# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1553995'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H35 N2 Nd O11'
_chemical_formula_weight         827.91

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

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 246 59 ' '
2 0.732 0.107 0.266 45 6 ' '
3 0.268 -0.107 0.734 45 5 ' '
4 1.000 0.500 0.500 246 59 ' '
5 0.732 0.393 0.766 45 6 ' '
6 0.268 0.607 0.234 46 5 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_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                   15.986(7)
_cell_length_b                   8.403(3)
_cell_length_c                   28.487(13)
_cell_angle_alpha                90
_cell_angle_beta                 96.253(5)
_cell_angle_gamma                90
_cell_volume                     3804(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11051
_cell_measurement_theta_min      2.0280
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_F_000             1676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.024
_exptl_absorpt_coefficient_mu    1.414
_shelx_estimated_absorpt_T_min   0.890
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8318
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38478
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.528
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_reflns_number_total             8703
_reflns_number_gt                7182
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000       246        59 ' '
   2  0.732  0.107  0.266        45         6 ' '
   3  0.268 -0.107  0.734        45         5 ' '
   4  1.000  0.500  0.500       246        59 ' '
   5  0.732  0.393  0.766        45         6 ' '
   6  0.268  0.607  0.234        46         5 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_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)+(0.0832P)²+12.2291P] 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         8703
_refine_ls_number_parameters     479
_refine_ls_number_restraints     426
_refine_ls_R_factor_all          0.1089
_refine_ls_R_factor_gt           0.0879
_refine_ls_wR_factor_ref         0.2108
_refine_ls_wR_factor_gt          0.1979
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_restrained_S_all      1.174
_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 0.40920(3) 0.18252(5) 0.96124(2) 0.04345(17) Uani 1 1 d . . . . .
O1 O 0.3449(4) -0.0859(7) 0.9536(2) 0.0500(14) Uani 1 1 d . . . . .
O2 O 0.3037(4) 0.0786(7) 0.8959(2) 0.0540(15) Uani 1 1 d . . . . .
O3 O -0.2702(4) -0.2831(7) 1.0224(2) 0.0543(16) Uani 1 1 d . . . . .
O4 O -0.3771(4) -0.4263(7) 0.9908(2) 0.0580(17) Uani 1 1 d . . . . .
O5 O 0.5021(4) -0.4262(8) 0.5950(2) 0.0631(18) Uani 1 1 d . . . . .
O6 O 0.4314(4) -0.5585(7) 0.53630(19) 0.0570(17) Uani 1 1 d . . . . .
O8 O 0.5484(4) 0.2875(7) 0.9914(2) 0.0548(15) Uani 1 1 d . . . . .
H8A H 0.588392 0.202024 0.995443 0.066 Uiso 1 1 d R U . . .
H8B H 0.566242 0.361990 0.971878 0.082 Uiso 1 1 d R U . . .
N1 N 0.1136(4) -0.5575(7) 0.8182(2) 0.0387(14) Uani 1 1 d . . . . .
N2 N 0.4307(13) 0.579(2) 0.8521(7) 0.081(5) Uani 0.5 1 d . U P A 1
O7 O 0.4145(4) 0.3865(8) 0.9040(2) 0.0617(16) Uani 0.5 1 d D . P A 1
C1 C 0.3014(5) -0.0573(10) 0.9139(3) 0.0483(16) Uani 1 1 d . U . . .
C2 C 0.2492(6) -0.1880(9) 0.8896(3) 0.0502(14) Uani 1 1 d . U . . .
C3 C 0.2539(6) -0.3375(10) 0.9071(3) 0.0557(16) Uani 1 1 d . U . . .
H3 H 0.287720 -0.358836 0.935017 0.067 Uiso 1 1 calc R U . . .
C4 C 0.2076(6) -0.4609(10) 0.8832(3) 0.0547(16) Uani 1 1 d . U . . .
H4 H 0.210452 -0.563522 0.895512 0.066 Uiso 1 1 calc R U . . .
C5 C 0.1593(5) -0.4306(10) 0.8424(3) 0.0460(14) Uani 1 1 d . U . . .
C6 C 0.1555(7) -0.2803(11) 0.8247(4) 0.0650(18) Uani 1 1 d . U . . .
H6 H 0.122079 -0.260239 0.796548 0.078 Uiso 1 1 calc R U . . .
C7 C 0.2000(7) -0.1560(11) 0.8475(4) 0.0665(18) Uani 1 1 d . U . . .
H7 H 0.197030 -0.053820 0.834964 0.080 Uiso 1 1 calc R U . . .
C8 C 0.0482(5) -0.6393(10) 0.8351(3) 0.0466(14) Uani 1 1 d . U . . .
C9 C 0.0013(5) -0.5983(10) 0.8715(3) 0.0518(15) Uani 1 1 d . U . . .
H9 H 0.016108 -0.510047 0.890291 0.062 Uiso 1 1 calc R U . . .
C10 C -0.0669(6) -0.6889(11) 0.8794(3) 0.0634(15) Uani 1 1 d . U . . .
C11 C -0.0845(6) -0.8298(12) 0.8533(4) 0.0710(18) Uani 1 1 d . U . . .
H11 H -0.127509 -0.896085 0.861028 0.085 Uiso 1 1 calc R U . . .
C12 C -0.0396(6) -0.8716(12) 0.8168(4) 0.0680(17) Uani 1 1 d . U . . .
H12 H -0.053006 -0.963521 0.799367 0.082 Uiso 1 1 calc R U . . .
C13 C 0.0275(5) -0.7728(11) 0.8059(3) 0.0538(14) Uani 1 1 d . U . . .
C14 C 0.0833(5) -0.7708(10) 0.7702(3) 0.0484(13) Uani 1 1 d . U . . .
C15 C 0.0910(6) -0.8628(11) 0.7297(3) 0.0552(16) Uani 1 1 d . U . . .
H15 H 0.057167 -0.951961 0.723242 0.066 Uiso 1 1 calc R U . . .
C16 C 0.1492(6) -0.8197(11) 0.6995(3) 0.0546(15) Uani 1 1 d . U . . .
H16 H 0.154277 -0.881527 0.672934 0.065 Uiso 1 1 calc R U . . .
C17 C 0.2006(5) -0.6857(10) 0.7079(3) 0.0483(13) Uani 1 1 d . U . . .
C18 C 0.1941(5) -0.5937(10) 0.7483(3) 0.0436(14) Uani 1 1 d . U . . .
H18 H 0.228591 -0.505405 0.754728 0.052 Uiso 1 1 calc R U . . .
C19 C 0.1360(5) -0.6354(9) 0.7786(3) 0.0410(13) Uani 1 1 d . U . . .
C20 C -0.1248(6) -0.6329(12) 0.9142(4) 0.0678(16) Uani 1 1 d . U . . .
C21 C -0.0987(6) -0.5276(12) 0.9504(3) 0.0649(17) Uani 1 1 d . U . . .
H21 H -0.041618 -0.504128 0.956299 0.078 Uiso 1 1 calc R U . . .
C22 C -0.1529(6) -0.4573(11) 0.9776(3) 0.0633(17) Uani 1 1 d . U . . .
H22 H -0.132828 -0.385335 1.000958 0.076 Uiso 1 1 calc R U . . .
C23 C -0.2366(6) -0.4917(11) 0.9708(3) 0.0633(16) Uani 1 1 d . U . . .
C24 C -0.2660(6) -0.6034(12) 0.9366(4) 0.0709(18) Uani 1 1 d . U . . .
H24 H -0.322576 -0.631990 0.933011 0.085 Uiso 1 1 calc R U . . .
C25 C -0.2109(6) -0.6718(12) 0.9080(4) 0.0739(18) Uani 1 1 d . U . . .
H25 H -0.230929 -0.743693 0.884657 0.089 Uiso 1 1 calc R U . . .
C26 C -0.2975(6) -0.3980(11) 0.9968(3) 0.0582(19) Uani 1 1 d . U . . .
C27 C 0.2609(5) -0.6401(10) 0.6737(3) 0.0498(14) Uani 1 1 d . U . . .
C28 C 0.2445(6) -0.6689(10) 0.6258(3) 0.0521(15) Uani 1 1 d . U . . .
H28 H 0.194887 -0.720310 0.614422 0.063 Uiso 1 1 calc R U . . .
C29 C 0.3004(6) -0.6229(11) 0.5943(3) 0.0537(15) Uani 1 1 d . U . . .
H29 H 0.287470 -0.642006 0.562144 0.064 Uiso 1 1 calc R U . . .
C30 C 0.3753(6) -0.5488(11) 0.6105(3) 0.0523(14) Uani 1 1 d . U . . .
C31 C 0.3913(6) -0.5156(11) 0.6581(3) 0.0581(16) Uani 1 1 d . U . . .
H31 H 0.440419 -0.462119 0.669314 0.070 Uiso 1 1 calc R U . . .
C32 C 0.3351(6) -0.5612(11) 0.6896(3) 0.0559(16) Uani 1 1 d . U . . .
H32 H 0.347258 -0.538714 0.721628 0.067 Uiso 1 1 calc R U . . .
C33 C 0.4412(6) -0.5079(11) 0.5782(3) 0.0536(18) Uani 1 1 d . U . . .
C36 C 0.4705(18) 0.675(3) 0.8922(10) 0.094(5) Uani 0.5 1 d . U P A 1
H36A H 0.485333 0.778043 0.880833 0.140 Uiso 0.5 1 calc R U P A 1
H36B H 0.431553 0.688301 0.915330 0.140 Uiso 0.5 1 calc R U P A 1
H36C H 0.520179 0.622525 0.906330 0.140 Uiso 0.5 1 calc R U P A 1
C37 C 0.403(2) 0.695(4) 0.8059(9) 0.131(11) Uani 0.5 1 d . U P A 1
H37A H 0.433468 0.793725 0.809520 0.197 Uiso 0.5 1 calc R U P A 1
H37B H 0.415686 0.643049 0.777539 0.197 Uiso 0.5 1 calc R U P A 1
H37C H 0.343647 0.716579 0.803845 0.197 Uiso 0.5 1 calc R U P A 1
N2A N 0.4663(13) 0.392(3) 0.8344(5) 0.102(3) Uani 0.5 1 d D U P A 2
O7A O 0.4145(4) 0.3865(8) 0.9040(2) 0.0617(16) Uani 0.5 1 d D . P A 2
C37A C 0.5301(16) 0.427(4) 0.7970(9) 0.112(6) Uani 0.5 1 d D U P A 2
H37D H 0.518272 0.358376 0.770287 0.168 Uiso 0.5 1 calc R U P A 2
H37E H 0.524263 0.536191 0.786960 0.168 Uiso 0.5 1 calc R U P A 2
H37F H 0.586624 0.409294 0.811193 0.168 Uiso 0.5 1 calc R U P A 2
C34A C 0.4571(16) 0.457(3) 0.8780(6) 0.101(4) Uani 0.5 1 d D U P A 2
C35A C 0.5205(16) 0.584(3) 0.8881(10) 0.107(5) Uani 0.5 1 d D U P A 2
H35A H 0.542720 0.614215 0.859431 0.160 Uiso 0.5 1 calc R U P A 2
H35B H 0.494604 0.674885 0.901073 0.160 Uiso 0.5 1 calc R U P A 2
H35C H 0.565319 0.545940 0.910449 0.160 Uiso 0.5 1 calc R U P A 2
C36A C 0.4032(16) 0.279(3) 0.8168(10) 0.096(4) Uani 0.5 1 d D U P A 2
H36D H 0.415174 0.240415 0.786538 0.145 Uiso 0.5 1 calc R U P A 2
H36E H 0.403090 0.190972 0.838432 0.145 Uiso 0.5 1 calc R U P A 2
H36F H 0.348951 0.329125 0.813779 0.145 Uiso 0.5 1 calc R U P A 2
C34 C 0.4060(18) 0.424(2) 0.8648(4) 0.098(4) Uani 0.5 1 d D U P A 1
C35 C 0.3661(18) 0.309(3) 0.8237(5) 0.094(4) Uani 0.5 1 d D U P A 1
H35D H 0.364665 0.363062 0.793911 0.141 Uiso 0.5 1 calc R U P A 1
H35E H 0.399653 0.214735 0.823124 0.141 Uiso 0.5 1 calc R U P A 1
H35F H 0.309871 0.280983 0.829394 0.141 Uiso 0.5 1 calc R U P A 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
Nd1 O6 2.371(6) 4_556 ?
Nd1 O7A 2.373(6) . ?
Nd1 O7 2.373(6) . ?
Nd1 O5 2.430(5) 2_656 ?
Nd1 O8 2.460(6) . ?
Nd1 O3 2.469(6) 3_557 ?
Nd1 O1 2.479(5) . ?
Nd1 O2 2.528(6) . ?
Nd1 O4 2.545(5) 3_557 ?
Nd1 C1 2.888(8) . ?
Nd1 C26 2.892(8) 3_557 ?
O1 C1 1.284(10) . ?
O2 C1 1.255(10) . ?
O3 C26 1.260(10) . ?
O4 C26 1.287(10) . ?
O5 C33 1.244(11) . ?
O6 C33 1.260(10) . ?
N1 C8 1.382(8) . ?
N1 C19 1.385(8) . ?
N1 C5 1.427(9) . ?
N2 C34 1.41(3) . ?
N2 C36 1.49(3) . ?
N2 C37 1.66(3) . ?
O7 C34 1.154(10) . ?
C1 C2 1.502(11) . ?
C2 C3 1.350(12) . ?
C2 C7 1.386(14) . ?
C3 C4 1.405(11) . ?
C4 C5 1.348(12) . ?
C5 C6 1.359(12) . ?
C6 C7 1.385(12) . ?
C8 C9 1.386(9) . ?
C8 C13 1.415(11) . ?
C9 C10 1.369(10) . ?
C10 C11 1.410(11) . ?
C10 C20 1.505(10) . ?
C11 C12 1.373(11) . ?
C12 C13 1.417(11) . ?
C13 C14 1.424(9) . ?
C14 C15 1.405(11) . ?
C14 C19 1.420(10) . ?
C15 C16 1.381(11) . ?
C16 C17 1.399(12) . ?
C17 C18 1.402(10) . ?
C17 C27 1.493(10) . ?
C18 C19 1.379(9) . ?
C20 C21 1.388(12) . ?
C20 C25 1.406(13) . ?
C21 C22 1.360(10) . ?
C22 C23 1.362(12) . ?
C23 C24 1.397(12) . ?
C23 C26 1.507(11) . ?
C24 C25 1.388(11) . ?
C27 C28 1.381(11) . ?
C27 C32 1.393(12) . ?
C28 C29 1.389(10) . ?
C29 C30 1.384(13) . ?
C30 C31 1.382(12) . ?
C30 C33 1.511(10) . ?
C31 C32 1.391(10) . ?
N2A C34A 1.381(9) . ?
N2A C36A 1.435(10) . ?
N2A C37A 1.582(10) . ?
O7A C34A 1.214(9) . ?
C34A C35A 1.479(9) . ?
C34 C35 1.596(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Nd1 O7A 157.5(2) 4_556 . ?
O6 Nd1 O7 157.5(2) 4_556 . ?
O6 Nd1 O5 112.9(2) 4_556 2_656 ?
O7 Nd1 O5 75.6(2) . 2_656 ?
O6 Nd1 O8 78.6(2) 4_556 . ?
O7A Nd1 O8 83.2(2) . . ?
O7 Nd1 O8 83.2(2) . . ?
O5 Nd1 O8 78.1(2) 2_656 . ?
O6 Nd1 O3 91.7(2) 4_556 3_557 ?
O7 Nd1 O3 89.0(2) . 3_557 ?
O5 Nd1 O3 148.8(2) 2_656 3_557 ?
O8 Nd1 O3 127.58(19) . 3_557 ?
O6 Nd1 O1 72.47(19) 4_556 . ?
O7A Nd1 O1 130.0(2) . . ?
O7 Nd1 O1 130.0(2) . . ?
O5 Nd1 O1 82.3(2) 2_656 . ?
O8 Nd1 O1 135.0(2) . . ?
O3 Nd1 O1 87.41(19) 3_557 . ?
O6 Nd1 O2 122.35(19) 4_556 . ?
O7A Nd1 O2 79.3(2) . . ?
O7 Nd1 O2 79.3(2) . . ?
O5 Nd1 O2 77.0(2) 2_656 . ?
O8 Nd1 O2 152.45(19) . . ?
O3 Nd1 O2 73.46(19) 3_557 . ?
O1 Nd1 O2 52.0(2) . . ?
O6 Nd1 O4 83.6(2) 4_556 3_557 ?
O7 Nd1 O4 79.2(2) . 3_557 ?
O5 Nd1 O4 145.33(19) 2_656 3_557 ?
O8 Nd1 O4 75.62(19) . 3_557 ?
O3 Nd1 O4 52.04(18) 3_557 3_557 ?
O1 Nd1 O4 132.34(17) . 3_557 ?
O2 Nd1 O4 121.1(2) . 3_557 ?
O6 Nd1 C1 97.9(2) 4_556 . ?
O7A Nd1 C1 104.3(2) . . ?
O7 Nd1 C1 104.3(2) . . ?
O5 Nd1 C1 78.0(2) 2_656 . ?
O8 Nd1 C1 152.2(2) . . ?
O3 Nd1 C1 79.8(2) 3_557 . ?
O1 Nd1 C1 26.3(2) . . ?
O2 Nd1 C1 25.7(2) . . ?
O4 Nd1 C1 131.8(2) 3_557 . ?
O6 Nd1 C26 86.6(2) 4_556 3_557 ?
O7A Nd1 C26 84.4(2) . 3_557 ?
O7 Nd1 C26 84.4(2) . 3_557 ?
O5 Nd1 C26 159.9(3) 2_656 3_557 ?
O8 Nd1 C26 101.9(2) . 3_557 ?
O3 Nd1 C26 25.7(2) 3_557 3_557 ?
O1 Nd1 C26 109.7(2) . 3_557 ?
O2 Nd1 C26 97.4(2) . 3_557 ?
O4 Nd1 C26 26.4(2) 3_557 3_557 ?
C1 Nd1 C26 105.4(2) . 3_557 ?
C1 O1 Nd1 95.0(5) . . ?
C1 O2 Nd1 93.4(5) . . ?
C26 O3 Nd1 96.3(5) . 3_557 ?
C26 O4 Nd1 92.0(4) . 3_557 ?
C33 O5 Nd1 116.3(5) . 2_646 ?
C33 O6 Nd1 173.4(6) . 4 ?
C8 N1 C19 108.7(6) . . ?
C8 N1 C5 124.7(6) . . ?
C19 N1 C5 125.7(6) . . ?
C34 N2 C36 114.4(17) . . ?
C34 N2 C37 133.3(19) . . ?
C36 N2 C37 109.9(19) . . ?
C34 O7 Nd1 148.6(10) . . ?
O2 C1 O1 119.6(7) . . ?
O2 C1 C2 121.0(8) . . ?
O1 C1 C2 119.3(8) . . ?
O2 C1 Nd1 60.9(4) . . ?
O1 C1 Nd1 58.8(4) . . ?
C2 C1 Nd1 177.0(6) . . ?
C3 C2 C7 120.2(8) . . ?
C3 C2 C1 120.3(9) . . ?
C7 C2 C1 119.4(8) . . ?
C2 C3 C4 120.2(9) . . ?
C5 C4 C3 120.0(8) . . ?
C4 C5 C6 119.6(8) . . ?
C4 C5 N1 119.4(7) . . ?
C6 C5 N1 121.0(8) . . ?
C5 C6 C7 121.8(10) . . ?
C6 C7 C2 118.3(9) . . ?
N1 C8 C9 128.9(7) . . ?
N1 C8 C13 109.0(6) . . ?
C9 C8 C13 121.8(7) . . ?
C10 C9 C8 119.3(7) . . ?
C9 C10 C11 119.8(7) . . ?
C9 C10 C20 119.5(7) . . ?
C11 C10 C20 120.6(7) . . ?
C12 C11 C10 121.6(8) . . ?
C11 C12 C13 119.1(8) . . ?
C8 C13 C12 117.9(7) . . ?
C8 C13 C14 106.7(6) . . ?
C12 C13 C14 135.3(8) . . ?
C15 C14 C19 118.5(7) . . ?
C15 C14 C13 134.2(8) . . ?
C19 C14 C13 107.2(6) . . ?
C16 C15 C14 119.3(8) . . ?
C15 C16 C17 122.0(7) . . ?
C16 C17 C18 119.2(7) . . ?
C16 C17 C27 120.4(7) . . ?
C18 C17 C27 120.4(7) . . ?
C19 C18 C17 119.2(7) . . ?
C18 C19 N1 129.8(7) . . ?
C18 C19 C14 121.7(6) . . ?
N1 C19 C14 108.4(6) . . ?
C21 C20 C25 116.9(8) . . ?
C21 C20 C10 122.1(8) . . ?
C25 C20 C10 120.5(8) . . ?
C22 C21 C20 122.7(9) . . ?
C21 C22 C23 120.3(8) . . ?
C22 C23 C24 119.5(8) . . ?
C22 C23 C26 119.8(8) . . ?
C24 C23 C26 120.5(8) . . ?
C25 C24 C23 120.0(9) . . ?
C24 C25 C20 120.3(9) . . ?
O3 C26 O4 119.5(7) . . ?
O3 C26 C23 118.8(8) . . ?
O4 C26 C23 121.4(7) . . ?
O3 C26 Nd1 58.1(4) . 3_557 ?
O4 C26 Nd1 61.6(4) . 3_557 ?
C23 C26 Nd1 172.3(6) . 3_557 ?
C28 C27 C32 118.0(7) . . ?
C28 C27 C17 122.2(8) . . ?
C32 C27 C17 119.8(7) . . ?
C27 C28 C29 121.6(9) . . ?
C30 C29 C28 120.2(8) . . ?
C31 C30 C29 118.7(7) . . ?
C31 C30 C33 119.1(9) . . ?
C29 C30 C33 122.3(8) . . ?
C30 C31 C32 121.0(9) . . ?
C31 C32 C27 120.5(8) . . ?
O5 C33 O6 124.1(7) . . ?
O5 C33 C30 117.3(8) . . ?
O6 C33 C30 118.5(9) . . ?
C34A N2A C36A 116.0(16) . . ?
C34A N2A C37A 132.0(18) . . ?
C36A N2A C37A 111.8(18) . . ?
C34A O7A Nd1 146.8(16) . . ?
O7A C34A N2A 118.4(11) . . ?
O7A C34A C35A 130.7(12) . . ?
N2A C34A C35A 109.0(16) . . ?
O7 C34 N2 119.5(15) . . ?
O7 C34 C35 122.6(13) . . ?
N2 C34 C35 117.9(14) . . ?

