# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

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

data_cedbamh
_database_code_depnum_ccdc_archive 'CCDC 1959625'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C30 H41 Ce N5 O8 P, 0.5(H4 N), 6.5(H2 O), Cl0.5'
_chemical_formula_sum            'C30 H56 Ce Cl0.50 N5.50 O14.50 P'
_chemical_formula_weight         914.61

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'
Ce Ce -0.2486 2.6331 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.7568(8)
_cell_length_b                   12.4231(9)
_cell_length_c                   14.5497(10)
_cell_angle_alpha                68.256(2)
_cell_angle_beta                 79.612(2)
_cell_angle_gamma                78.900(2)
_cell_volume                     1923.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9024
_cell_measurement_theta_min      2.4722
_cell_measurement_theta_max      27.5189

_exptl_crystal_description       bar
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_F_000             944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.061
_exptl_absorpt_coefficient_mu    1.332
_shelx_estimated_absorpt_T_min   0.751
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            40790
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.338
_diffrn_reflns_theta_max         27.531
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8828
_reflns_number_gt                8293
_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.
 
 _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 Instrument Service v6.2.9'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0340P)²+4.0147P] 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         8828
_refine_ls_number_parameters     489
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0732
_refine_ls_wR_factor_gt          0.0718
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Ce1 Ce 0.42461(2) 0.54600(2) 0.68216(2) 0.00996(5) Uani 1 1 d . . . . .
N1 N 0.20540(17) 0.68228(17) 0.66482(15) 0.0121(4) Uani 1 1 d . . . . .
C2 C 0.1845(2) 0.7522(2) 0.73129(18) 0.0152(5) Uani 1 1 d . . . . .
H21 H 0.1024 0.7901 0.7322 0.018 Uiso 1 1 calc R U . . .
H22 H 0.2352 0.8148 0.7040 0.018 Uiso 1 1 calc R U . . .
C3 C 0.2086(2) 0.6790(2) 0.83697(18) 0.0161(5) Uani 1 1 d . . . . .
H31 H 0.1942 0.7301 0.8776 0.019 Uiso 1 1 calc R U . . .
H32 H 0.1541 0.6201 0.8662 0.019 Uiso 1 1 calc R U . . .
N4 N 0.33014(18) 0.61864(18) 0.84117(15) 0.0135(4) Uani 1 1 d . . . . .
C5 C 0.3369(2) 0.5192(2) 0.93716(18) 0.0163(5) Uani 1 1 d . . . . .
H51 H 0.2897 0.5439 0.9914 0.020 Uiso 1 1 calc R U . . .
H52 H 0.4190 0.4975 0.9519 0.020 Uiso 1 1 calc R U . . .
C6 C 0.2931(2) 0.4133(2) 0.93468(18) 0.0163(5) Uani 1 1 d . . . . .
H61 H 0.2957 0.3505 1.0008 0.020 Uiso 1 1 calc R U . . .
H62 H 0.2110 0.4347 0.9204 0.020 Uiso 1 1 calc R U . . .
N7 N 0.36480(18) 0.36939(18) 0.85779(15) 0.0138(4) Uani 1 1 d . . . . .
C8 C 0.3040(2) 0.2857(2) 0.84004(18) 0.0167(5) Uani 1 1 d . . . . .
H81 H 0.2726 0.2317 0.9050 0.020 Uiso 1 1 calc R U . . .
H82 H 0.3612 0.2384 0.8064 0.020 Uiso 1 1 calc R U . . .
C9 C 0.2054(2) 0.3452(2) 0.77729(18) 0.0157(5) Uani 1 1 d . . . . .
H91 H 0.1711 0.2853 0.7655 0.019 Uiso 1 1 calc R U . . .
H92 H 0.1437 0.3851 0.8143 0.019 Uiso 1 1 calc R U . . .
N10 N 0.24414(17) 0.43206(17) 0.67993(15) 0.0128(4) Uani 1 1 d . . . . .
C11 C 0.1409(2) 0.5158(2) 0.64077(19) 0.0151(5) Uani 1 1 d . . . . .
H111 H 0.0735 0.4728 0.6546 0.018 Uiso 1 1 calc R U . . .
H112 H 0.1575 0.5529 0.5676 0.018 Uiso 1 1 calc R U . . .
C12 C 0.1096(2) 0.6099(2) 0.68738(19) 0.0155(5) Uani 1 1 d . . . . .
H121 H 0.0381 0.6612 0.6621 0.019 Uiso 1 1 calc R U . . .
H122 H 0.0926 0.5728 0.7605 0.019 Uiso 1 1 calc R U . . .
C20 C 0.2049(2) 0.7647(2) 0.56113(18) 0.0139(4) Uani 1 1 d . . . . .
H201 H 0.1343 0.8238 0.5562 0.017 Uiso 1 1 calc R U . . .
H202 H 0.2022 0.7217 0.5165 0.017 Uiso 1 1 calc R U . . .
P1 P 0.33543(5) 0.83804(5) 0.52154(5) 0.01263(12) Uani 1 1 d . . . . .
O11 O 0.42541(15) 0.75780(14) 0.58809(13) 0.0143(3) Uani 1 1 d . . . . .
O12 O 0.30662(16) 0.96298(15) 0.51625(14) 0.0179(4) Uani 1 1 d . . . . .
C21 C 0.3908(2) 0.8300(2) 0.39842(18) 0.0158(5) Uani 1 1 d . . . . .
H211 H 0.4759 0.8327 0.3877 0.019 Uiso 1 1 calc R U . . .
H212 H 0.3796 0.7527 0.3991 0.019 Uiso 1 1 calc R U . . .
N22 N 0.33829(19) 0.92238(19) 0.31032(16) 0.0176(4) Uani 1 1 d . . . . .
H221 H 0.3565 0.8902 0.2549 0.021 Uiso 1 1 calc R U . . .
C30 C 0.3933(2) 1.0339(2) 0.2738(2) 0.0213(5) Uani 1 1 d . . . . .
H301 H 0.3487 1.0948 0.2222 0.026 Uiso 1 1 calc R U . . .
H302 H 0.3885 1.0620 0.3300 0.026 Uiso 1 1 calc R U . . .
C31 C 0.5192(2) 1.0166(2) 0.2309(2) 0.0192(5) Uani 1 1 d . . . . .
C32 C 0.5463(3) 1.0303(2) 0.1303(2) 0.0225(5) Uani 1 1 d . . . . .
H321 H 0.4853 1.0460 0.0903 0.027 Uiso 1 1 calc R U . . .
C33 C 0.6617(3) 1.0212(3) 0.0883(2) 0.0303(7) Uani 1 1 d . . . . .
H331 H 0.6800 1.0319 0.0194 0.036 Uiso 1 1 calc R U . . .
C34 C 0.7505(3) 0.9962(3) 0.1475(3) 0.0363(8) Uani 1 1 d . . . . .
H341 H 0.8296 0.9897 0.1188 0.044 Uiso 1 1 calc R U . . .
C35 C 0.7249(3) 0.9810(3) 0.2472(3) 0.0348(7) Uani 1 1 d . . . . .
H351 H 0.7861 0.9626 0.2874 0.042 Uiso 1 1 calc R U . . .
C36 C 0.6092(3) 0.9925(2) 0.2888(2) 0.0268(6) Uani 1 1 d . . . . .
H361 H 0.5915 0.9839 0.3573 0.032 Uiso 1 1 calc R U . . .
C40 C 0.2059(3) 0.9482(3) 0.3277(2) 0.0297(6) Uani 1 1 d . . . . .
H401 H 0.1733 0.8737 0.3627 0.036 Uiso 1 1 calc R U . . .
H402 H 0.1843 0.9960 0.3712 0.036 Uiso 1 1 calc R U . . .
C41 C 0.1531(3) 1.0122(3) 0.2320(2) 0.0314(7) Uani 1 1 d . . . . .
C42 C 0.1278(3) 0.9495(4) 0.1787(3) 0.0415(8) Uani 1 1 d . . . . .
H421 H 0.1422 0.8664 0.2033 0.050 Uiso 1 1 calc R U . . .
C43 C 0.0816(4) 1.0079(4) 0.0898(3) 0.0535(11) Uani 1 1 d . . . . .
H431 H 0.0646 0.9648 0.0532 0.064 Uiso 1 1 calc R U . . .
C44 C 0.0592(3) 1.1306(5) 0.0530(3) 0.0553(12) Uani 1 1 d . . . . .
H441 H 0.0277 1.1707 -0.0084 0.066 Uiso 1 1 calc R U . . .
C45 C 0.0835(3) 1.1914(4) 0.1066(3) 0.0506(11) Uani 1 1 d . . . . .
H451 H 0.0688 1.2745 0.0819 0.061 Uiso 1 1 calc R U . . .
C46 C 0.1291(3) 1.1345(3) 0.1958(3) 0.0372(8) Uani 1 1 d . . . . .
H461 H 0.1442 1.1782 0.2328 0.045 Uiso 1 1 calc R U . . .
C50 C 0.4093(2) 0.7000(2) 0.83618(19) 0.0167(5) Uani 1 1 d . . . . .
H501 H 0.3949 0.7164 0.8992 0.020 Uiso 1 1 calc R U . . .
H502 H 0.3920 0.7748 0.7812 0.020 Uiso 1 1 calc R U . . .
C51 C 0.5374(2) 0.6507(2) 0.81926(18) 0.0159(5) Uani 1 1 d . . . . .
O51 O 0.56063(16) 0.57417(17) 0.77694(14) 0.0192(4) Uani 1 1 d . . . . .
O52 O 0.61034(17) 0.68908(17) 0.84623(14) 0.0218(4) Uani 1 1 d . . . . .
C60 C 0.4776(2) 0.3059(2) 0.89232(19) 0.0179(5) Uani 1 1 d . . . . .
H601 H 0.4648 0.2334 0.9496 0.022 Uiso 1 1 calc R U . . .
H602 H 0.5156 0.3553 0.9143 0.022 Uiso 1 1 calc R U . . .
C61 C 0.5554(2) 0.2758(2) 0.80740(19) 0.0172(5) Uani 1 1 d . . . . .
O61 O 0.54919(16) 0.35129(15) 0.72058(13) 0.0177(4) Uani 1 1 d . . . . .
O62 O 0.61887(19) 0.17934(18) 0.82794(15) 0.0271(4) Uani 1 1 d . . . . .
C70 C 0.2983(2) 0.3738(2) 0.60753(18) 0.0141(5) Uani 1 1 d . . . . .
H701 H 0.2372 0.3455 0.5871 0.017 Uiso 1 1 calc R U . . .
H702 H 0.3546 0.3052 0.6395 0.017 Uiso 1 1 calc R U . . .
C71 C 0.3617(2) 0.4580(2) 0.51521(18) 0.0125(4) Uani 1 1 d . . . . .
O71 O 0.38021(14) 0.55169(15) 0.52152(12) 0.0131(3) Uani 1 1 d . . . . .
O72 O 0.39196(15) 0.42757(15) 0.44052(13) 0.0147(3) Uani 1 1 d . . . . .
Cl1 Cl 0.03367(18) 0.5364(2) 0.06990(17) 0.0644(6) Uani 0.5 1 d . U P . .
N1A N 0.1969(3) 0.6241(3) 0.3417(3) 0.0659(11) Uani 0.5 1 d . . P A 1
O1W O 0.1969(3) 0.6241(3) 0.3417(3) 0.0659(11) Uani 0.5 1 d . . P B 2
H11W H 0.1413 0.6819 0.3332 0.079 Uiso 1 1 d R U . . .
H12W H 0.2584 0.6371 0.3583 0.079 Uiso 1 1 d R U . . .
H13A H 0.2238 0.6003 0.2846 0.079 Uiso 0.5 1 d R U P B 1
H14A H 0.1967 0.5543 0.3795 0.079 Uiso 0.5 1 d R U P B 1
O2W O 0.3370(2) 0.1950(2) 0.4553(3) 0.0550(8) Uani 1 1 d . . . . .
H21W H 0.3414 0.1123 0.4758 0.050(12) Uiso 1 1 d R . . . .
H22W H 0.4009 0.2010 0.4388 0.09(2) Uiso 1 1 d R . . . .
O3W O 0.0653(2) 1.0555(3) 0.5403(3) 0.0598(8) Uani 1 1 d . . . . .
H31W H 0.1415 1.0347 0.5367 0.088(19) Uiso 1 1 d R . . . .
H32W H 0.0298 1.1234 0.5479 0.105 Uiso 1 1 d R U . . .
O4W O 0.1675(3) 0.3729(4) 0.2167(3) 0.0865(13) Uani 1 1 d . . . . .
H41W H 0.1725 0.4468 0.1918 0.104 Uiso 1 1 d R U . . .
H42W H 0.2292 0.3509 0.2003 0.104 Uiso 1 1 d R U . . .
O5W O -0.0012(2) 0.7222(2) 0.4246(2) 0.0506(7) Uani 1 1 d . . . . .
H51W H -0.0492 0.6989 0.4789 0.061 Uiso 1 1 d R U . . .
H52W H -0.0309 0.7603 0.3714 0.061 Uiso 1 1 d R U . . .
O6WA O 0.2385(6) 0.6137(6) 0.1616(6) 0.0813(16) Uani 0.574(6) 1 d . . P C 3
H61W H 0.1550 0.6485 0.1446 0.098 Uiso 1 1 d R U . . .
H62W H 0.2366 0.6533 0.0956 0.098 Uiso 1 1 d R U . . .
O6WB O 0.1822(9) 0.7071(8) 0.1068(7) 0.0813(16) Uani 0.426(6) 1 d . . P C 4
O7WA O 0.1609(3) 0.3794(3) 0.4030(2) 0.0359(7) Uani 0.752(5) 1 d . . P D 5
H71W H 0.2248 0.3301 0.4208 0.043 Uiso 1 1 d R U . . .
H72W H 0.1829 0.3849 0.3532 0.043 Uiso 1 1 d R U . . .
O7WB O 0.2442(9) 0.3832(9) 0.3660(7) 0.0359(7) Uani 0.248(5) 1 d . . P D 6


_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
Ce1 O51 2.4391(18) . ?
Ce1 O71 2.4584(17) . ?
Ce1 O11 2.4764(17) . ?
Ce1 O61 2.4977(18) . ?
Ce1 O72 2.5288(17) 2_666 ?
Ce1 N7 2.762(2) . ?
Ce1 N4 2.763(2) . ?
Ce1 N10 2.779(2) . ?
Ce1 N1 2.795(2) . ?
N1 C20 1.477(3) . ?
N1 C2 1.485(3) . ?
N1 C12 1.491(3) . ?
C2 C3 1.514(3) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.480(3) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.475(3) . ?
N4 C5 1.486(3) . ?
C5 C6 1.516(4) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.481(3) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.476(3) . ?
N7 C8 1.487(3) . ?
C8 C9 1.508(4) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.484(3) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.478(3) . ?
N10 C11 1.485(3) . ?
C11 C12 1.514(3) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.830(2) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.4994(18) . ?
P1 O11 1.5161(18) . ?
P1 C21 1.825(3) . ?
C21 N22 1.504(3) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C30 1.515(3) . ?
N22 C40 1.522(4) . ?
N22 H221 1.0000 . ?
C30 C31 1.507(4) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36 1.390(4) . ?
C31 C32 1.393(4) . ?
C32 C33 1.386(4) . ?
C32 H321 0.9500 . ?
C33 C34 1.389(5) . ?
C33 H331 0.9500 . ?
C34 C35 1.375(5) . ?
C34 H341 0.9500 . ?
C35 C36 1.390(5) . ?
C35 H351 0.9500 . ?
C36 H361 0.9500 . ?
C40 C41 1.503(4) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C41 C42 1.384(5) . ?
C41 C46 1.401(5) . ?
C42 C43 1.379(5) . ?
C42 H421 0.9500 . ?
C43 C44 1.404(7) . ?
C43 H431 0.9500 . ?
C44 C45 1.364(7) . ?
C44 H441 0.9500 . ?
C45 C46 1.378(5) . ?
C45 H451 0.9500 . ?
C46 H461 0.9500 . ?
C50 C51 1.525(4) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.239(3) . ?
C51 O51 1.277(3) . ?
C60 C61 1.519(4) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.246(3) . ?
C61 O61 1.269(3) . ?
C70 C71 1.534(3) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.250(3) . ?
C71 O71 1.263(3) . ?
O72 Ce1 2.5288(17) 2_666 ?
N1A H11W 0.8605 . ?
N1A H12W 0.8638 . ?
N1A H13A 0.9631 . ?
N1A H14A 0.8370 . ?
O1W H11W 0.8605 . ?
O1W H12W 0.8638 . ?
O2W H21W 0.9516 . ?
O2W H22W 0.7556 . ?
O3W H31W 0.8807 . ?
O3W H32W 0.9029 . ?
O4W H41W 0.8621 . ?
O4W H42W 0.7531 . ?
O5W H51W 0.8714 . ?
O5W H52W 0.8403 . ?
O6WA H61W 1.0273 . ?
O6WA H62W 0.9048 . ?
O6WB H61W 0.8150 . ?
O6WB H62W 0.8716 . ?
O7WA H71W 0.8843 . ?
O7WA H72W 0.7071 . ?
O7WB H71W 0.8523 . ?
O7WB H72W 0.7712 . ?

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
O51 Ce1 O71 148.58(6) . . ?
O51 Ce1 O11 83.98(6) . . ?
O71 Ce1 O11 81.25(6) . . ?
O51 Ce1 O61 80.72(6) . . ?
O71 Ce1 O61 95.04(6) . . ?
O11 Ce1 O61 143.43(6) . . ?
O51 Ce1 O72 77.77(6) . 2_666 ?
O71 Ce1 O72 71.29(5) . 2_666 ?
O11 Ce1 O72 71.58(6) . 2_666 ?
O61 Ce1 O72 72.79(6) . 2_666 ?
O51 Ce1 N7 84.20(6) . . ?
O71 Ce1 N7 121.29(6) . . ?
O11 Ce1 N7 148.87(6) . . ?
O61 Ce1 N7 61.67(6) . . ?
O72 Ce1 N7 133.09(6) 2_666 . ?
O51 Ce1 N4 62.76(6) . . ?
O71 Ce1 N4 141.83(6) . . ?
O11 Ce1 N4 84.03(6) . . ?
O61 Ce1 N4 116.99(6) . . ?
O72 Ce1 N4 135.49(6) 2_666 . ?
N7 Ce1 N4 64.97(6) . . ?
O51 Ce1 N10 148.45(6) . . ?
O71 Ce1 N10 60.93(6) . . ?
O11 Ce1 N10 121.23(6) . . ?
O61 Ce1 N10 86.69(6) . . ?
O72 Ce1 N10 125.71(6) 2_666 . ?
N7 Ce1 N10 64.41(6) . . ?
N4 Ce1 N10 98.72(6) . . ?
O51 Ce1 N1 120.02(6) . . ?
O71 Ce1 N1 77.50(6) . . ?
O11 Ce1 N1 64.27(6) . . ?
O61 Ce1 N1 150.63(6) . . ?
O72 Ce1 N1 128.83(6) 2_666 . ?
N7 Ce1 N1 97.71(6) . . ?
N4 Ce1 N1 64.38(6) . . ?
N10 Ce1 N1 64.74(6) . . ?
C20 N1 C2 107.79(18) . . ?
C20 N1 C12 108.44(18) . . ?
C2 N1 C12 110.10(18) . . ?
C20 N1 Ce1 108.07(13) . . ?
C2 N1 Ce1 110.23(14) . . ?
C12 N1 Ce1 112.08(14) . . ?
N1 C2 C3 112.7(2) . . ?
N1 C2 H21 109.1 . . ?
C3 C2 H21 109.1 . . ?
N1 C2 H22 109.1 . . ?
C3 C2 H22 109.1 . . ?
H21 C2 H22 107.8 . . ?
N4 C3 C2 112.0(2) . . ?
N4 C3 H31 109.2 . . ?
C2 C3 H31 109.2 . . ?
N4 C3 H32 109.2 . . ?
C2 C3 H32 109.2 . . ?
H31 C3 H32 107.9 . . ?
C50 N4 C3 109.93(19) . . ?
C50 N4 C5 108.41(19) . . ?
C3 N4 C5 109.10(19) . . ?
C50 N4 Ce1 102.77(14) . . ?
C3 N4 Ce1 115.36(14) . . ?
C5 N4 Ce1 110.94(14) . . ?
N4 C5 C6 111.9(2) . . ?
N4 C5 H51 109.2 . . ?
C6 C5 H51 109.2 . . ?
N4 C5 H52 109.2 . . ?
C6 C5 H52 109.2 . . ?
H51 C5 H52 107.9 . . ?
N7 C6 C5 111.3(2) . . ?
N7 C6 H61 109.4 . . ?
C5 C6 H61 109.4 . . ?
N7 C6 H62 109.4 . . ?
C5 C6 H62 109.4 . . ?
H61 C6 H62 108.0 . . ?
C60 N7 C6 110.13(19) . . ?
C60 N7 C8 107.51(19) . . ?
C6 N7 C8 109.87(19) . . ?
C60 N7 Ce1 104.50(14) . . ?
C6 N7 Ce1 113.22(14) . . ?
C8 N7 Ce1 111.36(14) . . ?
N7 C8 C9 113.1(2) . . ?
N7 C8 H81 109.0 . . ?
C9 C8 H81 109.0 . . ?
N7 C8 H82 109.0 . . ?
C9 C8 H82 109.0 . . ?
H81 C8 H82 107.8 . . ?
N10 C9 C8 112.4(2) . . ?
N10 C9 H91 109.1 . . ?
C8 C9 H91 109.1 . . ?
N10 C9 H92 109.1 . . ?
C8 C9 H92 109.1 . . ?
H91 C9 H92 107.8 . . ?
C70 N10 C9 110.81(19) . . ?
C70 N10 C11 109.08(19) . . ?
C9 N10 C11 108.66(19) . . ?
C70 N10 Ce1 101.10(13) . . ?
C9 N10 Ce1 115.02(14) . . ?
C11 N10 Ce1 111.90(14) . . ?
N10 C11 C12 111.8(2) . . ?
N10 C11 H111 109.3 . . ?
C12 C11 H111 109.3 . . ?
N10 C11 H112 109.3 . . ?
C12 C11 H112 109.3 . . ?
H111 C11 H112 107.9 . . ?
N1 C12 C11 112.04(19) . . ?
N1 C12 H121 109.2 . . ?
C11 C12 H121 109.2 . . ?
N1 C12 H122 109.2 . . ?
C11 C12 H122 109.2 . . ?
H121 C12 H122 107.9 . . ?
N1 C20 P1 110.56(16) . . ?
N1 C20 H201 109.5 . . ?
P1 C20 H201 109.5 . . ?
N1 C20 H202 109.5 . . ?
P1 C20 H202 109.5 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 118.58(10) . . ?
O12 P1 C21 110.61(11) . . ?
O11 P1 C21 104.53(11) . . ?
O12 P1 C20 111.25(11) . . ?
O11 P1 C20 105.61(10) . . ?
C21 P1 C20 105.24(12) . . ?
P1 O11 Ce1 126.14(9) . . ?
N22 C21 P1 117.56(17) . . ?
N22 C21 H211 107.9 . . ?
P1 C21 H211 107.9 . . ?
N22 C21 H212 107.9 . . ?
P1 C21 H212 107.9 . . ?
H211 C21 H212 107.2 . . ?
C21 N22 C30 112.6(2) . . ?
C21 N22 C40 113.4(2) . . ?
C30 N22 C40 111.0(2) . . ?
C21 N22 H221 106.4 . . ?
C30 N22 H221 106.4 . . ?
C40 N22 H221 106.4 . . ?
C31 C30 N22 112.3(2) . . ?
C31 C30 H301 109.1 . . ?
N22 C30 H301 109.1 . . ?
C31 C30 H302 109.1 . . ?
N22 C30 H302 109.1 . . ?
H301 C30 H302 107.9 . . ?
C36 C31 C32 119.3(3) . . ?
C36 C31 C30 121.1(3) . . ?
C32 C31 C30 119.5(3) . . ?
C33 C32 C31 120.3(3) . . ?
C33 C32 H321 119.8 . . ?
C31 C32 H321 119.8 . . ?
C32 C33 C34 119.6(3) . . ?
C32 C33 H331 120.2 . . ?
C34 C33 H331 120.2 . . ?
C35 C34 C33 120.7(3) . . ?
C35 C34 H341 119.7 . . ?
C33 C34 H341 119.7 . . ?
C34 C35 C36 119.7(3) . . ?
C34 C35 H351 120.1 . . ?
C36 C35 H351 120.1 . . ?
C35 C36 C31 120.4(3) . . ?
C35 C36 H361 119.8 . . ?
C31 C36 H361 119.8 . . ?
C41 C40 N22 112.2(2) . . ?
C41 C40 H401 109.2 . . ?
N22 C40 H401 109.2 . . ?
C41 C40 H402 109.2 . . ?
N22 C40 H402 109.2 . . ?
H401 C40 H402 107.9 . . ?
C42 C41 C46 119.5(3) . . ?
C42 C41 C40 119.6(3) . . ?
C46 C41 C40 120.9(3) . . ?
C43 C42 C41 119.8(4) . . ?
C43 C42 H421 120.1 . . ?
C41 C42 H421 120.1 . . ?
C42 C43 C44 120.6(4) . . ?
C42 C43 H431 119.7 . . ?
C44 C43 H431 119.7 . . ?
C45 C44 C43 119.1(4) . . ?
C45 C44 H441 120.5 . . ?
C43 C44 H441 120.5 . . ?
C44 C45 C46 121.2(4) . . ?
C44 C45 H451 119.4 . . ?
C46 C45 H451 119.4 . . ?
C45 C46 C41 119.9(4) . . ?
C45 C46 H461 120.1 . . ?
C41 C46 H461 120.1 . . ?
N4 C50 C51 112.1(2) . . ?
N4 C50 H501 109.2 . . ?
C51 C50 H501 109.2 . . ?
N4 C50 H502 109.2 . . ?
C51 C50 H502 109.2 . . ?
H501 C50 H502 107.9 . . ?
O52 C51 O51 125.3(2) . . ?
O52 C51 C50 117.6(2) . . ?
O51 C51 C50 117.0(2) . . ?
C51 O51 Ce1 122.94(16) . . ?
N7 C60 C61 109.1(2) . . ?
N7 C60 H601 109.9 . . ?
C61 C60 H601 109.9 . . ?
N7 C60 H602 109.9 . . ?
C61 C60 H602 109.9 . . ?
H601 C60 H602 108.3 . . ?
O62 C61 O61 125.3(2) . . ?
O62 C61 C60 117.9(2) . . ?
O61 C61 C60 116.7(2) . . ?
C61 O61 Ce1 124.57(16) . . ?
N10 C70 C71 111.00(19) . . ?
N10 C70 H701 109.4 . . ?
C71 C70 H701 109.4 . . ?
N10 C70 H702 109.4 . . ?
C71 C70 H702 109.4 . . ?
H701 C70 H702 108.0 . . ?
O72 C71 O71 125.5(2) . . ?
O72 C71 C70 117.3(2) . . ?
O71 C71 C70 117.1(2) . . ?
C71 O71 Ce1 118.17(15) . . ?
C71 O72 Ce1 129.90(15) . 2_666 ?
H11W N1A H12W 113.3 . . ?
H11W N1A H13A 115.2 . . ?
H12W N1A H13A 105.4 . . ?
H11W N1A H14A 129.5 . . ?
H12W N1A H14A 98.1 . . ?
H13A N1A H14A 91.2 . . ?
H11W O1W H12W 113.3 . . ?
H21W O2W H22W 99.5 . . ?
H31W O3W H32W 123.3 . . ?
H41W O4W H42W 98.1 . . ?
H51W O5W H52W 117.1 . . ?
H61W O6WA H62W 67.9 . . ?
H61W O6WB H62W 79.9 . . ?
H71W O7WA H72W 87.3 . . ?
H71W O7WB H72W 85.8 . . ?

_refine_diff_density_max         1.899
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.099

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

data_dbam_er
_database_code_depnum_ccdc_archive 'CCDC 1959626'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H40 Er N5 O8 P, 4(H2 O), H4 N'
_chemical_formula_sum            'C30 H52 Er N6 O12 P'
_chemical_formula_weight         887.00

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'

_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                   24.3204(4)
_cell_length_b                   10.42140(10)
_cell_length_c                   15.1910(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.6020(10)
_cell_angle_gamma                90
_cell_volume                     3669.93(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8367
_cell_measurement_theta_min      2.6359
_cell_measurement_theta_max      27.4809

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_F_000             1812
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.112
_exptl_absorpt_coefficient_mu    2.397
_shelx_estimated_absorpt_T_min   0.476
_shelx_estimated_absorpt_T_max   0.775
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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 8.3333
_diffrn_reflns_number            29367
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.757
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8434
_reflns_number_gt                6985
_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.
 
 _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 Instrument Service v2014.11.0.1'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0293P)²+3.1781P] 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         8434
_refine_ls_number_parameters     478
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0300
_refine_ls_wR_factor_ref         0.0702
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
Er1 Er 0.31895(2) 0.55415(2) 0.31470(2) 0.01168(5) Uani 1 1 d . . . . .
N1 N 0.23122(11) 0.5129(2) 0.37432(17) 0.0140(5) Uani 1 1 d . . . . .
C2 C 0.25229(14) 0.4614(3) 0.4701(2) 0.0171(7) Uani 1 1 d . . . . .
H21 H 0.2607 0.3688 0.4675 0.020 Uiso 1 1 calc R U . . .
H22 H 0.2214 0.4704 0.4998 0.020 Uiso 1 1 calc R U . . .
C3 C 0.30620(14) 0.5294(3) 0.5289(2) 0.0167(7) Uani 1 1 d . . . . .
H31 H 0.2969 0.6203 0.5369 0.020 Uiso 1 1 calc R U . . .
H32 H 0.3190 0.4892 0.5909 0.020 Uiso 1 1 calc R U . . .
N4 N 0.35379(11) 0.5236(2) 0.48703(17) 0.0145(5) Uani 1 1 d . . . . .
C5 C 0.39795(14) 0.6222(3) 0.5315(2) 0.0190(7) Uani 1 1 d . . . . .
H51 H 0.4352 0.5982 0.5223 0.023 Uiso 1 1 calc R U . . .
H52 H 0.4034 0.6231 0.5987 0.023 Uiso 1 1 calc R U . . .
C6 C 0.38127(15) 0.7552(3) 0.4929(2) 0.0204(7) Uani 1 1 d . . . . .
H61 H 0.3461 0.7834 0.5074 0.025 Uiso 1 1 calc R U . . .
H62 H 0.4127 0.8162 0.5223 0.025 Uiso 1 1 calc R U . . .
N7 N 0.37032(11) 0.7562(3) 0.39086(17) 0.0172(6) Uani 1 1 d . . . . .
C8 C 0.33691(15) 0.8733(3) 0.3494(2) 0.0202(7) Uani 1 1 d . . . . .
H81 H 0.3434 0.8918 0.2894 0.024 Uiso 1 1 calc R U . . .
H82 H 0.3512 0.9475 0.3907 0.024 Uiso 1 1 calc R U . . .
C9 C 0.27305(14) 0.8575(3) 0.3347(2) 0.0176(7) Uani 1 1 d . . . . .
H91 H 0.2661 0.8468 0.3952 0.021 Uiso 1 1 calc R U . . .
H92 H 0.2526 0.9358 0.3052 0.021 Uiso 1 1 calc R U . . .
N10 N 0.24974(11) 0.7448(2) 0.27558(17) 0.0148(5) Uani 1 1 d . . . . .
C11 C 0.19274(13) 0.7081(3) 0.2841(2) 0.0171(7) Uani 1 1 d . . . . .
H111 H 0.1720 0.6547 0.2304 0.020 Uiso 1 1 calc R U . . .
H112 H 0.1696 0.7865 0.2833 0.020 Uiso 1 1 calc R U . . .
C12 C 0.19852(14) 0.6339(3) 0.3726(2) 0.0166(7) Uani 1 1 d . . . . .
H121 H 0.2188 0.6875 0.4265 0.020 Uiso 1 1 calc R U . . .
H122 H 0.1597 0.6136 0.3770 0.020 Uiso 1 1 calc R U . . .
C20 C 0.19401(13) 0.4158(3) 0.3136(2) 0.0165(7) Uani 1 1 d . . . . .
H201 H 0.1724 0.4563 0.2543 0.020 Uiso 1 1 calc R U . . .
H202 H 0.1657 0.3828 0.3432 0.020 Uiso 1 1 calc R U . . .
P1 P 0.23699(3) 0.28232(8) 0.29146(6) 0.01455(17) Uani 1 1 d . . . . .
O11 O 0.29757(10) 0.34037(19) 0.30363(14) 0.0147(4) Uani 1 1 d . . . . .
O12 O 0.23427(10) 0.1695(2) 0.35065(15) 0.0214(5) Uani 1 1 d . . . . .
C21 C 0.20436(14) 0.2472(3) 0.1703(2) 0.0177(7) Uani 1 1 d . . . . .
H211 H 0.2079 0.3232 0.1333 0.021 Uiso 1 1 calc R U . . .
H212 H 0.2254 0.1753 0.1524 0.021 Uiso 1 1 calc R U . . .
N22 N 0.14320(12) 0.2128(3) 0.14933(19) 0.0195(6) Uani 1 1 d . . . . .
C30 C 0.13639(15) 0.0788(3) 0.1716(3) 0.0255(8) Uani 1 1 d . . . . .
H301 H 0.1640 0.0591 0.2329 0.031 Uiso 1 1 calc R U . . .
H302 H 0.1462 0.0235 0.1255 0.031 Uiso 1 1 calc R U . . .
C31 C 0.07626(15) 0.0465(3) 0.1732(2) 0.0237(8) Uani 1 1 d . . . . .
C32 C 0.05309(17) -0.0733(3) 0.1426(3) 0.0307(9) Uani 1 1 d . . . . .
H321 H 0.0744 -0.1321 0.1180 0.037 Uiso 1 1 calc R U . . .
C33 C -0.00127(18) -0.1079(4) 0.1479(3) 0.0424(11) Uani 1 1 d . . . . .
H331 H -0.0166 -0.1905 0.1281 0.051 Uiso 1 1 calc R U . . .
C34 C -0.03246(18) -0.0223(4) 0.1817(3) 0.0439(11) Uani 1 1 d . . . . .
H341 H -0.0696 -0.0454 0.1850 0.053 Uiso 1 1 calc R U . . .
C35 C -0.01035(19) 0.0969(4) 0.2111(3) 0.0447(11) Uani 1 1 d . . . . .
H351 H -0.0323 0.1560 0.2343 0.054 Uiso 1 1 calc R U . . .
C36 C 0.04395(17) 0.1315(4) 0.2069(3) 0.0341(9) Uani 1 1 d . . . . .
H361 H 0.0590 0.2141 0.2274 0.041 Uiso 1 1 calc R U . . .
C40 C 0.11219(15) 0.2386(3) 0.0520(2) 0.0259(8) Uani 1 1 d . . . . .
H401 H 0.0738 0.1974 0.0363 0.031 Uiso 1 1 calc R U . . .
H402 H 0.1336 0.1989 0.0130 0.031 Uiso 1 1 calc R U . . .
C41 C 0.10439(15) 0.3785(3) 0.0293(2) 0.0235(8) Uani 1 1 d . . . . .
C42 C 0.1223(2) 0.4323(4) -0.0406(3) 0.0435(11) Uani 1 1 d . . . . .
H421 H 0.1418 0.3811 -0.0735 0.052 Uiso 1 1 calc R U . . .
C43 C 0.1118(2) 0.5617(5) -0.0630(3) 0.0564(14) Uani 1 1 d . . . . .
H431 H 0.1239 0.5977 -0.1116 0.068 Uiso 1 1 calc R U . . .
C44 C 0.0843(2) 0.6374(5) -0.0157(3) 0.0517(13) Uani 1 1 d . . . . .
H441 H 0.0776 0.7257 -0.0309 0.062 Uiso 1 1 calc R U . . .
C45 C 0.0662(2) 0.5844(4) 0.0543(3) 0.0466(12) Uani 1 1 d . . . . .
H451 H 0.0465 0.6357 0.0867 0.056 Uiso 1 1 calc R U . . .
C46 C 0.07692(17) 0.4562(4) 0.0769(3) 0.0309(9) Uani 1 1 d . . . . .
H461 H 0.0652 0.4209 0.1260 0.037 Uiso 1 1 calc R U . . .
C50 C 0.38169(14) 0.3964(3) 0.4994(2) 0.0180(7) Uani 1 1 d . . . . .
H501 H 0.3518 0.3289 0.4888 0.022 Uiso 1 1 calc R U . . .
H502 H 0.4072 0.3881 0.5637 0.022 Uiso 1 1 calc R U . . .
C51 C 0.41714(14) 0.3772(3) 0.4324(2) 0.0205(7) Uani 1 1 d . . . . .
O51 O 0.40772(9) 0.4566(2) 0.36523(15) 0.0169(5) Uani 1 1 d . . . . .
O52 O 0.45026(12) 0.2841(3) 0.44467(18) 0.0396(7) Uani 1 1 d . . . . .
C60 C 0.42497(14) 0.7575(3) 0.3669(2) 0.0209(7) Uani 1 1 d . . . . .
H601 H 0.4535 0.7012 0.4100 0.025 Uiso 1 1 calc R U . . .
H602 H 0.4408 0.8457 0.3736 0.025 Uiso 1 1 calc R U . . .
C61 C 0.41536(14) 0.7115(3) 0.2680(2) 0.0181(7) Uani 1 1 d . . . . .
O61 O 0.36816(9) 0.6517(2) 0.22963(15) 0.0184(5) Uani 1 1 d . . . . .
O62 O 0.45383(10) 0.7284(2) 0.23196(16) 0.0246(5) Uani 1 1 d . . . . .
C70 C 0.24391(15) 0.7702(3) 0.1774(2) 0.0186(7) Uani 1 1 d . . . . .
H701 H 0.2746 0.8303 0.1737 0.022 Uiso 1 1 calc R U . . .
H702 H 0.2063 0.8120 0.1480 0.022 Uiso 1 1 calc R U . . .
C71 C 0.24798(13) 0.6477(3) 0.1242(2) 0.0166(7) Uani 1 1 d . . . . .
O71 O 0.25518(9) 0.54298(19) 0.17039(14) 0.0149(5) Uani 1 1 d . . . . .
O72 O 0.24523(11) 0.6573(2) 0.04227(15) 0.0239(5) Uani 1 1 d . . . . .
N1A N 0.47296(14) 0.4378(3) 0.2334(2) 0.0246(7) Uani 1 1 d . . . . .
H11A H 0.4541(18) 0.436(4) 0.275(3) 0.033(12) Uiso 1 1 d . . . . .
H12A H 0.4889(15) 0.368(4) 0.249(2) 0.012(9) Uiso 1 1 d . . . . .
H13A H 0.4536(15) 0.438(3) 0.172(2) 0.038(12) Uiso 1 1 d . . . . .
H14A H 0.4943 0.5104 0.2395 0.065(17) Uiso 1 1 d R . . . .
O1W O 0.41927(14) 0.4282(3) 0.0419(2) 0.0359(7) Uani 1 1 d . . . . .
H11W H 0.4318 0.3592 0.0099 0.043 Uiso 1 1 d R U . . .
H12W H 0.385(3) 0.427(6) 0.035(5) 0.10(3) Uiso 1 1 d . . . . .
O2W O 0.30024(13) 0.4130(3) 0.0162(2) 0.0349(7) Uani 1 1 d . . . . .
H21W H 0.2810(19) 0.391(4) -0.033(3) 0.038(13) Uiso 1 1 d . . . . .
H22W H 0.2851(19) 0.472(4) 0.032(3) 0.038(13) Uiso 1 1 d . . . . .
O3W O 0.43210(14) 0.0959(3) 0.2814(2) 0.0556(9) Uani 1 1 d . . . . .
H31W H 0.4105 0.1768 0.2678 0.067 Uiso 1 1 d R U . . .
H32W H 0.4126 0.0433 0.2264 0.067 Uiso 1 1 d R U . . .
O4W O 0.34606(13) 0.2528(3) 0.1695(2) 0.0453(8) Uani 1 1 d . . . . .
H41W H 0.3319 0.2772 0.2086 0.058(16) Uiso 1 1 d R . . . .
H42W H 0.3254 0.3085 0.1203 0.083(19) Uiso 1 1 d 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 O61 2.252(2) . ?
Er1 O71 2.273(2) . ?
Er1 O11 2.282(2) . ?
Er1 O51 2.298(2) . ?
Er1 N4 2.516(3) . ?
Er1 N7 2.541(3) . ?
Er1 N10 2.555(3) . ?
Er1 N1 2.593(3) . ?
N1 C20 1.480(4) . ?
N1 C12 1.487(4) . ?
N1 C2 1.489(4) . ?
C2 C3 1.520(4) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.481(4) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.475(4) . ?
N4 C5 1.492(4) . ?
C5 C6 1.512(5) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.492(4) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.481(4) . ?
N7 C8 1.495(4) . ?
C8 C9 1.510(4) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.483(4) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.478(4) . ?
N10 C11 1.481(4) . ?
C11 C12 1.520(4) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.831(3) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.494(2) . ?
P1 O11 1.551(2) . ?
P1 C21 1.808(3) . ?
C21 N22 1.468(4) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C30 1.459(4) . ?
N22 C40 1.467(4) . ?
C30 C31 1.507(5) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36 1.381(5) . ?
C31 C32 1.391(5) . ?
C32 C33 1.396(6) . ?
C32 H321 0.9500 . ?
C33 C34 1.368(7) . ?
C33 H331 0.9500 . ?
C34 C35 1.373(6) . ?
C34 H341 0.9500 . ?
C35 C36 1.389(6) . ?
C35 H351 0.9500 . ?
C36 H361 0.9500 . ?
C40 C41 1.497(5) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C41 C42 1.383(5) . ?
C41 C46 1.384(5) . ?
C42 C43 1.395(6) . ?
C42 H421 0.9500 . ?
C43 C44 1.371(7) . ?
C43 H431 0.9500 . ?
C44 C45 1.382(7) . ?
C44 H441 0.9500 . ?
C45 C46 1.385(5) . ?
C45 H451 0.9500 . ?
C46 H461 0.9500 . ?
C50 C51 1.532(4) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.238(4) . ?
C51 O51 1.280(4) . ?
C60 C61 1.526(4) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.232(4) . ?
C61 O61 1.281(4) . ?
C70 C71 1.530(4) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.231(4) . ?
C71 O71 1.280(4) . ?
N1A H11A 0.88(4) . ?
N1A H12A 0.83(4) . ?
N1A H13A 0.90(4) . ?
N1A H14A 0.9059 . ?
O1W H11W 0.9670 . ?
O1W H12W 0.80(6) . ?
O2W H21W 0.78(5) . ?
O2W H22W 0.79(4) . ?
O3W H31W 0.9815 . ?
O3W H32W 0.9926 . ?
O4W H41W 0.8131 . ?
O4W H42W 0.9586 . ?

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
O61 Er1 O71 78.21(8) . . ?
O61 Er1 O11 123.17(8) . . ?
O71 Er1 O11 78.77(7) . . ?
O61 Er1 O51 77.45(8) . . ?
O71 Er1 O51 126.69(8) . . ?
O11 Er1 O51 76.28(8) . . ?
O61 Er1 N4 125.72(8) . . ?
O71 Er1 N4 156.02(8) . . ?
O11 Er1 N4 87.18(8) . . ?
O51 Er1 N4 67.03(8) . . ?
O61 Er1 N7 67.29(8) . . ?
O71 Er1 N7 125.42(8) . . ?
O11 Er1 N7 155.77(8) . . ?
O51 Er1 N7 86.08(8) . . ?
N4 Er1 N7 70.52(8) . . ?
O61 Er1 N10 86.71(8) . . ?
O71 Er1 N10 66.81(8) . . ?
O11 Er1 N10 128.50(8) . . ?
O51 Er1 N10 155.22(8) . . ?
N4 Er1 N10 109.34(8) . . ?
N7 Er1 N10 70.14(8) . . ?
O61 Er1 N1 155.70(8) . . ?
O71 Er1 N1 86.27(8) . . ?
O11 Er1 N1 70.78(8) . . ?
O51 Er1 N1 126.80(8) . . ?
N4 Er1 N1 70.70(8) . . ?
N7 Er1 N1 108.75(8) . . ?
N10 Er1 N1 69.91(8) . . ?
C20 N1 C12 110.2(2) . . ?
C20 N1 C2 109.1(2) . . ?
C12 N1 C2 110.3(2) . . ?
C20 N1 Er1 107.96(18) . . ?
C12 N1 Er1 110.20(18) . . ?
C2 N1 Er1 108.95(18) . . ?
N1 C2 C3 112.8(3) . . ?
N1 C2 H21 109.0 . . ?
C3 C2 H21 109.0 . . ?
N1 C2 H22 109.0 . . ?
C3 C2 H22 109.0 . . ?
H21 C2 H22 107.8 . . ?
N4 C3 C2 112.0(3) . . ?
N4 C3 H31 109.2 . . ?
C2 C3 H31 109.2 . . ?
N4 C3 H32 109.2 . . ?
C2 C3 H32 109.2 . . ?
H31 C3 H32 107.9 . . ?
C50 N4 C3 111.8(2) . . ?
C50 N4 C5 108.7(2) . . ?
C3 N4 C5 109.1(2) . . ?
C50 N4 Er1 104.07(17) . . ?
C3 N4 Er1 112.40(18) . . ?
C5 N4 Er1 110.72(18) . . ?
N4 C5 C6 112.6(3) . . ?
N4 C5 H51 109.1 . . ?
C6 C5 H51 109.1 . . ?
N4 C5 H52 109.1 . . ?
C6 C5 H52 109.1 . . ?
H51 C5 H52 107.8 . . ?
N7 C6 C5 110.6(3) . . ?
N7 C6 H61 109.5 . . ?
C5 C6 H61 109.5 . . ?
N7 C6 H62 109.5 . . ?
C5 C6 H62 109.5 . . ?
H61 C6 H62 108.1 . . ?
C60 N7 C6 111.4(3) . . ?
C60 N7 C8 107.6(3) . . ?
C6 N7 C8 110.3(3) . . ?
C60 N7 Er1 104.48(19) . . ?
C6 N7 Er1 112.10(19) . . ?
C8 N7 Er1 110.78(18) . . ?
N7 C8 C9 112.2(3) . . ?
N7 C8 H81 109.2 . . ?
C9 C8 H81 109.2 . . ?
N7 C8 H82 109.2 . . ?
C9 C8 H82 109.2 . . ?
H81 C8 H82 107.9 . . ?
N10 C9 C8 111.3(3) . . ?
N10 C9 H91 109.4 . . ?
C8 C9 H91 109.4 . . ?
N10 C9 H92 109.4 . . ?
C8 C9 H92 109.4 . . ?
H91 C9 H92 108.0 . . ?
C70 N10 C11 109.1(2) . . ?
C70 N10 C9 111.8(2) . . ?
C11 N10 C9 110.4(2) . . ?
C70 N10 Er1 103.26(18) . . ?
C11 N10 Er1 110.34(18) . . ?
C9 N10 Er1 111.77(18) . . ?
N10 C11 C12 111.7(3) . . ?
N10 C11 H111 109.3 . . ?
C12 C11 H111 109.3 . . ?
N10 C11 H112 109.3 . . ?
C12 C11 H112 109.3 . . ?
H111 C11 H112 107.9 . . ?
N1 C12 C11 110.7(2) . . ?
N1 C12 H121 109.5 . . ?
C11 C12 H121 109.5 . . ?
N1 C12 H122 109.5 . . ?
C11 C12 H122 109.5 . . ?
H121 C12 H122 108.1 . . ?
N1 C20 P1 111.0(2) . . ?
N1 C20 H201 109.4 . . ?
P1 C20 H201 109.4 . . ?
N1 C20 H202 109.4 . . ?
P1 C20 H202 109.4 . . ?
H201 C20 H202 108.0 . . ?
O12 P1 O11 116.65(13) . . ?
O12 P1 C21 111.58(14) . . ?
O11 P1 C21 107.99(13) . . ?
O12 P1 C20 110.84(14) . . ?
O11 P1 C20 104.84(13) . . ?
C21 P1 C20 103.98(15) . . ?
P1 O11 Er1 125.20(12) . . ?
N22 C21 P1 112.0(2) . . ?
N22 C21 H211 109.2 . . ?
P1 C21 H211 109.2 . . ?
N22 C21 H212 109.2 . . ?
P1 C21 H212 109.2 . . ?
H211 C21 H212 107.9 . . ?
C30 N22 C40 110.5(3) . . ?
C30 N22 C21 111.2(3) . . ?
C40 N22 C21 110.6(3) . . ?
N22 C30 C31 113.3(3) . . ?
N22 C30 H301 108.9 . . ?
C31 C30 H301 108.9 . . ?
N22 C30 H302 108.9 . . ?
C31 C30 H302 108.9 . . ?
H301 C30 H302 107.7 . . ?
C36 C31 C32 118.8(3) . . ?
C36 C31 C30 121.8(3) . . ?
C32 C31 C30 119.4(3) . . ?
C31 C32 C33 120.5(4) . . ?
C31 C32 H321 119.8 . . ?
C33 C32 H321 119.8 . . ?
C34 C33 C32 119.7(4) . . ?
C34 C33 H331 120.1 . . ?
C32 C33 H331 120.1 . . ?
C33 C34 C35 120.3(4) . . ?
C33 C34 H341 119.8 . . ?
C35 C34 H341 119.8 . . ?
C34 C35 C36 120.3(4) . . ?
C34 C35 H351 119.9 . . ?
C36 C35 H351 119.9 . . ?
C31 C36 C35 120.4(4) . . ?
C31 C36 H361 119.8 . . ?
C35 C36 H361 119.8 . . ?
N22 C40 C41 113.6(3) . . ?
N22 C40 H401 108.8 . . ?
C41 C40 H401 108.8 . . ?
N22 C40 H402 108.8 . . ?
C41 C40 H402 108.8 . . ?
H401 C40 H402 107.7 . . ?
C42 C41 C46 118.6(4) . . ?
C42 C41 C40 121.6(4) . . ?
C46 C41 C40 119.8(3) . . ?
C41 C42 C43 120.1(4) . . ?
C41 C42 H421 119.9 . . ?
C43 C42 H421 119.9 . . ?
C44 C43 C42 120.8(4) . . ?
C44 C43 H431 119.6 . . ?
C42 C43 H431 119.6 . . ?
C43 C44 C45 119.4(4) . . ?
C43 C44 H441 120.3 . . ?
C45 C44 H441 120.3 . . ?
C44 C45 C46 119.8(5) . . ?
C44 C45 H451 120.1 . . ?
C46 C45 H451 120.1 . . ?
C41 C46 C45 121.2(4) . . ?
C41 C46 H461 119.4 . . ?
C45 C46 H461 119.4 . . ?
N4 C50 C51 111.3(3) . . ?
N4 C50 H501 109.4 . . ?
C51 C50 H501 109.4 . . ?
N4 C50 H502 109.4 . . ?
C51 C50 H502 109.4 . . ?
H501 C50 H502 108.0 . . ?
O52 C51 O51 125.3(3) . . ?
O52 C51 C50 118.3(3) . . ?
O51 C51 C50 116.3(3) . . ?
C51 O51 Er1 118.4(2) . . ?
N7 C60 C61 111.0(3) . . ?
N7 C60 H601 109.4 . . ?
C61 C60 H601 109.4 . . ?
N7 C60 H602 109.4 . . ?
C61 C60 H602 109.4 . . ?
H601 C60 H602 108.0 . . ?
O62 C61 O61 124.3(3) . . ?
O62 C61 C60 118.8(3) . . ?
O61 C61 C60 116.8(3) . . ?
C61 O61 Er1 121.1(2) . . ?
N10 C70 C71 112.4(3) . . ?
N10 C70 H701 109.1 . . ?
C71 C70 H701 109.1 . . ?
N10 C70 H702 109.1 . . ?
C71 C70 H702 109.1 . . ?
H701 C70 H702 107.9 . . ?
O72 C71 O71 125.5(3) . . ?
O72 C71 C70 118.3(3) . . ?
O71 C71 C70 116.2(3) . . ?
C71 O71 Er1 115.15(18) . . ?
H11A N1A H12A 95(3) . . ?
H11A N1A H13A 120(3) . . ?
H12A N1A H13A 110(3) . . ?
H11A N1A H14A 110.5 . . ?
H12A N1A H14A 120.2 . . ?
H13A N1A H14A 102.2 . . ?
H11W O1W H12W 113.2 . . ?
H21W O2W H22W 108(4) . . ?
H31W O3W H32W 102.0 . . ?
H41W O4W H42W 98.1 . . ?

_refine_diff_density_max         1.798
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.112

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

data_tb-dbam
_database_code_depnum_ccdc_archive 'CCDC 1959637'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 N5 O9 P Tb, 3(H2 O), H4 N'
_chemical_formula_sum            'C30 H52 N6 O12 P Tb'
_chemical_formula_weight         878.66

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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   47.048(2)
_cell_length_b                   10.2943(4)
_cell_length_c                   15.2057(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.717(2)
_cell_angle_gamma                90
_cell_volume                     7363.9(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9936
_cell_measurement_theta_min      2.3667
_cell_measurement_theta_max      26.0048

_exptl_crystal_description       prism
_exptl_crystal_colour            pink
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_F_000             3600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.219
_exptl_absorpt_coefficient_mu    2.031
_shelx_estimated_absorpt_T_min   0.475
_shelx_estimated_absorpt_T_max   0.665
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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 8.3333
_diffrn_reflns_number            19510
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.731
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7234
_reflns_number_gt                6599
_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.
 
