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

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

data_ip11748
_database_code_depnum_ccdc_archive 'CCDC 1880057'
loop_
_audit_author_name
_audit_author_address
'Berthold Kersting'
;University of  Leipzig
Germany
;
_audit_update_record             
;
2019-02-13 deposited with the CCDC.	2019-02-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/8
_shelx_SHELXL_version_number     2014/8
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H33 N O5.50'
_chemical_formula_weight         579.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

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

_cell_length_a                   11.516(2)
_cell_length_b                   14.372(3)
_cell_length_c                   18.060(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2989.1(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    181(2)
_cell_measurement_reflns_used    6500
_cell_measurement_theta_min      6.0
_cell_measurement_theta_max      56.0

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_F_000             1224
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    0.086
_shelx_estimated_absorpt_T_min   0.980
_shelx_estimated_absorpt_T_max   0.988
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      181(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19399
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.531
_diffrn_reflns_theta_max         24.980
_diffrn_reflns_theta_full        24.980
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5261
_reflns_number_gt                3947
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_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       'STOE IPDS software'
_computing_cell_refinement       'STOE IPDS software'
_computing_data_reduction        'STOE X-AREA'
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_computing_molecular_graphics    ' ORTEP 3 for Windows '
_computing_publication_material  ' POVRAY 3.1 for Windows '
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0805P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1460 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.3(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5261
_refine_ls_number_parameters     400
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0822
_refine_ls_wR_factor_gt          0.0757
_refine_ls_goodness_of_fit_ref   0.627
_refine_ls_restrained_S_all      0.627
_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
O1 O 0.98591(16) 0.30140(12) 0.23766(9) 0.0422(4) Uani 1 1 d . . . . .
O2 O 0.79978(17) 0.39493(12) 0.28482(9) 0.0478(5) Uani 1 1 d . . . . .
H2 H 0.8489 0.3633 0.2614 0.072 Uiso 1 1 calc R U . . .
O3 O 0.86975(19) 0.43680(13) 0.41898(11) 0.0564(5) Uani 1 1 d . . . . .
H3 H 0.8353 0.4201 0.3802 0.085 Uiso 1 1 calc R U . . .
O4 O 1.07856(19) 0.36415(14) 0.38373(11) 0.0599(5) Uani 1 1 d . . . . .
H4 H 1.0169 0.3815 0.4044 0.090 Uiso 1 1 calc R U . . .
O5 O 0.6193(2) 0.22761(19) 0.27310(12) 0.0745(7) Uani 1 1 d . . . . .
H5 H 0.6843 0.2026 0.2659 0.112 Uiso 1 1 calc R U . . .
N1 N 0.8321(2) 0.17914(14) 0.30412(12) 0.0504(6) Uani 1 1 d . . . . .
C1 C 0.9667(3) 0.39587(18) 0.12915(13) 0.0455(7) Uani 1 1 d . . . . .
C2 C 0.8374(3) 0.3778(2) 0.12629(14) 0.0533(7) Uani 1 1 d . . . . .
H2A H 0.8200 0.3187 0.1522 0.064 Uiso 1 1 calc R U . . .
H2B H 0.8129 0.3710 0.0740 0.064 Uiso 1 1 calc R U . . .
C3 C 0.7690(3) 0.4560(2) 0.16192(15) 0.0521(7) Uani 1 1 d . . . . .
C4 C 0.7192(4) 0.5258(3) 0.11930(17) 0.0765(11) Uani 1 1 d . . . . .
H4A H 0.7288 0.5246 0.0671 0.092 Uiso 1 1 calc R U . . .
C5 C 0.6564(4) 0.5963(3) 0.1509(2) 0.0913(14) Uani 1 1 d . . . . .
H5A H 0.6244 0.6440 0.1207 0.110 Uiso 1 1 calc R U . . .
C6 C 0.6395(3) 0.5982(2) 0.22718(19) 0.0739(10) Uani 1 1 d . . . . .
H6 H 0.5936 0.6461 0.2486 0.089 Uiso 1 1 calc R U . . .
C7 C 0.6888(2) 0.53100(19) 0.27218(15) 0.0500(7) Uani 1 1 d . . . . .
C8 C 0.6693(3) 0.5331(2) 0.35550(16) 0.0531(7) Uani 1 1 d . . . . .
H8A H 0.5954 0.5660 0.3657 0.064 Uiso 1 1 calc R U . . .
H8B H 0.6607 0.4684 0.3735 0.064 Uiso 1 1 calc R U . . .
C9 C 0.7656(3) 0.58004(18) 0.39916(13) 0.0467(7) Uani 1 1 d . . . . .
C10 C 0.7613(3) 0.67542(19) 0.41337(14) 0.0535(7) Uani 1 1 d . . . . .
H10 H 0.6976 0.7109 0.3955 0.064 Uiso 1 1 calc R U . . .
C11 C 0.8484(3) 0.7191(2) 0.45305(15) 0.0621(9) Uani 1 1 d . . . . .
H11 H 0.8430 0.7838 0.4633 0.075 Uiso 1 1 calc R U . . .
C12 C 0.9423(3) 0.6695(2) 0.47758(15) 0.0611(9) Uani 1 1 d . . . . .
H12 H 1.0019 0.7007 0.5042 0.073 Uiso 1 1 calc R U . . .
C13 C 0.9523(3) 0.5750(2) 0.46446(13) 0.0526(7) Uani 1 1 d . . . . .
C14 C 1.0593(3) 0.5213(2) 0.48721(15) 0.0631(9) Uani 1 1 d . . . . .
H14A H 1.0360 0.4580 0.5029 0.076 Uiso 1 1 calc R U . . .
H14B H 1.0955 0.5525 0.5303 0.076 Uiso 1 1 calc R U . . .
C15 C 1.1484(3) 0.5136(2) 0.42523(15) 0.0550(7) Uani 1 1 d . . . . .
C16 C 1.2294(3) 0.5837(2) 0.41533(17) 0.0644(9) Uani 1 1 d . . . . .
H16 H 1.2282 0.6360 0.4475 0.077 Uiso 1 1 calc R U . . .
C17 C 1.3123(3) 0.5797(3) 0.35990(18) 0.0658(9) Uani 1 1 d . . . . .
H17 H 1.3684 0.6278 0.3551 0.079 Uiso 1 1 calc R U . . .
C18 C 1.3126(3) 0.5054(2) 0.31187(18) 0.0620(8) Uani 1 1 d . . . . .
H18 H 1.3694 0.5028 0.2738 0.074 Uiso 1 1 calc R U . . .
C19 C 1.2317(2) 0.4341(2) 0.31778(15) 0.0510(7) Uani 1 1 d . . . . .
C20 C 1.2249(3) 0.3573(2) 0.26066(16) 0.0538(7) Uani 1 1 d . . . . .
H20A H 1.1901 0.3012 0.2834 0.065 Uiso 1 1 calc R U . . .
H20B H 1.3041 0.3411 0.2438 0.065 Uiso 1 1 calc R U . . .
C21 C 1.1519(2) 0.38716(17) 0.19437(14) 0.0462(6) Uani 1 1 d . . . . .
C22 C 1.2000(3) 0.44567(19) 0.14127(15) 0.0544(7) Uani 1 1 d . . . . .
H22 H 1.2789 0.4642 0.1456 0.065 Uiso 1 1 calc R U . . .
C23 C 1.1344(3) 0.47729(19) 0.08230(15) 0.0567(8) Uani 1 1 d . . . . .
H23 H 1.1691 0.5154 0.0455 0.068 Uiso 1 1 calc R U . . .
C24 C 1.0192(3) 0.4537(2) 0.07681(14) 0.0552(8) Uani 1 1 d . . . . .
H24 H 0.9744 0.4771 0.0367 0.066 Uiso 1 1 calc R U . . .
C25 C 1.0367(2) 0.36136(17) 0.18579(13) 0.0418(6) Uani 1 1 d . . . . .
C26 C 1.1518(3) 0.4384(2) 0.37621(15) 0.0513(7) Uani 1 1 d . . . . .
C27 C 0.8616(3) 0.53198(18) 0.42640(13) 0.0463(6) Uani 1 1 d . . . . .
C28 C 0.7533(2) 0.46074(18) 0.23886(14) 0.0431(6) Uani 1 1 d . . . . .
C29 C 0.9905(3) 0.20359(18) 0.21769(14) 0.0475(6) Uani 1 1 d . . . . .
H29A H 1.0710 0.1855 0.2049 0.057 Uiso 1 1 calc R U . . .
H29B H 0.9401 0.1914 0.1743 0.057 Uiso 1 1 calc R U . . .
C30 C 0.9487(3) 0.14898(19) 0.28372(16) 0.0555(7) Uani 1 1 d . . . . .
H30A H 0.9479 0.0818 0.2717 0.067 Uiso 1 1 calc R U . . .
H30B H 1.0022 0.1587 0.3259 0.067 Uiso 1 1 calc R U . . .
C31 C 0.8132(3) 0.2049(2) 0.37053(14) 0.0515(7) Uani 1 1 d . . . . .
H31 H 0.8741 0.1996 0.4057 0.062 Uiso 1 1 calc R U . . .
C32 C 0.7017(2) 0.24203(18) 0.39468(14) 0.0479(6) Uani 1 1 d . . . . .
C33 C 0.6114(3) 0.2556(2) 0.34466(16) 0.0537(7) Uani 1 1 d . . . . .
C34 C 0.5107(3) 0.3003(2) 0.36721(19) 0.0639(8) Uani 1 1 d . . . . .
H34 H 0.4498 0.3110 0.3327 0.077 Uiso 1 1 calc R U . . .
C35 C 0.4988(3) 0.3294(2) 0.43954(19) 0.0656(9) Uani 1 1 d . . . . .
H35 H 0.4297 0.3601 0.4546 0.079 Uiso 1 1 calc R U . . .
C36 C 0.5857(3) 0.3143(3) 0.48992(19) 0.0724(10) Uani 1 1 d . . . . .
H36 H 0.5761 0.3329 0.5400 0.087 Uiso 1 1 calc R U . . .
C37 C 0.6866(3) 0.2721(2) 0.46753(16) 0.0656(9) Uani 1 1 d . . . . .
H37 H 0.7475 0.2631 0.5023 0.079 Uiso 1 1 calc R U . . .
OW1 O 1.5095(13) 0.3571(11) 0.1650(8) 0.115(4) Uiso 0.25 1 d . . P . .
OW2 O 1.4815(14) 0.2783(12) 0.1711(9) 0.130(5) Uiso 0.25 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C25 1.401(3) . ?
O1 C29 1.452(3) . ?
O2 C28 1.367(3) . ?
O3 C27 1.378(3) . ?
O4 C26 1.367(3) . ?
O5 C33 1.357(3) . ?
N1 C31 1.274(3) . ?
N1 C30 1.458(4) . ?
C1 C25 1.393(4) . ?
C1 C24 1.396(4) . ?
C1 C2 1.513(4) . ?
C2 C3 1.515(4) . ?
C3 C4 1.389(4) . ?
C3 C28 1.403(4) . ?
C4 C5 1.369(5) . ?
C5 C6 1.392(5) . ?
C6 C7 1.384(4) . ?
C7 C28 1.391(4) . ?
C7 C8 1.522(4) . ?
C8 C9 1.519(4) . ?
C9 C27 1.394(4) . ?
C9 C10 1.395(4) . ?
C10 C11 1.383(5) . ?
C11 C12 1.369(5) . ?
C12 C13 1.383(4) . ?
C13 C27 1.395(4) . ?
C13 C14 1.511(5) . ?
C14 C15 1.522(5) . ?
C15 C16 1.385(4) . ?
C15 C26 1.398(4) . ?
C16 C17 1.384(5) . ?
C17 C18 1.376(5) . ?
C18 C19 1.389(4) . ?
C19 C26 1.402(4) . ?
C19 C20 1.512(4) . ?
C20 C21 1.524(4) . ?
C21 C25 1.386(4) . ?
C21 C22 1.390(4) . ?
C22 C23 1.383(4) . ?
C23 C24 1.373(5) . ?
C29 C30 1.507(4) . ?
C31 C32 1.457(4) . ?
C32 C33 1.391(4) . ?
C32 C37 1.395(4) . ?
C33 C34 1.387(4) . ?
C34 C35 1.378(5) . ?
C35 C36 1.370(5) . ?
C36 C37 1.372(5) . ?
OW1 OW2 1.183(19) . ?

