# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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. 
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data_kp271
_database_code_depnum_ccdc_archive 'CCDC 1939447'
loop_
_audit_author_name
_audit_author_address
'Olaf Fuhr'
;Karlsruher Institut fuer Technologie (KIT)
Germany
;
_audit_update_record             
;
2020-01-21 deposited with the CCDC.	2020-01-24 downloaded from the CCDC.
;
_audit_creation_date             2018-10-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C34 H34 Br2 N11 O5 Yb, H2 O, 2(C H4 O), 2(N O3), C2 H3 N'
_chemical_formula_sum            'C38 H47 Br2 N14 O14 Yb'
_chemical_formula_weight         1256.75
_chemical_melting_point          ?
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'
Br Br -0.6763 1.2805 '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'
Yb Yb -7.2108 4.4329 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3185(3)
_cell_length_b                   16.0985(5)
_cell_length_c                   16.1412(5)
_cell_angle_alpha                118.099(2)
_cell_angle_beta                 96.000(2)
_cell_angle_gamma                92.008(2)
_cell_volume                     2341.39(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    58511
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      73.53
_cell_measurement_theta_min      5.49
_shelx_estimated_absorpt_T_max   0.784
_shelx_estimated_absorpt_T_min   0.268
_exptl_absorpt_coefficient_mu    6.383
_exptl_absorpt_correction_T_max  0.4162
_exptl_absorpt_correction_T_min  0.1042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1250
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20575
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.866
_diffrn_reflns_theta_min         5.490
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'Eiger R 4M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_target            Ga
_diffrn_source_type              'Metaljet D2'
_diffrn_source_voltage           70
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8177
_reflns_number_total             8960
_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_data_collection       
;
X-Area Pilatus3_SV 1.31.144.0 (STOE, 2018)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.0.0 (STOE, 2018)
X-Area LANA 1.72.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.681
_refine_diff_density_min         -2.941
_refine_diff_density_rms         0.225
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         8960
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0601
_refine_ls_restrained_S_all      1.066
_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)+(0.1256P)²+2.2806P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1604
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H12A-O13
 1.82 with sigma of 0.02
 H13-O14
 1.84 with sigma of 0.02
 H13-H14A = H13-H14B
 2.2 with sigma of 0.02
3.a Free rotating group:
 O14(H14A,H14B)
3.b Ternary CH refined with riding coordinates:
 N5(H5), N6(H6)
3.c Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B)
3.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N8(H8), N10(H10), C3(H3A), C4(H4), C5(H5A), C6(H6A), C8(H8A),
 C12(H12), C14(H14), C24(H24), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33),
  C34(H34)
3.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C38(H38A,H38B,H38C), C37(H37A,H37B,
 H37C), C36(H36A,H36B,H36C)
3.f Idealised tetrahedral OH refined as rotating group:
 O13(H13), O12(H12A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.84054(2) 0.80940(2) 0.61139(2) 0.01934(12) Uani 1 1 d . . . . .
Br1 Br 1.23744(6) 0.82814(4) 0.22901(4) 0.03501(16) Uani 1 1 d . . . . .
Br2 Br 0.13998(5) 0.55028(4) 0.48823(4) 0.03048(15) Uani 1 1 d . . . . .
O1 O 0.9265(3) 0.7499(2) 0.4828(2) 0.0235(6) Uani 1 1 d . . . . .
O2 O 0.6735(3) 0.7212(2) 0.4988(2) 0.0226(6) Uani 1 1 d . . . . .
O3 O 0.7394(4) 0.9172(2) 0.5685(3) 0.0307(7) Uani 1 1 d . . . . .
O4 O 0.6394(3) 0.8852(3) 0.6628(3) 0.0330(8) Uani 1 1 d . . . . .
O5 O 0.5488(5) 0.9695(3) 0.6021(4) 0.0554(13) Uani 1 1 d . . . . .
N1 N 0.8928(4) 0.9338(3) 0.7667(3) 0.0252(8) Uani 1 1 d . . . . .
N2 N 0.9957(4) 1.0765(3) 0.8739(3) 0.0279(9) Uani 1 1 d . . . . .
H2 H 1.048150 1.129025 0.897855 0.033 Uiso 1 1 calc R . . . .
N3 N 1.0370(4) 1.0100(3) 0.7141(3) 0.0276(8) Uani 1 1 d . . . . .
H3 H 1.087138 1.060310 0.724846 0.033 Uiso 1 1 calc R . . . .
N4 N 1.0150(4) 0.9310(3) 0.6265(3) 0.0230(8) Uani 1 1 d . . . . .
N5 N 0.7933(4) 0.6070(3) 0.3175(3) 0.0251(8) Uani 1 1 d . . . . .
H5 H 0.788118 0.656121 0.384227 0.030 Uiso 1 1 calc R . . . .
N6 N 0.5797(4) 0.7542(3) 0.3602(3) 0.0249(8) Uani 1 1 d . . . . .
H6 H 0.651578 0.758449 0.409048 0.030 Uiso 1 1 calc R . . . .
N7 N 0.7513(4) 0.6897(3) 0.6501(3) 0.0214(7) Uani 1 1 d . . . . .
N8 N 0.8351(4) 0.6736(3) 0.7137(3) 0.0257(8) Uani 1 1 d . . . . .
H8 H 0.807109 0.648053 0.747016 0.031 Uiso 1 1 calc R . . . .
N9 N 1.0052(4) 0.7479(3) 0.6770(3) 0.0220(8) Uani 1 1 d . . . . .
N10 N 1.0588(4) 0.6831(3) 0.7721(3) 0.0267(8) Uani 1 1 d . . . . .
H10 H 1.049253 0.651890 0.803795 0.032 Uiso 1 1 calc R . . . .
N11 N 0.6386(4) 0.9261(3) 0.6116(3) 0.0344(10) Uani 1 1 d . . . . .
C1 C 0.8517(5) 0.9591(3) 0.8543(3) 0.0269(10) Uani 1 1 d . . . . .
C2 C 0.9145(5) 1.0488(3) 0.9223(3) 0.0269(10) Uani 1 1 d . . . . .
C3 C 0.8937(6) 1.0904(4) 1.0157(4) 0.0342(11) Uani 1 1 d . . . . .
H3A H 0.936799 1.150445 1.060881 0.041 Uiso 1 1 calc R . . . .
C4 C 0.8069(6) 1.0408(4) 1.0414(4) 0.0384(12) Uani 1 1 d . . . . .
H4 H 0.788795 1.068090 1.104995 0.046 Uiso 1 1 calc R . . . .
C5 C 0.7464(6) 0.9515(4) 0.9746(4) 0.0386(12) Uani 1 1 d . . . . .
H5A H 0.689245 0.918645 0.994158 0.046 Uiso 1 1 calc R . . . .
C6 C 0.7678(5) 0.9095(4) 0.8803(4) 0.0330(11) Uani 1 1 d . . . . .
H6A H 0.726076 0.848844 0.835369 0.040 Uiso 1 1 calc R . . . .
C7 C 0.9777(5) 1.0059(3) 0.7823(3) 0.0254(9) Uani 1 1 d . . . . .
C8 C 1.0765(5) 0.9343(3) 0.5617(3) 0.0260(9) Uani 1 1 d . . . . .
H8A H 1.130140 0.990736 0.579002 0.031 Uiso 1 1 calc R . . . .
C9 C 1.0699(5) 0.8587(3) 0.4651(3) 0.0237(9) Uani 1 1 d . . . . .
C10 C 0.9986(4) 0.7696(3) 0.4308(3) 0.0223(9) Uani 1 1 d . . . . .
C11 C 1.0042(5) 0.6982(3) 0.3369(3) 0.0241(9) Uani 1 1 d . . . . .
C12 C 1.0749(5) 0.7165(4) 0.2776(3) 0.0268(10) Uani 1 1 d . . . . .
H12 H 1.077072 0.668826 0.214258 0.032 Uiso 1 1 calc R . . . .
C13 C 1.1426(5) 0.8052(4) 0.3118(4) 0.0270(10) Uani 1 1 d . . . . .
C14 C 1.1428(5) 0.8750(4) 0.4042(4) 0.0265(10) Uani 1 1 d . . . . .
H14 H 1.192326 0.934260 0.426707 0.032 Uiso 1 1 calc R . . . .
C15 C 0.9362(5) 0.6020(3) 0.3042(3) 0.0276(10) Uani 1 1 d . . . . .
H15A H 0.979754 0.572868 0.340323 0.033 Uiso 1 1 calc R . . . .
H15B H 0.943352 0.561242 0.236248 0.033 Uiso 1 1 calc R . . . .
C16 C 0.7357(6) 0.5146(4) 0.3046(4) 0.0344(11) Uani 1 1 d . . . . .
H16A H 0.740456 0.464966 0.239785 0.052 Uiso 1 1 calc GR . . . .
H16B H 0.644010 0.519255 0.315642 0.052 Uiso 1 1 calc GR . . . .
H16C H 0.784830 0.498787 0.349796 0.052 Uiso 1 1 calc GR . . . .
C17 C 0.7203(5) 0.6375(4) 0.2524(4) 0.0292(10) Uani 1 1 d . . . . .
H17A H 0.715853 0.586163 0.186258 0.035 Uiso 1 1 calc R . . . .
H17B H 0.770066 0.693724 0.257397 0.035 Uiso 1 1 calc R . . . .
C18 C 0.5821(5) 0.6612(4) 0.2731(4) 0.0288(10) Uani 1 1 d . . . . .
H18A H 0.532689 0.663137 0.218114 0.035 Uiso 1 1 calc R . . . .
H18B H 0.537688 0.610603 0.281249 0.035 Uiso 1 1 calc R . . . .
C19 C 0.6056(6) 0.8362(4) 0.3432(4) 0.0355(12) Uani 1 1 d . . . . .
H19A H 0.539975 0.831828 0.292501 0.053 Uiso 1 1 calc GR . . . .
H19B H 0.693074 0.835454 0.324567 0.053 Uiso 1 1 calc GR . . . .
H19C H 0.600684 0.895154 0.401467 0.053 Uiso 1 1 calc GR . . . .
C20 C 0.4526(5) 0.7585(4) 0.3999(4) 0.0285(10) Uani 1 1 d . . . . .
H20A H 0.378743 0.737863 0.347919 0.034 Uiso 1 1 calc R . . . .
H20B H 0.443841 0.824848 0.446706 0.034 Uiso 1 1 calc R . . . .
C21 C 0.4444(5) 0.6969(3) 0.4471(3) 0.0231(9) Uani 1 1 d . . . . .
C22 C 0.5555(4) 0.6888(3) 0.5016(3) 0.0209(8) Uani 1 1 d . . . . .
C23 C 0.5347(4) 0.6436(3) 0.5570(3) 0.0229(9) Uani 1 1 d . . . . .
