# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2020

####################################################################### 
# 
# 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_nj299
_database_code_depnum_ccdc_archive 'CCDC 2013179'
loop_
_audit_author_name
_audit_author_address
'Rosario Scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT910_nj299               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         16 Note  
RESPONSE: These missing reflections are hidden by the beam-stop.
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H102 K2 N8 Nd2 O12'
_chemical_formula_sum            'C78 H102 K2 N8 Nd2 O12'
_chemical_formula_weight         1710.35

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   19.1572(10)
_cell_length_b                   19.9660(6)
_cell_length_c                   21.4402(9)
_cell_angle_alpha                90
_cell_angle_beta                 113.990(5)
_cell_angle_gamma                90
_cell_volume                     7492.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    140.00(10)
_cell_measurement_reflns_used    12712
_cell_measurement_theta_min      3.5230
_cell_measurement_theta_max      32.2610

_exptl_crystal_description       needle
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_F_000             3520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.047
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 2 0.1126
1 0 -2 0.0941
0 1 0 0.0216
-1 1 0 0.0250
0 1 2 0.0727
-1 0 0 0.0245
1 0 0 0.0236
-1 -2 0 0.0293
1 -2 0 0.0216
1 2 0 0.0220
_exptl_absorpt_coefficient_mu    1.549
_shelx_estimated_absorpt_T_min   0.737
_shelx_estimated_absorpt_T_max   0.931
_exptl_absorpt_correction_T_min  0.777
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.66a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      140.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.2665
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     20.00  47.00   1.00  150.00    --  -17.94  37.00 120.00   27
  2  ω    -37.00   0.00   1.00  150.00    --  -17.94  37.00 120.00   37
  3  ω    -79.00  14.00   1.00  150.00    --  -17.94 -77.00  90.00   93
  4  ω    -15.00  55.00   1.00  150.00    --  -17.94  57.00 150.00   70
  5  ω    -77.00 -48.00   1.00  150.00    --  -17.94 162.00-156.00   29
  6  ω     35.00  69.00   1.00  150.00    --   18.87 178.00  30.00   34
  7  ω     34.00 106.00   1.00  150.00    --   18.87-178.00 -30.00   72
  8  ω    -14.00  92.00   1.00  150.00    --   18.87  77.00  30.00  106
;
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_number            53552
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         3.290
_diffrn_reflns_theta_max         32.737
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12961
_reflns_number_gt                9233
_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       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Mercury 4.2.0 (CCDC, 2019)'
_computing_publication_material  'CIFTab (Sheldrick, 2016)'
_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)+(0.0295P)²+20.3421P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12961
_refine_ls_number_parameters     552
_refine_ls_number_restraints     406
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0940
_refine_ls_wR_factor_gt          0.0782
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.064
_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
Nd1 Nd 0.49422(2) 0.33145(2) 0.65725(2) 0.01997(4) Uani 1 1 d . . . . .
K1 K 0.50758(6) 0.22612(4) 0.50436(4) 0.0455(2) Uani 1 1 d D . . . .
O1 O 0.45853(13) 0.22391(10) 0.60373(10) 0.0279(4) Uani 1 1 d . . . . .
O2 O 0.58117(12) 0.42034(10) 0.68427(10) 0.0265(4) Uani 1 1 d . . . . .
O3 O 0.58684(12) 0.30222(10) 0.61265(10) 0.0264(4) Uani 1 1 d . . . . .
O4 O 0.57247(18) 0.23993(17) 0.41234(14) 0.0606(8) Uani 1 1 d . . . . .
O5 O 0.6473(3) 0.15877(19) 0.5673(2) 0.0450(11) Uani 0.695(5) 1 d D U P A 1
O6 O 0.5978(9) 0.1303(6) 0.5512(5) 0.077(3) Uani 0.305(5) 1 d D U P A 2
O7 O 0.4414(5) 0.1315(4) 0.3995(4) 0.0693(19) Uani 0.689(13) 1 d D U P A 1
O8 O 0.4091(11) 0.1507(9) 0.3909(8) 0.078(4) Uani 0.311(13) 1 d D U P A 2
N1 N 0.33755(14) 0.34100(12) 0.58773(12) 0.0237(5) Uani 1 1 d . . . . .
N2 N 0.42644(13) 0.28282(12) 0.72346(11) 0.0218(5) Uani 1 1 d . . . . .
N3 N 0.43039(14) 0.45013(12) 0.66318(12) 0.0247(5) Uani 1 1 d . . . . .
N4 N 0.44750(14) 0.36512(13) 0.52758(12) 0.0261(5) Uani 1 1 d . . . . .
C1 C 0.30700(17) 0.28699(15) 0.61671(15) 0.0263(6) Uani 1 1 d . . . . .
H1A H 0.315979 0.243392 0.599229 0.032 Uiso 1 1 calc R U . . .
H1B H 0.251083 0.292958 0.600612 0.032 Uiso 1 1 calc R U . . .
C2 C 0.34256(16) 0.28503(15) 0.69462(14) 0.0244(6) Uani 1 1 d . . . . .
H2A H 0.326151 0.325186 0.712202 0.029 Uiso 1 1 calc R U . . .
H2B H 0.323382 0.245098 0.710112 0.029 Uiso 1 1 calc R U . . .
C3 C 0.45532(16) 0.21292(14) 0.73777(14) 0.0227(5) Uani 1 1 d . . . . .
H3 H 0.444371 0.196613 0.776975 0.027 Uiso 1 1 calc R U . . .
C4 C 0.42157(16) 0.16197(14) 0.68084(14) 0.0239(6) Uani 1 1 d . . . . .
C5 C 0.38671(19) 0.10480(15) 0.69145(16) 0.0299(6) Uani 1 1 d . . . . .
H5 H 0.382264 0.099851 0.733752 0.036 Uiso 1 1 calc R U . . .
C6 C 0.3579(2) 0.05426(16) 0.64274(17) 0.0364(7) Uani 1 1 d . . . . .
H6 H 0.333984 0.015817 0.651355 0.044 Uiso 1 1 calc R U . . .
C7 C 0.36520(19) 0.06168(16) 0.58159(17) 0.0341(7) Uani 1 1 d . . . . .
H7 H 0.346748 0.027581 0.547904 0.041 Uiso 1 1 calc R U . . .
C8 C 0.39898(18) 0.11809(15) 0.56892(15) 0.0293(6) Uani 1 1 d . . . . .
H8 H 0.402896 0.122185 0.526315 0.035 Uiso 1 1 calc R U . . .
C9 C 0.42780(17) 0.16977(14) 0.61741(14) 0.0242(5) Uani 1 1 d . . . . .
C10 C 0.30406(17) 0.40649(15) 0.59292(15) 0.0278(6) Uani 1 1 d . . . . .
H10A H 0.252474 0.399131 0.591837 0.033 Uiso 1 1 calc R U . . .
H10B H 0.298369 0.434192 0.552844 0.033 Uiso 1 1 calc R U . . .
C11 C 0.35194(17) 0.44404(15) 0.65713(15) 0.0281(6) Uani 1 1 d . . . . .
H11A H 0.330086 0.489188 0.655970 0.034 Uiso 1 1 calc R U . . .
H11B H 0.351507 0.419933 0.697325 0.034 Uiso 1 1 calc R U . . .
C12 C 0.45633(18) 0.51015(15) 0.66827(14) 0.0263(6) Uani 1 1 d . . . . .
H12 H 0.422262 0.545024 0.667514 0.032 Uiso 1 1 calc R U . . .
C13 C 0.53150(18) 0.53069(15) 0.67504(15) 0.0264(6) Uani 1 1 d . . . . .
C14 C 0.5461(2) 0.59993(16) 0.67605(16) 0.0333(7) Uani 1 1 d . . . . .
H14 H 0.506617 0.630609 0.672019 0.040 Uiso 1 1 calc R U . . .
C15 C 0.6158(2) 0.62438(16) 0.68270(17) 0.0363(8) Uani 1 1 d . . . . .
H15 H 0.624652 0.671264 0.683729 0.044 Uiso 1 1 calc R U . . .
C16 C 0.6733(2) 0.57916(16) 0.68792(16) 0.0338(7) Uani 1 1 d . . . . .
H16 H 0.721552 0.595504 0.691996 0.041 Uiso 1 1 calc R U . . .
C17 C 0.66127(18) 0.51112(16) 0.68726(15) 0.0293(6) Uani 1 1 d . . . . .
H17 H 0.701264 0.481415 0.690288 0.035 Uiso 1 1 calc R U . . .
C18 C 0.59076(17) 0.48438(15) 0.68218(14) 0.0252(6) Uani 1 1 d . . . . .
C19 C 0.32076(17) 0.32655(16) 0.51518(14) 0.0274(6) Uani 1 1 d . . . . .
H19A H 0.265368 0.332671 0.487628 0.033 Uiso 1 1 calc R U . . .
H19B H 0.333326 0.279137 0.510966 0.033 Uiso 1 1 calc R U . . .
C20 C 0.36484(18) 0.37085(17) 0.48649(15) 0.0300(6) Uani 1 1 d . . . . .
H20A H 0.353169 0.357574 0.438795 0.036 Uiso 1 1 calc R U . . .
H20B H 0.348775 0.418015 0.486253 0.036 Uiso 1 1 calc R U . . .
C21 C 0.49191(18) 0.39457(15) 0.50444(15) 0.0269(6) Uani 1 1 d . . . . .
H21 H 0.466995 0.416927 0.458942 0.032 Uiso 1 1 calc R U . . .
C22 C 0.57507(17) 0.39194(15) 0.53461(14) 0.0249(6) Uani 1 1 d . . . . .
C23 C 0.61355(19) 0.43586(16) 0.50833(16) 0.0306(7) Uani 1 1 d . . . . .
H23 H 0.584479 0.465884 0.472901 0.037 Uiso 1 1 calc R U . . .
C24 C 0.6916(2) 0.43697(17) 0.53201(17) 0.0346(7) Uani 1 1 d . . . . .
H24 H 0.716320 0.467250 0.513365 0.042 Uiso 1 1 calc R U . . .
C25 C 0.73410(19) 0.39288(16) 0.58390(17) 0.0329(7) Uani 1 1 d . . . . .
H25 H 0.788294 0.393552 0.601139 0.040 Uiso 1 1 calc R U . . .
C26 C 0.69877(19) 0.34847(16) 0.61050(16) 0.0300(6) Uani 1 1 d . . . . .
H26 H 0.729248 0.318664 0.645530 0.036 Uiso 1 1 calc R U . . .
C27 C 0.61858(18) 0.34572(14) 0.58742(15) 0.0251(6) Uani 1 1 d . . . . .
C28 C 0.6518(2) 0.2582(2) 0.4460(2) 0.0542(11) Uani 1 1 d . . . . .
H28A H 0.684690 0.217908 0.458563 0.065 Uiso 1 1 calc R U . . .
H28B H 0.661204 0.284490 0.487862 0.065 Uiso 1 1 calc R U . . .
C29 C 0.6670(3) 0.2993(2) 0.3952(2) 0.0578(11) Uani 1 1 d . . . . .
H29A H 0.721331 0.296224 0.402338 0.069 Uiso 1 1 calc R U . . .
H29B H 0.653843 0.346889 0.397682 0.069 Uiso 1 1 calc R U . . .
C30 C 0.6155(2) 0.2686(3) 0.3277(2) 0.0570(12) Uani 1 1 d . . . . .
H30A H 0.644996 0.239572 0.309796 0.068 Uiso 1 1 calc R U . . .
H30B H 0.589504 0.303811 0.293641 0.068 Uiso 1 1 calc R U . . .
C31 C 0.5583(3) 0.2280(2) 0.3441(2) 0.0545(11) Uani 1 1 d . . . . .
H31A H 0.505616 0.241668 0.314105 0.065 Uiso 1 1 calc R U . . .
H31B H 0.564232 0.179745 0.336801 0.065 Uiso 1 1 calc R U . . .
C32 C 0.6623(4) 0.1455(3) 0.6377(3) 0.0457(14) Uani 0.695(5) 1 d D U P A 1
H32A H 0.637700 0.179673 0.655508 0.055 Uiso 0.695(5) 1 calc R U P A 1
H32B H 0.717915 0.145462 0.666243 0.055 Uiso 0.695(5) 1 calc R U P A 1
C33 C 0.6282(4) 0.0768(3) 0.6372(3) 0.0528(15) Uani 0.695(5) 1 d D U P A 1
H33A H 0.577010 0.080563 0.637834 0.063 Uiso 0.695(5) 1 calc R U P A 1
H33B H 0.661601 0.050060 0.677077 0.063 Uiso 0.695(5) 1 calc R U P A 1
C34 C 0.6231(5) 0.0450(3) 0.5707(3) 0.0622(17) Uani 0.695(5) 1 d D U P A 1
H34A H 0.650812 0.001814 0.579268 0.075 Uiso 0.695(5) 1 calc R U P A 1
H34B H 0.569262 0.037618 0.538708 0.075 Uiso 0.695(5) 1 calc R U P A 1
C35 C 0.6610(4) 0.0969(3) 0.5432(4) 0.0494(16) Uani 0.695(5) 1 d D U P A 1
H35A H 0.716604 0.088294 0.560191 0.059 Uiso 0.695(5) 1 calc R U P A 1
H35B H 0.638670 0.096219 0.492714 0.059 Uiso 0.695(5) 1 calc R U P A 1
C36 C 0.6138(10) 0.1312(9) 0.6207(6) 0.061(3) Uani 0.305(5) 1 d D U P A 2
H36A H 0.573828 0.107895 0.630594 0.073 Uiso 0.305(5) 1 calc R U P A 2
H36B H 0.619948 0.177439 0.638744 0.073 Uiso 0.305(5) 1 calc R U P A 2
C37 C 0.6885(9) 0.0932(8) 0.6486(7) 0.061(3) Uani 0.305(5) 1 d D U P A 2
H37A H 0.732196 0.124593 0.667029 0.073 Uiso 0.305(5) 1 calc R U P A 2
H37B H 0.690576 0.062468 0.685557 0.073 Uiso 0.305(5) 1 calc R U P A 2
C38 C 0.6908(10) 0.0546(8) 0.5896(7) 0.065(3) Uani 0.305(5) 1 d D U P A 2
H38A H 0.685212 0.006089 0.595781 0.078 Uiso 0.305(5) 1 calc R U P A 2
H38B H 0.740004 0.062176 0.585753 0.078 Uiso 0.305(5) 1 calc R U P A 2
C39 C 0.6253(11) 0.0797(8) 0.5265(8) 0.063(4) Uani 0.305(5) 1 d D U P A 2
H39A H 0.643260 0.095724 0.491898 0.076 Uiso 0.305(5) 1 calc R U P A 2
H39B H 0.586340 0.044342 0.506120 0.076 Uiso 0.305(5) 1 calc R U P A 2
C40 C 0.4754(4) 0.0818(4) 0.3740(4) 0.058(2) Uani 0.689(13) 1 d D U P A 1
H40A H 0.478014 0.038542 0.397386 0.070 Uiso 0.689(13) 1 calc R U P A 1
H40B H 0.527634 0.095193 0.380519 0.070 Uiso 0.689(13) 1 calc R U P A 1
C41 C 0.4234(6) 0.0764(5) 0.2983(4) 0.071(2) Uani 0.689(13) 1 d D U P A 1
H41A H 0.442393 0.104489 0.270444 0.085 Uiso 0.689(13) 1 calc R U P A 1
H41B H 0.419001 0.029466 0.282375 0.085 Uiso 0.689(13) 1 calc R U P A 1
C42 C 0.3476(5) 0.1023(5) 0.2954(5) 0.075(3) Uani 0.689(13) 1 d D U P A 1
H42A H 0.314974 0.120136 0.249661 0.090 Uiso 0.689(13) 1 calc R U P A 1
H42B H 0.319293 0.067313 0.308277 0.090 Uiso 0.689(13) 1 calc R U P A 1
C43 C 0.3750(6) 0.1568(6) 0.3477(7) 0.075(3) Uani 0.689(13) 1 d D U P A 1
H43A H 0.386370 0.197997 0.327880 0.090 Uiso 0.689(13) 1 calc R U P A 1
H43B H 0.336130 0.167266 0.365644 0.090 Uiso 0.689(13) 1 calc R U P A 1
C44 C 0.4430(17) 0.0870(11) 0.3932(10) 0.091(5) Uani 0.311(13) 1 d D U P A 2
H44A H 0.420718 0.054907 0.415121 0.109 Uiso 0.311(13) 1 calc R U P A 2
H44B H 0.498315 0.090503 0.422518 0.109 Uiso 0.311(13) 1 calc R U P A 2
C45 C 0.4338(15) 0.0585(13) 0.3243(11) 0.093(5) Uani 0.311(13) 1 d D U P A 2
H45A H 0.479994 0.065734 0.315374 0.112 Uiso 0.311(13) 1 calc R U P A 2
H45B H 0.421167 0.010160 0.320574 0.112 Uiso 0.311(13) 1 calc R U P A 2
C46 C 0.3676(16) 0.0999(12) 0.2779(10) 0.076(5) Uani 0.311(13) 1 d D U P A 2
H46A H 0.321191 0.071984 0.257012 0.092 Uiso 0.311(13) 1 calc R U P A 2
H46B H 0.379261 0.120106 0.241045 0.092 Uiso 0.311(13) 1 calc R U P A 2
C47 C 0.3559(15) 0.1536(14) 0.3218(8) 0.067(4) Uani 0.311(13) 1 d D U P A 2
H47A H 0.359854 0.197928 0.302784 0.080 Uiso 0.311(13) 1 calc R U P A 2
H47B H 0.303589 0.149497 0.320000 0.080 Uiso 0.311(13) 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
Nd1 O2 2.340(2) . ?
Nd1 O1 2.399(2) . ?
Nd1 O3 2.405(2) . ?
Nd1 N2 2.478(2) . ?
Nd1 N2 2.575(2) 2_656 ?
Nd1 N4 2.638(2) . ?
Nd1 N3 2.693(2) . ?
Nd1 N1 2.762(2) . ?
Nd1 Nd1 3.8922(3) 2_656 ?
Nd1 K1 3.9895(7) . ?
K1 O6 2.499(10) . ?
K1 O1 2.655(2) . ?
K1 O3 2.672(2) . ?
K1 O4 2.740(3) . ?
K1 O5 2.803(4) . ?
K1 O7 2.813(5) . ?
K1 O8 2.831(12) . ?
K1 N4 3.121(3) . ?
K1 C27 3.212(3) . ?
K1 C21 3.377(3) . ?
K1 C22 3.517(3) . ?
K1 C9 3.534(3) . ?
O1 C9 1.320(3) . ?
O2 C18 1.295(3) . ?
O3 C27 1.298(3) . ?
O4 C31 1.396(4) . ?
O4 C28 1.440(5) . ?
O5 C35 1.404(6) . ?
O5 C32 1.440(6) . ?
O6 C39 1.344(12) . ?
O6 C36 1.393(12) . ?
O7 C43 1.398(9) . ?
O7 C40 1.412(8) . ?
O8 C47 1.417(13) . ?
O8 C44 1.421(14) . ?
N1 C1 1.479(4) . ?
N1 C10 1.480(4) . ?
N1 C19 1.483(4) . ?
N2 C2 1.469(4) . ?
N2 C3 1.487(4) . ?
N3 C12 1.285(4) . ?
N3 C11 1.460(4) . ?
N4 C21 1.288(4) . ?
N4 C20 1.471(4) . ?
C1 C2 1.527(4) . ?
C3 C4 1.517(4) . ?
C3 C3 1.573(6) 2_656 ?
C4 C5 1.387(4) . ?
C4 C9 1.421(4) . ?
C5 C6 1.395(4) . ?
C6 C7 1.382(5) . ?
C7 C8 1.380(4) . ?
C8 C9 1.408(4) . ?
C10 C11 1.507(4) . ?
C12 C13 1.447(4) . ?
C13 C14 1.409(4) . ?
C13 C18 1.423(4) . ?
C14 C15 1.373(5) . ?
C15 C16 1.393(5) . ?
C16 C17 1.377(4) . ?
C17 C18 1.415(4) . ?
C19 C20 1.515(4) . ?
C21 C22 1.456(4) . ?
C22 C23 1.403(4) . ?
C22 C27 1.436(4) . ?
C23 C24 1.371(5) . ?
C24 C25 1.392(5) . ?
C25 C26 1.373(4) . ?
C26 C27 1.411(4) . ?
C28 C29 1.485(6) . ?
C29 C30 1.509(6) . ?
C30 C31 1.514(6) . ?
C32 C33 1.518(7) . ?
C33 C34 1.527(7) . ?
C34 C35 1.516(8) . ?
C36 C37 1.511(13) . ?
C37 C38 1.498(12) . ?
C38 C39 1.508(13) . ?
C40 C41 1.523(9) . ?
C41 C42 1.520(10) . ?
C42 C43 1.496(10) . ?
C44 C45 1.524(14) . ?
C45 C46 1.501(14) . ?
C46 C47 1.502(14) . ?