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
C25 O1 C29 114.47(18) . . ?
C31 N1 C30 118.8(3) . . ?
C25 C1 C24 117.3(3) . . ?
C25 C1 C2 122.2(2) . . ?
C24 C1 C2 120.3(3) . . ?
C1 C2 C3 111.7(2) . . ?
C4 C3 C28 117.4(3) . . ?
C4 C3 C2 121.0(3) . . ?
C28 C3 C2 121.6(2) . . ?
C5 C4 C3 121.5(3) . . ?
C4 C5 C6 120.0(3) . . ?
C7 C6 C5 120.7(3) . . ?
C6 C7 C28 118.1(3) . . ?
C6 C7 C8 120.4(3) . . ?
C28 C7 C8 121.4(2) . . ?
C9 C8 C7 114.5(2) . . ?
C27 C9 C10 116.8(3) . . ?
C27 C9 C8 122.9(2) . . ?
C10 C9 C8 120.4(3) . . ?
C11 C10 C9 121.0(3) . . ?
C12 C11 C10 120.3(3) . . ?
C11 C12 C13 121.4(3) . . ?
C12 C13 C27 117.2(3) . . ?
C12 C13 C14 121.5(3) . . ?
C27 C13 C14 121.2(3) . . ?
C13 C14 C15 112.7(2) . . ?
C16 C15 C26 117.5(3) . . ?
C16 C15 C14 119.8(3) . . ?
C26 C15 C14 122.7(3) . . ?
C17 C16 C15 121.9(3) . . ?
C18 C17 C16 119.3(3) . . ?
C17 C18 C19 121.5(3) . . ?
C18 C19 C26 117.7(3) . . ?
C18 C19 C20 121.4(3) . . ?
C26 C19 C20 120.8(3) . . ?
C19 C20 C21 111.0(2) . . ?
C25 C21 C22 117.8(3) . . ?
C25 C21 C20 122.7(2) . . ?
C22 C21 C20 119.5(3) . . ?
C23 C22 C21 120.8(3) . . ?
C24 C23 C22 120.2(3) . . ?
C23 C24 C1 121.1(3) . . ?
C21 C25 C1 122.7(2) . . ?
C21 C25 O1 119.3(2) . . ?
C1 C25 O1 117.9(2) . . ?
O4 C26 C15 121.6(3) . . ?
O4 C26 C19 116.4(3) . . ?
C15 C26 C19 122.0(3) . . ?
O3 C27 C9 120.8(2) . . ?
O3 C27 C13 115.9(3) . . ?
C9 C27 C13 123.2(2) . . ?
O2 C28 C7 116.7(2) . . ?
O2 C28 C3 121.1(2) . . ?
C7 C28 C3 122.2(3) . . ?
O1 C29 C30 107.2(2) . . ?
N1 C30 C29 109.8(2) . . ?
N1 C31 C32 122.6(3) . . ?
C33 C32 C37 118.5(3) . . ?
C33 C32 C31 121.0(2) . . ?
C37 C32 C31 120.3(3) . . ?
O5 C33 C34 118.3(3) . . ?
O5 C33 C32 121.8(3) . . ?
C34 C33 C32 119.9(3) . . ?
C35 C34 C33 120.1(3) . . ?
C36 C35 C34 120.6(3) . . ?
C35 C36 C37 119.5(3) . . ?
C36 C37 C32 121.3(3) . . ?

_refine_diff_density_max         0.115
_refine_diff_density_min         -0.093
_refine_diff_density_rms         0.024

####################################################################### 
# 
# 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_ip2-2161n
_database_code_depnum_ccdc_archive 'CCDC 1880058'
loop_
_audit_author_name
_audit_author_address
'Berthold Kersting'
;University of  Leipzig
Germany
;
_audit_update_record             
;
2019-02-13 deposited with the CCDC.	2019-02-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT231_ip2-2161n           
;
PROBLEM: Hirshfeld Test (Solvent)   N3       --C75      .       14.0 s.u.  
RESPONSE: Solvate Molecule
;

_vrf_PLAT919_ip2-2161n           
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          2 Check 
RESPONSE: 
Due to large unit cell a small mask had to
be used \ during integration (A = 6, B = 0, EMS = 0.006) 
to avoid overlaps. This results in the outer regions of the most 
intense reflections being cut off.
;
_vrf_PLAT934_ip2-2161n           
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          3 Check 
RESPONSE: Due to large unit cell a small mask had to
be used \ during integration (A = 6, B = 0, EMS = 0.006) 
to avoid overlaps. This results in the outer regions of the most 
intense reflections being cut off.
;



# end Validation Reply Form

_audit_creation_method           SHELXL-2014/8
_shelx_SHELXL_version_number     2014/8
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86 H84 N6 O10 Sm2'
_chemical_formula_weight         1662.29

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   22.6899(5)
_cell_length_b                   25.2258(5)
_cell_length_c                   26.5373(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15189.2(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    23650
_cell_measurement_theta_min      5.3
_cell_measurement_theta_max      23.4