C24 C 0.4125(5) 0.6021(3) 0.5514(3) 0.0266(10) Uani 1 1 d . . . . .
H24 H 0.400674 0.569665 0.586760 0.032 Uiso 1 1 calc R . . . .
C25 C 0.3077(5) 0.6077(3) 0.4945(3) 0.0248(9) Uani 1 1 d . . . . .
C26 C 0.3215(5) 0.6564(3) 0.4434(3) 0.0261(10) Uani 1 1 d . . . . .
H26 H 0.247596 0.661775 0.406519 0.031 Uiso 1 1 calc R . . . .
C27 C 0.6394(5) 0.6395(3) 0.6224(3) 0.0247(9) Uani 1 1 d . . . . .
H27 H 0.624437 0.596776 0.646414 0.030 Uiso 1 1 calc R . . . .
C28 C 0.9634(5) 0.7005(3) 0.7199(3) 0.0222(9) Uani 1 1 d . . . . .
C29 C 1.1410(5) 0.7643(3) 0.7065(3) 0.0241(9) Uani 1 1 d . . . . .
C30 C 1.1750(5) 0.7246(3) 0.7655(3) 0.0252(9) Uani 1 1 d . . . . .
C31 C 1.3021(5) 0.7321(4) 0.8078(4) 0.0298(10) Uani 1 1 d . . . . .
H31 H 1.322735 0.705837 0.848802 0.036 Uiso 1 1 calc R . . . .
C32 C 1.3976(5) 0.7798(4) 0.7874(4) 0.0335(11) Uani 1 1 d . . . . .
H32 H 1.486045 0.786205 0.814567 0.040 Uiso 1 1 calc R . . . .
C33 C 1.3656(5) 0.8181(4) 0.7280(4) 0.0343(11) Uani 1 1 d . . . . .
H33 H 1.433226 0.850341 0.715294 0.041 Uiso 1 1 calc R . . . .
C34 C 1.2374(5) 0.8112(4) 0.6860(4) 0.0310(10) Uani 1 1 d . . . . .
H34 H 1.217092 0.837641 0.645121 0.037 Uiso 1 1 calc R . . . .
O14 O 1.5291(8) 0.6704(7) 0.9269(5) 0.130(4) Uani 1 1 d D . . . .
H14A H 1.579407 0.689963 0.978990 0.195 Uiso 1 1 d DG . . . .
H14B H 1.557434 0.621879 0.884111 0.195 Uiso 1 1 d DG . . . .
O13 O 1.3218(9) 0.5763(6) 0.9440(5) 0.105(3) Uani 1 1 d D . . . .
H13 H 1.383786 0.614869 0.950189 0.158 Uiso 1 1 calc DGR . . . .
C38 C 1.3335(14) 0.5612(10) 1.0253(7) 0.114(5) Uani 1 1 d . . . . .
H38A H 1.251579 0.528785 1.025794 0.171 Uiso 1 1 calc GR . . . .
H38B H 1.351361 0.622242 1.083215 0.171 Uiso 1 1 calc GR . . . .
H38C H 1.405468 0.522129 1.022299 0.171 Uiso 1 1 calc GR . . . .
O6 O 1.1530(4) 1.2066(3) 0.8054(3) 0.0431(9) Uani 1 1 d . . . . .
O7 O 1.2131(5) 1.2179(4) 0.9437(3) 0.0557(13) Uani 1 1 d . . . . .
O8 O 1.3350(5) 1.2891(4) 0.8896(4) 0.0555(13) Uani 1 1 d . . . . .
N12 N 1.2343(5) 1.2384(4) 0.8789(4) 0.0409(11) Uani 1 1 d . . . . .
O9 O 0.8234(4) 0.5230(3) 0.7529(3) 0.0422(9) Uani 1 1 d . . . . .
O10 O 0.6157(4) 0.5388(3) 0.7592(3) 0.0438(10) Uani 1 1 d . . . . .
O11 O 0.7073(5) 0.4374(3) 0.7925(4) 0.0502(11) Uani 1 1 d . . . . .
N13 N 0.7158(5) 0.4996(3) 0.7694(3) 0.0340(10) Uani 1 1 d . . . . .
O12 O 1.0866(6) 0.6194(5) 0.9039(4) 0.0667(15) Uani 1 1 d . . . . .
H12A H 1.163799 0.619784 0.926713 0.100 Uiso 1 1 calc DGR . . . .
C37 C 1.0015(12) 0.6236(11) 0.9674(8) 0.103(4) Uani 1 1 d . . . . .
H37A H 0.975068 0.559436 0.955493 0.154 Uiso 1 1 calc GR . . . .
H37B H 0.923768 0.653468 0.958771 0.154 Uiso 1 1 calc GR . . . .
H37C H 1.045887 0.660893 1.032524 0.154 Uiso 1 1 calc GR . . . .
N14 N 1.3334(7) 1.0460(5) 0.7605(6) 0.0652(18) Uani 1 1 d . . . . .
C35 C 1.4204(7) 1.0615(5) 0.8161(6) 0.0552(18) Uani 1 1 d . . . . .
C36 C 1.5319(9) 1.0808(9) 0.8862(7) 0.078(3) Uani 1 1 d . . . . .
H36A H 1.611155 1.093829 0.864037 0.117 Uiso 1 1 calc GR . . . .
H36B H 1.540955 1.025844 0.896499 0.117 Uiso 1 1 calc GR . . . .
H36C H 1.519577 1.135993 0.945909 0.117 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Yb1 O1 2.141(3) . ?
Yb1 O2 2.244(3) . ?
Yb1 O3 2.385(3) . ?
Yb1 O4 2.463(4) . ?
Yb1 N1 2.345(4) . ?
Yb1 N4 2.518(4) . ?
Yb1 N7 2.467(4) . ?
Yb1 N9 2.391(4) . ?
Br1 C13 1.896(5) . ?
Br2 C25 1.904(5) . ?
O1 C10 1.313(6) . ?
O2 C22 1.321(6) . ?
O3 N11 1.286(6) . ?
O4 N11 1.276(6) . ?
O5 N11 1.219(6) . ?
N1 C1 1.392(6) . ?
N1 C7 1.337(6) . ?
N2 C2 1.396(7) . ?
N2 C7 1.363(6) . ?
N3 N4 1.374(5) . ?
N3 C7 1.339(7) . ?
N4 C8 1.300(7) . ?
N5 C15 1.511(6) . ?
N5 C16 1.494(6) . ?
N5 C17 1.504(6) . ?
N6 C18 1.498(6) . ?
N6 C19 1.490(6) . ?
N6 C20 1.509(6) . ?
N7 N8 1.396(5) . ?
N7 C27 1.293(6) . ?
N8 C28 1.356(6) . ?
N9 C28 1.336(6) . ?
N9 C29 1.406(6) . ?
N10 C28 1.351(6) . ?
N10 C30 1.390(7) . ?
C1 C2 1.415(7) . ?
C1 C6 1.381(8) . ?
C2 C3 1.376(7) . ?
C3 C4 1.397(9) . ?
C4 C5 1.399(8) . ?
C5 C6 1.390(8) . ?
C8 C9 1.449(7) . ?
C9 C10 1.413(7) . ?
C9 C14 1.410(7) . ?
C10 C11 1.416(6) . ?
C11 C12 1.389(7) . ?
C11 C15 1.500(7) . ?
C12 C13 1.393(7) . ?
C13 C14 1.380(7) . ?
C17 C18 1.519(7) . ?
C20 C21 1.515(6) . ?
C21 C22 1.418(6) . ?
C21 C26 1.389(7) . ?
C22 C23 1.421(6) . ?
C23 C24 1.380(7) . ?
C23 C27 1.455(7) . ?
C24 C25 1.379(7) . ?
C25 C26 1.391(7) . ?
C29 C30 1.399(7) . ?
C29 C34 1.386(7) . ?
C30 C31 1.387(7) . ?
C31 C32 1.386(8) . ?
C32 C33 1.385(8) . ?
C33 C34 1.397(8) . ?
O13 C38 1.437(13) . ?
O6 N12 1.250(7) . ?
O7 N12 1.271(7) . ?
O8 N12 1.244(7) . ?
O9 N13 1.254(6) . ?
O10 N13 1.264(6) . ?
O11 N13 1.225(6) . ?
O12 C37 1.397(12) . ?
N14 C35 1.131(11) . ?
C35 C36 1.440(12) . ?

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 Yb1 O2 75.82(12) . . ?
O1 Yb1 O3 90.20(13) . . ?
O1 Yb1 O4 136.07(13) . . ?
O1 Yb1 N1 137.71(13) . . ?
O1 Yb1 N4 72.67(12) . . ?
O1 Yb1 N7 113.43(12) . . ?
O1 Yb1 N9 88.61(13) . . ?
O1 Yb1 N11 113.09(14) . . ?
O1 Yb1 C7 117.45(13) . . ?
O2 Yb1 O3 75.43(12) . . ?
O2 Yb1 O4 72.51(12) . . ?
O2 Yb1 N1 143.64(13) . . ?
O2 Yb1 N4 133.54(12) . . ?
O2 Yb1 N7 71.77(12) . . ?
O2 Yb1 N9 124.65(12) . . ?
O2 Yb1 N11 70.44(12) . . ?
O2 Yb1 C7 152.28(12) . . ?
O3 Yb1 O4 52.92(13) . . ?
O3 Yb1 N4 71.47(13) . . ?
O3 Yb1 N7 132.42(13) . . ?
O3 Yb1 N9 158.71(13) . . ?
O3 Yb1 N11 26.53(14) . . ?
O3 Yb1 C7 80.09(13) . . ?
O4 Yb1 N4 109.64(13) . . ?
O4 Yb1 N7 84.47(13) . . ?
O4 Yb1 N11 26.48(14) . . ?
O4 Yb1 C7 82.45(12) . . ?
N1 Yb1 O3 88.61(14) . . ?
N1 Yb1 O4 71.82(13) . . ?
N1 Yb1 N4 66.95(14) . . ?
N1 Yb1 N7 97.92(13) . . ?
N1 Yb1 N9 78.13(13) . . ?
N1 Yb1 N11 80.68(14) . . ?
N1 Yb1 C7 21.51(14) . . ?
N4 Yb1 N11 91.69(13) . . ?
N4 Yb1 C7 45.52(13) . . ?
N7 Yb1 N4 153.15(13) . . ?
N7 Yb1 N11 108.17(14) . . ?
N7 Yb1 C7 118.18(12) . . ?
N9 Yb1 O4 134.65(13) . . ?
N9 Yb1 N4 87.91(13) . . ?
N9 Yb1 N7 66.72(13) . . ?
N9 Yb1 N11 157.12(13) . . ?
N9 Yb1 C7 81.62(13) . . ?