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
O2 Nd1 O1 146.40(7) . . ?
O2 Nd1 O3 73.53(7) . . ?
O1 Nd1 O3 72.87(7) . . ?
O2 Nd1 N2 129.89(7) . . ?
O1 Nd1 N2 79.03(7) . . ?
O3 Nd1 N2 140.88(7) . . ?
O2 Nd1 N2 88.10(7) . 2_656 ?
O1 Nd1 N2 94.36(7) . 2_656 ?
O3 Nd1 N2 94.04(7) . 2_656 ?
N2 Nd1 N2 61.22(9) . 2_656 ?
O2 Nd1 N4 88.28(7) . . ?
O1 Nd1 N4 79.36(7) . . ?
O3 Nd1 N4 68.39(7) . . ?
N2 Nd1 N4 132.16(8) . . ?
N2 Nd1 N4 162.37(8) 2_656 . ?
O2 Nd1 N3 67.18(7) . . ?
O1 Nd1 N3 139.76(8) . . ?
O3 Nd1 N3 130.91(7) . . ?
N2 Nd1 N3 87.94(7) . . ?
N2 Nd1 N3 112.39(7) 2_656 . ?
N4 Nd1 N3 81.92(7) . . ?
O2 Nd1 N1 126.10(7) . . ?
O1 Nd1 N1 76.57(7) . . ?
O3 Nd1 N1 128.14(7) . . ?
N2 Nd1 N1 68.21(7) . . ?
N2 Nd1 N1 129.42(7) 2_656 . ?
N4 Nd1 N1 65.48(7) . . ?
N3 Nd1 N1 63.26(7) . . ?
O2 Nd1 Nd1 90.46(5) . 2_656 ?
O1 Nd1 Nd1 112.06(5) . 2_656 ?
O3 Nd1 Nd1 131.43(5) . 2_656 ?
N2 Nd1 Nd1 40.55(5) . 2_656 ?
N2 Nd1 Nd1 38.73(5) 2_656 2_656 ?
N4 Nd1 Nd1 158.56(6) . 2_656 ?
N3 Nd1 Nd1 77.88(5) . 2_656 ?
N1 Nd1 Nd1 98.59(5) . 2_656 ?
O2 Nd1 K1 109.04(5) . . ?
O1 Nd1 K1 40.20(5) . . ?
O3 Nd1 K1 40.63(5) . . ?
N2 Nd1 K1 119.19(5) . . ?
N2 Nd1 K1 114.09(5) 2_656 . ?
N4 Nd1 K1 51.39(6) . . ?
N3 Nd1 K1 133.20(5) . . ?
N1 Nd1 K1 90.66(5) . . ?
Nd1 Nd1 K1 147.519(13) 2_656 . ?
O6 K1 O1 94.4(3) . . ?
O6 K1 O3 91.7(3) . . ?
O1 K1 O3 64.77(6) . . ?
O6 K1 O4 85.7(3) . . ?
O1 K1 O4 172.50(9) . . ?
O3 K1 O4 107.73(8) . . ?
O1 K1 O5 100.71(9) . . ?
O3 K1 O5 76.13(10) . . ?
O4 K1 O5 76.77(11) . . ?
O1 K1 O7 116.02(17) . . ?
O3 K1 O7 171.4(2) . . ?
O4 K1 O7 71.39(17) . . ?
O5 K1 O7 95.4(2) . . ?
O6 K1 O8 92.8(5) . . ?
O1 K1 O8 110.5(5) . . ?
O3 K1 O8 173.7(5) . . ?
O4 K1 O8 76.9(5) . . ?
O6 K1 N4 148.9(3) . . ?
O1 K1 N4 67.23(6) . . ?
O3 K1 N4 58.12(6) . . ?
O4 K1 N4 109.27(9) . . ?
O5 K1 N4 133.76(10) . . ?
O7 K1 N4 130.5(2) . . ?
O8 K1 N4 116.7(4) . . ?
O6 K1 C27 98.8(4) . . ?
O1 K1 C27 86.44(7) . . ?
O3 K1 C27 23.24(6) . . ?
O4 K1 C27 86.13(8) . . ?
O5 K1 C27 78.60(11) . . ?
O7 K1 C27 157.52(17) . . ?
O8 K1 C27 158.7(4) . . ?
N4 K1 C27 56.93(7) . . ?
O6 K1 C21 144.1(4) . . ?
O1 K1 C21 87.46(7) . . ?
O3 K1 C21 56.79(7) . . ?
O4 K1 C21 88.08(9) . . ?
O5 K1 C21 123.04(11) . . ?
O7 K1 C21 131.1(2) . . ?
O8 K1 C21 120.1(4) . . ?
N4 K1 C21 22.43(7) . . ?
C27 K1 C21 45.42(8) . . ?
O6 K1 C22 120.3(4) . . ?
O1 K1 C22 95.23(6) . . ?
O3 K1 C22 42.95(6) . . ?
O4 K1 C22 78.33(8) . . ?
O5 K1 C22 98.93(11) . . ?
O7 K1 C22 142.35(18) . . ?
O8 K1 C22 136.5(4) . . ?
N4 K1 C22 42.72(7) . . ?
C27 K1 C22 24.09(7) . . ?
C21 K1 C22 24.28(7) . . ?
O6 K1 C9 84.4(3) . . ?
O1 K1 C9 18.50(6) . . ?
O3 K1 C9 80.59(6) . . ?
O4 K1 C9 167.21(9) . . ?
O5 K1 C9 96.41(9) . . ?
O7 K1 C9 98.89(17) . . ?
O8 K1 C9 95.6(4) . . ?
N4 K1 C9 83.30(7) . . ?
C27 K1 C9 103.29(7) . . ?
C21 K1 C9 104.68(7) . . ?
C22 K1 C9 113.72(7) . . ?
C9 O1 Nd1 133.85(17) . . ?
C9 O1 K1 121.82(17) . . ?
Nd1 O1 K1 104.12(7) . . ?
C18 O2 Nd1 146.8(2) . . ?
C27 O3 Nd1 123.35(18) . . ?
C27 O3 K1 102.45(17) . . ?
Nd1 O3 K1 103.48(8) . . ?
C31 O4 C28 106.5(3) . . ?
C31 O4 K1 141.8(3) . . ?
C28 O4 K1 111.1(2) . . ?
C35 O5 C32 103.7(4) . . ?
C35 O5 K1 122.0(4) . . ?
C32 O5 K1 109.7(4) . . ?
C39 O6 C36 118.7(12) . . ?
C39 O6 K1 137.3(9) . . ?
C36 O6 K1 103.6(8) . . ?
C43 O7 C40 111.1(7) . . ?
C43 O7 K1 111.2(6) . . ?
C40 O7 K1 130.7(5) . . ?
C47 O8 C44 101.3(16) . . ?
C47 O8 K1 145.3(17) . . ?
C44 O8 K1 108.1(11) . . ?
C1 N1 C10 110.8(2) . . ?
C1 N1 C19 110.2(2) . . ?
C10 N1 C19 109.6(2) . . ?
C1 N1 Nd1 104.58(16) . . ?
C10 N1 Nd1 115.44(17) . . ?
C19 N1 Nd1 106.11(17) . . ?
C2 N2 C3 111.5(2) . . ?
C2 N2 Nd1 119.03(17) . . ?
C3 N2 Nd1 104.37(16) . . ?
C2 N2 Nd1 120.63(16) . 2_656 ?
C3 N2 Nd1 97.42(15) . 2_656 ?
Nd1 N2 Nd1 100.72(8) . 2_656 ?
C12 N3 C11 115.7(3) . . ?
C12 N3 Nd1 131.1(2) . . ?
C11 N3 Nd1 113.15(18) . . ?
C21 N4 C20 116.9(2) . . ?
C21 N4 Nd1 121.9(2) . . ?
C20 N4 Nd1 118.20(17) . . ?
C21 N4 K1 90.01(18) . . ?
C20 N4 K1 110.54(18) . . ?
Nd1 N4 K1 87.27(7) . . ?
N1 C1 C2 113.7(2) . . ?
N2 C2 C1 112.7(2) . . ?
N2 C3 C4 117.5(2) . . ?
N2 C3 C3 109.39(14) . 2_656 ?
C4 C3 C3 108.6(2) . 2_656 ?
C5 C4 C9 118.7(3) . . ?
C5 C4 C3 119.7(3) . . ?
C9 C4 C3 121.5(2) . . ?
C4 C5 C6 122.9(3) . . ?
C7 C6 C5 118.1(3) . . ?
C8 C7 C6 120.7(3) . . ?
C7 C8 C9 121.8(3) . . ?
O1 C9 C8 120.8(3) . . ?
O1 C9 C4 121.4(2) . . ?
C8 C9 C4 117.8(3) . . ?
O1 C9 K1 39.68(12) . . ?
C8 C9 K1 82.88(17) . . ?
C4 C9 K1 156.8(2) . . ?
N1 C10 C11 112.7(2) . . ?
N3 C11 C10 110.2(2) . . ?
N3 C12 C13 127.4(3) . . ?
C14 C13 C18 119.4(3) . . ?
C14 C13 C12 117.6(3) . . ?
C18 C13 C12 123.0(3) . . ?
C15 C14 C13 121.9(3) . . ?
C14 C15 C16 118.8(3) . . ?
C17 C16 C15 121.0(3) . . ?
C16 C17 C18 121.6(3) . . ?
O2 C18 C17 121.0(3) . . ?
O2 C18 C13 121.8(3) . . ?
C17 C18 C13 117.2(3) . . ?
N1 C19 C20 113.1(2) . . ?
N4 C20 C19 110.7(2) . . ?
N4 C21 C22 125.9(3) . . ?
N4 C21 K1 67.56(17) . . ?
C22 C21 K1 83.27(17) . . ?
C23 C22 C27 119.2(3) . . ?
C23 C22 C21 117.2(3) . . ?
C27 C22 C21 123.6(3) . . ?
C23 C22 K1 136.7(2) . . ?
C27 C22 K1 65.95(16) . . ?
C21 C22 K1 72.45(16) . . ?
C24 C23 C22 122.3(3) . . ?
C23 C24 C25 118.7(3) . . ?
C26 C25 C24 120.9(3) . . ?
C25 C26 C27 122.0(3) . . ?
O3 C27 C26 120.5(3) . . ?
O3 C27 C22 122.6(3) . . ?
C26 C27 C22 116.9(3) . . ?
O3 C27 K1 54.31(14) . . ?
C26 C27 K1 127.2(2) . . ?
C22 C27 K1 89.96(18) . . ?
O4 C28 C29 104.7(3) . . ?
C28 C29 C30 103.4(4) . . ?
C29 C30 C31 104.4(3) . . ?
O4 C31 C30 107.5(3) . . ?
O5 C32 C33 104.9(5) . . ?
C32 C33 C34 104.3(5) . . ?
C35 C34 C33 102.7(5) . . ?
O5 C35 C34 105.5(5) . . ?
O6 C36 C37 100.3(11) . . ?
C38 C37 C36 105.8(12) . . ?
C37 C38 C39 106.7(12) . . ?
O6 C39 C38 102.3(11) . . ?
O7 C40 C41 104.9(6) . . ?
C42 C41 C40 102.7(7) . . ?
C43 C42 C41 100.2(8) . . ?
O7 C43 C42 105.2(8) . . ?
O8 C44 C45 115.5(17) . . ?
C46 C45 C44 99.8(17) . . ?
C45 C46 C47 106.2(18) . . ?
O8 C47 C46 113.5(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C1 C2 -77.3(3) . . . . ?
C19 N1 C1 C2 161.3(2) . . . . ?
Nd1 N1 C1 C2 47.7(3) . . . . ?
C3 N2 C2 C1 -94.8(3) . . . . ?
Nd1 N2 C2 C1 26.8(3) . . . . ?
Nd1 N2 C2 C1 151.99(19) 2_656 . . . ?
N1 C1 C2 N2 -53.0(3) . . . . ?
C2 N2 C3 C4 50.6(3) . . . . ?
Nd1 N2 C3 C4 -79.1(2) . . . . ?
Nd1 N2 C3 C4 177.7(2) 2_656 . . . ?
C2 N2 C3 C3 174.9(2) . . . 2_656 ?
Nd1 N2 C3 C3 45.2(3) . . . 2_656 ?
Nd1 N2 C3 C3 -57.9(3) 2_656 . . 2_656 ?
N2 C3 C4 C5 -122.5(3) . . . . ?
C3 C3 C4 C5 112.8(3) 2_656 . . . ?
N2 C3 C4 C9 60.5(4) . . . . ?
C3 C3 C4 C9 -64.3(3) 2_656 . . . ?
C9 C4 C5 C6 0.5(5) . . . . ?
C3 C4 C5 C6 -176.7(3) . . . . ?
C4 C5 C6 C7 0.5(5) . . . . ?
C5 C6 C7 C8 -1.0(5) . . . . ?
C6 C7 C8 C9 0.5(5) . . . . ?
Nd1 O1 C9 C8 167.1(2) . . . . ?
K1 O1 C9 C8 -19.0(4) . . . . ?
Nd1 O1 C9 C4 -11.9(4) . . . . ?
K1 O1 C9 C4 161.9(2) . . . . ?
Nd1 O1 C9 K1 -173.9(3) . . . . ?
C7 C8 C9 O1 -178.6(3) . . . . ?
C7 C8 C9 C4 0.4(5) . . . . ?
C7 C8 C9 K1 169.3(3) . . . . ?
C5 C4 C9 O1 178.2(3) . . . . ?
C3 C4 C9 O1 -4.8(4) . . . . ?
C5 C4 C9 C8 -0.9(4) . . . . ?
C3 C4 C9 C8 176.2(3) . . . . ?
C5 C4 C9 K1 -151.7(4) . . . . ?
C3 C4 C9 K1 25.4(7) . . . . ?
C1 N1 C10 C11 92.6(3) . . . . ?
C19 N1 C10 C11 -145.6(3) . . . . ?
Nd1 N1 C10 C11 -26.0(3) . . . . ?
C12 N3 C11 C10 123.2(3) . . . . ?
Nd1 N3 C11 C10 -54.9(3) . . . . ?
N1 C10 C11 N3 53.5(3) . . . . ?
C11 N3 C12 C13 179.8(3) . . . . ?
Nd1 N3 C12 C13 -2.6(4) . . . . ?
N3 C12 C13 C14 176.6(3) . . . . ?
N3 C12 C13 C18 -4.9(5) . . . . ?
C18 C13 C14 C15 1.0(5) . . . . ?
C12 C13 C14 C15 179.6(3) . . . . ?
C13 C14 C15 C16 0.6(5) . . . . ?
C14 C15 C16 C17 -0.7(5) . . . . ?
C15 C16 C17 C18 -0.8(5) . . . . ?
Nd1 O2 C18 C17 -158.3(2) . . . . ?
Nd1 O2 C18 C13 22.0(5) . . . . ?
C16 C17 C18 O2 -177.3(3) . . . . ?
C16 C17 C18 C13 2.4(4) . . . . ?
C14 C13 C18 O2 177.2(3) . . . . ?
C12 C13 C18 O2 -1.2(4) . . . . ?
C14 C13 C18 C17 -2.5(4) . . . . ?
C12 C13 C18 C17 179.0(3) . . . . ?
C1 N1 C19 C20 -167.2(2) . . . . ?
C10 N1 C19 C20 70.7(3) . . . . ?
Nd1 N1 C19 C20 -54.6(3) . . . . ?
C21 N4 C20 C19 172.6(3) . . . . ?
Nd1 N4 C20 C19 -26.6(3) . . . . ?
K1 N4 C20 C19 71.7(3) . . . . ?
N1 C19 C20 N4 56.6(3) . . . . ?
C20 N4 C21 C22 -176.1(3) . . . . ?
Nd1 N4 C21 C22 23.9(4) . . . . ?
K1 N4 C21 C22 -62.9(3) . . . . ?
C20 N4 C21 K1 -113.2(2) . . . . ?
Nd1 N4 C21 K1 86.80(16) . . . . ?
N4 C21 C22 C23 -169.9(3) . . . . ?
K1 C21 C22 C23 134.1(2) . . . . ?
N4 C21 C22 C27 12.2(5) . . . . ?
K1 C21 C22 C27 -43.7(3) . . . . ?
N4 C21 C22 K1 55.9(3) . . . . ?
C27 C22 C23 C24 -1.0(5) . . . . ?
C21 C22 C23 C24 -178.9(3) . . . . ?
K1 C22 C23 C24 -85.9(4) . . . . ?
C22 C23 C24 C25 0.1(5) . . . . ?
C23 C24 C25 C26 0.8(5) . . . . ?
C24 C25 C26 C27 -0.7(5) . . . . ?
Nd1 O3 C27 C26 128.3(2) . . . . ?
K1 O3 C27 C26 -116.1(3) . . . . ?
Nd1 O3 C27 C22 -52.9(3) . . . . ?
K1 O3 C27 C22 62.6(3) . . . . ?
Nd1 O3 C27 K1 -115.5(2) . . . . ?
C25 C26 C27 O3 178.6(3) . . . . ?
C25 C26 C27 C22 -0.2(4) . . . . ?
C25 C26 C27 K1 112.3(3) . . . . ?
C23 C22 C27 O3 -177.8(3) . . . . ?
C21 C22 C27 O3 0.0(4) . . . . ?
K1 C22 C27 O3 -46.1(2) . . . . ?
C23 C22 C27 C26 1.0(4) . . . . ?
C21 C22 C27 C26 178.8(3) . . . . ?
K1 C22 C27 C26 132.6(3) . . . . ?
C23 C22 C27 K1 -131.6(2) . . . . ?
C21 C22 C27 K1 46.2(3) . . . . ?
C31 O4 C28 C29 37.5(5) . . . . ?
K1 O4 C28 C29 -149.2(3) . . . . ?
O4 C28 C29 C30 -33.1(4) . . . . ?
C28 C29 C30 C31 17.2(5) . . . . ?
C28 O4 C31 C30 -26.1(5) . . . . ?
K1 O4 C31 C30 164.0(3) . . . . ?
C29 C30 C31 O4 4.9(5) . . . . ?
C35 O5 C32 C33 -40.5(7) . . . . ?
K1 O5 C32 C33 91.3(5) . . . . ?
O5 C32 C33 C34 21.0(8) . . . . ?
C32 C33 C34 C35 4.6(8) . . . . ?
C32 O5 C35 C34 44.1(7) . . . . ?
K1 O5 C35 C34 -80.0(6) . . . . ?
C33 C34 C35 O5 -29.7(8) . . . . ?
C39 O6 C36 C37 27(2) . . . . ?
K1 O6 C36 C37 -158.5(12) . . . . ?
O6 C36 C37 C38 -20.1(19) . . . . ?
C36 C37 C38 C39 10(2) . . . . ?
C36 O6 C39 C38 -21(2) . . . . ?
K1 O6 C39 C38 167.0(15) . . . . ?
C37 C38 C39 O6 5(2) . . . . ?
C43 O7 C40 C41 -0.1(9) . . . . ?
K1 O7 C40 C41 -147.5(6) . . . . ?
O7 C40 C41 C42 -23.8(8) . . . . ?
C40 C41 C42 C43 37.0(9) . . . . ?
C40 O7 C43 C42 24.7(11) . . . . ?
K1 O7 C43 C42 178.7(7) . . . . ?
C41 C42 C43 O7 -38.1(11) . . . . ?
C47 O8 C44 C45 20(3) . . . . ?
K1 O8 C44 C45 -141.6(19) . . . . ?
O8 C44 C45 C46 -19(3) . . . . ?
C44 C45 C46 C47 10(3) . . . . ?
C44 O8 C47 C46 -12(3) . . . . ?
K1 O8 C47 C46 135(3) . . . . ?
C45 C46 C47 O8 1(4) . . . . ?

_refine_diff_density_max         2.049
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.125



####################################################################### 
# 
# 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_bch11
_database_code_depnum_ccdc_archive 'CCDC 2013180'
loop_
_audit_author_name
_audit_author_address
'Rosario Scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_audit_creation_date             2020-03-19
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C66 H78 Eu2 K2 N8 O9'
_chemical_formula_sum            'C66 H78 Eu2 K2 N8 O9'
_chemical_formula_weight         1509.48
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54 H54 N8 O6 K2 Eu2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   16.1474(4)
_cell_length_b                   26.3520(7)
_cell_length_c                   16.7297(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.589(2)
_cell_angle_gamma                90
_cell_volume                     7096.0(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11383
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      75.1830
_cell_measurement_theta_min      4.0480
_shelx_estimated_absorpt_T_max   0.125
_shelx_estimated_absorpt_T_min   0.058
_exptl_absorpt_coefficient_mu    14.031
_exptl_absorpt_correction_T_max  0.159
_exptl_absorpt_correction_T_min  0.038
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense black'
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3064
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 3 -11 0.1567
9 -2 4 0.1778
1 -3 10 0.1048
-10 -3 -2 0.2127
-10 5 -1 0.2115
-10 7 0 0.2103
-2 16 3 0.1372
0 -16 -3 0.1369
-1 -11 -8 0.1503
-3 12 8 0.1324
0 11 8 0.1272
-6 -14 0 0.1514
-3 -16 1 0.1252
0 -17 1 0.1303
1 17 -1 0.1517
1 11 -8 0.1594
-10 -5 3 0.1791
-5 -10 7 0.1182
-3 -11 8 0.1056
-1 0 -11 0.1352
-8 1 -6 0.2068
1 0 -11 0.1523
-3 0 11 0.0983
-10 1 5 0.1878
1 -14 -6 0.1481
-4 14 5 0.1323
-2 14 6 0.1301
2 -15 5 0.1299
-1 -16 5 0.1209
-1 15 -5 0.1575

_exptl_crystal_size_max          0.473
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.254
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.2857 3.4331 -10.6352 -0.6750 -0.7125 0.1918
9.4812 -1.7807 3.6860 0.1484 0.1582 -0.9762
1.3737 -3.4602 10.4031 0.6455 0.6816 -0.3446
-9.8821 -3.0301 -2.2096 0.1630 -0.1924 0.9677
-9.9952 4.5199 -0.7263 -0.1373 0.1589 0.9777
-9.5049 7.0619 -0.1411 -0.2407 0.2799 0.9294
-1.7232 16.2703 2.9557 -0.6410 0.7493 0.1664
-0.0693 -16.3007 -3.2532 0.6499 -0.7600 0.0091
-1.0000 -11.0011 -8.0000 0.1757 -0.9523 0.2089
-3.0000 12.0008 7.9998 -0.1771 1.0129 0.1737
0.0000 11.0010 8.0000 -0.1638 0.9596 -0.1142
-6.0000 -14.0005 -0.0002 0.7612 -0.3944 0.5164
-3.0000 -16.0002 1.0000 0.8711 -0.4020 0.2054
-0.0000 -16.9999 1.0002 0.8844 -0.4553 -0.0825
1.0000 17.0000 -1.0002 -0.8964 0.4480 -0.0122
1.0000 10.9991 -8.0002 -0.9316 -0.2782 0.1012
-10.0000 -5.0005 2.9996 0.5076 0.1474 0.8706
-5.0000 -9.9996 7.0000 0.8830 0.2619 0.3009
-3.0000 -10.9993 8.0001 0.9556 0.2928 0.0883
-1.0000 -0.0015 -11.0002 -0.5077 -0.8386 0.3079
-8.0000 0.9986 -6.0005 -0.2370 -0.3716 0.8778
1.0000 -0.0013 -11.0001 -0.5316 -0.8533 0.1184
-3.0000 0.0011 11.0000 0.5556 0.8679 0.0710
-10.0000 0.9998 4.9995 0.3066 0.4890 0.8541
1.0000 -14.0007 -5.9999 0.3940 -0.9070 -0.0305
-4.0000 14.0003 4.9997 -0.4054 0.8521 0.3340
-2.0000 14.0006 5.9998 -0.3821 0.9144 0.1252
2.0000 -14.9992 5.0004 0.9510 -0.0997 -0.3421
-1.0000 -15.9995 5.0002 1.0361 -0.1090 -0.0616
-1.0000 14.9993 -5.0003 -0.9630 0.0924 0.2473

