# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  from this site to visualise CIF-encoded structures and 
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data_rpso591_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H20 Cl N2 O2 P'
_chemical_formula_weight         398.81

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0038(4)
_cell_length_b                   10.2770(4)
_cell_length_c                   11.3976(4)
_cell_angle_alpha                111.639(2)
_cell_angle_beta                 114.435(2)
_cell_angle_gamma                95.410(2)
_cell_volume                     948.52(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2587
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      25.77

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             416
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8818
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_process_details   'Bruker, SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8778
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         26.04
_reflns_number_total             3724
_reflns_number_gt                2987
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0411P)²+0.3714P] 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         3724
_refine_ls_number_parameters     247
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.0937
_refine_ls_wR_factor_gt          0.0871
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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
Cl1 Cl 0.66878(7) 1.20283(8) 0.89321(6) 0.0521(2) Uani 1 1 d . . .
P1 P 0.69830(5) 0.26068(5) 0.41707(5) 0.01957(13) Uani 1 1 d . . .
O1 O 0.58868(15) 0.22899(14) 0.46738(14) 0.0248(3) Uani 1 1 d . . .
O2 O 0.88167(16) 1.14863(14) 0.74194(15) 0.0296(3) Uani 1 1 d . . .
N1 N 0.87267(18) 0.61149(16) 0.61300(17) 0.0226(4) Uani 1 1 d . . .
N2 N 0.7289(2) 0.91841(18) 0.6460(2) 0.0286(4) Uani 1 1 d . . .
H2A H 0.640(3) 0.865(2) 0.618(2) 0.034 Uiso 1 1 d . . .
C1 C 0.8948(2) 0.5137(2) 0.6664(2) 0.0217(4) Uani 1 1 d . . .
C2 C 0.9196(2) 0.5452(2) 0.8040(2) 0.0295(5) Uani 1 1 d . . .
H2 H 0.9340 0.4737 0.8386 0.035 Uiso 1 1 calc R . .
C3 C 0.9230(2) 0.6840(2) 0.8905(2) 0.0354(5) Uani 1 1 d . . .
H3 H 0.9438 0.7102 0.9868 0.042 Uiso 1 1 calc R . .
C4 C 0.8958(2) 0.7829(2) 0.8350(2) 0.0318(5) Uani 1 1 d . . .
H4 H 0.8946 0.8773 0.8913 0.038 Uiso 1 1 calc R . .
C5 C 0.8703(2) 0.7427(2) 0.6954(2) 0.0250(4) Uani 1 1 d . . .
C6 C 0.8398(3) 0.8441(2) 0.6250(2) 0.0322(5) Uani 1 1 d . . .
H6A H 0.9376 0.9183 0.6653 0.039 Uiso 1 1 calc R . .
H6B H 0.8015 0.7867 0.5203 0.039 Uiso 1 1 calc R . .
C7 C 0.7594(2) 1.0646(2) 0.7016(2) 0.0232(4) Uani 1 1 d . . .
C8 C 0.6271(2) 1.1198(2) 0.7104(2) 0.0259(4) Uani 1 1 d . . .
H8A H 0.5316 1.0373 0.6521 0.031 Uiso 1 1 calc R . .
H8B H 0.6117 1.1920 0.6713 0.031 Uiso 1 1 calc R . .
C9 C 0.8904(2) 0.36596(19) 0.5659(2) 0.0225(4) Uani 1 1 d . . .
H9A H 0.9290 0.3102 0.6211 0.027 Uiso 1 1 calc R . .
H9B H 0.9595 0.3801 0.5269 0.027 Uiso 1 1 calc R . .
C10 C 0.7245(2) 0.09677(19) 0.3068(2) 0.0220(4) Uani 1 1 d . . .
C11 C 0.6773(2) 0.0511(2) 0.1613(2) 0.0284(5) Uani 1 1 d . . .
H11 H 0.6334 0.1093 0.1164 0.034 Uiso 1 1 calc R . .
C12 C 0.6943(3) -0.0799(2) 0.0811(2) 0.0339(5) Uani 1 1 d . . .
H12 H 0.6625 -0.1106 -0.0183 0.041 Uiso 1 1 calc R . .
C13 C 0.7573(2) -0.1648(2) 0.1458(2) 0.0318(5) Uani 1 1 d . . .
H13 H 0.7681 -0.2544 0.0907 0.038 Uiso 1 1 calc R . .
C14 C 0.8048(2) -0.1202(2) 0.2906(2) 0.0300(5) Uani 1 1 d . . .
H14 H 0.8484 -0.1790 0.3348 0.036 Uiso 1 1 calc R . .
C15 C 0.7889(2) 0.0099(2) 0.3713(2) 0.0256(4) Uani 1 1 d . . .
H15 H 0.8219 0.0403 0.4708 0.031 Uiso 1 1 calc R . .
C16 C 0.6397(2) 0.36381(19) 0.31669(19) 0.0207(4) Uani 1 1 d . . .
C17 C 0.7208(2) 0.3998(2) 0.2533(2) 0.0240(4) Uani 1 1 d . . .
H17 H 0.8048 0.3627 0.2554 0.029 Uiso 1 1 calc R . .
C18 C 0.6792(2) 0.4893(2) 0.1875(2) 0.0292(5) Uani 1 1 d . . .
H18 H 0.7342 0.5131 0.1437 0.035 Uiso 1 1 calc R . .
C19 C 0.5575(2) 0.5448(2) 0.1850(2) 0.0325(5) Uani 1 1 d . . .
H19 H 0.5296 0.6070 0.1404 0.039 Uiso 1 1 calc R . .
C20 C 0.4771(2) 0.5093(2) 0.2477(2) 0.0334(5) Uani 1 1 d . . .
H20 H 0.3938 0.5475 0.2461 0.040 Uiso 1 1 calc R . .
C21 C 0.5165(2) 0.4186(2) 0.3130(2) 0.0263(4) Uani 1 1 d . . .
H21 H 0.4599 0.3938 0.3551 0.032 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
Cl1 C8 1.7739(19) . ?
P1 O1 1.4927(13) . ?
P1 C16 1.7979(19) . ?
P1 C10 1.8107(19) . ?
P1 C9 1.8163(19) . ?
O2 C7 1.223(2) . ?
N1 C5 1.338(2) . ?
N1 C1 1.345(2) . ?
N2 C7 1.343(2) . ?
N2 C6 1.455(3) . ?
N2 H2A 0.86(2) . ?
C1 C2 1.383(3) . ?
C1 C9 1.511(3) . ?
C2 C3 1.391(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.375(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.515(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.514(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.390(3) . ?
C10 C15 1.398(3) . ?
C11 C12 1.393(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.377(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.383(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.393(3) . ?
C16 C21 1.394(3) . ?
C17 C18 1.380(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.380(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.385(3) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?

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 P1 C16 112.07(8) . . ?
O1 P1 C10 112.90(8) . . ?
C16 P1 C10 108.28(9) . . ?
O1 P1 C9 112.28(8) . . ?
C16 P1 C9 106.69(9) . . ?
C10 P1 C9 104.12(9) . . ?
C5 N1 C1 118.31(17) . . ?
C7 N2 C6 122.34(17) . . ?
C7 N2 H2A 119.9(15) . . ?
C6 N2 H2A 117.7(15) . . ?
N1 C1 C2 122.61(17) . . ?
N1 C1 C9 115.61(16) . . ?
C2 C1 C9 121.79(18) . . ?
C1 C2 C3 118.5(2) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 119.19(19) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C3 C4 C5 118.95(18) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N1 C5 C4 122.41(19) . . ?
N1 C5 C6 114.76(17) . . ?
C4 C5 C6 122.82(17) . . ?
N2 C6 C5 113.23(17) . . ?
N2 C6 H6A 108.9 . . ?
C5 C6 H6A 108.9 . . ?
N2 C6 H6B 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
O2 C7 N2 124.42(18) . . ?
O2 C7 C8 121.52(17) . . ?
N2 C7 C8 114.07(17) . . ?
C7 C8 Cl1 109.15(14) . . ?
C7 C8 H8A 109.8 . . ?
Cl1 C8 H8A 109.9 . . ?
C7 C8 H8B 109.8 . . ?
Cl1 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
C1 C9 P1 112.33(13) . . ?
C1 C9 H9A 109.1 . . ?
P1 C9 H9A 109.1 . . ?
C1 C9 H9B 109.1 . . ?
P1 C9 H9B 109.1 . . ?
H9A C9 H9B 107.9 . . ?
C11 C10 C15 119.22(17) . . ?
C11 C10 P1 123.11(15) . . ?
C15 C10 P1 117.60(14) . . ?
C10 C11 C12 120.15(19) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 120.0(2) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.26(19) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 120.2(2) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C10 120.18(19) . . ?
C14 C15 H15 119.9 . . ?
C10 C15 H15 119.9 . . ?
C17 C16 C21 119.61(18) . . ?
C17 C16 P1 122.07(14) . . ?
C21 C16 P1 118.12(15) . . ?
C18 C17 C16 120.08(18) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.27(19) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C20 C19 C18 119.77(19) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.65(19) . . ?
C19 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C20 C21 C16 119.62(19) . . ?
C20 C21 H21 120.2 . . ?
C16 C21 H21 120.2 . . ?

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
C5 N1 C1 C2 -2.0(3) . . . . ?
C5 N1 C1 C9 177.83(16) . . . . ?
N1 C1 C2 C3 -0.6(3) . . . . ?
C9 C1 C2 C3 179.62(18) . . . . ?
C1 C2 C3 C4 2.5(3) . . . . ?
C2 C3 C4 C5 -1.9(3) . . . . ?
C1 N1 C5 C4 2.7(3) . . . . ?
C1 N1 C5 C6 -178.18(16) . . . . ?
C3 C4 C5 N1 -0.7(3) . . . . ?
C3 C4 C5 C6 -179.82(19) . . . . ?
C7 N2 C6 C5 126.1(2) . . . . ?
N1 C5 C6 N2 135.16(18) . . . . ?
C4 C5 C6 N2 -45.7(3) . . . . ?
C6 N2 C7 O2 -1.4(3) . . . . ?
C6 N2 C7 C8 178.28(18) . . . . ?
O2 C7 C8 Cl1 -73.3(2) . . . . ?
N2 C7 C8 Cl1 106.99(17) . . . . ?
N1 C1 C9 P1 -70.57(19) . . . . ?
C2 C1 C9 P1 109.25(18) . . . . ?
O1 P1 C9 C1 -61.44(15) . . . . ?
C16 P1 C9 C1 61.71(15) . . . . ?
C10 P1 C9 C1 176.11(13) . . . . ?
O1 P1 C10 C11 113.73(17) . . . . ?
C16 P1 C10 C11 -10.96(19) . . . . ?
C9 P1 C10 C11 -124.22(17) . . . . ?
O1 P1 C10 C15 -63.27(17) . . . . ?
C16 P1 C10 C15 172.04(14) . . . . ?
C9 P1 C10 C15 58.77(16) . . . . ?
C15 C10 C11 C12 0.0(3) . . . . ?
P1 C10 C11 C12 -176.92(16) . . . . ?
C10 C11 C12 C13 0.3(3) . . . . ?
C11 C12 C13 C14 -0.4(3) . . . . ?
C12 C13 C14 C15 0.2(3) . . . . ?
C13 C14 C15 C10 0.2(3) . . . . ?
C11 C10 C15 C14 -0.3(3) . . . . ?
P1 C10 C15 C14 176.86(15) . . . . ?
O1 P1 C16 C17 -176.87(14) . . . . ?
C10 P1 C16 C17 -51.70(17) . . . . ?
C9 P1 C16 C17 59.85(17) . . . . ?
O1 P1 C16 C21 8.35(17) . . . . ?
C10 P1 C16 C21 133.52(15) . . . . ?
C9 P1 C16 C21 -114.93(15) . . . . ?
C21 C16 C17 C18 0.1(3) . . . . ?
P1 C16 C17 C18 -174.63(15) . . . . ?
C16 C17 C18 C19 0.5(3) . . . . ?
C17 C18 C19 C20 -0.5(3) . . . . ?
C18 C19 C20 C21 -0.1(3) . . . . ?
C19 C20 C21 C16 0.7(3) . . . . ?
C17 C16 C21 C20 -0.7(3) . . . . ?
P1 C16 C21 C20 174.26(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O1 0.86(2) 2.04(2) 2.882(2) 167(2) 2_666

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.04
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.048
_iucr_refine_instruction_details 
;
TITL rpso591_0m in P-1
CELL 0.71073 10.0038 10.2770 11.3976 111.639 114.435 95.410
ZERR 2.00 0.0004 0.0004 0.0004 0.002 0.002 0.002
LATT 1
SFAC C H N O P CL
UNIT 42 40 4 4 2 2
TEMP -100.160
SIZE 0.172 0.210 0.423
ACTA
OMIT 0   0   1
OMIT -1   1   0
OMIT 0  -1   1
OMIT 1   0   0
OMIT 0   1   0
OMIT -1   0   1
L.S. 10
FMAP 2
PLAN 5
BOND $H
EQIV $1 -x+1, -y+1, -z+1
HTAB N2 O1_$1
CONF
WGHT    0.041100    0.371400
FVAR       0.19519
CL1   6    0.668776    1.202833    0.893214    11.00000    0.04787    0.07982 =
         0.03126    0.01757    0.02481    0.03399
P1    5    0.698302    0.260676    0.417070    11.00000    0.01885    0.01875 =
         0.02106    0.00829    0.01027    0.00522
O1    4    0.588678    0.228986    0.467380    11.00000    0.02303    0.02554 =
         0.02671    0.01108    0.01383    0.00465
O2    4    0.881667    1.148634    0.741943    11.00000    0.02695    0.02400 =
         0.03424    0.00837    0.01653    0.00473
N1    3    0.872671    0.611489    0.613004    11.00000    0.02088    0.01986 =
         0.02503    0.00646    0.01256    0.00551
N2    3    0.728867    0.918407    0.646000    11.00000    0.02450    0.02132 =
         0.03873    0.00922    0.01813    0.00537
H2A   2    0.639538    0.865130    0.617830    11.00000   -1.20000
C1    1    0.894806    0.513729    0.666408    11.00000    0.01290    0.02449 =
         0.02126    0.00689    0.00620    0.00359
C2    1    0.919612    0.545236    0.803994    11.00000    0.02577    0.03683 =
         0.02618    0.01437    0.01247    0.00958
AFIX  43
H2    2    0.933998    0.473730    0.838559    11.00000   -1.20000
AFIX   0
C3    1    0.922998    0.684022    0.890519    11.00000    0.02938    0.04780 =
         0.02209    0.00853    0.01312    0.00965
AFIX  43
H3    2    0.943826    0.710194    0.986797    11.00000   -1.20000
AFIX   0
C4    1    0.895824    0.782930    0.834999    11.00000    0.02798    0.02793 =
         0.02740    0.00003    0.01420    0.00624
AFIX  43
H4    2    0.894571    0.877293    0.891319    11.00000   -1.20000
AFIX   0
C5    1    0.870256    0.742696    0.695365    11.00000    0.01761    0.02261 =
         0.03175    0.00709    0.01426    0.00368
C6    1    0.839807    0.844092    0.625036    11.00000    0.03669    0.02415 =
         0.04505    0.01350    0.02895    0.01226
AFIX  23
H6A   2    0.937647    0.918323    0.665274    11.00000   -1.20000
H6B   2    0.801533    0.786674    0.520271    11.00000   -1.20000
AFIX   0
C7    1    0.759378    1.064644    0.701594    11.00000    0.02612    0.02343 =
         0.02014    0.00858    0.01245    0.00659
C8    1    0.627103    1.119840    0.710390    11.00000    0.02765    0.02625 =
         0.02621    0.01203    0.01415    0.01100
AFIX  23
H8A   2    0.531567    1.037345    0.652135    11.00000   -1.20000
H8B   2    0.611714    1.192002    0.671337    11.00000   -1.20000
AFIX   0
C9    1    0.890414    0.365963    0.565898    11.00000    0.02084    0.02154 =
         0.02316    0.00980    0.00913    0.00704
AFIX  23
H9A   2    0.928983    0.310171    0.621080    11.00000   -1.20000
H9B   2    0.959523    0.380067    0.526861    11.00000   -1.20000
AFIX   0
C10   1    0.724467    0.096766    0.306847    11.00000    0.01761    0.01937 =
         0.02562    0.00748    0.01033    0.00359
C11   1    0.677337    0.051085    0.161274    11.00000    0.03005    0.02643 =
         0.02474    0.00926    0.01169    0.00890
AFIX  43
H11   2    0.633435    0.109318    0.116369    11.00000   -1.20000
AFIX   0
C12   1    0.694331   -0.079871    0.081099    11.00000    0.03619    0.03334 =
         0.02528    0.00649    0.01496    0.00938
AFIX  43
H12   2    0.662472   -0.110616   -0.018266    11.00000   -1.20000
AFIX   0
C13   1    0.757282   -0.164796    0.145778    11.00000    0.03108    0.02352 =
         0.03988    0.00763    0.02195    0.00879
AFIX  43
H13   2    0.768138   -0.254383    0.090704    11.00000   -1.20000
AFIX   0
C14   1    0.804781   -0.120176    0.290641    11.00000    0.03152    0.02436 =
         0.04095    0.01644    0.02103    0.01204
AFIX  43
H14   2    0.848411   -0.179043    0.334806    11.00000   -1.20000
AFIX   0
C15   1    0.788912    0.009885    0.371306    11.00000    0.02677    0.02405 =
         0.02800    0.01118    0.01550    0.00778
AFIX  43
H15   2    0.821904    0.040276    0.470819    11.00000   -1.20000
AFIX   0
C16   1    0.639720    0.363814    0.316694    11.00000    0.01896    0.01852 =
         0.01892    0.00608    0.00678    0.00345
C17   1    0.720763    0.399826    0.253327    11.00000    0.02260    0.02279 =
         0.02538    0.00914    0.01207    0.00634
AFIX  43
H17   2    0.804755    0.362725    0.255417    11.00000   -1.20000
AFIX   0
C18   1    0.679168    0.489347    0.187514    11.00000    0.03284    0.02708 =
         0.02728    0.01331    0.01417    0.00493
AFIX  43
H18   2    0.734153    0.513052    0.143727    11.00000   -1.20000
AFIX   0
C19   1    0.557516    0.544795    0.185046    11.00000    0.03458    0.02607 =
         0.03424    0.01746    0.01082    0.01047
AFIX  43
H19   2    0.529626    0.607019    0.140358    11.00000   -1.20000
AFIX   0
C20   1    0.477064    0.509305    0.247718    11.00000    0.02586    0.03015 =
         0.04534    0.01837    0.01581    0.01408
AFIX  43
H20   2    0.393791    0.547500    0.246060    11.00000   -1.20000
AFIX   0
C21   1    0.516491    0.418565    0.313012    11.00000    0.02246    0.02391 =
         0.03150    0.01031    0.01403    0.00710
AFIX  43
H21   2    0.459894    0.393764    0.355056    11.00000   -1.20000
 
HKLF 4 1 1 0 0 0 1 0 0 0 1
 
REM  rpso591_0m in P-1
REM R1 =  0.0382 for   2987 Fo > 4sig(Fo)  and  0.0514 for all   3724 data
REM    247 parameters refined using      0 restraints
 
END  
     
WGHT      0.0411      0.3711 
REM Highest difference peak  0.335,  deepest hole -0.467,  1-sigma level  0.048
Q1    1   0.6876  1.1223  0.8896  11.00000  0.05    0.33
Q2    1   0.7982  0.3198  0.4971  11.00000  0.05    0.33
Q3    1   0.7271  0.1750  0.3619  11.00000  0.05    0.30
Q4    1   0.7362  1.2736  0.9017  11.00000  0.05    0.29
Q5    1   0.6719  0.3205  0.3574  11.00000  0.05    0.27
;
_database_code_depnum_ccdc_archive 'CCDC 977749'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_twin4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H50 Er N7 O21 P2'
_chemical_formula_weight         1194.07

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'
Er Er -0.2586 4.9576 '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/c

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

_cell_length_a                   13.1332(9)
_cell_length_b                   11.4606(8)
_cell_length_c                   16.4028(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.252(3)
_cell_angle_gamma                90.00
_cell_volume                     2466.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1290
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      20.52

_exptl_crystal_description       rod
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1210
_exptl_absorpt_coefficient_mu    1.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6243
_exptl_absorpt_correction_T_max  0.7499
_exptl_absorpt_process_details   'Bruker, SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5076
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         26.45
_reflns_number_total             5076
_reflns_number_gt                4505
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0755P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5076
_refine_ls_number_parameters     343
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.1258
_refine_ls_wR_factor_gt          0.0970
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_restrained_S_all      1.268
_refine_ls_shift/su_max          0.007
_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
Er1 Er 0.5000 0.41023(2) 0.2500 0.01733(12) Uani 1 2 d S . .
O1 O 0.4266(3) 0.3627(3) 0.12306(19) 0.0257(7) Uani 1 1 d . . .
O2 O 0.5270(3) 0.4213(3) -0.1618(2) 0.0229(7) Uani 1 1 d . . .
O3 O 0.6564(2) 0.4715(3) 0.21387(19) 0.0215(7) Uani 1 1 d . . .
O4 O 0.8163(5) 0.1196(6) 0.2167(4) 0.0786(18) Uani 1 1 d . . .
O5 O 0.8918(4) 0.1124(5) 0.0997(5) 0.082(2) Uani 1 1 d . . .
O6 O 0.7561(4) 0.2144(5) 0.1089(3) 0.0643(14) Uani 1 1 d . . .
O7 O 0.5000 0.8591(5) 0.2500 0.0485(16) Uani 1 2 d S . .
O8 O 0.5317(4) 1.0209(4) 0.1900(3) 0.0528(12) Uani 1 1 d . . .
O9 O 0.5908(3) 0.2438(3) 0.2082(2) 0.0276(7) Uani 1 1 d D . .
H9A H 0.570(4) 0.171(2) 0.209(4) 0.041 Uiso 1 1 d D . .
H9B H 0.654(2) 0.243(4) 0.189(4) 0.041 Uiso 1 1 d D . .
O10 O 0.8100(4) 0.1694(5) -0.0649(4) 0.0633(14) Uani 1 1 d D . .
H10B H 0.794(7) 0.175(8) -0.015(2) 0.095 Uiso 1 1 d D . .
H10A H 0.845(6) 0.110(5) -0.074(5) 0.095 Uiso 1 1 d D . .
O11 O 0.0807(6) -0.0098(8) 0.1619(7) 0.136(4) Uani 1 1 d D . .
H11B H 0.024(6) 0.026(13) 0.160(10) 0.204 Uiso 1 1 d D . .
H11A H 0.114(10) 0.007(15) 0.206(6) 0.204 Uiso 1 1 d D . .
N1 N 0.4164(3) 0.2611(4) 0.0831(2) 0.0239(8) Uani 1 1 d . . .
N2 N 0.6116(3) 0.3101(4) -0.0687(3) 0.0279(9) Uani 1 1 d D . .
H2A H 0.661(3) 0.265(4) -0.063(4) 0.034 Uiso 1 1 d D . .
N3 N 0.8235(5) 0.1468(5) 0.1428(5) 0.0593(16) Uani 1 1 d . . .
N4 N 0.5000 0.9663(6) 0.2500 0.0337(14) Uani 1 2 d S . .
P1 P 0.73059(9) 0.56524(11) 0.24052(7) 0.0198(3) Uani 1 1 d . . .
C1 C 0.3494(4) 0.1801(5) 0.1076(3) 0.0278(11) Uani 1 1 d . . .
H1 H 0.3151 0.1913 0.1568 0.033 Uiso 1 1 calc R . .
C2 C 0.3309(4) 0.0825(5) 0.0622(4) 0.0367(13) Uani 1 1 d . . .
H2 H 0.2845 0.0252 0.0802 0.044 Uiso 1 1 calc R . .
C3 C 0.3799(5) 0.0667(5) -0.0106(4) 0.0385(14) Uani 1 1 d . . .
H3 H 0.3652 0.0009 -0.0442 0.046 Uiso 1 1 calc R . .
C4 C 0.4508(4) 0.1491(5) -0.0329(3) 0.0318(11) Uani 1 1 d . . .
H4 H 0.4865 0.1386 -0.0816 0.038 Uiso 1 1 calc R . .
C5 C 0.4701(4) 0.2457(4) 0.0147(3) 0.0238(10) Uani 1 1 d . . .
C6 C 0.5458(4) 0.3397(5) -0.0027(3) 0.0296(11) Uani 1 1 d . . .
H6A H 0.5087 0.4125 -0.0168 0.036 Uiso 1 1 calc R . .
H6B H 0.5885 0.3546 0.0473 0.036 Uiso 1 1 calc R . .
C7 C 0.5978(3) 0.3540(4) -0.1430(3) 0.0224(10) Uani 1 1 d . . .
C8 C 0.6723(4) 0.6846(4) 0.2942(3) 0.0242(10) Uani 1 1 d . . .
H8A H 0.7267 0.7316 0.3218 0.029 Uiso 1 1 calc R . .
H8B H 0.6361 0.7356 0.2538 0.029 Uiso 1 1 calc R . .
C9 C 0.8330(3) 0.5037(4) 0.3018(3) 0.0233(10) Uani 1 1 d . . .
C10 C 0.8533(4) 0.3856(5) 0.2918(3) 0.0310(11) Uani 1 1 d . . .
H10 H 0.8101 0.3394 0.2571 0.037 Uiso 1 1 calc R . .
C11 C 0.9370(4) 0.3352(6) 0.3328(3) 0.0380(13) Uani 1 1 d . . .
H11 H 0.9516 0.2548 0.3253 0.046 Uiso 1 1 calc R . .
C12 C 0.9985(4) 0.4019(5) 0.3841(4) 0.0390(14) Uani 1 1 d . . .
H12 H 1.0556 0.3672 0.4119 0.047 Uiso 1 1 calc R . .
C13 C 0.9783(4) 0.5178(6) 0.3954(3) 0.0386(14) Uani 1 1 d . . .
H13 H 1.0211 0.5627 0.4314 0.046 Uiso 1 1 calc R . .
C14 C 0.8955(4) 0.5704(5) 0.3546(3) 0.0334(12) Uani 1 1 d . . .
H14 H 0.8815 0.6509 0.3626 0.040 Uiso 1 1 calc R . .
C15 C 0.7825(4) 0.6369(5) 0.1543(3) 0.0243(10) Uani 1 1 d . . .
C16 C 0.8440(4) 0.7347(5) 0.1650(3) 0.0344(12) Uani 1 1 d . . .
H16 H 0.8615 0.7621 0.2184 0.041 Uiso 1 1 calc R . .
C17 C 0.8800(5) 0.7925(5) 0.0974(4) 0.0421(14) Uani 1 1 d . . .
H17 H 0.9219 0.8597 0.1045 0.051 Uiso 1 1 calc R . .
C18 C 0.8547(4) 0.7520(5) 0.0200(3) 0.0393(13) Uani 1 1 d . . .
H18 H 0.8786 0.7924 -0.0260 0.047 Uiso 1 1 calc R . .
C19 C 0.7952(4) 0.6537(5) 0.0087(3) 0.0324(12) Uani 1 1 d . . .
H19 H 0.7797 0.6252 -0.0448 0.039 Uiso 1 1 calc R . .
C20 C 0.7580(4) 0.5964(4) 0.0765(3) 0.0261(10) Uani 1 1 d . . .
H20 H 0.7158 0.5296 0.0692 0.031 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
Er1 O3 2.272(3) 2_655 ?
Er1 O3 2.272(3) . ?
Er1 O1 2.324(3) 2_655 ?
Er1 O1 2.324(3) . ?
Er1 O9 2.365(3) 2_655 ?
Er1 O9 2.365(3) . ?
Er1 O2 2.430(3) 4_566 ?
Er1 O2 2.430(3) 3_665 ?
O1 N1 1.340(5) . ?
O2 C7 1.238(6) . ?
O2 Er1 2.430(3) 3_665 ?
O3 P1 1.503(3) . ?
O4 N3 1.259(9) . ?
O5 N3 1.228(8) . ?
O6 N3 1.287(8) . ?
O7 N4 1.228(9) . ?
O8 N4 1.251(5) . ?
O9 H9A 0.879(19) . ?
O9 H9B 0.893(19) . ?
O10 H10B 0.85(2) . ?
O10 H10A 0.84(2) . ?
O11 H11B 0.85(2) . ?
O11 H11A 0.85(2) . ?
N1 C1 1.351(6) . ?
N1 C5 1.360(6) . ?
N2 C7 1.324(6) . ?
N2 C6 1.451(7) . ?
N2 H2A 0.84(2) . ?
N4 O8 1.251(5) 2_655 ?
P1 C9 1.792(5) . ?
P1 C15 1.792(5) . ?
P1 C8 1.813(5) . ?
C1 C2 1.360(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.390(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.501(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.514(6) 4_565 ?
C8 C7 1.514(6) 4_566 ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.390(7) . ?
C9 C14 1.397(7) . ?
C10 C11 1.390(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.369(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.392(8) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.384(7) . ?
C15 C16 1.390(7) . ?
C16 C17 1.389(8) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.381(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.397(7) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?

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 Er1 O3 144.00(16) 2_655 . ?
O3 Er1 O1 100.72(12) 2_655 2_655 ?
O3 Er1 O1 87.63(12) . 2_655 ?
O3 Er1 O1 87.63(12) 2_655 . ?
O3 Er1 O1 100.72(12) . . ?
O1 Er1 O1 152.91(17) 2_655 . ?
O3 Er1 O9 72.66(12) 2_655 2_655 ?
O3 Er1 O9 142.78(12) . 2_655 ?
O1 Er1 O9 75.36(12) 2_655 2_655 ?
O1 Er1 O9 82.82(12) . 2_655 ?
O3 Er1 O9 142.78(12) 2_655 . ?
O3 Er1 O9 72.66(12) . . ?
O1 Er1 O9 82.82(12) 2_655 . ?
O1 Er1 O9 75.36(12) . . ?
O9 Er1 O9 72.52(17) 2_655 . ?
O3 Er1 O2 73.24(11) 2_655 4_566 ?
O3 Er1 O2 78.31(11) . 4_566 ?
O1 Er1 O2 66.85(12) 2_655 4_566 ?
O1 Er1 O2 139.92(12) . 4_566 ?
O9 Er1 O2 122.09(12) 2_655 4_566 ?
O9 Er1 O2 138.56(11) . 4_566 ?
O3 Er1 O2 78.32(11) 2_655 3_665 ?
O3 Er1 O2 73.24(11) . 3_665 ?
O1 Er1 O2 139.92(12) 2_655 3_665 ?
O1 Er1 O2 66.85(12) . 3_665 ?
O9 Er1 O2 138.56(11) 2_655 3_665 ?
O9 Er1 O2 122.09(12) . 3_665 ?
O2 Er1 O2 74.82(16) 4_566 3_665 ?
N1 O1 Er1 132.2(3) . . ?
C7 O2 Er1 137.2(3) . 3_665 ?
P1 O3 Er1 136.64(19) . . ?
Er1 O9 H9A 127(3) . . ?
Er1 O9 H9B 126(3) . . ?
H9A O9 H9B 107(3) . . ?
H10B O10 H10A 113(4) . . ?
H11B O11 H11A 110(4) . . ?
O1 N1 C1 120.4(4) . . ?
O1 N1 C5 118.1(4) . . ?
C1 N1 C5 121.4(4) . . ?
C7 N2 C6 122.3(4) . . ?
C7 N2 H2A 114(4) . . ?
C6 N2 H2A 123(4) . . ?
O5 N3 O4 124.0(7) . . ?
O5 N3 O6 116.8(8) . . ?
O4 N3 O6 119.2(6) . . ?
O7 N4 O8 120.0(3) . . ?
O7 N4 O8 120.0(3) . 2_655 ?
O8 N4 O8 119.9(7) . 2_655 ?
O3 P1 C9 110.2(2) . . ?
O3 P1 C15 111.1(2) . . ?
C9 P1 C15 108.8(2) . . ?
O3 P1 C8 113.6(2) . . ?
C9 P1 C8 110.3(2) . . ?
C15 P1 C8 102.6(2) . . ?
N1 C1 C2 120.5(5) . . ?
N1 C1 H1 119.7 . . ?
C2 C1 H1 119.7 . . ?
C1 C2 C3 119.8(5) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 118.5(5) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C5 C4 C3 120.7(5) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
N1 C5 C4 118.9(5) . . ?
N1 C5 C6 115.7(4) . . ?
C4 C5 C6 125.4(5) . . ?
N2 C6 C5 113.1(4) . . ?
N2 C6 H6A 109.0 . . ?
C5 C6 H6A 109.0 . . ?
N2 C6 H6B 109.0 . . ?
C5 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
O2 C7 N2 122.7(4) . . ?
O2 C7 C8 120.8(4) . 4_565 ?
N2 C7 C8 116.5(4) . 4_565 ?
C7 C8 P1 113.9(3) 4_566 . ?
C7 C8 H8A 108.8 4_566 . ?
P1 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 4_566 . ?
P1 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C10 C9 C14 119.6(5) . . ?
C10 C9 P1 117.4(4) . . ?
C14 C9 P1 122.8(4) . . ?
C9 C10 C11 120.0(5) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 119.9(6) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C13 C12 C11 120.7(5) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 120.5(5) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C13 C14 C9 119.3(5) . . ?
C13 C14 H14 120.3 . . ?
C9 C14 H14 120.3 . . ?
C20 C15 C16 120.0(5) . . ?
C20 C15 P1 119.5(4) . . ?
C16 C15 P1 120.5(4) . . ?
C17 C16 C15 120.0(5) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 C16 119.7(5) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C19 120.9(5) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C18 C19 C20 119.4(5) . . ?
C18 C19 H19 120.3 . . ?
C20 C19 H19 120.3 . . ?
C15 C20 C19 120.1(5) . . ?
C15 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?

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
O3 Er1 O1 N1 -118.1(4) 2_655 . . . ?
O3 Er1 O1 N1 97.1(4) . . . . ?
O1 Er1 O1 N1 -9.0(4) 2_655 . . . ?
O9 Er1 O1 N1 -45.3(4) 2_655 . . . ?
O9 Er1 O1 N1 28.4(4) . . . . ?
O2 Er1 O1 N1 -178.3(3) 4_566 . . . ?
O2 Er1 O1 N1 163.6(4) 3_665 . . . ?
O3 Er1 O3 P1 41.4(3) 2_655 . . . ?
O1 Er1 O3 P1 -63.7(3) 2_655 . . . ?
O1 Er1 O3 P1 142.3(3) . . . . ?
O9 Er1 O3 P1 -125.5(3) 2_655 . . . ?
O9 Er1 O3 P1 -146.9(3) . . . . ?
O2 Er1 O3 P1 3.2(3) 4_566 . . . ?
O2 Er1 O3 P1 80.6(3) 3_665 . . . ?
Er1 O1 N1 C1 72.4(5) . . . . ?
Er1 O1 N1 C5 -111.9(4) . . . . ?
Er1 O3 P1 C9 103.3(3) . . . . ?
Er1 O3 P1 C15 -136.1(3) . . . . ?
Er1 O3 P1 C8 -21.0(4) . . . . ?
O1 N1 C1 C2 172.9(4) . . . . ?
C5 N1 C1 C2 -2.7(7) . . . . ?
N1 C1 C2 C3 -1.0(8) . . . . ?
C1 C2 C3 C4 3.1(9) . . . . ?
C2 C3 C4 C5 -1.8(9) . . . . ?
O1 N1 C5 C4 -171.6(4) . . . . ?
C1 N1 C5 C4 4.1(7) . . . . ?
O1 N1 C5 C6 7.5(6) . . . . ?
C1 N1 C5 C6 -176.8(4) . . . . ?
C3 C4 C5 N1 -1.8(8) . . . . ?
C3 C4 C5 C6 179.2(5) . . . . ?
C7 N2 C6 C5 102.6(5) . . . . ?
N1 C5 C6 N2 171.0(4) . . . . ?
C4 C5 C6 N2 -9.9(7) . . . . ?
Er1 O2 C7 N2 144.4(4) 3_665 . . . ?
Er1 O2 C7 C8 -37.1(7) 3_665 . . 4_565 ?
C6 N2 C7 O2 -1.4(8) . . . . ?
C6 N2 C7 C8 -180.0(4) . . . 4_565 ?
O3 P1 C8 C7 44.1(4) . . . 4_566 ?
C9 P1 C8 C7 -80.1(4) . . . 4_566 ?
C15 P1 C8 C7 164.1(3) . . . 4_566 ?
O3 P1 C9 C10 23.5(4) . . . . ?
C15 P1 C9 C10 -98.5(4) . . . . ?
C8 P1 C9 C10 149.7(4) . . . . ?
O3 P1 C9 C14 -160.2(4) . . . . ?
C15 P1 C9 C14 77.8(5) . . . . ?
C8 P1 C9 C14 -34.0(5) . . . . ?
C14 C9 C10 C11 -1.6(8) . . . . ?
P1 C9 C10 C11 174.8(4) . . . . ?
C9 C10 C11 C12 1.1(8) . . . . ?
C10 C11 C12 C13 0.0(9) . . . . ?
C11 C12 C13 C14 -0.5(9) . . . . ?
C12 C13 C14 C9 -0.1(8) . . . . ?
C10 C9 C14 C13 1.1(8) . . . . ?
P1 C9 C14 C13 -175.1(4) . . . . ?
O3 P1 C15 C20 -4.9(5) . . . . ?
C9 P1 C15 C20 116.6(4) . . . . ?
C8 P1 C15 C20 -126.6(4) . . . . ?
O3 P1 C15 C16 172.9(4) . . . . ?
C9 P1 C15 C16 -65.6(5) . . . . ?
C8 P1 C15 C16 51.2(5) . . . . ?
C20 C15 C16 C17 0.7(8) . . . . ?
P1 C15 C16 C17 -177.1(5) . . . . ?
C15 C16 C17 C18 -0.3(9) . . . . ?
C16 C17 C18 C19 -1.0(9) . . . . ?
C17 C18 C19 C20 1.7(9) . . . . ?
C16 C15 C20 C19 0.1(8) . . . . ?
P1 C15 C20 C19 177.9(4) . . . . ?
C18 C19 C20 C15 -1.3(8) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9A O8 0.879(19) 1.82(2) 2.683(5) 169(6) 1_545
O9 H9B O6 0.893(19) 1.95(3) 2.785(6) 155(5) .
O9 H9B O4 0.893(19) 2.58(4) 3.284(7) 136(5) .
O10 H10B O6 0.85(2) 2.16(2) 3.009(8) 172(9) .
O10 H10B O5 0.85(2) 2.35(7) 2.940(9) 127(7) .
O10 H10A O11 0.84(2) 2.11(5) 2.849(10) 147(8) 3_655
O11 H11B O5 0.85(2) 2.20(7) 2.993(11) 155(15) 1_455
O11 H11A O4 0.85(2) 2.00(9) 2.790(10) 153(17) 2_655
N2 H2A O10 0.84(2) 2.24(2) 3.064(7) 168(6) .