N11 Yb1 C7 81.84(12) . . ?
C10 O1 Yb1 144.3(3) . . ?
C22 O2 Yb1 133.1(3) . . ?
N11 O3 Yb1 97.5(3) . . ?
N11 O4 Yb1 94.1(3) . . ?
C1 N1 Yb1 136.5(3) . . ?
C7 N1 Yb1 118.5(3) . . ?
C7 N1 C1 104.9(4) . . ?
C7 N2 C2 106.4(4) . . ?
C7 N3 N4 116.2(4) . . ?
N3 N4 Yb1 114.3(3) . . ?
C8 N4 Yb1 129.6(3) . . ?
C8 N4 N3 115.7(4) . . ?
C16 N5 C15 110.1(4) . . ?
C16 N5 C17 112.5(4) . . ?
C17 N5 C15 110.5(4) . . ?
C18 N6 C20 110.8(4) . . ?
C19 N6 C18 112.4(4) . . ?
C19 N6 C20 111.3(4) . . ?
N8 N7 Yb1 114.8(3) . . ?
C27 N7 Yb1 131.2(3) . . ?
C27 N7 N8 114.0(4) . . ?
C28 N8 N7 114.5(4) . . ?
C28 N9 Yb1 116.3(3) . . ?
C28 N9 C29 103.2(4) . . ?
C29 N9 Yb1 138.3(3) . . ?
C28 N10 C30 106.1(4) . . ?
O3 N11 Yb1 56.0(2) . . ?
O4 N11 Yb1 59.4(2) . . ?
O4 N11 O3 115.1(4) . . ?
O5 N11 Yb1 173.4(4) . . ?
O5 N11 O3 121.5(5) . . ?
O5 N11 O4 123.4(5) . . ?
N1 C1 C2 109.5(4) . . ?
C6 C1 N1 129.9(5) . . ?
C6 C1 C2 120.5(5) . . ?
N2 C2 C1 105.7(4) . . ?
C3 C2 N2 132.4(5) . . ?
C3 C2 C1 121.9(5) . . ?
C2 C3 C4 117.4(5) . . ?
C3 C4 C5 120.7(5) . . ?
C6 C5 C4 121.8(6) . . ?
C1 C6 C5 117.6(5) . . ?
N1 C7 Yb1 40.0(2) . . ?
N1 C7 N2 113.5(4) . . ?
N1 C7 N3 123.4(4) . . ?
N2 C7 Yb1 153.4(4) . . ?
N3 C7 Yb1 83.4(3) . . ?
N3 C7 N2 123.0(4) . . ?
N4 C8 C9 125.2(4) . . ?
C10 C9 C8 123.5(4) . . ?
C14 C9 C8 117.4(4) . . ?
C14 C9 C10 119.1(4) . . ?
O1 C10 C9 122.6(4) . . ?
O1 C10 C11 118.1(4) . . ?
C9 C10 C11 119.4(4) . . ?
C10 C11 C15 118.6(4) . . ?
C12 C11 C10 120.5(4) . . ?
C12 C11 C15 120.9(4) . . ?
C11 C12 C13 119.5(4) . . ?
C12 C13 Br1 118.5(4) . . ?
C14 C13 Br1 120.2(4) . . ?
C14 C13 C12 121.3(5) . . ?
C13 C14 C9 120.2(5) . . ?
C11 C15 N5 111.5(4) . . ?
N5 C17 C18 114.0(4) . . ?
N6 C18 C17 112.6(4) . . ?
N6 C20 C21 112.3(4) . . ?
C22 C21 C20 121.3(4) . . ?
C26 C21 C20 117.5(4) . . ?
C26 C21 C22 120.9(4) . . ?
O2 C22 C21 120.3(4) . . ?
O2 C22 C23 122.1(4) . . ?
C21 C22 C23 117.5(4) . . ?
C22 C23 C27 122.1(4) . . ?
C24 C23 C22 120.9(4) . . ?
C24 C23 C27 117.0(4) . . ?
C25 C24 C23 119.8(5) . . ?
C24 C25 Br2 119.1(4) . . ?
C24 C25 C26 121.4(5) . . ?
C26 C25 Br2 119.5(4) . . ?
C21 C26 C25 119.2(4) . . ?
N7 C27 C23 124.7(4) . . ?
N9 C28 N8 123.0(4) . . ?
N9 C28 N10 114.7(4) . . ?
N10 C28 N8 122.3(4) . . ?
C30 C29 N9 110.0(4) . . ?
C34 C29 N9 130.2(5) . . ?
C34 C29 C30 119.7(5) . . ?
N10 C30 C29 105.9(4) . . ?
C31 C30 N10 131.1(5) . . ?
C31 C30 C29 123.0(5) . . ?
C32 C31 C30 116.9(5) . . ?
C33 C32 C31 120.8(5) . . ?
C32 C33 C34 122.4(5) . . ?
C29 C34 C33 117.3(5) . . ?
O6 N12 O7 119.0(5) . . ?
O8 N12 O6 121.4(5) . . ?
O8 N12 O7 119.7(5) . . ?
O9 N13 O10 119.4(5) . . ?
O11 N13 O9 120.1(5) . . ?
O11 N13 O10 120.5(5) . . ?
N14 C35 C36 179.5(11) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT971_kp271               
;
PROBLEM: Check Calcd Resid. Dens.  0.83A   From Yb1             2.65 eA-3  
RESPONSE: Typical Fourier ripple close to heavy atom.
;
####################################################################### 
# 
# 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_kp265
_database_code_depnum_ccdc_archive 'CCDC 1956885'
loop_
_audit_author_name
_audit_author_address
'Olaf Fuhr'
;Karlsruher Institut fuer Technologie (KIT)
Germany
;
_audit_update_record             
;
2020-01-21 deposited with the CCDC.	2020-01-24 downloaded from the CCDC.
;
_audit_creation_date             2018-11-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H34 Br2 N12 O8 Y, N O3, 3(C2 H3 N)'
_chemical_formula_sum            'C40 H43 Br2 N16 O11 Y'
_chemical_formula_weight         1172.63
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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'
Br Br -0.9501 1.0411 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.4640 1.6217 '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      hexagonal
_space_group_IT_number           178
_space_group_name_H-M_alt        'P 61 2 2'
_space_group_name_Hall           'P 61 2 (0 0 -1)'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'y, x, -z+1/3'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'-y, -x, -z+5/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'

_cell_length_a                   12.93430(10)
_cell_length_b                   12.93430(10)
_cell_length_c                   46.4828(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6734.55(14)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    182029
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      64.85
_cell_measurement_theta_min      3.43
_shelx_estimated_absorpt_T_max   0.534
_shelx_estimated_absorpt_T_min   0.510
_exptl_absorpt_coefficient_mu    3.114
_exptl_absorpt_correction_T_max  0.4782
_exptl_absorpt_correction_T_min  0.2399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0064
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            69788
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.484
_diffrn_reflns_theta_min         3.433
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'Eiger R 4M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_target            Ga
_diffrn_source_type              'Metaljet D2'
_diffrn_source_voltage           70
_reflns_Friedel_coverage         0.651
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5377
_reflns_number_total             5433
_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_data_collection       
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 
;
 Flack x determined using 2110 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5433
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0266
_refine_ls_restrained_S_all      1.072
_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)+(0.0456P)²+5.6618P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0760
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N9-C20
 1.16 with sigma of 0.02
 C21-C20
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C20) = Uiso(N9) = Uiso(C21)
4. Others
 Fixed Sof: N9(0.5) C20(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
5.a Ternary CH refined with riding coordinates:
 N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), C7(H7), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16),
 C17(H17)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Y1 Y 0.38202(2) 0.76403(3) 0.250000 0.01923(9) Uani 1 2 d S T P . .
Br1 Br 0.16375(3) 1.05173(3) 0.36444(2) 0.03223(10) Uani 1 1 d . . . . .
O1 O 0.3889(2) 0.93403(19) 0.26621(5) 0.0237(4) Uani 1 1 d . . . . .
O2 O 0.4156(2) 0.7250(2) 0.19904(5) 0.0288(5) Uani 1 1 d . . . . .
O3 O 0.3245(2) 0.8254(2) 0.20437(5) 0.0283(5) Uani 1 1 d . . . . .
O4 O 0.3644(2) 0.7894(3) 0.16137(5) 0.0398(6) Uani 1 1 d . . . . .
N1 N 0.5995(2) 1.1102(3) 0.28108(6) 0.0289(6) Uani 1 1 d . . . . .
H1 H 0.549662 1.036578 0.269469 0.035 Uiso 1 1 calc R . . . .
N2 N 0.1644(2) 0.7485(2) 0.25554(5) 0.0223(5) Uani 1 1 d . . . . .
N3 N 0.0740(2) 0.6596(2) 0.23956(6) 0.0256(5) Uani 1 1 d . . . . .
H3 H 0.005752 0.657272 0.236455 0.031 Uiso 1 1 calc R . . . .
N4 N 0.2035(2) 0.5846(2) 0.22986(5) 0.0239(5) Uani 1 1 d . . . . .
N5 N 0.0122(3) 0.4750(3) 0.21602(6) 0.0309(6) Uani 1 1 d . . . . .
H5 H -0.063076 0.454169 0.213330 0.037 Uiso 1 1 calc R . . . .
N6 N 0.3685(2) 0.7801(3) 0.18757(6) 0.0275(5) Uani 1 1 d . . . . .
C1 C 0.5975(3) 1.2115(3) 0.26593(8) 0.0347(7) Uani 1 1 d . . . . .
H1A H 0.520194 1.207210 0.269857 0.042 Uiso 1 1 calc R . . . .
H1B H 0.661466 1.287756 0.273921 0.042 Uiso 1 1 calc R . . . .
C2 C 0.7216(3) 1.1257(4) 0.28293(10) 0.0431(9) Uani 1 1 d . . . . .
H2A H 0.758421 1.144016 0.263802 0.065 Uiso 1 1 calc GR . . . .
H2B H 0.716148 1.051797 0.290076 0.065 Uiso 1 1 calc GR . . . .
H2C H 0.770514 1.191313 0.296130 0.065 Uiso 1 1 calc GR . . . .
C3 C 0.5428(3) 1.0896(3) 0.31039(7) 0.0289(6) Uani 1 1 d . . . . .
H3A H 0.557881 1.032258 0.321091 0.035 Uiso 1 1 calc R . . . .
H3B H 0.580788 1.165793 0.321174 0.035 Uiso 1 1 calc R . . . .
C4 C 0.4105(3) 1.0421(3) 0.30903(7) 0.0246(6) Uani 1 1 d . . . . .
C5 C 0.3386(3) 0.9595(3) 0.28772(6) 0.0222(5) Uani 1 1 d . . . . .