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_number            7266
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.228
_diffrn_reflns_theta_min         4.968
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -22.00   1.00    3.98    --  -40.66 -38.00-150.00   93
  2  ω   -114.00 -23.00   1.00    3.98    --  -40.66 -38.00 120.00   91
  3  ω    -84.00 -20.00   1.00    3.98    --  -40.66 -38.00  30.00   64
  4  ω    -68.00  32.00   1.00    3.98    --  -40.66  57.00   0.00  100
  5  ω     54.00 102.00   1.00    3.98    --   40.66-144.00 120.00   48
  6  ω     46.00  96.00   1.00    3.98    --   40.66-125.00-150.00   50
  7  ω     29.00 105.00   1.00   15.90    --  112.00 -94.00 -90.00   76
  8  ω     96.00 121.00   1.00   15.90    --  112.00-125.00 120.00   25
  9  ω     39.00 114.00   1.00   15.90    --  112.00 -30.00-150.00   75
 10  ω     49.00  77.00   1.00   15.90    --  112.00-125.00 120.00   28
 11  ω     30.00 145.00   1.00   15.90    --  112.00 -15.00  30.00  115
 12  ω     44.00 137.00   1.00   15.90    --  112.00 -61.00 -60.00   93
 13  ω     49.00 130.00   1.00   15.90    --  112.00 -45.00 120.00   81
 14  ω    148.00 175.00   1.00   15.90    --  112.00 125.00 -30.00   27
 15  ω     83.00 116.00   1.00   15.90    --  112.00-125.00  60.00   33
 16  ω    124.00 175.00   1.00   15.90    --  112.00 125.00 -90.00   51
 17  ω     92.00 120.00   1.00   15.90    --  112.00-125.00-120.00   28
 18  ω    108.00 134.00   1.00   15.90    --  112.00 125.00 -30.00   26
 19  ω     42.00 157.00   1.00   15.90    --  112.00 -15.00 -90.00  115
 20  ω     88.00 141.00   1.00   15.90    --  112.00 -77.00   0.00   53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0119621000
_diffrn_orient_matrix_UB_12      -0.0492466000
_diffrn_orient_matrix_UB_13      0.0472492000
_diffrn_orient_matrix_UB_21      -0.0073277000
_diffrn_orient_matrix_UB_22      0.0313070000
_diffrn_orient_matrix_UB_23      0.0769007000
_diffrn_orient_matrix_UB_31      -0.0947290000
_diffrn_orient_matrix_UB_32      0.0037148000
_diffrn_orient_matrix_UB_33      -0.0193776000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6816
_reflns_number_total             7266
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.653
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7266
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0523
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1036P)²+15.1136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1476
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C33_$1-C33
 1.54 with sigma of 0.02
 C34-C34_$1
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C33 \\sim C34 \\sim C32 \\sim O5: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 2A
4. Others
 Sof(H32C)=Sof(H32D)=Sof(C34)=Sof(H34A)=Sof(H34B)=1-FVAR(1)
 Sof(H32A)=Sof(H32B)=Sof(C33)=Sof(H33A)=Sof(H33B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B),
 C20(H20A,H20B), C30(H30A,H30B), C31(H31A,H31B), C28(H28A,H28B), C29(H29A,H29B),
  C32(H32C,H32D), C32(H32A,H32B), C34(H34A,H34B), C33(H33A,H33B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C14(H14), C15(H15),
 C16(H16), C17(H17), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.56753(2) 0.62808(2) 0.58808(2) 0.03004(11) Uani 1 1 d . . . . .
K1 K 0.40103(5) 0.68449(4) 0.47105(5) 0.0385(2) Uani 1 1 d . . . . .
O1 O 0.4186(2) 0.63301(13) 0.6067(2) 0.0421(7) Uani 1 1 d . . . . .
O2 O 0.5449(2) 0.71653(12) 0.5454(2) 0.0418(7) Uani 1 1 d . . . . .
O3 O 0.5148(2) 0.61528(12) 0.44888(19) 0.0378(6) Uani 1 1 d . . . . .
N1 N 0.6972(2) 0.58079(16) 0.6843(2) 0.0406(8) Uani 1 1 d . . . . .
N2 N 0.5374(3) 0.61723(16) 0.7429(2) 0.0388(8) Uani 1 1 d . . . . .
N3 N 0.7096(2) 0.67824(16) 0.5981(2) 0.0409(8) Uani 1 1 d . . . . .
N4 N 0.6065(2) 0.53619(13) 0.5384(2) 0.0341(7) Uani 1 1 d . . . . .
C1 C 0.6679(3) 0.5700(2) 0.7640(3) 0.0452(10) Uani 1 1 d . . . . .
H1A H 0.716646 0.564680 0.802905 0.054 Uiso 1 1 calc R U . . .
H1B H 0.635244 0.538173 0.761054 0.054 Uiso 1 1 calc R U . . .
C2 C 0.6148(3) 0.6122(2) 0.7943(3) 0.0485(11) Uani 1 1 d . . . . .
H2A H 0.601801 0.604712 0.849951 0.058 Uiso 1 1 calc R U . . .
H2B H 0.645896 0.644630 0.794802 0.058 Uiso 1 1 calc R U . . .
C3 C 0.4700(3) 0.61331(18) 0.7773(3) 0.0393(9) Uani 1 1 d . . . . .
H3 H 0.475949 0.608694 0.833778 0.047 Uiso 1 1 calc R U . . .
C4 C 0.3858(3) 0.61500(17) 0.7411(3) 0.0374(9) Uani 1 1 d . . . . .
C5 C 0.3224(3) 0.6058(2) 0.7918(3) 0.0514(12) Uani 1 1 d . . . . .
H5 H 0.337031 0.599841 0.847097 0.062 Uiso 1 1 calc R U . . .
C6 C 0.2393(3) 0.6051(3) 0.7642(4) 0.0571(13) Uani 1 1 d . . . . .
H6 H 0.197490 0.598991 0.799882 0.068 Uiso 1 1 calc R U . . .
C7 C 0.2186(3) 0.6136(2) 0.6838(3) 0.0470(11) Uani 1 1 d . . . . .
H7 H 0.161861 0.612768 0.663679 0.056 Uiso 1 1 calc R U . . .
C8 C 0.2786(3) 0.62323(16) 0.6327(3) 0.0419(10) Uani 1 1 d . . . . .
H8 H 0.261981 0.629365 0.577733 0.050 Uiso 1 1 calc R U . . .
C9 C 0.3646(3) 0.62446(14) 0.6580(3) 0.0345(9) Uani 1 1 d . . . . .
C10 C 0.7699(3) 0.6148(2) 0.6933(3) 0.0443(10) Uani 1 1 d . . . . .
H10A H 0.820429 0.594360 0.707245 0.053 Uiso 1 1 calc R U . . .
H10B H 0.763071 0.638720 0.737858 0.053 Uiso 1 1 calc R U . . .
C11 C 0.7810(3) 0.6448(2) 0.6168(3) 0.0456(10) Uani 1 1 d . . . . .
H11A H 0.832468 0.665305 0.623950 0.055 Uiso 1 1 calc R U . . .
H11B H 0.786605 0.621052 0.571653 0.055 Uiso 1 1 calc R U . . .
C12 C 0.7250(3) 0.7257(2) 0.5950(3) 0.0471(11) Uani 1 1 d . . . . .
H12 H 0.781530 0.735119 0.605896 0.057 Uiso 1 1 calc R U . . .
C13 C 0.6676(3) 0.7668(2) 0.5771(3) 0.0481(11) Uani 1 1 d . . . . .
C14 C 0.6998(5) 0.8162(2) 0.5830(4) 0.0669(16) Uani 1 1 d . . . . .
H14 H 0.756913 0.820300 0.600104 0.080 Uiso 1 1 calc R U . . .
C15 C 0.6542(6) 0.8583(3) 0.5659(5) 0.077(2) Uani 1 1 d . . . . .
H15 H 0.678845 0.890957 0.570768 0.093 Uiso 1 1 calc R U . . .
C16 C 0.5691(5) 0.8529(2) 0.5405(4) 0.0657(16) Uani 1 1 d . . . . .
H16 H 0.535580 0.882004 0.529053 0.079 Uiso 1 1 calc R U . . .
C17 C 0.5352(4) 0.8052(2) 0.5324(3) 0.0519(12) Uani 1 1 d . . . . .
H17 H 0.478464 0.802208 0.512932 0.062 Uiso 1 1 calc R U . . .
C18 C 0.5810(3) 0.76019(16) 0.5518(2) 0.0391(9) Uani 1 1 d . . . . .
C19 C 0.7202(2) 0.53356(18) 0.6485(3) 0.0436(10) Uani 1 1 d . . . . .
H19A H 0.746242 0.511179 0.690862 0.052 Uiso 1 1 calc R U . . .
H19B H 0.761968 0.540456 0.609698 0.052 Uiso 1 1 calc R U . . .
C20 C 0.6450(3) 0.50542(18) 0.6046(3) 0.0415(9) Uani 1 1 d . . . . .
H20A H 0.663964 0.472751 0.583234 0.050 Uiso 1 1 calc R U . . .
H20B H 0.603252 0.497965 0.643213 0.050 Uiso 1 1 calc R U . . .
C21 C 0.5943(2) 0.51445(15) 0.4711(3) 0.0355(8) Uani 1 1 d . . . . .
H21 H 0.609128 0.479602 0.469460 0.043 Uiso 1 1 calc R U . . .
C22 C 0.5604(2) 0.53647(15) 0.3961(2) 0.0330(8) Uani 1 1 d . . . . .
C23 C 0.5640(3) 0.50626(17) 0.3272(3) 0.0404(9) Uani 1 1 d . . . . .
H23 H 0.585655 0.472838 0.332965 0.048 Uiso 1 1 calc R U . . .
C24 C 0.5373(3) 0.52321(19) 0.2515(3) 0.0437(10) Uani 1 1 d . . . . .
H24 H 0.540688 0.501981 0.206027 0.052 Uiso 1 1 calc R U . . .
C25 C 0.5050(3) 0.57234(18) 0.2433(3) 0.0405(9) Uani 1 1 d . . . . .
H25 H 0.486996 0.584799 0.191501 0.049 Uiso 1 1 calc R U . . .
C26 C 0.4991(3) 0.60277(17) 0.3092(3) 0.0362(8) Uani 1 1 d . . . . .
H26 H 0.477230 0.636044 0.301591 0.043 Uiso 1 1 calc R U . . .
C27 C 0.5246(2) 0.58638(16) 0.3885(2) 0.0326(8) Uani 1 1 d . . . . .
O4 O 0.4294(2) 0.73563(15) 0.3417(2) 0.0497(8) Uani 1 1 d . . . . .
C30 C 0.5370(4) 0.7414(2) 0.2542(3) 0.0530(12) Uani 1 1 d . . . . .
H30A H 0.570261 0.769646 0.234504 0.064 Uiso 1 1 calc R U . . .
H30B H 0.568884 0.709426 0.251246 0.064 Uiso 1 1 calc R U . . .
C31 C 0.5144(3) 0.7514(2) 0.3393(3) 0.0524(12) Uani 1 1 d . . . . .
H31A H 0.550916 0.731673 0.378203 0.063 Uiso 1 1 calc R U . . .
H31B H 0.520352 0.787864 0.352438 0.063 Uiso 1 1 calc R U . . .
C28 C 0.3882(3) 0.7448(2) 0.2644(3) 0.0485(11) Uani 1 1 d . . . . .
H28A H 0.365838 0.779761 0.260871 0.058 Uiso 1 1 calc R U . . .
H28B H 0.341805 0.720580 0.253266 0.058 Uiso 1 1 calc R U . . .
C29 C 0.4534(4) 0.7374(3) 0.2061(3) 0.0651(16) Uani 1 1 d . . . . .
H29A H 0.448273 0.763810 0.163882 0.078 Uiso 1 1 calc R U . . .
H29B H 0.447157 0.703679 0.180140 0.078 Uiso 1 1 calc R U . . .
O5 O 0.250000 0.73390(19) 0.500000 0.0465(10) Uani 1 2 d S TU P A .
C32 C 0.2669(5) 0.7653(3) 0.5676(4) 0.0746(18) Uani 1 1 d . U . . .
H32C H 0.316780 0.753013 0.600154 0.089 Uiso 0.50(2) 1 calc R U P A 2
H32D H 0.219356 0.765115 0.601422 0.089 Uiso 0.50(2) 1 calc R U P A 2
H32A H 0.327487 0.768740 0.581081 0.089 Uiso 0.50(2) 1 calc R U P A 1
H32B H 0.240793 0.751850 0.614749 0.089 Uiso 0.50(2) 1 calc R U P A 1
C34 C 0.2816(8) 0.8185(6) 0.5373(7) 0.088(4) Uani 0.50(2) 1 d D U P A 2
H34A H 0.339269 0.823160 0.522679 0.105 Uiso 0.50(2) 1 calc R U P A 2
H34B H 0.268253 0.844644 0.576713 0.105 Uiso 0.50(2) 1 calc R U P A 2
C33 C 0.2308(15) 0.8128(7) 0.5422(8) 0.102(5) Uani 0.50(2) 1 d D U P A 1
H33A H 0.250821 0.841427 0.576755 0.122 Uiso 0.50(2) 1 calc R U P A 1
H33B H 0.169291 0.811865 0.537240 0.122 Uiso 0.50(2) 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
Eu1 K1 3.5255(9) . ?
Eu1 O1 2.453(3) . ?
Eu1 O2 2.457(3) . ?
Eu1 O3 2.438(3) . ?
Eu1 N1 2.826(4) . ?
Eu1 N2 2.688(4) . ?
Eu1 N3 2.642(4) . ?
Eu1 N4 2.652(4) . ?
K1 O1 2.640(3) . ?
K1 O2 2.683(3) . ?
K1 O3 2.636(3) . ?
K1 O4 2.621(3) . ?
K1 O5 2.840(3) . ?
O1 C9 1.290(6) . ?
O2 C18 1.290(5) . ?
O3 C27 1.285(5) . ?
N1 C1 1.478(6) . ?
N1 C10 1.474(6) . ?
N1 C19 1.442(6) . ?
N2 C2 1.466(6) . ?
N2 C3 1.276(6) . ?
N3 C11 1.465(7) . ?
N3 C12 1.276(7) . ?
N4 C20 1.469(5) . ?
N4 C21 1.266(6) . ?
C1 C2 1.517(8) . ?
C3 C4 1.444(7) . ?
C4 C5 1.402(6) . ?
C4 C9 1.427(7) . ?
C5 C6 1.384(8) . ?
C6 C7 1.378(8) . ?
C7 C8 1.367(7) . ?
C8 C9 1.420(7) . ?
C10 C11 1.527(7) . ?
C12 C13 1.441(8) . ?
C13 C14 1.404(7) . ?
C13 C18 1.439(7) . ?
C14 C15 1.349(11) . ?
C15 C16 1.413(11) . ?
C16 C17 1.371(8) . ?
C17 C18 1.423(7) . ?
C19 C20 1.556(6) . ?
C21 C22 1.448(6) . ?
C22 C23 1.407(6) . ?
C22 C27 1.439(6) . ?
C23 C24 1.378(7) . ?
C24 C25 1.398(7) . ?
C25 C26 1.373(7) . ?
C26 C27 1.424(6) . ?
O4 C31 1.437(7) . ?
O4 C28 1.427(6) . ?
C30 C31 1.520(7) . ?
C30 C29 1.520(8) . ?
C28 C29 1.504(8) . ?
O5 C32 1.410(7) . ?
O5 C32 1.410(7) 2_556 ?
C32 C34 1.514(18) . ?
C32 C33 1.43(2) . ?
C34 C34 1.546(18) 2_556 ?
C33 C33 1.587(19) 2_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 K1 48.43(8) . . ?
O1 Eu1 O2 82.10(11) . . ?
O1 Eu1 N1 129.79(11) . . ?
O1 Eu1 N2 68.19(12) . . ?
O1 Eu1 N3 145.16(12) . . ?
O1 Eu1 N4 110.37(11) . . ?
O2 Eu1 K1 49.42(8) . . ?
O2 Eu1 N1 132.07(11) . . ?
O2 Eu1 N2 110.31(12) . . ?
O2 Eu1 N3 69.62(12) . . ?
O2 Eu1 N4 143.96(11) . . ?
O3 Eu1 K1 48.34(7) . . ?
O3 Eu1 O1 81.82(11) . . ?
O3 Eu1 O2 79.69(11) . . ?
O3 Eu1 N1 132.00(11) . . ?
O3 Eu1 N2 146.02(12) . . ?
O3 Eu1 N3 111.41(12) . . ?
O3 Eu1 N4 69.40(10) . . ?
N1 Eu1 K1 178.11(8) . . ?
N2 Eu1 K1 113.03(9) . . ?
N2 Eu1 N1 65.63(12) . . ?
N3 Eu1 K1 116.37(9) . . ?
N3 Eu1 N1 65.44(12) . . ?
N3 Eu1 N2 102.43(12) . . ?
N3 Eu1 N4 104.47(12) . . ?
N4 Eu1 K1 113.63(8) . . ?
N4 Eu1 N1 65.92(11) . . ?
N4 Eu1 N2 105.69(12) . . ?
O1 K1 Eu1 44.05(7) . . ?
O1 K1 O2 74.56(10) . . ?
O1 K1 O5 97.09(9) . . ?
O2 K1 Eu1 44.07(7) . . ?
O2 K1 O5 120.03(10) . . ?
O3 K1 Eu1 43.72(7) . . ?
O3 K1 O1 74.77(10) . . ?
O3 K1 O2 72.26(10) . . ?
O3 K1 O5 163.50(12) . . ?
O4 K1 Eu1 119.96(8) . . ?
O4 K1 O1 163.81(11) . . ?
O4 K1 O2 91.06(11) . . ?
O4 K1 O3 93.99(11) . . ?
O4 K1 O5 96.57(10) . . ?
O5 K1 Eu1 136.52(3) . . ?
Eu1 O1 K1 87.52(10) . . ?
C9 O1 Eu1 142.8(3) . . ?
C9 O1 K1 129.0(3) . . ?
Eu1 O2 K1 86.51(10) . . ?
C18 O2 Eu1 140.1(3) . . ?
C18 O2 K1 133.4(3) . . ?
Eu1 O3 K1 87.94(10) . . ?
C27 O3 Eu1 141.0(3) . . ?
C27 O3 K1 130.6(3) . . ?
C1 N1 Eu1 108.8(3) . . ?
C10 N1 Eu1 109.7(3) . . ?
C10 N1 C1 109.5(4) . . ?
C19 N1 Eu1 110.3(3) . . ?
C19 N1 C1 108.7(4) . . ?
C19 N1 C10 109.7(4) . . ?
C2 N2 Eu1 111.4(3) . . ?
C3 N2 Eu1 132.1(3) . . ?
C3 N2 C2 116.5(4) . . ?
C11 N3 Eu1 112.2(3) . . ?
C12 N3 Eu1 131.1(3) . . ?
C12 N3 C11 116.5(4) . . ?
C20 N4 Eu1 111.4(3) . . ?
C21 N4 Eu1 131.9(3) . . ?
C21 N4 C20 116.6(4) . . ?
N1 C1 C2 113.0(4) . . ?
N2 C2 C1 110.3(4) . . ?
N2 C3 C4 128.1(4) . . ?
C5 C4 C3 116.7(4) . . ?
C5 C4 C9 119.3(4) . . ?
C9 C4 C3 123.9(4) . . ?
C6 C5 C4 122.4(5) . . ?
C7 C6 C5 118.5(5) . . ?
C8 C7 C6 120.8(5) . . ?
C7 C8 C9 122.9(5) . . ?
O1 C9 C4 123.8(4) . . ?
O1 C9 C8 120.2(4) . . ?
C8 C9 C4 116.1(4) . . ?
N1 C10 C11 112.1(4) . . ?
N3 C11 C10 110.3(4) . . ?
N3 C12 C13 128.4(4) . . ?
C14 C13 C12 117.0(5) . . ?
C14 C13 C18 118.6(6) . . ?
C18 C13 C12 124.4(4) . . ?
C15 C14 C13 123.7(7) . . ?
C14 C15 C16 118.8(6) . . ?
C17 C16 C15 119.6(6) . . ?
C16 C17 C18 123.0(6) . . ?
O2 C18 C13 123.6(4) . . ?
O2 C18 C17 120.2(5) . . ?
C17 C18 C13 116.3(4) . . ?
N1 C19 C20 113.0(3) . . ?
N4 C20 C19 111.1(4) . . ?
N4 C21 C22 127.6(4) . . ?
C23 C22 C21 116.5(4) . . ?
C23 C22 C27 119.1(4) . . ?
C27 C22 C21 124.4(4) . . ?
C24 C23 C22 122.6(4) . . ?
C23 C24 C25 118.5(4) . . ?
C26 C25 C24 120.7(4) . . ?
C25 C26 C27 122.5(4) . . ?
O3 C27 C22 123.0(4) . . ?
O3 C27 C26 120.6(4) . . ?
C26 C27 C22 116.4(4) . . ?
C31 O4 K1 113.7(3) . . ?
C28 O4 K1 137.3(3) . . ?
C28 O4 C31 107.6(4) . . ?
C29 C30 C31 103.8(4) . . ?
O4 C31 C30 106.2(4) . . ?
O4 C28 C29 105.4(4) . . ?
C28 C29 C30 106.6(5) . . ?
K1 O5 K1 125.42(19) 2_556 . ?
C32 O5 K1 104.3(3) . 2_556 ?
C32 O5 K1 107.0(3) . . ?
C32 O5 K1 107.0(3) 2_556 2_556 ?
C32 O5 K1 104.3(3) 2_556 . ?
C32 O5 C32 108.1(8) . 2_556 ?
O5 C32 K1 52.5(2) . 2_556 ?
O5 C32 C34 107.5(6) . . ?
O5 C32 C33 103.1(8) . . ?
C34 C32 K1 130.3(5) . 2_556 ?
C33 C32 K1 100.8(10) . 2_556 ?
C32 C34 C34 99.2(6) . 2_556 ?
C32 C33 C33 94.9(11) . 2_556 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Eu1 O1 C9 C4 13.3(7) . . . . ?
Eu1 O1 C9 C8 -165.6(3) . . . . ?
Eu1 O2 C18 C13 16.2(7) . . . . ?
Eu1 O2 C18 C17 -164.7(3) . . . . ?
Eu1 O3 C27 C22 21.6(7) . . . . ?
Eu1 O3 C27 C26 -158.9(3) . . . . ?
Eu1 N1 C1 C2 -39.5(5) . . . . ?
Eu1 N1 C10 C11 -36.6(5) . . . . ?
Eu1 N1 C19 C20 -34.8(4) . . . . ?
Eu1 N2 C2 C1 -53.3(5) . . . . ?
Eu1 N2 C3 C4 -1.9(8) . . . . ?
Eu1 N3 C11 C10 -55.1(4) . . . . ?
Eu1 N3 C12 C13 -6.6(7) . . . . ?
Eu1 N4 C20 C19 -53.4(4) . . . . ?
Eu1 N4 C21 C22 6.5(6) . . . . ?
K1 O1 C9 C4 -153.6(3) . . . . ?
K1 O1 C9 C8 27.5(6) . . . . ?
K1 O2 C18 C13 -163.3(3) . . . . ?
K1 O2 C18 C17 15.8(6) . . . . ?
K1 O3 C27 C22 -148.9(3) . . . . ?
K1 O3 C27 C26 30.6(6) . . . . ?
K1 O4 C31 C30 137.0(4) . . . . ?
K1 O4 C28 C29 -133.7(5) . . . . ?
K1 O5 C32 K1 -134.7(3) . . . 2_556 ?
K1 O5 C32 C34 -127.8(7) 2_556 . . . ?
K1 O5 C32 C34 97.6(7) . . . . ?
K1 O5 C32 C33 131.7(8) . . . . ?
K1 O5 C32 C33 -93.6(9) 2_556 . . . ?
K1 C32 C34 C34 -19.9(17) 2_556 . . 2_556 ?
K1 C32 C33 C33 -100.2(17) 2_556 . . 2_556 ?
N1 C1 C2 N2 65.0(5) . . . . ?
N1 C10 C11 N3 63.1(5) . . . . ?
N1 C19 C20 N4 61.4(5) . . . . ?
N2 C3 C4 C5 175.3(5) . . . . ?
N2 C3 C4 C9 -3.6(8) . . . . ?
N3 C12 C13 C14 175.7(5) . . . . ?
N3 C12 C13 C18 -6.1(8) . . . . ?
N4 C21 C22 C23 171.2(4) . . . . ?
N4 C21 C22 C27 -8.4(7) . . . . ?
C1 N1 C10 C11 -156.0(4) . . . . ?
C1 N1 C19 C20 84.4(5) . . . . ?
C2 N2 C3 C4 -177.8(5) . . . . ?
C3 N2 C2 C1 123.4(5) . . . . ?
C3 C4 C5 C6 -178.4(5) . . . . ?
C3 C4 C9 O1 -0.7(7) . . . . ?
C3 C4 C9 C8 178.2(4) . . . . ?
C4 C5 C6 C7 0.3(9) . . . . ?
C5 C4 C9 O1 -179.6(4) . . . . ?
C5 C4 C9 C8 -0.7(6) . . . . ?
C5 C6 C7 C8 -1.0(9) . . . . ?
C6 C7 C8 C9 0.9(8) . . . . ?
C7 C8 C9 O1 179.0(4) . . . . ?
C7 C8 C9 C4 0.0(6) . . . . ?
C9 C4 C5 C6 0.5(8) . . . . ?
C10 N1 C1 C2 80.5(5) . . . . ?
C10 N1 C19 C20 -155.8(4) . . . . ?
C11 N3 C12 C13 179.1(5) . . . . ?
C12 N3 C11 C10 120.3(5) . . . . ?
C12 C13 C14 C15 178.0(6) . . . . ?
C12 C13 C18 O2 2.8(7) . . . . ?
C12 C13 C18 C17 -176.5(4) . . . . ?
C13 C14 C15 C16 0.0(11) . . . . ?
C14 C13 C18 O2 -179.1(5) . . . . ?
C14 C13 C18 C17 1.7(7) . . . . ?
C14 C15 C16 C17 -1.2(11) . . . . ?
C15 C16 C17 C18 2.8(9) . . . . ?
C16 C17 C18 O2 177.8(5) . . . . ?
C16 C17 C18 C13 -3.0(7) . . . . ?
C18 C13 C14 C15 -0.4(9) . . . . ?
C19 N1 C1 C2 -159.7(4) . . . . ?
C19 N1 C10 C11 84.8(5) . . . . ?
C20 N4 C21 C22 -177.7(4) . . . . ?
C21 N4 C20 C19 129.9(4) . . . . ?
C21 C22 C23 C24 -177.2(4) . . . . ?
C21 C22 C27 O3 -4.3(6) . . . . ?
C21 C22 C27 C26 176.2(4) . . . . ?
C22 C23 C24 C25 -0.3(7) . . . . ?
C23 C22 C27 O3 176.1(4) . . . . ?
C23 C22 C27 C26 -3.5(6) . . . . ?
C23 C24 C25 C26 -0.8(7) . . . . ?
C24 C25 C26 C27 -0.4(7) . . . . ?
C25 C26 C27 O3 -177.1(4) . . . . ?
C25 C26 C27 C22 2.5(6) . . . . ?
C27 C22 C23 C24 2.5(7) . . . . ?
O4 C28 C29 C30 -18.7(7) . . . . ?
C31 O4 C28 C29 31.8(6) . . . . ?
C31 C30 C29 C28 -0.3(7) . . . . ?
C28 O4 C31 C30 -32.3(6) . . . . ?
C29 C30 C31 O4 19.2(6) . . . . ?
O5 C32 C34 C34 35.4(14) . . . 2_556 ?
O5 C32 C33 C33 -46.5(19) . . . 2_556 ?
C32 O5 C32 K1 113.6(2) 2_556 . . 2_556 ?
C32 O5 C32 C34 -14.2(6) 2_556 . . . ?
C32 O5 C32 C33 19.9(8) 2_556 . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.536 0.000 0.500 463.9 71.7 '1.8 THF'
2 -0.829 0.500 0.000 463.9 71.7 '1.8 THF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.991
_oxdiff_exptl_absorpt_empirical_full_min 0.562
####################################################################### 
# 
# 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_dt483
_database_code_depnum_ccdc_archive 'CCDC 2013182'
loop_
_audit_author_name
_audit_author_address
'Rosario Scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_audit_creation_date             2020-06-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72.48 H90.96 K2 N8 O10.62 Sm2'
_chemical_formula_sum            'C72.48 H90.96 K2 N8 O10.62 Sm2'
_chemical_formula_weight         1623.07
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C66 H78 N8 O9 K2 Sm2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.9002(3)
_cell_length_b                   19.5477(2)
_cell_length_c                   21.6120(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.4471(18)
_cell_angle_gamma                90
_cell_volume                     7268.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13969
_cell_measurement_temperature    140.01(10)
_cell_measurement_theta_max      72.5780
_cell_measurement_theta_min      3.3940
_shelx_estimated_absorpt_T_max   0.523
_shelx_estimated_absorpt_T_min   0.057
_exptl_absorpt_coefficient_mu    13.537
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_correction_T_min  0.110
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3315
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 11 0 0.0396
-6 -11 0 0.0450
-3 -1 14 0.2504
10 -4 0 0.0420
-10 4 0 0.0109
1 -13 0 0.0382
3 6 -12 0.2049
4 -2 -14 0.2307

_exptl_crystal_size_max          0.499
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.055
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.0162 10.7556 -0.2584 0.2326 0.9711 0.0545
-5.9976 -10.7507 0.1830 -0.2326 -0.9713 -0.0490
-3.4442 -0.9853 13.8503 0.0094 0.0440 -0.9990
10.3712 -4.4860 0.2007 -0.8909 0.4241 -0.1624
-10.4096 4.4806 -0.1021 0.8919 -0.4246 0.1554
0.6745 -12.6482 0.3909 -0.7515 -0.6424 -0.1504
2.9618 6.1047 -12.1684 0.2881 0.2450 0.9257
3.9104 -2.2435 -13.7449 -0.2194 -0.1890 0.9572

