# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

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

data_sad
_database_code_depnum_ccdc_archive 'CCDC 1826195'
_audit_update_record             
;
2018-02-27 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_audit_creation_date             2017-01-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H57 N4 Nd1 O6, 2(H2 O)'
_chemical_formula_sum            'C42 H61 N4 Nd O8'
_chemical_formula_weight         894.18
_chemical_absolute_configuration ?
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      trigonal
_space_group_IT_number           159
_space_group_name_H-M_alt        'P 3 1 c'
_space_group_name_Hall           'P 3 -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   15.881(2)
_cell_length_b                   15.881(2)
_cell_length_c                   10.323(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2254.7(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23017
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.067
_cell_measurement_theta_min      2.962
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.203
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.651588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1220 before and 0.0595 after correction.
The Ratio of minimum to maximum transmission is 0.6516.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23017
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.067
_diffrn_reflns_theta_min         2.962
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                4095
_reflns_number_total             4351
_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       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2016 (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         0.956
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 
;
 Flack x determined using 1937 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         4351
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0276
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0350P)²+0.6234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0722
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O5(0.5) H5A(0.5) H5B(0.5) O6(0.08333) H6A(0.08333) H6B(0.08333)
 O7(0.08333) H7A(0.08333) H7B(0.08333)
5.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Nd1 Nd 0.3333 0.6667 0.25066(4) 0.02137(8) Uani 1 3 d S TU P . .
O4 O 0.3521(3) 1.1219(3) 0.4741(4) 0.0470(9) Uani 1 1 d . U . . .
N4 N 0.3333 0.6667 -0.0101(6) 0.0263(11) Uani 1 3 d S TU P . .
O1 O 0.2795(2) 0.7513(2) 0.3577(3) 0.0327(6) Uani 1 1 d . U . . .
N1 N 0.4064(2) 0.8367(2) 0.1549(3) 0.0299(6) Uani 1 1 d . U . . .
C2 C 0.3618(3) 0.9216(3) 0.3146(4) 0.0283(7) Uani 1 1 d . U . . .
C6 C 0.2398(3) 0.8518(3) 0.4860(4) 0.0276(7) Uani 1 1 d . U . . .
C22 C 0.4488(3) 0.8429(3) 0.0270(4) 0.0330(8) Uani 1 1 d . U . . .
H22A H 0.5021 0.8298 0.0333 0.040 Uiso 1 1 calc R . . . .
H22B H 0.4734 0.9075 -0.0091 0.040 Uiso 1 1 calc R . . . .
C7 C 0.4092(3) 0.9139(3) 0.1990(4) 0.0287(7) Uani 1 1 d . U . . .
H7 H 0.4454 0.9708 0.1517 0.034 Uiso 1 1 calc R . . . .
C23 C 0.3685(3) 0.7674(3) -0.0586(4) 0.0322(8) Uani 1 1 d . U . . .
H23A H 0.3146 0.7798 -0.0611 0.039 Uiso 1 1 calc R . . . .
H23B H 0.3929 0.7730 -0.1463 0.039 Uiso 1 1 calc R . . . .
C1 C 0.2939(3) 0.8381(3) 0.3864(4) 0.0262(7) Uani 1 1 d . U . . .
C29 C 0.1576(3) 0.7622(3) 0.5551(4) 0.0328(8) Uani 1 1 d . U . . .
C3 C 0.3780(3) 1.0146(3) 0.3464(4) 0.0312(7) Uani 1 1 d . U . . .
H3 H 0.4223 1.0682 0.2984 0.037 Uiso 1 1 calc R . . . .
C4 C 0.3294(3) 1.0275(3) 0.4471(4) 0.0325(8) Uani 1 1 d . U . . .
C31 C 0.1065(4) 0.7922(4) 0.6574(5) 0.0468(11) Uani 1 1 d . U . . .
H31A H 0.1526 0.8318 0.7224 0.070 Uiso 1 1 calc GR . . . .
H31B H 0.0547 0.7350 0.6971 0.070 Uiso 1 1 calc GR . . . .
H31C H 0.0803 0.8284 0.6162 0.070 Uiso 1 1 calc GR . . . .
C30 C 0.1977(5) 0.7043(4) 0.6234(5) 0.0523(13) Uani 1 1 d . U . . .
H30A H 0.2281 0.6832 0.5609 0.078 Uiso 1 1 calc GR . . . .
H30B H 0.1455 0.6486 0.6650 0.078 Uiso 1 1 calc GR . . . .
H30C H 0.2447 0.7446 0.6870 0.078 Uiso 1 1 calc GR . . . .
C5 C 0.2597(3) 0.9453(3) 0.5158(4) 0.0309(7) Uani 1 1 d . U . . .
H5 H 0.2260 0.9540 0.5832 0.037 Uiso 1 1 calc R . . . .
C32 C 0.0802(3) 0.6988(4) 0.4552(5) 0.0452(11) Uani 1 1 d . U . . .
H32A H 0.0574 0.7370 0.4115 0.068 Uiso 1 1 calc GR . . . .
H32B H 0.0268 0.6452 0.4983 0.068 Uiso 1 1 calc GR . . . .
H32C H 0.1079 0.6746 0.3931 0.068 Uiso 1 1 calc GR . . . .
C28 C 0.2993(5) 1.1361(4) 0.5742(6) 0.0532(13) Uani 1 1 d . U . . .
H28A H 0.2311 1.0997 0.5550 0.080 Uiso 1 1 calc GR . . . .
H28B H 0.3196 1.2039 0.5804 0.080 Uiso 1 1 calc GR . . . .
H28C H 0.3115 1.1142 0.6550 0.080 Uiso 1 1 calc GR . . . .
O5 O 0.0628(15) 0.9449(18) 0.3485(16) 0.149(8) Uani 0.5 1 d . U . A 1
H5A H 0.0010 0.9135 0.3393 0.224 Uiso 0.5 1 d R . . A 1
H5B H 0.0860 1.0019 0.3167 0.224 Uiso 0.5 1 d R . . A 1
O6 O 0.0000 1.0000 0.28(3) 0.27(7) Uani 0.25 3 d S TU P B 2
H6A H -0.0011 1.0472 0.2402 0.403 Uiso 0.0833 1 d R . . B 2
H6B H 0.0584 1.0157 0.2962 0.403 Uiso 0.0833 1 d R . . B 2
O7 O 0.0000 1.0000 0.480(8) 0.15(2) Uani 0.25 3 d S TU P C 3
H7A H 0.0336 1.0165 0.4107 0.220 Uiso 0.0833 1 d R . . C 3
H7B H -0.0602 0.9757 0.4617 0.220 Uiso 0.0833 1 d R . . C 3


_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 N4 2.692(6) . ?
Nd1 O1 2.216(3) 3_565 ?
Nd1 O1 2.216(3) . ?
Nd1 O1 2.216(3) 2_665 ?
Nd1 N1 2.547(3) 2_665 ?
Nd1 N1 2.547(3) 3_565 ?
Nd1 N1 2.547(3) . ?
O4 C4 1.384(5) . ?
O4 C28 1.417(7) . ?
N4 C23 1.492(5) 2_665 ?
N4 C23 1.492(5) . ?
N4 C23 1.493(5) 3_565 ?
O1 C1 1.313(5) . ?
N1 C22 1.463(5) . ?
N1 C7 1.288(5) . ?
C2 C7 1.447(5) . ?
C2 C1 1.428(5) . ?
C2 C3 1.407(5) . ?
C6 C1 1.425(5) . ?
C6 C29 1.542(5) . ?
C6 C5 1.390(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.522(6) . ?
C7 H7 0.9300 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C29 C31 1.546(7) . ?
C29 C30 1.528(7) . ?
C29 C32 1.533(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.370(6) . ?
C4 C5 1.409(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C5 H5 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
O5 H5A 0.8558 . ?
O5 H5B 0.8549 . ?
O6 H6A 0.8543 . ?
O6 H6B 0.8513 . ?
O7 H7A 0.8498 . ?
O7 H7B 0.8542 . ?