C6 C 0.2132(3) 0.9063(3) 0.28961(7) 0.0237(6) Uani 1 1 d . . . . .
C7 C 0.1616(3) 0.9371(3) 0.31206(7) 0.0255(6) Uani 1 1 d . . . . .
H7 H 0.077433 0.903289 0.313000 0.031 Uiso 1 1 calc R . . . .
C8 C 0.2338(3) 1.0169(3) 0.33286(7) 0.0262(6) Uani 1 1 d . . . . .
C9 C 0.3571(3) 1.0697(3) 0.33155(7) 0.0261(6) Uani 1 1 d . . . . .
H9 H 0.405272 1.124771 0.345994 0.031 Uiso 1 1 calc R . . . .
C10 C 0.1326(3) 0.8126(3) 0.27025(6) 0.0246(6) Uani 1 1 d . . . . .
H10 H 0.053214 0.797811 0.268321 0.029 Uiso 1 1 calc R . . . .
C11 C 0.0976(3) 0.5755(3) 0.22891(6) 0.0234(6) Uani 1 1 d . . . . .
C12 C 0.1871(3) 0.4805(3) 0.21637(7) 0.0270(6) Uani 1 1 d . . . . .
C13 C 0.0681(3) 0.4114(3) 0.20790(7) 0.0297(7) Uani 1 1 d . . . . .
C14 C 0.0246(4) 0.3027(4) 0.19396(10) 0.0438(9) Uani 1 1 d . . . . .
H14 H -0.056680 0.256281 0.188386 0.053 Uiso 1 1 calc R . . . .
C15 C 0.1064(5) 0.2657(4) 0.18863(10) 0.0497(11) Uani 1 1 d . . . . .
H15 H 0.080524 0.192021 0.178956 0.060 Uiso 1 1 calc R . . . .
C16 C 0.2255(4) 0.3331(4) 0.19702(9) 0.0453(10) Uani 1 1 d . . . . .
H16 H 0.278734 0.304160 0.193268 0.054 Uiso 1 1 calc R . . . .
C17 C 0.2673(4) 0.4418(4) 0.21076(8) 0.0361(8) Uani 1 1 d . . . . .
H17 H 0.348775 0.488446 0.216182 0.043 Uiso 1 1 calc R . . . .
O5 O -0.1903(4) 0.4833(5) 0.23780(16) 0.117(2) Uani 1 1 d . . . . .
O6 O -0.1763(2) 0.6473(5) 0.250000 0.086(2) Uani 1 2 d S T P . .
N7 N -0.2314(2) 0.5372(5) 0.250000 0.0515(13) Uani 1 2 d S T P . .
N8 N 0.4247(12) 0.5238(12) 0.1240(3) 0.179(5) Uiso 1 1 d . . . . .
C18 C 0.4894(10) 0.5968(10) 0.1390(2) 0.113(3) Uiso 1 1 d . . . . .
C19 C 0.5816(9) 0.7053(9) 0.1492(2) 0.117(3) Uiso 1 1 d . . . . .
H19A H 0.647759 0.738092 0.135433 0.176 Uiso 1 1 calc GR . . . .
H19B H 0.609582 0.692458 0.167777 0.176 Uiso 1 1 calc GR . . . .
H19C H 0.552338 0.761436 0.151731 0.176 Uiso 1 1 calc GR . . . .
N9 N -0.0183(12) 0.1349(12) 0.2525(3) 0.085(2) Uiso 0.5 1 d D . . A -1
C20 C 0.0294(13) 0.0948(11) 0.2495(5) 0.085(2) Uiso 0.5 1 d D . . A -1
C21 C 0.1419(13) 0.0689(15) 0.2478(3) 0.085(2) Uiso 0.5 1 d D . . A -1
H21A H 0.173490 0.083129 0.228172 0.128 Uiso 0.5 1 calc GR . . A -1
H21B H 0.114158 -0.014141 0.253212 0.128 Uiso 0.5 1 calc GR . . A -1
H21C H 0.204942 0.122479 0.261106 0.128 Uiso 0.5 1 calc GR . . 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
Y1 O1 2.284(2) 11 ?
Y1 O1 2.284(2) . ?
Y1 O2 2.504(2) 11 ?
Y1 O2 2.505(2) . ?
Y1 O3 2.504(2) 11 ?
Y1 O3 2.504(2) . ?
Y1 N2 2.732(3) . ?
Y1 N2 2.732(3) 11 ?
Y1 N4 2.497(3) 11 ?
Y1 N4 2.497(3) . ?
Br1 C8 1.895(3) . ?
O1 C5 1.322(4) . ?
O2 N6 1.263(4) . ?
O3 N6 1.269(4) . ?
O4 N6 1.227(4) . ?
N1 C1 1.499(4) . ?
N1 C2 1.492(5) . ?
N1 C3 1.507(4) . ?
N2 N3 1.377(4) . ?
N2 C10 1.291(4) . ?
N3 C11 1.361(4) . ?
N4 C11 1.316(4) . ?
N4 C12 1.401(4) . ?
N5 C11 1.354(4) . ?
N5 C13 1.391(5) . ?
C1 C1 1.496(7) 11 ?
C3 C4 1.503(5) . ?
C4 C5 1.411(4) . ?
C4 C9 1.395(4) . ?
C5 C6 1.413(4) . ?
C6 C7 1.399(4) . ?
C6 C10 1.450(4) . ?
C7 C8 1.381(4) . ?
C8 C9 1.387(5) . ?
C12 C13 1.396(5) . ?
C12 C17 1.384(5) . ?
C13 C14 1.386(5) . ?
C14 C15 1.384(7) . ?
C15 C16 1.394(7) . ?
C16 C17 1.383(5) . ?
O5 N7 1.209(5) . ?
O6 N7 1.233(7) . ?
N8 C18 1.135(14) . ?
C18 C19 1.395(14) . ?
N9 C20 0.995(15) . ?
C20 C21 1.650(17) . ?

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 Y1 O1 67.00(11) 11 . ?
O1 Y1 O2 73.27(8) 11 . ?
O1 Y1 O2 125.37(8) . . ?
O1 Y1 O2 73.28(8) . 11 ?
O1 Y1 O2 125.37(8) 11 11 ?
O1 Y1 O3 81.32(8) 11 11 ?
O1 Y1 O3 81.32(8) . . ?
O1 Y1 O3 72.13(8) 11 . ?
O1 Y1 O3 72.13(8) . 11 ?
O1 Y1 N2 121.59(8) . 11 ?
O1 Y1 N2 121.60(8) 11 . ?
O1 Y1 N2 65.33(8) . . ?
O1 Y1 N2 65.33(8) 11 11 ?
O1 Y1 N4 138.67(8) . 11 ?
O1 Y1 N4 126.27(9) . . ?
O1 Y1 N4 138.67(8) 11 . ?
O1 Y1 N4 126.27(9) 11 11 ?
O1 Y1 N6 70.30(8) . 11 ?
O1 Y1 N6 103.55(8) 11 11 ?
O1 Y1 N6 103.54(8) . . ?
O1 Y1 N6 70.30(8) 11 . ?
O2 Y1 O2 159.90(11) 11 . ?
O2 Y1 N2 68.13(7) 11 . ?
O2 Y1 N2 110.49(7) . . ?
O2 Y1 N2 68.14(7) . 11 ?
O2 Y1 N2 110.49(7) 11 11 ?
O2 Y1 N6 157.56(7) . 11 ?
O2 Y1 N6 25.48(8) 11 11 ?
O2 Y1 N6 25.48(8) . . ?
O2 Y1 N6 157.56(7) 11 . ?
O3 Y1 O2 51.07(7) . . ?
O3 Y1 O2 136.40(7) 11 . ?
O3 Y1 O2 51.08(7) 11 11 ?
O3 Y1 O2 136.40(7) . 11 ?
O3 Y1 O3 148.13(12) 11 . ?
O3 Y1 N2 112.97(7) . 11 ?
O3 Y1 N2 69.20(7) 11 11 ?
O3 Y1 N2 69.20(7) . . ?
O3 Y1 N2 112.97(7) 11 . ?
O3 Y1 N6 150.22(8) . 11 ?
O3 Y1 N6 150.22(8) 11 . ?
O3 Y1 N6 25.60(8) 11 11 ?
O3 Y1 N6 25.60(8) . . ?
N2 Y1 N2 172.67(11) 11 . ?
N2 Y1 N6 90.16(7) 11 11 ?
N2 Y1 N6 90.16(7) . . ?
N2 Y1 N6 90.29(7) 11 . ?
N2 Y1 N6 90.29(7) . 11 ?
N4 Y1 O2 95.05(8) . 11 ?
N4 Y1 O2 68.34(8) 11 11 ?
N4 Y1 O2 68.34(8) . . ?
N4 Y1 O2 95.06(8) 11 . ?
N4 Y1 O3 72.18(8) 11 11 ?
N4 Y1 O3 72.18(8) . . ?
N4 Y1 O3 138.41(8) . 11 ?
N4 Y1 O3 138.41(8) 11 . ?
N4 Y1 N2 111.72(8) . 11 ?
N4 Y1 N2 61.78(8) . . ?
N4 Y1 N2 111.72(8) 11 . ?
N4 Y1 N2 61.78(8) 11 11 ?
N4 Y1 N4 72.78(12) . 11 ?
N4 Y1 N6 117.78(8) 11 . ?
N4 Y1 N6 68.49(8) . . ?
N4 Y1 N6 117.78(8) . 11 ?
N4 Y1 N6 68.49(8) 11 11 ?
N6 Y1 N6 172.93(12) . 11 ?
C5 O1 Y1 134.67(19) . . ?
N6 O2 Y1 96.00(17) . . ?
N6 O3 Y1 95.86(17) . . ?
C1 N1 C3 111.1(3) . . ?
C2 N1 C1 113.0(3) . . ?
C2 N1 C3 111.1(3) . . ?
N3 N2 Y1 115.12(18) . . ?
C10 N2 Y1 130.6(2) . . ?
C10 N2 N3 114.3(3) . . ?
C11 N3 N2 115.3(3) . . ?
C11 N4 Y1 122.2(2) . . ?
C11 N4 C12 104.4(3) . . ?
C12 N4 Y1 133.3(2) . . ?
C11 N5 C13 105.8(3) . . ?
O2 N6 Y1 58.52(15) . . ?
O2 N6 O3 117.0(3) . . ?
O3 N6 Y1 58.53(14) . . ?
O4 N6 Y1 178.7(3) . . ?
O4 N6 O2 122.0(3) . . ?
O4 N6 O3 120.9(3) . . ?
C1 C1 N1 113.6(3) 11 . ?
C4 C3 N1 112.9(3) . . ?
C5 C4 C3 121.6(3) . . ?
C9 C4 C3 118.1(3) . . ?