_refine_diff_density_max         1.496
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.130

####################################################################### 
# 
# 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_HO
_database_code_depnum_ccdc_archive 'CCDC 1554001'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H35 Ho N2 O11'
_chemical_formula_weight         848.60
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'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 218 83 ' '
2 0.740 0.125 0.265 38 6 ' '
3 0.260 -0.125 0.734 39 6 ' '
4 1.000 0.500 0.500 218 83 ' '
5 0.740 0.375 0.765 38 6 ' '
6 0.260 0.625 0.235 38 6 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_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                   15.682(5)
_cell_length_b                   8.316(3)
_cell_length_c                   28.526(11)
_cell_angle_alpha                90
_cell_angle_beta                 96.325(9)
_cell_angle_gamma                90
_cell_volume                     3697(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10313
_cell_measurement_theta_min      2.0457
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_F_000             1704
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.021
_exptl_absorpt_coefficient_mu    2.190
_shelx_estimated_absorpt_T_min   0.806
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8257
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37160
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_av_R_equivalents  0.0866
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.553
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_reflns_number_total             8471
_reflns_number_gt                7042
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000       218        83 ' '
   2  0.740  0.125  0.265        38         6 ' '
   3  0.260 -0.125  0.734        39         6 ' '
   4  1.000  0.500  0.500       218        83 ' '
   5  0.740  0.375  0.765        38         6 ' '
   6  0.260  0.625  0.235        38         6 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_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)+(0.0544P)²+17.8854P] 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         8471
_refine_ls_number_parameters     479
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0842
_refine_ls_wR_factor_ref         0.1804
_refine_ls_wR_factor_gt          0.1685
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.182
_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
Ho1 Ho 0.40746(2) 0.18720(5) 0.95915(2) 0.03168(13) Uani 1 1 d . . . . .
O1 O 0.3066(4) 0.0876(8) 0.8937(2) 0.0440(15) Uani 1 1 d . . . . .
O2 O 0.3449(4) -0.0751(8) 0.9526(2) 0.0429(15) Uani 1 1 d . . . . .
O3 O 0.5006(4) -0.4382(9) 0.5882(2) 0.0456(16) Uani 1 1 d . . . . .
O4 O 0.4233(4) -0.5741(8) 0.53188(19) 0.0406(14) Uani 1 1 d . . . . .
O5 O -0.2701(4) -0.2837(8) 1.0262(2) 0.0379(14) Uani 1 1 d . . . . .
O6 O -0.3784(4) -0.4312(8) 0.9962(2) 0.0426(15) Uani 1 1 d . . . . .
O8 O 0.5446(4) 0.2784(7) 0.9912(2) 0.0397(14) Uani 1 1 d . . . . .
H8B H 0.555205 0.385179 0.980142 0.048 Uiso 1 1 d R U . . .
H8A H 0.583769 0.214741 0.982837 0.060 Uiso 1 1 d R U . . .
N1 N 0.1125(4) -0.5579(10) 0.8179(2) 0.0368(16) Uani 1 1 d . . . . .
N2 N 0.4324(16) 0.571(3) 0.8528(9) 0.092(7) Uani 0.5 1 d . U P A 1
O7 O 0.4205(4) 0.3804(8) 0.9041(2) 0.0460(16) Uani 0.5 1 d . . P A 1
N2A N 0.4698(17) 0.394(3) 0.8304(5) 0.099(8) Uani 0.5 1 d D U P A 2
O7A O 0.4205(4) 0.3804(8) 0.9041(2) 0.0460(16) Uani 0.5 1 d D . P A 2
C1 C 0.3030(6) -0.0459(12) 0.9127(3) 0.039(2) Uani 1 1 d . . . . .
C2 C 0.2491(6) -0.1813(11) 0.8879(3) 0.0366(19) Uani 1 1 d . . . . .
C3 C 0.2547(8) -0.3320(13) 0.9050(3) 0.059(3) Uani 1 1 d . . . . .
H3 H 0.289054 -0.351992 0.933107 0.071 Uiso 1 1 calc R U . . .
C4 C 0.2106(7) -0.4576(12) 0.8820(3) 0.055(3) Uani 1 1 d . . . . .
H4 H 0.215849 -0.561460 0.894054 0.066 Uiso 1 1 calc R U . . .
C5 C 0.1593(5) -0.4272(12) 0.8414(3) 0.040(2) Uani 1 1 d . . . . .
C6 C 0.1528(9) -0.2772(14) 0.8230(5) 0.078(4) Uani 1 1 d . . . . .
H6 H 0.118335 -0.257465 0.794911 0.094 Uiso 1 1 calc R U . . .
C7 C 0.1986(9) -0.1531(16) 0.8469(5) 0.085(4) Uani 1 1 d . . . . .
H7 H 0.194542 -0.049408 0.834609 0.102 Uiso 1 1 calc R U . . .
C8 C 0.0496(5) -0.6460(11) 0.8373(3) 0.0333(19) Uani 1 1 d . . . . .
C9 C 0.0027(6) -0.6035(11) 0.8734(3) 0.041(2) Uani 1 1 d . . . . .
H9 H 0.015954 -0.510033 0.890541 0.049 Uiso 1 1 calc R U . . .
C10 C -0.0649(6) -0.7017(13) 0.8841(3) 0.047(2) Uani 1 1 d . . . . .
C11 C -0.0803(8) -0.8441(14) 0.8585(4) 0.068(4) Uani 1 1 d . . . . .
H11 H -0.123769 -0.911837 0.866260 0.082 Uiso 1 1 calc R U . . .
C12 C -0.0344(7) -0.8884(15) 0.8225(4) 0.066(4) Uani 1 1 d . . . . .
H12 H -0.045348 -0.985704 0.806879 0.079 Uiso 1 1 calc R U . . .
C13 C 0.0295(6) -0.7841(12) 0.8094(3) 0.046(2) Uani 1 1 d . . . . .
C14 C 0.0842(6) -0.7819(12) 0.7720(3) 0.041(2) Uani 1 1 d . . . . .
C15 C 0.0922(7) -0.8782(14) 0.7323(4) 0.060(3) Uani 1 1 d . . . . .
H15 H 0.059079 -0.970514 0.726940 0.072 Uiso 1 1 calc R U . . .
C16 C 0.1496(7) -0.8347(14) 0.7013(4) 0.062(3) Uani 1 1 d . . . . .
H16 H 0.155407 -0.900348 0.675507 0.074 Uiso 1 1 calc R U . . .
C17 C 0.1997(6) -0.6947(13) 0.7074(3) 0.043(2) Uani 1 1 d . . . . .
C18 C 0.1932(6) -0.5991(11) 0.7473(3) 0.036(2) Uani 1 1 d . . . . .
H18 H 0.227935 -0.509000 0.753127 0.044 Uiso 1 1 calc R U . . .
C19 C 0.1348(6) -0.6409(11) 0.7777(3) 0.038(2) Uani 1 1 d . . . . .
C20 C -0.1222(7) -0.6440(12) 0.9187(4) 0.050(3) Uani 1 1 d . . . . .
C21 C -0.0937(6) -0.5351(14) 0.9544(3) 0.050(3) Uani 1 1 d . . . . .
H21 H -0.035594 -0.510355 0.959775 0.060 Uiso 1 1 calc R U . . .
C22 C -0.1507(6) -0.4634(13) 0.9818(3) 0.049(3) Uani 1 1 d . . . . .
H22 H -0.130205 -0.389327 1.004766 0.058 Uiso 1 1 calc R U . . .
C23 C -0.2366(6) -0.4990(12) 0.9760(3) 0.040(2) Uani 1 1 d . . . . .
C24 C -0.2673(8) -0.6102(15) 0.9418(4) 0.067(4) Uani 1 1 d . . . . .
H24 H -0.325433 -0.634983 0.937229 0.081 Uiso 1 1 calc R U . . .
C25 C -0.2092(7) -0.6854(15) 0.9141(4) 0.069(4) Uani 1 1 d . . . . .
H25 H -0.229314 -0.763807 0.892360 0.082 Uiso 1 1 calc R U . . .
C26 C -0.2982(5) -0.4025(11) 1.0013(3) 0.0342(19) Uani 1 1 d . . . . .
C27 C 0.2596(6) -0.6486(12) 0.6727(3) 0.042(2) Uani 1 1 d . . . . .
C28 C 0.2394(6) -0.6803(12) 0.6246(3) 0.043(2) Uani 1 1 d . . . . .
H28 H 0.188309 -0.732327 0.614118 0.051 Uiso 1 1 calc R U . . .
C29 C 0.2958(6) -0.6339(13) 0.5921(3) 0.044(2) Uani 1 1 d . . . . .
H29 H 0.281051 -0.653216 0.560166 0.053 Uiso 1 1 calc R U . . .
C30 C 0.3726(6) -0.5603(12) 0.6070(3) 0.039(2) Uani 1 1 d . . . . .
C31 C 0.3909(6) -0.5251(13) 0.6542(3) 0.050(3) Uani 1 1 d . . . . .
H31 H 0.441686 -0.472014 0.664545 0.060 Uiso 1 1 calc R U . . .
C32 C 0.3348(6) -0.5674(15) 0.6866(3) 0.055(3) Uani 1 1 d . . . . .
H32 H 0.348254 -0.540481 0.718222 0.066 Uiso 1 1 calc R U . . .
C33 C 0.4359(5) -0.5191(11) 0.5731(3) 0.0342(19) Uani 1 1 d . . . . .
C34 C 0.4107(17) 0.419(3) 0.8642(9) 0.063(6) Uani 0.5 1 d . U P A 1
C35 C 0.374(2) 0.315(4) 0.8240(10) 0.076(9) Uani 0.5 1 d . U P A 1
H35A H 0.372523 0.374599 0.795036 0.114 Uiso 0.5 1 calc R U P A 1
H35B H 0.408234 0.220856 0.822315 0.114 Uiso 0.5 1 calc R U P A 1
H35C H 0.316224 0.284643 0.828858 0.114 Uiso 0.5 1 calc R U P A 1
C36 C 0.4719(17) 0.669(3) 0.8925(9) 0.066(7) Uani 0.5 1 d . . P A 1
H36A H 0.485008 0.774212 0.881265 0.098 Uiso 0.5 1 calc R U P A 1
H36B H 0.432671 0.678982 0.915933 0.098 Uiso 0.5 1 calc R U P A 1
H36C H 0.523745 0.618452 0.906205 0.098 Uiso 0.5 1 calc R U P A 1
C37 C 0.406(2) 0.703(5) 0.8055(10) 0.122(11) Uani 0.5 1 d . U P A 1
H37A H 0.436661 0.802589 0.811506 0.183 Uiso 0.5 1 calc R U P A 1
H37B H 0.422497 0.655832 0.777032 0.183 Uiso 0.5 1 calc R U P A 1
H37C H 0.345730 0.723233 0.801956 0.183 Uiso 0.5 1 calc R U P A 1
C34A C 0.464(2) 0.440(5) 0.8732(12) 0.093(9) Uani 0.5 1 d . U P A 2
C35A C 0.525(3) 0.585(5) 0.8894(14) 0.126(13) Uani 0.5 1 d . U P A 2
H35D H 0.554670 0.619990 0.863465 0.189 Uiso 0.5 1 calc R U P A 2
H35E H 0.491113 0.672641 0.899346 0.189 Uiso 0.5 1 calc R U P A 2
H35F H 0.565842 0.552477 0.915088 0.189 Uiso 0.5 1 calc R U P A 2
C36A C 0.4080(19) 0.261(4) 0.8139(9) 0.064(7) Uani 0.5 1 d . . P A 2
H36D H 0.415438 0.233131 0.781915 0.095 Uiso 0.5 1 calc R U P A 2
H36E H 0.419076 0.168661 0.833740 0.095 Uiso 0.5 1 calc R U P A 2
H36F H 0.350279 0.297319 0.815417 0.095 Uiso 0.5 1 calc R U P A 2
C37A C 0.553(3) 0.406(8) 0.7869(16) 0.24(3) Uani 0.5 1 d D U P A 2
H37D H 0.531168 0.355385 0.757822 0.366 Uiso 0.5 1 calc R U P A 2
H37E H 0.565813 0.516651 0.781176 0.366 Uiso 0.5 1 calc R U P A 2
H37F H 0.604520 0.351914 0.799851 0.366 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ho1 O4 2.267(6) 4_556 ?
Ho1 O7A 2.271(6) . ?
Ho1 O7 2.271(6) . ?
Ho1 O3 2.328(6) 2_656 ?
Ho1 O8 2.367(6) . ?
Ho1 O5 2.379(6) 3_557 ?
Ho1 O2 2.390(7) . ?
Ho1 O1 2.454(6) . ?
Ho1 O6 2.465(6) 3_557 ?
Ho1 C1 2.778(9) . ?
Ho1 C26 2.800(8) 3_557 ?
O1 C1 1.240(11) . ?
O2 C1 1.273(10) . ?
O3 C33 1.253(11) . ?
O4 C33 1.256(10) . ?
O5 C26 1.266(10) . ?
O6 C26 1.273(10) . ?
N1 C8 1.392(10) . ?
N1 C19 1.415(10) . ?
N1 C5 1.436(11) . ?
N2 C34 1.36(4) . ?
N2 C36 1.48(3) . ?
N2 C37 1.75(4) . ?
O7 C34 1.18(3) . ?
N2A C34A 1.29(3) . ?
N2A C36A 1.51(4) . ?
N2A C37A 1.901(10) . ?
O7A C34A 1.28(4) . ?
C1 C2 1.533(12) . ?
C2 C3 1.345(13) . ?
C2 C7 1.358(15) . ?
C3 C4 1.378(13) . ?
C4 C5 1.358(12) . ?
C5 C6 1.353(15) . ?
C6 C7 1.393(15) . ?
C8 C9 1.375(11) . ?
C8 C13 1.412(12) . ?
C9 C10 1.399(13) . ?
C10 C11 1.399(14) . ?
C10 C20 1.485(12) . ?
C11 C12 1.368(13) . ?
C12 C13 1.407(13) . ?
C13 C14 1.442(12) . ?
C14 C15 1.404(12) . ?
C14 C19 1.414(12) . ?
C15 C16 1.376(13) . ?
C16 C17 1.404(14) . ?
C17 C18 1.402(12) . ?
C17 C27 1.488(12) . ?
C18 C19 1.374(11) . ?
C20 C21 1.398(14) . ?
C20 C25 1.400(14) . ?
C21 C22 1.387(12) . ?
C22 C23 1.371(12) . ?
C23 C24 1.391(14) . ?
C23 C26 1.500(12) . ?
C24 C25 1.416(14) . ?
C27 C32 1.379(13) . ?
C27 C28 1.397(12) . ?
C28 C29 1.404(12) . ?
C29 C30 1.376(13) . ?
C30 C31 1.376(12) . ?
C30 C33 1.501(11) . ?
C31 C32 1.390(12) . ?
C34 C35 1.50(4) . ?
C34A C35A 1.58(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ho1 O7A 156.5(2) 4_556 . ?
O4 Ho1 O7 156.5(2) 4_556 . ?
O4 Ho1 O3 109.4(2) 4_556 2_656 ?
O7 Ho1 O3 78.9(2) . 2_656 ?
O4 Ho1 O8 77.1(2) 4_556 . ?
O7A Ho1 O8 83.9(2) . . ?
O7 Ho1 O8 83.9(2) . . ?
O3 Ho1 O8 76.9(2) 2_656 . ?
O4 Ho1 O5 89.3(2) 4_556 3_557 ?
O7 Ho1 O5 92.0(2) . 3_557 ?
O3 Ho1 O5 152.2(2) 2_656 3_557 ?
O8 Ho1 O5 128.7(2) . 3_557 ?
O4 Ho1 O2 72.3(2) 4_556 . ?
O7A Ho1 O2 131.2(2) . . ?
O7 Ho1 O2 131.2(2) . . ?
O3 Ho1 O2 79.7(2) 2_656 . ?
O8 Ho1 O2 132.1(2) . . ?
O5 Ho1 O2 87.1(2) 3_557 . ?
O4 Ho1 O1 123.5(2) 4_556 . ?
O7A Ho1 O1 79.2(2) . . ?
O7 Ho1 O1 79.2(2) . . ?
O3 Ho1 O1 78.3(2) 2_656 . ?
O8 Ho1 O1 152.1(2) . . ?
O5 Ho1 O1 74.2(2) 3_557 . ?
O2 Ho1 O1 53.7(2) . . ?
O4 Ho1 O6 82.9(2) 4_556 3_557 ?
O7 Ho1 O6 79.1(2) . 3_557 ?
O3 Ho1 O6 146.1(2) 2_656 3_557 ?
O8 Ho1 O6 75.4(2) . 3_557 ?
O5 Ho1 O6 53.7(2) 3_557 3_557 ?
O2 Ho1 O6 133.9(2) . 3_557 ?
O1 Ho1 O6 122.0(2) . 3_557 ?
O4 Ho1 C1 98.4(3) 4_556 . ?
O7A Ho1 C1 104.9(3) . . ?
O7 Ho1 C1 104.9(3) . . ?
O3 Ho1 C1 77.4(3) 2_656 . ?
O8 Ho1 C1 150.5(2) . . ?
O5 Ho1 C1 79.7(2) 3_557 . ?
O2 Ho1 C1 27.2(2) . . ?
O1 Ho1 C1 26.5(2) . . ?
O6 Ho1 C1 133.4(2) 3_557 . ?
O4 Ho1 C26 84.6(2) 4_556 3_557 ?
O7A Ho1 C26 86.1(2) . 3_557 ?
O7 Ho1 C26 86.1(2) . 3_557 ?
O3 Ho1 C26 165.0(3) 2_656 3_557 ?
O8 Ho1 C26 102.1(2) . 3_557 ?
O5 Ho1 C26 26.8(2) 3_557 3_557 ?
O2 Ho1 C26 110.5(2) . 3_557 ?
O1 Ho1 C26 98.6(2) . 3_557 ?
O6 Ho1 C26 27.0(2) 3_557 3_557 ?
C1 Ho1 C26 106.4(3) . 3_557 ?
C1 O1 Ho1 91.5(5) . . ?
C1 O2 Ho1 93.6(6) . . ?
C33 O3 Ho1 124.8(5) . 2_646 ?
C33 O4 Ho1 175.9(6) . 4 ?
C26 O5 Ho1 95.5(5) . 3_557 ?
C26 O6 Ho1 91.3(5) . 3_557 ?
C8 N1 C19 108.3(7) . . ?
C8 N1 C5 124.1(6) . . ?
C19 N1 C5 126.1(7) . . ?
C34 N2 C36 115(2) . . ?
C34 N2 C37 136(2) . . ?
C36 N2 C37 107(2) . . ?
C34 O7 Ho1 148.0(14) . . ?
C34A N2A C36A 114(2) . . ?
C34A N2A C37A 136(3) . . ?
C36A N2A C37A 107(3) . . ?
C34A O7A Ho1 147.9(17) . . ?
O1 C1 O2 121.2(8) . . ?
O1 C1 C2 120.2(8) . . ?
O2 C1 C2 118.5(8) . . ?
O1 C1 Ho1 62.0(5) . . ?
O2 C1 Ho1 59.2(5) . . ?
C2 C1 Ho1 176.9(7) . . ?
C3 C2 C7 118.8(9) . . ?
C3 C2 C1 120.3(8) . . ?
C7 C2 C1 120.7(9) . . ?
C2 C3 C4 121.6(9) . . ?
C5 C4 C3 118.9(10) . . ?
C6 C5 C4 121.0(9) . . ?
C6 C5 N1 120.2(8) . . ?
C4 C5 N1 118.8(9) . . ?
C5 C6 C7 118.7(11) . . ?
C2 C7 C6 120.9(12) . . ?
C9 C8 N1 128.5(8) . . ?
C9 C8 C13 121.7(8) . . ?
N1 C8 C13 109.2(7) . . ?
C8 C9 C10 119.7(8) . . ?
C9 C10 C11 118.0(8) . . ?
C9 C10 C20 119.1(9) . . ?
C11 C10 C20 122.6(9) . . ?
C12 C11 C10 123.1(10) . . ?
C11 C12 C13 118.8(10) . . ?
C12 C13 C8 118.3(8) . . ?
C12 C13 C14 134.7(9) . . ?
C8 C13 C14 107.0(7) . . ?
C15 C14 C19 117.9(8) . . ?
C15 C14 C13 134.7(9) . . ?
C19 C14 C13 107.3(8) . . ?
C16 C15 C14 119.3(9) . . ?
C15 C16 C17 122.4(9) . . ?
C18 C17 C16 118.7(8) . . ?
C18 C17 C27 120.1(9) . . ?
C16 C17 C27 121.2(8) . . ?
C19 C18 C17 118.8(8) . . ?
C18 C19 N1 129.0(9) . . ?
C18 C19 C14 122.8(8) . . ?
N1 C19 C14 108.2(7) . . ?
C21 C20 C25 117.3(9) . . ?
C21 C20 C10 121.6(9) . . ?
C25 C20 C10 120.8(9) . . ?
C22 C21 C20 121.0(9) . . ?
C23 C22 C21 121.7(9) . . ?
C22 C23 C24 119.2(9) . . ?
C22 C23 C26 120.1(8) . . ?
C24 C23 C26 120.1(9) . . ?
C23 C24 C25 119.5(10) . . ?
C20 C25 C24 121.2(10) . . ?
O5 C26 O6 119.3(7) . . ?
O5 C26 C23 119.0(7) . . ?
O6 C26 C23 121.6(8) . . ?
O5 C26 Ho1 57.7(4) . 3_557 ?
O6 C26 Ho1 61.7(4) . 3_557 ?
C23 C26 Ho1 172.2(6) . 3_557 ?
C32 C27 C28 118.1(8) . . ?
C32 C27 C17 121.1(8) . . ?
C28 C27 C17 120.8(8) . . ?
C27 C28 C29 120.2(9) . . ?
C30 C29 C28 120.9(8) . . ?
C29 C30 C31 118.5(8) . . ?
C29 C30 C33 121.5(8) . . ?
C31 C30 C33 120.0(8) . . ?
C30 C31 C32 121.2(9) . . ?
C27 C32 C31 121.0(8) . . ?
O4 C33 O3 123.7(7) . . ?
O4 C33 C30 118.2(8) . . ?
O3 C33 C30 117.9(7) . . ?
O7 C34 N2 118(2) . . ?
O7 C34 C35 126(2) . . ?
N2 C34 C35 116(3) . . ?
O7A C34A N2A 129(3) . . ?
O7A C34A C35A 117(3) . . ?
N2A C34A C35A 114(3) . . ?