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 Nd1 N4 119.92(8) 2_665 . ?
O1 Nd1 N4 119.92(8) 3_565 . ?
O1 Nd1 N4 119.91(8) . . ?
O1 Nd1 O1 97.29(10) . 2_665 ?
O1 Nd1 O1 97.29(10) 2_665 3_565 ?
O1 Nd1 O1 97.29(10) . 3_565 ?
O1 Nd1 N1 86.93(11) . 2_665 ?
O1 Nd1 N1 167.17(11) . 3_565 ?
O1 Nd1 N1 70.10(10) 2_665 2_665 ?
O1 Nd1 N1 70.10(10) 3_565 3_565 ?
O1 Nd1 N1 70.09(10) . . ?
O1 Nd1 N1 86.93(11) 2_665 3_565 ?
O1 Nd1 N1 167.17(11) 3_565 2_665 ?
O1 Nd1 N1 167.17(11) 2_665 . ?
O1 Nd1 N1 86.93(11) 3_565 . ?
N1 Nd1 N4 67.15(8) 2_665 . ?
N1 Nd1 N4 67.15(8) . . ?
N1 Nd1 N4 67.15(8) 3_565 . ?
N1 Nd1 N1 105.89(9) 2_665 3_565 ?
N1 Nd1 N1 105.89(9) . 3_565 ?
N1 Nd1 N1 105.89(9) . 2_665 ?
C4 O4 C28 117.7(4) . . ?
C23 N4 Nd1 109.6(3) 3_565 . ?
C23 N4 Nd1 109.6(3) 2_665 . ?
C23 N4 Nd1 109.6(3) . . ?
C23 N4 C23 109.3(3) 2_665 . ?
C23 N4 C23 109.3(3) . 3_565 ?
C23 N4 C23 109.3(3) 2_665 3_565 ?
C1 O1 Nd1 146.3(3) . . ?
C22 N1 Nd1 111.8(2) . . ?
C7 N1 Nd1 130.8(3) . . ?
C7 N1 C22 117.4(3) . . ?
C1 C2 C7 122.2(3) . . ?
C3 C2 C7 116.8(3) . . ?
C3 C2 C1 120.7(4) . . ?
C1 C6 C29 119.3(3) . . ?
C5 C6 C1 119.3(4) . . ?
C5 C6 C29 121.3(4) . . ?
N1 C22 H22A 110.3 . . ?
N1 C22 H22B 110.3 . . ?
N1 C22 C23 107.2(3) . . ?
H22A C22 H22B 108.5 . . ?
C23 C22 H22A 110.3 . . ?
C23 C22 H22B 110.3 . . ?
N1 C7 C2 126.8(3) . . ?
N1 C7 H7 116.6 . . ?
C2 C7 H7 116.6 . . ?
N4 C23 C22 111.6(4) . . ?
N4 C23 H23A 109.3 . . ?
N4 C23 H23B 109.3 . . ?
C22 C23 H23A 109.3 . . ?
C22 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
O1 C1 C2 120.8(3) . . ?
O1 C1 C6 121.4(3) . . ?
C6 C1 C2 117.8(3) . . ?
C6 C29 C31 111.3(4) . . ?
C30 C29 C6 110.7(4) . . ?
C30 C29 C31 108.1(4) . . ?
C30 C29 C32 110.7(5) . . ?
C32 C29 C6 109.0(4) . . ?
C32 C29 C31 106.8(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 120.9(4) . . ?
C4 C3 H3 119.5 . . ?
O4 C4 C5 124.1(4) . . ?
C3 C4 O4 117.0(4) . . ?
C3 C4 C5 118.9(4) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C6 C5 C4 122.2(4) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H5A O5 H5B 109.6 . . ?
H6A O6 H6B 109.9 . . ?
H7A O7 H7B 110.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C23 H23A O4 0.97 2.54 3.449(6) 155.7 5_674
O5 H5A O5 0.86 2.10 2.81(3) 139.6 3_465
O5 H5B O5 0.85 2.15 2.81(3) 133.3 2_675

_shelx_SHELXL_version_number     2014/7
_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_sad_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1826198'
_audit_update_record             
;
2018-02-27 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_audit_creation_date             2017-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H57 Eu1 N4 O6, 2(H2 O)'
_chemical_formula_sum            'C42 H61 Eu N4 O8'
_chemical_formula_weight         901.90
_chemical_absolute_configuration ?
_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 0.0033 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'
Eu Eu -0.1578 3.6682 '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'

_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      trigonal
_space_group_IT_number           159
_space_group_name_H-M_alt        'P 3 1 c'
_space_group_name_Hall           'P 3 -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   15.815(2)
_cell_length_b                   15.815(2)
_cell_length_c                   10.364(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2245.1(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23017
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.448
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.113637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.4735 before and 0.0898 after correction.
The Ratio of minimum to maximum transmission is 0.1136.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23017
_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         29.990
_diffrn_reflns_theta_min         2.974
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4095
_reflns_number_total             4351
_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       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2016 (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.138
_refine_diff_density_min         -1.277
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.040(17)
_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     180
_refine_ls_number_reflns         4351
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0271
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0335P)²+0.5364P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0706
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O5(0.5) H5A(0.5) H5B(0.5) O6(0.08333) H6A(0.08333) H6B(0.08333)
 O7(0.08333) H7A(0.08333) H7B(0.08333)
5.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_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
Eu1 Eu 0.3333 0.6667 0.25064(4) 0.02162(8) Uani 1 3 d S TU P . .
O4 O 0.3523(3) 1.1220(3) 0.4742(4) 0.0430(8) Uani 1 1 d . U . . .
N4 N 0.3333 0.6667 -0.0102(6) 0.0235(10) Uani 1 3 d S TU P . .
O1 O 0.2795(2) 0.7513(2) 0.3578(3) 0.0294(6) Uani 1 1 d . U . . .
N1 N 0.4065(2) 0.8367(2) 0.1549(3) 0.0267(6) Uani 1 1 d . U . . .
C2 C 0.3620(3) 0.9216(3) 0.3146(4) 0.0253(7) Uani 1 1 d . U . . .
C6 C 0.2398(3) 0.8517(3) 0.4862(4) 0.0247(7) Uani 1 1 d . U . . .
C22 C 0.4488(3) 0.8429(3) 0.0270(4) 0.0299(7) Uani 1 1 d . U . . .
H22A H 0.5024 0.8298 0.0330 0.036 Uiso 1 1 calc R . . . .
H22B H 0.4735 0.9078 -0.0088 0.036 Uiso 1 1 calc R . . . .
C7 C 0.4092(3) 0.9140(3) 0.1991(4) 0.0257(7) Uani 1 1 d . U . . .
H7 H 0.4454 0.9711 0.1519 0.031 Uiso 1 1 calc R . . . .
C23 C 0.3686(3) 0.7674(3) -0.0586(4) 0.0291(7) Uani 1 1 d . U . . .
H23A H 0.3145 0.7799 -0.0614 0.035 Uiso 1 1 calc R . . . .
H23B H 0.3933 0.7730 -0.1458 0.035 Uiso 1 1 calc R . . . .
C1 C 0.2940(3) 0.8381(3) 0.3864(3) 0.0231(6) Uani 1 1 d . U . . .
C29 C 0.1575(3) 0.7624(3) 0.5549(4) 0.0293(8) Uani 1 1 d . U . . .
C3 C 0.3781(3) 1.0146(3) 0.3462(4) 0.0282(7) Uani 1 1 d . U . . .
H3 H 0.4224 1.0683 0.2982 0.034 Uiso 1 1 calc R . . . .
C4 C 0.3294(3) 1.0276(3) 0.4471(4) 0.0294(8) Uani 1 1 d . U . . .
C31 C 0.1063(4) 0.7923(4) 0.6572(5) 0.0433(11) Uani 1 1 d . U . . .
H31A H 0.1531 0.8335 0.7206 0.065 Uiso 1 1 calc GR . . . .
H31B H 0.0556 0.7349 0.6984 0.065 Uiso 1 1 calc GR . . . .
H31C H 0.0784 0.8271 0.6162 0.065 Uiso 1 1 calc GR . . . .
C30 C 0.1978(5) 0.7044(4) 0.6234(5) 0.0487(12) Uani 1 1 d . U . . .
H30A H 0.2275 0.6824 0.5612 0.073 Uiso 1 1 calc GR . . . .
H30B H 0.1455 0.6490 0.6660 0.073 Uiso 1 1 calc GR . . . .
H30C H 0.2456 0.7453 0.6859 0.073 Uiso 1 1 calc GR . . . .
C5 C 0.2596(3) 0.9454(3) 0.5157(4) 0.0280(7) Uani 1 1 d . U . . .
H5 H 0.2258 0.9541 0.5829 0.034 Uiso 1 1 calc R . . . .
C32 C 0.0803(3) 0.6989(4) 0.4549(5) 0.0414(11) Uani 1 1 d . U . . .
H32A H 0.0579 0.7374 0.4107 0.062 Uiso 1 1 calc GR . . . .
H32B H 0.0262 0.6452 0.4976 0.062 Uiso 1 1 calc GR . . . .
H32C H 0.1083 0.6743 0.3939 0.062 Uiso 1 1 calc GR . . . .
C28 C 0.2991(4) 1.1360(4) 0.5743(6) 0.0489(12) Uani 1 1 d . U . . .
H28A H 0.2307 1.1008 0.5540 0.073 Uiso 1 1 calc GR . . . .
H28B H 0.3206 1.2042 0.5822 0.073 Uiso 1 1 calc GR . . . .
H28C H 0.3100 1.1123 0.6542 0.073 Uiso 1 1 calc GR . . . .
O5 O 0.0617(16) 0.9443(19) 0.3484(16) 0.148(8) Uani 0.5 1 d . U . A 1
H5A H 0.0000 0.9136 0.3385 0.222 Uiso 0.5 1 d R . . A 1
H5B H 0.0855 1.0022 0.3192 0.222 Uiso 0.5 1 d R . . A 1
O6 O 0.0000 1.0000 0.297(9) 0.17(4) Uani 0.25 3 d S TU P B 2
H6A H 0.0600 1.0359 0.2770 0.262 Uiso 0.0833 1 d R . . B 2
H6B H -0.0237 0.9461 0.2566 0.262 Uiso 0.0833 1 d R . . B 2
O7 O 0.0000 1.0000 0.477(6) 0.14(2) Uani 0.25 3 d S TU P C 3
H7A H 0.0418 1.0179 0.4169 0.215 Uiso 0.0833 1 d R . . C 3
H7B H -0.0565 0.9806 0.4460 0.215 Uiso 0.0833 1 d R . . C 3