C9 C4 C5 119.8(3) . . ?
O1 C5 C4 120.0(3) . . ?
O1 C5 C6 120.9(3) . . ?
C4 C5 C6 119.1(3) . . ?
C5 C6 C10 122.6(3) . . ?
C7 C6 C5 120.1(3) . . ?
C7 C6 C10 117.1(3) . . ?
C8 C7 C6 119.6(3) . . ?
C7 C8 Br1 119.6(2) . . ?
C7 C8 C9 121.3(3) . . ?
C9 C8 Br1 119.1(2) . . ?
C8 C9 C4 120.0(3) . . ?
N2 C10 C6 122.6(3) . . ?
N4 C11 N3 123.8(3) . . ?
N4 C11 N5 114.4(3) . . ?
N5 C11 N3 121.8(3) . . ?
C13 C12 N4 109.3(3) . . ?
C17 C12 N4 130.6(3) . . ?
C17 C12 C13 120.1(3) . . ?
N5 C13 C12 106.1(3) . . ?
C14 C13 N5 131.2(4) . . ?
C14 C13 C12 122.7(4) . . ?
C15 C14 C13 116.2(4) . . ?
C14 C15 C16 122.0(4) . . ?
C17 C16 C15 120.9(4) . . ?
C16 C17 C12 118.2(4) . . ?
O5 N7 O5 120.1(6) . 11_455 ?
O5 N7 O6 120.0(3) 11_455 . ?
O5 N7 O6 120.0(3) . . ?
N8 C18 C19 162.1(13) . . ?
N9 C20 C21 162.2(19) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_kp263
_database_code_depnum_ccdc_archive 'CCDC 1956883'
loop_
_audit_author_name
_audit_author_address
'Olaf Fuhr'
;Karlsruher Institut fuer Technologie (KIT)
Germany
;
_audit_update_record             
;
2020-01-21 deposited with the CCDC.	2020-01-24 downloaded from the CCDC.
;
_audit_creation_date             2018-10-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H34 Br2 N12 O8 Sm, N O3, 3(C2 H3 N)'
_chemical_formula_sum            'C40 H43 Br2 N16 O11 Sm'
_chemical_formula_weight         1234.07
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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'
Br Br -0.9501 1.0411 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -2.2059 10.7078 '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      hexagonal
_space_group_IT_number           178
_space_group_name_H-M_alt        'P 61 2 2'
_space_group_name_Hall           'P 61 2 (0 0 -1)'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/6'
'-y, x-y, z+1/3'
'-x, -y, z+1/2'
'-x+y, -x, z+2/3'
'y, -x+y, z+5/6'
'x-y, -y, -z'
'-x, -x+y, -z+2/3'
'y, x, -z+1/3'
'-y, -x, -z+5/6'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/6'

_cell_length_a                   13.00110(10)
_cell_length_b                   13.00110(10)
_cell_length_c                   46.6691(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     6831.56(12)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    193153
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      66.90
_cell_measurement_theta_min      2.47
_shelx_estimated_absorpt_T_max   0.361
_shelx_estimated_absorpt_T_min   0.280
_exptl_absorpt_coefficient_mu    8.544
_exptl_absorpt_correction_T_max  0.1993
_exptl_absorpt_correction_T_min  0.0383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.800
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3690
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0097
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            90987
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         66.413
_diffrn_reflns_theta_min         3.415
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'Eiger R 4M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_target            Ga
_diffrn_source_type              'Metaljet D2'
_diffrn_source_voltage           70
_reflns_Friedel_coverage         0.664
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                5918
_reflns_number_total             6066
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'

_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.023(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6066
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0235
_refine_ls_restrained_S_all      1.068
_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)+(0.0451P)²+2.7612P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0655
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.977(3)
 0.023(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed Sof: N9(0.5) C20(0.5) C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
4.a Ternary CH refined with riding coordinates:
 N1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B)
4.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N5(H5), C7(H7), C9(H9), C10(H10), C14(H14), C15(H15), C16(H16),
 C17(H17)
4.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.76030(2) 0.38015(2) 0.083333 0.02467(6) Uani 1 2 d S T P . .
Br1 Br 1.04720(4) 0.16242(4) -0.03153(2) 0.03857(10) Uani 1 1 d . . . . .
O1 O 0.9336(2) 0.3876(2) 0.06705(5) 0.0296(4) Uani 1 1 d . . . . .
O2 O 0.7225(2) 0.3091(2) 0.03079(5) 0.0348(5) Uani 1 1 d . . . . .
O3 O 0.8241(2) 0.5001(2) 0.03614(5) 0.0351(5) Uani 1 1 d . . . . .
O4 O 0.7871(3) 0.4238(3) -0.00674(6) 0.0477(6) Uani 1 1 d . . . . .
N1 N 1.1085(3) 0.5972(3) 0.05204(7) 0.0354(6) Uani 1 1 d . . . . .
H1 H 1.035079 0.547290 0.063519 0.043 Uiso 1 1 calc R . . . .
N2 N 0.7453(2) 0.1622(2) 0.07764(6) 0.0274(5) Uani 1 1 d . . . . .
N3 N 0.6569(3) 0.0717(2) 0.09357(6) 0.0307(5) Uani 1 1 d . . . . .
H3 H 0.655289 0.004086 0.096581 0.037 Uiso 1 1 calc R . . . .
N4 N 0.5797(2) 0.1985(2) 0.10364(6) 0.0296(5) Uani 1 1 d . . . . .
N5 N 0.4730(3) 0.0080(3) 0.11721(7) 0.0370(6) Uani 1 1 d . . . . .
H5 H 0.453186 -0.066736 0.119819 0.044 Uiso 1 1 calc R . . . .
N6 N 0.7779(3) 0.4107(3) 0.01948(6) 0.0337(6) Uani 1 1 d . . . . .
C1 C 1.2088(3) 0.5959(4) 0.06743(9) 0.0422(8) Uani 1 1 d . . . . .
H1A H 1.284755 0.659517 0.059473 0.051 Uiso 1 1 calc R . . . .
H1B H 1.204967 0.519080 0.063664 0.051 Uiso 1 1 calc R . . . .
C2 C 1.1226(4) 0.7180(4) 0.05005(11) 0.0498(10) Uani 1 1 d . . . . .
H2A H 1.191864 0.768898 0.038176 0.075 Uiso 1 1 calc GR . . . .
H2B H 1.133773 0.752245 0.069282 0.075 Uiso 1 1 calc GR . . . .
H2C H 1.051235 0.712301 0.041367 0.075 Uiso 1 1 calc GR . . . .
C3 C 1.0886(3) 0.5403(3) 0.02297(8) 0.0354(7) Uani 1 1 d . . . . .
H3A H 1.164890 0.577590 0.012423 0.042 Uiso 1 1 calc R . . . .
H3B H 1.032619 0.556215 0.012098 0.042 Uiso 1 1 calc R . . . .
C4 C 1.0397(3) 0.4076(3) 0.02417(7) 0.0303(6) Uani 1 1 d . . . . .
C5 C 0.9580(3) 0.3369(3) 0.04555(7) 0.0281(6) Uani 1 1 d . . . . .
C6 C 0.9037(3) 0.2123(3) 0.04342(7) 0.0289(6) Uani 1 1 d . . . . .
C7 C 0.9334(3) 0.1606(3) 0.02092(7) 0.0312(6) Uani 1 1 d . . . . .
H7 H 0.899047 0.076748 0.019882 0.037 Uiso 1 1 calc R . . . .
C8 C 1.0132(3) 0.2326(3) 0.00022(7) 0.0321(6) Uani 1 1 d . . . . .
C9 C 1.0662(3) 0.3545(3) 0.00159(7) 0.0315(6) Uani 1 1 d . . . . .
H9 H 1.120802 0.402327 -0.012844 0.038 Uiso 1 1 calc R . . . .
C10 C 0.8101(3) 0.1319(3) 0.06285(7) 0.0298(6) Uani 1 1 d . . . . .
H10 H 0.795849 0.053083 0.064742 0.036 Uiso 1 1 calc R . . . .
C11 C 0.5724(3) 0.0933(3) 0.10428(7) 0.0287(6) Uani 1 1 d . . . . .
C12 C 0.4766(3) 0.1807(3) 0.11715(7) 0.0322(6) Uani 1 1 d . . . . .
C13 C 0.4085(3) 0.0619(3) 0.12556(8) 0.0357(7) Uani 1 1 d . . . . .
C14 C 0.3002(4) 0.0176(4) 0.13957(10) 0.0507(10) Uani 1 1 d . . . . .
H14 H 0.254661 -0.063450 0.145053 0.061 Uiso 1 1 calc R . . . .
C15 C 0.2624(4) 0.0979(5) 0.14510(11) 0.0556(11) Uani 1 1 d . . . . .
H15 H 0.189602 0.071538 0.155006 0.067 Uiso 1 1 calc R . . . .
C16 C 0.3275(4) 0.2159(4) 0.13663(10) 0.0501(10) Uani 1 1 d . . . . .
H16 H 0.296890 0.267557 0.140171 0.060 Uiso 1 1 calc R . . . .
C17 C 0.4366(4) 0.2597(4) 0.12304(8) 0.0413(8) Uani 1 1 d . . . . .
H17 H 0.482456 0.341146 0.117929 0.050 Uiso 1 1 calc R . . . .
O5 O 0.4799(5) -0.1920(4) 0.09536(15) 0.111(2) Uani 1 1 d . . . . .
O6 O 0.6443(5) -0.1779(2) 0.083333 0.097(2) Uani 1 2 d S T P . .
N7 N 0.5350(5) -0.2325(2) 0.083333 0.0540(13) Uani 1 2 d S T P . .
N8 N 0.5190(10) 0.0990(10) -0.0414(3) 0.172(5) Uani 1 1 d . . . . .
C18 C 0.5908(10) 0.1038(9) -0.0288(3) 0.120(4) Uani 1 1 d . . . . .
C19 C 0.6984(9) 0.1217(8) -0.0187(2) 0.112(3) Uani 1 1 d . . . . .
H19A H 0.725863 0.078721 -0.030857 0.168 Uiso 1 1 calc GR . . . .
H19B H 0.688827 0.092341 0.001015 0.168 Uiso 1 1 calc GR . . . .
H19C H 0.756993 0.206737 -0.019105 0.168 Uiso 1 1 calc GR . . . .
N9 N 1.0670(15) 0.1462(15) 0.0854(4) 0.110(4) Uiso 0.5 1 d . . . A -1
C20 C 1.0972(9) 0.0748(9) 0.0833(3) 0.065(3) Uiso 0.5 1 d . . . A -1
C21 C 1.1348(14) -0.0112(15) 0.0810(3) 0.086(4) Uiso 0.5 1 d . . . A -1
H21A H 1.103502 -0.056650 0.063250 0.128 Uiso 0.5 1 calc GR . . A -1
H21B H 1.104931 -0.065253 0.097441 0.128 Uiso 0.5 1 calc GR . . A -1
H21C H 1.221785 0.029378 0.080727 0.128 Uiso 0.5 1 calc GR . . 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 O1 2.334(2) . ?