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        26.45
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.095
_refine_diff_density_min         -2.108
_refine_diff_density_rms         0.325
_iucr_refine_instruction_details 
;
TITL twin4 in P2/c
CELL 0.71073 13.1332 11.4606 16.4028 90.000 92.252 90.000
ZERR 2.00 0.0009 0.0008 0.0011 0.000 0.003 0.000
LATT 1
SYMM -x, y, -z+1/2
SFAC C H N O P ER
UNIT 80 100 14 42 4 2
TEMP -100.150
SIZE 0.165 0.278 0.281
ACTA
DFIX 0.85 o9 h9a o9 h9b
DFIX 1.45 h9a h9b
DFIX 0.83 o10 h10a o10 h10b
DFIX 1.41 h10a h10b
DFIX 0.83 o11 h11a o11 h11b
DFIX 1.41 h11a h11b
DFIX 0.84 N2 h2a
L.S. 10
FMAP 2
PLAN 10
EQIV $1 x, y-1, z
EQIV $2 -x+1, -y, -z
EQIV $3 x-1, y, z
EQIV $4 -x+1, y, -z+1/2
HTAB O9 O8_$1
HTAB O9 O6
HTAB O9 O4
HTAB O10 O6
HTAB O10 O5
HTAB O10 O11_$2
HTAB O11 O5_$3
HTAB O11 O4_$4
HTAB N2 O10
HTAB
BOND $H
CONF
WGHT    0.075500
FVAR       0.08994
ER1   6    0.500000    0.410228    0.250000    10.50000    0.01841    0.01939 =
         0.01426    0.00000    0.00151    0.00000
O1    4    0.426619    0.362723    0.123060    11.00000    0.03421    0.02378 =
         0.01861   -0.00642   -0.00440   -0.00144
O2    4    0.527030    0.421345   -0.161777    11.00000    0.02448    0.02081 =
         0.02357    0.00373    0.00332    0.00241
O3    4    0.656442    0.471483    0.213867    11.00000    0.01787    0.02388 =
         0.02308   -0.00444    0.00317   -0.00100
O4    4    0.816266    0.119606    0.216695    11.00000    0.08666    0.07431 =
         0.07429   -0.00544   -0.00517    0.02675
O5    4    0.891832    0.112434    0.099721    11.00000    0.05541    0.07248 =
         0.11922   -0.03841    0.03178    0.00367
O6    4    0.756086    0.214442    0.108919    11.00000    0.06141    0.06513 =
         0.06850   -0.00223    0.02828    0.01161
O7    4    0.500000    0.859136    0.250000    10.50000    0.04550    0.01516 =
         0.08454    0.00000   -0.00064    0.00000
O8    4    0.531705    1.020929    0.190021    11.00000    0.09017    0.02616 =
         0.04310   -0.00615    0.01460   -0.00607
O9    4    0.590795    0.243825    0.208167    11.00000    0.03134    0.02438 =
         0.02738   -0.00263    0.00674   -0.00078
H9A   2    0.569755    0.171057    0.209248    11.00000   -1.50000
H9B   2    0.653719    0.242984    0.189453    11.00000   -1.50000
O10   4    0.809995    0.169364   -0.064913    11.00000    0.05559    0.04447 =
         0.08796    0.01808   -0.01960   -0.00013
H10B  2    0.794334    0.174833   -0.015109    11.00000   -1.50000
H10A  2    0.845265    0.110308   -0.074194    11.00000   -1.50000
O11   4    0.080707   -0.009789    0.161925    11.00000    0.07438    0.10442 =
         0.22839   -0.09412   -0.01275    0.00717
H11B  2    0.023602    0.025605    0.160182    11.00000   -1.50000
H11A  2    0.113890    0.007151    0.205982    11.00000   -1.50000
N1    3    0.416374    0.261121    0.083119    11.00000    0.02530    0.02636 =
         0.01954    0.00005   -0.00371    0.00067
N2    3    0.611553    0.310138   -0.068724    11.00000    0.03393    0.02673 =
         0.02326    0.00615    0.00258    0.00294
H2A   2    0.661233    0.264717   -0.063240    11.00000   -1.20000
N3    3    0.823499    0.146751    0.142761    11.00000    0.04513    0.04573 =
         0.08708   -0.01733    0.00410    0.00147
N4    3    0.500000    0.966270    0.250000    10.50000    0.03816    0.02383 =
         0.03828    0.00000   -0.00787    0.00000
P1    5    0.730586    0.565240    0.240517    11.00000    0.01781    0.02381 =
         0.01809   -0.00064    0.00289   -0.00093
C1    1    0.349446    0.180057    0.107567    11.00000    0.02306    0.03333 =
         0.02669    0.00095   -0.00239   -0.00412
AFIX  43
H1    2    0.315075    0.191292    0.156850    11.00000   -1.20000
AFIX   0
C2    1    0.330854    0.082452    0.062192    11.00000    0.02909    0.03528 =
         0.04570    0.00141   -0.00058   -0.00930
AFIX  43
H2    2    0.284459    0.025226    0.080172    11.00000   -1.20000
AFIX   0
C3    1    0.379940    0.066676   -0.010570    11.00000    0.04374    0.02980 =
         0.04164   -0.01086   -0.00360   -0.00378
AFIX  43
H3    2    0.365194    0.000880   -0.044228    11.00000   -1.20000
AFIX   0
C4    1    0.450833    0.149065   -0.032880    11.00000    0.03796    0.02877 =
         0.02854   -0.00676    0.00055    0.00016
AFIX  43
H4    2    0.486514    0.138553   -0.081612    11.00000   -1.20000
AFIX   0
C5    1    0.470070    0.245734    0.014683    11.00000    0.02994    0.02495 =
         0.01630    0.00239   -0.00220    0.00307
C6    1    0.545828    0.339656   -0.002712    11.00000    0.04432    0.02526 =
         0.01941    0.00253    0.00336   -0.00454
AFIX  23
H6A   2    0.508654    0.412512   -0.016804    11.00000   -1.20000
H6B   2    0.588494    0.354640    0.047293    11.00000   -1.20000
AFIX   0
C7    1    0.597820    0.354032   -0.143011    11.00000    0.02179    0.02252 =
         0.02289    0.00090    0.00083   -0.00280
C8    1    0.672300    0.684626    0.294178    11.00000    0.02469    0.02000 =
         0.02814   -0.00111    0.00339   -0.00086
AFIX  23
H8A   2    0.726705    0.731605    0.321790    11.00000   -1.20000
H8B   2    0.636144    0.735621    0.253842    11.00000   -1.20000
AFIX   0
C9    1    0.833000    0.503684    0.301776    11.00000    0.01761    0.03193 =
         0.02030    0.00342    0.00155   -0.00171
C10   1    0.853332    0.385614    0.291838    11.00000    0.02832    0.03673 =
         0.02822    0.00034    0.00348    0.00389
AFIX  43
H10   2    0.810097    0.339379    0.257097    11.00000   -1.20000
AFIX   0
C11   1    0.936973    0.335223    0.332767    11.00000    0.03603    0.05150 =
         0.02680    0.00575    0.00488    0.01837
AFIX  43
H11   2    0.951603    0.254834    0.325316    11.00000   -1.20000
AFIX   0
C12   1    0.998523    0.401926    0.384071    11.00000    0.02347    0.06225 =
         0.03148    0.00940    0.00298    0.01040
AFIX  43
H12   2    1.055630    0.367197    0.411909    11.00000   -1.20000
AFIX   0
C13   1    0.978303    0.517834    0.395406    11.00000    0.02436    0.05754 =
         0.03330    0.00694   -0.00603   -0.00914
AFIX  43
H13   2    1.021106    0.562710    0.431373    11.00000   -1.20000
AFIX   0
C14   1    0.895455    0.570412    0.354598    11.00000    0.03141    0.03733 =
         0.03125    0.00299   -0.00262   -0.00723
AFIX  43
H14   2    0.881517    0.650856    0.362581    11.00000   -1.20000
AFIX   0
C15   1    0.782454    0.636850    0.154325    11.00000    0.02261    0.02814 =
         0.02262    0.00116    0.00572    0.00049
C16   1    0.844014    0.734724    0.164966    11.00000    0.04211    0.03399 =
         0.02760   -0.00376    0.00664   -0.01073
AFIX  43
H16   2    0.861463    0.762085    0.218373    11.00000   -1.20000
AFIX   0
C17   1    0.880027    0.792540    0.097441    11.00000    0.04975    0.03307 =
         0.04476   -0.00030    0.01726   -0.01074
AFIX  43
H17   2    0.921890    0.859661    0.104523    11.00000   -1.20000
AFIX   0
C18   1    0.854718    0.752038    0.020045    11.00000    0.04441    0.04321 =
         0.03109    0.01355    0.01233    0.00648
AFIX  43
H18   2    0.878583    0.792418   -0.026042    11.00000   -1.20000
AFIX   0
C19   1    0.795199    0.653651    0.008671    11.00000    0.02934    0.04498 =
         0.02280    0.00061    0.00024    0.00402
AFIX  43
H19   2    0.779719    0.625172   -0.044779    11.00000   -1.20000
AFIX   0
C20   1    0.757951    0.596369    0.076524    11.00000    0.01814    0.03509 =
         0.02511    0.00309    0.00065    0.00108
AFIX  43
H20   2    0.715755    0.529554    0.069247    11.00000   -1.20000
 
HKLF 4 1 1 0 0 0 1 0 0 0 1
 
REM  twin4 in P2/c
REM R1 =  0.0342 for   4505 Fo > 4sig(Fo)  and  0.0440 for all   5076 data
REM    343 parameters refined using     10 restraints
 
END  
     
WGHT      0.0755      0.0000 
REM Highest difference peak  1.095,  deepest hole -2.108,  1-sigma level  0.325
Q1    1   0.7871  0.1881  0.0465  11.00000  0.05    1.09
Q2    1   0.6868  0.2195  0.0693  11.00000  0.05    0.75
Q3    1   0.3652  0.0846  0.0122  11.00000  0.05    0.74
Q4    1   0.5229  0.2710  0.0081  11.00000  0.05    0.72
Q5    1   0.6347  0.2997 -0.0574  11.00000  0.05    0.71
Q6    1   0.4394  0.2002 -0.0256  11.00000  0.05    0.71
Q7    1   0.4013  0.1107 -0.0250  11.00000  0.05    0.70
Q8    1   0.5604  0.3077 -0.0472  11.00000  0.05    0.66
Q9    1   0.4540  0.1250 -0.0173  11.00000  0.05    0.66
Q10   1   0.4584  0.8964  0.2442  11.00000  0.05    0.64
;
_database_code_depnum_ccdc_archive 'CCDC 977751'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rprd526_0m_sq_s
_vrf_PLAT420_rprd526_0m_sq_s     
;
RESPONSE:  O16 is part of a partially occupied solvent position
and may form H-bonds with severely disordered solvent that was
accounted for using SQUEEZE.
;
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C71 H74 Eu2 N10 O30 P4'
_chemical_formula_weight         1975.20

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'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.0923(9)
_cell_length_b                   25.3538(18)
_cell_length_c                   18.0674(14)
_cell_angle_alpha                90
_cell_angle_beta                 104.373(4)
_cell_angle_gamma                90
_cell_volume                     4922.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      28.30

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             1992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.511
_exptl_crystal_size_mid          0.436
_exptl_crystal_size_min          0.288
_exptl_absorpt_coefficient_mu    1.401
_shelx_estimated_absorpt_T_min   0.535
_shelx_estimated_absorpt_T_max   0.688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_T_max  0.69

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56754
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.462
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             11283
_reflns_number_gt                10580
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²+14.4989P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11283
_refine_ls_number_parameters     560
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0418
_refine_ls_wR_factor_ref         0.1006
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_restrained_S_all      1.234
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.68708(2) -0.00628(2) 0.32915(2) 0.02071(6) Uani 1 1 d . . . . .
O1 O 1.1695(2) 0.06448(10) 0.59826(14) 0.0264(5) Uani 1 1 d . . . . .
O2 O 0.8900(2) 0.03726(10) 0.35941(14) 0.0260(5) Uani 1 1 d . . . . .
O3 O 0.7870(2) -0.03192(10) 0.23241(13) 0.0250(5) Uani 1 1 d . . . . .
O4 O 1.4123(2) 0.08685(10) 0.71132(14) 0.0261(5) Uani 1 1 d . . . . .
O5 O 0.6614(3) 0.07796(11) 0.25682(16) 0.0362(7) Uani 1 1 d . . . . .
O6 O 0.5377(3) 0.01633(11) 0.20142(16) 0.0341(6) Uani 1 1 d . . . . .
O7 O 0.5485(4) 0.09006(13) 0.14166(19) 0.0544(9) Uani 1 1 d . . . . .
O8 O 0.5790(3) -0.04320(13) 0.43146(17) 0.0422(7) Uani 1 1 d . . . . .
O9 O 0.4720(3) 0.00627(12) 0.34145(19) 0.0408(7) Uani 1 1 d . . . . .
O10 O 0.3825(4) -0.0293(2) 0.4228(2) 0.0722(13) Uani 1 1 d . . . . .
O11 O 0.0230(6) 0.16832(17) 0.2466(3) 0.0897(17) Uani 1 1 d . . . . .
O12 O 0.0902(5) 0.23971(17) 0.3030(2) 0.0769(13) Uani 1 1 d . . . . .
O13 O 0.1256(9) 0.2233(2) 0.1977(4) 0.155(4) Uani 1 1 d . . . . .
N1 N 1.1675(3) 0.11009(12) 0.56155(16) 0.0226(6) Uani 1 1 d . . . . .
N2 N 1.0918(3) 0.05636(13) 0.36651(16) 0.0265(6) Uani 1 1 d . . . . .
H50 H 1.1485 0.0634 0.3414 0.032 Uiso 1 1 calc R U . . .
N3 N 0.5804(3) 0.06215(13) 0.19797(19) 0.0322(7) Uani 1 1 d . . . . .
N4 N 0.4759(4) -0.02247(17) 0.4002(2) 0.0434(9) Uani 1 1 d . . . . .
N5 N 0.0759(5) 0.21144(16) 0.2484(3) 0.0567(12) Uani 1 1 d . . . . .
P1 P 0.88567(8) -0.00989(4) 0.19692(5) 0.02178(18) Uani 1 1 d . . . . .
P2 P 1.37337(9) 0.14076(4) 0.73060(5) 0.02480(19) Uani 1 1 d . . . . .
C1 C 1.1829(3) 0.15605(15) 0.6012(2) 0.0256(7) Uani 1 1 d . . . . .
C2 C 1.1701(4) 0.20309(16) 0.5612(2) 0.0334(9) Uani 1 1 d . . . . .
H2 H 1.1818 0.2356 0.5881 0.040 Uiso 1 1 calc R U . . .
C3 C 1.1404(4) 0.20298(16) 0.4823(2) 0.0349(9) Uani 1 1 d . . . . .
H3 H 1.1286 0.2353 0.4548 0.042 Uiso 1 1 calc R U . . .
C4 C 1.1281(4) 0.15532(16) 0.4438(2) 0.0303(8) Uani 1 1 d . . . . .
H4 H 1.1101 0.1549 0.3896 0.036 Uiso 1 1 calc R U . . .
C5 C 1.1418(3) 0.10826(14) 0.48401(19) 0.0230(7) Uani 1 1 d . . . . .
C6 C 1.1280(3) 0.05416(15) 0.44909(19) 0.0258(7) Uani 1 1 d . . . . .
H6A H 1.2080 0.0351 0.4657 0.031 Uiso 1 1 calc R U . . .
H6B H 1.0645 0.0343 0.4676 0.031 Uiso 1 1 calc R U . . .
C7 C 0.9745(3) 0.04806(13) 0.32751(19) 0.0232(7) Uani 1 1 d . . . . .
C8 C 0.9478(3) 0.05181(14) 0.24123(19) 0.0245(7) Uani 1 1 d . . . . .
H8A H 1.0255 0.0605 0.2263 0.029 Uiso 1 1 calc R U . . .
H8B H 0.8871 0.0805 0.2229 0.029 Uiso 1 1 calc R U . . .
C9 C 1.0113(3) -0.05603(15) 0.2039(2) 0.0262(7) Uani 1 1 d . . . . .
C10 C 1.1367(4) -0.04323(17) 0.2298(2) 0.0322(8) Uani 1 1 d . . . . .
H10 H 1.1605 -0.0083 0.2459 0.039 Uiso 1 1 calc R U . . .
C11 C 1.2271(4) -0.0816(2) 0.2323(2) 0.0412(10) Uani 1 1 d . . . . .
H11 H 1.3126 -0.0727 0.2499 0.049 Uiso 1 1 calc R U . . .
C12 C 1.1934(5) -0.1324(2) 0.2092(3) 0.0482(12) Uani 1 1 d . . . . .
H12 H 1.2557 -0.1585 0.2114 0.058 Uiso 1 1 calc R U . . .
C13 C 1.0697(5) -0.1455(2) 0.1831(3) 0.0532(13) Uani 1 1 d . . . . .
H13 H 1.0467 -0.1806 0.1670 0.064 Uiso 1 1 calc R U . . .
C14 C 0.9782(4) -0.10760(17) 0.1803(3) 0.0389(10) Uani 1 1 d . . . . .
H14 H 0.8929 -0.1168 0.1622 0.047 Uiso 1 1 calc R U . . .
C15 C 0.8240(3) 0.00319(15) 0.09745(19) 0.0249(7) Uani 1 1 d . . . . .
C16 C 0.8921(4) 0.0292(2) 0.0544(2) 0.0489(13) Uani 1 1 d . . . . .
H16 H 0.9720 0.0431 0.0779 0.059 Uiso 1 1 calc R U . . .
C17 C 0.8424(5) 0.0351(2) -0.0243(2) 0.0544(14) Uani 1 1 d . . . . .
H17 H 0.8878 0.0541 -0.0539 0.065 Uiso 1 1 calc R U . . .
C18 C 0.7298(4) 0.01397(19) -0.0588(2) 0.0386(10) Uani 1 1 d . . . . .
H18 H 0.6984 0.0171 -0.1126 0.046 Uiso 1 1 calc R U . . .
C19 C 0.6617(5) -0.0118(2) -0.0165(3) 0.0480(12) Uani 1 1 d . . . . .
H19 H 0.5825 -0.0261 -0.0407 0.058 Uiso 1 1 calc R U . . .
C20 C 0.7087(4) -0.0171(2) 0.0622(2) 0.0405(10) Uani 1 1 d . . . . .
H20 H 0.6611 -0.0348 0.0917 0.049 Uiso 1 1 calc R U . . .
C21 C 1.2101(3) 0.15354(15) 0.6866(2) 0.0265(7) Uani 1 1 d . . . . .
H21A H 1.1591 0.1253 0.7014 0.032 Uiso 1 1 calc R U . . .
H21B H 1.1859 0.1874 0.7061 0.032 Uiso 1 1 calc R U . . .
C22 C 1.3980(4) 0.14871(15) 0.8317(2) 0.0270(8) Uani 1 1 d . . . . .
C23 C 1.4885(4) 0.11720(17) 0.8780(2) 0.0351(9) Uani 1 1 d . . . . .
H23 H 1.5321 0.0920 0.8555 0.042 Uiso 1 1 calc R U . . .
C24 C 1.5156(4) 0.12225(18) 0.9566(2) 0.0407(10) Uani 1 1 d . . . . .
H24 H 1.5776 0.1006 0.9880 0.049 Uiso 1 1 calc R U . . .
C25 C 1.4531(5) 0.15843(19) 0.9892(2) 0.0447(11) Uani 1 1 d . . . . .
H25 H 1.4717 0.1618 1.0432 0.054 Uiso 1 1 calc R U . . .
C26 C 1.3630(6) 0.1902(2) 0.9438(3) 0.0549(14) Uani 1 1 d . . . . .
H26 H 1.3201 0.2153 0.9667 0.066 Uiso 1 1 calc R U . . .
C27 C 1.3352(5) 0.18540(19) 0.8650(2) 0.0454(12) Uani 1 1 d . . . . .
H27 H 1.2733 0.2072 0.8339 0.055 Uiso 1 1 calc R U . . .
C28 C 1.4641(4) 0.19038(16) 0.6974(2) 0.0356(9) Uani 1 1 d . . . . .
C29 C 1.4655(7) 0.2420(2) 0.7223(3) 0.0659(17) Uani 1 1 d . . . . .
H29 H 1.4148 0.2522 0.7552 0.079 Uiso 1 1 calc R U . . .
C30 C 1.5414(8) 0.2789(2) 0.6991(4) 0.084(2) Uani 1 1 d . . . . .
H30 H 1.5438 0.3142 0.7169 0.101 Uiso 1 1 calc R U . . .
C31 C 1.6120(7) 0.2644(2) 0.6511(4) 0.073(2) Uani 1 1 d . . . . .
H31 H 1.6642 0.2896 0.6355 0.087 Uiso 1 1 calc R U . . .
C32 C 1.6083(6) 0.2141(3) 0.6252(4) 0.0691(17) Uani 1 1 d . . . . .
H32 H 1.6571 0.2044 0.5909 0.083 Uiso 1 1 calc R U . . .
C33 C 1.5338(5) 0.1764(2) 0.6484(3) 0.0498(12) Uani 1 1 d . . . . .
H33 H 1.5317 0.1413 0.6300 0.060 Uiso 1 1 calc R U . . .
O14 O 0.7018(9) 0.0548(3) 0.4395(7) 0.032(2) Uani 0.5 1 d G . P A -1
O15 O 0.6434(5) 0.1312(2) 0.4779(3) 0.063(2) Uani 0.5 1 d G . P A -1
C35 C 0.8414(6) 0.1008(4) 0.5400(6) 0.064(4) Uani 0.5 1 d G . P A -1
H35A H 0.8234 0.1047 0.5901 0.096 Uiso 0.5 1 calc R U P A -1
H35B H 0.8827 0.1327 0.5281 0.096 Uiso 0.5 1 calc R U P A -1
H35C H 0.8961 0.0703 0.5407 0.096 Uiso 0.5 1 calc R U P A -1
C36 C 0.7239(5) 0.0927(2) 0.4811(3) 0.046(2) Uani 0.5 1 d G . P A -1
C37 C 0.5241(5) 0.1276(3) 0.4218(4) 0.083(5) Uani 0.5 1 d G . P A -1
H37A H 0.5376 0.1228 0.3701 0.100 Uiso 0.5 1 calc R U P A -1
H37B H 0.4768 0.0969 0.4334 0.100 Uiso 0.5 1 calc R U P A -1
C38 C 0.4561(7) 0.1746(3) 0.4243(6) 0.073(4) Uani 0.5 1 d G . P A -1
H38A H 0.4368 0.1776 0.4742 0.110 Uiso 0.5 1 calc R U P A -1
H38B H 0.3785 0.1737 0.3840 0.110 Uiso 0.5 1 calc R U P A -1
H38C H 0.5059 0.2050 0.4164 0.110 Uiso 0.5 1 calc R U P A -1
O16 O 0.7029(11) 0.0591(4) 0.4232(7) 0.032(2) Uani 0.5 1 d D . P A -2
H16A H 0.638(6) 0.084(3) 0.428(5) 0.038 Uiso 0.5 1 d D U P B -2
H16B H 0.696(8) 0.041(3) 0.468(3) 0.038 Uiso 0.5 1 d D U P C -2
O17 O 0.8877(7) 0.1123(3) 0.5175(4) 0.0416(18) Uani 0.5 1 d . . P D -2
H17A H 0.8619 0.0845 0.4936 0.062 Uiso 0.5 1 calc R U P D -2
C39 C 0.8794(9) 0.1074(5) 0.5962(5) 0.051(3) Uani 0.5 1 d . . P D -2
H39A H 0.8876 0.1423 0.6201 0.076 Uiso 0.5 1 calc R U P D -2
H39B H 0.9464 0.0844 0.6242 0.076 Uiso 0.5 1 calc R U P D -2
H39C H 0.7987 0.0921 0.5973 0.076 Uiso 0.5 1 calc R U P D -2


_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
Eu1 O1 2.322(2) 3_756 ?
Eu1 O16 2.349(8) . ?
Eu1 O4 2.350(2) 3_756 ?
Eu1 O3 2.381(2) . ?
Eu1 O2 2.444(3) . ?
Eu1 O9 2.471(3) . ?
Eu1 O5 2.483(3) . ?
Eu1 O14 2.497(7) . ?
Eu1 O6 2.550(3) . ?
Eu1 O8 2.613(3) . ?
Eu1 N3 2.939(3) . ?
Eu1 N4 2.966(4) . ?
O1 N1 1.330(4) . ?
O1 Eu1 2.322(2) 3_756 ?
O2 C7 1.246(4) . ?
O3 P1 1.506(3) . ?
O4 P2 1.500(3) . ?
O4 Eu1 2.350(2) 3_756 ?
O5 N3 1.275(4) . ?
O6 N3 1.262(4) . ?
O7 N3 1.217(4) . ?
O8 N4 1.258(5) . ?
O9 N4 1.280(5) . ?
O10 N4 1.216(5) . ?
O11 N5 1.237(5) . ?
O12 N5 1.198(6) . ?
O13 N5 1.217(6) . ?
N1 C1 1.356(5) . ?
N1 C5 1.359(4) . ?
N2 C7 1.334(5) . ?
N2 C6 1.447(4) . ?
P1 C15 1.788(4) . ?
P1 C9 1.800(4) . ?
P1 C8 1.814(4) . ?
P2 C22 1.790(4) . ?
P2 C28 1.804(4) . ?
P2 C21 1.817(4) . ?
P2 Eu1 3.5890(10) 3_756 ?
C1 C2 1.383(5) . ?
C1 C21 1.498(5) . ?
C2 C3 1.381(6) . ?
C3 C4 1.384(6) . ?
C4 C5 1.385(5) . ?
C5 C6 1.502(5) . ?
C7 C8 1.516(5) . ?
C9 C10 1.391(5) . ?
C9 C14 1.396(6) . ?
C10 C11 1.389(6) . ?
C11 C12 1.377(7) . ?
C12 C13 1.377(7) . ?
C13 C14 1.389(7) . ?
C15 C20 1.379(5) . ?
C15 C16 1.380(5) . ?
C16 C17 1.399(6) . ?
C17 C18 1.360(7) . ?
C18 C19 1.369(7) . ?
C19 C20 1.394(6) . ?
C22 C27 1.386(6) . ?
C22 C23 1.389(5) . ?
C23 C24 1.384(5) . ?
C24 C25 1.368(7) . ?
C25 C26 1.383(7) . ?
C26 C27 1.384(6) . ?
C28 C33 1.360(7) . ?
C28 C29 1.382(7) . ?
C29 C30 1.392(8) . ?
C30 C31 1.355(10) . ?
C31 C32 1.357(9) . ?
C32 C33 1.393(7) . ?
O14 C36 1.2074 . ?
O15 C36 1.3142 . ?
O15 C37 1.4563 . ?
C35 C36 1.4778 . ?
C37 C38 1.4167 . ?
O17 C39 1.454(10) . ?

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 Eu1 O16 97.0(3) 3_756 . ?
O1 Eu1 O4 79.97(9) 3_756 3_756 ?
O16 Eu1 O4 141.6(4) . 3_756 ?
O1 Eu1 O3 82.10(9) 3_756 . ?
O16 Eu1 O3 139.4(4) . . ?
O4 Eu1 O3 78.59(9) 3_756 . ?
O1 Eu1 O2 72.37(9) 3_756 . ?
O16 Eu1 O2 67.7(3) . . ?
O4 Eu1 O2 142.85(9) 3_756 . ?
O3 Eu1 O2 73.54(8) . . ?
O1 Eu1 O9 124.90(10) 3_756 . ?
O16 Eu1 O9 75.2(3) . . ?
O4 Eu1 O9 75.59(10) 3_756 . ?
O3 Eu1 O9 137.49(10) . . ?
O2 Eu1 O9 141.07(9) . . ?
O1 Eu1 O5 144.77(10) 3_756 . ?
O16 Eu1 O5 75.6(4) . . ?
O4 Eu1 O5 126.90(9) 3_756 . ?
O3 Eu1 O5 82.06(10) . . ?
O2 Eu1 O5 73.03(9) . . ?
O9 Eu1 O5 87.11(11) . . ?
O1 Eu1 O14 92.5(2) 3_756 . ?
O4 Eu1 O14 136.0(4) 3_756 . ?
O3 Eu1 O14 143.6(3) . . ?
O2 Eu1 O14 70.6(3) . . ?
O9 Eu1 O14 73.8(3) . . ?
O5 Eu1 O14 82.1(3) . . ?
O1 Eu1 O6 148.67(9) 3_756 . ?
O16 Eu1 O6 114.3(3) . . ?
O4 Eu1 O6 76.38(9) 3_756 . ?
O3 Eu1 O6 73.35(9) . . ?
O2 Eu1 O6 117.16(9) . . ?
O9 Eu1 O6 68.12(11) . . ?
O5 Eu1 O6 50.69(9) . . ?
O14 Eu1 O6 118.8(2) . . ?
O1 Eu1 O8 75.10(10) 3_756 . ?
O16 Eu1 O8 72.9(4) . . ?
O4 Eu1 O8 69.31(9) 3_756 . ?
O3 Eu1 O8 143.16(10) . . ?
O2 Eu1 O8 124.21(9) . . ?
O9 Eu1 O8 50.21(11) . . ?
O5 Eu1 O8 131.88(11) . . ?
O14 Eu1 O8 66.9(4) . . ?
O6 Eu1 O8 114.31(10) . . ?
O1 Eu1 N3 155.93(10) 3_756 . ?
O16 Eu1 N3 96.3(3) . . ?
O4 Eu1 N3 101.45(9) 3_756 . ?
O3 Eu1 N3 74.75(9) . . ?
O2 Eu1 N3 94.47(9) . . ?
O9 Eu1 N3 77.99(11) . . ?
O5 Eu1 N3 25.46(9) . . ?
O14 Eu1 N3 102.2(3) . . ?
O6 Eu1 N3 25.34(9) . . ?
O8 Eu1 N3 128.20(11) . . ?
O1 Eu1 N4 99.85(11) 3_756 . ?
O16 Eu1 N4 73.1(4) . . ?
O4 Eu1 N4 69.79(10) 3_756 . ?
O3 Eu1 N4 147.33(9) . . ?
O2 Eu1 N4 138.43(9) . . ?
O9 Eu1 N4 25.18(12) . . ?
O5 Eu1 N4 110.33(12) . . ?
O14 Eu1 N4 69.0(3) . . ?
O6 Eu1 N4 91.00(11) . . ?
O8 Eu1 N4 25.05(11) . . ?
N3 Eu1 N4 103.16(12) . . ?
N1 O1 Eu1 139.3(2) . 3_756 ?
C7 O2 Eu1 138.8(2) . . ?
P1 O3 Eu1 136.99(15) . . ?
P2 O4 Eu1 136.42(16) . 3_756 ?
N3 O5 Eu1 97.7(2) . . ?
N3 O6 Eu1 94.8(2) . . ?
N4 O8 Eu1 93.4(2) . . ?
N4 O9 Eu1 99.6(3) . . ?
O1 N1 C1 120.0(3) . . ?
O1 N1 C5 117.2(3) . . ?
C1 N1 C5 122.7(3) . . ?
C7 N2 C6 121.6(3) . . ?
O7 N3 O6 122.8(3) . . ?
O7 N3 O5 120.8(4) . . ?
O6 N3 O5 116.4(3) . . ?
O7 N3 Eu1 172.9(3) . . ?
O6 N3 Eu1 59.84(18) . . ?
O5 N3 Eu1 56.87(18) . . ?
O10 N4 O8 123.1(5) . . ?
O10 N4 O9 120.1(5) . . ?
O8 N4 O9 116.7(3) . . ?
O10 N4 Eu1 174.1(3) . . ?
O8 N4 Eu1 61.6(2) . . ?
O9 N4 Eu1 55.23(19) . . ?
O12 N5 O13 118.7(5) . . ?
O12 N5 O11 121.0(5) . . ?
O13 N5 O11 119.9(5) . . ?
O3 P1 C15 111.07(16) . . ?
O3 P1 C9 111.14(16) . . ?
C15 P1 C9 106.73(17) . . ?
O3 P1 C8 111.61(16) . . ?
C15 P1 C8 107.00(17) . . ?
C9 P1 C8 109.08(18) . . ?
O4 P2 C22 111.08(16) . . ?
O4 P2 C28 109.98(19) . . ?
C22 P2 C28 107.69(18) . . ?
O4 P2 C21 111.94(16) . . ?
C22 P2 C21 108.05(18) . . ?
C28 P2 C21 107.93(19) . . ?
O4 P2 Eu1 26.83(10) . 3_756 ?
C22 P2 Eu1 112.57(12) . 3_756 ?
C28 P2 Eu1 129.84(15) . 3_756 ?
C21 P2 Eu1 86.91(12) . 3_756 ?
N1 C1 C2 118.8(3) . . ?
N1 C1 C21 118.3(3) . . ?
C2 C1 C21 122.9(3) . . ?
C3 C2 C1 120.3(4) . . ?
C2 C3 C4 119.3(4) . . ?
C3 C4 C5 120.3(3) . . ?
N1 C5 C4 118.6(3) . . ?
N1 C5 C6 115.9(3) . . ?
C4 C5 C6 125.5(3) . . ?
N2 C6 C5 111.8(3) . . ?
O2 C7 N2 122.5(3) . . ?
O2 C7 C8 120.8(3) . . ?
N2 C7 C8 116.7(3) . . ?
C7 C8 P1 110.8(2) . . ?
C10 C9 C14 119.1(4) . . ?
C10 C9 P1 124.4(3) . . ?
C14 C9 P1 116.5(3) . . ?
C11 C10 C9 120.0(4) . . ?
C12 C11 C10 120.4(4) . . ?
C11 C12 C13 120.1(4) . . ?
C12 C13 C14 120.1(5) . . ?
C13 C14 C9 120.2(4) . . ?
C20 C15 C16 119.6(4) . . ?
C20 C15 P1 118.3(3) . . ?
C16 C15 P1 121.9(3) . . ?
C15 C16 C17 119.5(4) . . ?
C18 C17 C16 120.6(4) . . ?
C17 C18 C19 120.3(4) . . ?
C18 C19 C20 119.9(4) . . ?
C15 C20 C19 120.2(4) . . ?
C1 C21 P2 112.5(3) . . ?
C27 C22 C23 119.4(4) . . ?
C27 C22 P2 123.6(3) . . ?
C23 C22 P2 117.0(3) . . ?
C24 C23 C22 120.4(4) . . ?
C25 C24 C23 120.0(4) . . ?
C24 C25 C26 120.3(4) . . ?
C25 C26 C27 120.2(4) . . ?
C26 C27 C22 119.8(4) . . ?
C33 C28 C29 119.7(5) . . ?
C33 C28 P2 119.3(3) . . ?
C29 C28 P2 121.0(4) . . ?
C28 C29 C30 119.8(6) . . ?
C31 C30 C29 120.0(6) . . ?
C30 C31 C32 120.2(6) . . ?
C31 C32 C33 120.7(6) . . ?
C28 C33 C32 119.6(5) . . ?
C36 O14 Eu1 162.5(9) . . ?
C36 O15 C37 118.3 . . ?
O14 C36 O15 122.3 . . ?
O14 C36 C35 124.4 . . ?
O15 C36 C35 113.4 . . ?
C38 C37 O15 108.9 . . ?