 _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 Instrument Service v2014.11.0.1'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0069P)²+127.5554P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7234
_refine_ls_number_parameters     484
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0522
_refine_ls_wR_factor_ref         0.1159
_refine_ls_wR_factor_gt          0.1142
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_restrained_S_all      1.239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Tb1 Tb 0.16123(2) 0.77332(3) 0.10150(2) 0.01311(9) Uani 1 1 d . . . . .
O1C O 0.17564(9) 0.6377(4) 0.2385(3) 0.0167(9) Uani 1 1 d . . . . .
H11C H 0.1736 0.5485 0.2319 0.020 Uiso 1 1 d R U . . .
H12C H 0.1650 0.6297 0.2860 0.020 Uiso 1 1 d R U . . .
N1 N 0.11372(10) 0.7549(5) -0.0004(3) 0.0157(11) Uani 1 1 d . . . . .
C2 C 0.12055(13) 0.6995(6) -0.0878(4) 0.0181(13) Uani 1 1 d . . . . .
H21 H 0.1042 0.7130 -0.1283 0.022 Uiso 1 1 calc R U . . .
H22 H 0.1236 0.6048 -0.0818 0.022 Uiso 1 1 calc R U . . .
C3 C 0.14673(13) 0.7609(6) -0.1267(4) 0.0177(13) Uani 1 1 d . . . . .
H31 H 0.1506 0.7204 -0.1844 0.021 Uiso 1 1 calc R U . . .
H32 H 0.1431 0.8546 -0.1367 0.021 Uiso 1 1 calc R U . . .
N4 N 0.17219(11) 0.7457(5) -0.0685(3) 0.0148(10) Uani 1 1 d . . . . .
C5 C 0.19481(13) 0.8367(6) -0.0969(4) 0.0203(13) Uani 1 1 d . . . . .
H51 H 0.1959 0.8357 -0.1619 0.024 Uiso 1 1 calc R U . . .
H52 H 0.2134 0.8070 -0.0730 0.024 Uiso 1 1 calc R U . . .
C6 C 0.18929(14) 0.9740(6) -0.0662(4) 0.0191(13) Uani 1 1 d . . . . .
H61 H 0.2050 1.0311 -0.0853 0.023 Uiso 1 1 calc R U . . .
H62 H 0.1714 1.0063 -0.0935 0.023 Uiso 1 1 calc R U . . .
N7 N 0.18699(11) 0.9798(5) 0.0313(3) 0.0181(11) Uani 1 1 d . . . . .
C8 C 0.17330(14) 1.1042(6) 0.0562(4) 0.0200(14) Uani 1 1 d . . . . .
H81 H 0.1806 1.1746 0.0184 0.024 Uiso 1 1 calc R U . . .
H82 H 0.1785 1.1252 0.1179 0.024 Uiso 1 1 calc R U . . .
C9 C 0.14139(14) 1.0987(6) 0.0470(4) 0.0216(14) Uani 1 1 d . . . . .
H91 H 0.1331 1.1819 0.0668 0.026 Uiso 1 1 calc R U . . .
H92 H 0.1361 1.0859 -0.0156 0.026 Uiso 1 1 calc R U . . .
N10 N 0.12985(11) 0.9908(5) 0.1001(3) 0.0177(11) Uani 1 1 d . . . . .
C11 C 0.10021(14) 0.9626(6) 0.0711(4) 0.0224(14) Uani 1 1 d . . . . .
H111 H 0.0900 1.0454 0.0611 0.027 Uiso 1 1 calc R U . . .
H112 H 0.0903 0.9148 0.1182 0.027 Uiso 1 1 calc R U . . .
C12 C 0.09942(13) 0.8827(6) -0.0126(4) 0.0193(13) Uani 1 1 d . . . . .
H121 H 0.0794 0.8683 -0.0310 0.023 Uiso 1 1 calc R U . . .
H122 H 0.1089 0.9313 -0.0601 0.023 Uiso 1 1 calc R U . . .
C20 C 0.09421(12) 0.6630(6) 0.0450(4) 0.0174(13) Uani 1 1 d . . . . .
H201 H 0.0784 0.6382 0.0047 0.021 Uiso 1 1 calc R U . . .
H202 H 0.0859 0.7059 0.0971 0.021 Uiso 1 1 calc R U . . .
P1 P 0.11370(3) 0.51797(15) 0.07944(10) 0.0152(3) Uani 1 1 d . . . . .
O11 O 0.14457(8) 0.5628(4) 0.0874(3) 0.0150(9) Uani 1 1 d . . . . .
O12 O 0.10830(9) 0.4061(4) 0.0190(3) 0.0221(10) Uani 1 1 d . . . . .
C21 C 0.10075(13) 0.4859(7) 0.1887(4) 0.0231(14) Uani 1 1 d . . . . .
H211 H 0.1115 0.4128 0.2152 0.028 Uiso 1 1 calc R U . . .
H212 H 0.1037 0.5635 0.2262 0.028 Uiso 1 1 calc R U . . .
N22 N 0.07029(12) 0.4535(6) 0.1847(4) 0.0247(12) Uani 1 1 d . . . . .
C30 C 0.06573(15) 0.3145(7) 0.1664(6) 0.0366(19) Uani 1 1 d . . . . .
H301 H 0.0672 0.2655 0.2223 0.044 Uiso 1 1 calc R U . . .
H302 H 0.0810 0.2831 0.1274 0.044 Uiso 1 1 calc R U . . .
C31 C 0.03741(15) 0.2872(7) 0.1239(5) 0.0289(16) Uani 1 1 d . . . . .
C32A C 0.0252(3) 0.1637(15) 0.1254(12) 0.039(4) Uani 0.500(10) 1 d . . P A 1
H32A H 0.0348 0.0959 0.1562 0.046 Uiso 0.500(10) 1 calc R U P A 1
C33A C -0.0005(4) 0.137(2) 0.0830(14) 0.059(6) Uani 0.500(10) 1 d . . P A 1
H33A H -0.0088 0.0533 0.0867 0.071 Uiso 0.500(10) 1 calc R U P A 1
C32B C 0.0142(3) 0.2478(13) 0.1694(11) 0.034(4) Uani 0.500(10) 1 d . . P A 2
H32B H 0.0152 0.2388 0.2316 0.041 Uiso 0.500(10) 1 calc R U P A 2
C33B C -0.0110(4) 0.2208(17) 0.1234(14) 0.048(5) Uani 0.500(10) 1 d . . P A 2
H33B H -0.0271 0.1939 0.1555 0.057 Uiso 0.500(10) 1 calc R U P A 2
C34 C -0.0132(2) 0.2311(11) 0.0371(8) 0.059(3) Uani 1 1 d . . . . .
H34A H -0.0292 0.2070 0.0018 0.071 Uiso 0.500(10) 1 calc R U P A 1
H34B H -0.0307 0.2148 0.0069 0.071 Uiso 0.500(10) 1 calc R U P A 2
C35A C 0.0204(3) 0.3829(16) 0.0759(12) 0.042(5) Uani 0.500(10) 1 d . . P A 1
H35A H 0.0274 0.4690 0.0713 0.051 Uiso 0.500(10) 1 calc R U P A 1
C36A C -0.0059(4) 0.3534(18) 0.0362(13) 0.051(5) Uani 0.500(10) 1 d . . P A 1
H36A H -0.0176 0.4184 0.0102 0.062 Uiso 0.500(10) 1 calc R U P A 1
C35B C 0.0129(3) 0.2697(18) -0.0106(13) 0.047(5) Uani 0.500(10) 1 d . . P A 2
H35B H 0.0125 0.2766 -0.0729 0.057 Uiso 0.500(10) 1 calc R U P A 2
C36B C 0.0381(3) 0.2956(15) 0.0358(10) 0.032(4) Uani 0.500(10) 1 d . . P A 2
H36B H 0.0551 0.3184 0.0062 0.038 Uiso 0.500(10) 1 calc R U P A 2
C40 C 0.05498(16) 0.4945(9) 0.2637(5) 0.043(2) Uani 1 1 d . . . . .
H401 H 0.0655 0.4669 0.3174 0.051 Uiso 0.465(13) 1 calc R U P B 3
H402 H 0.0358 0.4550 0.2644 0.051 Uiso 0.465(13) 1 calc R U P B 3
H403 H 0.0358 0.4550 0.2607 0.051 Uiso 0.535(13) 1 calc R U P B 4
H404 H 0.0649 0.4559 0.3152 0.051 Uiso 0.535(13) 1 calc R U P B 4
C41A C 0.0525(4) 0.6536(12) 0.2604(11) 0.028(3) Uani 0.465(13) 1 d G . P B 3
C42A C 0.0347(4) 0.7085(15) 0.1969(10) 0.044(3) Uani 0.465(13) 1 d G U P B 3
H421 H 0.0251 0.6545 0.1555 0.052 Uiso 0.465(13) 1 calc R U P B 3
C43A C 0.0310(3) 0.8424(16) 0.1938(10) 0.062(4) Uani 0.465(13) 1 d G U P B 3
H431 H 0.0189 0.8799 0.1504 0.075 Uiso 0.465(13) 1 calc R U P B 3
C44A C 0.0451(3) 0.9214(12) 0.2543(12) 0.065(4) Uani 0.465(13) 1 d G U P B 3
H441 H 0.0426 1.0129 0.2523 0.079 Uiso 0.465(13) 1 calc R U P B 3
C45A C 0.0629(3) 0.8665(15) 0.3179(11) 0.067(4) Uani 0.465(13) 1 d G U P B 3
H451 H 0.0725 0.9206 0.3593 0.080 Uiso 0.465(13) 1 calc R U P B 3
C46A C 0.0666(3) 0.7327(16) 0.3210(10) 0.053(5) Uani 0.465(13) 1 d G . P B 3
H461 H 0.0787 0.6952 0.3644 0.064 Uiso 0.465(13) 1 calc R U P B 3
C41B C 0.0516(4) 0.6240(10) 0.2806(9) 0.028(3) Uani 0.535(13) 1 d G . P B 4
C42B C 0.0389(4) 0.6991(13) 0.2150(8) 0.044(3) Uani 0.535(13) 1 d G U P B 4
H422 H 0.0321 0.6593 0.1624 0.052 Uiso 0.535(13) 1 calc R U P B 4
C43B C 0.0361(3) 0.8325(13) 0.2263(9) 0.062(4) Uani 0.535(13) 1 d G U P B 4
H432 H 0.0275 0.8838 0.1815 0.075 Uiso 0.535(13) 1 calc R U P B 4
C44B C 0.0460(3) 0.8907(11) 0.3032(10) 0.065(4) Uani 0.535(13) 1 d G U P B 4
H442 H 0.0441 0.9819 0.3110 0.079 Uiso 0.535(13) 1 calc R U P B 4
C45B C 0.0587(3) 0.8157(14) 0.3689(9) 0.067(4) Uani 0.535(13) 1 d G U P B 4
H452 H 0.0654 0.8555 0.4214 0.080 Uiso 0.535(13) 1 calc R U P B 4
C46B C 0.0615(3) 0.6823(13) 0.3575(9) 0.053(5) Uani 0.535(13) 1 d G . P B 4
H462 H 0.0701 0.6310 0.4023 0.064 Uiso 0.535(13) 1 calc R U P B 4
C50 C 0.18359(13) 0.6130(6) -0.0744(4) 0.0168(13) Uani 1 1 d . . . . .
H501 H 0.1939 0.6031 -0.1303 0.020 Uiso 1 1 calc R U . . .
H502 H 0.1677 0.5501 -0.0747 0.020 Uiso 1 1 calc R U . . .
C51 C 0.20369(13) 0.5826(6) 0.0024(4) 0.0172(13) Uani 1 1 d . . . . .
O51 O 0.20336(9) 0.6595(4) 0.0676(3) 0.0193(9) Uani 1 1 d . . . . .
O52 O 0.21885(10) 0.4844(5) -0.0042(3) 0.0278(11) Uani 1 1 d . . . . .
C60 C 0.21560(13) 0.9771(7) 0.0726(4) 0.0227(14) Uani 1 1 d . . . . .
H601 H 0.2254 1.0607 0.0621 0.027 Uiso 1 1 calc R U . . .
H602 H 0.2270 0.9069 0.0462 0.027 Uiso 1 1 calc R U . . .
C61 C 0.21292(14) 0.9540(6) 0.1721(4) 0.0215(14) Uani 1 1 d . . . . .
O61 O 0.19139(9) 0.8934(4) 0.1975(3) 0.0215(10) Uani 1 1 d . . . . .
O62 O 0.23250(10) 0.9948(5) 0.2209(3) 0.0300(12) Uani 1 1 d . . . . .
C70 C 0.12917(14) 1.0260(6) 0.1939(4) 0.0195(13) Uani 1 1 d . . . . .
H701 H 0.1126 1.0829 0.2047 0.023 Uiso 1 1 calc R U . . .
H702 H 0.1466 1.0752 0.2096 0.023 Uiso 1 1 calc R U . . .
C71 C 0.12722(13) 0.9062(6) 0.2517(4) 0.0177(13) Uani 1 1 d . . . . .
O71 O 0.12874(9) 0.7978(4) 0.2135(3) 0.0181(9) Uani 1 1 d . . . . .
O72 O 0.12480(11) 0.9224(4) 0.3326(3) 0.0284(11) Uani 1 1 d . . . . .
N1A N 0.22586(11) 0.6630(5) 0.3402(3) 0.0221(12) Uani 1 1 d . . . . .
H11A H 0.2084 0.6748 0.3190 0.026 Uiso 1 1 d R U . . .
H12A H 0.2344 0.7263 0.3469 0.026 Uiso 1 1 d R U . . .
H13A H 0.2198 0.6395 0.3901 0.026 Uiso 1 1 d R U . . .
H14A H 0.2377 0.6109 0.3187 0.026 Uiso 1 1 d R U . . .
O1W O 0.17908(10) 0.3782(4) 0.1831(3) 0.0275(11) Uani 1 1 d . . . . .
H11W H 0.1695 0.3952 0.1470 0.033 Uiso 1 1 d R U . . .
H12W H 0.1976 0.3593 0.1707 0.033 Uiso 1 1 d R U . . .
O2W O 0.23870(10) 0.3775(4) 0.1444(3) 0.0271(11) Uani 1 1 d . . . . .
H21W H 0.2479 0.4322 0.1894 0.032 Uiso 1 1 d R U . . .
H22W H 0.2297 0.4213 0.0974 0.032 Uiso 1 1 d R U . . .
O3W O 0.14497(12) 0.6750(5) 0.3905(3) 0.0354(13) Uani 1 1 d . . . . .
H31W H 0.1334 0.6497 0.4293 0.042 Uiso 1 1 d R U . . .
H32W H 0.1341 0.7472 0.3689 0.042 Uiso 1 1 d R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O11 2.314(4) . ?
Tb1 O71 2.317(4) . ?
Tb1 O51 2.365(4) . ?
Tb1 O61 2.371(4) . ?
Tb1 O1C 2.591(4) . ?
Tb1 N4 2.657(5) . ?
Tb1 N7 2.676(5) . ?
Tb1 N10 2.682(5) . ?
Tb1 N1 2.710(5) . ?
O1C H11C 0.9283 . ?
O1C H12C 0.8867 . ?
N1 C2 1.484(7) . ?
N1 C12 1.488(8) . ?
N1 C20 1.493(8) . ?
C2 C3 1.512(9) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.489(7) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.471(7) . ?
N4 C5 1.486(8) . ?
C5 C6 1.512(9) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.489(7) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.479(8) . ?
N7 C8 1.484(8) . ?
C8 C9 1.507(9) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.480(8) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.472(7) . ?
N10 C11 1.485(8) . ?
C11 C12 1.517(9) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.825(6) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.493(4) . ?
P1 O11 1.527(4) . ?
P1 C21 1.807(6) . ?
C21 N22 1.472(8) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C40 1.471(9) . ?
N22 C30 1.472(9) . ?
C30 C31 1.501(10) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36B 1.344(17) . ?
C31 C32B 1.361(15) . ?
C31 C32A 1.394(16) . ?
C31 C35A 1.460(17) . ?
C32A C33A 1.39(3) . ?
C32A H32A 0.9500 . ?
C33A C34 1.33(2) . ?
C33A H33A 0.9500 . ?
C32B C33B 1.40(2) . ?
C32B H32B 0.9500 . ?
C33B C34 1.32(2) . ?
C33B H33B 0.9500 . ?
C34 C36A 1.31(2) . ?
C34 C35B 1.49(2) . ?
C34 H34A 0.9500 . ?
C34 H34B 0.9500 . ?
C35A C36A 1.40(2) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C35B C36B 1.40(2) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C40 C41B 1.367(14) . ?
C40 C41A 1.642(16) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C40 H403 0.9900 . ?
C40 H404 0.9900 . ?
C41A C42A 1.3900 . ?
C41A C46A 1.3900 . ?
C42A C43A 1.3900 . ?
C42A H421 0.9500 . ?
C43A C44A 1.3900 . ?
C43A H431 0.9500 . ?
C44A C45A 1.3900 . ?
C44A H441 0.9500 . ?
C45A C46A 1.3900 . ?
C45A H451 0.9500 . ?
C46A H461 0.9500 . ?
C41B C42B 1.3900 . ?
C41B C46B 1.3900 . ?
C42B C43B 1.3900 . ?
C42B H422 0.9500 . ?
C43B C44B 1.3900 . ?
C43B H432 0.9500 . ?
C44B C45B 1.3900 . ?
C44B H442 0.9500 . ?
C45B C46B 1.3900 . ?
C45B H452 0.9500 . ?
C46B H462 0.9500 . ?
C50 C51 1.526(8) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.242(7) . ?
C51 O51 1.269(7) . ?
C60 C61 1.537(8) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.248(7) . ?
C61 O61 1.255(8) . ?
C70 C71 1.517(8) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.248(7) . ?
C71 O71 1.260(7) . ?
N1A H11A 0.8857 . ?
N1A H12A 0.7722 . ?
N1A H13A 0.8493 . ?
N1A H14A 0.8428 . ?
O1W H11W 0.7271 . ?
O1W H12W 0.9161 . ?
O2W H21W 0.9819 . ?
O2W H22W 0.9422 . ?
O3W H31W 0.8474 . ?
O3W H32W 0.9590 . ?

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
O11 Tb1 O71 86.82(14) . . ?
O11 Tb1 O51 78.43(14) . . ?
O71 Tb1 O51 140.96(14) . . ?
O11 Tb1 O61 138.16(14) . . ?
O71 Tb1 O61 83.43(15) . . ?
O51 Tb1 O61 84.01(15) . . ?
O11 Tb1 O1C 69.82(13) . . ?
O71 Tb1 O1C 68.64(14) . . ?
O51 Tb1 O1C 72.35(14) . . ?
O61 Tb1 O1C 68.72(14) . . ?
O11 Tb1 N4 83.05(14) . . ?
O71 Tb1 N4 149.87(15) . . ?
O51 Tb1 N4 63.99(14) . . ?
O61 Tb1 N4 122.19(15) . . ?
O1C Tb1 N4 132.25(14) . . ?
O11 Tb1 N7 149.51(15) . . ?
O71 Tb1 N7 120.87(15) . . ?
O51 Tb1 N7 85.50(16) . . ?
O61 Tb1 N7 63.95(14) . . ?
O1C Tb1 N7 129.30(14) . . ?
N4 Tb1 N7 66.59(15) . . ?
O11 Tb1 N10 126.55(15) . . ?
O71 Tb1 N10 63.04(15) . . ?
O51 Tb1 N10 151.01(15) . . ?
O61 Tb1 N10 83.96(15) . . ?
O1C Tb1 N10 126.48(14) . . ?
N4 Tb1 N10 101.26(14) . . ?
N7 Tb1 N10 65.52(16) . . ?
O11 Tb1 N1 66.75(14) . . ?
O71 Tb1 N1 83.17(15) . . ?
O51 Tb1 N1 121.88(14) . . ?
O61 Tb1 N1 150.63(15) . . ?
O1C Tb1 N1 128.87(14) . . ?
N4 Tb1 N1 66.75(15) . . ?
N7 Tb1 N1 101.66(15) . . ?
N10 Tb1 N1 66.68(15) . . ?
Tb1 O1C H11C 114.9 . . ?
Tb1 O1C H12C 124.1 . . ?
H11C O1C H12C 86.5 . . ?
C2 N1 C12 109.3(4) . . ?
C2 N1 C20 108.2(5) . . ?
C12 N1 C20 109.8(5) . . ?
C2 N1 Tb1 110.6(3) . . ?
C12 N1 Tb1 112.2(3) . . ?
C20 N1 Tb1 106.7(3) . . ?
N1 C2 C3 112.1(5) . . ?
N1 C2 H21 109.2 . . ?
C3 C2 H21 109.2 . . ?
N1 C2 H22 109.2 . . ?
C3 C2 H22 109.2 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 112.1(5) . . ?
N4 C3 H31 109.2 . . ?
C2 C3 H31 109.2 . . ?
N4 C3 H32 109.2 . . ?
C2 C3 H32 109.2 . . ?
H31 C3 H32 107.9 . . ?
C50 N4 C5 107.8(5) . . ?
C50 N4 C3 110.6(5) . . ?
C5 N4 C3 109.5(5) . . ?
C50 N4 Tb1 103.6(3) . . ?
C5 N4 Tb1 111.4(3) . . ?
C3 N4 Tb1 113.7(3) . . ?
N4 C5 C6 111.9(5) . . ?
N4 C5 H51 109.2 . . ?
C6 C5 H51 109.2 . . ?
N4 C5 H52 109.2 . . ?
C6 C5 H52 109.2 . . ?
H51 C5 H52 107.9 . . ?
N7 C6 C5 111.2(5) . . ?
N7 C6 H61 109.4 . . ?
C5 C6 H61 109.4 . . ?
N7 C6 H62 109.4 . . ?
C5 C6 H62 109.4 . . ?
H61 C6 H62 108.0 . . ?
C60 N7 C8 107.7(5) . . ?
C60 N7 C6 110.2(5) . . ?
C8 N7 C6 109.0(5) . . ?
C60 N7 Tb1 103.3(4) . . ?
C8 N7 Tb1 112.5(4) . . ?
C6 N7 Tb1 113.8(3) . . ?
N7 C8 C9 112.3(5) . . ?
N7 C8 H81 109.2 . . ?
C9 C8 H81 109.2 . . ?
N7 C8 H82 109.2 . . ?
C9 C8 H82 109.2 . . ?
H81 C8 H82 107.9 . . ?
N10 C9 C8 110.5(5) . . ?
N10 C9 H91 109.6 . . ?
C8 C9 H91 109.6 . . ?
N10 C9 H92 109.6 . . ?
C8 C9 H92 109.6 . . ?
H91 C9 H92 108.1 . . ?
C70 N10 C9 110.9(5) . . ?
C70 N10 C11 107.7(5) . . ?
C9 N10 C11 109.5(5) . . ?
C70 N10 Tb1 102.5(3) . . ?
C9 N10 Tb1 115.1(4) . . ?
C11 N10 Tb1 110.7(4) . . ?
N10 C11 C12 111.6(5) . . ?
N10 C11 H111 109.3 . . ?
C12 C11 H111 109.3 . . ?
N10 C11 H112 109.3 . . ?
C12 C11 H112 109.3 . . ?
H111 C11 H112 108.0 . . ?
N1 C12 C11 111.6(5) . . ?
N1 C12 H121 109.3 . . ?
C11 C12 H121 109.3 . . ?
N1 C12 H122 109.3 . . ?
C11 C12 H122 109.3 . . ?
H121 C12 H122 108.0 . . ?
N1 C20 P1 109.9(4) . . ?
N1 C20 H201 109.7 . . ?
P1 C20 H201 109.7 . . ?
N1 C20 H202 109.7 . . ?
P1 C20 H202 109.7 . . ?
H201 C20 H202 108.2 . . ?
O12 P1 O11 115.8(3) . . ?
O12 P1 C21 111.6(3) . . ?
O11 P1 C21 108.3(3) . . ?
O12 P1 C20 111.9(3) . . ?
O11 P1 C20 104.5(3) . . ?
C21 P1 C20 103.8(3) . . ?
P1 O11 Tb1 127.6(2) . . ?
N22 C21 P1 110.0(4) . . ?
N22 C21 H211 109.7 . . ?
P1 C21 H211 109.7 . . ?
N22 C21 H212 109.7 . . ?
P1 C21 H212 109.7 . . ?
H211 C21 H212 108.2 . . ?
C40 N22 C21 112.8(6) . . ?
C40 N22 C30 111.2(6) . . ?
C21 N22 C30 111.6(5) . . ?
N22 C30 C31 112.9(6) . . ?
N22 C30 H301 109.0 . . ?
C31 C30 H301 109.0 . . ?
N22 C30 H302 109.0 . . ?
C31 C30 H302 109.0 . . ?
H301 C30 H302 107.8 . . ?
C36B C31 C32B 123.8(11) . . ?
C32A C31 C35A 113.6(11) . . ?
C36B C31 C30 112.7(8) . . ?
C32B C31 C30 123.4(10) . . ?
C32A C31 C30 121.8(9) . . ?
C35A C31 C30 124.6(8) . . ?
C33A C32A C31 121.8(16) . . ?
C33A C32A H32A 119.1 . . ?
C31 C32A H32A 119.1 . . ?
C34 C33A C32A 118.9(17) . . ?
C34 C33A H33A 120.6 . . ?
C32A C33A H33A 120.6 . . ?
C31 C32B C33B 119.0(15) . . ?
C31 C32B H32B 120.5 . . ?
C33B C32B H32B 120.5 . . ?
C34 C33B C32B 122.7(15) . . ?
C34 C33B H33B 118.7 . . ?
C32B C33B H33B 118.7 . . ?
C36A C34 C33A 126.1(14) . . ?
C33B C34 C35B 116.7(12) . . ?
C36A C34 H34A 117.0 . . ?
C33A C34 H34A 117.0 . . ?
C33B C34 H34B 121.7 . . ?
C35B C34 H34B 121.7 . . ?
C36A C35A C31 123.0(14) . . ?
C36A C35A H35A 118.5 . . ?
C31 C35A H35A 118.5 . . ?
C34 C36A C35A 115.9(16) . . ?
C34 C36A H36A 122.1 . . ?
C35A C36A H36A 122.1 . . ?
C36B C35B C34 120.3(15) . . ?
C36B C35B H35B 119.8 . . ?
C34 C35B H35B 119.8 . . ?
C31 C36B C35B 117.4(13) . . ?
C31 C36B H36B 121.3 . . ?
C35B C36B H36B 121.3 . . ?
C41B C40 N22 119.6(9) . . ?
N22 C40 C41A 107.3(9) . . ?
N22 C40 H401 110.3 . . ?
C41A C40 H401 110.3 . . ?
N22 C40 H402 110.3 . . ?
C41A C40 H402 110.3 . . ?
H401 C40 H402 108.5 . . ?
C41B C40 H403 107.4 . . ?
N22 C40 H403 107.4 . . ?
C41B C40 H404 107.4 . . ?
N22 C40 H404 107.4 . . ?
H403 C40 H404 107.0 . . ?
C42A C41A C46A 120.0 . . ?
C42A C41A C40 117.9(10) . . ?
C46A C41A C40 122.0(10) . . ?
C43A C42A C41A 120.0 . . ?
C43A C42A H421 120.0 . . ?
C41A C42A H421 120.0 . . ?
C42A C43A C44A 120.0 . . ?
C42A C43A H431 120.0 . . ?
C44A C43A H431 120.0 . . ?
C43A C44A C45A 120.0 . . ?
C43A C44A H441 120.0 . . ?
C45A C44A H441 120.0 . . ?
C46A C45A C44A 120.0 . . ?
C46A C45A H451 120.0 . . ?
C44A C45A H451 120.0 . . ?
C45A C46A C41A 120.0 . . ?
C45A C46A H461 120.0 . . ?
C41A C46A H461 120.0 . . ?
C40 C41B C42B 117.3(10) . . ?
C40 C41B C46B 122.6(10) . . ?
C42B C41B C46B 120.0 . . ?
C41B C42B C43B 120.0 . . ?
C41B C42B H422 120.0 . . ?
C43B C42B H422 120.0 . . ?
C44B C43B C42B 120.0 . . ?
C44B C43B H432 120.0 . . ?
C42B C43B H432 120.0 . . ?
C43B C44B C45B 120.0 . . ?
C43B C44B H442 120.0 . . ?
C45B C44B H442 120.0 . . ?
C46B C45B C44B 120.0 . . ?
C46B C45B H452 120.0 . . ?
C44B C45B H452 120.0 . . ?
C45B C46B C41B 120.0 . . ?
C45B C46B H462 120.0 . . ?
C41B C46B H462 120.0 . . ?
N4 C50 C51 111.5(5) . . ?
N4 C50 H501 109.3 . . ?
C51 C50 H501 109.3 . . ?
N4 C50 H502 109.3 . . ?
C51 C50 H502 109.3 . . ?
H501 C50 H502 108.0 . . ?
O52 C51 O51 125.7(6) . . ?
O52 C51 C50 117.1(5) . . ?
O51 C51 C50 117.2(5) . . ?
C51 O51 Tb1 119.8(4) . . ?
N7 C60 C61 109.6(5) . . ?
N7 C60 H601 109.8 . . ?
C61 C60 H601 109.8 . . ?
N7 C60 H602 109.8 . . ?
C61 C60 H602 109.8 . . ?
H601 C60 H602 108.2 . . ?
O62 C61 O61 125.2(6) . . ?
O62 C61 C60 117.6(6) . . ?
O61 C61 C60 117.2(5) . . ?
C61 O61 Tb1 123.2(4) . . ?
N10 C70 C71 111.3(5) . . ?
N10 C70 H701 109.4 . . ?
C71 C70 H701 109.4 . . ?
N10 C70 H702 109.4 . . ?
C71 C70 H702 109.4 . . ?
H701 C70 H702 108.0 . . ?
O72 C71 O71 125.3(6) . . ?
O72 C71 C70 118.0(5) . . ?
O71 C71 C70 116.7(5) . . ?
C71 O71 Tb1 118.5(4) . . ?
H11A N1A H12A 114.3 . . ?
H11A N1A H13A 92.6 . . ?
H12A N1A H13A 107.5 . . ?
H11A N1A H14A 124.1 . . ?
H12A N1A H14A 104.0 . . ?
H13A N1A H14A 113.3 . . ?
H11W O1W H12W 118.4 . . ?
H21W O2W H22W 116.4 . . ?
H31W O3W H32W 97.5 . . ?

_refine_diff_density_max         2.231
_refine_diff_density_min         -2.719
_refine_diff_density_rms         0.146

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

data_eudo3apdbam
_database_code_depnum_ccdc_archive 'CCDC 1959629'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 Eu N5 O9 P, 3(H2 O), H4 N'
_chemical_formula_sum            'C30 H52 Eu N6 O12 P'
_chemical_formula_weight         871.70

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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   47.136(3)
_cell_length_b                   10.3082(5)
_cell_length_c                   15.2253(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.685(2)
_cell_angle_gamma                90
_cell_volume                     7397.3(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9811
_cell_measurement_theta_min      2.5928
_cell_measurement_theta_max      27.5212

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_F_000             3584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.506
_exptl_crystal_size_mid          0.378
_exptl_crystal_size_min          0.096
_exptl_absorpt_coefficient_mu    1.806
_shelx_estimated_absorpt_T_min   0.462
_shelx_estimated_absorpt_T_max   0.846
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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 8.3333
_diffrn_reflns_number            33793
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.338
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8492
_reflns_number_gt                8117
_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.
 
 _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 Instrument Service v2013.12.0.0'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+161.8198P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8492
_refine_ls_number_parameters     438
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1369
_refine_ls_wR_factor_gt          0.1358
_refine_ls_goodness_of_fit_ref   1.382
_refine_ls_restrained_S_all      1.382
_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 0.16126(2) 0.77245(3) 0.10356(2) 0.01094(9) Uani 1 1 d . . . . .
O1C O 0.17546(9) 0.6369(4) 0.2408(3) 0.0148(9) Uani 1 1 d . . . . .
H11C H 0.1739 0.5548 0.2258 0.018 Uiso 1 1 d R U . . .
H12C H 0.1631 0.6352 0.2842 0.018 Uiso 1 1 d R U . . .
N1 N 0.11361(11) 0.7539(5) 0.0006(3) 0.0124(10) Uani 1 1 d . . . . .
C2 C 0.12086(13) 0.6988(6) -0.0867(4) 0.0161(12) Uani 1 1 d . . . . .
H21 H 0.1046 0.7114 -0.1276 0.019 Uiso 1 1 calc R U . . .
H22 H 0.1241 0.6043 -0.0805 0.019 Uiso 1 1 calc R U . . .
C3 C 0.14702(13) 0.7608(6) -0.1253(4) 0.0151(12) Uani 1 1 d . . . . .
H31 H 0.1509 0.7205 -0.1830 0.018 Uiso 1 1 calc R U . . .
H32 H 0.1433 0.8542 -0.1352 0.018 Uiso 1 1 calc R U . . .
N4 N 0.17238(11) 0.7461(5) -0.0675(3) 0.0122(10) Uani 1 1 d . . . . .
C5 C 0.19490(13) 0.8380(7) -0.0953(4) 0.0178(13) Uani 1 1 d . . . . .
H51 H 0.1961 0.8375 -0.1602 0.021 Uiso 1 1 calc R U . . .
H52 H 0.2134 0.8087 -0.0713 0.021 Uiso 1 1 calc R U . . .
C6 C 0.18916(14) 0.9751(7) -0.0642(4) 0.0179(13) Uani 1 1 d . . . . .
H61 H 0.2047 1.0327 -0.0834 0.021 Uiso 1 1 calc R U . . .
H62 H 0.1713 1.0068 -0.0914 0.021 Uiso 1 1 calc R U . . .
N7 N 0.18689(12) 0.9812(5) 0.0332(3) 0.0170(11) Uani 1 1 d . . . . .
C8 C 0.17292(15) 1.1050(6) 0.0580(4) 0.0200(13) Uani 1 1 d . . . . .
H81 H 0.1802 1.1757 0.0203 0.024 Uiso 1 1 calc R U . . .
H82 H 0.1779 1.1261 0.1197 0.024 Uiso 1 1 calc R U . . .
C9 C 0.14112(15) 1.0978(6) 0.0482(4) 0.0190(13) Uani 1 1 d . . . . .
H91 H 0.1327 1.1810 0.0673 0.023 Uiso 1 1 calc R U . . .
H92 H 0.1360 1.0845 -0.0144 0.023 Uiso 1 1 calc R U . . .
N10 N 0.12922(12) 0.9904(5) 0.1013(3) 0.0157(10) Uani 1 1 d . . . . .
C11 C 0.09993(14) 0.9623(7) 0.0722(4) 0.0187(13) Uani 1 1 d . . . . .
H111 H 0.0897 1.0450 0.0616 0.022 Uiso 1 1 calc R U . . .
H112 H 0.0900 0.9149 0.1192 0.022 Uiso 1 1 calc R U . . .
C12 C 0.09934(13) 0.8811(6) -0.0119(4) 0.0163(12) Uani 1 1 d . . . . .
H121 H 0.0794 0.8665 -0.0305 0.020 Uiso 1 1 calc R U . . .
H122 H 0.1089 0.9295 -0.0593 0.020 Uiso 1 1 calc R U . . .
C20 C 0.09420(13) 0.6618(6) 0.0454(4) 0.0160(12) Uani 1 1 d . . . . .
H201 H 0.0785 0.6374 0.0049 0.019 Uiso 1 1 calc R U . . .
H202 H 0.0859 0.7043 0.0974 0.019 Uiso 1 1 calc R U . . .
P1 P 0.11354(3) 0.51589(16) 0.07981(10) 0.0132(3) Uani 1 1 d . . . . .
O11 O 0.14447(9) 0.5598(4) 0.0883(3) 0.0136(8) Uani 1 1 d . . . . .
O12 O 0.10813(10) 0.4044(5) 0.0192(3) 0.0198(10) Uani 1 1 d . . . . .
C21 C 0.10009(14) 0.4843(8) 0.1891(4) 0.0232(14) Uani 1 1 d . . . . .
H211 H 0.1108 0.4118 0.2162 0.028 Uiso 1 1 calc R U . . .
H212 H 0.1028 0.5621 0.2263 0.028 Uiso 1 1 calc R U . . .
N22 N 0.06992(12) 0.4512(6) 0.1844(4) 0.0233(12) Uani 1 1 d . . . . .
C30 C 0.06532(17) 0.3140(8) 0.1662(6) 0.0362(19) Uani 1 1 d . . . . .
H301 H 0.0667 0.2648 0.2219 0.043 Uiso 1 1 calc R U . . .
H302 H 0.0805 0.2824 0.1271 0.043 Uiso 1 1 calc R U . . .
C31 C 0.03719(16) 0.2877(7) 0.1240(6) 0.0294(17) Uani 1 1 d . . . . .
C32A C 0.0204(4) 0.3823(17) 0.0745(12) 0.036(3) Uani 0.492(7) 1 d . . P A 1
H32A H 0.0276 0.4680 0.0687 0.043 Uiso 0.492(7) 1 calc R U P A 1
C32B C 0.0373(3) 0.2958(16) 0.0361(12) 0.036(3) Uani 0.508(7) 1 d . . P A 2
H32B H 0.0541 0.3189 0.0061 0.043 Uiso 0.508(7) 1 calc R U P A 2
C33A C -0.0055(4) 0.352(2) 0.0356(14) 0.046(3) Uani 0.492(7) 1 d . . P A 1
H33A H -0.0170 0.4175 0.0092 0.056 Uiso 0.492(7) 1 calc R U P A 1
C34 C -0.0136(2) 0.2293(12) 0.0365(8) 0.059(3) Uani 1 1 d . . . . .
H34A H -0.0298 0.2065 0.0020 0.070 Uiso 0.492(7) 1 calc R U P A 1
H34B H -0.0310 0.2108 0.0065 0.070 Uiso 0.508(7) 1 calc R U P A 2
C35A C -0.0008(4) 0.134(2) 0.0827(15) 0.050(4) Uani 0.492(7) 1 d . . P A 1
H35A H -0.0089 0.0497 0.0864 0.059 Uiso 0.492(7) 1 calc R U P A 1
C36A C 0.0252(4) 0.1632(17) 0.1251(13) 0.038(3) Uani 0.492(7) 1 d . . P A 1
H36A H 0.0349 0.0960 0.1557 0.046 Uiso 0.492(7) 1 calc R U P A 1
C33B C 0.0124(4) 0.2698(19) -0.0105(14) 0.046(3) Uani 0.508(7) 1 d . . P A 2
H33B H 0.0120 0.2780 -0.0727 0.056 Uiso 0.508(7) 1 calc R U P A 2
C35B C -0.0111(4) 0.221(2) 0.1223(15) 0.050(4) Uani 0.508(7) 1 d . . P A 2
H35B H -0.0273 0.1955 0.1543 0.059 Uiso 0.508(7) 1 calc R U P A 2
C36B C 0.0139(4) 0.2462(16) 0.1703(13) 0.038(3) Uani 0.508(7) 1 d . . P A 2
H36B H 0.0148 0.2353 0.2322 0.046 Uiso 0.508(7) 1 calc R U P A 2
C40 C 0.05478(17) 0.4933(11) 0.2641(5) 0.042(2) Uani 1 1 d . . . . .
H401 H 0.0656 0.4673 0.3173 0.050 Uiso 0.383(3) 1 calc R U P B 3
H402 H 0.0358 0.4519 0.2660 0.050 Uiso 0.383(3) 1 calc R U P B 3
H403 H 0.0645 0.4566 0.3165 0.050 Uiso 0.196(3) 1 calc R U P B 4
H404 H 0.0352 0.4581 0.2621 0.050 Uiso 0.196(3) 1 calc R U P B 4
H405 H 0.0354 0.4562 0.2610 0.050 Uiso 0.420(3) 1 calc R U P B 5
H406 H 0.0645 0.4531 0.3153 0.050 Uiso 0.420(3) 1 calc R U P B 5
C41C C 0.0514(4) 0.6535(11) 0.2607(11) 0.024(2) Uiso 0.383(3) 1 d G . P B 3
C42C C 0.0362(3) 0.7194(14) 0.1958(9) 0.029(3) Uiso 0.383(3) 1 d G . P B 3
H42C H 0.0275 0.6726 0.1490 0.035 Uiso 0.383(3) 1 calc R U P B 3
C43C C 0.0338(3) 0.8536(14) 0.1994(9) 0.030(3) Uiso 0.383(3) 1 d G . P B 3
H43C H 0.0234 0.8987 0.1551 0.036 Uiso 0.383(3) 1 calc R U P B 3
C44C C 0.0466(4) 0.9220(11) 0.2680(12) 0.051(4) Uiso 0.383(3) 1 d G . P B 3
H44C H 0.0449 1.0138 0.2704 0.061 Uiso 0.383(3) 1 calc R U P B 3
C45C C 0.0617(4) 0.8561(16) 0.3328(10) 0.049(4) Uiso 0.383(3) 1 d G . P B 3
H45C H 0.0705 0.9029 0.3797 0.059 Uiso 0.383(3) 1 calc R U P B 3
C46C C 0.0642(3) 0.7218(16) 0.3292(10) 0.039(3) Uiso 0.383(3) 1 d G . P B 3
H46C H 0.0745 0.6768 0.3735 0.047 Uiso 0.383(3) 1 calc R U P B 3
C41D C 0.0533(7) 0.644(2) 0.273(2) 0.024(2) Uiso 0.196(3) 1 d G . P B 4
C42D C 0.0317(6) 0.668(2) 0.2128(19) 0.029(3) Uiso 0.196(3) 1 d G . P B 4
H42D H 0.0223 0.5978 0.1845 0.035 Uiso 0.196(3) 1 calc R U P B 4
C43D C 0.0238(6) 0.795(3) 0.1935(18) 0.030(3) Uiso 0.196(3) 1 d G . P B 4
H43D H 0.0090 0.8113 0.1520 0.036 Uiso 0.196(3) 1 calc R U P B 4
C44D C 0.0376(7) 0.898(2) 0.235(2) 0.051(4) Uiso 0.196(3) 1 d G . P B 4
H44D H 0.0322 0.9846 0.2217 0.061 Uiso 0.196(3) 1 calc R U P B 4
C45D C 0.0592(7) 0.874(3) 0.296(2) 0.049(4) Uiso 0.196(3) 1 d G . P B 4
H45D H 0.0686 0.9442 0.3239 0.059 Uiso 0.196(3) 1 calc R U P B 4
C46D C 0.0671(6) 0.747(3) 0.315(2) 0.039(3) Uiso 0.196(3) 1 d G . P B 4
H46D H 0.0819 0.7306 0.3564 0.047 Uiso 0.196(3) 1 calc R U P B 4
C41E C 0.0523(3) 0.6178(10) 0.2804(9) 0.024(2) Uiso 0.420(3) 1 d G . P B 5
C42E C 0.0394(3) 0.6941(12) 0.2160(7) 0.029(3) Uiso 0.420(3) 1 d G . P B 5
H42E H 0.0328 0.6557 0.1629 0.035 Uiso 0.420(3) 1 calc R U P B 5
C43E C 0.0362(3) 0.8267(12) 0.2294(8) 0.030(3) Uiso 0.420(3) 1 d G . P B 5
H43E H 0.0275 0.8788 0.1854 0.036 Uiso 0.420(3) 1 calc R U P B 5
C44E C 0.0459(3) 0.8829(10) 0.3071(9) 0.051(4) Uiso 0.420(3) 1 d G . P B 5
H44E H 0.0437 0.9736 0.3163 0.061 Uiso 0.420(3) 1 calc R U P B 5
C45E C 0.0588(3) 0.8066(14) 0.3715(8) 0.049(4) Uiso 0.420(3) 1 d G . P B 5
H45E H 0.0654 0.8451 0.4246 0.059 Uiso 0.420(3) 1 calc R U P B 5
C46E C 0.0619(3) 0.6740(13) 0.3581(8) 0.039(3) Uiso 0.420(3) 1 d G . P B 5
H46E H 0.0707 0.6219 0.4021 0.047 Uiso 0.420(3) 1 calc R U P B 5
C50 C 0.18399(13) 0.6135(6) -0.0738(4) 0.0145(12) Uani 1 1 d . . . . .
H501 H 0.1943 0.6045 -0.1299 0.017 Uiso 1 1 calc R U . . .
H502 H 0.1682 0.5504 -0.0743 0.017 Uiso 1 1 calc R U . . .
C51 C 0.20410(13) 0.5821(6) 0.0021(4) 0.0147(12) Uani 1 1 d . . . . .
O51 O 0.20383(9) 0.6574(5) 0.0683(3) 0.0173(9) Uani 1 1 d . . . . .
O52 O 0.21905(11) 0.4835(5) -0.0046(3) 0.0258(11) Uani 1 1 d . . . . .
C60 C 0.21549(15) 0.9787(8) 0.0742(4) 0.0248(15) Uani 1 1 d . . . . .
H601 H 0.2252 1.0622 0.0632 0.030 Uiso 1 1 calc R U . . .
H602 H 0.2269 0.9085 0.0478 0.030 Uiso 1 1 calc R U . . .
C61 C 0.21316(15) 0.9563(6) 0.1735(4) 0.0193(13) Uani 1 1 d . . . . .
O61 O 0.19179(10) 0.8943(5) 0.1999(3) 0.0205(10) Uani 1 1 d . . . . .
O62 O 0.23276(12) 0.9982(5) 0.2216(3) 0.0307(13) Uani 1 1 d . . . . .
C70 C 0.12873(16) 1.0258(6) 0.1953(4) 0.0195(13) Uani 1 1 d . . . . .
H701 H 0.1123 1.0833 0.2061 0.023 Uiso 1 1 calc R U . . .
H702 H 0.1462 1.0743 0.2106 0.023 Uiso 1 1 calc R U . . .
C71 C 0.12664(14) 0.9069(6) 0.2537(4) 0.0157(12) Uani 1 1 d . . . . .
O71 O 0.12806(10) 0.7981(4) 0.2154(3) 0.0161(9) Uani 1 1 d . . . . .
O72 O 0.12474(12) 0.9238(5) 0.3338(3) 0.0262(11) Uani 1 1 d . . . . .
N1A N 0.22582(12) 0.6650(6) 0.3409(4) 0.0201(11) Uani 1 1 d . . . . .
H11A H 0.2090 0.6742 0.3106 0.024 Uiso 1 1 d R U . . .
H12A H 0.2340 0.7361 0.3508 0.024 Uiso 1 1 d R U . . .
H13A H 0.2202 0.6237 0.3882 0.024 Uiso 1 1 d R U . . .
H14A H 0.2377 0.6148 0.3203 0.024 Uiso 1 1 d R U . . .
O1W O 0.17899(11) 0.3781(5) 0.1847(3) 0.0257(11) Uani 1 1 d . . . . .
H11W H 0.1733 0.4127 0.1423 0.031 Uiso 1 1 d R U . . .
H12W H 0.1964 0.3735 0.1708 0.031 Uiso 1 1 d R U . . .
O2W O 0.23868(11) 0.3784(5) 0.1442(3) 0.0259(11) Uani 1 1 d . . . . .
H21W H 0.2443 0.4325 0.1865 0.031 Uiso 1 1 d R U . . .
H22W H 0.2299 0.4263 0.0983 0.031 Uiso 1 1 d R U . . .
O3W O 0.14491(13) 0.6759(5) 0.3915(3) 0.0334(13) Uani 1 1 d . . . . .
H31W H 0.1346 0.6465 0.4289 0.040 Uiso 1 1 d R U . . .
H32W H 0.1347 0.7432 0.3771 0.040 Uiso 1 1 d R U . . .


_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 O11 2.341(4) . ?
Eu1 O71 2.341(4) . ?
Eu1 O51 2.397(5) . ?
Eu1 O61 2.398(4) . ?
Eu1 O1C 2.594(4) . ?
Eu1 N4 2.676(5) . ?
Eu1 N7 2.696(5) . ?
Eu1 N10 2.707(5) . ?
Eu1 N1 2.731(5) . ?
Eu1 C71 3.146(6) . ?
Eu1 C51 3.222(6) . ?
Eu1 C61 3.263(6) . ?
O1C H11C 0.8790 . ?
O1C H12C 0.8864 . ?
N1 C12 1.485(8) . ?
N1 C2 1.488(7) . ?
N1 C20 1.490(8) . ?
C2 C3 1.514(9) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.484(7) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.476(8) . ?
N4 C5 1.488(8) . ?
C5 C6 1.516(9) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.490(7) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.480(8) . ?
N7 C8 1.486(9) . ?
C8 C9 1.506(10) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.485(8) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C11 1.473(8) . ?
N10 C70 1.478(7) . ?
C11 C12 1.530(9) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.832(7) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.494(5) . ?
P1 O11 1.531(4) . ?
P1 C21 1.817(6) . ?
C21 N22 1.463(9) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C30 1.457(11) . ?
N22 C40 1.480(9) . ?
C30 C31 1.491(11) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C32B 1.341(19) . ?
C31 C36B 1.380(17) . ?
C31 C36A 1.404(19) . ?
C31 C32A 1.458(19) . ?
C32A C33A 1.39(2) . ?
C32A H32A 0.9500 . ?
C32B C33B 1.39(2) . ?
C32B H32B 0.9500 . ?
C33A C34 1.32(2) . ?
C33A H33A 0.9500 . ?
C34 C35B 1.31(2) . ?
C34 C35A 1.35(3) . ?
C34 C33B 1.49(2) . ?
C34 H34A 0.9500 . ?
C34 H34B 0.9500 . ?
C35A C36A 1.41(3) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C33B H33B 0.9500 . ?
C35B C36B 1.40(3) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C40 C41E 1.313(14) . ?
C40 C41D 1.56(3) . ?
C40 C41C 1.660(16) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C40 H403 0.9900 . ?
C40 H404 0.9900 . ?
C40 H405 0.9900 . ?
C40 H406 0.9900 . ?
C41C C42C 1.3900 . ?
C41C C46C 1.3900 . ?
C42C C43C 1.3900 . ?
C42C H42C 0.9500 . ?
C43C C44C 1.3900 . ?
C43C H43C 0.9500 . ?
C44C C45C 1.3900 . ?
C44C H44C 0.9500 . ?
C45C C46C 1.3900 . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
C41D C42D 1.3900 . ?
C41D C46D 1.3900 . ?
C42D C43D 1.3900 . ?
C42D H42D 0.9500 . ?
C43D C44D 1.3900 . ?
C43D H43D 0.9500 . ?
C44D C45D 1.3900 . ?
C44D H44D 0.9500 . ?
C45D C46D 1.3900 . ?
C45D H45D 0.9500 . ?
C46D H46D 0.9500 . ?
C41E C42E 1.3900 . ?
C41E C46E 1.3900 . ?
C42E C43E 1.3900 . ?
C42E H42E 0.9500 . ?
C43E C44E 1.3900 . ?
C43E H43E 0.9500 . ?
C44E C45E 1.3900 . ?
C44E H44E 0.9500 . ?
C45E C46E 1.3900 . ?
C45E H45E 0.9500 . ?
C46E H46E 0.9500 . ?
C50 C51 1.521(8) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.242(8) . ?
C51 O51 1.272(7) . ?
C60 C61 1.535(9) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.249(8) . ?
C61 O61 1.263(8) . ?
C70 C71 1.518(9) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.236(7) . ?
C71 O71 1.266(8) . ?
N1A H11A 0.9171 . ?
N1A H12A 0.8406 . ?
N1A H13A 0.8793 . ?
N1A H14A 0.8284 . ?
O1W H11W 0.7824 . ?
O1W H12W 0.8523 . ?
O2W H21W 0.8895 . ?
O2W H22W 0.9469 . ?
O3W H31W 0.8108 . ?
O3W H32W 0.8706 . ?