Sm1 O1 2.334(2) 12 ?
Sm1 O2 2.580(2) 12 ?
Sm1 O2 2.580(2) . ?
Sm1 O3 2.584(2) . ?
Sm1 O3 2.584(2) 12 ?
Sm1 N2 2.754(3) . ?
Sm1 N2 2.754(3) 12 ?
Sm1 N4 2.538(3) 12 ?
Sm1 N4 2.538(3) . ?
Br1 C8 1.904(3) . ?
O1 C5 1.323(4) . ?
O2 N6 1.262(4) . ?
O3 N6 1.271(4) . ?
O4 N6 1.233(4) . ?
N1 C1 1.496(5) . ?
N1 C2 1.491(5) . ?
N1 C3 1.504(5) . ?
N2 N3 1.381(4) . ?
N2 C10 1.293(4) . ?
N3 C11 1.358(4) . ?
N4 C11 1.322(4) . ?
N4 C12 1.392(4) . ?
N5 C11 1.353(4) . ?
N5 C13 1.392(5) . ?
C1 C1 1.501(8) 12 ?
C3 C4 1.513(5) . ?
C4 C5 1.411(4) . ?
C4 C9 1.394(5) . ?
C5 C6 1.410(4) . ?
C6 C7 1.402(4) . ?
C6 C10 1.457(4) . ?
C7 C8 1.384(5) . ?
C8 C9 1.378(5) . ?
C12 C13 1.398(5) . ?
C12 C17 1.392(5) . ?
C13 C14 1.389(5) . ?
C14 C15 1.383(7) . ?
C15 C16 1.388(7) . ?
C16 C17 1.389(6) . ?
O5 N7 1.217(5) . ?
O6 N7 1.231(7) . ?
N8 C18 1.077(12) . ?
C18 C19 1.382(13) . ?
N9 C20 1.179(19) . ?
C20 C21 1.43(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sm1 O1 66.52(11) . 12 ?
O1 Sm1 O2 73.29(8) 12 12 ?
O1 Sm1 O2 124.31(8) . 12 ?
O1 Sm1 O2 124.31(8) 12 . ?
O1 Sm1 O2 73.29(8) . . ?
O1 Sm1 O3 81.37(8) 12 . ?
O1 Sm1 O3 71.67(8) . . ?
O1 Sm1 O3 71.67(8) 12 12 ?
O1 Sm1 O3 81.37(8) . 12 ?
O1 Sm1 N2 65.25(8) 12 12 ?
O1 Sm1 N2 65.26(8) . . ?
O1 Sm1 N2 121.40(8) 12 . ?
O1 Sm1 N2 121.40(8) . 12 ?
O1 Sm1 N4 125.78(9) 12 12 ?
O1 Sm1 N4 138.99(8) . 12 ?
O1 Sm1 N4 138.99(8) 12 . ?
O1 Sm1 N4 125.79(9) . . ?
O1 Sm1 N6 70.29(8) . . ?
O1 Sm1 N6 103.10(8) 12 . ?
O2 Sm1 O2 160.99(11) . 12 ?
O2 Sm1 O3 137.71(8) . 12 ?
O2 Sm1 O3 49.61(8) . . ?
O2 Sm1 O3 137.71(8) 12 . ?
O2 Sm1 O3 49.61(8) 12 12 ?
O2 Sm1 N2 110.04(8) 12 . ?
O2 Sm1 N2 68.72(8) . . ?
O2 Sm1 N2 110.05(8) . 12 ?
O2 Sm1 N2 68.72(8) 12 12 ?
O2 Sm1 N6 24.70(8) . . ?
O2 Sm1 N6 158.49(8) 12 . ?
O3 Sm1 O3 147.74(12) . 12 ?
O3 Sm1 N2 112.01(8) . . ?
O3 Sm1 N2 112.01(8) 12 12 ?
O3 Sm1 N2 70.07(8) 12 . ?
O3 Sm1 N2 70.07(8) . 12 ?
O3 Sm1 N6 24.92(8) . . ?
O3 Sm1 N6 150.48(8) 12 . ?
N2 Sm1 N2 172.98(11) 12 . ?
N2 Sm1 N6 90.35(8) 12 . ?
N2 Sm1 N6 90.12(8) . . ?
N4 Sm1 O2 68.65(8) 12 . ?
N4 Sm1 O2 95.72(8) . . ?
N4 Sm1 O2 68.65(8) . 12 ?
N4 Sm1 O2 95.72(8) 12 12 ?
N4 Sm1 O3 72.35(9) 12 . ?
N4 Sm1 O3 72.36(9) . 12 ?
N4 Sm1 O3 138.43(8) 12 12 ?
N4 Sm1 O3 138.43(8) . . ?
N4 Sm1 N2 112.33(8) . 12 ?
N4 Sm1 N2 61.44(8) . . ?
N4 Sm1 N2 61.44(8) 12 12 ?
N4 Sm1 N2 112.33(8) 12 . ?
N4 Sm1 N4 73.57(12) 12 . ?
N4 Sm1 N6 117.91(9) . . ?
N4 Sm1 N6 68.77(8) 12 . ?
C5 O1 Sm1 133.88(19) . . ?
N6 O2 Sm1 96.63(18) . . ?
N6 O3 Sm1 96.17(18) . . ?
C1 N1 C3 111.4(3) . . ?
C2 N1 C1 113.2(3) . . ?
C2 N1 C3 111.2(3) . . ?
N3 N2 Sm1 115.18(18) . . ?
C10 N2 Sm1 130.0(2) . . ?
C10 N2 N3 114.8(3) . . ?
C11 N3 N2 115.9(3) . . ?
C11 N4 Sm1 121.7(2) . . ?
C11 N4 C12 104.6(3) . . ?
C12 N4 Sm1 133.6(2) . . ?
C11 N5 C13 106.3(3) . . ?
O2 N6 Sm1 58.67(16) . . ?
O2 N6 O3 117.6(3) . . ?
O3 N6 Sm1 58.91(15) . . ?
O4 N6 Sm1 179.0(2) . . ?
O4 N6 O2 121.6(3) . . ?
O4 N6 O3 120.8(3) . . ?
N1 C1 C1 114.1(3) . 12 ?
N1 C3 C4 113.4(3) . . ?
C5 C4 C3 121.3(3) . . ?
C9 C4 C3 118.0(3) . . ?
C9 C4 C5 120.3(3) . . ?
O1 C5 C4 120.1(3) . . ?
O1 C5 C6 121.3(3) . . ?
C6 C5 C4 118.7(3) . . ?
C5 C6 C10 122.6(3) . . ?
C7 C6 C5 120.3(3) . . ?
C7 C6 C10 117.0(3) . . ?
C8 C7 C6 119.5(3) . . ?
C7 C8 Br1 119.6(3) . . ?
C9 C8 Br1 119.0(3) . . ?
C9 C8 C7 121.4(3) . . ?
C8 C9 C4 119.9(3) . . ?
N2 C10 C6 123.4(3) . . ?
N4 C11 N3 123.9(3) . . ?
N4 C11 N5 113.8(3) . . ?
N5 C11 N3 122.2(3) . . ?
N4 C12 C13 109.7(3) . . ?
C17 C12 N4 130.6(3) . . ?
C17 C12 C13 119.7(3) . . ?
N5 C13 C12 105.6(3) . . ?
C14 C13 N5 131.6(4) . . ?
C14 C13 C12 122.8(4) . . ?
C15 C14 C13 116.3(4) . . ?
C14 C15 C16 122.1(4) . . ?
C15 C16 C17 121.0(4) . . ?
C16 C17 C12 118.0(4) . . ?
O5 N7 O5 118.8(7) 12_545 . ?
O5 N7 O6 120.6(3) . . ?
O5 N7 O6 120.6(3) 12_545 . ?
N8 C18 C19 166.1(16) . . ?
N9 C20 C21 179.3(19) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.977(3)
2 0.023(3)

####################################################################### 
# 
# 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_kp269
_database_code_depnum_ccdc_archive 'CCDC 1956884'
loop_
_audit_author_name
_audit_author_address
'Olaf Fuhr'
;Karlsruher Institut fuer Technologie (KIT)
Germany
;
_audit_update_record             
;
2020-01-21 deposited with the CCDC.	2020-01-24 downloaded from the CCDC.
;
_audit_creation_date             2020-01-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C34 H36 Br2 Er N11 O6, 2(N O3)'
_chemical_formula_sum            'C34 H36 Br2 Er N13 O12'
_chemical_formula_weight         1145.84
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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'
Br Br -0.9338 1.0006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -10.7818 8.7525 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.4509(3)
_cell_length_b                   18.1610(4)
_cell_length_c                   21.2663(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.752(2)
_cell_angle_gamma                90
_cell_volume                     4798.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8534
_cell_measurement_temperature    180
_cell_measurement_theta_max      64.26
_cell_measurement_theta_min      20.55
_shelx_estimated_absorpt_T_max   0.808
_shelx_estimated_absorpt_T_min   0.319
_exptl_absorpt_coefficient_mu    7.403
_exptl_absorpt_correction_T_max  0.4326
_exptl_absorpt_correction_T_min  0.0267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2260
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29620
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.496
_diffrn_reflns_theta_min         2.786
_diffrn_ambient_temperature      180
_diffrn_detector                 'Eiger R 4M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_target            Ga
_diffrn_source_type              'Metaljet D2'
_diffrn_source_voltage           70
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9099
_reflns_number_total             11293
_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_data_collection       
;
X-Area Pilatus3_SV 1.31.153.0 (STOE, 2018)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;

_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.815
_refine_diff_density_min         -1.063
_refine_diff_density_rms         0.128
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         11293
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0534
_refine_ls_restrained_S_all      1.070
_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)+(0.1090P)²+3.3376P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1651
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O13-O15
 2.11 with sigma of 0.02
 O15-N14 = O14-N14 = O13-N14
 1.22 with sigma of 0.02
3. Restrained planarity
 N14, O13, O14, O15
 with sigma of 0.1
4. Others
 Fixed Sof: O10(0.5) O12(0.5) N13(0.5) N14(0.5) O14(0.5) O15(0.5) O13(0.5)
5.a Rotating group:
 O6(H6A,H6B)
5.b Ternary CH refined with riding coordinates:
 N5(H5), N6(H6)
5.c Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B)
5.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N8(H8), N10(H10), C3(H3A), C4(H4), C5(H5A), C6(H6C), C8(H8A),
 C12(H12), C14(H14), C24(H24), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33),
  C34(H34)
5.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.28061(2) 0.33280(2) 0.28195(2) 0.03052(9) Uani 1 1 d . . . . .