_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 N4 2.703(6) . ?
Eu1 O1 2.212(3) 3_565 ?
Eu1 O1 2.212(3) . ?
Eu1 O1 2.212(3) 2_665 ?
Eu1 N1 2.538(3) 2_665 ?
Eu1 N1 2.538(3) 3_565 ?
Eu1 N1 2.538(3) . ?
O4 C4 1.378(5) . ?
O4 C28 1.421(6) . ?
N4 C23 1.487(4) 2_665 ?
N4 C23 1.487(4) . ?
N4 C23 1.487(4) 3_565 ?
O1 C1 1.307(4) . ?
N1 C22 1.467(5) . ?
N1 C7 1.286(5) . ?
C2 C7 1.447(5) . ?
C2 C1 1.426(5) . ?
C2 C3 1.400(5) . ?
C6 C1 1.427(5) . ?
C6 C29 1.536(5) . ?
C6 C5 1.386(5) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.519(6) . ?
C7 H7 0.9300 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C29 C31 1.545(6) . ?
C29 C30 1.528(7) . ?
C29 C32 1.532(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.375(6) . ?
C4 C5 1.406(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C5 H5 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
O5 H5A 0.8520 . ?
O5 H5B 0.8522 . ?
O6 H6A 0.8521 . ?
O6 H6B 0.8499 . ?
O7 H7A 0.8501 . ?
O7 H7B 0.8514 . ?

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 N4 120.13(8) 2_665 . ?
O1 Eu1 N4 120.13(8) 3_565 . ?
O1 Eu1 N4 120.13(8) . . ?
O1 Eu1 O1 97.02(10) . 2_665 ?
O1 Eu1 O1 97.01(10) 2_665 3_565 ?
O1 Eu1 O1 97.02(10) . 3_565 ?
O1 Eu1 N1 87.09(11) . 2_665 ?
O1 Eu1 N1 167.19(11) . 3_565 ?
O1 Eu1 N1 70.38(10) 2_665 2_665 ?
O1 Eu1 N1 70.38(10) 3_565 3_565 ?
O1 Eu1 N1 70.38(10) . . ?
O1 Eu1 N1 87.09(11) 2_665 3_565 ?
O1 Eu1 N1 167.19(11) 3_565 2_665 ?
O1 Eu1 N1 167.19(11) 2_665 . ?
O1 Eu1 N1 87.09(11) 3_565 . ?
N1 Eu1 N4 66.99(7) 2_665 . ?
N1 Eu1 N4 66.99(7) . . ?
N1 Eu1 N4 66.99(7) 3_565 . ?
N1 Eu1 N1 105.71(8) 2_665 3_565 ?
N1 Eu1 N1 105.71(8) . 3_565 ?
N1 Eu1 N1 105.71(8) . 2_665 ?
C4 O4 C28 117.5(4) . . ?
C23 N4 Eu1 109.7(3) 3_565 . ?
C23 N4 Eu1 109.7(3) 2_665 . ?
C23 N4 Eu1 109.7(3) . . ?
C23 N4 C23 109.2(3) 2_665 . ?
C23 N4 C23 109.2(3) . 3_565 ?
C23 N4 C23 109.2(3) 2_665 3_565 ?
C1 O1 Eu1 146.2(2) . . ?
C22 N1 Eu1 112.1(2) . . ?
C7 N1 Eu1 130.5(3) . . ?
C7 N1 C22 117.4(3) . . ?
C1 C2 C7 122.4(3) . . ?
C3 C2 C7 116.8(3) . . ?
C3 C2 C1 120.5(3) . . ?
C1 C6 C29 119.6(3) . . ?
C5 C6 C1 119.3(3) . . ?
C5 C6 C29 121.0(4) . . ?
N1 C22 H22A 110.2 . . ?
N1 C22 H22B 110.2 . . ?
N1 C22 C23 107.5(3) . . ?
H22A C22 H22B 108.5 . . ?
C23 C22 H22A 110.2 . . ?
C23 C22 H22B 110.2 . . ?
N1 C7 C2 126.9(3) . . ?
N1 C7 H7 116.6 . . ?
C2 C7 H7 116.6 . . ?
N4 C23 C22 111.3(3) . . ?
N4 C23 H23A 109.4 . . ?
N4 C23 H23B 109.4 . . ?
C22 C23 H23A 109.4 . . ?
C22 C23 H23B 109.4 . . ?
H23A C23 H23B 108.0 . . ?
O1 C1 C2 120.6(3) . . ?
O1 C1 C6 121.3(3) . . ?
C2 C1 C6 118.1(3) . . ?
C6 C29 C31 111.7(4) . . ?
C30 C29 C6 110.6(4) . . ?
C30 C29 C31 107.8(4) . . ?
C30 C29 C32 110.8(4) . . ?
C32 C29 C6 108.7(4) . . ?
C32 C29 C31 107.3(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.0(4) . . ?
C4 C3 H3 119.5 . . ?
O4 C4 C5 124.0(4) . . ?
C3 C4 O4 117.0(4) . . ?
C3 C4 C5 119.1(4) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C6 C5 C4 122.0(4) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H5A O5 H5B 109.6 . . ?
H6A O6 H6B 109.6 . . ?
H7A O7 H7B 109.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C23 H23A O4 0.97 2.53 3.432(6) 155.5 5_674
O5 H5A O5 0.85 2.08 2.79(3) 139.7 3_465
O5 H5B O5 0.85 2.12 2.79(3) 134.8 2_675