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            25997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.753
_diffrn_reflns_theta_min         3.422
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -76.00  -9.00   1.00    4.00    --  -40.91 125.00 -90.00   67
  2  ω   -115.00 -35.00   1.00    4.00    --  -40.91 -38.00 120.00   80
  3  ω   -118.00  -3.00   1.00    4.00    --  -40.91 -19.00-180.00  115
  4  ω      8.00  46.00   1.00    4.00    --   40.91 -99.00  60.00   38
  5  ω     38.00  96.00   1.00    4.00    --   40.91-125.00-180.00   58
  6  ω     49.00 109.00   1.00   16.00    --  105.15-111.00 150.00   60
  7  ω     29.00 129.00   1.00   16.00    --  105.15 -30.00 150.00  100
  8  ω    112.00 139.00   1.00   16.00    --  105.15  77.00 -60.00   27
  9  ω     62.00  87.00   1.00   16.00    --  105.15 178.00 -60.00   25
 10  ω    105.00 130.00   1.00   16.00    --  105.15 111.00-180.00   25
 11  ω     64.00 109.00   1.00   16.00    --  105.15-111.00   0.00   45
 12  ω    118.00 177.00   1.00   16.00    --  105.15  77.00 -90.00   59
 13  ω    106.00 136.00   1.00   16.00    --  105.15 111.00-150.00   30
 14  ω    142.00 169.00   1.00   16.00    --  105.15 111.00-150.00   27
 15  ω     76.00 108.00   1.00   16.00    --  105.15-111.00-120.00   32
 16  ω     36.00 130.00   1.00   16.00    --  105.15 -30.00-120.00   94
 17  ω    107.00 175.00   1.00   16.00    --  105.15 111.00 -60.00   68
 18  ω     40.00 106.00   1.00   16.00    --  105.15 -94.00  30.00   66
 19  ω     48.00 131.00   1.00   16.00    --  105.15 -77.00-150.00   83
 20  ω     33.00 133.00   1.00   16.00    --  105.15 -30.00 -30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0615618000
_diffrn_orient_matrix_UB_12      0.0558023000
_diffrn_orient_matrix_UB_13      -0.0106632000
_diffrn_orient_matrix_UB_21      0.0642033000
_diffrn_orient_matrix_UB_22      0.0549247000
_diffrn_orient_matrix_UB_23      0.0230517000
_diffrn_orient_matrix_UB_31      -0.0103077000
_diffrn_orient_matrix_UB_32      0.0090495000
_diffrn_orient_matrix_UB_33      -0.0740470000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6443
_reflns_number_total             7150
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Shedlrick, 2015)'
_refine_diff_density_max         1.608
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         7150
_refine_ls_number_restraints     312
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0398
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0821P)²+15.9840P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1152
_refine_ls_wR_factor_ref         0.1203
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O4-C28 = O4-C31 = O5-C32 = O5-C35 = O6-C39 = O6-C36
 1.43 with sigma of 0.02
 C35-C34 = C34-C33 = C33-C32 = C29-C28 = C30-C29 = C31-C30 = C39-C38 = C38-C37
 = C37-C36
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim O5 \\sim O6 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O4) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C35) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(O6)
\\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 K1, O4, O5, O6, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: K1(0.77) K2(0.23) O4(0.77) O5(0.77) O6(0.77) C28(0.77) H28A(0.77)
 H28B(0.77) C29(0.77) H29A(0.77) H29B(0.77) C30(0.77) H30A(0.77) H30B(0.77)
 C31(0.77) H31A(0.77) H31B(0.77) C32(0.77) H32A(0.77) H32B(0.77) C33(0.77)
 H33A(0.77) H33B(0.77) C34(0.77) H34A(0.77) H34B(0.77) C35(0.77) H35A(0.77)
 H35B(0.77) C36(0.77) H36A(0.77) H36B(0.77) C37(0.77) H37A(0.77) H37B(0.77)
 C38(0.77) H38A(0.77) H38B(0.77) C39(0.77) H39A(0.77) H39B(0.77)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C21(H21)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B),
 C20(H20A,H20B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16),
 C17(H17), C23(H23), C24(H24), C25(H25), C26(H26)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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 0.50772(2) 0.33624(2) 0.34140(2) 0.02837(9) Uani 1 1 d . . . . .
K1 K 0.49138(9) 0.22713(7) 0.49071(7) 0.0511(3) Uani 0.77 1 d . . P A 1
K2 K 0.4253(4) 0.1756(3) 0.4073(4) 0.0718(16) Uani 0.23 1 d . . P A 2
O1 O 0.41928(17) 0.42557(15) 0.31441(15) 0.0357(6) Uani 1 1 d . . . . .
O2 O 0.41156(18) 0.30411(15) 0.38035(16) 0.0389(6) Uani 1 1 d . . . . .
O3 O 0.54397(17) 0.22757(14) 0.39442(14) 0.0361(6) Uani 1 1 d . . . . .
O4 O 0.3605(7) 0.1525(5) 0.4345(5) 0.121(2) Uani 0.77 1 d D U P A 1
O5 O 0.5639(8) 0.1412(7) 0.6024(6) 0.156(3) Uani 0.77 1 d D U P A 1
O6 O 0.4314(5) 0.2381(5) 0.5857(4) 0.103(2) Uani 0.77 1 d D U P A 1
N1 N 0.6662(2) 0.34463(18) 0.41115(18) 0.0335(7) Uani 1 1 d . . . . .
N2 N 0.5717(2) 0.45660(18) 0.33636(17) 0.0329(7) Uani 1 1 d . . . . .
N3 N 0.5525(2) 0.36765(19) 0.46867(18) 0.0372(8) Uani 1 1 d . . . . .
N4 N 0.57450(18) 0.28747(16) 0.27610(16) 0.0296(6) Uani 1 1 d . . . . .
C1 C 0.6995(2) 0.4115(2) 0.4079(2) 0.0379(9) Uani 1 1 d . . . . .
H1A H 0.752629 0.404844 0.410596 0.046 Uiso 1 1 calc R U . . .
H1B H 0.703710 0.439057 0.447683 0.046 Uiso 1 1 calc R U . . .
C2 C 0.6521(2) 0.4507(2) 0.3439(2) 0.0363(8) Uani 1 1 d . . . . .
H2A H 0.674571 0.496884 0.346168 0.044 Uiso 1 1 calc R U . . .
H2B H 0.653334 0.426655 0.304025 0.044 Uiso 1 1 calc R U . . .
C3 C 0.5455(3) 0.5182(2) 0.33174(19) 0.0341(8) Uani 1 1 d . . . . .
H3 H 0.580218 0.553892 0.333232 0.041 Uiso 1 1 calc R U . . .
C4 C 0.4689(3) 0.5389(2) 0.3245(2) 0.0349(8) Uani 1 1 d . . . . .
C5 C 0.4535(3) 0.6091(2) 0.3240(2) 0.0445(10) Uani 1 1 d . . . . .
H5 H 0.493485 0.640830 0.328533 0.053 Uiso 1 1 calc R U . . .
C6 C 0.3828(3) 0.6335(3) 0.3173(3) 0.0501(11) Uani 1 1 d . . . . .
H6 H 0.373249 0.681275 0.316155 0.060 Uiso 1 1 calc R U . . .
C7 C 0.3251(3) 0.5866(3) 0.3123(2) 0.0464(11) Uani 1 1 d . . . . .
H7 H 0.276308 0.602933 0.309033 0.056 Uiso 1 1 calc R U . . .
C8 C 0.3371(3) 0.5177(2) 0.3118(2) 0.0416(10) Uani 1 1 d . . . . .
H8 H 0.296370 0.487132 0.307998 0.050 Uiso 1 1 calc R U . . .
C9 C 0.4091(3) 0.4907(2) 0.31690(19) 0.0352(8) Uani 1 1 d . . . . .
C10 C 0.6821(3) 0.3281(2) 0.4830(2) 0.0388(9) Uani 1 1 d . . . . .
H10A H 0.738326 0.334059 0.511486 0.047 Uiso 1 1 calc R U . . .
H10B H 0.669063 0.279506 0.485834 0.047 Uiso 1 1 calc R U . . .
C11 C 0.6368(3) 0.3721(3) 0.5113(2) 0.0440(10) Uani 1 1 d . . . . .
H11A H 0.647551 0.357029 0.558078 0.053 Uiso 1 1 calc R U . . .
H11B H 0.653862 0.420279 0.513489 0.053 Uiso 1 1 calc R U . . .
C12 C 0.5073(3) 0.3933(3) 0.4936(2) 0.0415(10) Uani 1 1 d . . . . .
H12 H 0.532474 0.415524 0.539189 0.050 Uiso 1 1 calc R U . A 1
C13 C 0.4231(3) 0.3906(2) 0.4626(2) 0.0372(9) Uani 1 1 d . . . . .
C14 C 0.3837(3) 0.4325(3) 0.4908(2) 0.0456(10) Uani 1 1 d . . . . .
H14 H 0.412891 0.461454 0.527944 0.055 Uiso 1 1 calc R U . . .
C15 C 0.3043(3) 0.4328(3) 0.4662(3) 0.0477(11) Uani 1 1 d . . . . .
H15 H 0.279041 0.460838 0.486876 0.057 Uiso 1 1 calc R U . . .
C16 C 0.2608(3) 0.3920(2) 0.4109(3) 0.0454(10) Uani 1 1 d . . . . .
H16 H 0.205651 0.393153 0.392889 0.054 Uiso 1 1 calc R U . . .
C17 C 0.2970(3) 0.3500(2) 0.3820(3) 0.0422(10) Uani 1 1 d . . . . .
H17 H 0.266087 0.322310 0.344410 0.051 Uiso 1 1 calc R U . . .
C18 C 0.3792(3) 0.3467(2) 0.4066(2) 0.0371(9) Uani 1 1 d . . . . .
C19 C 0.6975(2) 0.2902(2) 0.3817(2) 0.0343(8) Uani 1 1 d . . . . .
H19A H 0.689432 0.245276 0.398820 0.041 Uiso 1 1 calc R U . . .
H19B H 0.754154 0.297086 0.397201 0.041 Uiso 1 1 calc R U . . .
C20 C 0.6591(2) 0.2893(2) 0.3034(2) 0.0316(8) Uani 1 1 d . . . . .
H20A H 0.675390 0.330569 0.286076 0.038 Uiso 1 1 calc R U . . .
H20B H 0.677691 0.248734 0.287015 0.038 Uiso 1 1 calc R U . . .
C21 C 0.5457(2) 0.21596(19) 0.2619(2) 0.0302(8) Uani 1 1 d . . . . .
H21 H 0.555943 0.199650 0.222474 0.036 Uiso 1 1 calc R U . . .
C22 C 0.5799(2) 0.16272(19) 0.3180(2) 0.0337(9) Uani 1 1 d . . . . .
C23 C 0.6139(3) 0.1044(2) 0.3072(2) 0.0406(9) Uani 1 1 d . . . . .
H23 H 0.618584 0.099260 0.265333 0.049 Uiso 1 1 calc R U . . .
C24 C 0.6420(3) 0.0522(2) 0.3559(3) 0.0483(11) Uani 1 1 d . . . . .
H24 H 0.665551 0.012487 0.347393 0.058 Uiso 1 1 calc R U . . .
C25 C 0.6348(3) 0.0595(2) 0.4160(2) 0.0452(10) Uani 1 1 d . . . . .
H25 H 0.652206 0.024053 0.449006 0.054 Uiso 1 1 calc R U . . .
C26 C 0.6021(2) 0.1184(2) 0.4294(2) 0.0380(9) Uani 1 1 d . . . . .
H26 H 0.598632 0.122825 0.471792 0.046 Uiso 1 1 calc R U . . .
C27 C 0.5740(2) 0.1718(2) 0.3813(2) 0.0342(8) Uani 1 1 d . . . . .
C28 C 0.3405(9) 0.1378(7) 0.3633(6) 0.116(3) Uani 0.77 1 d D U P A 1
H28A H 0.362655 0.172813 0.343326 0.139 Uiso 0.77 1 calc R U P A 1
H28B H 0.283348 0.136912 0.337125 0.139 Uiso 0.77 1 calc R U P A 1
C29 C 0.3765(9) 0.0654(7) 0.3624(6) 0.119(3) Uani 0.77 1 d D U P A 1
H29A H 0.343642 0.038055 0.322222 0.142 Uiso 0.77 1 calc R U P A 1
H29B H 0.429962 0.068650 0.365036 0.142 Uiso 0.77 1 calc R U P A 1
C30 C 0.3751(9) 0.0380(8) 0.4279(7) 0.123(3) Uani 0.77 1 d D U P A 1
H30A H 0.428196 0.024933 0.460175 0.147 Uiso 0.77 1 calc R U P A 1
H30B H 0.341429 -0.002957 0.418112 0.147 Uiso 0.77 1 calc R U P A 1
C31 C 0.3434(9) 0.0946(6) 0.4589(7) 0.118(3) Uani 0.77 1 d D U P A 1
H31A H 0.286581 0.089803 0.444297 0.141 Uiso 0.77 1 calc R U P A 1
H31B H 0.369221 0.093525 0.509214 0.141 Uiso 0.77 1 calc R U P A 1
C32 C 0.5089(12) 0.0903(11) 0.6084(9) 0.181(4) Uani 0.77 1 d D U P A 1
H32A H 0.500036 0.053240 0.574861 0.217 Uiso 0.77 1 calc R U P A 1
H32B H 0.458404 0.112550 0.598971 0.217 Uiso 0.77 1 calc R U P A 1
C33 C 0.5422(12) 0.0611(11) 0.6792(9) 0.178(4) Uani 0.77 1 d D U P A 1
H33A H 0.511923 0.075849 0.704804 0.214 Uiso 0.77 1 calc R U P A 1
H33B H 0.543381 0.010444 0.678181 0.214 Uiso 0.77 1 calc R U P A 1
C34 C 0.6194(11) 0.0890(9) 0.7083(9) 0.152(4) Uani 0.77 1 d D U P A 1
H34A H 0.657519 0.052999 0.711141 0.182 Uiso 0.77 1 calc R U P A 1
H34B H 0.631687 0.105553 0.754950 0.182 Uiso 0.77 1 calc R U P A 1
C35 C 0.6251(9) 0.1464(8) 0.6658(7) 0.123(3) Uani 0.77 1 d D U P A 1
H35A H 0.622658 0.190607 0.687049 0.148 Uiso 0.77 1 calc R U P A 1
H35B H 0.675182 0.144043 0.661352 0.148 Uiso 0.77 1 calc R U P A 1
C36 C 0.3488(7) 0.2577(6) 0.5536(6) 0.099(3) Uani 0.77 1 d D U P A 1
H36A H 0.315747 0.216496 0.537443 0.119 Uiso 0.77 1 calc R U P A 1
H36B H 0.338979 0.288047 0.514231 0.119 Uiso 0.77 1 calc R U P A 1
C37 C 0.3307(7) 0.2943(6) 0.6063(5) 0.097(2) Uani 0.77 1 d D U P A 1
H37A H 0.275569 0.288174 0.598362 0.116 Uiso 0.77 1 calc R U P A 1
H37B H 0.342343 0.343749 0.607418 0.116 Uiso 0.77 1 calc R U P A 1
C38 C 0.3853(7) 0.2586(6) 0.6717(5) 0.098(2) Uani 0.77 1 d D U P A 1
H38A H 0.355425 0.228539 0.689063 0.117 Uiso 0.77 1 calc R U P A 1
H38B H 0.413630 0.292813 0.707087 0.117 Uiso 0.77 1 calc R U P A 1
C39 C 0.4434(8) 0.2155(7) 0.6532(5) 0.101(3) Uani 0.77 1 d D U P A 1
H39A H 0.497631 0.224140 0.686012 0.121 Uiso 0.77 1 calc R U P A 1
H39B H 0.432280 0.166051 0.653232 0.121 Uiso 0.77 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
Sm1 Sm1 3.8389(4) 2_655 ?
Sm1 K1 3.9853(13) . ?
Sm1 K2 4.019(6) . ?
Sm1 O1 2.319(3) . ?
Sm1 O2 2.382(3) . ?
Sm1 O3 2.376(3) . ?
Sm1 N1 2.745(4) . ?
Sm1 N2 2.668(3) . ?
Sm1 N3 2.595(4) . ?
Sm1 N4 2.551(3) 2_655 ?
Sm1 N4 2.443(3) . ?
K1 O2 2.693(3) . ?
K1 O3 2.651(3) . ?
K1 O4 2.690(9) . ?
K1 O5 2.790(11) . ?
K1 O6 2.733(8) . ?
K1 N3 3.092(4) . ?
K1 C12 3.260(5) . ?
K1 C13 3.404(5) . ?
K1 C18 3.174(5) . ?
K1 C27 3.500(5) . ?
K2 O2 2.567(7) . ?
K2 O3 2.580(7) . ?
K2 C18 3.454(7) . ?
K2 C27 3.086(7) . ?
O1 C9 1.292(5) . ?
O2 C18 1.296(5) . ?
O3 C27 1.312(5) . ?
O4 C28 1.454(12) . ?
O4 C31 1.345(12) . ?
O5 C32 1.483(15) . ?
O5 C35 1.383(14) . ?
O6 C36 1.473(12) . ?
O6 C39 1.448(11) . ?
N1 C1 1.466(6) . ?
N1 C10 1.490(5) . ?
N1 C19 1.482(5) . ?
N2 C2 1.464(5) . ?
N2 C3 1.290(6) . ?
N3 C11 1.476(6) . ?
N3 C12 1.285(6) . ?
N4 C20 1.459(5) . ?
N4 C21 1.485(5) . ?
C1 C2 1.508(6) . ?
C3 C4 1.448(6) . ?
C4 C5 1.403(6) . ?
C4 C9 1.427(6) . ?
C5 C6 1.369(7) . ?
C6 C7 1.394(8) . ?
C7 C8 1.368(7) . ?
C8 C9 1.421(6) . ?
C10 C11 1.510(6) . ?
C12 C13 1.449(6) . ?
C13 C14 1.406(6) . ?
C13 C18 1.434(7) . ?
C14 C15 1.369(7) . ?
C15 C16 1.389(8) . ?
C16 C17 1.372(7) . ?
C17 C18 1.420(7) . ?
C19 C20 1.540(5) . ?
C21 C21 1.586(7) 2_655 ?
C21 C22 1.525(6) . ?
C22 C23 1.377(6) . ?
C22 C27 1.428(7) . ?
C23 C24 1.404(7) . ?
C24 C25 1.369(7) . ?
C25 C26 1.392(7) . ?
C26 C27 1.412(6) . ?
C28 C29 1.574(15) . ?
C29 C30 1.524(13) . ?
C30 C31 1.538(14) . ?
C32 C33 1.505(16) . ?
C33 C34 1.437(16) . ?
C34 C35 1.483(14) . ?
C36 C37 1.501(13) . ?
C37 C38 1.529(13) . ?
C38 C39 1.562(13) . ?

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
Sm1 Sm1 K1 146.60(2) 2_655 . ?
Sm1 Sm1 K2 119.28(11) 2_655 . ?
O1 Sm1 Sm1 90.07(7) . 2_655 ?
O1 Sm1 K1 108.50(7) . . ?
O1 Sm1 K2 109.43(12) . . ?
O1 Sm1 O2 73.23(10) . . ?
O1 Sm1 O3 145.95(10) . . ?
O1 Sm1 N1 127.04(10) . . ?
O1 Sm1 N2 67.51(10) . . ?
O1 Sm1 N3 88.47(11) . . ?
O1 Sm1 N4 87.27(10) . 2_655 ?
O1 Sm1 N4 129.76(10) . . ?
O2 Sm1 Sm1 128.29(8) . 2_655 ?
O2 Sm1 K1 41.11(8) . . ?
O2 Sm1 K2 37.28(11) . . ?
O2 Sm1 N1 129.83(11) . . ?
O2 Sm1 N2 132.23(10) . . ?
O2 Sm1 N3 69.48(11) . . ?
O2 Sm1 N4 90.78(11) . 2_655 ?
O2 Sm1 N4 138.90(11) . . ?
O3 Sm1 Sm1 112.35(7) . 2_655 ?
O3 Sm1 K1 40.05(7) . . ?
O3 Sm1 K2 37.56(12) . . ?
O3 Sm1 O2 72.76(10) . . ?
O3 Sm1 N1 75.95(10) . . ?
O3 Sm1 N2 139.72(10) . . ?
O3 Sm1 N3 78.33(11) . . ?
O3 Sm1 N4 94.66(10) . 2_655 ?
O3 Sm1 N4 79.33(10) . . ?
N1 Sm1 Sm1 99.56(8) . 2_655 ?
N1 Sm1 K1 91.14(8) . . ?
N1 Sm1 K2 110.31(13) . . ?
N2 Sm1 Sm1 78.50(7) . 2_655 ?
N2 Sm1 K1 133.89(7) . . ?
N2 Sm1 K2 162.21(13) . . ?
N2 Sm1 N1 63.87(10) . . ?
N3 Sm1 Sm1 160.64(8) . 2_655 ?
N3 Sm1 K1 50.86(9) . . ?
N3 Sm1 K2 79.25(14) . . ?
N3 Sm1 N1 66.46(11) . . ?
N3 Sm1 N2 83.12(11) . . ?
N4 Sm1 Sm1 40.79(8) . 2_655 ?
N4 Sm1 Sm1 38.74(7) 2_655 2_655 ?
N4 Sm1 K1 112.74(8) 2_655 . ?
N4 Sm1 K1 119.38(8) . . ?
N4 Sm1 K2 105.57(12) . . ?
N4 Sm1 K2 83.96(14) 2_655 . ?
N4 Sm1 N1 130.23(10) 2_655 . ?
N4 Sm1 N1 68.49(11) . . ?
N4 Sm1 N2 112.87(10) 2_655 . ?
N4 Sm1 N2 88.24(10) . . ?
N4 Sm1 N3 160.20(11) 2_655 . ?
N4 Sm1 N3 133.23(11) . . ?
N4 Sm1 N4 61.74(13) . 2_655 ?
O2 K1 Sm1 35.56(6) . . ?
O2 K1 O5 175.6(3) . . ?
O2 K1 O6 111.5(2) . . ?
O2 K1 N3 58.34(10) . . ?
O2 K1 C12 58.23(11) . . ?
O2 K1 C13 44.40(10) . . ?
O2 K1 C18 23.75(11) . . ?
O2 K1 C27 79.47(10) . . ?
O3 K1 Sm1 35.21(6) . . ?
O3 K1 O2 63.74(9) . . ?
O3 K1 O4 102.8(2) . . ?
O3 K1 O5 118.1(3) . . ?
O3 K1 O6 174.8(2) . . ?
O3 K1 N3 65.86(10) . . ?
O3 K1 C12 87.14(11) . . ?
O3 K1 C13 95.42(10) . . ?
O3 K1 C18 85.82(10) . . ?
O3 K1 C27 18.91(9) . . ?
O4 K1 Sm1 106.82(18) . . ?
O4 K1 O2 80.2(2) . . ?
O4 K1 O5 95.5(3) . . ?
O4 K1 O6 78.0(3) . . ?
O4 K1 N3 138.1(2) . . ?
O4 K1 C12 127.5(3) . . ?
O4 K1 C13 102.6(3) . . ?
O4 K1 C18 82.5(2) . . ?
O4 K1 C27 96.4(2) . . ?
O5 K1 Sm1 147.9(3) . . ?
O5 K1 N3 125.9(3) . . ?
O5 K1 C12 125.1(3) . . ?
O5 K1 C13 137.2(3) . . ?
O5 K1 C18 155.7(3) . . ?
O5 K1 C27 101.6(3) . . ?
O6 K1 Sm1 139.59(19) . . ?
O6 K1 O5 66.8(4) . . ?
O6 K1 N3 110.1(2) . . ?
O6 K1 C12 88.4(2) . . ?
O6 K1 C13 79.4(2) . . ?
O6 K1 C18 89.2(2) . . ?
O6 K1 C27 166.2(2) . . ?
N3 K1 Sm1 40.60(7) . . ?
N3 K1 C12 23.15(11) . . ?
N3 K1 C13 43.70(10) . . ?
N3 K1 C18 57.41(11) . . ?
N3 K1 C27 82.58(10) . . ?
C12 K1 Sm1 56.27(8) . . ?
C12 K1 C13 24.99(11) . . ?
C12 K1 C27 104.89(11) . . ?
C13 K1 Sm1 60.26(7) . . ?
C13 K1 C27 114.28(10) . . ?
C18 K1 Sm1 53.11(8) . . ?
C18 K1 C12 46.50(12) . . ?
C18 K1 C13 24.87(12) . . ?
C18 K1 C27 102.70(11) . . ?
C27 K1 Sm1 54.03(7) . . ?
O2 K2 Sm1 34.19(10) . . ?
O2 K2 O3 66.50(17) . . ?
O2 K2 C18 18.24(11) . . ?
O2 K2 C27 89.8(2) . . ?
O3 K2 Sm1 34.15(10) . . ?
O3 K2 C18 81.24(18) . . ?
O3 K2 C27 24.78(11) . . ?
C18 K2 Sm1 51.42(11) . . ?
C27 K2 Sm1 55.84(12) . . ?
C27 K2 C18 105.6(2) . . ?
C9 O1 Sm1 146.7(3) . . ?
Sm1 O2 K1 103.34(11) . . ?
Sm1 O2 K2 108.53(17) . . ?
C18 O2 Sm1 123.6(3) . . ?
C18 O2 K1 99.4(3) . . ?
C18 O2 K2 123.4(3) . . ?
Sm1 O3 K1 104.75(11) . . ?
Sm1 O3 K2 108.29(18) . . ?
C27 O3 Sm1 134.6(3) . . ?
C27 O3 K1 120.2(3) . . ?
C27 O3 K2 99.7(3) . . ?
C28 O4 K1 111.9(7) . . ?
C31 O4 K1 127.2(9) . . ?
C31 O4 C28 104.4(9) . . ?
C32 O5 K1 111.6(10) . . ?
C35 O5 K1 136.3(9) . . ?
C35 O5 C32 106.9(12) . . ?
C36 O6 K1 110.8(6) . . ?
C39 O6 K1 142.3(7) . . ?
C39 O6 C36 104.3(8) . . ?
C1 N1 Sm1 114.8(2) . . ?
C1 N1 C10 109.8(3) . . ?
C1 N1 C19 111.3(3) . . ?
C10 N1 Sm1 105.2(3) . . ?
C19 N1 Sm1 105.1(2) . . ?
C19 N1 C10 110.4(3) . . ?
C2 N2 Sm1 113.2(2) . . ?
C3 N2 Sm1 131.3(3) . . ?
C3 N2 C2 115.5(4) . . ?
Sm1 N3 K1 88.53(11) . . ?
C11 N3 Sm1 118.0(3) . . ?
C11 N3 K1 109.4(3) . . ?
C12 N3 Sm1 123.7(3) . . ?
C12 N3 K1 85.8(3) . . ?
C12 N3 C11 116.6(4) . . ?
Sm1 N4 Sm1 100.47(11) . 2_655 ?
C20 N4 Sm1 119.9(2) . . ?
C20 N4 Sm1 120.5(2) . 2_655 ?
C20 N4 C21 110.7(3) . . ?
C21 N4 Sm1 97.2(2) . 2_655 ?
C21 N4 Sm1 104.7(2) . . ?
N1 C1 C2 113.2(3) . . ?
N2 C2 C1 109.7(3) . . ?
N2 C3 C4 127.2(4) . . ?
C5 C4 C3 117.9(4) . . ?
C5 C4 C9 119.6(4) . . ?
C9 C4 C3 122.4(4) . . ?
C6 C5 C4 122.0(5) . . ?
C5 C6 C7 118.6(4) . . ?
C8 C7 C6 121.4(5) . . ?
C7 C8 C9 121.5(5) . . ?
O1 C9 C4 122.1(4) . . ?
O1 C9 C8 121.1(4) . . ?
C8 C9 C4 116.8(4) . . ?
N1 C10 C11 113.3(4) . . ?
N3 C11 C10 111.1(4) . . ?
N3 C12 K1 71.1(3) . . ?
N3 C12 C13 125.9(4) . . ?
C13 C12 K1 83.1(3) . . ?
C12 C13 K1 71.9(3) . . ?
C14 C13 K1 134.4(3) . . ?
C14 C13 C12 117.2(4) . . ?
C14 C13 C18 119.2(4) . . ?
C18 C13 K1 68.5(2) . . ?
C18 C13 C12 123.6(4) . . ?
C15 C14 C13 121.8(5) . . ?
C14 C15 C16 119.6(4) . . ?
C17 C16 C15 120.4(5) . . ?
C16 C17 C18 122.1(5) . . ?
O2 C18 K1 56.8(2) . . ?
O2 C18 K2 38.3(2) . . ?
O2 C18 C13 122.7(4) . . ?
O2 C18 C17 120.5(4) . . ?
C13 C18 K1 86.6(3) . . ?
C13 C18 K2 121.2(3) . . ?
C17 C18 K1 128.1(3) . . ?
C17 C18 K2 106.3(3) . . ?
C17 C18 C13 116.8(4) . . ?
N1 C19 C20 113.0(3) . . ?
N4 C20 C19 112.5(3) . . ?
N4 C21 C21 108.88(19) . 2_655 ?
N4 C21 C22 118.7(3) . . ?
C22 C21 C21 107.6(3) . 2_655 ?
C23 C22 C21 120.2(4) . . ?
C23 C22 C27 119.6(4) . . ?
C27 C22 C21 120.1(4) . . ?
C22 C23 C24 122.2(4) . . ?
C25 C24 C23 118.7(4) . . ?
C24 C25 C26 120.7(4) . . ?
C25 C26 C27 121.6(4) . . ?
O3 C27 K1 40.9(2) . . ?
O3 C27 K2 55.5(2) . . ?
O3 C27 C22 121.5(4) . . ?
O3 C27 C26 121.3(4) . . ?
C22 C27 K1 156.7(3) . . ?
C22 C27 K2 127.9(3) . . ?
C26 C27 K1 82.4(3) . . ?
C26 C27 K2 88.7(3) . . ?
C26 C27 C22 117.2(4) . . ?
O4 C28 C29 105.5(11) . . ?
C30 C29 C28 97.5(10) . . ?
C29 C30 C31 108.2(11) . . ?
O4 C31 C30 103.5(11) . . ?
O5 C32 C33 109.3(15) . . ?
C34 C33 C32 102.9(15) . . ?
C33 C34 C35 109.7(15) . . ?
O5 C35 C34 108.3(13) . . ?
O6 C36 C37 107.3(9) . . ?
C36 C37 C38 101.8(10) . . ?
C37 C38 C39 106.6(9) . . ?
O6 C39 C38 105.1(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sm1 O1 C9 C4 22.6(7) . . . . ?
Sm1 O1 C9 C8 -157.7(4) . . . . ?
Sm1 O2 C18 K1 -113.0(3) . . . . ?
Sm1 O2 C18 K2 -153.7(5) . . . . ?
Sm1 O2 C18 C13 -53.3(5) . . . . ?
Sm1 O2 C18 C17 128.9(4) . . . . ?
Sm1 O3 C27 K1 -170.8(5) . . . . ?
Sm1 O3 C27 K2 -128.1(4) . . . . ?
Sm1 O3 C27 C22 -11.1(6) . . . . ?
Sm1 O3 C27 C26 168.7(3) . . . . ?
Sm1 N1 C1 C2 -28.0(4) . . . . ?
Sm1 N1 C10 C11 -54.0(4) . . . . ?
Sm1 N1 C19 C20 46.2(4) . . . . ?
Sm1 N2 C2 C1 -53.9(4) . . . . ?
Sm1 N2 C3 C4 -3.3(6) . . . . ?
Sm1 N3 C11 C10 -25.7(5) . . . . ?
Sm1 N3 C12 K1 85.4(3) . . . . ?
Sm1 N3 C12 C13 19.2(7) . . . . ?
Sm1 N4 C20 C19 27.5(4) . . . . ?
Sm1 N4 C20 C19 153.2(3) 2_655 . . . ?
Sm1 N4 C21 C21 -58.1(4) 2_655 . . 2_655 ?
Sm1 N4 C21 C21 44.8(4) . . . 2_655 ?
Sm1 N4 C21 C22 178.4(3) 2_655 . . . ?
Sm1 N4 C21 C22 -78.7(3) . . . . ?
K1 O2 C18 C13 59.8(4) . . . . ?
K1 O2 C18 C17 -118.0(4) . . . . ?
K1 O3 C27 C22 159.7(3) . . . . ?
K1 O3 C27 C26 -20.5(5) . . . . ?
K1 O4 C28 C29 94.6(10) . . . . ?
K1 O4 C31 C30 -89.5(12) . . . . ?
K1 O5 C32 C33 -162.1(15) . . . . ?
K1 O5 C35 C34 163.6(13) . . . . ?
K1 O6 C36 C37 -153.4(7) . . . . ?
K1 O6 C39 C38 171.0(8) . . . . ?
K1 N3 C11 C10 73.3(4) . . . . ?
K1 N3 C12 C13 -66.2(5) . . . . ?
K1 C12 C13 C14 131.3(4) . . . . ?
K1 C12 C13 C18 -47.2(4) . . . . ?
K1 C13 C14 C15 -87.9(6) . . . . ?
K1 C13 C18 O2 -46.4(3) . . . . ?
K1 C13 C18 C17 131.4(4) . . . . ?
K2 O2 C18 C13 100.5(5) . . . . ?
K2 O2 C18 C17 -77.3(5) . . . . ?
K2 O3 C27 C22 117.0(4) . . . . ?
K2 O3 C27 C26 -63.3(4) . . . . ?
O4 C28 C29 C30 27.0(14) . . . . ?
O5 C32 C33 C34 -8(3) . . . . ?
O6 C36 C37 C38 -31.9(11) . . . . ?
N1 C1 C2 N2 54.4(5) . . . . ?
N1 C10 C11 N3 55.9(5) . . . . ?
N1 C19 C20 N4 -52.0(5) . . . . ?
N2 C3 C4 C5 176.6(4) . . . . ?
N2 C3 C4 C9 -4.4(6) . . . . ?
N3 C12 C13 K1 60.7(5) . . . . ?
N3 C12 C13 C14 -168.0(5) . . . . ?
N3 C12 C13 C18 13.5(7) . . . . ?
N4 C21 C22 C23 -123.3(4) . . . . ?
N4 C21 C22 C27 59.1(5) . . . . ?
C1 N1 C10 C11 70.0(5) . . . . ?
C1 N1 C19 C20 -78.7(4) . . . . ?
C2 N2 C3 C4 -179.5(4) . . . . ?
C3 N2 C2 C1 123.0(4) . . . . ?
C3 C4 C5 C6 179.9(4) . . . . ?
C3 C4 C9 O1 -1.6(6) . . . . ?
C3 C4 C9 C8 178.6(4) . . . . ?
C4 C5 C6 C7 1.4(8) . . . . ?
C5 C4 C9 O1 177.3(4) . . . . ?
C5 C4 C9 C8 -2.4(6) . . . . ?
C5 C6 C7 C8 -2.0(8) . . . . ?
C6 C7 C8 C9 0.4(7) . . . . ?
C7 C8 C9 O1 -177.9(4) . . . . ?
C7 C8 C9 C4 1.8(6) . . . . ?
C9 C4 C5 C6 0.8(7) . . . . ?
C10 N1 C1 C2 -146.3(4) . . . . ?
C10 N1 C19 C20 159.1(3) . . . . ?
C11 N3 C12 K1 -109.6(4) . . . . ?
C11 N3 C12 C13 -175.7(4) . . . . ?
C12 N3 C11 C10 168.4(4) . . . . ?
C12 C13 C14 C15 -178.7(4) . . . . ?
C12 C13 C18 K1 48.5(4) . . . . ?
C12 C13 C18 K2 47.6(5) . . . . ?
C12 C13 C18 O2 2.1(7) . . . . ?
C12 C13 C18 C17 180.0(4) . . . . ?
C13 C14 C15 C16 -1.6(7) . . . . ?
C14 C13 C18 K1 -129.9(4) . . . . ?
C14 C13 C18 K2 -130.9(4) . . . . ?
C14 C13 C18 O2 -176.4(4) . . . . ?
C14 C13 C18 C17 1.5(6) . . . . ?
C14 C15 C16 C17 1.8(7) . . . . ?
C15 C16 C17 C18 -0.4(7) . . . . ?
C16 C17 C18 K1 106.9(5) . . . . ?
C16 C17 C18 K2 137.6(4) . . . . ?
C16 C17 C18 O2 176.7(4) . . . . ?
C16 C17 C18 C13 -1.3(7) . . . . ?
C18 C13 C14 C15 -0.2(7) . . . . ?
C19 N1 C1 C2 91.2(4) . . . . ?
C19 N1 C10 C11 -166.9(4) . . . . ?
C20 N4 C21 C21 175.4(4) . . . 2_655 ?
C20 N4 C21 C22 51.9(4) . . . . ?
C21 N4 C20 C19 -94.6(4) . . . . ?
C21 C21 C22 C23 112.6(4) 2_655 . . . ?
C21 C21 C22 C27 -65.0(5) 2_655 . . . ?
C21 C22 C23 C24 -176.2(4) . . . . ?
C21 C22 C27 K1 30.6(9) . . . . ?
C21 C22 C27 K2 64.2(5) . . . . ?
C21 C22 C27 O3 -4.4(6) . . . . ?
C21 C22 C27 C26 175.8(4) . . . . ?
C22 C23 C24 C25 0.4(8) . . . . ?
C23 C22 C27 K1 -147.0(6) . . . . ?
C23 C22 C27 K2 -113.4(4) . . . . ?
C23 C22 C27 O3 178.0(4) . . . . ?
C23 C22 C27 C26 -1.8(6) . . . . ?
C23 C24 C25 C26 -1.7(8) . . . . ?
C24 C25 C26 C27 1.3(7) . . . . ?
C25 C26 C27 K1 167.3(4) . . . . ?
C25 C26 C27 K2 133.3(4) . . . . ?
C25 C26 C27 O3 -179.3(4) . . . . ?
C25 C26 C27 C22 0.5(6) . . . . ?
C27 C22 C23 C24 1.4(7) . . . . ?
C28 O4 C31 C30 43.3(15) . . . . ?
C28 C29 C30 C31 -2.0(15) . . . . ?
C29 C30 C31 O4 -25.5(16) . . . . ?
C31 O4 C28 C29 -46.4(15) . . . . ?
C32 O5 C35 C34 12(2) . . . . ?
C32 C33 C34 C35 15(3) . . . . ?
C33 C34 C35 O5 -18(2) . . . . ?
C35 O5 C32 C33 -3(3) . . . . ?
C36 O6 C39 C38 -30.7(12) . . . . ?
C36 C37 C38 C39 12.3(12) . . . . ?
C37 C38 C39 O6 11.2(13) . . . . ?
C39 O6 C36 C37 40.6(12) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.574
_oxdiff_exptl_absorpt_empirical_full_min 0.385
####################################################################### 
# 
# 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_bch5
_database_code_depnum_ccdc_archive 'CCDC 2013183'
loop_
_audit_author_name
_audit_author_address
'Rosario Scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT220_bch5                
;
PROBLEM: NonSolvent Resd 1  C   Ueq(max) / Ueq(min) Range        6.5 Ratio 
RESPONSE: Some THF molecules are quite disordered and this
causes this large range of Ueq values.
;
_vrf_PLAT410_bch5                
;
PROBLEM: Short Intra H...H Contact  H12A     ..H27A     .       1.83 Ang.  
RESPONSE: These hydrogens were clearly located on the difference
map and then placed on calculated coordinates. This short H...H distance is
not the result of wrongly assigned hydrogens.
;
_vrf_PLAT910_bch5                
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         21 Note  
RESPONSE: These reflections are hidden by the beam stop. This is
quite usual with Mo radiation and the setup of our instrument.
;
# end Validation Reply Form