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
O11 Eu1 O71 87.12(15) . . ?
O11 Eu1 O51 78.32(15) . . ?
O71 Eu1 O51 141.94(15) . . ?
O11 Eu1 O61 138.65(15) . . ?
O71 Eu1 O61 84.11(16) . . ?
O51 Eu1 O61 84.16(16) . . ?
O11 Eu1 O1C 70.08(14) . . ?
O71 Eu1 O1C 69.12(14) . . ?
O51 Eu1 O1C 72.86(14) . . ?
O61 Eu1 O1C 69.03(14) . . ?
O11 Eu1 N4 83.02(15) . . ?
O71 Eu1 N4 149.26(15) . . ?
O51 Eu1 N4 63.74(15) . . ?
O61 Eu1 N4 121.69(15) . . ?
O1C Eu1 N4 132.62(14) . . ?
O11 Eu1 N7 149.37(15) . . ?
O71 Eu1 N7 120.35(16) . . ?
O51 Eu1 N7 85.74(17) . . ?
O61 Eu1 N7 63.68(15) . . ?
O1C Eu1 N7 129.58(15) . . ?
N4 Eu1 N7 66.45(16) . . ?
O11 Eu1 N10 126.00(16) . . ?
O71 Eu1 N10 62.47(15) . . ?
O51 Eu1 N10 151.17(16) . . ?
O61 Eu1 N10 84.49(17) . . ?
O1C Eu1 N10 126.57(14) . . ?
N4 Eu1 N10 100.81(15) . . ?
N7 Eu1 N10 65.49(17) . . ?
O11 Eu1 N1 66.59(15) . . ?
O71 Eu1 N1 82.70(15) . . ?
O51 Eu1 N1 121.45(15) . . ?
O61 Eu1 N1 150.64(16) . . ?
O1C Eu1 N1 128.85(14) . . ?
N4 Eu1 N1 66.65(15) . . ?
N7 Eu1 N1 101.37(15) . . ?
N10 Eu1 N1 66.15(15) . . ?
O11 Eu1 C71 107.87(16) . . ?
O71 Eu1 C71 20.75(16) . . ?
O51 Eu1 C71 145.43(15) . . ?
O61 Eu1 C71 68.74(17) . . ?
O1C Eu1 C71 77.48(15) . . ?
N4 Eu1 C71 149.44(16) . . ?
N7 Eu1 C71 100.13(17) . . ?
N10 Eu1 C71 49.43(15) . . ?
N1 Eu1 C71 91.02(15) . . ?
O11 Eu1 C51 66.14(15) . . ?
O71 Eu1 C51 147.71(15) . . ?
O51 Eu1 C51 20.05(15) . . ?
O61 Eu1 C51 103.71(16) . . ?
O1C Eu1 C51 84.31(14) . . ?
N4 Eu1 C51 48.76(15) . . ?
N7 Eu1 C51 90.53(17) . . ?
N10 Eu1 C51 148.41(15) . . ?
N1 Eu1 C51 101.43(15) . . ?
C71 Eu1 C51 161.75(16) . . ?
O11 Eu1 C61 145.83(15) . . ?
O71 Eu1 C61 101.65(16) . . ?
O51 Eu1 C61 74.58(17) . . ?
O61 Eu1 C61 18.92(16) . . ?
O1C Eu1 C61 82.22(15) . . ?
N4 Eu1 C61 102.81(16) . . ?
N7 Eu1 C61 47.81(15) . . ?
N10 Eu1 C61 86.46(17) . . ?
N1 Eu1 C61 146.77(16) . . ?
C71 Eu1 C61 84.27(17) . . ?
C51 Eu1 C61 92.20(17) . . ?
Eu1 O1C H11C 106.9 . . ?
Eu1 O1C H12C 116.5 . . ?
H11C O1C H12C 97.0 . . ?
C12 N1 C2 109.3(5) . . ?
C12 N1 C20 110.0(5) . . ?
C2 N1 C20 108.3(5) . . ?
C12 N1 Eu1 112.3(4) . . ?
C2 N1 Eu1 110.1(3) . . ?
C20 N1 Eu1 106.7(3) . . ?
N1 C2 C3 112.5(5) . . ?
N1 C2 H21 109.1 . . ?
C3 C2 H21 109.1 . . ?
N1 C2 H22 109.1 . . ?
C3 C2 H22 109.1 . . ?
H21 C2 H22 107.8 . . ?
N4 C3 C2 112.3(5) . . ?
N4 C3 H31 109.1 . . ?
C2 C3 H31 109.1 . . ?
N4 C3 H32 109.1 . . ?
C2 C3 H32 109.1 . . ?
H31 C3 H32 107.9 . . ?
C50 N4 C3 110.6(5) . . ?
C50 N4 C5 107.7(5) . . ?
C3 N4 C5 109.8(5) . . ?
C50 N4 Eu1 103.6(3) . . ?
C3 N4 Eu1 113.7(3) . . ?
C5 N4 Eu1 111.2(3) . . ?
N4 C5 C6 112.0(5) . . ?
N4 C5 H51 109.2 . . ?
C6 C5 H51 109.2 . . ?
N4 C5 H52 109.2 . . ?
C6 C5 H52 109.2 . . ?
H51 C5 H52 107.9 . . ?
N7 C6 C5 111.4(5) . . ?
N7 C6 H61 109.3 . . ?
C5 C6 H61 109.3 . . ?
N7 C6 H62 109.3 . . ?
C5 C6 H62 109.3 . . ?
H61 C6 H62 108.0 . . ?
C60 N7 C8 108.2(5) . . ?
C60 N7 C6 110.1(5) . . ?
C8 N7 C6 109.0(5) . . ?
C60 N7 Eu1 103.2(4) . . ?
C8 N7 Eu1 112.5(4) . . ?
C6 N7 Eu1 113.6(4) . . ?
N7 C8 C9 112.1(5) . . ?
N7 C8 H81 109.2 . . ?
C9 C8 H81 109.2 . . ?
N7 C8 H82 109.2 . . ?
C9 C8 H82 109.2 . . ?
H81 C8 H82 107.9 . . ?
N10 C9 C8 111.4(5) . . ?
N10 C9 H91 109.3 . . ?
C8 C9 H91 109.3 . . ?
N10 C9 H92 109.3 . . ?
C8 C9 H92 109.3 . . ?
H91 C9 H92 108.0 . . ?
C11 N10 C70 108.3(5) . . ?
C11 N10 C9 110.0(5) . . ?
C70 N10 C9 110.7(5) . . ?
C11 N10 Eu1 111.2(4) . . ?
C70 N10 Eu1 102.0(4) . . ?
C9 N10 Eu1 114.3(4) . . ?
N10 C11 C12 111.5(5) . . ?
N10 C11 H111 109.3 . . ?
C12 C11 H111 109.3 . . ?
N10 C11 H112 109.3 . . ?
C12 C11 H112 109.3 . . ?
H111 C11 H112 108.0 . . ?
N1 C12 C11 111.8(5) . . ?
N1 C12 H121 109.2 . . ?
C11 C12 H121 109.2 . . ?
N1 C12 H122 109.2 . . ?
C11 C12 H122 109.2 . . ?
H121 C12 H122 107.9 . . ?
N1 C20 P1 110.4(4) . . ?
N1 C20 H201 109.6 . . ?
P1 C20 H201 109.6 . . ?
N1 C20 H202 109.6 . . ?
P1 C20 H202 109.6 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 115.8(3) . . ?
O12 P1 C21 111.6(3) . . ?
O11 P1 C21 108.5(3) . . ?
O12 P1 C20 112.0(3) . . ?
O11 P1 C20 104.6(3) . . ?
C21 P1 C20 103.4(3) . . ?
O12 P1 Eu1 138.8(2) . . ?
O11 P1 Eu1 32.26(17) . . ?
C21 P1 Eu1 105.8(2) . . ?
C20 P1 Eu1 74.1(2) . . ?
P1 O11 Eu1 127.3(2) . . ?
N22 C21 P1 110.3(4) . . ?
N22 C21 H211 109.6 . . ?
P1 C21 H211 109.6 . . ?
N22 C21 H212 109.6 . . ?
P1 C21 H212 109.6 . . ?
H211 C21 H212 108.1 . . ?
C30 N22 C21 112.2(6) . . ?
C30 N22 C40 111.6(7) . . ?
C21 N22 C40 111.7(6) . . ?
N22 C30 C31 112.8(7) . . ?
N22 C30 H301 109.0 . . ?
C31 C30 H301 109.0 . . ?
N22 C30 H302 109.0 . . ?
C31 C30 H302 109.0 . . ?
H301 C30 H302 107.8 . . ?
C32B C31 C36B 122.7(13) . . ?
C36A C31 C32A 113.7(12) . . ?
C32B C31 C30 114.0(9) . . ?
C36B C31 C30 123.0(11) . . ?
C36A C31 C30 121.2(10) . . ?
C32A C31 C30 125.1(9) . . ?
C33A C32A C31 122.7(16) . . ?
C33A C32A H32A 118.7 . . ?
C31 C32A H32A 118.7 . . ?
C31 C32B C33B 119.1(16) . . ?
C31 C32B H32B 120.5 . . ?
C33B C32B H32B 120.5 . . ?
C34 C33A C32A 117.6(18) . . ?
C34 C33A H33A 121.2 . . ?
C32A C33A H33A 121.2 . . ?
C33A C34 C35A 125.1(15) . . ?
C35B C34 C33B 115.5(13) . . ?
C33A C34 H34A 117.4 . . ?
C35A C34 H34A 117.4 . . ?
C35B C34 H34B 122.3 . . ?
C33B C34 H34B 122.3 . . ?
C34 C35A C36A 117.7(17) . . ?
C34 C35A H35A 121.2 . . ?
C36A C35A H35A 121.2 . . ?
C31 C36A C35A 122.6(17) . . ?
C31 C36A H36A 118.7 . . ?
C35A C36A H36A 118.7 . . ?
C32B C33B C34 120.3(17) . . ?
C32B C33B H33B 119.9 . . ?
C34 C33B H33B 119.9 . . ?
C34 C35B C36B 124.9(16) . . ?
C34 C35B H35B 117.5 . . ?
C36B C35B H35B 117.5 . . ?
C31 C36B C35B 117.4(16) . . ?
C31 C36B H36B 121.3 . . ?
C35B C36B H36B 121.3 . . ?
C41E C40 N22 119.2(9) . . ?
N22 C40 C41D 112.9(15) . . ?
N22 C40 C41C 108.3(8) . . ?
N22 C40 H401 110.0 . . ?
C41C C40 H401 110.0 . . ?
N22 C40 H402 110.0 . . ?
C41C C40 H402 110.0 . . ?
H401 C40 H402 108.4 . . ?
N22 C40 H403 109.0 . . ?
C41D C40 H403 109.0 . . ?
N22 C40 H404 109.0 . . ?
C41D C40 H404 109.0 . . ?
H403 C40 H404 107.8 . . ?
C41E C40 H405 107.5 . . ?
N22 C40 H405 107.5 . . ?
C41E C40 H406 107.5 . . ?
N22 C40 H406 107.5 . . ?
H405 C40 H406 107.0 . . ?
C42C C41C C46C 120.0 . . ?
C42C C41C C40 123.8(10) . . ?
C46C C41C C40 116.1(10) . . ?
C43C C42C C41C 120.0 . . ?
C43C C42C H42C 120.0 . . ?
C41C C42C H42C 120.0 . . ?
C44C C43C C42C 120.0 . . ?
C44C C43C H43C 120.0 . . ?
C42C C43C H43C 120.0 . . ?
C43C C44C C45C 120.0 . . ?
C43C C44C H44C 120.0 . . ?
C45C C44C H44C 120.0 . . ?
C46C C45C C44C 120.0 . . ?
C46C C45C H45C 120.0 . . ?
C44C C45C H45C 120.0 . . ?
C45C C46C C41C 120.0 . . ?
C45C C46C H46C 120.0 . . ?
C41C C46C H46C 120.0 . . ?
C42D C41D C46D 120.0 . . ?
C42D C41D C40 98.5(19) . . ?
C46D C41D C40 141.3(19) . . ?
C41D C42D C43D 120.0 . . ?
C41D C42D H42D 120.0 . . ?
C43D C42D H42D 120.0 . . ?
C44D C43D C42D 120.0 . . ?
C44D C43D H43D 120.0 . . ?
C42D C43D H43D 120.0 . . ?
C45D C44D C43D 120.0 . . ?
C45D C44D H44D 120.0 . . ?
C43D C44D H44D 120.0 . . ?
C44D C45D C46D 120.0 . . ?
C44D C45D H45D 120.0 . . ?
C46D C45D H45D 120.0 . . ?
C45D C46D C41D 120.0 . . ?
C45D C46D H46D 120.0 . . ?
C41D C46D H46D 120.0 . . ?
C40 C41E C42E 117.3(10) . . ?
C40 C41E C46E 122.7(10) . . ?
C42E C41E C46E 120.0 . . ?
C43E C42E C41E 120.0 . . ?
C43E C42E H42E 120.0 . . ?
C41E C42E H42E 120.0 . . ?
C44E C43E C42E 120.0 . . ?
C44E C43E H43E 120.0 . . ?
C42E C43E H43E 120.0 . . ?
C43E C44E C45E 120.0 . . ?
C43E C44E H44E 120.0 . . ?
C45E C44E H44E 120.0 . . ?
C46E C45E C44E 120.0 . . ?
C46E C45E H45E 120.0 . . ?
C44E C45E H45E 120.0 . . ?
C45E C46E C41E 120.0 . . ?
C45E C46E H46E 120.0 . . ?
C41E C46E H46E 120.0 . . ?
N4 C50 C51 112.0(5) . . ?
N4 C50 H501 109.2 . . ?
C51 C50 H501 109.2 . . ?
N4 C50 H502 109.2 . . ?
C51 C50 H502 109.2 . . ?
H501 C50 H502 107.9 . . ?
O52 C51 O51 125.2(6) . . ?
O52 C51 C50 117.4(5) . . ?
O51 C51 C50 117.4(6) . . ?
O52 C51 Eu1 153.8(4) . . ?
O51 C51 Eu1 40.3(3) . . ?
C50 C51 Eu1 81.2(3) . . ?
C51 O51 Eu1 119.7(4) . . ?
N7 C60 C61 110.0(6) . . ?
N7 C60 H601 109.7 . . ?
C61 C60 H601 109.7 . . ?
N7 C60 H602 109.7 . . ?
C61 C60 H602 109.7 . . ?
H601 C60 H602 108.2 . . ?
O62 C61 O61 125.2(6) . . ?
O62 C61 C60 117.6(6) . . ?
O61 C61 C60 117.2(5) . . ?
O62 C61 Eu1 159.8(5) . . ?
O61 C61 Eu1 38.0(3) . . ?
C60 C61 Eu1 80.1(3) . . ?
C61 O61 Eu1 123.1(4) . . ?
N10 C70 C71 111.7(5) . . ?
N10 C70 H701 109.3 . . ?
C71 C70 H701 109.3 . . ?
N10 C70 H702 109.3 . . ?
C71 C70 H702 109.3 . . ?
H701 C70 H702 107.9 . . ?
O72 C71 O71 125.7(6) . . ?
O72 C71 C70 118.1(6) . . ?
O71 C71 C70 116.1(5) . . ?
O72 C71 Eu1 145.4(5) . . ?
O71 C71 Eu1 40.9(3) . . ?
C70 C71 Eu1 83.8(3) . . ?
C71 O71 Eu1 118.3(4) . . ?
H11A N1A H12A 113.1 . . ?
H11A N1A H13A 101.3 . . ?
H12A N1A H13A 114.7 . . ?
H11A N1A H14A 117.2 . . ?
H12A N1A H14A 107.5 . . ?
H13A N1A H14A 102.6 . . ?
H11W O1W H12W 98.1 . . ?
H21W O2W H22W 109.4 . . ?
H31W O3W H32W 98.2 . . ?

_refine_diff_density_max         2.529
_refine_diff_density_min         -4.418
_refine_diff_density_rms         0.160

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

data_er_do3apdbam
_database_code_depnum_ccdc_archive 'CCDC 1959628'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H40 Er N5 O8 P, Na, 4.25(H2 O)'
_chemical_formula_sum            'C30 H48.50 Er N5 Na O12.25 P'
_chemical_formula_weight         896.46

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.2212(10)
_cell_length_b                   15.3230(13)
_cell_length_c                   25.162(2)
_cell_angle_alpha                77.957(3)
_cell_angle_beta                 78.577(3)
_cell_angle_gamma                89.761(3)
_cell_volume                     3774.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9886
_cell_measurement_theta_min      2.4030
_cell_measurement_theta_max      25.9871

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_F_000             1822
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.179
_exptl_absorpt_coefficient_mu    2.341
_shelx_estimated_absorpt_T_min   0.448
_shelx_estimated_absorpt_T_max   0.679
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_T_max  0.68
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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 8.3333
_diffrn_reflns_number            41419
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.360
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14762
_reflns_number_gt                13327
_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.
 
 _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 Instrument Service v2014.11.0.1'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+149.0700P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14762
_refine_ls_number_parameters     942
_refine_ls_number_restraints     138
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0915
_refine_ls_wR_factor_ref         0.2082
_refine_ls_wR_factor_gt          0.2019
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.089
_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
Er1A Er 0.81808(8) 0.55869(5) 0.81244(3) 0.02867(19) Uani 1 1 d . . . . .
O1A O 0.956(2) 0.4062(16) 0.8479(10) 0.037(5) Uiso 0.5 1 d . . P . .
N1A N 0.8896(13) 0.6815(8) 0.7182(5) 0.023(3) Uani 1 1 d . . . . .
C2A C 0.9422(17) 0.7634(9) 0.7317(7) 0.026(3) Uani 1 1 d . . . . .
H2A H 1.0335 0.7529 0.7387 0.031 Uiso 1 1 calc R U . . .
H2B H 0.9483 0.8136 0.6993 0.031 Uiso 1 1 calc R U . . .
C3A C 0.8579(17) 0.7888(10) 0.7807(7) 0.030(4) Uani 1 1 d . . . . .
H3A H 0.7682 0.8034 0.7730 0.037 Uiso 1 1 calc R U . . .
H3B H 0.8980 0.8429 0.7878 0.037 Uiso 1 1 calc R U . . .
N4A N 0.8449(14) 0.7155(10) 0.8307(6) 0.029(3) Uani 1 1 d . . . . .
C5A C 0.7325(18) 0.7334(14) 0.8742(8) 0.038(4) Uani 1 1 d . . . . .
H5A H 0.7342 0.7978 0.8747 0.046 Uiso 1 1 calc R U . . .
H5B H 0.7440 0.6997 0.9110 0.046 Uiso 1 1 calc R U . . .
C6A C 0.600(2) 0.7070(13) 0.8640(8) 0.036(4) Uani 1 1 d . . . . .
H6A H 0.5277 0.7176 0.8943 0.043 Uiso 1 1 calc R U . . .
H6B H 0.5844 0.7443 0.8287 0.043 Uiso 1 1 calc R U . . .
N7A N 0.5952(17) 0.6131(10) 0.8610(6) 0.035(4) Uani 1 1 d . . . . .
C8A C 0.4801(19) 0.5970(12) 0.8341(8) 0.038(4) Uani 1 1 d . . . . .
H8A H 0.4498 0.5334 0.8462 0.046 Uiso 1 1 calc R U . . .
H8B H 0.4045 0.6336 0.8463 0.046 Uiso 1 1 calc R U . . .
C9A C 0.5213(16) 0.6207(10) 0.7716(7) 0.027(3) Uani 1 1 d . . . . .
H9A H 0.4472 0.6041 0.7552 0.032 Uiso 1 1 calc R U . . .
H9B H 0.5384 0.6861 0.7594 0.032 Uiso 1 1 calc R U . . .
N10A N 0.6411(13) 0.5753(9) 0.7513(6) 0.026(3) Uani 1 1 d . U . . .
C11A C 0.6986(17) 0.6214(11) 0.6928(7) 0.026(4) Uani 1 1 d . . . . .
H11A H 0.7551 0.5796 0.6740 0.031 Uiso 1 1 calc R U . . .
H11B H 0.6250 0.6380 0.6727 0.031 Uiso 1 1 calc R U . . .
C12A C 0.7797(18) 0.7024(10) 0.6899(7) 0.027(4) Uani 1 1 d . . . . .
H12A H 0.8150 0.7308 0.6506 0.032 Uiso 1 1 calc R U . . .
H12B H 0.7225 0.7455 0.7071 0.032 Uiso 1 1 calc R U . . .
C20A C 1.0031(15) 0.6440(11) 0.6825(7) 0.021(3) Uani 1 1 d . . . . .
H20A H 1.0487 0.6924 0.6519 0.026 Uiso 1 1 calc R U . . .
H20B H 0.9675 0.5984 0.6658 0.026 Uiso 1 1 calc R U . . .
P1A P 1.1224(4) 0.5938(3) 0.72390(18) 0.0227(8) Uani 1 1 d . . . . .
O11A O 1.0470(12) 0.5684(8) 0.7823(5) 0.029(2) Uani 1 1 d . U . . .
O12A O 1.2417(12) 0.6541(8) 0.7150(6) 0.035(3) Uani 1 1 d . . . . .
C21A C 1.1659(18) 0.4939(10) 0.6974(7) 0.027(4) Uani 1 1 d . . . . .
H21A H 1.2299 0.4602 0.7179 0.032 Uiso 1 1 calc R U . . .
H21B H 1.0847 0.4552 0.7035 0.032 Uiso 1 1 calc R U . . .
N22A N 1.2261(15) 0.5166(10) 0.6375(6) 0.029(3) Uani 1 1 d . . . . .
C30A C 1.3650(18) 0.5380(13) 0.6297(7) 0.033(4) Uani 1 1 d . . . . .
H30A H 1.4152 0.4824 0.6321 0.040 Uiso 1 1 calc R U . . .
H30B H 1.3807 0.5672 0.6596 0.040 Uiso 1 1 calc R U . . .
C31A C 1.4176(19) 0.6015(12) 0.5724(8) 0.036(4) Uiso 1 1 d . . . . .
C32A C 1.544(4) 0.603(2) 0.5556(15) 0.041(6) Uiso 0.522(15) 1 d . . P A 1
H32A H 1.5994 0.5667 0.5770 0.049 Uiso 0.522(15) 1 calc R U P A 1
C33A C 1.601(4) 0.662(3) 0.5019(18) 0.050(7) Uiso 0.522(15) 1 d . . P A 1
H33A H 1.6928 0.6614 0.4852 0.060 Uiso 0.522(15) 1 calc R U P A 1
C35A C 1.395(5) 0.698(3) 0.484(2) 0.059(9) Uiso 0.522(15) 1 d . . P A 1
H35A H 1.3456 0.7126 0.4556 0.071 Uiso 0.522(15) 1 calc R U P A 1
C36A C 1.326(4) 0.647(2) 0.5370(15) 0.038(6) Uiso 0.522(15) 1 d . . P A 1
H36A H 1.2319 0.6424 0.5481 0.046 Uiso 0.522(15) 1 calc R U P A 1
C32B C 1.469(4) 0.571(3) 0.5265(17) 0.041(6) Uiso 0.478(15) 1 d . . P A 2
H32B H 1.4846 0.5101 0.5267 0.049 Uiso 0.478(15) 1 calc R U P A 2
C33B C 1.502(5) 0.651(3) 0.4703(19) 0.050(7) Uiso 0.478(15) 1 d . . P A 2
H33B H 1.5170 0.6363 0.4347 0.060 Uiso 0.478(15) 1 calc R U P A 2
C35B C 1.452(5) 0.758(4) 0.529(2) 0.059(9) Uiso 0.478(15) 1 d . . P A 2
H35B H 1.4488 0.8194 0.5292 0.071 Uiso 0.478(15) 1 calc R U P A 2
C36B C 1.409(4) 0.694(3) 0.5751(17) 0.038(6) Uiso 0.478(15) 1 d . . P A 2
H36B H 1.3732 0.7100 0.6093 0.046 Uiso 0.478(15) 1 calc R U P A 2
C34A C 1.507(3) 0.723(2) 0.4747(13) 0.078(8) Uiso 1 1 d . . . . .
H34A H 1.5363 0.7791 0.4508 0.094 Uiso 0.522(15) 1 calc R U P A 1
H34B H 1.5472 0.7662 0.4427 0.094 Uiso 0.478(15) 1 calc R U P A 2
C40A C 1.197(2) 0.4477(13) 0.6086(8) 0.043(5) Uani 1 1 d . . . . .
H40A H 1.2522 0.4623 0.5706 0.052 Uiso 0.61(2) 1 calc R U P B 3
H40B H 1.2271 0.3904 0.6277 0.052 Uiso 0.61(2) 1 calc R U P B 3
H40C H 1.2522 0.4623 0.5706 0.052 Uiso 0.39(2) 1 calc R U P B 3
H40D H 1.2271 0.3904 0.6277 0.052 Uiso 0.39(2) 1 calc R U P B 3
C41A C 1.0629(19) 0.4336(15) 0.6037(11) 0.032(7) Uani 0.61(2) 1 d G . P B 3
C42A C 0.999(2) 0.5067(12) 0.5788(11) 0.039(9) Uani 0.61(2) 1 d G . P B 3
H42A H 1.0424 0.5642 0.5687 0.047 Uiso 0.61(2) 1 calc R U P B 3
C43A C 0.872(2) 0.4955(15) 0.5686(10) 0.049(9) Uani 0.61(2) 1 d G . P B 3
H43A H 0.8286 0.5454 0.5516 0.059 Uiso 0.61(2) 1 calc R U P B 3
C44A C 0.809(2) 0.4113(18) 0.5833(11) 0.077(14) Uani 0.61(2) 1 d G . P B 3
H44A H 0.7221 0.4037 0.5764 0.092 Uiso 0.61(2) 1 calc R U P B 3
C45A C 0.873(3) 0.3383(15) 0.6082(11) 0.079(11) Uani 0.61(2) 1 d G U P B 3
H45A H 0.8294 0.2807 0.6183 0.094 Uiso 0.61(2) 1 calc R U P B 3
C46A C 1.000(3) 0.3494(14) 0.6184(11) 0.058(8) Uani 0.61(2) 1 d G . P B 3
H46A H 1.0433 0.2995 0.6354 0.069 Uiso 0.61(2) 1 calc R U P B 3
C41B C 1.040(3) 0.463(3) 0.6004(19) 0.032(7) Uani 0.39(2) 1 d G . P B 4
C42B C 1.017(3) 0.538(3) 0.5618(18) 0.039(9) Uani 0.39(2) 1 d G . P B 4
H42B H 1.0874 0.5806 0.5439 0.047 Uiso 0.39(2) 1 calc R U P B 4
C43B C 0.891(4) 0.550(2) 0.5493(15) 0.049(9) Uani 0.39(2) 1 d G . P B 4
H43B H 0.8749 0.6006 0.5229 0.059 Uiso 0.39(2) 1 calc R U P B 4
C44B C 0.788(3) 0.487(3) 0.5754(18) 0.077(14) Uani 0.39(2) 1 d G . P B 4
H44B H 0.7016 0.4952 0.5669 0.092 Uiso 0.39(2) 1 calc R U P B 4
C45B C 0.811(4) 0.413(3) 0.6141(18) 0.079(11) Uani 0.39(2) 1 d G U P B 4
H45B H 0.7408 0.3697 0.6319 0.094 Uiso 0.39(2) 1 calc R U P B 4
C46B C 0.937(4) 0.401(2) 0.6265(16) 0.058(8) Uani 0.39(2) 1 d G . P B 4
H46B H 0.9533 0.3497 0.6530 0.069 Uiso 0.39(2) 1 calc R U P B 4
C50A C 0.971(2) 0.7122(14) 0.8531(9) 0.044(5) Uani 1 1 d . . . . .
H50A H 0.9757 0.7623 0.8721 0.053 Uiso 1 1 calc R U . . .
H50B H 1.0497 0.7175 0.8225 0.053 Uiso 1 1 calc R U . . .
C51A C 0.969(3) 0.621(2) 0.8951(9) 0.068(8) Uani 1 1 d . . . . .
O51A O 0.8913(17) 0.5581(10) 0.8931(5) 0.049(4) Uani 1 1 d . . . . .
O51B O 1.057(3) 0.6190(17) 0.9251(9) 0.117(10) Uani 1 1 d . . . . .
C60A C 0.569(2) 0.5534(15) 0.9173(8) 0.048(5) Uani 1 1 d . . . . .
H60A H 0.4757 0.5581 0.9362 0.057 Uiso 1 1 calc R U . . .
H60B H 0.6289 0.5717 0.9399 0.057 Uiso 1 1 calc R U . . .
C61A C 0.595(2) 0.4552(14) 0.9114(8) 0.041(5) Uani 1 1 d . . . . .
O61A O 0.6854(14) 0.4460(8) 0.8727(6) 0.042(3) Uani 1 1 d . . . . .
O61B O 0.5309(19) 0.3959(11) 0.9476(6) 0.066(5) Uani 1 1 d . . . . .
C70A C 0.6070(16) 0.4816(10) 0.7522(7) 0.026(3) Uani 1 1 d . . . . .
H70A H 0.5631 0.4793 0.7208 0.031 Uiso 1 1 calc R U . . .
H70B H 0.5429 0.4562 0.7870 0.031 Uiso 1 1 calc R U . . .
C71A C 0.7309(18) 0.4253(10) 0.7481(7) 0.027(4) Uani 1 1 d . . . . .
O71A O 0.8362(11) 0.4599(7) 0.7553(4) 0.024(2) Uani 1 1 d . . . . .
O71B O 0.7211(13) 0.3488(8) 0.7413(6) 0.037(3) Uani 1 1 d . . . . .
Er1X Er 0.59982(7) 0.93527(5) 1.19069(3) 0.02295(17) Uani 1 1 d . . . . .
N1X N 0.5879(14) 0.8143(8) 1.2803(5) 0.023(3) Uani 1 1 d . . . . .
C2X C 0.6515(16) 0.7318(10) 1.2667(7) 0.027(3) Uani 1 1 d . . . . .
H2X H 0.6251 0.6813 1.2988 0.032 Uiso 1 1 calc R U . . .
H2Y H 0.7499 0.7405 1.2595 0.032 Uiso 1 1 calc R U . . .
C3X C 0.611(2) 0.7094(11) 1.2168(8) 0.037(4) Uani 1 1 d . . . . .
H3X H 0.5136 0.6971 1.2247 0.044 Uiso 1 1 calc R U . . .
H3Y H 0.6559 0.6547 1.2087 0.044 Uiso 1 1 calc R U . . .
N4X N 0.6487(16) 0.7847(9) 1.1666(6) 0.032(3) Uani 1 1 d . . . . .
C5X C 0.575(2) 0.7710(13) 1.1235(9) 0.044(5) Uani 1 1 d . . . . .
H5X H 0.5760 0.7070 1.1217 0.053 Uiso 1 1 calc R U . . .
H5Y H 0.6219 0.8056 1.0869 0.053 Uiso 1 1 calc R U . . .
C6X C 0.433(2) 0.7989(12) 1.1344(10) 0.044(5) Uani 1 1 d . . . . .
H6X H 0.3831 0.7606 1.1693 0.053 Uiso 1 1 calc R U . . .
H6Y H 0.3896 0.7903 1.1038 0.053 Uiso 1 1 calc R U . . .
N7X N 0.4249(16) 0.8953(9) 1.1392(6) 0.032(3) Uani 1 1 d . . . . .
C8X C 0.2909(19) 0.9126(12) 1.1665(9) 0.042(5) Uani 1 1 d . . . . .
H8X H 0.2250 0.8827 1.1516 0.050 Uiso 1 1 calc R U . . .
H8Y H 0.2773 0.9776 1.1576 0.050 Uiso 1 1 calc R U . . .
C9X C 0.2646(17) 0.8804(11) 1.2295(8) 0.035(4) Uani 1 1 d . . . . .
H9X H 0.1730 0.8948 1.2461 0.041 Uiso 1 1 calc R U . . .
H9Y H 0.2727 0.8148 1.2392 0.041 Uiso 1 1 calc R U . . .
N10X N 0.3639(12) 0.9256(8) 1.2514(5) 0.019(3) Uani 1 1 d . . . . .
C11X C 0.3669(16) 0.8769(11) 1.3093(7) 0.026(3) Uani 1 1 d . . . . .
H11X H 0.2742 0.8609 1.3298 0.031 Uiso 1 1 calc R U . . .
H11Y H 0.4070 0.9170 1.3284 0.031 Uiso 1 1 calc R U . . .
C12X C 0.4471(16) 0.7916(11) 1.3106(8) 0.029(4) Uani 1 1 d . . . . .
H12X H 0.4462 0.7616 1.3495 0.035 Uiso 1 1 calc R U . . .
H12Y H 0.4053 0.7499 1.2930 0.035 Uiso 1 1 calc R U . . .
C20X C 0.6622(17) 0.8506(11) 1.3160(6) 0.026(4) Uani 1 1 d . . . . .
H20X H 0.6780 0.8019 1.3464 0.031 Uiso 1 1 calc R U . . .
H20Y H 0.6081 0.8954 1.3328 0.031 Uiso 1 1 calc R U . . .
P1X P 0.8214(4) 0.9025(3) 1.27656(19) 0.0258(9) Uani 1 1 d . . . . .
O11X O 0.7949(11) 0.9312(7) 1.2165(5) 0.025(2) Uani 1 1 d . U . . .
O12X O 0.9349(11) 0.8422(9) 1.2847(6) 0.040(3) Uani 1 1 d . . . . .
C21X C 0.8336(17) 1.0023(12) 1.3044(8) 0.031(4) Uani 1 1 d . . . . .
H21X H 0.9151 1.0383 1.2838 0.037 Uiso 1 1 calc R U . . .
H21Y H 0.7553 1.0392 1.2997 0.037 Uiso 1 1 calc R U . . .
N22X N 0.8386(15) 0.9771(10) 1.3622(7) 0.032(3) Uani 1 1 d . . . . .
C30X C 0.979(2) 0.9544(15) 1.3727(9) 0.047(5) Uani 1 1 d . . . . .
H30X H 1.0256 0.9250 1.3432 0.057 Uiso 1 1 calc R U . . .
H30Y H 1.0292 1.0106 1.3700 0.057 Uiso 1 1 calc R U . . .
C31X C 0.9789(18) 0.8965(13) 1.4263(8) 0.036(4) Uani 1 1 d . . . . .
C32X C 0.992(4) 0.916(3) 1.4732(18) 0.051(7) Uani 0.509(15) 1 d . . P C 5
H32X H 0.9985 0.9782 1.4732 0.061 Uiso 0.509(15) 1 calc R U P C 5
C33X C 0.998(4) 0.865(3) 1.5177(17) 0.047(7) Uani 0.509(15) 1 d . U P C 5
H33X H 1.0172 0.8879 1.5475 0.056 Uiso 0.509(15) 1 calc R U P C 5
C34X C 0.975(4) 0.764(3) 1.5252(16) 0.037(6) Uani 0.509(15) 1 d . U P C 5
H34X H 0.9617 0.7230 1.5599 0.044 Uiso 0.509(15) 1 calc R U P C 5
C35X C 0.977(4) 0.741(3) 1.4736(18) 0.049(7) Uani 0.509(15) 1 d . U P C 5
H35X H 0.9785 0.6801 1.4717 0.059 Uiso 0.509(15) 1 calc R U P C 5
C36X C 0.977(5) 0.808(3) 1.4237(18) 0.051(7) Uani 0.509(15) 1 d . U P C 5
H36X H 0.9767 0.7905 1.3897 0.062 Uiso 0.509(15) 1 calc R U P C 5
C32Y C 1.093(4) 0.891(3) 1.4523(19) 0.051(7) Uani 0.491(15) 1 d . . P C 6
H32Y H 1.1677 0.9298 1.4333 0.061 Uiso 0.491(15) 1 calc R U P C 6
C33Y C 1.104(5) 0.840(3) 1.4993(18) 0.047(7) Uani 0.491(15) 1 d . U P C 6
H33Y H 1.1870 0.8337 1.5110 0.056 Uiso 0.491(15) 1 calc R U P C 6
C34Y C 1.010(4) 0.802(3) 1.5251(16) 0.037(6) Uani 0.491(15) 1 d . U P C 6
H34Y H 1.0163 0.7782 1.5626 0.044 Uiso 0.491(15) 1 calc R U P C 6
C35Y C 0.868(5) 0.781(3) 1.5105(19) 0.049(7) Uani 0.491(15) 1 d . U P C 6
H35Y H 0.7986 0.7404 1.5323 0.059 Uiso 0.491(15) 1 calc R U P C 6
C36Y C 0.869(5) 0.840(3) 1.4562(19) 0.051(7) Uani 0.491(15) 1 d . U P C 6
H36Y H 0.7922 0.8390 1.4404 0.062 Uiso 0.491(15) 1 calc R U P C 6
C40X C 0.788(2) 1.0471(16) 1.3919(9) 0.046(5) Uani 1 1 d . . . . .
H40X H 0.8066 1.0303 1.4298 0.055 Uiso 1 1 calc R U . D 7
H40Y H 0.8404 1.1029 1.3731 0.055 Uiso 1 1 calc R U . D 7
C41X C 0.6468(17) 1.0668(15) 1.3972(9) 0.026(5) Uani 0.55(2) 1 d G U P E 7
C42X C 0.596(2) 1.1515(14) 1.3853(9) 0.052(9) Uani 0.55(2) 1 d G . P E 7
H42X H 0.6557 1.2020 1.3696 0.063 Uiso 0.55(2) 1 calc R U P E 7
C43X C 0.459(3) 1.1623(17) 1.3963(11) 0.081(16) Uani 0.55(2) 1 d G . P E 7
H43X H 0.4248 1.2202 1.3882 0.097 Uiso 0.55(2) 1 calc R U P E 7
C44X C 0.3726(18) 1.089(2) 1.4193(12) 0.055(9) Uani 0.55(2) 1 d G . P E 7
H44X H 0.2789 1.0959 1.4269 0.066 Uiso 0.55(2) 1 calc R U P E 7
C45X C 0.423(2) 1.0038(18) 1.4312(12) 0.065(12) Uani 0.55(2) 1 d G . P E 7
H45X H 0.3637 0.9534 1.4469 0.078 Uiso 0.55(2) 1 calc R U P E 7
C46X C 0.560(2) 0.9930(13) 1.4202(11) 0.033(6) Uani 0.55(2) 1 d G U P E 7
H46X H 0.5946 0.9351 1.4283 0.040 Uiso 0.55(2) 1 calc R U P E 7
C41Y C 0.629(2) 1.0312(19) 1.4035(11) 0.026(5) Uani 0.45(2) 1 d G U P E 8
C42Y C 0.565(3) 1.1024(19) 1.3766(11) 0.052(9) Uani 0.45(2) 1 d G . P E 8
H42Y H 0.6161 1.1515 1.3521 0.063 Uiso 0.45(2) 1 calc R U P E 8
C43Y C 0.426(3) 1.102(2) 1.3858(13) 0.081(16) Uani 0.45(2) 1 d G . P E 8
H43Y H 0.3826 1.1505 1.3674 0.097 Uiso 0.45(2) 1 calc R U P E 8
C44Y C 0.351(2) 1.030(3) 1.4217(15) 0.055(9) Uani 0.45(2) 1 d G . P E 8
H44Y H 0.2566 1.0296 1.4279 0.066 Uiso 0.45(2) 1 calc R U P E 8
C45Y C 0.415(3) 0.959(2) 1.4485(14) 0.065(12) Uani 0.45(2) 1 d G . P E 8
H45Y H 0.3640 0.9097 1.4731 0.078 Uiso 0.45(2) 1 calc R U P E 8
C46Y C 0.554(3) 0.9594(17) 1.4394(12) 0.033(6) Uani 0.45(2) 1 d G U P E 8
H46Y H 0.5974 0.9107 1.4577 0.040 Uiso 0.45(2) 1 calc R U P E 8
C50X C 0.7908(18) 0.7886(12) 1.1428(7) 0.033(4) Uani 1 1 d . . . . .
H50X H 0.8103 0.7418 1.1209 0.040 Uiso 1 1 calc R U . . .
H50Y H 0.8415 0.7762 1.1731 0.040 Uiso 1 1 calc R U . . .
C51X C 0.837(2) 0.8803(13) 1.1053(9) 0.046(5) Uani 1 1 d . . . . .
O51X O 0.7462(14) 0.9415(7) 1.1098(5) 0.037(3) Uani 1 1 d . . . . .
O52X O 0.940(2) 0.8881(13) 1.0742(9) 0.093(8) Uani 1 1 d . . . . .
C60X C 0.456(3) 0.9555(13) 1.0850(9) 0.050(6) Uani 1 1 d . . . . .
H60X H 0.3788 0.9549 1.0664 0.060 Uiso 1 1 calc R U . . .
H60Y H 0.5338 0.9341 1.0618 0.060 Uiso 1 1 calc R U . . .
C61X C 0.485(3) 1.0495(13) 1.0896(9) 0.053(6) Uani 1 1 d . . . . .
O61X O 0.5271(14) 1.0568(7) 1.1347(5) 0.035(3) Uani 1 1 d . . . . .
O62X O 0.421(3) 1.1041(17) 1.0574(12) 0.034(5) Uani 0.5 1 d . . P F 9
O62Y O 0.497(3) 1.1225(17) 1.0499(12) 0.034(5) Uani 0.5 1 d . . P F 10
C70X C 0.3327(16) 1.0194(11) 1.2526(8) 0.027(4) Uani 1 1 d . . . . .
H70X H 0.2620 1.0213 1.2855 0.033 Uiso 1 1 calc R U . . .
H70Y H 0.2982 1.0466 1.2191 0.033 Uiso 1 1 calc R U . . .
C71X C 0.4536(15) 1.0721(10) 1.2548(6) 0.019(3) Uani 1 1 d . . . . .
O71X O 0.5656(10) 1.0356(7) 1.2465(5) 0.023(2) Uani 1 1 d . . . . .
O72X O 0.4352(13) 1.1482(8) 1.2643(6) 0.034(3) Uani 1 1 d . . . . .
Na1A Na 1.181(2) 0.6994(16) 0.9532(9) 0.071(6) Uani 0.5 1 d . U P G 11
Na2A Na 1.200(4) 0.921(2) 0.9805(13) 0.122(10) Uani 0.5 1 d . U P G 11
Na1B Na 1.154(3) 0.7566(17) 0.9542(11) 0.096(7) Uani 0.5 1 d . U P G 12
Na2B Na 1.048(2) 1.0010(18) 1.0090(11) 0.091(7) Uani 0.5 1 d . U P H 12
O1W O 1.168(2) 0.5492(9) 1.0081(6) 0.085(7) Uani 1 1 d . . . . .
O2W O 1.2563(18) 0.8153(11) 0.8724(6) 0.070(5) Uani 1 1 d . . . . .
O3W O 1.355(3) 0.750(2) 0.9966(14) 0.049(6) Uani 0.5 1 d . U P . .
O4W O 1.159(4) 0.6666(15) 1.0720(12) 0.060(9) Uani 0.5 1 d . . P . .
O5W O 1.155(4) 1.088(2) 1.0491(16) 0.078(13) Uani 0.5 1 d . . P . .
O6W O 0.949(4) 0.736(3) 1.0091(18) 0.085(11) Uani 0.5 1 d . U P . .
O7W O 1.122(3) 0.802(2) 1.0431(14) 0.065(9) Uiso 0.5 1 d . . P . .
O8WA O 1.143(3) 0.432(2) 0.8569(13) 0.052(8) Uiso 0.5 1 d . . P I 13
O8WB O 1.209(2) 0.4582(13) 0.8499(9) 0.023(4) Uani 0.5 1 d . . P J 14
O9W O 0.9641(13) 0.2801(9) 0.7757(6) 0.044(3) Uani 1 1 d . . . . .
O10W O 1.2863(14) 0.7830(9) 0.7675(7) 0.052(4) Uani 1 1 d . . . . .
O11W O 1.254(3) 0.410(3) 0.9612(11) 0.062(10) Uani 0.5 1 d . . P . .


_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
Er1A O71A 2.278(10) . ?
Er1A O61A 2.287(13) . ?
Er1A O51A 2.295(13) . ?
Er1A O11A 2.308(12) . ?
Er1A N4A 2.565(14) . ?
Er1A N10A 2.576(14) . ?
Er1A N7A 2.585(16) . ?
Er1A N1A 2.676(13) . ?
Er1A O1A 2.80(2) . ?
N1A C12A 1.445(19) . ?
N1A C2A 1.496(19) . ?
N1A C20A 1.510(19) . ?
C2A C3A 1.48(2) . ?
C3A N4A 1.49(2) . ?
N4A C5A 1.49(2) . ?
N4A C50A 1.50(2) . ?
C5A C6A 1.50(3) . ?
C6A N7A 1.46(2) . ?
N7A C60A 1.49(2) . ?
N7A C8A 1.51(2) . ?
C8A C9A 1.51(2) . ?
C9A N10A 1.46(2) . ?
N10A C70A 1.47(2) . ?
N10A C11A 1.50(2) . ?
C11A C12A 1.48(2) . ?
C20A P1A 1.824(16) . ?
P1A O12A 1.485(13) . ?
P1A O11A 1.489(12) . ?
P1A C21A 1.814(16) . ?
C21A N22A 1.48(2) . ?
N22A C30A 1.42(2) . ?
N22A C40A 1.46(2) . ?
C30A C31A 1.56(3) . ?
C31A C32A 1.28(4) . ?
C31A C32B 1.34(4) . ?
C31A C36B 1.43(4) . ?
C31A C36A 1.49(4) . ?
C32A C33A 1.47(6) . ?
C33A C34A 1.51(5) . ?
C35A C34A 1.17(5) . ?
C35A C36A 1.43(6) . ?
C32B C33B 1.64(6) . ?
C33B C34A 1.14(5) . ?
C35B C36B 1.35(6) . ?
C35B C34A 1.56(6) . ?
C40A C41A 1.42(3) . ?
C40A C41B 1.66(4) . ?
C41A C42A 1.3900 . ?
C41A C46A 1.3900 . ?
C42A C43A 1.3900 . ?
C43A C44A 1.3900 . ?
C44A C45A 1.3900 . ?
C45A C46A 1.3900 . ?
C41B C42B 1.3900 . ?
C41B C46B 1.3900 . ?
C42B C43B 1.3900 . ?
C43B C44B 1.3900 . ?
C44B C45B 1.3900 . ?
C45B C46B 1.3900 . ?
C50A C51A 1.56(3) . ?
C51A O51A 1.27(3) . ?
C51A O51B 1.28(3) . ?
O51B Na1A 2.09(4) . ?
O51B Na1B 2.63(4) . ?
C60A C61A 1.56(3) . ?
C61A O61B 1.23(2) . ?
C61A O61A 1.23(2) . ?
C70A C71A 1.53(2) . ?
C71A O71B 1.225(19) . ?
C71A O71A 1.26(2) . ?
Er1X O11X 2.213(11) . ?
Er1X O51X 2.259(12) . ?
Er1X O71X 2.270(10) . ?
Er1X O61X 2.306(11) . ?
Er1X N4X 2.528(13) . ?
Er1X N7X 2.552(13) . ?
Er1X N10X 2.573(12) . ?
Er1X N1X 2.586(12) . ?
N1X C20X 1.474(19) . ?
N1X C2X 1.492(19) . ?
N1X C12X 1.49(2) . ?
C2X C3X 1.50(2) . ?
C3X N4X 1.51(2) . ?
N4X C50X 1.45(2) . ?
N4X C5X 1.49(2) . ?
C5X C6X 1.51(3) . ?
C6X N7X 1.51(2) . ?
N7X C60X 1.45(3) . ?
N7X C8X 1.46(3) . ?
C8X C9X 1.53(3) . ?
C9X N10X 1.483(19) . ?
N10X C70X 1.476(18) . ?
N10X C11X 1.50(2) . ?
C11X C12X 1.54(2) . ?
C20X P1X 1.819(18) . ?
P1X O12X 1.499(11) . ?
P1X O11X 1.561(12) . ?
P1X C21X 1.823(17) . ?
C21X N22X 1.44(2) . ?
N22X C40X 1.47(2) . ?
N22X C30X 1.53(2) . ?
C30X C31X 1.45(3) . ?
C31X C32X 1.31(5) . ?
C31X C36X 1.38(5) . ?
C31X C36Y 1.41(5) . ?
C31X C32Y 1.44(4) . ?
C32X C33X 1.24(6) . ?
C33X C34X 1.52(6) . ?
C34X C35X 1.41(6) . ?
C35X C36X 1.44(6) . ?
C32Y C33Y 1.30(6) . ?
C33Y C34Y 1.13(6) . ?
C34Y C35Y 1.62(6) . ?
C35Y C36Y 1.47(6) . ?
C40X C41X 1.46(3) . ?
C40X C41Y 1.61(3) . ?
C41X C42X 1.3900 . ?
C41X C46X 1.3900 . ?
C42X C43X 1.3900 . ?
C43X C44X 1.3900 . ?
C44X C45X 1.3900 . ?
C45X C46X 1.3900 . ?
C41Y C42Y 1.3900 . ?
C41Y C46Y 1.3900 . ?
C42Y C43Y 1.3900 . ?
C43Y C44Y 1.3900 . ?
C44Y C45Y 1.3900 . ?
C45Y C46Y 1.3900 . ?
C50X C51X 1.54(3) . ?
C51X O52X 1.18(3) . ?
C51X O51X 1.32(2) . ?
C51X Na2B 3.08(3) 2_777 ?
O51X Na2A 2.73(3) 2_777 ?
O52X Na2B 2.24(3) . ?
O52X Na2B 2.39(3) 2_777 ?
C60X C61X 1.51(3) . ?
C61X O62X 1.31(3) . ?
C61X O61X 1.31(2) . ?
C61X O62Y 1.32(3) . ?
C70X C71X 1.50(2) . ?
C71X O72X 1.244(18) . ?
C71X O71X 1.271(18) . ?
Na1A O2W 2.40(3) . ?
Na1A O1W 2.41(2) . ?
Na1A O3W 2.47(4) . ?
Na1A O6W 2.63(5) . ?
Na1A O4W 2.89(3) . ?
Na1A O7W 2.98(4) . ?
Na1A Na2A 3.61(4) . ?
Na2A O7W 2.18(5) . ?
Na2A O51X 2.73(3) 2_777 ?
Na1B O2W 2.13(3) . ?
Na1B O6W 2.25(5) . ?
Na1B O7W 2.44(4) . ?
Na1B O3W 2.49(4) . ?
Na1B O4W 3.01(4) . ?
Na2B Na2B 1.15(4) 2_777 ?
Na2B O5W 2.24(4) . ?
Na2B O52X 2.39(3) 2_777 ?
Na2B C51X 3.08(3) 2_777 ?

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
O71A Er1A O61A 82.6(4) . . ?
O71A Er1A O51A 132.7(4) . . ?
O61A Er1A O51A 78.9(6) . . ?
O71A Er1A O11A 81.4(4) . . ?
O61A Er1A O11A 129.7(4) . . ?
O51A Er1A O11A 78.0(5) . . ?
O71A Er1A N4A 152.3(4) . . ?
O61A Er1A N4A 124.1(5) . . ?
O51A Er1A N4A 66.8(5) . . ?
O11A Er1A N4A 85.4(4) . . ?
O71A Er1A N10A 66.2(4) . . ?
O61A Er1A N10A 88.0(5) . . ?
O51A Er1A N10A 154.1(5) . . ?
O11A Er1A N10A 126.7(4) . . ?
N4A Er1A N10A 104.1(4) . . ?
O71A Er1A N7A 124.9(4) . . ?
O61A Er1A N7A 66.9(5) . . ?
O51A Er1A N7A 86.3(5) . . ?
O11A Er1A N7A 152.9(5) . . ?
N4A Er1A N7A 68.1(5) . . ?
N10A Er1A N7A 67.9(4) . . ?
O71A Er1A N1A 84.5(4) . . ?
O61A Er1A N1A 154.9(5) . . ?
O51A Er1A N1A 125.1(5) . . ?
O11A Er1A N1A 68.8(4) . . ?
N4A Er1A N1A 68.0(4) . . ?
N10A Er1A N1A 67.1(4) . . ?
N7A Er1A N1A 104.2(4) . . ?
O71A Er1A O1A 66.4(5) . . ?
O61A Er1A O1A 66.1(6) . . ?
O51A Er1A O1A 66.2(6) . . ?
O11A Er1A O1A 63.8(6) . . ?
N4A Er1A O1A 127.8(6) . . ?
N10A Er1A O1A 128.1(6) . . ?
N7A Er1A O1A 128.9(6) . . ?
N1A Er1A O1A 126.9(6) . . ?
C12A N1A C2A 110.7(12) . . ?
C12A N1A C20A 111.0(12) . . ?
C2A N1A C20A 107.8(12) . . ?
C12A N1A Er1A 112.0(10) . . ?
C2A N1A Er1A 108.4(9) . . ?
C20A N1A Er1A 106.8(9) . . ?
C3A C2A N1A 113.0(14) . . ?
C2A C3A N4A 111.3(12) . . ?
C3A N4A C5A 109.2(13) . . ?
C3A N4A C50A 109.7(15) . . ?
C5A N4A C50A 108.4(13) . . ?
C3A N4A Er1A 114.5(9) . . ?
C5A N4A Er1A 110.9(11) . . ?
C50A N4A Er1A 104.0(10) . . ?
N4A C5A C6A 111.6(14) . . ?
N7A C6A C5A 110.8(16) . . ?
C6A N7A C60A 111.7(15) . . ?
C6A N7A C8A 108.5(14) . . ?
C60A N7A C8A 106.8(16) . . ?
C6A N7A Er1A 114.0(12) . . ?
C60A N7A Er1A 103.3(11) . . ?
C8A N7A Er1A 112.4(11) . . ?
C9A C8A N7A 110.9(16) . . ?
N10A C9A C8A 112.1(13) . . ?
C9A N10A C70A 110.2(12) . . ?
C9A N10A C11A 108.7(12) . . ?
C70A N10A C11A 108.7(13) . . ?
C9A N10A Er1A 115.1(10) . . ?
C70A N10A Er1A 102.2(9) . . ?
C11A N10A Er1A 111.6(9) . . ?
C12A C11A N10A 112.2(13) . . ?
N1A C12A C11A 111.3(12) . . ?
N1A C20A P1A 110.3(10) . . ?
O12A P1A O11A 115.2(7) . . ?
O12A P1A C21A 111.1(8) . . ?
O11A P1A C21A 109.6(7) . . ?
O12A P1A C20A 111.2(7) . . ?
O11A P1A C20A 106.4(7) . . ?
C21A P1A C20A 102.6(7) . . ?
P1A O11A Er1A 127.2(6) . . ?
N22A C21A P1A 111.0(11) . . ?
C30A N22A C40A 113.6(15) . . ?
C30A N22A C21A 110.1(14) . . ?
C40A N22A C21A 112.3(15) . . ?
N22A C30A C31A 111.4(14) . . ?
C32B C31A C36B 125(3) . . ?
C32A C31A C36A 123(3) . . ?
C32A C31A C30A 114(2) . . ?
C32B C31A C30A 123(2) . . ?
C36B C31A C30A 113(2) . . ?
C36A C31A C30A 122(2) . . ?
C31A C32A C33A 117(3) . . ?
C32A C33A C34A 117(3) . . ?
C34A C35A C36A 124(5) . . ?
C35A C36A C31A 114(3) . . ?
C31A C32B C33B 113(3) . . ?
C34A C33B C32B 119(4) . . ?
C36B C35B C34A 116(4) . . ?
C35B C36B C31A 120(4) . . ?
C35A C34A C33A 116(4) . . ?
C33B C34A C35B 125(4) . . ?
C41A C40A N22A 118.7(19) . . ?
N22A C40A C41B 105(2) . . ?
C42A C41A C46A 120.0 . . ?
C42A C41A C40A 117.4(17) . . ?
C46A C41A C40A 122.4(17) . . ?
C43A C42A C41A 120.0 . . ?
C44A C43A C42A 120.0 . . ?
C43A C44A C45A 120.0 . . ?
C46A C45A C44A 120.0 . . ?
C45A C46A C41A 120.0 . . ?
C42B C41B C46B 120.0 . . ?
C42B C41B C40A 117(3) . . ?
C46B C41B C40A 122(3) . . ?
C43B C42B C41B 120.0 . . ?
C44B C43B C42B 120.0 . . ?
C43B C44B C45B 120.0 . . ?
C46B C45B C44B 120.0 . . ?
C45B C46B C41B 120.0 . . ?
N4A C50A C51A 108(2) . . ?
O51A C51A O51B 128(3) . . ?
O51A C51A C50A 118.4(18) . . ?
O51B C51A C50A 113(3) . . ?
C51A O51A Er1A 119.4(14) . . ?
C51A O51B Na1A 143(2) . . ?
C51A O51B Na1B 126(2) . . ?
N7A C60A C61A 109.1(15) . . ?
O61B C61A O61A 127(2) . . ?
O61B C61A C60A 117.1(18) . . ?
O61A C61A C60A 115.5(18) . . ?
C61A O61A Er1A 125.7(13) . . ?
N10A C70A C71A 111.6(13) . . ?
O71B C71A O71A 124.1(16) . . ?
O71B C71A C70A 119.2(16) . . ?
O71A C71A C70A 116.6(13) . . ?
C71A O71A Er1A 118.9(10) . . ?
O11X Er1X O51X 77.4(5) . . ?
O11X Er1X O71X 80.5(4) . . ?
O51X Er1X O71X 129.9(4) . . ?
O11X Er1X O61X 124.4(5) . . ?
O51X Er1X O61X 78.8(4) . . ?
O71X Er1X O61X 77.6(4) . . ?
O11X Er1X N4X 87.5(4) . . ?
O51X Er1X N4X 65.9(5) . . ?
O71X Er1X N4X 156.2(4) . . ?
O61X Er1X N4X 125.8(4) . . ?
O11X Er1X N7X 156.6(4) . . ?
O51X Er1X N7X 85.3(5) . . ?
O71X Er1X N7X 122.9(4) . . ?
O61X Er1X N7X 66.2(5) . . ?
N4X Er1X N7X 70.9(4) . . ?
O11X Er1X N10X 128.6(4) . . ?
O51X Er1X N10X 153.8(5) . . ?
O71X Er1X N10X 65.6(4) . . ?
O61X Er1X N10X 85.9(4) . . ?
N4X Er1X N10X 108.3(5) . . ?
N7X Er1X N10X 69.0(5) . . ?
O11X Er1X N1X 70.4(4) . . ?
O51X Er1X N1X 125.7(4) . . ?
O71X Er1X N1X 86.6(4) . . ?
O61X Er1X N1X 155.2(5) . . ?
N4X Er1X N1X 70.0(4) . . ?
N7X Er1X N1X 108.7(5) . . ?
N10X Er1X N1X 70.1(4) . . ?
C20X N1X C2X 109.5(12) . . ?
C20X N1X C12X 109.3(13) . . ?
C2X N1X C12X 109.1(12) . . ?
C20X N1X Er1X 107.2(9) . . ?
C2X N1X Er1X 110.0(9) . . ?
C12X N1X Er1X 111.7(9) . . ?
N1X C2X C3X 111.6(13) . . ?
C2X C3X N4X 111.4(14) . . ?
C50X N4X C5X 107.9(15) . . ?
C50X N4X C3X 111.9(13) . . ?
C5X N4X C3X 109.1(15) . . ?
C50X N4X Er1X 105.6(10) . . ?
C5X N4X Er1X 110.3(10) . . ?
C3X N4X Er1X 111.8(10) . . ?
N4X C5X C6X 112.9(16) . . ?
C5X C6X N7X 111.4(16) . . ?
C60X N7X C8X 108.1(15) . . ?
C60X N7X C6X 111.6(15) . . ?
C8X N7X C6X 110.0(16) . . ?
C60X N7X Er1X 105.0(12) . . ?
C8X N7X Er1X 111.2(10) . . ?
C6X N7X Er1X 110.8(9) . . ?
N7X C8X C9X 113.3(13) . . ?
N10X C9X C8X 108.4(15) . . ?
C70X N10X C9X 112.4(12) . . ?
C70X N10X C11X 108.3(13) . . ?
C9X N10X C11X 109.3(13) . . ?
C70X N10X Er1X 104.2(9) . . ?
C9X N10X Er1X 112.7(10) . . ?
C11X N10X Er1X 109.8(8) . . ?
N10X C11X C12X 112.4(13) . . ?
N1X C12X C11X 110.1(14) . . ?
N1X C20X P1X 111.2(11) . . ?
O12X P1X O11X 117.4(7) . . ?
O12X P1X C20X 111.8(8) . . ?
O11X P1X C20X 102.9(7) . . ?
O12X P1X C21X 111.9(8) . . ?
O11X P1X C21X 108.7(7) . . ?
C20X P1X C21X 102.8(8) . . ?
P1X O11X Er1X 127.4(6) . . ?
N22X C21X P1X 109.8(12) . . ?
C21X N22X C40X 111.5(15) . . ?
C21X N22X C30X 113.5(15) . . ?
C40X N22X C30X 108.7(15) . . ?
C31X C30X N22X 113.9(18) . . ?
C32X C31X C36X 118(3) . . ?
C36Y C31X C32Y 115(3) . . ?
C32X C31X C30X 130(3) . . ?
C36X C31X C30X 112(2) . . ?
C36Y C31X C30X 123(2) . . ?
C32Y C31X C30X 122(3) . . ?
C33X C32X C31X 128(4) . . ?
C32X C33X C34X 121(4) . . ?
C35X C34X C33X 111(4) . . ?
C34X C35X C36X 122(4) . . ?
C31X C36X C35X 119(4) . . ?
C33Y C32Y C31X 127(4) . . ?
C34Y C33Y C32Y 117(5) . . ?
C33Y C34Y C35Y 132(4) . . ?
C36Y C35Y C34Y 105(4) . . ?
C31X C36Y C35Y 123(4) . . ?
C41X C40X N22X 118.3(17) . . ?
N22X C40X C41Y 103.5(18) . . ?
C42X C41X C46X 120.0 . . ?
C42X C41X C40X 125.5(18) . . ?
C46X C41X C40X 114.3(18) . . ?
C43X C42X C41X 120.0 . . ?
C42X C43X C44X 120.0 . . ?
C45X C44X C43X 120.0 . . ?
C44X C45X C46X 120.00(5) . . ?
C45X C46X C41X 120.0 . . ?
C42Y C41Y C46Y 120.0 . . ?
C42Y C41Y C40X 113.0(19) . . ?
C46Y C41Y C40X 126.8(19) . . ?
C43Y C42Y C41Y 120.0 . . ?
C44Y C43Y C42Y 120.0 . . ?
C43Y C44Y C45Y 120.0 . . ?
C44Y C45Y C46Y 120.0 . . ?
C45Y C46Y C41Y 120.0 . . ?
N4X C50X C51X 111.7(13) . . ?
O52X C51X O51X 127(2) . . ?
O52X C51X C50X 119.4(17) . . ?
O51X C51X C50X 113.3(17) . . ?
O52X C51X Na2B 44.6(14) . 2_777 ?
O51X C51X Na2B 85.5(12) . 2_777 ?
C50X C51X Na2B 151.2(14) . 2_777 ?
C51X O51X Er1X 120.4(12) . . ?
C51X O51X Na2A 110.2(14) . 2_777 ?
Er1X O51X Na2A 128.3(8) . 2_777 ?
C51X O52X Na2B 133.9(17) . . ?
C51X O52X Na2B 115.2(18) . 2_777 ?
Na2B O52X Na2B 28.7(11) . 2_777 ?
N7X C60X C61X 111.6(15) . . ?
O62X C61X O61X 132(2) . . ?
O61X C61X O62Y 116(2) . . ?
O62X C61X C60X 108(2) . . ?
O61X C61X C60X 115.3(15) . . ?
O62Y C61X C60X 127(2) . . ?
C61X O61X Er1X 121.5(10) . . ?
N10X C70X C71X 111.2(12) . . ?
O72X C71X O71X 126.0(14) . . ?
O72X C71X C70X 116.7(13) . . ?
O71X C71X C70X 117.3(13) . . ?
C71X O71X Er1X 120.1(9) . . ?
O51B Na1A O2W 102.4(11) . . ?
O51B Na1A O1W 70.3(10) . . ?
O2W Na1A O1W 155.0(12) . . ?
O51B Na1A O3W 162.5(14) . . ?
O2W Na1A O3W 89.2(12) . . ?
O1W Na1A O3W 93.6(11) . . ?
O51B Na1A O6W 81.0(14) . . ?
O2W Na1A O6W 110.9(13) . . ?
O1W Na1A O6W 91.9(13) . . ?
O3W Na1A O6W 107.2(14) . . ?
O51B Na1A O4W 115.8(12) . . ?
O2W Na1A O4W 139.5(13) . . ?
O1W Na1A O4W 59.0(7) . . ?
O3W Na1A O4W 57.4(11) . . ?
O6W Na1A O4W 65.1(12) . . ?
O51B Na1A O7W 130.9(14) . . ?
O2W Na1A O7W 102.2(10) . . ?
O1W Na1A O7W 100.1(9) . . ?
O3W Na1A O7W 56.9(11) . . ?
O6W Na1A O7W 50.6(12) . . ?
O4W Na1A O7W 42.1(8) . . ?
O51B Na1A Na2A 140.5(12) . . ?
O2W Na1A Na2A 65.2(8) . . ?
O1W Na1A Na2A 135.4(11) . . ?
O3W Na1A Na2A 56.4(11) . . ?
O6W Na1A Na2A 70.5(12) . . ?
O4W Na1A Na2A 76.5(9) . . ?
O7W Na1A Na2A 37.1(9) . . ?
O7W Na2A O51X 167(2) . 2_777 ?
O7W Na2A Na1A 55.5(12) . . ?
O51X Na2A Na1A 116.5(11) 2_777 . ?
O2W Na1B O6W 142.4(19) . . ?
O2W Na1B O7W 133.9(15) . . ?
O6W Na1B O7W 61.9(15) . . ?
O2W Na1B O3W 95.3(14) . . ?
O6W Na1B O3W 119.8(16) . . ?
O7W Na1B O3W 64.7(13) . . ?
O2W Na1B O51B 94.3(11) . . ?
O6W Na1B O51B 78.1(15) . . ?
O7W Na1B O51B 131.7(15) . . ?
O3W Na1B O51B 123.3(15) . . ?
O2W Na1B O4W 150.2(16) . . ?
O6W Na1B O4W 67.2(14) . . ?
O7W Na1B O4W 44.0(10) . . ?
O3W Na1B O4W 55.5(12) . . ?
O51B Na1B O4W 97.2(11) . . ?
Na2B Na2B O5W 141(3) 2_777 . ?
Na2B Na2B O52X 83(3) 2_777 . ?
O5W Na2B O52X 109.1(16) . . ?
Na2B Na2B O52X 68(2) 2_777 2_777 ?
O5W Na2B O52X 93.9(14) . 2_777 ?
O52X Na2B O52X 151.3(11) . 2_777 ?
Na2B Na2B C51X 84(3) 2_777 2_777 ?
O5W Na2B C51X 89.8(14) . 2_777 ?
O52X Na2B C51X 161.0(14) . 2_777 ?
O52X Na2B C51X 20.2(6) 2_777 2_777 ?
Na2A O7W Na1A 87.4(14) . . ?

