1 116.1(3) . . ?
Tb1 O3 Na1 101.87(12) . . ?
O3 C18 C13 123.8(4) . . ?
O3 C18 C17 118.8(4) . . ?
C13 C18 C17 117.4(4) . . ?
C18 C13 C14 120.4(4) . . ?
C18 C13 C12 122.5(4) . . ?
C14 C13 C12 117.0(4) . . ?
O4 C17 C16 125.2(4) . . ?
O4 C17 C18 114.1(4) . . ?
C16 C17 C18 120.7(5) . . ?
C17 C16 C15 120.9(5) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C15 C14 C13 120.8(5) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 119.7(5) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C17 O4 C20 118.3(4) . . ?
C17 O4 Na1 117.2(3) . . ?
C20 O4 Na1 122.7(3) . . ?
C28 C27 C32 121.2(4) . . ?
C28 C27 O8 123.7(4) . . ?
C32 C27 O8 115.0(4) . . ?
C31 C32 C27 119.3(5) . . ?
C31 C32 H32 120.4 . . ?
C27 C32 H32 120.4 . . ?
C27 C28 C29 119.1(5) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C32 C31 C30 120.0(5) . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C28 C29 C30 119.8(5) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
Tb1 Cl1 Na1 134.99(6) . 1_545 ?
C31 C30 C29 120.5(5) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.045
_refine_diff_density_min         -1.489
_refine_diff_density_rms         0.088
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5-HovaldienPONa
_database_code_depnum_ccdc_archive 'CCDC 1432157'
_audit_update_record             
;
2015-10-20 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H33 Cl Ho N3 Na O8 P'
_chemical_formula_weight         841.95

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'
Na Na 0.0362 0.0249 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pbca '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   22.220(4)
_cell_length_b                   8.3683(16)
_cell_length_c                   36.890(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6859(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5221
_cell_measurement_theta_min      2.66
_cell_measurement_theta_max      24.01

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3360
_exptl_absorpt_coefficient_mu    2.497
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.4275
_exptl_absorpt_correction_T_max  0.7883
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42754
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         1.43
_diffrn_reflns_theta_max         27.47
_reflns_number_total             7821
_reflns_number_gt                5183
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0554P)²+0.0000P] where P=(Fo²+2Fc²)/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_number_reflns         7821
_refine_ls_number_parameters     426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_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
Ho1 Ho 0.518042(10) 1.04282(2) 0.142432(6) 0.03100(9) Uani 1 1 d . . .
Na1 Na 0.50970(9) 0.6359(2) 0.17608(6) 0.0428(5) Uani 1 1 d . . .
C11 C 0.6340(3) 1.2588(7) 0.10923(17) 0.0554(16) Uani 1 1 d . . .
H11A H 0.6745 1.2585 0.0994 0.066 Uiso 1 1 calc R . .
H11B H 0.6283 1.3573 0.1227 0.066 Uiso 1 1 calc R . .
C10 C 0.5894(3) 1.2500(7) 0.07908(15) 0.0500(15) Uani 1 1 d . . .
H10A H 0.5941 1.3413 0.0631 0.060 Uiso 1 1 calc R . .
H10B H 0.5958 1.1536 0.0650 0.060 Uiso 1 1 calc R . .
C9 C 0.4796(2) 1.2348(7) 0.06794(16) 0.0512(15) Uani 1 1 d . . .
H9A H 0.4819 1.1325 0.0556 0.061 Uiso 1 1 calc R . .
H9B H 0.4828 1.3190 0.0500 0.061 Uiso 1 1 calc R . .
C8 C 0.4207(3) 1.2488(7) 0.08830(18) 0.0583(17) Uani 1 1 d . . .
H8A H 0.4181 1.3525 0.1000 0.070 Uiso 1 1 calc R . .
H8B H 0.3872 1.2390 0.0715 0.070 Uiso 1 1 calc R . .
C7 C 0.3648(3) 1.0735(7) 0.12443(17) 0.0481(14) Uani 1 1 d . . .
H7 H 0.3331 1.1244 0.1127 0.058 Uiso 1 1 calc R . .
C6 C 0.3481(2) 0.9507(6) 0.15004(15) 0.0423(13) Uani 1 1 d . . .
C5 C 0.2866(3) 0.9241(7) 0.15568(19) 0.0578(17) Uani 1 1 d . . .
H5 H 0.2583 0.9857 0.1434 0.069 Uiso 1 1 calc R . .
C4 C 0.2679(3) 0.8076(8) 0.1792(2) 0.069(2) Uani 1 1 d . . .
H4 H 0.2270 0.7935 0.1835 0.083 Uiso 1 1 calc R . .
C3 C 0.3087(3) 0.7118(7) 0.19658(17) 0.0565(16) Uani 1 1 d . . .
H3 H 0.2953 0.6320 0.2121 0.068 Uiso 1 1 calc R . .
C2 C 0.3697(3) 0.7324(6) 0.19119(15) 0.0428(13) Uani 1 1 d . . .
C1 C 0.3912(2) 0.8557(6) 0.16759(14) 0.0360(12) Uani 1 1 d . . .
C19 C 0.3974(3) 0.5303(8) 0.2342(2) 0.082(2) Uani 1 1 d . . .
H19A H 0.3774 0.5856 0.2535 0.123 Uiso 1 1 calc R . .
H19B H 0.4327 0.4781 0.2434 0.123 Uiso 1 1 calc R . .
H19C H 0.3707 0.4520 0.2240 0.123 Uiso 1 1 calc R . .
C12 C 0.6732(3) 1.0597(7) 0.14647(15) 0.0482(14) Uani 1 1 d . . .
H12 H 0.7095 1.1033 0.1387 0.058 Uiso 1 1 calc R . .
C13 C 0.6775(3) 0.9279(6) 0.17221(16) 0.0451(14) Uani 1 1 d . . .
C14 C 0.7357(3) 0.8911(8) 0.18556(19) 0.0635(18) Uani 1 1 d . . .