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_F_000             6768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.470
_exptl_absorpt_coefficient_mu    1.595
_shelx_estimated_absorpt_T_min   0.448
_shelx_estimated_absorpt_T_max   0.521
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_process_details   
;
Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. 
and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) 
Acta Cryst. 1965, 1035-1038.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48009
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.778
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14906
_reflns_number_gt                11481
_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       'STOE IPDS software'
_computing_cell_refinement       'STOE IPDS software'
_computing_data_reduction        'STOE X-AREA'
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_computing_molecular_graphics    ' ORTEP 3 for Windows '
_computing_publication_material  ' POVRAY 3.1 for Windows '
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0751P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/8 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00137(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         14906
_refine_ls_number_parameters     945
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1208
_refine_ls_wR_factor_gt          0.1137
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_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
C1 C -0.0409(2) -0.02816(17) 0.22608(16) 0.0481(10) Uani 1 1 d . . . . .
C2 C -0.0402(2) -0.05511(17) 0.27272(16) 0.0470(9) Uani 1 1 d . . . . .
C3 C -0.0850(2) -0.09237(17) 0.28211(18) 0.0552(11) Uani 1 1 d . . . . .
H3 H -0.0852 -0.1109 0.3133 0.066 Uiso 1 1 calc R U . . .
C4 C -0.1285(2) -0.10266(18) 0.2473(2) 0.0595(12) Uani 1 1 d . . . . .
H4B H -0.1578 -0.1286 0.2542 0.071 Uiso 1 1 calc R U . . .
C5 C -0.1296(2) -0.07492(18) 0.2021(2) 0.0605(12) Uani 1 1 d . . . . .
H5 H -0.1600 -0.0819 0.1784 0.073 Uiso 1 1 calc R U . . .
C6 C -0.0872(2) -0.03742(17) 0.19108(16) 0.0507(10) Uani 1 1 d . . . . .
C7 C -0.0891(2) -0.0046(2) 0.14322(18) 0.0595(12) Uani 1 1 d . . . . .
H7A H -0.0872 0.0333 0.1525 0.071 Uiso 1 1 calc R U . . .
H7B H -0.1274 -0.0108 0.1263 0.071 Uiso 1 1 calc R U . . .
C8 C -0.0399(2) -0.01650(19) 0.10612(16) 0.0579(12) Uani 1 1 d . . . . .
C9 C -0.0417(3) -0.0628(2) 0.07741(18) 0.0651(14) Uani 1 1 d . . . . .
H9 H -0.0747 -0.0857 0.0801 0.078 Uiso 1 1 calc R U . . .
C10 C 0.0036(3) -0.0756(2) 0.04535(19) 0.0700(15) Uani 1 1 d . . . . .
H10 H 0.0012 -0.1067 0.0253 0.084 Uiso 1 1 calc R U . . .
C11 C 0.0527(3) -0.0436(2) 0.04203(18) 0.0692(15) Uani 1 1 d . . . . .
H11 H 0.0839 -0.0532 0.0200 0.083 Uiso 1 1 calc R U . . .
C12 C 0.0573(2) 0.0026(2) 0.07036(16) 0.0594(13) Uani 1 1 d . . . . .
C13 C 0.0094(2) 0.01635(18) 0.10025(15) 0.0556(12) Uani 1 1 d . . . . .
C14 C 0.1149(2) 0.03417(19) 0.06875(16) 0.0614(13) Uani 1 1 d . . . . .
H14A H 0.1279 0.0379 0.0333 0.074 Uiso 1 1 calc R U . . .
H14B H 0.1079 0.0701 0.0824 0.074 Uiso 1 1 calc R U . . .
C15 C 0.1628(2) 0.00736(19) 0.09887(17) 0.0582(12) Uani 1 1 d . . . . .
C16 C 0.2003(3) -0.0289(2) 0.0765(2) 0.0726(15) Uani 1 1 d . . . . .
H16 H 0.1976 -0.0351 0.0412 0.087 Uiso 1 1 calc R U . . .
C17 C 0.2418(3) -0.0563(3) 0.1044(2) 0.0807(17) Uani 1 1 d . . . . .
H17 H 0.2672 -0.0812 0.0885 0.097 Uiso 1 1 calc R U . . .
C18 C 0.2458(2) -0.0470(2) 0.1562(2) 0.0678(14) Uani 1 1 d . . . . .
H18 H 0.2745 -0.0656 0.1754 0.081 Uiso 1 1 calc R U . . .
C19 C 0.2087(2) -0.01123(18) 0.18022(18) 0.0553(11) Uani 1 1 d . . . . .
C20 C 0.1668(2) 0.01672(17) 0.15078(17) 0.0517(11) Uani 1 1 d . . . . .
C21 C 0.2097(2) -0.00463(18) 0.23667(18) 0.0539(10) Uani 1 1 d . . . . .
H21A H 0.2002 0.0326 0.2452 0.065 Uiso 1 1 calc R U . . .
H21B H 0.2498 -0.0123 0.2493 0.065 Uiso 1 1 calc R U . . .
C22 C 0.16576(19) -0.04127(16) 0.26263(16) 0.0453(9) Uani 1 1 d . . . . .
C23 C 0.1775(2) -0.09567(17) 0.26577(18) 0.0528(10) Uani 1 1 d . . . . .
H23 H 0.2144 -0.1088 0.2543 0.063 Uiso 1 1 calc R U . . .
C24 C 0.1364(2) -0.13069(17) 0.28531(17) 0.0528(11) Uani 1 1 d . . . . .
H24 H 0.1457 -0.1673 0.2885 0.063 Uiso 1 1 calc R U . . .
C25 C 0.0821(2) -0.11205(16) 0.30000(16) 0.0499(10) Uani 1 1 d . . . . .
H25 H 0.0535 -0.1365 0.3120 0.060 Uiso 1 1 calc R U . . .
C26 C 0.0677(2) -0.05819(17) 0.29773(15) 0.0441(9) Uani 1 1 d . . . . .
C27 C 0.1115(2) -0.02271(15) 0.28089(13) 0.0425(9) Uani 1 1 d . . . . .
C28 C 0.0059(2) -0.04042(17) 0.31132(15) 0.0479(10) Uani 1 1 d . . . . .
H28A H -0.0051 -0.0564 0.3441 0.057 Uiso 1 1 calc R U . . .
H28B H 0.0058 -0.0014 0.3156 0.057 Uiso 1 1 calc R U . . .
C29 C -0.0126(2) 0.10823(18) 0.09614(16) 0.0555(11) Uani 1 1 d . . . . .
H29A H -0.0496 0.0977 0.0791 0.067 Uiso 1 1 calc R U . . .
H29B H 0.0165 0.1185 0.0702 0.067 Uiso 1 1 calc R U . . .
C30 C -0.0237(2) 0.1539(2) 0.13201(17) 0.0571(11) Uani 1 1 d . . . . .
H30A H -0.0321 0.1866 0.1127 0.069 Uiso 1 1 calc R U . . .
H30B H -0.0583 0.1460 0.1534 0.069 Uiso 1 1 calc R U . . .
C31 C 0.0571(2) 0.20514(17) 0.15834(16) 0.0492(10) Uani 1 1 d . . . . .
H31 H 0.0413 0.2300 0.1351 0.059 Uiso 1 1 calc R U . . .
C32 C 0.1107(2) 0.22039(16) 0.18386(15) 0.0456(9) Uani 1 1 d . . . . .
C33 C 0.1402(3) 0.26525(18) 0.16407(18) 0.0601(12) Uani 1 1 d . . . . .
H33 H 0.1235 0.2832 0.1360 0.072 Uiso 1 1 calc R U . . .
C34 C 0.1918(3) 0.2834(2) 0.1841(2) 0.0676(14) Uani 1 1 d . . . . .
H34 H 0.2116 0.3127 0.1693 0.081 Uiso 1 1 calc R U . . .
C35 C 0.2150(2) 0.2589(2) 0.2262(2) 0.0657(13) Uani 1 1 d . . . . .
H35 H 0.2508 0.2715 0.2404 0.079 Uiso 1 1 calc R U . . .
C36 C 0.18645(19) 0.21594(18) 0.24778(17) 0.0525(11) Uani 1 1 d . . . . .
H36 H 0.2024 0.2004 0.2774 0.063 Uiso 1 1 calc R U . . .
C37 C 0.13424(18) 0.19458(15) 0.22689(15) 0.0411(9) Uani 1 1 d . . . . .
C38 C 0.0856(2) 0.28070(16) 0.41471(18) 0.0568(12) Uani 1 1 d . . . . .
C39 C 0.1443(3) 0.29554(18) 0.4219(2) 0.0645(14) Uani 1 1 d . . . . .
C40 C 0.1611(3) 0.3128(2) 0.4696(2) 0.0687(14) Uani 1 1 d . . . . .
H40 H 0.2006 0.3241 0.4750 0.082 Uiso 1 1 calc R U . . .
C41 C 0.1219(3) 0.3139(2) 0.5092(2) 0.0703(15) Uani 1 1 d . . . . .
H41 H 0.1340 0.3265 0.5413 0.084 Uiso 1 1 calc R U . . .
C42 C 0.0644(2) 0.29648(18) 0.50157(19) 0.0592(12) Uani 1 1 d . . . . .
H42 H 0.0377 0.2962 0.5291 0.071 Uiso 1 1 calc R U . . .
C43 C 0.0451(2) 0.27931(16) 0.45423(18) 0.0532(11) Uani 1 1 d . . . . .
C44 C -0.0176(2) 0.25827(17) 0.44936(19) 0.0548(11) Uani 1 1 d . . . . .
H44A H -0.0282 0.2555 0.4133 0.066 Uiso 1 1 calc R U . . .
H44B H -0.0453 0.2834 0.4655 0.066 Uiso 1 1 calc R U . . .
C45 C -0.0233(2) 0.20404(16) 0.47415(17) 0.0488(10) Uani 1 1 d . . . . .
C46 C -0.0419(2) 0.19761(19) 0.52407(18) 0.0578(12) Uani 1 1 d . . . . .
H46 H -0.0538 0.2278 0.5429 0.069 Uiso 1 1 calc R U . . .
C47 C -0.0435(3) 0.1486(2) 0.54630(19) 0.0688(14) Uani 1 1 d . . . . .
H47 H -0.0562 0.1450 0.5802 0.083 Uiso 1 1 calc R U . . .
C48 C -0.0262(2) 0.10401(19) 0.51886(17) 0.0584(12) Uani 1 1 d . . . . .
H48 H -0.0275 0.0701 0.5343 0.070 Uiso 1 1 calc R U . . .
C49 C -0.00706(18) 0.10850(15) 0.46924(15) 0.0415(8) Uani 1 1 d . . . . .
C50 C -0.00597(18) 0.15905(15) 0.44660(15) 0.0411(8) Uani 1 1 d . . . . .
C51 C 0.01539(18) 0.06086(15) 0.43987(15) 0.0421(9) Uani 1 1 d . . . . .
H51A H -0.0025 0.0282 0.4538 0.051 Uiso 1 1 calc R U . . .