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
Eu1 O1 N1 C1 -78.8(4) 3_756 . . . ?
Eu1 O1 N1 C5 105.3(3) 3_756 . . . ?
Eu1 O6 N3 O7 172.3(4) . . . . ?
Eu1 O6 N3 O5 -6.6(4) . . . . ?
Eu1 O5 N3 O7 -172.1(4) . . . . ?
Eu1 O5 N3 O6 6.9(4) . . . . ?
Eu1 O8 N4 O10 175.9(4) . . . . ?
Eu1 O8 N4 O9 -3.1(4) . . . . ?
Eu1 O9 N4 O10 -175.7(4) . . . . ?
Eu1 O9 N4 O8 3.3(4) . . . . ?
Eu1 O3 P1 C15 -117.4(2) . . . . ?
Eu1 O3 P1 C9 124.0(2) . . . . ?
Eu1 O3 P1 C8 2.0(3) . . . . ?
Eu1 O4 P2 C22 98.6(2) 3_756 . . . ?
Eu1 O4 P2 C28 -142.3(2) 3_756 . . . ?
Eu1 O4 P2 C21 -22.3(3) 3_756 . . . ?
O1 N1 C1 C2 -174.7(3) . . . . ?
C5 N1 C1 C2 1.0(5) . . . . ?
O1 N1 C1 C21 3.8(5) . . . . ?
C5 N1 C1 C21 179.5(3) . . . . ?
N1 C1 C2 C3 0.9(6) . . . . ?
C21 C1 C2 C3 -177.5(4) . . . . ?
C1 C2 C3 C4 -2.3(7) . . . . ?
C2 C3 C4 C5 1.9(6) . . . . ?
O1 N1 C5 C4 174.4(3) . . . . ?
C1 N1 C5 C4 -1.4(5) . . . . ?
O1 N1 C5 C6 -4.5(5) . . . . ?
C1 N1 C5 C6 179.8(3) . . . . ?
C3 C4 C5 N1 0.0(6) . . . . ?
C3 C4 C5 C6 178.7(4) . . . . ?
C7 N2 C6 C5 -101.4(4) . . . . ?
N1 C5 C6 N2 175.8(3) . . . . ?
C4 C5 C6 N2 -3.0(5) . . . . ?
Eu1 O2 C7 N2 -156.3(3) . . . . ?
Eu1 O2 C7 C8 23.1(5) . . . . ?
C6 N2 C7 O2 -1.0(5) . . . . ?
C6 N2 C7 C8 179.6(3) . . . . ?
O2 C7 C8 P1 -58.9(4) . . . . ?
N2 C7 C8 P1 120.5(3) . . . . ?
O3 P1 C8 C7 44.9(3) . . . . ?
C15 P1 C8 C7 166.6(3) . . . . ?
C9 P1 C8 C7 -78.3(3) . . . . ?
O3 P1 C9 C10 -131.6(3) . . . . ?
C15 P1 C9 C10 107.2(3) . . . . ?
C8 P1 C9 C10 -8.1(4) . . . . ?
O3 P1 C9 C14 49.5(3) . . . . ?
C15 P1 C9 C14 -71.7(3) . . . . ?
C8 P1 C9 C14 173.0(3) . . . . ?
C14 C9 C10 C11 -0.3(6) . . . . ?
P1 C9 C10 C11 -179.2(3) . . . . ?
C9 C10 C11 C12 -0.1(7) . . . . ?
C10 C11 C12 C13 0.4(7) . . . . ?
C11 C12 C13 C14 -0.3(8) . . . . ?
C12 C13 C14 C9 -0.1(8) . . . . ?
C10 C9 C14 C13 0.4(6) . . . . ?
P1 C9 C14 C13 179.3(4) . . . . ?
O3 P1 C15 C20 -12.9(4) . . . . ?
C9 P1 C15 C20 108.4(4) . . . . ?
C8 P1 C15 C20 -134.9(4) . . . . ?
O3 P1 C15 C16 172.2(4) . . . . ?
C9 P1 C15 C16 -66.5(4) . . . . ?
C8 P1 C15 C16 50.2(4) . . . . ?
C20 C15 C16 C17 0.7(8) . . . . ?
P1 C15 C16 C17 175.5(4) . . . . ?
C15 C16 C17 C18 -2.1(9) . . . . ?
C16 C17 C18 C19 2.3(9) . . . . ?
C17 C18 C19 C20 -1.0(8) . . . . ?
C16 C15 C20 C19 0.6(7) . . . . ?
P1 C15 C20 C19 -174.4(4) . . . . ?
C18 C19 C20 C15 -0.5(8) . . . . ?
N1 C1 C21 P2 81.4(4) . . . . ?
C2 C1 C21 P2 -100.2(4) . . . . ?
O4 P2 C21 C1 -66.1(3) . . . . ?
C22 P2 C21 C1 171.3(3) . . . . ?
C28 P2 C21 C1 55.1(3) . . . . ?
Eu1 P2 C21 C1 -76.0(3) 3_756 . . . ?
O4 P2 C22 C27 -157.5(4) . . . . ?
C28 P2 C22 C27 82.0(4) . . . . ?
C21 P2 C22 C27 -34.3(4) . . . . ?
Eu1 P2 C22 C27 -128.6(4) 3_756 . . . ?
O4 P2 C22 C23 24.9(4) . . . . ?
C28 P2 C22 C23 -95.6(4) . . . . ?
C21 P2 C22 C23 148.0(3) . . . . ?
Eu1 P2 C22 C23 53.8(4) 3_756 . . . ?
C27 C22 C23 C24 0.2(7) . . . . ?
P2 C22 C23 C24 178.0(4) . . . . ?
C22 C23 C24 C25 0.0(7) . . . . ?
C23 C24 C25 C26 -0.2(8) . . . . ?
C24 C25 C26 C27 0.2(9) . . . . ?
C25 C26 C27 C22 0.0(9) . . . . ?
C23 C22 C27 C26 -0.2(8) . . . . ?
P2 C22 C27 C26 -177.8(4) . . . . ?
O4 P2 C28 C33 12.9(4) . . . . ?
C22 P2 C28 C33 134.1(4) . . . . ?
C21 P2 C28 C33 -109.4(4) . . . . ?
Eu1 P2 C28 C33 -8.1(5) 3_756 . . . ?
O4 P2 C28 C29 -165.8(4) . . . . ?
C22 P2 C28 C29 -44.7(5) . . . . ?
C21 P2 C28 C29 71.8(5) . . . . ?
Eu1 P2 C28 C29 173.1(4) 3_756 . . . ?
C33 C28 C29 C30 -2.2(9) . . . . ?
P2 C28 C29 C30 176.6(5) . . . . ?
C28 C29 C30 C31 1.2(11) . . . . ?
C29 C30 C31 C32 0.4(11) . . . . ?
C30 C31 C32 C33 -1.0(10) . . . . ?
C29 C28 C33 C32 1.6(8) . . . . ?
P2 C28 C33 C32 -177.2(4) . . . . ?
C31 C32 C33 C28 0.0(9) . . . . ?
Eu1 O14 C36 O15 91.7(11) . . . . ?
Eu1 O14 C36 C35 -88.4(11) . . . . ?
C37 O15 C36 O14 -0.3 . . . . ?
C37 O15 C36 C35 179.8 . . . . ?
C36 O15 C37 C38 -175.7 . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C2 H2 O13 0.95 2.45 3.228(7) 138.9 4_666
C4 H4 O11 0.95 2.55 3.480(6) 167.0 1_655
C4 H4 O12 0.95 2.64 3.272(6) 124.6 1_655
C6 H6A O8 0.99 2.63 3.437(5) 139.2 3_756
C21 H21A O3 0.99 2.65 3.410(5) 133.4 3_756
C21 H21B O13 0.99 2.36 3.282(6) 155.3 4_666
C27 H27 O12 0.95 2.38 3.277(6) 156.4 4_666
O17 H17A O16 0.84 2.01 2.681(11) 136.7 .

_refine_diff_density_max         1.291
_refine_diff_density_min         -1.635
_refine_diff_density_rms         0.100

_shelxl_version_number           2013-3



_database_code_depnum_ccdc_archive 'CCDC 977752'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rprd648_0m_sq_s
_vrf_PLAT220_rprd648_0m_sq_s     
;
RESPONSE:  Disorder modeling did not improve structure quality
;
_vrf_PLAT415_rprd648_0m_sq_s     
;
RESPONSE: Partially occupied and/or disordered solvent molecules
;
_vrf_PLAT420_rprd648_0m_sq_s     
;
RESPONSE: Non-traditional hydrogen bonds to C-H groups may be present
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C137 H148 Dy3 N17 O52 P8'
_chemical_formula_weight         3599.98

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.1711(5)
_cell_length_b                   36.6811(13)
_cell_length_c                   28.7076(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17028.6(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7897
_cell_measurement_theta_min      2.98
_cell_measurement_theta_max      21.37

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_F_000             7292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.163
_exptl_absorpt_coefficient_mu    1.460
_shelx_estimated_absorpt_T_min   0.655
_shelx_estimated_absorpt_T_max   0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_T_max  0.80

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83047
_diffrn_reflns_av_unetI/netI     0.0961
_diffrn_reflns_av_R_equivalents  0.1087
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.049
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             17393
_reflns_number_gt                13208
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.864
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0681P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 5023 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.011(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         17393
_refine_ls_number_parameters     980
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1349
_refine_ls_wR_factor_gt          0.1209
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.24954(3) 0.31741(2) 0.47808(2) 0.02164(12) Uani 1 1 d . . . . .
Dy2 Dy 0.0000 0.39896(2) 0.2500 0.01967(16) Uani 1 2 d S T P . .
P1 P 0.14855(18) 0.34572(8) 0.18674(9) 0.0236(6) Uani 1 1 d . . . . .
P2 P 0.12382(18) 0.25328(8) 0.53782(9) 0.0231(6) Uani 1 1 d . . . . .
P3 P 0.1494(2) 0.38127(8) 0.55360(10) 0.0278(7) Uani 1 1 d . . . . .
P4 P 0.12017(19) 0.46874(8) 0.19424(9) 0.0250(7) Uani 1 1 d . . . . .
O1 O 0.1203(4) 0.3139(2) 0.4446(2) 0.0215(16) Uani 1 1 d . . . . .
O2 O 0.0604(4) 0.3442(2) 0.2848(2) 0.0211(16) Uani 1 1 d . . . . .
O3 O 0.0990(4) 0.3792(2) 0.1977(2) 0.0238(17) Uani 1 1 d . . . . .
O4 O 0.2045(4) 0.2658(2) 0.5183(3) 0.0242(16) Uani 1 1 d . . . . .
O5 O 0.1171(4) 0.41328(19) 0.2946(2) 0.0228(16) Uani 1 1 d . . . . .
O6 O 0.2077(5) 0.3757(2) 0.4474(2) 0.0251(17) Uani 1 1 d . . . . .
O7 O 0.1642(5) 0.3431(2) 0.5358(2) 0.0280(19) Uani 1 1 d . . . . .
O8 O 0.0397(4) 0.4500(2) 0.2042(2) 0.0244(17) Uani 1 1 d . . . . .
O9 O 0.2514(5) 0.26301(18) 0.4236(2) 0.0239(15) Uani 1 1 d . . . . .
O10 O 0.3586(4) 0.2698(2) 0.4684(2) 0.0271(17) Uani 1 1 d . . . . .
O11 O 0.3457(5) 0.2205(2) 0.4259(3) 0.0310(19) Uani 1 1 d . . . . .
O12 O 0.3472(4) 0.3635(2) 0.5114(3) 0.0265(18) Uani 1 1 d . . . . .
O13 O 0.3373(5) 0.3130(2) 0.5490(2) 0.0306(18) Uani 1 1 d . . . . .
O14 O 0.4278(5) 0.3546(2) 0.5705(3) 0.037(2) Uani 1 1 d . . . . .
O15 O 0.2950(7) 0.3929(4) 0.3560(4) 0.079(4) Uani 1 1 d . . . . .
O16 O 0.3383(10) 0.4421(4) 0.3293(6) 0.119(6) Uani 1 1 d . . . . .
O17 O 0.4227(8) 0.4038(4) 0.3631(6) 0.103(5) Uani 1 1 d . . . . .
O18 O 0.0177(5) 0.4804(2) 0.4717(3) 0.038(2) Uani 1 1 d . . . . .
O19 O 0.1343(8) 0.5000 0.5000 0.035(3) Uani 1 2 d S T P . .
N1 N 0.0846(5) 0.2845(3) 0.4269(3) 0.022(2) Uani 1 1 d . . . . .
N2 N 0.1468(6) 0.2988(2) 0.3050(3) 0.024(2) Uani 1 1 d . . . . .
H2A H 0.1770 0.2802 0.2959 0.029 Uiso 1 1 calc R U . . .
N3 N 0.1416(6) 0.4447(3) 0.3133(3) 0.028(2) Uani 1 1 d . . . . .
N4 N 0.1173(6) 0.4224(3) 0.4369(3) 0.024(2) Uani 1 1 d . . . . .
H4A H 0.0899 0.4402 0.4504 0.029 Uiso 1 1 calc R U . . .
N5 N 0.3191(6) 0.2496(3) 0.4387(3) 0.027(2) Uani 1 1 d . . . . .
N6 N 0.3730(6) 0.3439(3) 0.5453(4) 0.032(2) Uani 1 1 d . . . . .
N7 N 0.3522(9) 0.4126(4) 0.3528(6) 0.075(5) Uani 1 1 d . . . . .
N8 N 0.0584(9) 0.5000 0.5000 0.022(3) Uani 1 2 d S T P . .
C1 C 0.0430(6) 0.2609(3) 0.4552(4) 0.022(2) Uani 1 1 d . . . . .
C2 C 0.0062(8) 0.2307(3) 0.4372(4) 0.032(3) Uani 1 1 d . . . . .
H2 H -0.0232 0.2144 0.4570 0.038 Uiso 1 1 calc R U . . .
C3 C 0.0121(8) 0.2236(3) 0.3886(4) 0.038(3) Uani 1 1 d . . . . .
H3 H -0.0118 0.2023 0.3755 0.045 Uiso 1 1 calc R U . . .
C4 C 0.0538(7) 0.2486(3) 0.3608(4) 0.029(3) Uani 1 1 d . . . . .
H4 H 0.0570 0.2444 0.3282 0.035 Uiso 1 1 calc R U . . .
C5 C 0.0908(7) 0.2796(3) 0.3795(4) 0.026(3) Uani 1 1 d . . . . .
C6 C 0.1406(7) 0.3072(3) 0.3546(4) 0.026(3) Uani 1 1 d . . . . .
H6A H 0.1149 0.3315 0.3586 0.032 Uiso 1 1 calc R U . . .
H6B H 0.1968 0.3081 0.3683 0.032 Uiso 1 1 calc R U . . .
C7 C 0.1079(6) 0.3186(3) 0.2739(3) 0.021(2) Uani 1 1 d . . . . .
C8 C 0.1199(8) 0.3073(3) 0.2233(4) 0.026(3) Uani 1 1 d . . . . .
H8A H 0.0680 0.2964 0.2115 0.031 Uiso 1 1 calc R U . . .
H8B H 0.1637 0.2884 0.2215 0.031 Uiso 1 1 calc R U . . .
C9 C 0.1322(6) 0.3321(3) 0.1272(3) 0.023(2) Uani 1 1 d . . . . .
C10 C 0.1514(7) 0.2977(3) 0.1111(4) 0.029(3) Uani 1 1 d . . . . .
H10 H 0.1687 0.2793 0.1321 0.034 Uiso 1 1 calc R U . . .
C11 C 0.1453(7) 0.2904(4) 0.0638(4) 0.031(3) Uani 1 1 d . . . . .
H11 H 0.1565 0.2665 0.0525 0.037 Uiso 1 1 calc R U . . .
C12 C 0.1237(6) 0.3170(3) 0.0338(3) 0.026(2) Uani 1 1 d . . . . .
H12 H 0.1219 0.3117 0.0014 0.032 Uiso 1 1 calc R U . . .
C13 C 0.1038(7) 0.3517(3) 0.0490(4) 0.030(3) Uani 1 1 d . . . . .
H13 H 0.0873 0.3699 0.0273 0.036 Uiso 1 1 calc R U . . .
C14 C 0.1083(7) 0.3598(3) 0.0967(3) 0.026(3) Uani 1 1 d . . . . .
H14 H 0.0954 0.3835 0.1080 0.031 Uiso 1 1 calc R U . . .
C15 C 0.2567(8) 0.3548(3) 0.1948(4) 0.033(3) Uani 1 1 d . . . . .
C16 C 0.3133(9) 0.3511(6) 0.1595(5) 0.089(4) Uani 1 1 d . . . . .
H16 H 0.2979 0.3392 0.1313 0.107 Uiso 1 1 calc R U . . .
C17 C 0.3951(9) 0.3648(7) 0.1648(5) 0.089(4) Uani 1 1 d . . . . .
H17 H 0.4332 0.3639 0.1396 0.107 Uiso 1 1 calc R U . . .
C18 C 0.4173(9) 0.3792(7) 0.2065(5) 0.089(4) Uani 1 1 d . . . . .
H18 H 0.4721 0.3879 0.2108 0.107 Uiso 1 1 calc R U . . .
C19 C 0.3635(8) 0.3813(5) 0.2413(4) 0.062(5) Uani 1 1 d . . . . .
H19 H 0.3814 0.3911 0.2703 0.074 Uiso 1 1 calc R U . . .
C20 C 0.2821(7) 0.3696(4) 0.2371(4) 0.035(3) Uani 1 1 d . . . . .
H20 H 0.2447 0.3716 0.2625 0.042 Uiso 1 1 calc R U . . .
C21 C 0.0378(6) 0.2727(3) 0.5057(3) 0.026(3) Uani 1 1 d . . . . .
H21A H -0.0151 0.2643 0.5194 0.031 Uiso 1 1 calc R U . . .
H21B H 0.0396 0.2996 0.5077 0.031 Uiso 1 1 calc R U . . .
C22 C 0.1125(7) 0.2045(3) 0.5327(4) 0.031(3) Uani 1 1 d . . . . .
C23 C 0.1693(7) 0.1860(4) 0.5058(4) 0.036(3) Uani 1 1 d . . . . .
H23 H 0.2148 0.1982 0.4920 0.043 Uiso 1 1 calc R U . . .
C24 C 0.1573(9) 0.1477(4) 0.4994(5) 0.045(4) Uani 1 1 d . . . . .
H24 H 0.1969 0.1342 0.4820 0.053 Uiso 1 1 calc R U . . .
C25 C 0.0900(7) 0.1296(3) 0.5179(5) 0.039(3) Uani 1 1 d . . . . .
H25 H 0.0818 0.1044 0.5122 0.047 Uiso 1 1 calc R U . . .
C26 C 0.0342(9) 0.1492(4) 0.5453(5) 0.044(4) Uani 1 1 d . . . . .
H26 H -0.0112 0.1369 0.5593 0.053 Uiso 1 1 calc R U . . .
C27 C 0.0443(7) 0.1864(4) 0.5523(4) 0.035(3) Uani 1 1 d . . . . .
H27 H 0.0052 0.1996 0.5704 0.043 Uiso 1 1 calc R U . . .
C28 C 0.1121(7) 0.2667(3) 0.5979(3) 0.028(3) Uani 1 1 d . . . . .
C29 C 0.1863(8) 0.2740(4) 0.6227(4) 0.041(3) Uani 1 1 d . . . . .
H29 H 0.2388 0.2720 0.6081 0.049 Uiso 1 1 calc R U . . .
C30 C 0.1790(9) 0.2845(4) 0.6693(5) 0.053(4) Uani 1 1 d . . . . .
H30 H 0.2275 0.2902 0.6865 0.063 Uiso 1 1 calc R U . . .
C31 C 0.1032(10) 0.2867(5) 0.6908(5) 0.064(5) Uani 1 1 d . . . . .
H31 H 0.1006 0.2928 0.7229 0.077 Uiso 1 1 calc R U . . .
C32 C 0.0297(8) 0.2802(4) 0.6665(4) 0.051(4) Uani 1 1 d . . . . .
H32 H -0.0225 0.2827 0.6813 0.061 Uiso 1 1 calc R U . . .
C33 C 0.0354(8) 0.2695(4) 0.6188(4) 0.047(4) Uani 1 1 d . . . . .
H33 H -0.0133 0.2643 0.6015 0.056 Uiso 1 1 calc R U . . .
C34 C 0.1770(7) 0.4702(3) 0.2862(4) 0.028(3) Uani 1 1 d . . . . .
C35 C 0.2004(9) 0.5026(4) 0.3054(4) 0.043(3) Uani 1 1 d . . . . .
H35 H 0.2266 0.5204 0.2864 0.052 Uiso 1 1 calc R U . . .
C36 C 0.1866(9) 0.5099(4) 0.3519(4) 0.042(3) Uani 1 1 d . . . . .
H36 H 0.1962 0.5334 0.3647 0.050 Uiso 1 1 calc R U . . .
C37 C 0.1580(8) 0.4812(3) 0.3792(4) 0.036(3) Uani 1 1 d . . . . .
H37 H 0.1544 0.4843 0.4120 0.043 Uiso 1 1 calc R U . . .
C38 C 0.1354(7) 0.4492(3) 0.3603(4) 0.025(3) Uani 1 1 d . . . . .
C39 C 0.1052(7) 0.4156(3) 0.3874(3) 0.025(3) Uani 1 1 d . . . . .
H39A H 0.0459 0.4112 0.3809 0.030 Uiso 1 1 calc R U . . .
H39B H 0.1368 0.3937 0.3777 0.030 Uiso 1 1 calc R U . . .
C40 C 0.1700(7) 0.4019(3) 0.4625(3) 0.023(2) Uani 1 1 d . . . . .
C41 C 0.1854(7) 0.4147(3) 0.5118(3) 0.024(2) Uani 1 1 d . . . . .
H41A H 0.1563 0.4381 0.5170 0.029 Uiso 1 1 calc R U . . .
H41B H 0.2453 0.4190 0.5163 0.029 Uiso 1 1 calc R U . . .
C42 C 0.0415(8) 0.3890(3) 0.5627(4) 0.030(3) Uani 1 1 d . . . . .
C43 C 0.0104(8) 0.4258(3) 0.5640(4) 0.029(3) Uani 1 1 d . . . . .
H43 H 0.0475 0.4457 0.5606 0.035 Uiso 1 1 calc R U . . .
C44 C -0.0721(8) 0.4322(3) 0.5702(4) 0.031(3) Uani 1 1 d . . . . .
H44 H -0.0929 0.4565 0.5703 0.037 Uiso 1 1 calc R U . . .
C45 C -0.1258(8) 0.4025(4) 0.5764(4) 0.044(3) Uani 1 1 d . . . . .
H45 H -0.1833 0.4065 0.5805 0.052 Uiso 1 1 calc R U . . .
C46 C -0.0940(7) 0.3660(4) 0.5765(4) 0.033(3) Uani 1 1 d . . . . .
H46 H -0.1301 0.3459 0.5814 0.040 Uiso 1 1 calc R U . . .
C47 C -0.0135(8) 0.3605(3) 0.5696(4) 0.030(3) Uani 1 1 d . . . . .
H47 H 0.0069 0.3362 0.5695 0.036 Uiso 1 1 calc R U . . .
C48 C 0.2014(8) 0.3898(3) 0.6080(4) 0.033(3) Uani 1 1 d . . . . .
C49 C 0.1642(10) 0.3777(5) 0.6485(4) 0.058(4) Uani 1 1 d . . . . .
H49 H 0.1108 0.3670 0.6473 0.069 Uiso 1 1 calc R U . . .
C50 C 0.2045(12) 0.3813(6) 0.6905(5) 0.076(6) Uani 1 1 d . . . . .
H50 H 0.1794 0.3725 0.7183 0.091 Uiso 1 1 calc R U . . .
C51 C 0.2805(11) 0.3974(5) 0.6921(5) 0.068(5) Uani 1 1 d . . . . .
H51 H 0.3076 0.3998 0.7213 0.081 Uiso 1 1 calc R U . . .
C52 C 0.3189(10) 0.4101(5) 0.6526(5) 0.059(5) Uani 1 1 d . . . . .
H52 H 0.3712 0.4218 0.6548 0.071 Uiso 1 1 calc R U . . .
C53 C 0.2817(9) 0.4060(4) 0.6103(4) 0.044(4) Uani 1 1 d . . . . .
H53 H 0.3088 0.4138 0.5827 0.052 Uiso 1 1 calc R U . . .
C54 C 0.1993(8) 0.4597(3) 0.2370(4) 0.032(3) Uani 1 1 d . . . . .
H54A H 0.2124 0.4333 0.2364 0.038 Uiso 1 1 calc R U . . .
H54B H 0.2501 0.4730 0.2279 0.038 Uiso 1 1 calc R U . . .
C55 C 0.1673(7) 0.4561(3) 0.1394(4) 0.025(3) Uani 1 1 d . . . . .
C56 C 0.2449(9) 0.4415(3) 0.1359(4) 0.039(3) Uani 1 1 d . . . . .
H56 H 0.2771 0.4377 0.1631 0.047 Uiso 1 1 calc R U . . .
C57 C 0.2770(8) 0.4321(4) 0.0924(4) 0.042(4) Uani 1 1 d . . . . .
H57 H 0.3300 0.4211 0.0905 0.051 Uiso 1 1 calc R U . . .
C58 C 0.2329(8) 0.4386(4) 0.0520(4) 0.039(3) Uani 1 1 d . . . . .
H58 H 0.2554 0.4327 0.0224 0.047 Uiso 1 1 calc R U . . .
C59 C 0.1566(8) 0.4536(3) 0.0561(4) 0.033(3) Uani 1 1 d . . . . .
H59 H 0.1252 0.4577 0.0286 0.039 Uiso 1 1 calc R U . . .
C60 C 0.1224(7) 0.4632(3) 0.0988(4) 0.026(2) Uani 1 1 d . . . . .
H60 H 0.0695 0.4745 0.1003 0.031 Uiso 1 1 calc R U . . .
C61 C 0.1042(8) 0.5170(3) 0.1922(4) 0.034(3) Uani 1 1 d . . . . .
C62 C 0.1708(10) 0.5406(4) 0.1911(4) 0.049(4) Uani 1 1 d . . . . .
H62 H 0.2263 0.5321 0.1908 0.058 Uiso 1 1 calc R U . . .
C63 C 0.1503(15) 0.5801(4) 0.1903(5) 0.071(6) Uani 1 1 d . . . . .
H63 H 0.1935 0.5977 0.1898 0.086 Uiso 1 1 calc R U . . .
C64 C 0.0711(13) 0.5911(4) 0.1904(5) 0.058(5) Uani 1 1 d . . . . .
H64 H 0.0595 0.6165 0.1896 0.070 Uiso 1 1 calc R U . . .
C65 C 0.0102(13) 0.5683(4) 0.1915(5) 0.057(4) Uani 1 1 d . . . . .
H65 H -0.0449 0.5773 0.1918 0.069 Uiso 1 1 calc R U . . .
C66 C 0.0236(8) 0.5313(4) 0.1923(4) 0.041(3) Uani 1 1 d . . . . .
H66 H -0.0223 0.5152 0.1930 0.049 Uiso 1 1 calc R U . . .
O23 O 0.3278(5) 0.3332(2) 0.4115(3) 0.0311(19) Uani 1 1 d . . . . .
H23A H 0.3012 0.3360 0.3822 0.037 Uiso 1 1 calc R U . . .
H23B H 0.3858 0.3368 0.4140 0.037 Uiso 1 1 calc R U . . .
O24 O -0.1180(8) 0.2150(3) 0.6518(4) 0.071(3) Uani 1 1 d D . . . .
H24A H -0.1467 0.2321 0.6626 0.106 Uiso 1 1 calc DR U . . .
C67 C -0.0736(17) 0.1983(6) 0.6882(8) 0.155(13) Uani 1 1 d D . . . .
H67A H -0.0569 0.1738 0.6787 0.232 Uiso 1 1 calc R U . . .
H67B H -0.1087 0.1968 0.7160 0.232 Uiso 1 1 calc R U . . .
H67C H -0.0243 0.2129 0.6953 0.232 Uiso 1 1 calc R U . . .
O25 O 0.3398(9) 0.4373(4) -0.0568(5) 0.090(4) Uani 1 1 d . . . . .
H25A H 0.3736 0.4295 -0.0766 0.135 Uiso 1 1 calc R U . . .
C68 C 0.3156(12) 0.4709(4) -0.0688(7) 0.077(5) Uani 1 1 d . . . . .
H68A H 0.2557 0.4710 -0.0740 0.115 Uiso 1 1 calc R U . . .
H68B H 0.3439 0.4782 -0.0974 0.115 Uiso 1 1 calc R U . . .
H68C H 0.3293 0.4879 -0.0437 0.115 Uiso 1 1 calc R U . . .
O26 O 0.3662(10) 0.4623(5) 0.5025(7) 0.043(5) Uani 0.5 1 d . . P . .
H26A H 0.3369 0.4813 0.5022 0.065 Uiso 0.5 1 calc R U P . .
C69 C 0.375(2) 0.4484(8) 0.4551(10) 0.057(9) Uani 0.5 1 d . . P . .
H69A H 0.3377 0.4619 0.4343 0.085 Uiso 0.5 1 calc R U P . .
H69B H 0.3599 0.4225 0.4546 0.085 Uiso 0.5 1 calc R U P . .
H69C H 0.4319 0.4514 0.4447 0.085 Uiso 0.5 1 calc R U P . .
O27 O 0.4789(14) 0.4267(5) 0.5594(8) 0.141(7) Uiso 1 1 d D . . . .
H27A H 0.469(17) 0.408(5) 0.539(7) 0.212 Uiso 1 1 d D U . . .
H27B H 0.497(18) 0.415(6) 0.585(5) 0.212 Uiso 1 1 d D U . . .
N9 N 0.2676(8) 0.2135(5) 0.2894(5) 0.072(5) Uani 1 1 d . . . . .
O20 O 0.259(2) 0.1800(9) 0.2711(10) 0.073(3) Uani 0.362(12) 1 d . . P A 1
O21 O 0.324(2) 0.2131(11) 0.3149(13) 0.073(3) Uani 0.362(12) 1 d . . P A 1
O22 O 0.224(2) 0.2378(11) 0.2723(11) 0.073(3) Uani 0.362(12) 1 d . . P A 1
O20A O 0.2828(11) 0.2516(6) 0.2904(7) 0.073(3) Uani 0.638(12) 1 d . . P A 2
O21A O 0.3222(14) 0.1947(6) 0.2996(7) 0.073(3) Uani 0.638(12) 1 d . . P A 2
O22A O 0.2004(13) 0.2094(6) 0.2788(7) 0.073(3) Uani 0.638(12) 1 d . . P A 2