_audit_creation_date             2020-06-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C86 H118 K4 N8 Nd2 O14'
_chemical_formula_sum            'C86 H118 K4 N8 Nd2 O14'
_chemical_formula_weight         1932.76
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54 H54 O6 N8 K4'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.5916(2)
_cell_length_b                   17.4426(3)
_cell_length_c                   22.1502(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.3459(18)
_cell_angle_gamma                90
_cell_volume                     4459.02(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    33162
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.1540
_cell_measurement_theta_min      3.6060
_shelx_estimated_absorpt_T_max   0.827
_shelx_estimated_absorpt_T_min   0.747
_exptl_absorpt_coefficient_mu    1.403
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1996
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 14 25 0.0684
-9 2 -24 0.0865
-3 -14 -25 0.0757
8 -21 1 0.0722
9 -1 25 0.0536
3 15 -25 0.0968
-7 21 -7 0.1077
-10 20 2 0.1041
-10 1 26 0.0762
-6 -10 27 0.0676
10 -1 -26 0.0985
-10 -12 -17 0.0934
-13 -3 -17 0.0950
6 19 15 0.0821
11 9 17 0.0775
-14 -12 -2 0.1000
-10 -19 -2 0.1006
10 19 2 0.0897
16 5 2 0.0975

_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.141
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.8379 13.6290 24.7981 -0.0247 -0.9549 0.2960
-8.9391 2.2283 -24.2909 0.0228 0.8944 0.4467
-2.6722 -13.9168 -24.6416 0.0246 0.9498 -0.3118
8.4643 -20.9831 0.5074 0.0014 0.0363 -0.9993
8.5906 -0.8318 24.9048 -0.0235 -0.9208 -0.3893
2.9415 14.6418 -24.8706 0.7700 0.4182 0.4820
-6.6686 21.3848 -7.4836 0.1931 0.1042 0.9756
-9.6784 19.8190 2.2653 -0.1182 -0.0650 0.9909
-10.4323 1.4694 25.7206 -0.8340 -0.4536 0.3142
-5.6855 -10.3468 27.0622 -0.8505 -0.4621 -0.2512
10.3934 -1.3242 -25.7884 0.8359 0.4546 -0.3077
-10.0000 -12.0003 -17.0005 -0.3838 0.9110 -0.0284
-13.0000 -3.0003 -17.0002 -0.3600 0.8720 0.3788
6.0000 19.0004 15.0007 0.3599 -0.8397 0.4063
11.0000 9.0003 17.0004 0.3758 -0.8980 -0.1073
-14.0000 -12.0003 -1.9998 -0.7932 0.6009 0.0568
-10.0000 -19.0003 -2.0001 -0.7383 0.5855 -0.3149
10.0000 19.0003 2.0001 0.7383 -0.5855 0.3149
16.0000 5.0002 1.9996 0.7601 -0.5615 -0.3625

_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            70708
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.486
_diffrn_reflns_theta_min         3.531
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -29.00  66.00   1.00   15.00    --  -10.00  77.00  90.00   95
  2  ω     33.00  58.00   1.00   15.00    --  -10.00  57.00-120.00   25
  3  ω    -17.00  30.00   1.00   15.00    --  -10.00 -99.00 120.00   47
  4  ω    -76.00 -47.00   1.00   15.00    --  -10.00 -37.00-180.00   29
  5  ω    -25.00   2.00   1.00   15.00    --  -10.00  77.00 -30.00   27
  6  ω    -98.00 -33.00   1.00   15.00    --  -10.00   0.00   0.00   65
  7  ω     53.00  78.00   1.00   15.00    --  -10.00   0.00   0.00   25
  8  ω     -8.00  29.00   1.00   15.00    --  -10.00 -99.00  30.00   37
  9  ω    -38.00 -11.00   1.00   15.00    --   10.47   0.00-180.00   27
 10  ω    -19.00  38.00   1.00   15.00    --   10.47 -99.00 -90.00   57
 11  ω     58.00  83.00   1.00   15.00    --   10.47 178.00  90.00   25
 12  ω      9.00  34.00   1.00   15.00    --   10.47 -37.00   0.00   25
 13  ω    -13.00  85.00   1.00   15.00    --   10.47  37.00  30.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0440359000
_diffrn_orient_matrix_UB_12      0.0173185000
_diffrn_orient_matrix_UB_13      -0.0155546000
_diffrn_orient_matrix_UB_21      -0.0273909000
_diffrn_orient_matrix_UB_22      -0.0134568000
_diffrn_orient_matrix_UB_23      -0.0279750000
_diffrn_orient_matrix_UB_31      -0.0329686000
_diffrn_orient_matrix_UB_32      0.0342516000
_diffrn_orient_matrix_UB_33      -0.0031145000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9933
_reflns_number_total             11477
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         11477
_refine_ls_number_restraints     431
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0258
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0217P)²+4.2824P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0586
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C48-C47 = C49-C48 = C50-C49
 1.54 with sigma of 0.02
 C54-C53 = C53-C52 = C52-C51
 1.54 with sigma of 0.02
 O9-C54 = O9-C51 = O8-C47 = O8-C50
 1.43 with sigma of 0.02
 C45-C41 \\sim C42-C41 \\sim C43-C42 \\sim C46-C45 \\sim C44-C43 \\sim C46-C44
 with sigma of 0.02
 O7-C41 \\sim O7-C44
 with sigma of 0.02
 O6-C37 \\sim O5-C36 \\sim O6-C40 \\sim O5-C33
 with sigma of 0.02
 C36-C35 \\sim C35-C34 \\sim C34-C33 \\sim C38-C37 \\sim C39-C38 \\sim C40-C39
 with sigma of 0.02
 K1-O6 \\sim K1-O5 \\sim K2-O9 \\sim K2-O8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O5 \\sim O6 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim
C39 \\sim C40: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
C42 \\sim C43 \\sim C45 \\sim C46: within 2A with sigma of 0.005 and sigma for
terminal atoms of 2 within 2A
O8 \\sim O9 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim
C53 \\sim C54: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
4. Rigid body (RIGU) restrains
 O8, O9, C47, C48, C49, C50, C51, C52, C53, C54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O9)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=
 Sof(H53A)=Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=1-FVAR(1)
 Sof(O8)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=Sof(H48B)=Sof(C49)=
 Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=FVAR(1)
 Sof(O6)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=1-FVAR(2)
 Sof(O5)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(C36)=Sof(H36A)=Sof(H36B)=FVAR(2)
 Sof(H41C)=Sof(H41D)=Sof(H44C)=Sof(H44D)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=
 Sof(H46A)=Sof(H46B)=1-FVAR(3)
 Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=
 Sof(H44A)=Sof(H44B)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C41(H41C,H41D), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C44(H44C,H44D),
  C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,
 H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
 C54(H54A,H54B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C15(H15), C16(H16), C17(H17),
 C18(H18), C22(H22), C23(H23), C24(H24), C25(H25)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.50254(2) 0.40725(2) 0.47472(2) 0.01019(3) Uani 1 1 d . . . . .
K1 K 0.48746(4) 0.40396(3) 0.29898(2) 0.01863(9) Uani 1 1 d D . . . .
K2 K 0.81695(4) 0.64027(2) 0.54071(2) 0.01890(9) Uani 1 1 d D . . . .
O1 O 0.36758(11) 0.35487(7) 0.39145(6) 0.0144(3) Uani 1 1 d . . . . .
O2 O 0.63163(11) 0.38133(8) 0.39428(6) 0.0148(3) Uani 1 1 d . . . . .
O3 O 0.62799(12) 0.67849(8) 0.47575(6) 0.0177(3) Uani 1 1 d . . . . .
O4 O 0.30679(13) 0.46359(9) 0.22483(7) 0.0248(3) Uani 1 1 d . . . . .
O5 O 0.4893(5) 0.2924(5) 0.2154(4) 0.0397(10) Uani 0.760(4) 1 d D U P A 1
O6 O 0.4945(15) 0.2976(16) 0.2116(13) 0.0418(14) Uani 0.240(4) 1 d D U P A 2
O7 O 0.62197(15) 0.47998(10) 0.22194(7) 0.0324(4) Uani 1 1 d D . . . .
O8 O 0.9207(2) 0.77083(14) 0.51633(13) 0.0398(6) Uani 0.776(3) 1 d D U P B 1
O9 O 0.9655(8) 0.7468(5) 0.5080(5) 0.0446(13) Uani 0.224(3) 1 d D U P B 2
N1 N 0.55027(14) 0.25919(9) 0.45403(7) 0.0165(3) Uani 1 1 d . . . . .
N2 N 0.67365(13) 0.34953(9) 0.55430(7) 0.0132(3) Uani 1 1 d . . . . .
N3 N 0.67889(13) 0.50130(9) 0.49538(7) 0.0117(3) Uani 1 1 d . . . . .
N4 N 0.50041(13) 0.53499(9) 0.41943(7) 0.0118(3) Uani 1 1 d . . . . .
C1 C 0.32854(16) 0.28833(11) 0.37132(9) 0.0155(4) Uani 1 1 d . . . . .
C2 C 0.22321(17) 0.28471(12) 0.33353(9) 0.0203(4) Uani 1 1 d . . . . .
H2 H 0.183688 0.331244 0.323091 0.024 Uiso 1 1 calc R U . . .
C3 C 0.17505(18) 0.21677(13) 0.31107(11) 0.0270(5) Uani 1 1 d . . . . .
H3 H 0.104075 0.217453 0.285894 0.032 Uiso 1 1 calc R U . . .
C4 C 0.2301(2) 0.14763(13) 0.32522(12) 0.0339(6) Uani 1 1 d . . . . .
H4 H 0.197129 0.100507 0.310704 0.041 Uiso 1 1 calc R U . . .
C5 C 0.3343(2) 0.14914(13) 0.36099(12) 0.0309(5) Uani 1 1 d . . . . .
H5 H 0.373485 0.102036 0.369809 0.037 Uiso 1 1 calc R U . . .
C6 C 0.38496(18) 0.21695(12) 0.38489(10) 0.0213(4) Uani 1 1 d . . . . .
C7 C 0.49590(19) 0.20863(12) 0.42114(10) 0.0233(4) Uani 1 1 d . . . . .
H7 H 0.531784 0.159744 0.420088 0.028 Uiso 1 1 calc R U . . .
C8 C 0.66429(17) 0.23825(11) 0.48281(9) 0.0180(4) Uani 1 1 d . . . . .
H8A H 0.725156 0.261991 0.460427 0.022 Uiso 1 1 calc R U . . .
H8B H 0.673976 0.181910 0.481391 0.022 Uiso 1 1 calc R U . . .
C9 C 0.67760(17) 0.26516(10) 0.54830(9) 0.0168(4) Uani 1 1 d . . . . .
H9A H 0.614910 0.242425 0.569942 0.020 Uiso 1 1 calc R U . . .
H9B H 0.752378 0.246262 0.567998 0.020 Uiso 1 1 calc R U . . .
C10 C 0.65348(16) 0.36951(11) 0.61766(8) 0.0150(4) Uani 1 1 d . . . . .
H10A H 0.728541 0.368124 0.642920 0.018 Uiso 1 1 calc R U . . .
H10B H 0.602791 0.330013 0.633424 0.018 Uiso 1 1 calc R U . . .
C11 C 0.78291(16) 0.38351(11) 0.53722(9) 0.0145(4) Uani 1 1 d . . . . .
H11A H 0.800022 0.362289 0.497575 0.017 Uiso 1 1 calc R U . . .
H11B H 0.846876 0.368373 0.567633 0.017 Uiso 1 1 calc R U . . .
C12 C 0.77918(16) 0.47102(10) 0.53287(8) 0.0135(4) Uani 1 1 d . . . . .
H12A H 0.779080 0.492414 0.574265 0.016 Uiso 1 1 calc R U . . .
H12B H 0.850602 0.489005 0.516046 0.016 Uiso 1 1 calc R U . . .
C13 C 0.71568(15) 0.52713(10) 0.43674(8) 0.0117(3) Uani 1 1 d . . . . .
H13 H 0.764767 0.573751 0.445164 0.014 Uiso 1 1 calc R U . . .
C14 C 0.78866(16) 0.46966(11) 0.40527(8) 0.0132(4) Uani 1 1 d . . . . .
C15 C 0.90228(16) 0.48569(11) 0.39474(8) 0.0159(4) Uani 1 1 d . . . . .
H15 H 0.934666 0.533722 0.407446 0.019 Uiso 1 1 calc R U . . .
C16 C 0.97052(17) 0.43370(12) 0.36615(9) 0.0197(4) Uani 1 1 d . . . . .
H16 H 1.047881 0.446249 0.359096 0.024 Uiso 1 1 calc R U . . .
C17 C 0.92341(17) 0.36332(12) 0.34819(9) 0.0209(4) Uani 1 1 d . . . . .
H17 H 0.969225 0.326942 0.329228 0.025 Uiso 1 1 calc R U . . .
C18 C 0.80994(17) 0.34568(11) 0.35771(9) 0.0174(4) Uani 1 1 d . . . . .
H18 H 0.779173 0.297197 0.345046 0.021 Uiso 1 1 calc R U . . .
C19 C 0.73896(16) 0.39809(10) 0.38581(8) 0.0135(4) Uani 1 1 d . . . . .
C20 C 0.60924(16) 0.55235(10) 0.39315(8) 0.0132(4) Uani 1 1 d . . . . .
H20 H 0.610056 0.520408 0.355706 0.016 Uiso 1 1 calc R U . . .
C21 C 0.61804(16) 0.63558(11) 0.37353(9) 0.0156(4) Uani 1 1 d . . . . .
C22 C 0.61203(17) 0.65453(12) 0.31237(9) 0.0204(4) Uani 1 1 d . . . . .
H22 H 0.607890 0.614580 0.283098 0.024 Uiso 1 1 calc R U . . .
C23 C 0.61192(18) 0.73061(14) 0.29269(10) 0.0274(5) Uani 1 1 d . . . . .
H23 H 0.608432 0.742469 0.250697 0.033 Uiso 1 1 calc R U . . .
C24 C 0.61697(18) 0.78810(13) 0.33554(12) 0.0297(5) Uani 1 1 d . . . . .
H24 H 0.616021 0.840138 0.322844 0.036 Uiso 1 1 calc R U . . .
C25 C 0.62339(18) 0.77115(12) 0.39670(11) 0.0245(5) Uani 1 1 d . . . . .
H25 H 0.627621 0.811882 0.425295 0.029 Uiso 1 1 calc R U . . .
C26 C 0.62381(16) 0.69444(11) 0.41777(9) 0.0166(4) Uani 1 1 d . . . . .
C27 C 0.40214(16) 0.55152(11) 0.37542(8) 0.0149(4) Uani 1 1 d . . . . .
H27A H 0.342299 0.511684 0.378934 0.018 Uiso 1 1 calc R U . . .
H27B H 0.428085 0.547762 0.334185 0.018 Uiso 1 1 calc R U . . .
C28 C 0.20191(19) 0.47851(13) 0.25293(10) 0.0254(5) Uani 1 1 d . . . . .
H28A H 0.187619 0.534370 0.254949 0.031 Uiso 1 1 calc R U . . .
H28B H 0.207800 0.457514 0.294632 0.031 Uiso 1 1 calc R U . . .
C29 C 0.1042(2) 0.43932(16) 0.21373(11) 0.0344(6) Uani 1 1 d . . . . .
H29A H 0.050043 0.413317 0.239043 0.041 Uiso 1 1 calc R U . . .
H29B H 0.060521 0.476640 0.186797 0.041 Uiso 1 1 calc R U . . .
C30 C 0.1674(2) 0.38160(15) 0.17726(11) 0.0341(5) Uani 1 1 d . . . . .
H30A H 0.183076 0.333354 0.200099 0.041 Uiso 1 1 calc R U . . .
H30B H 0.122949 0.369958 0.137978 0.041 Uiso 1 1 calc R U . . .
C31 C 0.2774(2) 0.42390(14) 0.16849(10) 0.0300(5) Uani 1 1 d . . . . .
H31A H 0.339693 0.387705 0.159985 0.036 Uiso 1 1 calc R U . . .
H31B H 0.265275 0.460667 0.134445 0.036 Uiso 1 1 calc R U . . .
C33 C 0.4273(6) 0.2227(4) 0.2142(4) 0.0466(10) Uani 0.760(4) 1 d D U P A 1
H33A H 0.357786 0.225600 0.184738 0.056 Uiso 0.760(4) 1 calc R U P A 1
H33B H 0.402481 0.211079 0.254764 0.056 Uiso 0.760(4) 1 calc R U P A 1
C34 C 0.5098(4) 0.1620(2) 0.1954(2) 0.0431(8) Uani 0.760(4) 1 d D U P A 1
H34A H 0.558701 0.141656 0.230829 0.052 Uiso 0.760(4) 1 calc R U P A 1
H34B H 0.467519 0.119133 0.174064 0.052 Uiso 0.760(4) 1 calc R U P A 1
C35 C 0.5808(3) 0.20550(19) 0.15366(17) 0.0372(8) Uani 0.760(4) 1 d D U P A 1
H35A H 0.540616 0.209281 0.112330 0.045 Uiso 0.760(4) 1 calc R U P A 1
H35B H 0.657712 0.181498 0.151410 0.045 Uiso 0.760(4) 1 calc R U P A 1
C36 C 0.5914(3) 0.2837(2) 0.1845(2) 0.0460(9) Uani 0.760(4) 1 d D U P A 1
H36A H 0.661587 0.285845 0.213560 0.055 Uiso 0.760(4) 1 calc R U P A 1
H36B H 0.596277 0.324902 0.154045 0.055 Uiso 0.760(4) 1 calc R U P A 1
C37 C 0.6106(10) 0.2702(6) 0.2224(6) 0.0402(13) Uani 0.240(4) 1 d D U P A 2
H37A H 0.658387 0.307687 0.247266 0.048 Uiso 0.240(4) 1 calc R U P A 2
H37B H 0.644845 0.263463 0.183436 0.048 Uiso 0.240(4) 1 calc R U P A 2
C38 C 0.6089(10) 0.1956(6) 0.2548(6) 0.0463(16) Uani 0.240(4) 1 d D U P A 2
H38A H 0.605446 0.202271 0.298998 0.056 Uiso 0.240(4) 1 calc R U P A 2
H38B H 0.675848 0.162841 0.247304 0.056 Uiso 0.240(4) 1 calc R U P A 2
C39 C 0.4958(10) 0.1650(8) 0.2236(7) 0.0471(15) Uani 0.240(4) 1 d D U P A 2
H39A H 0.458362 0.130095 0.251160 0.057 Uiso 0.240(4) 1 calc R U P A 2
H39B H 0.510639 0.136181 0.186655 0.057 Uiso 0.240(4) 1 calc R U P A 2
C40 C 0.416(2) 0.2346(11) 0.2068(14) 0.0427(14) Uani 0.240(4) 1 d D U P A 2
H40A H 0.378199 0.229708 0.165104 0.051 Uiso 0.240(4) 1 calc R U P A 2
H40B H 0.356040 0.240017 0.235459 0.051 Uiso 0.240(4) 1 calc R U P A 2
C41 C 0.7459(2) 0.48493(16) 0.23142(11) 0.0356(6) Uani 1 1 d D . . . .
H41A H 0.779909 0.433781 0.240947 0.043 Uiso 0.820(7) 1 calc R U P C 1
H41B H 0.769476 0.520089 0.265443 0.043 Uiso 0.820(7) 1 calc R U P C 1
H41C H 0.782725 0.437559 0.217772 0.043 Uiso 0.180(7) 1 calc R U P C 2
H41D H 0.771715 0.493746 0.274740 0.043 Uiso 0.180(7) 1 calc R U P C 2
C42 C 0.7856(3) 0.5150(3) 0.17359(17) 0.0434(10) Uani 0.820(7) 1 d D U P C 1
H42A H 0.795112 0.473190 0.144192 0.052 Uiso 0.820(7) 1 calc R U P C 1
H42B H 0.859293 0.543651 0.180842 0.052 Uiso 0.820(7) 1 calc R U P C 1
C43 C 0.6839(3) 0.5683(3) 0.1519(2) 0.0467(10) Uani 0.820(7) 1 d D U P C 1
H43A H 0.689529 0.618228 0.173292 0.056 Uiso 0.820(7) 1 calc R U P C 1
H43B H 0.679929 0.577258 0.107608 0.056 Uiso 0.820(7) 1 calc R U P C 1
C44 C 0.5819(2) 0.52221(18) 0.16897(12) 0.0418(6) Uani 1 1 d D . . . .
H44A H 0.517304 0.556507 0.177461 0.050 Uiso 0.820(7) 1 calc R U P C 1
H44B H 0.554407 0.486971 0.135657 0.050 Uiso 0.820(7) 1 calc R U P C 1
H44C H 0.542986 0.570058 0.179994 0.050 Uiso 0.180(7) 1 calc R U P C 2
H44D H 0.526677 0.491310 0.142247 0.050 Uiso 0.180(7) 1 calc R U P C 2
C45 C 0.7753(14) 0.5542(10) 0.1924(7) 0.0442(18) Uani 0.180(7) 1 d D U P C 2
H45A H 0.760251 0.603528 0.212378 0.053 Uiso 0.180(7) 1 calc R U P C 2
H45B H 0.856589 0.552790 0.182161 0.053 Uiso 0.180(7) 1 calc R U P C 2
C46 C 0.6906(12) 0.5402(13) 0.1375(7) 0.0460(18) Uani 0.180(7) 1 d D U P C 2
H46A H 0.714275 0.496294 0.113132 0.055 Uiso 0.180(7) 1 calc R U P C 2
H46B H 0.680260 0.586258 0.111444 0.055 Uiso 0.180(7) 1 calc R U P C 2
C47 C 1.0363(3) 0.7960(2) 0.5158(2) 0.0464(8) Uani 0.776(3) 1 d D U P B 1
H47A H 1.081766 0.759211 0.493558 0.056 Uiso 0.776(3) 1 calc R U P B 1
H47B H 1.073507 0.801448 0.557617 0.056 Uiso 0.776(3) 1 calc R U P B 1
C48 C 1.0291(3) 0.8717(2) 0.4844(2) 0.0588(9) Uani 0.776(3) 1 d D U P B 1
H48A H 1.047627 0.866690 0.441850 0.071 Uiso 0.776(3) 1 calc R U P B 1
H48B H 1.082960 0.909098 0.505536 0.071 Uiso 0.776(3) 1 calc R U P B 1
C49 C 0.9032(4) 0.8963(3) 0.4873(3) 0.0758(11) Uani 0.776(3) 1 d D U P B 1
H49A H 0.899238 0.943745 0.511593 0.091 Uiso 0.776(3) 1 calc R U P B 1
H49B H 0.865475 0.905991 0.446045 0.091 Uiso 0.776(3) 1 calc R U P B 1
C50 C 0.8499(3) 0.8366(2) 0.5142(2) 0.0604(9) Uani 0.776(3) 1 d D U P B 1
H50A H 0.774795 0.825202 0.490965 0.073 Uiso 0.776(3) 1 calc R U P B 1
H50B H 0.834550 0.851301 0.555895 0.073 Uiso 0.776(3) 1 calc R U P B 1
C51 C 0.9422(11) 0.7678(7) 0.4458(6) 0.0482(14) Uani 0.224(3) 1 d D U P B 2
H51A H 0.868966 0.744407 0.427948 0.058 Uiso 0.224(3) 1 calc R U P B 2
H51B H 1.006060 0.751689 0.421936 0.058 Uiso 0.224(3) 1 calc R U P B 2
C52 C 0.9325(13) 0.8538(7) 0.4477(7) 0.0623(14) Uani 0.224(3) 1 d D U P B 2
H52A H 0.855823 0.868967 0.427888 0.075 Uiso 0.224(3) 1 calc R U P B 2
H52B H 0.992261 0.876132 0.423771 0.075 Uiso 0.224(3) 1 calc R U P B 2
C53 C 0.9480(15) 0.8914(8) 0.5171(7) 0.0616(13) Uani 0.224(3) 1 d D U P B 2
H53A H 1.004537 0.934051 0.521374 0.074 Uiso 0.224(3) 1 calc R U P B 2
H53B H 0.873660 0.906833 0.532228 0.074 Uiso 0.224(3) 1 calc R U P B 2
C54 C 0.9985(12) 0.8118(7) 0.5457(7) 0.0507(12) Uani 0.224(3) 1 d D U P B 2
H54A H 1.084047 0.814886 0.551477 0.061 Uiso 0.224(3) 1 calc R U P B 2
H54B H 0.969817 0.804363 0.585996 0.061 Uiso 0.224(3) 1 calc R U P B 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
Nd1 Nd1 3.42619(19) 3_666 ?
Nd1 K1 3.8808(4) . ?
Nd1 K2 3.7793(4) 3_666 ?
Nd1 O1 2.4792(13) . ?
Nd1 O2 2.4730(13) . ?
Nd1 O3 2.4574(13) 3_666 ?
Nd1 N1 2.6895(16) . ?
Nd1 N2 2.7209(15) . ?
Nd1 N3 2.6277(15) . ?
Nd1 N3 2.7687(15) 3_666 ?
Nd1 N4 2.5550(15) 3_666 ?
Nd1 N4 2.5416(15) . ?
K1 O1 2.7185(14) . ?
K1 O2 2.5976(14) . ?
K1 O4 2.7431(15) . ?
K1 O5 2.687(4) . ?
K1 O6 2.687(14) . ?
K1 O7 2.7563(16) . ?
K1 C1 3.2524(19) . ?
K1 C19 3.3413(19) . ?
K2 O1 2.7274(14) 3_666 ?
K2 O3 2.5934(15) . ?
K2 O8 2.654(2) . ?
K2 O9 2.679(8) . ?
K2 N3 3.0241(16) . ?
K2 C1 2.9671(19) 3_666 ?
K2 C2 3.151(2) 3_666 ?
K2 C16 3.323(2) 3_766 ?
K2 C26 3.491(2) . ?
O1 C1 1.309(2) . ?
O2 C19 1.308(2) . ?
O3 C26 1.311(2) . ?
O4 C28 1.440(3) . ?
O4 C31 1.440(3) . ?
O5 C33 1.411(6) . ?
O5 C36 1.429(7) . ?
O6 C37 1.427(15) . ?
O6 C40 1.423(14) . ?
O7 C41 1.435(3) . ?
O7 C44 1.426(3) . ?
O8 C47 1.412(4) . ?
O8 C50 1.408(4) . ?
O9 C51 1.427(13) . ?
O9 C54 1.438(14) . ?
N1 C7 1.273(3) . ?
N1 C8 1.459(2) . ?
N2 C9 1.479(2) . ?
N2 C10 1.486(2) . ?
N2 C11 1.479(2) . ?
N3 C12 1.463(2) . ?
N3 C13 1.475(2) . ?
N4 C20 1.469(2) . ?
N4 C27 1.457(2) . ?
C1 C2 1.416(3) . ?
C1 C6 1.425(3) . ?
C2 C3 1.383(3) . ?
C3 C4 1.387(3) . ?
C4 C5 1.382(3) . ?
C5 C6 1.402(3) . ?
C6 C7 1.458(3) . ?
C8 C9 1.519(3) . ?
C10 C27 1.534(3) 3_666 ?
C11 C12 1.530(3) . ?
C13 C14 1.522(2) . ?
C13 C20 1.558(3) . ?
C14 C15 1.387(3) . ?
C14 C19 1.425(3) . ?
C15 C16 1.394(3) . ?
C16 C17 1.387(3) . ?
C17 C18 1.386(3) . ?
C18 C19 1.413(3) . ?
C20 C21 1.522(3) . ?
C21 C22 1.390(3) . ?
C21 C26 1.417(3) . ?
C22 C23 1.397(3) . ?
C23 C24 1.378(4) . ?
C24 C25 1.382(3) . ?
C25 C26 1.417(3) . ?
C28 C29 1.523(3) . ?
C29 C30 1.521(3) . ?
C30 C31 1.502(3) . ?
C33 C34 1.511(7) . ?
C34 C35 1.500(5) . ?
C35 C36 1.526(4) . ?
C37 C38 1.487(12) . ?
C38 C39 1.521(12) . ?
C39 C40 1.548(13) . ?
C41 C42 1.496(4) . ?
C41 C45 1.543(12) . ?
C42 C43 1.544(5) . ?
C43 C44 1.507(5) . ?
C44 C46 1.528(13) . ?
C45 C46 1.510(14) . ?
C47 C48 1.490(5) . ?
C48 C49 1.528(6) . ?
C49 C50 1.376(6) . ?
C51 C52 1.506(14) . ?
C52 C53 1.666(16) . ?
C53 C54 1.613(15) . ?