H51B H 0.0029 0.0641 0.4042 0.051 Uiso 1 1 calc R U . . .
C52 C 0.08173(19) 0.05619(15) 0.44216(14) 0.0402(8) Uani 1 1 d . . . . .
C53 C 0.1087(2) 0.03870(16) 0.48630(16) 0.0483(10) Uani 1 1 d . . . . .
H53 H 0.0847 0.0283 0.5140 0.058 Uiso 1 1 calc R U . . .
C54 C 0.1693(2) 0.03600(18) 0.49102(17) 0.0570(12) Uani 1 1 d . . . . .
H54 H 0.1866 0.0219 0.5207 0.068 Uiso 1 1 calc R U . . .
C55 C 0.2042(2) 0.0540(2) 0.45224(18) 0.0576(12) Uani 1 1 d . . . . .
H55 H 0.2458 0.0543 0.4565 0.069 Uiso 1 1 calc R U . . .
C56 C 0.18014(19) 0.07193(17) 0.40641(16) 0.0485(10) Uani 1 1 d . . . . .
C57 C 0.11862(18) 0.07021(14) 0.40123(14) 0.0385(8) Uani 1 1 d . . . . .
C58 C 0.22085(19) 0.09456(19) 0.36672(17) 0.0550(11) Uani 1 1 d . . . . .
H58A H 0.2540 0.0697 0.3613 0.066 Uiso 1 1 calc R U . . .
H58B H 0.1990 0.0978 0.3346 0.066 Uiso 1 1 calc R U . . .
C59 C 0.2452(2) 0.1480(2) 0.38101(19) 0.0647(14) Uani 1 1 d . . . . .
C60 C 0.3030(2) 0.1560(3) 0.3969(3) 0.115(3) Uani 1 1 d . . . . .
H60 H 0.3287 0.1264 0.3997 0.138 Uiso 1 1 calc R U . . .
C61 C 0.3238(3) 0.2057(4) 0.4086(4) 0.145(4) Uani 1 1 d . . . . .
H61 H 0.3631 0.2098 0.4203 0.174 Uiso 1 1 calc R U . . .
C62 C 0.2886(3) 0.2489(3) 0.4037(3) 0.119(3) Uani 1 1 d . . . . .
H62 H 0.3039 0.2830 0.4116 0.143 Uiso 1 1 calc R U . . .
C63 C 0.2308(2) 0.2443(2) 0.3872(2) 0.0747(17) Uani 1 1 d . . . . .
C64 C 0.2081(2) 0.1930(2) 0.37751(17) 0.0576(12) Uani 1 1 d . . . . .
C65 C 0.1909(3) 0.2908(2) 0.3804(2) 0.0793(18) Uani 1 1 d . . . . .
H65A H 0.1709 0.2877 0.3474 0.095 Uiso 1 1 calc R U . . .
H65B H 0.2149 0.3235 0.3798 0.095 Uiso 1 1 calc R U . . .
C66 C 0.0369(3) 0.30957(18) 0.33915(19) 0.0669(14) Uani 1 1 d . . . . .
H66A H 0.0601 0.3428 0.3410 0.080 Uiso 1 1 calc R U . . .
H66B H -0.0025 0.3160 0.3540 0.080 Uiso 1 1 calc R U . . .
C67 C 0.0312(3) 0.29154(18) 0.28554(18) 0.0710(15) Uani 1 1 d . . . . .
H67A H 0.0062 0.3168 0.2666 0.085 Uiso 1 1 calc R U . . .
H67B H 0.0706 0.2907 0.2695 0.085 Uiso 1 1 calc R U . . .
C68 C -0.0457(3) 0.2325(2) 0.26320(18) 0.0665(14) Uani 1 1 d . . . . .
H68 H -0.0632 0.2637 0.2500 0.080 Uiso 1 1 calc R U . . .
C69 C -0.0796(2) 0.1838(2) 0.25727(18) 0.0644(14) Uani 1 1 d . . . . .
C70 C -0.1379(3) 0.1878(3) 0.2402(3) 0.098(2) Uani 1 1 d . . . . .
H70 H -0.1534 0.2220 0.2332 0.118 Uiso 1 1 calc R U . . .
C71 C -0.1738(3) 0.1441(4) 0.2333(3) 0.124(3) Uani 1 1 d . . . . .
H71 H -0.2134 0.1485 0.2223 0.148 Uiso 1 1 calc R U . . .
C72 C -0.1522(2) 0.0956(3) 0.2421(3) 0.095(2) Uani 1 1 d . . . . .
H72 H -0.1763 0.0654 0.2362 0.114 Uiso 1 1 calc R U . . .
C73 C -0.0947(2) 0.0889(2) 0.25974(19) 0.0630(13) Uani 1 1 d . . . . .
H73 H -0.0807 0.0543 0.2669 0.076 Uiso 1 1 calc R U . . .
C74 C -0.05740(18) 0.13246(19) 0.26717(15) 0.0481(10) Uani 1 1 d . . . . .
C75 C -0.1627(4) 0.2017(3) 0.4000(3) 0.115(3) Uani 1 1 d . . . . .
H75A H -0.1201 0.2078 0.4057 0.138 Uiso 1 1 calc R U . . .
H75B H -0.1716 0.2102 0.3644 0.138 Uiso 1 1 calc R U . . .
C76 C -0.2006(6) 0.2398(4) 0.4365(4) 0.166(4) Uani 1 1 d . . . . .
H76A H -0.2423 0.2382 0.4269 0.248 Uiso 1 1 calc R U . . .
H76B H -0.1865 0.2764 0.4332 0.248 Uiso 1 1 calc R U . . .
H76C H -0.1961 0.2281 0.4715 0.248 Uiso 1 1 calc R U . . .
C77 C -0.2411(3) 0.1283(3) 0.4066(3) 0.100(2) Uani 1 1 d . . . . .
H77A H -0.2472 0.0904 0.4146 0.120 Uiso 1 1 calc R U . . .
H77B H -0.2621 0.1492 0.4326 0.120 Uiso 1 1 calc R U . . .
C78 C -0.2681(4) 0.1388(3) 0.3591(3) 0.118(3) Uani 1 1 d . . . . .
H78A H -0.2654 0.1768 0.3517 0.177 Uiso 1 1 calc R U . . .
H78B H -0.3096 0.1282 0.3603 0.177 Uiso 1 1 calc R U . . .
H78C H -0.2478 0.1187 0.3327 0.177 Uiso 1 1 calc R U . . .
C79 C -0.1365(4) 0.1115(4) 0.3819(3) 0.122(3) Uani 1 1 d . . . . .
H79A H -0.0969 0.1263 0.3890 0.147 Uiso 1 1 calc R U . . .
H79B H -0.1450 0.1181 0.3458 0.147 Uiso 1 1 calc R U . . .
C80 C -0.1344(4) 0.0507(4) 0.3906(3) 0.125(3) Uani 1 1 d . . . . .
H80A H -0.1195 0.0434 0.4246 0.187 Uiso 1 1 calc R U . . .
H80B H -0.1082 0.0343 0.3657 0.187 Uiso 1 1 calc R U . . .
H80C H -0.1741 0.0359 0.3871 0.187 Uiso 1 1 calc R U . . .
C83 C 0.1303(3) 0.1512(2) 0.5479(2) 0.0795(17) Uani 1 1 d . . . . .
C84 C 0.1412(3) 0.1713(2) 0.5000(2) 0.0815(17) Uani 1 1 d . . . . .
H84A H 0.1049 0.1703 0.4801 0.122 Uiso 1 1 calc R U . . .
H84B H 0.1715 0.1498 0.4834 0.122 Uiso 1 1 calc R U . . .
H84C H 0.1550 0.2080 0.5027 0.122 Uiso 1 1 calc R U . . .
C85 C 0.1906(4) -0.0922(3) 0.4457(3) 0.098(2) Uani 1 1 d . . . . .
C86 C 0.1794(4) -0.0679(2) 0.3996(2) 0.101(3) Uani 1 1 d . . . . .
H86A H 0.1608 -0.0934 0.3767 0.151 Uiso 1 1 calc R U . . .
H86B H 0.2166 -0.0555 0.3849 0.151 Uiso 1 1 calc R U . . .
H86C H 0.1529 -0.0376 0.4047 0.151 Uiso 1 1 calc R U . . .
N4 N 0.1359(4) -0.1945(3) 0.1613(3) 0.120(2) Uani 1 1 d . . . . .
C81 C 0.1153(3) -0.1527(3) 0.1606(2) 0.0776(16) Uani 1 1 d . . . . .
C82 C 0.0871(3) -0.1015(2) 0.1622(2) 0.0761(16) Uani 1 1 d . . . . .
H82A H 0.0613 -0.0975 0.1328 0.114 Uiso 1 1 calc R U . . .
H82B H 0.1172 -0.0736 0.1618 0.114 Uiso 1 1 calc R U . . .
H82C H 0.0636 -0.0986 0.1931 0.114 Uiso 1 1 calc R U . . .
N1 N 0.02850(17) 0.16176(14) 0.16363(12) 0.0460(8) Uani 1 1 d . . . . .
N2 N 0.0047(2) 0.23833(14) 0.28396(13) 0.0566(10) Uani 1 1 d . . . . .
N3 N -0.1783(2) 0.1396(3) 0.4110(2) 0.117(3) Uani 1 1 d . . . . .
H3A H -0.1677 0.1331 0.4471 0.141 Uiso 1 1 calc R U . . .
N5 N 0.1199(5) 0.1343(3) 0.5863(3) 0.169(4) Uani 1 1 d . . . . .
N6 N 0.1955(4) -0.1126(3) 0.4837(3) 0.130(3) Uani 1 1 d . . . . .
O1 O -0.00053(14) 0.00805(11) 0.21608(10) 0.0490(7) Uani 1 1 d . . . . .
O2 O 0.00974(15) 0.06518(11) 0.12641(10) 0.0514(7) Uani 1 1 d . . . . .
O3 O 0.13054(14) 0.05072(12) 0.17231(10) 0.0516(7) Uani 1 1 d . . . . .
O4 O 0.10119(13) 0.03096(10) 0.28113(9) 0.0426(6) Uani 1 1 d . . . . .
H4 H 0.1029 0.0467 0.3115 0.086(18) Uiso 1 1 d R . . . .
O5 O 0.06711(15) 0.26686(11) 0.36586(12) 0.0561(8) Uani 1 1 d . . . . .
O6 O 0.15299(14) 0.18722(12) 0.36379(11) 0.0539(7) Uani 1 1 d . . . . .
O7 O 0.01032(14) 0.16479(10) 0.39937(11) 0.0492(7) Uani 1 1 d . . . . .
O8 O 0.09286(12) 0.08321(10) 0.35615(9) 0.0387(6) Uani 1 1 d . . . . .
O9 O -0.00208(12) 0.12328(11) 0.28170(10) 0.0420(6) Uani 1 1 d . . . . .
O10 O 0.10804(12) 0.15328(10) 0.24855(10) 0.0410(6) Uani 1 1 d . . . . .
Sm1 Sm 0.05527(2) 0.07861(2) 0.21479(2) 0.04049(8) Uani 1 1 d . . . . .
Sm2 Sm 0.06606(2) 0.17078(2) 0.33274(2) 0.03956(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.320(5) . ?
C1 C2 1.412(6) . ?
C1 C6 1.421(6) . ?
C2 C3 1.407(7) . ?
C2 C28 1.510(6) . ?
C3 C4 1.377(7) . ?
C4 C5 1.389(7) . ?
C5 C6 1.382(6) . ?
C6 C7 1.516(6) . ?
C7 C8 1.517(7) . ?
C8 C9 1.394(7) . ?
C8 C13 1.402(7) . ?
C9 C10 1.374(8) . ?
C10 C11 1.377(8) . ?
C11 C12 1.391(7) . ?
C12 C13 1.388(7) . ?
C12 C14 1.531(7) . ?
C13 O2 1.414(5) . ?
C14 C15 1.509(7) . ?
C15 C16 1.385(7) . ?
C15 C20 1.401(6) . ?
C16 C17 1.382(9) . ?
C17 C18 1.399(8) . ?
C18 C19 1.389(7) . ?
C19 C20 1.418(7) . ?
C19 C21 1.507(7) . ?
C20 O3 1.319(5) . ?
C21 C22 1.524(6) . ?
C22 C23 1.400(6) . ?
C22 C27 1.403(6) . ?
C23 C24 1.385(7) . ?
C24 C25 1.376(7) . ?
C25 C26 1.398(6) . ?
C26 C27 1.410(6) . ?
C26 C28 1.517(6) . ?
C27 O4 1.374(5) . ?
C29 O2 1.443(5) . ?
C29 C30 1.516(7) . ?
C30 N1 1.465(6) . ?
C31 N1 1.280(6) . ?
C31 C32 1.443(6) . ?
C32 C33 1.416(6) . ?
C32 C37 1.419(6) . ?
C33 C34 1.366(8) . ?
C34 C35 1.381(8) . ?
C35 C36 1.387(6) . ?
C36 C37 1.415(6) . ?
C37 O10 1.330(5) . ?