_shelx_SHELXL_version_number     2014/7
_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_sad2
_database_code_depnum_ccdc_archive 'CCDC 1826199'
_audit_update_record             
;
2018-02-27 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_audit_creation_date             2017-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H57 N4 O6 Yb1, 2(H2 O)'
_chemical_formula_sum            'C42 H61 N4 O8 Yb'
_chemical_formula_weight         922.98
_chemical_absolute_configuration ?
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 '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      trigonal
_space_group_IT_number           159
_space_group_name_H-M_alt        'P 3 1 c'
_space_group_name_Hall           'P 3 -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   15.723(2)
_cell_length_b                   15.723(2)
_cell_length_c                   10.448(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2236.8(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    21529
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3.0
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.142
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.294015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2004/1 (Bruker,2004) was used for absorption correction. R(int) was 0.2544 before and 0.1040 after correction. The Ratio of minimum to maximum transmission is 0.2940. The λ/2 correction factor is 0.0015.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             950
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21529
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.992
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3638
_reflns_number_total             3999
_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       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    ?
_refine_diff_density_max         0.823
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.133(19)
_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     178
_refine_ls_number_reflns         3999
_refine_ls_number_restraints     290
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0335P)²+1.1894P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0823
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 C2, Yb1, O1, N4, N1, C1, C23, C7, C22, C6, H23A, H23B, H7, H22A, H22B, C5,
 C29, C3, C4, H5, C31, C30, C32, H3, O4, H31A, H31B, H31C, H30A, H30B, H30C,
 H32A, H32B, H32C, C28, H28A, H28B, H28C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C6 \\sim Yb1 \\sim O1 \\sim N4 \\sim N1 \\sim C1 \\sim C23 \\sim C7 \\sim C22
\\sim C2 \\sim H23A \\sim H23B \\sim H7 \\sim H22A \\sim H22B \\sim C5 \\sim
C29 \\sim C3 \\sim C4 \\sim H5 \\sim C31 \\sim C30 \\sim C32 \\sim H3 \\sim O4
\\sim H31A \\sim H31B \\sim H31C \\sim H30A \\sim H30B \\sim H30C \\sim H32A
\\sim H32B \\sim H32C \\sim C28 \\sim H28A \\sim H28B \\sim H28C: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O6) = Uanis(O7)
4. Others
 Fixed Sof: O5(0.5) H5A(0.5) H5B(0.5) O6(0.08333) H6A(0.08333) H6B(0.08333)
 O7(0.08333) H7A(0.08333) H7B(0.08333)
5.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.6667 0.3333 0.74988(5) 0.02658(10) Uani 1 3 d S TU P . .
O1 O 0.7213(3) 0.4664(3) 0.6407(4) 0.0317(8) Uani 1 1 d . U . . .
C6 C 0.7587(4) 0.6035(4) 0.5081(5) 0.0286(10) Uani 1 1 d . U . . .
C1 C 0.7049(4) 0.5365(4) 0.6081(5) 0.0260(9) Uani 1 1 d . U . . .
C3 C 0.6194(4) 0.6294(4) 0.6441(5) 0.0331(11) Uani 1 1 d . U . . .
H3 H 0.5734 0.6390 0.6915 0.040 Uiso 1 1 calc R U . . .
C4 C 0.6692(4) 0.6910(5) 0.5435(6) 0.0347(12) Uani 1 1 d . U . . .
C5 C 0.7379(4) 0.6773(4) 0.4764(6) 0.0332(11) Uani 1 1 d . U . . .
H5 H 0.7717 0.7197 0.4068 0.040 Uiso 1 1 calc R U . . .
C2 C 0.6360(4) 0.5530(4) 0.6768(5) 0.0279(9) Uani 1 1 d . U . . .
C29 C 0.8418(4) 0.5970(5) 0.4403(5) 0.0344(11) Uani 1 1 d . U . . .
C31 C 0.8912(6) 0.6755(6) 0.3350(7) 0.0535(19) Uani 1 1 d . U . . .
H31A H 0.8418 0.6685 0.2723 0.080 Uiso 1 1 calc GR U . . .
H31B H 0.9418 0.6667 0.2922 0.080 Uiso 1 1 calc GR U . . .
H31C H 0.9215 0.7410 0.3735 0.080 Uiso 1 1 calc GR U . . .
C30 C 0.8024(7) 0.4954(6) 0.3782(8) 0.0567(19) Uani 1 1 d . U . . .
H30A H 0.7780 0.4449 0.4449 0.085 Uiso 1 1 calc GR U . . .
H30B H 0.8554 0.4939 0.3307 0.085 Uiso 1 1 calc GR U . . .
H30C H 0.7488 0.4828 0.3194 0.085 Uiso 1 1 calc GR U . . .
C32 C 0.9209(5) 0.6153(6) 0.5391(7) 0.0487(16) Uani 1 1 d . U . . .
H32A H 0.9428 0.6786 0.5812 0.073 Uiso 1 1 calc GR U . . .
H32B H 0.9768 0.6162 0.4962 0.073 Uiso 1 1 calc GR U . . .
H32C H 0.8938 0.5627 0.6032 0.073 Uiso 1 1 calc GR U . . .
O4 O 0.6464(4) 0.7632(4) 0.5153(5) 0.0492(12) Uani 1 1 d . U . . .
C28 C 0.7018(6) 0.8309(6) 0.4174(8) 0.0560(19) Uani 1 1 d . U . . .
H28A H 0.6938 0.7954 0.3372 0.084 Uiso 1 1 calc GR U . . .
H28B H 0.7713 0.8665 0.4415 0.084 Uiso 1 1 calc GR U . . .
H28C H 0.6785 0.8778 0.4059 0.084 Uiso 1 1 calc GR U . . .
C7 C 0.5882(4) 0.4982(4) 0.7913(5) 0.0294(10) Uani 1 1 d . U . . .
H7 H 0.5502 0.5194 0.8379 0.035 Uiso 1 1 calc R U . . .
N4 N 0.6667 0.3333 1.0030(8) 0.0296(16) Uani 1 3 d S TU P . .
N1 N 0.5915(3) 0.4241(3) 0.8370(4) 0.0308(9) Uani 1 1 d . U . . .
C22 C 0.5484(4) 0.3898(5) 0.9636(5) 0.0355(12) Uani 1 1 d . U . . .
H22A H 0.4939 0.3210 0.9589 0.043 Uiso 1 1 calc R U . . .
H22B H 0.5222 0.4311 0.9971 0.043 Uiso 1 1 calc R U . . .
C23 C 0.6287(4) 0.3970(4) 1.0502(5) 0.0341(11) Uani 1 1 d . U . . .
H23A H 0.6830 0.4659 1.0537 0.041 Uiso 1 1 calc R U . . .
H23B H 0.6025 0.3767 1.1380 0.041 Uiso 1 1 calc R U . . .
O5 O 0.935(2) 0.887(2) 0.651(2) 0.223(15) Uani 0.5 1 d . . . A 1
H5A H 0.9924 0.8963 0.6355 0.335 Uiso 0.5 1 d R . . A 1
H5B H 0.9400 0.9348 0.6952 0.335 Uiso 0.5 1 d R . . A 1
O6 O 1.0000 1.0000 0.797(7) 0.18(3) Uani 0.25 3 d S T P B 2
H6A H 1.0078 1.0493 0.7538 0.265 Uiso 0.0833 1 d R . . B 2
H6B H 1.0020 0.9607 0.7433 0.265 Uiso 0.0833 1 d R . . B 2
O7 O 1.0000 1.0000 0.538(7) 0.18(3) Uani 0.25 3 d S T P C 3
H7A H 1.0606 1.0415 0.5487 0.265 Uiso 0.0833 1 d R . . C 3
H7B H 0.9716 0.9839 0.6104 0.265 Uiso 0.0833 1 d R . . C 3


_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 2.150(4) 3_665 ?
Yb1 O1 2.150(4) . ?
Yb1 O1 2.150(4) 2_655 ?
Yb1 N4 2.645(8) . ?
Yb1 N1 2.439(5) . ?
Yb1 N1 2.439(5) 2_655 ?
Yb1 N1 2.439(5) 3_665 ?
O1 C1 1.297(6) . ?
C6 C1 1.423(7) . ?
C6 C5 1.395(8) . ?
C6 C29 1.533(7) . ?
C1 C2 1.426(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.377(8) . ?
C3 C2 1.394(8) . ?
C4 C5 1.391(9) . ?
C4 O4 1.382(7) . ?
C5 H5 0.9500 . ?
C2 C7 1.446(7) . ?
C29 C31 1.542(9) . ?
C29 C30 1.539(10) . ?
C29 C32 1.529(9) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O4 C28 1.418(8) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C7 H7 0.9500 . ?
C7 N1 1.285(7) . ?
N4 C23 1.483(6) 2_655 ?
N4 C23 1.483(6) 3_665 ?
N4 C23 1.483(6) . ?
N1 C22 1.461(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.511(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
O5 H5A 0.8497 . ?
O5 H5B 0.8501 . ?
O6 H6A 0.8500 . ?
O6 H6B 0.8439 . ?
O7 H7A 0.8503 . ?
O7 H7B 0.8492 . ?