Br1 Br 0.46813(6) 0.63205(4) 0.04024(3) 0.0636(2) Uani 1 1 d . . . . .
Br2 Br -0.20478(5) 0.44390(4) 0.48141(3) 0.05407(17) Uani 1 1 d . . . . .
O1 O 0.3275(3) 0.44190(16) 0.25039(15) 0.0356(7) Uani 1 1 d . . . . .
O2 O 0.1430(2) 0.40867(17) 0.30102(15) 0.0346(6) Uani 1 1 d . . . . .
O3 O 0.1600(3) 0.25434(19) 0.3315(2) 0.0506(9) Uani 1 1 d . . . . .
O4 O 0.0167(4) 0.2428(3) 0.2687(3) 0.0758(14) Uani 1 1 d . . . . .
O5 O 0.0303(4) 0.1858(3) 0.3593(3) 0.0729(13) Uani 1 1 d . . . . .
O6 O 0.1523(3) 0.3162(2) 0.19582(19) 0.0528(9) Uani 1 1 d . . . . .
H6A H 0.135006 0.359817 0.174011 0.079 Uiso 1 1 d GR . . . .
H6B H 0.084636 0.302125 0.208137 0.079 Uiso 1 1 d GR . . . .
N1 N 0.3348(3) 0.2070(2) 0.2556(2) 0.0379(8) Uani 1 1 d . . . . .
N2 N 0.3944(4) 0.1252(2) 0.1866(2) 0.0447(10) Uani 1 1 d . . . . .
H2 H 0.421400 0.108271 0.152279 0.054 Uiso 1 1 calc R . . . .
N3 N 0.3924(4) 0.2503(2) 0.1589(2) 0.0482(11) Uani 1 1 d . . . . .
H3 H 0.413661 0.240708 0.121124 0.058 Uiso 1 1 calc R . . . .
N4 N 0.3756(3) 0.3217(2) 0.1792(2) 0.0384(9) Uani 1 1 d . . . . .
N5 N 0.2242(3) 0.5654(2) 0.28861(19) 0.0368(8) Uani 1 1 d . . . . .
H5 H 0.221748 0.510661 0.283354 0.044 Uiso 1 1 calc R . . . .
N6 N 0.0220(3) 0.4857(2) 0.2218(2) 0.0411(9) Uani 1 1 d . . . . .
H6 H 0.092113 0.460837 0.233748 0.049 Uiso 1 1 calc R . . . .
N7 N 0.2756(3) 0.3610(2) 0.40091(18) 0.0352(8) Uani 1 1 d . . . . .
N8 N 0.3687(3) 0.3442(2) 0.4366(2) 0.0405(9) Uani 1 1 d . . . . .
H8 H 0.371526 0.342370 0.477979 0.049 Uiso 1 1 calc R . . . .
N9 N 0.4523(3) 0.32768(18) 0.3414(2) 0.0344(8) Uani 1 1 d . . . . .
N10 N 0.5538(3) 0.3192(2) 0.4324(2) 0.0413(9) Uani 1 1 d . . . . .
H10 H 0.571237 0.320284 0.473161 0.050 Uiso 1 1 calc R . . . .
N11 N 0.0674(4) 0.2276(3) 0.3191(3) 0.0520(11) Uani 1 1 d . . . . .
C1 C 0.3274(4) 0.1353(2) 0.2810(2) 0.0377(10) Uani 1 1 d . . . . .
C2 C 0.3639(4) 0.0843(2) 0.2374(3) 0.0396(10) Uani 1 1 d . . . . .
C3 C 0.3697(4) 0.0096(3) 0.2497(3) 0.0502(14) Uani 1 1 d . . . . .
H3A H 0.395620 -0.024127 0.220084 0.060 Uiso 1 1 calc R . . . .
C4 C 0.3361(4) -0.0138(3) 0.3071(3) 0.0542(15) Uani 1 1 d . . . . .
H4 H 0.337236 -0.064859 0.316911 0.065 Uiso 1 1 calc R . . . .
C5 C 0.3004(5) 0.0367(3) 0.3508(3) 0.0554(14) Uani 1 1 d . . . . .
H5A H 0.279658 0.019155 0.390292 0.066 Uiso 1 1 calc R . . . .
C6 C 0.2943(4) 0.1120(3) 0.3381(3) 0.0481(12) Uani 1 1 d . . . . .
H6C H 0.268437 0.145748 0.367717 0.058 Uiso 1 1 calc R . . . .
C7 C 0.3743(4) 0.1967(3) 0.2003(2) 0.0403(10) Uani 1 1 d . . . . .
C8 C 0.3998(4) 0.3715(3) 0.1385(2) 0.0401(10) Uani 1 1 d . . . . .
H8A H 0.424220 0.354808 0.099537 0.048 Uiso 1 1 calc R . . . .
C9 C 0.3925(4) 0.4497(2) 0.1476(2) 0.0346(9) Uani 1 1 d . . . . .
C10 C 0.3593(3) 0.4812(2) 0.2037(2) 0.0314(8) Uani 1 1 d . . . . .
C11 C 0.3612(4) 0.5592(2) 0.2093(2) 0.0337(9) Uani 1 1 d . . . . .
C12 C 0.3924(4) 0.6035(3) 0.1606(3) 0.0407(10) Uani 1 1 d . . . . .
H12 H 0.391973 0.655591 0.164556 0.049 Uiso 1 1 calc R . . . .
C13 C 0.4239(5) 0.5708(3) 0.1063(2) 0.0456(11) Uani 1 1 d . . . . .
C14 C 0.4236(4) 0.4958(3) 0.0983(3) 0.0437(11) Uani 1 1 d . . . . .
H14 H 0.444086 0.474956 0.059923 0.052 Uiso 1 1 calc R . . . .
C15 C 0.3341(4) 0.5912(2) 0.2709(2) 0.0379(10) Uani 1 1 d . . . . .
H15A H 0.334676 0.645583 0.268116 0.045 Uiso 1 1 calc R . . . .
H15B H 0.389269 0.576219 0.304132 0.045 Uiso 1 1 calc R . . . .
C16 C 0.2107(5) 0.5817(3) 0.3566(3) 0.0532(13) Uani 1 1 d . . . . .
H16A H 0.262313 0.552573 0.382935 0.080 Uiso 1 1 calc GR . . . .
H16B H 0.137284 0.569100 0.366823 0.080 Uiso 1 1 calc GR . . . .
H16C H 0.223501 0.634247 0.364597 0.080 Uiso 1 1 calc GR . . . .
C17 C 0.1365(4) 0.5978(3) 0.2441(3) 0.0483(12) Uani 1 1 d . . . . .
H17A H 0.129222 0.650924 0.253491 0.058 Uiso 1 1 calc R . . . .
H17B H 0.158132 0.593243 0.200335 0.058 Uiso 1 1 calc R . . . .
C18 C 0.0285(4) 0.5609(3) 0.2489(3) 0.0466(12) Uani 1 1 d . . . . .
H18A H 0.012605 0.558305 0.293898 0.056 Uiso 1 1 calc R . . . .
H18B H -0.027740 0.591882 0.227007 0.056 Uiso 1 1 calc R . . . .
C19 C 0.0086(6) 0.4856(5) 0.1523(3) 0.0712(19) Uani 1 1 d . . . . .
H19A H 0.003209 0.434698 0.137085 0.107 Uiso 1 1 calc GR . . . .
H19B H 0.070835 0.509506 0.135123 0.107 Uiso 1 1 calc GR . . . .
H19C H -0.057081 0.512433 0.138701 0.107 Uiso 1 1 calc GR . . . .
C20 C -0.0641(4) 0.4417(3) 0.2504(2) 0.0438(11) Uani 1 1 d . . . . .
H20A H -0.134136 0.467051 0.243126 0.053 Uiso 1 1 calc R . . . .
H20B H -0.069924 0.392720 0.229945 0.053 Uiso 1 1 calc R . . . .
C21 C -0.0387(4) 0.4323(3) 0.3194(2) 0.0381(10) Uani 1 1 d . . . . .
C22 C 0.0669(3) 0.4125(2) 0.3417(2) 0.0320(9) Uani 1 1 d . . . . .
C23 C 0.0895(4) 0.3999(2) 0.4066(2) 0.0347(9) Uani 1 1 d . . . . .
C24 C 0.0081(4) 0.4108(3) 0.4482(2) 0.0393(10) Uani 1 1 d . . . . .
H24 H 0.023240 0.404420 0.492195 0.047 Uiso 1 1 calc R . . . .
C25 C -0.0934(4) 0.4305(3) 0.4254(2) 0.0406(10) Uani 1 1 d . . . . .
C26 C -0.1184(4) 0.4410(3) 0.3617(3) 0.0398(10) Uani 1 1 d . . . . .
H26 H -0.189558 0.454030 0.346907 0.048 Uiso 1 1 calc R . . . .
C27 C 0.1949(4) 0.3803(3) 0.4330(2) 0.0380(10) Uani 1 1 d . . . . .
H27 H 0.206527 0.381596 0.477621 0.046 Uiso 1 1 calc R . . . .
C28 C 0.4551(4) 0.3309(2) 0.4034(2) 0.0361(10) Uani 1 1 d . . . . .
C29 C 0.5590(4) 0.3112(2) 0.3281(2) 0.0354(9) Uani 1 1 d . . . . .
C30 C 0.6211(4) 0.3053(2) 0.3853(3) 0.0398(10) Uani 1 1 d . . . . .
C31 C 0.7297(4) 0.2873(3) 0.3869(3) 0.0478(13) Uani 1 1 d . . . . .
H31 H 0.770980 0.281799 0.425836 0.057 Uiso 1 1 calc R . . . .
C32 C 0.7750(4) 0.2777(3) 0.3310(3) 0.0549(15) Uani 1 1 d . . . . .
H32 H 0.848789 0.264458 0.331024 0.066 Uiso 1 1 calc R . . . .
C33 C 0.7157(4) 0.2867(3) 0.2739(3) 0.0463(12) Uani 1 1 d . . . . .
H33 H 0.750766 0.281585 0.235750 0.056 Uiso 1 1 calc R . . . .
C34 C 0.6057(4) 0.3031(2) 0.2711(3) 0.0398(10) Uani 1 1 d . . . . .
H34 H 0.564910 0.308478 0.232044 0.048 Uiso 1 1 calc R . . . .
O10 O 0.5959(5) 0.5837(3) 0.4421(3) 0.0308(12) Uiso 0.5 1 d . . . . .
O11 O 0.500000 0.500000 0.500000 0.171(6) Uiso 1 2 d S T P . .