_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 2.304(7) . ?
Dy1 O4 2.332(7) . ?
Dy1 O7 2.353(7) . ?
Dy1 O23 2.365(7) . ?
Dy1 O6 2.411(7) . ?
Dy1 O13 2.487(7) . ?
Dy1 O10 2.498(7) . ?
Dy1 O12 2.502(7) . ?
Dy1 O9 2.535(6) . ?
Dy1 N6 2.941(11) . ?
Dy2 O3 2.311(7) . ?
Dy2 O3 2.311(7) 3 ?
Dy2 O5 2.346(7) 3 ?
Dy2 O5 2.347(7) . ?
Dy2 O8 2.378(7) . ?
Dy2 O8 2.378(7) 3 ?
Dy2 O2 2.446(7) 3 ?
Dy2 O2 2.446(7) . ?
P1 O3 1.499(8) . ?
P1 C15 1.796(13) . ?
P1 C9 1.800(10) . ?
P1 C8 1.819(11) . ?
P2 O4 1.493(7) . ?
P2 C28 1.803(11) . ?
P2 C22 1.805(13) . ?
P2 C21 1.814(10) . ?
P3 O7 1.509(8) . ?
P3 C42 1.786(13) . ?
P3 C48 1.801(12) . ?
P3 C41 1.814(11) . ?
P4 O8 1.498(8) . ?
P4 C61 1.789(12) . ?
P4 C54 1.804(12) . ?
P4 C55 1.809(12) . ?
O1 N1 1.324(11) . ?
O2 C7 1.255(13) . ?
O5 N3 1.331(11) . ?
O6 C40 1.216(13) . ?
O9 N5 1.275(11) . ?
O10 N5 1.297(11) . ?
O11 N5 1.210(12) . ?
O12 N6 1.277(12) . ?
O13 N6 1.277(13) . ?
O14 N6 1.210(12) . ?
O15 N7 1.178(16) . ?
O16 N7 1.293(18) . ?
O17 N7 1.222(16) . ?
O18 N8 1.271(10) . ?
O19 N8 1.228(16) . ?
N1 C1 1.364(13) . ?
N1 C5 1.378(13) . ?
N2 C7 1.309(13) . ?
N2 C6 1.458(13) . ?
N3 C34 1.346(14) . ?
N3 C38 1.364(13) . ?
N4 C40 1.354(13) . ?
N4 C39 1.455(13) . ?
N8 O18 1.270(10) 4_566 ?
C1 C2 1.359(15) . ?
C1 C21 1.516(14) . ?
C2 C3 1.421(14) . ?
C3 C4 1.389(16) . ?
C4 C5 1.392(15) . ?
C5 C6 1.479(15) . ?
C7 C8 1.524(13) . ?
C9 C10 1.380(15) . ?
C9 C14 1.396(15) . ?
C10 C11 1.387(15) . ?
C11 C12 1.347(17) . ?
C12 C13 1.386(16) . ?
C13 C14 1.405(14) . ?
C15 C16 1.373(18) . ?
C15 C20 1.394(15) . ?
C16 C17 1.42(2) . ?
C17 C18 1.36(2) . ?
C18 C19 1.329(19) . ?
C19 C20 1.390(17) . ?
C22 C23 1.379(17) . ?
C22 C27 1.405(16) . ?
C23 C24 1.430(18) . ?
C24 C25 1.380(18) . ?
C25 C26 1.395(19) . ?
C26 C27 1.389(18) . ?
C28 C33 1.382(17) . ?
C28 C29 1.421(17) . ?
C29 C30 1.396(18) . ?
C30 C31 1.38(2) . ?
C31 C32 1.398(19) . ?
C32 C33 1.428(17) . ?
C34 C35 1.363(17) . ?
C34 C54 1.507(15) . ?
C35 C36 1.381(17) . ?
C36 C37 1.390(16) . ?
C37 C38 1.345(16) . ?
C38 C39 1.539(15) . ?
C40 C41 1.511(14) . ?
C42 C47 1.387(16) . ?
C42 C43 1.441(15) . ?
C43 C44 1.367(17) . ?
C44 C45 1.406(18) . ?
C45 C46 1.434(19) . ?
C46 C47 1.331(16) . ?
C48 C49 1.382(19) . ?
C48 C53 1.428(19) . ?
C49 C50 1.379(19) . ?
C50 C51 1.36(2) . ?
C51 C52 1.38(2) . ?
C52 C53 1.363(16) . ?
C55 C56 1.368(18) . ?
C55 C60 1.400(15) . ?
C56 C57 1.396(16) . ?
C57 C58 1.380(18) . ?
C58 C59 1.356(17) . ?
C59 C60 1.390(15) . ?
C61 C62 1.382(18) . ?
C61 C66 1.406(17) . ?
C62 C63 1.49(2) . ?
C63 C64 1.34(2) . ?
C64 C65 1.29(2) . ?
C65 C66 1.375(18) . ?
O24 C67 1.406(17) . ?
O25 C68 1.335(19) . ?
O26 C69 1.46(3) . ?
N9 O22A 1.14(2) . ?
N9 O21A 1.16(2) . ?
N9 O21 1.17(4) . ?
N9 O22 1.24(4) . ?
N9 O20 1.34(3) . ?
N9 O20A 1.42(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 Dy1 O4 82.9(2) . . ?
O1 Dy1 O7 77.5(3) . . ?
O4 Dy1 O7 78.1(3) . . ?
O1 Dy1 O23 99.3(2) . . ?
O4 Dy1 O23 140.0(3) . . ?
O7 Dy1 O23 141.7(3) . . ?
O1 Dy1 O6 69.1(3) . . ?
O4 Dy1 O6 144.4(2) . . ?
O7 Dy1 O6 74.8(2) . . ?
O23 Dy1 O6 68.7(3) . . ?
O1 Dy1 O13 148.8(2) . . ?
O4 Dy1 O13 73.8(3) . . ?
O7 Dy1 O13 77.6(3) . . ?
O23 Dy1 O13 111.9(3) . . ?
O6 Dy1 O13 121.2(3) . . ?
O1 Dy1 O10 123.7(2) . . ?
O4 Dy1 O10 73.1(2) . . ?
O7 Dy1 O10 140.6(2) . . ?
O23 Dy1 O10 72.7(3) . . ?
O6 Dy1 O10 141.1(2) . . ?
O13 Dy1 O10 69.0(2) . . ?
O1 Dy1 O12 140.4(3) . . ?
O4 Dy1 O12 123.8(2) . . ?
O7 Dy1 O12 80.3(3) . . ?
O23 Dy1 O12 78.8(3) . . ?
O6 Dy1 O12 73.6(2) . . ?
O13 Dy1 O12 51.0(3) . . ?
O10 Dy1 O12 93.9(2) . . ?
O1 Dy1 O9 73.1(2) . . ?
O4 Dy1 O9 70.7(2) . . ?
O7 Dy1 O9 139.1(3) . . ?
O23 Dy1 O9 71.8(3) . . ?
O6 Dy1 O9 118.4(2) . . ?
O13 Dy1 O9 116.5(2) . . ?
O10 Dy1 O9 51.2(2) . . ?
O12 Dy1 O9 139.4(2) . . ?
O1 Dy1 N6 155.2(3) . . ?
O4 Dy1 N6 99.0(3) . . ?
O7 Dy1 N6 78.7(3) . . ?
O23 Dy1 N6 94.9(3) . . ?
O6 Dy1 N6 97.9(3) . . ?
O13 Dy1 N6 25.5(3) . . ?
O10 Dy1 N6 79.9(3) . . ?
O12 Dy1 N6 25.6(3) . . ?
O9 Dy1 N6 131.1(3) . . ?
O3 Dy2 O3 143.4(4) . 3 ?
O3 Dy2 O5 106.0(2) . 3 ?
O3 Dy2 O5 82.3(2) 3 3 ?
O3 Dy2 O5 82.3(2) . . ?
O3 Dy2 O5 106.0(2) 3 . ?
O5 Dy2 O5 154.1(3) 3 . ?
O3 Dy2 O8 72.6(3) . . ?
O3 Dy2 O8 142.5(3) 3 . ?
O5 Dy2 O8 74.9(2) 3 . ?
O5 Dy2 O8 84.7(2) . . ?
O3 Dy2 O8 142.5(3) . 3 ?
O3 Dy2 O8 72.6(3) 3 3 ?
O5 Dy2 O8 84.7(2) 3 3 ?
O5 Dy2 O8 74.9(2) . 3 ?
O8 Dy2 O8 76.0(3) . 3 ?
O3 Dy2 O2 75.8(3) . 3 ?
O3 Dy2 O2 74.4(2) 3 3 ?
O5 Dy2 O2 68.8(2) 3 3 ?
O5 Dy2 O2 136.8(2) . 3 ?
O8 Dy2 O2 121.9(2) . 3 ?
O8 Dy2 O2 139.9(2) 3 3 ?
O3 Dy2 O2 74.4(2) . . ?
O3 Dy2 O2 75.8(3) 3 . ?
O5 Dy2 O2 136.8(2) 3 . ?
O5 Dy2 O2 68.8(2) . . ?
O8 Dy2 O2 139.9(2) . . ?
O8 Dy2 O2 121.9(2) 3 . ?
O2 Dy2 O2 69.7(3) 3 . ?
O3 P1 C15 109.9(5) . . ?
O3 P1 C9 110.4(5) . . ?
C15 P1 C9 108.4(5) . . ?
O3 P1 C8 112.2(5) . . ?
C15 P1 C8 108.6(5) . . ?
C9 P1 C8 107.2(5) . . ?
O4 P2 C28 111.6(5) . . ?
O4 P2 C22 111.3(5) . . ?
C28 P2 C22 109.7(6) . . ?
O4 P2 C21 111.0(5) . . ?
C28 P2 C21 107.4(5) . . ?
C22 P2 C21 105.6(6) . . ?
O7 P3 C42 110.6(5) . . ?
O7 P3 C48 112.4(5) . . ?
C42 P3 C48 107.6(5) . . ?
O7 P3 C41 110.6(5) . . ?
C42 P3 C41 107.7(5) . . ?
C48 P3 C41 107.8(6) . . ?
O8 P4 C61 109.5(5) . . ?
O8 P4 C54 113.7(5) . . ?
C61 P4 C54 107.8(6) . . ?
O8 P4 C55 114.4(5) . . ?
C61 P4 C55 106.7(5) . . ?
C54 P4 C55 104.2(5) . . ?
N1 O1 Dy1 127.0(6) . . ?
C7 O2 Dy2 139.4(6) . . ?
P1 O3 Dy2 139.8(4) . . ?
P2 O4 Dy1 135.2(4) . . ?
N3 O5 Dy2 130.8(6) . . ?
C40 O6 Dy1 135.2(7) . . ?
P3 O7 Dy1 134.7(5) . . ?
P4 O8 Dy2 134.5(4) . . ?
N5 O9 Dy1 95.9(6) . . ?
N5 O10 Dy1 97.1(6) . . ?
N6 O12 Dy1 96.8(7) . . ?
N6 O13 Dy1 97.5(6) . . ?
O1 N1 C1 120.2(9) . . ?
O1 N1 C5 117.1(9) . . ?
C1 N1 C5 122.7(10) . . ?
C7 N2 C6 121.0(10) . . ?
O5 N3 C34 119.8(9) . . ?
O5 N3 C38 118.8(9) . . ?
C34 N3 C38 121.3(10) . . ?
C40 N4 C39 121.4(9) . . ?
O11 N5 O9 122.8(9) . . ?
O11 N5 O10 121.9(9) . . ?
O9 N5 O10 115.3(9) . . ?
O14 N6 O13 124.6(10) . . ?
O14 N6 O12 120.9(10) . . ?
O13 N6 O12 114.5(9) . . ?
O14 N6 Dy1 175.4(8) . . ?
O13 N6 Dy1 57.0(5) . . ?
O12 N6 Dy1 57.7(5) . . ?
O15 N7 O17 123.5(15) . . ?
O15 N7 O16 114.6(15) . . ?
O17 N7 O16 120.7(16) . . ?
O19 N8 O18 121.2(7) . 4_566 ?
O19 N8 O18 121.2(7) . . ?
O18 N8 O18 117.6(13) 4_566 . ?
C2 C1 N1 120.5(10) . . ?
C2 C1 C21 124.8(10) . . ?
N1 C1 C21 114.6(10) . . ?
C1 C2 C3 119.4(10) . . ?
C4 C3 C2 118.6(11) . . ?
C3 C4 C5 121.6(10) . . ?
N1 C5 C4 117.2(10) . . ?
N1 C5 C6 115.3(10) . . ?
C4 C5 C6 127.4(10) . . ?
N2 C6 C5 111.3(9) . . ?
O2 C7 N2 122.6(9) . . ?
O2 C7 C8 121.3(9) . . ?
N2 C7 C8 116.0(10) . . ?
C7 C8 P1 111.8(8) . . ?
C10 C9 C14 121.1(10) . . ?
C10 C9 P1 122.6(8) . . ?
C14 C9 P1 115.8(8) . . ?
C9 C10 C11 119.4(11) . . ?
C12 C11 C10 120.1(11) . . ?
C11 C12 C13 121.8(10) . . ?
C12 C13 C14 119.2(10) . . ?
C9 C14 C13 118.2(11) . . ?
C16 C15 C20 119.2(13) . . ?
C16 C15 P1 122.4(10) . . ?
C20 C15 P1 118.1(9) . . ?
C15 C16 C17 120.3(15) . . ?
C18 C17 C16 118.6(15) . . ?
C19 C18 C17 120.9(15) . . ?
C18 C19 C20 122.5(13) . . ?
C19 C20 C15 118.3(11) . . ?
C1 C21 P2 109.4(7) . . ?
C23 C22 C27 121.0(12) . . ?
C23 C22 P2 117.8(10) . . ?
C27 C22 P2 121.0(10) . . ?
C22 C23 C24 117.8(12) . . ?
C25 C24 C23 121.9(13) . . ?
C24 C25 C26 118.7(12) . . ?
C27 C26 C25 120.8(13) . . ?
C26 C27 C22 119.9(12) . . ?
C33 C28 C29 121.8(11) . . ?
C33 C28 P2 122.0(9) . . ?
C29 C28 P2 116.3(9) . . ?
C30 C29 C28 117.5(13) . . ?
C31 C30 C29 121.4(13) . . ?
C30 C31 C32 121.6(13) . . ?
C31 C32 C33 118.1(12) . . ?
C28 C33 C32 119.6(12) . . ?
N3 C34 C35 119.4(10) . . ?
N3 C34 C54 117.7(10) . . ?
C35 C34 C54 122.4(11) . . ?
C34 C35 C36 121.0(12) . . ?
C35 C36 C37 117.0(12) . . ?
C38 C37 C36 121.5(11) . . ?
C37 C38 N3 119.1(11) . . ?
C37 C38 C39 125.6(10) . . ?
N3 C38 C39 115.2(10) . . ?
N4 C39 C38 108.2(9) . . ?
O6 C40 N4 123.9(9) . . ?
O6 C40 C41 119.9(9) . . ?
N4 C40 C41 116.0(9) . . ?
C40 C41 P3 110.8(7) . . ?
C47 C42 C43 118.5(11) . . ?
C47 C42 P3 121.9(9) . . ?
C43 C42 P3 119.5(9) . . ?
C44 C43 C42 120.5(11) . . ?
C43 C44 C45 118.9(11) . . ?
C44 C45 C46 120.3(12) . . ?
C47 C46 C45 119.4(13) . . ?
C46 C47 C42 122.3(12) . . ?
C49 C48 C53 119.3(12) . . ?
C49 C48 P3 118.0(11) . . ?
C53 C48 P3 122.6(10) . . ?
C50 C49 C48 120.0(16) . . ?
C51 C50 C49 119.7(17) . . ?
C50 C51 C52 121.7(15) . . ?
C53 C52 C51 119.8(16) . . ?
C52 C53 C48 119.3(14) . . ?
C34 C54 P4 114.9(9) . . ?
C56 C55 C60 119.1(11) . . ?
C56 C55 P4 123.5(9) . . ?
C60 C55 P4 117.3(9) . . ?
C55 C56 C57 120.3(12) . . ?
C58 C57 C56 121.1(12) . . ?
C59 C58 C57 117.9(11) . . ?
C58 C59 C60 122.8(11) . . ?
C59 C60 C55 118.7(11) . . ?
C62 C61 C66 119.2(12) . . ?
C62 C61 P4 120.5(11) . . ?
C66 C61 P4 120.3(10) . . ?
C61 C62 C63 115.9(15) . . ?
C64 C63 C62 120.4(16) . . ?
C65 C64 C63 122.1(16) . . ?
C64 C65 C66 121.3(17) . . ?
C65 C66 C61 121.1(15) . . ?
O22A N9 O21A 136(3) . . ?
O21 N9 O22 135(3) . . ?
O21 N9 O20 108(3) . . ?
O22 N9 O20 117(3) . . ?
O22A N9 O20A 107.5(17) . . ?
O21A N9 O20A 117(2) . . ?

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
C15 P1 O3 Dy2 -116.8(7) . . . . ?
C9 P1 O3 Dy2 123.7(7) . . . . ?
C8 P1 O3 Dy2 4.1(8) . . . . ?
C28 P2 O4 Dy1 -92.1(7) . . . . ?
C22 P2 O4 Dy1 144.9(6) . . . . ?
C21 P2 O4 Dy1 27.6(8) . . . . ?
C42 P3 O7 Dy1 137.7(6) . . . . ?
C48 P3 O7 Dy1 -102.0(7) . . . . ?
C41 P3 O7 Dy1 18.5(8) . . . . ?
C61 P4 O8 Dy2 -141.3(6) . . . . ?
C54 P4 O8 Dy2 -20.6(8) . . . . ?
C55 P4 O8 Dy2 99.1(7) . . . . ?
Dy1 O1 N1 C1 84.5(10) . . . . ?
Dy1 O1 N1 C5 -96.5(9) . . . . ?
Dy2 O5 N3 C34 -77.6(12) . . . . ?
Dy2 O5 N3 C38 107.0(10) . . . . ?
Dy1 O9 N5 O11 174.0(8) . . . . ?
Dy1 O9 N5 O10 -7.2(8) . . . . ?
Dy1 O10 N5 O11 -173.9(8) . . . . ?
Dy1 O10 N5 O9 7.3(8) . . . . ?
Dy1 O13 N6 O14 -174.8(10) . . . . ?
Dy1 O13 N6 O12 3.8(9) . . . . ?
Dy1 O12 N6 O14 174.9(9) . . . . ?
Dy1 O12 N6 O13 -3.8(9) . . . . ?
O1 N1 C1 C2 179.9(10) . . . . ?
C5 N1 C1 C2 0.9(16) . . . . ?
O1 N1 C1 C21 3.6(13) . . . . ?
C5 N1 C1 C21 -175.4(9) . . . . ?
N1 C1 C2 C3 0.6(18) . . . . ?
C21 C1 C2 C3 176.6(11) . . . . ?
C1 C2 C3 C4 -1.7(19) . . . . ?
C2 C3 C4 C5 1.3(19) . . . . ?
O1 N1 C5 C4 179.6(9) . . . . ?
C1 N1 C5 C4 -1.3(16) . . . . ?
O1 N1 C5 C6 3.0(14) . . . . ?
C1 N1 C5 C6 -178.0(10) . . . . ?
C3 C4 C5 N1 0.2(17) . . . . ?
C3 C4 C5 C6 176.4(12) . . . . ?
C7 N2 C6 C5 109.0(12) . . . . ?
N1 C5 C6 N2 177.3(9) . . . . ?
C4 C5 C6 N2 1.1(17) . . . . ?
Dy2 O2 C7 N2 159.7(8) . . . . ?
Dy2 O2 C7 C8 -23.7(17) . . . . ?
C6 N2 C7 O2 -3.8(16) . . . . ?
C6 N2 C7 C8 179.4(10) . . . . ?
O2 C7 C8 P1 53.2(14) . . . . ?
N2 C7 C8 P1 -130.1(9) . . . . ?
O3 P1 C8 C7 -42.7(10) . . . . ?
C15 P1 C8 C7 79.0(9) . . . . ?
C9 P1 C8 C7 -164.0(8) . . . . ?
O3 P1 C9 C10 -162.3(9) . . . . ?
C15 P1 C9 C10 77.2(11) . . . . ?
C8 P1 C9 C10 -39.8(11) . . . . ?
O3 P1 C9 C14 25.3(10) . . . . ?
C15 P1 C9 C14 -95.2(9) . . . . ?
C8 P1 C9 C14 147.8(9) . . . . ?
C14 C9 C10 C11 -1.3(17) . . . . ?
P1 C9 C10 C11 -173.2(9) . . . . ?
C9 C10 C11 C12 2.3(17) . . . . ?
C10 C11 C12 C13 -2.5(18) . . . . ?
C11 C12 C13 C14 1.6(17) . . . . ?
C10 C9 C14 C13 0.4(17) . . . . ?
P1 C9 C14 C13 172.9(9) . . . . ?
C12 C13 C14 C9 -0.5(17) . . . . ?
O3 P1 C15 C16 -121.2(14) . . . . ?
C9 P1 C15 C16 -0.4(16) . . . . ?
C8 P1 C15 C16 115.7(15) . . . . ?
O3 P1 C15 C20 52.4(11) . . . . ?
C9 P1 C15 C20 173.2(10) . . . . ?
C8 P1 C15 C20 -70.6(11) . . . . ?
C20 C15 C16 C17 -5(3) . . . . ?
P1 C15 C16 C17 168.5(15) . . . . ?
C15 C16 C17 C18 5(3) . . . . ?
C16 C17 C18 C19 -2(4) . . . . ?
C17 C18 C19 C20 -1(3) . . . . ?
C18 C19 C20 C15 1(3) . . . . ?
C16 C15 C20 C19 2(2) . . . . ?
P1 C15 C20 C19 -171.4(11) . . . . ?
C2 C1 C21 P2 91.5(12) . . . . ?
N1 C1 C21 P2 -92.4(10) . . . . ?
O4 P2 C21 C1 60.1(9) . . . . ?
C28 P2 C21 C1 -177.7(8) . . . . ?
C22 P2 C21 C1 -60.7(9) . . . . ?
O4 P2 C22 C23 -10.4(11) . . . . ?
C28 P2 C22 C23 -134.4(9) . . . . ?
C21 P2 C22 C23 110.1(9) . . . . ?
O4 P2 C22 C27 174.6(9) . . . . ?
C28 P2 C22 C27 50.6(11) . . . . ?
C21 P2 C22 C27 -64.8(10) . . . . ?
C27 C22 C23 C24 -1.3(17) . . . . ?
P2 C22 C23 C24 -176.3(9) . . . . ?
C22 C23 C24 C25 2.3(19) . . . . ?
C23 C24 C25 C26 -3(2) . . . . ?
C24 C25 C26 C27 2.5(19) . . . . ?
C25 C26 C27 C22 -1.6(18) . . . . ?
C23 C22 C27 C26 1.0(17) . . . . ?
P2 C22 C27 C26 175.8(9) . . . . ?
O4 P2 C28 C33 157.7(11) . . . . ?
C22 P2 C28 C33 -78.4(12) . . . . ?
C21 P2 C28 C33 35.9(12) . . . . ?
O4 P2 C28 C29 -22.5(11) . . . . ?
C22 P2 C28 C29 101.4(10) . . . . ?
C21 P2 C28 C29 -144.3(9) . . . . ?
C33 C28 C29 C30 0(2) . . . . ?
P2 C28 C29 C30 180.0(11) . . . . ?
C28 C29 C30 C31 2(2) . . . . ?
C29 C30 C31 C32 -3(3) . . . . ?
C30 C31 C32 C33 3(3) . . . . ?
C29 C28 C33 C32 0(2) . . . . ?
P2 C28 C33 C32 179.9(11) . . . . ?
C31 C32 C33 C28 -1(2) . . . . ?
O5 N3 C34 C35 178.7(11) . . . . ?
C38 N3 C34 C35 -6.0(18) . . . . ?
O5 N3 C34 C54 -9.3(16) . . . . ?
C38 N3 C34 C54 166.1(11) . . . . ?
N3 C34 C35 C36 -1(2) . . . . ?
C54 C34 C35 C36 -173.1(13) . . . . ?
C34 C35 C36 C37 8(2) . . . . ?
C35 C36 C37 C38 -8(2) . . . . ?
C36 C37 C38 N3 0.7(19) . . . . ?
C36 C37 C38 C39 178.4(12) . . . . ?
O5 N3 C38 C37 -178.3(10) . . . . ?
C34 N3 C38 C37 6.4(17) . . . . ?
O5 N3 C38 C39 3.9(15) . . . . ?
C34 N3 C38 C39 -171.5(10) . . . . ?
C40 N4 C39 C38 -116.2(11) . . . . ?
C37 C38 C39 N4 -8.6(16) . . . . ?
N3 C38 C39 N4 169.1(9) . . . . ?
Dy1 O6 C40 N4 -143.9(8) . . . . ?
Dy1 O6 C40 C41 40.5(15) . . . . ?
C39 N4 C40 O6 -3.4(17) . . . . ?
C39 N4 C40 C41 172.4(9) . . . . ?
O6 C40 C41 P3 -67.3(12) . . . . ?
N4 C40 C41 P3 116.8(9) . . . . ?
O7 P3 C41 C40 36.2(9) . . . . ?
C42 P3 C41 C40 -84.7(9) . . . . ?
C48 P3 C41 C40 159.5(8) . . . . ?
O7 P3 C42 C47 22.6(10) . . . . ?
C48 P3 C42 C47 -100.5(10) . . . . ?
C41 P3 C42 C47 143.5(9) . . . . ?
O7 P3 C42 C43 -158.8(8) . . . . ?
C48 P3 C42 C43 78.1(10) . . . . ?
C41 P3 C42 C43 -37.9(10) . . . . ?
C47 C42 C43 C44 -2.5(16) . . . . ?
P3 C42 C43 C44 178.9(9) . . . . ?
C42 C43 C44 C45 1.6(17) . . . . ?
C43 C44 C45 C46 0.4(17) . . . . ?
C44 C45 C46 C47 -1.4(17) . . . . ?
C45 C46 C47 C42 0.5(17) . . . . ?
C43 C42 C47 C46 1.4(16) . . . . ?
P3 C42 C47 C46 -180.0(9) . . . . ?
O7 P3 C48 C49 -81.4(11) . . . . ?
C42 P3 C48 C49 40.5(12) . . . . ?
C41 P3 C48 C49 156.4(10) . . . . ?
O7 P3 C48 C53 93.8(10) . . . . ?
C42 P3 C48 C53 -144.2(10) . . . . ?
C41 P3 C48 C53 -28.3(11) . . . . ?
C53 C48 C49 C50 0(2) . . . . ?
P3 C48 C49 C50 175.2(13) . . . . ?
C48 C49 C50 C51 1(3) . . . . ?
C49 C50 C51 C52 0(3) . . . . ?
C50 C51 C52 C53 -2(3) . . . . ?
C51 C52 C53 C48 3(2) . . . . ?
C49 C48 C53 C52 -1.8(18) . . . . ?
P3 C48 C53 C52 -177.0(11) . . . . ?
N3 C34 C54 P4 91.7(12) . . . . ?
C35 C34 C54 P4 -96.5(13) . . . . ?
O8 P4 C54 C34 -58.2(10) . . . . ?
C61 P4 C54 C34 63.5(10) . . . . ?
C55 P4 C54 C34 176.6(9) . . . . ?
O8 P4 C55 C56 -122.2(10) . . . . ?
C61 P4 C55 C56 116.6(11) . . . . ?
C54 P4 C55 C56 2.7(12) . . . . ?
O8 P4 C55 C60 60.8(10) . . . . ?
C61 P4 C55 C60 -60.5(10) . . . . ?
C54 P4 C55 C60 -174.4(9) . . . . ?
C60 C55 C56 C57 -3.4(18) . . . . ?
P4 C55 C56 C57 179.6(10) . . . . ?
C55 C56 C57 C58 3(2) . . . . ?
C56 C57 C58 C59 -2(2) . . . . ?
C57 C58 C59 C60 1(2) . . . . ?
C58 C59 C60 C55 -2.3(18) . . . . ?
C56 C55 C60 C59 3.2(17) . . . . ?
P4 C55 C60 C59 -179.6(9) . . . . ?
O8 P4 C61 C62 169.4(9) . . . . ?
C54 P4 C61 C62 45.2(11) . . . . ?
C55 P4 C61 C62 -66.2(11) . . . . ?
O8 P4 C61 C66 -9.7(10) . . . . ?
C54 P4 C61 C66 -133.9(9) . . . . ?
C55 P4 C61 C66 114.6(9) . . . . ?
C66 C61 C62 C63 0.3(16) . . . . ?
P4 C61 C62 C63 -178.9(9) . . . . ?
C61 C62 C63 C64 -0.5(18) . . . . ?
C62 C63 C64 C65 1(2) . . . . ?
C63 C64 C65 C66 -1(2) . . . . ?
C64 C65 C66 C61 0(2) . . . . ?
C62 C61 C66 C65 -0.2(17) . . . . ?
P4 C61 C66 C65 179.0(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O22 0.88 1.86 2.73(3) 170.0 .
N2 H2A O20A 0.88 2.01 2.83(2) 154.2 .
N4 H4A O18 0.88 1.98 2.849(12) 171.0 .
N4 H4A N8 0.88 2.67 3.507(10) 160.6 .
O23 H23A O15 0.95 2.22 2.759(15) 115.0 .
O24 H24A O21 0.84 2.16 2.96(4) 157.9 8_456
O24 H24A O20A 0.84 1.87 2.61(2) 147.5 8_456
O25 H25A O27 0.84 2.44 2.96(3) 120.9 3_655
O27 H27A O14 0.90(3) 2.3(2) 2.79(2) 117(21) .

_refine_diff_density_max         1.197
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.129

_shelxl_version_number           2013-2
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.951 0.000 0.000 34 12 ' '
2 0.451 0.500 0.000 34 12 ' '
3 1.000 0.087 0.250 616 239 ' '
4 0.500 0.587 0.250 616 239 ' '
5 0.500 0.159 0.250 12 3 ' '
6 1.000 0.659 0.250 12 3 ' '
7 0.051 0.001 0.504 32 11 ' '
8 0.551 0.501 0.504 32 11 ' '
9 0.000 -0.087 0.750 615 239 ' '
10 0.500 0.413 0.750 615 239 ' '
11 0.000 0.341 0.750 12 3 ' '
12 0.500 0.841 0.750 12 3 ' '
_platon_squeeze_details          
;
TITL rprd648_0m in C222(1)
CELL   16.1711   36.6811   28.7076     90.00     90.00     90.00
SPGR C2221
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.500 0.258 0.753 !       5.85 eA-3
C102 0.330 0.363 0.815 !       3.31 eA-3
C103 0.027 0.023 0.652 !       3.16 eA-3
C104 0.533 0.484 0.186 !       2.72 eA-3
C105 0.381 0.499 0.231 !       2.60 eA-3
C106 0.341 0.358 0.868 !       2.59 eA-3
C107 0.108 0.015 0.749 !       2.31 eA-3
C108 0.091 0.201 0.221 !       2.28 eA-3
C109 0.848 0.102 0.137 !       2.03 eA-3
C110 0.987 0.039 0.360 !       1.94 eA-3
C111 0.548 0.417 0.719 !       1.92 eA-3
Q112 0.751 0.322 0.729 !       1.81 eA-3
C113 0.423 0.431 0.775 !       1.80 eA-3
C114 0.140 0.024 0.263 !       1.80 eA-3
Q115 0.124 0.782 0.799 !       1.77 eA-3
Q116 0.624 0.282 0.799 !       1.77 eA-3
C117 0.464 0.483 0.645 !       1.74 eA-3
C118 0.469 0.447 0.098 !       1.73 eA-3
C119 0.061 0.179 0.230 !       1.62 eA-3
C120 0.858 0.078 0.174 !       1.59 eA-3
C121 0.544 0.492 0.152 !       1.59 eA-3
C122 0.876 0.012 0.259 !       1.58 eA-3
C123 0.074 0.895 0.699 !       1.57 eA-3
C124 0.574 0.395 0.699 !       1.57 eA-3
C125 0.094 0.083 0.305 !       1.57 eA-3
C126 0.030 0.202 0.237 !       1.56 eA-3
C127 0.435 0.339 0.695 !       1.52 eA-3
C128 0.188 0.169 0.347 !       1.51 eA-3
C129 0.064 0.081 0.315 !       1.49 eA-3
Q130 0.488 0.428 0.200 !       1.47 eA-3
C131 0.422 0.328 0.706 !       1.47 eA-3
Q132 0.420 0.439 0.117 !       1.46 eA-3
C133 0.996 0.102 0.211 !       1.41 eA-3
Q134 0.458 0.445 0.149 !       1.40 eA-3
Q135 0.894 0.096 0.121 !       1.39 eA-3
Q136 0.874 0.006 0.676 !       1.39 eA-3
C137 0.924 0.023 0.276 !       1.38 eA-3
C138 0.589 0.470 0.418 !       1.38 eA-3
C139 0.357 0.342 0.888 !       1.38 eA-3
Q140 0.084 0.193 0.279 !       1.36 eA-3
C141 0.420 0.375 0.840 !       1.33 eA-3
Q142 0.409 0.444 0.058 !       1.31 eA-3
Q143 0.604 0.493 0.813 !       1.31 eA-3
Q144 0.792 0.165 0.206 !       1.29 eA-3
C145 0.501 0.366 0.696 !       1.28 eA-3
Q146 0.594 0.445 0.226 !       1.26 eA-3
C147 0.084 0.007 0.695 !       1.26 eA-3
Q148 0.505 0.266 0.295 !       1.25 eA-3
Q149 0.483 0.438 0.885 !       1.25 eA-3
C150 0.061 0.029 0.611 !       1.25 eA-3
C151 0.903 0.119 0.121 !       1.25 eA-3
C152 0.107 0.016 0.139 !       1.23 eA-3
C153 0.123 0.007 0.117 !       1.22 eA-3
C154 0.595 0.361 0.595 !       1.22 eA-3
Q155 1.000 0.102 0.750 !       1.21 eA-3
C156 1.000 0.070 0.755 !       1.21 eA-3
C157 0.392 0.366 0.811 !       1.21 eA-3
Q158 0.436 0.430 0.204 !       1.20 eA-3
Q159 0.546 0.275 0.320 !       1.20 eA-3
C160 0.469 0.280 0.774 !       1.19 eA-3
C161 0.497 0.314 0.791 !       1.19 eA-3
C162 0.949 0.173 0.233 !       1.18 eA-3
C163 0.470 0.460 0.066 !       1.17 eA-3
Q164 0.536 0.432 0.326 !       1.15 eA-3
Q165 0.592 0.279 0.834 !       1.14 eA-3
C166 0.374 0.321 0.862 !       1.14 eA-3
C167 0.989 0.026 0.327 !       1.14 eA-3
C168 0.597 0.499 0.786 !       1.13 eA-3
Q169 0.446 0.463 0.337 !       1.12 eA-3
C170 0.828 0.025 0.408 !       1.12 eA-3
Q171 0.091 0.020 0.860 !       1.11 eA-3
Q172 0.013 0.049 0.843 !       1.10 eA-3
Q173 0.123 0.008 0.791 !       1.10 eA-3
Q174 0.487 0.276 0.702 !       1.10 eA-3
Q175 0.467 0.454 0.372 !       1.09 eA-3
C176 0.527 0.375 0.772 !       1.09 eA-3
C177 0.467 0.480 0.882 !       1.08 eA-3
C178 0.582 0.265 0.805 !       1.07 eA-3
Q179 0.145 0.032 0.662 !       1.07 eA-3
C180 0.940 0.030 0.313 !       1.07 eA-3
C181 0.071 0.007 0.653 !       1.07 eA-3
Q182 0.949 0.031 0.625 !       1.06 eA-3
Q183 0.547 0.418 0.268 !       1.06 eA-3
C184 0.434 0.431 0.864 !       1.05 eA-3
Q185 0.221 0.360 0.878 !       1.05 eA-3
Q186 0.150 0.195 0.342 !       1.05 eA-3
Q187 0.143 0.032 0.147 !       1.05 eA-3
C188 0.943 0.031 0.970 !       1.04 eA-3
C189 0.606 0.462 0.461 !       1.04 eA-3
Q190 0.538 0.344 0.632 !       1.04 eA-3
C191 0.528 0.437 0.226 !       1.04 eA-3
Q192 0.896 0.127 0.717 !       1.03 eA-3
Q193 0.406 0.469 0.277 !       1.03 eA-3
Q194 0.408 0.490 0.398 !       1.03 eA-3
Q195 0.011 0.110 0.131 !       1.03 eA-3
Q196 0.878 0.190 0.179 !       1.03 eA-3
Q197 0.800 0.196 0.147 !       1.03 eA-3
Q198 0.077 0.040 0.498 !       1.02 eA-3
C199 0.843 0.179 0.127 !       1.02 eA-3
;

_database_code_depnum_ccdc_archive 'CCDC 977753'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rdsorp507_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H23 N2 O5 P'
_chemical_formula_weight         402.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.5148(4)
_cell_length_b                   10.5452(4)
_cell_length_c                   10.9891(4)
_cell_angle_alpha                67.994(2)
_cell_angle_beta                 85.172(2)
_cell_angle_gamma                81.411(2)
_cell_volume                     1010.32(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3524
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      26.08

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9576
_exptl_absorpt_correction_T_max  0.9635
_exptl_absorpt_process_details   'Bruker, SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15916
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         26.02
_reflns_number_total             3966
_reflns_number_gt                3037
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0594P)²+0.3267P] 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         3966
_refine_ls_number_parameters     268
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_ref         0.1149
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.020
_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
P1 P 0.15672(5) 1.05833(5) 0.72218(5) 0.02382(15) Uani 1 1 d . . .
N1 N -0.20157(18) 0.57918(16) 1.04152(16) 0.0275(4) Uani 1 1 d . . .
N2 N -0.18035(18) 0.93095(17) 0.80298(16) 0.0264(4) Uani 1 1 d . . .
H2A H -0.215(2) 1.007(2) 0.824(2) 0.040 Uiso 1 1 d . . .
O1 O -0.31849(16) 0.55670(15) 0.99945(15) 0.0376(4) Uani 1 1 d . . .
O2 O -0.02636(15) 0.83717(13) 0.68183(14) 0.0310(3) Uani 1 1 d . . .
O3 O 0.14995(15) 1.00669(14) 0.86788(13) 0.0324(3) Uani 1 1 d . . .
O4 O 0.41515(17) 0.61843(16) 0.09799(17) 0.0418(4) Uani 1 1 d D . .
H4A H 0.4978(13) 0.606(3) 0.069(3) 0.063 Uiso 1 1 d D . .
H4B H 0.369(2) 0.573(2) 0.071(3) 0.063 Uiso 1 1 d D . .
O5 O 0.2795(3) 0.8643(2) 0.10012(19) 0.0675(6) Uani 1 1 d D . .
H5A H 0.250(4) 0.905(3) 0.0252(17) 0.101 Uiso 1 1 d D . .
H5B H 0.319(4) 0.7867(18) 0.105(3) 0.101 Uiso 1 1 d D . .
C1 C -0.1287(2) 0.4771(2) 1.1396(2) 0.0329(5) Uani 1 1 d . . .
H1 H -0.1609 0.3891 1.1772 0.039 Uiso 1 1 calc R . .
C2 C -0.0089(2) 0.4999(2) 1.1849(2) 0.0339(5) Uani 1 1 d . . .
H2 H 0.0426 0.4277 1.2529 0.041 Uiso 1 1 calc R . .
C3 C 0.0370(2) 0.6289(2) 1.1309(2) 0.0321(5) Uani 1 1 d . . .
H3 H 0.1188 0.6467 1.1628 0.039 Uiso 1 1 calc R . .
C4 C -0.0384(2) 0.7312(2) 1.02995(19) 0.0281(4) Uani 1 1 d . . .
H4 H -0.0079 0.8200 0.9921 0.034 Uiso 1 1 calc R . .
C5 C -0.1569(2) 0.70566(19) 0.98399(19) 0.0247(4) Uani 1 1 d . . .
C6 C -0.2439(2) 0.8052(2) 0.8715(2) 0.0300(5) Uani 1 1 d . . .
H6A H -0.2544 0.7602 0.8088 0.036 Uiso 1 1 calc R . .
H6B H -0.3401 0.8288 0.9052 0.036 Uiso 1 1 calc R . .
C7 C -0.0741(2) 0.93518(19) 0.71412(18) 0.0245(4) Uani 1 1 d . . .
C8 C -0.0152(2) 1.07176(19) 0.65434(19) 0.0263(4) Uani 1 1 d . . .
H8A H -0.0821 1.1442 0.6730 0.032 Uiso 1 1 calc R . .
H8B H -0.0047 1.0983 0.5579 0.032 Uiso 1 1 calc R . .
C9 C 0.2098(2) 1.22909(19) 0.64940(19) 0.0248(4) Uani 1 1 d . . .
C10 C 0.1536(2) 1.3278(2) 0.5346(2) 0.0335(5) Uani 1 1 d . . .
H10 H 0.0847 1.3064 0.4899 0.040 Uiso 1 1 calc R . .
C11 C 0.1977(3) 1.4581(2) 0.4849(2) 0.0396(5) Uani 1 1 d . . .
H11 H 0.1587 1.5254 0.4064 0.048 Uiso 1 1 calc R . .
C12 C 0.2976(2) 1.4900(2) 0.5487(2) 0.0377(5) Uani 1 1 d . . .
H12 H 0.3272 1.5792 0.5144 0.045 Uiso 1 1 calc R . .
C13 C 0.3547(2) 1.3924(2) 0.6623(2) 0.0366(5) Uani 1 1 d . . .
H13 H 0.4242 1.4142 0.7059 0.044 Uiso 1 1 calc R . .
C14 C 0.3109(2) 1.2627(2) 0.7131(2) 0.0325(5) Uani 1 1 d . . .
H14 H 0.3500 1.1961 0.7920 0.039 Uiso 1 1 calc R . .
C15 C 0.2802(2) 0.94714(18) 0.66126(19) 0.0242(4) Uani 1 1 d . . .
C16 C 0.3544(2) 0.8308(2) 0.7513(2) 0.0309(5) Uani 1 1 d . . .
H16 H 0.3401 0.8117 0.8427 0.037 Uiso 1 1 calc R . .
C17 C 0.4496(2) 0.7424(2) 0.7075(2) 0.0352(5) Uani 1 1 d . . .
H17 H 0.5013 0.6636 0.7690 0.042 Uiso 1 1 calc R . .
C18 C 0.4689(2) 0.7691(2) 0.5751(2) 0.0335(5) Uani 1 1 d . . .
H18 H 0.5331 0.7078 0.5455 0.040 Uiso 1 1 calc R . .
C19 C 0.3951(2) 0.8853(2) 0.4843(2) 0.0332(5) Uani 1 1 d . . .
H19 H 0.4088 0.9033 0.3930 0.040 Uiso 1 1 calc R . .
C20 C 0.3016(2) 0.9745(2) 0.52728(19) 0.0279(4) Uani 1 1 d . . .
H20 H 0.2520 1.0546 0.4654 0.034 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
P1 O3 1.4845(14) . ?
P1 C15 1.8022(19) . ?
P1 C9 1.8062(19) . ?
P1 C8 1.819(2) . ?
N1 O1 1.325(2) . ?
N1 C1 1.355(3) . ?
N1 C5 1.361(2) . ?
N2 C7 1.339(3) . ?
N2 C6 1.451(2) . ?
N2 H2A 0.93(2) . ?
O2 C7 1.228(2) . ?
O4 H4A 0.834(10) . ?
O4 H4B 0.833(10) . ?
O5 H5A 0.825(10) . ?
O5 H5B 0.831(10) . ?
C1 C2 1.367(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.386(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.502(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.513(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.387(3) . ?
C9 C14 1.394(3) . ?
C10 C11 1.390(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.377(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.390(3) . ?
C15 C20 1.393(3) . ?
C16 C17 1.389(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.377(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?