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
Nd1 Nd1 K1 109.958(8) 3_666 . ?
Nd1 Nd1 K2 100.963(7) 3_666 3_666 ?
K2 Nd1 K1 87.353(9) 3_666 . ?
O1 Nd1 Nd1 124.22(3) . 3_666 ?
O1 Nd1 K1 44.11(3) . . ?
O1 Nd1 K2 46.11(3) . 3_666 ?
O1 Nd1 N1 69.20(5) . . ?
O1 Nd1 N2 135.80(4) . . ?
O1 Nd1 N3 87.11(4) . 3_666 ?
O1 Nd1 N3 141.85(4) . . ?
O1 Nd1 N4 140.04(5) . 3_666 ?
O1 Nd1 N4 89.28(5) . . ?
O2 Nd1 Nd1 115.99(3) . 3_666 ?
O2 Nd1 K1 41.26(3) . . ?
O2 Nd1 K2 123.25(3) . 3_666 ?
O2 Nd1 O1 77.22(4) . . ?
O2 Nd1 N1 63.49(5) . . ?
O2 Nd1 N2 86.88(4) . . ?
O2 Nd1 N3 143.30(4) . 3_666 ?
O2 Nd1 N3 74.13(4) . . ?
O2 Nd1 N4 78.02(5) . . ?
O2 Nd1 N4 142.56(5) . 3_666 ?
O3 Nd1 Nd1 113.50(3) 3_666 3_666 ?
O3 Nd1 K1 117.82(3) 3_666 . ?
O3 Nd1 K2 42.94(3) 3_666 3_666 ?
O3 Nd1 O1 74.68(4) 3_666 . ?
O3 Nd1 O2 130.50(4) 3_666 . ?
O3 Nd1 N1 68.70(5) 3_666 . ?
O3 Nd1 N2 85.85(5) 3_666 . ?
O3 Nd1 N3 143.47(5) 3_666 . ?
O3 Nd1 N3 74.39(4) 3_666 3_666 ?
O3 Nd1 N4 76.64(5) 3_666 3_666 ?
O3 Nd1 N4 140.35(5) 3_666 . ?
N1 Nd1 Nd1 166.56(4) . 3_666 ?
N1 Nd1 K1 78.79(4) . . ?
N1 Nd1 K2 89.39(4) . 3_666 ?
N1 Nd1 N2 66.79(5) . . ?
N1 Nd1 N3 140.08(5) . 3_666 ?
N2 Nd1 Nd1 99.87(3) . 3_666 ?
N2 Nd1 K1 127.32(3) . . ?
N2 Nd1 K2 128.79(3) . 3_666 ?
N2 Nd1 N3 125.62(4) . 3_666 ?
N3 Nd1 Nd1 52.43(3) . 3_666 ?
N3 Nd1 Nd1 48.79(3) 3_666 3_666 ?
N3 Nd1 K1 106.51(3) 3_666 . ?
N3 Nd1 K1 98.37(3) . . ?
N3 Nd1 K2 153.19(3) . 3_666 ?
N3 Nd1 K2 52.28(3) 3_666 3_666 ?
N3 Nd1 N1 117.39(5) . . ?
N3 Nd1 N2 67.04(5) . . ?
N3 Nd1 N3 101.22(4) . 3_666 ?
N4 Nd1 Nd1 47.59(3) 3_666 3_666 ?
N4 Nd1 Nd1 47.93(3) . 3_666 ?
N4 Nd1 K1 62.10(3) . . ?
N4 Nd1 K1 157.38(3) 3_666 . ?
N4 Nd1 K2 94.17(3) 3_666 3_666 ?
N4 Nd1 K2 100.56(3) . 3_666 ?
N4 Nd1 N1 123.75(5) 3_666 . ?
N4 Nd1 N1 138.82(5) . . ?
N4 Nd1 N2 127.61(5) . . ?
N4 Nd1 N2 67.84(5) 3_666 . ?
N4 Nd1 N3 60.60(5) . . ?
N4 Nd1 N3 70.78(5) 3_666 . ?
N4 Nd1 N3 58.53(5) 3_666 3_666 ?
N4 Nd1 N3 68.70(5) . 3_666 ?
N4 Nd1 N4 95.52(4) . 3_666 ?
O1 K1 Nd1 39.40(3) . . ?
O1 K1 O4 98.93(4) . . ?
O1 K1 O7 167.52(5) . . ?
O1 K1 C1 23.18(4) . . ?
O1 K1 C19 92.09(4) . . ?
O2 K1 Nd1 38.89(3) . . ?
O2 K1 O1 71.04(4) . . ?
O2 K1 O4 160.34(5) . . ?
O2 K1 O5 113.84(18) . . ?
O2 K1 O6 114.8(6) . . ?
O2 K1 O7 102.59(5) . . ?
O2 K1 C1 81.75(5) . . ?
O2 K1 C19 21.06(4) . . ?
O4 K1 Nd1 123.75(3) . . ?
O4 K1 O7 83.76(5) . . ?
O4 K1 C1 95.41(5) . . ?
O4 K1 C19 158.87(5) . . ?
O5 K1 Nd1 134.4(2) . . ?
O5 K1 O1 109.2(2) . . ?
O5 K1 O4 85.22(17) . . ?
O5 K1 O7 83.1(2) . . ?
O5 K1 C1 86.1(2) . . ?
O5 K1 C19 108.17(14) . . ?
O6 K1 Nd1 137.0(8) . . ?
O6 K1 O1 112.2(7) . . ?
O6 K1 O4 84.5(6) . . ?
O6 K1 O7 80.2(7) . . ?
O6 K1 C1 89.1(7) . . ?
O6 K1 C19 108.1(4) . . ?
O7 K1 Nd1 129.69(4) . . ?
O7 K1 C1 169.22(5) . . ?
O7 K1 C19 81.81(5) . . ?
C1 K1 Nd1 59.31(3) . . ?
C1 K1 C19 101.61(5) . . ?
C19 K1 Nd1 57.84(3) . . ?
O1 K2 Nd1 40.93(3) 3_666 3_666 ?
O1 K2 N3 77.87(4) 3_666 . ?
O1 K2 C1 26.14(4) 3_666 3_666 ?
O1 K2 C2 46.53(4) 3_666 3_666 ?
O1 K2 C16 104.13(5) 3_666 3_766 ?
O1 K2 C26 86.70(4) 3_666 . ?
O3 K2 Nd1 40.21(3) . 3_666 ?
O3 K2 O1 68.44(4) . 3_666 ?
O3 K2 O8 92.39(6) . . ?
O3 K2 O9 101.7(2) . . ?
O3 K2 N3 68.18(4) . . ?
O3 K2 C1 75.76(5) . 3_666 ?
O3 K2 C2 101.36(5) . 3_666 ?
O3 K2 C16 169.50(5) . 3_766 ?
O3 K2 C26 18.27(4) . . ?
O8 K2 Nd1 128.94(6) . 3_666 ?
O8 K2 O1 118.61(7) . 3_666 ?
O8 K2 N3 148.86(7) . . ?
O8 K2 C1 93.98(7) . 3_666 ?
O8 K2 C2 86.02(8) . 3_666 ?
O8 K2 C16 97.80(7) . 3_766 ?
O8 K2 C26 83.04(7) . . ?
O9 K2 N3 143.1(2) . . ?
O9 K2 C26 89.0(2) . . ?
N3 K2 Nd1 46.40(3) . 3_666 ?
N3 K2 C2 120.61(5) . 3_666 ?
N3 K2 C16 103.51(5) . 3_766 ?
N3 K2 C26 71.15(4) . . ?
C1 K2 Nd1 62.57(4) 3_666 3_666 ?
C1 K2 N3 103.82(5) 3_666 . ?
C1 K2 C2 26.54(5) 3_666 3_666 ?
C1 K2 C16 100.90(5) 3_666 3_766 ?
C1 K2 C26 92.07(5) 3_666 . ?
C2 K2 Nd1 86.95(4) 3_666 3_666 ?
C2 K2 C16 76.97(5) 3_666 3_766 ?
C2 K2 C26 116.13(5) 3_666 . ?
C16 K2 Nd1 129.39(4) 3_766 3_666 ?
C16 K2 C26 166.88(5) 3_766 . ?
C26 K2 Nd1 55.73(3) . 3_666 ?
Nd1 O1 K1 96.49(4) . . ?
Nd1 O1 K2 92.96(4) . 3_666 ?
K1 O1 K2 152.56(6) . 3_666 ?
C1 O1 Nd1 138.98(12) . . ?
C1 O1 K1 101.97(11) . . ?
C1 O1 K2 87.21(10) . 3_666 ?
Nd1 O2 K1 99.85(5) . . ?
C19 O2 Nd1 135.21(11) . . ?
C19 O2 K1 113.44(11) . . ?
Nd1 O3 K2 96.84(5) 3_666 . ?
C26 O3 Nd1 126.77(12) . 3_666 ?
C26 O3 K2 123.40(11) . . ?
C28 O4 K1 115.96(12) . . ?
C31 O4 K1 116.24(13) . . ?
C31 O4 C28 108.71(16) . . ?
C33 O5 K1 126.8(5) . . ?
C33 O5 C36 110.0(5) . . ?
C36 O5 K1 117.8(4) . . ?
C37 O6 K1 101.7(10) . . ?
C40 O6 K1 121.6(17) . . ?
C40 O6 C37 110(2) . . ?
C41 O7 K1 123.69(13) . . ?
C44 O7 K1 126.74(14) . . ?
C44 O7 C41 109.53(18) . . ?
C47 O8 K2 135.8(2) . . ?
C50 O8 K2 115.6(2) . . ?
C50 O8 C47 107.3(3) . . ?
C51 O9 K2 111.7(7) . . ?
C51 O9 C54 112.0(10) . . ?
C54 O9 K2 122.2(9) . . ?
C7 N1 Nd1 131.61(14) . . ?
C7 N1 C8 117.18(17) . . ?
C8 N1 Nd1 110.98(11) . . ?
C9 N2 Nd1 109.68(11) . . ?
C9 N2 C10 109.11(14) . . ?
C9 N2 C11 109.97(15) . . ?
C10 N2 Nd1 110.84(11) . . ?
C11 N2 Nd1 106.02(10) . . ?
C11 N2 C10 111.19(15) . . ?
Nd1 N3 Nd1 78.78(4) . 3_666 ?
Nd1 N3 K2 81.32(4) 3_666 . ?
Nd1 N3 K2 159.59(6) . . ?
C12 N3 Nd1 115.96(11) . . ?
C12 N3 Nd1 130.80(11) . 3_666 ?
C12 N3 K2 74.51(9) . . ?
C12 N3 C13 109.30(14) . . ?
C13 N3 Nd1 108.74(10) . . ?
C13 N3 Nd1 108.85(10) . 3_666 ?
C13 N3 K2 81.96(9) . . ?
Nd1 N4 Nd1 84.48(4) . 3_666 ?
C20 N4 Nd1 111.57(11) . 3_666 ?
C20 N4 Nd1 113.67(11) . . ?
C27 N4 Nd1 117.88(11) . . ?
C27 N4 Nd1 117.34(11) . 3_666 ?
C27 N4 C20 109.92(14) . . ?
K2 C1 K1 116.48(6) 3_666 . ?
O1 C1 K1 54.85(9) . . ?
O1 C1 K2 66.65(9) . 3_666 ?
O1 C1 C2 119.52(18) . . ?
O1 C1 C6 124.44(17) . . ?
C2 C1 K1 103.48(13) . . ?
C2 C1 K2 84.00(11) . 3_666 ?
C2 C1 C6 116.04(17) . . ?
C6 C1 K1 112.07(13) . . ?
C6 C1 K2 120.39(13) . 3_666 ?
C1 C2 K2 69.46(11) . 3_666 ?
C3 C2 K2 125.88(15) . 3_666 ?
C3 C2 C1 123.2(2) . . ?
C2 C3 C4 120.1(2) . . ?
C5 C4 C3 118.2(2) . . ?
C4 C5 C6 123.0(2) . . ?
C1 C6 C7 124.51(18) . . ?
C5 C6 C1 119.32(19) . . ?
C5 C6 C7 116.14(19) . . ?
N1 C7 C6 127.62(19) . . ?
N1 C8 C9 110.31(16) . . ?
N2 C9 C8 113.09(15) . . ?
N2 C10 C27 114.18(15) . 3_666 ?
N2 C11 C12 113.34(15) . . ?
N3 C12 C11 114.35(15) . . ?
N3 C13 C14 114.88(14) . . ?
N3 C13 C20 110.78(14) . . ?
C14 C13 C20 110.13(14) . . ?
C15 C14 C13 121.42(17) . . ?
C15 C14 C19 119.28(17) . . ?
C19 C14 C13 119.30(16) . . ?
C14 C15 C16 122.23(18) . . ?
C15 C16 K2 112.95(13) . 3_766 ?
C17 C16 K2 94.80(13) . 3_766 ?
C17 C16 C15 118.77(18) . . ?
C18 C17 C16 120.45(18) . . ?
C17 C18 C19 121.56(18) . . ?
O2 C19 K1 45.50(9) . . ?
O2 C19 C14 121.03(16) . . ?
O2 C19 C18 121.28(17) . . ?
C14 C19 K1 116.99(12) . . ?
C18 C19 K1 106.20(12) . . ?
C18 C19 C14 117.69(17) . . ?
N4 C20 C13 110.86(14) . . ?
N4 C20 C21 113.13(15) . . ?
C21 C20 C13 112.10(15) . . ?
C22 C21 C20 120.46(18) . . ?
C22 C21 C26 119.78(18) . . ?
C26 C21 C20 119.60(16) . . ?
C21 C22 C23 121.9(2) . . ?
C24 C23 C22 118.5(2) . . ?
C23 C24 C25 121.0(2) . . ?
C24 C25 C26 121.5(2) . . ?
O3 C26 K2 38.33(9) . . ?
O3 C26 C21 121.28(17) . . ?
O3 C26 C25 121.46(19) . . ?
C21 C26 K2 109.21(12) . . ?
C21 C26 C25 117.26(19) . . ?
C25 C26 K2 119.66(14) . . ?
N4 C27 C10 114.85(15) . 3_666 ?
O4 C28 C29 106.56(17) . . ?
C30 C29 C28 103.35(19) . . ?
C31 C30 C29 101.55(19) . . ?
O4 C31 C30 105.02(18) . . ?
O5 C33 C34 106.0(6) . . ?
C35 C34 C33 102.3(4) . . ?
C34 C35 C36 101.7(3) . . ?
O5 C36 C35 105.9(4) . . ?
O6 C37 C38 108.6(17) . . ?
C37 C38 C39 97.9(10) . . ?
C38 C39 C40 107.7(13) . . ?
O6 C40 C39 103.1(19) . . ?
O7 C41 C42 106.2(2) . . ?
O7 C41 C45 103.6(6) . . ?
C41 C42 C43 101.0(3) . . ?
C44 C43 C42 101.2(3) . . ?
O7 C44 C43 106.2(2) . . ?
O7 C44 C46 105.2(7) . . ?
C46 C45 C41 99.4(12) . . ?
C45 C46 C44 99.6(11) . . ?
O8 C47 C48 105.5(3) . . ?
C47 C48 C49 104.0(3) . . ?
C50 C49 C48 105.9(4) . . ?
C49 C50 O8 110.3(4) . . ?
O9 C51 C52 103.7(11) . . ?
C51 C52 C53 114.6(11) . . ?
C54 C53 C52 91.5(11) . . ?
O9 C54 C53 112.6(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Nd1 O1 C1 K1 -114.82(17) . . . . ?
Nd1 O1 C1 K2 91.30(15) . . . 3_666 ?
Nd1 O1 C1 C2 159.25(14) . . . . ?
Nd1 O1 C1 C6 -20.6(3) . . . . ?
Nd1 O2 C19 K1 -134.56(19) . . . . ?
Nd1 O2 C19 C14 -35.8(3) . . . . ?
Nd1 O2 C19 C18 143.45(15) . . . . ?
Nd1 O3 C26 K2 -132.14(18) 3_666 . . . ?
Nd1 O3 C26 C21 -50.6(2) 3_666 . . . ?
Nd1 O3 C26 C25 128.56(16) 3_666 . . . ?
Nd1 N1 C7 C6 -1.9(3) . . . . ?
Nd1 N1 C8 C9 48.54(17) . . . . ?
Nd1 N2 C9 C8 42.41(18) . . . . ?
Nd1 N2 C10 C27 -34.72(18) . . . 3_666 ?
Nd1 N2 C11 C12 52.77(16) . . . . ?
Nd1 N3 C12 C11 116.53(15) 3_666 . . . ?
Nd1 N3 C12 C11 18.81(19) . . . . ?
Nd1 N3 C13 C14 -78.62(15) . . . . ?
Nd1 N3 C13 C14 -162.80(12) 3_666 . . . ?
Nd1 N3 C13 C20 -37.22(15) 3_666 . . . ?
Nd1 N3 C13 C20 46.97(15) . . . . ?
Nd1 N4 C20 C13 -39.46(17) . . . . ?
Nd1 N4 C20 C13 54.00(16) 3_666 . . . ?
Nd1 N4 C20 C21 -166.37(12) . . . . ?
Nd1 N4 C20 C21 -72.91(16) 3_666 . . . ?
Nd1 N4 C27 C10 32.44(19) 3_666 . . 3_666 ?
Nd1 N4 C27 C10 131.12(13) . . . 3_666 ?
K1 O1 C1 K2 -153.88(7) . . . 3_666 ?
K1 O1 C1 C2 -85.93(17) . . . . ?
K1 O1 C1 C6 94.27(19) . . . . ?
K1 O2 C19 C14 98.71(17) . . . . ?
K1 O2 C19 C18 -81.99(19) . . . . ?
K1 O4 C28 C29 -128.11(16) . . . . ?
K1 O4 C31 C30 105.54(17) . . . . ?
K1 O5 C33 C34 -138.7(6) . . . . ?
K1 O5 C36 C35 165.3(4) . . . . ?
K1 O6 C37 C38 101.8(13) . . . . ?
K1 O6 C40 C39 -112(2) . . . . ?
K1 O7 C41 C42 167.7(2) . . . . ?
K1 O7 C41 C45 -160.1(8) . . . . ?
K1 O7 C44 C43 166.2(2) . . . . ?
K1 O7 C44 C46 -170.3(9) . . . . ?
K1 C1 C2 K2 -115.84(7) . . . 3_666 ?
K1 C1 C2 C3 123.98(19) . . . . ?
K1 C1 C6 C5 -118.82(19) . . . . ?
K1 C1 C6 C7 59.2(2) . . . . ?
K2 O1 C1 K1 153.88(7) 3_666 . . . ?
K2 O1 C1 C2 67.96(17) 3_666 . . . ?
K2 O1 C1 C6 -111.85(19) 3_666 . . . ?
K2 O3 C26 C21 81.5(2) . . . . ?
K2 O3 C26 C25 -99.30(19) . . . . ?
K2 O8 C47 C48 167.7(3) . . . . ?
K2 O8 C50 C49 -165.4(4) . . . . ?
K2 O9 C51 C52 127.1(9) . . . . ?
K2 O9 C54 C53 -111.0(11) . . . . ?
K2 N3 C12 C11 -179.97(15) . . . . ?
K2 N3 C13 C14 119.28(14) . . . . ?
K2 N3 C13 C20 -115.14(13) . . . . ?
K2 C1 C2 C3 -120.2(2) 3_666 . . . ?
K2 C1 C6 C5 98.5(2) 3_666 . . . ?
K2 C1 C6 C7 -83.5(2) 3_666 . . . ?
K2 C2 C3 C4 -87.5(2) 3_666 . . . ?
K2 C16 C17 C18 120.51(19) 3_766 . . . ?
O1 C1 C2 K2 -58.84(15) . . . 3_666 ?
O1 C1 C2 C3 -179.01(19) . . . . ?
O1 C1 C6 C5 179.6(2) . . . . ?
O1 C1 C6 C7 -2.4(3) . . . . ?
O4 C28 C29 C30 18.8(3) . . . . ?
O5 C33 C34 C35 -32.7(7) . . . . ?
O6 C37 C38 C39 35.7(14) . . . . ?
O7 C41 C42 C43 33.3(4) . . . . ?
O7 C41 C45 C46 -40.1(15) . . . . ?
O7 C44 C46 C45 -37.0(16) . . . . ?
O8 C47 C48 C49 18.1(6) . . . . ?
O9 C51 C52 C53 -1.5(15) . . . . ?
N1 C8 C9 N2 -63.8(2) . . . . ?
N2 C11 C12 N3 -50.9(2) . . . . ?
N3 C13 C14 C15 -116.64(19) . . . . ?
N3 C13 C14 C19 63.8(2) . . . . ?
N3 C13 C20 N4 -6.8(2) . . . . ?
N3 C13 C20 C21 120.70(16) . . . . ?
N4 C20 C21 C22 -109.85(19) . . . . ?
N4 C20 C21 C26 65.5(2) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C1 C6 C7 N1 12.4(4) . . . . ?
C2 C1 C6 C5 -0.3(3) . . . . ?
C2 C1 C6 C7 177.8(2) . . . . ?
C2 C3 C4 C5 -1.2(4) . . . . ?
C3 C4 C5 C6 1.8(4) . . . . ?
C4 C5 C6 C1 -1.1(4) . . . . ?
C4 C5 C6 C7 -179.3(2) . . . . ?
C5 C6 C7 N1 -169.5(2) . . . . ?
C6 C1 C2 K2 120.98(17) . . . 3_666 ?
C6 C1 C2 C3 0.8(3) . . . . ?
C7 N1 C8 C9 -136.28(19) . . . . ?
C8 N1 C7 C6 -175.9(2) . . . . ?
C9 N2 C10 C27 -155.60(16) . . . 3_666 ?
C9 N2 C11 C12 171.27(15) . . . . ?
C10 N2 C9 C8 164.00(16) . . . . ?
C10 N2 C11 C12 -67.78(19) . . . . ?
C11 N2 C9 C8 -73.81(19) . . . . ?
C11 N2 C10 C27 82.94(19) . . . 3_666 ?
C12 N3 C13 C14 48.9(2) . . . . ?
C12 N3 C13 C20 174.45(14) . . . . ?
C13 N3 C12 C11 -104.50(17) . . . . ?
C13 C14 C15 C16 179.82(17) . . . . ?
C13 C14 C19 K1 52.69(19) . . . . ?
C13 C14 C19 O2 0.4(3) . . . . ?
C13 C14 C19 C18 -178.93(16) . . . . ?
C13 C20 C21 C22 123.90(18) . . . . ?
C13 C20 C21 C26 -60.8(2) . . . . ?
C14 C13 C20 N4 121.43(16) . . . . ?
C14 C13 C20 C21 -111.10(17) . . . . ?
C14 C15 C16 K2 -110.28(17) . . . 3_766 ?
C14 C15 C16 C17 -0.6(3) . . . . ?
C15 C14 C19 K1 -126.86(15) . . . . ?
C15 C14 C19 O2 -179.16(17) . . . . ?
C15 C14 C19 C18 1.5(3) . . . . ?
C15 C16 C17 C18 1.0(3) . . . . ?
C16 C17 C18 C19 -0.1(3) . . . . ?
C17 C18 C19 K1 132.15(17) . . . . ?
C17 C18 C19 O2 179.50(18) . . . . ?
C17 C18 C19 C14 -1.2(3) . . . . ?
C19 C14 C15 C16 -0.6(3) . . . . ?
C20 N4 C27 C10 -96.43(18) . . . 3_666 ?
C20 C13 C14 C15 117.43(19) . . . . ?
C20 C13 C14 C19 -62.1(2) . . . . ?
C20 C21 C22 C23 175.58(18) . . . . ?
C20 C21 C26 K2 44.22(19) . . . . ?
C20 C21 C26 O3 3.7(3) . . . . ?
C20 C21 C26 C25 -175.51(17) . . . . ?
C21 C22 C23 C24 -0.5(3) . . . . ?
C22 C21 C26 K2 -140.41(15) . . . . ?
C22 C21 C26 O3 179.08(17) . . . . ?
C22 C21 C26 C25 -0.1(3) . . . . ?
C22 C23 C24 C25 0.7(3) . . . . ?
C23 C24 C25 C26 -0.7(3) . . . . ?
C24 C25 C26 K2 136.36(18) . . . . ?
C24 C25 C26 O3 -178.86(19) . . . . ?
C24 C25 C26 C21 0.4(3) . . . . ?
C26 C21 C22 C23 0.2(3) . . . . ?
C27 N4 C20 C13 -174.04(14) . . . . ?
C27 N4 C20 C21 59.05(19) . . . . ?
C28 O4 C31 C30 -27.5(2) . . . . ?
C28 C29 C30 C31 -34.2(2) . . . . ?
C29 C30 C31 O4 38.2(2) . . . . ?
C31 O4 C28 C29 5.1(2) . . . . ?
C33 O5 C36 C35 9.2(8) . . . . ?
C33 C34 C35 C36 36.7(5) . . . . ?
C34 C35 C36 O5 -29.1(6) . . . . ?
C36 O5 C33 C34 14.7(8) . . . . ?
C37 O6 C40 C39 7(3) . . . . ?
C37 C38 C39 C40 -31.0(18) . . . . ?
C38 C39 C40 O6 16(2) . . . . ?
C40 O6 C37 C38 -28(2) . . . . ?
C41 O7 C44 C43 -11.5(3) . . . . ?
C41 O7 C44 C46 11.9(9) . . . . ?
C41 C42 C43 C44 -38.8(5) . . . . ?
C41 C45 C46 C44 45.8(18) . . . . ?
C42 C43 C44 O7 31.5(4) . . . . ?
C44 O7 C41 C42 -14.4(3) . . . . ?
C44 O7 C41 C45 17.7(8) . . . . ?
C47 O8 C50 C49 25.5(6) . . . . ?
C47 C48 C49 C50 -3.3(6) . . . . ?
C48 C49 C50 O8 -13.0(7) . . . . ?
C50 O8 C47 C48 -26.5(5) . . . . ?
C51 O9 C54 C53 25.5(16) . . . . ?
C51 C52 C53 C54 13.6(15) . . . . ?
C52 C53 C54 O9 -21.9(15) . . . . ?
C54 O9 C51 C52 -14.0(14) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.000 141.9 34.0 '0.9 C4H8O'
2 0.500 0.000 0.500 141.9 34.0 '0.9 C4H8O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.507
_oxdiff_exptl_absorpt_empirical_full_min 0.586
####################################################################### 
# 
# 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_bch40
_database_code_depnum_ccdc_archive 'CCDC 2013181'
loop_
_audit_author_name
_audit_author_address
'Rosario Scopelliti'
;epfl
Switzerland
;
_audit_update_record             
;
2020-06-30 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT410_bch40               
;
PROBLEM: Short Intra H...H Contact  H11B     ..H20A     .       1.82 Ang.  
RESPONSE: These hydrogens were clearly located on the difference map
and then placed on calculated coordinates. This short H...H distance is not 
the result of wrongly assigned hydrogens.
;
_vrf_PLAT910_bch40               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).         21 Note  
RESPONSE: These reflections are hidden by the beam stop. This is quite
usual with Mo radiation and the setup of our instruments. 
;
# end Validation Reply Form