_refine_diff_density_max         7.077
_refine_diff_density_min         -5.420
_refine_diff_density_rms         0.250

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

data_prdbamh
_database_code_depnum_ccdc_archive 'CCDC 1959634'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C30 H41 N5 O8 P Pr, 0.5(H4 N), 6.5(H2 O), Cl0.5'
_chemical_formula_sum            'C30 H56 Cl0.50 N5.50 O14.50 P Pr'
_chemical_formula_weight         915.40

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'
Cl Cl 0.1484 0.1585 '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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   11.7803(8)
_cell_length_b                   12.4274(9)
_cell_length_c                   14.5862(11)
_cell_angle_alpha                68.147(2)
_cell_angle_beta                 79.566(2)
_cell_angle_gamma                78.962(2)
_cell_volume                     1931.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9588
_cell_measurement_theta_min      2.6806
_cell_measurement_theta_max      27.5276

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_F_000             946
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.123
_exptl_absorpt_coefficient_mu    1.409
_shelx_estimated_absorpt_T_min   0.656
_shelx_estimated_absorpt_T_max   0.846
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            40904
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.286
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8886
_reflns_number_gt                8518
_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.
 
 _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 Instrument Service v6.2.9'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0383P)²+5.0724P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8886
_refine_ls_number_parameters     491
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0785
_refine_ls_wR_factor_gt          0.0776
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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
Pr1 Pr 0.42305(2) 0.54615(2) 0.68227(2) 0.00828(5) Uani 1 1 d . . . . .
N1 N 0.20553(18) 0.68083(18) 0.66465(15) 0.0098(4) Uani 1 1 d . . . . .
C2 C 0.1838(2) 0.7514(2) 0.73056(18) 0.0124(5) Uani 1 1 d . . . . .
H21 H 0.1016 0.7885 0.7316 0.015 Uiso 1 1 calc R U . . .
H22 H 0.2338 0.8146 0.7030 0.015 Uiso 1 1 calc R U . . .
C3 C 0.2084(2) 0.6785(2) 0.83630(18) 0.0131(5) Uani 1 1 d . . . . .
H31 H 0.1941 0.7298 0.8765 0.016 Uiso 1 1 calc R U . . .
H32 H 0.1540 0.6193 0.8659 0.016 Uiso 1 1 calc R U . . .
N4 N 0.32974(18) 0.61833(18) 0.84040(15) 0.0112(4) Uani 1 1 d . . . . .
C5 C 0.3367(2) 0.5195(2) 0.93683(18) 0.0134(5) Uani 1 1 d . . . . .
H51 H 0.2893 0.5445 0.9906 0.016 Uiso 1 1 calc R U . . .
H52 H 0.4185 0.4983 0.9516 0.016 Uiso 1 1 calc R U . . .
C6 C 0.2934(2) 0.4130(2) 0.93512(18) 0.0137(5) Uani 1 1 d . . . . .
H61 H 0.2968 0.3502 1.0011 0.016 Uiso 1 1 calc R U . . .
H62 H 0.2111 0.4336 0.9216 0.016 Uiso 1 1 calc R U . . .
N7 N 0.36445(19) 0.36983(18) 0.85795(15) 0.0117(4) Uani 1 1 d . . . . .
C8 C 0.3045(2) 0.2848(2) 0.84122(19) 0.0141(5) Uani 1 1 d . . . . .
H81 H 0.2730 0.2312 0.9063 0.017 Uiso 1 1 calc R U . . .
H82 H 0.3620 0.2372 0.8082 0.017 Uiso 1 1 calc R U . . .
C9 C 0.2064(2) 0.3439(2) 0.77803(19) 0.0141(5) Uani 1 1 d . . . . .
H91 H 0.1723 0.2838 0.7666 0.017 Uiso 1 1 calc R U . . .
H92 H 0.1447 0.3843 0.8144 0.017 Uiso 1 1 calc R U . . .
N10 N 0.24602(18) 0.43051(18) 0.68023(15) 0.0111(4) Uani 1 1 d . . . . .
C11 C 0.1421(2) 0.5141(2) 0.64076(19) 0.0130(5) Uani 1 1 d . . . . .
H111 H 0.0751 0.4706 0.6547 0.016 Uiso 1 1 calc R U . . .
H112 H 0.1588 0.5513 0.5677 0.016 Uiso 1 1 calc R U . . .
C12 C 0.1104(2) 0.6081(2) 0.68733(19) 0.0128(5) Uani 1 1 d . . . . .
H121 H 0.0389 0.6591 0.6622 0.015 Uiso 1 1 calc R U . . .
H122 H 0.0935 0.5708 0.7604 0.015 Uiso 1 1 calc R U . . .
C20 C 0.2052(2) 0.7632(2) 0.56104(18) 0.0116(5) Uani 1 1 d . . . . .
H201 H 0.1347 0.8220 0.5559 0.014 Uiso 1 1 calc R U . . .
H202 H 0.2031 0.7200 0.5165 0.014 Uiso 1 1 calc R U . . .
P1 P 0.33534(5) 0.83726(5) 0.52166(5) 0.00963(12) Uani 1 1 d . . . . .
O11 O 0.42500(15) 0.75678(15) 0.58840(13) 0.0116(3) Uani 1 1 d . . . . .
O12 O 0.30683(16) 0.96207(15) 0.51641(14) 0.0142(4) Uani 1 1 d . . . . .
C21 C 0.3908(2) 0.8300(2) 0.39829(18) 0.0123(5) Uani 1 1 d . . . . .
H211 H 0.4758 0.8329 0.3877 0.015 Uiso 1 1 calc R U . . .
H212 H 0.3799 0.7527 0.3990 0.015 Uiso 1 1 calc R U . . .
N22 N 0.33909(19) 0.92199(19) 0.30999(16) 0.0132(4) Uani 1 1 d . . . . .
H221 H 0.3579 0.8899 0.2546 0.016 Uiso 1 1 calc R U . . .
C30 C 0.3933(2) 1.0338(2) 0.2741(2) 0.0166(5) Uani 1 1 d . . . . .
H301 H 0.3489 1.0947 0.2224 0.020 Uiso 1 1 calc R U . . .
H302 H 0.3878 1.0616 0.3303 0.020 Uiso 1 1 calc R U . . .
C31 C 0.5190(2) 1.0170(2) 0.23166(19) 0.0148(5) Uani 1 1 d . . . . .
C32 C 0.5475(2) 1.0303(2) 0.1313(2) 0.0176(5) Uani 1 1 d . . . . .
H321 H 0.4871 1.0456 0.0910 0.021 Uiso 1 1 calc R U . . .
C33 C 0.6630(3) 1.0215(3) 0.0896(2) 0.0245(6) Uani 1 1 d . . . . .
H331 H 0.6818 1.0323 0.0208 0.029 Uiso 1 1 calc R U . . .
C34 C 0.7513(3) 0.9965(3) 0.1495(3) 0.0294(7) Uani 1 1 d . . . . .
H341 H 0.8306 0.9897 0.1216 0.035 Uiso 1 1 calc R U . . .
C35 C 0.7240(3) 0.9815(3) 0.2494(3) 0.0272(7) Uani 1 1 d . . . . .
H351 H 0.7846 0.9634 0.2900 0.033 Uiso 1 1 calc R U . . .
C36 C 0.6080(3) 0.9930(2) 0.2906(2) 0.0215(6) Uani 1 1 d . . . . .
H361 H 0.5895 0.9844 0.3589 0.026 Uiso 1 1 calc R U . . .
C40 C 0.2072(2) 0.9456(2) 0.3282(2) 0.0180(5) Uani 1 1 d . . . . .
H401 H 0.1757 0.8704 0.3624 0.022 Uiso 1 1 calc R U . . .
H402 H 0.1849 0.9924 0.3723 0.022 Uiso 1 1 calc R U . . .
C41 C 0.1543(2) 1.0104(3) 0.2326(2) 0.0200(6) Uani 1 1 d . . . . .
C42 C 0.1303(3) 0.9480(3) 0.1783(2) 0.0282(7) Uani 1 1 d . . . . .
H421 H 0.1456 0.8650 0.2023 0.034 Uiso 1 1 calc R U . . .
C43 C 0.0842(3) 1.0070(4) 0.0890(3) 0.0378(8) Uani 1 1 d . . . . .
H431 H 0.0682 0.9642 0.0519 0.045 Uiso 1 1 calc R U . . .
C44 C 0.0612(3) 1.1283(4) 0.0536(3) 0.0404(10) Uani 1 1 d . . . . .
H441 H 0.0304 1.1684 -0.0079 0.048 Uiso 1 1 calc R U . . .
C45 C 0.0833(3) 1.1905(3) 0.1080(3) 0.0359(9) Uani 1 1 d . . . . .
H451 H 0.0671 1.2735 0.0840 0.043 Uiso 1 1 calc R U . . .
C46 C 0.1293(3) 1.1320(3) 0.1979(2) 0.0273(7) Uani 1 1 d . . . . .
H461 H 0.1436 1.1750 0.2356 0.033 Uiso 1 1 calc R U . . .
C50 C 0.4085(2) 0.7006(2) 0.8345(2) 0.0136(5) Uani 1 1 d . . . . .
H501 H 0.3942 0.7175 0.8971 0.016 Uiso 1 1 calc R U . . .
H502 H 0.3909 0.7752 0.7793 0.016 Uiso 1 1 calc R U . . .
C51 C 0.5367(2) 0.6514(2) 0.81737(18) 0.0132(5) Uani 1 1 d . . . . .
O51 O 0.55910(16) 0.57616(17) 0.77372(15) 0.0171(4) Uani 1 1 d . . . . .
O52 O 0.60918(17) 0.68869(18) 0.84509(15) 0.0186(4) Uani 1 1 d . . . . .
C60 C 0.4776(2) 0.3073(2) 0.89171(19) 0.0148(5) Uani 1 1 d . . . . .
H601 H 0.4655 0.2350 0.9495 0.018 Uiso 1 1 calc R U . . .
H602 H 0.5158 0.3574 0.9125 0.018 Uiso 1 1 calc R U . . .
C61 C 0.5542(2) 0.2769(2) 0.80661(19) 0.0136(5) Uani 1 1 d . . . . .
O61 O 0.54733(16) 0.35274(16) 0.71981(14) 0.0150(4) Uani 1 1 d . . . . .
O62 O 0.61703(18) 0.18052(18) 0.82682(15) 0.0213(4) Uani 1 1 d . . . . .
C70 C 0.3003(2) 0.3721(2) 0.60836(18) 0.0126(5) Uani 1 1 d . . . . .
H701 H 0.2396 0.3431 0.5883 0.015 Uiso 1 1 calc R U . . .
H702 H 0.3569 0.3041 0.6403 0.015 Uiso 1 1 calc R U . . .
C71 C 0.3629(2) 0.4568(2) 0.51595(18) 0.0107(4) Uani 1 1 d . . . . .
O71 O 0.38141(15) 0.55069(15) 0.52276(13) 0.0109(3) Uani 1 1 d . . . . .
O72 O 0.39342(16) 0.42747(16) 0.44088(13) 0.0130(3) Uani 1 1 d . . . . .
Cl1 Cl 0.03443(14) 0.53821(16) 0.06910(13) 0.0424(5) Uani 0.5 1 d . . P . .
N1A N 0.1995(3) 0.6229(3) 0.3414(3) 0.0728(14) Uani 0.5 1 d . . P A 1
O1W O 0.1995(3) 0.6229(3) 0.3414(3) 0.0728(14) Uani 0.5 1 d . . P B 2
H11W H 0.1440 0.6807 0.3330 0.087 Uiso 1 1 d R U . . .
H12W H 0.2611 0.6359 0.3580 0.087 Uiso 1 1 d R U . . .
H13A H 0.2265 0.5991 0.2843 0.087 Uiso 0.5 1 d R U P B 1
H14A H 0.1994 0.5531 0.3792 0.087 Uiso 0.5 1 d R U P B 1
O2W O 0.3377(2) 0.1950(2) 0.4547(3) 0.0502(8) Uani 1 1 d . . . . .
H21W H 0.3413 0.1213 0.4751 0.053(14) Uiso 1 1 d R . . . .
H22W H 0.4070 0.2181 0.4396 0.064(16) Uiso 1 1 d R . . . .
O3W O 0.0647(2) 1.0555(3) 0.5389(3) 0.0506(8) Uani 1 1 d . . . . .
H31W H 0.1372 1.0255 0.5380 0.057(15) Uiso 1 1 d R . . . .
H32W H 0.0312 1.1087 0.5660 0.069 Uiso 1 1 d R U . . .
O4W O 0.1690(2) 0.3695(3) 0.2232(3) 0.0571(9) Uani 1 1 d . . . . .
H41W H 0.2414 0.3601 0.1965 0.052(14) Uiso 1 1 d R . . . .
H42W H 0.1306 0.4225 0.1791 0.063 Uiso 1 1 d R U . . .
O5W O 0.0038(3) 0.7220(3) 0.4189(2) 0.0468(7) Uani 1 1 d . . . . .
H51W H -0.0258 0.7601 0.3658 0.048(13) Uiso 1 1 d R . . . .
H52W H -0.0541 0.6978 0.4733 0.057 Uiso 1 1 d R U . . .
O6WA O 0.2401(5) 0.6117(5) 0.1631(5) 0.0629(13) Uani 0.607(6) 1 d . . P C 3
H61W H 0.2525 0.6904 0.1273 0.075 Uiso 1 1 d R U . . .
H62W H 0.1927 0.6246 0.1151 0.075 Uiso 1 1 d R U . . .
O6WB O 0.1798(9) 0.7036(8) 0.1052(7) 0.0629(13) Uani 0.393(6) 1 d . . P C 4
O7WA O 0.1622(3) 0.3783(3) 0.4066(3) 0.0288(7) Uani 0.650(5) 1 d . . P D 5
H71W H 0.2294 0.3302 0.4197 0.035 Uiso 1 1 d R U . . .
H72W H 0.1875 0.3850 0.3520 0.035 Uiso 1 1 d R U . . .
O7WB O 0.2484(6) 0.3836(6) 0.3646(5) 0.0288(7) Uani 0.350(5) 1 d . . P D 6


_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
Pr1 O51 2.4208(19) . ?
Pr1 O71 2.4418(17) . ?
Pr1 O11 2.4638(17) . ?
Pr1 O61 2.4867(18) . ?
Pr1 O72 2.5367(18) 2_666 ?
Pr1 N4 2.753(2) . ?
Pr1 N7 2.757(2) . ?
Pr1 N10 2.760(2) . ?
Pr1 N1 2.777(2) . ?
N1 C20 1.477(3) . ?
N1 C2 1.487(3) . ?
N1 C12 1.488(3) . ?
C2 C3 1.518(3) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.482(3) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.477(3) . ?
N4 C5 1.487(3) . ?
C5 C6 1.516(4) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.481(3) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.476(3) . ?
N7 C8 1.488(3) . ?
C8 C9 1.511(4) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.490(3) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.476(3) . ?
N10 C11 1.494(3) . ?
C11 C12 1.516(4) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.831(3) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.4987(18) . ?
P1 O11 1.5188(18) . ?
P1 C21 1.829(3) . ?
C21 N22 1.503(3) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C30 1.512(3) . ?
N22 C40 1.518(3) . ?
N22 H221 1.0000 . ?
C30 C31 1.505(4) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36 1.393(4) . ?
C31 C32 1.395(4) . ?
C32 C33 1.389(4) . ?
C32 H321 0.9500 . ?
C33 C34 1.395(5) . ?
C33 H331 0.9500 . ?
C34 C35 1.382(5) . ?
C34 H341 0.9500 . ?
C35 C36 1.394(5) . ?
C35 H351 0.9500 . ?
C36 H361 0.9500 . ?
C40 C41 1.506(4) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C41 C42 1.390(5) . ?
C41 C46 1.393(4) . ?
C42 C43 1.386(5) . ?
C42 H421 0.9500 . ?
C43 C44 1.389(6) . ?
C43 H431 0.9500 . ?
C44 C45 1.379(6) . ?
C44 H441 0.9500 . ?
C45 C46 1.392(5) . ?
C45 H451 0.9500 . ?
C46 H461 0.9500 . ?
C50 C51 1.530(4) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.235(3) . ?
C51 O51 1.279(3) . ?
C60 C61 1.520(4) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.243(3) . ?
C61 O61 1.272(3) . ?
C70 C71 1.532(3) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.251(3) . ?
C71 O71 1.269(3) . ?
O72 Pr1 2.5367(18) 2_666 ?
N1A H11W 0.8619 . ?
N1A H12W 0.8655 . ?
N1A H13A 0.9655 . ?
N1A H14A 0.8366 . ?
O1W H11W 0.8619 . ?
O1W H12W 0.8655 . ?
O2W H21W 0.8456 . ?
O2W H22W 0.8807 . ?
O3W H31W 0.8641 . ?
O3W H32W 0.8872 . ?
O4W H41W 0.8766 . ?
O4W H42W 0.8531 . ?
O5W H51W 0.8418 . ?
O5W H52W 0.9436 . ?
O6WA H61W 0.9473 . ?
O6WA H62W 0.9226 . ?
O6WB H61W 0.9332 . ?
O6WB H62W 0.9231 . ?
O7WA H71W 0.8991 . ?
O7WA H72W 0.7768 . ?
O7WB H71W 0.8544 . ?
O7WB H72W 0.7673 . ?

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
O51 Pr1 O71 147.32(6) . . ?
O51 Pr1 O11 83.17(6) . . ?
O71 Pr1 O11 81.47(6) . . ?
O51 Pr1 O61 80.99(6) . . ?
O71 Pr1 O61 94.33(6) . . ?
O11 Pr1 O61 142.91(6) . . ?
O51 Pr1 O72 77.20(6) . 2_666 ?
O71 Pr1 O72 70.61(6) . 2_666 ?
O11 Pr1 O72 71.42(6) . 2_666 ?
O61 Pr1 O72 72.44(6) . 2_666 ?
O51 Pr1 N4 63.09(6) . . ?
O71 Pr1 N4 142.64(6) . . ?
O11 Pr1 N4 84.16(6) . . ?
O61 Pr1 N4 117.15(6) . . ?
O72 Pr1 N4 135.51(6) 2_666 . ?
O51 Pr1 N7 84.69(7) . . ?
O71 Pr1 N7 121.66(6) . . ?
O11 Pr1 N7 148.95(6) . . ?
O61 Pr1 N7 61.85(6) . . ?
O72 Pr1 N7 132.87(6) 2_666 . ?
N4 Pr1 N7 64.88(6) . . ?
O51 Pr1 N10 149.18(6) . . ?
O71 Pr1 N10 61.17(6) . . ?
O11 Pr1 N10 121.96(6) . . ?
O61 Pr1 N10 86.15(6) . . ?
O72 Pr1 N10 125.12(6) 2_666 . ?
N4 Pr1 N10 99.32(6) . . ?
N7 Pr1 N10 64.58(6) . . ?
O51 Pr1 N1 120.32(6) . . ?
O71 Pr1 N1 77.98(6) . . ?
O11 Pr1 N1 64.66(6) . . ?
O61 Pr1 N1 150.64(6) . . ?
O72 Pr1 N1 128.82(6) 2_666 . ?
N4 Pr1 N1 64.71(6) . . ?
N7 Pr1 N1 97.92(6) . . ?
N10 Pr1 N1 65.21(6) . . ?
C20 N1 C2 107.56(19) . . ?
C20 N1 C12 108.56(19) . . ?
C2 N1 C12 110.04(19) . . ?
C20 N1 Pr1 108.03(14) . . ?
C2 N1 Pr1 110.47(14) . . ?
C12 N1 Pr1 112.02(14) . . ?
N1 C2 C3 112.5(2) . . ?
N1 C2 H21 109.1 . . ?
C3 C2 H21 109.1 . . ?
N1 C2 H22 109.1 . . ?
C3 C2 H22 109.1 . . ?
H21 C2 H22 107.8 . . ?
N4 C3 C2 112.1(2) . . ?
N4 C3 H31 109.2 . . ?
C2 C3 H31 109.2 . . ?
N4 C3 H32 109.2 . . ?
C2 C3 H32 109.2 . . ?
H31 C3 H32 107.9 . . ?
C50 N4 C3 109.71(19) . . ?
C50 N4 C5 108.43(19) . . ?
C3 N4 C5 109.00(19) . . ?
C50 N4 Pr1 102.75(14) . . ?
C3 N4 Pr1 115.22(15) . . ?
C5 N4 Pr1 111.41(14) . . ?
N4 C5 C6 111.8(2) . . ?
N4 C5 H51 109.3 . . ?
C6 C5 H51 109.3 . . ?
N4 C5 H52 109.3 . . ?
C6 C5 H52 109.3 . . ?
H51 C5 H52 107.9 . . ?
N7 C6 C5 111.2(2) . . ?
N7 C6 H61 109.4 . . ?
C5 C6 H61 109.4 . . ?
N7 C6 H62 109.4 . . ?
C5 C6 H62 109.4 . . ?
H61 C6 H62 108.0 . . ?
C60 N7 C6 110.0(2) . . ?
C60 N7 C8 107.2(2) . . ?
C6 N7 C8 110.0(2) . . ?
C60 N7 Pr1 104.26(15) . . ?
C6 N7 Pr1 113.54(14) . . ?
C8 N7 Pr1 111.55(14) . . ?
N7 C8 C9 112.6(2) . . ?
N7 C8 H81 109.1 . . ?
C9 C8 H81 109.1 . . ?
N7 C8 H82 109.1 . . ?
C9 C8 H82 109.1 . . ?
H81 C8 H82 107.8 . . ?
N10 C9 C8 112.3(2) . . ?
N10 C9 H91 109.1 . . ?
C8 C9 H91 109.1 . . ?
N10 C9 H92 109.1 . . ?
C8 C9 H92 109.1 . . ?
H91 C9 H92 107.9 . . ?
C70 N10 C9 111.12(19) . . ?
C70 N10 C11 109.04(19) . . ?
C9 N10 C11 108.16(19) . . ?
C70 N10 Pr1 101.54(14) . . ?
C9 N10 Pr1 115.15(15) . . ?
C11 N10 Pr1 111.63(14) . . ?
N10 C11 C12 111.6(2) . . ?
N10 C11 H111 109.3 . . ?
C12 C11 H111 109.3 . . ?
N10 C11 H112 109.3 . . ?
C12 C11 H112 109.3 . . ?
H111 C11 H112 108.0 . . ?
N1 C12 C11 112.0(2) . . ?
N1 C12 H121 109.2 . . ?
C11 C12 H121 109.2 . . ?
N1 C12 H122 109.2 . . ?
C11 C12 H122 109.2 . . ?
H121 C12 H122 107.9 . . ?
N1 C20 P1 110.55(16) . . ?
N1 C20 H201 109.5 . . ?
P1 C20 H201 109.5 . . ?
N1 C20 H202 109.5 . . ?
P1 C20 H202 109.5 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 118.49(11) . . ?
O12 P1 C21 110.44(11) . . ?
O11 P1 C21 104.74(11) . . ?
O12 P1 C20 111.57(11) . . ?
O11 P1 C20 105.41(10) . . ?
C21 P1 C20 105.18(12) . . ?
P1 O11 Pr1 126.04(10) . . ?
N22 C21 P1 118.09(17) . . ?
N22 C21 H211 107.8 . . ?
P1 C21 H211 107.8 . . ?
N22 C21 H212 107.8 . . ?
P1 C21 H212 107.8 . . ?
H211 C21 H212 107.1 . . ?
C21 N22 C30 112.5(2) . . ?
C21 N22 C40 112.47(19) . . ?
C30 N22 C40 111.5(2) . . ?
C21 N22 H221 106.6 . . ?
C30 N22 H221 106.6 . . ?
C40 N22 H221 106.6 . . ?
C31 C30 N22 112.1(2) . . ?
C31 C30 H301 109.2 . . ?
N22 C30 H301 109.2 . . ?
C31 C30 H302 109.2 . . ?
N22 C30 H302 109.2 . . ?
H301 C30 H302 107.9 . . ?
C36 C31 C32 119.3(3) . . ?
C36 C31 C30 120.7(3) . . ?
C32 C31 C30 119.9(2) . . ?
C33 C32 C31 120.7(3) . . ?
C33 C32 H321 119.6 . . ?
C31 C32 H321 119.6 . . ?
C32 C33 C34 119.4(3) . . ?
C32 C33 H331 120.3 . . ?
C34 C33 H331 120.3 . . ?
C35 C34 C33 120.3(3) . . ?
C35 C34 H341 119.8 . . ?
C33 C34 H341 119.8 . . ?
C34 C35 C36 120.2(3) . . ?
C34 C35 H351 119.9 . . ?
C36 C35 H351 119.9 . . ?
C31 C36 C35 120.1(3) . . ?
C31 C36 H361 120.0 . . ?
C35 C36 H361 120.0 . . ?
C41 C40 N22 111.8(2) . . ?
C41 C40 H401 109.3 . . ?
N22 C40 H401 109.3 . . ?
C41 C40 H402 109.3 . . ?
N22 C40 H402 109.3 . . ?
H401 C40 H402 107.9 . . ?
C42 C41 C46 119.6(3) . . ?
C42 C41 C40 119.5(3) . . ?
C46 C41 C40 120.8(3) . . ?
C43 C42 C41 120.0(3) . . ?
C43 C42 H421 120.0 . . ?
C41 C42 H421 120.0 . . ?
C42 C43 C44 120.3(4) . . ?
C42 C43 H431 119.8 . . ?
C44 C43 H431 119.8 . . ?
C45 C44 C43 119.9(3) . . ?
C45 C44 H441 120.0 . . ?
C43 C44 H441 120.0 . . ?
C44 C45 C46 120.1(3) . . ?
C44 C45 H451 119.9 . . ?
C46 C45 H451 119.9 . . ?
C45 C46 C41 120.0(3) . . ?
C45 C46 H461 120.0 . . ?
C41 C46 H461 120.0 . . ?
N4 C50 C51 111.9(2) . . ?
N4 C50 H501 109.2 . . ?
C51 C50 H501 109.2 . . ?
N4 C50 H502 109.2 . . ?
C51 C50 H502 109.2 . . ?
H501 C50 H502 107.9 . . ?
O52 C51 O51 125.8(2) . . ?
O52 C51 C50 117.6(2) . . ?
O51 C51 C50 116.5(2) . . ?
C51 O51 Pr1 123.65(16) . . ?
N7 C60 C61 108.9(2) . . ?
N7 C60 H601 109.9 . . ?
C61 C60 H601 109.9 . . ?
N7 C60 H602 109.9 . . ?
C61 C60 H602 109.9 . . ?
H601 C60 H602 108.3 . . ?
O62 C61 O61 125.4(2) . . ?
O62 C61 C60 118.0(2) . . ?
O61 C61 C60 116.6(2) . . ?
C61 O61 Pr1 124.58(16) . . ?
N10 C70 C71 110.9(2) . . ?
N10 C70 H701 109.5 . . ?
C71 C70 H701 109.5 . . ?
N10 C70 H702 109.5 . . ?
C71 C70 H702 109.5 . . ?
H701 C70 H702 108.1 . . ?
O72 C71 O71 125.2(2) . . ?
O72 C71 C70 118.0(2) . . ?
O71 C71 C70 116.8(2) . . ?
C71 O71 Pr1 118.72(15) . . ?
C71 O72 Pr1 130.51(16) . 2_666 ?
H11W N1A H12W 113.4 . . ?
H11W N1A H13A 115.2 . . ?
H12W N1A H13A 105.5 . . ?
H11W N1A H14A 129.5 . . ?
H12W N1A H14A 98.0 . . ?
H13A N1A H14A 91.2 . . ?
H11W O1W H12W 113.4 . . ?
H21W O2W H22W 112.5 . . ?
H31W O3W H32W 125.8 . . ?
H41W O4W H42W 107.9 . . ?
H51W O5W H52W 111.3 . . ?
H61W O6WA H62W 84.2 . . ?
H61W O6WB H62W 84.9 . . ?
H71W O7WA H72W 82.4 . . ?
H71W O7WB H72W 86.0 . . ?

_refine_diff_density_max         1.833
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.109

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

data_dbam_yb
_database_code_depnum_ccdc_archive 'CCDC 1959627'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H40 N5 O8 P Yb, Na, 6(H2 O)'
_chemical_formula_sum            'C30 H52 N5 Na O14 P Yb'
_chemical_formula_weight         933.76

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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   49.3984(12)
_cell_length_b                   10.1801(2)
_cell_length_c                   15.3464(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.544(2)
_cell_angle_gamma                90
_cell_volume                     7533.2(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9229
_cell_measurement_theta_min      2.4038
_cell_measurement_theta_max      26.0154

_exptl_crystal_description       'thin plate'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_F_000             3800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.447
_exptl_crystal_size_mid          0.312
_exptl_crystal_size_min          0.088
_exptl_absorpt_coefficient_mu    2.608
_shelx_estimated_absorpt_T_min   0.389
_shelx_estimated_absorpt_T_max   0.803
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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 8.3333
_diffrn_reflns_number            46263
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.689
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7410
_reflns_number_gt                6343
_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.
 
 _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 Instrument Service v2014.11.0.1'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0444P)²+77.5617P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7410
_refine_ls_number_parameters     514
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1039
_refine_ls_wR_factor_gt          0.0990
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Yb1 Yb 0.40467(2) 0.20591(2) 0.43685(2) 0.01992(8) Uani 1 1 d . . . . .
N1 N 0.35944(9) 0.2372(4) 0.3183(3) 0.0227(9) Uani 1 1 d . . . . .
C2 C 0.36581(12) 0.2960(5) 0.2366(3) 0.0273(12) Uani 1 1 d . . . . .
H21 H 0.3689 0.3916 0.2458 0.033 Uiso 1 1 calc R U . . .
H22 H 0.3497 0.2837 0.1861 0.033 Uiso 1 1 calc R U . . .
C3 C 0.39131(12) 0.2349(6) 0.2131(3) 0.0297(12) Uani 1 1 d . . . . .
H31 H 0.3876 0.1410 0.1982 0.036 Uiso 1 1 calc R U . . .
H32 H 0.3952 0.2793 0.1597 0.036 Uiso 1 1 calc R U . . .
N4 N 0.41569(10) 0.2461(5) 0.2874(3) 0.0271(10) Uani 1 1 d . . . . .
C5 C 0.43755(13) 0.1553(6) 0.2719(4) 0.0347(13) Uani 1 1 d . . . . .
H51 H 0.4558 0.1859 0.3063 0.042 Uiso 1 1 calc R U . . .
H52 H 0.4381 0.1569 0.2078 0.042 Uiso 1 1 calc R U . . .
C6 C 0.43277(13) 0.0160(6) 0.2989(4) 0.0350(13) Uani 1 1 d . . . . .
H61 H 0.4155 -0.0182 0.2603 0.042 Uiso 1 1 calc R U . . .
H62 H 0.4483 -0.0401 0.2901 0.042 Uiso 1 1 calc R U . . .
N7 N 0.43053(10) 0.0095(5) 0.3938(3) 0.0284(10) Uani 1 1 d . . . . .
C8 C 0.41710(13) -0.1172(6) 0.4102(4) 0.0332(13) Uani 1 1 d . . . . .
H81 H 0.4224 -0.1387 0.4746 0.040 Uiso 1 1 calc R U . . .
H82 H 0.4240 -0.1885 0.3770 0.040 Uiso 1 1 calc R U . . .
C9 C 0.38587(12) -0.1104(5) 0.3817(4) 0.0299(12) Uani 1 1 d . . . . .
H91 H 0.3804 -0.0994 0.3161 0.036 Uiso 1 1 calc R U . . .
H92 H 0.3777 -0.1936 0.3975 0.036 Uiso 1 1 calc R U . . .
N10 N 0.37489(9) 0.0006(4) 0.4257(3) 0.0238(9) Uani 1 1 d . . . . .
C11 C 0.34599(11) 0.0293(5) 0.3793(3) 0.0280(12) Uani 1 1 d . . . . .
H111 H 0.3365 0.0775 0.4202 0.034 Uiso 1 1 calc R U . . .
H112 H 0.3359 -0.0543 0.3627 0.034 Uiso 1 1 calc R U . . .
C12 C 0.34501(11) 0.1104(5) 0.2962(3) 0.0258(11) Uani 1 1 d . . . . .
H121 H 0.3539 0.0610 0.2543 0.031 Uiso 1 1 calc R U . . .
H122 H 0.3254 0.1268 0.2663 0.031 Uiso 1 1 calc R U . . .
C20 C 0.34168(11) 0.3295(5) 0.3558(3) 0.0229(11) Uani 1 1 d . . . . .
H201 H 0.3334 0.2832 0.4005 0.028 Uiso 1 1 calc R U . . .
H202 H 0.3264 0.3611 0.3075 0.028 Uiso 1 1 calc R U . . .
P1 P 0.36209(3) 0.46984(13) 0.40861(9) 0.0222(3) Uani 1 1 d . . . . .
O11 O 0.39157(8) 0.4174(3) 0.4374(2) 0.0247(8) Uani 1 1 d . . . . .
O12 O 0.35822(8) 0.5870(4) 0.3488(3) 0.0325(9) Uani 1 1 d . . . . .
C21 C 0.34857(11) 0.4993(6) 0.5075(4) 0.0288(12) Uani 1 1 d . . . . .
H211 H 0.3514 0.4202 0.5460 0.035 Uiso 1 1 calc R U . . .
H212 H 0.3587 0.5732 0.5419 0.035 Uiso 1 1 calc R U . . .
N22 N 0.31890(9) 0.5305(4) 0.4820(3) 0.0268(10) Uani 1 1 d . . . . .
C30 C 0.31428(12) 0.6700(6) 0.4604(4) 0.0369(14) Uani 1 1 d . . . . .
H301 H 0.3292 0.7023 0.4322 0.044 Uiso 1 1 calc R U . . .
H302 H 0.3153 0.7200 0.5164 0.044 Uiso 1 1 calc R U . . .
C31 C 0.28662(13) 0.6955(6) 0.3984(4) 0.0363(14) Uani 1 1 d . . . . .
C32A C 0.2758(3) 0.8193(13) 0.3925(10) 0.048(4) Uani 0.522(9) 1 d . . P A 1
H32A H 0.2858 0.8871 0.4281 0.057 Uiso 0.522(9) 1 calc R U P A 1
C33A C 0.2507(3) 0.8491(17) 0.3363(11) 0.065(5) Uani 0.522(9) 1 d . . P A 1
H33A H 0.2425 0.9335 0.3361 0.078 Uiso 0.522(9) 1 calc R U P A 1
C34 C 0.23752(19) 0.7451(11) 0.2774(8) 0.084(3) Uani 1 1 d . . . . .
H34 H 0.2232 0.7667 0.2273 0.101 Uiso 1 1 calc R U . A 1
C35A C 0.2447(3) 0.625(2) 0.2915(14) 0.094(8) Uani 0.522(9) 1 d . . P A 1
H35A H 0.2326 0.5572 0.2643 0.112 Uiso 0.522(9) 1 calc R U P A 1
C36A C 0.2700(3) 0.5935(14) 0.3462(11) 0.063(5) Uani 0.522(9) 1 d . . P A 1
H36A H 0.2765 0.5054 0.3496 0.076 Uiso 0.522(9) 1 calc R U P A 1
C32B C 0.2633(3) 0.7328(13) 0.4220(11) 0.042(4) Uani 0.478(9) 1 d . . P A 2
H32B H 0.2631 0.7485 0.4829 0.050 Uiso 0.478(9) 1 calc R U P A 2
C33B C 0.2382(3) 0.7493(14) 0.3532(14) 0.052(5) Uani 0.478(9) 1 d . . P A 2
H33B H 0.2213 0.7644 0.3716 0.063 Uiso 0.478(9) 1 calc R U P A 2
C35B C 0.2641(3) 0.7114(15) 0.2436(11) 0.050(4) Uani 0.478(9) 1 d . . P A 2
H35B H 0.2641 0.7057 0.1818 0.060 Uiso 0.478(9) 1 calc R U P A 2
C36B C 0.2879(3) 0.6902(12) 0.3092(10) 0.039(3) Uani 0.478(9) 1 d . . P A 2
H36B H 0.3050 0.6720 0.2930 0.047 Uiso 0.478(9) 1 calc R U P A 2
C40 C 0.30427(13) 0.4911(7) 0.5512(5) 0.0434(16) Uani 1 1 d . . . . .
H401 H 0.3141 0.5315 0.6080 0.052 Uiso 0.575(7) 1 calc R U P B 3
H402 H 0.2855 0.5310 0.5360 0.052 Uiso 0.575(7) 1 calc R U P B 3
H403 H 0.2864 0.5385 0.5442 0.052 Uiso 0.425(7) 1 calc R U P B 4
H404 H 0.3157 0.5090 0.6115 0.052 Uiso 0.425(7) 1 calc R U P B 4
C41A C 0.3008(2) 0.3533(7) 0.5680(6) 0.033(3) Uani 0.575(7) 1 d G . P B 3
C42A C 0.2891(2) 0.2771(9) 0.4943(5) 0.044(3) Uani 0.575(7) 1 d G . P B 3
H42A H 0.2845 0.3157 0.4366 0.053 Uiso 0.575(7) 1 calc R U P B 3
C43A C 0.2841(2) 0.1443(9) 0.5049(6) 0.057(3) Uani 0.575(7) 1 d G . P B 3
H43A H 0.2761 0.0923 0.4546 0.069 Uiso 0.575(7) 1 calc R U P B 3
C44A C 0.2908(2) 0.0878(7) 0.5893(8) 0.069(4) Uani 0.575(7) 1 d G . P B 3
H44A H 0.2874 -0.0029 0.5966 0.083 Uiso 0.575(7) 1 calc R U P B 3
C45A C 0.3025(2) 0.1640(9) 0.6630(6) 0.071(4) Uani 0.575(7) 1 d G . P B 3
H45A H 0.3071 0.1254 0.7207 0.085 Uiso 0.575(7) 1 calc R U P B 3
C46A C 0.30753(19) 0.2968(9) 0.6524(5) 0.056(3) Uani 0.575(7) 1 d G . P B 3
H46A H 0.3155 0.3489 0.7027 0.067 Uiso 0.575(7) 1 calc R U P B 3
C41B C 0.2991(3) 0.3336(10) 0.5354(9) 0.033(3) Uani 0.425(7) 1 d G . P B 4
C42B C 0.2807(3) 0.2840(13) 0.4611(8) 0.044(3) Uani 0.425(7) 1 d G . P B 4
H42B H 0.2718 0.3417 0.4151 0.053 Uiso 0.425(7) 1 calc R U P B 4
C43B C 0.2754(3) 0.1499(14) 0.4540(9) 0.057(3) Uani 0.425(7) 1 d G . P B 4
H43B H 0.2628 0.1160 0.4032 0.069 Uiso 0.425(7) 1 calc R U P B 4
C44B C 0.2885(3) 0.0654(11) 0.5212(11) 0.069(4) Uani 0.425(7) 1 d G . P B 4
H44B H 0.2849 -0.0263 0.5163 0.083 Uiso 0.425(7) 1 calc R U P B 4
C45B C 0.3069(3) 0.1150(12) 0.5955(9) 0.071(4) Uani 0.425(7) 1 d G . P B 4
H45B H 0.3158 0.0572 0.6414 0.085 Uiso 0.425(7) 1 calc R U P B 4
C46B C 0.3122(3) 0.2491(13) 0.6026(8) 0.056(3) Uani 0.425(7) 1 d G . P B 4
H46B H 0.3248 0.2829 0.6534 0.067 Uiso 0.425(7) 1 calc R U P B 4
C50 C 0.42724(12) 0.3811(6) 0.2941(4) 0.0316(13) Uani 1 1 d . . . . .
H501 H 0.4119 0.4458 0.2845 0.038 Uiso 1 1 calc R U . . .
H502 H 0.4380 0.3946 0.2473 0.038 Uiso 1 1 calc R U . . .
C51 C 0.44584(13) 0.4022(7) 0.3849(4) 0.0411(15) Uani 1 1 d . . . . .
O51 O 0.44481(8) 0.3185(4) 0.4453(3) 0.0301(9) Uani 1 1 d . . . . .
O52 O 0.46094(13) 0.4996(6) 0.3960(4) 0.078(2) Uani 1 1 d . . . . .
C60 C 0.45795(13) 0.0147(6) 0.4557(4) 0.0366(14) Uani 1 1 d . . . . .
H601 H 0.4696 0.0822 0.4352 0.044 Uiso 1 1 calc R U . . .
H602 H 0.4674 -0.0712 0.4559 0.044 Uiso 1 1 calc R U . . .
C61 C 0.45485(13) 0.0474(7) 0.5500(4) 0.0393(14) Uani 1 1 d . . . . .
O61 O 0.43364(8) 0.1125(4) 0.5575(2) 0.0293(8) Uani 1 1 d . . . . .
O62 O 0.47306(11) 0.0105(7) 0.6141(3) 0.0764(19) Uani 1 1 d . . . . .
C70 C 0.37491(12) -0.0317(5) 0.5199(3) 0.0269(12) Uani 1 1 d . . . . .
H701 H 0.3919 -0.0816 0.5463 0.032 Uiso 1 1 calc R U . . .
H702 H 0.3587 -0.0879 0.5222 0.032 Uiso 1 1 calc R U . . .
C71 C 0.37372(10) 0.0929(5) 0.5745(3) 0.0229(11) Uani 1 1 d . . . . .
O71 O 0.37782(7) 0.2008(3) 0.5376(2) 0.0218(7) Uani 1 1 d . . . . .
O72 O 0.36981(9) 0.0814(4) 0.6508(2) 0.0326(9) Uani 1 1 d . . . . .
Na1 Na 0.47691(8) 0.6503(5) 0.3059(3) 0.0908(12) Uani 1 1 d . . . . .
O1W O 0.43783(11) 0.6873(6) 0.1950(4) 0.0690(17) Uani 1 1 d . . . . .
O2WA O 0.50335(18) 0.6952(12) 0.4457(6) 0.081(3) Uani 0.656(10) 1 d . . P C 5
O2WB O 0.5048(3) 0.581(2) 0.4674(12) 0.081(3) Uani 0.344(10) 1 d . . P C 6
O3W O 0.5000 0.4616(16) 0.2500 0.138(5) Uani 1 2 d S T P C .
O4W O 0.5000 0.8290(12) 0.2500 0.099(3) Uani 1 2 d S T P C .
O5W O 0.38509(10) 0.6546(4) 0.2191(3) 0.0418(10) Uani 1 1 d . . . . .
O6WA O 0.4292(2) 0.5606(12) 0.5728(7) 0.068(3) Uani 0.622(13) 1 d . . P D 7
O6WB O 0.4219(4) 0.630(2) 0.5480(12) 0.068(3) Uani 0.378(13) 1 d . . P D 8
O7WA O 0.5199(2) 0.3004(10) 0.4011(7) 0.059(2) Uiso 0.506(3) 1 d . . P E 9
O7WB O 0.5077(4) 0.236(2) 0.3538(13) 0.059(2) Uiso 0.281(3) 1 d . . P F 10
O7WC O 0.5188(5) 0.422(2) 0.4446(17) 0.059(2) Uiso 0.213(3) 1 d . . P G 11


_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
Yb1 O71 2.246(3) . ?
Yb1 O11 2.249(4) . ?
Yb1 O51 2.269(4) . ?
Yb1 O61 2.286(4) . ?
Yb1 N4 2.504(4) . ?
Yb1 N7 2.537(4) . ?
Yb1 N10 2.541(4) . ?
Yb1 N1 2.576(4) . ?
Yb1 C51 3.077(6) . ?
Yb1 C71 3.086(5) . ?
Yb1 C61 3.145(6) . ?
Yb1 C50 3.207(5) . ?
N1 C12 1.478(6) . ?
N1 C20 1.484(7) . ?
N1 C2 1.484(6) . ?
C2 C3 1.517(8) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.472(7) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C5 1.479(7) . ?
N4 C50 1.484(7) . ?
C5 C6 1.510(8) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.486(7) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.477(8) . ?
N7 C8 1.496(7) . ?
C8 C9 1.511(8) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.478(7) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C11 1.480(7) . ?
N10 C70 1.483(6) . ?
C11 C12 1.511(7) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.833(5) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.492(4) . ?
P1 O11 1.524(4) . ?
P1 C21 1.811(5) . ?
C21 N22 1.467(7) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C40 1.464(7) . ?
N22 C30 1.465(7) . ?
C30 C31 1.508(9) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C32B 1.336(14) . ?
C31 C32A 1.365(13) . ?
C31 C36B 1.384(16) . ?
C31 C36A 1.451(16) . ?
C32A C33A 1.38(2) . ?
C32A H32A 0.9500 . ?
C33A C34 1.45(2) . ?
C33A H33A 0.9500 . ?
C34 C33B 1.16(2) . ?
C34 C35A 1.28(2) . ?
C34 C35B 1.553(18) . ?
C34 H34 0.9500 . ?
C35A C36A 1.39(2) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C32B C33B 1.45(2) . ?
C32B H32B 0.9500 . ?
C33B H33B 0.9500 . ?
C35B C36B 1.39(2) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C40 C41A 1.443(9) . ?
C40 C41B 1.634(13) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C40 H403 0.9900 . ?
C40 H404 0.9900 . ?
C41A C42A 1.3900 . ?
C41A C46A 1.3900 . ?
C42A C43A 1.3900 . ?
C42A H42A 0.9500 . ?
C43A C44A 1.3900 . ?
C43A H43A 0.9500 . ?
C44A C45A 1.3900 . ?
C44A H44A 0.9500 . ?
C45A C46A 1.3900 . ?
C45A H45A 0.9500 . ?
C46A H46A 0.9500 . ?
C41B C42B 1.3900 . ?
C41B C46B 1.3900 . ?
C42B C43B 1.3900 . ?
C42B H42B 0.9500 . ?
C43B C44B 1.3900 . ?
C43B H43B 0.9500 . ?
C44B C45B 1.3900 . ?
C44B H44B 0.9500 . ?
C45B C46B 1.3900 . ?
C45B H45B 0.9500 . ?
C46B H46B 0.9500 . ?
C50 C51 1.508(9) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.230(8) . ?
C51 O51 1.269(7) . ?
O52 Na1 2.315(7) . ?
C60 C61 1.525(8) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.239(7) . ?
C61 O61 1.265(7) . ?
C70 C71 1.529(7) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.233(6) . ?
C71 O71 1.272(6) . ?
Na1 O2WA 2.303(9) . ?
Na1 O1W 2.311(7) . ?
Na1 O4W 2.402(10) . ?
Na1 O3W 2.481(13) . ?
Na1 O2WB 2.656(19) . ?
Na1 Na1 3.138(8) 2_655 ?
O3W Na1 2.481(13) 2_655 ?
O4W Na1 2.402(10) 2_655 ?