C38 C43 1.395(7) . ?
C38 C39 1.397(8) . ?
C38 O5 1.406(6) . ?
C39 C40 1.393(7) . ?
C39 C65 1.532(7) . ?
C40 C41 1.377(8) . ?
C41 C42 1.391(8) . ?
C42 C43 1.400(7) . ?
C43 C44 1.523(7) . ?
C44 C45 1.524(6) . ?
C45 C46 1.400(6) . ?
C45 C50 1.406(6) . ?
C46 C47 1.370(7) . ?
C47 C48 1.396(7) . ?
C48 C49 1.391(6) . ?
C49 C50 1.410(5) . ?
C49 C51 1.520(5) . ?
C50 O7 1.315(5) . ?
C51 C52 1.511(6) . ?
C52 C53 1.393(5) . ?
C52 C57 1.416(6) . ?
C53 C54 1.382(7) . ?
C54 C55 1.376(7) . ?
C55 C56 1.408(6) . ?
C56 C57 1.403(6) . ?
C56 C58 1.513(7) . ?
C57 O8 1.371(4) . ?
C58 C59 1.507(7) . ?
C59 C60 1.392(7) . ?
C59 C64 1.416(8) . ?
C60 C61 1.374(10) . ?
C61 C62 1.357(13) . ?
C62 C63 1.388(9) . ?
C63 C64 1.415(7) . ?
C63 C65 1.492(9) . ?
C64 O6 1.311(6) . ?
C66 O5 1.460(6) . ?
C66 C67 1.499(7) . ?
C67 N2 1.472(7) . ?
C68 N2 1.277(7) . ?
C68 C69 1.458(8) . ?
C69 C70 1.401(8) . ?
C69 C74 1.414(7) . ?
C70 C71 1.382(12) . ?
C71 C72 1.340(11) . ?
C72 C73 1.396(7) . ?
C73 C74 1.401(7) . ?
C74 O9 1.333(5) . ?
C75 C76 1.614(13) . ?
C75 N3 1.631(10) . ?
C77 C78 1.426(9) . ?
C77 N3 1.458(8) . ?
C79 N3 1.416(11) . ?
C79 C80 1.553(12) . ?
C83 N5 1.130(9) . ?
C83 C84 1.390(9) . ?
C85 N6 1.137(8) . ?
C85 C86 1.393(9) . ?
N4 C81 1.154(9) . ?
C81 C82 1.443(9) . ?
N1 Sm1 2.571(3) . ?
N2 Sm2 2.553(4) . ?
O1 Sm1 2.185(3) . ?
O2 Sm1 2.585(3) . ?
O3 Sm1 2.164(3) . ?
O4 Sm1 2.373(3) . ?
O5 Sm2 2.578(3) . ?
O6 Sm2 2.177(3) . ?
O7 Sm2 2.179(3) . ?
O8 Sm2 2.374(2) . ?
O9 Sm2 2.379(3) . ?
O9 Sm1 2.473(3) . ?
O10 Sm1 2.405(3) . ?
O10 Sm2 2.469(3) . ?
Sm1 Sm2 3.9066(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
O1 C1 C2 120.1(4) . . ?
O1 C1 C6 119.6(4) . . ?
C2 C1 C6 120.1(4) . . ?
C3 C2 C1 118.0(4) . . ?
C3 C2 C28 123.0(4) . . ?
C1 C2 C28 119.0(4) . . ?
C4 C3 C2 121.7(4) . . ?
C3 C4 C5 119.8(4) . . ?
C6 C5 C4 121.0(5) . . ?
C5 C6 C1 119.3(4) . . ?
C5 C6 C7 122.0(4) . . ?
C1 C6 C7 118.6(4) . . ?
C6 C7 C8 114.5(4) . . ?
C9 C8 C13 117.2(5) . . ?
C9 C8 C7 119.9(5) . . ?
C13 C8 C7 122.9(4) . . ?
C10 C9 C8 120.9(5) . . ?
C9 C10 C11 120.4(5) . . ?
C10 C11 C12 121.1(5) . . ?
C13 C12 C11 117.3(5) . . ?
C13 C12 C14 123.6(4) . . ?
C11 C12 C14 119.0(5) . . ?
C12 C13 C8 122.7(4) . . ?
C12 C13 O2 119.6(4) . . ?
C8 C13 O2 117.6(4) . . ?
C15 C14 C12 111.5(4) . . ?
C16 C15 C20 119.5(5) . . ?
C16 C15 C14 120.8(5) . . ?
C20 C15 C14 119.5(4) . . ?
C17 C16 C15 121.3(5) . . ?
C16 C17 C18 119.2(5) . . ?
C19 C18 C17 121.3(6) . . ?
C18 C19 C20 118.5(5) . . ?
C18 C19 C21 121.2(5) . . ?
C20 C19 C21 120.2(4) . . ?
O3 C20 C15 119.6(5) . . ?
O3 C20 C19 120.2(4) . . ?
C15 C20 C19 120.1(4) . . ?
C19 C21 C22 111.9(4) . . ?
C23 C22 C27 118.3(4) . . ?
C23 C22 C21 119.8(4) . . ?
C27 C22 C21 121.8(4) . . ?
C24 C23 C22 121.3(4) . . ?
C25 C24 C23 119.4(4) . . ?
C24 C25 C26 121.9(4) . . ?
C25 C26 C27 117.8(4) . . ?
C25 C26 C28 119.5(4) . . ?
C27 C26 C28 122.7(4) . . ?
O4 C27 C22 118.7(4) . . ?
O4 C27 C26 120.2(4) . . ?
C22 C27 C26 121.0(4) . . ?
C2 C28 C26 114.0(3) . . ?
O2 C29 C30 106.3(3) . . ?
N1 C30 C29 109.2(4) . . ?
N1 C31 C32 127.1(4) . . ?
C33 C32 C37 119.1(4) . . ?
C33 C32 C31 115.9(4) . . ?
C37 C32 C31 124.9(4) . . ?
C34 C33 C32 122.0(5) . . ?
C33 C34 C35 119.4(4) . . ?
C34 C35 C36 120.4(5) . . ?
C35 C36 C37 121.8(5) . . ?
O10 C37 C36 120.2(4) . . ?
O10 C37 C32 122.6(4) . . ?
C36 C37 C32 117.2(4) . . ?
C43 C38 C39 122.2(5) . . ?
C43 C38 O5 119.4(5) . . ?
C39 C38 O5 118.4(4) . . ?
C40 C39 C38 118.0(5) . . ?
C40 C39 C65 119.2(5) . . ?
C38 C39 C65 122.7(5) . . ?
C41 C40 C39 121.5(5) . . ?
C40 C41 C42 119.3(5) . . ?
C41 C42 C43 121.5(5) . . ?
C38 C43 C42 117.4(5) . . ?
C38 C43 C44 124.1(4) . . ?
C42 C43 C44 118.5(4) . . ?
C43 C44 C45 110.9(4) . . ?
C46 C45 C50 118.9(4) . . ?
C46 C45 C44 122.6(4) . . ?
C50 C45 C44 118.4(4) . . ?
C47 C46 C45 121.3(4) . . ?
C46 C47 C48 119.7(4) . . ?
C49 C48 C47 121.1(4) . . ?
C48 C49 C50 118.9(4) . . ?
C48 C49 C51 121.7(4) . . ?
C50 C49 C51 119.4(3) . . ?
O7 C50 C45 119.0(4) . . ?
O7 C50 C49 120.7(3) . . ?
C45 C50 C49 120.2(4) . . ?
C52 C51 C49 112.0(3) . . ?
C53 C52 C57 117.7(4) . . ?
C53 C52 C51 119.7(4) . . ?
C57 C52 C51 122.6(3) . . ?
C54 C53 C52 121.9(4) . . ?
C55 C54 C53 119.3(4) . . ?
C54 C55 C56 121.9(4) . . ?
C57 C56 C55 117.4(4) . . ?
C57 C56 C58 123.4(4) . . ?
C55 C56 C58 119.1(4) . . ?
O8 C57 C56 120.1(4) . . ?
O8 C57 C52 118.5(3) . . ?
C56 C57 C52 121.4(4) . . ?
C59 C58 C56 112.7(4) . . ?
C60 C59 C64 117.7(5) . . ?
C60 C59 C58 123.4(6) . . ?
C64 C59 C58 118.9(4) . . ?
C61 C60 C59 121.5(8) . . ?
C62 C61 C60 120.7(6) . . ?
C61 C62 C63 121.2(6) . . ?
C62 C63 C64 118.6(6) . . ?
C62 C63 C65 123.0(5) . . ?
C64 C63 C65 118.4(5) . . ?
O6 C64 C63 120.0(5) . . ?
O6 C64 C59 119.8(4) . . ?
C63 C64 C59 120.2(5) . . ?
C63 C65 C39 113.2(5) . . ?
O5 C66 C67 106.1(4) . . ?
N2 C67 C66 109.8(4) . . ?
N2 C68 C69 128.0(4) . . ?
C70 C69 C74 117.6(6) . . ?
C70 C69 C68 118.2(6) . . ?
C74 C69 C68 124.3(4) . . ?
C71 C70 C69 122.8(7) . . ?
C72 C71 C70 119.4(6) . . ?
C71 C72 C73 120.6(7) . . ?
C72 C73 C74 121.3(6) . . ?
O9 C74 C73 118.3(4) . . ?
O9 C74 C69 123.3(4) . . ?
C73 C74 C69 118.4(4) . . ?
C76 C75 N3 110.4(7) . . ?
C78 C77 N3 117.0(7) . . ?
N3 C79 C80 115.7(7) . . ?
N5 C83 C84 178.0(10) . . ?
N6 C85 C86 175.1(10) . . ?
N4 C81 C82 176.4(7) . . ?
C31 N1 C30 117.6(4) . . ?
C31 N1 Sm1 129.5(3) . . ?
C30 N1 Sm1 112.5(3) . . ?
C68 N2 C67 118.9(4) . . ?
C68 N2 Sm2 129.0(3) . . ?
C67 N2 Sm2 111.8(3) . . ?
C79 N3 C77 120.8(8) . . ?
C79 N3 C75 103.7(6) . . ?
C77 N3 C75 112.7(6) . . ?
C1 O1 Sm1 165.6(3) . . ?
C13 O2 C29 112.4(3) . . ?
C13 O2 Sm1 124.2(2) . . ?
C29 O2 Sm1 123.2(2) . . ?
C20 O3 Sm1 158.4(3) . . ?
C27 O4 Sm1 124.8(2) . . ?
C38 O5 C66 113.8(3) . . ?
C38 O5 Sm2 123.4(2) . . ?
C66 O5 Sm2 121.6(3) . . ?
C64 O6 Sm2 172.2(3) . . ?
C50 O7 Sm2 160.8(3) . . ?
C57 O8 Sm2 124.1(2) . . ?
C74 O9 Sm2 133.5(3) . . ?
C74 O9 Sm1 111.5(2) . . ?
Sm2 O9 Sm1 107.23(10) . . ?
C37 O10 Sm1 132.5(2) . . ?
C37 O10 Sm2 115.1(2) . . ?
Sm1 O10 Sm2 106.56(10) . . ?
O3 Sm1 O1 101.57(11) . . ?
O3 Sm1 O4 82.83(10) . . ?
O1 Sm1 O4 80.22(10) . . ?
O3 Sm1 O10 93.20(10) . . ?
O1 Sm1 O10 157.05(9) . . ?
O4 Sm1 O10 84.37(9) . . ?
O3 Sm1 O9 159.63(10) . . ?
O1 Sm1 O9 93.16(10) . . ?
O4 Sm1 O9 85.94(9) . . ?
O10 Sm1 O9 68.76(9) . . ?
O3 Sm1 N1 100.18(11) . . ?
O1 Sm1 N1 122.41(11) . . ?
O4 Sm1 N1 155.34(10) . . ?
O10 Sm1 N1 71.06(10) . . ?
O9 Sm1 N1 83.29(10) . . ?
O3 Sm1 O2 78.47(11) . . ?
O1 Sm1 O2 71.08(9) . . ?
O4 Sm1 O2 141.47(9) . . ?
O10 Sm1 O2 129.76(9) . . ?
O9 Sm1 O2 120.06(10) . . ?
N1 Sm1 O2 62.19(10) . . ?
O3 Sm1 Sm2 124.15(8) . . ?
O1 Sm1 Sm2 120.58(7) . . ?
O4 Sm1 Sm2 71.31(6) . . ?
O10 Sm1 Sm2 37.28(6) . . ?
O9 Sm1 Sm2 35.57(6) . . ?
N1 Sm1 Sm2 87.27(7) . . ?
O2 Sm1 Sm2 146.09(7) . . ?
O6 Sm2 O7 103.40(12) . . ?
O6 Sm2 O8 81.15(10) . . ?
O7 Sm2 O8 82.64(10) . . ?
O6 Sm2 O9 154.16(11) . . ?
O7 Sm2 O9 92.86(10) . . ?
O8 Sm2 O9 81.19(9) . . ?
O6 Sm2 O10 91.55(10) . . ?
O7 Sm2 O10 161.07(10) . . ?
O8 Sm2 O10 88.38(9) . . ?
O9 Sm2 O10 69.23(9) . . ?
O6 Sm2 N2 123.98(13) . . ?
O7 Sm2 N2 98.10(12) . . ?
O8 Sm2 N2 153.31(11) . . ?
O9 Sm2 N2 72.12(11) . . ?
O10 Sm2 N2 82.59(10) . . ?
O6 Sm2 O5 71.56(11) . . ?
O7 Sm2 O5 78.10(10) . . ?
O8 Sm2 O5 141.55(9) . . ?
O9 Sm2 O5 132.33(10) . . ?
O10 Sm2 O5 118.23(9) . . ?
N2 Sm2 O5 63.28(12) . . ?
O6 Sm2 Sm1 118.25(8) . . ?
O7 Sm2 Sm1 124.92(8) . . ?
O8 Sm2 Sm1 70.85(6) . . ?
O9 Sm2 Sm1 37.20(7) . . ?
O10 Sm2 Sm1 36.16(6) . . ?
N2 Sm2 Sm1 87.52(8) . . ?
O5 Sm2 Sm1 146.42(7) . . ?