H14 H 0.7689 0.9447 0.1762 0.076 Uiso 1 1 calc R . .
C15 C 0.7440(3) 0.7784(8) 0.2120(2) 0.0676(19) Uani 1 1 d . . .
H15 H 0.7823 0.7576 0.2210 0.081 Uiso 1 1 calc R . .
C16 C 0.6947(3) 0.6961(8) 0.22483(17) 0.0631(18) Uani 1 1 d . . .
H16 H 0.7001 0.6196 0.2428 0.076 Uiso 1 1 calc R . .
C17 C 0.6380(3) 0.7243(6) 0.21177(15) 0.0439(13) Uani 1 1 d . . .
C18 C 0.6274(3) 0.8444(6) 0.18476(14) 0.0394(12) Uani 1 1 d . . .
C20 C 0.5912(4) 0.5325(8) 0.25192(18) 0.075(2) Uani 1 1 d . . .
H20A H 0.6162 0.4448 0.2446 0.113 Uiso 1 1 calc R . .
H20B H 0.5519 0.4934 0.2581 0.113 Uiso 1 1 calc R . .
H20C H 0.6087 0.5840 0.2726 0.113 Uiso 1 1 calc R . .
C21 C 0.4351(2) 0.6473(6) 0.04995(14) 0.0388(12) Uani 1 1 d . . .
C26 C 0.4109(3) 0.5719(6) 0.02054(15) 0.0494(15) Uani 1 1 d . . .
H26 H 0.4354 0.5381 0.0016 0.059 Uiso 1 1 calc R . .
C25 C 0.3498(3) 0.5466(8) 0.01936(19) 0.0664(19) Uani 1 1 d . . .
H25 H 0.3328 0.4976 -0.0008 0.080 Uiso 1 1 calc R . .
C24 C 0.3138(3) 0.5928(8) 0.0475(2) 0.074(2) Uani 1 1 d . . .
H24 H 0.2727 0.5718 0.0469 0.089 Uiso 1 1 calc R . .
C23 C 0.3382(3) 0.6693(7) 0.07639(18) 0.0608(17) Uani 1 1 d . . .
H23 H 0.3133 0.7037 0.0951 0.073 Uiso 1 1 calc R . .
C22 C 0.3990(3) 0.6969(7) 0.07854(16) 0.0493(14) Uani 1 1 d . . .
H22 H 0.4156 0.7475 0.0986 0.059 Uiso 1 1 calc R . .
C27 C 0.6345(2) 0.8054(6) 0.04999(15) 0.0427(13) Uani 1 1 d . . .
C28 C 0.6873(3) 0.8538(7) 0.06575(18) 0.0546(16) Uani 1 1 d . . .
H28 H 0.7004 0.8079 0.0873 0.066 Uiso 1 1 calc R . .
C29 C 0.7208(3) 0.9719(8) 0.0491(2) 0.075(2) Uani 1 1 d . . .
H29 H 0.7571 1.0042 0.0593 0.090 Uiso 1 1 calc R . .
C30 C 0.7009(3) 1.0422(8) 0.0175(2) 0.073(2) Uani 1 1 d . . .
H30 H 0.7228 1.1241 0.0067 0.088 Uiso 1 1 calc R . .
C31 C 0.6485(3) 0.9903(8) 0.00218(18) 0.070(2) Uani 1 1 d . . .
H31 H 0.6355 1.0360 -0.0194 0.084 Uiso 1 1 calc R . .
C32 C 0.6144(3) 0.8705(8) 0.01821(17) 0.0589(16) Uani 1 1 d . . .
H32 H 0.5787 0.8356 0.0076 0.071 Uiso 1 1 calc R . .
Cl2 Cl 0.50839(9) 1.29042(18) 0.18569(4) 0.0689(5) Uani 1 1 d . . .
N3 N 0.6259(2) 1.1218(5) 0.13341(12) 0.0436(11) Uani 1 1 d . . .
N2 N 0.52852(19) 1.2491(5) 0.09493(12) 0.0399(10) Uani 1 1 d . . .
H2 H 0.5235 1.3452 0.1061 0.048 Uiso 1 1 calc R . .
N1 N 0.4173(2) 1.1211(5) 0.11582(12) 0.0425(11) Uani 1 1 d . . .
O1 O 0.44957(16) 0.8725(4) 0.16356(9) 0.0396(8) Uani 1 1 d . . .
O2 O 0.41439(18) 0.6426(4) 0.20661(11) 0.0541(10) Uani 1 1 d . . .
O3 O 0.57243(15) 0.8724(4) 0.17402(9) 0.0419(9) Uani 1 1 d . . .
O4 O 0.58631(19) 0.6463(4) 0.22241(10) 0.0550(11) Uani 1 1 d . . .
O7 O 0.49788(15) 0.6677(4) 0.04923(9) 0.0419(9) Uani 1 1 d . . .
O8 O 0.60282(16) 0.6837(4) 0.06751(10) 0.0444(9) Uani 1 1 d . . .
O5 O 0.52934(15) 0.8850(4) 0.09283(9) 0.0360(8) Uani 1 1 d . . .
O6 O 0.52779(17) 0.5941(4) 0.11349(10) 0.0443(9) Uani 1 1 d . . .
P1 P 0.53748(6) 0.71170(15) 0.08476(4) 0.0354(3) Uani 1 1 d . . .


_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
Ho1 O3 2.203(3) . ?
Ho1 O1 2.226(3) . ?
Ho1 O5 2.271(3) . ?
Ho1 N2 2.471(4) . ?
Ho1 N3 2.509(4) . ?
Ho1 N1 2.530(4) . ?
Ho1 Cl2 2.6241(15) . ?
Ho1 Na1 3.629(2) . ?
Na1 O6 2.369(4) . ?
Na1 O2 2.399(4) . ?
Na1 O4 2.414(4) . ?
Na1 O3 2.422(4) . ?