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 O1 94.45(15) 3_665 2_655 ?
O1 Yb1 O1 94.45(15) 3_665 . ?
O1 Yb1 O1 94.45(15) 2_655 . ?
O1 Yb1 N4 122.05(11) 2_655 . ?
O1 Yb1 N4 122.05(11) . . ?
O1 Yb1 N4 122.05(11) 3_665 . ?
O1 Yb1 N1 85.21(15) 3_665 2_655 ?
O1 Yb1 N1 167.09(15) . 2_655 ?
O1 Yb1 N1 72.73(15) 2_655 2_655 ?
O1 Yb1 N1 72.73(15) . . ?
O1 Yb1 N1 72.73(15) 3_665 3_665 ?
O1 Yb1 N1 85.21(15) 2_655 . ?
O1 Yb1 N1 167.09(15) 3_665 . ?
O1 Yb1 N1 167.09(15) 2_655 3_665 ?
O1 Yb1 N1 85.21(15) . 3_665 ?
N1 Yb1 N4 68.08(11) 2_655 . ?
N1 Yb1 N4 68.08(10) . . ?
N1 Yb1 N4 68.08(10) 3_665 . ?
N1 Yb1 N1 106.91(11) 3_665 . ?
N1 Yb1 N1 106.91(11) 3_665 2_655 ?
N1 Yb1 N1 106.91(11) 2_655 . ?
C1 O1 Yb1 144.5(3) . . ?
C1 C6 C29 120.1(5) . . ?
C5 C6 C1 119.3(5) . . ?
C5 C6 C29 120.5(5) . . ?
O1 C1 C6 121.6(5) . . ?
O1 C1 C2 120.9(5) . . ?
C6 C1 C2 117.4(5) . . ?
C4 C3 H3 119.7 . . ?
C4 C3 C2 120.5(5) . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 119.2(6) . . ?
C3 C4 O4 116.8(5) . . ?
O4 C4 C5 124.0(6) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 C6 122.2(5) . . ?
C4 C5 H5 118.9 . . ?
C1 C2 C7 121.6(5) . . ?
C3 C2 C1 121.3(5) . . ?
C3 C2 C7 116.7(5) . . ?
C6 C29 C31 112.5(5) . . ?
C6 C29 C30 110.5(5) . . ?
C30 C29 C31 108.0(6) . . ?
C32 C29 C6 108.4(5) . . ?
C32 C29 C31 107.1(6) . . ?
C32 C29 C30 110.3(6) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C4 O4 C28 117.2(5) . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C2 C7 H7 116.5 . . ?
N1 C7 C2 127.1(5) . . ?
N1 C7 H7 116.5 . . ?
C23 N4 Yb1 109.4(4) . . ?
C23 N4 Yb1 109.4(4) 3_665 . ?
C23 N4 Yb1 109.4(4) 2_655 . ?
C23 N4 C23 109.5(4) 3_665 . ?
C23 N4 C23 109.5(4) 3_665 2_655 ?
C23 N4 C23 109.5(4) 2_655 . ?
C7 N1 Yb1 130.1(4) . . ?
C7 N1 C22 116.7(5) . . ?
C22 N1 Yb1 113.2(3) . . ?
N1 C22 H22A 110.2 . . ?
N1 C22 H22B 110.2 . . ?
N1 C22 C23 107.4(4) . . ?
H22A C22 H22B 108.5 . . ?
C23 C22 H22A 110.2 . . ?
C23 C22 H22B 110.2 . . ?
N4 C23 C22 110.7(5) . . ?
N4 C23 H23A 109.5 . . ?
N4 C23 H23B 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.1 . . ?
H5A O5 H5B 109.5 . . ?
H6A O6 H6B 106.1 . . ?
H7A O7 H7B 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C23 H23A O4 0.99 2.50 3.420(8) 155.3 4
O5 H5A O5 0.85 2.19 2.67(5) 115.7 2_765
O5 H5B O5 0.85 2.01 2.67(5) 133.4 3_675

_shelx_SHELXL_version_number     2014/7
_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_sad_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1826196'
_audit_update_record             
;
2018-02-27 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_audit_creation_date             2017-01-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H57 Er1 N4 O6, 2(H2 O)'
_chemical_formula_sum            'C42 H61 Er N4 O8'
_chemical_formula_weight         917.20
_chemical_absolute_configuration ?
_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 0.0033 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'
Er Er -0.2586 4.9576 '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'