_refine_diff_density_max         1.059
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.144

####################################################################### 
# 
# 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_SM
_database_code_depnum_ccdc_archive 'CCDC 1553996'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H33 N2 O10 Sm'
_chemical_formula_weight         816.00

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

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 227 86 ' '
2 0.735 0.128 0.265 40 6 ' '
3 0.265 -0.128 0.735 41 6 ' '
4 1.000 0.500 0.500 227 86 ' '
5 0.735 0.372 0.765 41 6 ' '
6 0.265 0.628 0.235 41 6 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_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                   15.793(7)
_cell_length_b                   8.363(3)
_cell_length_c                   28.515(12)
_cell_angle_alpha                90
_cell_angle_beta                 96.516(7)
_cell_angle_gamma                90
_cell_volume                     3742(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10319
_cell_measurement_theta_min      2.0433
_cell_measurement_theta_max      27.4816

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_F_000             1644
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.027
_exptl_absorpt_coefficient_mu    1.619
_shelx_estimated_absorpt_T_min   0.841
_shelx_estimated_absorpt_T_max   0.958
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7955
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37343
_diffrn_reflns_av_unetI/netI     0.0638
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.596
_diffrn_reflns_theta_max         27.461
_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
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_reflns_number_total             8539
_reflns_number_gt                7084
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000       227        86 ' '
   2  0.735  0.128  0.265        40         6 ' '
   3  0.265 -0.128  0.735        41         6 ' '
   4  1.000  0.500  0.500       227        86 ' '
   5  0.735  0.372  0.765        41         6 ' '
   6  0.265  0.628  0.235        41         6 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_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)+(0.0888P)²+11.4823P] 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         8539
_refine_ls_number_parameters     479
_refine_ls_number_restraints     432
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0770
_refine_ls_wR_factor_ref         0.1976
_refine_ls_wR_factor_gt          0.1846
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.118
_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 0.40798(2) 0.18539(4) 0.95994(2) 0.03375(14) Uani 1 1 d . . . . .
O1 O 0.3040(3) 0.0812(6) 0.89398(19) 0.0449(12) Uani 1 1 d . . . . .
O2 O 0.3442(3) -0.0806(6) 0.95252(18) 0.0432(12) Uani 1 1 d . . . . .
O3 O 0.4995(3) -0.4303(7) 0.59189(18) 0.0489(13) Uani 1 1 d . . . . .
O4 O 0.4273(3) -0.5663(6) 0.53434(17) 0.0441(12) Uani 1 1 d . . . . .
O5 O -0.2679(3) -0.2852(6) 1.02444(19) 0.0442(12) Uani 1 1 d . . . . .
O6 O -0.3767(3) -0.4298(6) 0.99375(19) 0.0458(12) Uani 1 1 d . . . . .
O8 O 0.5477(3) 0.2837(6) 0.99121(19) 0.0416(12) Uani 1 1 d . . . . .
H8A H 0.590225 0.202796 0.988529 0.050 Uiso 1 1 d R U . . .
H8B H 0.561171 0.370378 0.975857 0.062 Uiso 1 1 d R U . . .
N1 N 0.1125(4) -0.5610(7) 0.8173(2) 0.0375(13) Uani 1 1 d . . . . .
N2 N 0.4337(12) 0.574(2) 0.8519(6) 0.080(5) Uani 0.5 1 d D U P A 1
O7 O 0.4178(4) 0.3857(7) 0.9036(2) 0.0536(14) Uani 0.5 1 d . . P A 1
N2A N 0.4688(14) 0.395(3) 0.8294(7) 0.103(7) Uani 0.5 1 d D U P A 2
O7A O 0.4178(4) 0.3857(7) 0.9036(2) 0.0536(14) Uani 0.5 1 d . . P A 2
C1 C 0.3023(5) -0.0534(9) 0.9124(3) 0.0417(15) Uani 1 1 d . U . . .
C2 C 0.2463(5) -0.1844(7) 0.8876(2) 0.0343(13) Uani 1 1 d . U . . .
C3 C 0.2538(6) -0.3354(9) 0.9052(3) 0.0521(18) Uani 1 1 d . U . . .
H3 H 0.289729 -0.354916 0.932781 0.063 Uiso 1 1 calc R U . . .
C4 C 0.2094(6) -0.4585(10) 0.8829(3) 0.0555(19) Uani 1 1 d . U . . .
H4 H 0.213210 -0.560436 0.895941 0.067 Uiso 1 1 calc R U . . .
C5 C 0.1591(5) -0.4322(10) 0.8411(3) 0.0428(15) Uani 1 1 d . U . . .
C6 C 0.1525(7) -0.2803(12) 0.8228(4) 0.068(2) Uani 1 1 d . U . . .
H6 H 0.116379 -0.260089 0.795340 0.082 Uiso 1 1 calc R U . . .
C7 C 0.2003(7) -0.1555(12) 0.8455(4) 0.069(2) Uani 1 1 d . U . . .
H7 H 0.200356 -0.054573 0.831801 0.083 Uiso 1 1 calc R U . . .
C8 C 0.0494(5) -0.6474(9) 0.8364(3) 0.0404(15) Uani 1 1 d . U . . .
C9 C 0.0028(5) -0.6031(9) 0.8732(3) 0.0437(16) Uani 1 1 d . U . . .
H9 H 0.016516 -0.511181 0.890732 0.052 Uiso 1 1 calc R U . . .
C10 C -0.0643(5) -0.6998(10) 0.8827(3) 0.0524(17) Uani 1 1 d . U . . .
C11 C -0.0807(6) -0.8433(11) 0.8577(4) 0.066(2) Uani 1 1 d . U . . .
H11 H -0.123998 -0.909949 0.865638 0.079 Uiso 1 1 calc R U . . .
C12 C -0.0343(6) -0.8879(11) 0.8218(4) 0.066(2) Uani 1 1 d . U . . .
H12 H -0.044696 -0.984621 0.806079 0.080 Uiso 1 1 calc R U . . .
C13 C 0.0299(5) -0.7822(10) 0.8094(3) 0.0505(17) Uani 1 1 d . U . . .
C14 C 0.0834(5) -0.7819(10) 0.7714(3) 0.0475(16) Uani 1 1 d . U . . .
C15 C 0.0905(6) -0.8748(12) 0.7311(3) 0.058(2) Uani 1 1 d . U . . .
H15 H 0.056726 -0.965238 0.725074 0.070 Uiso 1 1 calc R U . . .
C16 C 0.1480(6) -0.8308(11) 0.7005(3) 0.057(2) Uani 1 1 d . U . . .
H16 H 0.152881 -0.894348 0.674221 0.069 Uiso 1 1 calc R U . . .
C17 C 0.1998(5) -0.6930(10) 0.7076(3) 0.0447(15) Uani 1 1 d . U . . .
C18 C 0.1921(5) -0.6014(9) 0.7475(2) 0.0410(15) Uani 1 1 d . U . . .
H18 H 0.226591 -0.512059 0.753792 0.049 Uiso 1 1 calc R U . . .
C19 C 0.1340(5) -0.6423(9) 0.7775(3) 0.0406(15) Uani 1 1 d . U . . .
C20 C -0.1218(5) -0.6456(11) 0.9175(3) 0.0550(18) Uani 1 1 d . U . . .
C21 C -0.0947(5) -0.5372(11) 0.9539(3) 0.0530(18) Uani 1 1 d . U . . .
H21 H -0.036836 -0.514271 0.960057 0.064 Uiso 1 1 calc R U . . .
C22 C -0.1499(5) -0.4649(10) 0.9804(3) 0.0500(17) Uani 1 1 d . U . . .
H22 H -0.129214 -0.391673 1.003408 0.060 Uiso 1 1 calc R U . . .
C23 C -0.2355(5) -0.4977(9) 0.9738(3) 0.0464(16) Uani 1 1 d . U . . .
C24 C -0.2650(6) -0.6122(11) 0.9399(3) 0.063(2) Uani 1 1 d . U . . .
H24 H -0.322261 -0.640497 0.935973 0.075 Uiso 1 1 calc R U . . .
C25 C -0.2087(6) -0.6831(11) 0.9123(4) 0.064(2) Uani 1 1 d . U . . .
H25 H -0.229349 -0.757839 0.889745 0.077 Uiso 1 1 calc R U . . .
C26 C -0.2960(5) -0.4022(9) 0.9991(3) 0.0398(15) Uani 1 1 d . U . . .
C27 C 0.2587(5) -0.6487(10) 0.6737(3) 0.0453(15) Uani 1 1 d . U . . .
C28 C 0.2404(5) -0.6798(9) 0.6251(3) 0.0445(16) Uani 1 1 d . U . . .
H28 H 0.190010 -0.731723 0.613937 0.053 Uiso 1 1 calc R U . . .
C29 C 0.2970(4) -0.6336(10) 0.5936(3) 0.0407(15) Uani 1 1 d . U . . .
H29 H 0.284077 -0.654999 0.561591 0.049 Uiso 1 1 calc R U . . .
C30 C 0.3727(5) -0.5557(10) 0.6094(3) 0.0435(15) Uani 1 1 d . U . . .
C31 C 0.3902(5) -0.5202(11) 0.6563(3) 0.0525(18) Uani 1 1 d . U . . .
H31 H 0.439601 -0.464277 0.666907 0.063 Uiso 1 1 calc R U . . .
C32 C 0.3343(5) -0.5675(11) 0.6886(3) 0.0527(18) Uani 1 1 d . U . . .
H32 H 0.347766 -0.544317 0.720434 0.063 Uiso 1 1 calc R U . . .
C33 C 0.4382(5) -0.5128(9) 0.5761(3) 0.0419(16) Uani 1 1 d . U . . .
C34 C 0.4090(14) 0.426(3) 0.8647(7) 0.070(4) Uani 0.5 1 d D U P A 1
C35 C 0.3722(16) 0.315(3) 0.8232(8) 0.071(5) Uani 0.5 1 d D U P A 1
H35A H 0.370405 0.371819 0.793944 0.107 Uiso 0.5 1 calc R U P A 1
H35B H 0.407953 0.222134 0.822156 0.107 Uiso 0.5 1 calc R U P A 1
H35C H 0.315639 0.281576 0.828102 0.107 Uiso 0.5 1 calc R U P A 1
C36 C 0.4694(17) 0.674(3) 0.8922(9) 0.079(5) Uani 0.5 1 d . U P A 1
H36A H 0.485481 0.776718 0.880721 0.119 Uiso 0.5 1 calc R U P A 1
H36B H 0.427319 0.688973 0.913614 0.119 Uiso 0.5 1 calc R U P A 1
H36C H 0.518678 0.622948 0.908398 0.119 Uiso 0.5 1 calc R U P A 1
C37 C 0.418(2) 0.660(4) 0.8088(8) 0.124(10) Uani 0.5 1 d D U P A 1
H37A H 0.445404 0.762072 0.812147 0.185 Uiso 0.5 1 calc R U P A 1
H37B H 0.440372 0.600586 0.784052 0.185 Uiso 0.5 1 calc R U P A 1
H37C H 0.357774 0.674093 0.801036 0.185 Uiso 0.5 1 calc R U P A 1
C34A C 0.4588(16) 0.451(3) 0.8741(7) 0.083(4) Uani 0.5 1 d D U P A 2
C35A C 0.5191(19) 0.589(3) 0.8875(10) 0.103(6) Uani 0.5 1 d . U P A 2
H35D H 0.544753 0.623191 0.860204 0.154 Uiso 0.5 1 calc R U P A 2
H35E H 0.487966 0.676344 0.899096 0.154 Uiso 0.5 1 calc R U P A 2
H35F H 0.562814 0.555047 0.911581 0.154 Uiso 0.5 1 calc R U P A 2
C36A C 0.4032(14) 0.259(3) 0.8148(9) 0.068(5) Uani 0.5 1 d D U P A 2
H36D H 0.410805 0.221931 0.783734 0.102 Uiso 0.5 1 calc R U P A 2
H36E H 0.412052 0.172457 0.836835 0.102 Uiso 0.5 1 calc R U P A 2
H36F H 0.346339 0.299942 0.814904 0.102 Uiso 0.5 1 calc R U P A 2
C37A C 0.545(3) 0.412(5) 0.7906(14) 0.174(16) Uani 0.5 1 d . U P A 2
H37D H 0.526590 0.353485 0.762284 0.261 Uiso 0.5 1 calc R U P A 2
H37E H 0.551964 0.522798 0.782898 0.261 Uiso 0.5 1 calc R U P A 2
H37F H 0.597938 0.369742 0.804955 0.261 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O4 2.332(5) 4_556 ?
Sm1 O7A 2.338(6) . ?
Sm1 O7 2.338(6) . ?
Sm1 O3 2.397(5) 2_656 ?
Sm1 O8 2.428(5) . ?
Sm1 O2 2.441(5) . ?
Sm1 O5 2.452(5) 3_557 ?
Sm1 O1 2.509(5) . ?
Sm1 O6 2.513(5) 3_557 ?
Sm1 C1 2.846(7) . ?
Sm1 C26 2.873(7) 3_557 ?
O1 C1 1.244(9) . ?
O2 C1 1.275(9) . ?
O3 C33 1.232(9) . ?
O4 C33 1.265(9) . ?
O5 C26 1.266(8) . ?
O6 C26 1.287(8) . ?
N1 C8 1.391(9) . ?
N1 C19 1.398(9) . ?
N1 C5 1.430(9) . ?
N2 C34 1.36(3) . ?
N2 C37 1.421(10) . ?
N2 C36 1.49(3) . ?
O7 C34 1.15(2) . ?
N2A C34A 1.383(10) . ?
N2A C36A 1.564(10) . ?
N2A C37A 1.73(4) . ?
O7A C34A 1.24(3) . ?
C1 C2 1.530(10) . ?
C2 C7 1.354(12) . ?
C2 C3 1.359(10) . ?
C3 C4 1.362(11) . ?
C4 C5 1.374(10) . ?
C5 C6 1.373(12) . ?
C6 C7 1.402(13) . ?
C8 C13 1.381(10) . ?
C8 C9 1.397(10) . ?
C9 C10 1.385(10) . ?
C10 C11 1.405(11) . ?
C10 C20 1.488(11) . ?
C11 C12 1.377(11) . ?
C12 C13 1.419(11) . ?
C13 C14 1.449(10) . ?
C14 C15 1.401(11) . ?
C14 C19 1.414(10) . ?
C15 C16 1.378(11) . ?
C16 C17 1.415(11) . ?
C17 C18 1.388(10) . ?
C17 C27 1.464(10) . ?
C18 C19 1.368(10) . ?
C20 C25 1.399(12) . ?
C20 C21 1.409(11) . ?
C21 C22 1.359(10) . ?
C22 C23 1.371(10) . ?
C23 C24 1.402(11) . ?
C23 C26 1.491(10) . ?
C24 C25 1.385(12) . ?
C27 C32 1.397(11) . ?
C27 C28 1.407(10) . ?
C28 C29 1.393(10) . ?
C29 C30 1.391(10) . ?
C30 C31 1.367(11) . ?
C30 C33 1.524(10) . ?
C31 C32 1.402(10) . ?
C34 C35 1.562(10) . ?
C34A C35A 1.52(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
O4 Sm1 O7A 156.8(2) 4_556 . ?
O4 Sm1 O7 156.8(2) 4_556 . ?
O4 Sm1 O3 111.27(19) 4_556 2_656 ?
O7 Sm1 O3 76.9(2) . 2_656 ?
O4 Sm1 O8 77.94(18) 4_556 . ?
O7A Sm1 O8 83.20(19) . . ?
O7 Sm1 O8 83.20(19) . . ?
O3 Sm1 O8 76.76(19) 2_656 . ?
O4 Sm1 O2 72.53(17) 4_556 . ?
O7A Sm1 O2 130.70(19) . . ?
O7 Sm1 O2 130.70(19) . . ?
O3 Sm1 O2 81.55(19) 2_656 . ?
O8 Sm1 O2 133.57(17) . . ?
O4 Sm1 O5 90.42(19) 4_556 3_557 ?
O7 Sm1 O5 90.7(2) . 3_557 ?
O3 Sm1 O5 151.06(18) 2_656 3_557 ?
O8 Sm1 O5 128.25(17) . 3_557 ?
O2 Sm1 O5 87.38(18) . 3_557 ?
O4 Sm1 O1 122.71(18) 4_556 . ?
O7A Sm1 O1 79.78(19) . . ?
O7 Sm1 O1 79.78(19) . . ?
O3 Sm1 O1 77.91(19) 2_656 . ?
O8 Sm1 O1 152.07(18) . . ?
O2 Sm1 O1 52.40(16) . . ?
O5 Sm1 O1 74.16(18) 3_557 . ?
O4 Sm1 O6 83.24(18) 4_556 3_557 ?
O7 Sm1 O6 79.1(2) . 3_557 ?
O3 Sm1 O6 145.34(18) 2_656 3_557 ?
O8 Sm1 O6 75.91(17) . 3_557 ?
O2 Sm1 O6 133.06(17) . 3_557 ?
O5 Sm1 O6 52.56(16) 3_557 3_557 ?
O1 Sm1 O6 121.69(17) . 3_557 ?
O4 Sm1 C1 98.2(2) 4_556 . ?
O7A Sm1 C1 104.9(2) . . ?
O7 Sm1 C1 104.9(2) . . ?
O3 Sm1 C1 77.8(2) 2_656 . ?
O8 Sm1 C1 150.7(2) . . ?
O2 Sm1 C1 26.51(19) . . ?
O5 Sm1 C1 80.4(2) 3_557 . ?
O1 Sm1 C1 25.91(19) . . ?
O6 Sm1 C1 132.93(19) 3_557 . ?
O4 Sm1 C26 85.5(2) 4_556 3_557 ?
O7A Sm1 C26 85.4(2) . 3_557 ?
O7 Sm1 C26 85.4(2) . 3_557 ?
O3 Sm1 C26 162.2(2) 2_656 3_557 ?
O8 Sm1 C26 102.3(2) . 3_557 ?
O2 Sm1 C26 110.08(19) . 3_557 ?
O5 Sm1 C26 26.00(18) 3_557 3_557 ?
O1 Sm1 C26 98.2(2) . 3_557 ?
O6 Sm1 C26 26.59(17) 3_557 3_557 ?
C1 Sm1 C26 106.3(2) . 3_557 ?
C1 O1 Sm1 92.3(4) . . ?
C1 O2 Sm1 94.7(4) . . ?
C33 O3 Sm1 120.6(5) . 2_646 ?
C33 O4 Sm1 175.5(5) . 4 ?
C26 O5 Sm1 95.9(4) . 3_557 ?
C26 O6 Sm1 92.5(4) . 3_557 ?
C8 N1 C19 108.4(6) . . ?
C8 N1 C5 124.0(6) . . ?
C19 N1 C5 126.2(6) . . ?
C34 N2 C37 132(2) . . ?
C34 N2 C36 113.9(17) . . ?
C37 N2 C36 113.3(19) . . ?
C34 O7 Sm1 149.2(11) . . ?
C34A N2A C36A 110(2) . . ?
C34A N2A C37A 136(2) . . ?
C36A N2A C37A 112(2) . . ?
C34A O7A Sm1 149.1(13) . . ?
O1 C1 O2 120.5(7) . . ?
O1 C1 C2 119.4(6) . . ?
O2 C1 C2 120.1(7) . . ?
O1 C1 Sm1 61.8(4) . . ?
O2 C1 Sm1 58.8(4) . . ?
C2 C1 Sm1 178.8(6) . . ?
C7 C2 C3 120.6(7) . . ?
C7 C2 C1 120.4(7) . . ?
C3 C2 C1 118.2(7) . . ?
C2 C3 C4 120.7(8) . . ?
C3 C4 C5 120.1(8) . . ?
C6 C5 C4 119.3(7) . . ?
C6 C5 N1 120.3(7) . . ?
C4 C5 N1 120.4(7) . . ?
C5 C6 C7 120.0(9) . . ?
C2 C7 C6 118.9(9) . . ?
C13 C8 N1 109.3(6) . . ?
C13 C8 C9 122.1(7) . . ?
N1 C8 C9 128.2(7) . . ?
C10 C9 C8 118.3(7) . . ?
C9 C10 C11 119.9(7) . . ?
C9 C10 C20 119.5(7) . . ?
C11 C10 C20 120.5(7) . . ?
C12 C11 C10 121.8(8) . . ?
C11 C12 C13 118.1(8) . . ?
C8 C13 C12 119.3(7) . . ?
C8 C13 C14 107.7(6) . . ?
C12 C13 C14 133.0(8) . . ?
C15 C14 C19 117.6(7) . . ?
C15 C14 C13 136.0(7) . . ?
C19 C14 C13 106.2(7) . . ?
C16 C15 C14 119.3(8) . . ?
C15 C16 C17 122.7(8) . . ?
C18 C17 C16 117.6(7) . . ?
C18 C17 C27 121.5(7) . . ?
C16 C17 C27 120.9(7) . . ?
C19 C18 C17 120.2(7) . . ?
C18 C19 N1 129.0(7) . . ?
C18 C19 C14 122.6(7) . . ?
N1 C19 C14 108.4(6) . . ?
C25 C20 C21 115.7(7) . . ?
C25 C20 C10 121.9(8) . . ?
C21 C20 C10 121.9(7) . . ?
C22 C21 C20 122.3(8) . . ?
C21 C22 C23 121.4(8) . . ?
C22 C23 C24 118.3(7) . . ?
C22 C23 C26 120.2(7) . . ?
C24 C23 C26 121.2(7) . . ?
C25 C24 C23 120.0(8) . . ?
C24 C25 C20 122.0(8) . . ?
O5 C26 O6 118.9(6) . . ?
O5 C26 C23 119.2(6) . . ?
O6 C26 C23 121.8(6) . . ?
O5 C26 Sm1 58.1(4) . 3_557 ?
O6 C26 Sm1 60.9(4) . 3_557 ?
C23 C26 Sm1 172.8(5) . 3_557 ?
C32 C27 C28 117.5(7) . . ?
C32 C27 C17 120.5(7) . . ?
C28 C27 C17 121.9(7) . . ?
C29 C28 C27 120.5(7) . . ?
C30 C29 C28 120.8(7) . . ?
C31 C30 C29 119.3(7) . . ?
C31 C30 C33 118.9(7) . . ?
C29 C30 C33 121.8(7) . . ?
C30 C31 C32 120.5(8) . . ?
C27 C32 C31 121.2(7) . . ?
O3 C33 O4 124.1(7) . . ?
O3 C33 C30 117.6(7) . . ?
O4 C33 C30 118.3(7) . . ?
O7 C34 N2 121.0(17) . . ?
O7 C34 C35 123(2) . . ?
N2 C34 C35 115.6(19) . . ?
O7A C34A N2A 127(2) . . ?
O7A C34A C35A 121.6(19) . . ?
N2A C34A C35A 111(2) . . ?