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
O71 Yb1 O11 78.83(12) . . ?
O71 Yb1 O51 127.71(13) . . ?
O11 Yb1 O51 76.40(14) . . ?
O71 Yb1 O61 78.03(13) . . ?
O11 Yb1 O61 121.71(13) . . ?
O51 Yb1 O61 77.18(14) . . ?
O71 Yb1 N4 155.93(14) . . ?
O11 Yb1 N4 88.10(14) . . ?
O51 Yb1 N4 66.98(14) . . ?
O61 Yb1 N4 125.96(14) . . ?
O71 Yb1 N7 124.56(13) . . ?
O11 Yb1 N7 156.54(14) . . ?
O51 Yb1 N7 85.97(14) . . ?
O61 Yb1 N7 67.72(14) . . ?
N4 Yb1 N7 70.61(15) . . ?
O71 Yb1 N10 66.89(13) . . ?
O11 Yb1 N10 128.70(14) . . ?
O51 Yb1 N10 154.86(14) . . ?
O61 Yb1 N10 87.92(14) . . ?
N4 Yb1 N10 108.09(14) . . ?
N7 Yb1 N10 69.56(15) . . ?
O71 Yb1 N1 86.42(13) . . ?
O11 Yb1 N1 71.22(13) . . ?
O51 Yb1 N1 126.24(14) . . ?
O61 Yb1 N1 156.54(14) . . ?
N4 Yb1 N1 70.16(14) . . ?
N7 Yb1 N1 108.79(14) . . ?
N10 Yb1 N1 69.72(14) . . ?
O71 Yb1 C51 135.71(15) . . ?
O11 Yb1 C51 65.54(16) . . ?
O51 Yb1 C51 21.34(16) . . ?
O61 Yb1 C51 98.47(16) . . ?
N4 Yb1 C51 50.89(16) . . ?
N7 Yb1 C51 92.63(17) . . ?
N10 Yb1 C51 157.29(15) . . ?
N1 Yb1 C51 104.92(16) . . ?
O71 Yb1 C71 20.89(13) . . ?
O11 Yb1 C71 99.72(13) . . ?
O51 Yb1 C71 134.87(14) . . ?
O61 Yb1 C71 66.86(13) . . ?
N4 Yb1 C71 157.90(14) . . ?
N7 Yb1 C71 103.70(14) . . ?
N10 Yb1 C71 51.23(13) . . ?
N1 Yb1 C71 92.67(13) . . ?
C51 Yb1 C71 150.80(15) . . ?
O71 Yb1 C61 96.92(14) . . ?
O11 Yb1 C61 133.00(15) . . ?
O51 Yb1 C61 69.71(16) . . ?
O61 Yb1 C61 19.95(15) . . ?
N4 Yb1 C61 106.71(16) . . ?
N7 Yb1 C61 50.09(16) . . ?
N10 Yb1 C61 89.46(16) . . ?
N1 Yb1 C61 155.76(16) . . ?
C51 Yb1 C61 89.44(18) . . ?
C71 Yb1 C61 83.06(15) . . ?
O71 Yb1 C50 145.90(14) . . ?
O11 Yb1 C50 67.22(14) . . ?
O51 Yb1 C50 47.87(14) . . ?
O61 Yb1 C50 122.34(15) . . ?
N4 Yb1 C50 26.66(14) . . ?
N7 Yb1 C50 89.49(15) . . ?
N10 Yb1 C50 133.93(13) . . ?
N1 Yb1 C50 79.97(14) . . ?
C51 Yb1 C50 27.67(16) . . ?
C71 Yb1 C50 166.46(15) . . ?
C61 Yb1 C50 108.25(16) . . ?
C12 N1 C20 110.2(4) . . ?
C12 N1 C2 109.8(4) . . ?
C20 N1 C2 108.9(4) . . ?
C12 N1 Yb1 110.8(3) . . ?
C20 N1 Yb1 107.4(3) . . ?
C2 N1 Yb1 109.6(3) . . ?
N1 C2 C3 112.0(4) . . ?
N1 C2 H21 109.2 . . ?
C3 C2 H21 109.2 . . ?
N1 C2 H22 109.2 . . ?
C3 C2 H22 109.2 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 111.5(4) . . ?
N4 C3 H31 109.3 . . ?
C2 C3 H31 109.3 . . ?
N4 C3 H32 109.3 . . ?
C2 C3 H32 109.3 . . ?
H31 C3 H32 108.0 . . ?
C3 N4 C5 109.3(4) . . ?
C3 N4 C50 111.3(4) . . ?
C5 N4 C50 107.9(4) . . ?
C3 N4 Yb1 113.1(3) . . ?
C5 N4 Yb1 110.9(3) . . ?
C50 N4 Yb1 104.1(3) . . ?
N4 C5 C6 112.3(5) . . ?
N4 C5 H51 109.1 . . ?
C6 C5 H51 109.1 . . ?
N4 C5 H52 109.1 . . ?
C6 C5 H52 109.1 . . ?
H51 C5 H52 107.9 . . ?
N7 C6 C5 111.1(5) . . ?
N7 C6 H61 109.4 . . ?
C5 C6 H61 109.4 . . ?
N7 C6 H62 109.4 . . ?
C5 C6 H62 109.4 . . ?
H61 C6 H62 108.0 . . ?
C60 N7 C6 112.1(4) . . ?
C60 N7 C8 107.5(4) . . ?
C6 N7 C8 109.5(4) . . ?
C60 N7 Yb1 104.3(3) . . ?
C6 N7 Yb1 111.7(3) . . ?
C8 N7 Yb1 111.6(3) . . ?
N7 C8 C9 111.9(4) . . ?
N7 C8 H81 109.2 . . ?
C9 C8 H81 109.2 . . ?
N7 C8 H82 109.2 . . ?
C9 C8 H82 109.2 . . ?
H81 C8 H82 107.9 . . ?
N10 C9 C8 110.8(4) . . ?
N10 C9 H91 109.5 . . ?
C8 C9 H91 109.5 . . ?
N10 C9 H92 109.5 . . ?
C8 C9 H92 109.5 . . ?
H91 C9 H92 108.1 . . ?
C9 N10 C11 110.0(4) . . ?
C9 N10 C70 110.7(4) . . ?
C11 N10 C70 108.0(4) . . ?
C9 N10 Yb1 113.3(3) . . ?
C11 N10 Yb1 110.7(3) . . ?
C70 N10 Yb1 103.8(3) . . ?
N10 C11 C12 111.4(4) . . ?
N10 C11 H111 109.3 . . ?
C12 C11 H111 109.3 . . ?
N10 C11 H112 109.3 . . ?
C12 C11 H112 109.3 . . ?
H111 C11 H112 108.0 . . ?
N1 C12 C11 111.0(4) . . ?
N1 C12 H121 109.4 . . ?
C11 C12 H121 109.4 . . ?
N1 C12 H122 109.4 . . ?
C11 C12 H122 109.4 . . ?
H121 C12 H122 108.0 . . ?
N1 C20 P1 110.5(3) . . ?
N1 C20 H201 109.6 . . ?
P1 C20 H201 109.6 . . ?
N1 C20 H202 109.6 . . ?
P1 C20 H202 109.6 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 116.4(2) . . ?
O12 P1 C21 111.2(2) . . ?
O11 P1 C21 108.6(2) . . ?
O12 P1 C20 111.5(2) . . ?
O11 P1 C20 104.7(2) . . ?
C21 P1 C20 103.4(3) . . ?
O12 P1 Yb1 135.00(16) . . ?
O11 P1 Yb1 32.40(13) . . ?
C21 P1 Yb1 110.87(19) . . ?
C20 P1 Yb1 72.81(17) . . ?
P1 O11 Yb1 126.3(2) . . ?
N22 C21 P1 109.9(4) . . ?
N22 C21 H211 109.7 . . ?
P1 C21 H211 109.7 . . ?
N22 C21 H212 109.7 . . ?
P1 C21 H212 109.7 . . ?
H211 C21 H212 108.2 . . ?
C40 N22 C30 110.6(5) . . ?
C40 N22 C21 111.7(4) . . ?
C30 N22 C21 111.6(4) . . ?
N22 C30 C31 112.6(5) . . ?
N22 C30 H301 109.1 . . ?
C31 C30 H301 109.1 . . ?
N22 C30 H302 109.1 . . ?
C31 C30 H302 109.1 . . ?
H301 C30 H302 107.8 . . ?
C32B C31 C36B 120.3(10) . . ?
C32A C31 C36A 117.1(10) . . ?
C32B C31 C30 126.5(9) . . ?
C32A C31 C30 119.4(8) . . ?
C36B C31 C30 112.8(7) . . ?
C36A C31 C30 123.4(7) . . ?
C31 C32A C33A 122.1(14) . . ?
C31 C32A H32A 119.0 . . ?
C33A C32A H32A 119.0 . . ?
C32A C33A C34 116.7(12) . . ?
C32A C33A H33A 121.7 . . ?
C34 C33A H33A 121.7 . . ?
C35A C34 C33A 121.5(12) . . ?
C33B C34 C35B 120.2(12) . . ?
C35A C34 H34 119.3 . . ?
C33A C34 H34 119.3 . . ?
C34 C35A C36A 120.4(16) . . ?
C34 C35A H35A 119.8 . . ?
C36A C35A H35A 119.8 . . ?
C35A C36A C31 119.7(14) . . ?
C35A C36A H36A 120.1 . . ?
C31 C36A H36A 120.1 . . ?
C31 C32B C33B 119.2(13) . . ?
C31 C32B H32B 120.4 . . ?
C33B C32B H32B 120.4 . . ?
C34 C33B C32B 124.0(13) . . ?
C34 C33B H33B 118.0 . . ?
C32B C33B H33B 118.0 . . ?
C36B C35B C34 115.8(13) . . ?
C36B C35B H35B 122.1 . . ?
C34 C35B H35B 122.1 . . ?
C31 C36B C35B 119.9(12) . . ?
C31 C36B H36B 120.0 . . ?
C35B C36B H36B 120.0 . . ?
C41A C40 N22 119.4(6) . . ?
N22 C40 C41B 104.3(7) . . ?
C41A C40 H401 107.5 . . ?
N22 C40 H401 107.5 . . ?
C41A C40 H402 107.5 . . ?
N22 C40 H402 107.5 . . ?
H401 C40 H402 107.0 . . ?
N22 C40 H403 110.9 . . ?
C41B C40 H403 110.9 . . ?
N22 C40 H404 110.9 . . ?
C41B C40 H404 110.9 . . ?
H403 C40 H404 108.9 . . ?
C42A C41A C46A 120.0 . . ?
C42A C41A C40 116.2(6) . . ?
C46A C41A C40 123.7(6) . . ?
C41A C42A C43A 120.0 . . ?
C41A C42A H42A 120.0 . . ?
C43A C42A H42A 120.0 . . ?
C44A C43A C42A 120.0 . . ?
C44A C43A H43A 120.0 . . ?
C42A C43A H43A 120.0 . . ?
C43A C44A C45A 120.0 . . ?
C43A C44A H44A 120.0 . . ?
C45A C44A H44A 120.0 . . ?
C46A C45A C44A 120.0 . . ?
C46A C45A H45A 120.0 . . ?
C44A C45A H45A 120.0 . . ?
C45A C46A C41A 120.0 . . ?
C45A C46A H46A 120.0 . . ?
C41A C46A H46A 120.0 . . ?
C42B C41B C46B 120.0 . . ?
C42B C41B C40 122.1(8) . . ?
C46B C41B C40 117.8(8) . . ?
C41B C42B C43B 120.0 . . ?
C41B C42B H42B 120.0 . . ?
C43B C42B H42B 120.0 . . ?
C44B C43B C42B 120.0 . . ?
C44B C43B H43B 120.0 . . ?
C42B C43B H43B 120.0 . . ?
C43B C44B C45B 120.0 . . ?
C43B C44B H44B 120.0 . . ?
C45B C44B H44B 120.0 . . ?
C44B C45B C46B 120.0 . . ?
C44B C45B H45B 120.0 . . ?
C46B C45B H45B 120.0 . . ?
C45B C46B C41B 120.0 . . ?
C45B C46B H46B 120.0 . . ?
C41B C46B H46B 120.0 . . ?
N4 C50 C51 110.2(5) . . ?
N4 C50 Yb1 49.2(2) . . ?
C51 C50 Yb1 71.4(3) . . ?
N4 C50 H501 109.6 . . ?
C51 C50 H501 109.6 . . ?
Yb1 C50 H501 96.0 . . ?
N4 C50 H502 109.6 . . ?
C51 C50 H502 109.6 . . ?
Yb1 C50 H502 153.2 . . ?
H501 C50 H502 108.1 . . ?
O52 C51 O51 124.0(6) . . ?
O52 C51 C50 118.2(6) . . ?
O51 C51 C50 117.8(5) . . ?
O52 C51 Yb1 154.5(5) . . ?
O51 C51 Yb1 40.6(3) . . ?
C50 C51 Yb1 80.9(3) . . ?
C51 O51 Yb1 118.1(4) . . ?
C51 O52 Na1 136.6(5) . . ?
N7 C60 C61 110.6(5) . . ?
N7 C60 H601 109.5 . . ?
C61 C60 H601 109.5 . . ?
N7 C60 H602 109.5 . . ?
C61 C60 H602 109.5 . . ?
H601 C60 H602 108.1 . . ?
O62 C61 O61 124.1(6) . . ?
O62 C61 C60 118.8(6) . . ?
O61 C61 C60 117.1(5) . . ?
O62 C61 Yb1 160.7(5) . . ?
O61 C61 Yb1 38.1(3) . . ?
C60 C61 Yb1 79.5(3) . . ?
C61 O61 Yb1 122.0(4) . . ?
N10 C70 C71 111.0(4) . . ?
N10 C70 H701 109.4 . . ?
C71 C70 H701 109.4 . . ?
N10 C70 H702 109.4 . . ?
C71 C70 H702 109.4 . . ?
H701 C70 H702 108.0 . . ?
O72 C71 O71 125.3(5) . . ?
O72 C71 C70 118.3(5) . . ?
O71 C71 C70 116.4(4) . . ?
O72 C71 Yb1 152.7(4) . . ?
O71 C71 Yb1 39.0(2) . . ?
C70 C71 Yb1 81.4(3) . . ?
C71 O71 Yb1 120.1(3) . . ?
O2WA Na1 O1W 150.2(4) . . ?
O2WA Na1 O52 76.9(3) . . ?
O1W Na1 O52 102.1(3) . . ?
O2WA Na1 O4W 88.0(3) . . ?
O1W Na1 O4W 89.95(19) . . ?
O52 Na1 O4W 164.8(3) . . ?
O2WA Na1 O3W 105.4(3) . . ?
O1W Na1 O3W 104.2(2) . . ?
O52 Na1 O3W 86.3(3) . . ?
O4W Na1 O3W 100.0(3) . . ?
O1W Na1 O2WB 155.7(4) . . ?
O52 Na1 O2WB 56.1(4) . . ?
O4W Na1 O2WB 110.1(4) . . ?
O3W Na1 O2WB 86.1(5) . . ?
O2WA Na1 Na1 100.2(3) . 2_655 ?
O1W Na1 Na1 100.8(2) . 2_655 ?
O52 Na1 Na1 135.1(2) . 2_655 ?
O4W Na1 Na1 49.2(2) . 2_655 ?
O3W Na1 Na1 50.8(3) . 2_655 ?
O2WB Na1 Na1 102.7(4) . 2_655 ?
Na1 O3W Na1 78.5(5) . 2_655 ?
Na1 O4W Na1 81.6(4) . 2_655 ?

_refine_diff_density_max         1.497
_refine_diff_density_min         -1.411
_refine_diff_density_rms         0.137

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

data_nd_dbamh
_database_code_depnum_ccdc_archive 'CCDC 1959632'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H44 N5 Nd O8 P, 3(H2 O)'
_chemical_formula_sum            'C30 H47 N5 Nd O11 P'
_chemical_formula_weight         828.93

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'
Nd Nd -0.1943 3.0179 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   10.5893(5)
_cell_length_b                   12.4277(6)
_cell_length_c                   14.6008(8)
_cell_angle_alpha                112.071(2)
_cell_angle_beta                 92.429(2)
_cell_angle_gamma                109.292(2)
_cell_volume                     1649.94(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9921
_cell_measurement_theta_min      2.2324
_cell_measurement_theta_max      27.1533

_exptl_crystal_description       bar
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_F_000             850
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.032
_exptl_absorpt_coefficient_mu    1.690
_shelx_estimated_absorpt_T_min   0.663
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            7581
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.232
_diffrn_reflns_theta_max         27.566
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7581
_reflns_number_gt                6521
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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 Instrument Service v6.2.6'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0147P)²+5.0899P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7581
_refine_ls_number_parameters     446
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.0798
_refine_ls_wR_factor_gt          0.0742
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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
Nd1 Nd 0.42573(2) 0.93978(2) 0.66449(2) 0.01026(6) Uani 1 1 d . . . . .
N1 N 0.1773(4) 0.7393(3) 0.5965(3) 0.0135(7) Uani 1 1 d . . . . .
C2 C 0.1613(4) 0.6685(4) 0.6603(3) 0.0157(9) Uani 1 1 d . . . . .
H21 H 0.2226 0.6212 0.6460 0.019 Uiso 1 1 calc R U . . .
H22 H 0.0665 0.6071 0.6421 0.019 Uiso 1 1 calc R U . . .
C3 C 0.1928(4) 0.7513(4) 0.7711(3) 0.0160(9) Uani 1 1 d . . . . .
H31 H 0.1261 0.7927 0.7867 0.019 Uiso 1 1 calc R U . . .
H32 H 0.1829 0.6991 0.8096 0.019 Uiso 1 1 calc R U . . .
N4 N 0.3326(3) 0.8482(3) 0.8036(3) 0.0138(8) Uani 1 1 d . . . . .
C5 C 0.3403(4) 0.9506(4) 0.8999(3) 0.0154(9) Uani 1 1 d . . . . .
H51 H 0.4368 0.9969 0.9347 0.018 Uiso 1 1 calc R U . . .
H52 H 0.2895 0.9142 0.9433 0.018 Uiso 1 1 calc R U . . .
C6 C 0.2833(4) 1.0406(4) 0.8864(3) 0.0163(9) Uani 1 1 d . . . . .
H61 H 0.1857 0.9955 0.8544 0.020 Uiso 1 1 calc R U . . .
H62 H 0.2900 1.1064 0.9532 0.020 Uiso 1 1 calc R U . . .
N7 N 0.3573(4) 1.0999(3) 0.8234(3) 0.0141(8) Uani 1 1 d . . . . .
C8 C 0.2782(4) 1.1616(4) 0.7899(3) 0.0166(9) Uani 1 1 d . . . . .
H81 H 0.3398 1.2240 0.7690 0.020 Uiso 1 1 calc R U . . .
H82 H 0.2420 1.2069 0.8472 0.020 Uiso 1 1 calc R U . . .
C9 C 0.1611(4) 1.0697(4) 0.7034(3) 0.0162(9) Uani 1 1 d . . . . .
H91 H 0.0940 1.0133 0.7265 0.019 Uiso 1 1 calc R U . . .
H92 H 0.1151 1.1162 0.6818 0.019 Uiso 1 1 calc R U . . .
N10 N 0.2068(3) 0.9936(3) 0.6162(3) 0.0131(7) Uani 1 1 d . . . . .
C11 C 0.0878(4) 0.8781(4) 0.5519(3) 0.0168(9) Uani 1 1 d . . . . .
H111 H 0.1056 0.8444 0.4828 0.020 Uiso 1 1 calc R U . . .
H112 H 0.0061 0.8995 0.5483 0.020 Uiso 1 1 calc R U . . .
C12 C 0.0601(4) 0.7788(4) 0.5927(3) 0.0181(10) Uani 1 1 d . . . . .
H121 H 0.0404 0.8120 0.6613 0.022 Uiso 1 1 calc R U . . .
H122 H -0.0215 0.7051 0.5495 0.022 Uiso 1 1 calc R U . . .
C20 C 0.1793(4) 0.6558(4) 0.4938(3) 0.0176(9) Uani 1 1 d . . . . .
H201 H 0.1726 0.6954 0.4472 0.021 Uiso 1 1 calc R U . . .
H202 H 0.0995 0.5761 0.4710 0.021 Uiso 1 1 calc R U . . .
P1 P 0.33677(11) 0.62337(11) 0.49023(8) 0.0144(2) Uani 1 1 d . . . . .
O11 O 0.4386(3) 0.7341(3) 0.5785(2) 0.0145(6) Uani 1 1 d . . . . .
O12 O 0.3114(3) 0.4945(3) 0.4816(2) 0.0221(7) Uani 1 1 d . . . . .
C21 C 0.3954(4) 0.6411(4) 0.3789(3) 0.0163(9) Uani 1 1 d . . . . .
H211 H 0.3766 0.7119 0.3739 0.020 Uiso 1 1 calc R U . . .
H212 H 0.4955 0.6652 0.3901 0.020 Uiso 1 1 calc R U . . .
N22 N 0.3353(3) 0.5294(3) 0.2782(3) 0.0166(7) Uani 1 1 d . . . . .
H221 H 0.3468 0.5629 0.2253 0.020 Uiso 1 1 calc R U . . .
C30 C 0.4129(5) 0.4428(4) 0.2587(3) 0.0192(10) Uani 1 1 d . . . . .
H301 H 0.4264 0.4269 0.3192 0.023 Uiso 1 1 calc R U . . .
H302 H 0.3579 0.3616 0.2024 0.023 Uiso 1 1 calc R U . . .
C31 C 0.5499(4) 0.4958(4) 0.2330(3) 0.0157(8) Uani 1 1 d . . . . .
C32 C 0.6693(5) 0.5549(4) 0.3051(3) 0.0213(10) Uani 1 1 d . . . . .
H321 H 0.6651 0.5654 0.3727 0.026 Uiso 1 1 calc R U . . .
C33 C 0.7946(5) 0.5983(5) 0.2786(4) 0.0257(10) Uani 1 1 d . . . . .
H331 H 0.8757 0.6395 0.3282 0.031 Uiso 1 1 calc R U . . .
C34 C 0.8013(5) 0.5819(4) 0.1806(4) 0.0263(11) Uani 1 1 d . . . . .
H341 H 0.8872 0.6113 0.1627 0.032 Uiso 1 1 calc R U . . .
C35 C 0.6837(5) 0.5227(4) 0.1082(4) 0.0222(11) Uani 1 1 d . . . . .
H351 H 0.6887 0.5102 0.0404 0.027 Uiso 1 1 calc R U . . .
C36 C 0.5582(4) 0.4817(4) 0.1351(3) 0.0181(9) Uani 1 1 d . . . . .
H361 H 0.4772 0.4435 0.0857 0.022 Uiso 1 1 calc R U . . .
C40 C 0.1840(4) 0.4599(4) 0.2661(3) 0.0229(10) Uani 1 1 d . . . . .
H401 H 0.1710 0.4060 0.3033 0.027 Uiso 1 1 calc R U . . .
H402 H 0.1418 0.5217 0.2975 0.027 Uiso 1 1 calc R U . . .
C41 C 0.1100(4) 0.3793(4) 0.1583(4) 0.0227(11) Uani 1 1 d . . . . .
C42 C 0.0947(5) 0.2548(5) 0.1106(4) 0.0363(13) Uani 1 1 d . . . . .
H421 H 0.1389 0.2197 0.1430 0.044 Uiso 1 1 calc R U . . .
C43 C 0.0133(6) 0.1809(6) 0.0142(5) 0.0490(19) Uani 1 1 d . . . . .
H431 H 0.0043 0.0960 -0.0191 0.059 Uiso 1 1 calc R U . . .
C44 C -0.0533(6) 0.2297(7) -0.0328(4) 0.0501(17) Uani 1 1 d . . . . .
H441 H -0.1101 0.1784 -0.0973 0.060 Uiso 1 1 calc R U . . .
C45 C -0.0369(6) 0.3531(6) 0.0145(5) 0.0471(17) Uani 1 1 d . . . . .
H451 H -0.0820 0.3878 -0.0175 0.056 Uiso 1 1 calc R U . . .
C46 C 0.0455(5) 0.4277(5) 0.1091(4) 0.0323(12) Uani 1 1 d . . . . .
H461 H 0.0576 0.5136 0.1404 0.039 Uiso 1 1 calc R U . . .
C50 C 0.4329(4) 0.7946(4) 0.8182(3) 0.0173(9) Uani 1 1 d . . . . .
H501 H 0.4132 0.7138 0.7600 0.021 Uiso 1 1 calc R U . . .
H502 H 0.4238 0.7778 0.8793 0.021 Uiso 1 1 calc R U . . .
C51 C 0.5792(5) 0.8820(4) 0.8293(3) 0.0173(9) Uani 1 1 d . . . . .
O51 O 0.5929(3) 0.9635(3) 0.7931(2) 0.0174(7) Uani 1 1 d . . . . .
O52 O 0.6726(3) 0.8662(3) 0.8687(2) 0.0217(7) Uani 1 1 d . . . . .
C60 C 0.4907(4) 1.1978(4) 0.8833(3) 0.0176(9) Uani 1 1 d . . . . .
H601 H 0.5409 1.1625 0.9152 0.021 Uiso 1 1 calc R U . . .
H602 H 0.4764 1.2677 0.9371 0.021 Uiso 1 1 calc R U . . .
C61 C 0.5724(4) 1.2451(4) 0.8145(3) 0.0149(9) Uani 1 1 d . . . . .
O61 O 0.5586(3) 1.1660(3) 0.7256(2) 0.0174(6) Uani 1 1 d . . . . .
O62 O 0.6468(3) 1.3585(3) 0.8488(2) 0.0221(7) Uani 1 1 d . . . . .
C70 C 0.2611(4) 1.0635(4) 0.5552(3) 0.0163(8) Uani 1 1 d . . . . .
H701 H 0.3231 1.1497 0.6001 0.020 Uiso 1 1 calc R U . . .
H702 H 0.1849 1.0690 0.5178 0.020 Uiso 1 1 calc R U . . .
C71 C 0.3382(4) 0.9999(4) 0.4808(3) 0.0138(9) Uani 1 1 d . . . . .
O71 O 0.3667(3) 0.9144(3) 0.4932(2) 0.0130(6) Uani 1 1 d . . . . .
O72 O 0.3694(3) 1.0378(3) 0.4135(2) 0.0155(6) Uani 1 1 d . . . . .
O1W O 0.2699(3) 0.2453(3) 0.4273(2) 0.0270(8) Uani 1 1 d . . . . .
H11W H 0.2838 0.3141 0.4324 0.032 Uiso 1 1 d R U . . .
H12W H 0.3389 0.2196 0.4122 0.032 Uiso 1 1 d R U . . .
O2WA O 0.1116(8) 0.0811(11) 0.2342(7) 0.053(3) Uani 0.600(13) 1 d . . P A 1
O2WB O 0.1318(14) 0.0293(18) 0.2525(11) 0.053(3) Uani 0.400(13) 1 d . . P A 2
O3WA O 0.1357(6) -0.2025(7) 0.2806(5) 0.0284(16) Uani 0.55 1 d . U P B 3
O3WB O 0.1448(16) -0.2618(15) 0.2858(12) 0.043(4) Uiso 0.3 1 d . . P C 4
O3WC O 0.122(2) -0.079(2) 0.2968(15) 0.023(4) Uiso 0.15 1 d . . P D 5


_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
Nd1 O51 2.388(3) . ?
Nd1 O71 2.427(3) . ?
Nd1 O11 2.442(3) . ?
Nd1 O61 2.465(3) . ?
Nd1 O72 2.476(3) 2_676 ?
Nd1 N7 2.738(3) . ?
Nd1 N10 2.749(3) . ?
Nd1 N4 2.749(4) . ?
Nd1 N1 2.775(3) . ?
N1 C20 1.474(5) . ?
N1 C12 1.484(5) . ?
N1 C2 1.484(5) . ?
C2 C3 1.505(6) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.484(5) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.474(5) . ?
N4 C5 1.477(5) . ?
C5 C6 1.503(6) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.481(5) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.483(5) . ?
N7 C8 1.483(5) . ?
C8 C9 1.512(6) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.483(5) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.475(5) . ?
N10 C11 1.490(5) . ?
C11 C12 1.514(6) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.839(4) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.488(3) . ?
P1 O11 1.512(3) . ?
P1 C21 1.828(4) . ?
C21 N22 1.515(5) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C30 1.512(5) . ?
N22 C40 1.514(5) . ?
N22 H221 1.0000 . ?
C30 C31 1.510(6) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36 1.384(6) . ?
C31 C32 1.393(6) . ?
C32 C33 1.388(6) . ?
C32 H321 0.9500 . ?
C33 C34 1.375(7) . ?
C33 H331 0.9500 . ?
C34 C35 1.381(7) . ?
C34 H341 0.9500 . ?
C35 C36 1.388(6) . ?
C35 H351 0.9500 . ?
C36 H361 0.9500 . ?
C40 C41 1.512(6) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C41 C46 1.379(7) . ?
C41 C42 1.386(7) . ?
C42 C43 1.404(8) . ?
C42 H421 0.9500 . ?
C43 C44 1.375(10) . ?
C43 H431 0.9500 . ?
C44 C45 1.370(9) . ?
C44 H441 0.9500 . ?
C45 C46 1.389(8) . ?
C45 H451 0.9500 . ?
C46 H461 0.9500 . ?
C50 C51 1.531(6) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.229(5) . ?
C51 O51 1.280(5) . ?
C60 C61 1.511(6) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.249(5) . ?
C61 O61 1.266(5) . ?
C70 C71 1.525(6) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.253(5) . ?
C71 O71 1.266(5) . ?
O72 Nd1 2.476(3) 2_676 ?
O1W H11W 0.7924 . ?
O1W H12W 0.8936 . ?

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
O51 Nd1 O71 147.96(10) . . ?
O51 Nd1 O11 83.71(10) . . ?
O71 Nd1 O11 82.47(10) . . ?
O51 Nd1 O61 80.71(10) . . ?
O71 Nd1 O61 93.34(10) . . ?
O11 Nd1 O61 142.91(10) . . ?
O51 Nd1 O72 77.76(10) . 2_676 ?
O71 Nd1 O72 70.42(9) . 2_676 ?
O11 Nd1 O72 70.75(10) . 2_676 ?
O61 Nd1 O72 73.14(10) . 2_676 ?
O51 Nd1 N7 83.07(10) . . ?
O71 Nd1 N7 121.91(10) . . ?
O11 Nd1 N7 148.27(10) . . ?
O61 Nd1 N7 62.02(10) . . ?
O72 Nd1 N7 133.42(10) 2_676 . ?
O51 Nd1 N10 147.74(10) . . ?
O71 Nd1 N10 61.55(10) . . ?
O11 Nd1 N10 122.52(10) . . ?
O61 Nd1 N10 85.92(10) . . ?
O72 Nd1 N10 125.94(10) 2_676 . ?
N7 Nd1 N10 64.76(11) . . ?
O51 Nd1 N4 62.82(10) . . ?
O71 Nd1 N4 142.91(10) . . ?
O11 Nd1 N4 83.21(10) . . ?
O61 Nd1 N4 117.97(10) . . ?
O72 Nd1 N4 134.79(10) 2_676 . ?
N7 Nd1 N4 65.09(10) . . ?
N10 Nd1 N4 99.16(10) . . ?
O51 Nd1 N1 120.76(10) . . ?
O71 Nd1 N1 78.35(10) . . ?
O11 Nd1 N1 64.81(10) . . ?
O61 Nd1 N1 150.39(10) . . ?
O72 Nd1 N1 128.11(10) 2_676 . ?
N7 Nd1 N1 98.18(10) . . ?
N10 Nd1 N1 65.04(11) . . ?
N4 Nd1 N1 64.60(10) . . ?
C20 N1 C12 108.8(3) . . ?
C20 N1 C2 108.2(3) . . ?
C12 N1 C2 109.8(3) . . ?
C20 N1 Nd1 106.8(2) . . ?
C12 N1 Nd1 112.5(2) . . ?
C2 N1 Nd1 110.6(2) . . ?
N1 C2 C3 113.0(3) . . ?
N1 C2 H21 109.0 . . ?
C3 C2 H21 109.0 . . ?
N1 C2 H22 109.0 . . ?
C3 C2 H22 109.0 . . ?
H21 C2 H22 107.8 . . ?
N4 C3 C2 112.1(3) . . ?
N4 C3 H31 109.2 . . ?
C2 C3 H31 109.2 . . ?
N4 C3 H32 109.2 . . ?
C2 C3 H32 109.2 . . ?
H31 C3 H32 107.9 . . ?
C50 N4 C5 108.9(3) . . ?
C50 N4 C3 110.4(3) . . ?
C5 N4 C3 109.0(3) . . ?
C50 N4 Nd1 102.0(2) . . ?
C5 N4 Nd1 111.0(2) . . ?
C3 N4 Nd1 115.3(3) . . ?
N4 C5 C6 112.8(3) . . ?
N4 C5 H51 109.0 . . ?
C6 C5 H51 109.0 . . ?
N4 C5 H52 109.0 . . ?
C6 C5 H52 109.0 . . ?
H51 C5 H52 107.8 . . ?
N7 C6 C5 111.5(3) . . ?
N7 C6 H61 109.3 . . ?
C5 C6 H61 109.3 . . ?
N7 C6 H62 109.3 . . ?
C5 C6 H62 109.3 . . ?
H61 C6 H62 108.0 . . ?
C6 N7 C60 109.8(3) . . ?
C6 N7 C8 109.9(3) . . ?
C60 N7 C8 107.7(3) . . ?
C6 N7 Nd1 113.8(2) . . ?
C60 N7 Nd1 103.7(2) . . ?
C8 N7 Nd1 111.6(2) . . ?
N7 C8 C9 112.6(3) . . ?
N7 C8 H81 109.1 . . ?
C9 C8 H81 109.1 . . ?
N7 C8 H82 109.1 . . ?
C9 C8 H82 109.1 . . ?
H81 C8 H82 107.8 . . ?
N10 C9 C8 112.2(3) . . ?
N10 C9 H91 109.2 . . ?
C8 C9 H91 109.2 . . ?
N10 C9 H92 109.2 . . ?
C8 C9 H92 109.2 . . ?
H91 C9 H92 107.9 . . ?
C70 N10 C9 110.9(3) . . ?
C70 N10 C11 108.5(3) . . ?
C9 N10 C11 108.7(3) . . ?
C70 N10 Nd1 101.4(2) . . ?
C9 N10 Nd1 115.1(2) . . ?
C11 N10 Nd1 111.9(2) . . ?
N10 C11 C12 111.7(3) . . ?
N10 C11 H111 109.3 . . ?
C12 C11 H111 109.3 . . ?
N10 C11 H112 109.3 . . ?
C12 C11 H112 109.3 . . ?
H111 C11 H112 107.9 . . ?
N1 C12 C11 111.9(3) . . ?
N1 C12 H121 109.2 . . ?
C11 C12 H121 109.2 . . ?
N1 C12 H122 109.2 . . ?
C11 C12 H122 109.2 . . ?
H121 C12 H122 107.9 . . ?
N1 C20 P1 110.8(3) . . ?
N1 C20 H201 109.5 . . ?
P1 C20 H201 109.5 . . ?
N1 C20 H202 109.5 . . ?
P1 C20 H202 109.5 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 119.31(19) . . ?
O12 P1 C21 110.47(19) . . ?
O11 P1 C21 104.87(18) . . ?
O12 P1 C20 111.6(2) . . ?
O11 P1 C20 104.51(18) . . ?
C21 P1 C20 104.9(2) . . ?
P1 O11 Nd1 126.61(16) . . ?
N22 C21 P1 117.7(3) . . ?
N22 C21 H211 107.9 . . ?
P1 C21 H211 107.9 . . ?
N22 C21 H212 107.9 . . ?
P1 C21 H212 107.9 . . ?
H211 C21 H212 107.2 . . ?
C30 N22 C40 111.7(3) . . ?
C30 N22 C21 111.6(3) . . ?
C40 N22 C21 112.7(3) . . ?
C30 N22 H221 106.8 . . ?
C40 N22 H221 106.8 . . ?
C21 N22 H221 106.8 . . ?
C31 C30 N22 112.5(3) . . ?
C31 C30 H301 109.1 . . ?
N22 C30 H301 109.1 . . ?
C31 C30 H302 109.1 . . ?
N22 C30 H302 109.1 . . ?
H301 C30 H302 107.8 . . ?
C36 C31 C32 119.0(4) . . ?
C36 C31 C30 119.6(4) . . ?
C32 C31 C30 121.4(4) . . ?
C33 C32 C31 120.2(4) . . ?
C33 C32 H321 119.9 . . ?
C31 C32 H321 119.9 . . ?
C34 C33 C32 120.1(4) . . ?
C34 C33 H331 119.9 . . ?
C32 C33 H331 119.9 . . ?
C33 C34 C35 120.3(4) . . ?
C33 C34 H341 119.9 . . ?
C35 C34 H341 119.9 . . ?
C34 C35 C36 119.7(4) . . ?
C34 C35 H351 120.2 . . ?
C36 C35 H351 120.2 . . ?
C31 C36 C35 120.7(4) . . ?
C31 C36 H361 119.6 . . ?
C35 C36 H361 119.6 . . ?
C41 C40 N22 114.6(3) . . ?
C41 C40 H401 108.6 . . ?
N22 C40 H401 108.6 . . ?
C41 C40 H402 108.6 . . ?
N22 C40 H402 108.6 . . ?
H401 C40 H402 107.6 . . ?
C46 C41 C42 118.9(5) . . ?
C46 C41 C40 119.0(4) . . ?
C42 C41 C40 121.9(5) . . ?
C41 C42 C43 119.5(6) . . ?
C41 C42 H421 120.3 . . ?
C43 C42 H421 120.3 . . ?
C44 C43 C42 121.0(6) . . ?
C44 C43 H431 119.5 . . ?
C42 C43 H431 119.5 . . ?
C45 C44 C43 119.2(6) . . ?
C45 C44 H441 120.4 . . ?
C43 C44 H441 120.4 . . ?
C44 C45 C46 120.4(6) . . ?
C44 C45 H451 119.8 . . ?
C46 C45 H451 119.8 . . ?
C41 C46 C45 121.1(5) . . ?
C41 C46 H461 119.4 . . ?
C45 C46 H461 119.4 . . ?
N4 C50 C51 112.1(4) . . ?
N4 C50 H501 109.2 . . ?
C51 C50 H501 109.2 . . ?
N4 C50 H502 109.2 . . ?
C51 C50 H502 109.2 . . ?
H501 C50 H502 107.9 . . ?
O52 C51 O51 125.8(4) . . ?
O52 C51 C50 118.2(4) . . ?
O51 C51 C50 115.9(4) . . ?
C51 O51 Nd1 123.2(3) . . ?
N7 C60 C61 109.0(3) . . ?
N7 C60 H601 109.9 . . ?
C61 C60 H601 109.9 . . ?
N7 C60 H602 109.9 . . ?
C61 C60 H602 109.9 . . ?
H601 C60 H602 108.3 . . ?
O62 C61 O61 125.0(4) . . ?
O62 C61 C60 118.1(4) . . ?
O61 C61 C60 116.9(4) . . ?
C61 O61 Nd1 124.1(3) . . ?
N10 C70 C71 111.2(4) . . ?
N10 C70 H701 109.4 . . ?
C71 C70 H701 109.4 . . ?
N10 C70 H702 109.4 . . ?
C71 C70 H702 109.4 . . ?
H701 C70 H702 108.0 . . ?
O72 C71 O71 125.6(4) . . ?
O72 C71 C70 117.2(4) . . ?
O71 C71 C70 117.2(4) . . ?
C71 O71 Nd1 117.8(3) . . ?
C71 O72 Nd1 130.4(3) . 2_676 ?
H11W O1W H12W 114.5 . . ?

_refine_diff_density_max         1.285
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.163

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

data_scdbamoh
_database_code_depnum_ccdc_archive 'CCDC 1959635'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H40 N5 O8 P Sc, 4(H2 O), H4 N'
_chemical_formula_sum            'C30 H52 N6 O12 P Sc'
_chemical_formula_weight         764.70

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'
Sc Sc 0.2519 0.3716 '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                   24.0303(16)
_cell_length_b                   10.3449(6)
_cell_length_c                   15.1430(11)
_cell_angle_alpha                90
_cell_angle_beta                 107.497(3)
_cell_angle_gamma                90
_cell_volume                     3590.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9387
_cell_measurement_theta_min      2.4218
_cell_measurement_theta_max      27.5248

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_F_000             1624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.092
_exptl_absorpt_coefficient_mu    0.318
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            98010
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.160
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8266
_reflns_number_gt                7311
_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.
 
 _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 Instrument Service v6.2.9'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0492P)²+3.3755P] 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         8266
_refine_ls_number_parameters     492
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0389
_refine_ls_wR_factor_ref         0.1028
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Sc1 Sc 0.31993(2) 0.55765(3) 0.31925(2) 0.00884(8) Uani 1 1 d . . . . .
N1 N 0.23178(6) 0.51937(13) 0.37487(9) 0.0129(3) Uani 1 1 d . . . . .
C2 C 0.25107(7) 0.46479(16) 0.47042(11) 0.0154(3) Uani 1 1 d . . . . .
H21 H 0.2584 0.3710 0.4671 0.019 Uiso 1 1 calc R U . . .
H22 H 0.2195 0.4759 0.4994 0.019 Uiso 1 1 calc R U . . .
C3 C 0.30586(7) 0.52985(16) 0.53001(11) 0.0155(3) Uani 1 1 d . . . . .
H31 H 0.2974 0.6217 0.5392 0.019 Uiso 1 1 calc R U . . .
H32 H 0.3186 0.4876 0.5915 0.019 Uiso 1 1 calc R U . . .
N4 N 0.35315(6) 0.52200(13) 0.48634(9) 0.0134(3) Uani 1 1 d . . . . .
C5 C 0.40010(7) 0.61636(16) 0.53362(11) 0.0174(3) Uani 1 1 d . . . . .
H51 H 0.4374 0.5895 0.5240 0.021 Uiso 1 1 calc R U . . .
H52 H 0.4054 0.6156 0.6010 0.021 Uiso 1 1 calc R U . . .
C6 C 0.38523(8) 0.75153(17) 0.49688(11) 0.0188(3) Uani 1 1 d . . . . .
H61 H 0.3505 0.7829 0.5128 0.023 Uiso 1 1 calc R U . . .
H62 H 0.4182 0.8104 0.5256 0.023 Uiso 1 1 calc R U . . .
N7 N 0.37315(6) 0.75131(13) 0.39464(9) 0.0145(3) Uani 1 1 d . . . . .
C8 C 0.34207(8) 0.87248(15) 0.35428(12) 0.0181(3) Uani 1 1 d . . . . .
H81 H 0.3493 0.8909 0.2945 0.022 Uiso 1 1 calc R U . . .
H82 H 0.3577 0.9456 0.3966 0.022 Uiso 1 1 calc R U . . .
C9 C 0.27728(8) 0.86109(15) 0.33893(12) 0.0173(3) Uani 1 1 d . . . . .
H91 H 0.2696 0.8519 0.3993 0.021 Uiso 1 1 calc R U . . .
H92 H 0.2575 0.9404 0.3085 0.021 Uiso 1 1 calc R U . . .
N10 N 0.25392(6) 0.74745(13) 0.28013(9) 0.0135(3) Uani 1 1 d . . . . .
C11 C 0.19480(7) 0.71532(16) 0.28610(12) 0.0166(3) Uani 1 1 d . . . . .
H111 H 0.1736 0.6632 0.2316 0.020 Uiso 1 1 calc R U . . .
H112 H 0.1726 0.7961 0.2855 0.020 Uiso 1 1 calc R U . . .
C12 C 0.19885(7) 0.64024(15) 0.37382(12) 0.0157(3) Uani 1 1 d . . . . .
H121 H 0.2188 0.6933 0.4286 0.019 Uiso 1 1 calc R U . . .
H122 H 0.1592 0.6197 0.3766 0.019 Uiso 1 1 calc R U . . .
C20 C 0.19415(7) 0.42230(15) 0.31233(11) 0.0134(3) Uani 1 1 d . . . . .
H201 H 0.1728 0.4635 0.2527 0.016 Uiso 1 1 calc R U . . .
H202 H 0.1651 0.3878 0.3408 0.016 Uiso 1 1 calc R U . . .
P1 P 0.23960(2) 0.29098(4) 0.29221(3) 0.01131(9) Uani 1 1 d . . . . .
O11 O 0.29936(5) 0.35406(10) 0.30727(7) 0.0121(2) Uani 1 1 d . . . . .
O12 O 0.23731(5) 0.17672(11) 0.35139(8) 0.0183(2) Uani 1 1 d . . . . .
C21 C 0.20858(7) 0.25273(15) 0.17043(11) 0.0147(3) Uani 1 1 d . . . . .
H211 H 0.2122 0.3286 0.1327 0.018 Uiso 1 1 calc R U . . .
H212 H 0.2306 0.1803 0.1541 0.018 Uiso 1 1 calc R U . . .
N23 N 0.14670(6) 0.21668(13) 0.14898(10) 0.0154(3) Uani 1 1 d . . . . .
C30 C 0.14038(7) 0.08139(16) 0.17262(13) 0.0193(3) Uani 1 1 d . . . . .
H301 H 0.1679 0.0631 0.2346 0.023 Uiso 1 1 calc R U . . .
H302 H 0.1510 0.0251 0.1273 0.023 Uiso 1 1 calc R U . . .
C31 C 0.07902(7) 0.04863(16) 0.17315(12) 0.0188(3) Uani 1 1 d . . . . .
C32 C 0.05515(8) -0.07132(17) 0.14137(14) 0.0245(4) Uani 1 1 d . . . . .
H321 H 0.0766 -0.1305 0.1163 0.029 Uiso 1 1 calc R U . . .
C33 C 0.00001(8) -0.1052(2) 0.14602(15) 0.0314(5) Uani 1 1 d . . . . .
H331 H -0.0158 -0.1878 0.1251 0.038 Uiso 1 1 calc R U . . .
C34 C -0.03170(9) -0.0188(2) 0.18105(16) 0.0341(5) Uani 1 1 d . . . . .
H341 H -0.0693 -0.0421 0.1844 0.041 Uiso 1 1 calc R U . . .
C35 C -0.00885(9) 0.1013(2) 0.21122(16) 0.0328(4) Uani 1 1 d . . . . .
H351 H -0.0310 0.1615 0.2341 0.039 Uiso 1 1 calc R U . . .
C36 C 0.04657(8) 0.13451(18) 0.20809(14) 0.0254(4) Uani 1 1 d . . . . .
H361 H 0.0624 0.2167 0.2301 0.030 Uiso 1 1 calc R U . . .
C40 C 0.11531(8) 0.24029(17) 0.05097(12) 0.0201(3) Uani 1 1 d . . . . .
H401 H 0.0770 0.1963 0.0351 0.024 Uiso 1 1 calc R U . . .
H402 H 0.1378 0.2022 0.0123 0.024 Uiso 1 1 calc R U . . .
C41 C 0.10581(7) 0.38187(17) 0.02845(12) 0.0196(3) Uani 1 1 d . . . . .
C42 C 0.12185(10) 0.4371(2) -0.04394(15) 0.0330(5) Uani 1 1 d . . . . .
H421 H 0.1414 0.3867 -0.0779 0.040 Uiso 1 1 calc R U . . .
C43 C 0.10926(12) 0.5665(2) -0.06669(17) 0.0460(6) Uani 1 1 d . . . . .
H431 H 0.1198 0.6032 -0.1169 0.055 Uiso 1 1 calc R U . . .
C44 C 0.08188(11) 0.6417(2) -0.01770(16) 0.0395(5) Uani 1 1 d . . . . .
H441 H 0.0735 0.7299 -0.0338 0.047 Uiso 1 1 calc R U . . .
C45 C 0.06666(9) 0.5880(2) 0.05503(15) 0.0316(4) Uani 1 1 d . . . . .
H451 H 0.0481 0.6398 0.0898 0.038 Uiso 1 1 calc R U . . .
C46 C 0.07815(8) 0.45921(18) 0.07782(13) 0.0239(4) Uani 1 1 d . . . . .
H461 H 0.0671 0.4231 0.1277 0.029 Uiso 1 1 calc R U . . .
C50 C 0.38024(7) 0.39248(15) 0.49676(11) 0.0144(3) Uani 1 1 d . . . . .
H501 H 0.3496 0.3253 0.4857 0.017 Uiso 1 1 calc R U . . .
H502 H 0.4066 0.3818 0.5606 0.017 Uiso 1 1 calc R U . . .
C51 C 0.41474(7) 0.37643(17) 0.42755(11) 0.0163(3) Uani 1 1 d . . . . .
O51 O 0.40490(5) 0.46163(11) 0.36301(8) 0.0138(2) Uani 1 1 d . . . . .
O52 O 0.44824(6) 0.28294(14) 0.43609(9) 0.0273(3) Uani 1 1 d . . . . .
C60 C 0.42785(7) 0.74818(16) 0.36899(11) 0.0161(3) Uani 1 1 d . . . . .
H601 H 0.4561 0.6888 0.4108 0.019 Uiso 1 1 calc R U . . .
H602 H 0.4454 0.8356 0.3756 0.019 Uiso 1 1 calc R U . . .
C61 C 0.41477(7) 0.70243(15) 0.26919(11) 0.0142(3) Uani 1 1 d . . . . .
O61 O 0.36590(5) 0.64432(11) 0.23478(8) 0.0142(2) Uani 1 1 d . . . . .
O62 O 0.45116(5) 0.71995(12) 0.22766(8) 0.0190(2) Uani 1 1 d . . . . .
C70 C 0.24925(7) 0.77105(15) 0.18209(11) 0.0152(3) Uani 1 1 d . . . . .
H701 H 0.2815 0.8280 0.1782 0.018 Uiso 1 1 calc R U . . .
H702 H 0.2120 0.8155 0.1514 0.018 Uiso 1 1 calc R U . . .
C71 C 0.25187(7) 0.64401(15) 0.13227(11) 0.0125(3) Uani 1 1 d . . . . .
O71 O 0.25952(5) 0.54258(10) 0.18257(8) 0.0125(2) Uani 1 1 d . . . . .
O72 O 0.24801(5) 0.64735(11) 0.04907(8) 0.0177(2) Uani 1 1 d . . . . .
N1A N 0.47295(7) 0.42932(15) 0.23460(11) 0.0179(3) Uani 1 1 d . . . . .
H11A H 0.4506(12) 0.428(2) 0.172(2) 0.040(7) Uiso 1 1 d . . . . .
H12A H 0.4937(12) 0.360(3) 0.250(2) 0.046(7) Uiso 1 1 d . . . . .
H13A H 0.4986(12) 0.495(3) 0.2405(19) 0.041(7) Uiso 1 1 d . . . . .
H14A H 0.4499(11) 0.438(2) 0.2690(17) 0.031(6) Uiso 1 1 d . . . . .
O1W O 0.30196(6) 0.41369(14) 0.01625(10) 0.0247(3) Uani 1 1 d . . . . .
H11W H 0.2838(12) 0.475(3) 0.0311(19) 0.041(7) Uiso 1 1 d . . . . .
H12W H 0.2813(12) 0.390(3) -0.035(2) 0.039(7) Uiso 1 1 d . . . . .
O2W O 0.34842(6) 0.25846(15) 0.17255(10) 0.0287(3) Uani 1 1 d . . . . .
H21W H 0.3343(13) 0.292(3) 0.215(2) 0.055(8) Uiso 1 1 d . . . . .
H22W H 0.3344(12) 0.305(3) 0.124(2) 0.045(8) Uiso 1 1 d . . . . .
O3W O 0.43111(7) 0.08892(15) 0.27728(12) 0.0375(4) Uani 1 1 d . . . . .
H31W H 0.4069 0.1406 0.2360 0.081(12) Uiso 1 1 d R . . . .
H32W H 0.4425 0.1614 0.3198 0.098 Uiso 1 1 d R U . . .
O4W O 0.42252(7) 0.42495(14) 0.04134(10) 0.0279(3) Uani 1 1 d . . . . .
H41W H 0.4334(18) 0.362(4) 0.005(3) 0.106(14) Uiso 1 1 d . . . . .
H42W H 0.3876(14) 0.427(3) 0.036(2) 0.048(8) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sc1 O61 2.1236(11) . ?
Sc1 O71 2.1468(11) . ?
Sc1 O11 2.1585(11) . ?
Sc1 O51 2.1866(11) . ?
Sc1 N4 2.4415(14) . ?
Sc1 N7 2.4646(14) . ?
Sc1 N10 2.4814(14) . ?
Sc1 N1 2.5350(13) . ?
N1 C12 1.477(2) . ?
N1 C20 1.486(2) . ?
N1 C2 1.491(2) . ?
C2 C3 1.512(2) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.479(2) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.477(2) . ?
N4 C5 1.501(2) . ?
C5 C6 1.508(2) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.487(2) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.479(2) . ?
N7 C8 1.493(2) . ?
C8 C9 1.508(2) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.480(2) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.475(2) . ?
N10 C11 1.488(2) . ?
C11 C12 1.516(2) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.8253(16) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.4942(12) . ?
P1 O11 1.5307(11) . ?
P1 C21 1.8129(16) . ?
C21 N23 1.472(2) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N23 C30 1.464(2) . ?
N23 C40 1.469(2) . ?
C30 C31 1.515(2) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36 1.388(3) . ?
C31 C32 1.391(2) . ?
C32 C33 1.393(3) . ?
C32 H321 0.9500 . ?
C33 C34 1.380(3) . ?
C33 H331 0.9500 . ?
C34 C35 1.380(3) . ?
C34 H341 0.9500 . ?
C35 C36 1.390(3) . ?
C35 H351 0.9500 . ?
C36 H361 0.9500 . ?
C40 C41 1.506(2) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C41 C42 1.390(3) . ?
C41 C46 1.393(3) . ?
C42 C43 1.392(3) . ?
C42 H421 0.9500 . ?
C43 C44 1.372(4) . ?
C43 H431 0.9500 . ?
C44 C45 1.377(3) . ?
C44 H441 0.9500 . ?
C45 C46 1.383(3) . ?
C45 H451 0.9500 . ?
C46 H461 0.9500 . ?
C50 C51 1.528(2) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.240(2) . ?
C51 O51 1.284(2) . ?
C60 C61 1.523(2) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.234(2) . ?
C61 O61 1.282(2) . ?
C70 C71 1.526(2) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.2356(19) . ?
C71 O71 1.2770(19) . ?
N1A H11A 0.94(3) . ?
N1A H12A 0.86(3) . ?
N1A H13A 0.91(3) . ?
N1A H14A 0.87(3) . ?
O1W H11W 0.83(3) . ?
O1W H12W 0.82(3) . ?
O2W H21W 0.89(3) . ?
O2W H22W 0.86(3) . ?
O3W H31W 0.8921 . ?
O3W H32W 0.9723 . ?
O4W H41W 0.94(5) . ?
O4W H42W 0.82(3) . ?