Na1 O1 2.433(4) . ?
Na1 Cl2 2.913(3) 1_545 ?
C11 N3 1.464(7) . ?
C11 C10 1.491(8) . ?
C10 N2 1.474(7) . ?
C9 N2 1.480(7) . ?
C9 C8 1.514(8) . ?
C8 N1 1.476(7) . ?
C7 N1 1.274(7) . ?
C7 C6 1.444(8) . ?
C6 C5 1.400(8) . ?
C6 C1 1.404(7) . ?
C5 C4 1.370(9) . ?
C4 C3 1.370(9) . ?
C3 C2 1.379(7) . ?
C2 O2 1.370(6) . ?
C2 C1 1.432(7) . ?
C1 O1 1.313(6) . ?
C19 O2 1.436(6) . ?
C12 N3 1.268(7) . ?
C12 C13 1.458(8) . ?
C13 C18 1.395(8) . ?
C13 C14 1.417(8) . ?
C14 C15 1.368(9) . ?
C15 C16 1.379(9) . ?
C16 C17 1.371(8) . ?
C17 O4 1.378(7) . ?
C17 C18 1.434(7) . ?
C18 O3 1.304(6) . ?
C20 O4 1.450(6) . ?
C21 C26 1.365(7) . ?
C21 C22 1.389(7) . ?
C21 O7 1.406(6) . ?
C26 C25 1.374(9) . ?
C25 C24 1.367(9) . ?
C24 C23 1.355(8) . ?
C23 C22 1.372(8) . ?
C27 C32 1.368(8) . ?
C27 C28 1.371(8) . ?
C27 O8 1.397(6) . ?
C28 C29 1.381(9) . ?
C29 C30 1.379(10) . ?
C30 C31 1.363(10) . ?
C31 C32 1.390(9) . ?
Cl2 Na1 2.913(3) 1_565 ?
O7 P1 1.621(4) . ?
O8 P1 1.602(4) . ?
O5 P1 1.491(3) . ?
O6 P1 1.462(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
O3 Ho1 O1 77.01(13) . . ?
O3 Ho1 O5 89.38(12) . . ?
O1 Ho1 O5 89.16(12) . . ?
O3 Ho1 N2 140.88(13) . . ?
O1 Ho1 N2 139.48(13) . . ?
O5 Ho1 N2 79.88(13) . . ?
O3 Ho1 N3 73.53(14) . . ?
O1 Ho1 N3 150.27(14) . . ?
O5 Ho1 N3 86.60(14) . . ?
N2 Ho1 N3 68.40(14) . . ?
O3 Ho1 N1 149.12(14) . . ?
O1 Ho1 N1 72.37(13) . . ?
O5 Ho1 N1 86.32(13) . . ?
N2 Ho1 N1 68.11(14) . . ?
N3 Ho1 N1 136.50(15) . . ?
O3 Ho1 Cl2 103.55(10) . . ?
O1 Ho1 Cl2 103.70(10) . . ?
O5 Ho1 Cl2 163.42(9) . . ?
N2 Ho1 Cl2 83.54(11) . . ?
N3 Ho1 Cl2 87.17(11) . . ?
N1 Ho1 Cl2 87.66(11) . . ?
O3 Ho1 Na1 40.51(10) . . ?
O1 Ho1 Na1 40.93(9) . . ?
O5 Ho1 Na1 74.66(9) . . ?
N2 Ho1 Na1 154.54(11) . . ?
N3 Ho1 Na1 109.96(11) . . ?
N1 Ho1 Na1 109.31(10) . . ?
Cl2 Ho1 Na1 121.92(5) . . ?
O6 Na1 O2 127.63(16) . . ?
O6 Na1 O4 125.15(16) . . ?
O2 Na1 O4 106.81(16) . . ?
O6 Na1 O3 89.56(13) . . ?
O2 Na1 O3 120.22(15) . . ?
O4 Na1 O3 65.61(13) . . ?
O6 Na1 O1 91.62(14) . . ?
O2 Na1 O1 65.49(13) . . ?
O4 Na1 O1 119.49(15) . . ?
O3 Na1 O1 69.20(13) . . ?
O6 Na1 Cl2 88.51(11) . 1_545 ?
O2 Na1 Cl2 87.56(11) . 1_545 ?
O4 Na1 Cl2 87.51(11) . 1_545 ?
O3 Na1 Cl2 145.16(12) . 1_545 ?
O1 Na1 Cl2 145.63(12) . 1_545 ?
O6 Na1 Ho1 78.25(9) . . ?
O2 Na1 Ho1 100.57(11) . . ?
O4 Na1 Ho1 99.92(11) . . ?
O3 Na1 Ho1 36.20(8) . . ?
O1 Na1 Ho1 36.82(8) . . ?
Cl2 Na1 Ho1 166.76(8) 1_545 . ?
N3 C11 C10 109.6(5) . . ?
N2 C10 C11 108.3(5) . . ?
N2 C9 C8 107.2(5) . . ?
N1 C8 C9 109.2(4) . . ?
N1 C7 C6 128.5(5) . . ?
C5 C6 C1 120.5(5) . . ?
C5 C6 C7 117.5(5) . . ?
C1 C6 C7 121.9(5) . . ?
C4 C5 C6 120.2(6) . . ?
C3 C4 C5 120.8(6) . . ?
C4 C3 C2 120.6(6) . . ?
O2 C2 C3 125.7(5) . . ?
O2 C2 C1 113.9(5) . . ?
C3 C2 C1 120.4(6) . . ?
O1 C1 C6 124.2(5) . . ?
O1 C1 C2 118.4(5) . . ?
C6 C1 C2 117.4(5) . . ?
N3 C12 C13 127.7(5) . . ?
C18 C13 C14 120.3(5) . . ?
C18 C13 C12 122.9(5) . . ?
C14 C13 C12 116.8(6) . . ?
C15 C14 C13 121.3(6) . . ?
C14 C15 C16 118.8(6) . . ?