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 P1 C15 111.91(8) . . ?
O3 P1 C9 112.73(9) . . ?
C15 P1 C9 107.20(9) . . ?
O3 P1 C8 112.03(9) . . ?
C15 P1 C8 107.16(9) . . ?
C9 P1 C8 105.38(9) . . ?
O1 N1 C1 120.03(16) . . ?
O1 N1 C5 118.70(16) . . ?
C1 N1 C5 121.27(18) . . ?
C7 N2 C6 120.93(17) . . ?
C7 N2 H2A 121.6(14) . . ?
C6 N2 H2A 117.5(14) . . ?
H4A O4 H4B 104.4(19) . . ?
H5A O5 H5B 108(2) . . ?
N1 C1 C2 120.44(18) . . ?
N1 C1 H1 119.8 . . ?
C2 C1 H1 119.8 . . ?
C1 C2 C3 119.7(2) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 118.9(2) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C5 C4 C3 120.63(18) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
N1 C5 C4 119.06(18) . . ?
N1 C5 C6 115.02(17) . . ?
C4 C5 C6 125.91(17) . . ?
N2 C6 C5 112.43(17) . . ?
N2 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
N2 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
O2 C7 N2 123.67(18) . . ?
O2 C7 C8 121.41(18) . . ?
N2 C7 C8 114.92(16) . . ?
C7 C8 P1 110.08(13) . . ?
C7 C8 H8A 109.6 . . ?
P1 C8 H8A 109.6 . . ?
C7 C8 H8B 109.6 . . ?
P1 C8 H8B 109.6 . . ?
H8A C8 H8B 108.2 . . ?
C10 C9 C14 118.94(18) . . ?
C10 C9 P1 123.08(16) . . ?
C14 C9 P1 117.98(15) . . ?
C9 C10 C11 120.1(2) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C12 C11 C10 120.4(2) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 119.9(2) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 120.2(2) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C9 120.4(2) . . ?
C13 C14 H14 119.8 . . ?
C9 C14 H14 119.8 . . ?
C16 C15 C20 119.74(18) . . ?
C16 C15 P1 118.57(15) . . ?
C20 C15 P1 121.69(15) . . ?
C17 C16 C15 119.98(19) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 C16 119.99(19) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.43(19) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C20 C19 C18 119.8(2) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C15 120.06(19) . . ?
C19 C20 H20 120.0 . . ?
C15 C20 H20 120.0 . . ?

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 N1 C1 C2 -179.13(17) . . . . ?
C5 N1 C1 C2 1.1(3) . . . . ?
N1 C1 C2 C3 0.8(3) . . . . ?
C1 C2 C3 C4 -1.4(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
O1 N1 C5 C4 177.87(16) . . . . ?
C1 N1 C5 C4 -2.4(3) . . . . ?
O1 N1 C5 C6 -3.2(2) . . . . ?
C1 N1 C5 C6 176.55(17) . . . . ?
C3 C4 C5 N1 1.8(3) . . . . ?
C3 C4 C5 C6 -177.07(19) . . . . ?
C7 N2 C6 C5 80.4(2) . . . . ?
N1 C5 C6 N2 -172.10(16) . . . . ?
C4 C5 C6 N2 6.8(3) . . . . ?
C6 N2 C7 O2 2.1(3) . . . . ?
C6 N2 C7 C8 -177.93(17) . . . . ?
O2 C7 C8 P1 -74.7(2) . . . . ?
N2 C7 C8 P1 105.37(17) . . . . ?
O3 P1 C8 C7 -54.22(15) . . . . ?
C15 P1 C8 C7 68.90(15) . . . . ?
C9 P1 C8 C7 -177.15(13) . . . . ?
O3 P1 C9 C10 -142.77(17) . . . . ?
C15 P1 C9 C10 93.64(18) . . . . ?
C8 P1 C9 C10 -20.28(19) . . . . ?
O3 P1 C9 C14 36.46(18) . . . . ?
C15 P1 C9 C14 -87.13(17) . . . . ?
C8 P1 C9 C14 158.95(15) . . . . ?
C14 C9 C10 C11 -0.1(3) . . . . ?
P1 C9 C10 C11 179.08(17) . . . . ?
C9 C10 C11 C12 0.2(3) . . . . ?
C10 C11 C12 C13 0.2(3) . . . . ?
C11 C12 C13 C14 -0.6(3) . . . . ?
C12 C13 C14 C9 0.6(3) . . . . ?
C10 C9 C14 C13 -0.2(3) . . . . ?
P1 C9 C14 C13 -179.49(16) . . . . ?
O3 P1 C15 C16 -0.61(19) . . . . ?
C9 P1 C15 C16 123.48(16) . . . . ?
C8 P1 C15 C16 -123.80(16) . . . . ?
O3 P1 C15 C20 178.83(15) . . . . ?
C9 P1 C15 C20 -57.08(18) . . . . ?
C8 P1 C15 C20 55.64(18) . . . . ?
C20 C15 C16 C17 0.0(3) . . . . ?
P1 C15 C16 C17 179.50(16) . . . . ?
C15 C16 C17 C18 -0.9(3) . . . . ?
C16 C17 C18 C19 0.9(3) . . . . ?
C17 C18 C19 C20 0.0(3) . . . . ?
C18 C19 C20 C15 -0.8(3) . . . . ?
C16 C15 C20 C19 0.8(3) . . . . ?
P1 C15 C20 C19 -178.64(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O5 0.93(2) 1.85(2) 2.762(2) 169(2) 2_576
O4 H4A O1 0.834(10) 1.927(11) 2.756(2) 172(3) 1_654
O4 H4B O1 0.833(10) 1.941(13) 2.749(2) 163(2) 2_566
O5 H5A O3 0.825(10) 1.903(11) 2.719(2) 170(4) 1_554
O5 H5B O4 0.831(10) 1.898(11) 2.726(2) 174(3) .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.053
_iucr_refine_instruction_details 
;
TITL rdsorp507_0m in P-1
CELL 0.71073 9.5148 10.5452 10.9891 67.994 85.172 81.411
ZERR 2.00 0.0004 0.0004 0.0004 0.002 0.002 0.002
LATT 1
SFAC C  H  N  O  P
UNIT 40  46  4  10  2
OMIT -1 0 1
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN 5
SIZE 0.221 0.223 0.258
CONF
EQIV $1 -x, -y+2, -z+1
EQIV $2 x+1, y, z-1
EQIV $3 -x, -y+1, -z+1
EQIV $4 x, y, z-1
HTAB N2 O5_$1
HTAB O4 O1_$2
HTAB O4 O1_$3
HTAB O5 O3_$4
HTAB O5 O4
DANG 1.312545 0.020000 H4a H4b
DANG 1.312545 0.020000 H5a H5b
DFIX 0.830000 0.010000 O4 H4A
DFIX 0.830000 0.010000 O4 H4B
DFIX 0.830000 0.010000 O5 H5A
DFIX 0.830000 0.010000 O5 H5B
TEMP -100.150
WGHT    0.059400    0.326700
FVAR       0.24361
P1    5    0.156718    1.058325    0.722184    11.00000    0.02676    0.02167 =
         0.02199   -0.00791   -0.00065   -0.00028
N1    3   -0.201568    0.579175    1.041521    11.00000    0.02846    0.02704 =
         0.03036   -0.01424    0.00779   -0.00844
N2    3   -0.180351    0.930952    0.802980    11.00000    0.02805    0.02298 =
         0.02710   -0.00825    0.00004   -0.00285
H2A   2   -0.214707    1.007013    0.824439    11.00000   -1.50000
O1    4   -0.318487    0.556703    0.999449    11.00000    0.03158    0.03723 =
         0.04982   -0.01998    0.00440   -0.01426
O2    4   -0.026356    0.837166    0.681826    11.00000    0.03447    0.02520 =
         0.03384   -0.01332    0.00214   -0.00082
O3    4    0.149951    1.006692    0.867877    11.00000    0.03911    0.03211 =
         0.02284   -0.00875   -0.00073    0.00114
O4    4    0.415145    0.618430    0.097986    11.00000    0.03580    0.04128 =
         0.05722   -0.03015   -0.00883    0.00411
H4A   2    0.497791    0.606388    0.068920    11.00000   -1.50000
H4B   2    0.369302    0.572989    0.071349    11.00000   -1.50000
O5    4    0.279505    0.864311    0.100121    11.00000    0.10589    0.05118 =
         0.04916   -0.03288   -0.03683    0.03618
H5A   2    0.249590    0.905186    0.025231    11.00000   -1.50000
H5B   2    0.318947    0.786724    0.105143    11.00000   -1.50000
C1    1   -0.128657    0.477113    1.139607    11.00000    0.04477    0.02249 =
         0.02910   -0.00827    0.00893   -0.00641
AFIX  43
H1    2   -0.160932    0.389118    1.177209    11.00000   -1.20000
AFIX   0
C2    1   -0.008905    0.499895    1.184862    11.00000    0.04277    0.02972 =
         0.02614   -0.00894    0.00100   -0.00022
AFIX  43
H2    2    0.042573    0.427687    1.252916    11.00000   -1.20000
AFIX   0
C3    1    0.037008    0.628879    1.130946    11.00000    0.03508    0.03480 =
         0.02769   -0.01307   -0.00026   -0.00437
AFIX  43
H3    2    0.118827    0.646722    1.162756    11.00000   -1.20000
AFIX   0
C4    1   -0.038413    0.731245    1.029950    11.00000    0.03291    0.02635 =
         0.02666   -0.01120    0.00259   -0.00657
AFIX  43
H4    2   -0.007945    0.820026    0.992067    11.00000   -1.20000
AFIX   0
C5    1   -0.156893    0.705664    0.983991    11.00000    0.02779    0.02384 =
         0.02418   -0.01169    0.00667   -0.00465
C6    1   -0.243927    0.805177    0.871525    11.00000    0.02909    0.02987 =
         0.03089   -0.01037    0.00131   -0.00664
AFIX  23
H6A   2   -0.254447    0.760208    0.808834    11.00000   -1.20000
H6B   2   -0.340089    0.828769    0.905213    11.00000   -1.20000
AFIX   0
C7    1   -0.074124    0.935184    0.714116    11.00000    0.02387    0.02462 =
         0.02388   -0.00783   -0.00425   -0.00099
C8    1   -0.015210    1.071757    0.654342    11.00000    0.02828    0.02204 =
         0.02552   -0.00681    0.00030    0.00029
AFIX  23
H8A   2   -0.082062    1.144202    0.672954    11.00000   -1.20000
H8B   2   -0.004704    1.098280    0.557886    11.00000   -1.20000
AFIX   0
C9    1    0.209827    1.229090    0.649396    11.00000    0.02469    0.02490 =
         0.02741   -0.01378    0.00193   -0.00154
C10   1    0.153576    1.327835    0.534627    11.00000    0.03412    0.02718 =
         0.03880   -0.00938   -0.00974   -0.00498
AFIX  43
H10   2    0.084744    1.306426    0.489935    11.00000   -1.20000
AFIX   0
C11   1    0.197748    1.458051    0.484903    11.00000    0.04269    0.02726 =
         0.04469   -0.00676   -0.00825   -0.00521
AFIX  43
H11   2    0.158730    1.525397    0.406394    11.00000   -1.20000
AFIX   0
C12   1    0.297633    1.489992    0.548696    11.00000    0.04008    0.02984 =
         0.04913   -0.02057    0.00646   -0.01056
AFIX  43
H12   2    0.327228    1.579237    0.514426    11.00000   -1.20000
AFIX   0
C13   1    0.354652    1.392387    0.662317    11.00000    0.03520    0.04666 =
         0.03922   -0.02632    0.00273   -0.01337
AFIX  43
H13   2    0.424248    1.414190    0.705928    11.00000   -1.20000
AFIX   0
C14   1    0.310915    1.262710    0.713143    11.00000    0.03386    0.03883 =
         0.02811   -0.01605   -0.00042   -0.00514
AFIX  43
H14   2    0.350024    1.196143    0.791996    11.00000   -1.20000
AFIX   0
C15   1    0.280208    0.947143    0.661260    11.00000    0.02389    0.02190 =
         0.02773   -0.01011   -0.00142   -0.00293
C16   1    0.354416    0.830804    0.751302    11.00000    0.03349    0.02725 =
         0.02808   -0.00739   -0.00095    0.00046
AFIX  43
H16   2    0.340076    0.811724    0.842746    11.00000   -1.20000
AFIX   0
C17   1    0.449576    0.742422    0.707527    11.00000    0.03039    0.02503 =
         0.04480   -0.00893   -0.00182    0.00260
AFIX  43
H17   2    0.501296    0.663583    0.768991    11.00000   -1.20000
AFIX   0
C18   1    0.468899    0.769119    0.575080    11.00000    0.02683    0.03107 =
         0.04877   -0.02318    0.00510   -0.00341
AFIX  43
H18   2    0.533068    0.707812    0.545507    11.00000   -1.20000
AFIX   0
C19   1    0.395074    0.885284    0.484264    11.00000    0.02942    0.04224 =
         0.03426   -0.02153    0.00232   -0.00572
AFIX  43
H19   2    0.408805    0.903261    0.392960    11.00000   -1.20000
AFIX   0
C20   1    0.301630    0.974527    0.527284    11.00000    0.02553    0.02957 =
         0.02787   -0.01002   -0.00400   -0.00077
AFIX  43
H20   2    0.252003    1.054573    0.465430    11.00000   -1.20000
HKLF 4 1 1 0 0 0 1 0 0 0 1
 
REM  rdsorp507_0m in P-1
REM R1 =  0.0395 for   3037 Fo > 4sig(Fo)  and  0.0589 for all   3966 data
REM    268 parameters refined using      6 restraints
 
END  
     
WGHT      0.0594      0.3267 
REM Highest difference peak  0.642,  deepest hole -0.272,  1-sigma level  0.053
Q1    1  -0.5007  0.9963  0.9373  11.00000  0.05    0.64
Q2    1   0.1766  1.1544  0.6840  11.00000  0.05    0.25
Q3    1   0.2279  1.0070  0.6879  11.00000  0.05    0.24
Q4    1   0.0613  1.0666  0.6791  11.00000  0.05    0.23
Q5    1  -0.3208  0.4735  1.0267  11.00000  0.05    0.18
;
_database_code_depnum_ccdc_archive 'CCDC 977754'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rpso481_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H30 N2 O4 P2'
_chemical_formula_weight         580.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   14.8196(13)
_cell_length_b                   12.6867(10)
_cell_length_c                   16.4438(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.425(5)
_cell_angle_gamma                90.00
_cell_volume                     2915.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    4511
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      26.01

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1216
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9362
_exptl_absorpt_correction_T_max  0.9716
_exptl_absorpt_process_details   'Bruker, SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27090
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.10
_reflns_number_total             6400
_reflns_number_gt                4673
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0505P)²+1.0373P] 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         6400
_refine_ls_number_parameters     373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1135
_refine_ls_wR_factor_gt          0.0994
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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
P1 P 0.05291(3) 0.26947(4) 0.41044(3) 0.02307(13) Uani 1 1 d . . .
P2 P 0.72345(3) 0.20839(4) 0.72299(3) 0.01975(13) Uani 1 1 d . . .
N1 N 0.48414(11) 0.36786(12) 0.60243(10) 0.0199(3) Uani 1 1 d . . .
H2A H 0.2395(14) 0.4132(16) 0.3907(14) 0.024 Uiso 1 1 d . . .
N2 N 0.24830(11) 0.43322(13) 0.44419(11) 0.0241(4) Uani 1 1 d . . .
O1 O 0.51889(10) 0.46355(10) 0.61421(9) 0.0295(3) Uani 1 1 d . . .
O2 O 0.17532(10) 0.47323(12) 0.54165(9) 0.0355(4) Uani 1 1 d . . .
O3 O 0.12705(10) 0.19938(11) 0.39721(9) 0.0290(3) Uani 1 1 d . . .
O4 O 0.69867(9) 0.10899(10) 0.75955(8) 0.0248(3) Uani 1 1 d . . .
C1 C 0.53778(13) 0.28540(15) 0.64701(12) 0.0222(4) Uani 1 1 d . . .
C2 C 0.49705(15) 0.18692(16) 0.63712(15) 0.0326(5) Uani 1 1 d . . .
H2 H 0.5326 0.1295 0.6692 0.039 Uiso 1 1 calc R . .
C3 C 0.40499(16) 0.16985(16) 0.58121(16) 0.0362(6) Uani 1 1 d . . .
H3 H 0.3777 0.1013 0.5748 0.043 Uiso 1 1 calc R . .
C4 C 0.35348(14) 0.25357(16) 0.53501(14) 0.0282(5) Uani 1 1 d . . .
H4 H 0.2908 0.2426 0.4955 0.034 Uiso 1 1 calc R . .
C5 C 0.39301(13) 0.35316(15) 0.54617(12) 0.0209(4) Uani 1 1 d . . .
C6 C 0.34494(13) 0.45200(15) 0.50227(13) 0.0244(4) Uani 1 1 d . . .
H6A H 0.3428 0.5038 0.5466 0.029 Uiso 1 1 calc R . .
H6B H 0.3834 0.4830 0.4693 0.029 Uiso 1 1 calc R . .
C7 C 0.17161(14) 0.44221(16) 0.46995(13) 0.0253(4) Uani 1 1 d . . .
C8 C 0.07773(14) 0.40891(16) 0.40323(13) 0.0272(5) Uani 1 1 d . . .
H8A H 0.0799 0.4243 0.3449 0.033 Uiso 1 1 calc R . .
H8B H 0.0250 0.4508 0.4114 0.033 Uiso 1 1 calc R . .
C9 C -0.06369(14) 0.25000(17) 0.33123(13) 0.0270(5) Uani 1 1 d . . .
C10 C -0.13912(15) 0.3196(2) 0.32231(14) 0.0365(5) Uani 1 1 d . . .
H10 H -0.1291 0.3820 0.3561 0.044 Uiso 1 1 calc R . .
C11 C -0.22897(16) 0.2973(2) 0.26368(16) 0.0480(7) Uani 1 1 d . . .
H11 H -0.2804 0.3450 0.2569 0.058 Uiso 1 1 calc R . .
C12 C -0.24390(17) 0.2067(2) 0.21542(15) 0.0482(7) Uani 1 1 d . . .
H12 H -0.3056 0.1921 0.1755 0.058 Uiso 1 1 calc R . .
C13 C -0.16984(17) 0.1364(2) 0.22433(14) 0.0411(6) Uani 1 1 d . . .
H13 H -0.1808 0.0734 0.1912 0.049 Uiso 1 1 calc R . .
C14 C -0.07946(16) 0.15834(17) 0.28186(13) 0.0309(5) Uani 1 1 d . . .
H14 H -0.0282 0.1108 0.2876 0.037 Uiso 1 1 calc R . .
C15 C 0.03630(13) 0.24443(17) 0.51217(13) 0.0269(5) Uani 1 1 d . . .
C16 C 0.05594(17) 0.1428(2) 0.54474(16) 0.0418(6) Uani 1 1 d . . .
H16 H 0.0803 0.0919 0.5151 0.050 Uiso 1 1 calc R . .
C17 C 0.0401(2) 0.1159(3) 0.62041(18) 0.0583(8) Uani 1 1 d . . .
H17 H 0.0532 0.0463 0.6425 0.070 Uiso 1 1 calc R . .
C18 C 0.00547(19) 0.1894(3) 0.66361(17) 0.0636(9) Uani 1 1 d . . .
H18 H -0.0048 0.1706 0.7158 0.076 Uiso 1 1 calc R . .
C19 C -0.01435(18) 0.2897(3) 0.63200(17) 0.0559(8) Uani 1 1 d . . .
H19 H -0.0380 0.3404 0.6624 0.067 Uiso 1 1 calc R . .
C20 C -0.00006(16) 0.3175(2) 0.55589(15) 0.0399(6) Uani 1 1 d . . .
H20 H -0.0152 0.3867 0.5335 0.048 Uiso 1 1 calc R . .
C21 C 0.63612(13) 0.31270(15) 0.70664(13) 0.0221(4) Uani 1 1 d . . .
H21A H 0.6315 0.3328 0.7633 0.026 Uiso 1 1 calc R . .
H21B H 0.6594 0.3751 0.6833 0.026 Uiso 1 1 calc R . .
C22 C 0.83502(13) 0.26095(15) 0.79379(12) 0.0214(4) Uani 1 1 d . . .
C23 C 0.85523(15) 0.36748(17) 0.80672(15) 0.0347(5) Uani 1 1 d . . .
H23 H 0.8102 0.4184 0.7751 0.042 Uiso 1 1 calc R . .
C24 C 0.94177(17) 0.39928(18) 0.86622(18) 0.0475(7) Uani 1 1 d . . .
H24 H 0.9546 0.4723 0.8768 0.057 Uiso 1 1 calc R . .
C25 C 1.00915(16) 0.32643(18) 0.91002(16) 0.0407(6) Uani 1 1 d . . .
H25 H 1.0684 0.3491 0.9501 0.049 Uiso 1 1 calc R . .
C26 C 0.99041(15) 0.22028(17) 0.89553(14) 0.0313(5) Uani 1 1 d . . .
H26 H 1.0373 0.1697 0.9247 0.038 Uiso 1 1 calc R . .
C27 C 0.90325(14) 0.18746(16) 0.83858(13) 0.0250(4) Uani 1 1 d . . .
H27 H 0.8899 0.1143 0.8300 0.030 Uiso 1 1 calc R . .
C28 C 0.73947(13) 0.18593(15) 0.62023(12) 0.0225(4) Uani 1 1 d . . .
C29 C 0.75717(15) 0.08347(17) 0.59860(14) 0.0314(5) Uani 1 1 d . . .
H29 H 0.7571 0.0266 0.6361 0.038 Uiso 1 1 calc R . .
C30 C 0.77491(16) 0.0649(2) 0.52209(16) 0.0402(6) Uani 1 1 d . . .
H30 H 0.7867 -0.0049 0.5073 0.048 Uiso 1 1 calc R . .
C31 C 0.77559(16) 0.1466(2) 0.46767(15) 0.0406(6) Uani 1 1 d . . .
H31 H 0.7882 0.1332 0.4156 0.049 Uiso 1 1 calc R . .
C32 C 0.75799(16) 0.2484(2) 0.48827(15) 0.0384(6) Uani 1 1 d . . .
H32 H 0.7581 0.3048 0.4502 0.046 Uiso 1 1 calc R . .
C33 C 0.74030(15) 0.26817(17) 0.56427(13) 0.0295(5) Uani 1 1 d . . .
H33 H 0.7286 0.3383 0.5785 0.035 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
P1 O3 1.4847(14) . ?
P1 C15 1.798(2) . ?
P1 C9 1.802(2) . ?
P1 C8 1.819(2) . ?
P2 O4 1.4945(14) . ?
P2 C22 1.8037(19) . ?
P2 C28 1.805(2) . ?
P2 C21 1.8075(19) . ?
N1 O1 1.308(2) . ?
N1 C1 1.370(2) . ?
N1 C5 1.372(2) . ?
N2 C7 1.343(3) . ?
N2 C6 1.453(2) . ?
N2 H2A 0.88(2) . ?
O2 C7 1.227(2) . ?
C1 C2 1.374(3) . ?
C1 C21 1.502(3) . ?
C2 C3 1.385(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.503(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.517(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C14 1.393(3) . ?
C9 C10 1.394(3) . ?
C10 C11 1.389(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.372(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.387(3) . ?
C15 C16 1.389(3) . ?
C16 C17 1.384(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.371(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.369(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.382(4) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.385(3) . ?
C22 C27 1.392(3) . ?
C23 C24 1.389(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.375(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.380(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.384(3) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C33 1.394(3) . ?
C28 C29 1.395(3) . ?
C29 C30 1.388(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.372(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.382(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.382(3) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?

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 P1 C15 111.55(9) . . ?
O3 P1 C9 112.99(9) . . ?
C15 P1 C9 104.67(9) . . ?
O3 P1 C8 113.41(9) . . ?
C15 P1 C8 109.02(10) . . ?
C9 P1 C8 104.62(10) . . ?
O4 P2 C22 110.33(8) . . ?
O4 P2 C28 111.70(9) . . ?
C22 P2 C28 106.55(9) . . ?
O4 P2 C21 114.70(9) . . ?
C22 P2 C21 106.42(9) . . ?
C28 P2 C21 106.67(9) . . ?
O1 N1 C1 119.99(15) . . ?
O1 N1 C5 118.48(15) . . ?
C1 N1 C5 121.52(16) . . ?
C7 N2 C6 122.10(17) . . ?
C7 N2 H2A 118.6(14) . . ?
C6 N2 H2A 119.3(14) . . ?
N1 C1 C2 118.52(17) . . ?
N1 C1 C21 115.97(16) . . ?
C2 C1 C21 125.44(17) . . ?
C1 C2 C3 121.18(19) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 H2 119.4 . . ?
C4 C3 C2 119.19(19) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 119.97(18) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N1 C5 C4 119.57(17) . . ?
N1 C5 C6 114.41(16) . . ?
C4 C5 C6 126.02(17) . . ?
N2 C6 C5 112.65(16) . . ?
N2 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
N2 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
O2 C7 N2 123.93(18) . . ?
O2 C7 C8 121.43(19) . . ?
N2 C7 C8 114.64(18) . . ?
C7 C8 P1 112.35(14) . . ?
C7 C8 H8A 109.1 . . ?
P1 C8 H8A 109.1 . . ?
C7 C8 H8B 109.1 . . ?
P1 C8 H8B 109.1 . . ?
H8A C8 H8B 107.9 . . ?
C14 C9 C10 119.65(19) . . ?
C14 C9 P1 118.07(16) . . ?
C10 C9 P1 122.14(17) . . ?
C11 C10 C9 119.6(2) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C12 C11 C10 120.3(2) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.6(2) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 119.7(2) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 H13 120.2 . . ?
C13 C14 C9 120.1(2) . . ?
C13 C14 H14 119.9 . . ?
C9 C14 H14 119.9 . . ?
C20 C15 C16 119.2(2) . . ?
C20 C15 P1 124.13(18) . . ?
C16 C15 P1 116.54(18) . . ?
C17 C16 C15 120.0(3) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 C16 120.2(3) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C19 C18 C17 120.4(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C18 C19 C20 120.2(3) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C19 C20 C15 120.1(3) . . ?
C19 C20 H20 119.9 . . ?
C15 C20 H20 119.9 . . ?
C1 C21 P2 114.81(13) . . ?
C1 C21 H21A 108.6 . . ?
P2 C21 H21A 108.6 . . ?
C1 C21 H21B 108.6 . . ?
P2 C21 H21B 108.6 . . ?
H21A C21 H21B 107.5 . . ?
C23 C22 C27 119.35(18) . . ?
C23 C22 P2 124.38(15) . . ?
C27 C22 P2 116.26(15) . . ?
C22 C23 C24 119.55(19) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C25 C24 C23 120.9(2) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 119.7(2) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C27 119.98(19) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C22 120.45(19) . . ?
C26 C27 H27 119.8 . . ?
C22 C27 H27 119.8 . . ?
C33 C28 C29 119.03(19) . . ?
C33 C28 P2 122.17(15) . . ?
C29 C28 P2 118.68(16) . . ?
C30 C29 C28 119.8(2) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C31 C30 C29 120.5(2) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C32 120.2(2) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C33 119.9(2) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C32 C33 C28 120.5(2) . . ?
C32 C33 H33 119.8 . . ?
C28 C33 H33 119.8 . . ?

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 N1 C1 C2 176.08(19) . . . . ?
C5 N1 C1 C2 -2.7(3) . . . . ?
O1 N1 C1 C21 -1.0(3) . . . . ?
C5 N1 C1 C21 -179.77(17) . . . . ?
N1 C1 C2 C3 2.2(3) . . . . ?
C21 C1 C2 C3 179.0(2) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C2 C3 C4 C5 -1.4(4) . . . . ?
O1 N1 C5 C4 -177.66(18) . . . . ?
C1 N1 C5 C4 1.1(3) . . . . ?
O1 N1 C5 C6 1.8(3) . . . . ?
C1 N1 C5 C6 -179.48(17) . . . . ?
C3 C4 C5 N1 1.0(3) . . . . ?
C3 C4 C5 C6 -178.4(2) . . . . ?
C7 N2 C6 C5 92.2(2) . . . . ?
N1 C5 C6 N2 -179.25(16) . . . . ?
C4 C5 C6 N2 0.1(3) . . . . ?
C6 N2 C7 O2 5.0(3) . . . . ?
C6 N2 C7 C8 -174.07(17) . . . . ?
O2 C7 C8 P1 -89.7(2) . . . . ?
N2 C7 C8 P1 89.33(19) . . . . ?
O3 P1 C8 C7 -60.05(17) . . . . ?
C15 P1 C8 C7 64.89(17) . . . . ?
C9 P1 C8 C7 176.40(15) . . . . ?
O3 P1 C9 C14 16.1(2) . . . . ?
C15 P1 C9 C14 -105.43(18) . . . . ?
C8 P1 C9 C14 139.96(17) . . . . ?
O3 P1 C9 C10 -168.27(18) . . . . ?
C15 P1 C9 C10 70.2(2) . . . . ?
C8 P1 C9 C10 -44.4(2) . . . . ?
C14 C9 C10 C11 -0.6(3) . . . . ?
P1 C9 C10 C11 -176.15(19) . . . . ?
C9 C10 C11 C12 0.8(4) . . . . ?
C10 C11 C12 C13 -0.1(4) . . . . ?
C11 C12 C13 C14 -0.7(4) . . . . ?
C12 C13 C14 C9 0.9(3) . . . . ?
C10 C9 C14 C13 -0.2(3) . . . . ?
P1 C9 C14 C13 175.53(17) . . . . ?
O3 P1 C15 C20 156.13(17) . . . . ?
C9 P1 C15 C20 -81.4(2) . . . . ?
C8 P1 C15 C20 30.1(2) . . . . ?
O3 P1 C15 C16 -28.13(19) . . . . ?
C9 P1 C15 C16 94.38(18) . . . . ?
C8 P1 C15 C16 -154.15(16) . . . . ?
C20 C15 C16 C17 -0.6(3) . . . . ?
P1 C15 C16 C17 -176.58(19) . . . . ?
C15 C16 C17 C18 -0.4(4) . . . . ?
C16 C17 C18 C19 0.5(4) . . . . ?
C17 C18 C19 C20 0.3(4) . . . . ?
C18 C19 C20 C15 -1.3(4) . . . . ?
C16 C15 C20 C19 1.5(3) . . . . ?
P1 C15 C20 C19 177.11(18) . . . . ?
N1 C1 C21 P2 -151.11(15) . . . . ?
C2 C1 C21 P2 32.0(3) . . . . ?
O4 P2 C21 C1 -59.20(17) . . . . ?
C22 P2 C21 C1 178.51(14) . . . . ?
C28 P2 C21 C1 65.04(16) . . . . ?
O4 P2 C22 C23 -145.10(19) . . . . ?
C28 P2 C22 C23 93.5(2) . . . . ?
C21 P2 C22 C23 -20.1(2) . . . . ?
O4 P2 C22 C27 33.76(18) . . . . ?
C28 P2 C22 C27 -87.67(17) . . . . ?
C21 P2 C22 C27 158.78(16) . . . . ?
C27 C22 C23 C24 -2.2(4) . . . . ?
P2 C22 C23 C24 176.67(19) . . . . ?
C22 C23 C24 C25 2.5(4) . . . . ?
C23 C24 C25 C26 -0.7(4) . . . . ?
C24 C25 C26 C27 -1.5(4) . . . . ?
C25 C26 C27 C22 1.8(3) . . . . ?
C23 C22 C27 C26 0.0(3) . . . . ?
P2 C22 C27 C26 -178.88(17) . . . . ?
O4 P2 C28 C33 164.43(15) . . . . ?
C22 P2 C28 C33 -75.01(18) . . . . ?
C21 P2 C28 C33 38.36(18) . . . . ?
O4 P2 C28 C29 -19.42(18) . . . . ?
C22 P2 C28 C29 101.14(17) . . . . ?
C21 P2 C28 C29 -145.49(16) . . . . ?
C33 C28 C29 C30 -0.2(3) . . . . ?
P2 C28 C29 C30 -176.50(16) . . . . ?
C28 C29 C30 C31 0.3(3) . . . . ?
C29 C30 C31 C32 -0.4(3) . . . . ?
C30 C31 C32 C33 0.4(3) . . . . ?
C31 C32 C33 C28 -0.4(3) . . . . ?
C29 C28 C33 C32 0.3(3) . . . . ?
P2 C28 C33 C32 176.43(16) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O4 0.88(2) 2.06(2) 2.926(2) 168.2(19) 4_565