_refine_diff_density_max         2.309
_refine_diff_density_min         -1.938
_refine_diff_density_rms         0.148

####################################################################### 
# 
# 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_EU
_database_code_depnum_ccdc_archive 'CCDC 1553997'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H33 Eu N2 O10'
_chemical_formula_weight         817.60

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

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 222 56 ' '
2 0.738 0.124 0.267 43 5 ' '
3 0.262 -0.125 0.733 43 5 ' '
4 1.000 0.500 0.500 222 56 ' '
5 0.738 0.375 0.767 43 5 ' '
6 0.262 0.624 0.233 43 5 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_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                   15.776(3)
_cell_length_b                   8.3587(16)
_cell_length_c                   28.529(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.501(4)
_cell_angle_gamma                90
_cell_volume                     3737.9(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9716
_cell_measurement_theta_min      2.0435
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_F_000             1648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.727
_shelx_estimated_absorpt_T_min   0.724
_shelx_estimated_absorpt_T_max   0.919
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8668
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37589
_diffrn_reflns_av_unetI/netI     0.0531
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.540
_diffrn_reflns_theta_max         27.521
_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
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_reflns_number_total             8578
_reflns_number_gt                7402
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000       222        56 ' '
   2  0.738  0.124  0.267        43         5 ' '
   3  0.262 -0.125  0.733        43         5 ' '
   4  1.000  0.500  0.500       222        56 ' '
   5  0.738  0.375  0.767        43         5 ' '
   6  0.262  0.624  0.233        43         5 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_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)+(0.0564P)²+7.5532P] 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         8578
_refine_ls_number_parameters     479
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1325
_refine_ls_wR_factor_gt          0.1253
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.004
_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 0.40734(2) 0.18622(3) 0.95963(2) 0.02757(9) Uani 1 1 d . . . . .
O1 O 0.3038(2) 0.0838(5) 0.89367(13) 0.0402(9) Uani 1 1 d . . . . .
O2 O 0.3441(2) -0.0788(5) 0.95221(13) 0.0394(9) Uani 1 1 d . . . . .
O3 O 0.5001(2) -0.4338(5) 0.59087(13) 0.0431(9) Uani 1 1 d . . . . .
O4 O 0.4255(2) -0.5684(4) 0.53348(12) 0.0371(8) Uani 1 1 d . . . . .
O5 O -0.2680(2) -0.2863(5) 1.02526(13) 0.0382(9) Uani 1 1 d . . . . .
O6 O -0.3763(2) -0.4309(4) 0.99449(13) 0.0387(9) Uani 1 1 d . . . . .
O8 O 0.5465(2) 0.2829(4) 0.99153(13) 0.0375(8) Uani 1 1 d . . . . .
H8A H 0.589553 0.202502 0.988310 0.045 Uiso 1 1 d R U . . .
H8B H 0.561018 0.368144 0.976064 0.056 Uiso 1 1 d R U . . .
N1 N 0.1125(3) -0.5605(5) 0.81752(14) 0.0332(9) Uani 1 1 d . . . . .
N2A N 0.4335(9) 0.5737(16) 0.8526(5) 0.074(4) Uani 0.5 1 d . . P A 1
O7A O 0.4184(3) 0.3854(5) 0.90377(15) 0.0458(10) Uani 0.5 1 d . . P A 1
N2 N 0.4689(11) 0.394(2) 0.8308(5) 0.088(5) Uani 0.5 1 d . . P A 2
O7 O 0.4184(3) 0.3854(5) 0.90377(15) 0.0458(10) Uani 0.5 1 d . . P A 2
C1 C 0.3017(3) -0.0508(6) 0.91225(18) 0.0339(11) Uani 1 1 d . . . . .
C2 C 0.2477(3) -0.1830(6) 0.88740(18) 0.0318(10) Uani 1 1 d . . . . .
C3 C 0.1978(6) -0.1547(8) 0.8464(3) 0.079(3) Uani 1 1 d . . . . .
H3 H 0.193852 -0.051747 0.833972 0.094 Uiso 1 1 calc R U . . .
C4 C 0.1526(5) -0.2793(8) 0.8227(3) 0.077(3) Uani 1 1 d . . . . .
H4 H 0.118318 -0.259306 0.794633 0.092 Uiso 1 1 calc R U . . .
C5 C 0.1584(3) -0.4308(7) 0.84083(18) 0.0336(11) Uani 1 1 d . . . . .
C6 C 0.2088(4) -0.4597(7) 0.8820(2) 0.0509(16) Uani 1 1 d . . . . .
H6 H 0.212335 -0.562246 0.894758 0.061 Uiso 1 1 calc R U . . .
C7 C 0.2549(4) -0.3344(7) 0.9050(2) 0.0509(16) Uani 1 1 d . . . . .
H7 H 0.290869 -0.354485 0.932549 0.061 Uiso 1 1 calc R U . . .
C8 C 0.1344(3) -0.6431(6) 0.77791(18) 0.0329(11) Uani 1 1 d . . . . .
C9 C 0.1922(3) -0.5985(7) 0.74741(17) 0.0344(11) Uani 1 1 d . . . . .
H9 H 0.225964 -0.507764 0.752984 0.041 Uiso 1 1 calc R U . . .
C10 C 0.1981(3) -0.6951(7) 0.70773(19) 0.0400(13) Uani 1 1 d . . . . .
C11 C 0.1478(4) -0.8331(9) 0.7008(2) 0.0579(19) Uani 1 1 d . . . . .
H11 H 0.152679 -0.896401 0.674483 0.070 Uiso 1 1 calc R U . . .
C12 C 0.0916(4) -0.8776(8) 0.7319(2) 0.0557(18) Uani 1 1 d . . . . .
H12 H 0.059051 -0.969975 0.726623 0.067 Uiso 1 1 calc R U . . .
C13 C 0.0837(3) -0.7832(7) 0.77141(19) 0.0380(12) Uani 1 1 d . . . . .
C14 C 0.0299(4) -0.7858(7) 0.8095(2) 0.0400(13) Uani 1 1 d . . . . .
C15 C -0.0340(4) -0.8901(8) 0.8220(3) 0.0595(19) Uani 1 1 d . . . . .
H15 H -0.045188 -0.986148 0.806061 0.071 Uiso 1 1 calc R U . . .
C16 C -0.0797(4) -0.8458(8) 0.8586(3) 0.061(2) Uani 1 1 d . . . . .
H16 H -0.122548 -0.913256 0.866725 0.073 Uiso 1 1 calc R U . . .
C17 C -0.0637(4) -0.7027(7) 0.8838(2) 0.0425(13) Uani 1 1 d . . . . .
C18 C 0.0029(3) -0.6037(7) 0.87332(18) 0.0357(12) Uani 1 1 d . . . . .
H18 H 0.015998 -0.510362 0.890356 0.043 Uiso 1 1 calc R U . . .
C19 C 0.0492(3) -0.6486(6) 0.83662(18) 0.0314(11) Uani 1 1 d . . . . .
C20 C 0.2586(3) -0.6480(7) 0.67291(19) 0.0386(12) Uani 1 1 d . . . . .
C21 C 0.3340(4) -0.5680(9) 0.68773(19) 0.0518(17) Uani 1 1 d . . . . .
H21 H 0.347100 -0.543963 0.719555 0.062 Uiso 1 1 calc R U . . .
C22 C 0.3908(4) -0.5226(8) 0.6556(2) 0.0486(15) Uani 1 1 d . . . . .
H22 H 0.441097 -0.469412 0.666299 0.058 Uiso 1 1 calc R U . . .
C23 C 0.3720(3) -0.5568(7) 0.60846(18) 0.0348(11) Uani 1 1 d . . . . .
C24 C 0.2962(3) -0.6337(7) 0.59291(18) 0.0380(12) Uani 1 1 d . . . . .
H24 H 0.282640 -0.654741 0.560931 0.046 Uiso 1 1 calc R U . . .
C25 C 0.2401(4) -0.6799(7) 0.62485(19) 0.0410(13) Uani 1 1 d . . . . .
H25 H 0.189692 -0.732533 0.613989 0.049 Uiso 1 1 calc R U . . .
C26 C 0.4363(3) -0.5151(7) 0.57488(18) 0.0353(12) Uani 1 1 d . . . . .
C27 C -0.1213(4) -0.6470(7) 0.9186(2) 0.0422(13) Uani 1 1 d . . . . .
C28 C -0.2079(4) -0.6871(8) 0.9133(3) 0.061(2) Uani 1 1 d . . . . .
H28 H -0.227918 -0.764052 0.891214 0.073 Uiso 1 1 calc R U . . .
C29 C -0.2650(4) -0.6132(8) 0.9407(3) 0.059(2) Uani 1 1 d . . . . .
H29 H -0.322519 -0.640295 0.936311 0.071 Uiso 1 1 calc R U . . .
C30 C -0.2361(3) -0.4989(7) 0.97477(19) 0.0382(12) Uani 1 1 d . . . . .
C31 C -0.1491(3) -0.4658(8) 0.9813(2) 0.0446(14) Uani 1 1 d . . . . .
H31 H -0.128160 -0.393604 1.004614 0.053 Uiso 1 1 calc R U . . .
C32 C -0.0936(4) -0.5378(8) 0.9541(2) 0.0477(15) Uani 1 1 d . . . . .
H32 H -0.035821 -0.513098 0.959457 0.057 Uiso 1 1 calc R U . . .
C33 C -0.2961(3) -0.4027(6) 1.00009(18) 0.0341(11) Uani 1 1 d . . . . .
C34A C 0.4102(10) 0.422(2) 0.8646(6) 0.063(4) Uani 0.5 1 d . . P A 1
C35A C 0.4038(16) 0.708(4) 0.8053(7) 0.142(9) Uani 0.5 1 d . U P A 1
H35A H 0.435977 0.804845 0.810156 0.213 Uiso 0.5 1 calc R U P A 1
H35B H 0.415439 0.659218 0.776134 0.213 Uiso 0.5 1 calc R U P A 1
H35C H 0.344033 0.731058 0.803871 0.213 Uiso 0.5 1 calc R U P A 1
C36A C 0.4750(11) 0.6690(18) 0.8920(6) 0.064(4) Uani 0.5 1 d . U P A 1
H36B H 0.489176 0.772716 0.880670 0.077 Uiso 0.5 1 calc R U P A 1