C17 C16 C15 121.6(6) . . ?
C16 C17 O4 125.8(5) . . ?
C16 C17 C18 121.1(6) . . ?
O4 C17 C18 113.2(5) . . ?
O3 C18 C13 123.8(5) . . ?
O3 C18 C17 119.4(5) . . ?
C13 C18 C17 116.8(5) . . ?
C26 C21 C22 120.9(5) . . ?
C26 C21 O7 115.6(5) . . ?
C22 C21 O7 123.5(5) . . ?
C21 C26 C25 119.1(6) . . ?
C24 C25 C26 120.6(6) . . ?
C23 C24 C25 119.8(6) . . ?
C24 C23 C22 121.2(6) . . ?
C23 C22 C21 118.3(5) . . ?
C32 C27 C28 121.7(6) . . ?
C32 C27 O8 121.5(5) . . ?
C28 C27 O8 116.8(5) . . ?
C27 C28 C29 118.9(7) . . ?
C30 C29 C28 120.6(7) . . ?
C31 C30 C29 119.2(7) . . ?
C30 C31 C32 121.3(7) . . ?
C27 C32 C31 118.3(6) . . ?
Ho1 Cl2 Na1 135.14(7) . 1_565 ?
C12 N3 C11 116.9(5) . . ?
C12 N3 Ho1 129.3(4) . . ?
C11 N3 Ho1 113.8(3) . . ?
C10 N2 C9 114.1(4) . . ?
C10 N2 Ho1 111.8(3) . . ?
C9 N2 Ho1 110.6(3) . . ?
C7 N1 C8 116.3(5) . . ?
C7 N1 Ho1 129.3(4) . . ?
C8 N1 Ho1 114.2(3) . . ?
C1 O1 Ho1 141.6(3) . . ?
C1 O1 Na1 115.7(3) . . ?
Ho1 O1 Na1 102.26(14) . . ?
C2 O2 C19 117.5(5) . . ?
C2 O2 Na1 117.3(3) . . ?
C19 O2 Na1 123.3(4) . . ?
C18 O3 Ho1 142.2(3) . . ?
C18 O3 Na1 112.4(3) . . ?
Ho1 O3 Na1 103.29(14) . . ?
C17 O4 C20 117.6(5) . . ?
C17 O4 Na1 113.7(3) . . ?
C20 O4 Na1 124.1(4) . . ?
C21 O7 P1 123.4(3) . . ?
C27 O8 P1 122.3(3) . . ?
P1 O5 Ho1 137.7(2) . . ?
P1 O6 Na1 129.2(2) . . ?
O6 P1 O5 119.4(2) . . ?
O6 P1 O8 108.8(2) . . ?
O5 P1 O8 109.35(19) . . ?
O6 P1 O7 110.7(2) . . ?
O5 P1 O7 108.5(2) . . ?
O8 P1 O7 97.9(2) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.121
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6-HovaldienPOH
_database_code_depnum_ccdc_archive 'CCDC 1432220'
_audit_update_record             
;
2015-10-20 deposited with the CCDC.
2015-11-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H33 Ho N3 O8 P'
_chemical_formula_weight         783.51

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'
Ho Ho -0.2175 4.6783 '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           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.990(2)
_cell_length_b                   11.579(2)
_cell_length_c                   27.216(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.817(6)
_cell_angle_gamma                90.00
_cell_volume                     3168.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6050
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      26.56

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_absorpt_coefficient_mu    2.603
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5739
_exptl_absorpt_correction_T_max  0.7120
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17969
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         26.00
_reflns_number_total             6206
_reflns_number_gt                5115
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0249P)²+7.0642P] where P=(Fo²+2Fc²)/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_number_reflns         6206
_refine_ls_number_parameters     408
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0798
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.087
_refine_ls_shift/su_max          0.006
_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
Ho1 Ho 0.425388(11) 0.444818(10) 0.750111(5) 0.02755(3) Uani 1 1 d . . .
C1 C 0.5012(3) 0.5209(2) 0.64883(11) 0.0384(8) Uani 1 1 d . . .
C2 C 0.4416(3) 0.5629(3) 0.59600(11) 0.0450(8) Uani 1 1 d . . .
C3 C 0.5095(3) 0.5647(3) 0.56350(13) 0.0591(10) Uani 1 1 d . . .
H3 H 0.4691 0.5958 0.5292 0.071 Uiso 1 1 calc R . .
C4 C 0.6366(3) 0.5213(4) 0.58073(14) 0.0669(11) Uani 1 1 d . . .
H4 H 0.6811 0.5222 0.5580 0.080 Uiso 1 1 calc R . .
C5 C 0.6965(3) 0.4772(3) 0.63102(13) 0.0588(10) Uani 1 1 d . . .
H5 H 0.7829 0.4489 0.6430 0.071 Uiso 1 1 calc R . .
C6 C 0.6289(3) 0.4742(3) 0.66515(12) 0.0444(8) Uani 1 1 d . . .
C7 C 0.6949(3) 0.4154(3) 0.71582(12) 0.0447(9) Uani 1 1 d . . .
H7 H 0.7832 0.3949 0.7250 0.054 Uiso 1 1 calc R . .
C8 C 0.7302(3) 0.3141(3) 0.79405(13) 0.0521(10) Uani 1 1 d . . .
H8A H 0.7108 0.2337 0.7838 0.063 Uiso 1 1 calc R . .
H8B H 0.8231 0.3279 0.8015 0.063 Uiso 1 1 calc R . .
C9 C 0.7074(3) 0.3367(3) 0.84280(13) 0.0534(10) Uani 1 1 d . . .
H9A H 0.7569 0.2813 0.8704 0.064 Uiso 1 1 calc R . .
H9B H 0.7392 0.4134 0.8562 0.064 Uiso 1 1 calc R . .
C10 C 0.5371(3) 0.3569(3) 0.87714(11) 0.0479(9) Uani 1 1 d . . .