O12 O 0.4685(10) 0.5098(7) 0.4065(6) 0.091(3) Uiso 0.5 1 d . . . . .
N13 N 0.5225(10) 0.5366(7) 0.4493(6) 0.067(3) Uiso 0.5 1 d . . . . .
O7 O 0.5322(5) 0.2290(3) 0.0615(2) 0.0797(16) Uani 1 1 d . . . . .
O8 O 0.6999(5) 0.2255(4) 0.0477(3) 0.102(2) Uani 1 1 d . . . . .
O9 O 0.6410(6) 0.2849(6) 0.1262(4) 0.146(4) Uani 1 1 d . . . . .
N12 N 0.6265(6) 0.2457(4) 0.0796(3) 0.0684(16) Uani 1 1 d . . . . .
N14 N -0.1290(8) 0.6474(5) 0.3815(5) 0.050(2) Uiso 0.5 1 d D . . . .
O14 O -0.1749(10) 0.7065(6) 0.3935(6) 0.091(3) Uiso 0.5 1 d D . . . .
O15 O -0.1701(16) 0.5914(11) 0.3972(11) 0.178(8) Uiso 0.5 1 d D . . . .
O13 O -0.0333(10) 0.6444(8) 0.3843(7) 0.099(4) Uiso 0.5 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O1 2.184(3) . ?
Er1 O2 2.256(3) . ?
Er1 O3 2.367(4) . ?
Er1 O6 2.369(4) . ?
Er1 N1 2.457(4) . ?
Er1 N4 2.561(4) . ?
Er1 N7 2.586(4) . ?
Er1 N9 2.413(4) . ?
Br1 C13 1.902(5) . ?
Br2 C25 1.902(5) . ?
O1 C10 1.306(5) . ?
O2 C22 1.327(5) . ?
O3 N11 1.263(6) . ?
O4 N11 1.239(7) . ?
O5 N11 1.254(7) . ?
N1 C1 1.416(6) . ?
N1 C7 1.316(6) . ?
N2 C2 1.383(7) . ?
N2 C7 1.357(6) . ?
N3 N4 1.387(5) . ?
N3 C7 1.341(7) . ?
N4 C8 1.300(7) . ?
N5 C15 1.517(6) . ?
N5 C16 1.497(6) . ?
N5 C17 1.517(6) . ?
N6 C18 1.484(7) . ?
N6 C19 1.476(7) . ?
N6 C20 1.497(7) . ?
N7 N8 1.377(5) . ?
N7 C27 1.300(6) . ?
N8 C28 1.345(7) . ?
N9 C28 1.318(6) . ?
N9 C29 1.409(6) . ?
N10 C28 1.355(6) . ?
N10 C30 1.371(7) . ?
C1 C2 1.408(7) . ?
C1 C6 1.374(8) . ?
C2 C3 1.383(7) . ?
C3 C4 1.382(9) . ?
C4 C5 1.399(9) . ?
C5 C6 1.395(8) . ?
C8 C9 1.436(6) . ?
C9 C10 1.410(6) . ?
C9 C14 1.415(7) . ?
C10 C11 1.421(6) . ?
C11 C12 1.388(7) . ?
C11 C15 1.492(7) . ?
C12 C13 1.378(7) . ?
C13 C14 1.372(7) . ?
C17 C18 1.512(7) . ?
C20 C21 1.491(7) . ?
C21 C22 1.414(6) . ?
C21 C26 1.391(7) . ?
C22 C23 1.409(7) . ?
C23 C24 1.401(7) . ?
C23 C27 1.439(7) . ?
C24 C25 1.371(7) . ?
C25 C26 1.383(7) . ?
C29 C30 1.402(7) . ?
C29 C34 1.384(7) . ?
C30 C31 1.390(7) . ?
C31 C32 1.360(9) . ?
C32 C33 1.389(9) . ?
C33 C34 1.400(7) . ?
O10 N13 1.267(13) . ?
O11 N13 1.313(12) . ?
O11 N13 1.313(12) 3_666 ?
O12 N13 1.199(16) . ?
O7 N12 1.248(8) . ?
O8 N12 1.228(7) . ?
O9 N12 1.226(9) . ?
N14 O14 1.251(12) . ?
N14 O15 1.195(15) . ?
N14 O13 1.190(12) . ?

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 Er1 O2 73.90(12) . . ?
O1 Er1 O3 150.84(12) . . ?
O1 Er1 O6 93.35(14) . . ?
O1 Er1 N1 133.65(13) . . ?
O1 Er1 N4 70.19(12) . . ?
O1 Er1 N7 98.35(12) . . ?
O1 Er1 N9 87.16(12) . . ?
O2 Er1 O3 77.07(12) . . ?
O2 Er1 O6 74.66(13) . . ?
O2 Er1 N1 146.31(12) . . ?
O2 Er1 N4 126.89(12) . . ?
O2 Er1 N7 68.67(11) . . ?
O2 Er1 N9 125.90(12) . . ?
O3 Er1 O6 81.48(15) . . ?
O3 Er1 N1 74.56(13) . . ?
O3 Er1 N4 132.42(13) . . ?
O3 Er1 N7 68.12(13) . . ?
O3 Er1 N9 108.04(14) . . ?
O6 Er1 N1 83.47(14) . . ?
O6 Er1 N4 69.87(14) . . ?
O6 Er1 N7 136.35(13) . . ?
O6 Er1 N9 158.34(15) . . ?
N1 Er1 N4 65.34(13) . . ?
N1 Er1 N7 115.59(13) . . ?
N4 Er1 N7 153.21(13) . . ?
N9 Er1 N1 80.61(13) . . ?
N9 Er1 N4 90.09(14) . . ?
N9 Er1 N7 64.65(13) . . ?
C10 O1 Er1 146.1(3) . . ?
C22 O2 Er1 137.1(3) . . ?
N11 O3 Er1 137.4(4) . . ?
C1 N1 Er1 137.9(3) . . ?
C7 N1 Er1 117.4(3) . . ?
C7 N1 C1 104.3(4) . . ?
C7 N2 C2 106.4(4) . . ?
C7 N3 N4 116.1(4) . . ?
N3 N4 Er1 115.2(3) . . ?
C8 N4 Er1 130.8(3) . . ?
C8 N4 N3 113.4(4) . . ?
C15 N5 C17 110.5(4) . . ?
C16 N5 C15 109.8(4) . . ?
C16 N5 C17 113.8(4) . . ?
C18 N6 C20 110.9(4) . . ?
C19 N6 C18 112.9(5) . . ?
C19 N6 C20 111.6(5) . . ?
N8 N7 Er1 115.0(3) . . ?
C27 N7 Er1 129.5(3) . . ?
C27 N7 N8 115.0(4) . . ?
C28 N8 N7 115.1(4) . . ?
C28 N9 Er1 119.2(3) . . ?
C28 N9 C29 104.3(4) . . ?
C29 N9 Er1 135.8(3) . . ?
C28 N10 C30 106.0(4) . . ?
O4 N11 O3 120.0(5) . . ?
O4 N11 O5 122.4(5) . . ?
O5 N11 O3 117.6(5) . . ?
C2 C1 N1 108.7(4) . . ?
C6 C1 N1 130.7(5) . . ?
C6 C1 C2 120.5(4) . . ?
N2 C2 C1 106.1(4) . . ?
N2 C2 C3 131.4(5) . . ?
C3 C2 C1 122.4(5) . . ?
C4 C3 C2 117.0(5) . . ?
C3 C4 C5 120.8(5) . . ?
C6 C5 C4 122.0(6) . . ?
C1 C6 C5 117.2(6) . . ?
N1 C7 N2 114.4(5) . . ?
N1 C7 N3 124.8(4) . . ?
N3 C7 N2 120.8(5) . . ?
N4 C8 C9 125.3(5) . . ?
C10 C9 C8 122.7(4) . . ?
C10 C9 C14 119.7(4) . . ?
C14 C9 C8 117.6(4) . . ?
O1 C10 C9 122.8(4) . . ?
O1 C10 C11 119.0(4) . . ?
C9 C10 C11 118.2(4) . . ?
C10 C11 C15 117.3(4) . . ?
C12 C11 C10 121.2(4) . . ?
C12 C11 C15 121.3(4) . . ?
C13 C12 C11 119.0(4) . . ?
C12 C13 Br1 118.6(4) . . ?
C14 C13 Br1 119.2(4) . . ?
C14 C13 C12 122.2(5) . . ?
C13 C14 C9 119.6(5) . . ?
C11 C15 N5 110.9(4) . . ?
C18 C17 N5 113.2(4) . . ?
N6 C18 C17 114.1(4) . . ?
C21 C20 N6 110.5(4) . . ?
C22 C21 C20 119.4(4) . . ?
C26 C21 C20 120.6(4) . . ?
C26 C21 C22 120.0(5) . . ?
O2 C22 C21 118.9(4) . . ?
O2 C22 C23 121.7(4) . . ?
C23 C22 C21 119.4(4) . . ?
C22 C23 C27 122.8(4) . . ?
C24 C23 C22 119.2(4) . . ?
C24 C23 C27 117.9(4) . . ?
C25 C24 C23 120.1(5) . . ?
C24 C25 Br2 120.3(4) . . ?
C24 C25 C26 121.7(4) . . ?
C26 C25 Br2 118.0(4) . . ?
C25 C26 C21 119.5(4) . . ?
N7 C27 C23 125.4(4) . . ?
N8 C28 N10 121.5(5) . . ?
N9 C28 N8 124.2(4) . . ?
N9 C28 N10 114.3(5) . . ?
C30 C29 N9 108.3(4) . . ?
C34 C29 N9 130.8(4) . . ?
C34 C29 C30 120.8(4) . . ?
N10 C30 C29 107.0(4) . . ?
N10 C30 C31 131.6(5) . . ?
C31 C30 C29 121.3(5) . . ?
C32 C31 C30 117.8(5) . . ?
C31 C32 C33 121.5(5) . . ?
C32 C33 C34 121.6(5) . . ?
C29 C34 C33 116.8(5) . . ?
N13 O11 N13 180.0 . 3_666 ?
O10 N13 O11 129.3(10) . . ?
O12 N13 O10 123.8(13) . . ?
O12 N13 O11 106.1(11) . . ?
O8 N12 O7 118.5(7) . . ?
O9 N12 O7 118.4(6) . . ?
O9 N12 O8 122.9(8) . . ?
O15 N14 O14 117.6(15) . . ?
O13 N14 O14 119.8(12) . . ?
O13 N14 O15 113.1(13) . . ?

_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 0.000 0.500 400.6 85.5 '4(C2 H3N)'
2 0.000 0.500 0.000 400.6 85.5 '4(C2 H3N)'

_olex2_submission_special_instructions 'No special instructions were received'