H36C H 0.436894 0.680706 0.915706 0.077 Uiso 0.5 1 calc R U P A 1
H36A H 0.526132 0.615964 0.905299 0.077 Uiso 0.5 1 calc R U P A 1
C37A C 0.3725(12) 0.311(3) 0.8232(6) 0.069(6) Uani 0.5 1 d . . P A 1
H37A H 0.371954 0.367319 0.793841 0.103 Uiso 0.5 1 calc R U P A 1
H37B H 0.407138 0.216777 0.822508 0.103 Uiso 0.5 1 calc R U P A 1
H37C H 0.315351 0.280905 0.827864 0.103 Uiso 0.5 1 calc R U P A 1
C34 C 0.4620(12) 0.448(2) 0.8728(6) 0.076(5) Uani 0.5 1 d . . P A 2
C35 C 0.4094(12) 0.265(2) 0.8133(6) 0.061(4) Uani 0.5 1 d . U P A 2
H35D H 0.420196 0.234661 0.782085 0.091 Uiso 0.5 1 calc R U P A 2
H35E H 0.417696 0.174037 0.833910 0.091 Uiso 0.5 1 calc R U P A 2
H35F H 0.351754 0.302310 0.812622 0.091 Uiso 0.5 1 calc R U P A 2
C36 C 0.5381(19) 0.431(4) 0.7926(10) 0.179(12) Uani 0.5 1 d . U P A 2
H36D H 0.523489 0.369099 0.764558 0.269 Uiso 0.5 1 calc R U P A 2
H36E H 0.536344 0.542936 0.784741 0.269 Uiso 0.5 1 calc R U P A 2
H36F H 0.594473 0.403251 0.806396 0.269 Uiso 0.5 1 calc R U P A 2
C37 C 0.5299(17) 0.580(3) 0.8874(9) 0.133(9) Uani 0.5 1 d . U P A 2
H37D H 0.556269 0.612632 0.860240 0.199 Uiso 0.5 1 calc R U P A 2
H37E H 0.502644 0.670132 0.900099 0.199 Uiso 0.5 1 calc R U P A 2
H37F H 0.572625 0.537922 0.910858 0.199 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O4 2.314(4) 4_556 ?
Eu1 O7 2.325(4) . ?
Eu1 O7A 2.325(4) . ?
Eu1 O3 2.386(3) 2_656 ?
Eu1 O8 2.418(3) . ?
Eu1 O2 2.429(4) . ?
Eu1 O5 2.436(4) 3_557 ?
Eu1 O1 2.500(4) . ?
Eu1 O6 2.506(4) 3_557 ?
Eu1 C1 2.832(5) . ?
Eu1 C33 2.851(5) 3_557 ?
Eu1 C26 3.230(5) 2_656 ?
O1 C1 1.246(6) . ?
O2 C1 1.276(6) . ?
O3 C26 1.256(7) . ?
O4 C26 1.256(6) . ?
O5 C33 1.259(6) . ?
O6 C33 1.278(6) . ?
N1 C19 1.400(6) . ?
N1 C8 1.400(6) . ?
N1 C5 1.426(6) . ?
N2A C34A 1.37(2) . ?
N2A C36A 1.469(19) . ?
N2A C35A 1.78(3) . ?
O7A C34A 1.151(17) . ?
N2 C34 1.30(2) . ?
N2 C35 1.48(3) . ?
N2 C36 1.66(3) . ?
O7 C34 1.289(17) . ?
C1 C2 1.520(7) . ?
C2 C3 1.355(8) . ?
C2 C7 1.362(8) . ?
C3 C4 1.393(9) . ?
C4 C5 1.367(9) . ?
C5 C6 1.364(7) . ?
C6 C7 1.396(8) . ?
C8 C9 1.381(7) . ?
C8 C13 1.418(7) . ?
C9 C10 1.402(7) . ?
C10 C11 1.400(8) . ?
C10 C20 1.507(7) . ?
C11 C12 1.375(8) . ?
C12 C13 1.392(8) . ?
C13 C14 1.454(7) . ?
C14 C19 1.397(7) . ?
C14 C15 1.408(8) . ?
C15 C16 1.384(8) . ?
C16 C17 1.403(8) . ?
C17 C18 1.396(7) . ?
C17 C27 1.495(7) . ?
C18 C19 1.395(7) . ?
C20 C21 1.387(8) . ?
C20 C25 1.395(7) . ?
C21 C22 1.404(7) . ?
C22 C23 1.375(7) . ?
C23 C24 1.386(7) . ?
C23 C26 1.513(7) . ?
C24 C25 1.395(7) . ?
C27 C32 1.396(8) . ?
C27 C28 1.398(8) . ?
C28 C29 1.402(8) . ?
C29 C30 1.401(8) . ?
C30 C31 1.392(7) . ?
C30 C33 1.490(7) . ?
C31 C32 1.374(7) . ?
C34A C37A 1.57(2) . ?
C34 C37 1.56(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
O4 Eu1 O7 156.60(14) 4_556 . ?
O4 Eu1 O7A 156.60(14) 4_556 . ?
O4 Eu1 O3 110.45(14) 4_556 2_656 ?
O7A Eu1 O3 77.79(15) . 2_656 ?
O4 Eu1 O8 77.63(13) 4_556 . ?
O7 Eu1 O8 83.30(14) . . ?
O7A Eu1 O8 83.30(14) . . ?
O3 Eu1 O8 77.05(14) 2_656 . ?
O4 Eu1 O2 72.45(12) 4_556 . ?
O7 Eu1 O2 130.95(14) . . ?
O7A Eu1 O2 130.95(14) . . ?
O3 Eu1 O2 80.64(14) 2_656 . ?
O8 Eu1 O2 133.15(13) . . ?
O4 Eu1 O5 90.38(13) 4_556 3_557 ?
O7A Eu1 O5 90.85(14) . 3_557 ?
O3 Eu1 O5 151.38(13) 2_656 3_557 ?
O8 Eu1 O5 128.15(13) . 3_557 ?
O2 Eu1 O5 87.63(13) . 3_557 ?
O4 Eu1 O1 122.86(13) 4_556 . ?
O7 Eu1 O1 79.79(14) . . ?
O7A Eu1 O1 79.79(14) . . ?
O3 Eu1 O1 78.13(13) 2_656 . ?
O8 Eu1 O1 152.38(13) . . ?
O2 Eu1 O1 52.76(12) . . ?
O5 Eu1 O1 74.02(13) 3_557 . ?
O4 Eu1 O6 83.31(13) 4_556 3_557 ?
O7A Eu1 O6 78.93(14) . 3_557 ?
O3 Eu1 O6 145.87(13) 2_656 3_557 ?
O8 Eu1 O6 75.74(12) . 3_557 ?
O2 Eu1 O6 133.40(12) . 3_557 ?
O5 Eu1 O6 52.66(12) 3_557 3_557 ?
O1 Eu1 O6 121.52(13) . 3_557 ?
O4 Eu1 C1 98.18(14) 4_556 . ?
O7 Eu1 C1 105.05(16) . . ?
O7A Eu1 C1 105.05(16) . . ?
O3 Eu1 C1 77.59(14) 2_656 . ?
O8 Eu1 C1 150.87(14) . . ?
O2 Eu1 C1 26.70(14) . . ?
O5 Eu1 C1 80.25(13) 3_557 . ?
O1 Eu1 C1 26.08(14) . . ?
O6 Eu1 C1 132.91(13) 3_557 . ?
O4 Eu1 C33 85.51(14) 4_556 3_557 ?
O7 Eu1 C33 85.38(15) . 3_557 ?
O7A Eu1 C33 85.38(15) . 3_557 ?
O3 Eu1 C33 163.14(15) 2_656 3_557 ?
O8 Eu1 C33 102.13(14) . 3_557 ?
O2 Eu1 C33 110.39(14) . 3_557 ?
O5 Eu1 C33 26.08(13) 3_557 3_557 ?
O1 Eu1 C33 98.11(14) . 3_557 ?
O6 Eu1 C33 26.62(13) 3_557 3_557 ?
C1 Eu1 C33 106.29(15) . 3_557 ?
O4 Eu1 C26 92.03(14) 4_556 2_656 ?
O7A Eu1 C26 92.56(14) . 2_656 ?
O3 Eu1 C26 19.27(13) 2_656 2_656 ?
O8 Eu1 C26 66.22(13) . 2_656 ?
O2 Eu1 C26 79.55(13) . 2_656 ?
O5 Eu1 C26 165.57(13) 3_557 2_656 ?
O1 Eu1 C26 92.80(13) . 2_656 ?
O6 Eu1 C26 141.77(12) 3_557 2_656 ?
C1 Eu1 C26 85.33(14) . 2_656 ?
C33 Eu1 C26 168.35(14) 3_557 2_656 ?
C1 O1 Eu1 92.0(3) . . ?
C1 O2 Eu1 94.6(3) . . ?
C26 O3 Eu1 121.9(3) . 2_646 ?
C26 O4 Eu1 175.5(4) . 4 ?
C33 O5 Eu1 95.7(3) . 3_557 ?
C33 O6 Eu1 91.9(3) . 3_557 ?
C19 N1 C8 107.9(4) . . ?
C19 N1 C5 124.4(4) . . ?
C8 N1 C5 126.4(4) . . ?
C34A N2A C36A 114.8(13) . . ?
C34A N2A C35A 135.7(14) . . ?
C36A N2A C35A 107.2(13) . . ?
C34A O7A Eu1 147.8(9) . . ?
C34 N2 C35 116.6(15) . . ?
C34 N2 C36 132(2) . . ?
C35 N2 C36 110.8(17) . . ?
C34 O7 Eu1 147.8(10) . . ?
O1 C1 O2 120.6(5) . . ?
O1 C1 C2 119.9(5) . . ?
O2 C1 C2 119.5(5) . . ?
O1 C1 Eu1 61.9(3) . . ?
O2 C1 Eu1 58.7(3) . . ?
C2 C1 Eu1 177.7(4) . . ?
C3 C2 C7 119.8(5) . . ?
C3 C2 C1 121.0(5) . . ?
C7 C2 C1 118.9(5) . . ?
C2 C3 C4 120.2(6) . . ?
C5 C4 C3 120.1(6) . . ?
C6 C5 C4 119.8(5) . . ?
C6 C5 N1 118.9(5) . . ?
C4 C5 N1 121.3(5) . . ?
C5 C6 C7 119.6(6) . . ?
C2 C7 C6 120.4(5) . . ?
C9 C8 N1 128.0(5) . . ?
C9 C8 C13 122.9(5) . . ?
N1 C8 C13 109.0(4) . . ?
C8 C9 C10 117.5(5) . . ?
C11 C10 C9 120.0(5) . . ?
C11 C10 C20 120.9(5) . . ?
C9 C10 C20 119.1(5) . . ?
C12 C11 C10 121.9(5) . . ?
C11 C12 C13 119.4(6) . . ?
C12 C13 C8 118.3(5) . . ?
C12 C13 C14 135.2(5) . . ?
C8 C13 C14 106.4(4) . . ?
C19 C14 C15 119.1(5) . . ?
C19 C14 C13 107.0(4) . . ?
C15 C14 C13 133.9(5) . . ?
C16 C15 C14 118.3(6) . . ?
C15 C16 C17 122.4(6) . . ?
C18 C17 C16 119.4(5) . . ?
C18 C17 C27 119.1(5) . . ?
C16 C17 C27 121.2(5) . . ?
C19 C18 C17 118.2(5) . . ?
C18 C19 C14 122.4(5) . . ?
C18 C19 N1 127.5(5) . . ?
C14 C19 N1 109.7(4) . . ?
C21 C20 C25 118.0(5) . . ?
C21 C20 C10 120.7(5) . . ?
C25 C20 C10 121.3(5) . . ?
C20 C21 C22 121.3(5) . . ?
C23 C22 C21 120.0(5) . . ?
C22 C23 C24 119.5(5) . . ?
C22 C23 C26 119.1(5) . . ?
C24 C23 C26 121.4(5) . . ?
C23 C24 C25 120.5(5) . . ?
C20 C25 C24 120.7(5) . . ?
O3 C26 O4 123.4(5) . . ?
O3 C26 C23 117.5(5) . . ?
O4 C26 C23 119.0(5) . . ?
O3 C26 Eu1 38.8(2) . 2_646 ?
O4 C26 Eu1 85.7(3) . 2_646 ?
C23 C26 Eu1 154.6(4) . 2_646 ?
C32 C27 C28 117.2(5) . . ?
C32 C27 C17 121.4(5) . . ?
C28 C27 C17 120.9(6) . . ?
C27 C28 C29 121.0(6) . . ?
C30 C29 C28 120.6(6) . . ?
C31 C30 C29 117.9(5) . . ?
C31 C30 C33 119.9(5) . . ?
C29 C30 C33 122.0(5) . . ?
C32 C31 C30 121.3(5) . . ?
C31 C32 C27 121.9(5) . . ?
O5 C33 O6 119.6(5) . . ?
O5 C33 C30 119.4(5) . . ?
O6 C33 C30 120.9(5) . . ?
O5 C33 Eu1 58.2(3) . 3_557 ?
O6 C33 Eu1 61.5(3) . 3_557 ?
C30 C33 Eu1 172.6(4) . 3_557 ?
O7A C34A N2A 118.9(14) . . ?
O7A C34A C37A 124.5(15) . . ?
N2A C34A C37A 116.6(15) . . ?
O7 C34 N2 126.9(18) . . ?
O7 C34 C37 120.4(17) . . ?
N2 C34 C37 111.4(18) . . ?

_refine_diff_density_max         1.404
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.119

####################################################################### 
# 
# 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_DY
_database_code_depnum_ccdc_archive 'CCDC 1554000'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H33 Dy N2 O10'
_chemical_formula_weight         828.15