_refine_diff_density_max         1.995
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.131

####################################################################### 
# 
# 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_gd2
_database_code_depnum_ccdc_archive 'CCDC 1880059'
loop_
_audit_author_name
_audit_author_address
'Berthold Kersting'
;University of  Leipzig
Germany
;
_audit_update_record             
;
2019-02-13 deposited with the CCDC.	2019-02-22 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT919_gd2                 
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          4 Check 
RESPONSE: Due to large unit cell a small mask had to
be used \ during integration (A = 6, B = 0, EMS = 0.006) 
to avoid overlaps. This results in the outer regions of the most 
intense reflections being cut off.
;

_vrf_PLAT934_gd2                 
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          4 Check 
RESPONSE: ...
due to large unit cell a small mask had to
be used \ during integration (A = 6, B = 0, EMS = 0.006) 
to avoid overlaps. This results in the outer regions of the most 
intense reflections being cut off.
;

#end Validation Reply Form



_audit_creation_method           SHELXL-2014/8
_shelx_SHELXL_version_number     2014/8
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C86 H84 Gd2 N6 O10'
_chemical_formula_weight         1676.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   22.7767(8)
_cell_length_b                   25.1415(11)
_cell_length_c                   26.5012(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     15175.7(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    24523
_cell_measurement_theta_min      5.6
_cell_measurement_theta_max      25.6

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_F_000             6800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.797
_shelx_estimated_absorpt_T_min   0.589
_shelx_estimated_absorpt_T_max   0.738
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_process_details   
;
Busing, W. R. & Levy, H. A. (1957) Acta Cryst. 10, 180-182. 
and Coppens, P., Leiserowitz, L. & Rabinovich, D. (1965) 
Acta Cryst. 1965, 1035-1038.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51122
_diffrn_reflns_av_unetI/netI     0.0622
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.778
_diffrn_reflns_theta_max         27.364
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             16712
_reflns_number_gt                10439
_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       'STOE IPDS software'
_computing_cell_refinement       'STOE IPDS software'
_computing_data_reduction        'STOE X-AREA'
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_computing_molecular_graphics    ' ORTEP 3 for Windows '
_computing_publication_material  ' POVRAY 3.1 for Windows '