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
O61 Sc1 O71 76.90(4) . . ?
O61 Sc1 O11 120.59(4) . . ?
O71 Sc1 O11 77.10(4) . . ?
O61 Sc1 O51 76.52(4) . . ?
O71 Sc1 O51 123.94(4) . . ?
O11 Sc1 O51 75.62(4) . . ?
O61 Sc1 N4 128.38(5) . . ?
O71 Sc1 N4 154.66(5) . . ?
O11 Sc1 N4 86.27(4) . . ?
O51 Sc1 N4 68.45(4) . . ?
O61 Sc1 N7 69.17(4) . . ?
O71 Sc1 N7 127.73(4) . . ?
O11 Sc1 N7 154.94(4) . . ?
O51 Sc1 N7 85.51(4) . . ?
N4 Sc1 N7 71.36(5) . . ?
O61 Sc1 N10 86.17(4) . . ?
O71 Sc1 N10 68.21(4) . . ?
O11 Sc1 N10 129.65(4) . . ?
O51 Sc1 N10 154.62(5) . . ?
N4 Sc1 N10 110.69(4) . . ?
N7 Sc1 N10 70.90(5) . . ?
O61 Sc1 N1 154.69(5) . . ?
O71 Sc1 N1 85.33(4) . . ?
O11 Sc1 N1 71.48(4) . . ?
O51 Sc1 N1 128.74(4) . . ?
N4 Sc1 N1 71.19(4) . . ?
N7 Sc1 N1 110.01(4) . . ?
N10 Sc1 N1 70.42(4) . . ?
C12 N1 C20 110.09(12) . . ?
C12 N1 C2 109.88(12) . . ?
C20 N1 C2 108.33(12) . . ?
C12 N1 Sc1 111.27(9) . . ?
C20 N1 Sc1 107.64(9) . . ?
C2 N1 Sc1 109.55(9) . . ?
N1 C2 C3 111.79(13) . . ?
N1 C2 H21 109.3 . . ?
C3 C2 H21 109.3 . . ?
N1 C2 H22 109.3 . . ?
C3 C2 H22 109.3 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 110.91(13) . . ?
N4 C3 H31 109.5 . . ?
C2 C3 H31 109.5 . . ?
N4 C3 H32 109.5 . . ?
C2 C3 H32 109.5 . . ?
H31 C3 H32 108.0 . . ?
C50 N4 C3 112.04(12) . . ?
C50 N4 C5 107.15(12) . . ?
C3 N4 C5 108.63(12) . . ?
C50 N4 Sc1 104.12(9) . . ?
C3 N4 Sc1 113.54(10) . . ?
C5 N4 Sc1 111.15(9) . . ?
N4 C5 C6 111.49(13) . . ?
N4 C5 H51 109.3 . . ?
C6 C5 H51 109.3 . . ?
N4 C5 H52 109.3 . . ?
C6 C5 H52 109.3 . . ?
H51 C5 H52 108.0 . . ?
N7 C6 C5 109.46(13) . . ?
N7 C6 H61 109.8 . . ?
C5 C6 H61 109.8 . . ?
N7 C6 H62 109.8 . . ?
C5 C6 H62 109.8 . . ?
H61 C6 H62 108.2 . . ?
C60 N7 C6 111.28(13) . . ?
C60 N7 C8 106.61(12) . . ?
C6 N7 C8 110.00(13) . . ?
C60 N7 Sc1 103.82(9) . . ?
C6 N7 Sc1 113.28(10) . . ?
C8 N7 Sc1 111.52(10) . . ?
N7 C8 C9 111.33(13) . . ?
N7 C8 H81 109.4 . . ?
C9 C8 H81 109.4 . . ?
N7 C8 H82 109.4 . . ?
C9 C8 H82 109.4 . . ?
H81 C8 H82 108.0 . . ?
N10 C9 C8 110.01(13) . . ?
N10 C9 H91 109.7 . . ?
C8 C9 H91 109.7 . . ?
N10 C9 H92 109.7 . . ?
C8 C9 H92 109.7 . . ?
H91 C9 H92 108.2 . . ?
C70 N10 C9 111.99(12) . . ?
C70 N10 C11 108.24(13) . . ?
C9 N10 C11 109.71(12) . . ?
C70 N10 Sc1 102.76(9) . . ?
C9 N10 Sc1 112.67(10) . . ?
C11 N10 Sc1 111.24(9) . . ?
N10 C11 C12 110.90(13) . . ?
N10 C11 H111 109.5 . . ?
C12 C11 H111 109.5 . . ?
N10 C11 H112 109.5 . . ?
C12 C11 H112 109.5 . . ?
H111 C11 H112 108.0 . . ?
N1 C12 C11 109.63(13) . . ?
N1 C12 H121 109.7 . . ?
C11 C12 H121 109.7 . . ?
N1 C12 H122 109.7 . . ?
C11 C12 H122 109.7 . . ?
H121 C12 H122 108.2 . . ?
N1 C20 P1 109.22(10) . . ?
N1 C20 H201 109.8 . . ?
P1 C20 H201 109.8 . . ?
N1 C20 H202 109.8 . . ?
P1 C20 H202 109.8 . . ?
H201 C20 H202 108.3 . . ?
O12 P1 O11 116.74(7) . . ?
O12 P1 C21 111.06(7) . . ?
O11 P1 C21 108.97(7) . . ?
O12 P1 C20 110.91(7) . . ?
O11 P1 C20 103.86(7) . . ?
C21 P1 C20 104.39(7) . . ?
P1 O11 Sc1 127.55(6) . . ?
N23 C21 P1 111.04(11) . . ?
N23 C21 H211 109.4 . . ?
P1 C21 H211 109.4 . . ?
N23 C21 H212 109.4 . . ?
P1 C21 H212 109.4 . . ?
H211 C21 H212 108.0 . . ?
C30 N23 C40 110.27(13) . . ?
C30 N23 C21 111.14(13) . . ?
C40 N23 C21 111.02(13) . . ?
N23 C30 C31 112.82(14) . . ?
N23 C30 H301 109.0 . . ?
C31 C30 H301 109.0 . . ?
N23 C30 H302 109.0 . . ?
C31 C30 H302 109.0 . . ?
H301 C30 H302 107.8 . . ?
C36 C31 C32 118.86(17) . . ?
C36 C31 C30 121.21(15) . . ?
C32 C31 C30 119.89(16) . . ?
C31 C32 C33 120.44(19) . . ?
C31 C32 H321 119.8 . . ?
C33 C32 H321 119.8 . . ?
C34 C33 C32 120.02(18) . . ?
C34 C33 H331 120.0 . . ?
C32 C33 H331 120.0 . . ?
C33 C34 C35 119.99(18) . . ?
C33 C34 H341 120.0 . . ?
C35 C34 H341 120.0 . . ?
C34 C35 C36 120.1(2) . . ?
C34 C35 H351 120.0 . . ?
C36 C35 H351 120.0 . . ?
C31 C36 C35 120.60(18) . . ?
C31 C36 H361 119.7 . . ?
C35 C36 H361 119.7 . . ?
N23 C40 C41 112.80(14) . . ?
N23 C40 H401 109.0 . . ?
C41 C40 H401 109.0 . . ?
N23 C40 H402 109.0 . . ?
C41 C40 H402 109.0 . . ?
H401 C40 H402 107.8 . . ?
C42 C41 C46 118.52(18) . . ?
C42 C41 C40 121.32(18) . . ?
C46 C41 C40 120.11(16) . . ?
C41 C42 C43 120.0(2) . . ?
C41 C42 H421 120.0 . . ?
C43 C42 H421 120.0 . . ?
C44 C43 C42 121.0(2) . . ?
C44 C43 H431 119.5 . . ?
C42 C43 H431 119.5 . . ?
C43 C44 C45 119.3(2) . . ?
C43 C44 H441 120.3 . . ?
C45 C44 H441 120.3 . . ?
C44 C45 C46 120.4(2) . . ?
C44 C45 H451 119.8 . . ?
C46 C45 H451 119.8 . . ?
C45 C46 C41 120.74(19) . . ?
C45 C46 H461 119.6 . . ?
C41 C46 H461 119.6 . . ?
N4 C50 C51 109.74(13) . . ?
N4 C50 H501 109.7 . . ?
C51 C50 H501 109.7 . . ?
N4 C50 H502 109.7 . . ?
C51 C50 H502 109.7 . . ?
H501 C50 H502 108.2 . . ?
O52 C51 O51 125.44(15) . . ?
O52 C51 C50 118.83(15) . . ?
O51 C51 C50 115.71(14) . . ?
C51 O51 Sc1 118.94(10) . . ?
N7 C60 C61 109.43(13) . . ?
N7 C60 H601 109.8 . . ?
C61 C60 H601 109.8 . . ?
N7 C60 H602 109.8 . . ?
C61 C60 H602 109.8 . . ?
H601 C60 H602 108.2 . . ?
O62 C61 O61 124.35(15) . . ?
O62 C61 C60 119.56(14) . . ?
O61 C61 C60 116.07(14) . . ?
C61 O61 Sc1 122.13(10) . . ?
N10 C70 C71 110.67(12) . . ?
N10 C70 H701 109.5 . . ?
C71 C70 H701 109.5 . . ?
N10 C70 H702 109.5 . . ?
C71 C70 H702 109.5 . . ?
H701 C70 H702 108.1 . . ?
O72 C71 O71 125.76(14) . . ?
O72 C71 C70 118.57(14) . . ?
O71 C71 C70 115.64(13) . . ?
C71 O71 Sc1 116.73(10) . . ?
H11A N1A H12A 112(2) . . ?
H11A N1A H13A 106(2) . . ?
H12A N1A H13A 106(2) . . ?
H11A N1A H14A 109(2) . . ?
H12A N1A H14A 110(2) . . ?
H13A N1A H14A 114(2) . . ?
H11W O1W H12W 105(3) . . ?
H21W O2W H22W 106(3) . . ?
H31W O3W H32W 89.8 . . ?
H41W O4W H42W 115(3) . . ?

_refine_diff_density_max         1.459
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.064

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

data_smdbamoh
_database_code_depnum_ccdc_archive 'CCDC 1959636'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 N5 O9 P Sm, 3(H2 O), H4 N'
_chemical_formula_sum            'C30 H52 N6 O12 P Sm'
_chemical_formula_weight         870.09

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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   47.041(8)
_cell_length_b                   10.2877(14)
_cell_length_c                   15.205(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.6500(10)
_cell_angle_gamma                90
_cell_volume                     7357.9(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9270
_cell_measurement_theta_min      2.4258
_cell_measurement_theta_max      27.5592

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_F_000             3576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.131
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_coefficient_mu    1.706
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            102754
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.368
_diffrn_reflns_theta_max         28.040
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8668
_reflns_number_gt                8435
_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.
 
 _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 Instrument Service v6.2.9'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+252.6453P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8668
_refine_ls_number_parameters     459
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0626
_refine_ls_wR_factor_ref         0.1674
_refine_ls_wR_factor_gt          0.1671
_refine_ls_goodness_of_fit_ref   1.465
_refine_ls_restrained_S_all      1.463
_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
Sm1 Sm 0.16114(2) 0.77237(3) 0.39598(2) 0.00908(10) Uani 1 1 d . . . . .
O1C O 0.17516(11) 0.6361(5) 0.2582(3) 0.0122(10) Uani 1 1 d . . . . .
H11C H 0.1655 0.6322 0.2173 0.015 Uiso 1 1 d R U . . .
H12C H 0.1739 0.5548 0.2774 0.015 Uiso 1 1 d R U . . .
N1 N 0.11349(12) 0.7530(6) 0.4998(4) 0.0107(11) Uani 1 1 d . . . . .
C2 C 0.12082(15) 0.6980(7) 0.5869(4) 0.0135(14) Uani 1 1 d . . . . .
H21 H 0.1241 0.6034 0.5810 0.016 Uiso 1 1 calc R U . . .
H22 H 0.1047 0.7107 0.6272 0.016 Uiso 1 1 calc R U . . .
C3 C 0.14692(15) 0.7610(7) 0.6257(4) 0.0136(13) Uani 1 1 d . . . . .
H31 H 0.1431 0.8545 0.6352 0.016 Uiso 1 1 calc R U . . .
H32 H 0.1512 0.7213 0.6836 0.016 Uiso 1 1 calc R U . . .
N4 N 0.17230(12) 0.7467(6) 0.5676(4) 0.0102(11) Uani 1 1 d . . . . .
C5 C 0.19496(16) 0.8388(8) 0.5951(5) 0.0154(14) Uani 1 1 d . . . . .
H51 H 0.2133 0.8096 0.5710 0.018 Uiso 1 1 calc R U . . .
H52 H 0.1967 0.8386 0.6601 0.018 Uiso 1 1 calc R U . . .
C6 C 0.18888(16) 0.9764(7) 0.5636(4) 0.0152(14) Uani 1 1 d . . . . .
H61 H 0.1709 1.0072 0.5895 0.018 Uiso 1 1 calc R U . . .
H62 H 0.2043 1.0348 0.5841 0.018 Uiso 1 1 calc R U . . .
N7 N 0.18663(13) 0.9823(6) 0.4665(4) 0.0141(12) Uani 1 1 d . . . . .
C8 C 0.17256(18) 1.1058(7) 0.4417(5) 0.0170(15) Uani 1 1 d . . . . .
H81 H 0.1771 1.1270 0.3800 0.020 Uiso 1 1 calc R U . . .
H82 H 0.1801 1.1766 0.4794 0.020 Uiso 1 1 calc R U . . .
C9 C 0.14063(17) 1.0984(7) 0.4514(5) 0.0155(14) Uani 1 1 d . . . . .
H91 H 0.1359 1.0850 0.5140 0.019 Uiso 1 1 calc R U . . .
H92 H 0.1319 1.1814 0.4320 0.019 Uiso 1 1 calc R U . . .
N10 N 0.12889(14) 0.9906(6) 0.3984(4) 0.0130(12) Uani 1 1 d . . . . .
C11 C 0.09948(16) 0.9612(8) 0.4280(5) 0.0171(15) Uani 1 1 d . . . . .
H111 H 0.0892 0.9134 0.3809 0.021 Uiso 1 1 calc R U . . .
H112 H 0.0892 1.0439 0.4382 0.021 Uiso 1 1 calc R U . . .
C12 C 0.09923(16) 0.8803(7) 0.5124(4) 0.0138(14) Uani 1 1 d . . . . .
H121 H 0.1091 0.9288 0.5601 0.017 Uiso 1 1 calc R U . . .
H122 H 0.0793 0.8656 0.5305 0.017 Uiso 1 1 calc R U . . .
C20 C 0.09410(15) 0.6605(7) 0.4551(5) 0.0130(13) Uani 1 1 d . . . . .
H201 H 0.0853 0.7029 0.4030 0.016 Uiso 1 1 calc R U . . .
H202 H 0.0787 0.6355 0.4955 0.016 Uiso 1 1 calc R U . . .
P1 P 0.11336(4) 0.51501(18) 0.42058(11) 0.0112(3) Uani 1 1 d . . . . .
O11 O 0.14439(10) 0.5585(5) 0.4119(3) 0.0114(9) Uani 1 1 d . . . . .
O12 O 0.10772(11) 0.4033(5) 0.4811(3) 0.0175(11) Uani 1 1 d . . . . .
C21 C 0.10004(16) 0.4850(9) 0.3112(5) 0.0209(16) Uani 1 1 d . . . . .
H211 H 0.1025 0.5636 0.2745 0.025 Uiso 1 1 calc R U . . .
H212 H 0.1108 0.4129 0.2841 0.025 Uiso 1 1 calc R U . . .
N22 N 0.06982(14) 0.4511(7) 0.3155(4) 0.0205(14) Uani 1 1 d . . . . .
C30 C 0.06520(19) 0.3147(10) 0.3331(7) 0.033(2) Uani 1 1 d . . . . .
H301 H 0.0808 0.2823 0.3716 0.040 Uiso 1 1 calc R U . . .
H302 H 0.0660 0.2660 0.2770 0.040 Uiso 1 1 calc R U . . .
C31 C 0.03692(18) 0.2876(8) 0.3768(6) 0.0255(18) Uani 1 1 d . . . . .
C32A C 0.0136(4) 0.2481(17) 0.3301(14) 0.032(3) Uani 0.517(9) 1 d . . P A 1
H32A H 0.0141 0.2388 0.2680 0.038 Uiso 0.517(9) 1 calc R U P A 1
C33A C -0.0115(4) 0.221(2) 0.3774(16) 0.045(4) Uani 0.517(9) 1 d . . P A 1
H33A H -0.0279 0.1964 0.3445 0.054 Uiso 0.517(9) 1 calc R U P A 1
C34 C -0.0139(2) 0.2287(13) 0.4645(9) 0.050(3) Uani 1 1 d . . . . .
H341 H -0.0307 0.2321 0.4981 0.060 Uiso 1 1 d R U . A .
C35A C 0.0124(4) 0.270(2) 0.5113(15) 0.038(3) Uani 0.517(9) 1 d . . P A 1
H35A H 0.0125 0.2787 0.5735 0.045 Uiso 0.517(9) 1 calc R U P A 1
C36A C 0.0368(4) 0.2942(17) 0.4638(13) 0.030(3) Uani 0.517(9) 1 d . . P A 1
H36A H 0.0538 0.3165 0.4944 0.035 Uiso 0.517(9) 1 calc R U P A 1
C32B C 0.0250(4) 0.1622(18) 0.3759(14) 0.032(3) Uani 0.483(9) 1 d . . P A 2
H32B H 0.0344 0.0945 0.3453 0.038 Uiso 0.483(9) 1 calc R U P A 2
C33B C -0.0003(5) 0.136(2) 0.4186(17) 0.045(4) Uani 0.483(9) 1 d . . P A 2
H33B H -0.0081 0.0505 0.4157 0.054 Uiso 0.483(9) 1 calc R U P A 2
C35B C -0.0057(4) 0.352(2) 0.4654(15) 0.038(3) Uani 0.483(9) 1 d . . P A 2
H35B H -0.0171 0.4170 0.4915 0.045 Uiso 0.483(9) 1 calc R U P A 2
C36B C 0.0207(4) 0.3828(19) 0.4263(13) 0.030(3) Uani 0.483(9) 1 d . . P A 2
H36B H 0.0281 0.4684 0.4326 0.035 Uiso 0.483(9) 1 calc R U P A 2
C40 C 0.05457(19) 0.4934(12) 0.2360(6) 0.036(2) Uani 1 1 d . . . . .
H401 H 0.0641 0.4533 0.1850 0.044 Uiso 1 1 calc R U . B 3
H402 H 0.0351 0.4566 0.2382 0.044 Uiso 1 1 calc R U . B 3
C41C C 0.0521(3) 0.6185(13) 0.2199(10) 0.018(3) Uani 0.506(16) 1 d G U P C 3
C42C C 0.0617(3) 0.6781(18) 0.1437(10) 0.043(5) Uani 0.506(16) 1 d G . P C 3
H42C H 0.0704 0.6277 0.0991 0.052 Uiso 0.506(16) 1 calc R U P C 3
C43C C 0.0585(4) 0.8115(19) 0.1328(12) 0.072(9) Uani 0.506(16) 1 d G . P C 3
H43C H 0.0651 0.8523 0.0808 0.086 Uiso 0.506(16) 1 calc R U P C 3
C44C C 0.0458(5) 0.8852(14) 0.1981(14) 0.063(7) Uani 0.506(16) 1 d G . P C 3
H44C H 0.0436 0.9764 0.1906 0.076 Uiso 0.506(16) 1 calc R U P C 3
C45C C 0.0362(4) 0.8256(15) 0.2742(12) 0.046(4) Uani 0.506(16) 1 d G U P C 3
H45C H 0.0275 0.8759 0.3188 0.056 Uiso 0.506(16) 1 calc R U P C 3
C46C C 0.0394(4) 0.6922(15) 0.2851(9) 0.033(4) Uani 0.506(16) 1 d G U P C 3
H46C H 0.0328 0.6514 0.3372 0.039 Uiso 0.506(16) 1 calc R U P C 3
C41D C 0.0513(4) 0.6556(13) 0.2393(10) 0.018(3) Uani 0.494(16) 1 d G U P C 4
C42D C 0.0651(3) 0.7312(19) 0.1772(10) 0.043(5) Uani 0.494(16) 1 d G . P C 4
H42D H 0.0766 0.6909 0.1340 0.052 Uiso 0.494(16) 1 calc R U P C 4
C43D C 0.0621(4) 0.8655(19) 0.1782(14) 0.072(9) Uani 0.494(16) 1 d G . P C 4
H43D H 0.0715 0.9172 0.1358 0.086 Uiso 0.494(16) 1 calc R U P C 4
C44D C 0.0452(5) 0.9244(13) 0.2413(15) 0.063(7) Uani 0.494(16) 1 d G . P C 4
H44D H 0.0432 1.0162 0.2420 0.076 Uiso 0.494(16) 1 calc R U P C 4
C45D C 0.0314(4) 0.8488(16) 0.3035(12) 0.046(4) Uani 0.494(16) 1 d G U P C 4
H45D H 0.0199 0.8890 0.3466 0.056 Uiso 0.494(16) 1 calc R U P C 4
C46D C 0.0344(4) 0.7144(16) 0.3024(10) 0.033(4) Uani 0.494(16) 1 d G U P C 4
H46D H 0.0250 0.6628 0.3449 0.039 Uiso 0.494(16) 1 calc R U P C 4
C50 C 0.18410(15) 0.6140(7) 0.5744(4) 0.0120(13) Uani 1 1 d . . . . .
H501 H 0.1683 0.5505 0.5746 0.014 Uiso 1 1 calc R U . . .
H502 H 0.1946 0.6053 0.6309 0.014 Uiso 1 1 calc R U . . .
C51 C 0.20419(15) 0.5824(7) 0.4980(5) 0.0125(13) Uani 1 1 d . . . . .
O51 O 0.20404(11) 0.6573(5) 0.4319(3) 0.0139(10) Uani 1 1 d . . . . .
O52 O 0.21937(12) 0.4837(6) 0.5052(4) 0.0222(12) Uani 1 1 d . . . . .
C60 C 0.21515(17) 0.9807(8) 0.4250(5) 0.0194(16) Uani 1 1 d . . . . .
H601 H 0.2268 0.9111 0.4521 0.023 Uiso 1 1 calc R U . . .
H602 H 0.2248 1.0647 0.4363 0.023 Uiso 1 1 calc R U . . .
C61 C 0.21303(17) 0.9580(7) 0.3260(5) 0.0171(15) Uani 1 1 d . . . . .
O61 O 0.19173(12) 0.8960(5) 0.2994(3) 0.0175(11) Uani 1 1 d . . . . .
O62 O 0.23268(13) 1.0000(6) 0.2778(4) 0.0238(13) Uani 1 1 d . . . . .
C70 C 0.12817(18) 1.0261(7) 0.3047(4) 0.0165(15) Uani 1 1 d . . . . .
H701 H 0.1456 1.0755 0.2903 0.020 Uiso 1 1 calc R U . . .
H702 H 0.1116 1.0831 0.2929 0.020 Uiso 1 1 calc R U . . .
C71 C 0.12621(16) 0.9066(7) 0.2462(4) 0.0144(14) Uani 1 1 d . . . . .
O71 O 0.12759(11) 0.7988(5) 0.2844(3) 0.0141(10) Uani 1 1 d . . . . .
O72 O 0.12436(14) 0.9237(6) 0.1656(3) 0.0227(12) Uani 1 1 d . . . . .
N1A N 0.22576(14) 0.6658(6) 0.1586(4) 0.0164(12) Uani 1 1 d . . . . .
H11A H 0.2103 0.7004 0.1954 0.020 Uiso 1 1 d R U . . .
H12A H 0.2364 0.7422 0.1519 0.020 Uiso 1 1 d R U . . .
H13A H 0.2193 0.6199 0.1148 0.020 Uiso 1 1 d R U . . .
H14A H 0.2401 0.6165 0.1883 0.020 Uiso 1 1 d R U . . .
O1W O 0.17918(13) 0.3791(6) 0.3150(4) 0.0212(12) Uani 1 1 d . . . . .
H11W H 0.1732 0.4180 0.3553 0.025 Uiso 1 1 d R U . . .
H12W H 0.1981 0.3880 0.3347 0.025 Uiso 1 1 d R U . . .
O2W O 0.23867(13) 0.3797(5) 0.3556(4) 0.0213(12) Uani 1 1 d . . . . .
H21W H 0.2299 0.4249 0.3986 0.026 Uiso 1 1 d R U . . .
H22W H 0.2463 0.4401 0.3153 0.026 Uiso 1 1 d R U . . .
O3W O 0.14502(14) 0.6772(6) 0.1078(4) 0.0269(14) Uani 1 1 d . . . . .
H31W H 0.1356 0.7537 0.1333 0.032 Uiso 1 1 d R U . . .
H32W H 0.1337 0.6440 0.0745 0.032 Uiso 1 1 d R U . . .


_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
Sm1 O71 2.320(5) . ?
Sm1 O11 2.351(5) . ?
Sm1 O51 2.398(5) . ?
Sm1 O61 2.428(5) . ?
Sm1 O1C 2.612(5) . ?
Sm1 N4 2.669(6) . ?
Sm1 N7 2.687(6) . ?
Sm1 N10 2.710(6) . ?
Sm1 N1 2.763(6) . ?
O1C H11C 0.7661 . ?
O1C H12C 0.8884 . ?
N1 C20 1.478(9) . ?
N1 C2 1.478(8) . ?
N1 C12 1.485(9) . ?
C2 C3 1.503(10) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.500(9) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.476(9) . ?
N4 C5 1.483(9) . ?
C5 C6 1.520(10) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.481(9) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C8 1.479(10) . ?
N7 C60 1.489(9) . ?
C8 C9 1.513(11) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.475(9) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.471(9) . ?
N10 C11 1.490(10) . ?
C11 C12 1.531(10) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.830(7) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.498(5) . ?
P1 O11 1.534(5) . ?
P1 C21 1.797(7) . ?
C21 N22 1.466(10) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C30 1.446(12) . ?
N22 C40 1.465(10) . ?
C30 C31 1.520(13) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36A 1.32(2) . ?
C31 C32A 1.364(18) . ?
C31 C32B 1.41(2) . ?
C31 C36B 1.45(2) . ?
C32A C33A 1.42(3) . ?
C32A H32A 0.9500 . ?
C33A C34 1.33(3) . ?
C33A H33A 0.9500 . ?
C34 C35B 1.32(3) . ?
C34 C33B 1.35(3) . ?
C34 C35A 1.48(2) . ?
C34 H341 0.9468 . ?
C35A C36A 1.39(3) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C32B C33B 1.39(3) . ?
C32B H32B 0.9500 . ?
C33B H33B 0.9500 . ?
C35B C36B 1.42(3) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C40 C41C 1.314(17) . ?
C40 C41D 1.676(18) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C41C C42C 1.3900 . ?
C41C C46C 1.3900 . ?
C42C C43C 1.3900 . ?
C42C H42C 0.9500 . ?
C43C C44C 1.3900 . ?
C43C H43C 0.9500 . ?
C44C C45C 1.3900 . ?
C44C H44C 0.9500 . ?
C45C C46C 1.3900 . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
C41D C42D 1.3900 . ?
C41D C46D 1.3900 . ?
C42D C43D 1.3900 . ?
C42D H42D 0.9500 . ?
C43D C44D 1.3900 . ?
C43D H43D 0.9500 . ?
C44D C45D 1.3900 . ?
C44D H44D 0.9500 . ?
C45D C46D 1.3900 . ?
C45D H45D 0.9500 . ?
C46D H46D 0.9500 . ?
C50 C51 1.540(10) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.246(9) . ?
C51 O51 1.266(9) . ?
C60 C61 1.525(10) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O61 1.251(9) . ?
C61 O62 1.263(9) . ?
C70 C71 1.519(10) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.239(8) . ?
C71 O71 1.254(9) . ?
N1A H11A 0.9881 . ?
N1A H12A 0.9388 . ?
N1A H13A 0.8684 . ?
N1A H14A 0.9538 . ?
O1W H11W 0.7876 . ?
O1W H12W 0.9424 . ?
O2W H21W 0.9053 . ?
O2W H22W 0.9467 . ?
O3W H31W 0.9859 . ?
O3W H32W 0.8047 . ?

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
O71 Sm1 O11 87.65(17) . . ?
O71 Sm1 O51 142.03(17) . . ?
O11 Sm1 O51 78.25(17) . . ?
O71 Sm1 O61 84.20(18) . . ?
O11 Sm1 O61 138.96(17) . . ?
O51 Sm1 O61 83.88(19) . . ?
O71 Sm1 O1C 69.63(16) . . ?
O11 Sm1 O1C 70.63(16) . . ?
O51 Sm1 O1C 72.44(16) . . ?
O61 Sm1 O1C 68.83(16) . . ?
O71 Sm1 N4 148.35(18) . . ?
O11 Sm1 N4 82.47(17) . . ?
O51 Sm1 N4 64.69(17) . . ?
O61 Sm1 N4 122.15(17) . . ?
O1C Sm1 N4 133.04(16) . . ?
O71 Sm1 N7 119.63(18) . . ?
O11 Sm1 N7 149.28(17) . . ?
O51 Sm1 N7 86.29(19) . . ?
O61 Sm1 N7 63.62(17) . . ?
O1C Sm1 N7 129.48(17) . . ?
N4 Sm1 N7 66.90(18) . . ?
O71 Sm1 N10 62.40(18) . . ?
O11 Sm1 N10 125.85(18) . . ?
O51 Sm1 N10 151.15(18) . . ?
O61 Sm1 N10 84.85(19) . . ?
O1C Sm1 N10 127.01(16) . . ?
N4 Sm1 N10 99.94(17) . . ?
N7 Sm1 N10 64.93(19) . . ?
O71 Sm1 N1 82.93(17) . . ?
O11 Sm1 N1 66.34(17) . . ?
O51 Sm1 N1 121.35(17) . . ?
O61 Sm1 N1 150.89(18) . . ?
O1C Sm1 N1 129.30(16) . . ?
N4 Sm1 N1 65.55(17) . . ?
N7 Sm1 N1 101.02(18) . . ?
N10 Sm1 N1 66.05(18) . . ?
Sm1 O1C H11C 121.7 . . ?
Sm1 O1C H12C 102.9 . . ?
H11C O1C H12C 100.2 . . ?
C20 N1 C2 107.6(5) . . ?
C20 N1 C12 110.5(5) . . ?
C2 N1 C12 108.8(5) . . ?
C20 N1 Sm1 106.5(4) . . ?
C2 N1 Sm1 110.9(4) . . ?
C12 N1 Sm1 112.4(4) . . ?
N1 C2 C3 111.6(6) . . ?
N1 C2 H21 109.3 . . ?
C3 C2 H21 109.3 . . ?
N1 C2 H22 109.3 . . ?
C3 C2 H22 109.3 . . ?
H21 C2 H22 108.0 . . ?
N4 C3 C2 112.3(5) . . ?
N4 C3 H31 109.1 . . ?
C2 C3 H31 109.1 . . ?
N4 C3 H32 109.1 . . ?
C2 C3 H32 109.1 . . ?
H31 C3 H32 107.9 . . ?
C50 N4 C5 107.6(5) . . ?
C50 N4 C3 110.5(5) . . ?
C5 N4 C3 110.2(5) . . ?
C50 N4 Sm1 103.3(4) . . ?
C5 N4 Sm1 110.2(4) . . ?
C3 N4 Sm1 114.6(4) . . ?
N4 C5 C6 112.0(6) . . ?
N4 C5 H51 109.2 . . ?
C6 C5 H51 109.2 . . ?
N4 C5 H52 109.2 . . ?
C6 C5 H52 109.2 . . ?
H51 C5 H52 107.9 . . ?
N7 C6 C5 111.3(6) . . ?
N7 C6 H61 109.4 . . ?
C5 C6 H61 109.4 . . ?
N7 C6 H62 109.4 . . ?
C5 C6 H62 109.4 . . ?
H61 C6 H62 108.0 . . ?
C8 N7 C6 108.4(6) . . ?
C8 N7 C60 107.7(6) . . ?
C6 N7 C60 111.6(6) . . ?
C8 N7 Sm1 113.1(4) . . ?
C6 N7 Sm1 113.1(4) . . ?
C60 N7 Sm1 102.8(4) . . ?
N7 C8 C9 111.9(6) . . ?
N7 C8 H81 109.2 . . ?
C9 C8 H81 109.2 . . ?
N7 C8 H82 109.2 . . ?
C9 C8 H82 109.2 . . ?
H81 C8 H82 107.9 . . ?
N10 C9 C8 110.5(6) . . ?
N10 C9 H91 109.5 . . ?
C8 C9 H91 109.5 . . ?
N10 C9 H92 109.5 . . ?
C8 C9 H92 109.5 . . ?
H91 C9 H92 108.1 . . ?
C70 N10 C9 110.3(6) . . ?
C70 N10 C11 109.4(6) . . ?
C9 N10 C11 109.3(6) . . ?
C70 N10 Sm1 101.5(4) . . ?
C9 N10 Sm1 115.1(4) . . ?
C11 N10 Sm1 111.0(4) . . ?
N10 C11 C12 112.3(6) . . ?
N10 C11 H111 109.1 . . ?
C12 C11 H111 109.1 . . ?
N10 C11 H112 109.1 . . ?
C12 C11 H112 109.1 . . ?
H111 C11 H112 107.9 . . ?
N1 C12 C11 111.3(5) . . ?
N1 C12 H121 109.4 . . ?
C11 C12 H121 109.4 . . ?
N1 C12 H122 109.4 . . ?
C11 C12 H122 109.4 . . ?
H121 C12 H122 108.0 . . ?
N1 C20 P1 110.7(5) . . ?
N1 C20 H201 109.5 . . ?
P1 C20 H201 109.5 . . ?
N1 C20 H202 109.5 . . ?
P1 C20 H202 109.5 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 116.9(3) . . ?
O12 P1 C21 112.0(4) . . ?
O11 P1 C21 107.0(3) . . ?
O12 P1 C20 111.1(3) . . ?
O11 P1 C20 105.1(3) . . ?
C21 P1 C20 103.7(4) . . ?
P1 O11 Sm1 127.0(3) . . ?
N22 C21 P1 109.1(5) . . ?
N22 C21 H211 109.9 . . ?
P1 C21 H211 109.9 . . ?
N22 C21 H212 109.9 . . ?
P1 C21 H212 109.9 . . ?
H211 C21 H212 108.3 . . ?
C30 N22 C40 111.6(8) . . ?
C30 N22 C21 112.8(7) . . ?
C40 N22 C21 111.0(7) . . ?
N22 C30 C31 113.2(8) . . ?
N22 C30 H301 108.9 . . ?
C31 C30 H301 108.9 . . ?
N22 C30 H302 108.9 . . ?
C31 C30 H302 108.9 . . ?
H301 C30 H302 107.8 . . ?
C36A C31 C32A 121.5(14) . . ?
C32B C31 C36B 114.3(13) . . ?
C36A C31 C30 116.2(10) . . ?
C32A C31 C30 122.1(12) . . ?
C32B C31 C30 121.0(11) . . ?
C36B C31 C30 124.6(10) . . ?
C31 C32A C33A 117.7(18) . . ?
C31 C32A H32A 121.1 . . ?
C33A C32A H32A 121.1 . . ?
C34 C33A C32A 125.0(16) . . ?
C34 C33A H33A 117.5 . . ?
C32A C33A H33A 117.5 . . ?
C35B C34 C33B 122.9(17) . . ?
C33A C34 C35A 114.5(14) . . ?
C35B C34 H341 101.9 . . ?
C33A C34 H341 128.2 . . ?
C33B C34 H341 135.1 . . ?
C35A C34 H341 115.4 . . ?
C36A C35A C34 119.6(18) . . ?
C36A C35A H35A 120.2 . . ?
C34 C35A H35A 120.2 . . ?
C31 C36A C35A 121.6(17) . . ?
C31 C36A H36A 119.2 . . ?
C35A C36A H36A 119.2 . . ?
C33B C32B C31 121.4(19) . . ?
C33B C32B H32B 119.3 . . ?
C31 C32B H32B 119.3 . . ?
C34 C33B C32B 121.0(18) . . ?
C34 C33B H33B 119.5 . . ?
C32B C33B H33B 119.5 . . ?
C34 C35B C36B 118.0(19) . . ?
C34 C35B H35B 121.0 . . ?
C36B C35B H35B 121.0 . . ?
C35B C36B C31 122.0(17) . . ?
C35B C36B H36B 119.0 . . ?
C31 C36B H36B 119.0 . . ?
C41C C40 N22 119.1(10) . . ?
N22 C40 C41D 108.4(9) . . ?
C41C C40 H401 107.5 . . ?
N22 C40 H401 107.5 . . ?
C41C C40 H402 107.5 . . ?
N22 C40 H402 107.5 . . ?
H401 C40 H402 107.0 . . ?
C40 C41C C42C 124.0(11) . . ?
C40 C41C C46C 116.0(11) . . ?
C42C C41C C46C 120.0 . . ?
C43C C42C C41C 120.0 . . ?
C43C C42C H42C 120.0 . . ?
C41C C42C H42C 120.0 . . ?
C44C C43C C42C 120.0 . . ?
C44C C43C H43C 120.0 . . ?
C42C C43C H43C 120.0 . . ?
C43C C44C C45C 120.0 . . ?
C43C C44C H44C 120.0 . . ?
C45C C44C H44C 120.0 . . ?
C46C C45C C44C 120.0 . . ?
C46C C45C H45C 120.0 . . ?
C44C C45C H45C 120.0 . . ?
C45C C46C C41C 120.0 . . ?
C45C C46C H46C 120.0 . . ?
C41C C46C H46C 120.0 . . ?
C42D C41D C46D 120.0 . . ?
C42D C41D C40 119.5(10) . . ?
C46D C41D C40 120.5(10) . . ?
C41D C42D C43D 120.0 . . ?
C41D C42D H42D 120.0 . . ?
C43D C42D H42D 120.0 . . ?
C42D C43D C44D 120.0 . . ?
C42D C43D H43D 120.0 . . ?
C44D C43D H43D 120.0 . . ?
C45D C44D C43D 120.0 . . ?
C45D C44D H44D 120.0 . . ?
C43D C44D H44D 120.0 . . ?
C46D C45D C44D 120.0 . . ?
C46D C45D H45D 120.0 . . ?
C44D C45D H45D 120.0 . . ?
C45D C46D C41D 120.0 . . ?
C45D C46D H46D 120.0 . . ?
C41D C46D H46D 120.0 . . ?
N4 C50 C51 112.1(6) . . ?
N4 C50 H501 109.2 . . ?
C51 C50 H501 109.2 . . ?
N4 C50 H502 109.2 . . ?
C51 C50 H502 109.2 . . ?
H501 C50 H502 107.9 . . ?
O52 C51 O51 124.3(7) . . ?
O52 C51 C50 117.5(6) . . ?
O51 C51 C50 118.2(6) . . ?
C51 O51 Sm1 118.6(4) . . ?
N7 C60 C61 111.8(6) . . ?
N7 C60 H601 109.3 . . ?
C61 C60 H601 109.3 . . ?
N7 C60 H602 109.3 . . ?
C61 C60 H602 109.3 . . ?
H601 C60 H602 107.9 . . ?
O61 C61 O62 125.1(7) . . ?
O61 C61 C60 116.1(6) . . ?
O62 C61 C60 118.7(7) . . ?
C61 O61 Sm1 123.3(5) . . ?
N10 C70 C71 111.5(6) . . ?
N10 C70 H701 109.3 . . ?
C71 C70 H701 109.3 . . ?
N10 C70 H702 109.3 . . ?
C71 C70 H702 109.3 . . ?
H701 C70 H702 108.0 . . ?
O72 C71 O71 125.8(7) . . ?
O72 C71 C70 117.8(7) . . ?
O71 C71 C70 116.3(6) . . ?
C71 O71 Sm1 118.3(5) . . ?
H11A N1A H12A 99.0 . . ?
H11A N1A H13A 112.2 . . ?
H12A N1A H13A 123.6 . . ?
H11A N1A H14A 116.4 . . ?
H12A N1A H14A 96.9 . . ?
H13A N1A H14A 108.3 . . ?
H11W O1W H12W 92.9 . . ?
H21W O2W H22W 108.0 . . ?
H31W O3W H32W 106.7 . . ?

_refine_diff_density_max         3.990
_refine_diff_density_min         -6.087
_refine_diff_density_rms         0.210

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

data_nddo3apdbam
_database_code_depnum_ccdc_archive 'CCDC 1959633'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 N5 Nd O9 P, 3(H2 O), H4 N'
_chemical_formula_sum            'C30 H52 N6 Nd O12 P'
_chemical_formula_weight         863.98

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'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   47.142(2)
_cell_length_b                   10.3053(4)
_cell_length_c                   15.3151(7)
_cell_angle_alpha                90
_cell_angle_beta                 90.722(2)
_cell_angle_gamma                90
_cell_volume                     7439.7(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9941
_cell_measurement_theta_min      2.7867
_cell_measurement_theta_max      27.5154

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_F_000             3560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.535
_exptl_crystal_size_mid          0.475
_exptl_crystal_size_min          0.108
_exptl_absorpt_coefficient_mu    1.505
_shelx_estimated_absorpt_T_min   0.500
_shelx_estimated_absorpt_T_max   0.854
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/2 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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 8.3333
_diffrn_reflns_number            26394
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.330
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7322
_reflns_number_gt                6678
_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.
 
 _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 Instrument Service v2013.12.0.0'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0001P)²+649.2667P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7322
_refine_ls_number_parameters     418
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.1147
_refine_ls_R_factor_gt           0.1067
_refine_ls_wR_factor_ref         0.2357
_refine_ls_wR_factor_gt          0.2324
_refine_ls_goodness_of_fit_ref   1.293
_refine_ls_restrained_S_all      1.289
_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_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
Nd1 Nd 0.16146(2) 0.77122(6) 0.10711(4) 0.00937(18) Uani 1 1 d . . . . .
O1C O 0.17546(19) 0.6352(9) 0.2459(5) 0.0135(18) Uani 1 1 d . U . . .
H11C H 0.1765 0.5692 0.2310 0.016 Uiso 1 1 d R U . . .
H12C H 0.1683 0.6463 0.2996 0.016 Uiso 1 1 d R U . . .
N1 N 0.1138(2) 0.7508(10) 0.0024(6) 0.009(2) Uani 1 1 d . U . . .
C2 C 0.1214(3) 0.6968(12) -0.0835(8) 0.013(3) Uani 1 1 d . U . . .
H21 H 0.1051 0.7079 -0.1243 0.016 Uiso 1 1 calc R U . . .
H22 H 0.1249 0.6026 -0.0772 0.016 Uiso 1 1 calc R U . . .
C3 C 0.1471(3) 0.7596(13) -0.1225(8) 0.014(3) Uani 1 1 d . U . . .
H31 H 0.1510 0.7194 -0.1798 0.016 Uiso 1 1 calc R U . . .
H32 H 0.1432 0.8529 -0.1322 0.016 Uiso 1 1 calc R U . . .
N4 N 0.1724(2) 0.7455(11) -0.0650(6) 0.014(2) Uani 1 1 d . . . . .
C5 C 0.1952(3) 0.8411(13) -0.0919(8) 0.016(3) Uani 1 1 d . U . . .
H51 H 0.2137 0.8129 -0.0673 0.019 Uiso 1 1 calc R U . . .
H52 H 0.1966 0.8411 -0.1564 0.019 Uiso 1 1 calc R U . . .
C6 C 0.1889(3) 0.9764(14) -0.0611(9) 0.018(3) Uani 1 1 d . U . . .
H61 H 0.2041 1.0354 -0.0808 0.022 Uiso 1 1 calc R U . . .
H62 H 0.1708 1.0061 -0.0880 0.022 Uiso 1 1 calc R U . . .
N7 N 0.1868(2) 0.9840(11) 0.0357(7) 0.014(2) Uani 1 1 d . . . . .
C8 C 0.1721(3) 1.1057(13) 0.0621(9) 0.018(3) Uani 1 1 d . U . . .
H81 H 0.1767 1.1244 0.1240 0.022 Uiso 1 1 calc R U . . .
H82 H 0.1793 1.1785 0.0266 0.022 Uiso 1 1 calc R U . . .
C9 C 0.1408(3) 1.0985(13) 0.0512(8) 0.014(3) Uani 1 1 d . U . . .
H91 H 0.1360 1.0838 -0.0111 0.017 Uiso 1 1 calc R U . . .
H92 H 0.1323 1.1820 0.0690 0.017 Uiso 1 1 calc R U . . .
N10 N 0.1287(2) 0.9918(10) 0.1045(7) 0.013(2) Uani 1 1 d . U . . .
C11 C 0.0997(3) 0.9605(13) 0.0743(8) 0.014(3) Uani 1 1 d . U . . .
H111 H 0.0891 1.0421 0.0635 0.017 Uiso 1 1 calc R U . . .
H112 H 0.0898 0.9120 0.1207 0.017 Uiso 1 1 calc R U . . .
C12 C 0.0996(3) 0.8802(12) -0.0085(8) 0.011(2) Uani 1 1 d . . . . .
H121 H 0.0797 0.8663 -0.0279 0.013 Uiso 1 1 calc R U . . .
H122 H 0.1094 0.9294 -0.0548 0.013 Uiso 1 1 calc R U . . .
C20 C 0.0944(3) 0.6591(12) 0.0473(8) 0.013(3) Uani 1 1 d . . . . .
H201 H 0.0786 0.6353 0.0074 0.015 Uiso 1 1 calc R U . . .
H202 H 0.0863 0.7019 0.0992 0.015 Uiso 1 1 calc R U . . .
P1 P 0.11345(7) 0.5125(3) 0.08124(19) 0.0096(6) Uani 1 1 d . . . . .
O11 O 0.14421(18) 0.5554(8) 0.0908(5) 0.0106(17) Uani 1 1 d . . . . .
O12 O 0.1078(2) 0.4023(9) 0.0198(6) 0.019(2) Uani 1 1 d . . . . .
C21 C 0.0994(3) 0.4780(16) 0.1891(9) 0.020(3) Uani 1 1 d . . . . .
H211 H 0.1098 0.4038 0.2152 0.024 Uiso 1 1 calc R U . . .
H212 H 0.1023 0.5544 0.2274 0.024 Uiso 1 1 calc R U . . .
N22 N 0.0698(3) 0.4480(12) 0.1837(8) 0.023(3) Uani 1 1 d . U . . .
C30 C 0.0648(3) 0.3112(15) 0.1656(13) 0.033(4) Uani 1 1 d . . . . .
H301 H 0.0661 0.2620 0.2211 0.040 Uiso 1 1 calc R U . . .
H302 H 0.0799 0.2788 0.1269 0.040 Uiso 1 1 calc R U . . .
C31 C 0.0368(3) 0.2864(14) 0.1238(12) 0.028(4) Uani 1 1 d . . . . .
C32A C 0.0209(7) 0.377(4) 0.072(2) 0.038(4) Uani 0.498(15) 1 d . . P A 1
H32A H 0.0287 0.4605 0.0634 0.045 Uiso 0.498(15) 1 calc R U P A 1
C33A C -0.0048(9) 0.351(4) 0.033(3) 0.054(6) Uani 0.498(15) 1 d . . P A 1
H33A H -0.0157 0.4172 0.0054 0.065 Uiso 0.498(15) 1 calc R U P A 1
C34 C -0.0138(4) 0.229(2) 0.0357(16) 0.057(6) Uani 1 1 d . . . . .
H34 H -0.0306 0.2041 0.0054 0.069 Uiso 1 1 calc R U . A 1
C35A C 0.0002(9) 0.145(4) 0.079(3) 0.054(6) Uani 0.498(15) 1 d . . P A 1
H35A H -0.0079 0.0610 0.0802 0.065 Uiso 0.498(15) 1 calc R U P A 1
C36A C 0.0255(7) 0.159(4) 0.124(2) 0.038(4) Uani 0.498(15) 1 d . . P A 1
H36A H 0.0346 0.0886 0.1527 0.045 Uiso 0.498(15) 1 calc R U P A 1
C32B C 0.0365(7) 0.300(4) 0.040(2) 0.038(4) Uani 0.502(15) 1 d . . P A 2
H32B H 0.0530 0.3294 0.0109 0.045 Uiso 0.502(15) 1 calc R U P A 2
C33B C 0.0113(9) 0.269(4) -0.010(3) 0.054(6) Uani 0.502(15) 1 d . . P A 2
H33B H 0.0111 0.2758 -0.0722 0.065 Uiso 0.502(15) 1 calc R U P A 2
C35B C -0.0120(9) 0.214(4) 0.122(3) 0.054(6) Uani 0.502(15) 1 d . . P A 2
H35B H -0.0279 0.1829 0.1531 0.065 Uiso 0.502(15) 1 calc R U P A 2
C36B C 0.0130(7) 0.244(4) 0.168(2) 0.038(4) Uani 0.502(15) 1 d . . P A 2
H36B H 0.0137 0.2354 0.2294 0.045 Uiso 0.502(15) 1 calc R U P A 2
C40 C 0.0541(4) 0.4898(19) 0.2634(11) 0.038(4) Uani 1 1 d . . . . .
H401 H 0.0644 0.4593 0.3163 0.045 Uiso 0.5 1 calc R U P B 3
H402 H 0.0350 0.4501 0.2629 0.045 Uiso 0.5 1 calc R U P B 3
H403 H 0.0347 0.4538 0.2593 0.045 Uiso 0.5 1 calc R U P C 4
H404 H 0.0635 0.4493 0.3148 0.045 Uiso 0.5 1 calc R U P C 4
C41C C 0.0512(6) 0.6480(19) 0.2661(17) 0.027(4) Uiso 0.5 1 d G . P D 3
C42C C 0.0344(6) 0.706(2) 0.2021(16) 0.039(5) Uiso 0.5 1 d G . P D 3
H42C H 0.0252 0.6546 0.1589 0.047 Uiso 0.5 1 calc R U P D 3
C43C C 0.0310(6) 0.840(3) 0.2012(17) 0.050(7) Uiso 0.5 1 d G . P D 3
H43C H 0.0195 0.8801 0.1575 0.061 Uiso 0.5 1 calc R U P D 3
C44C C 0.0445(7) 0.9160(19) 0.264(2) 0.059(9) Uiso 0.5 1 d G . P D 3
H44C H 0.0422 1.0076 0.2638 0.071 Uiso 0.5 1 calc R U P D 3
C45C C 0.0613(6) 0.858(2) 0.3284(17) 0.066(10) Uiso 0.5 1 d G . P D 3
H45C H 0.0705 0.9094 0.3716 0.079 Uiso 0.5 1 calc R U P D 3
C46C C 0.0647(5) 0.724(3) 0.3293(15) 0.043(7) Uiso 0.5 1 d G . P D 3
H46C H 0.0762 0.6839 0.3730 0.052 Uiso 0.5 1 calc R U P D 3
C41D C 0.0520(6) 0.6174(19) 0.2788(16) 0.027(4) Uiso 0.5 1 d G . P D 4
C42D C 0.0395(6) 0.697(2) 0.2161(14) 0.039(5) Uiso 0.5 1 d G . P D 4
H42D H 0.0321 0.6608 0.1634 0.047 Uiso 0.5 1 calc R U P D 4
C43D C 0.0376(6) 0.830(2) 0.2303(17) 0.050(7) Uiso 0.5 1 d G . P D 4
H43D H 0.0291 0.8845 0.1875 0.061 Uiso 0.5 1 calc R U P D 4
C44D C 0.0484(7) 0.8833(19) 0.3074(19) 0.059(9) Uiso 0.5 1 d G . P D 4
H44D H 0.0471 0.9741 0.3171 0.071 Uiso 0.5 1 calc R U P D 4
C45D C 0.0609(6) 0.804(3) 0.3701(15) 0.066(10) Uiso 0.5 1 d G . P D 4
H45D H 0.0682 0.8400 0.4227 0.079 Uiso 0.5 1 calc R U P D 4
C46D C 0.0627(5) 0.671(2) 0.3558(14) 0.043(7) Uiso 0.5 1 d G . P D 4
H46D H 0.0713 0.6162 0.3986 0.052 Uiso 0.5 1 calc R U P D 4
C50 C 0.1844(3) 0.6129(13) -0.0719(8) 0.015(3) Uani 1 1 d . U . . .
H501 H 0.1947 0.6050 -0.1276 0.018 Uiso 1 1 calc R U . . .
H502 H 0.1687 0.5491 -0.0729 0.018 Uiso 1 1 calc R U . . .
C51 C 0.2042(3) 0.5816(14) 0.0023(9) 0.016(3) Uani 1 1 d . U . . .
O51 O 0.2047(2) 0.6553(10) 0.0698(6) 0.021(2) Uani 1 1 d . . . . .
O52 O 0.2190(2) 0.4828(11) -0.0036(7) 0.033(3) Uani 1 1 d . . . . .
C60 C 0.2156(3) 0.9829(16) 0.0762(10) 0.028(4) Uani 1 1 d . . . . .
H601 H 0.2251 1.0671 0.0655 0.034 Uiso 1 1 calc R U . . .
H602 H 0.2271 0.9137 0.0492 0.034 Uiso 1 1 calc R U . . .
C61 C 0.2137(3) 0.9589(14) 0.1756(9) 0.020(3) Uani 1 1 d . . . . .
O61 O 0.1926(2) 0.8972(10) 0.2034(6) 0.024(2) Uani 1 1 d . . . . .
O62 O 0.2335(2) 1.0029(12) 0.2219(7) 0.038(3) Uani 1 1 d . . . . .
C70 C 0.1279(3) 1.0268(13) 0.1970(8) 0.017(3) Uani 1 1 d . U . . .
H701 H 0.1114 1.0840 0.2068 0.020 Uiso 1 1 calc R U . . .
H702 H 0.1453 1.0765 0.2122 0.020 Uiso 1 1 calc R U . . .
C71 C 0.1259(3) 0.9100(13) 0.2568(8) 0.016(3) Uani 1 1 d . . . . .
O71 O 0.12751(19) 0.7981(8) 0.2194(6) 0.0145(19) Uani 1 1 d . U . . .
O72 O 0.1244(2) 0.9278(10) 0.3361(6) 0.023(2) Uani 1 1 d . U . . .
N1A N 0.2257(3) 0.6686(12) 0.3414(8) 0.022(3) Uani 1 1 d . . . . .
H11A H 0.2083 0.6804 0.3203 0.027 Uiso 1 1 d R U . . .
H12A H 0.2343 0.7319 0.3482 0.027 Uiso 1 1 d R U . . .
H13A H 0.2187 0.6401 0.4004 0.027 Uiso 1 1 d R U . . .
H14A H 0.2376 0.6164 0.3199 0.027 Uiso 1 1 d R U . . .
O1W O 0.1792(2) 0.3794(9) 0.1879(6) 0.021(2) Uani 1 1 d . . . . .
H11W H 0.1697 0.3964 0.1518 0.025 Uiso 1 1 d R U . . .
H12W H 0.1978 0.3605 0.1755 0.025 Uiso 1 1 d R U . . .
O2W O 0.2387(2) 0.3799(10) 0.1458(7) 0.029(3) Uani 1 1 d . . . . .
H21W H 0.2408 0.4538 0.1696 0.035 Uiso 1 1 d R U . . .
H22W H 0.2297 0.4237 0.0987 0.035 Uiso 1 1 d R U . . .
O3W O 0.1448(2) 0.6784(11) 0.3941(7) 0.032(3) Uani 1 1 d . . . . .
H31W H 0.1332 0.6531 0.4329 0.039 Uiso 1 1 d R U . . .
H32W H 0.1338 0.7505 0.3725 0.039 Uiso 1 1 d R U . . .