H10A H 0.5628 0.4362 0.8880 0.057 Uiso 1 1 calc R . .
H10B H 0.5865 0.3069 0.9072 0.057 Uiso 1 1 calc R . .
C11 C 0.3912(3) 0.3423(3) 0.86180(13) 0.0546(10) Uani 1 1 d . . .
H11A H 0.3663 0.2622 0.8527 0.065 Uiso 1 1 calc R . .
H11B H 0.3692 0.3634 0.8917 0.065 Uiso 1 1 calc R . .
C12 C 0.2156(3) 0.4669(3) 0.81603(12) 0.0458(9) Uani 1 1 d . . .
H12 H 0.1987 0.4550 0.8465 0.055 Uiso 1 1 calc R . .
C13 C 0.1240(3) 0.5391(3) 0.77578(13) 0.0459(9) Uani 1 1 d . . .
C14 C 0.0235(3) 0.5925(4) 0.78724(16) 0.0698(12) Uani 1 1 d . . .
H14 H 0.0205 0.5807 0.8205 0.084 Uiso 1 1 calc R . .
C15 C -0.0692(4) 0.6610(4) 0.75067(17) 0.0832(14) Uani 1 1 d . . .
H15 H -0.1333 0.6976 0.7593 0.100 Uiso 1 1 calc R . .
C16 C -0.0681(3) 0.6760(3) 0.70093(17) 0.0647(12) Uani 1 1 d . . .
H16 H -0.1323 0.7224 0.6758 0.078 Uiso 1 1 calc R . .
C17 C 0.0261(3) 0.6235(3) 0.68781(14) 0.0483(10) Uani 1 1 d . . .
C18 C 0.1283(3) 0.5553(2) 0.72579(12) 0.0398(8) Uani 1 1 d . . .
C19 C 0.2149(3) 0.5294(3) 0.57430(16) 0.0662(13) Uani 1 1 d . . .
H19A H 0.2303 0.4560 0.5614 0.099 Uiso 1 1 calc R . .
H19B H 0.1296 0.5586 0.5505 0.099 Uiso 1 1 calc R . .
H19C H 0.2165 0.5201 0.6096 0.099 Uiso 1 1 calc R . .
C20 C -0.0570(4) 0.7085(4) 0.60076(17) 0.0820(16) Uani 1 1 d . . .
H20A H -0.1462 0.6829 0.5924 0.123 Uiso 1 1 calc R . .
H20B H -0.0404 0.7079 0.5687 0.123 Uiso 1 1 calc R . .
H20C H -0.0458 0.7854 0.6150 0.123 Uiso 1 1 calc R . .
C21 C 0.1131(3) 0.1753(3) 0.61078(13) 0.0486(9) Uani 1 1 d U . .
C22 C 0.0322(4) 0.1079(4) 0.56897(16) 0.0766(13) Uani 1 1 d U . .
H22 H 0.0571 0.0327 0.5653 0.092 Uiso 1 1 calc R . .
C23 C -0.0859(4) 0.1520(5) 0.53239(18) 0.0934(15) Uani 1 1 d U . .
H23 H -0.1417 0.1066 0.5041 0.112 Uiso 1 1 calc R . .
C24 C -0.1201(4) 0.2619(4) 0.53797(17) 0.0871(14) Uani 1 1 d U . .
H24 H -0.1985 0.2926 0.5126 0.105 Uiso 1 1 calc R . .
C25 C -0.0411(4) 0.3287(4) 0.58051(16) 0.0745(12) Uani 1 1 d U . .
H25 H -0.0674 0.4034 0.5843 0.089 Uiso 1 1 calc R . .
C26 C 0.0775(3) 0.2852(3) 0.61782(14) 0.0566(10) Uani 1 1 d U . .
H26 H 0.1316 0.3296 0.6469 0.068 Uiso 1 1 calc R . .
C27 C 0.4350(3) 0.2178(3) 0.59624(11) 0.0492(9) Uani 1 1 d U . .
C28 C 0.5657(3) 0.1936(3) 0.61114(14) 0.0594(10) Uani 1 1 d U . .
H28 H 0.6258 0.2016 0.6467 0.071 Uiso 1 1 calc R . .
C29 C 0.6075(4) 0.1569(4) 0.57233(16) 0.0792(12) Uani 1 1 d U . .
H29 H 0.6969 0.1408 0.5814 0.095 Uiso 1 1 calc R . .
C30 C 0.5174(5) 0.1443(5) 0.52067(17) 0.0961(13) Uani 1 1 d U . .
H30 H 0.5457 0.1200 0.4944 0.115 Uiso 1 1 calc R . .
C31 C 0.3863(5) 0.1669(5) 0.50720(17) 0.1050(15) Uani 1 1 d U . .
H31 H 0.3249 0.1557 0.4721 0.126 Uiso 1 1 calc R . .
C32 C 0.3445(4) 0.2064(4) 0.54558(15) 0.0846(13) Uani 1 1 d U . .
H32 H 0.2557 0.2247 0.5366 0.102 Uiso 1 1 calc R . .
N1 N 0.6459(2) 0.3886(2) 0.74918(10) 0.0407(7) Uani 1 1 d . . .
N2 N 0.5674(2) 0.3280(2) 0.83148(9) 0.0418(7) Uani 1 1 d . . .
H2 H 0.5442 0.2527 0.8234 0.050 Uiso 1 1 calc R . .
N3 N 0.3184(2) 0.4163(2) 0.81544(9) 0.0368(6) Uani 1 1 d . . .
O1 O 0.43778(18) 0.52593(17) 0.68016(7) 0.0391(5) Uani 1 1 d . . .
O2 O 0.3150(2) 0.6078(2) 0.57638(8) 0.0550(7) Uani 1 1 d . . .
O3 O 0.22217(17) 0.51330(18) 0.71357(8) 0.0405(6) Uani 1 1 d . . .
O4 O 0.0339(2) 0.6332(2) 0.63937(10) 0.0597(8) Uani 1 1 d . . .