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0850P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/8 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00220(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         16712
_refine_ls_number_parameters     942
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1325
_refine_ls_wR_factor_gt          0.1160
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_restrained_S_all      0.877
_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
C1 C -0.0397(3) -0.0281(2) 0.2265(2) 0.0510(13) Uani 1 1 d . . . . .
C2 C -0.0388(3) -0.0549(2) 0.2739(2) 0.0497(13) Uani 1 1 d . . . . .
C3 C -0.0833(3) -0.0922(2) 0.2834(3) 0.0607(16) Uani 1 1 d . . . . .
H3 H -0.0833 -0.1109 0.3146 0.073 Uiso 1 1 calc R U . . .
C4 C -0.1273(3) -0.1026(2) 0.2485(3) 0.0656(17) Uani 1 1 d . . . . .
H4A H -0.1566 -0.1285 0.2556 0.079 Uiso 1 1 calc R U . . .
C5 C -0.1282(3) -0.0749(2) 0.2035(3) 0.0619(15) Uani 1 1 d . . . . .
H5 H -0.1586 -0.0819 0.1799 0.074 Uiso 1 1 calc R U . . .
C6 C -0.0861(3) -0.0374(2) 0.1918(2) 0.0559(14) Uani 1 1 d . . . . .
C7 C -0.0881(3) -0.0050(3) 0.1437(2) 0.0631(16) Uani 1 1 d . . . . .
H7A H -0.1263 -0.0114 0.1269 0.076 Uiso 1 1 calc R U . . .
H7B H -0.0863 0.0332 0.1527 0.076 Uiso 1 1 calc R U . . .
C8 C -0.0394(3) -0.0169(2) 0.1065(2) 0.0603(15) Uani 1 1 d . . . . .
C9 C -0.0410(4) -0.0629(3) 0.0769(3) 0.0703(19) Uani 1 1 d . . . . .
H9 H -0.0740 -0.0860 0.0791 0.084 Uiso 1 1 calc R U . . .
C10 C 0.0044(4) -0.0755(3) 0.0447(3) 0.0732(19) Uani 1 1 d . . . . .
H10 H 0.0022 -0.1069 0.0248 0.088 Uiso 1 1 calc R U . . .
C11 C 0.0527(4) -0.0431(3) 0.0412(2) 0.0709(19) Uani 1 1 d . . . . .
H11 H 0.0834 -0.0522 0.0185 0.085 Uiso 1 1 calc R U . . .
C12 C 0.0580(3) 0.0029(2) 0.0701(2) 0.0598(15) Uani 1 1 d . . . . .
C13 C 0.0100(3) 0.0162(2) 0.1004(2) 0.0570(15) Uani 1 1 d . . . . .
C14 C 0.1148(3) 0.0349(2) 0.0681(2) 0.0666(17) Uani 1 1 d . . . . .
H14A H 0.1275 0.0388 0.0326 0.080 Uiso 1 1 calc R U . . .
H14B H 0.1078 0.0709 0.0820 0.080 Uiso 1 1 calc R U . . .
C15 C 0.1629(3) 0.0078(2) 0.0983(2) 0.0603(15) Uani 1 1 d . . . . .
C16 C 0.2002(4) -0.0285(3) 0.0757(3) 0.077(2) Uani 1 1 d . . . . .
H16 H 0.1973 -0.0350 0.0404 0.092 Uiso 1 1 calc R U . . .
C17 C 0.2417(4) -0.0556(3) 0.1039(3) 0.085(2) Uani 1 1 d . . . . .
H17 H 0.2672 -0.0802 0.0879 0.103 Uiso 1 1 calc R U . . .
C18 C 0.2459(3) -0.0467(3) 0.1548(3) 0.0700(18) Uani 1 1 d . . . . .
H18 H 0.2747 -0.0655 0.1737 0.084 Uiso 1 1 calc R U . . .
C19 C 0.2091(3) -0.0109(2) 0.1799(3) 0.0587(15) Uani 1 1 d . . . . .
C20 C 0.1672(3) 0.0172(2) 0.1498(2) 0.0571(15) Uani 1 1 d . . . . .
C21 C 0.2102(3) -0.0045(2) 0.2359(3) 0.0591(15) Uani 1 1 d . . . . .
H21A H 0.2010 0.0329 0.2446 0.071 Uiso 1 1 calc R U . . .
H21B H 0.2502 -0.0124 0.2485 0.071 Uiso 1 1 calc R U . . .
C22 C 0.1665(3) -0.0410(2) 0.2623(2) 0.0500(13) Uani 1 1 d . . . . .
C23 C 0.1787(3) -0.0955(2) 0.2651(2) 0.0586(15) Uani 1 1 d . . . . .
H23 H 0.2153 -0.1086 0.2535 0.070 Uiso 1 1 calc R U . . .
C24 C 0.1375(3) -0.1307(2) 0.2849(2) 0.0593(15) Uani 1 1 d . . . . .
H24 H 0.1468 -0.1674 0.2879 0.071 Uiso 1 1 calc R U . . .
C25 C 0.0836(3) -0.1122(2) 0.3000(2) 0.0548(14) Uani 1 1 d . . . . .
H25 H 0.0552 -0.1367 0.3122 0.066 Uiso 1 1 calc R U . . .
C26 C 0.0693(3) -0.0581(2) 0.2979(2) 0.0500(13) Uani 1 1 d . . . . .
C27 C 0.1127(3) -0.02269(19) 0.2802(2) 0.0472(12) Uani 1 1 d . . . . .
C28 C 0.0073(3) -0.0403(2) 0.3117(2) 0.0541(14) Uani 1 1 d . . . . .
H28A H -0.0033 -0.0563 0.3446 0.065 Uiso 1 1 calc R U . . .
H28B H 0.0073 -0.0012 0.3161 0.065 Uiso 1 1 calc R U . . .
C29 C -0.0128(3) 0.1082(2) 0.0971(2) 0.0591(15) Uani 1 1 d . . . . .
H29A H -0.0499 0.0973 0.0805 0.071 Uiso 1 1 calc R U . . .
H29B H 0.0157 0.1189 0.0707 0.071 Uiso 1 1 calc R U . . .
C30 C -0.0237(3) 0.1538(2) 0.1333(2) 0.0616(15) Uani 1 1 d . . . . .
H30A H -0.0318 0.1869 0.1143 0.074 Uiso 1 1 calc R U . . .
H30B H -0.0582 0.1459 0.1548 0.074 Uiso 1 1 calc R U . . .
C31 C 0.0577(3) 0.2044(2) 0.1597(2) 0.0536(14) Uani 1 1 d . . . . .
H31 H 0.0420 0.2296 0.1366 0.064 Uiso 1 1 calc R U . . .
C32 C 0.1115(3) 0.2192(2) 0.1847(2) 0.0513(13) Uani 1 1 d . . . . .
C33 C 0.1411(3) 0.2642(2) 0.1642(3) 0.0643(16) Uani 1 1 d . . . . .
H33 H 0.1248 0.2821 0.1360 0.077 Uiso 1 1 calc R U . . .
C34 C 0.1932(3) 0.2821(2) 0.1849(3) 0.073(2) Uani 1 1 d . . . . .
H34 H 0.2132 0.3115 0.1703 0.087 Uiso 1 1 calc R U . . .
C35 C 0.2158(3) 0.2572(2) 0.2267(3) 0.0664(17) Uani 1 1 d . . . . .
H35 H 0.2515 0.2696 0.2410 0.080 Uiso 1 1 calc R U . . .
C36 C 0.1871(3) 0.2141(2) 0.2482(2) 0.0575(14) Uani 1 1 d . . . . .
H36 H 0.2031 0.1981 0.2776 0.069 Uiso 1 1 calc R U . . .
C37 C 0.1346(2) 0.19342(19) 0.2275(2) 0.0460(12) Uani 1 1 d . . . . .
C38 C 0.0851(3) 0.2807(2) 0.4143(2) 0.0578(15) Uani 1 1 d . . . . .
C39 C 0.1437(3) 0.2954(2) 0.4210(3) 0.0684(18) Uani 1 1 d . . . . .
C40 C 0.1605(3) 0.3133(3) 0.4688(3) 0.0728(19) Uani 1 1 d . . . . .
H40 H 0.1999 0.3244 0.4742 0.087 Uiso 1 1 calc R U . . .
C41 C 0.1214(4) 0.3150(3) 0.5082(3) 0.076(2) Uani 1 1 d . . . . .
H41 H 0.1333 0.3283 0.5402 0.092 Uiso 1 1 calc R U . . .
C42 C 0.0640(3) 0.2971(2) 0.5007(3) 0.0628(16) Uani 1 1 d . . . . .
H42 H 0.0374 0.2968 0.5283 0.075 Uiso 1 1 calc R U . . .
C43 C 0.0449(3) 0.2798(2) 0.4539(2) 0.0568(15) Uani 1 1 d . . . . .
C44 C -0.0177(3) 0.2591(2) 0.4491(3) 0.0599(15) Uani 1 1 d . . . . .
H44A H -0.0282 0.2561 0.4129 0.072 Uiso 1 1 calc R U . . .
H44B H -0.0451 0.2845 0.4651 0.072 Uiso 1 1 calc R U . . .
C45 C -0.0235(3) 0.2044(2) 0.4745(2) 0.0544(14) Uani 1 1 d . . . . .
C46 C -0.0427(3) 0.1982(3) 0.5241(3) 0.0669(17) Uani 1 1 d . . . . .
H46 H -0.0549 0.2285 0.5428 0.080 Uiso 1 1 calc R U . . .
C47 C -0.0443(3) 0.1488(3) 0.5464(3) 0.077(2) Uani 1 1 d . . . . .
H47 H -0.0574 0.1449 0.5803 0.093 Uiso 1 1 calc R U . . .
C48 C -0.0262(3) 0.1042(3) 0.5186(3) 0.0684(17) Uani 1 1 d . . . . .
H48 H -0.0270 0.0702 0.5342 0.082 Uiso 1 1 calc R U . . .
C49 C -0.0074(2) 0.1084(2) 0.4691(2) 0.0489(12) Uani 1 1 d . . . . .
C50 C -0.0062(2) 0.1591(2) 0.4462(2) 0.0495(12) Uani 1 1 d . . . . .
C51 C 0.0153(3) 0.0611(2) 0.4399(2) 0.0499(13) Uani 1 1 d . . . . .
H51A H -0.0027 0.0283 0.4537 0.060 Uiso 1 1 calc R U . . .
H51B H 0.0029 0.0644 0.4042 0.060 Uiso 1 1 calc R U . . .
C52 C 0.0809(3) 0.0559(2) 0.4419(2) 0.0479(12) Uani 1 1 d . . . . .
C53 C 0.1083(3) 0.0386(2) 0.4865(2) 0.0558(14) Uani 1 1 d . . . . .
H53 H 0.0846 0.0280 0.5142 0.067 Uiso 1 1 calc R U . . .
C54 C 0.1686(3) 0.0364(2) 0.4911(2) 0.0639(17) Uani 1 1 d . . . . .
H54 H 0.1860 0.0229 0.5210 0.077 Uiso 1 1 calc R U . . .
C55 C 0.2033(3) 0.0539(3) 0.4519(3) 0.0661(17) Uani 1 1 d . . . . .
H55 H 0.2448 0.0539 0.4558 0.079 Uiso 1 1 calc R U . . .
C56 C 0.1788(3) 0.0719(2) 0.4058(2) 0.0547(14) Uani 1 1 d . . . . .
C57 C 0.1175(2) 0.06996(18) 0.4010(2) 0.0449(11) Uani 1 1 d . . . . .
C58 C 0.2193(3) 0.0940(2) 0.3658(3) 0.0605(16) Uani 1 1 d . . . . .
H58A H 0.1974 0.0969 0.3336 0.073 Uiso 1 1 calc R U . . .
H58B H 0.2521 0.0687 0.3605 0.073 Uiso 1 1 calc R U . . .
C59 C 0.2442(3) 0.1480(3) 0.3794(3) 0.0651(17) Uani 1 1 d . . . . .
C60 C 0.3016(3) 0.1552(4) 0.3953(4) 0.112(4) Uani 1 1 d . . . . .
H60 H 0.3266 0.1251 0.3984 0.135 Uiso 1 1 calc R U . . .
C61 C 0.3234(4) 0.2051(5) 0.4066(5) 0.143(5) Uani 1 1 d . . . . .
H61 H 0.3627 0.2089 0.4182 0.171 Uiso 1 1 calc R U . . .
C62 C 0.2877(4) 0.2498(4) 0.4011(4) 0.111(4) Uani 1 1 d . . . . .
H62 H 0.3031 0.2842 0.4080 0.134 Uiso 1 1 calc R U . . .
C63 C 0.2300(3) 0.2443(3) 0.3858(3) 0.073(2) Uani 1 1 d . . . . .
C64 C 0.2071(3) 0.1930(3) 0.3766(2) 0.0611(15) Uani 1 1 d . . . . .
C65 C 0.1895(4) 0.2916(3) 0.3790(3) 0.079(2) Uani 1 1 d . . . . .
H65A H 0.1692 0.2887 0.3461 0.094 Uiso 1 1 calc R U . . .
H65B H 0.2131 0.3247 0.3786 0.094 Uiso 1 1 calc R U . . .
C66 C 0.0373(4) 0.3096(2) 0.3377(2) 0.0704(19) Uani 1 1 d . . . . .
H66A H 0.0609 0.3426 0.3392 0.085 Uiso 1 1 calc R U . . .
H66B H -0.0018 0.3168 0.3525 0.085 Uiso 1 1 calc R U . . .
C67 C 0.0314(4) 0.2908(2) 0.2847(3) 0.0725(19) Uani 1 1 d . . . . .
H67A H 0.0062 0.3157 0.2655 0.087 Uiso 1 1 calc R U . . .
H67B H 0.0705 0.2901 0.2684 0.087 Uiso 1 1 calc R U . . .
C68 C -0.0452(3) 0.2310(3) 0.2632(3) 0.0685(18) Uani 1 1 d . . . . .
H68 H -0.0629 0.2622 0.2498 0.082 Uiso 1 1 calc R U . . .
C69 C -0.0786(3) 0.1819(3) 0.2584(2) 0.0639(16) Uani 1 1 d . . . . .
C70 C -0.1372(4) 0.1867(4) 0.2423(3) 0.096(3) Uani 1 1 d . . . . .
H70 H -0.1530 0.2209 0.2354 0.116 Uiso 1 1 calc R U . . .
C71 C -0.1729(4) 0.1412(5) 0.2363(4) 0.124(4) Uani 1 1 d . . . . .
H71 H -0.2126 0.1452 0.2259 0.148 Uiso 1 1 calc R U . . .
C72 C -0.1515(3) 0.0928(4) 0.2451(4) 0.095(3) Uani 1 1 d . . . . .
H72 H -0.1755 0.0624 0.2398 0.114 Uiso 1 1 calc R U . . .
C73 C -0.0939(3) 0.0868(3) 0.2620(3) 0.0668(17) Uani 1 1 d . . . . .
H73 H -0.0797 0.0522 0.2693 0.080 Uiso 1 1 calc R U . . .
C74 C -0.0563(3) 0.1305(2) 0.2685(2) 0.0530(13) Uani 1 1 d . . . . .
C75 C -0.1641(5) 0.2024(4) 0.4026(4) 0.118(4) Uani 1 1 d . . . . .
H75A H -0.1220 0.2087 0.4095 0.141 Uiso 1 1 calc R U . . .
H75B H -0.1713 0.2099 0.3665 0.141 Uiso 1 1 calc R U . . .
C76 C -0.2017(7) 0.2413(6) 0.4354(7) 0.184(6) Uani 1 1 d . . . . .
H76A H -0.2427 0.2401 0.4242 0.276 Uiso 1 1 calc R U . . .
H76B H -0.1866 0.2776 0.4317 0.276 Uiso 1 1 calc R U . . .
H76C H -0.1994 0.2307 0.4709 0.276 Uiso 1 1 calc R U . . .
C77 C -0.2414(4) 0.1287(4) 0.4092(4) 0.106(3) Uani 1 1 d . . . . .
H77A H -0.2460 0.0905 0.4172 0.127 Uiso 1 1 calc R U . . .
H77B H -0.2635 0.1491 0.4348 0.127 Uiso 1 1 calc R U . . .
C78 C -0.2676(4) 0.1386(3) 0.3603(5) 0.122(4) Uani 1 1 d . . . . .
H78A H -0.2639 0.1764 0.3519 0.183 Uiso 1 1 calc R U . . .
H78B H -0.3092 0.1287 0.3611 0.183 Uiso 1 1 calc R U . . .
H78C H -0.2473 0.1173 0.3346 0.183 Uiso 1 1 calc R U . . .
C79 C -0.1380(5) 0.1132(5) 0.3838(4) 0.118(3) Uani 1 1 d . . . . .
H79A H -0.0983 0.1276 0.3902 0.142 Uiso 1 1 calc R U . . .
H79B H -0.1472 0.1197 0.3478 0.142 Uiso 1 1 calc R U . . .
C80 C -0.1363(5) 0.0531(4) 0.3924(4) 0.118(3) Uani 1 1 d . . . . .
H80A H -0.1242 0.0459 0.4273 0.177 Uiso 1 1 calc R U . . .
H80B H -0.1082 0.0369 0.3691 0.177 Uiso 1 1 calc R U . . .
H80C H -0.1754 0.0381 0.3865 0.177 Uiso 1 1 calc R U . . .
C83 C 0.1300(4) 0.1524(3) 0.5475(3) 0.092(3) Uani 1 1 d D . . . .
C84 C 0.1420(4) 0.1718(3) 0.4996(3) 0.090(2) Uani 1 1 d D . . . .
H84A H 0.1066 0.1884 0.4856 0.135 Uiso 1 1 calc R U . . .
H84B H 0.1546 0.1425 0.4777 0.135 Uiso 1 1 calc R U . . .
H84C H 0.1734 0.1984 0.5017 0.135 Uiso 1 1 calc R U . . .