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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 220 58 ' '
2 0.740 0.134 0.267 39 5 ' '
3 0.260 -0.135 0.733 40 5 ' '
4 1.000 0.500 0.500 219 58 ' '
5 0.740 0.365 0.767 39 5 ' '
6 0.260 0.634 0.233 39 5 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_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                   15.735(7)
_cell_length_b                   8.290(3)
_cell_length_c                   28.436(12)
_cell_angle_alpha                90
_cell_angle_beta                 96.414(8)
_cell_angle_gamma                90
_cell_volume                     3686(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    11228
_cell_measurement_theta_min      2.0478
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_F_000             1660
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.038
_exptl_absorpt_coefficient_mu    2.077
_shelx_estimated_absorpt_T_min   0.724
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8936
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36766
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.560
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_reflns_number_total             8414
_reflns_number_gt                7359
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000       220        58 ' '
   2  0.740  0.134  0.267        39         5 ' '
   3  0.260 -0.135  0.733        40         5 ' '
   4  1.000  0.500  0.500       219        58 ' '
   5  0.740  0.365  0.767        39         5 ' '
   6  0.260  0.634  0.233        39         5 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_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)+(0.0594P)²+10.3643P] 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         8414
_refine_ls_number_parameters     479
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.1319
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.40756(2) 0.18728(3) 0.95925(2) 0.02887(9) Uani 1 1 d . . . . .
O1 O 0.3060(3) 0.0871(5) 0.89302(14) 0.0429(9) Uani 1 1 d . . . . .
O2 O 0.3446(3) -0.0766(5) 0.95185(13) 0.0394(9) Uani 1 1 d . . . . .
O3 O 0.5001(3) -0.4358(6) 0.58869(13) 0.0470(10) Uani 1 1 d . . . . .
O4 O 0.4230(3) -0.5728(5) 0.53206(12) 0.0386(9) Uani 1 1 d . . . . .
O5 O -0.3779(2) -0.4318(5) 0.99529(14) 0.0405(9) Uani 1 1 d . . . . .
O6 O -0.2699(2) -0.2852(5) 1.02599(13) 0.0379(9) Uani 1 1 d . . . . .
O8 O 0.5447(2) 0.2810(5) 0.99146(15) 0.0412(9) Uani 1 1 d . . . . .
H8A H 0.587811 0.202339 0.986802 0.049 Uiso 1 1 d R U . . .
H8B H 0.556411 0.371575 0.978290 0.062 Uiso 1 1 d R U . . .
N1 N 0.1130(3) -0.5612(6) 0.81792(14) 0.0363(10) Uani 1 1 d . . . . .
N2 N 0.4348(11) 0.5698(14) 0.8533(4) 0.093(5) Uani 0.5 1 d D U P A 1
O7 O 0.4195(3) 0.3841(5) 0.90342(15) 0.0508(11) Uani 0.5 1 d D . P A 1
N2A N 0.4704(11) 0.389(2) 0.8302(5) 0.095(5) Uani 0.5 1 d D U P A 2
O7A O 0.4195(3) 0.3841(5) 0.90342(15) 0.0508(11) Uani 0.5 1 d . . P A 2
C1 C 0.3035(3) -0.0469(7) 0.91174(19) 0.0357(11) Uani 1 1 d . . . . .
C2 C 0.2488(4) -0.1811(6) 0.88692(17) 0.0323(11) Uani 1 1 d . . . . .
C3 C 0.1992(6) -0.1530(9) 0.8463(3) 0.074(3) Uani 1 1 d . . . . .
H3 H 0.195804 -0.049384 0.833624 0.089 Uiso 1 1 calc R U . . .
C4 C 0.1525(6) -0.2787(9) 0.8227(3) 0.071(3) Uani 1 1 d . . . . .
H4 H 0.117641 -0.258828 0.794660 0.085 Uiso 1 1 calc R U . . .
C5 C 0.1587(3) -0.4302(7) 0.84125(17) 0.0336(11) Uani 1 1 d . . . . .
C6 C 0.2102(5) -0.4577(8) 0.8821(2) 0.0559(18) Uani 1 1 d . . . . .
H6 H 0.214667 -0.561332 0.894636 0.067 Uiso 1 1 calc R U . . .
C7 C 0.2556(5) -0.3341(7) 0.9048(2) 0.0501(16) Uani 1 1 d . . . . .
H7 H 0.291168 -0.354327 0.932564 0.060 Uiso 1 1 calc R U . . .
C8 C 0.1350(3) -0.6428(7) 0.77811(17) 0.0330(11) Uani 1 1 d . . . . .
C9 C 0.1939(4) -0.6002(7) 0.74749(18) 0.0393(13) Uani 1 1 d . . . . .
H9 H 0.228647 -0.510006 0.753395 0.047 Uiso 1 1 calc R U . . .
C10 C 0.1998(4) -0.6949(8) 0.7080(2) 0.0440(14) Uani 1 1 d . . . . .
C11 C 0.1489(5) -0.8360(9) 0.7010(2) 0.0572(19) Uani 1 1 d . . . . .
H11 H 0.153778 -0.900544 0.674640 0.069 Uiso 1 1 calc R U . . .
C12 C 0.0926(5) -0.8789(9) 0.7323(2) 0.0557(18) Uani 1 1 d . . . . .
H12 H 0.059898 -0.971984 0.727303 0.067 Uiso 1 1 calc R U . . .
C13 C 0.0846(4) -0.7830(7) 0.7716(2) 0.0390(13) Uani 1 1 d . . . . .
C14 C 0.0302(4) -0.7870(7) 0.8097(2) 0.0410(13) Uani 1 1 d . . . . .
C15 C -0.0345(5) -0.8904(8) 0.8221(3) 0.0581(19) Uani 1 1 d . . . . .
H15 H -0.046389 -0.986463 0.805822 0.070 Uiso 1 1 calc R U . . .
C16 C -0.0802(5) -0.8473(8) 0.8590(3) 0.0566(18) Uani 1 1 d . . . . .
H16 H -0.122615 -0.916003 0.867474 0.068 Uiso 1 1 calc R U . . .
C17 C -0.0641(4) -0.7017(7) 0.8839(2) 0.0415(13) Uani 1 1 d . . . . .
C18 C 0.0027(3) -0.6043(7) 0.87352(18) 0.0366(12) Uani 1 1 d . . . . .
H18 H 0.016119 -0.510694 0.890781 0.044 Uiso 1 1 calc R U . . .
C19 C 0.0495(3) -0.6487(7) 0.83675(18) 0.0337(11) Uani 1 1 d . . . . .
C20 C 0.2589(4) -0.6496(7) 0.6728(2) 0.0402(13) Uani 1 1 d . . . . .
C21 C 0.3354(4) -0.5714(9) 0.6869(2) 0.0525(17) Uani 1 1 d . . . . .
H21 H 0.349700 -0.549500 0.718917 0.063 Uiso 1 1 calc R U . . .
C22 C 0.3913(4) -0.5245(9) 0.6550(2) 0.0516(17) Uani 1 1 d . . . . .
H22 H 0.441628 -0.470432 0.665562 0.062 Uiso 1 1 calc R U . . .
C23 C 0.3717(3) -0.5586(7) 0.60723(18) 0.0366(11) Uani 1 1 d . . . . .
C24 C 0.2957(4) -0.6354(8) 0.59228(19) 0.0394(13) Uani 1 1 d . . . . .
H24 H 0.281807 -0.657479 0.560282 0.047 Uiso 1 1 calc R U . . .
C25 C 0.2396(4) -0.6802(7) 0.6245(2) 0.0408(13) Uani 1 1 d . . . . .
H25 H 0.188504 -0.731175 0.613669 0.049 Uiso 1 1 calc R U . . .
C26 C 0.4355(3) -0.5186(6) 0.57318(18) 0.0337(11) Uani 1 1 d . . . . .
C27 C -0.1224(4) -0.6463(7) 0.9187(2) 0.0419(13) Uani 1 1 d . . . . .
C28 C -0.2094(5) -0.6862(8) 0.9132(3) 0.0575(19) Uani 1 1 d . . . . .
H28 H -0.229438 -0.763561 0.891036 0.069 Uiso 1 1 calc R U . . .
C29 C -0.2664(4) -0.6117(8) 0.9405(2) 0.0515(17) Uani 1 1 d . . . . .
H29 H -0.324236 -0.637415 0.935784 0.062 Uiso 1 1 calc R U . . .
C30 C -0.2370(4) -0.4983(7) 0.97508(19) 0.0367(12) Uani 1 1 d . . . . .
C31 C -0.1507(4) -0.4669(8) 0.9821(2) 0.0446(14) Uani 1 1 d . . . . .
H31 H -0.129747 -0.396485 1.006042 0.053 Uiso 1 1 calc R U . . .
C32 C -0.0944(4) -0.5377(9) 0.9543(2) 0.0467(15) Uani 1 1 d . . . . .
H32 H -0.036627 -0.511992 0.959497 0.056 Uiso 1 1 calc R U . . .
C33 C -0.2973(3) -0.4014(6) 1.00068(19) 0.0345(11) Uani 1 1 d . . . . .
C34 C 0.4136(13) 0.4264(16) 0.8633(4) 0.079(5) Uani 0.5 1 d D U P A 1
C35 C 0.3699(12) 0.316(2) 0.8210(7) 0.077(7) Uani 0.5 1 d D . P A 1
H35A H 0.371343 0.371036 0.791408 0.115 Uiso 0.5 1 calc R U P A 1
H35B H 0.400647 0.215835 0.820281 0.115 Uiso 0.5 1 calc R U P A 1
H35C H 0.311621 0.294020 0.825883 0.115 Uiso 0.5 1 calc R U P A 1
C36 C 0.4758(13) 0.6645(14) 0.8945(6) 0.078(5) Uani 0.5 1 d D U P A 1
H36A H 0.489757 0.770485 0.884133 0.117 Uiso 0.5 1 calc R U P A 1
H36B H 0.436861 0.673067 0.918101 0.117 Uiso 0.5 1 calc R U P A 1
H36C H 0.527001 0.610861 0.907748 0.117 Uiso 0.5 1 calc R U P A 1
C37 C 0.4139(16) 0.669(2) 0.8074(5) 0.125(8) Uani 0.5 1 d D U P A 1
H37A H 0.439780 0.774132 0.811451 0.187 Uiso 0.5 1 calc R U P A 1
H37B H 0.435939 0.614930 0.781539 0.187 Uiso 0.5 1 calc R U P A 1
H37C H 0.353051 0.681084 0.800703 0.187 Uiso 0.5 1 calc R U P A 1
C34A C 0.4693(15) 0.448(3) 0.8762(6) 0.107(7) Uani 0.5 1 d D U P A 2
C35A C 0.5274(18) 0.579(3) 0.8900(10) 0.140(10) Uani 0.5 1 d D U P A 2
H35D H 0.558213 0.607505 0.863975 0.210 Uiso 0.5 1 calc R U P A 2
H35E H 0.495557 0.670554 0.899017 0.210 Uiso 0.5 1 calc R U P A 2
H35F H 0.567003 0.545545 0.916380 0.210 Uiso 0.5 1 calc R U P A 2
C36A C 0.4060(13) 0.263(2) 0.8161(7) 0.074(6) Uani 0.5 1 d D . P A 2
H36D H 0.411121 0.229071 0.784245 0.111 Uiso 0.5 1 calc R U P A 2
H36E H 0.415473 0.171939 0.837013 0.111 Uiso 0.5 1 calc R U P A 2
H36F H 0.349693 0.305071 0.817964 0.111 Uiso 0.5 1 calc R U P A 2
C37A C 0.549(2) 0.409(4) 0.7930(12) 0.194(14) Uani 0.5 1 d . U P A 2
H37D H 0.531698 0.355100 0.763597 0.290 Uiso 0.5 1 calc R U P A 2
H37E H 0.558933 0.520858 0.787183 0.290 Uiso 0.5 1 calc R U P A 2
H37F H 0.601265 0.360634 0.807563 0.290 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O4 2.266(4) 4_556 ?
Dy1 O7A 2.299(4) . ?
Dy1 O7 2.299(4) . ?
Dy1 O3 2.335(4) 2_656 ?
Dy1 O8 2.378(4) . ?
Dy1 O6 2.393(4) 3_557 ?
Dy1 O2 2.401(4) . ?
Dy1 O1 2.474(4) . ?
Dy1 O5 2.476(4) 3_557 ?
Dy1 C1 2.789(5) . ?
Dy1 C33 2.811(5) 3_557 ?
O1 C1 1.234(7) . ?
O2 C1 1.270(6) . ?
O3 C26 1.264(7) . ?
O4 C26 1.248(6) . ?
O5 C33 1.285(6) . ?
O6 C33 1.250(6) . ?
N1 C19 1.389(7) . ?
N1 C8 1.395(6) . ?
N1 C5 1.425(7) . ?
N2 C34 1.275(9) . ?
N2 C36 1.496(9) . ?
N2 C37 1.549(8) . ?
O7 C34 1.187(9) . ?
N2A C34A 1.398(10) . ?
N2A C36A 1.483(10) . ?
N2A C37A 1.73(3) . ?
O7A C34A 1.28(2) . ?
C1 C2 1.530(7) . ?
C2 C3 1.341(9) . ?
C2 C7 1.366(8) . ?
C3 C4 1.402(9) . ?
C4 C5 1.362(9) . ?
C5 C6 1.358(8) . ?
C6 C7 1.370(8) . ?
C8 C9 1.387(7) . ?
C8 C13 1.408(8) . ?
C9 C10 1.382(8) . ?
C10 C11 1.419(9) . ?
C10 C20 1.488(8) . ?
C11 C12 1.373(8) . ?
C12 C13 1.389(8) . ?
C13 C14 1.454(7) . ?
C14 C19 1.395(8) . ?
C14 C15 1.406(8) . ?
C15 C16 1.382(8) . ?
C16 C17 1.408(9) . ?
C17 C18 1.383(8) . ?
C17 C27 1.495(7) . ?
C18 C19 1.394(7) . ?
C20 C21 1.386(8) . ?
C20 C25 1.397(8) . ?
C21 C22 1.389(8) . ?
C22 C23 1.388(8) . ?
C23 C24 1.379(8) . ?
C23 C26 1.508(7) . ?
C24 C25 1.392(7) . ?
C27 C32 1.388(8) . ?
C27 C28 1.399(9) . ?
C28 C29 1.395(8) . ?
C29 C30 1.400(8) . ?
C30 C31 1.374(8) . ?
C30 C33 1.494(7) . ?
C31 C32 1.381(8) . ?
C34 C35 1.606(10) . ?
C34A C35A 1.442(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Dy1 O7A 156.89(16) 4_556 . ?
O4 Dy1 O7 156.89(16) 4_556 . ?
O4 Dy1 O3 109.89(15) 4_556 2_656 ?
O7 Dy1 O3 78.62(16) . 2_656 ?
O4 Dy1 O8 77.60(14) 4_556 . ?
O7A Dy1 O8 83.87(16) . . ?
O7 Dy1 O8 83.87(16) . . ?
O3 Dy1 O8 76.75(16) 2_656 . ?
O4 Dy1 O6 89.33(14) 4_556 3_557 ?
O7 Dy1 O6 91.49(15) . 3_557 ?
O3 Dy1 O6 152.22(14) 2_656 3_557 ?
O8 Dy1 O6 128.42(14) . 3_557 ?
O4 Dy1 O2 72.51(13) 4_556 . ?
O7A Dy1 O2 130.60(15) . . ?
O7 Dy1 O2 130.60(15) . . ?
O3 Dy1 O2 80.11(16) 2_656 . ?
O8 Dy1 O2 132.79(13) . . ?
O6 Dy1 O2 87.23(14) 3_557 . ?
O4 Dy1 O1 123.30(14) 4_556 . ?
O7A Dy1 O1 78.95(15) . . ?
O7 Dy1 O1 78.95(15) . . ?
O3 Dy1 O1 78.46(15) 2_656 . ?
O8 Dy1 O1 152.14(15) . . ?
O6 Dy1 O1 74.16(14) 3_557 . ?
O2 Dy1 O1 53.27(13) . . ?
O4 Dy1 O5 82.71(14) 4_556 3_557 ?
O7 Dy1 O5 79.31(16) . 3_557 ?
O3 Dy1 O5 145.93(15) 2_656 3_557 ?
O8 Dy1 O5 75.36(14) . 3_557 ?
O6 Dy1 O5 53.41(12) 3_557 3_557 ?
O2 Dy1 O5 133.75(13) . 3_557 ?
O1 Dy1 O5 121.93(14) . 3_557 ?
O4 Dy1 C1 98.52(15) 4_556 . ?
O7A Dy1 C1 104.38(17) . . ?
O7 Dy1 C1 104.38(17) . . ?
O3 Dy1 C1 77.45(16) 2_656 . ?
O8 Dy1 C1 150.70(15) . . ?
O6 Dy1 C1 80.06(14) 3_557 . ?
O2 Dy1 C1 27.03(15) . . ?
O1 Dy1 C1 26.25(15) . . ?
O5 Dy1 C1 133.47(14) 3_557 . ?
O4 Dy1 C33 84.38(15) 4_556 3_557 ?
O7A Dy1 C33 86.20(16) . 3_557 ?
O7 Dy1 C33 86.20(16) . 3_557 ?
O3 Dy1 C33 164.82(15) 2_656 3_557 ?
O8 Dy1 C33 102.24(16) . 3_557 ?
O6 Dy1 C33 26.26(14) 3_557 3_557 ?
O2 Dy1 C33 110.09(15) . 3_557 ?
O1 Dy1 C33 98.34(16) . 3_557 ?
O5 Dy1 C33 27.20(14) 3_557 3_557 ?
C1 Dy1 C33 106.29(16) . 3_557 ?
C1 O1 Dy1 91.3(3) . . ?
C1 O2 Dy1 93.8(3) . . ?
C26 O3 Dy1 124.2(3) . 2_646 ?
C26 O4 Dy1 175.4(4) . 4 ?
C33 O5 Dy1 91.0(3) . 3_557 ?
C33 O6 Dy1 95.9(3) . 3_557 ?
C19 N1 C8 108.3(4) . . ?
C19 N1 C5 124.5(4) . . ?
C8 N1 C5 126.1(4) . . ?
C34 N2 C36 114.6(8) . . ?
C34 N2 C37 130.5(13) . . ?
C36 N2 C37 114.4(13) . . ?
C34 O7 Dy1 150.4(7) . . ?
C34A N2A C36A 114.9(16) . . ?
C34A N2A C37A 129(2) . . ?
C36A N2A C37A 114.6(19) . . ?
C34A O7A Dy1 144.8(12) . . ?
O1 C1 O2 121.6(5) . . ?
O1 C1 C2 119.9(5) . . ?
O2 C1 C2 118.5(5) . . ?
O1 C1 Dy1 62.5(3) . . ?
O2 C1 Dy1 59.2(3) . . ?
C2 C1 Dy1 177.5(4) . . ?
C3 C2 C7 119.8(5) . . ?
C3 C2 C1 120.9(5) . . ?
C7 C2 C1 119.1(5) . . ?
C2 C3 C4 120.4(7) . . ?
C5 C4 C3 119.3(6) . . ?
C6 C5 C4 119.8(5) . . ?
C6 C5 N1 119.5(5) . . ?
C4 C5 N1 120.8(5) . . ?
C5 C6 C7 120.5(6) . . ?
C2 C7 C6 120.2(6) . . ?
C9 C8 N1 129.0(5) . . ?
C9 C8 C13 122.3(5) . . ?
N1 C8 C13 108.6(4) . . ?
C10 C9 C8 118.4(5) . . ?
C9 C10 C11 119.6(5) . . ?
C9 C10 C20 120.4(5) . . ?
C11 C10 C20 119.9(5) . . ?
C12 C11 C10 121.1(6) . . ?
C11 C12 C13 119.9(6) . . ?
C12 C13 C8 118.5(5) . . ?
C12 C13 C14 134.5(6) . . ?
C8 C13 C14 107.0(5) . . ?
C19 C14 C15 118.8(5) . . ?
C19 C14 C13 106.3(5) . . ?
C15 C14 C13 134.8(6) . . ?
C16 C15 C14 119.0(6) . . ?
C15 C16 C17 121.6(6) . . ?
C18 C17 C16 119.4(5) . . ?
C18 C17 C27 119.9(5) . . ?
C16 C17 C27 120.5(5) . . ?
C17 C18 C19 119.0(5) . . ?
N1 C19 C14 109.8(4) . . ?
N1 C19 C18 127.9(5) . . ?
C14 C19 C18 122.0(5) . . ?
C21 C20 C25 117.1(5) . . ?
C21 C20 C10 120.7(5) . . ?
C25 C20 C10 122.1(5) . . ?
C20 C21 C22 122.3(5) . . ?
C23 C22 C21 119.7(6) . . ?
C24 C23 C22 119.1(5) . . ?
C24 C23 C26 121.4(5) . . ?
C22 C23 C26 119.5(5) . . ?
C23 C24 C25 120.8(5) . . ?
C24 C25 C20 121.0(5) . . ?
O4 C26 O3 124.0(5) . . ?
O4 C26 C23 118.4(5) . . ?
O3 C26 C23 117.6(5) . . ?
C32 C27 C28 117.5(5) . . ?
C32 C27 C17 120.9(5) . . ?
C28 C27 C17 121.2(5) . . ?
C29 C28 C27 121.0(6) . . ?
C28 C29 C30 120.3(6) . . ?
C31 C30 C29 118.2(5) . . ?
C31 C30 C33 119.9(5) . . ?
C29 C30 C33 121.6(5) . . ?
C30 C31 C32 121.5(6) . . ?
C31 C32 C27 121.4(6) . . ?
O6 C33 O5 119.4(5) . . ?
O6 C33 C30 119.9(5) . . ?
O5 C33 C30 120.6(5) . . ?
O6 C33 Dy1 57.9(3) . 3_557 ?
O5 C33 Dy1 61.7(3) . 3_557 ?
C30 C33 Dy1 172.7(4) . 3_557 ?
O7 C34 N2 119.7(11) . . ?
O7 C34 C35 122.2(12) . . ?
N2 C34 C35 117.8(11) . . ?
O7A C34A N2A 119.6(16) . . ?
O7A C34A C35A 124.0(19) . . ?
N2A C34A C35A 116(2) . . ?

_refine_diff_density_max         1.715
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.126

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1553998'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H33 Gd N2 O10'
_chemical_formula_weight         822.90

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

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 217 67 ' '
2 0.741 0.128 0.268 39 5 ' '
3 0.259 -0.128 0.732 40 5 ' '
4 1.000 0.500 0.500 217 67 ' '
5 0.741 0.372 0.768 40 5 ' '
6 0.259 0.628 0.232 39 5 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_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                   15.696(4)
_cell_length_b                   8.307(2)
_cell_length_c                   28.470(8)
_cell_angle_alpha                90
_cell_angle_beta                 96.418(5)
_cell_angle_gamma                90
_cell_volume                     3689.0(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10999
_cell_measurement_theta_min      2.0489
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.167
_exptl_crystal_size_min          0.055
_exptl_absorpt_coefficient_mu    1.848
_shelx_estimated_absorpt_T_min   0.732
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8479
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36696
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.555
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_reflns_number_total             8442
_reflns_number_gt                7344
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000       217        67 ' '
   2  0.741  0.128  0.268        39         5 ' '
   3  0.259 -0.128  0.732        40         5 ' '
   4  1.000  0.500  0.500       217        67 ' '
   5  0.741  0.372  0.768        40         5 ' '
   6  0.259  0.628  0.232        39         5 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_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)+(0.0581P)²+3.5893P] 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         8442
_refine_ls_number_parameters     479
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1264
_refine_ls_wR_factor_gt          0.1199
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.001