O5 O 0.35709(17) 0.26737(16) 0.71635(7) 0.0363(5) Uani 1 1 d . . .
O6 O 0.46629(18) 0.09141(16) 0.69639(7) 0.0377(5) Uani 1 1 d . . .
O7 O 0.2307(2) 0.12322(17) 0.64527(9) 0.0482(7) Uani 1 1 d . . .
O8 O 0.3931(2) 0.26171(17) 0.63444(7) 0.0438(6) Uani 1 1 d . . .
P1 P 0.36788(7) 0.18602(6) 0.67711(3) 0.03149(18) Uani 1 1 d . . .


_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
Ho1 O1 2.176(2) . ?
Ho1 O3 2.1936(18) . ?
Ho1 O6 2.2401(18) 2_656 ?
Ho1 O5 2.2522(18) . ?
Ho1 N3 2.518(3) . ?
Ho1 N1 2.519(3) . ?
Ho1 N2 2.526(2) . ?
C1 O1 1.303(4) . ?
C1 C6 1.399(4) . ?
C1 C2 1.404(4) . ?
C2 C3 1.369(5) . ?
C2 O2 1.375(4) . ?
C3 C4 1.376(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.356(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.404(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.443(4) . ?
C7 N1 1.267(4) . ?
C7 H7 0.9300 . ?
C8 C9 1.470(5) . ?
C8 N1 1.477(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.445(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.450(4) . ?
C10 C11 1.494(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N3 1.467(4) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N3 1.278(4) . ?
C12 C13 1.422(4) . ?
C12 H12 0.9300 . ?
C13 C18 1.393(5) . ?
C13 C14 1.407(5) . ?
C14 C15 1.356(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.370(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.367(5) . ?
C16 H16 0.9300 . ?
C17 O4 1.360(5) . ?
C17 C18 1.419(4) . ?
C18 O3 1.299(4) . ?
C19 O2 1.410(5) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O4 1.419(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C26 1.367(5) . ?
C21 C22 1.370(5) . ?
C21 O7 1.392(3) . ?
C22 C23 1.376(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.353(7) . ?
C23 H23 0.9300 . ?
C24 C25 1.372(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.384(5) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C32 1.342(4) . ?
C27 C28 1.355(5) . ?
C27 O8 1.392(4) . ?
C28 C29 1.378(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.362(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.361(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.378(7) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
N2 H2 0.9100 . ?
O5 P1 1.464(2) . ?
O6 P1 1.4788(19) . ?
O6 Ho1 2.2402(18) 2_646 ?
O7 P1 1.580(2) . ?
O8 P1 1.566(2) . ?

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
O1 Ho1 O3 81.91(8) . . ?
O1 Ho1 O6 92.12(7) . 2_656 ?
O3 Ho1 O6 101.38(7) . 2_656 ?
O1 Ho1 O5 99.51(7) . . ?
O3 Ho1 O5 91.96(7) . . ?
O6 Ho1 O5 163.44(6) 2_656 . ?
O1 Ho1 N3 152.42(7) . . ?
O3 Ho1 N3 71.78(8) . . ?
O6 Ho1 N3 85.26(8) 2_656 . ?
O5 Ho1 N3 89.71(8) . . ?
O1 Ho1 N1 72.69(8) . . ?
O3 Ho1 N1 153.66(8) . . ?
O6 Ho1 N1 86.63(8) 2_656 . ?
O5 Ho1 N1 85.63(7) . . ?
N3 Ho1 N1 134.31(8) . . ?
O1 Ho1 N2 139.77(8) . . ?
O3 Ho1 N2 138.31(9) . . ?
O6 Ho1 N2 81.83(7) 2_656 . ?
O5 Ho1 N2 81.68(7) . . ?
N3 Ho1 N2 67.06(8) . . ?
N1 Ho1 N2 67.29(9) . . ?
O1 C1 C6 122.9(3) . . ?
O1 C1 C2 120.2(3) . . ?
C6 C1 C2 116.9(3) . . ?
C3 C2 O2 118.3(3) . . ?
C3 C2 C1 121.1(3) . . ?
O2 C2 C1 120.6(3) . . ?
C2 C3 C4 121.2(3) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.4(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 120.7(3) . . ?
C1 C6 C7 122.6(3) . . ?
C5 C6 C7 116.6(3) . . ?
N1 C7 C6 127.2(3) . . ?
N1 C7 H7 116.4 . . ?
C6 C7 H7 116.4 . . ?
C9 C8 N1 111.3(3) . . ?
C9 C8 H8A 109.4 . . ?
N1 C8 H8A 109.4 . . ?
C9 C8 H8B 109.4 . . ?
N1 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
N2 C9 C8 110.5(2) . . ?
N2 C9 H9A 109.5 . . ?
C8 C9 H9A 109.5 . . ?
N2 C9 H9B 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
N2 C10 C11 109.0(2) . . ?
N2 C10 H10A 109.9 . . ?
C11 C10 H10A 109.9 . . ?
N2 C10 H10B 109.9 . . ?
C11 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
N3 C11 C10 109.0(3) . . ?
N3 C11 H11A 109.9 . . ?
C10 C11 H11A 109.9 . . ?
N3 C11 H11B 109.9 . . ?
C10 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
N3 C12 C13 127.9(3) . . ?
N3 C12 H12 116.1 . . ?
C13 C12 H12 116.1 . . ?
C18 C13 C14 119.8(3) . . ?
C18 C13 C12 122.6(3) . . ?
C14 C13 C12 117.6(3) . . ?
C15 C14 C13 121.3(4) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 119.7(4) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 120.8(3) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
O4 C17 C16 124.6(3) . . ?
O4 C17 C18 114.3(3) . . ?
C16 C17 C18 121.2(3) . . ?
O3 C18 C13 122.9(2) . . ?
O3 C18 C17 119.9(3) . . ?
C13 C18 C17 117.2(3) . . ?