_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
Nd1 O71 2.380(9) . ?
Nd1 O11 2.380(8) . ?
Nd1 O51 2.438(10) . ?
Nd1 O61 2.442(9) . ?
Nd1 O1C 2.624(8) . ?
Nd1 N4 2.705(10) . ?
Nd1 N7 2.731(10) . ?
Nd1 N10 2.746(11) . ?
Nd1 N1 2.752(9) . ?
O1C H11C 0.7194 . ?
O1C H12C 0.8991 . ?
N1 C2 1.477(15) . ?
N1 C20 1.489(16) . ?
N1 C12 1.501(15) . ?
C2 C3 1.504(17) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.482(15) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.482(17) . ?
N4 C5 1.517(16) . ?
C5 C6 1.503(19) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.490(16) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.486(17) . ?
N7 C8 1.491(18) . ?
C8 C9 1.484(18) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.487(16) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.462(16) . ?
N10 C11 1.476(16) . ?
C11 C12 1.513(17) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.830(13) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.497(9) . ?
P1 O11 1.521(9) . ?
P1 C21 1.822(14) . ?
C21 N22 1.430(17) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C30 1.46(2) . ?
N22 C40 1.50(2) . ?
C30 C31 1.49(2) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C32B 1.30(4) . ?
C31 C36B 1.38(3) . ?
C31 C36A 1.42(4) . ?
C31 C32A 1.43(4) . ?
C32A C33A 1.37(5) . ?
C32A H32A 0.9500 . ?
C33A C34 1.33(5) . ?
C33A H33A 0.9500 . ?
C34 C35A 1.26(5) . ?
C34 C35B 1.33(5) . ?
C34 C33B 1.44(4) . ?
C34 H34 0.9500 . ?
C35A C36A 1.38(6) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C32B C33B 1.44(5) . ?
C32B H32B 0.9500 . ?
C33B H33B 0.9500 . ?
C35B C36B 1.39(5) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C40 C41D 1.34(3) . ?
C40 C41C 1.64(3) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C40 H403 0.9900 . ?
C40 H404 0.9900 . ?
C41C C42C 1.3900 . ?
C41C C46C 1.3900 . ?
C42C C43C 1.3900 . ?
C42C H42C 0.9500 . ?
C43C C44C 1.3900 . ?
C43C H43C 0.9500 . ?
C44C C45C 1.3900 . ?
C44C H44C 0.9500 . ?
C45C C46C 1.3900 . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
C41D C42D 1.3900 . ?
C41D C46D 1.3900 . ?
C42D C43D 1.3900 . ?
C42D H42D 0.9500 . ?
C43D C44D 1.3900 . ?
C43D H43D 0.9500 . ?
C44D C45D 1.3900 . ?
C44D H44D 0.9500 . ?
C45D C46D 1.3900 . ?
C45D H45D 0.9500 . ?
C46D H46D 0.9500 . ?
C50 C51 1.498(18) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.238(17) . ?
C51 O51 1.283(17) . ?
C60 C61 1.55(2) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.252(17) . ?
C61 O61 1.258(17) . ?
C70 C71 1.517(18) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.231(16) . ?
C71 O71 1.291(16) . ?
N1A H11A 0.8880 . ?
N1A H12A 0.7733 . ?
N1A H13A 1.0093 . ?
N1A H14A 0.8449 . ?
O1W H11W 0.7306 . ?
O1W H12W 0.9181 . ?
O2W H21W 0.8495 . ?
O2W H22W 0.9467 . ?
O3W H31W 0.8512 . ?
O3W H32W 0.9610 . ?

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
O71 Nd1 O11 87.3(3) . . ?
O71 Nd1 O51 143.0(3) . . ?
O11 Nd1 O51 78.7(3) . . ?
O71 Nd1 O61 84.7(3) . . ?
O11 Nd1 O61 139.7(3) . . ?
O51 Nd1 O61 84.4(4) . . ?
O71 Nd1 O1C 69.0(3) . . ?
O11 Nd1 O1C 70.6(3) . . ?
O51 Nd1 O1C 74.1(3) . . ?
O61 Nd1 O1C 69.6(3) . . ?
O71 Nd1 N4 148.6(3) . . ?
O11 Nd1 N4 82.8(3) . . ?
O51 Nd1 N4 63.4(3) . . ?
O61 Nd1 N4 121.3(3) . . ?
O1C Nd1 N4 133.4(3) . . ?
O71 Nd1 N7 119.8(3) . . ?
O11 Nd1 N7 149.2(3) . . ?
O51 Nd1 N7 85.9(3) . . ?
O61 Nd1 N7 63.4(3) . . ?
O1C Nd1 N7 130.3(3) . . ?
N4 Nd1 N7 66.4(3) . . ?
O71 Nd1 N10 62.1(3) . . ?
O11 Nd1 N10 125.5(3) . . ?
O51 Nd1 N10 150.8(3) . . ?
O61 Nd1 N10 84.4(3) . . ?
O1C Nd1 N10 126.1(3) . . ?
N4 Nd1 N10 100.4(3) . . ?
N7 Nd1 N10 65.0(3) . . ?
O71 Nd1 N1 83.0(3) . . ?
O11 Nd1 N1 65.9(3) . . ?
O51 Nd1 N1 120.3(3) . . ?
O61 Nd1 N1 150.8(3) . . ?
O1C Nd1 N1 128.8(3) . . ?
N4 Nd1 N1 65.8(3) . . ?
N7 Nd1 N1 100.7(3) . . ?
N10 Nd1 N1 66.5(3) . . ?
Nd1 O1C H11C 105.4 . . ?
Nd1 O1C H12C 125.4 . . ?
H11C O1C H12C 116.0 . . ?
C2 N1 C20 109.3(9) . . ?
C2 N1 C12 110.3(9) . . ?
C20 N1 C12 109.9(9) . . ?
C2 N1 Nd1 110.1(7) . . ?
C20 N1 Nd1 106.3(7) . . ?
C12 N1 Nd1 110.9(7) . . ?
N1 C2 C3 113.4(10) . . ?
N1 C2 H21 108.9 . . ?
C3 C2 H21 108.9 . . ?
N1 C2 H22 108.9 . . ?
C3 C2 H22 108.9 . . ?
H21 C2 H22 107.7 . . ?
N4 C3 C2 111.7(10) . . ?
N4 C3 H31 109.3 . . ?
C2 C3 H31 109.3 . . ?
N4 C3 H32 109.3 . . ?
C2 C3 H32 109.3 . . ?
H31 C3 H32 107.9 . . ?
C3 N4 C50 110.6(10) . . ?
C3 N4 C5 110.0(9) . . ?
C50 N4 C5 108.0(10) . . ?
C3 N4 Nd1 114.0(7) . . ?
C50 N4 Nd1 103.7(7) . . ?
C5 N4 Nd1 110.2(7) . . ?
C6 C5 N4 112.0(10) . . ?
C6 C5 H51 109.2 . . ?
N4 C5 H51 109.2 . . ?
C6 C5 H52 109.2 . . ?
N4 C5 H52 109.2 . . ?
H51 C5 H52 107.9 . . ?
N7 C6 C5 112.1(11) . . ?
N7 C6 H61 109.2 . . ?
C5 C6 H61 109.2 . . ?
N7 C6 H62 109.2 . . ?
C5 C6 H62 109.2 . . ?
H61 C6 H62 107.9 . . ?
C60 N7 C6 110.0(11) . . ?
C60 N7 C8 108.6(11) . . ?
C6 N7 C8 110.5(10) . . ?
C60 N7 Nd1 103.2(8) . . ?
C6 N7 Nd1 113.0(8) . . ?
C8 N7 Nd1 111.1(8) . . ?
C9 C8 N7 113.1(11) . . ?
C9 C8 H81 109.0 . . ?
N7 C8 H81 109.0 . . ?
C9 C8 H82 109.0 . . ?
N7 C8 H82 109.0 . . ?
H81 C8 H82 107.8 . . ?
C8 C9 N10 111.2(11) . . ?
C8 C9 H91 109.4 . . ?
N10 C9 H91 109.4 . . ?
C8 C9 H92 109.4 . . ?
N10 C9 H92 109.4 . . ?
H91 C9 H92 108.0 . . ?
C70 N10 C11 108.8(10) . . ?
C70 N10 C9 111.4(10) . . ?
C11 N10 C9 110.4(10) . . ?
C70 N10 Nd1 102.2(7) . . ?
C11 N10 Nd1 110.0(7) . . ?
C9 N10 Nd1 113.7(7) . . ?
N10 C11 C12 112.0(10) . . ?
N10 C11 H111 109.2 . . ?
C12 C11 H111 109.2 . . ?
N10 C11 H112 109.2 . . ?
C12 C11 H112 109.2 . . ?
H111 C11 H112 107.9 . . ?
N1 C12 C11 113.3(9) . . ?
N1 C12 H121 108.9 . . ?
C11 C12 H121 108.9 . . ?
N1 C12 H122 108.9 . . ?
C11 C12 H122 108.9 . . ?
H121 C12 H122 107.7 . . ?
N1 C20 P1 110.6(8) . . ?
N1 C20 H201 109.5 . . ?
P1 C20 H201 109.5 . . ?
N1 C20 H202 109.5 . . ?
P1 C20 H202 109.5 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 116.3(5) . . ?
O12 P1 C21 111.0(6) . . ?
O11 P1 C21 109.1(5) . . ?
O12 P1 C20 111.4(6) . . ?
O11 P1 C20 104.6(5) . . ?
C21 P1 C20 103.6(7) . . ?
P1 O11 Nd1 127.3(5) . . ?
N22 C21 P1 110.8(9) . . ?
N22 C21 H211 109.5 . . ?
P1 C21 H211 109.5 . . ?
N22 C21 H212 109.5 . . ?
P1 C21 H212 109.5 . . ?
H211 C21 H212 108.1 . . ?
C21 N22 C30 112.0(12) . . ?
C21 N22 C40 112.4(12) . . ?
C30 N22 C40 110.7(13) . . ?
N22 C30 C31 112.9(13) . . ?
N22 C30 H301 109.0 . . ?
C31 C30 H301 109.0 . . ?
N22 C30 H302 109.0 . . ?
C31 C30 H302 109.0 . . ?
H301 C30 H302 107.8 . . ?
C32B C31 C36B 121(2) . . ?
C36A C31 C32A 114(2) . . ?
C32B C31 C30 114(2) . . ?
C36B C31 C30 125(2) . . ?
C36A C31 C30 120(2) . . ?
C32A C31 C30 125.9(18) . . ?
C33A C32A C31 125(3) . . ?
C33A C32A H32A 117.6 . . ?
C31 C32A H32A 117.6 . . ?
C34 C33A C32A 117(4) . . ?
C34 C33A H33A 121.7 . . ?
C32A C33A H33A 121.7 . . ?
C35A C34 C33A 120(3) . . ?
C35B C34 C33B 118(3) . . ?
C35A C34 H34 120.1 . . ?
C33A C34 H34 120.1 . . ?
C34 C35A C36A 129(4) . . ?
C34 C35A H35A 115.3 . . ?
C36A C35A H35A 115.3 . . ?
C35A C36A C31 115(3) . . ?
C35A C36A H36A 122.6 . . ?
C31 C36A H36A 122.6 . . ?
C31 C32B C33B 120(3) . . ?
C31 C32B H32B 119.9 . . ?
C33B C32B H32B 119.9 . . ?
C32B C33B C34 119(4) . . ?
C32B C33B H33B 120.7 . . ?
C34 C33B H33B 120.7 . . ?
C34 C35B C36B 121(4) . . ?
C34 C35B H35B 119.5 . . ?
C36B C35B H35B 119.5 . . ?
C31 C36B C35B 121(3) . . ?
C31 C36B H36B 119.7 . . ?
C35B C36B H36B 119.7 . . ?
C41D C40 N22 117.6(18) . . ?
N22 C40 C41C 110.4(16) . . ?
N22 C40 H401 109.6 . . ?
C41C C40 H401 109.6 . . ?
N22 C40 H402 109.6 . . ?
C41C C40 H402 109.6 . . ?
H401 C40 H402 108.1 . . ?
C41D C40 H403 107.9 . . ?
N22 C40 H403 107.9 . . ?
C41D C40 H404 107.9 . . ?
N22 C40 H404 107.9 . . ?
H403 C40 H404 107.2 . . ?
C42C C41C C46C 120.0 . . ?
C42C C41C C40 117.4(16) . . ?
C46C C41C C40 122.6(16) . . ?
C43C C42C C41C 120.0 . . ?
C43C C42C H42C 120.0 . . ?
C41C C42C H42C 120.0 . . ?
C42C C43C C44C 120.0 . . ?
C42C C43C H43C 120.0 . . ?
C44C C43C H43C 120.0 . . ?
C43C C44C C45C 120.0 . . ?
C43C C44C H44C 120.0 . . ?
C45C C44C H44C 120.0 . . ?
C46C C45C C44C 120.0 . . ?
C46C C45C H45C 120.0 . . ?
C44C C45C H45C 120.0 . . ?
C45C C46C C41C 120.0 . . ?
C45C C46C H46C 120.0 . . ?
C41C C46C H46C 120.0 . . ?
C40 C41D C42D 119.3(18) . . ?
C40 C41D C46D 120.6(18) . . ?
C42D C41D C46D 120.0 . . ?
C43D C42D C41D 120.0 . . ?
C43D C42D H42D 120.0 . . ?
C41D C42D H42D 120.0 . . ?
C42D C43D C44D 120.0 . . ?
C42D C43D H43D 120.0 . . ?
C44D C43D H43D 120.0 . . ?
C43D C44D C45D 120.0 . . ?
C43D C44D H44D 120.0 . . ?
C45D C44D H44D 120.0 . . ?
C46D C45D C44D 120.0 . . ?
C46D C45D H45D 120.0 . . ?
C44D C45D H45D 120.0 . . ?
C45D C46D C41D 120.0 . . ?
C45D C46D H46D 120.0 . . ?
C41D C46D H46D 120.0 . . ?
N4 C50 C51 112.2(11) . . ?
N4 C50 H501 109.2 . . ?
C51 C50 H501 109.2 . . ?
N4 C50 H502 109.2 . . ?
C51 C50 H502 109.2 . . ?
H501 C50 H502 107.9 . . ?
O52 C51 O51 122.7(13) . . ?
O52 C51 C50 118.0(12) . . ?
O51 C51 C50 119.3(12) . . ?
C51 O51 Nd1 118.2(8) . . ?
N7 C60 C61 110.3(12) . . ?
N7 C60 H601 109.6 . . ?
C61 C60 H601 109.6 . . ?
N7 C60 H602 109.6 . . ?
C61 C60 H602 109.6 . . ?
H601 C60 H602 108.1 . . ?
O62 C61 O61 125.4(13) . . ?
O62 C61 C60 116.6(13) . . ?
O61 C61 C60 118.1(12) . . ?
C61 O61 Nd1 122.4(9) . . ?
N10 C70 C71 113.1(11) . . ?
N10 C70 H701 109.0 . . ?
C71 C70 H701 109.0 . . ?
N10 C70 H702 109.0 . . ?
C71 C70 H702 109.0 . . ?
H701 C70 H702 107.8 . . ?
O72 C71 O71 125.2(12) . . ?
O72 C71 C70 118.9(12) . . ?
O71 C71 C70 115.8(11) . . ?
C71 O71 Nd1 117.9(8) . . ?
H11A N1A H12A 114.4 . . ?
H11A N1A H13A 93.0 . . ?
H12A N1A H13A 107.6 . . ?
H11A N1A H14A 123.9 . . ?
H12A N1A H14A 104.0 . . ?
H13A N1A H14A 113.0 . . ?
H11W O1W H12W 118.2 . . ?
H21W O2W H22W 87.0 . . ?
H31W O3W H32W 97.6 . . ?

_refine_diff_density_max         3.271
_refine_diff_density_min         -7.708
_refine_diff_density_rms         0.257

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

data_gd-dbam
_database_code_depnum_ccdc_archive 'CCDC 1959630'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H42 Gd N5 O9 P, Ca0.5 O3 H6, 3(H2 O)'
_chemical_formula_sum            'C30 H54 Ca0.50 Gd N5 O15 P'
_chemical_formula_weight         933.04

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'
Ca Ca 0.2262 0.3064 '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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_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'
'x, -y, z-1/2'

_cell_length_a                   24.2222(7)
_cell_length_b                   10.1613(2)
_cell_length_c                   15.4093(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.4550(10)
_cell_angle_gamma                90
_cell_volume                     3775.50(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9940
_cell_measurement_theta_min      2.5899
_cell_measurement_theta_max      27.4911

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_F_000             1912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.475
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.092
_exptl_absorpt_coefficient_mu    1.941
_shelx_estimated_absorpt_T_min   0.459
_shelx_estimated_absorpt_T_max   0.842
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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 8.3333
_diffrn_reflns_number            31807
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.689
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8663
_reflns_number_gt                7451
_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.
 
 _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 Instrument Service v2014.11.0.1'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0683P)²+25.5694P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8663
_refine_ls_number_parameters     495
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0616
_refine_ls_wR_factor_ref         0.1548
_refine_ls_wR_factor_gt          0.1484
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_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_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
Gd1 Gd 0.31473(2) 0.28123(3) 0.45432(2) 0.02987(11) Uani 1 1 d . . . . .
O1C O 0.3428(3) 0.1468(6) 0.3175(5) 0.076(2) Uani 1 1 d . . . . .
H11C H 0.3356 0.0720 0.3133 0.092 Uiso 1 1 d R U . . .
H12C H 0.3678 0.1729 0.2843 0.092 Uiso 1 1 d R U . . .
N1 N 0.22145(19) 0.2534(5) 0.5357(3) 0.0254(9) Uani 1 1 d . . . . .
C2 C 0.2348(3) 0.1917(7) 0.6237(4) 0.0362(14) Uani 1 1 d . . . . .
H21 H 0.2417 0.0964 0.6164 0.043 Uiso 1 1 calc R U . . .
H22 H 0.2025 0.2013 0.6581 0.043 Uiso 1 1 calc R U . . .
C3 C 0.2848(3) 0.2536(7) 0.6727(4) 0.0411(15) Uani 1 1 d . . . . .
H31 H 0.2773 0.3480 0.6824 0.049 Uiso 1 1 calc R U . . .
H32 H 0.2919 0.2108 0.7304 0.049 Uiso 1 1 calc R U . . .
N4 N 0.3344(2) 0.2412(6) 0.6249(4) 0.0403(13) Uani 1 1 d . . . . .
C5 C 0.3780(3) 0.3348(8) 0.6625(5) 0.0518(19) Uani 1 1 d . . . . .
H51 H 0.4144 0.3075 0.6442 0.062 Uiso 1 1 calc R U . . .
H52 H 0.3802 0.3300 0.7269 0.062 Uiso 1 1 calc R U . . .
C6 C 0.3665(3) 0.4748(7) 0.6343(4) 0.0467(17) Uani 1 1 d . . . . .
H61 H 0.3309 0.5039 0.6545 0.056 Uiso 1 1 calc R U . . .
H62 H 0.3962 0.5328 0.6612 0.056 Uiso 1 1 calc R U . . .
N7 N 0.3638(2) 0.4865(6) 0.5373(3) 0.0396(13) Uani 1 1 d . . . . .
C8 C 0.3357(3) 0.6139(7) 0.5092(4) 0.0387(14) Uani 1 1 d . . . . .
H81 H 0.3487 0.6843 0.5506 0.046 Uiso 1 1 calc R U . . .
H82 H 0.3463 0.6386 0.4509 0.046 Uiso 1 1 calc R U . . .
C9 C 0.2740(2) 0.6036(6) 0.5057(3) 0.0306(12) Uani 1 1 d . . . . .
H91 H 0.2631 0.5869 0.5650 0.037 Uiso 1 1 calc R U . . .
H92 H 0.2572 0.6881 0.4850 0.037 Uiso 1 1 calc R U . . .
N10 N 0.25254(19) 0.4961(5) 0.4467(3) 0.0250(9) Uani 1 1 d . . . . .
C11 C 0.1946(2) 0.4629(6) 0.4648(3) 0.0280(11) Uani 1 1 d . . . . .
H111 H 0.1760 0.4147 0.4144 0.034 Uiso 1 1 calc R U . . .
H112 H 0.1737 0.5453 0.4720 0.034 Uiso 1 1 calc R U . . .
C12 C 0.1932(2) 0.3803(6) 0.5454(3) 0.0282(11) Uani 1 1 d . . . . .
H121 H 0.2116 0.4283 0.5960 0.034 Uiso 1 1 calc R U . . .
H122 H 0.1542 0.3642 0.5566 0.034 Uiso 1 1 calc R U . . .
C20 C 0.1845(2) 0.1623(6) 0.4828(3) 0.0261(11) Uani 1 1 d . . . . .
H201 H 0.1686 0.2076 0.4292 0.031 Uiso 1 1 calc R U . . .
H202 H 0.1535 0.1352 0.5163 0.031 Uiso 1 1 calc R U . . .
P1 P 0.22324(6) 0.01661(15) 0.45331(9) 0.0279(3) Uani 1 1 d . . . . .
O11 O 0.28314(17) 0.0643(4) 0.4538(3) 0.0339(9) Uani 1 1 d . . . . .
O12 O 0.2138(2) -0.0973(5) 0.5113(3) 0.0415(10) Uani 1 1 d . . . . .
C21 C 0.1964(3) -0.0158(6) 0.3416(4) 0.0341(13) Uani 1 1 d . . . . .
H211 H 0.2020 0.0623 0.3050 0.041 Uiso 1 1 calc R U . . .
H212 H 0.2165 -0.0908 0.3184 0.041 Uiso 1 1 calc R U . . .
N22 N 0.1368(2) -0.0466(5) 0.3383(3) 0.0345(11) Uani 1 1 d . . . . .
C30 C 0.1277(3) -0.1870(7) 0.3555(6) 0.0495(18) Uani 1 1 d . . . . .
H301 H 0.1578 -0.2191 0.3982 0.059 Uiso 1 1 calc R U . . .
H302 H 0.1296 -0.2371 0.3008 0.059 Uiso 1 1 calc R U . . .
C31 C 0.0724(3) -0.2136(6) 0.3905(5) 0.0381(14) Uani 1 1 d . . . . .
C32A C 0.0516(6) -0.3375(16) 0.3866(10) 0.051(4) Uani 0.503(10) 1 d . . P A 1
H32A H 0.0722 -0.4060 0.3627 0.061 Uiso 0.503(10) 1 calc R U P A 1
C33A C 0.0013(7) -0.3658(18) 0.4166(12) 0.065(5) Uani 0.503(10) 1 d . . P A 1
H33A H -0.0149 -0.4502 0.4067 0.078 Uiso 0.503(10) 1 calc R U P A 1
C32B C 0.0224(7) -0.2507(14) 0.3372(12) 0.055(5) Uani 0.497(10) 1 d . . P A 2
H32B H 0.0225 -0.2577 0.2757 0.066 Uiso 0.497(10) 1 calc R U P A 2
C33B C -0.0249(6) -0.2755(13) 0.3759(14) 0.057(5) Uani 0.497(10) 1 d . . P A 2
H33B H -0.0577 -0.2989 0.3405 0.068 Uiso 0.497(10) 1 calc R U P A 2
C34 C -0.0266(4) -0.2678(10) 0.4629(8) 0.069(3) Uani 1 1 d . . . . .
H341 H -0.0598 -0.2871 0.4885 0.083 Uiso 1 1 d R U . A .
C35A C -0.0062(7) -0.144(2) 0.4655(14) 0.070(6) Uani 0.503(10) 1 d . . P A 1
H35A H -0.0264 -0.0744 0.4893 0.085 Uiso 0.503(10) 1 calc R U P A 1
C36A C 0.0435(6) -0.1181(15) 0.4337(11) 0.053(4) Uani 0.503(10) 1 d . . P A 1
H36A H 0.0590 -0.0325 0.4411 0.063 Uiso 0.503(10) 1 calc R U P A 1
C35B C 0.0231(7) -0.2287(17) 0.5165(13) 0.057(4) Uani 0.497(10) 1 d . . P A 2
H35B H 0.0233 -0.2205 0.5779 0.069 Uiso 0.497(10) 1 calc R U P A 2
C36B C 0.0710(6) -0.2032(14) 0.4744(10) 0.043(3) Uani 0.497(10) 1 d . . P A 2
H36B H 0.1038 -0.1773 0.5088 0.051 Uiso 0.497(10) 1 calc R U P A 2
C40 C 0.1063(3) -0.0073(9) 0.2554(4) 0.057(2) Uani 1 1 d . . . . .
H401 H 0.1237 -0.0520 0.2078 0.069 Uiso 0.527(10) 1 calc R U P B 3
H402 H 0.0681 -0.0420 0.2548 0.069 Uiso 0.527(10) 1 calc R U P B 3
H403 H 0.0696 -0.0510 0.2483 0.069 Uiso 0.473(10) 1 calc R U P B 4
H404 H 0.1272 -0.0328 0.2059 0.069 Uiso 0.473(10) 1 calc R U P B 4
C41C C 0.1027(7) 0.1196(9) 0.2361(8) 0.034(3) Uani 0.527(10) 1 d G . P B 3
C42C C 0.0782(7) 0.1978(12) 0.2957(8) 0.049(4) Uani 0.527(10) 1 d G . P B 3
H42C H 0.0652 0.1591 0.3461 0.059 Uiso 0.527(10) 1 calc R U P B 3
C43C C 0.0727(7) 0.3324(12) 0.2816(9) 0.075(5) Uani 0.527(10) 1 d G . P B 3
H43C H 0.0560 0.3859 0.3224 0.090 Uiso 0.527(10) 1 calc R U P B 3
C44C C 0.0918(6) 0.3889(10) 0.2079(9) 0.067(3) Uani 0.527(10) 1 d G U P B 3
H44C H 0.0881 0.4810 0.1983 0.080 Uiso 0.527(10) 1 calc R U P B 3
C45C C 0.1163(6) 0.3108(13) 0.1483(8) 0.082(4) Uani 0.527(10) 1 d G U P B 3
H45C H 0.1293 0.3494 0.0979 0.098 Uiso 0.527(10) 1 calc R U P B 3
C46C C 0.1218(6) 0.1761(12) 0.1624(8) 0.068(4) Uani 0.527(10) 1 d G . P B 3
H46C H 0.1386 0.1226 0.1216 0.081 Uiso 0.527(10) 1 calc R U P B 3
C41D C 0.0985(7) 0.1584(11) 0.2581(9) 0.034(3) Uani 0.473(10) 1 d G . P B 4
C42D C 0.0661(8) 0.2187(14) 0.3165(11) 0.049(4) Uani 0.473(10) 1 d G . P B 4
H42D H 0.0482 0.1669 0.3569 0.059 Uiso 0.473(10) 1 calc R U P B 4
C43D C 0.0599(7) 0.3547(15) 0.3158(11) 0.075(5) Uani 0.473(10) 1 d G . P B 4
H43D H 0.0378 0.3958 0.3557 0.090 Uiso 0.473(10) 1 calc R U P B 4
C44D C 0.0860(6) 0.4304(11) 0.2566(11) 0.067(3) Uani 0.473(10) 1 d G U P B 4
H44D H 0.0817 0.5233 0.2561 0.080 Uiso 0.473(10) 1 calc R U P B 4
C45D C 0.1183(6) 0.3702(14) 0.1983(10) 0.082(4) Uani 0.473(10) 1 d G U P B 4
H45D H 0.1362 0.4219 0.1579 0.098 Uiso 0.473(10) 1 calc R U P B 4
C46D C 0.1246(6) 0.2342(14) 0.1990(9) 0.068(4) Uani 0.473(10) 1 d G . P B 4
H46D H 0.1467 0.1930 0.1591 0.081 Uiso 0.473(10) 1 calc R U P B 4
C50 C 0.3576(3) 0.1071(8) 0.6301(5) 0.0522(19) Uani 1 1 d . . . . .
H501 H 0.3268 0.0427 0.6247 0.063 Uiso 1 1 calc R U . . .
H502 H 0.3785 0.0946 0.6880 0.063 Uiso 1 1 calc R U . . .
C51 C 0.3958(4) 0.0800(10) 0.5599(7) 0.075(3) Uani 1 1 d . . . . .
O51 O 0.39711(19) 0.1627(6) 0.4985(4) 0.0572(14) Uani 1 1 d . . . . .
O52 O 0.4224(4) -0.0283(9) 0.5618(7) 0.118(3) Uani 1 1 d . . . . .
C60 C 0.4197(3) 0.4915(8) 0.5070(6) 0.054(2) Uani 1 1 d . . . . .
H601 H 0.4430 0.4202 0.5348 0.064 Uiso 1 1 calc R U . . .
H602 H 0.4375 0.5767 0.5236 0.064 Uiso 1 1 calc R U . . .
C61 C 0.4154(3) 0.4757(8) 0.4080(6) 0.055(2) Uani 1 1 d . . . . .
O61 O 0.3767(2) 0.4027(5) 0.3739(4) 0.0515(13) Uani 1 1 d . . . . .
O62 O 0.4503(2) 0.5348(6) 0.3679(5) 0.0687(18) Uani 1 1 d . . . . .
C70 C 0.2516(3) 0.5355(6) 0.3549(3) 0.0339(13) Uani 1 1 d . . . . .
H701 H 0.2859 0.5849 0.3462 0.041 Uiso 1 1 calc R U . . .
H702 H 0.2196 0.5945 0.3398 0.041 Uiso 1 1 calc R U . . .
C71 C 0.2473(3) 0.4162(6) 0.2948(3) 0.0333(13) Uani 1 1 d . . . . .
O71 O 0.2529(2) 0.3044(4) 0.3310(2) 0.0367(10) Uani 1 1 d . . . . .
O72 O 0.2399(2) 0.4347(5) 0.2151(2) 0.0491(13) Uani 1 1 d . . . . .
O1W O 0.2716(3) 0.1682(5) 0.1639(3) 0.0627(17) Uani 1 1 d . . . . .
H11W H 0.2579 0.2355 0.1756 0.075 Uiso 1 1 d R U . . .
H12W H 0.2596 0.1549 0.1078 0.075 Uiso 1 1 d R U . . .
O2W O 0.3491(3) 0.8845(6) 0.3673(4) 0.0674(16) Uani 1 1 d . . . . .
H21W H 0.3828 0.8603 0.3725 0.081 Uiso 1 1 d R U . . .
H22W H 0.3417 0.9068 0.4217 0.081 Uiso 1 1 d R U . . .
O3W O 0.4618(3) 0.8020(8) 0.3859(5) 0.086(2) Uani 1 1 d . . . . .
H31W H 0.4738 0.7885 0.3344 0.103 Uiso 1 1 d R U . . .
H32W H 0.4780 0.7962 0.4380 0.103 Uiso 1 1 d R U . . .
Ca1 Ca 0.5000 0.1889(2) 0.2500 0.0550(6) Uani 1 2 d S T P . .
O4W O 0.4851(4) 0.1671(9) 0.3961(5) 0.097(2) Uiso 1 1 d . . . . .
O5W O 0.5000 0.3954(9) 0.2500 0.071(2) Uiso 1 2 d S . P C .
O6W O 0.5000 -0.0395(13) 0.2500 0.106(4) Uiso 1 2 d S . P C .
O7WA O 0.4207(4) 0.1926(9) 0.2038(6) 0.045(2) Uiso 0.55 1 d . . P C 5
O7WB O 0.4384(5) 0.2464(11) 0.2979(7) 0.043(2) Uiso 0.45 1 d . . P C 6


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O71 2.317(4) . ?
Gd1 O11 2.333(4) . ?
Gd1 O51 2.374(5) . ?
Gd1 O61 2.380(5) . ?
Gd1 N10 2.649(5) . ?
Gd1 O1C 2.655(6) . ?
Gd1 N4 2.657(5) . ?
Gd1 N7 2.666(6) . ?
Gd1 N1 2.701(5) . ?
O1C H11C 0.7818 . ?
O1C H12C 0.8706 . ?
N1 C12 1.474(7) . ?
N1 C20 1.478(7) . ?
N1 C2 1.502(7) . ?
C2 C3 1.504(9) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.473(9) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.474(9) . ?
N4 C5 1.495(9) . ?
C5 C6 1.506(10) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.494(8) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.477(8) . ?
N7 C8 1.507(9) . ?
C8 C9 1.493(9) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.484(7) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.468(6) . ?
N10 C11 1.496(7) . ?
C11 C12 1.501(8) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.833(6) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.492(5) . ?
P1 O11 1.529(4) . ?
P1 C21 1.812(6) . ?
C21 N22 1.473(8) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C40 1.470(9) . ?
N22 C30 1.471(9) . ?
C30 C31 1.515(10) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36B 1.301(17) . ?
C31 C32A 1.355(16) . ?
C31 C36A 1.401(16) . ?
C31 C32B 1.448(15) . ?
C32A C33A 1.37(2) . ?
C32A H32A 0.9500 . ?
C33A C34 1.43(2) . ?
C33A H33A 0.9500 . ?
C32B C33B 1.37(3) . ?
C32B H32B 0.9500 . ?
C33B C34 1.35(2) . ?
C33B H33B 0.9500 . ?
C34 C35A 1.35(2) . ?
C34 C35B 1.448(19) . ?
C34 H341 0.9500 . ?
C35A C36A 1.37(2) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C35B C36B 1.41(2) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C40 C41C 1.324(13) . ?
C40 C41D 1.696(15) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C40 H403 0.9900 . ?
C40 H404 0.9900 . ?
C41C C42C 1.3900 . ?
C41C C46C 1.3900 . ?
C42C C43C 1.3900 . ?
C42C H42C 0.9500 . ?
C43C C44C 1.3900 . ?
C43C H43C 0.9500 . ?
C44C C45C 1.3900 . ?
C44C H44C 0.9500 . ?
C45C C46C 1.3900 . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
C41D C42D 1.3900 . ?
C41D C46D 1.3900 . ?
C42D C43D 1.3900 . ?
C42D H42D 0.9500 . ?
C43D C44D 1.3900 . ?
C43D H43D 0.9500 . ?
C44D C45D 1.3900 . ?
C44D H44D 0.9500 . ?
C45D C46D 1.3900 . ?
C45D H45D 0.9500 . ?
C46D H46D 0.9500 . ?
C50 C51 1.514(13) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O51 1.267(11) . ?
C51 O52 1.274(11) . ?
C60 C61 1.527(12) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.248(8) . ?
C61 O61 1.269(10) . ?
C70 C71 1.523(8) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.240(6) . ?
C71 O71 1.267(7) . ?
O1W H11W 0.7885 . ?
O1W H12W 0.8965 . ?
O2W H21W 0.8497 . ?
O2W H22W 0.9016 . ?
O3W H31W 0.8815 . ?
O3W H32W 0.8618 . ?
Ca1 O7WB 1.822(11) 2_655 ?
Ca1 O7WB 1.822(11) . ?
Ca1 O7WA 1.983(9) . ?
Ca1 O7WA 1.984(9) 2_655 ?
Ca1 O5W 2.098(10) . ?
Ca1 O6W 2.321(13) . ?
Ca1 O4W 2.324(8) . ?
Ca1 O4W 2.324(8) 2_655 ?

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
O71 Gd1 O11 84.66(15) . . ?
O71 Gd1 O51 138.33(19) . . ?
O11 Gd1 O51 77.77(17) . . ?
O71 Gd1 O61 84.88(19) . . ?
O11 Gd1 O61 135.33(16) . . ?
O51 Gd1 O61 81.86(19) . . ?
O71 Gd1 N10 63.85(14) . . ?
O11 Gd1 N10 126.42(14) . . ?
O51 Gd1 N10 152.84(18) . . ?
O61 Gd1 N10 86.17(16) . . ?
O71 Gd1 O1C 66.14(18) . . ?
O11 Gd1 O1C 67.66(16) . . ?
O51 Gd1 O1C 72.2(2) . . ?
O61 Gd1 O1C 68.38(18) . . ?
N10 Gd1 O1C 125.20(17) . . ?
O71 Gd1 N4 150.21(17) . . ?
O11 Gd1 N4 83.50(16) . . ?
O51 Gd1 N4 64.6(2) . . ?
O61 Gd1 N4 122.11(19) . . ?
N10 Gd1 N4 102.59(16) . . ?
O1C Gd1 N4 132.17(19) . . ?
O71 Gd1 N7 122.53(16) . . ?
O11 Gd1 N7 150.67(15) . . ?
O51 Gd1 N7 86.28(19) . . ?
O61 Gd1 N7 64.52(17) . . ?
N10 Gd1 N7 66.55(15) . . ?
O1C Gd1 N7 130.34(18) . . ?
N4 Gd1 N7 67.38(17) . . ?
O71 Gd1 N1 83.52(15) . . ?
O11 Gd1 N1 67.29(14) . . ?
O51 Gd1 N1 122.07(17) . . ?
O61 Gd1 N1 153.20(16) . . ?
N10 Gd1 N1 67.03(14) . . ?
O1C Gd1 N1 127.13(17) . . ?
N4 Gd1 N1 66.69(16) . . ?
N7 Gd1 N1 102.33(15) . . ?
Gd1 O1C H11C 119.6 . . ?
Gd1 O1C H12C 123.7 . . ?
H11C O1C H12C 114.3 . . ?
C12 N1 C20 110.0(4) . . ?
C12 N1 C2 109.6(4) . . ?
C20 N1 C2 107.7(4) . . ?
C12 N1 Gd1 111.8(3) . . ?
C20 N1 Gd1 107.4(3) . . ?
C2 N1 Gd1 110.2(3) . . ?
N1 C2 C3 111.8(5) . . ?
N1 C2 H21 109.2 . . ?
C3 C2 H21 109.2 . . ?
N1 C2 H22 109.2 . . ?
C3 C2 H22 109.2 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 111.7(5) . . ?
N4 C3 H31 109.3 . . ?
C2 C3 H31 109.3 . . ?
N4 C3 H32 109.3 . . ?
C2 C3 H32 109.3 . . ?
H31 C3 H32 107.9 . . ?
C3 N4 C50 112.2(6) . . ?
C3 N4 C5 109.3(6) . . ?
C50 N4 C5 108.4(5) . . ?
C3 N4 Gd1 113.8(3) . . ?
C50 N4 Gd1 103.1(4) . . ?
C5 N4 Gd1 109.9(4) . . ?
N4 C5 C6 112.6(5) . . ?
N4 C5 H51 109.1 . . ?
C6 C5 H51 109.1 . . ?
N4 C5 H52 109.1 . . ?
C6 C5 H52 109.1 . . ?
H51 C5 H52 107.8 . . ?
N7 C6 C5 110.7(6) . . ?
N7 C6 H61 109.5 . . ?
C5 C6 H61 109.5 . . ?
N7 C6 H62 109.5 . . ?
C5 C6 H62 109.5 . . ?
H61 C6 H62 108.1 . . ?
C60 N7 C6 111.4(5) . . ?
C60 N7 C8 106.4(5) . . ?
C6 N7 C8 109.3(6) . . ?
C60 N7 Gd1 104.8(5) . . ?
C6 N7 Gd1 113.2(4) . . ?
C8 N7 Gd1 111.5(4) . . ?
C9 C8 N7 111.9(5) . . ?
C9 C8 H81 109.2 . . ?
N7 C8 H81 109.2 . . ?
C9 C8 H82 109.2 . . ?
N7 C8 H82 109.2 . . ?
H81 C8 H82 107.9 . . ?
N10 C9 C8 111.4(5) . . ?
N10 C9 H91 109.3 . . ?
C8 C9 H91 109.3 . . ?
N10 C9 H92 109.3 . . ?
C8 C9 H92 109.3 . . ?
H91 C9 H92 108.0 . . ?
C70 N10 C9 111.2(5) . . ?
C70 N10 C11 108.2(4) . . ?
C9 N10 C11 109.4(4) . . ?
C70 N10 Gd1 103.0(3) . . ?
C9 N10 Gd1 114.5(3) . . ?
C11 N10 Gd1 110.2(3) . . ?
N10 C11 C12 112.0(4) . . ?
N10 C11 H111 109.2 . . ?
C12 C11 H111 109.2 . . ?
N10 C11 H112 109.2 . . ?
C12 C11 H112 109.2 . . ?
H111 C11 H112 107.9 . . ?
N1 C12 C11 111.0(4) . . ?
N1 C12 H121 109.4 . . ?
C11 C12 H121 109.4 . . ?
N1 C12 H122 109.4 . . ?
C11 C12 H122 109.4 . . ?
H121 C12 H122 108.0 . . ?
N1 C20 P1 110.1(4) . . ?
N1 C20 H201 109.6 . . ?
P1 C20 H201 109.6 . . ?
N1 C20 H202 109.6 . . ?
P1 C20 H202 109.6 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 116.2(3) . . ?
O12 P1 C21 111.5(3) . . ?
O11 P1 C21 108.5(3) . . ?
O12 P1 C20 111.5(3) . . ?
O11 P1 C20 104.5(2) . . ?
C21 P1 C20 103.7(3) . . ?
P1 O11 Gd1 127.6(2) . . ?
N22 C21 P1 109.5(4) . . ?
N22 C21 H211 109.8 . . ?
P1 C21 H211 109.8 . . ?
N22 C21 H212 109.8 . . ?
P1 C21 H212 109.8 . . ?
H211 C21 H212 108.2 . . ?
C40 N22 C30 110.4(6) . . ?
C40 N22 C21 112.5(5) . . ?
C30 N22 C21 111.3(5) . . ?
N22 C30 C31 113.0(5) . . ?
N22 C30 H301 109.0 . . ?
C31 C30 H301 109.0 . . ?
N22 C30 H302 109.0 . . ?
C31 C30 H302 109.0 . . ?
H301 C30 H302 107.8 . . ?
C32A C31 C36A 117.7(11) . . ?
C36B C31 C32B 119.0(12) . . ?
C36B C31 C30 116.5(8) . . ?
C32A C31 C30 119.2(9) . . ?
C36A C31 C30 122.9(8) . . ?
C32B C31 C30 124.4(10) . . ?
C31 C32A C33A 121.1(15) . . ?
C31 C32A H32A 119.4 . . ?
C33A C32A H32A 119.4 . . ?
C32A C33A C34 119.9(14) . . ?
C32A C33A H33A 120.1 . . ?
C34 C33A H33A 120.1 . . ?
C33B C32B C31 119.5(16) . . ?
C33B C32B H32B 120.3 . . ?
C31 C32B H32B 120.3 . . ?
C34 C33B C32B 122.0(13) . . ?
C34 C33B H33B 119.0 . . ?
C32B C33B H33B 119.0 . . ?
C35A C34 C33A 118.4(12) . . ?
C33B C34 C35B 118.7(12) . . ?
C33B C34 H341 120.5 . . ?
C35A C34 H341 120.1 . . ?
C33A C34 H341 121.4 . . ?
C35B C34 H341 120.8 . . ?
C34 C35A C36A 119.8(17) . . ?
C34 C35A H35A 120.1 . . ?
C36A C35A H35A 120.1 . . ?
C35A C36A C31 122.4(15) . . ?
C35A C36A H36A 118.8 . . ?
C31 C36A H36A 118.8 . . ?
C36B C35B C34 117.7(16) . . ?
C36B C35B H35B 121.1 . . ?
C34 C35B H35B 121.1 . . ?
C31 C36B C35B 123.0(13) . . ?
C31 C36B H36B 118.5 . . ?
C35B C36B H36B 118.5 . . ?
C41C C40 N22 118.5(8) . . ?
N22 C40 C41D 107.3(7) . . ?
C41C C40 H401 107.7 . . ?
N22 C40 H401 107.7 . . ?
C41C C40 H402 107.7 . . ?
N22 C40 H402 107.7 . . ?
H401 C40 H402 107.1 . . ?
N22 C40 H403 110.3 . . ?
C41D C40 H403 110.3 . . ?
N22 C40 H404 110.3 . . ?
C41D C40 H404 110.3 . . ?
H403 C40 H404 108.5 . . ?
C40 C41C C42C 115.5(9) . . ?
C40 C41C C46C 124.5(9) . . ?
C42C C41C C46C 120.0 . . ?
C43C C42C C41C 120.0 . . ?
C43C C42C H42C 120.0 . . ?
C41C C42C H42C 120.0 . . ?
C42C C43C C44C 120.0 . . ?
C42C C43C H43C 120.0 . . ?
C44C C43C H43C 120.0 . . ?
C45C C44C C43C 120.0 . . ?
C45C C44C H44C 120.0 . . ?
C43C C44C H44C 120.0 . . ?
C44C C45C C46C 120.0 . . ?
C44C C45C H45C 120.0 . . ?
C46C C45C H45C 120.0 . . ?
C45C C46C C41C 120.0 . . ?
C45C C46C H46C 120.0 . . ?
C41C C46C H46C 120.0 . . ?
C42D C41D C46D 120.0 . . ?
C42D C41D C40 121.6(9) . . ?
C46D C41D C40 118.3(9) . . ?
C43D C42D C41D 120.0 . . ?
C43D C42D H42D 120.0 . . ?
C41D C42D H42D 120.0 . . ?
C42D C43D C44D 120.0 . . ?
C42D C43D H43D 120.0 . . ?
C44D C43D H43D 120.0 . . ?
C43D C44D C45D 120.0 . . ?
C43D C44D H44D 120.0 . . ?
C45D C44D H44D 120.0 . . ?
C46D C45D C44D 120.0 . . ?
C46D C45D H45D 120.0 . . ?
C44D C45D H45D 120.0 . . ?
C45D C46D C41D 120.0 . . ?
C45D C46D H46D 120.0 . . ?
C41D C46D H46D 120.0 . . ?
N4 C50 C51 112.7(6) . . ?
N4 C50 H501 109.1 . . ?
C51 C50 H501 109.1 . . ?
N4 C50 H502 109.1 . . ?
C51 C50 H502 109.1 . . ?
H501 C50 H502 107.8 . . ?
O51 C51 O52 122.8(11) . . ?
O51 C51 C50 118.2(7) . . ?
O52 C51 C50 118.8(9) . . ?
C51 O51 Gd1 118.1(5) . . ?
N7 C60 C61 109.5(6) . . ?
N7 C60 H601 109.8 . . ?
C61 C60 H601 109.8 . . ?
N7 C60 H602 109.8 . . ?
C61 C60 H602 109.8 . . ?
H601 C60 H602 108.2 . . ?
O62 C61 O61 125.8(9) . . ?
O62 C61 C60 117.2(8) . . ?
O61 C61 C60 117.0(6) . . ?
C61 O61 Gd1 124.4(5) . . ?
N10 C70 C71 111.2(5) . . ?
N10 C70 H701 109.4 . . ?
C71 C70 H701 109.4 . . ?
N10 C70 H702 109.4 . . ?
C71 C70 H702 109.4 . . ?
H701 C70 H702 108.0 . . ?
O72 C71 O71 124.9(6) . . ?
O72 C71 C70 118.5(5) . . ?
O71 C71 C70 116.6(4) . . ?
C71 O71 Gd1 119.0(4) . . ?
H11W O1W H12W 104.1 . . ?
H21W O2W H22W 105.0 . . ?
H31W O3W H32W 131.8 . . ?
O7WB Ca1 O7WB 142.6(7) 2_655 . ?
O7WA Ca1 O7WA 177.9(5) . 2_655 ?
O7WB Ca1 O5W 71.3(4) 2_655 . ?
O7WB Ca1 O5W 71.3(4) . . ?
O7WA Ca1 O5W 88.9(3) . . ?
O7WA Ca1 O5W 88.9(3) 2_655 . ?
O7WB Ca1 O6W 108.7(4) 2_655 . ?
O7WB Ca1 O6W 108.7(4) . . ?
O7WA Ca1 O6W 91.1(3) . . ?
O7WA Ca1 O6W 91.1(3) 2_655 . ?
O5W Ca1 O6W 180.0 . . ?
O7WB Ca1 O4W 129.2(4) 2_655 . ?
O7WB Ca1 O4W 55.2(4) . . ?
O7WA Ca1 O4W 96.6(3) . . ?
O7WA Ca1 O4W 83.6(3) 2_655 . ?
O5W Ca1 O4W 95.5(2) . . ?
O6W Ca1 O4W 84.5(2) . . ?
O7WB Ca1 O4W 55.2(4) 2_655 2_655 ?
O7WB Ca1 O4W 129.2(4) . 2_655 ?
O7WA Ca1 O4W 83.6(3) . 2_655 ?
O7WA Ca1 O4W 96.6(3) 2_655 2_655 ?
O5W Ca1 O4W 95.5(2) . 2_655 ?
O6W Ca1 O4W 84.5(2) . 2_655 ?
O4W Ca1 O4W 169.0(5) . 2_655 ?