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.10
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.055
_iucr_refine_instruction_details 
;
TITL rpso481_0m in P2(1)/n
CELL 0.71073 14.8196 12.6867 16.4438 90.000 109.425 90.000
ZERR 4.00 0.0013 0.0010 0.0014 0.000 0.005 0.000
LATT 1
SYMM -x+1/2, y+1/2, -z+1/2
SFAC C H N O P
UNIT 132 120 8 16 8
TEMP -100.150
SIZE 0.152 0.236 0.351
ACTA
OMIT     2   0   0
OMIT    -1   1   2
OMIT     2   1   0
OMIT    -2   1   2
OMIT     1   1   1
OMIT    -2   0   2
OMIT    -1   1   1
OMIT    -2   1   1
OMIT     1   0   1
OMIT    -1   0   3
L.S. 10
FMAP 2
PLAN 10
BOND $H
CONF
EQIV $1 x-1/2, -y+1/2, z-1/2
HTAB N2 O4_$1
WGHT    0.050500    1.037300
FVAR       0.06715
P1    5    0.052907    0.269474    0.410444    11.00000    0.01713    0.02792 =
         0.02227   -0.00203    0.00402   -0.00056
P2    5    0.723453    0.208387    0.722986    11.00000    0.01835    0.01799 =
         0.02107    0.00068    0.00409    0.00066
N1    3    0.484138    0.367864    0.602435    11.00000    0.01900    0.01827 =
         0.02179   -0.00088    0.00586   -0.00208
H2A   2    0.239511    0.413174    0.390668    11.00000   -1.20000
N2    3    0.248297    0.433223    0.444191    11.00000    0.02060    0.02671 =
         0.02030   -0.00074    0.00070   -0.00067
O1    4    0.518889    0.463550    0.614215    11.00000    0.02622    0.01737 =
         0.03640    0.00205   -0.00101   -0.00698
O2    4    0.175322    0.473229    0.541645    11.00000    0.03150    0.04586 =
         0.02691   -0.00741    0.00678   -0.00219
O3    4    0.127054    0.199385    0.397215    11.00000    0.02399    0.03195 =
         0.03127   -0.00415    0.00930    0.00172
O4    4    0.698666    0.108990    0.759553    11.00000    0.02665    0.02051 =
         0.02481    0.00123    0.00530   -0.00260
C1    1    0.537781    0.285403    0.647006    11.00000    0.01972    0.02077 =
         0.02528   -0.00107    0.00654    0.00072
C2    1    0.497051    0.186918    0.637121    11.00000    0.02688    0.02010 =
         0.04400    0.00166    0.00258    0.00139
AFIX  43
H2    2    0.532648    0.129479    0.669201    11.00000   -1.20000
AFIX   0
C3    1    0.404994    0.169847    0.581208    11.00000    0.02729    0.01981 =
         0.05320   -0.00091    0.00239   -0.00508
AFIX  43
H3    2    0.377680    0.101315    0.574767    11.00000   -1.20000
AFIX   0
C4    1    0.353481    0.253572    0.535006    11.00000    0.01997    0.02484 =
         0.03454   -0.00334    0.00212   -0.00282
AFIX  43
H4    2    0.290805    0.242635    0.495515    11.00000   -1.20000
AFIX   0
C5    1    0.393005    0.353161    0.546168    11.00000    0.01725    0.02360 =
         0.02105   -0.00153    0.00550   -0.00167
C6    1    0.344938    0.452002    0.502272    11.00000    0.01961    0.02261 =
         0.02628    0.00031    0.00154   -0.00219
AFIX  23
H6A   2    0.342765    0.503813    0.546603    11.00000   -1.20000
H6B   2    0.383441    0.482951    0.469275    11.00000   -1.20000
AFIX   0
C7    1    0.171614    0.442208    0.469945    11.00000    0.02312    0.02248 =
         0.02649    0.00253    0.00309   -0.00022
C8    1    0.077728    0.408906    0.403226    11.00000    0.02161    0.02954 =
         0.02648   -0.00006    0.00282    0.00052
AFIX  23
H8A   2    0.079937    0.424304    0.344897    11.00000   -1.20000
H8B   2    0.025021    0.450812    0.411357    11.00000   -1.20000
AFIX   0
C9    1   -0.063695    0.250000    0.331226    11.00000    0.01993    0.03882 =
         0.02085   -0.00038    0.00505   -0.00453
C10   1   -0.139119    0.319616    0.322310    11.00000    0.02372    0.05347 =
         0.02931   -0.00395    0.00487    0.00249
AFIX  43
H10   2   -0.129130    0.381969    0.356149    11.00000   -1.20000
AFIX   0
C11   1   -0.228974    0.297330    0.263677    11.00000    0.02187    0.07684 =
         0.03914   -0.00472    0.00191    0.00505
AFIX  43
H11   2   -0.280358    0.345045    0.256943    11.00000   -1.20000
AFIX   0
C12   1   -0.243902    0.206729    0.215420    11.00000    0.02774    0.08108 =
         0.02858   -0.00183   -0.00041   -0.01293
AFIX  43
H12   2   -0.305645    0.192145    0.175532    11.00000   -1.20000
AFIX   0
C13   1   -0.169837    0.136409    0.224326    11.00000    0.03982    0.05518 =
         0.02698   -0.00803    0.00946   -0.01992
AFIX  43
H13   2   -0.180844    0.073435    0.191200    11.00000   -1.20000
AFIX   0
C14   1   -0.079460    0.158343    0.281859    11.00000    0.03030    0.03682 =
         0.02648   -0.00150    0.01074   -0.00827
AFIX  43
H14   2   -0.028212    0.110755    0.287605    11.00000   -1.20000
AFIX   0
C15   1    0.036303    0.244427    0.512169    11.00000    0.01474    0.03911 =
         0.02406    0.00025    0.00266   -0.00194
C16   1    0.055945    0.142849    0.544741    11.00000    0.03606    0.04985 =
         0.03982    0.01050    0.01307    0.00235
AFIX  43
H16   2    0.080272    0.091883    0.515101    11.00000   -1.20000
AFIX   0
C17   1    0.040053    0.115923    0.620410    11.00000    0.04682    0.07525 =
         0.04995    0.02775    0.01234   -0.00527
AFIX  43
H17   2    0.053151    0.046307    0.642472    11.00000   -1.20000
AFIX   0
C18   1    0.005472    0.189411    0.663611    11.00000    0.03125    0.12847 =
         0.03109    0.01345    0.01028   -0.01327
AFIX  43
H18   2   -0.004797    0.170641    0.715776    11.00000   -1.20000
AFIX   0
C19   1   -0.014351    0.289714    0.631996    11.00000    0.03334    0.10459 =
         0.03293   -0.01384    0.01526   -0.00388
AFIX  43
H19   2   -0.037981    0.340366    0.662426    11.00000   -1.20000
AFIX   0
C20   1   -0.000060    0.317460    0.555890    11.00000    0.03105    0.05808 =
         0.03195   -0.00724    0.01238    0.00264
AFIX  43
H20   2   -0.015178    0.386697    0.533494    11.00000   -1.20000
AFIX   0
C21   1    0.636122    0.312698    0.706642    11.00000    0.01936    0.01962 =
         0.02607   -0.00170    0.00606    0.00078
AFIX  23
H21A  2    0.631524    0.332766    0.763312    11.00000   -1.20000
H21B  2    0.659373    0.375055    0.683286    11.00000   -1.20000
AFIX   0
C22   1    0.835022    0.260947    0.793786    11.00000    0.01948    0.02109 =
         0.02228    0.00114    0.00496    0.00222
C23   1    0.855230    0.367482    0.806721    11.00000    0.02597    0.02137 =
         0.04633    0.00464   -0.00181    0.00032
AFIX  43
H23   2    0.810218    0.418447    0.775121    11.00000   -1.20000
AFIX   0
C24   1    0.941773    0.399278    0.866224    11.00000    0.03398    0.02317 =
         0.06825    0.00322   -0.00605   -0.00650
AFIX  43
H24   2    0.954575    0.472299    0.876799    11.00000   -1.20000
AFIX   0
C25   1    1.009152    0.326431    0.910016    11.00000    0.02367    0.03685 =
         0.05028    0.00274   -0.00295   -0.00333
AFIX  43
H25   2    1.068370    0.349117    0.950083    11.00000   -1.20000
AFIX   0
C26   1    0.990411    0.220281    0.895532    11.00000    0.02187    0.03162 =
         0.03438    0.00416    0.00150    0.00436
AFIX  43
H26   2    1.037338    0.169744    0.924654    11.00000   -1.20000
AFIX   0
C27   1    0.903254    0.187456    0.838583    11.00000    0.02415    0.02020 =
         0.02948    0.00134    0.00719    0.00260
AFIX  43
H27   2    0.889868    0.114282    0.829984    11.00000   -1.20000
AFIX   0
C28   1    0.739465    0.185928    0.620227    11.00000    0.01635    0.02546 =
         0.02377   -0.00200    0.00407   -0.00079
C29   1    0.757171    0.083475    0.598598    11.00000    0.02820    0.02939 =
         0.03747   -0.00282    0.01211    0.00089
AFIX  43
H29   2    0.757086    0.026574    0.636129    11.00000   -1.20000
AFIX   0
C30   1    0.774913    0.064900    0.522091    11.00000    0.03146    0.04585 =
         0.04724   -0.01758    0.01820   -0.00252
AFIX  43
H30   2    0.786677   -0.004933    0.507316    11.00000   -1.20000
AFIX   0
C31   1    0.775585    0.146624    0.467665    11.00000    0.02826    0.06537 =
         0.03134   -0.01263    0.01419   -0.00625
AFIX  43
H31   2    0.788190    0.133183    0.415627    11.00000   -1.20000
AFIX   0
C32   1    0.757992    0.248437    0.488269    11.00000    0.03502    0.05233 =
         0.02844    0.00513    0.01139   -0.00521
AFIX  43
H32   2    0.758055    0.304798    0.450250    11.00000   -1.20000
AFIX   0
C33   1    0.740301    0.268172    0.564267    11.00000    0.02788    0.03254 =
         0.02700    0.00109    0.00771    0.00095
AFIX  43
H33   2    0.728630    0.338288    0.578458    11.00000   -1.20000
 
HKLF 4 1 1 0 0 0 1 0 0 0 1
 
REM  rpso481_0m in P2(1)/n
REM R1 =  0.0423 for   4673 Fo > 4sig(Fo)  and  0.0681 for all   6400 data
REM    373 parameters refined using      0 restraints
 
END  
     
WGHT      0.0505      1.0374 
REM Highest difference peak  0.314,  deepest hole -0.377,  1-sigma level  0.055
Q1    1   0.9584  0.4005  0.8160  11.00000  0.05    0.31
Q2    1   0.7399  0.1998  0.6701  11.00000  0.05    0.30
Q3    1   0.7858  0.2451  0.7570  11.00000  0.05    0.27
Q4    1   0.0565  0.2771  0.4763  11.00000  0.05    0.27
Q5    1   0.0362  0.2639  0.4666  11.00000  0.05    0.26
Q6    1  -0.0099  0.2598  0.3619  11.00000  0.05    0.26
Q7    1   1.0359  0.3427  0.8720  11.00000  0.05    0.25
Q8    1   0.7308  0.2198  0.5898  11.00000  0.05    0.24
Q9    1   0.0595  0.3503  0.4176  11.00000  0.05    0.23
Q10   1   0.1223  0.4257  0.4389  11.00000  0.05    0.23
;
_database_code_depnum_ccdc_archive 'CCDC 977755'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rpso510
_audit_creation_method           SHELXL-97
_audit_creation_date             2012-05-09
_audit_update_record             2012-05-09
_chemical_formula_sum            'C21 H23 N5 O13 P Yb'
_chemical_formula_weight         757.450
_refine_ls_R_factor_all          0.053
_cell_length_a                   16.7262(19)
_cell_length_b                   11.4988(12)
_cell_length_c                   14.6506(17)
_cell_angle_alpha                90.000
_cell_angle_beta                 109.599(6)
_cell_angle_gamma                90.000
_cell_volume                     2654.5(5)
_cell_formula_units_Z            4
_symmetry_int_tables_number      14
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_symmetry_space_group_name_Hall  -P_2ybc

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,0.500+y,0.500-z
3 -x,-y,-z
4 x,0.500-y,0.500+z

loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_radius_bond
Yb ? 1.200
P ? 1.200
O ? 1.200
H ? 1.200
N ? 1.200
C ? 1.200


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_attached_hydrogens
_atom_site_calc_flag
_atom_site_thermal_displace_type
_atom_site_u_iso_or_equiv
Yb1 Yb 0.2988(0) 0.060() 0.1735(0) 1.000 4 e ? d Uani 0.01713(6)
P1 P 0.1732(1) 0.2692(1) 0.0188(1) 1.000 4 e ? d Uani 0.0167(2)
O1 O 0.5874(2) 0.4661(3) 0.3376(2) 1.000 4 e ? d Uani 0.0247(7)
O2 O 0.3649(2) 0.2081(3) 0.1252(2) 1.000 4 e ? d Uani 0.0217(7)
O3 O 0.1877(2) 0.1778(3) 0.0962(2) 1.000 4 e ? d Uani 0.0190(7)
O4 O 0.2270(2) 0.0118(3) 0.2842(2) 1.000 4 e ? d Uani 0.0266(8)
O5 O 0.3186(2) -0.1135(3) 0.2709(3) 1.000 4 e ? d Uani 0.0300(8)
O6 O 0.2429(3) -0.1538(4) 0.3618(3) 1.000 4 e ? d Uani 0.0476(11)
O7 O 0.3079(2) 0.2350(3) 0.2830(2) 1.000 4 e ? d Uani 0.0252(7)
O8 O 0.4111(2) 0.1131(3) 0.3217(2) 1.000 4 e ? d Uani 0.0305(8)
O9 O 0.4224(2) 0.2727(3) 0.4045(3) 1.000 4 e ? d Uani 0.0367(9)
O10 O 0.2611(2) 0.0143(3) 0.0004(2) 1.000 4 e ? d Uani 0.0258(8)
O11 O 0.1986(2) -0.0805(3) 0.0840(2) 1.000 4 e ? d Uani 0.0309(8)
O12 O 0.1633(3) -0.1128(3) -0.0706(3) 1.000 4 e ? d Uani 0.0423(10)
O13 O 0.4060(3) 0.6158(4) 0.0312(5) 1.000 4 e ? d Uani 0.089(2)
H13A H 0.4572 0.6342 0.0441 1.000 4 e ? calc Uiso 0.13300
N1 N 0.5109(2) 0.5069(3) 0.3311(3) 1.000 4 e ? d Uani 0.0223(9)
N2 N 0.3898(3) 0.3913(3) 0.0911(3) 1.000 4 e ? d Uani 0.0240(9)
H2A H 0.377(3) 0.451(3) 0.052(3) 1.000 4 e ? d Uiso 0.02900
N3 N 0.2630(3) -0.0884(4) 0.3081(3) 1.000 4 e ? d Uani 0.0285(10)
N4 N 0.3809(2) 0.2094(3) 0.3381(3) 1.000 4 e ? d Uani 0.0218(9)
N5 N 0.2061(3) -0.0612(4) 0.0013(3) 1.000 4 e ? d Uani 0.0272(9)
C1 C 0.5031(3) 0.5720(5) 0.4048(4) 1.000 4 e ? d Uani 0.0338(13)
H1 H 0.5516 0.5893 0.4594 1.000 4 e ? calc Uiso 0.04100
C2 C 0.4252(4) 0.6127(6) 0.3998(5) 1.000 4 e ? d Uani 0.0503(17)
H2 H 0.4197 0.6601 0.4504 1.000 4 e ? calc Uiso 0.06000
C3 C 0.3544(4) 0.5854(5) 0.3219(5) 1.000 4 e ? d Uani 0.0489(17)
H3 H 0.2999 0.6130 0.3184 1.000 4 e ? calc Uiso 0.05900
C4 C 0.3645(3) 0.5174(5) 0.2495(4) 1.000 4 e ? d Uani 0.0359(13)
H4 H 0.3160 0.4966 0.1959 1.000 4 e ? calc Uiso 0.04300
C5 C 0.4435(3) 0.4785(4) 0.2528(4) 1.000 4 e ? d Uani 0.0231(10)
C6 C 0.4632(3) 0.4036(4) 0.1791(3) 1.000 4 e ? d Uani 0.0245(11)
H6A H 0.5107 0.4386 0.1626 1.000 4 e ? calc Uiso 0.02900
H6B H 0.4814 0.3258 0.2073 1.000 4 e ? calc Uiso 0.02900
C7 C 0.3442(3) 0.2942(4) 0.0713(3) 1.000 4 e ? d Uani 0.0174(9)
C8 C 0.2669(3) 0.2897(4) -0.0173(3) 1.000 4 e ? d Uani 0.0201(10)
H8A H 0.2717 0.2247 -0.0594 1.000 4 e ? calc Uiso 0.02400
H8B H 0.2615 0.3631 -0.0543 1.000 4 e ? calc Uiso 0.02400
C9 C 0.0896(3) 0.2279(4) -0.0901(3) 1.000 4 e ? d Uani 0.0202(10)
C10 C 0.0394(3) 0.1328(4) -0.0863(4) 1.000 4 e ? d Uani 0.0294(12)
H10 H 0.0493 0.0918 -0.0272 1.000 4 e ? calc Uiso 0.03500
C11 C -0.0252(3) 0.0986(5) -0.1695(4) 1.000 4 e ? d Uani 0.0371(14)
H11 H -0.0599 0.0340 -0.1673 1.000 4 e ? calc Uiso 0.04500
C12 C -0.0393(3) 0.1575(5) -0.2553(4) 1.000 4 e ? d Uani 0.0416(15)
H12 H -0.0833 0.1329 -0.3121 1.000 4 e ? calc Uiso 0.05000
C13 C 0.0104(3) 0.2526(6) -0.2589(4) 1.000 4 e ? d Uani 0.0385(14)
H13 H -0.0001 0.2936 -0.3181 1.000 4 e ? calc Uiso 0.04600
C14 C 0.0751(3) 0.2880(5) -0.1771(4) 1.000 4 e ? d Uani 0.0289(11)
H14 H 0.1095 0.3527 -0.1798 1.000 4 e ? calc Uiso 0.03500
C15 C 0.1517(3) 0.4079(4) 0.0614(3) 1.000 4 e ? d Uani 0.020(1)
C16 C 0.1445(3) 0.4154(4) 0.1520(4) 1.000 4 e ? d Uani 0.0276(11)
H16 H 0.1491 0.3473 0.1902 1.000 4 e ? calc Uiso 0.03300
C17 C 0.1305(4) 0.5227(5) 0.1877(4) 1.000 4 e ? d Uani 0.0383(14)
H17 H 0.1246 0.5282 0.2498 1.000 4 e ? calc Uiso 0.04600
C18 C 0.1254(4) 0.6214(5) 0.1323(5) 1.000 4 e ? d Uani 0.0420(15)
H18 H 0.1154 0.6947 0.1564 1.000 4 e ? calc Uiso 0.05000
C19 C 0.1345(4) 0.6149(5) 0.0437(5) 1.000 4 e ? d Uani 0.0498(17)
H19 H 0.1315 0.6835 0.0065 1.000 4 e ? calc Uiso 0.06000
C20 C 0.1482(4) 0.5086(5) 0.0076(4) 1.000 4 e ? d Uani 0.0375(14)
H20 H 0.1553 0.5043 -0.0540 1.000 4 e ? calc Uiso 0.04500
C21 C 0.3579(5) 0.7147(7) 0.0749(6) 1.000 4 e ? d Uani 0.077(2)
H21A H 0.3952 0.7384 0.1394 1.000 4 e ? calc Uiso 0.11500
H21B H 0.3053 0.6822 0.0797 1.000 4 e ? calc Uiso 0.11500
H21C H 0.3446 0.7823 0.0318 1.000 4 e ? calc Uiso 0.11500



loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Yb1 O1 . 2_645 2.241(3) no
Yb1 O2 . . 2.268(3) no
Yb1 O3 . . 2.271(3) no
Yb1 O11 . . 2.380(3) no
Yb1 O4 . . 2.384(3) no
Yb1 O5 . . 2.411(3) no
Yb1 O8 . . 2.425(3) no
Yb1 O10 . . 2.457(3) no
Yb1 O7 . . 2.545(3) no
Yb1 N3 . . 2.819(4) no
Yb1 N5 . . 2.844(4) no
Yb1 N4 . . 2.904(4) no
P1 O3 . . 1.505(3) no
P1 C15 . . 1.793(4) no
P1 C9 . . 1.798(5) no
P1 C8 . . 1.830(5) no
O1 N1 . . 1.337(5) no
O1 Yb1 . 2_655 2.241(3) no
O2 C7 . . 1.241(5) no
O4 N3 . . 1.292(5) no
O5 N3 . . 1.258(5) no
O6 N3 . . 1.215(5) no
O7 N4 . . 1.252(5) no
O8 N4 . . 1.272(5) no
O9 N4 . . 1.226(5) no
O10 N5 . . 1.267(5) no
O11 N5 . . 1.279(5) no
O12 N5 . . 1.212(5) no
O13 C21 . . 1.641(10) no
O13 H13A . . 0.8400 no
N1 C5 . . 1.352(6) no
N1 C1 . . 1.355(6) no
N2 C7 . . 1.328(6) no
N2 C6 . . 1.459(6) no
N2 H2A . . 0.874(19) no
C1 C2 . . 1.364(8) no
C1 H1 . . 0.9500 no
C2 C3 . . 1.377(8) no
C2 H2 . . 0.9500 no
C3 C4 . . 1.374(8) no
C3 H3 . . 0.9500 no
C4 C5 . . 1.380(7) no
C4 H4 . . 0.9500 no
C5 C6 . . 1.502(7) no
C6 H6A . . 0.9900 no
C6 H6B . . 0.9900 no
C7 C8 . . 1.495(6) no
C8 H8A . . 0.9900 no
C8 H8B . . 0.9900 no
C9 C10 . . 1.391(7) no
C9 C14 . . 1.397(7) no
C10 C11 . . 1.388(7) no
C10 H10 . . 0.9500 no
C11 C12 . . 1.376(9) no
C11 H11 . . 0.9500 no
C12 C13 . . 1.386(8) no
C12 H12 . . 0.9500 no
C13 C14 . . 1.380(7) no
C13 H13 . . 0.9500 no
C14 H14 . . 0.9500 no
C15 C16 . . 1.376(7) no
C15 C20 . . 1.390(7) no
C16 C17 . . 1.391(7) no
C16 H16 . . 0.9500 no
C17 C18 . . 1.381(8) no
C17 H17 . . 0.9500 no
C18 C19 . . 1.359(9) no
C18 H18 . . 0.9500 no
C19 C20 . . 1.380(8) no
C19 H19 . . 0.9500 no
C20 H20 . . 0.9500 no
C21 H21A . . 0.9800 no
C21 H21B . . 0.9800 no
C21 H21C . . 0.9800 no

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Yb1 O2 2_645 . . 79.92(11) no
O1 Yb1 O3 2_645 . . 145.47(12) no
O2 Yb1 O3 . . . 78.43(11) no
O1 Yb1 O11 2_645 . . 95.20(12) no
O2 Yb1 O11 . . . 131.64(11) no
O3 Yb1 O11 . . . 79.81(12) no
O1 Yb1 O4 2_645 . . 124.78(12) no
O2 Yb1 O4 . . . 142.73(12) no
O3 Yb1 O4 . . . 87.94(11) no
O11 Yb1 O4 . . . 78.18(12) no
O1 Yb1 O5 2_645 . . 72.08(12) no
O2 Yb1 O5 . . . 145.22(11) no
O3 Yb1 O5 . . . 135.72(11) no
O11 Yb1 O5 . . . 72.29(12) no
O4 Yb1 O5 . . . 53.50(11) no
O1 Yb1 O8 2_645 . . 76.40(12) no
O2 Yb1 O8 . . . 77.18(12) no
O3 Yb1 O8 . . . 123.71(11) no
O11 Yb1 O8 . . . 148.77(12) no
O4 Yb1 O8 . . . 82.23(12) no
O5 Yb1 O8 . . . 76.52(12) no
O1 Yb1 O10 2_645 . . 75.65(11) no
O2 Yb1 O10 . . . 79.75(11) no
O3 Yb1 O10 . . . 74.27(11) no
O11 Yb1 O10 . . . 52.85(11) no
O4 Yb1 O10 . . . 129.73(11) no
O5 Yb1 O10 . . . 111.76(12) no
O8 Yb1 O10 . . . 146.30(12) no
O1 Yb1 O7 2_645 . . 123.62(11) no
O2 Yb1 O7 . . . 70.77(11) no
O3 Yb1 O7 . . . 73.11(11) no
O11 Yb1 O7 . . . 140.03(12) no
O4 Yb1 O7 . . . 72.10(11) no
O5 Yb1 O7 . . . 108.28(11) no
O8 Yb1 O7 . . . 51.08(11) no
O10 Yb1 O7 . . . 139.50(11) no
O1 Yb1 N3 2_645 . . 98.24(12) no
O2 Yb1 N3 . . . 155.82(12) no
O3 Yb1 N3 . . . 112.33(12) no
O11 Yb1 N3 . . . 72.49(12) no
O4 Yb1 N3 . . . 27.14(12) no
O5 Yb1 N3 . . . 26.39(12) no
O8 Yb1 N3 . . . 78.96(12) no
O10 Yb1 N3 . . . 123.45(12) no
O7 Yb1 N3 . . . 91.11(12) no
O1 Yb1 N5 2_645 . . 85.56(12) no
O2 Yb1 N5 . . . 105.60(12) no
O3 Yb1 N5 . . . 74.84(11) no
O11 Yb1 N5 . . . 26.48(12) no
O4 Yb1 N5 . . . 103.93(12) no
O5 Yb1 N5 . . . 92.60(12) no
O8 Yb1 N5 . . . 161.05(11) no
O10 Yb1 N5 . . . 26.39(11) no
O7 Yb1 N5 . . . 147.81(11) no
N3 Yb1 N5 . . . 98.25(12) no
O1 Yb1 N4 2_645 . . 99.70(11) no
O2 Yb1 N4 . . . 70.75(11) no
O3 Yb1 N4 . . . 98.15(11) no
O11 Yb1 N4 . . . 155.36(11) no
O4 Yb1 N4 . . . 77.21(11) no
O5 Yb1 N4 . . . 93.74(12) no
O8 Yb1 N4 . . . 25.66(11) no
O10 Yb1 N4 . . . 150.48(11) no
O7 Yb1 N4 . . . 25.49(10) no
N3 Yb1 N4 . . . 85.97(11) no
N5 Yb1 N4 . . . 172.77(11) no
O3 P1 C15 . . . 111.1(2) no
O3 P1 C9 . . . 111.4(2) no
C15 P1 C9 . . . 110.9(2) no
O3 P1 C8 . . . 111.78(19) no
C15 P1 C8 . . . 106.1(2) no
C9 P1 C8 . . . 105.3(2) no
N1 O1 Yb1 . . 2_655 129.9(3) no
C7 O2 Yb1 . . . 137.5(3) no
P1 O3 Yb1 . . . 133.67(18) no
N3 O4 Yb1 . . . 95.5(3) no
N3 O5 Yb1 . . . 95.2(3) no
N4 O7 Yb1 . . . 93.5(2) no
N4 O8 Yb1 . . . 98.7(2) no
N5 O10 Yb1 . . . 94.1(3) no
N5 O11 Yb1 . . . 97.5(3) no
C21 O13 H13A . . . 109.50 no
O1 N1 C5 . . . 118.8(4) no
O1 N1 C1 . . . 118.9(4) no
C5 N1 C1 . . . 122.3(4) no
C7 N2 C6 . . . 121.8(4) no
C7 N2 H2A . . . 121.(3) no
C6 N2 H2A . . . 117.(3) no
O6 N3 O5 . . . 122.9(4) no
O6 N3 O4 . . . 121.5(4) no
O5 N3 O4 . . . 115.6(4) no
O6 N3 Yb1 . . . 176.0(4) no
O5 N3 Yb1 . . . 58.4(2) no
O4 N3 Yb1 . . . 57.3(2) no
O9 N4 O7 . . . 122.8(4) no
O9 N4 O8 . . . 120.8(4) no
O7 N4 O8 . . . 116.4(4) no
O9 N4 Yb1 . . . 173.7(3) no
O7 N4 Yb1 . . . 61.1(2) no
O8 N4 Yb1 . . . 55.6(2) no
O12 N5 O10 . . . 123.0(4) no
O12 N5 O11 . . . 121.4(4) no
O10 N5 O11 . . . 115.5(4) no
O12 N5 Yb1 . . . 176.9(4) no
O10 N5 Yb1 . . . 59.5(2) no
O11 N5 Yb1 . . . 56.1(2) no
N1 C1 C2 . . . 119.5(5) no
N1 C1 H1 . . . 120.30 no
C2 C1 H1 . . . 120.30 no
C1 C2 C3 . . . 120.5(6) no
C1 C2 H2 . . . 119.80 no
C3 C2 H2 . . . 119.80 no
C4 C3 C2 . . . 118.4(6) no
C4 C3 H3 . . . 120.80 no
C2 C3 H3 . . . 120.80 no
C3 C4 C5 . . . 121.4(5) no
C3 C4 H4 . . . 119.30 no
C5 C4 H4 . . . 119.30 no
N1 C5 C4 . . . 117.9(5) no
N1 C5 C6 . . . 115.3(4) no
C4 C5 C6 . . . 126.8(4) no
N2 C6 C5 . . . 111.6(4) no
N2 C6 H6A . . . 109.30 no
C5 C6 H6A . . . 109.30 no
N2 C6 H6B . . . 109.30 no
C5 C6 H6B . . . 109.30 no
H6A C6 H6B . . . 108.00 no
O2 C7 N2 . . . 121.0(4) no
O2 C7 C8 . . . 120.0(4) no
N2 C7 C8 . . . 119.0(4) no
C7 C8 P1 . . . 109.2(3) no
C7 C8 H8A . . . 109.80 no
P1 C8 H8A . . . 109.80 no
C7 C8 H8B . . . 109.80 no
P1 C8 H8B . . . 109.80 no
H8A C8 H8B . . . 108.30 no
C10 C9 C14 . . . 120.2(4) no
C10 C9 P1 . . . 118.1(4) no
C14 C9 P1 . . . 121.6(4) no
C11 C10 C9 . . . 119.3(5) no
C11 C10 H10 . . . 120.40 no
C9 C10 H10 . . . 120.40 no
C12 C11 C10 . . . 120.5(5) no
C12 C11 H11 . . . 119.70 no
C10 C11 H11 . . . 119.70 no
C11 C12 C13 . . . 120.1(5) no
C11 C12 H12 . . . 119.90 no
C13 C12 H12 . . . 119.90 no
C14 C13 C12 . . . 120.4(5) no
C14 C13 H13 . . . 119.80 no
C12 C13 H13 . . . 119.80 no
C13 C14 C9 . . . 119.5(5) no
C13 C14 H14 . . . 120.30 no
C9 C14 H14 . . . 120.30 no
C16 C15 C20 . . . 119.6(4) no
C16 C15 P1 . . . 118.9(4) no
C20 C15 P1 . . . 121.3(4) no
C15 C16 C17 . . . 119.9(5) no
C15 C16 H16 . . . 120.10 no
C17 C16 H16 . . . 120.10 no
C18 C17 C16 . . . 119.6(5) no
C18 C17 H17 . . . 120.20 no
C16 C17 H17 . . . 120.20 no
C19 C18 C17 . . . 120.8(5) no
C19 C18 H18 . . . 119.60 no
C17 C18 H18 . . . 119.60 no
C18 C19 C20 . . . 120.0(6) no
C18 C19 H19 . . . 120.00 no
C20 C19 H19 . . . 120.00 no
C19 C20 C15 . . . 120.1(5) no
C19 C20 H20 . . . 120.00 no
C15 C20 H20 . . . 120.00 no
O13 C21 H21A . . . 109.50 no
O13 C21 H21B . . . 109.50 no
H21A C21 H21B . . . 109.50 no
O13 C21 H21C . . . 109.50 no
H21A C21 H21C . . . 109.50 no
H21B C21 H21C . . . 109.50 no

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 Yb1 P1 O3 2_645 . . . 159.7(3) no
O2 Yb1 P1 O3 . . . . -153.4(3) no
O11 Yb1 P1 O3 . . . . 65.3(3) no
O4 Yb1 P1 O3 . . . . -11.6(3) no
O5 Yb1 P1 O3 . . . . 25.0(3) no
O8 Yb1 P1 O3 . . . . -102.1(3) no
O10 Yb1 P1 O3 . . . . 115.4(3) no
O7 Yb1 P1 O3 . . . . -78.0(3) no
N3 Yb1 P1 O3 . . . . 1.3(3) no
N5 Yb1 P1 O3 . . . . 88.9(3) no
N4 Yb1 P1 O3 . . . . -90.6(3) no
O1 Yb1 P1 C15 2_645 . . . -126.7(2) no
O2 Yb1 P1 C15 . . . . -79.8(2) no
O3 Yb1 P1 C15 . . . . 73.6(3) no
O11 Yb1 P1 C15 . . . . 138.9(2) no
O4 Yb1 P1 C15 . . . . 62.1(2) no
O5 Yb1 P1 C15 . . . . 98.6(3) no
O8 Yb1 P1 C15 . . . . -28.5(2) no
O10 Yb1 P1 C15 . . . . -171.0(2) no
O7 Yb1 P1 C15 . . . . -4.4(2) no
N3 Yb1 P1 C15 . . . . 74.9(2) no
N5 Yb1 P1 C15 . . . . 162.5(2) no
N4 Yb1 P1 C15 . . . . -16.9(2) no
O1 Yb1 P1 C9 2_645 . . . 82.4(2) no
O2 Yb1 P1 C9 . . . . 129.3(2) no
O3 Yb1 P1 C9 . . . . -77.3(3) no
O11 Yb1 P1 C9 . . . . -12.0(2) no
O4 Yb1 P1 C9 . . . . -88.8(2) no
O5 Yb1 P1 C9 . . . . -52.3(3) no
O8 Yb1 P1 C9 . . . . -179.4(2) no
O10 Yb1 P1 C9 . . . . 38.1(2) no
O7 Yb1 P1 C9 . . . . -155.3(2) no
N3 Yb1 P1 C9 . . . . -76.0(2) no
N5 Yb1 P1 C9 . . . . 11.6(2) no
N4 Yb1 P1 C9 . . . . -167.84(19) no
O1 Yb1 P1 C8 2_645 . . . -21.63(18) no
O2 Yb1 P1 C8 . . . . 25.24(17) no
O3 Yb1 P1 C8 . . . . 178.6(3) no
O11 Yb1 P1 C8 . . . . -116.03(17) no
O4 Yb1 P1 C8 . . . . 167.09(17) no
O5 Yb1 P1 C8 . . . . -156.3(2) no
O8 Yb1 P1 C8 . . . . 76.55(18) no
O10 Yb1 P1 C8 . . . . -65.96(17) no
O7 Yb1 P1 C8 . . . . 100.60(17) no
N3 Yb1 P1 C8 . . . . 179.96(18) no
N5 Yb1 P1 C8 . . . . -92.49(17) no
N4 Yb1 P1 C8 . . . . 88.09(17) no
O1 Yb1 O2 C7 2_645 . . . 142.6(4) no
O3 Yb1 O2 C7 . . . . -10.4(4) no
O11 Yb1 O2 C7 . . . . 54.6(5) no
O4 Yb1 O2 C7 . . . . -81.1(5) no
O5 Yb1 O2 C7 . . . . 179.1(4) no
O8 Yb1 O2 C7 . . . . -139.2(4) no
O10 Yb1 O2 C7 . . . . 65.5(4) no
O7 Yb1 O2 C7 . . . . -86.3(4) no
N3 Yb1 O2 C7 . . . . -129.7(4) no
N5 Yb1 O2 C7 . . . . 60.1(4) no
N4 Yb1 O2 C7 . . . . -113.4(4) no
C15 P1 O3 Yb1 . . . . -119.7(3) no
C9 P1 O3 Yb1 . . . . 116.1(3) no
C8 P1 O3 Yb1 . . . . -1.4(3) no
O1 Yb1 O3 P1 2_645 . . . -28.4(4) no
O2 Yb1 O3 P1 . . . . 23.8(2) no
O11 Yb1 O3 P1 . . . . -112.8(3) no
O4 Yb1 O3 P1 . . . . 168.9(3) no
O5 Yb1 O3 P1 . . . . -163.9(2) no
O8 Yb1 O3 P1 . . . . 89.6(3) no
O10 Yb1 O3 P1 . . . . -58.7(2) no
O7 Yb1 O3 P1 . . . . 97.0(3) no
N3 Yb1 O3 P1 . . . . -178.9(2) no
N5 Yb1 O3 P1 . . . . -86.1(3) no
N4 Yb1 O3 P1 . . . . 92.1(3) no
O1 Yb1 O4 N3 2_645 . . . -13.5(3) no
O2 Yb1 O4 N3 . . . . -137.6(2) no
O3 Yb1 O4 N3 . . . . 154.6(3) no
O11 Yb1 O4 N3 . . . . 74.6(3) no
O5 Yb1 O4 N3 . . . . -2.0(2) no
O8 Yb1 O4 N3 . . . . -80.9(3) no
O10 Yb1 O4 N3 . . . . 87.1(3) no
O7 Yb1 O4 N3 . . . . -132.5(3) no
N5 Yb1 O4 N3 . . . . 80.8(3) no
N4 Yb1 O4 N3 . . . . -106.5(3) no
O1 Yb1 O5 N3 2_645 . . . 172.1(3) no
O2 Yb1 O5 N3 . . . . 134.1(3) no
O3 Yb1 O5 N3 . . . . -32.6(3) no
O11 Yb1 O5 N3 . . . . -86.2(3) no
O4 Yb1 O5 N3 . . . . 2.0(2) no
O8 Yb1 O5 N3 . . . . 92.3(3) no
O10 Yb1 O5 N3 . . . . -122.1(3) no
O7 Yb1 O5 N3 . . . . 51.7(3) no
N5 Yb1 O5 N3 . . . . -103.4(3) no
N4 Yb1 O5 N3 . . . . 73.1(3) no
O1 Yb1 O7 N4 2_645 . . . -22.5(3) no
O2 Yb1 O7 N4 . . . . -85.4(3) no
O3 Yb1 O7 N4 . . . . -168.8(3) no
O11 Yb1 O7 N4 . . . . 141.8(2) no
O4 Yb1 O7 N4 . . . . 97.9(3) no
O5 Yb1 O7 N4 . . . . 57.8(3) no
O8 Yb1 O7 N4 . . . . 3.4(2) no
O10 Yb1 O7 N4 . . . . -131.1(2) no
N3 Yb1 O7 N4 . . . . 78.2(3) no
N5 Yb1 O7 N4 . . . . -174.3(2) no
O1 Yb1 O8 N4 2_645 . . . 154.7(3) no
O2 Yb1 O8 N4 . . . . 72.1(3) no
O3 Yb1 O8 N4 . . . . 5.7(3) no
O11 Yb1 O8 N4 . . . . -128.0(3) no
O4 Yb1 O8 N4 . . . . -76.6(3) no
O5 Yb1 O8 N4 . . . . -130.8(3) no
O10 Yb1 O8 N4 . . . . 120.0(3) no
O7 Yb1 O8 N4 . . . . -3.4(2) no
N3 Yb1 O8 N4 . . . . -103.9(3) no
N5 Yb1 O8 N4 . . . . 172.9(3) no
O1 Yb1 O10 N5 2_645 . . . 109.6(3) no
O2 Yb1 O10 N5 . . . . -168.3(3) no
O3 Yb1 O10 N5 . . . . -87.5(3) no
O11 Yb1 O10 N5 . . . . 1.5(2) no
O4 Yb1 O10 N5 . . . . -13.9(3) no
O5 Yb1 O10 N5 . . . . 46.0(3) no
O8 Yb1 O10 N5 . . . . 144.4(2) no
O7 Yb1 O10 N5 . . . . -124.9(2) no
N3 Yb1 O10 N5 . . . . 19.2(3) no
N4 Yb1 O10 N5 . . . . -166.1(2) no
O1 Yb1 O11 N5 2_645 . . . -69.1(3) no
O2 Yb1 O11 N5 . . . . 12.0(3) no
O3 Yb1 O11 N5 . . . . 76.4(3) no
O4 Yb1 O11 N5 . . . . 166.4(3) no
O5 Yb1 O11 N5 . . . . -138.4(3) no
O8 Yb1 O11 N5 . . . . -141.3(3) no
O10 Yb1 O11 N5 . . . . -1.5(2) no
O7 Yb1 O11 N5 . . . . 124.0(3) no
N3 Yb1 O11 N5 . . . . -166.1(3) no
N4 Yb1 O11 N5 . . . . 163.7(3) no
Yb1 O1 N1 C5 2_655 . . . 110.3(4) no
Yb1 O1 N1 C1 2_655 . . . -71.9(5) no
Yb1 O5 N3 O6 . . . . 175.6(4) no
Yb1 O5 N3 O4 . . . . -3.4(4) no
Yb1 O4 N3 O6 . . . . -175.5(4) no
Yb1 O4 N3 O5 . . . . 3.4(4) no
Yb1 O7 N4 O9 . . . . 174.2(4) no
Yb1 O7 N4 O8 . . . . -5.6(4) no
Yb1 O8 N4 O9 . . . . -173.9(4) no
Yb1 O8 N4 O7 . . . . 6.0(4) no
Yb1 O10 N5 O12 . . . . 177.8(4) no
Yb1 O10 N5 O11 . . . . -2.5(4) no
Yb1 O11 N5 O12 . . . . -177.7(4) no
Yb1 O11 N5 O10 . . . . 2.6(4) no
O1 N1 C1 C2 . . . . -179.0(5) no
C5 N1 C1 C2 . . . . -1.2(8) no
N1 C1 C2 C3 . . . . 1.7(10) no
C1 C2 C3 C4 . . . . -0.5(10) no
C2 C3 C4 C5 . . . . -1.2(10) no
O1 N1 C5 C4 . . . . 177.3(4) no
C1 N1 C5 C4 . . . . -0.5(7) no
O1 N1 C5 C6 . . . . -0.9(6) no
C1 N1 C5 C6 . . . . -178.7(4) no
C3 C4 C5 N1 . . . . 1.7(8) no
C3 C4 C5 C6 . . . . 179.7(6) no
C7 N2 C6 C5 . . . . -104.4(5) no
N1 C5 C6 N2 . . . . -171.7(4) no
C4 C5 C6 N2 . . . . 10.3(7) no
Yb1 O2 C7 N2 . . . . 147.3(4) no
Yb1 O2 C7 C8 . . . . -32.5(6) no
C6 N2 C7 O2 . . . . -3.2(7) no
C6 N2 C7 C8 . . . . 176.5(4) no
O2 C7 C8 P1 . . . . 63.1(5) no
N2 C7 C8 P1 . . . . -116.7(4) no
O3 P1 C8 C7 . . . . -44.4(4) no
C15 P1 C8 C7 . . . . 76.8(3) no
C9 P1 C8 C7 . . . . -165.6(3) no
Yb1 P1 C8 C7 . . . . -45.1(3) no
O3 P1 C9 C10 . . . . 11.2(4) no
C15 P1 C9 C10 . . . . -113.1(4) no
C8 P1 C9 C10 . . . . 132.6(4) no
Yb1 P1 C9 C10 . . . . 40.8(4) no
O3 P1 C9 C14 . . . . -168.1(4) no
C15 P1 C9 C14 . . . . 67.6(4) no
C8 P1 C9 C14 . . . . -46.8(4) no
Yb1 P1 C9 C14 . . . . -138.5(3) no
C14 C9 C10 C11 . . . . -0.1(7) no
P1 C9 C10 C11 . . . . -179.5(4) no
C9 C10 C11 C12 . . . . 0.4(8) no
C10 C11 C12 C13 . . . . -0.7(8) no
C11 C12 C13 C14 . . . . 0.8(8) no
C12 C13 C14 C9 . . . . -0.6(8) no
C10 C9 C14 C13 . . . . 0.3(7) no
P1 C9 C14 C13 . . . . 179.6(4) no
O3 P1 C15 C16 . . . . -4.6(5) no
C9 P1 C15 C16 . . . . 119.9(4) no
C8 P1 C15 C16 . . . . -126.3(4) no
Yb1 P1 C15 C16 . . . . -33.6(5) no
O3 P1 C15 C20 . . . . 170.7(4) no
C9 P1 C15 C20 . . . . -64.8(5) no
C8 P1 C15 C20 . . . . 49.1(5) no
Yb1 P1 C15 C20 . . . . 141.7(4) no
C20 C15 C16 C17 . . . . 2.5(8) no
P1 C15 C16 C17 . . . . 178.0(4) no
C15 C16 C17 C18 . . . . -1.1(8) no
C16 C17 C18 C19 . . . . -0.5(9) no
C17 C18 C19 C20 . . . . 0.7(10) no
C18 C19 C20 C15 . . . . 0.8(10) no
C16 C15 C20 C19 . . . . -2.4(8) no
P1 C15 C20 C19 . . . . -177.7(5) no