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 0.40739(2) 0.18686(3) 0.95936(2) 0.02530(9) Uani 1 1 d . . . . .
O1 O -0.3050(3) -0.0867(4) 1.10694(12) 0.0405(9) Uani 1 1 d . . . . .
O2 O -0.3443(2) 0.0776(4) 1.04790(12) 0.0392(8) Uani 1 1 d . . . . .
O3 O -0.4235(2) 0.5718(4) 1.46753(11) 0.0368(8) Uani 1 1 d . . . . .
O4 O -0.5002(2) 0.4352(5) 1.41058(12) 0.0434(9) Uani 1 1 d . . . . .
O5 O 0.2688(2) 0.2863(4) 0.97425(12) 0.0364(8) Uani 1 1 d . . . . .
O6 O 0.3774(2) 0.4321(4) 1.00472(13) 0.0397(8) Uani 1 1 d . . . . .
O8 O 0.5452(2) 0.2816(4) 0.99150(13) 0.0378(8) Uani 1 1 d . . . . .
H8A H 0.588241 0.201827 0.987713 0.045 Uiso 1 1 d R U . . .
H8B H 0.557817 0.370898 0.977586 0.057 Uiso 1 1 d R U . . .
N1 N -0.1129(3) 0.5620(5) 1.18214(13) 0.0334(9) Uani 1 1 d . . . . .
N2 N 0.4314(11) 0.5746(17) 0.8527(5) 0.090(5) Uani 0.5 1 d . . P A 1
O7 O 0.4191(3) 0.3832(5) 0.90356(13) 0.0449(9) Uani 0.5 1 d . . P A 1
N2A N 0.4682(11) 0.393(2) 0.8305(5) 0.094(5) Uani 0.5 1 d . . P A 2
O7A O 0.4191(3) 0.3832(5) 0.90356(13) 0.0449(9) Uani 0.5 1 d . . P A 2
C1 C -0.3031(3) 0.0489(6) 1.08804(17) 0.0343(11) Uani 1 1 d . . . . .
C2 C -0.2489(3) 0.1814(6) 1.11296(17) 0.0322(11) Uani 1 1 d . . . . .
C3 C -0.2557(4) 0.3358(7) 1.0950(2) 0.0487(15) Uani 1 1 d . . . . .
H3 H -0.291402 0.356606 1.067363 0.058 Uiso 1 1 calc R U . . .
C4 C -0.2096(5) 0.4586(7) 1.1179(2) 0.0550(17) Uani 1 1 d . . . . .
H4 H -0.213340 0.561917 1.105271 0.066 Uiso 1 1 calc R U . . .
C5 C -0.1586(3) 0.4312(6) 1.15885(16) 0.0335(11) Uani 1 1 d . . . . .
C6 C -0.1524(5) 0.2780(8) 1.1773(3) 0.071(2) Uani 1 1 d . . . . .
H6 H -0.117046 0.258205 1.205162 0.086 Uiso 1 1 calc R U . . .
C7 C -0.1991(5) 0.1526(8) 1.1544(3) 0.075(2) Uani 1 1 d . . . . .
H7 H -0.196297 0.049698 1.167369 0.089 Uiso 1 1 calc R U . . .
C8 C -0.0485(3) 0.6496(6) 1.16316(16) 0.0312(10) Uani 1 1 d . . . . .
C9 C -0.0029(3) 0.6056(6) 1.12648(16) 0.0337(11) Uani 1 1 d . . . . .
H9 H -0.016721 0.512518 1.109143 0.040 Uiso 1 1 calc R U . . .
C10 C 0.0640(4) 0.7033(6) 1.11611(19) 0.0385(12) Uani 1 1 d . . . . .
C11 C 0.0794(4) 0.8480(7) 1.1411(2) 0.0526(17) Uani 1 1 d . . . . .
H11 H 0.121822 0.916886 1.132627 0.063 Uiso 1 1 calc R U . . .
C12 C 0.0342(4) 0.8915(7) 1.1777(2) 0.0531(17) Uani 1 1 d . . . . .
H12 H 0.045962 0.987850 1.193753 0.064 Uiso 1 1 calc R U . . .
C13 C -0.0302(3) 0.7877(6) 1.19039(19) 0.0366(12) Uani 1 1 d . . . . .
C14 C -0.0844(3) 0.7847(6) 1.22829(18) 0.0371(12) Uani 1 1 d . . . . .
C15 C -0.0923(4) 0.8818(8) 1.2673(2) 0.0517(16) Uani 1 1 d . . . . .
H15 H -0.059813 0.975238 1.272179 0.062 Uiso 1 1 calc R U . . .
C16 C -0.1494(5) 0.8370(8) 1.2988(2) 0.0575(18) Uani 1 1 d . . . . .
H16 H -0.154616 0.901490 1.325029 0.069 Uiso 1 1 calc R U . . .
C17 C -0.1994(4) 0.6970(7) 1.29217(18) 0.0390(12) Uani 1 1 d . . . . .
C18 C -0.1928(3) 0.6012(7) 1.25273(16) 0.0365(12) Uani 1 1 d . . . . .
H18 H -0.227108 0.510419 1.247015 0.044 Uiso 1 1 calc R U . . .
C19 C -0.1341(3) 0.6441(6) 1.22221(16) 0.0316(10) Uani 1 1 d . . . . .
C20 C 0.1226(4) 0.6473(6) 1.08107(18) 0.0384(12) Uani 1 1 d . . . . .
C21 C 0.0933(4) 0.5383(8) 1.04535(18) 0.0458(14) Uani 1 1 d . . . . .
H21 H 0.035232 0.513509 1.040060 0.055 Uiso 1 1 calc R U . . .
C22 C 0.1496(4) 0.4680(7) 1.01819(19) 0.0428(13) Uani 1 1 d . . . . .
H22 H 0.128736 0.396307 0.994565 0.051 Uiso 1 1 calc R U . . .
C23 C 0.2360(3) 0.5001(6) 1.02475(18) 0.0356(11) Uani 1 1 d . . . . .
C24 C 0.2657(4) 0.6140(7) 1.0591(2) 0.0525(16) Uani 1 1 d . . . . .
H24 H 0.323677 0.640332 1.063643 0.063 Uiso 1 1 calc R U . . .
C25 C 0.2091(4) 0.6872(7) 1.0862(2) 0.0571(18) Uani 1 1 d . . . . .
H25 H 0.229236 0.764781 1.108219 0.068 Uiso 1 1 calc R U . . .
C26 C 0.2965(3) 0.4032(6) 0.99947(16) 0.0307(10) Uani 1 1 d . . . . .
C27 C -0.2592(4) 0.6506(7) 1.32655(17) 0.0380(12) Uani 1 1 d . . . . .
C28 C -0.2398(4) 0.6811(6) 1.37520(18) 0.0390(12) Uani 1 1 d . . . . .
H28 H -0.188809 0.732675 1.386029 0.047 Uiso 1 1 calc R U . . .
C29 C -0.2959(3) 0.6351(7) 1.40739(17) 0.0361(11) Uani 1 1 d . . . . .
H29 H -0.282103 0.656195 1.439413 0.043 Uiso 1 1 calc R U . . .
C30 C -0.3717(3) 0.5586(6) 1.39203(16) 0.0336(10) Uani 1 1 d . . . . .
C31 C -0.3907(4) 0.5235(8) 1.34450(18) 0.0466(14) Uani 1 1 d . . . . .
H31 H -0.440836 0.468480 1.333936 0.056 Uiso 1 1 calc R U . . .
C32 C -0.3350(4) 0.5707(8) 1.31273(17) 0.0487(15) Uani 1 1 d . . . . .
H32 H -0.349073 0.547704 1.280842 0.058 Uiso 1 1 calc R U . . .
C33 C -0.4355(3) 0.5176(6) 1.42610(16) 0.0328(11) Uani 1 1 d . . . . .
C34 C 0.4132(12) 0.423(2) 0.8638(6) 0.075(5) Uani 0.5 1 d . . P A 1
C35 C 0.3733(13) 0.312(3) 0.8233(7) 0.069(5) Uani 0.5 1 d . . P A 1
H35A H 0.374248 0.366408 0.793535 0.104 Uiso 0.5 1 calc R U P A 1
H35B H 0.405809 0.214552 0.823222 0.104 Uiso 0.5 1 calc R U P A 1
H35C H 0.315115 0.287662 0.828030 0.104 Uiso 0.5 1 calc R U P A 1
C36 C 0.4729(15) 0.674(2) 0.8952(8) 0.092(7) Uani 0.5 1 d . . P A 1
H36A H 0.484340 0.780754 0.884979 0.138 Uiso 0.5 1 calc R U P A 1
H36B H 0.434454 0.678036 0.919144 0.138 Uiso 0.5 1 calc R U P A 1
H36C H 0.525577 0.623407 0.907858 0.138 Uiso 0.5 1 calc R U P A 1
C37 C 0.4081(16) 0.702(3) 0.8051(7) 0.140(9) Uani 0.5 1 d . U P A 1
H37A H 0.434949 0.804476 0.811958 0.211 Uiso 0.5 1 calc R U P A 1
H37B H 0.429345 0.656272 0.777664 0.211 Uiso 0.5 1 calc R U P A 1
H37C H 0.347180 0.716182 0.799061 0.211 Uiso 0.5 1 calc R U P A 1
C34A C 0.4660(12) 0.442(2) 0.8735(6) 0.072(4) Uani 0.5 1 d . U P A 2
C35A C 0.5179(17) 0.595(3) 0.8892(7) 0.112(7) Uani 0.5 1 d . U P A 2
H35D H 0.550491 0.628253 0.864306 0.168 Uiso 0.5 1 calc R U P A 2
H35E H 0.479336 0.679151 0.895864 0.168 Uiso 0.5 1 calc R U P A 2
H35F H 0.556140 0.571294 0.917060 0.168 Uiso 0.5 1 calc R U P A 2
C36A C 0.4084(12) 0.263(2) 0.8137(6) 0.059(4) Uani 0.5 1 d . . P A 2
H36D H 0.415767 0.236425 0.781595 0.089 Uiso 0.5 1 calc R U P A 2
H36E H 0.419881 0.169228 0.833255 0.089 Uiso 0.5 1 calc R U P A 2
H36F H 0.350505 0.297654 0.815448 0.089 Uiso 0.5 1 calc R U P A 2
C37A C 0.5390(19) 0.416(4) 0.7941(10) 0.169(11) Uani 0.5 1 d . U P A 2
H37D H 0.519893 0.362919 0.764849 0.254 Uiso 0.5 1 calc R U P A 2
H37E H 0.546892 0.528313 0.788516 0.254 Uiso 0.5 1 calc R U P A 2
H37F H 0.592332 0.369319 0.807439 0.254 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O3 2.279(3) 2_547 ?
Gd1 O7A 2.298(4) . ?
Gd1 O7 2.298(4) . ?
Gd1 O4 2.348(3) 4_665 ?
Gd1 O8 2.385(4) . ?
Gd1 O5 2.409(4) . ?
Gd1 O2 2.409(4) 3_557 ?
Gd1 O1 2.482(4) 3_557 ?
Gd1 O6 2.485(3) . ?
Gd1 C1 2.801(5) 3_557 ?
Gd1 C26 2.829(5) . ?
O1 C1 1.250(6) . ?
O2 C1 1.271(6) . ?
O3 C33 1.257(6) . ?
O4 C33 1.263(6) . ?
O5 C26 1.257(6) . ?
O6 C26 1.283(6) . ?
N1 C8 1.402(6) . ?
N1 C19 1.401(6) . ?
N1 C5 1.425(6) . ?
N2 C34 1.33(2) . ?
N2 C36 1.55(3) . ?
N2 C37 1.73(3) . ?
O7 C34 1.173(17) . ?
N2A C34A 1.30(2) . ?
N2A C36A 1.48(2) . ?
N2A C37A 1.61(3) . ?
O7A C34A 1.286(18) . ?
C1 C2 1.518(7) . ?
C2 C7 1.362(8) . ?
C2 C3 1.381(7) . ?
C3 C4 1.373(7) . ?
C4 C5 1.356(7) . ?
C5 C6 1.377(8) . ?
C6 C7 1.393(9) . ?
C8 C9 1.380(6) . ?
C8 C13 1.396(7) . ?
C9 C10 1.384(7) . ?
C10 C11 1.405(7) . ?
C10 C20 1.504(7) . ?
C11 C12 1.371(7) . ?
C12 C13 1.407(7) . ?
C13 C14 1.447(6) . ?
C14 C15 1.389(7) . ?
C14 C19 1.404(7) . ?
C15 C16 1.388(8) . ?
C16 C17 1.405(8) . ?
C17 C18 1.390(7) . ?
C17 C27 1.480(7) . ?
C18 C19 1.382(6) . ?
C20 C25 1.389(8) . ?
C20 C21 1.401(7) . ?
C21 C22 1.368(7) . ?
C22 C23 1.375(7) . ?
C23 C24 1.403(7) . ?
C23 C26 1.490(6) . ?
C24 C25 1.381(8) . ?
C27 C32 1.380(8) . ?
C27 C28 1.407(7) . ?
C28 C29 1.394(7) . ?
C29 C30 1.376(7) . ?
C30 C31 1.384(7) . ?
C30 C33 1.508(6) . ?
C31 C32 1.384(7) . ?
C34 C35 1.55(3) . ?
C34A C35A 1.55(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
O3 Gd1 O7A 156.89(14) 2_547 . ?
O3 Gd1 O7 156.89(14) 2_547 . ?
O3 Gd1 O4 110.25(13) 2_547 4_665 ?
O7 Gd1 O4 78.20(14) . 4_665 ?
O3 Gd1 O8 77.56(13) 2_547 . ?
O7A Gd1 O8 83.81(14) . . ?
O7 Gd1 O8 83.81(14) . . ?
O4 Gd1 O8 77.04(14) 4_665 . ?
O3 Gd1 O5 89.63(13) 2_547 . ?
O7A Gd1 O5 91.24(13) . . ?
O7 Gd1 O5 91.24(13) . . ?
O4 Gd1 O5 151.91(13) 4_665 . ?
O8 Gd1 O5 128.12(12) . . ?
O3 Gd1 O2 72.45(12) 2_547 3_557 ?
O7 Gd1 O2 130.66(13) . 3_557 ?
O4 Gd1 O2 80.26(14) 4_665 3_557 ?
O8 Gd1 O2 132.86(12) . 3_557 ?
O5 Gd1 O2 87.52(13) . 3_557 ?
O3 Gd1 O1 123.40(13) 2_547 3_557 ?
O7 Gd1 O1 78.87(13) . 3_557 ?
O4 Gd1 O1 78.22(13) 4_665 3_557 ?
O8 Gd1 O1 152.19(13) . 3_557 ?
O5 Gd1 O1 74.20(12) . 3_557 ?
O2 Gd1 O1 53.42(12) 3_557 3_557 ?
O3 Gd1 O6 82.97(13) 2_547 . ?
O7A Gd1 O6 79.15(14) . . ?
O7 Gd1 O6 79.15(14) . . ?
O4 Gd1 O6 145.79(13) 4_665 . ?
O8 Gd1 O6 75.32(12) . . ?
O5 Gd1 O6 53.13(11) . . ?
O2 Gd1 O6 133.79(12) 3_557 . ?
O1 Gd1 O6 121.71(12) 3_557 . ?
O3 Gd1 C1 98.40(14) 2_547 3_557 ?
O7A Gd1 C1 104.51(15) . 3_557 ?
O7 Gd1 C1 104.51(15) . 3_557 ?
O4 Gd1 C1 77.26(15) 4_665 3_557 ?
O8 Gd1 C1 150.64(14) . 3_557 ?
O5 Gd1 C1 80.43(13) . 3_557 ?
O2 Gd1 C1 26.92(13) 3_557 3_557 ?
O1 Gd1 C1 26.51(13) 3_557 3_557 ?
O6 Gd1 C1 133.56(13) . 3_557 ?
O3 Gd1 C26 84.76(13) 2_547 . ?
O7A Gd1 C26 85.88(14) . . ?
O7 Gd1 C26 85.88(14) . . ?
O4 Gd1 C26 164.07(13) 4_665 . ?
O8 Gd1 C26 101.98(14) . . ?
O5 Gd1 C26 26.22(13) . . ?
O2 Gd1 C26 110.39(13) 3_557 . ?
O1 Gd1 C26 98.31(14) 3_557 . ?
O6 Gd1 C26 26.96(12) . . ?
C1 Gd1 C26 106.62(15) 3_557 . ?
C1 O1 Gd1 91.1(3) . 3_557 ?
C1 O2 Gd1 94.0(3) . 3_557 ?
C33 O3 Gd1 175.7(3) . 2_557 ?
C33 O4 Gd1 123.6(3) . 4_466 ?
C26 O5 Gd1 95.9(3) . . ?
C26 O6 Gd1 91.6(3) . . ?
C8 N1 C19 108.0(4) . . ?
C8 N1 C5 124.3(4) . . ?
C19 N1 C5 126.6(4) . . ?
C34 N2 C36 113.5(14) . . ?
C34 N2 C37 137.0(15) . . ?
C36 N2 C37 108.8(14) . . ?
C34 O7 Gd1 149.8(10) . . ?
C34A N2A C36A 116.9(14) . . ?
C34A N2A C37A 131.6(19) . . ?
C36A N2A C37A 109.8(17) . . ?
C34A O7A Gd1 145.6(9) . . ?
O1 C1 O2 121.4(4) . . ?
O1 C1 C2 119.4(5) . . ?
O2 C1 C2 119.1(5) . . ?
O1 C1 Gd1 62.4(3) . 3_557 ?
O2 C1 Gd1 59.1(2) . 3_557 ?
C2 C1 Gd1 177.9(4) . 3_557 ?
C7 C2 C3 119.8(5) . . ?
C7 C2 C1 121.0(5) . . ?
C3 C2 C1 119.0(5) . . ?
C4 C3 C2 120.0(5) . . ?
C5 C4 C3 120.8(5) . . ?
C4 C5 C6 119.6(5) . . ?
C4 C5 N1 119.3(5) . . ?
C6 C5 N1 121.1(5) . . ?
C5 C6 C7 120.1(6) . . ?
C2 C7 C6 119.7(6) . . ?
C9 C8 C13 123.1(5) . . ?
C9 C8 N1 127.7(5) . . ?
C13 C8 N1 109.0(4) . . ?
C8 C9 C10 118.4(5) . . ?
C9 C10 C11 119.0(5) . . ?
C9 C10 C20 119.7(4) . . ?
C11 C10 C20 121.1(5) . . ?
C12 C11 C10 122.4(5) . . ?
C11 C12 C13 118.8(5) . . ?
C8 C13 C12 118.0(5) . . ?
C8 C13 C14 107.3(4) . . ?
C12 C13 C14 134.6(5) . . ?
C15 C14 C19 119.0(5) . . ?
C15 C14 C13 134.2(5) . . ?
C19 C14 C13 106.7(4) . . ?
C16 C15 C14 118.8(5) . . ?
C15 C16 C17 121.8(5) . . ?
C18 C17 C16 119.5(5) . . ?
C18 C17 C27 119.6(5) . . ?
C16 C17 C27 120.9(5) . . ?
C19 C18 C17 118.4(5) . . ?
C18 C19 N1 128.5(5) . . ?
C18 C19 C14 122.5(4) . . ?
N1 C19 C14 109.0(4) . . ?
C25 C20 C21 117.9(5) . . ?
C25 C20 C10 121.3(5) . . ?
C21 C20 C10 120.4(5) . . ?
C22 C21 C20 120.4(5) . . ?
C21 C22 C23 122.0(5) . . ?
C22 C23 C24 118.2(5) . . ?
C22 C23 C26 120.1(5) . . ?
C24 C23 C26 121.4(5) . . ?
C25 C24 C23 120.1(6) . . ?
C24 C25 C20 121.3(5) . . ?
O5 C26 O6 119.1(4) . . ?
O5 C26 C23 119.6(4) . . ?
O6 C26 C23 121.2(4) . . ?
O5 C26 Gd1 57.9(2) . . ?
O6 C26 Gd1 61.4(2) . . ?
C23 C26 Gd1 172.7(3) . . ?
C32 C27 C28 116.8(5) . . ?
C32 C27 C17 121.8(5) . . ?
C28 C27 C17 121.4(5) . . ?
C29 C28 C27 121.0(5) . . ?
C30 C29 C28 120.3(5) . . ?
C29 C30 C31 119.5(4) . . ?
C29 C30 C33 120.8(4) . . ?
C31 C30 C33 119.7(5) . . ?
C32 C31 C30 119.8(5) . . ?
C27 C32 C31 122.5(5) . . ?
O3 C33 O4 123.5(4) . . ?
O3 C33 C30 118.9(5) . . ?
O4 C33 C30 117.6(4) . . ?
O7 C34 N2 120.0(17) . . ?
O7 C34 C35 122.0(16) . . ?
N2 C34 C35 117.5(15) . . ?
O7A C34A N2A 126.0(16) . . ?
O7A C34A C35A 116.3(16) . . ?
N2A C34A C35A 117.5(17) . . ?