C85 C 0.1912(5) -0.0918(4) 0.4441(4) 0.114(3) Uani 1 1 d D . . . .
C86 C 0.1832(6) -0.0680(3) 0.3978(3) 0.133(5) Uani 1 1 d D . . . .
H86A H 0.1666 -0.0939 0.3741 0.199 Uiso 1 1 calc R U . . .
H86B H 0.2211 -0.0553 0.3849 0.199 Uiso 1 1 calc R U . . .
H86C H 0.1562 -0.0378 0.4013 0.199 Uiso 1 1 calc R U . . .
N4 N 0.1346(4) -0.1947(3) 0.1614(3) 0.118(3) Uani 1 1 d D . . . .
C81 C 0.1150(4) -0.1526(3) 0.1607(3) 0.080(2) Uani 1 1 d D . . . .
C82 C 0.0873(4) -0.1014(3) 0.1623(3) 0.082(2) Uani 1 1 d D . . . .
H82A H 0.0590 -0.0986 0.1346 0.123 Uiso 1 1 calc R U . . .
H82B H 0.1171 -0.0736 0.1588 0.123 Uiso 1 1 calc R U . . .
H82C H 0.0668 -0.0972 0.1945 0.123 Uiso 1 1 calc R U . . .
N1 N 0.0287(2) 0.16096(17) 0.16510(17) 0.0512(11) Uani 1 1 d . . . . .
N2 N 0.0054(3) 0.23685(18) 0.28342(19) 0.0591(13) Uani 1 1 d . . . . .
N3 N -0.1789(3) 0.1425(3) 0.4137(3) 0.100(2) Uani 1 1 d . . . . .
H3A H -0.1679 0.1360 0.4497 0.120 Uiso 1 1 calc R U . . .
N5 N 0.1207(7) 0.1349(4) 0.5865(3) 0.186(6) Uani 1 1 d D . . . .
N6 N 0.1946(5) -0.1145(4) 0.4819(4) 0.151(4) Uani 1 1 d D . . . .
O1 O 0.00074(17) 0.00775(14) 0.21641(14) 0.0515(9) Uani 1 1 d . . . . .
O2 O 0.01056(19) 0.06503(14) 0.12702(14) 0.0553(10) Uani 1 1 d . . . . .
O3 O 0.13079(18) 0.05119(14) 0.17180(15) 0.0549(9) Uani 1 1 d . . . . .
O4 O 0.10206(17) 0.03149(12) 0.28051(13) 0.0468(8) Uani 1 1 d . . . . .
H4B H 0.1038 0.0472 0.3109 0.09(2) Uiso 1 1 d R . . . .
O5 O 0.06664(19) 0.26654(14) 0.36488(16) 0.0589(10) Uani 1 1 d . . . . .
O6 O 0.15161(18) 0.18732(15) 0.36352(16) 0.0565(10) Uani 1 1 d . . . . .
O7 O 0.01000(18) 0.16474(13) 0.39896(14) 0.0526(9) Uani 1 1 d . . . . .
O8 O 0.09148(16) 0.08355(12) 0.35571(13) 0.0443(8) Uani 1 1 d . . . . .
O9 O -0.00063(15) 0.12167(13) 0.28183(13) 0.0454(8) Uani 1 1 d . . . . .
O10 O 0.10804(16) 0.15207(12) 0.24957(14) 0.0449(8) Uani 1 1 d . . . . .
Gd1 Gd 0.05616(2) 0.07819(2) 0.21492(2) 0.04399(9) Uani 1 1 d . . . . .
Gd2 Gd 0.06560(2) 0.17041(2) 0.33280(2) 0.04384(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.315(6) . ?
C1 C6 1.421(9) . ?
C1 C2 1.426(8) . ?
C2 C3 1.404(8) . ?
C2 C28 1.499(8) . ?
C3 C4 1.388(10) . ?
C4 C5 1.383(9) . ?
C5 C6 1.380(8) . ?
C6 C7 1.514(8) . ?
C7 C8 1.513(10) . ?
C8 C9 1.398(9) . ?
C8 C13 1.409(9) . ?
C9 C10 1.378(11) . ?
C10 C11 1.374(10) . ?
C11 C12 1.393(8) . ?
C12 C13 1.396(9) . ?
C12 C14 1.524(9) . ?
C13 O2 1.416(7) . ?
C14 C15 1.518(10) . ?
C15 C16 1.383(9) . ?
C15 C20 1.390(9) . ?
C16 C17 1.383(11) . ?
C17 C18 1.372(11) . ?
C18 C19 1.398(9) . ?
C19 C20 1.427(9) . ?
C19 C21 1.495(9) . ?
C20 O3 1.327(7) . ?
C21 C22 1.522(8) . ?
C22 C27 1.393(8) . ?
C22 C23 1.401(7) . ?
C23 C24 1.389(9) . ?
C24 C25 1.374(9) . ?
C25 C26 1.400(7) . ?
C26 C27 1.410(8) . ?
C26 C28 1.526(8) . ?
C27 O4 1.384(6) . ?
C29 O2 1.446(7) . ?
C29 C30 1.517(9) . ?
C30 N1 1.472(8) . ?
C31 N1 1.286(7) . ?
C31 C32 1.441(8) . ?
C32 C37 1.409(8) . ?
C32 C33 1.424(8) . ?
C33 C34 1.382(10) . ?
C34 C35 1.372(10) . ?
C35 C36 1.388(8) . ?
C36 C37 1.414(8) . ?
C37 O10 1.338(6) . ?
C38 C43 1.393(9) . ?
C38 C39 1.397(9) . ?
C38 O5 1.421(7) . ?
C39 C40 1.398(10) . ?
C39 C65 1.526(10) . ?
C40 C41 1.372(10) . ?
C41 C42 1.399(10) . ?
C42 C43 1.385(9) . ?
C43 C44 1.521(9) . ?
C44 C45 1.538(8) . ?
C45 C46 1.395(9) . ?
C45 C50 1.418(7) . ?
C46 C47 1.376(10) . ?
C47 C48 1.403(9) . ?
C48 C49 1.385(8) . ?
C49 C50 1.411(7) . ?
C49 C51 1.510(7) . ?
C50 O7 1.314(7) . ?
C51 C52 1.502(8) . ?
C52 C53 1.404(8) . ?
C52 C57 1.412(8) . ?
C53 C54 1.380(9) . ?
C54 C55 1.378(10) . ?
C55 C56 1.416(9) . ?
C56 C57 1.403(8) . ?
C56 C58 1.511(9) . ?
C57 O8 1.381(6) . ?
C58 C59 1.517(8) . ?
C59 C60 1.385(10) . ?
C59 C64 1.415(9) . ?
C60 C61 1.382(13) . ?
C61 C62 1.396(15) . ?
C62 C63 1.382(11) . ?
C63 C64 1.412(9) . ?
C63 C65 1.518(11) . ?
C64 O6 1.317(7) . ?
C66 O5 1.463(7) . ?
C66 C67 1.489(9) . ?
C67 N2 1.481(8) . ?
C68 N2 1.279(9) . ?
C68 C69 1.457(10) . ?
C69 C70 1.407(10) . ?
C69 C74 1.415(8) . ?
C70 C71 1.411(14) . ?
C71 C72 1.331(13) . ?
C72 C73 1.395(10) . ?
C73 C74 1.403(9) . ?
C74 O9 1.334(6) . ?
C75 C76 1.565(18) . ?
C75 N3 1.571(12) . ?
C77 C78 1.449(13) . ?
C77 N3 1.469(10) . ?
C79 N3 1.428(13) . ?
C79 C80 1.528(14) . ?
C83 N5 1.143(10) . ?
C83 C84 1.387(10) . ?
C85 N6 1.155(10) . ?
C85 C86 1.377(11) . ?
N4 C81 1.149(9) . ?
C81 C82 1.434(9) . ?
N1 Gd1 2.543(4) . ?
N2 Gd2 2.527(5) . ?
O1 Gd1 2.175(3) . ?
O2 Gd1 2.572(4) . ?
O3 Gd1 2.158(4) . ?
O4 Gd1 2.344(3) . ?
O5 Gd2 2.562(4) . ?
O6 Gd2 2.164(4) . ?
O7 Gd2 2.167(4) . ?
O8 Gd2 2.342(3) . ?
O9 Gd2 2.367(3) . ?
O9 Gd1 2.452(3) . ?
O10 Gd1 2.385(3) . ?
O10 Gd2 2.452(4) . ?
Gd1 Gd2 3.8964(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 120.2(5) . . ?
O1 C1 C2 119.5(5) . . ?
C6 C1 C2 120.1(5) . . ?
C3 C2 C1 117.7(6) . . ?
C3 C2 C28 123.3(5) . . ?
C1 C2 C28 119.0(5) . . ?
C4 C3 C2 121.9(6) . . ?
C5 C4 C3 119.4(6) . . ?
C6 C5 C4 121.8(6) . . ?
C5 C6 C1 119.0(6) . . ?
C5 C6 C7 122.4(6) . . ?
C1 C6 C7 118.6(5) . . ?
C8 C7 C6 114.8(5) . . ?
C9 C8 C13 116.4(6) . . ?
C9 C8 C7 120.7(6) . . ?
C13 C8 C7 122.9(5) . . ?
C10 C9 C8 121.2(6) . . ?
C11 C10 C9 120.5(6) . . ?
C10 C11 C12 121.6(7) . . ?
C11 C12 C13 116.6(6) . . ?
C11 C12 C14 119.4(6) . . ?
C13 C12 C14 123.9(5) . . ?
C12 C13 C8 123.4(5) . . ?
C12 C13 O2 119.1(5) . . ?
C8 C13 O2 117.6(6) . . ?
C15 C14 C12 110.9(5) . . ?
C16 C15 C20 119.6(7) . . ?
C16 C15 C14 120.8(6) . . ?
C20 C15 C14 119.5(6) . . ?
C17 C16 C15 120.7(7) . . ?
C18 C17 C16 120.0(7) . . ?
C17 C18 C19 122.0(7) . . ?
C18 C19 C20 117.0(6) . . ?
C18 C19 C21 122.0(6) . . ?
C20 C19 C21 120.8(5) . . ?
O3 C20 C15 119.8(6) . . ?
O3 C20 C19 119.4(6) . . ?
C15 C20 C19 120.8(6) . . ?
C19 C21 C22 112.4(5) . . ?
C27 C22 C23 118.6(5) . . ?
C27 C22 C21 122.2(5) . . ?
C23 C22 C21 119.1(5) . . ?
C24 C23 C22 120.6(6) . . ?
C25 C24 C23 119.9(5) . . ?
C24 C25 C26 121.6(6) . . ?
C25 C26 C27 117.6(5) . . ?
C25 C26 C28 119.3(5) . . ?
C27 C26 C28 123.0(5) . . ?
O4 C27 C22 118.8(5) . . ?
O4 C27 C26 119.7(5) . . ?
C22 C27 C26 121.5(5) . . ?
C2 C28 C26 114.6(5) . . ?
O2 C29 C30 106.3(5) . . ?
N1 C30 C29 108.7(5) . . ?
N1 C31 C32 127.2(5) . . ?
C37 C32 C33 119.6(6) . . ?
C37 C32 C31 124.8(5) . . ?
C33 C32 C31 115.6(5) . . ?
C34 C33 C32 121.0(6) . . ?
C35 C34 C33 119.5(6) . . ?
C34 C35 C36 120.7(6) . . ?
C35 C36 C37 121.7(6) . . ?
O10 C37 C32 122.7(5) . . ?
O10 C37 C36 119.9(5) . . ?
C32 C37 C36 117.4(5) . . ?
C43 C38 C39 122.5(6) . . ?
C43 C38 O5 119.7(6) . . ?
C39 C38 O5 117.8(6) . . ?
C38 C39 C40 117.5(7) . . ?
C38 C39 C65 122.9(7) . . ?
C40 C39 C65 119.6(7) . . ?
C41 C40 C39 121.5(7) . . ?
C40 C41 C42 119.2(7) . . ?
C43 C42 C41 121.6(6) . . ?
C42 C43 C38 117.5(6) . . ?
C42 C43 C44 118.5(6) . . ?
C38 C43 C44 124.0(6) . . ?
C43 C44 C45 110.5(5) . . ?
C46 C45 C50 119.7(5) . . ?
C46 C45 C44 122.6(5) . . ?
C50 C45 C44 117.6(5) . . ?
C47 C46 C45 120.9(6) . . ?
C46 C47 C48 119.2(6) . . ?
C49 C48 C47 121.9(6) . . ?
C48 C49 C50 118.7(5) . . ?
C48 C49 C51 122.2(5) . . ?
C50 C49 C51 119.0(5) . . ?
O7 C50 C49 120.8(5) . . ?
O7 C50 C45 119.6(5) . . ?
C49 C50 C45 119.6(5) . . ?
C52 C51 C49 113.0(5) . . ?
C53 C52 C57 117.5(5) . . ?
C53 C52 C51 119.9(5) . . ?
C57 C52 C51 122.5(5) . . ?
C54 C53 C52 121.9(6) . . ?
C55 C54 C53 119.5(6) . . ?
C54 C55 C56 121.6(6) . . ?
C57 C56 C55 117.4(6) . . ?
C57 C56 C58 123.8(5) . . ?
C55 C56 C58 118.7(6) . . ?
O8 C57 C56 119.8(5) . . ?
O8 C57 C52 118.5(5) . . ?
C56 C57 C52 121.7(5) . . ?
C56 C58 C59 113.0(5) . . ?
C60 C59 C64 118.5(7) . . ?
C60 C59 C58 122.9(7) . . ?
C64 C59 C58 118.6(5) . . ?
C61 C60 C59 121.5(9) . . ?
C60 C61 C62 119.9(8) . . ?
C63 C62 C61 120.3(7) . . ?
C62 C63 C64 119.7(8) . . ?
C62 C63 C65 122.3(7) . . ?
C64 C63 C65 118.1(6) . . ?
O6 C64 C63 120.0(6) . . ?
O6 C64 C59 120.1(5) . . ?
C63 C64 C59 119.9(6) . . ?
C63 C65 C39 112.2(6) . . ?
O5 C66 C67 105.7(5) . . ?
N2 C67 C66 110.4(5) . . ?
N2 C68 C69 127.1(6) . . ?
C70 C69 C74 118.5(7) . . ?
C70 C69 C68 116.7(7) . . ?
C74 C69 C68 124.8(6) . . ?
C69 C70 C71 120.8(8) . . ?
C72 C71 C70 120.7(8) . . ?
C71 C72 C73 119.9(8) . . ?
C72 C73 C74 122.0(7) . . ?
O9 C74 C73 118.9(5) . . ?
O9 C74 C69 122.9(6) . . ?
C73 C74 C69 118.1(6) . . ?
C76 C75 N3 112.2(10) . . ?
C78 C77 N3 115.6(9) . . ?
N3 C79 C80 116.3(9) . . ?
N5 C83 C84 178.0(11) . . ?
N6 C85 C86 174.7(15) . . ?
N4 C81 C82 175.8(9) . . ?
C31 N1 C30 117.2(5) . . ?
C31 N1 Gd1 128.9(4) . . ?
C30 N1 Gd1 113.4(3) . . ?
C68 N2 C67 118.3(6) . . ?
C68 N2 Gd2 129.1(4) . . ?
C67 N2 Gd2 112.1(4) . . ?
C79 N3 C77 117.7(9) . . ?
C79 N3 C75 104.5(8) . . ?
C77 N3 C75 114.8(7) . . ?
C1 O1 Gd1 165.4(4) . . ?
C13 O2 C29 112.0(4) . . ?
C13 O2 Gd1 124.5(3) . . ?
C29 O2 Gd1 123.3(3) . . ?
C20 O3 Gd1 158.1(3) . . ?
C27 O4 Gd1 124.5(3) . . ?
C38 O5 C66 113.8(4) . . ?
C38 O5 Gd2 123.0(3) . . ?
C66 O5 Gd2 122.1(3) . . ?
C64 O6 Gd2 171.2(4) . . ?
C50 O7 Gd2 160.5(4) . . ?
C57 O8 Gd2 124.3(3) . . ?
C74 O9 Gd2 132.1(3) . . ?
C74 O9 Gd1 112.6(3) . . ?
Gd2 O9 Gd1 107.90(13) . . ?
C37 O10 Gd1 131.4(3) . . ?
C37 O10 Gd2 115.2(3) . . ?
Gd1 O10 Gd2 107.30(13) . . ?
O3 Gd1 O1 102.16(14) . . ?
O3 Gd1 O4 83.32(14) . . ?
O1 Gd1 O4 80.65(13) . . ?
O3 Gd1 O10 93.36(13) . . ?
O1 Gd1 O10 156.14(13) . . ?
O4 Gd1 O10 83.32(12) . . ?
O3 Gd1 O9 159.84(13) . . ?
O1 Gd1 O9 92.51(13) . . ?
O4 Gd1 O9 85.55(12) . . ?
O10 Gd1 O9 68.64(12) . . ?
O3 Gd1 N1 100.16(15) . . ?
O1 Gd1 N1 122.21(15) . . ?
O4 Gd1 N1 154.80(13) . . ?
O10 Gd1 N1 71.60(13) . . ?
O9 Gd1 N1 83.15(13) . . ?
O3 Gd1 O2 78.35(15) . . ?
O1 Gd1 O2 71.17(13) . . ?
O4 Gd1 O2 141.95(11) . . ?
O10 Gd1 O2 130.46(12) . . ?
O9 Gd1 O2 119.95(13) . . ?
N1 Gd1 O2 62.33(13) . . ?
O3 Gd1 Gd2 124.63(11) . . ?
O1 Gd1 Gd2 120.13(10) . . ?
O4 Gd1 Gd2 71.27(8) . . ?
O10 Gd1 Gd2 36.93(9) . . ?
O9 Gd1 Gd2 35.31(8) . . ?
N1 Gd1 Gd2 86.72(10) . . ?
O2 Gd1 Gd2 145.59(9) . . ?
O6 Gd2 O7 103.74(16) . . ?
O6 Gd2 O8 81.82(13) . . ?
O7 Gd2 O8 82.88(13) . . ?
O6 Gd2 O9 153.32(14) . . ?
O7 Gd2 O9 93.18(14) . . ?
O8 Gd2 O9 79.96(12) . . ?
O6 Gd2 O10 91.05(15) . . ?
O7 Gd2 O10 161.02(13) . . ?
O8 Gd2 O10 87.63(12) . . ?
O9 Gd2 O10 68.93(12) . . ?
O6 Gd2 N2 123.81(16) . . ?
O7 Gd2 N2 98.36(16) . . ?
O8 Gd2 N2 152.54(15) . . ?
O9 Gd2 N2 72.58(15) . . ?
O10 Gd2 N2 82.67(14) . . ?
O6 Gd2 O5 71.42(14) . . ?
O7 Gd2 O5 78.41(13) . . ?
O8 Gd2 O5 142.30(13) . . ?
O9 Gd2 O5 133.13(13) . . ?
O10 Gd2 O5 118.17(12) . . ?
N2 Gd2 O5 63.47(15) . . ?
O6 Gd2 Gd1 117.94(11) . . ?
O7 Gd2 Gd1 125.26(10) . . ?
O8 Gd2 Gd1 70.54(8) . . ?
O9 Gd2 Gd1 36.79(8) . . ?
O10 Gd2 Gd1 35.77(8) . . ?
N2 Gd2 Gd1 87.02(11) . . ?
O5 Gd2 Gd1 145.88(9) . . ?

_refine_diff_density_max         1.155
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.217