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O13 H13A O8 . . 2_655 0.8400 2.4200 3.096(6) 137.70 no
O13 H13A O9 . . 2_655 0.8400 2.4800 3.251(6) 153.40 no
N2 H2A O13 . . . 0.874(19) 2.01(3) 2.770(6) 145.(5) no
_database_code_depnum_ccdc_archive 'CCDC 977756'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rpso583

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H37 N3 O5 P2'
_chemical_formula_weight         653.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   18.635(2)
_cell_length_b                   31.142(3)
_cell_length_c                   5.6670(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3288.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1975
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      22.80

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    0.180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9581
_exptl_absorpt_correction_T_max  0.9829
_exptl_absorpt_process_details   'Bruker, SADABS'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24824
_diffrn_reflns_av_R_equivalents  0.1035
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         3.41
_diffrn_reflns_theta_max         25.73
_reflns_number_total             3186
_reflns_number_gt                2128
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0441P)²+1.6018P] 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         3186
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0476
_refine_ls_wR_factor_ref         0.1127
_refine_ls_wR_factor_gt          0.0976
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.68054(4) 0.06970(2) -0.01701(11) 0.01680(18) Uani 1 1 d . . .
O1 O 0.70378(10) 0.07629(5) -0.2663(3) 0.0229(4) Uani 1 1 d . . .
O2 O 0.81816(10) 0.13161(6) 0.0561(3) 0.0258(5) Uani 1 1 d . . .
N1 N 0.80501(16) 0.2500 0.4790(5) 0.0174(7) Uani 1 2 d S . .
N2 N 0.77934(12) 0.13288(6) 0.4352(4) 0.0169(5) Uani 1 1 d . . .
H2A H 0.7590(14) 0.1185(8) 0.554(5) 0.020 Uiso 1 1 d . . .
C1 C 0.77030(14) 0.21277(7) 0.4383(4) 0.0193(6) Uani 1 1 d . . .
C2 C 0.70071(16) 0.21160(9) 0.3567(6) 0.0347(8) Uani 1 1 d . . .
H2 H 0.6774 0.1850 0.3284 0.042 Uiso 1 1 calc R . .
C3 C 0.6654(2) 0.2500 0.3168(9) 0.0430(13) Uani 1 2 d S . .
H3 H 0.6171 0.2500 0.2624 0.052 Uiso 1 2 calc SR . .
C4 C 0.81423(14) 0.17320(7) 0.4938(5) 0.0209(6) Uani 1 1 d . . .
H4A H 0.8601 0.1749 0.4064 0.025 Uiso 1 1 calc R . .
H4B H 0.8257 0.1732 0.6644 0.025 Uiso 1 1 calc R . .
C5 C 0.78645(14) 0.11480(7) 0.2214(5) 0.0172(6) Uani 1 1 d . . .
C6 C 0.75145(13) 0.07079(7) 0.2001(4) 0.0162(6) Uani 1 1 d . . .
H6A H 0.7316 0.0624 0.3554 0.019 Uiso 1 1 calc R . .
H6B H 0.7885 0.0494 0.1565 0.019 Uiso 1 1 calc R . .
C7 C 0.61682(14) 0.11024(8) 0.0713(5) 0.0191(6) Uani 1 1 d . . .
C8 C 0.58105(14) 0.10905(8) 0.2860(5) 0.0254(7) Uani 1 1 d . . .
H8 H 0.5914 0.0870 0.3970 0.030 Uiso 1 1 calc R . .
C9 C 0.52997(16) 0.14029(9) 0.3379(6) 0.0343(8) Uani 1 1 d . . .
H9 H 0.5048 0.1395 0.4835 0.041 Uiso 1 1 calc R . .
C10 C 0.51606(17) 0.17270(9) 0.1750(7) 0.0411(9) Uani 1 1 d . . .
H10 H 0.4811 0.1939 0.2103 0.049 Uiso 1 1 calc R . .
C11 C 0.55209(17) 0.17437(9) -0.0354(6) 0.0389(8) Uani 1 1 d . . .
H11 H 0.5424 0.1968 -0.1447 0.047 Uiso 1 1 calc R . .
C12 C 0.60259(16) 0.14337(8) -0.0883(5) 0.0289(7) Uani 1 1 d . . .
H12 H 0.6278 0.1446 -0.2339 0.035 Uiso 1 1 calc R . .
C13 C 0.63692(13) 0.01827(7) 0.0130(4) 0.0166(5) Uani 1 1 d . . .
C14 C 0.59243(15) 0.00576(8) -0.1717(5) 0.0256(7) Uani 1 1 d . . .
H14 H 0.5848 0.0248 -0.3004 0.031 Uiso 1 1 calc R . .
C15 C 0.55913(16) -0.03393(8) -0.1707(5) 0.0267(7) Uani 1 1 d . . .
H15 H 0.5286 -0.0420 -0.2975 0.032 Uiso 1 1 calc R . .
C16 C 0.57040(14) -0.06187(8) 0.0153(5) 0.0227(6) Uani 1 1 d . . .
H16 H 0.5476 -0.0892 0.0163 0.027 Uiso 1 1 calc R . .
C17 C 0.61437(15) -0.05026(8) 0.1983(5) 0.0255(7) Uani 1 1 d . . .
H17 H 0.6225 -0.0697 0.3249 0.031 Uiso 1 1 calc R . .
C18 C 0.64728(15) -0.00992(8) 0.1991(5) 0.0250(7) Uani 1 1 d . . .
H18 H 0.6769 -0.0018 0.3279 0.030 Uiso 1 1 calc R . .
C19 C 0.9088(5) 0.2500 0.9432(11) 0.101(3) Uani 1 2 d S . .
H19A H 0.9487 0.2531 1.0547 0.151 Uiso 0.50 1 calc PR . .
H19B H 0.8838 0.2229 0.9736 0.151 Uiso 0.50 1 calc PR . .
H19C H 0.8753 0.2740 0.9630 0.151 Uiso 0.50 1 calc PR . .
O3 O 0.93567(17) 0.2500 0.7106(8) 0.0599(11) Uani 1 2 d S . .
H3A H 0.9047 0.2397 0.6191 0.090 Uiso 0.50 1 calc PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1 1.4916(18) . ?
P1 C7 1.804(3) . ?
P1 C13 1.804(2) . ?
P1 C6 1.806(3) . ?
O2 C5 1.225(3) . ?
N1 C1 1.348(3) 7_565 ?
N1 C1 1.348(3) . ?
N2 C5 1.342(3) . ?
N2 C4 1.452(3) . ?
N2 H2A 0.90(3) . ?
C1 C2 1.377(4) . ?
C1 C4 1.513(3) . ?
C2 C3 1.384(3) . ?
C2 H2 0.9500 . ?
C3 C2 1.384(3) 7_565 ?
C3 H3 0.9500 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.523(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.388(4) . ?
C7 C12 1.397(4) . ?
C8 C9 1.393(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.392(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.369(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.386(3) . ?
C13 C14 1.391(3) . ?
C14 C15 1.383(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.383(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.370(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.398(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 O3 1.410(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
O3 H3A 0.8400 . ?

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 P1 C7 110.95(11) . . ?
O1 P1 C13 110.01(11) . . ?
C7 P1 C13 107.38(12) . . ?
O1 P1 C6 115.48(11) . . ?
C7 P1 C6 106.22(11) . . ?
C13 P1 C6 106.39(11) . . ?
C1 N1 C1 118.7(3) 7_565 . ?
C5 N2 C4 121.6(2) . . ?
C5 N2 H2A 120.8(16) . . ?
C4 N2 H2A 116.8(16) . . ?
N1 C1 C2 122.1(2) . . ?
N1 C1 C4 113.9(2) . . ?
C2 C1 C4 123.9(2) . . ?
C1 C2 C3 118.7(3) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C2 C3 C2 119.6(4) . 7_565 ?
C2 C3 H3 120.2 . . ?
C2 C3 H3 120.2 7_565 . ?
N2 C4 C1 114.5(2) . . ?
N2 C4 H4A 108.6 . . ?
C1 C4 H4A 108.6 . . ?
N2 C4 H4B 108.6 . . ?
C1 C4 H4B 108.6 . . ?
H4A C4 H4B 107.6 . . ?
O2 C5 N2 124.0(2) . . ?
O2 C5 C6 122.1(2) . . ?
N2 C5 C6 114.0(2) . . ?
C5 C6 P1 112.60(16) . . ?
C5 C6 H6A 109.1 . . ?
P1 C6 H6A 109.1 . . ?
C5 C6 H6B 109.1 . . ?
P1 C6 H6B 109.1 . . ?
H6A C6 H6B 107.8 . . ?
C8 C7 C12 119.7(2) . . ?
C8 C7 P1 122.7(2) . . ?
C12 C7 P1 117.5(2) . . ?
C7 C8 C9 119.7(3) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C10 C9 C8 119.6(3) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
C11 C10 C9 120.9(3) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C12 119.8(3) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C11 C12 C7 120.3(3) . . ?
C11 C12 H12 119.8 . . ?
C7 C12 H12 119.8 . . ?
C18 C13 C14 118.6(2) . . ?
C18 C13 P1 124.8(2) . . ?
C14 C13 P1 116.51(19) . . ?
C15 C14 C13 121.0(2) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 119.8(3) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 120.1(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.1(2) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C13 C18 C17 120.4(2) . . ?
C13 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
O3 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C19 O3 H3A 109.5 . . ?

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
C1 N1 C1 C2 0.0(5) 7_565 . . . ?
C1 N1 C1 C4 -179.12(19) 7_565 . . . ?
N1 C1 C2 C3 -0.4(5) . . . . ?
C4 C1 C2 C3 178.6(3) . . . . ?
C1 C2 C3 C2 0.8(7) . . . 7_565 ?
C5 N2 C4 C1 89.3(3) . . . . ?
N1 C1 C4 N2 -175.9(2) . . . . ?
C2 C1 C4 N2 5.0(4) . . . . ?
C4 N2 C5 O2 -5.0(4) . . . . ?
C4 N2 C5 C6 174.9(2) . . . . ?
O2 C5 C6 P1 -62.3(3) . . . . ?
N2 C5 C6 P1 117.9(2) . . . . ?
O1 P1 C6 C5 66.0(2) . . . . ?
C7 P1 C6 C5 -57.4(2) . . . . ?
C13 P1 C6 C5 -171.60(17) . . . . ?
O1 P1 C7 C8 173.2(2) . . . . ?
C13 P1 C7 C8 52.9(2) . . . . ?
C6 P1 C7 C8 -60.6(2) . . . . ?
O1 P1 C7 C12 -5.4(2) . . . . ?
C13 P1 C7 C12 -125.6(2) . . . . ?
C6 P1 C7 C12 120.9(2) . . . . ?
C12 C7 C8 C9 1.6(4) . . . . ?
P1 C7 C8 C9 -176.9(2) . . . . ?
C7 C8 C9 C10 -0.8(4) . . . . ?
C8 C9 C10 C11 -0.2(4) . . . . ?
C9 C10 C11 C12 0.5(4) . . . . ?
C10 C11 C12 C7 0.3(4) . . . . ?
C8 C7 C12 C11 -1.3(4) . . . . ?
P1 C7 C12 C11 177.2(2) . . . . ?
O1 P1 C13 C18 137.9(2) . . . . ?
C7 P1 C13 C18 -101.3(2) . . . . ?
C6 P1 C13 C18 12.1(3) . . . . ?
O1 P1 C13 C14 -39.0(2) . . . . ?
C7 P1 C13 C14 81.9(2) . . . . ?
C6 P1 C13 C14 -164.7(2) . . . . ?
C18 C13 C14 C15 -0.1(4) . . . . ?
P1 C13 C14 C15 177.0(2) . . . . ?
C13 C14 C15 C16 -0.4(4) . . . . ?
C14 C15 C16 C17 0.0(4) . . . . ?
C15 C16 C17 C18 0.8(4) . . . . ?
C14 C13 C18 C17 0.9(4) . . . . ?
P1 C13 C18 C17 -175.9(2) . . . . ?
C16 C17 C18 C13 -1.3(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O1 0.90(3) 1.95(3) 2.820(3) 162(2) 1_556
O3 H3A N1 0.84 2.05 2.766(4) 143.4 .

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.73
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.061
_iucr_refine_instruction_details 
;
TITL rpso583 in Pnma
CELL 0.71073 18.6353 31.1424 5.6670 90.000 90.000 90.000
ZERR 4.00 0.0021 0.0031 0.0006 0.000 0.000 0.000
LATT 1
SYMM x+1/2, -y+1/2, -z+1/2
SYMM -x, y+1/2, -z
SYMM -x+1/2, -y, z+1/2
SFAC C  H  N  O  P
UNIT 144  148  12  20  8
L.S. 10
ACTA
BOND $H
FMAP 2
PLAN 10
CONF
OMIT 2   1   0
OMIT 2   0   0
OMIT 2   3   0
OMIT 0   4   0
OMIT 2   2   0
EQIV $1 x, y, z+1
HTAB n2 o1_$1
HTAB o3 n1
SIZE 0.096 0.187 0.240
TEMP -173.140
WGHT    0.044100    1.601800
FVAR       0.07766
P1    5    0.680539    0.069696   -0.017013    11.00000    0.01955    0.01398 =
         0.01689    0.00063   -0.00071    0.00013
O1    4    0.703777    0.076288   -0.266256    11.00000    0.02702    0.02464 =
         0.01716    0.00279    0.00048   -0.00261
O2    4    0.818160    0.131613    0.056128    11.00000    0.03036    0.02517 =
         0.02174    0.00327    0.00708   -0.00634
N1    3    0.805005    0.250000    0.478988    10.50000    0.02436    0.01027 =
         0.01767    0.00000   -0.00249    0.00000
N2    3    0.779336    0.132884    0.435177    11.00000    0.02188    0.00967 =
         0.01928    0.00060    0.00147   -0.00273
H2A   2    0.758952    0.118468    0.554401    11.00000   -1.20000
C1    1    0.770296    0.212767    0.438267    11.00000    0.02250    0.01407 =
         0.02144   -0.00058   -0.00048   -0.00034
C2    1    0.700714    0.211603    0.356697    11.00000    0.02688    0.01684 =
         0.06028   -0.00152   -0.01231   -0.00231
AFIX  43
H2    2    0.677435    0.184959    0.328365    11.00000   -1.20000
AFIX   0
C3    1    0.665361    0.250000    0.316800    10.50000    0.02553    0.01959 =
         0.08374    0.00000   -0.02479    0.00000
AFIX  43
H3    2    0.617143    0.249999    0.262384    10.50000   -1.20000
AFIX   0
C4    1    0.814228    0.173198    0.493772    11.00000    0.02247    0.01195 =
         0.02831    0.00077   -0.00374   -0.00245
AFIX  23
H4A   2    0.860147    0.174924    0.406433    11.00000   -1.20000
H4B   2    0.825664    0.173197    0.664371    11.00000   -1.20000
AFIX   0
C5    1    0.786452    0.114805    0.221416    11.00000    0.01570    0.01554 =
         0.02043    0.00138   -0.00393    0.00426
C6    1    0.751453    0.070788    0.200126    11.00000    0.01611    0.01514 =
         0.01739    0.00077    0.00232    0.00062
AFIX  23
H6A   2    0.731557    0.062424    0.355449    11.00000   -1.20000
H6B   2    0.788462    0.049410    0.156467    11.00000   -1.20000
AFIX   0
C7    1    0.616823    0.110239    0.071299    11.00000    0.01719    0.01509 =
         0.02503   -0.00374   -0.00831   -0.00008
C8    1    0.581050    0.109046    0.285980    11.00000    0.02022    0.02491 =
         0.03096   -0.00633   -0.00530    0.00007
AFIX  43
H8    2    0.591355    0.087032    0.396969    11.00000   -1.20000
AFIX   0
C9    1    0.529967    0.140289    0.337854    11.00000    0.02127    0.03799 =
         0.04377   -0.02019   -0.00532    0.00003
AFIX  43
H9    2    0.504765    0.139491    0.483506    11.00000   -1.20000
AFIX   0
C10   1    0.516061    0.172697    0.174965    11.00000    0.02444    0.02955 =
         0.06920   -0.02659   -0.02270    0.01127
AFIX  43
H10   2    0.481095    0.193947    0.210250    11.00000   -1.20000
AFIX   0
C11   1    0.552094    0.174366   -0.035448    11.00000    0.04170    0.02400 =
         0.05105   -0.00495   -0.02494    0.01004
AFIX  43
H11   2    0.542388    0.196768   -0.144660    11.00000   -1.20000
AFIX   0
C12   1    0.602590    0.143367   -0.088314    11.00000    0.02999    0.02265 =
         0.03397   -0.00158   -0.01223    0.00027
AFIX  43
H12   2    0.627776    0.144569   -0.233914    11.00000   -1.20000
AFIX   0
C13   1    0.636923    0.018267    0.012974    11.00000    0.01533    0.01655 =
         0.01801   -0.00336    0.00140    0.00286
C14   1    0.592427    0.005758   -0.171678    11.00000    0.02877    0.02525 =
         0.02284    0.00353   -0.00352   -0.00168
AFIX  43
H14   2    0.584790    0.024762   -0.300382    11.00000   -1.20000
AFIX   0
C15   1    0.559133   -0.033930   -0.170745    11.00000    0.03023    0.02533 =
         0.02465   -0.00153   -0.00512   -0.00733
AFIX  43
H15   2    0.528615   -0.041977   -0.297532    11.00000   -1.20000
AFIX   0
C16   1    0.570397   -0.061870    0.015315    11.00000    0.01878    0.01516 =
         0.03407   -0.00546    0.00266   -0.00277
AFIX  43
H16   2    0.547608   -0.089157    0.016252    11.00000   -1.20000
AFIX   0
C17   1    0.614370   -0.050260    0.198288    11.00000    0.03000    0.01932 =
         0.02707    0.00697   -0.00412   -0.00260
AFIX  43
H17   2    0.622510   -0.069660    0.324857    11.00000   -1.20000
AFIX   0
C18   1    0.647280   -0.009918    0.199071    11.00000    0.03004    0.02118 =
         0.02382    0.00200   -0.00748   -0.00317
AFIX  43
H18   2    0.676915   -0.001783    0.327938    11.00000   -1.20000
AFIX   0
C19   1    0.908806    0.250000    0.943201    10.50000    0.16201    0.07350 =
         0.06713    0.00000   -0.09015    0.00000
AFIX 137
H19A  2    0.948674    0.253126    1.054656    10.50000   -1.50000
H19B  2    0.883765    0.222886    0.973587    10.50000   -1.50000
H19C  2    0.875307    0.273988    0.963023    10.50000   -1.50000
AFIX   0
O3    4    0.935665    0.250000    0.710649    10.50000    0.02636    0.03178 =
         0.12148    0.00000   -0.02770    0.00000
AFIX  83
H3A   2    0.904707    0.239656    0.619131    10.50000   -1.50000
 
HKLF 4 1 1 0 0 0 1 0 0 0 1
 
REM  rpso583 in Pnma
REM R1 =  0.0476 for   2128 Fo > 4sig(Fo)  and  0.0870 for all   3186 data
REM    218 parameters refined using      0 restraints
 
END  
     
WGHT      0.0441      1.5969 
REM Highest difference peak  0.251,  deepest hole -0.357,  1-sigma level  0.061
Q1    1   0.8863  0.2500  0.9884  10.50000  0.05    0.25
Q2    1   0.6581  0.0977  0.0782  11.00000  0.05    0.25
Q3    1   0.9812  0.2500  0.9766  10.50000  0.05    0.24
Q4    1   0.6996  0.0699  0.1749  11.00000  0.05    0.23
Q5    1   0.6299  0.0135  0.1373  11.00000  0.05    0.23
Q6    1   1.0190  0.2500  0.6663  10.50000  0.05    0.23
Q7    1   0.6812  0.0662  0.4121  11.00000  0.05    0.22
Q8    1   0.7842  0.2319  0.4706  11.00000  0.05    0.22
Q9    1   0.8747  0.2500  0.3882  10.50000  0.05    0.21
Q10   1   0.6408  0.0933  0.0165  11.00000  0.05    0.21
;
_database_code_depnum_ccdc_archive 'CCDC 977757'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rpso675

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C35 H38 La N5 O14 P2'
_chemical_formula_weight         953.55

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pca2(1)

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

_cell_length_a                   24.7829(16)
_cell_length_b                   8.7977(6)
_cell_length_c                   18.1338(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3953.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9904
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      26.73

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7478
_exptl_absorpt_correction_T_max  0.8762
_exptl_absorpt_process_details   'Bruker, SADABs'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(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 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47044
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0378
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         26.76
_reflns_number_total             8387
_reflns_number_gt                7627
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_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    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0203P)²+0.0073P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.017(7)
_refine_ls_number_reflns         8387
_refine_ls_number_parameters     517
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0495
_refine_ls_wR_factor_gt          0.0476
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_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
La1 La 0.128995(5) -0.399502(14) 0.001890(9) 0.01233(4) Uani 1 1 d . . .
O1 O 0.11323(8) -0.1350(2) 0.05533(10) 0.0179(4) Uani 1 1 d . . .
O2 O 0.07116(7) -0.2561(2) -0.08430(10) 0.0180(4) Uani 1 1 d . . .
O3 O 0.15503(8) 0.5929(2) 0.12991(10) 0.0171(4) Uani 1 1 d . . .
O4 O 0.17707(8) -0.4939(2) -0.11741(11) 0.0206(4) Uani 1 1 d . . .
O5 O 0.09727(8) -0.5890(2) -0.10378(11) 0.0204(4) Uani 1 1 d . . .
O6 O 0.14612(11) -0.6496(3) -0.19925(14) 0.0540(8) Uani 1 1 d . . .
O7 O 0.19554(7) -0.1863(2) -0.05198(11) 0.0223(4) Uani 1 1 d . . .
O8 O 0.23454(7) -0.36936(19) 0.00654(15) 0.0218(4) Uani 1 1 d . . .
O9 O 0.28219(8) -0.1802(3) -0.03467(12) 0.0325(5) Uani 1 1 d . . .
O10 O 0.03677(8) -0.3697(2) 0.07964(12) 0.0228(5) Uani 1 1 d . . .
O11 O 0.05544(8) -0.5958(2) 0.04238(11) 0.0236(5) Uani 1 1 d . . .
O12 O -0.00797(10) -0.5605(3) 0.12369(14) 0.0435(7) Uani 1 1 d . . .
O13 O 0.17039(7) -0.6657(2) 0.03439(10) 0.0182(4) Uani 1 1 d . . .
H13A H 0.1525 -0.7151 0.0741 0.022 Uiso 1 1 calc R . .
O14 O 0.18099(8) 0.4693(3) 0.57317(12) 0.0322(5) Uani 1 1 d . . .
H14A H 0.2049 0.5281 0.5569 0.048 Uiso 1 1 calc R . .
P1 P 0.05106(3) -0.09629(8) -0.09246(4) 0.01476(14) Uani 1 1 d . . .
P2 P 0.18681(3) 0.58696(8) 0.20038(4) 0.01530(15) Uani 1 1 d . . .
N1 N 0.15901(9) 0.2298(3) 0.18557(12) 0.0159(5) Uani 1 1 d . . .
N2 N 0.08259(9) 0.0966(3) 0.08600(14) 0.0194(5) Uani 1 1 d . . .
H2A H 0.0733 0.1879 0.0707 0.023 Uiso 1 1 calc R . .
N3 N 0.14009(10) -0.5788(3) -0.14227(14) 0.0249(6) Uani 1 1 d . . .
N4 N 0.23879(10) -0.2433(3) -0.02759(13) 0.0214(5) Uani 1 1 d . . .
N5 N 0.02649(9) -0.5089(3) 0.08312(13) 0.0230(6) Uani 1 1 d . . .
C1 C 0.19903(11) 0.2783(3) 0.23058(15) 0.0173(6) Uani 1 1 d . . .
C2 C 0.21175(12) 0.2070(3) 0.29626(15) 0.0213(6) Uani 1 1 d . . .
H2 H 0.2401 0.2449 0.3264 0.026 Uiso 1 1 calc R . .
C3 C 0.18280(12) 0.0799(3) 0.31771(17) 0.0251(7) Uani 1 1 d . . .
H3 H 0.1916 0.0273 0.3619 0.030 Uiso 1 1 calc R . .
C4 C 0.14107(12) 0.0317(3) 0.27362(16) 0.0228(6) Uani 1 1 d . . .
H4 H 0.1200 -0.0538 0.2875 0.027 Uiso 1 1 calc R . .
C5 C 0.12989(11) 0.1092(3) 0.20834(16) 0.0186(6) Uani 1 1 d . . .
C6 C 0.08094(12) 0.0637(3) 0.16469(16) 0.0216(6) Uani 1 1 d . . .
H6A H 0.0754 -0.0469 0.1710 0.026 Uiso 1 1 calc R . .
H6B H 0.0492 0.1158 0.1860 0.026 Uiso 1 1 calc R . .
C7 C 0.09753(12) -0.0061(4) 0.03682(17) 0.0157(6) Uani 1 1 d . . .
C8 C 0.09397(12) 0.0372(3) -0.04375(16) 0.0165(7) Uani 1 1 d . . .
H8A H 0.1305 0.0368 -0.0658 0.020 Uiso 1 1 calc R . .
H8B H 0.0790 0.1411 -0.0484 0.020 Uiso 1 1 calc R . .
C9 C -0.01605(11) -0.0744(3) -0.05630(15) 0.0170(6) Uani 1 1 d . . .
C10 C -0.04543(11) -0.2041(4) -0.03908(17) 0.0257(7) Uani 1 1 d . . .
H10 H -0.0294 -0.3015 -0.0450 0.031 Uiso 1 1 calc R . .
C11 C -0.09795(11) -0.1926(3) -0.01323(16) 0.0275(8) Uani 1 1 d . . .
H11 H -0.1179 -0.2817 -0.0018 0.033 Uiso 1 1 calc R . .
C12 C -0.12084(10) -0.0521(3) -0.0043(3) 0.0253(7) Uani 1 1 d . . .
H12 H -0.1568 -0.0439 0.0133 0.030 Uiso 1 1 calc R . .
C13 C -0.09217(13) 0.0767(4) -0.02045(17) 0.0332(8) Uani 1 1 d . . .
H13 H -0.1082 0.1738 -0.0138 0.040 Uiso 1 1 calc R . .
C14 C -0.03952(13) 0.0656(3) -0.04658(18) 0.0281(7) Uani 1 1 d . . .
H14 H -0.0197 0.1552 -0.0577 0.034 Uiso 1 1 calc R . .
C15 C 0.05112(10) -0.0392(3) -0.18732(15) 0.0164(6) Uani 1 1 d . . .
C16 C 0.04649(11) 0.1128(3) -0.20795(16) 0.0208(6) Uani 1 1 d . . .
H16 H 0.0443 0.1893 -0.1711 0.025 Uiso 1 1 calc R . .
C17 C 0.04508(11) 0.1534(4) -0.28140(16) 0.0240(7) Uani 1 1 d . . .
H17 H 0.0411 0.2570 -0.2952 0.029 Uiso 1 1 calc R . .
C18 C 0.04952(11) 0.0417(4) -0.33493(16) 0.0248(7) Uani 1 1 d . . .
H18 H 0.0487 0.0693 -0.3856 0.030 Uiso 1 1 calc R . .
C19 C 0.05513(12) -0.1089(4) -0.31545(17) 0.0252(7) Uani 1 1 d . . .
H19 H 0.0586 -0.1844 -0.3526 0.030 Uiso 1 1 calc R . .
C20 C 0.05566(11) -0.1504(3) -0.24159(16) 0.0219(6) Uani 1 1 d . . .
H20 H 0.0591 -0.2543 -0.2281 0.026 Uiso 1 1 calc R . .
C21 C 0.22916(11) 0.4193(3) 0.20721(16) 0.0183(6) Uani 1 1 d . . .
H21A H 0.2462 0.4004 0.1587 0.022 Uiso 1 1 calc R . .
H21B H 0.2583 0.4394 0.2432 0.022 Uiso 1 1 calc R . .
C22 C 0.14074(12) 0.5826(3) 0.27693(16) 0.0184(6) Uani 1 1 d . . .
C23 C 0.08526(12) 0.5889(3) 0.26152(17) 0.0242(7) Uani 1 1 d . . .
H23 H 0.0731 0.6002 0.2121 0.029 Uiso 1 1 calc R . .
C24 C 0.04820(13) 0.5784(3) 0.31857(19) 0.0287(7) Uani 1 1 d . . .
H24 H 0.0106 0.5810 0.3083 0.034 Uiso 1 1 calc R . .
C25 C 0.06595(15) 0.5643(3) 0.39007(19) 0.0330(8) Uani 1 1 d . . .
H25 H 0.0405 0.5594 0.4292 0.040 Uiso 1 1 calc R . .
C26 C 0.12049(16) 0.5571(4) 0.40565(19) 0.0328(9) Uani 1 1 d . . .
H26 H 0.1323 0.5466 0.4553 0.039 Uiso 1 1 calc R . .
C27 C 0.15808(14) 0.5651(3) 0.34911(17) 0.0246(7) Uani 1 1 d . . .
H27 H 0.1955 0.5587 0.3598 0.030 Uiso 1 1 calc R . .
C28 C 0.23228(11) 0.7447(3) 0.20811(16) 0.0164(6) Uani 1 1 d . . .
C29 C 0.23151(11) 0.8586(3) 0.15468(15) 0.0185(6) Uani 1 1 d . . .
H29 H 0.2057 0.8547 0.1160 0.022 Uiso 1 1 calc R . .
C30 C 0.26829(11) 0.9779(3) 0.15774(16) 0.0205(6) Uani 1 1 d . . .
H30 H 0.2683 1.0536 0.1204 0.025 Uiso 1 1 calc R . .
C31 C 0.30501(11) 0.9862(3) 0.21544(16) 0.0222(7) Uani 1 1 d . . .
H31 H 0.3298 1.0684 0.2181 0.027 Uiso 1 1 calc R . .
C32 C 0.30544(12) 0.8750(3) 0.26869(17) 0.0234(7) Uani 1 1 d . . .
H32 H 0.3306 0.8809 0.3081 0.028 Uiso 1 1 calc R . .
C33 C 0.26970(12) 0.7550(3) 0.26555(16) 0.0196(7) Uani 1 1 d . . .
H33 H 0.2705 0.6789 0.3027 0.023 Uiso 1 1 calc R . .
C34 C 0.21425(10) -0.7518(3) 0.0048(2) 0.0248(6) Uani 1 1 d . . .
H34A H 0.2172 -0.7323 -0.0482 0.037 Uiso 1 1 calc R . .
H34B H 0.2077 -0.8603 0.0131 0.037 Uiso 1 1 calc R . .
H34C H 0.2479 -0.7217 0.0293 0.037 Uiso 1 1 calc R . .
C35 C 0.14428(16) 0.5533(5) 0.6188(2) 0.0442(11) Uani 1 1 d . . .
H35A H 0.1639 0.6348 0.6442 0.066 Uiso 1 1 calc R . .
H35B H 0.1281 0.4850 0.6553 0.066 Uiso 1 1 calc R . .
H35C H 0.1158 0.5975 0.5881 0.066 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
La1 O3 2.4105(18) 1_545 ?
La1 O2 2.4673(18) . ?
La1 O1 2.5512(19) . ?
La1 O4 2.6057(19) . ?
La1 O11 2.6165(19) . ?
La1 O13 2.6239(18) . ?
La1 O8 2.6305(16) . ?
La1 O5 2.6588(19) . ?
La1 O7 2.6817(19) . ?
La1 O10 2.698(2) . ?
La1 N3 3.066(3) . ?
O1 C7 1.245(4) . ?
O2 P1 1.4994(19) . ?
O3 P2 1.502(2) . ?
O3 La1 2.4104(18) 1_565 ?
O4 N3 1.265(3) . ?
O5 N3 1.273(3) . ?
O6 N3 1.216(3) . ?
O7 N4 1.263(3) . ?
O8 N4 1.275(3) . ?
O9 N4 1.217(3) . ?
O10 N5 1.253(3) . ?
O11 N5 1.283(3) . ?
O12 N5 1.215(3) . ?
O13 C34 1.429(3) . ?
O14 C35 1.435(4) . ?
P1 C15 1.792(3) . ?
P1 C9 1.798(3) . ?
P1 C8 1.814(3) . ?
P2 C28 1.794(3) . ?
P2 C22 1.798(3) . ?
P2 C21 1.814(3) . ?
N1 C5 1.348(3) . ?
N1 C1 1.353(3) . ?
N2 C7 1.322(4) . ?
N2 C6 1.457(4) . ?
C1 C2 1.382(4) . ?
C1 C21 1.509(4) . ?
C2 C3 1.384(4) . ?
C3 C4 1.374(4) . ?
C4 C5 1.394(4) . ?
C5 C6 1.503(4) . ?
C7 C8 1.512(4) . ?
C9 C14 1.374(4) . ?
C9 C10 1.389(4) . ?
C10 C11 1.387(4) . ?
C11 C12 1.370(4) . ?
C12 C13 1.369(4) . ?
C13 C14 1.392(4) . ?
C15 C20 1.392(4) . ?
C15 C16 1.394(4) . ?
C16 C17 1.379(4) . ?
C17 C18 1.385(4) . ?
C18 C19 1.378(4) . ?
C19 C20 1.388(4) . ?
C22 C27 1.386(4) . ?
C22 C23 1.404(4) . ?
C23 C24 1.387(4) . ?
C24 C25 1.375(5) . ?
C25 C26 1.382(5) . ?
C26 C27 1.387(5) . ?
C28 C29 1.394(4) . ?
C28 C33 1.397(4) . ?
C29 C30 1.391(4) . ?
C30 C31 1.389(4) . ?
C31 C32 1.374(4) . ?
C32 C33 1.379(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 La1 O2 141.24(6) 1_545 . ?
O3 La1 O1 72.57(6) 1_545 . ?
O2 La1 O1 71.66(6) . . ?
O3 La1 O4 131.94(7) 1_545 . ?
O2 La1 O4 84.41(6) . . ?
O1 La1 O4 132.54(6) . . ?
O3 La1 O11 84.14(6) 1_545 . ?
O2 La1 O11 96.34(6) . . ?
O1 La1 O11 112.89(6) . . ?
O4 La1 O11 109.95(6) . . ?
O3 La1 O13 69.77(6) 1_545 . ?
O2 La1 O13 145.66(6) . . ?
O1 La1 O13 142.08(6) . . ?
O4 La1 O13 73.94(6) . . ?
O11 La1 O13 67.68(6) . . ?
O3 La1 O8 72.89(8) 1_545 . ?
O2 La1 O8 123.12(7) . . ?
O1 La1 O8 92.76(6) . . ?
O4 La1 O8 66.68(7) . . ?
O11 La1 O8 138.62(6) . . ?
O13 La1 O8 72.18(6) . . ?
O3 La1 O5 139.10(6) 1_545 . ?
O2 La1 O5 72.07(6) . . ?
O1 La1 O5 143.18(6) . . ?
O4 La1 O5 48.47(6) . . ?
O11 La1 O5 65.31(6) . . ?
O13 La1 O5 73.61(6) . . ?
O8 La1 O5 112.36(7) . . ?
O3 La1 O7 101.87(6) 1_545 . ?
O2 La1 O7 76.64(6) . . ?
O1 La1 O7 66.08(6) . . ?
O4 La1 O7 68.85(6) . . ?
O11 La1 O7 172.93(6) . . ?
O13 La1 O7 117.75(6) . . ?
O8 La1 O7 47.91(6) . . ?
O5 La1 O7 110.96(6) . . ?
O3 La1 O10 74.11(6) 1_545 . ?
O2 La1 O10 77.83(6) . . ?
O1 La1 O10 65.36(6) . . ?
O4 La1 O10 148.45(6) . . ?
O11 La1 O10 47.73(6) . . ?
O13 La1 O10 107.50(6) . . ?
O8 La1 O10 144.66(7) . . ?
O5 La1 O10 100.79(6) . . ?
O7 La1 O10 130.03(6) . . ?
O3 La1 N3 141.53(7) 1_545 . ?
O2 La1 N3 77.00(6) . . ?
O1 La1 N3 143.81(6) . . ?
O4 La1 N3 24.08(6) . . ?
O11 La1 N3 87.83(6) . . ?
O13 La1 N3 72.37(6) . . ?
O8 La1 N3 89.43(7) . . ?
O5 La1 N3 24.40(6) . . ?
O7 La1 N3 89.66(6) . . ?
O10 La1 N3 124.86(6) . . ?
C7 O1 La1 140.93(18) . . ?
P1 O2 La1 137.31(11) . . ?
P2 O3 La1 163.89(12) . 1_565 ?
N3 O4 La1 98.78(15) . . ?
N3 O5 La1 95.99(15) . . ?
N4 O7 La1 96.71(15) . . ?
N4 O8 La1 98.87(14) . . ?
N5 O10 La1 95.93(15) . . ?
N5 O11 La1 99.08(15) . . ?
C34 O13 La1 133.31(17) . . ?
O2 P1 C15 110.93(12) . . ?
O2 P1 C9 111.82(12) . . ?
C15 P1 C9 108.72(12) . . ?
O2 P1 C8 111.38(12) . . ?
C15 P1 C8 106.59(14) . . ?
C9 P1 C8 107.18(14) . . ?
O3 P2 C28 111.66(12) . . ?
O3 P2 C22 108.95(13) . . ?
C28 P2 C22 110.81(13) . . ?
O3 P2 C21 112.93(12) . . ?
C28 P2 C21 105.08(13) . . ?
C22 P2 C21 107.29(13) . . ?
C5 N1 C1 117.1(2) . . ?
C7 N2 C6 122.2(2) . . ?
O6 N3 O4 121.1(3) . . ?
O6 N3 O5 122.1(3) . . ?
O4 N3 O5 116.7(2) . . ?
O6 N3 La1 178.1(2) . . ?
O4 N3 La1 57.14(13) . . ?
O5 N3 La1 59.61(13) . . ?
O9 N4 O7 122.1(3) . . ?
O9 N4 O8 121.4(2) . . ?
O7 N4 O8 116.4(2) . . ?
O12 N5 O10 122.6(3) . . ?
O12 N5 O11 121.3(2) . . ?
O10 N5 O11 116.1(2) . . ?
N1 C1 C2 123.0(3) . . ?
N1 C1 C21 116.9(2) . . ?
C2 C1 C21 120.1(3) . . ?
C1 C2 C3 119.4(3) . . ?
C4 C3 C2 118.4(3) . . ?
C3 C4 C5 119.5(3) . . ?
N1 C5 C4 122.6(3) . . ?
N1 C5 C6 118.7(2) . . ?
C4 C5 C6 118.5(3) . . ?
N2 C6 C5 116.1(2) . . ?
O1 C7 N2 121.9(3) . . ?
O1 C7 C8 120.5(3) . . ?
N2 C7 C8 117.6(3) . . ?
C7 C8 P1 110.0(2) . . ?
C14 C9 C10 119.1(3) . . ?
C14 C9 P1 122.3(2) . . ?
C10 C9 P1 118.6(2) . . ?
C11 C10 C9 120.5(3) . . ?
C12 C11 C10 119.6(3) . . ?
C13 C12 C11 120.4(3) . . ?
C12 C13 C14 120.1(3) . . ?
C9 C14 C13 120.2(3) . . ?
C20 C15 C16 119.4(3) . . ?
C20 C15 P1 118.8(2) . . ?
C16 C15 P1 121.8(2) . . ?
C17 C16 C15 120.6(3) . . ?
C16 C17 C18 119.4(3) . . ?
C19 C18 C17 120.7(3) . . ?
C18 C19 C20 120.1(3) . . ?
C19 C20 C15 119.8(3) . . ?
C1 C21 P2 113.65(19) . . ?
C27 C22 C23 119.7(3) . . ?
C27 C22 P2 122.3(2) . . ?
C23 C22 P2 117.9(2) . . ?
C24 C23 C22 119.8(3) . . ?
C25 C24 C23 119.8(3) . . ?
C24 C25 C26 120.7(3) . . ?
C25 C26 C27 120.2(3) . . ?
C22 C27 C26 119.7(3) . . ?
C29 C28 C33 118.7(3) . . ?
C29 C28 P2 119.6(2) . . ?
C33 C28 P2 121.7(2) . . ?
C30 C29 C28 120.4(3) . . ?
C31 C30 C29 120.0(3) . . ?
C32 C31 C30 119.8(3) . . ?
C31 C32 C33 120.7(3) . . ?
C32 C33 C28 120.4(3) . . ?