_audit_creation_date             2020-03-18
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C86 H118 K4 N8 O14 Sm2'
_chemical_formula_sum            'C86 H118 K4 N8 O14 Sm2'
_chemical_formula_weight         1944.98
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54 H54 N8 O6 K4 Sm2'
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'
K K 0.2009 0.2494 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.5872(5)
_cell_length_b                   17.4186(7)
_cell_length_c                   22.2099(9)
_cell_angle_alpha                90
_cell_angle_beta                 95.457(4)
_cell_angle_gamma                90
_cell_volume                     4462.4(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    11677
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.0150
_cell_measurement_theta_min      3.5780
_shelx_estimated_absorpt_T_max   0.832
_shelx_estimated_absorpt_T_min   0.758
_exptl_absorpt_coefficient_mu    1.554
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2004
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 17 23 0.0413
-2 -21 15 0.0833
4 -15 23 0.0772
-2 24 7 0.0338
-4 18 -19 0.0558
2 23 -12 0.0513
10 19 -6 0.0506
-11 -16 13 0.1029
2 -24 -3 0.0905
15 8 -5 0.0485
-15 -8 6 0.1064
-2 14 25 0.0399
14 -9 8 0.0444
0 -16 -23 0.0886
-14 7 -11 0.0736

_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.123
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-1.0125 16.6957 22.9490 -0.1095 0.0664 0.9918
-1.9968 -20.9942 15.0142 -0.1481 -0.9544 -0.1849
4.0019 -14.9887 23.0200 0.1993 -0.9630 0.2136
-2.0064 23.9950 6.9824 -0.1391 0.6263 0.7771
-4.0029 17.9890 -19.0213 -0.2078 0.9764 -0.0371
1.9961 22.9944 -12.0150 0.1418 0.9566 0.3108
9.9976 19.0032 -6.0000 0.6163 0.6616 0.4171
-10.9991 -16.0031 12.9980 -0.6914 -0.7031 -0.1739
2.0061 -23.9942 -2.9817 0.1311 -0.7074 -0.6780
15.2908 8.4875 -4.9605 0.9371 0.2779 0.2114
-15.3653 -8.0073 5.8212 -0.9434 -0.2798 -0.1782
-1.8686 14.3848 25.3389 -0.1659 -0.0499 0.9849
14.2415 -8.6683 8.0420 0.8499 -0.5204 0.0828
0.1026 -16.1558 -23.4831 0.0552 -0.0332 -0.9979
-14.0787 6.5174 -10.9515 -0.8339 0.5107 -0.2092

_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0973
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            55351
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         3.533
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00 -39.00   1.00   30.00    --  -10.00 -57.00-120.00   27
  2  ω     30.00  61.00   1.00   30.00    --  -10.00  57.00  30.00   31
  3  ω      5.00  31.00   1.00   30.00    --  -10.00 -99.00 -30.00   26
  4  ω    -21.00   4.00   1.00   30.00    --  -10.00 -57.00 -60.00   25
  5  ω      1.00  29.00   1.00   30.00    --  -10.00 -99.00 150.00   28
  6  ω    -20.00   5.00   1.00   30.00    --  -10.00 -99.00 -90.00   25
  7  ω    -42.00  33.00   1.00   30.00    --  -10.00  77.00-120.00   75
  8  ω    -12.00  52.00   1.00   30.00    --  -10.00  37.00-150.00   64
  9  ω    -83.00  11.00   1.00   30.00    --  -10.00 -37.00  60.00   94
 10  ω    -18.00   9.00   1.00   30.00    --   10.47  77.00  30.00   27
 11  ω     40.00  94.00   1.00   30.00    --   10.47-178.00  60.00   54
 12  ω     50.00  75.00   1.00   30.00    --   10.47 178.00 150.00   25
 13  ω     35.00  60.00   1.00   30.00    --   10.47 178.00 120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0607164000
_diffrn_orient_matrix_UB_12      -0.0001420000
_diffrn_orient_matrix_UB_13      -0.0019895000
_diffrn_orient_matrix_UB_21      -0.0058997000
_diffrn_orient_matrix_UB_22      0.0315110000
_diffrn_orient_matrix_UB_23      -0.0202919000
_diffrn_orient_matrix_UB_31      0.0075355000
_diffrn_orient_matrix_UB_32      0.0258080000
_diffrn_orient_matrix_UB_33      0.0247729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6718
_reflns_number_total             8454
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.421
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         8454
_refine_ls_number_restraints     316
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0436
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0444P)²+5.9996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.1018
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 K2-O7 \\sim K2-O9
 with sigma of 0.02
 C48-C46 \\sim C49-C48 \\sim C49-C47 \\sim C43-C42 \\sim C42-C41 \\sim C41-C40
\\sim C39-C38 \\sim C38-C37
 \\sim C37-C36 \\sim C52-C36 \\sim C52-C51 \\sim C51-C50
 with sigma of 0.02
 O9-C47 \\sim O9-C46 \\sim O7-C40 \\sim O7-C43 \\sim O6-C39 \\sim O6-C50 \\sim
O6-C36
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O7 \\sim C43 \\sim C42 \\sim C41 \\sim C40 \\sim C46 \\sim C48 \\sim C49 \\sim
C47 \\sim O9 \\sim C38 \\sim C39 \\sim O6 \\sim C36 \\sim C37 \\sim C50 \\sim
C51 \\sim C52: within 2A with sigma of 0.005 and sigma for terminal atoms of 2
within 2A
4. Others
 Sof(O9)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C49)=
 Sof(H49A)=Sof(H49B)=Sof(C48)=Sof(H48A)=Sof(H48B)=1-FVAR(1)
 Sof(O7)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(1)
 Sof(H36C)=Sof(H36D)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(C50)=Sof(H50A)=Sof(H50B)=1-FVAR(2)
 Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C21(H21)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B),
 C20(H20A,H20B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C36(H36C,H36D), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C47(H47A,H47B),
  C46(H46A,H46B), C49(H49A,H49B), C48(H48A,H48B), C51(H51A,H51B), C52(H52A,
 H52B), C50(H50A,H50B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16),
 C17(H17), C23(H23), C24(H24), C25(H25), C26(H26)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.49537(2) 0.40760(2) 0.52483(2) 0.01172(8) Uani 1 1 d . . . . .
K1 K 0.51256(8) 0.40376(6) 0.70076(4) 0.0195(2) Uani 1 1 d . . . . .
K2 K 0.18464(8) 0.64024(6) 0.45965(4) 0.0200(2) Uani 1 1 d D . . . .
O1 O 0.6301(2) 0.35651(17) 0.60737(13) 0.0164(7) Uani 1 1 d . . . . .
O2 O 0.6245(3) 0.32238(17) 0.47634(14) 0.0193(7) Uani 1 1 d . . . . .
O3 O 0.3691(2) 0.38153(17) 0.60474(13) 0.0168(7) Uani 1 1 d . . . . .
O4 O 0.3780(3) 0.4803(2) 0.77734(15) 0.0320(8) Uani 1 1 d . . . . .
O5 O 0.6933(3) 0.46502(19) 0.77480(14) 0.0243(7) Uani 1 1 d . . . . .
O6 O 0.5098(3) 0.2943(2) 0.78584(18) 0.0419(9) Uani 1 1 d D U . . .
O7 O 0.0809(4) 0.7714(3) 0.4842(3) 0.0455(12) Uani 0.766(6) 1 d D U P A 1
N1 N 0.3253(3) 0.34981(19) 0.44578(16) 0.0134(8) Uani 1 1 d . . . . .
N2 N 0.4486(3) 0.2598(2) 0.54525(16) 0.0174(8) Uani 1 1 d . . . . .
N3 N 0.4997(3) 0.4654(2) 0.42084(15) 0.0136(8) Uani 1 1 d . . . . .
N4 N 0.3208(3) 0.5012(2) 0.50473(15) 0.0121(7) Uani 1 1 d . . . . .
C1 C 0.3204(4) 0.2652(3) 0.4516(2) 0.0201(10) Uani 1 1 d . . . . .
H1A H 0.382283 0.242176 0.429565 0.024 Uiso 1 1 calc R U . . .
H1B H 0.245007 0.246755 0.432231 0.024 Uiso 1 1 calc R U . . .
C2 C 0.3348(4) 0.2379(3) 0.5167(2) 0.0186(10) Uani 1 1 d . . . . .
H2A H 0.273672 0.260877 0.539215 0.022 Uiso 1 1 calc R U . . .
H2B H 0.326390 0.181362 0.517911 0.022 Uiso 1 1 calc R U . . .
C3 C 0.5020(4) 0.2098(3) 0.5784(2) 0.0237(11) Uani 1 1 d . . . . .
H3 H 0.465626 0.161044 0.579986 0.028 Uiso 1 1 calc R U . . .
C4 C 0.6136(4) 0.2185(3) 0.6147(2) 0.0228(10) Uani 1 1 d . . . . .
C5 C 0.6656(4) 0.1509(3) 0.6389(3) 0.0339(13) Uani 1 1 d . . . . .
H5 H 0.627379 0.103393 0.630206 0.041 Uiso 1 1 calc R U . . .
C6 C 0.7700(4) 0.1505(3) 0.6747(3) 0.0337(13) Uani 1 1 d . . . . .
H6 H 0.804038 0.103611 0.689315 0.040 Uiso 1 1 calc R U . . .
C7 C 0.8234(4) 0.2197(3) 0.6887(2) 0.0281(12) Uani 1 1 d . . . . .
H7 H 0.894029 0.220943 0.714199 0.034 Uiso 1 1 calc R U . . .
C8 C 0.7751(4) 0.2871(3) 0.6661(2) 0.0209(10) Uani 1 1 d . . . . .
H8 H 0.814088 0.333957 0.676433 0.025 Uiso 1 1 calc R U . . .
C9 C 0.6699(4) 0.2900(3) 0.62805(19) 0.0163(9) Uani 1 1 d . . . . .
C10 C 0.3452(4) 0.3708(3) 0.38244(19) 0.0162(9) Uani 1 1 d . . . . .
H10A H 0.269948 0.369877 0.357290 0.019 Uiso 1 1 calc R U . . .
H10B H 0.395661 0.331462 0.366296 0.019 Uiso 1 1 calc R U . . .
C11 C 0.4008(4) 0.4495(3) 0.37637(19) 0.0152(9) Uani 1 1 d . . . . .
H11A H 0.426811 0.453840 0.335326 0.018 Uiso 1 1 calc R U . . .
H11B H 0.340984 0.489368 0.380143 0.018 Uiso 1 1 calc R U . . .
C12 C 0.6080(3) 0.4477(2) 0.39401(19) 0.0132(9) Uani 1 1 d . . . . .
H12 H 0.607960 0.479646 0.356604 0.016 Uiso 1 1 calc R U . . .
C13 C 0.6165(3) 0.3642(3) 0.37423(19) 0.0152(9) Uani 1 1 d . . . . .
C14 C 0.6112(4) 0.3449(3) 0.3137(2) 0.0210(10) Uani 1 1 d . . . . .
H14 H 0.607224 0.384811 0.284463 0.025 Uiso 1 1 calc R U . . .
C15 C 0.6114(4) 0.2690(3) 0.2940(2) 0.0285(12) Uani 1 1 d . . . . .
H15 H 0.608222 0.257270 0.252136 0.034 Uiso 1 1 calc R U . . .
C16 C 0.6165(4) 0.2111(3) 0.3369(3) 0.0318(13) Uani 1 1 d . . . . .
H16 H 0.616327 0.158976 0.324395 0.038 Uiso 1 1 calc R U . . .
C17 C 0.6217(4) 0.2288(3) 0.3978(2) 0.0252(11) Uani 1 1 d . . . . .
H17 H 0.625406 0.188155 0.426486 0.030 Uiso 1 1 calc R U . . .
C18 C 0.6218(4) 0.3056(3) 0.4188(2) 0.0202(10) Uani 1 1 d . . . . .
C19 C 0.2154(4) 0.3833(2) 0.4629(2) 0.0155(9) Uani 1 1 d . . . . .
H19A H 0.198366 0.361864 0.502330 0.019 Uiso 1 1 calc R U . . .
H19B H 0.151447 0.368304 0.432403 0.019 Uiso 1 1 calc R U . . .
C20 C 0.2196(4) 0.4709(2) 0.46742(19) 0.0141(9) Uani 1 1 d . . . . .
H20A H 0.219170 0.492399 0.426149 0.017 Uiso 1 1 calc R U . . .
H20B H 0.148444 0.488894 0.484426 0.017 Uiso 1 1 calc R U . . .
C21 C 0.2845(4) 0.5268(2) 0.56305(18) 0.0129(9) Uani 1 1 d . . . . .
H21 H 0.235425 0.573568 0.554677 0.016 Uiso 1 1 calc R U . . .
C22 C 0.2118(4) 0.4698(2) 0.59472(18) 0.0136(9) Uani 1 1 d . . . . .
C23 C 0.0983(4) 0.4856(3) 0.60549(18) 0.0157(9) Uani 1 1 d . . . . .
H23 H 0.065512 0.533664 0.593035 0.019 Uiso 1 1 calc R U . . .
C24 C 0.0310(4) 0.4331(3) 0.6341(2) 0.0199(10) Uani 1 1 d . . . . .
H24 H -0.046377 0.445560 0.641175 0.024 Uiso 1 1 calc R U . . .
C25 C 0.0772(4) 0.3631(3) 0.6518(2) 0.0196(10) Uani 1 1 d . . . . .
H25 H 0.031653 0.326577 0.670810 0.024 Uiso 1 1 calc R U . . .
C26 C 0.1919(4) 0.3459(3) 0.6418(2) 0.0176(10) Uani 1 1 d . . . . .
H26 H 0.223275 0.297508 0.654456 0.021 Uiso 1 1 calc R U . . .
C27 C 0.2617(4) 0.3979(2) 0.61375(19) 0.0150(9) Uani 1 1 d . . . . .
C28 C 0.2536(5) 0.4851(3) 0.7689(2) 0.0357(13) Uani 1 1 d . . . . .
H28A H 0.219378 0.433280 0.762661 0.043 Uiso 1 1 calc R U . . .
H28B H 0.228771 0.517038 0.733077 0.043 Uiso 1 1 calc R U . . .
C29 C 0.2160(6) 0.5202(5) 0.8241(3) 0.069(2) Uani 1 1 d . . . . .
H29A H 0.147005 0.553053 0.814339 0.083 Uiso 1 1 calc R U . . .
H29B H 0.196984 0.480283 0.853245 0.083 Uiso 1 1 calc R U . . .
C30 C 0.3152(6) 0.5662(5) 0.8488(4) 0.068(2) Uani 1 1 d . . . . .
H30A H 0.317589 0.570138 0.893382 0.081 Uiso 1 1 calc R U . . .
H30B H 0.312137 0.618570 0.831327 0.081 Uiso 1 1 calc R U . . .
C31 C 0.4184(5) 0.5226(4) 0.8304(2) 0.0411(14) Uani 1 1 d . . . . .
H31A H 0.480971 0.558377 0.821640 0.049 Uiso 1 1 calc R U . . .
H31B H 0.448685 0.487257 0.863099 0.049 Uiso 1 1 calc R U . . .
C32 C 0.7996(4) 0.4801(3) 0.7475(2) 0.0262(11) Uani 1 1 d . . . . .
H32A H 0.814993 0.536013 0.746676 0.031 Uiso 1 1 calc R U . . .
H32B H 0.794019 0.460381 0.705554 0.031 Uiso 1 1 calc R U . . .
C33 C 0.8950(4) 0.4394(3) 0.7861(2) 0.0346(13) Uani 1 1 d . . . . .
H33A H 0.940664 0.476067 0.812807 0.042 Uiso 1 1 calc R U . . .
H33B H 0.947834 0.412490 0.760598 0.042 Uiso 1 1 calc R U . . .
C34 C 0.8318(5) 0.3827(3) 0.8228(2) 0.0367(13) Uani 1 1 d . . . . .
H34A H 0.815605 0.334115 0.800442 0.044 Uiso 1 1 calc R U . . .
H34B H 0.876339 0.371398 0.862081 0.044 Uiso 1 1 calc R U . . .
C35 C 0.7218(4) 0.4258(3) 0.8312(2) 0.0309(12) Uani 1 1 d . . . . .
H35A H 0.659072 0.389922 0.839783 0.037 Uiso 1 1 calc R U . . .
H35B H 0.734255 0.462853 0.865011 0.037 Uiso 1 1 calc R U . . .
C36 C 0.5738(5) 0.2257(3) 0.7871(3) 0.0507(13) Uani 1 1 d D U . . .
H36A H 0.641772 0.228713 0.817599 0.061 Uiso 0.773(7) 1 calc R U P B 1
H36B H 0.601253 0.215219 0.747060 0.061 Uiso 0.773(7) 1 calc R U P B 1
H36C H 0.618052 0.220064 0.827257 0.061 Uiso 0.227(7) 1 calc R U P B 2
H36D H 0.630069 0.228180 0.756325 0.061 Uiso 0.227(7) 1 calc R U P B 2
C37 C 0.4906(7) 0.1630(4) 0.8039(4) 0.0473(15) Uani 0.773(7) 1 d D U P B 1
H37A H 0.442102 0.143932 0.767846 0.057 Uiso 0.773(7) 1 calc R U P B 1
H37B H 0.532643 0.119373 0.824364 0.057 Uiso 0.773(7) 1 calc R U P B 1
C38 C 0.4191(6) 0.2056(4) 0.8463(3) 0.0411(15) Uani 0.773(7) 1 d D U P B 1
H38A H 0.459156 0.208589 0.887589 0.049 Uiso 0.773(7) 1 calc R U P B 1
H38B H 0.341989 0.181664 0.847959 0.049 Uiso 0.773(7) 1 calc R U P B 1
C39 C 0.4096(6) 0.2839(5) 0.8164(4) 0.0457(15) Uani 0.773(7) 1 d D U P B 1
H39A H 0.339262 0.286406 0.787379 0.055 Uiso 0.773(7) 1 calc R U P B 1
H39B H 0.404449 0.324469 0.847171 0.055 Uiso 0.773(7) 1 calc R U P B 1
C40 C 0.1513(7) 0.8369(4) 0.4851(5) 0.0579(15) Uani 0.766(6) 1 d D U P A 1
H40A H 0.166798 0.850519 0.443379 0.069 Uiso 0.766(6) 1 calc R U P A 1
H40B H 0.226352 0.826482 0.508832 0.069 Uiso 0.766(6) 1 calc R U P A 1
C41 C 0.0942(7) 0.8989(5) 0.5116(6) 0.0659(17) Uani 0.766(6) 1 d D U P A 1
H41A H 0.095119 0.945456 0.486069 0.079 Uiso 0.766(6) 1 calc R U P A 1
H41B H 0.132378 0.910959 0.552324 0.079 Uiso 0.766(6) 1 calc R U P A 1
C42 C -0.0287(6) 0.8716(5) 0.5157(5) 0.0576(15) Uani 0.766(6) 1 d D U P A 1
H42A H -0.044975 0.866148 0.558456 0.069 Uiso 0.766(6) 1 calc R U P A 1
H42B H -0.085039 0.908153 0.495348 0.069 Uiso 0.766(6) 1 calc R U P A 1
C43 C -0.0360(6) 0.7958(5) 0.4846(5) 0.0500(14) Uani 0.766(6) 1 d D U P A 1
H43A H -0.080905 0.758799 0.506875 0.060 Uiso 0.766(6) 1 calc R U P A 1
H43B H -0.073430 0.800975 0.442837 0.060 Uiso 0.766(6) 1 calc R U P A 1
O9 O 0.0397(15) 0.7483(10) 0.4910(9) 0.0489(18) Uani 0.234(6) 1 d D U P A 2
C47 C 0.004(2) 0.8124(11) 0.4550(13) 0.0528(16) Uani 0.234(6) 1 d D U P A 2
H47A H -0.081812 0.813143 0.448372 0.063 Uiso 0.234(6) 1 calc R U P A 2
H47B H 0.034604 0.807711 0.415056 0.063 Uiso 0.234(6) 1 calc R U P A 2
C46 C 0.058(2) 0.7707(12) 0.5530(10) 0.0510(18) Uani 0.234(6) 1 d D U P A 2
H46A H 0.127026 0.745145 0.573606 0.061 Uiso 0.234(6) 1 calc R U P A 2
H46B H -0.010494 0.758700 0.574770 0.061 Uiso 0.234(6) 1 calc R U P A 2
C49 C 0.046(3) 0.8862(14) 0.4846(12) 0.0581(16) Uani 0.234(6) 1 d D U P A 2
H49A H -0.015601 0.925796 0.482898 0.070 Uiso 0.234(6) 1 calc R U P A 2
H49B H 0.114834 0.906838 0.466853 0.070 Uiso 0.234(6) 1 calc R U P A 2
C48 C 0.076(2) 0.8556(12) 0.5487(12) 0.0586(17) Uani 0.234(6) 1 d D U P A 2
H48A H 0.157886 0.867709 0.561849 0.070 Uiso 0.234(6) 1 calc R U P A 2
H48B H 0.027025 0.881949 0.576509 0.070 Uiso 0.234(6) 1 calc R U P A 2
C51 C 0.389(2) 0.1950(13) 0.7473(12) 0.046(2) Uani 0.227(7) 1 d D U P B 2
H51A H 0.390288 0.200082 0.702914 0.056 Uiso 0.227(7) 1 calc R U P B 2
H51B H 0.320005 0.165308 0.755995 0.056 Uiso 0.227(7) 1 calc R U P B 2
C52 C 0.4985(18) 0.1580(11) 0.7753(14) 0.049(2) Uani 0.227(7) 1 d D U P B 2
H52A H 0.485431 0.130677 0.813108 0.059 Uiso 0.227(7) 1 calc R U P B 2
H52B H 0.531039 0.121796 0.746944 0.059 Uiso 0.227(7) 1 calc R U P B 2
C50 C 0.3917(13) 0.2716(13) 0.7771(13) 0.0437(17) Uani 0.227(7) 1 d D U P B 2
H50A H 0.346122 0.309236 0.751267 0.052 Uiso 0.227(7) 1 calc R U P B 2
H50B H 0.358281 0.268295 0.816454 0.052 Uiso 0.227(7) 1 calc R U P B 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 Sm1 3.4077(4) 3_666 ?
Sm1 K1 3.8941(10) . ?
Sm1 K2 3.7839(10) 3_666 ?
Sm1 O1 2.459(3) . ?
Sm1 O2 2.431(3) . ?
Sm1 O3 2.447(3) . ?
Sm1 N1 2.706(3) . ?
Sm1 N2 2.679(4) . ?
Sm1 N3 2.525(3) . ?
Sm1 N3 2.517(4) 3_666 ?
Sm1 N4 2.786(3) 3_666 ?
Sm1 N4 2.604(3) . ?
K1 O1 2.715(3) . ?
K1 O3 2.605(3) . ?
K1 O4 2.758(4) . ?
K1 O5 2.752(3) . ?
K1 O6 2.686(4) . ?
K1 C9 3.228(4) . ?
K1 C11 3.287(4) 3_666 ?
K1 C12 3.538(4) 3_666 ?
K1 C27 3.336(4) . ?
K2 O1 2.727(3) 3_666 ?
K2 O2 2.595(3) 3_666 ?
K2 O7 2.662(5) . ?
K2 N4 3.009(4) . ?
K2 C8 3.141(4) 3_666 ?
K2 C9 2.956(4) 3_666 ?
K2 C18 3.473(5) 3_666 ?
K2 C24 3.349(5) 3_566 ?
K2 O9 2.659(13) . ?
O1 C9 1.314(5) . ?
O2 C18 1.309(5) . ?
O3 C27 1.312(5) . ?
O4 C28 1.439(6) . ?
O4 C31 1.430(6) . ?
O5 C32 1.447(6) . ?
O5 C35 1.438(6) . ?
O6 C36 1.406(6) . ?
O6 C39 1.411(7) . ?
O6 C50 1.420(14) . ?
O7 C40 1.402(8) . ?
O7 C43 1.421(8) . ?
N1 C1 1.481(6) . ?
N1 C10 1.492(5) . ?
N1 C19 1.483(5) . ?
N2 C2 1.458(5) . ?
N2 C3 1.263(6) . ?
N3 C11 1.467(5) . ?
N3 C12 1.472(5) . ?
N4 C20 1.468(5) . ?
N4 C21 1.469(5) . ?
C1 C2 1.517(6) . ?
C3 C4 1.466(6) . ?
C4 C5 1.406(7) . ?
C4 C9 1.424(6) . ?
C5 C6 1.383(7) . ?
C6 C7 1.378(7) . ?
C7 C8 1.375(7) . ?
C8 C9 1.417(6) . ?
C10 C11 1.526(6) . ?
C12 C13 1.524(6) . ?
C12 C21 1.560(6) 3_666 ?
C13 C14 1.381(6) . ?
C13 C18 1.419(6) . ?
C14 C15 1.392(7) . ?
C15 C16 1.384(8) . ?
C16 C17 1.383(7) . ?
C17 C18 1.417(6) . ?
C19 C20 1.528(6) . ?
C21 C22 1.518(6) . ?
C22 C23 1.386(6) . ?
C22 C27 1.425(6) . ?
C23 C24 1.394(6) . ?
C24 C25 1.374(7) . ?
C25 C26 1.400(6) . ?
C26 C27 1.400(6) . ?
C28 C29 1.473(8) . ?
C29 C30 1.465(9) . ?
C30 C31 1.506(9) . ?
C32 C33 1.511(7) . ?
C33 C34 1.513(8) . ?
C34 C35 1.506(7) . ?
C36 C37 1.525(9) . ?
C36 C52 1.475(14) . ?
C37 C38 1.508(9) . ?
C38 C39 1.515(9) . ?
C40 C41 1.423(10) . ?
C41 C42 1.513(9) . ?
C42 C43 1.488(9) . ?
O9 C47 1.413(15) . ?
O9 C46 1.426(15) . ?
C47 C49 1.505(15) . ?
C46 C48 1.497(15) . ?
C49 C48 1.529(15) . ?
C51 C52 1.501(15) . ?
C51 C50 1.489(15) . ?