_refine_diff_density_max         1.327
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.122

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1553999'
_audit_update_record             
;
2018-01-05 deposited with the CCDC.
2018-01-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H33 N2 O10 Tb'
_chemical_formula_weight         824.57

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

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 220 55 ' '
2 0.744 0.136 0.267 38 4 ' '
3 0.256 -0.136 0.733 38 4 ' '
4 1.000 0.500 0.500 220 55 ' '
5 0.744 0.364 0.767 38 4 ' '
6 0.256 0.636 0.233 38 4 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_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                   15.729(4)
_cell_length_b                   8.3089(18)
_cell_length_c                   28.483(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.448(4)
_cell_angle_gamma                90
_cell_volume                     3699.1(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9304
_cell_measurement_theta_min      2.0470
_cell_measurement_theta_max      27.4855

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_F_000             1656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.029
_exptl_absorpt_coefficient_mu    1.962
_shelx_estimated_absorpt_T_min   0.797
_shelx_estimated_absorpt_T_max   0.945
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8022
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Saturn724+ (2x2 bin mode)
;
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37244
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.555
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_reflns_number_total             8465
_reflns_number_gt                7358
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000       220        55 ' '
   2  0.744  0.136  0.267        38         4 ' '
   3  0.256 -0.136  0.733        38         4 ' '
   4  1.000  0.500  0.500       220        55 ' '
   5  0.744  0.364  0.767        38         4 ' '
   6  0.256  0.636  0.233        38         4 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_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)+(0.0634P)²+9.4916P] 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         8465
_refine_ls_number_parameters     479
_refine_ls_number_restraints     1031
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0573
_refine_ls_wR_factor_ref         0.1448
_refine_ls_wR_factor_gt          0.1373
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.088
_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
Tb1 Tb 0.40760(2) 0.18674(3) 0.95941(2) 0.02734(10) Uani 1 1 d . . . . .
O1 O -0.3061(3) -0.0863(5) 1.10677(15) 0.0396(10) Uani 1 1 d . . . . .
O2 O -0.3442(3) 0.0772(5) 1.04821(14) 0.0382(9) Uani 1 1 d . . . . .
O3 O -0.5001(3) 0.4343(6) 1.41039(15) 0.0440(11) Uani 1 1 d . . . . .
O4 O -0.4244(3) 0.5705(5) 1.46750(14) 0.0374(9) Uani 1 1 d . . . . .
O5 O 0.2692(3) 0.2857(5) 0.97429(15) 0.0377(10) Uani 1 1 d . . . . .
O6 O 0.3774(3) 0.4316(5) 1.00507(16) 0.0400(10) Uani 1 1 d . . . . .
O8 O 0.5456(3) 0.2819(5) 0.99134(16) 0.0376(10) Uani 1 1 d . . . . .
H8A H 0.590102 0.213855 0.981302 0.045 Uiso 1 1 d R U . . .
H8B H 0.554645 0.380057 0.981417 0.056 Uiso 1 1 d R U . . .
N1 N -0.1130(3) 0.5614(6) 1.18202(16) 0.0321(10) Uani 1 1 d . . . . .
N2 N 0.4327(12) 0.5742(15) 0.8516(4) 0.092(6) Uani 0.5 1 d D . P A 1
O7 O 0.4191(3) 0.3842(6) 0.90401(16) 0.0472(11) Uani 0.5 1 d D . P A 1
N2A N 0.4683(11) 0.392(2) 0.8299(5) 0.096(6) Uani 0.5 1 d D . P A 2
O7A O 0.4191(3) 0.3842(6) 0.90401(16) 0.0472(11) Uani 0.5 1 d . . P A 2
C1 C -0.3029(4) 0.0494(7) 1.0881(2) 0.0367(11) Uani 1 1 d . U . . .
C2 C -0.2494(4) 0.1818(7) 1.1128(2) 0.0346(11) Uani 1 1 d . U . . .
C3 C -0.2560(5) 0.3356(8) 1.0951(3) 0.0484(14) Uani 1 1 d . U . . .
H3 H -0.291751 0.356123 1.067534 0.058 Uiso 1 1 calc R U . . .
C4 C -0.2098(5) 0.4610(8) 1.1181(2) 0.0480(13) Uani 1 1 d . U . . .
H4 H -0.213933 0.564608 1.105717 0.058 Uiso 1 1 calc R U . . .
C5 C -0.1586(4) 0.4307(8) 1.1588(2) 0.0361(10) Uani 1 1 d . U . . .
C6 C -0.1525(5) 0.2779(9) 1.1775(3) 0.0532(13) Uani 1 1 d . U . . .
H6 H -0.117873 0.258389 1.205576 0.064 Uiso 1 1 calc R U . . .
C7 C -0.1983(5) 0.1527(9) 1.1542(3) 0.0564(15) Uani 1 1 d . U . . .
H7 H -0.194268 0.049180 1.166694 0.068 Uiso 1 1 calc R U . . .
C8 C -0.0488(4) 0.6489(7) 1.1633(2) 0.0361(10) Uani 1 1 d . U . . .
C9 C -0.0032(4) 0.6056(7) 1.1266(2) 0.0361(10) Uani 1 1 d . U . . .
H9 H -0.017103 0.512688 1.109171 0.043 Uiso 1 1 calc R U . . .
C10 C 0.0640(4) 0.7032(8) 1.1160(2) 0.0404(11) Uani 1 1 d . U . . .
C11 C 0.0789(5) 0.8465(8) 1.1412(3) 0.0471(13) Uani 1 1 d . U . . .
H11 H 0.121341 0.915038 1.132691 0.057 Uiso 1 1 calc R U . . .
C12 C 0.0348(4) 0.8915(8) 1.1776(2) 0.0454(12) Uani 1 1 d . U . . .
H12 H 0.046971 0.987698 1.193687 0.054 Uiso 1 1 calc R U . . .
C13 C -0.0306(4) 0.7870(8) 1.1903(2) 0.0383(11) Uani 1 1 d . U . . .
C14 C -0.0842(4) 0.7830(8) 1.2284(2) 0.0399(11) Uani 1 1 d . U . . .
C15 C -0.0911(4) 0.8802(9) 1.2679(2) 0.0461(12) Uani 1 1 d . U . . .
H15 H -0.058214 0.972889 1.272910 0.055 Uiso 1 1 calc R U . . .
C16 C -0.1480(5) 0.8357(9) 1.2992(2) 0.0473(13) Uani 1 1 d . U . . .
H16 H -0.152618 0.899516 1.325634 0.057 Uiso 1 1 calc R U . . .
C17 C -0.1996(4) 0.6959(8) 1.2923(2) 0.0417(11) Uani 1 1 d . U . . .
C18 C -0.1931(4) 0.6007(8) 1.2522(2) 0.0380(10) Uani 1 1 d . U . . .
H18 H -0.227851 0.510802 1.246010 0.046 Uiso 1 1 calc R U . . .
C19 C -0.1340(4) 0.6436(8) 1.2220(2) 0.0361(10) Uani 1 1 d . U . . .
C20 C 0.1219(4) 0.6472(8) 1.0811(2) 0.0415(11) Uani 1 1 d . U . . .
C21 C 0.0943(4) 0.5381(8) 1.0455(2) 0.0430(12) Uani 1 1 d . U . . .
H21 H 0.036440 0.513229 1.039908 0.052 Uiso 1 1 calc R U . . .
C22 C 0.1504(4) 0.4664(8) 1.0184(2) 0.0436(12) Uani 1 1 d . U . . .
H22 H 0.129613 0.394039 0.994960 0.052 Uiso 1 1 calc R U . . .
C23 C 0.2366(4) 0.4990(7) 1.0251(2) 0.0375(12) Uani 1 1 d . U . . .
C24 C 0.2660(4) 0.6123(8) 1.0596(2) 0.0468(13) Uani 1 1 d . U . . .
H24 H 0.323828 0.638034 1.064430 0.056 Uiso 1 1 calc R U . . .
C25 C 0.2087(4) 0.6865(8) 1.0867(3) 0.0471(13) Uani 1 1 d . U . . .
H25 H 0.228689 0.763662 1.108837 0.057 Uiso 1 1 calc R U . . .
C26 C 0.2972(4) 0.4024(7) 0.9995(2) 0.0334(11) Uani 1 1 d . U . . .
C27 C -0.2588(4) 0.6498(8) 1.3269(2) 0.0399(11) Uani 1 1 d . U . . .
C28 C -0.2404(4) 0.6814(8) 1.3753(2) 0.0399(11) Uani 1 1 d . U . . .
H28 H -0.189801 0.733755 1.386242 0.048 Uiso 1 1 calc R U . . .
C29 C -0.2967(4) 0.6356(8) 1.4071(2) 0.0375(11) Uani 1 1 d . U . . .
H29 H -0.283288 0.657565 1.439052 0.045 Uiso 1 1 calc R U . . .
C30 C -0.3718(4) 0.5584(8) 1.3918(2) 0.0363(11) Uani 1 1 d . U . . .
C31 C -0.3909(4) 0.5251(8) 1.3445(2) 0.0426(12) Uani 1 1 d . U . . .
H31 H -0.441796 0.473077 1.333858 0.051 Uiso 1 1 calc R U . . .
C32 C -0.3347(4) 0.5688(9) 1.3127(2) 0.0447(12) Uani 1 1 d . U . . .
H32 H -0.348057 0.543267 1.280898 0.054 Uiso 1 1 calc R U . . .
C33 C -0.4358(4) 0.5171(7) 1.42586(19) 0.0333(11) Uani 1 1 d . U . . .
C34 C 0.4122(15) 0.4205(16) 0.8628(4) 0.085(4) Uani 0.5 1 d D U P A 1
C35 C 0.3734(15) 0.317(3) 0.8246(4) 0.085(4) Uani 0.5 1 d D U P A 1
H35A H 0.374901 0.370331 0.794828 0.127 Uiso 0.5 1 calc R U P A 1
H35B H 0.404786 0.217695 0.824570 0.127 Uiso 0.5 1 calc R U P A 1
H35C H 0.315119 0.294418 0.829365 0.127 Uiso 0.5 1 calc R U P A 1
C36 C 0.4737(14) 0.678(2) 0.8948(6) 0.080(4) Uani 0.5 1 d D U P A 1
H36A H 0.486296 0.783743 0.884151 0.120 Uiso 0.5 1 calc R U P A 1
H36B H 0.434267 0.684948 0.918120 0.120 Uiso 0.5 1 calc R U P A 1
H36C H 0.525626 0.627300 0.908516 0.120 Uiso 0.5 1 calc R U P A 1
C37 C 0.4156(15) 0.667(2) 0.8084(6) 0.094(4) Uani 0.5 1 d D U P A 1
H37A H 0.439736 0.772621 0.813175 0.140 Uiso 0.5 1 calc R U P A 1
H37B H 0.440777 0.614115 0.783391 0.140 Uiso 0.5 1 calc R U P A 1
H37C H 0.354890 0.675625 0.800111 0.140 Uiso 0.5 1 calc R U P A 1
C34A C 0.4617(14) 0.454(2) 0.8761(6) 0.087(4) Uani 0.5 1 d D U P A 2
C35A C 0.5196(16) 0.592(3) 0.8903(8) 0.099(4) Uani 0.5 1 d D U P A 2
H35D H 0.546488 0.628308 0.863541 0.149 Uiso 0.5 1 calc R U P A 2
H35E H 0.486731 0.678863 0.901505 0.149 Uiso 0.5 1 calc R U P A 2
H35F H 0.562596 0.559165 0.914980 0.149 Uiso 0.5 1 calc R U P A 2
C36A C 0.4035(14) 0.259(3) 0.8136(8) 0.082(4) Uani 0.5 1 d D U P A 2
H36D H 0.412399 0.224523 0.782319 0.124 Uiso 0.5 1 calc R U P A 2
H36E H 0.411247 0.169330 0.834874 0.124 Uiso 0.5 1 calc R U P A 2
H36F H 0.346470 0.300256 0.813335 0.124 Uiso 0.5 1 calc R U P A 2
C37A C 0.5462(14) 0.418(3) 0.7941(8) 0.110(5) Uani 0.5 1 d D U P A 2
H37D H 0.531643 0.360206 0.765122 0.165 Uiso 0.5 1 calc R U P A 2
H37E H 0.551766 0.530473 0.787354 0.165 Uiso 0.5 1 calc R U P A 2
H37F H 0.599496 0.378157 0.809523 0.165 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O4 2.283(4) 2_547 ?
Tb1 O7A 2.298(4) . ?
Tb1 O7 2.298(4) . ?
Tb1 O3 2.351(4) 4_665 ?
Tb1 O8 2.391(4) . ?
Tb1 O2 2.408(4) 3_557 ?
Tb1 O5 2.409(4) . ?
Tb1 O1 2.474(4) 3_557 ?
Tb1 O6 2.489(4) . ?
Tb1 C1 2.809(6) 3_557 ?
Tb1 C26 2.824(6) . ?
O1 C1 1.251(7) . ?
O2 C1 1.264(7) . ?
O3 C33 1.261(7) . ?
O4 C33 1.260(7) . ?
O5 C26 1.256(7) . ?
O6 C26 1.278(7) . ?
N1 C8 1.397(7) . ?
N1 C19 1.399(7) . ?
N1 C5 1.423(7) . ?
N2 C34 1.363(9) . ?
N2 C37 1.451(9) . ?
N2 C36 1.579(10) . ?
O7 C34 1.206(9) . ?
N2A C34A 1.428(10) . ?
N2A C36A 1.538(10) . ?
N2A C37A 1.693(10) . ?
O7A C34A 1.239(19) . ?
C1 C2 1.511(8) . ?
C2 C7 1.371(10) . ?
C2 C3 1.373(9) . ?
C3 C4 1.391(9) . ?
C4 C5 1.358(9) . ?
C5 C6 1.376(10) . ?
C6 C7 1.390(10) . ?
C8 C9 1.382(8) . ?
C8 C13 1.393(8) . ?
C9 C10 1.391(8) . ?
C10 C11 1.397(9) . ?
C10 C20 1.496(8) . ?
C11 C12 1.364(8) . ?
C12 C13 1.423(8) . ?
C13 C14 1.448(8) . ?
C14 C15 1.398(8) . ?
C14 C19 1.399(8) . ?
C15 C16 1.384(9) . ?
C16 C17 1.418(9) . ?
C17 C18 1.403(8) . ?
C17 C27 1.480(8) . ?
C18 C19 1.382(8) . ?
C20 C21 1.394(9) . ?
C20 C25 1.395(9) . ?
C21 C22 1.371(8) . ?
C22 C23 1.375(9) . ?
C23 C24 1.401(9) . ?
C23 C26 1.497(8) . ?
C24 C25 1.394(9) . ?
C27 C32 1.391(9) . ?
C27 C28 1.400(8) . ?
C28 C29 1.389(8) . ?
C29 C30 1.372(9) . ?
C30 C31 1.375(8) . ?
C30 C33 1.513(7) . ?
C31 C32 1.384(8) . ?
C34 C35 1.466(9) . ?
C34A C35A 1.497(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Tb1 O7A 156.67(17) 2_547 . ?
O4 Tb1 O7 156.67(17) 2_547 . ?
O4 Tb1 O3 110.15(16) 2_547 4_665 ?
O7 Tb1 O3 78.24(17) . 4_665 ?
O4 Tb1 O8 77.62(15) 2_547 . ?
O7A Tb1 O8 83.51(16) . . ?
O7 Tb1 O8 83.51(16) . . ?
O3 Tb1 O8 76.85(16) 4_665 . ?
O4 Tb1 O2 72.64(14) 2_547 3_557 ?
O7 Tb1 O2 130.69(16) . 3_557 ?
O3 Tb1 O2 80.43(16) 4_665 3_557 ?
O8 Tb1 O2 133.16(15) . 3_557 ?
O4 Tb1 O5 89.91(15) 2_547 . ?
O7A Tb1 O5 91.12(16) . . ?
O7 Tb1 O5 91.12(16) . . ?
O3 Tb1 O5 151.81(15) 4_665 . ?
O8 Tb1 O5 128.30(15) . . ?
O2 Tb1 O5 87.34(15) 3_557 . ?
O4 Tb1 O1 123.44(15) 2_547 3_557 ?
O7 Tb1 O1 79.13(16) . 3_557 ?
O3 Tb1 O1 77.98(16) 4_665 3_557 ?
O8 Tb1 O1 151.81(15) . 3_557 ?
O2 Tb1 O1 53.07(14) 3_557 3_557 ?
O5 Tb1 O1 74.39(14) . 3_557 ?
O4 Tb1 O6 83.03(15) 2_547 . ?
O7A Tb1 O6 79.02(16) . . ?
O7 Tb1 O6 79.02(16) . . ?
O3 Tb1 O6 145.79(16) 4_665 . ?
O8 Tb1 O6 75.48(14) . . ?
O2 Tb1 O6 133.64(14) 3_557 . ?
O5 Tb1 O6 53.12(14) . . ?
O1 Tb1 O6 121.96(15) 3_557 . ?
O4 Tb1 C1 98.35(17) 2_547 3_557 ?
O7A Tb1 C1 104.80(18) . 3_557 ?
O7 Tb1 C1 104.80(18) . 3_557 ?
O3 Tb1 C1 77.47(17) 4_665 3_557 ?
O8 Tb1 C1 150.68(16) . 3_557 ?
O2 Tb1 C1 26.65(16) 3_557 3_557 ?
O5 Tb1 C1 80.24(16) . 3_557 ?
O1 Tb1 C1 26.43(16) 3_557 3_557 ?
O6 Tb1 C1 133.37(16) . 3_557 ?
O4 Tb1 C26 85.04(16) 2_547 . ?
O7A Tb1 C26 85.63(17) . . ?
O7 Tb1 C26 85.63(17) . . ?
O3 Tb1 C26 163.86(17) 4_665 . ?
O8 Tb1 C26 102.11(16) . . ?
O2 Tb1 C26 110.31(16) 3_557 . ?
O5 Tb1 C26 26.27(15) . . ?
O1 Tb1 C26 98.54(16) 3_557 . ?
O6 Tb1 C26 26.89(15) . . ?
C1 Tb1 C26 106.48(17) 3_557 . ?
C1 O1 Tb1 91.9(4) . 3_557 ?
C1 O2 Tb1 94.6(4) . 3_557 ?
C33 O3 Tb1 123.4(4) . 4_466 ?
C33 O4 Tb1 175.4(4) . 2_557 ?
C26 O5 Tb1 95.6(3) . . ?
C26 O6 Tb1 91.3(3) . . ?
C8 N1 C19 107.7(5) . . ?
C8 N1 C5 124.6(5) . . ?
C19 N1 C5 126.7(5) . . ?
C34 N2 C37 132.0(14) . . ?
C34 N2 C36 114.5(11) . . ?
C37 N2 C36 113.1(14) . . ?
C34 O7 Tb1 147.4(6) . . ?
C34A N2A C36A 115.0(14) . . ?
C34A N2A C37A 129.9(16) . . ?
C36A N2A C37A 114.2(16) . . ?
C34A O7A Tb1 149.7(12) . . ?
O1 C1 O2 120.4(5) . . ?
O1 C1 C2 120.3(5) . . ?
O2 C1 C2 119.3(6) . . ?
O1 C1 Tb1 61.7(3) . 3_557 ?
O2 C1 Tb1 58.7(3) . 3_557 ?
C2 C1 Tb1 177.6(5) . 3_557 ?
C7 C2 C3 119.5(6) . . ?
C7 C2 C1 121.0(6) . . ?
C3 C2 C1 119.4(6) . . ?
C2 C3 C4 120.7(7) . . ?
C5 C4 C3 119.4(7) . . ?
C4 C5 C6 120.7(6) . . ?
C4 C5 N1 118.4(6) . . ?
C6 C5 N1 121.0(6) . . ?
C5 C6 C7 119.7(7) . . ?
C2 C7 C6 120.0(7) . . ?
C9 C8 C13 122.7(5) . . ?
C9 C8 N1 127.8(5) . . ?
C13 C8 N1 109.3(5) . . ?
C8 C9 C10 118.9(6) . . ?
C9 C10 C11 118.3(5) . . ?
C9 C10 C20 119.7(6) . . ?
C11 C10 C20 121.8(6) . . ?
C12 C11 C10 123.6(6) . . ?
C11 C12 C13 118.0(6) . . ?
C8 C13 C12 118.2(5) . . ?
C8 C13 C14 107.1(5) . . ?
C12 C13 C14 134.6(6) . . ?
C15 C14 C19 119.3(5) . . ?
C15 C14 C13 133.9(6) . . ?
C19 C14 C13 106.6(5) . . ?
C16 C15 C14 118.6(6) . . ?
C15 C16 C17 122.1(6) . . ?
C18 C17 C16 118.8(6) . . ?
C18 C17 C27 120.3(6) . . ?
C16 C17 C27 120.8(6) . . ?
C19 C18 C17 118.4(6) . . ?
C18 C19 C14 122.6(5) . . ?
C18 C19 N1 128.1(6) . . ?
C14 C19 N1 109.3(5) . . ?
C21 C20 C25 117.1(6) . . ?
C21 C20 C10 121.6(6) . . ?
C25 C20 C10 120.9(6) . . ?
C22 C21 C20 121.7(6) . . ?
C21 C22 C23 121.5(6) . . ?
C22 C23 C24 118.2(6) . . ?
C22 C23 C26 119.9(5) . . ?
C24 C23 C26 121.6(6) . . ?
C25 C24 C23 120.1(6) . . ?
C24 C25 C20 121.3(6) . . ?
O5 C26 O6 119.7(5) . . ?
O5 C26 C23 119.4(5) . . ?
O6 C26 C23 120.7(5) . . ?
O5 C26 Tb1 58.1(3) . . ?
O6 C26 Tb1 61.8(3) . . ?
C23 C26 Tb1 172.4(4) . . ?
C32 C27 C28 117.0(6) . . ?
C32 C27 C17 121.0(6) . . ?
C28 C27 C17 122.0(6) . . ?
C29 C28 C27 120.9(6) . . ?
C30 C29 C28 120.7(6) . . ?
C29 C30 C31 119.3(5) . . ?
C29 C30 C33 120.9(5) . . ?
C31 C30 C33 119.6(6) . . ?
C30 C31 C32 120.3(6) . . ?
C31 C32 C27 121.8(6) . . ?
O4 C33 O3 123.0(5) . . ?
O4 C33 C30 119.3(5) . . ?
O3 C33 C30 117.7(5) . . ?
O7 C34 N2 117.6(9) . . ?
O7 C34 C35 124.1(10) . . ?
N2 C34 C35 117.9(13) . . ?
O7A C34A N2A 121.7(14) . . ?
O7A C34A C35A 122.8(15) . . ?
N2A C34A C35A 115.0(18) . . ?

_refine_diff_density_max         1.532
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.133