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
O3 La1 O1 C7 178.7(3) 1_545 . . . ?
O2 La1 O1 C7 -16.5(3) . . . . ?
O4 La1 O1 C7 47.2(3) . . . . ?
O11 La1 O1 C7 -105.7(3) . . . . ?
O13 La1 O1 C7 171.7(3) . . . . ?
O8 La1 O1 C7 107.6(3) . . . . ?
O5 La1 O1 C7 -26.8(3) . . . . ?
O7 La1 O1 C7 66.7(3) . . . . ?
O10 La1 O1 C7 -101.2(3) . . . . ?
N3 La1 O1 C7 14.8(3) . . . . ?
O3 La1 O2 P1 31.2(2) 1_545 . . . ?
O1 La1 O2 P1 7.68(15) . . . . ?
O4 La1 O2 P1 -130.75(16) . . . . ?
O11 La1 O2 P1 119.74(16) . . . . ?
O13 La1 O2 P1 178.75(12) . . . . ?
O8 La1 O2 P1 -73.35(17) . . . . ?
O5 La1 O2 P1 -178.80(18) . . . . ?
O7 La1 O2 P1 -61.19(16) . . . . ?
O10 La1 O2 P1 75.48(16) . . . . ?
N3 La1 O2 P1 -153.98(17) . . . . ?
O3 La1 O4 N3 124.70(16) 1_545 . . . ?
O2 La1 O4 N3 -70.41(16) . . . . ?
O1 La1 O4 N3 -129.15(16) . . . . ?
O11 La1 O4 N3 24.32(18) . . . . ?
O13 La1 O4 N3 82.65(16) . . . . ?
O8 La1 O4 N3 159.78(18) . . . . ?
O5 La1 O4 N3 0.53(15) . . . . ?
O7 La1 O4 N3 -148.23(18) . . . . ?
O10 La1 O4 N3 -14.8(2) . . . . ?
O3 La1 O5 N3 -110.48(16) 1_545 . . . ?
O2 La1 O5 N3 98.09(16) . . . . ?
O1 La1 O5 N3 108.38(17) . . . . ?
O4 La1 O5 N3 -0.52(15) . . . . ?
O11 La1 O5 N3 -155.86(17) . . . . ?
O13 La1 O5 N3 -83.35(15) . . . . ?
O8 La1 O5 N3 -21.12(17) . . . . ?
O7 La1 O5 N3 30.67(16) . . . . ?
O10 La1 O5 N3 171.40(15) . . . . ?
O3 La1 O7 N4 51.92(15) 1_545 . . . ?
O2 La1 O7 N4 -167.81(16) . . . . ?
O1 La1 O7 N4 116.58(16) . . . . ?
O4 La1 O7 N4 -78.70(15) . . . . ?
O13 La1 O7 N4 -21.30(16) . . . . ?
O8 La1 O7 N4 -1.56(14) . . . . ?
O5 La1 O7 N4 -103.26(15) . . . . ?
O10 La1 O7 N4 131.03(14) . . . . ?
N3 La1 O7 N4 -91.10(15) . . . . ?
O3 La1 O8 N4 -123.06(17) 1_545 . . . ?
O2 La1 O8 N4 17.59(19) . . . . ?
O1 La1 O8 N4 -52.25(17) . . . . ?
O4 La1 O8 N4 83.51(17) . . . . ?
O11 La1 O8 N4 177.68(14) . . . . ?
O13 La1 O8 N4 163.26(18) . . . . ?
O5 La1 O8 N4 100.17(16) . . . . ?
O7 La1 O8 N4 1.56(14) . . . . ?
O10 La1 O8 N4 -101.42(19) . . . . ?
N3 La1 O8 N4 91.61(17) . . . . ?
O3 La1 O10 N5 -90.43(16) 1_545 . . . ?
O2 La1 O10 N5 116.60(16) . . . . ?
O1 La1 O10 N5 -168.19(17) . . . . ?
O4 La1 O10 N5 59.4(2) . . . . ?
O11 La1 O10 N5 6.19(14) . . . . ?
O13 La1 O10 N5 -28.25(17) . . . . ?
O8 La1 O10 N5 -111.93(16) . . . . ?
O5 La1 O10 N5 47.80(16) . . . . ?
O7 La1 O10 N5 177.27(14) . . . . ?
N3 La1 O10 N5 52.12(18) . . . . ?
O3 La1 O11 N5 67.72(15) 1_545 . . . ?
O2 La1 O11 N5 -73.29(16) . . . . ?
O1 La1 O11 N5 -0.55(17) . . . . ?
O4 La1 O11 N5 -159.62(15) . . . . ?
O13 La1 O11 N5 138.23(17) . . . . ?
O8 La1 O11 N5 123.39(16) . . . . ?
O5 La1 O11 N5 -140.21(17) . . . . ?
O10 La1 O11 N5 -6.10(14) . . . . ?
N3 La1 O11 N5 -149.94(16) . . . . ?
O3 La1 O13 C34 -123.9(2) 1_545 . . . ?
O2 La1 O13 C34 77.1(3) . . . . ?
O1 La1 O13 C34 -116.8(2) . . . . ?
O4 La1 O13 C34 24.1(2) . . . . ?
O11 La1 O13 C34 144.2(2) . . . . ?
O8 La1 O13 C34 -46.0(2) . . . . ?
O5 La1 O13 C34 74.7(2) . . . . ?
O7 La1 O13 C34 -30.8(3) . . . . ?
O10 La1 O13 C34 171.1(2) . . . . ?
N3 La1 O13 C34 49.2(2) . . . . ?
La1 O2 P1 C15 140.43(15) . . . . ?
La1 O2 P1 C9 -98.02(17) . . . . ?
La1 O2 P1 C8 21.9(2) . . . . ?
La1 O3 P2 C28 59.0(4) 1_565 . . . ?
La1 O3 P2 C22 -178.2(4) 1_565 . . . ?
La1 O3 P2 C21 -59.1(4) 1_565 . . . ?
La1 O4 N3 O6 -179.2(3) . . . . ?
La1 O4 N3 O5 -0.9(3) . . . . ?
La1 O5 N3 O6 179.1(3) . . . . ?
La1 O5 N3 O4 0.9(3) . . . . ?
O3 La1 N3 O4 -79.45(19) 1_545 . . . ?
O2 La1 N3 O4 105.77(17) . . . . ?
O1 La1 N3 O4 75.4(2) . . . . ?
O11 La1 N3 O4 -157.21(17) . . . . ?
O13 La1 N3 O4 -89.96(17) . . . . ?
O8 La1 N3 O4 -18.50(16) . . . . ?
O5 La1 N3 O4 -179.0(3) . . . . ?
O7 La1 N3 O4 29.41(16) . . . . ?
O10 La1 N3 O4 170.65(15) . . . . ?
O3 La1 N3 O5 99.59(17) 1_545 . . . ?
O2 La1 N3 O5 -75.19(15) . . . . ?
O1 La1 N3 O5 -105.57(16) . . . . ?
O4 La1 N3 O5 179.0(3) . . . . ?
O11 La1 N3 O5 21.83(15) . . . . ?
O13 La1 N3 O5 89.08(15) . . . . ?
O8 La1 N3 O5 160.54(15) . . . . ?
O7 La1 N3 O5 -151.55(15) . . . . ?
O10 La1 N3 O5 -10.31(18) . . . . ?
La1 O7 N4 O9 -175.8(2) . . . . ?
La1 O7 N4 O8 2.7(2) . . . . ?
La1 O8 N4 O9 175.7(2) . . . . ?
La1 O8 N4 O7 -2.7(2) . . . . ?
La1 O10 N5 O12 168.0(2) . . . . ?
La1 O10 N5 O11 -10.5(2) . . . . ?
La1 O11 N5 O12 -167.6(2) . . . . ?
La1 O11 N5 O10 10.9(2) . . . . ?
C5 N1 C1 C2 2.1(4) . . . . ?
C5 N1 C1 C21 -176.2(2) . . . . ?
N1 C1 C2 C3 0.2(4) . . . . ?
C21 C1 C2 C3 178.4(3) . . . . ?
C1 C2 C3 C4 -2.0(4) . . . . ?
C2 C3 C4 C5 1.4(4) . . . . ?
C1 N1 C5 C4 -2.6(4) . . . . ?
C1 N1 C5 C6 172.6(2) . . . . ?
C3 C4 C5 N1 0.9(4) . . . . ?
C3 C4 C5 C6 -174.3(3) . . . . ?
C7 N2 C6 C5 95.8(3) . . . . ?
N1 C5 C6 N2 29.8(4) . . . . ?
C4 C5 C6 N2 -154.7(3) . . . . ?
La1 O1 C7 N2 163.2(2) . . . . ?
La1 O1 C7 C8 -15.7(5) . . . . ?
C6 N2 C7 O1 -3.1(4) . . . . ?
C6 N2 C7 C8 175.8(3) . . . . ?
O1 C7 C8 P1 56.3(4) . . . . ?
N2 C7 C8 P1 -122.6(2) . . . . ?
O2 P1 C8 C7 -57.1(3) . . . . ?
C15 P1 C8 C7 -178.2(2) . . . . ?
C9 P1 C8 C7 65.5(2) . . . . ?
O2 P1 C9 C14 169.1(2) . . . . ?
C15 P1 C9 C14 -68.1(3) . . . . ?
C8 P1 C9 C14 46.8(3) . . . . ?
O2 P1 C9 C10 -12.2(3) . . . . ?
C15 P1 C9 C10 110.6(2) . . . . ?
C8 P1 C9 C10 -134.5(2) . . . . ?
C14 C9 C10 C11 0.7(4) . . . . ?
P1 C9 C10 C11 -178.0(2) . . . . ?
C9 C10 C11 C12 -0.4(5) . . . . ?
C10 C11 C12 C13 -0.2(6) . . . . ?
C11 C12 C13 C14 0.4(6) . . . . ?
C10 C9 C14 C13 -0.6(5) . . . . ?
P1 C9 C14 C13 178.1(2) . . . . ?
C12 C13 C14 C9 0.0(5) . . . . ?
O2 P1 C15 C20 15.6(2) . . . . ?
C9 P1 C15 C20 -107.8(2) . . . . ?
C8 P1 C15 C20 137.0(2) . . . . ?
O2 P1 C15 C16 -164.7(2) . . . . ?
C9 P1 C15 C16 71.9(2) . . . . ?
C8 P1 C15 C16 -43.3(3) . . . . ?
C20 C15 C16 C17 1.5(4) . . . . ?
P1 C15 C16 C17 -178.1(2) . . . . ?
C15 C16 C17 C18 -1.4(4) . . . . ?
C16 C17 C18 C19 0.2(4) . . . . ?
C17 C18 C19 C20 0.9(4) . . . . ?
C18 C19 C20 C15 -0.7(4) . . . . ?
C16 C15 C20 C19 -0.5(4) . . . . ?
P1 C15 C20 C19 179.2(2) . . . . ?
N1 C1 C21 P2 61.5(3) . . . . ?
C2 C1 C21 P2 -116.9(2) . . . . ?
O3 P2 C21 C1 -79.9(2) . . . . ?
C28 P2 C21 C1 158.2(2) . . . . ?
C22 P2 C21 C1 40.2(2) . . . . ?
O3 P2 C22 C27 174.9(2) . . . . ?
C28 P2 C22 C27 -61.8(3) . . . . ?
C21 P2 C22 C27 52.4(3) . . . . ?
O3 P2 C22 C23 -1.5(3) . . . . ?
C28 P2 C22 C23 121.7(2) . . . . ?
C21 P2 C22 C23 -124.1(2) . . . . ?
C27 C22 C23 C24 0.3(4) . . . . ?
P2 C22 C23 C24 176.9(2) . . . . ?
C22 C23 C24 C25 1.0(4) . . . . ?
C23 C24 C25 C26 -1.4(5) . . . . ?
C24 C25 C26 C27 0.4(5) . . . . ?
C23 C22 C27 C26 -1.3(4) . . . . ?
P2 C22 C27 C26 -177.7(2) . . . . ?
C25 C26 C27 C22 0.9(5) . . . . ?
O3 P2 C28 C29 4.7(3) . . . . ?
C22 P2 C28 C29 -116.9(2) . . . . ?
C21 P2 C28 C29 127.5(2) . . . . ?
O3 P2 C28 C33 -173.6(2) . . . . ?
C22 P2 C28 C33 64.7(3) . . . . ?
C21 P2 C28 C33 -50.8(3) . . . . ?
C33 C28 C29 C30 1.6(4) . . . . ?
P2 C28 C29 C30 -176.8(2) . . . . ?
C28 C29 C30 C31 -1.8(4) . . . . ?
C29 C30 C31 C32 1.1(4) . . . . ?
C30 C31 C32 C33 -0.1(4) . . . . ?
C31 C32 C33 C28 -0.2(4) . . . . ?
C29 C28 C33 C32 -0.6(4) . . . . ?
P2 C28 C33 C32 177.7(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O13 H13A N1 0.95 2.09 2.905(3) 143.5 1_545
O13 H13A N2 0.95 2.41 3.159(3) 136.0 1_545
O14 H14A O8 0.84 1.97 2.803(3) 168.5 3_565
N2 H2A O11 0.88 2.02 2.898(3) 175.4 1_565

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.76
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.063
_iucr_refine_instruction_details 
;
TITL rpso675 in Pca2(1)
CELL 0.71073 24.7829 8.7977 18.1338 90.000 90.000 90.000
ZERR 4.00 0.0016 0.0006 0.0012 0.000 0.000 0.000
LATT -1
SYMM -x, -y, z+1/2
SYMM -x+1/2, y, z+1/2
SYMM x+1/2, -y, z
SFAC C  H  N  O  P  La
UNIT 140  152  20  56  8  4
L.S. 10
ACTA
BOND
CONF
EQIV $1 x, y-1, z
EQIV $2 -x+1/2, y+1, z+1/2
EQIV $3 x, y+1, z
HTAB O13 N1_$1
HTAB O13 N2_$1
HTAB O14 O8_$2
HTAB N2 O11_$3
OMIT 2   0   1
OMIT 2   0  -1
OMIT 0   0   2
OMIT 0   0  -2
OMIT 1   1   0
OMIT 0   1   0
OMIT 2   1   0
OMIT 2   0   2
OMIT 2   0  -2
OMIT 1   1  -1
OMIT 1   1   1
OMIT 2   0   0
FMAP 2
PLAN 10
SIZE 0.110 0.230 0.250
TEMP -173.120
WGHT    0.020300    0.007300
FVAR       0.09654
LA1   6    0.128995   -0.399502    0.001890    11.00000    0.01264    0.01143 =
         0.01292    0.00081   -0.00107    0.00064
O1    4    0.113231   -0.134954    0.055327    11.00000    0.02211    0.01411 =
         0.01760    0.00114   -0.00462    0.00275
O2    4    0.071159   -0.256150   -0.084297    11.00000    0.01711    0.01655 =
         0.02048   -0.00109   -0.00510    0.00230
O3    4    0.155031    0.592884    0.129913    11.00000    0.01792    0.01715 =
         0.01613    0.00181   -0.00259    0.00232
O4    4    0.177071   -0.493884   -0.117415    11.00000    0.02436    0.01981 =
         0.01768   -0.00258    0.00227   -0.00594
O5    4    0.097271   -0.588993   -0.103785    11.00000    0.02089    0.01947 =
         0.02069   -0.00218    0.00101   -0.00042
O6    4    0.146119   -0.649641   -0.199250    11.00000    0.05464    0.07168 =
         0.03554   -0.03597    0.02086   -0.03172
O7    4    0.195537   -0.186319   -0.051984    11.00000    0.01569    0.01993 =
         0.03115    0.00414   -0.00005    0.00042
O8    4    0.234543   -0.369355    0.006542    11.00000    0.01834    0.02460 =
         0.02254    0.00384    0.00211   -0.00076
O9    4    0.282189   -0.180160   -0.034669    11.00000    0.01837    0.04019 =
         0.03905    0.00094    0.00431   -0.01559
O10   4    0.036772   -0.369655    0.079644    11.00000    0.02252    0.01487 =
         0.03095    0.00018    0.00179    0.00281
O11   4    0.055437   -0.595837    0.042382    11.00000    0.02232    0.01786 =
         0.03070   -0.00046    0.00597    0.00083
O12   4   -0.007966   -0.560520    0.123691    11.00000    0.03256    0.03920 =
         0.05877    0.00283    0.02489   -0.01024
O13   4    0.170392   -0.665705    0.034395    11.00000    0.02156    0.01565 =
         0.01732    0.00238    0.00292    0.00478
AFIX  43
H13A  2    0.152520   -0.715130    0.074055    11.00000   -1.20000
AFIX   0
O14   4    0.180993    0.469336    0.573168    11.00000    0.02198    0.04270 =
         0.03190    0.00349    0.00498   -0.00598
AFIX 147
H14A  2    0.204913    0.528085    0.556897    11.00000   -1.50000
AFIX   0
P1    5    0.051058   -0.096288   -0.092458    11.00000    0.01519    0.01327 =
         0.01582    0.00041   -0.00385    0.00145
P2    5    0.186807    0.586958    0.200380    11.00000    0.01648    0.01597 =
         0.01346    0.00079   -0.00173    0.00133
N1    3    0.159015    0.229823    0.185568    11.00000    0.01766    0.01488 =
         0.01510   -0.00173    0.00102    0.00231
N2    3    0.082590    0.096637    0.085999    11.00000    0.02216    0.01285 =
         0.02308   -0.00151   -0.00271    0.00210
AFIX  43
H2A   2    0.073340    0.187901    0.070679    11.00000   -1.20000
AFIX   0
N3    3    0.140089   -0.578804   -0.142265    11.00000    0.02926    0.02661 =
         0.01874   -0.00308    0.00365   -0.00585
N4    3    0.238787   -0.243266   -0.027595    11.00000    0.02001    0.02529 =
         0.01877   -0.00670    0.00185   -0.00363
N5    3    0.026493   -0.508925    0.083120    11.00000    0.01453    0.02793 =
         0.02644    0.00203    0.00220    0.00113
C1    1    0.199025    0.278296    0.230583    11.00000    0.01948    0.01585 =
         0.01657   -0.00143    0.00222    0.00758
C2    1    0.211751    0.207036    0.296256    11.00000    0.02577    0.02293 =
         0.01528    0.00027   -0.00122    0.00517
AFIX  43
H2    2    0.240088    0.244912    0.326373    11.00000   -1.20000
AFIX   0
C3    1    0.182799    0.079932    0.317712    11.00000    0.03080    0.02630 =
         0.01816    0.00359    0.00506    0.01195
AFIX  43
H3    2    0.191570    0.027311    0.361861    11.00000   -1.20000
AFIX   0
C4    1    0.141066    0.031686    0.273625    11.00000    0.03015    0.01822 =
         0.02010    0.00327    0.00943    0.00191
AFIX  43
H4    2    0.119995   -0.053835    0.287543    11.00000   -1.20000
AFIX   0
C5    1    0.129888    0.109171    0.208336    11.00000    0.02176    0.01694 =
         0.01707   -0.00299    0.00642    0.00468
C6    1    0.080942    0.063715    0.164686    11.00000    0.02277    0.02017 =
         0.02192   -0.00205    0.00621   -0.00221
AFIX  23
H6A   2    0.075367   -0.046944    0.171025    11.00000   -1.20000
H6B   2    0.049159    0.115794    0.186026    11.00000   -1.20000
AFIX   0
C7    1    0.097525   -0.006059    0.036819    11.00000    0.01201    0.01517 =
         0.02002   -0.00103   -0.00541   -0.00296
C8    1    0.093968    0.037236   -0.043745    11.00000    0.01790    0.01338 =
         0.01820    0.00039   -0.00477   -0.00138
AFIX  23
H8A   2    0.130499    0.036810   -0.065835    11.00000   -1.20000
H8B   2    0.078994    0.141120   -0.048393    11.00000   -1.20000
AFIX   0
C9    1   -0.016047   -0.074433   -0.056300    11.00000    0.01836    0.02002 =
         0.01274    0.00227   -0.00330    0.00223
C10   1   -0.045433   -0.204118   -0.039076    11.00000    0.02090    0.01943 =
         0.03672   -0.00508   -0.00440   -0.00253
AFIX  43
H10   2   -0.029429   -0.301465   -0.045049    11.00000   -1.20000
AFIX   0
C11   1   -0.097952   -0.192638   -0.013225    11.00000    0.02182    0.02683 =
         0.03372   -0.00517    0.00094   -0.00605
AFIX  43
H11   2   -0.117938   -0.281719   -0.001794    11.00000   -1.20000
AFIX   0
C12   1   -0.120841   -0.052052   -0.004273    11.00000    0.01754    0.03929 =
         0.01907    0.00200   -0.00207    0.00169
AFIX  43
H12   2   -0.156843   -0.043882    0.013276    11.00000   -1.20000
AFIX   0
C13   1   -0.092169    0.076682   -0.020450    11.00000    0.03217    0.02993 =
         0.03763    0.00936    0.01024    0.01582
AFIX  43
H13   2   -0.108246    0.173755   -0.013826    11.00000   -1.20000
AFIX   0
C14   1   -0.039520    0.065648   -0.046579    11.00000    0.02973    0.01942 =
         0.03506    0.00793    0.00924    0.00695
AFIX  43
H14   2   -0.019742    0.155245   -0.057732    11.00000   -1.20000
AFIX   0
C15   1    0.051120   -0.039241   -0.187319    11.00000    0.01171    0.02060 =
         0.01682    0.00213   -0.00167    0.00094
C16   1    0.046485    0.112845   -0.207947    11.00000    0.02061    0.02057 =
         0.02118   -0.00121   -0.00019    0.00109
AFIX  43
H16   2    0.044273    0.189283   -0.171067    11.00000   -1.20000
AFIX   0
C17   1    0.045081    0.153394   -0.281404    11.00000    0.02183    0.02571 =
         0.02451    0.00828   -0.00066   -0.00497
AFIX  43
H17   2    0.041106    0.256981   -0.295165    11.00000   -1.20000
AFIX   0
C18   1    0.049517    0.041745   -0.334933    11.00000    0.01914    0.03857 =
         0.01658    0.00385    0.00215   -0.00400
AFIX  43
H18   2    0.048685    0.069266   -0.385578    11.00000   -1.20000
AFIX   0
C19   1    0.055125   -0.108865   -0.315454    11.00000    0.02204    0.03427 =
         0.01918   -0.00980   -0.00242   -0.00144
AFIX  43
H19   2    0.058630   -0.184351   -0.352607    11.00000   -1.20000
AFIX   0
C20   1    0.055658   -0.150366   -0.241587    11.00000    0.01876    0.02045 =
         0.02634   -0.00188   -0.00067    0.00291
AFIX  43
H20   2    0.059108   -0.254274   -0.228134    11.00000   -1.20000
AFIX   0
C21   1    0.229163    0.419336    0.207208    11.00000    0.01715    0.01869 =
         0.01909   -0.00140   -0.00283    0.00322
AFIX  23
H21A  2    0.246216    0.400441    0.158697    11.00000   -1.20000
H21B  2    0.258343    0.439382    0.243202    11.00000   -1.20000
AFIX   0
C22   1    0.140744    0.582569    0.276928    11.00000    0.02394    0.01475 =
         0.01662    0.00060    0.00524    0.00063
C23   1    0.085260    0.588862    0.261523    11.00000    0.02520    0.02051 =
         0.02698   -0.00131    0.00205    0.00400
AFIX  43
H23   2    0.073148    0.600246    0.212126    11.00000   -1.20000
AFIX   0
C24   1    0.048196    0.578422    0.318571    11.00000    0.02618    0.02053 =
         0.03927    0.00302    0.00977    0.00553
AFIX  43
H24   2    0.010622    0.581038    0.308277    11.00000   -1.20000
AFIX   0
C25   1    0.065948    0.564275    0.390068    11.00000    0.04761    0.01621 =
         0.03521    0.00374    0.02382    0.00360
AFIX  43
H25   2    0.040480    0.559381    0.429151    11.00000   -1.20000
AFIX   0
C26   1    0.120489    0.557102    0.405655    11.00000    0.06241    0.01997 =
         0.01602    0.00304    0.00529    0.00571
AFIX  43
H26   2    0.132265    0.546629    0.455250    11.00000   -1.20000
AFIX   0
C27   1    0.158081    0.565147    0.349108    11.00000    0.03237    0.02045 =
         0.02095   -0.00135   -0.00012    0.00027
AFIX  43
H27   2    0.195538    0.558745    0.359805    11.00000   -1.20000
AFIX   0
C28   1    0.232285    0.744734    0.208115    11.00000    0.01589    0.01718 =
         0.01611   -0.00299   -0.00054    0.00328
C29   1    0.231515    0.858598    0.154676    11.00000    0.01856    0.02107 =
         0.01586   -0.00102    0.00024    0.00439
AFIX  43
H29   2    0.205734    0.854723    0.115952    11.00000   -1.20000
AFIX   0
C30   1    0.268287    0.977855    0.157743    11.00000    0.01805    0.01991 =
         0.02356    0.00042    0.00573    0.00148
AFIX  43
H30   2    0.268278    1.053577    0.120394    11.00000   -1.20000
AFIX   0
C31   1    0.305013    0.986164    0.215435    11.00000    0.01585    0.02298 =
         0.02791   -0.00438    0.00833   -0.00197
AFIX  43
H31   2    0.329767    1.068432    0.218085    11.00000   -1.20000
AFIX   0
C32   1    0.305444    0.875019    0.268688    11.00000    0.01589    0.03007 =
         0.02416   -0.00406   -0.00418    0.00106
AFIX  43
H32   2    0.330631    0.880894    0.308078    11.00000   -1.20000
AFIX   0
C33   1    0.269697    0.755039    0.265549    11.00000    0.02240    0.01982 =
         0.01650    0.00117   -0.00171    0.00219
AFIX  43
H33   2    0.270515    0.678898    0.302680    11.00000   -1.20000
AFIX   0
C34   1    0.214254   -0.751776    0.004806    11.00000    0.02619    0.02632 =
         0.02190    0.00028    0.00174    0.01141
AFIX 137
H34A  2    0.217243   -0.732291   -0.048247    11.00000   -1.50000
H34B  2    0.207738   -0.860311    0.013088    11.00000   -1.50000
H34C  2    0.247856   -0.721739    0.029288    11.00000   -1.50000
AFIX   0
C35   1    0.144284    0.553296    0.618804    11.00000    0.02960    0.07026 =
         0.03287   -0.00078    0.00415    0.00484
AFIX 137
H35A  2    0.163857    0.634758    0.644164    11.00000   -1.50000
H35B  2    0.128131    0.484991    0.655344    11.00000   -1.50000
H35C  2    0.115786    0.597494    0.588079    11.00000   -1.50000
 
HKLF 4 1 1 0 0 0 1 0 0 0 1
 
REM  rpso675 in Pca2(1)
REM R1 =  0.0233 for   7627 Fo > 4sig(Fo)  and  0.0288 for all   8387 data
REM    517 parameters refined using      1 restraints
 
END  
     
WGHT      0.0203      0.0072 
REM Highest difference peak  0.812,  deepest hole -0.315,  1-sigma level  0.063
Q1    1   0.1284 -0.6069  0.0020  11.00000  0.05    0.81
Q2    1   0.0481 -0.0559 -0.1445  11.00000  0.05    0.38
Q3    1   0.0170 -0.0757 -0.0581  11.00000  0.05    0.30
Q4    1   0.2083  0.5054  0.2026  11.00000  0.05    0.29
Q5    1   0.2196  0.6486  0.2006  11.00000  0.05    0.28
Q6    1   0.1925  0.4728  0.2027  11.00000  0.05    0.27
Q7    1  -0.0111 -0.5637  0.0787  11.00000  0.05    0.27
Q8    1   0.0522  0.1097 -0.0821  11.00000  0.05    0.24
Q9    1   0.1299 -0.5101 -0.0002  11.00000  0.05    0.24
Q10   1   0.2818  0.5196  0.3049  11.00000  0.05    0.23
;
_database_code_depnum_ccdc_archive 'CCDC 977758'