_refine_diff_density_max         3.570
_refine_diff_density_min         -2.014
_refine_diff_density_rms         0.149

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

data_tbdo3apdbam
_database_code_depnum_ccdc_archive 'CCDC 1959638'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H41 N5 O8 P Tb, Cl, H2 O, H4 N'
_chemical_formula_sum            'C30 H47 Cl N6 O9 P Tb'
_chemical_formula_weight         861.07

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_H-M_alt        'P n'
_space_group_name_Hall           'P -2yac'

_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+1/2, -y, z+1/2'

_cell_length_a                   9.9701(2)
_cell_length_b                   15.3519(3)
_cell_length_c                   11.4210(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.9903(8)
_cell_angle_gamma                90
_cell_volume                     1741.47(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6617
_cell_measurement_theta_min      3.1324
_cell_measurement_theta_max      27.4874

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_F_000             876
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.348
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.062
_exptl_absorpt_coefficient_mu    2.213
_shelx_estimated_absorpt_T_min   0.513
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2014/3 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(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 8.3333
_diffrn_reflns_number            11698
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.326
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_point_group_measured_fraction_full 0.877
_reflns_number_total             6788
_reflns_number_gt                6464
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.695
_reflns_Friedel_fraction_max     0.698
_reflns_Friedel_fraction_full    0.753

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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 Instrument Service v2014.5.0.0'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0209P)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 2523 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6788
_refine_ls_number_parameters     454
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0228
_refine_ls_wR_factor_ref         0.0495
_refine_ls_wR_factor_gt          0.0484
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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_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
Tb1 Tb 0.08301(2) -0.10451(2) 0.13216(2) 0.00915(5) Uani 1 1 d . . . . .
N1 N -0.0468(4) -0.0284(2) -0.0488(3) 0.0119(8) Uani 1 1 d . . . . .
C2 C -0.1955(5) -0.0407(3) -0.0510(4) 0.0149(10) Uani 1 1 d . . . . .
H21 H -0.2375 -0.0266 -0.1305 0.018 Uiso 1 1 calc R U . . .
H22 H -0.2319 0.0001 0.0054 0.018 Uiso 1 1 calc R U . . .
C3 C -0.2324(5) -0.1328(3) -0.0200(4) 0.0151(10) Uani 1 1 d . . . . .
H31 H -0.3312 -0.1369 -0.0170 0.018 Uiso 1 1 calc R U . . .
H32 H -0.2064 -0.1730 -0.0819 0.018 Uiso 1 1 calc R U . . .
N4 N -0.1647(4) -0.1599(2) 0.0948(3) 0.0115(8) Uani 1 1 d . . . . .
C5 C -0.1719(5) -0.2563(3) 0.1068(4) 0.0175(11) Uani 1 1 d . . . . .
H51 H -0.2615 -0.2767 0.0736 0.021 Uiso 1 1 calc R U . . .
H52 H -0.1621 -0.2719 0.1912 0.021 Uiso 1 1 calc R U . . .
C6 C -0.0649(5) -0.3022(3) 0.0455(4) 0.0175(11) Uani 1 1 d . . . . .
H61 H -0.0726 -0.3658 0.0571 0.021 Uiso 1 1 calc R U . . .
H62 H -0.0782 -0.2902 -0.0399 0.021 Uiso 1 1 calc R U . . .
N7 N 0.0713(4) -0.2726(3) 0.0916(3) 0.0145(9) Uani 1 1 d . . . . .
C8 C 0.1716(5) -0.2949(3) 0.0073(4) 0.0194(11) Uani 1 1 d . . . . .
H81 H 0.1540 -0.3546 -0.0231 0.023 Uiso 1 1 calc R U . . .
H82 H 0.2631 -0.2940 0.0487 0.023 Uiso 1 1 calc R U . . .
C9 C 0.1659(5) -0.2317(3) -0.0945(4) 0.0163(10) Uani 1 1 d . . . . .
H91 H 0.2322 -0.2492 -0.1498 0.020 Uiso 1 1 calc R U . . .
H92 H 0.0752 -0.2336 -0.1373 0.020 Uiso 1 1 calc R U . . .
N10 N 0.1954(6) -0.1420(4) -0.0530(5) 0.0147(12) Uani 1 1 d . . . . .
C11 C 0.1518(5) -0.0779(3) -0.1478(4) 0.0159(10) Uani 1 1 d . . . . .
H111 H 0.1808 -0.0989 -0.2235 0.019 Uiso 1 1 calc R U . . .
H112 H 0.1967 -0.0213 -0.1297 0.019 Uiso 1 1 calc R U . . .
C12 C 0.0009(5) -0.0646(3) -0.1598(4) 0.0161(10) Uani 1 1 d . . . . .
H121 H -0.0237 -0.0241 -0.2256 0.019 Uiso 1 1 calc R U . . .
H122 H -0.0443 -0.1210 -0.1783 0.019 Uiso 1 1 calc R U . . .
C20 C -0.0158(5) 0.0661(3) -0.0409(4) 0.0140(10) Uani 1 1 d . . . . .
H201 H -0.0794 0.0986 -0.0963 0.017 Uiso 1 1 calc R U . . .
H202 H 0.0765 0.0765 -0.0636 0.017 Uiso 1 1 calc R U . . .
P1 P -0.02903(12) 0.10601(8) 0.10939(10) 0.0110(2) Uani 1 1 d . . . . .
O11 O 0.0054(3) 0.02778(19) 0.1882(3) 0.0130(7) Uani 1 1 d . . . . .
O12 O -0.1583(3) 0.1518(2) 0.1241(3) 0.0160(7) Uani 1 1 d . . . . .
C21 C 0.1143(4) 0.1786(3) 0.1427(5) 0.0128(11) Uani 1 1 d . . . . .
H211 H 0.1264 0.1857 0.2291 0.015 Uiso 1 1 calc R U . . .
H212 H 0.1954 0.1483 0.1191 0.015 Uiso 1 1 calc R U . . .
N22 N 0.1127(4) 0.2687(3) 0.0889(4) 0.0146(8) Uani 1 1 d . . . . .
H221 H 0.190(6) 0.300(3) 0.118(5) 0.015(16) Uiso 1 1 d . . . . .
C30 C 0.0109(5) 0.3300(3) 0.1359(4) 0.0182(11) Uani 1 1 d . . . . .
H301 H -0.0072 0.3785 0.0796 0.022 Uiso 1 1 calc R U . . .
H302 H -0.0747 0.2983 0.1421 0.022 Uiso 1 1 calc R U . . .
C31 C 0.0586(5) 0.3670(3) 0.2547(4) 0.0145(10) Uani 1 1 d . . . . .
C32 C 0.0061(7) 0.3367(4) 0.3567(6) 0.0210(16) Uani 1 1 d . . . . .
H321 H -0.0565 0.2899 0.3519 0.025 Uiso 1 1 calc R U . . .
C33 C 0.0443(6) 0.3742(4) 0.4645(5) 0.0286(13) Uani 1 1 d . . . . .
H331 H 0.0089 0.3524 0.5333 0.034 Uiso 1 1 calc R U . . .
C34 C 0.1326(7) 0.4426(4) 0.4729(5) 0.0313(15) Uani 1 1 d . . . . .
H341 H 0.1562 0.4695 0.5468 0.038 Uiso 1 1 calc R U . . .
C35 C 0.1875(6) 0.4723(4) 0.3728(5) 0.0291(13) Uani 1 1 d . . . . .
H351 H 0.2510 0.5186 0.3783 0.035 Uiso 1 1 calc R U . . .
C36 C 0.1498(6) 0.4345(3) 0.2646(5) 0.0238(12) Uani 1 1 d . . . . .
H361 H 0.1875 0.4554 0.1964 0.029 Uiso 1 1 calc R U . . .
C40 C 0.0932(5) 0.2654(3) -0.0443(4) 0.0152(10) Uani 1 1 d . . . . .
H401 H 0.1463 0.2165 -0.0730 0.018 Uiso 1 1 calc R U . . .
H402 H -0.0029 0.2546 -0.0694 0.018 Uiso 1 1 calc R U . . .
C41 C 0.1369(7) 0.3496(4) -0.0983(6) 0.0167(14) Uani 1 1 d . . . . .
C42 C 0.0430(6) 0.4060(3) -0.1538(6) 0.0274(13) Uani 1 1 d . . . . .
H421 H -0.0500 0.3919 -0.1577 0.033 Uiso 1 1 calc R U . . .
C43 C 0.0842(7) 0.4833(4) -0.2039(5) 0.0328(15) Uani 1 1 d . . . . .
H431 H 0.0193 0.5222 -0.2406 0.039 Uiso 1 1 calc R U . . .
C44 C 0.2189(6) 0.5031(4) -0.2001(5) 0.0288(13) Uani 1 1 d . . . . .
H441 H 0.2472 0.5557 -0.2341 0.035 Uiso 1 1 calc R U . . .
C45 C 0.3133(6) 0.4466(4) -0.1469(5) 0.0283(13) Uani 1 1 d . . . . .
H451 H 0.4064 0.4605 -0.1448 0.034 Uiso 1 1 calc R U . . .
C46 C 0.2731(5) 0.3698(3) -0.0965(4) 0.0199(11) Uani 1 1 d . . . . .
H461 H 0.3386 0.3310 -0.0607 0.024 Uiso 1 1 calc R U . . .
C50 C -0.2311(5) -0.1202(3) 0.1932(4) 0.0156(10) Uani 1 1 d . . . . .
H501 H -0.3189 -0.1489 0.2002 0.019 Uiso 1 1 calc R U . . .
H502 H -0.2481 -0.0577 0.1766 0.019 Uiso 1 1 calc R U . . .
C51 C -0.1433(7) -0.1295(4) 0.3088(5) 0.0130(13) Uani 1 1 d . . . . .
O51 O -0.0184(4) -0.1451(3) 0.3011(4) 0.0132(10) Uani 1 1 d . . . . .
O52 O -0.1962(4) -0.1204(2) 0.4015(3) 0.0187(8) Uani 1 1 d . . . . .
C60 C 0.1132(6) -0.3113(3) 0.2074(5) 0.0197(12) Uani 1 1 d . . . . .
H601 H 0.1489 -0.3706 0.1956 0.024 Uiso 1 1 calc R U . . .
H602 H 0.0332 -0.3171 0.2525 0.024 Uiso 1 1 calc R U . . .
C61 C 0.2198(5) -0.2581(3) 0.2792(4) 0.0171(11) Uani 1 1 d . . . . .
O61 O 0.2490(3) -0.1839(2) 0.2365(3) 0.0149(7) Uani 1 1 d . . . . .
O62 O 0.2671(4) -0.2886(2) 0.3732(3) 0.0254(8) Uani 1 1 d . . . . .
C70 C 0.3414(7) -0.1284(4) -0.0219(6) 0.0160(14) Uani 1 1 d . . . . .
H701 H 0.3867 -0.1206 -0.0950 0.019 Uiso 1 1 calc R U . . .
H702 H 0.3796 -0.1810 0.0185 0.019 Uiso 1 1 calc R U . . .
C71 C 0.3706(5) -0.0494(3) 0.0573(4) 0.0121(9) Uani 1 1 d . . . . .
O71 O 0.2710(3) -0.0195(2) 0.1075(3) 0.0138(7) Uani 1 1 d . . . . .
O72 O 0.4877(3) -0.0233(2) 0.0697(3) 0.0162(7) Uani 1 1 d . . . . .
Cl1 Cl 0.40750(13) 0.29131(8) 0.18891(11) 0.0206(3) Uani 1 1 d . . . . .
N1A N 0.5694(5) 0.1489(3) 0.0450(4) 0.0169(9) Uani 1 1 d . . . . .
H11A H 0.516(7) 0.186(4) 0.087(5) 0.039(18) Uiso 1 1 d . . . . .
H12A H 0.654(6) 0.152(3) 0.062(4) 0.008(13) Uiso 1 1 d . . . . .
H13A H 0.560(5) 0.147(3) -0.023(4) 0.05(2) Uiso 1 1 d . . . . .
H14A H 0.5400 0.0896 0.0548 0.032(17) Uiso 1 1 d R . . . .
O1W O 0.6886(5) 0.3582(3) 0.0875(4) 0.0391(11) Uani 1 1 d . . . . .
H11W H 0.610(8) 0.341(4) 0.106(6) 0.07(3) Uiso 1 1 d . . . . .
H12W H 0.7102 0.3011 0.1198 0.089 Uiso 0.5 1 d R U P . .
H13W H 0.6676 0.3347 0.0078 0.089 Uiso 0.5 1 d R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O11 2.284(3) . ?
Tb1 O61 2.303(3) . ?
Tb1 O71 2.321(3) . ?
Tb1 O51 2.340(4) . ?
Tb1 N10 2.543(5) . ?
Tb1 N4 2.612(4) . ?
Tb1 N1 2.617(4) . ?
Tb1 N7 2.623(4) . ?
N1 C20 1.484(6) . ?
N1 C2 1.492(6) . ?
N1 C12 1.500(6) . ?
C2 C3 1.511(7) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.481(6) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.484(6) . ?
N4 C5 1.490(6) . ?
C5 C6 1.501(7) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.484(6) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C60 1.477(6) . ?
N7 C8 1.488(6) . ?
C8 C9 1.512(7) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.478(7) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C70 1.483(8) . ?
N10 C11 1.499(7) . ?
C11 C12 1.512(7) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.838(5) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.490(3) . ?
P1 O11 1.522(3) . ?
P1 C21 1.826(4) . ?
C21 N22 1.513(6) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C30 1.517(6) . ?
N22 C40 1.518(6) . ?
N22 H221 0.94(6) . ?
C30 C31 1.509(7) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36 1.377(7) . ?
C31 C32 1.398(8) . ?
C32 C33 1.382(9) . ?
C32 H321 0.9500 . ?
C33 C34 1.368(9) . ?
C33 H331 0.9500 . ?
C34 C35 1.387(8) . ?
C34 H341 0.9500 . ?
C35 C36 1.387(7) . ?
C35 H351 0.9500 . ?
C36 H361 0.9500 . ?
C40 C41 1.512(8) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C41 C42 1.388(8) . ?
C41 C46 1.391(8) . ?
C42 C43 1.395(8) . ?
C42 H421 0.9500 . ?
C43 C44 1.374(9) . ?
C43 H431 0.9500 . ?
C44 C45 1.381(8) . ?
C44 H441 0.9500 . ?
C45 C46 1.386(7) . ?
C45 H451 0.9500 . ?
C46 H461 0.9500 . ?
C50 C51 1.525(7) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.232(7) . ?
C51 O51 1.278(8) . ?
C60 C61 1.523(7) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.228(6) . ?
C61 O61 1.281(6) . ?
C70 C71 1.525(8) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.232(5) . ?
C71 O71 1.274(6) . ?
N1A H11A 0.93(6) . ?
N1A H12A 0.85(5) . ?
N1A H13A 0.78(5) . ?
N1A H14A 0.9668 . ?
O1W H11W 0.87(7) . ?
O1W H12W 0.9688 . ?
O1W H13W 0.9843 . ?

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
O11 Tb1 O61 124.83(11) . . ?
O11 Tb1 O71 80.25(12) . . ?
O61 Tb1 O71 78.99(11) . . ?
O11 Tb1 O51 79.89(13) . . ?
O61 Tb1 O51 76.99(14) . . ?
O71 Tb1 O51 131.40(13) . . ?
O11 Tb1 N10 128.19(15) . . ?
O61 Tb1 N10 87.82(15) . . ?
O71 Tb1 N10 66.89(15) . . ?
O51 Tb1 N10 151.49(11) . . ?
O11 Tb1 N4 89.80(12) . . ?
O61 Tb1 N4 122.63(11) . . ?
O71 Tb1 N4 157.71(11) . . ?
O51 Tb1 N4 65.01(13) . . ?
N10 Tb1 N4 105.63(15) . . ?
O11 Tb1 N1 70.60(11) . . ?
O61 Tb1 N1 158.31(12) . . ?
O71 Tb1 N1 90.12(12) . . ?
O51 Tb1 N1 123.41(14) . . ?
N10 Tb1 N1 70.60(15) . . ?
N4 Tb1 N1 67.70(12) . . ?
O11 Tb1 N7 155.96(12) . . ?
O61 Tb1 N7 65.77(12) . . ?
O71 Tb1 N7 123.78(12) . . ?
O51 Tb1 N7 82.41(14) . . ?
N10 Tb1 N7 69.31(16) . . ?
N4 Tb1 N7 67.91(12) . . ?
N1 Tb1 N7 106.78(12) . . ?
C20 N1 C2 109.1(4) . . ?
C20 N1 C12 109.5(4) . . ?
C2 N1 C12 109.0(3) . . ?
C20 N1 Tb1 107.6(3) . . ?
C2 N1 Tb1 112.3(3) . . ?
C12 N1 Tb1 109.3(3) . . ?
N1 C2 C3 112.2(4) . . ?
N1 C2 H21 109.2 . . ?
C3 C2 H21 109.2 . . ?
N1 C2 H22 109.2 . . ?
C3 C2 H22 109.2 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 111.6(4) . . ?
N4 C3 H31 109.3 . . ?
C2 C3 H31 109.3 . . ?
N4 C3 H32 109.3 . . ?
C2 C3 H32 109.3 . . ?
H31 C3 H32 108.0 . . ?
C3 N4 C50 110.9(4) . . ?
C3 N4 C5 109.8(4) . . ?
C50 N4 C5 108.1(4) . . ?
C3 N4 Tb1 113.9(3) . . ?
C50 N4 Tb1 102.7(3) . . ?
C5 N4 Tb1 111.1(3) . . ?
N4 C5 C6 112.4(4) . . ?
N4 C5 H51 109.1 . . ?
C6 C5 H51 109.1 . . ?
N4 C5 H52 109.1 . . ?
C6 C5 H52 109.1 . . ?
H51 C5 H52 107.9 . . ?
N7 C6 C5 110.9(4) . . ?
N7 C6 H61 109.5 . . ?
C5 C6 H61 109.5 . . ?
N7 C6 H62 109.5 . . ?
C5 C6 H62 109.5 . . ?
H61 C6 H62 108.0 . . ?
C60 N7 C6 112.0(4) . . ?
C60 N7 C8 109.5(4) . . ?
C6 N7 C8 110.3(4) . . ?
C60 N7 Tb1 103.5(3) . . ?
C6 N7 Tb1 112.9(3) . . ?
C8 N7 Tb1 108.6(3) . . ?
N7 C8 C9 111.6(4) . . ?
N7 C8 H81 109.3 . . ?
C9 C8 H81 109.3 . . ?
N7 C8 H82 109.3 . . ?
C9 C8 H82 109.3 . . ?
H81 C8 H82 108.0 . . ?
N10 C9 C8 111.0(4) . . ?
N10 C9 H91 109.4 . . ?
C8 C9 H91 109.4 . . ?
N10 C9 H92 109.4 . . ?
C8 C9 H92 109.4 . . ?
H91 C9 H92 108.0 . . ?
C9 N10 C70 111.8(5) . . ?
C9 N10 C11 110.1(4) . . ?
C70 N10 C11 107.3(5) . . ?
C9 N10 Tb1 112.8(3) . . ?
C70 N10 Tb1 105.3(4) . . ?
C11 N10 Tb1 109.3(3) . . ?
N10 C11 C12 112.2(4) . . ?
N10 C11 H111 109.2 . . ?
C12 C11 H111 109.2 . . ?
N10 C11 H112 109.2 . . ?
C12 C11 H112 109.2 . . ?
H111 C11 H112 107.9 . . ?
N1 C12 C11 111.1(4) . . ?
N1 C12 H121 109.4 . . ?
C11 C12 H121 109.4 . . ?
N1 C12 H122 109.4 . . ?
C11 C12 H122 109.4 . . ?
H121 C12 H122 108.0 . . ?
N1 C20 P1 110.5(3) . . ?
N1 C20 H201 109.5 . . ?
P1 C20 H201 109.5 . . ?
N1 C20 H202 109.5 . . ?
P1 C20 H202 109.5 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 117.29(19) . . ?
O12 P1 C21 111.0(2) . . ?
O11 P1 C21 103.1(2) . . ?
O12 P1 C20 113.3(2) . . ?
O11 P1 C20 105.0(2) . . ?
C21 P1 C20 106.2(2) . . ?
P1 O11 Tb1 126.89(18) . . ?
N22 C21 P1 119.5(3) . . ?
N22 C21 H211 107.4 . . ?
P1 C21 H211 107.4 . . ?
N22 C21 H212 107.4 . . ?
P1 C21 H212 107.4 . . ?
H211 C21 H212 107.0 . . ?
C21 N22 C30 114.1(4) . . ?
C21 N22 C40 111.9(4) . . ?
C30 N22 C40 110.1(4) . . ?
C21 N22 H221 110(3) . . ?
C30 N22 H221 96(3) . . ?
C40 N22 H221 113(3) . . ?
C31 C30 N22 112.6(4) . . ?
C31 C30 H301 109.1 . . ?
N22 C30 H301 109.1 . . ?
C31 C30 H302 109.1 . . ?
N22 C30 H302 109.1 . . ?
H301 C30 H302 107.8 . . ?
C36 C31 C32 118.3(5) . . ?
C36 C31 C30 120.7(5) . . ?
C32 C31 C30 120.9(5) . . ?
C33 C32 C31 120.6(6) . . ?
C33 C32 H321 119.7 . . ?
C31 C32 H321 119.7 . . ?
C34 C33 C32 120.6(6) . . ?
C34 C33 H331 119.7 . . ?
C32 C33 H331 119.7 . . ?
C33 C34 C35 119.5(6) . . ?
C33 C34 H341 120.3 . . ?
C35 C34 H341 120.3 . . ?
C34 C35 C36 120.1(5) . . ?
C34 C35 H351 120.0 . . ?
C36 C35 H351 120.0 . . ?
C31 C36 C35 120.9(5) . . ?
C31 C36 H361 119.5 . . ?
C35 C36 H361 119.5 . . ?
C41 C40 N22 111.4(4) . . ?
C41 C40 H401 109.4 . . ?
N22 C40 H401 109.4 . . ?
C41 C40 H402 109.4 . . ?
N22 C40 H402 109.4 . . ?
H401 C40 H402 108.0 . . ?
C42 C41 C46 119.1(6) . . ?
C42 C41 C40 120.8(6) . . ?
C46 C41 C40 120.0(5) . . ?
C41 C42 C43 120.5(6) . . ?
C41 C42 H421 119.8 . . ?
C43 C42 H421 119.8 . . ?
C44 C43 C42 119.8(6) . . ?
C44 C43 H431 120.1 . . ?
C42 C43 H431 120.1 . . ?
C43 C44 C45 120.2(5) . . ?
C43 C44 H441 119.9 . . ?
C45 C44 H441 119.9 . . ?
C44 C45 C46 120.4(5) . . ?
C44 C45 H451 119.8 . . ?
C46 C45 H451 119.8 . . ?
C45 C46 C41 120.1(5) . . ?
C45 C46 H461 120.0 . . ?
C41 C46 H461 120.0 . . ?
N4 C50 C51 110.9(4) . . ?
N4 C50 H501 109.5 . . ?
C51 C50 H501 109.5 . . ?
N4 C50 H502 109.5 . . ?
C51 C50 H502 109.5 . . ?
H501 C50 H502 108.1 . . ?
O52 C51 O51 124.9(6) . . ?
O52 C51 C50 118.5(6) . . ?
O51 C51 C50 116.6(5) . . ?
C51 O51 Tb1 120.0(4) . . ?
N7 C60 C61 113.3(4) . . ?
N7 C60 H601 108.9 . . ?
C61 C60 H601 108.9 . . ?
N7 C60 H602 108.9 . . ?
C61 C60 H602 108.9 . . ?
H601 C60 H602 107.7 . . ?
O62 C61 O61 126.1(5) . . ?
O62 C61 C60 117.6(4) . . ?
O61 C61 C60 116.3(4) . . ?
C61 O61 Tb1 119.4(3) . . ?
N10 C70 C71 112.8(5) . . ?
N10 C70 H701 109.0 . . ?
C71 C70 H701 109.0 . . ?
N10 C70 H702 109.0 . . ?
C71 C70 H702 109.0 . . ?
H701 C70 H702 107.8 . . ?
O72 C71 O71 126.8(4) . . ?
O72 C71 C70 117.2(4) . . ?
O71 C71 C70 116.0(4) . . ?
C71 O71 Tb1 121.4(3) . . ?
H11A N1A H12A 116(5) . . ?
H11A N1A H13A 121(5) . . ?
H12A N1A H13A 105(5) . . ?
H11A N1A H14A 108.6 . . ?
H12A N1A H14A 109.1 . . ?
H13A N1A H14A 93.9 . . ?
H11W O1W H12W 78.5 . . ?
H11W O1W H13W 89.4 . . ?
H12W O1W H13W 92.5 . . ?

_refine_diff_density_max         0.807
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.082

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

data_hodbamoh
_database_code_depnum_ccdc_archive 'CCDC 1959631'
loop_
_audit_author_name
_audit_author_address
'Jan Kotek'
;Faculty of Science, Charles University, Prague
Czech Republic
;
_audit_update_record             
;
2019-10-16 deposited with the CCDC.	2019-12-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H40 Ho N5 O8 P, Ca0.5, 6(H2 O)'
_chemical_formula_sum            'C30 H52 Ca0.50 Ho N5 O14 P'
_chemical_formula_weight         922.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_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'
'x, -y, z-1/2'

_cell_length_a                   24.1798(13)
_cell_length_b                   10.1265(5)
_cell_length_c                   15.2799(8)
_cell_angle_alpha                90
_cell_angle_beta                 95.775(2)
_cell_angle_gamma                90
_cell_volume                     3722.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9855
_cell_measurement_theta_min      2.4166
_cell_measurement_theta_max      27.3718

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_F_000             1884
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.026
_exptl_absorpt_coefficient_mu    2.309
_shelx_estimated_absorpt_T_min   0.732
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'I\mS micro-focus sealed tube'
_diffrn_radiation_monochromator  'Quazar Mo multilayer optic'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            56881
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.182
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8553
_reflns_number_gt                7679
_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.
 
 _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 Instrument Service v6.2.9'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+139.5298P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8553
_refine_ls_number_parameters     485
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.1022
_refine_ls_wR_factor_ref         0.2429
_refine_ls_wR_factor_gt          0.2400
_refine_ls_goodness_of_fit_ref   1.338
_refine_ls_restrained_S_all      1.337
_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_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
Ho1 Ho 0.18635(2) 0.21792(6) 0.03440(4) 0.02468(17) Uani 1 1 d . . . . .
O1C O 0.1585(9) 0.364(2) 0.1756(15) 0.043(5) Uani 0.5 1 d . . P A 1
H11C H 0.1727 0.3397 0.2250 0.052 Uiso 0.5 1 d R U P A 1
H12C H 0.1247 0.3207 0.1760 0.052 Uiso 0.5 1 d R U P A 1
N1 N 0.2791(4) 0.2452(9) -0.0412(6) 0.021(2) Uani 1 1 d . . . . .
C2 C 0.2665(6) 0.3062(13) -0.1308(8) 0.030(3) Uani 1 1 d . . . . .
H21 H 0.2600 0.4021 -0.1242 0.036 Uiso 1 1 calc R U . . .
H22 H 0.2989 0.2948 -0.1648 0.036 Uiso 1 1 calc R U . . .
C3 C 0.2161(6) 0.2447(15) -0.1804(8) 0.035(3) Uani 1 1 d . . . . .
H31 H 0.2090 0.2875 -0.2387 0.042 Uiso 1 1 calc R U . . .
H32 H 0.2234 0.1498 -0.1901 0.042 Uiso 1 1 calc R U . . .
N4 N 0.1669(5) 0.2586(11) -0.1321(8) 0.034(3) Uani 1 1 d . . . . .
C5 C 0.1218(7) 0.1661(17) -0.1703(10) 0.048(4) Uani 1 1 d . . . . .
H51 H 0.0856 0.1960 -0.1523 0.057 Uiso 1 1 calc R U . . .
H52 H 0.1195 0.1701 -0.2353 0.057 Uiso 1 1 calc R U . . .
C6 C 0.1318(7) 0.0251(16) -0.1410(10) 0.042(4) Uani 1 1 d . . . . .
H61 H 0.1011 -0.0314 -0.1671 0.050 Uiso 1 1 calc R U . . .
H62 H 0.1669 -0.0072 -0.1618 0.050 Uiso 1 1 calc R U . . .
N7 N 0.1355(5) 0.0158(12) -0.0430(8) 0.031(2) Uani 1 1 d . . . . .
C8 C 0.1623(6) -0.1112(13) -0.0141(10) 0.035(3) Uani 1 1 d . . . . .
H81 H 0.1486 -0.1821 -0.0554 0.042 Uiso 1 1 calc R U . . .
H82 H 0.1516 -0.1344 0.0449 0.042 Uiso 1 1 calc R U . . .
C9 C 0.2243(6) -0.1033(12) -0.0104(8) 0.027(3) Uani 1 1 d . . . . .
H91 H 0.2408 -0.1880 0.0116 0.033 Uiso 1 1 calc R U . . .
H92 H 0.2352 -0.0887 -0.0704 0.033 Uiso 1 1 calc R U . . .
N10 N 0.2463(4) 0.0049(10) 0.0476(6) 0.021(2) Uani 1 1 d . . . . .
C11 C 0.3044(5) 0.0342(14) 0.0303(8) 0.028(3) Uani 1 1 d . . . . .
H111 H 0.3242 -0.0498 0.0226 0.034 Uiso 1 1 calc R U . . .
H112 H 0.3235 0.0802 0.0819 0.034 Uiso 1 1 calc R U . . .
C12 C 0.3074(6) 0.1189(13) -0.0506(8) 0.027(3) Uani 1 1 d . . . . .
H121 H 0.3468 0.1351 -0.0596 0.032 Uiso 1 1 calc R U . . .
H122 H 0.2897 0.0718 -0.1029 0.032 Uiso 1 1 calc R U . . .
C20 C 0.3156(5) 0.3358(13) 0.0129(7) 0.024(3) Uani 1 1 d . . . . .
H201 H 0.3465 0.3645 -0.0204 0.029 Uiso 1 1 calc R U . . .
H202 H 0.3317 0.2896 0.0667 0.029 Uiso 1 1 calc R U . . .
P1 P 0.27618(14) 0.4801(3) 0.0436(2) 0.0227(6) Uani 1 1 d . . . . .
O11 O 0.2165(4) 0.4311(9) 0.0428(6) 0.030(2) Uani 1 1 d . . . . .
O12 O 0.2850(4) 0.5952(9) -0.0138(6) 0.035(2) Uani 1 1 d . . . . .
C21 C 0.3030(5) 0.5107(14) 0.1564(8) 0.027(3) Uani 1 1 d . . . . .
H211 H 0.2821 0.5839 0.1807 0.032 Uiso 1 1 calc R U . . .
H212 H 0.2984 0.4308 0.1922 0.032 Uiso 1 1 calc R U . . .
N22 N 0.3630(4) 0.5457(11) 0.1602(7) 0.027(2) Uani 1 1 d . . . . .
C30 C 0.3713(6) 0.6856(13) 0.1433(12) 0.039(4) Uani 1 1 d . . . . .
H301 H 0.3694 0.7359 0.1985 0.047 Uiso 1 1 calc R U . . .
H302 H 0.3411 0.7175 0.0999 0.047 Uiso 1 1 calc R U . . .
C31 C 0.4266(6) 0.7113(13) 0.1088(9) 0.031(3) Uani 1 1 d . . . . .
C32A C 0.4753(13) 0.748(2) 0.166(2) 0.039(5) Uani 0.515(12) 1 d . . P B 2
H32A H 0.4747 0.7572 0.2275 0.047 Uiso 0.515(12) 1 calc R U P B 2
C33A C 0.5234(13) 0.768(3) 0.125(2) 0.045(5) Uiso 0.515(12) 1 d . . P B 2
H33A H 0.5569 0.7855 0.1611 0.054 Uiso 0.515(12) 1 calc R U P B 2
C34 C 0.5258(7) 0.7659(18) 0.0394(14) 0.056(5) Uani 1 1 d . . . . .
H34A H 0.5595 0.7843 0.0149 0.067 Uiso 0.515(12) 1 calc R U P B 2
H34B H 0.5571 0.7884 0.0097 0.067 Uiso 0.485(12) 1 calc R U P B 3
C35A C 0.4742(13) 0.734(3) -0.018(2) 0.046(6) Uani 0.515(12) 1 d . . P B 2
H35A H 0.4738 0.7306 -0.0801 0.055 Uiso 0.515(12) 1 calc R U P B 2
C36A C 0.4264(11) 0.708(2) 0.0231(19) 0.033(4) Uani 0.515(12) 1 d . . P B 2
H36A H 0.3928 0.6879 -0.0120 0.039 Uiso 0.515(12) 1 calc R U P B 2
C32B C 0.4502(14) 0.834(3) 0.115(2) 0.039(5) Uani 0.485(12) 1 d . . P B 3
H32B H 0.4307 0.9008 0.1424 0.047 Uiso 0.485(12) 1 calc R U P B 3
C33B C 0.5003(14) 0.869(4) 0.084(2) 0.045(5) Uiso 0.485(12) 1 d . . P B 3
H33B H 0.5161 0.9541 0.0919 0.054 Uiso 0.485(12) 1 calc R U P B 3
C35B C 0.5091(14) 0.639(3) 0.036(2) 0.046(6) Uani 0.485(12) 1 d . . P B 3
H35B H 0.5313 0.5702 0.0157 0.055 Uiso 0.485(12) 1 calc R U P B 3
C36B C 0.4568(12) 0.616(3) 0.064(2) 0.033(4) Uani 0.485(12) 1 d . . P B 3
H36B H 0.4404 0.5313 0.0535 0.039 Uiso 0.485(12) 1 calc R U P B 3
C40 C 0.3937(7) 0.498(2) 0.2442(10) 0.062(6) Uani 1 1 d . . . . .
H401 H 0.4320 0.5332 0.2459 0.074 Uiso 0.52(2) 1 calc R U P C 4
H402 H 0.3764 0.5416 0.2928 0.074 Uiso 0.52(2) 1 calc R U P C 4
H403 H 0.3728 0.5217 0.2945 0.074 Uiso 0.48(2) 1 calc R U P C 5
H404 H 0.4307 0.5407 0.2531 0.074 Uiso 0.48(2) 1 calc R U P C 5
C41C C 0.3980(12) 0.3747(19) 0.2636(15) 0.031(7) Uani 0.52(2) 1 d G . P C 4
C42C C 0.3791(11) 0.315(3) 0.3369(16) 0.053(8) Uani 0.52(2) 1 d G . P C 4
H42C H 0.3617 0.3665 0.3783 0.063 Uiso 0.52(2) 1 calc R U P C 4
C43C C 0.3856(11) 0.180(3) 0.3496(18) 0.075(12) Uani 0.52(2) 1 d G . P C 4
H43C H 0.3726 0.1388 0.3997 0.090 Uiso 0.52(2) 1 calc R U P C 4
C44C C 0.4110(13) 0.104(2) 0.289(2) 0.069(10) Uani 0.52(2) 1 d G . P C 4
H44C H 0.4154 0.0117 0.2978 0.082 Uiso 0.52(2) 1 calc R U P C 4
C45C C 0.4299(13) 0.164(3) 0.2158(19) 0.069(10) Uani 0.52(2) 1 d G . P C 4
H45C H 0.4473 0.1123 0.1745 0.083 Uiso 0.52(2) 1 calc R U P C 4
C46C C 0.4234(13) 0.299(3) 0.2031(14) 0.050(6) Uani 0.52(2) 1 d G U P C 4
H46C H 0.4363 0.3400 0.1530 0.060 Uiso 0.52(2) 1 calc R U P C 4
C41D C 0.4008(13) 0.337(2) 0.2389(17) 0.031(7) Uani 0.48(2) 1 d G . P C 5
C42D C 0.3736(11) 0.258(3) 0.2953(17) 0.053(8) Uani 0.48(2) 1 d G . P C 5
H42D H 0.3507 0.2972 0.3352 0.063 Uiso 0.48(2) 1 calc R U P C 5
C43D C 0.3797(12) 0.122(3) 0.293(2) 0.075(12) Uani 0.48(2) 1 d G . P C 5
H43D H 0.3611 0.0675 0.3316 0.090 Uiso 0.48(2) 1 calc R U P C 5
C44D C 0.4131(14) 0.064(2) 0.235(2) 0.069(10) Uani 0.48(2) 1 d G . P C 5
H44D H 0.4173 -0.0288 0.2333 0.082 Uiso 0.48(2) 1 calc R U P C 5
C45D C 0.4404(13) 0.144(3) 0.178(2) 0.069(10) Uani 0.48(2) 1 d G . P C 5
H45D H 0.4633 0.1044 0.1384 0.083 Uiso 0.48(2) 1 calc R U P C 5
C46D C 0.4342(12) 0.280(3) 0.1805(17) 0.050(6) Uani 0.48(2) 1 d G U P C 5
H46D H 0.4529 0.3340 0.1420 0.060 Uiso 0.48(2) 1 calc R U P C 5
C50 C 0.1436(6) 0.3933(16) -0.1395(10) 0.043(4) Uani 1 1 d . . . . .
H501 H 0.1228 0.4044 -0.1982 0.051 Uiso 1 1 calc R U . . .
H502 H 0.1744 0.4581 -0.1344 0.051 Uiso 1 1 calc R U . . .
C51 C 0.1059(7) 0.4208(17) -0.0701(13) 0.050(4) Uani 1 1 d . . . . .
O51 O 0.1059(4) 0.3370(11) -0.0047(7) 0.041(3) Uani 1 1 d . . . . .
O52 O 0.0772(6) 0.5243(15) -0.0748(12) 0.082(5) Uani 1 1 d . . . . .
C60 C 0.0796(6) 0.0195(15) -0.0104(10) 0.038(3) Uani 1 1 d . . . . .
H601 H 0.0597 -0.0642 -0.0253 0.046 Uiso 1 1 calc R U . . .
H602 H 0.0576 0.0929 -0.0389 0.046 Uiso 1 1 calc R U . . .
C61 C 0.0860(6) 0.0389(14) 0.0885(10) 0.035(3) Uani 1 1 d . . . . .
O61 O 0.1265(4) 0.1096(9) 0.1200(6) 0.033(2) Uani 1 1 d . . . . .
O62 O 0.0511(4) -0.0135(12) 0.1324(8) 0.047(3) Uani 1 1 d . . . . .
C70 C 0.2456(6) -0.0344(13) 0.1412(7) 0.025(3) Uani 1 1 d . . . . .
H701 H 0.2773 -0.0940 0.1586 0.030 Uiso 1 1 calc R U . . .
H702 H 0.2108 -0.0825 0.1489 0.030 Uiso 1 1 calc R U . . .
C71 C 0.2498(6) 0.0896(13) 0.1998(8) 0.028(3) Uani 1 1 d . . . . .
O71 O 0.2434(4) 0.1998(8) 0.1613(5) 0.028(2) Uani 1 1 d . . . . .
O72 O 0.2575(5) 0.0717(9) 0.2801(5) 0.037(2) Uani 1 1 d . . . . .
O1W O 0.0370(6) 0.7186(15) 0.1088(10) 0.076(4) Uani 1 1 d . . . . .
H11W H 0.0192 0.7755 0.1384 0.091 Uiso 1 1 d R U . . .
H12W H 0.0348 0.6285 0.1154 0.091 Uiso 1 1 d R U . . .
O2W O 0.1492(7) 0.6189(16) 0.1239(9) 0.081(5) Uani 1 1 d . . . . .
H21W H 0.1116 0.6454 0.0981 0.097 Uiso 1 1 d R U . . .
H22W H 0.1404 0.5415 0.1493 0.097 Uiso 1 1 d R U . . .
O3W O 0.2251(5) 0.3372(10) 0.3328(6) 0.049(3) Uani 1 1 d . . . . .
H31W H 0.2395 0.2672 0.3083 0.059 Uiso 1 1 d R U . . .
H32W H 0.2509 0.3800 0.3757 0.059 Uiso 1 1 d R U . . .
Ca1 Ca 0.0243(3) 0.6390(6) -0.2145(5) 0.0444(16) Uani 0.5 1 d . . P . .
O5W O 0.0000 0.4170(19) -0.2500 0.070(6) Uani 1 2 d S T P E .
O6W O 0.0170(9) 0.876(2) -0.2266(19) 0.053(7) Uani 0.5 1 d . . P E .
O7W O -0.1171(9) 0.692(2) -0.2549(18) 0.058(7) Uani 0.5 1 d . . P D 6
O8W O -0.0159(10) 0.666(2) -0.0857(15) 0.050(6) Uiso 0.5 1 d . . P E .
O9W O -0.0735(12) 0.678(3) -0.2745(19) 0.067(7) Uiso 0.5 1 d . . P E 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O71 2.272(9) . ?
Ho1 O11 2.277(10) . ?
Ho1 O51 2.315(9) . ?
Ho1 O61 2.321(9) . ?
Ho1 N4 2.574(11) . ?
Ho1 N10 2.596(10) . ?
Ho1 N7 2.608(12) . ?
Ho1 N1 2.639(10) . ?
Ho1 O1C 2.75(2) . ?
O1C H11C 0.8328 . ?
O1C H12C 0.9286 . ?
N1 C12 1.463(15) . ?
N1 C20 1.467(16) . ?
N1 C2 1.506(14) . ?
C2 C3 1.50(2) . ?
C2 H21 0.9900 . ?
C2 H22 0.9900 . ?
C3 N4 1.470(18) . ?
C3 H31 0.9900 . ?
C3 H32 0.9900 . ?
N4 C50 1.475(18) . ?
N4 C5 1.51(2) . ?
C5 C6 1.51(2) . ?
C5 H51 0.9900 . ?
C5 H52 0.9900 . ?
C6 N7 1.494(18) . ?
C6 H61 0.9900 . ?
C6 H62 0.9900 . ?
N7 C8 1.487(17) . ?
N7 C60 1.488(18) . ?
C8 C9 1.50(2) . ?
C8 H81 0.9900 . ?
C8 H82 0.9900 . ?
C9 N10 1.475(15) . ?
C9 H91 0.9900 . ?
C9 H92 0.9900 . ?
N10 C11 1.484(16) . ?
N10 C70 1.487(14) . ?
C11 C12 1.512(17) . ?
C11 H111 0.9900 . ?
C11 H112 0.9900 . ?
C12 H121 0.9900 . ?
C12 H122 0.9900 . ?
C20 P1 1.831(12) . ?
C20 H201 0.9900 . ?
C20 H202 0.9900 . ?
P1 O12 1.487(10) . ?
P1 O11 1.526(10) . ?
P1 C21 1.806(12) . ?
C21 N22 1.488(16) . ?
C21 H211 0.9900 . ?
C21 H212 0.9900 . ?
N22 C30 1.457(17) . ?
N22 C40 1.497(18) . ?
C30 C31 1.51(2) . ?
C30 H301 0.9900 . ?
C30 H302 0.9900 . ?
C31 C36A 1.31(3) . ?
C31 C32B 1.36(3) . ?
C31 C36B 1.42(3) . ?
C31 C32A 1.44(3) . ?
C32A C33A 1.39(4) . ?
C32A H32A 0.9500 . ?
C33A C34 1.31(4) . ?
C33A H33A 0.9500 . ?
C34 C35B 1.35(4) . ?
C34 C33B 1.42(4) . ?
C34 C35A 1.49(4) . ?
C34 H34A 0.9500 . ?
C34 H34B 0.9500 . ?
C35A C36A 1.39(4) . ?
C35A H35A 0.9500 . ?
C36A H36A 0.9500 . ?
C32B C33B 1.39(5) . ?
C32B H32B 0.9500 . ?
C33B H33B 0.9500 . ?
C35B C36B 1.40(4) . ?
C35B H35B 0.9500 . ?
C36B H36B 0.9500 . ?
C40 C41C 1.29(3) . ?
C40 C41D 1.64(3) . ?
C40 H401 0.9900 . ?
C40 H402 0.9900 . ?
C40 H403 0.9900 . ?
C40 H404 0.9900 . ?
C41C C42C 1.3900 . ?
C41C C46C 1.3900 . ?
C42C C43C 1.3900 . ?
C42C H42C 0.9500 . ?
C43C C44C 1.3900 . ?
C43C H43C 0.9500 . ?
C44C C45C 1.3900 . ?
C44C H44C 0.9500 . ?
C45C C46C 1.3900 . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
C41D C42D 1.3900 . ?
C41D C46D 1.3900 . ?
C42D C43D 1.3900 . ?
C42D H42D 0.9500 . ?
C43D C44D 1.3900 . ?
C43D H43D 0.9500 . ?
C44D C45D 1.3900 . ?
C44D H44D 0.9500 . ?
C45D C46D 1.3900 . ?
C45D H45D 0.9500 . ?
C46D H46D 0.9500 . ?
C50 C51 1.49(2) . ?
C50 H501 0.9900 . ?
C50 H502 0.9900 . ?
C51 O52 1.254(19) . ?
C51 O51 1.31(2) . ?
O52 Ca1 2.645(17) . ?
C60 C61 1.52(2) . ?
C60 H601 0.9900 . ?
C60 H602 0.9900 . ?
C61 O62 1.249(17) . ?
C61 O61 1.269(17) . ?
C70 C71 1.539(18) . ?
C70 H701 0.9900 . ?
C70 H702 0.9900 . ?
C71 O72 1.235(15) . ?
C71 O71 1.264(15) . ?
O1W H11W 0.8720 . ?
O1W H12W 0.9206 . ?
O2W H21W 0.9925 . ?
O2W H22W 0.9099 . ?
O3W H31W 0.8887 . ?
O3W H32W 0.9604 . ?
Ca1 O9W 1.28(3) 2_554 ?
Ca1 Ca1 1.517(14) 2_554 ?
Ca1 O8W 2.30(2) . ?
Ca1 O5W 2.37(2) . ?
Ca1 O7W 2.40(2) 2_554 ?
Ca1 O6W 2.41(2) . ?
Ca1 O9W 2.48(3) . ?
Ca1 O6W 2.72(2) 2_554 ?
Ca1 O8W 3.05(2) 2_554 ?
O5W Ca1 2.37(2) 2_554 ?
O6W O6W 1.03(5) 2_554 ?
O6W Ca1 2.72(2) 2_554 ?
O7W Ca1 2.40(2) 2_554 ?
O8W Ca1 3.05(2) 2_554 ?
O9W Ca1 1.28(3) 2_554 ?

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
O71 Ho1 O11 82.2(3) . . ?
O71 Ho1 O51 133.2(4) . . ?
O11 Ho1 O51 77.1(4) . . ?
O71 Ho1 O61 80.8(3) . . ?
O11 Ho1 O61 129.0(3) . . ?
O51 Ho1 O61 80.6(4) . . ?
O71 Ho1 N4 153.1(4) . . ?
O11 Ho1 N4 86.0(4) . . ?
O51 Ho1 N4 66.2(4) . . ?
O61 Ho1 N4 124.8(4) . . ?
O71 Ho1 N10 65.2(3) . . ?
O11 Ho1 N10 127.6(3) . . ?
O51 Ho1 N10 154.3(4) . . ?
O61 Ho1 N10 86.5(3) . . ?
N4 Ho1 N10 104.8(3) . . ?
O71 Ho1 N7 122.8(3) . . ?
O11 Ho1 N7 154.5(3) . . ?
O51 Ho1 N7 86.9(4) . . ?
O61 Ho1 N7 66.0(3) . . ?
N4 Ho1 N7 69.3(4) . . ?
N10 Ho1 N7 67.5(3) . . ?
O71 Ho1 N1 84.9(3) . . ?
O11 Ho1 N1 69.2(3) . . ?
O51 Ho1 N1 124.2(3) . . ?
O61 Ho1 N1 154.3(3) . . ?
N4 Ho1 N1 68.3(3) . . ?
N10 Ho1 N1 68.2(3) . . ?
N7 Ho1 N1 105.4(3) . . ?
O71 Ho1 O1C 63.2(5) . . ?
O11 Ho1 O1C 63.2(5) . . ?
O51 Ho1 O1C 70.0(6) . . ?
O61 Ho1 O1C 66.2(5) . . ?
N4 Ho1 O1C 130.8(5) . . ?
N10 Ho1 O1C 124.3(5) . . ?
N7 Ho1 O1C 129.4(5) . . ?
N1 Ho1 O1C 124.9(5) . . ?
Ho1 O1C H11C 116.3 . . ?
Ho1 O1C H12C 92.2 . . ?
H11C O1C H12C 97.9 . . ?
C12 N1 C20 110.0(10) . . ?
C12 N1 C2 108.9(9) . . ?
C20 N1 C2 108.1(10) . . ?
C12 N1 Ho1 112.1(7) . . ?
C20 N1 Ho1 107.9(6) . . ?
C2 N1 Ho1 109.7(7) . . ?
C3 C2 N1 111.7(11) . . ?
C3 C2 H21 109.3 . . ?
N1 C2 H21 109.3 . . ?
C3 C2 H22 109.3 . . ?
N1 C2 H22 109.3 . . ?
H21 C2 H22 107.9 . . ?
N4 C3 C2 111.3(11) . . ?
N4 C3 H31 109.4 . . ?
C2 C3 H31 109.4 . . ?
N4 C3 H32 109.4 . . ?
C2 C3 H32 109.4 . . ?
H31 C3 H32 108.0 . . ?
C3 N4 C50 111.8(12) . . ?
C3 N4 C5 109.7(12) . . ?
C50 N4 C5 106.8(11) . . ?
C3 N4 Ho1 113.8(7) . . ?
C50 N4 Ho1 104.7(9) . . ?
C5 N4 Ho1 109.6(9) . . ?
C6 C5 N4 112.6(12) . . ?
C6 C5 H51 109.1 . . ?
N4 C5 H51 109.1 . . ?
C6 C5 H52 109.1 . . ?
N4 C5 H52 109.1 . . ?
H51 C5 H52 107.8 . . ?
N7 C6 C5 110.4(13) . . ?
N7 C6 H61 109.6 . . ?
C5 C6 H61 109.6 . . ?
N7 C6 H62 109.6 . . ?
C5 C6 H62 109.6 . . ?
H61 C6 H62 108.1 . . ?
C8 N7 C60 107.7(11) . . ?
C8 N7 C6 109.5(11) . . ?
C60 N7 C6 111.7(11) . . ?
C8 N7 Ho1 111.9(8) . . ?
C60 N7 Ho1 103.3(8) . . ?
C6 N7 Ho1 112.5(9) . . ?
N7 C8 C9 111.6(11) . . ?
N7 C8 H81 109.3 . . ?
C9 C8 H81 109.3 . . ?
N7 C8 H82 109.3 . . ?
C9 C8 H82 109.3 . . ?
H81 C8 H82 108.0 . . ?
N10 C9 C8 111.2(10) . . ?
N10 C9 H91 109.4 . . ?
C8 C9 H91 109.4 . . ?
N10 C9 H92 109.4 . . ?
C8 C9 H92 109.4 . . ?
H91 C9 H92 108.0 . . ?
C9 N10 C11 109.4(9) . . ?
C9 N10 C70 109.9(10) . . ?
C11 N10 C70 109.1(9) . . ?
C9 N10 Ho1 113.9(7) . . ?
C11 N10 Ho1 110.5(7) . . ?
C70 N10 Ho1 103.7(7) . . ?
N10 C11 C12 112.5(10) . . ?
N10 C11 H111 109.1 . . ?
C12 C11 H111 109.1 . . ?
N10 C11 H112 109.1 . . ?
C12 C11 H112 109.1 . . ?
H111 C11 H112 107.8 . . ?
N1 C12 C11 110.8(10) . . ?
N1 C12 H121 109.5 . . ?
C11 C12 H121 109.5 . . ?
N1 C12 H122 109.5 . . ?
C11 C12 H122 109.5 . . ?
H121 C12 H122 108.1 . . ?
N1 C20 P1 110.2(8) . . ?
N1 C20 H201 109.6 . . ?
P1 C20 H201 109.6 . . ?
N1 C20 H202 109.6 . . ?
P1 C20 H202 109.6 . . ?
H201 C20 H202 108.1 . . ?
O12 P1 O11 116.3(6) . . ?
O12 P1 C21 111.7(6) . . ?
O11 P1 C21 108.2(6) . . ?
O12 P1 C20 111.4(6) . . ?
O11 P1 C20 104.7(6) . . ?
C21 P1 C20 103.6(6) . . ?
P1 O11 Ho1 127.3(5) . . ?
N22 C21 P1 109.5(8) . . ?
N22 C21 H211 109.8 . . ?
P1 C21 H211 109.8 . . ?
N22 C21 H212 109.8 . . ?
P1 C21 H212 109.8 . . ?
H211 C21 H212 108.2 . . ?
C30 N22 C21 112.1(11) . . ?
C30 N22 C40 113.5(13) . . ?
C21 N22 C40 110.7(11) . . ?
N22 C30 C31 111.9(11) . . ?
N22 C30 H301 109.2 . . ?
C31 C30 H301 109.2 . . ?
N22 C30 H302 109.2 . . ?
C31 C30 H302 109.2 . . ?
H301 C30 H302 107.9 . . ?
C32B C31 C36B 115(2) . . ?
C36A C31 C32A 122(2) . . ?
C36A C31 C30 115.6(16) . . ?
C32B C31 C30 120.8(19) . . ?
C36B C31 C30 124.4(15) . . ?
C32A C31 C30 122.2(18) . . ?
C33A C32A C31 116(3) . . ?
C33A C32A H32A 122.0 . . ?
C31 C32A H32A 122.0 . . ?
C34 C33A C32A 125(3) . . ?
C34 C33A H33A 117.7 . . ?
C32A C33A H33A 117.7 . . ?
C35B C34 C33B 125(2) . . ?
C33A C34 C35A 118(2) . . ?
C33A C34 H34A 120.9 . . ?
C35A C34 H34A 120.9 . . ?
C35B C34 H34B 117.4 . . ?
C33B C34 H34B 117.4 . . ?
C36A C35A C34 117(3) . . ?
C36A C35A H35A 121.3 . . ?
C34 C35A H35A 121.3 . . ?
C31 C36A C35A 122(3) . . ?
C31 C36A H36A 119.1 . . ?
C35A C36A H36A 119.1 . . ?
C31 C32B C33B 126(3) . . ?
C31 C32B H32B 117.2 . . ?
C33B C32B H32B 117.2 . . ?
C32B C33B C34 114(3) . . ?
C32B C33B H33B 122.8 . . ?
C34 C33B H33B 122.8 . . ?
C34 C35B C36B 115(3) . . ?
C34 C35B H35B 122.4 . . ?
C36B C35B H35B 122.4 . . ?
C35B C36B C31 124(2) . . ?
C35B C36B H36B 118.1 . . ?
C31 C36B H36B 118.1 . . ?
C41C C40 N22 122.1(19) . . ?
N22 C40 C41D 108.8(16) . . ?
C41C C40 H401 106.8 . . ?
N22 C40 H401 106.8 . . ?
C41C C40 H402 106.8 . . ?
N22 C40 H402 106.8 . . ?
H401 C40 H402 106.7 . . ?
N22 C40 H403 109.9 . . ?
C41D C40 H403 109.9 . . ?
N22 C40 H404 109.9 . . ?
C41D C40 H404 109.9 . . ?
H403 C40 H404 108.3 . . ?
C40 C41C C42C 125.7(19) . . ?
C40 C41C C46C 114.3(19) . . ?
C42C C41C C46C 120.0 . . ?
C41C C42C C43C 120.0 . . ?
C41C C42C H42C 120.0 . . ?
C43C C42C H42C 120.0 . . ?
C44C C43C C42C 120.0 . . ?
C44C C43C H43C 120.0 . . ?
C42C C43C H43C 120.0 . . ?
C43C C44C C45C 120.0 . . ?
C43C C44C H44C 120.0 . . ?
C45C C44C H44C 120.0 . . ?
C44C C45C C46C 120.0 . . ?
C44C C45C H45C 120.0 . . ?
C46C C45C H45C 120.0 . . ?
C45C C46C C41C 120.0 . . ?
C45C C46C H46C 120.0 . . ?
C41C C46C H46C 120.0 . . ?
C42D C41D C46D 120.0 . . ?
C42D C41D C40 118.9(17) . . ?
C46D C41D C40 121.1(17) . . ?
C41D C42D C43D 120.0 . . ?
C41D C42D H42D 120.0 . . ?
C43D C42D H42D 120.0 . . ?
C42D C43D C44D 120.0 . . ?
C42D C43D H43D 120.0 . . ?
C44D C43D H43D 120.0 . . ?
C45D C44D C43D 120.0 . . ?
C45D C44D H44D 120.0 . . ?
C43D C44D H44D 120.0 . . ?
C44D C45D C46D 120.0 . . ?
C44D C45D H45D 120.0 . . ?
C46D C45D H45D 120.0 . . ?
C45D C46D C41D 120.0 . . ?
C45D C46D H46D 120.0 . . ?
C41D C46D H46D 120.0 . . ?
N4 C50 C51 111.9(13) . . ?
N4 C50 H501 109.2 . . ?
C51 C50 H501 109.2 . . ?
N4 C50 H502 109.2 . . ?
C51 C50 H502 109.2 . . ?
H501 C50 H502 107.9 . . ?
O52 C51 O51 122.9(18) . . ?
O52 C51 C50 119.3(17) . . ?
O51 C51 C50 117.8(13) . . ?
C51 O51 Ho1 118.0(9) . . ?
C51 O52 Ca1 129.3(14) . . ?
N7 C60 C61 109.4(11) . . ?
N7 C60 H601 109.8 . . ?
C61 C60 H601 109.8 . . ?
N7 C60 H602 109.8 . . ?
C61 C60 H602 109.8 . . ?
H601 C60 H602 108.2 . . ?
O62 C61 O61 125.1(15) . . ?
O62 C61 C60 118.3(13) . . ?
O61 C61 C60 116.7(12) . . ?
C61 O61 Ho1 123.6(9) . . ?
N10 C70 C71 109.6(10) . . ?
N10 C70 H701 109.8 . . ?
C71 C70 H701 109.8 . . ?
N10 C70 H702 109.8 . . ?
C71 C70 H702 109.8 . . ?
H701 C70 H702 108.2 . . ?
O72 C71 O71 126.2(12) . . ?
O72 C71 C70 116.9(11) . . ?
O71 C71 C70 116.8(10) . . ?
C71 O71 Ho1 120.2(8) . . ?
H11W O1W H12W 124.1 . . ?
H21W O2W H22W 98.9 . . ?
H31W O3W H32W 113.1 . . ?
O9W Ca1 Ca1 124.7(15) 2_554 2_554 ?
O9W Ca1 O8W 123.6(15) 2_554 . ?
Ca1 Ca1 O8W 104.4(8) 2_554 . ?
O9W Ca1 O5W 118.4(14) 2_554 . ?
Ca1 Ca1 O5W 71.4(2) 2_554 . ?
O8W Ca1 O5W 101.1(7) . . ?
Ca1 Ca1 O7W 122.2(9) 2_554 2_554 ?
O8W Ca1 O7W 128.7(10) . 2_554 ?
O5W Ca1 O7W 112.4(7) . 2_554 ?
O9W Ca1 O6W 75.2(15) 2_554 . ?
Ca1 Ca1 O6W 84.2(6) 2_554 . ?
O8W Ca1 O6W 85.1(9) . . ?
O5W Ca1 O6W 155.6(7) . . ?
O7W Ca1 O6W 80.1(8) 2_554 . ?
O9W Ca1 O9W 139.9(16) 2_554 . ?
Ca1 Ca1 O9W 25.1(7) 2_554 . ?
O8W Ca1 O9W 80.1(9) . . ?
O5W Ca1 O9W 82.1(7) . . ?
O6W Ca1 O9W 75.7(9) . . ?
O9W Ca1 O52 82.1(14) 2_554 . ?
Ca1 Ca1 O52 148.7(5) 2_554 . ?
O8W Ca1 O52 64.7(7) . . ?
O5W Ca1 O52 81.8(4) . . ?
O7W Ca1 O52 82.4(7) 2_554 . ?
O6W Ca1 O52 121.7(8) . . ?
O9W Ca1 O52 137.3(8) . . ?
O9W Ca1 O6W 89.9(15) 2_554 2_554 ?
Ca1 Ca1 O6W 62.0(5) 2_554 2_554 ?
O8W Ca1 O6W 90.4(9) . 2_554 ?
O5W Ca1 O6W 133.4(6) . 2_554 ?
O7W Ca1 O6W 93.4(7) 2_554 2_554 ?
O6W Ca1 O6W 22.2(11) . 2_554 ?
O9W Ca1 O6W 55.4(8) . 2_554 ?
O52 Ca1 O6W 141.9(7) . 2_554 ?
O9W Ca1 O8W 79.1(14) 2_554 2_554 ?
Ca1 Ca1 O8W 46.8(6) 2_554 2_554 ?
O8W Ca1 O8W 148.8(6) . 2_554 ?
O5W Ca1 O8W 82.3(5) . 2_554 ?
O7W Ca1 O8W 75.8(8) 2_554 2_554 ?
O6W Ca1 O8W 80.7(9) . 2_554 ?
O9W Ca1 O8W 69.6(8) . 2_554 ?
O52 Ca1 O8W 145.6(6) . 2_554 ?
O6W Ca1 O8W 66.7(8) 2_554 2_554 ?
Ca1 O5W Ca1 37.3(5) . 2_554 ?
O6W O6W Ca1 95.8(6) 2_554 . ?
O6W O6W Ca1 62.0(5) 2_554 2_554 ?
Ca1 O6W Ca1 33.8(4) . 2_554 ?
Ca1 O8W Ca1 28.8(4) . 2_554 ?
Ca1 O9W Ca1 30.2(9) 2_554 . ?

_refine_diff_density_max         5.593
_refine_diff_density_min         -9.245
_refine_diff_density_rms         0.250