_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      trigonal
_space_group_IT_number           159
_space_group_name_H-M_alt        'P 3 1 c'
_space_group_name_Hall           'P 3 -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   15.718(2)
_cell_length_b                   15.718(2)
_cell_length_c                   10.432(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2232.0(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23004
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.180
_cell_measurement_theta_min      3.574
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.117446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.6346 before and 0.1222 after correction.
The Ratio of minimum to maximum transmission is 0.1174.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23004
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.180
_diffrn_reflns_theta_min         3.574
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  Incoatec-Bruker-AXS-enraf-noniusKappaAPEXII
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4092
_reflns_number_total             4348
_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       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2016 (Sheldrick, 2008)'
_computing_structure_solution    ?
_refine_diff_density_max         1.533
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.117(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4348
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0303
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0412P)²+1.0361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0800
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O5(0.5) H5A(0.5) H5B(0.5) O6(0.08333) H6A(0.08333) H6B(0.08333)
 O7(0.08333) H7A(0.08333) H7B(0.08333)
5.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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 0.3333 0.6667 0.25064(4) 0.02217(9) Uani 1 3 d S TU P . .
O4 O 0.3527(4) 1.1221(3) 0.4742(4) 0.0374(9) Uani 1 1 d . U . . .
N4 N 0.3333 0.6667 -0.0102(6) 0.0192(11) Uani 1 3 d S TU P . .
O1 O 0.2794(2) 0.7514(2) 0.3579(3) 0.0246(6) Uani 1 1 d . U . . .
N1 N 0.4065(3) 0.8366(3) 0.1550(3) 0.0219(7) Uani 1 1 d . U . . .
C2 C 0.3620(3) 0.9215(3) 0.3147(4) 0.0207(7) Uani 1 1 d . U . . .
C6 C 0.2399(3) 0.8516(3) 0.4863(4) 0.0203(7) Uani 1 1 d . U . . .
C22 C 0.4489(3) 0.8430(3) 0.0270(4) 0.0251(8) Uani 1 1 d . U . . .
H22A H 0.5029 0.8300 0.0327 0.030 Uiso 1 1 calc R . . . .
H22B H 0.4736 0.9083 -0.0081 0.030 Uiso 1 1 calc R . . . .
C7 C 0.4092(3) 0.9140(3) 0.1991(4) 0.0214(7) Uani 1 1 d . U . . .
H7 H 0.4452 0.9714 0.1521 0.026 Uiso 1 1 calc R . . . .
C23 C 0.3687(3) 0.7674(3) -0.0586(4) 0.0247(8) Uani 1 1 d . U . . .
H23A H 0.3143 0.7800 -0.0619 0.030 Uiso 1 1 calc R . . . .
H23B H 0.3939 0.7731 -0.1449 0.030 Uiso 1 1 calc R . . . .
C1 C 0.2941(3) 0.8381(3) 0.3864(4) 0.0183(7) Uani 1 1 d . U . . .
C29 C 0.1573(4) 0.7627(3) 0.5549(4) 0.0243(8) Uani 1 1 d . U . . .
C3 C 0.3782(3) 1.0145(3) 0.3461(4) 0.0238(8) Uani 1 1 d . U . . .
H3 H 0.4225 1.0686 0.2982 0.029 Uiso 1 1 calc R . . . .
C4 C 0.3293(3) 1.0277(3) 0.4471(5) 0.0248(9) Uani 1 1 d . U . . .
C31 C 0.1062(4) 0.7925(5) 0.6574(5) 0.0380(12) Uani 1 1 d . U . . .
H31A H 0.1540 0.8361 0.7181 0.057 Uiso 1 1 calc GR . . . .
H31B H 0.0573 0.7348 0.7009 0.057 Uiso 1 1 calc GR . . . .
H31C H 0.0754 0.8250 0.6168 0.057 Uiso 1 1 calc GR . . . .
C30 C 0.1979(5) 0.7045(5) 0.6235(6) 0.0434(13) Uani 1 1 d . U . . .
H30A H 0.2269 0.6814 0.5618 0.065 Uiso 1 1 calc GR . . . .
H30B H 0.1454 0.6495 0.6671 0.065 Uiso 1 1 calc GR . . . .
H30C H 0.2467 0.7462 0.6846 0.065 Uiso 1 1 calc GR . . . .
C5 C 0.2595(3) 0.9455(3) 0.5157(4) 0.0237(8) Uani 1 1 d . U . . .
H5 H 0.2256 0.9544 0.5826 0.028 Uiso 1 1 calc R . . . .
C32 C 0.0804(4) 0.6990(4) 0.4547(6) 0.0359(11) Uani 1 1 d . U . . .
H32A H 0.0583 0.7379 0.4101 0.054 Uiso 1 1 calc GR . . . .
H32B H 0.0256 0.6450 0.4965 0.054 Uiso 1 1 calc GR . . . .
H32C H 0.1091 0.6743 0.3946 0.054 Uiso 1 1 calc GR . . . .
C28 C 0.2990(5) 1.1358(4) 0.5745(7) 0.0432(13) Uani 1 1 d . U . . .
H28A H 0.2304 1.1023 0.5531 0.065 Uiso 1 1 calc GR . . . .
H28B H 0.3221 1.2047 0.5848 0.065 Uiso 1 1 calc GR . . . .
H28C H 0.3083 1.1098 0.6531 0.065 Uiso 1 1 calc GR . . . .
O5 O 0.060(2) 0.943(2) 0.3494(19) 0.146(10) Uani 0.5 1 d . U . A 1
H5A H -0.0020 0.9158 0.3431 0.220 Uiso 0.5 1 d R . . A 1
H5B H 0.0859 1.0019 0.3229 0.220 Uiso 0.5 1 d R . . A 1
O6 O 0.0000 1.0000 0.27(3) 0.20(7) Uani 0.25 3 d S TU P B 2
H6A H 0.0609 1.0251 0.2863 0.296 Uiso 0.0833 1 d R . . B 2
H6B H -0.0281 0.9397 0.2905 0.296 Uiso 0.0833 1 d R . . B 2
O7 O 0.0000 1.0000 0.479(9) 0.14(3) Uani 0.25 3 d S TU P C 2
H7A H -0.0336 0.9512 0.4303 0.208 Uiso 0.0833 1 d R . . C 2
H7B H 0.0441 1.0468 0.4359 0.208 Uiso 0.0833 1 d R . . C 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
Er1 N4 2.721(7) . ?
Er1 O1 2.207(3) 3_565 ?
Er1 O1 2.207(3) . ?
Er1 O1 2.207(3) 2_665 ?
Er1 N1 2.525(4) 2_665 ?
Er1 N1 2.525(4) 3_565 ?
Er1 N1 2.525(4) . ?
O4 C4 1.368(6) . ?
O4 C28 1.428(7) . ?
N4 C23 1.479(5) 2_665 ?
N4 C23 1.479(5) . ?
N4 C23 1.479(5) 3_565 ?
O1 C1 1.298(5) . ?
N1 C22 1.473(6) . ?
N1 C7 1.282(5) . ?
C2 C7 1.450(6) . ?
C2 C1 1.421(6) . ?
C2 C3 1.393(6) . ?
C6 C1 1.428(6) . ?
C6 C29 1.529(6) . ?
C6 C5 1.382(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.517(7) . ?
C7 H7 0.9300 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C29 C31 1.544(7) . ?
C29 C30 1.529(8) . ?
C29 C32 1.531(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.379(7) . ?
C4 C5 1.403(7) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C5 H5 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
O5 H5A 0.8478 . ?
O5 H5B 0.8485 . ?
O6 H6A 0.8482 . ?
O6 H6B 0.8470 . ?
O7 H7A 0.8512 . ?
O7 H7B 0.8476 . ?

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 N4 120.46(9) 2_665 . ?
O1 Er1 N4 120.46(9) 3_565 . ?
O1 Er1 N4 120.46(9) . . ?
O1 Er1 O1 96.58(12) . 2_665 ?
O1 Er1 O1 96.58(12) 2_665 3_565 ?
O1 Er1 O1 96.58(12) . 3_565 ?
O1 Er1 N1 87.36(13) . 2_665 ?
O1 Er1 N1 167.21(13) . 3_565 ?
O1 Er1 N1 70.82(12) 2_665 2_665 ?
O1 Er1 N1 70.82(12) 3_565 3_565 ?
O1 Er1 N1 70.82(12) . . ?
O1 Er1 N1 87.36(12) 2_665 3_565 ?
O1 Er1 N1 167.21(12) 3_565 2_665 ?
O1 Er1 N1 167.21(12) 2_665 . ?
O1 Er1 N1 87.35(12) 3_565 . ?
N1 Er1 N4 66.74(8) 2_665 . ?
N1 Er1 N4 66.74(8) . . ?
N1 Er1 N4 66.74(8) 3_565 . ?
N1 Er1 N1 105.43(10) 2_665 3_565 ?
N1 Er1 N1 105.43(10) . 3_565 ?
N1 Er1 N1 105.43(10) . 2_665 ?
C4 O4 C28 117.2(5) . . ?
C23 N4 Er1 109.9(3) 3_565 . ?
C23 N4 Er1 109.9(3) 2_665 . ?
C23 N4 Er1 109.9(3) . . ?
C23 N4 C23 109.0(3) 2_665 . ?
C23 N4 C23 109.0(3) . 3_565 ?
C23 N4 C23 109.0(3) 2_665 3_565 ?
C1 O1 Er1 146.1(3) . . ?
C22 N1 Er1 112.4(3) . . ?
C7 N1 Er1 130.0(3) . . ?
C7 N1 C22 117.5(4) . . ?
C1 C2 C7 122.8(4) . . ?
C3 C2 C7 116.7(4) . . ?
C3 C2 C1 120.2(4) . . ?
C1 C6 C29 120.2(4) . . ?
C5 C6 C1 119.3(4) . . ?
C5 C6 C29 120.4(4) . . ?
N1 C22 H22A 110.1 . . ?
N1 C22 H22B 110.1 . . ?
N1 C22 C23 108.1(3) . . ?
H22A C22 H22B 108.4 . . ?
C23 C22 H22A 110.1 . . ?
C23 C22 H22B 110.1 . . ?
N1 C7 C2 126.9(4) . . ?
N1 C7 H7 116.6 . . ?
C2 C7 H7 116.6 . . ?
N4 C23 C22 110.9(4) . . ?
N4 C23 H23A 109.4 . . ?
N4 C23 H23B 109.4 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 108.0 . . ?
O1 C1 C2 120.3(4) . . ?
O1 C1 C6 121.2(4) . . ?
C2 C1 C6 118.4(4) . . ?
C6 C29 C31 112.3(4) . . ?
C6 C29 C32 108.0(4) . . ?
C30 C29 C6 110.4(4) . . ?
C30 C29 C31 107.0(5) . . ?
C30 C29 C32 111.0(5) . . ?
C32 C29 C31 108.1(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 C2 121.0(4) . . ?
C4 C3 H3 119.5 . . ?
O4 C4 C3 116.9(4) . . ?
O4 C4 C5 123.7(4) . . ?
C3 C4 C5 119.3(4) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C6 C5 C4 121.6(4) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H5A O5 H5B 109.3 . . ?
H6A O6 H6B 108.0 . . ?
H7A O7 H7B 109.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C23 H23A O4 0.97 2.50 3.408(7) 155.2 5_674
O5 H5A O5 0.85 2.02 2.75(3) 144.0 3_465
O5 H5B O5 0.85 2.09 2.75(3) 134.7 2_675