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
Sm1 Sm1 K1 109.932(17) 3_666 . ?
Sm1 Sm1 K2 100.180(17) 3_666 3_666 ?
K2 Sm1 K1 87.05(2) 3_666 . ?
O1 Sm1 Sm1 123.09(7) . 3_666 ?
O1 Sm1 K1 43.73(7) . . ?
O1 Sm1 K2 45.99(7) . 3_666 ?
O1 Sm1 N1 136.12(10) . . ?
O1 Sm1 N2 69.53(10) . . ?
O1 Sm1 N3 139.47(10) . . ?
O1 Sm1 N3 88.67(10) . 3_666 ?
O1 Sm1 N4 141.49(10) . . ?
O1 Sm1 N4 86.36(10) . 3_666 ?
O2 Sm1 Sm1 113.18(7) . 3_666 ?
O2 Sm1 K1 117.33(7) . . ?
O2 Sm1 K2 42.83(7) . 3_666 ?
O2 Sm1 O1 74.65(10) . . ?
O2 Sm1 O3 130.06(10) . . ?
O2 Sm1 N1 85.78(10) . . ?
O2 Sm1 N2 68.35(10) . . ?
O2 Sm1 N3 139.63(11) . 3_666 ?
O2 Sm1 N3 76.81(11) . . ?
O2 Sm1 N4 143.85(10) . . ?
O2 Sm1 N4 74.15(10) . 3_666 ?
O3 Sm1 Sm1 116.71(7) . 3_666 ?
O3 Sm1 K1 41.08(7) . . ?
O3 Sm1 K2 122.76(7) . 3_666 ?
O3 Sm1 O1 76.89(9) . . ?
O3 Sm1 N1 87.30(10) . . ?
O3 Sm1 N2 63.54(10) . . ?
O3 Sm1 N3 143.39(10) . . ?
O3 Sm1 N3 78.66(11) . 3_666 ?
O3 Sm1 N4 143.14(10) . 3_666 ?
O3 Sm1 N4 74.47(10) . . ?
N1 Sm1 Sm1 100.65(7) . 3_666 ?
N1 Sm1 K1 127.55(8) . . ?
N1 Sm1 K2 128.61(7) . 3_666 ?
N1 Sm1 N4 125.82(10) . 3_666 ?
N2 Sm1 Sm1 167.38(8) . 3_666 ?
N2 Sm1 K1 78.79(8) . . ?
N2 Sm1 K2 89.15(8) . 3_666 ?
N2 Sm1 N1 66.77(10) . . ?
N2 Sm1 N4 139.43(10) . 3_666 ?
N3 Sm1 Sm1 47.57(8) 3_666 3_666 ?
N3 Sm1 Sm1 47.38(8) . 3_666 ?
N3 Sm1 K1 157.11(8) . . ?
N3 Sm1 K1 62.45(8) 3_666 . ?
N3 Sm1 K2 99.93(8) 3_666 3_666 ?
N3 Sm1 K2 93.82(8) . 3_666 ?
N3 Sm1 N1 128.30(10) 3_666 . ?
N3 Sm1 N1 68.37(11) . . ?
N3 Sm1 N2 139.38(11) 3_666 . ?
N3 Sm1 N2 124.08(11) . . ?
N3 Sm1 N3 94.95(10) 3_666 . ?
N3 Sm1 N4 60.92(10) 3_666 . ?
N3 Sm1 N4 58.30(10) . 3_666 ?
N3 Sm1 N4 68.22(10) 3_666 3_666 ?
N3 Sm1 N4 71.09(11) . . ?
N4 Sm1 Sm1 53.20(7) . 3_666 ?
N4 Sm1 Sm1 48.44(7) 3_666 3_666 ?
N4 Sm1 K1 98.49(7) . . ?
N4 Sm1 K1 106.20(7) 3_666 . ?
N4 Sm1 K2 153.16(8) . 3_666 ?
N4 Sm1 K2 51.85(7) 3_666 3_666 ?
N4 Sm1 N1 67.39(10) . . ?
N4 Sm1 N2 117.67(11) . . ?
N4 Sm1 N4 101.64(9) . 3_666 ?
O1 K1 Sm1 38.75(6) . . ?
O1 K1 O4 166.34(10) . . ?
O1 K1 O5 99.53(9) . . ?
O1 K1 C9 23.58(10) . . ?
O1 K1 C11 68.73(10) . 3_666 ?
O1 K1 C12 88.02(9) . 3_666 ?
O1 K1 C27 91.21(10) . . ?
O3 K1 Sm1 38.12(6) . . ?
O3 K1 O1 69.93(9) . . ?
O3 K1 O4 102.87(10) . . ?
O3 K1 O5 159.52(10) . . ?
O3 K1 O6 114.90(11) . . ?
O3 K1 C9 81.13(10) . . ?
O3 K1 C11 83.78(10) . 3_666 ?
O3 K1 C12 55.71(9) . 3_666 ?
O3 K1 C27 21.29(10) . . ?
O4 K1 Sm1 129.23(8) . . ?
O4 K1 C9 169.97(11) . . ?
O4 K1 C11 99.44(11) . 3_666 ?
O4 K1 C12 78.40(10) . 3_666 ?
O4 K1 C27 81.91(11) . . ?
O5 K1 Sm1 123.80(7) . . ?
O5 K1 O4 83.49(10) . . ?
O5 K1 C9 95.92(10) . . ?
O5 K1 C11 75.94(10) . 3_666 ?
O5 K1 C12 107.87(10) . 3_666 ?
O5 K1 C27 158.38(11) . . ?
O6 K1 Sm1 135.65(10) . . ?
O6 K1 O1 111.27(11) . . ?
O6 K1 O4 82.19(11) . . ?
O6 K1 O5 85.08(11) . . ?
O6 K1 C9 87.78(12) . . ?
O6 K1 C11 160.58(11) . 3_666 ?
O6 K1 C12 155.09(11) . 3_666 ?
O6 K1 C27 108.53(11) . . ?
C9 K1 Sm1 59.07(8) . . ?
C9 K1 C11 90.09(11) . 3_666 ?
C9 K1 C12 111.17(10) . 3_666 ?
C9 K1 C27 101.19(11) . . ?
C11 K1 Sm1 56.82(8) 3_666 . ?
C11 K1 C12 40.90(10) 3_666 3_666 ?
C11 K1 C27 90.82(10) 3_666 . ?
C12 K1 Sm1 53.90(7) 3_666 . ?
C27 K1 Sm1 57.36(8) . . ?
C27 K1 C12 53.46(10) . 3_666 ?
O1 K2 Sm1 40.43(6) 3_666 3_666 ?
O1 K2 N4 77.49(9) 3_666 . ?
O1 K2 C8 46.76(10) 3_666 3_666 ?
O1 K2 C9 26.34(10) 3_666 3_666 ?
O1 K2 C18 86.27(10) 3_666 3_666 ?
O1 K2 C24 104.37(10) 3_666 3_566 ?
O2 K2 Sm1 39.56(7) 3_666 3_666 ?
O2 K2 O1 67.66(9) 3_666 3_666 ?
O2 K2 O7 92.87(14) 3_666 . ?
O2 K2 N4 68.13(9) 3_666 . ?
O2 K2 C8 101.25(11) 3_666 3_666 ?
O2 K2 C9 75.42(11) 3_666 3_666 ?
O2 K2 C18 18.62(10) 3_666 3_666 ?
O2 K2 C24 169.25(11) 3_666 3_566 ?
O2 K2 O9 101.8(4) 3_666 . ?
O7 K2 Sm1 128.90(12) . 3_666 ?
O7 K2 O1 119.23(15) . 3_666 ?
O7 K2 N4 148.77(15) . . ?
O7 K2 C8 86.83(17) . 3_666 ?
O7 K2 C9 94.54(16) . 3_666 ?
O7 K2 C18 83.01(14) . 3_666 ?
O7 K2 C24 97.46(14) . 3_566 ?
N4 K2 Sm1 46.72(7) . 3_666 ?
N4 K2 C8 120.17(11) . 3_666 ?
N4 K2 C18 71.37(10) . 3_666 ?
N4 K2 C24 103.67(11) . 3_566 ?
C8 K2 Sm1 86.70(8) 3_666 3_666 ?
C8 K2 C18 116.25(12) 3_666 3_666 ?
C8 K2 C24 76.48(11) 3_666 3_566 ?
C9 K2 Sm1 62.31(8) 3_666 3_666 ?
C9 K2 N4 103.68(11) 3_666 . ?
C9 K2 C8 26.65(11) 3_666 3_666 ?
C9 K2 C18 91.95(12) 3_666 3_666 ?
C9 K2 C24 100.71(12) 3_666 3_566 ?
C18 K2 Sm1 55.54(7) 3_666 3_666 ?
C24 K2 Sm1 129.74(9) 3_566 3_666 ?
C24 K2 C18 167.24(11) 3_566 3_666 ?
O9 K2 N4 143.7(4) . . ?
O9 K2 C24 88.9(4) . 3_566 ?
Sm1 O1 K1 97.52(10) . . ?
Sm1 O1 K2 93.59(10) . 3_666 ?
K1 O1 K2 152.73(12) . 3_666 ?
C9 O1 Sm1 139.2(3) . . ?
C9 O1 K1 100.7(2) . . ?
C9 O1 K2 86.6(2) . 3_666 ?
Sm1 O2 K2 97.61(11) . 3_666 ?
C18 O2 Sm1 127.6(3) . . ?
C18 O2 K2 122.1(3) . 3_666 ?
Sm1 O3 K1 100.79(10) . . ?
C27 O3 Sm1 135.4(3) . . ?
C27 O3 K1 112.6(2) . . ?
C28 O4 K1 124.4(3) . . ?
C31 O4 K1 126.7(3) . . ?
C31 O4 C28 108.9(4) . . ?
C32 O5 K1 116.7(3) . . ?
C35 O5 K1 115.8(3) . . ?
C35 O5 C32 108.5(3) . . ?
C36 O6 K1 125.2(3) . . ?
C36 O6 C39 109.7(5) . . ?
C36 O6 C50 105.4(10) . . ?
C39 O6 K1 119.7(4) . . ?
C50 O6 K1 100.2(12) . . ?
C40 O7 K2 115.4(4) . . ?
C40 O7 C43 108.0(6) . . ?
C43 O7 K2 135.1(5) . . ?
C1 N1 Sm1 110.2(2) . . ?
C1 N1 C10 109.7(3) . . ?
C1 N1 C19 109.2(3) . . ?
C10 N1 Sm1 110.6(2) . . ?
C19 N1 Sm1 106.1(2) . . ?
C19 N1 C10 111.0(3) . . ?
C2 N2 Sm1 111.5(3) . . ?
C3 N2 Sm1 131.7(3) . . ?
C3 N2 C2 116.5(4) . . ?
Sm1 N3 Sm1 85.05(10) 3_666 . ?
C11 N3 Sm1 117.3(2) . . ?
C11 N3 Sm1 118.0(3) . 3_666 ?
C11 N3 C12 109.2(3) . . ?
C12 N3 Sm1 112.2(2) . . ?
C12 N3 Sm1 113.4(2) . 3_666 ?
Sm1 N4 Sm1 78.36(9) . 3_666 ?
Sm1 N4 K2 81.43(9) 3_666 . ?
Sm1 N4 K2 159.25(14) . . ?
C20 N4 Sm1 115.9(2) . . ?
C20 N4 Sm1 131.3(2) . 3_666 ?
C20 N4 K2 74.7(2) . . ?
C20 N4 C21 109.1(3) . . ?
C21 N4 Sm1 108.9(2) . 3_666 ?
C21 N4 Sm1 108.8(2) . . ?
C21 N4 K2 82.2(2) . . ?
N1 C1 C2 113.2(4) . . ?
N2 C2 C1 110.2(4) . . ?
N2 C3 C4 127.4(4) . . ?
C5 C4 C3 116.6(4) . . ?
C5 C4 C9 118.8(4) . . ?
C9 C4 C3 124.6(4) . . ?
C6 C5 C4 123.0(5) . . ?
C7 C6 C5 118.3(5) . . ?
C8 C7 C6 120.4(4) . . ?
C7 C8 K2 125.4(3) . 3_666 ?
C7 C8 C9 123.0(4) . . ?
C9 C8 K2 69.4(2) . 3_666 ?
K2 C9 K1 117.50(14) 3_666 . ?
O1 C9 K1 55.8(2) . . ?
O1 C9 K2 67.0(2) . 3_666 ?
O1 C9 C4 124.1(4) . . ?
O1 C9 C8 119.5(4) . . ?
C4 C9 K1 111.9(3) . . ?
C4 C9 K2 120.0(3) . 3_666 ?
C8 C9 K1 102.6(3) . . ?
C8 C9 K2 84.0(3) . 3_666 ?
C8 C9 C4 116.4(4) . . ?
N1 C10 C11 114.1(3) . . ?
N3 C11 C10 114.8(3) . . ?
N3 C12 C13 113.4(3) . . ?
N3 C12 C21 110.8(3) . 3_666 ?
C13 C12 C21 112.2(3) . 3_666 ?
C14 C13 C12 121.0(4) . . ?
C14 C13 C18 119.8(4) . . ?
C18 C13 C12 119.0(4) . . ?
C13 C14 C15 122.4(5) . . ?
C16 C15 C14 118.5(5) . . ?
C17 C16 C15 120.4(5) . . ?
C16 C17 C18 122.0(5) . . ?
O2 C18 K2 39.3(2) . 3_666 ?
O2 C18 C13 121.1(4) . . ?
O2 C18 C17 122.1(4) . . ?
C13 C18 K2 109.2(3) . 3_666 ?
C17 C18 K2 119.5(3) . 3_666 ?
C17 C18 C13 116.9(4) . . ?
N1 C19 C20 112.8(3) . . ?
N4 C20 C19 114.5(3) . . ?
N4 C21 C12 110.3(3) . 3_666 ?
N4 C21 C22 115.3(3) . . ?
C22 C21 C12 110.4(3) . 3_666 ?
C23 C22 C21 121.8(4) . . ?
C23 C22 C27 119.2(4) . . ?
C27 C22 C21 119.0(4) . . ?
C22 C23 C24 122.0(4) . . ?
C23 C24 K2 112.6(3) . 3_566 ?
C25 C24 K2 95.0(3) . 3_566 ?
C25 C24 C23 119.5(4) . . ?
C24 C25 C26 119.6(4) . . ?
C27 C26 C25 122.0(4) . . ?
O3 C27 K1 46.14(19) . . ?
O3 C27 C22 120.7(4) . . ?
O3 C27 C26 121.6(4) . . ?
C22 C27 K1 116.8(3) . . ?
C26 C27 K1 105.7(3) . . ?
C26 C27 C22 117.7(4) . . ?
O4 C28 C29 106.7(4) . . ?
C30 C29 C28 104.9(5) . . ?
C29 C30 C31 103.7(5) . . ?
O4 C31 C30 106.1(5) . . ?
O5 C32 C33 106.5(4) . . ?
C32 C33 C34 104.3(4) . . ?
C35 C34 C33 101.6(4) . . ?
O5 C35 C34 104.8(4) . . ?
O6 C36 C37 105.6(5) . . ?
O6 C36 C52 112.0(10) . . ?
C38 C37 C36 101.4(6) . . ?
C37 C38 C39 101.0(6) . . ?
O6 C39 C38 107.3(5) . . ?
O7 C40 C41 109.4(7) . . ?
C40 C41 C42 105.2(7) . . ?
C43 C42 C41 105.3(7) . . ?
O7 C43 C42 104.9(6) . . ?
C47 O9 K2 124.7(16) . . ?
C47 O9 C46 109.8(18) . . ?
C46 O9 K2 114.1(13) . . ?
O9 C47 C49 111(2) . . ?
O9 C46 C48 102.6(19) . . ?
C47 C49 C48 98(2) . . ?
C46 C48 C49 113(2) . . ?
C50 C51 C52 102.8(19) . . ?
C36 C52 C51 101.0(16) . . ?
O6 C50 C51 106.7(16) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Sm1 O1 C9 K1 -114.9(4) . . . . ?
Sm1 O1 C9 K2 91.6(3) . . . 3_666 ?
Sm1 O1 C9 C4 -20.1(7) . . . . ?
Sm1 O1 C9 C8 159.8(3) . . . . ?
Sm1 O2 C18 K2 132.9(4) . . . 3_666 ?
Sm1 O2 C18 C13 50.3(5) . . . . ?
Sm1 O2 C18 C17 -128.4(4) . . . . ?
Sm1 O3 C27 K1 -135.2(4) . . . . ?
Sm1 O3 C27 C22 -36.2(6) . . . . ?
Sm1 O3 C27 C26 143.5(3) . . . . ?
Sm1 N1 C1 C2 41.6(4) . . . . ?
Sm1 N1 C10 C11 -34.1(4) . . . . ?
Sm1 N1 C19 C20 52.6(4) . . . . ?
Sm1 N2 C2 C1 48.0(4) . . . . ?
Sm1 N2 C3 C4 -3.4(8) . . . . ?
Sm1 N3 C11 C10 -132.4(3) 3_666 . . . ?
Sm1 N3 C11 C10 -32.9(4) . . . . ?
Sm1 N3 C12 C13 166.5(3) 3_666 . . . ?
Sm1 N3 C12 C13 72.2(4) . . . . ?
Sm1 N3 C12 C21 -55.1(4) . . . 3_666 ?
Sm1 N3 C12 C21 39.3(4) 3_666 . . 3_666 ?
Sm1 N4 C20 C19 18.6(4) . . . . ?
Sm1 N4 C20 C19 116.0(4) 3_666 . . . ?
Sm1 N4 C21 C12 -36.3(4) 3_666 . . 3_666 ?
Sm1 N4 C21 C12 47.4(4) . . . 3_666 ?
Sm1 N4 C21 C22 -162.2(3) 3_666 . . . ?
Sm1 N4 C21 C22 -78.5(3) . . . . ?
K1 O1 C9 K2 -153.50(14) . . . 3_666 ?
K1 O1 C9 C4 94.8(4) . . . . ?
K1 O1 C9 C8 -85.3(4) . . . . ?
K1 O3 C27 C22 99.1(4) . . . . ?
K1 O3 C27 C26 -81.3(4) . . . . ?
K1 O4 C28 C29 171.5(4) . . . . ?
K1 O4 C31 C30 168.7(4) . . . . ?
K1 O5 C32 C33 -126.0(3) . . . . ?
K1 O5 C35 C34 105.1(4) . . . . ?
K1 O6 C36 C37 -136.8(5) . . . . ?
K1 O6 C36 C52 -111.0(14) . . . . ?
K1 O6 C39 C38 163.1(5) . . . . ?
K1 O6 C50 C51 106.8(18) . . . . ?
K2 O1 C9 K1 153.50(14) 3_666 . . . ?
K2 O1 C9 C4 -111.7(4) 3_666 . . . ?
K2 O1 C9 C8 68.2(4) 3_666 . . . ?
K2 O2 C18 C13 -82.5(5) 3_666 . . . ?
K2 O2 C18 C17 98.7(4) 3_666 . . . ?
K2 O7 C40 C41 -167.1(7) . . . . ?
K2 O7 C43 C42 168.0(6) . . . . ?
K2 N4 C20 C19 179.6(4) . . . . ?
K2 N4 C21 C12 -114.5(3) . . . 3_666 ?
K2 N4 C21 C22 119.7(3) . . . . ?
K2 C8 C9 K1 -116.88(17) 3_666 . . . ?
K2 C8 C9 O1 -59.3(3) 3_666 . . . ?
K2 C8 C9 C4 120.6(4) 3_666 . . . ?
K2 C24 C25 C26 120.5(4) 3_566 . . . ?
K2 O9 C47 C49 -115(2) . . . . ?
K2 O9 C46 C48 124.0(17) . . . . ?
O4 C28 C29 C30 26.0(8) . . . . ?
O5 C32 C33 C34 17.0(6) . . . . ?
O6 C36 C37 C38 -34.3(8) . . . . ?
O6 C36 C52 C51 18(2) . . . . ?
O7 C40 C41 C42 -11.4(12) . . . . ?
N1 C1 C2 N2 -62.5(5) . . . . ?
N1 C10 C11 N3 45.7(5) . . . . ?
N1 C19 C20 N4 -50.5(5) . . . . ?
N2 C3 C4 C5 -168.6(5) . . . . ?
N2 C3 C4 C9 13.3(8) . . . . ?
N3 C12 C13 C14 110.8(4) . . . . ?
N3 C12 C13 C18 -64.8(5) . . . . ?
N4 C21 C22 C23 -116.5(4) . . . . ?
N4 C21 C22 C27 63.3(5) . . . . ?
C1 N1 C10 C11 -155.8(3) . . . . ?
C1 N1 C19 C20 171.4(3) . . . . ?
C2 N2 C3 C4 -176.3(4) . . . . ?
C3 N2 C2 C1 -137.7(4) . . . . ?
C3 C4 C5 C6 -179.0(5) . . . . ?
C3 C4 C9 K1 59.8(5) . . . . ?
C3 C4 C9 K2 -84.0(5) . . . 3_666 ?
C3 C4 C9 O1 -2.7(7) . . . . ?
C3 C4 C9 C8 177.3(4) . . . . ?
C4 C5 C6 C7 2.0(9) . . . . ?
C5 C4 C9 K1 -118.3(4) . . . . ?
C5 C4 C9 K2 97.9(5) . . . 3_666 ?
C5 C4 C9 O1 179.1(5) . . . . ?
C5 C4 C9 C8 -0.8(7) . . . . ?
C5 C6 C7 C8 -1.7(8) . . . . ?
C6 C7 C8 K2 -86.7(5) . . . 3_666 ?
C6 C7 C8 C9 0.2(8) . . . . ?
C7 C8 C9 K1 123.5(4) . . . . ?
C7 C8 C9 K2 -119.6(4) . . . 3_666 ?
C7 C8 C9 O1 -178.9(4) . . . . ?
C7 C8 C9 C4 1.1(7) . . . . ?
C9 C4 C5 C6 -0.7(8) . . . . ?
C10 N1 C1 C2 163.6(3) . . . . ?
C10 N1 C19 C20 -67.6(4) . . . . ?
C11 N3 C12 C13 -59.6(4) . . . . ?
C11 N3 C12 C21 173.1(3) . . . 3_666 ?
C12 N3 C11 C10 96.1(4) . . . . ?
C12 C13 C14 C15 -175.9(4) . . . . ?
C12 C13 C18 K2 -44.6(4) . . . 3_666 ?
C12 C13 C18 O2 -2.9(6) . . . . ?
C12 C13 C18 C17 175.9(4) . . . . ?
C12 C21 C22 C23 117.7(4) 3_666 . . . ?
C12 C21 C22 C27 -62.5(5) 3_666 . . . ?
C13 C14 C15 C16 0.4(7) . . . . ?
C14 C13 C18 K2 139.7(3) . . . 3_666 ?
C14 C13 C18 O2 -178.6(4) . . . . ?
C14 C13 C18 C17 0.2(6) . . . . ?
C14 C15 C16 C17 -0.3(7) . . . . ?
C15 C16 C17 C18 0.2(7) . . . . ?
C16 C17 C18 K2 -135.4(4) . . . 3_666 ?
C16 C17 C18 O2 178.7(4) . . . . ?
C16 C17 C18 C13 -0.1(7) . . . . ?
C18 C13 C14 C15 -0.3(7) . . . . ?
C19 N1 C1 C2 -74.6(4) . . . . ?
C19 N1 C10 C11 83.4(4) . . . . ?
C20 N4 C21 C12 174.8(3) . . . 3_666 ?
C20 N4 C21 C22 48.9(4) . . . . ?
C21 N4 C20 C19 -104.6(4) . . . . ?
C21 C12 C13 C14 -122.7(4) 3_666 . . . ?
C21 C12 C13 C18 61.7(5) 3_666 . . . ?
C21 C22 C23 C24 179.4(4) . . . . ?
C21 C22 C27 K1 53.7(4) . . . . ?
C21 C22 C27 O3 0.8(6) . . . . ?
C21 C22 C27 C26 -178.8(4) . . . . ?
C22 C23 C24 K2 -110.7(4) . . . 3_566 ?
C22 C23 C24 C25 -0.5(7) . . . . ?
C23 C22 C27 K1 -126.4(3) . . . . ?
C23 C22 C27 O3 -179.3(4) . . . . ?
C23 C22 C27 C26 1.0(6) . . . . ?
C23 C24 C25 C26 0.9(7) . . . . ?
C24 C25 C26 C27 -0.3(7) . . . . ?
C25 C26 C27 K1 132.0(4) . . . . ?
C25 C26 C27 O3 179.7(4) . . . . ?
C25 C26 C27 C22 -0.6(6) . . . . ?
C27 C22 C23 C24 -0.5(6) . . . . ?
C28 O4 C31 C30 -10.1(6) . . . . ?
C28 C29 C30 C31 -31.4(8) . . . . ?
C29 C30 C31 O4 25.8(8) . . . . ?
C31 O4 C28 C29 -9.7(7) . . . . ?
C32 O5 C35 C34 -28.4(5) . . . . ?
C32 C33 C34 C35 -33.0(5) . . . . ?
C33 C34 C35 O5 37.8(5) . . . . ?
C35 O5 C32 C33 7.0(5) . . . . ?
C36 O6 C39 C38 7.9(9) . . . . ?
C36 O6 C50 C51 -24(2) . . . . ?
C36 C37 C38 C39 37.2(8) . . . . ?
C37 C38 C39 O6 -29.0(9) . . . . ?
C39 O6 C36 C37 16.8(8) . . . . ?
C40 O7 C43 C42 -27.5(10) . . . . ?
C40 C41 C42 C43 -5.5(12) . . . . ?
C41 C42 C43 O7 19.8(11) . . . . ?
C43 O7 C40 C41 24.9(11) . . . . ?
O9 C47 C49 C48 -17(3) . . . . ?
O9 C46 C48 C49 11(3) . . . . ?
C47 O9 C46 C48 -21(3) . . . . ?
C47 C49 C48 C46 3(3) . . . . ?
C46 O9 C47 C49 26(3) . . . . ?
C52 C51 C50 O6 35(3) . . . . ?
C50 O6 C36 C52 3.8(19) . . . . ?
C50 C51 C52 C36 -31(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.000 143.8 33.5 '0.8 THF'
2 0.500 0.000 0.500 143.8 33.5 '0.8 THF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.585
_oxdiff_exptl_absorpt_empirical_full_min 0.583