O2 C19 H19A 109.5 . . ?
O2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 121.4(3) . . ?
C26 C21 O7 123.3(3) . . ?
C22 C21 O7 115.3(3) . . ?
C21 C22 C23 119.7(4) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 119.5(4) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 121.0(4) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C26 120.1(4) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C21 C26 C25 118.3(3) . . ?
C21 C26 H26 120.9 . . ?
C25 C26 H26 120.9 . . ?
C32 C27 C28 122.9(4) . . ?
C32 C27 O8 118.2(3) . . ?
C28 C27 O8 118.8(3) . . ?
C27 C28 C29 118.4(3) . . ?
C27 C28 H28 120.8 . . ?
C29 C28 H28 120.8 . . ?
C30 C29 C28 119.8(4) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C31 C30 C29 120.4(5) . . ?
C31 C30 H30 119.8 . . ?
C29 C30 H30 119.8 . . ?
C30 C31 C32 120.0(4) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C27 C32 C31 118.4(4) . . ?
C27 C32 H32 120.8 . . ?
C31 C32 H32 120.8 . . ?
C7 N1 C8 115.4(3) . . ?
C7 N1 Ho1 129.27(19) . . ?
C8 N1 Ho1 115.3(2) . . ?
C9 N2 C10 113.2(2) . . ?
C9 N2 Ho1 112.2(2) . . ?
C10 N2 Ho1 110.68(17) . . ?
C9 N2 H2 106.8 . . ?
C10 N2 H2 106.8 . . ?
Ho1 N2 H2 106.8 . . ?
C12 N3 C11 115.8(3) . . ?
C12 N3 Ho1 128.0(2) . . ?
C11 N3 Ho1 115.8(2) . . ?
C1 O1 Ho1 142.45(17) . . ?
C2 O2 C19 115.1(3) . . ?
C18 O3 Ho1 141.94(18) . . ?
C17 O4 C20 117.9(3) . . ?
P1 O5 Ho1 140.59(13) . . ?
P1 O6 Ho1 155.86(14) . 2_646 ?
C21 O7 P1 126.2(2) . . ?
C27 O8 P1 124.08(19) . . ?
O5 P1 O6 118.73(11) . . ?
O5 P1 O8 105.76(11) . . ?
O6 P1 O8 110.76(12) . . ?
O5 P1 O7 110.85(13) . . ?
O6 P1 O7 104.63(11) . . ?
O8 P1 O7 105.43(12) . . ?

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
O1 C1 C2 C3 176.1(3) . . . . ?
C6 C1 C2 C3 -4.2(4) . . . . ?
O1 C1 C2 O2 -1.2(4) . . . . ?
C6 C1 C2 O2 178.5(3) . . . . ?
O2 C2 C3 C4 179.9(3) . . . . ?
C1 C2 C3 C4 2.6(5) . . . . ?
C2 C3 C4 C5 -0.8(6) . . . . ?
C3 C4 C5 C6 0.9(6) . . . . ?
O1 C1 C6 C5 -176.0(3) . . . . ?
C2 C1 C6 C5 4.3(4) . . . . ?
O1 C1 C6 C7 7.4(4) . . . . ?
C2 C1 C6 C7 -172.2(3) . . . . ?
C4 C5 C6 C1 -2.8(5) . . . . ?
C4 C5 C6 C7 173.9(3) . . . . ?
C1 C6 C7 N1 7.0(5) . . . . ?
C5 C6 C7 N1 -169.7(3) . . . . ?
N1 C8 C9 N2 53.3(4) . . . . ?
N2 C10 C11 N3 -58.0(3) . . . . ?
N3 C12 C13 C18 6.7(5) . . . . ?
N3 C12 C13 C14 -175.2(3) . . . . ?
C18 C13 C14 C15 -0.7(5) . . . . ?
C12 C13 C14 C15 -178.8(4) . . . . ?
C13 C14 C15 C16 2.0(6) . . . . ?
C14 C15 C16 C17 -0.6(6) . . . . ?
C15 C16 C17 O4 179.6(3) . . . . ?
C15 C16 C17 C18 -2.3(5) . . . . ?
C14 C13 C18 O3 176.4(3) . . . . ?
C12 C13 C18 O3 -5.5(5) . . . . ?
C14 C13 C18 C17 -2.1(4) . . . . ?
C12 C13 C18 C17 176.0(3) . . . . ?
O4 C17 C18 O3 3.3(4) . . . . ?
C16 C17 C18 O3 -175.0(3) . . . . ?
O4 C17 C18 C13 -178.2(3) . . . . ?
C16 C17 C18 C13 3.5(4) . . . . ?
C26 C21 C22 C23 1.6(7) . . . . ?
O7 C21 C22 C23 -179.4(4) . . . . ?
C21 C22 C23 C24 0.6(8) . . . . ?
C22 C23 C24 C25 -2.2(8) . . . . ?
C23 C24 C25 C26 1.8(8) . . . . ?
C22 C21 C26 C25 -2.0(6) . . . . ?
O7 C21 C26 C25 179.1(4) . . . . ?
C24 C25 C26 C21 0.3(7) . . . . ?
C32 C27 C28 C29 0.7(6) . . . . ?
O8 C27 C28 C29 -176.1(3) . . . . ?
C27 C28 C29 C30 -0.9(6) . . . . ?
C28 C29 C30 C31 -0.5(8) . . . . ?
C29 C30 C31 C32 2.1(9) . . . . ?
C28 C27 C32 C31 0.8(7) . . . . ?
O8 C27 C32 C31 177.7(4) . . . . ?
C30 C31 C32 C27 -2.2(8) . . . . ?
C6 C7 N1 C8 171.6(3) . . . . ?
C6 C7 N1 Ho1 -8.6(5) . . . . ?
C9 C8 N1 C7 149.4(3) . . . . ?
C9 C8 N1 Ho1 -30.5(3) . . . . ?
O1 Ho1 N1 C7 -0.4(2) . . . . ?