_shelx_SHELXL_version_number     2014/7
_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_sad2_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1826197'
_audit_update_record             
;
2018-02-27 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_audit_creation_date             2017-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H57 Lu1 N4 O6, 2(H2 O)'
_chemical_formula_sum            'C42 H61 Lu N4 O8'
_chemical_formula_weight         924.91
_chemical_absolute_configuration ?
_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 0.0033 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'
Lu Lu -0.4720 5.8584 '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'

_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      trigonal
_space_group_IT_number           159
_space_group_name_H-M_alt        'P 3 1 c'
_space_group_name_Hall           'P 3 -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   15.719(2)
_cell_length_b                   15.719(2)
_cell_length_c                   10.477(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2242.0(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    22307
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.569
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.253
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.506215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1924 before and 0.0807 after correction.
The Ratio of minimum to maximum transmission is 0.5062.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             952
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22307
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         3.569
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                2917
_reflns_number_total             3070
_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       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    ?
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.031(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0205
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0198P)²+0.9957P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0533
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Fixed Sof: O5(0.5) H5A(0.5) H5B(0.5) O6(0.08333) H6A(0.08333) H6B(0.08333)
 O7(0.08333) H7A(0.08333) H7B(0.08333)
5.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Lu1 Lu 0.3333 0.6667 0.24979(5) 0.02335(8) Uani 1 3 d S TU P . .
O4 O 0.3536(3) 1.1162(3) 0.4844(4) 0.0486(10) Uani 1 1 d . U . . .
N4 N 0.3333 0.6667 -0.0033(6) 0.0277(13) Uani 1 3 d S TU P . .
O1 O 0.2789(2) 0.7441(2) 0.3595(3) 0.0286(6) Uani 1 1 d . U . . .
N1 N 0.4085(3) 0.8323(3) 0.1620(4) 0.0278(7) Uani 1 1 d . U . . .
C2 C 0.3640(3) 0.9163(3) 0.3228(4) 0.0253(8) Uani 1 1 d . U . . .
C6 C 0.2414(3) 0.8441(3) 0.4919(4) 0.0270(8) Uani 1 1 d . U . . .
C22 C 0.4515(4) 0.8414(4) 0.0358(4) 0.0334(10) Uani 1 1 d . U . . .
H22A H 0.5058 0.8268 0.0402 0.040 Uiso 1 1 calc R . . . .
H22B H 0.4780 0.9091 0.0029 0.040 Uiso 1 1 calc R . . . .
C7 C 0.4118(3) 0.9094(3) 0.2081(4) 0.0279(8) Uani 1 1 d . U . . .
H7 H 0.4500 0.9687 0.1620 0.033 Uiso 1 1 calc R . . . .
C23 C 0.3709(4) 0.7687(3) -0.0510(4) 0.0321(9) Uani 1 1 d . U . . .
H23A H 0.3166 0.7833 -0.0538 0.039 Uiso 1 1 calc R . . . .
H23B H 0.3968 0.7747 -0.1387 0.039 Uiso 1 1 calc R . . . .
C1 C 0.2950(3) 0.8309(3) 0.3918(4) 0.0238(8) Uani 1 1 d . U . . .
C29 C 0.1587(4) 0.7541(4) 0.5588(5) 0.0323(9) Uani 1 1 d . U . . .
C3 C 0.3803(3) 1.0096(3) 0.3554(4) 0.0307(9) Uani 1 1 d . U . . .
H3 H 0.4259 1.0653 0.3077 0.037 Uiso 1 1 calc R . . . .
C4 C 0.3307(3) 1.0213(3) 0.4563(5) 0.0323(10) Uani 1 1 d . U . . .
C31 C 0.1094(5) 0.7828(5) 0.6644(6) 0.0519(15) Uani 1 1 d . U . . .
H31A H 0.1586 0.8238 0.7280 0.078 Uiso 1 1 calc GR . . . .
H31B H 0.0577 0.7233 0.7055 0.078 Uiso 1 1 calc GR . . . .
H31C H 0.0804 0.8196 0.6267 0.078 Uiso 1 1 calc GR . . . .
C30 C 0.1973(5) 0.6913(5) 0.6195(6) 0.0537(15) Uani 1 1 d . U . . .
H30A H 0.2256 0.6690 0.5531 0.081 Uiso 1 1 calc GR . . . .
H30B H 0.1432 0.6343 0.6616 0.081 Uiso 1 1 calc GR . . . .
H30C H 0.2480 0.7306 0.6826 0.081 Uiso 1 1 calc GR . . . .
C5 C 0.2618(3) 0.9383(4) 0.5232(5) 0.0313(9) Uani 1 1 d . U . . .
H5 H 0.2278 0.9466 0.5927 0.038 Uiso 1 1 calc R . . . .
C32 C 0.0794(4) 0.6939(5) 0.4595(6) 0.0457(13) Uani 1 1 d . U . . .
H32A H 0.0583 0.7359 0.4174 0.069 Uiso 1 1 calc GR . . . .
H32B H 0.0230 0.6392 0.5020 0.069 Uiso 1 1 calc GR . . . .
H32C H 0.1062 0.6680 0.3957 0.069 Uiso 1 1 calc GR . . . .
C28 C 0.2975(5) 1.1284(4) 0.5822(6) 0.0519(15) Uani 1 1 d . U . . .
H28A H 0.2277 1.0917 0.5596 0.078 Uiso 1 1 calc GR . . . .
H28B H 0.3186 1.1982 0.5910 0.078 Uiso 1 1 calc GR . . . .
H28C H 0.3078 1.1035 0.6631 0.078 Uiso 1 1 calc GR . . . .
O5 O 0.0577(15) 0.9417(18) 0.3545(15) 0.146(7) Uani 0.5 1 d . U . A 1
H5A H 0.0005 0.9004 0.3288 0.219 Uiso 0.5 1 d R . . A 1
H5B H 0.0773 0.9959 0.3161 0.219 Uiso 0.5 1 d R . . A 1
O6 O 0.0000 1.0000 0.308(5) 0.156(18) Uani 0.25 3 d S TU P B 2
H6A H 0.0595 1.0181 0.2911 0.233 Uiso 0.0833 1 d R . . B 2
H6B H -0.0330 0.9837 0.2394 0.233 Uiso 0.0833 1 d R . . B 2
O7 O 0.0000 1.0000 0.464(6) 0.19(3) Uani 0.25 3 d S TU P C 3
H7A H 0.0376 1.0582 0.4382 0.282 Uiso 0.0833 1 d R . . C 3
H7B H -0.0239 0.9649 0.3978 0.282 Uiso 0.0833 1 d R . . C 3


_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
Lu1 N4 2.652(7) . ?
Lu1 O1 2.139(3) 3_565 ?
Lu1 O1 2.139(3) . ?
Lu1 O1 2.139(3) 2_665 ?
Lu1 N1 2.438(4) . ?
Lu1 N1 2.438(4) 3_565 ?
Lu1 N1 2.438(4) 2_665 ?
O4 C4 1.381(6) . ?
O4 C28 1.425(7) . ?
N4 C23 1.491(5) . ?
N4 C23 1.491(5) 2_665 ?
N4 C23 1.491(5) 3_565 ?
O1 C1 1.302(5) . ?
N1 C22 1.460(6) . ?
N1 C7 1.281(6) . ?
C2 C7 1.451(6) . ?
C2 C1 1.430(6) . ?
C2 C3 1.398(6) . ?
C6 C1 1.424(6) . ?
C6 C29 1.531(6) . ?
C6 C5 1.388(6) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.513(7) . ?
C7 H7 0.9500 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C29 C31 1.543(7) . ?
C29 C30 1.532(8) . ?
C29 C32 1.534(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.380(7) . ?
C4 C5 1.397(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C5 H5 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O5 H5A 0.8474 . ?
O5 H5B 0.8490 . ?
O6 H6A 0.8490 . ?
O6 H6B 0.8497 . ?
O7 H7A 0.8471 . ?
O7 H7B 0.8463 . ?