O3 Ho1 N1 C7 15.4(4) . . . . ?
O6 Ho1 N1 C7 -93.7(3) 2_656 . . . ?
O5 Ho1 N1 C7 101.0(3) . . . . ?
N3 Ho1 N1 C7 -173.7(2) . . . . ?
N2 Ho1 N1 C7 -176.2(3) . . . . ?
O1 Ho1 N1 C8 179.4(2) . . . . ?
O3 Ho1 N1 C8 -164.78(19) . . . . ?
O6 Ho1 N1 C8 86.1(2) 2_656 . . . ?
O5 Ho1 N1 C8 -79.2(2) . . . . ?
N3 Ho1 N1 C8 6.1(2) . . . . ?
N2 Ho1 N1 C8 3.59(19) . . . . ?
C8 C9 N2 C10 -176.1(3) . . . . ?
C8 C9 N2 Ho1 -50.0(3) . . . . ?
C11 C10 N2 C9 -178.5(3) . . . . ?
C11 C10 N2 Ho1 54.6(3) . . . . ?
O1 Ho1 N2 C9 17.9(3) . . . . ?
O3 Ho1 N2 C9 -163.60(19) . . . . ?
O6 Ho1 N2 C9 -65.6(2) 2_656 . . . ?
O5 Ho1 N2 C9 112.8(2) . . . . ?
N3 Ho1 N2 C9 -153.9(2) . . . . ?
N1 Ho1 N2 C9 24.1(2) . . . . ?
O1 Ho1 N2 C10 145.48(18) . . . . ?
O3 Ho1 N2 C10 -36.1(2) . . . . ?
O6 Ho1 N2 C10 61.90(19) 2_656 . . . ?
O5 Ho1 N2 C10 -119.6(2) . . . . ?
N3 Ho1 N2 C10 -26.39(18) . . . . ?
N1 Ho1 N2 C10 151.7(2) . . . . ?
C13 C12 N3 C11 -177.1(3) . . . . ?
C13 C12 N3 Ho1 10.2(4) . . . . ?
C10 C11 N3 C12 -140.5(3) . . . . ?
C10 C11 N3 Ho1 33.1(3) . . . . ?
O1 Ho1 N3 C12 -0.1(3) . . . . ?
O3 Ho1 N3 C12 -18.3(2) . . . . ?
O6 Ho1 N3 C12 85.4(2) 2_656 . . . ?
O5 Ho1 N3 C12 -110.4(2) . . . . ?
N1 Ho1 N3 C12 166.0(2) . . . . ?
N2 Ho1 N3 C12 168.5(3) . . . . ?
O1 Ho1 N3 C11 -172.81(18) . . . . ?
O3 Ho1 N3 C11 169.1(2) . . . . ?
O6 Ho1 N3 C11 -87.3(2) 2_656 . . . ?
O5 Ho1 N3 C11 76.9(2) . . . . ?
N1 Ho1 N3 C11 -6.7(2) . . . . ?
N2 Ho1 N3 C11 -4.19(19) . . . . ?
C6 C1 O1 Ho1 -24.4(4) . . . . ?
C2 C1 O1 Ho1 155.2(2) . . . . ?
O3 Ho1 O1 C1 -155.0(3) . . . . ?
O6 Ho1 O1 C1 103.8(3) 2_656 . . . ?
O5 Ho1 O1 C1 -64.4(3) . . . . ?
N3 Ho1 O1 C1 -172.4(2) . . . . ?
N1 Ho1 O1 C1 18.0(3) . . . . ?
N2 Ho1 O1 C1 24.0(3) . . . . ?
C3 C2 O2 C19 120.4(3) . . . . ?
C1 C2 O2 C19 -62.2(4) . . . . ?
C13 C18 O3 Ho1 -19.1(5) . . . . ?
C17 C18 O3 Ho1 159.3(2) . . . . ?
O1 Ho1 O3 C18 -146.6(3) . . . . ?
O6 Ho1 O3 C18 -56.1(3) 2_656 . . . ?
O5 Ho1 O3 C18 114.0(3) . . . . ?
N3 Ho1 O3 C18 25.0(3) . . . . ?
N1 Ho1 O3 C18 -161.9(3) . . . . ?
N2 Ho1 O3 C18 34.4(3) . . . . ?
C16 C17 O4 C20 3.9(5) . . . . ?
C18 C17 O4 C20 -174.3(3) . . . . ?
O1 Ho1 O5 P1 30.38(17) . . . . ?
O3 Ho1 O5 P1 112.50(17) . . . . ?
O6 Ho1 O5 P1 -103.6(3) 2_656 . . . ?
N3 Ho1 O5 P1 -175.74(16) . . . . ?
N1 Ho1 O5 P1 -41.23(17) . . . . ?
N2 Ho1 O5 P1 -108.89(17) . . . . ?
C26 C21 O7 P1 -32.8(5) . . . . ?
C22 C21 O7 P1 148.3(3) . . . . ?
C32 C27 O8 P1 102.9(3) . . . . ?
C28 C27 O8 P1 -80.1(4) . . . . ?
Ho1 O5 P1 O6 98.70(18) . . . . ?
Ho1 O5 P1 O8 -26.39(19) . . . . ?
Ho1 O5 P1 O7 -140.17(15) . . . . ?
Ho1 O6 P1 O5 46.5(3) 2_646 . . . ?
Ho1 O6 P1 O8 169.1(2) 2_646 . . . ?
Ho1 O6 P1 O7 -77.8(3) 2_646 . . . ?
C27 O8 P1 O5 166.8(2) . . . . ?
C27 O8 P1 O6 36.9(2) . . . . ?
C27 O8 P1 O7 -75.7(2) . . . . ?
C21 O7 P1 O5 64.5(3) . . . . ?
C21 O7 P1 O6 -166.3(3) . . . . ?
C21 O7 P1 O8 -49.5(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.460
_refine_diff_density_min         -1.869
_refine_diff_density_rms         0.100