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 Lu1 N4 122.51(9) 2_665 . ?
O1 Lu1 N4 122.51(9) 3_565 . ?
O1 Lu1 N4 122.51(9) . . ?
O1 Lu1 O1 93.83(12) . 2_665 ?
O1 Lu1 O1 93.83(12) 2_665 3_565 ?
O1 Lu1 O1 93.83(12) . 3_565 ?
O1 Lu1 N1 73.34(12) . . ?
O1 Lu1 N1 167.05(12) . 3_565 ?
O1 Lu1 N1 167.05(12) 2_665 . ?
O1 Lu1 N1 73.34(12) 3_565 3_565 ?
O1 Lu1 N1 85.44(12) . 2_665 ?
O1 Lu1 N1 85.43(12) 2_665 3_565 ?
O1 Lu1 N1 85.44(12) 3_565 . ?
O1 Lu1 N1 73.34(12) 2_665 2_665 ?
O1 Lu1 N1 167.05(12) 3_565 2_665 ?
N1 Lu1 N4 67.83(9) . . ?
N1 Lu1 N4 67.83(9) 2_665 . ?
N1 Lu1 N4 67.83(9) 3_565 . ?
N1 Lu1 N1 106.65(10) . 3_565 ?
N1 Lu1 N1 106.65(10) 2_665 3_565 ?
N1 Lu1 N1 106.65(10) 2_665 . ?
C4 O4 C28 117.0(4) . . ?
C23 N4 Lu1 109.6(3) 3_565 . ?
C23 N4 Lu1 109.6(3) . . ?
C23 N4 Lu1 109.6(3) 2_665 . ?
C23 N4 C23 109.4(3) . 2_665 ?
C23 N4 C23 109.4(3) 2_665 3_565 ?
C23 N4 C23 109.4(3) . 3_565 ?
C1 O1 Lu1 144.4(3) . . ?
C22 N1 Lu1 113.6(3) . . ?
C7 N1 Lu1 129.6(3) . . ?
C7 N1 C22 116.8(4) . . ?
C1 C2 C7 121.8(4) . . ?
C3 C2 C7 116.8(4) . . ?
C3 C2 C1 121.1(4) . . ?
C1 C6 C29 119.5(4) . . ?
C5 C6 C1 119.4(4) . . ?
C5 C6 C29 120.9(4) . . ?
N1 C22 H22A 110.2 . . ?
N1 C22 H22B 110.2 . . ?
N1 C22 C23 107.3(4) . . ?
H22A C22 H22B 108.5 . . ?
C23 C22 H22A 110.2 . . ?
C23 C22 H22B 110.2 . . ?
N1 C7 C2 127.3(4) . . ?
N1 C7 H7 116.4 . . ?
C2 C7 H7 116.4 . . ?
N4 C23 C22 110.1(4) . . ?
N4 C23 H23A 109.6 . . ?
N4 C23 H23B 109.6 . . ?
C22 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
H23A C23 H23B 108.2 . . ?
O1 C1 C2 120.7(4) . . ?
O1 C1 C6 121.7(4) . . ?
C6 C1 C2 117.4(4) . . ?
C6 C29 C31 112.1(4) . . ?
C6 C29 C30 111.0(4) . . ?
C6 C29 C32 108.2(4) . . ?
C30 C29 C31 108.1(5) . . ?
C30 C29 C32 110.2(5) . . ?
C32 C29 C31 107.1(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3 119.8 . . ?
O4 C4 C5 124.3(4) . . ?
C3 C4 O4 116.6(4) . . ?
C3 C4 C5 119.1(4) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C6 C5 C4 122.4(4) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H5A O5 H5B 109.3 . . ?
H6A O6 H6B 109.0 . . ?
H7A O7 H7B 106.7 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C23 H23A O4 0.99 2.48 3.408(7) 155.2 5_674
O5 H5A O5 0.85 2.25 2.74(3) 116.4 3_465
O5 H5B O5 0.85 2.09 2.74(3) 132.2 2_675

_shelx_SHELXL_version_number     2014/7
_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_sad_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1826200'
_audit_update_record             
;
2018-02-27 deposited with the CCDC.
2018-06-20 downloaded from the CCDC.
;
_audit_creation_date             2017-01-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H57 N4 O6 Tb1, 2(H2 O)'
_chemical_formula_sum            'C42 H61 N4 O8 Tb'
_chemical_formula_weight         908.86
_chemical_absolute_configuration ?
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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      trigonal
_space_group_IT_number           159
_space_group_name_H-M_alt        'P 3 1 c'
_space_group_name_Hall           'P 3 -2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'

_cell_length_a                   15.772(2)
_cell_length_b                   15.772(2)
_cell_length_c                   10.385(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2237.2(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    24263
_cell_measurement_temperature    200
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.583
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.632
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.595844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1074 before and 0.0581 after correction.
The Ratio of minimum to maximum transmission is 0.5958.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            24263
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         2.583
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                3786
_reflns_number_total             4181
_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       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 
;
 Flack x determined using 1677 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         4181
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0254P)²+0.1124P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0622
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(O6) = Uanis(O7)
4. Others
 Fixed Sof: O5(0.5) H5A(0.5) H5B(0.5) O7(0.08333) H7A(0.08333) H7B(0.08333)
 O6(0.08333) H6A(0.08333) H6B(0.08333)
5.a Riding coordinates:
 O5(H5A,H5B), O7(H7A,H7B), O6(H6A,H6B)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C5(H5)
5.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C28(H28A,H28B,
 H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Tb1 Tb 0.6667 0.3333 0.74971(3) 0.02234(8) Uani 1 3 d S TU P . .
O4 O 0.2316(3) 0.3524(3) 0.5227(3) 0.0438(9) Uani 1 1 d . U . . .
N4 N 0.6667 0.3333 1.0078(6) 0.0257(12) Uani 1 3 d S TU P . .
O1 O 0.5302(2) 0.2796(2) 0.6415(3) 0.0290(6) Uani 1 1 d . U . . .
N1 N 0.5712(3) 0.4070(2) 0.8427(3) 0.0264(7) Uani 1 1 d . U . . .
C2 C 0.4418(3) 0.3620(3) 0.6826(3) 0.0248(8) Uani 1 1 d . U . . .
C6 C 0.3899(3) 0.2400(3) 0.5119(3) 0.0248(8) Uani 1 1 d . U . . .
C22 C 0.6070(3) 0.4496(3) 0.9707(4) 0.0308(9) Uani 1 1 d . U . . .
H22A H 0.5671 0.4750 1.0055 0.037 Uiso 1 1 calc R . . . .
H22B H 0.6742 0.5029 0.9652 0.037 Uiso 1 1 calc R . . . .
C7 C 0.4973(3) 0.4100(3) 0.7981(3) 0.0259(8) Uani 1 1 d . U . . .
H7 H 0.4768 0.4470 0.8445 0.031 Uiso 1 1 calc R . . . .
C23 C 0.6008(3) 0.3686(3) 1.0566(4) 0.0294(8) Uani 1 1 d . U . . .
H23A H 0.6194 0.3930 1.1437 0.035 Uiso 1 1 calc R . . . .
H23B H 0.5338 0.3146 1.0585 0.035 Uiso 1 1 calc R . . . .
C1 C 0.4583(3) 0.2943(3) 0.6120(3) 0.0245(7) Uani 1 1 d . U . . .
C29 C 0.3980(4) 0.1580(3) 0.4431(4) 0.0303(9) Uani 1 1 d . U . . .
C3 C 0.3652(3) 0.3782(3) 0.6512(4) 0.0301(8) Uani 1 1 d . U . . .
H3 H 0.3556 0.4225 0.6991 0.036 Uiso 1 1 calc R . . . .
C4 C 0.3034(3) 0.3292(3) 0.5499(4) 0.0300(9) Uani 1 1 d . U . . .
C31 C 0.3171(4) 0.1071(4) 0.3400(4) 0.0453(13) Uani 1 1 d . U . . .
H31A H 0.3228 0.1544 0.2773 0.068 Uiso 1 1 calc GR . . . .
H31B H 0.2540 0.0786 0.3804 0.068 Uiso 1 1 calc GR . . . .
H31C H 0.3243 0.0567 0.2983 0.068 Uiso 1 1 calc GR . . . .
C32 C 0.4973(4) 0.1977(4) 0.3773(5) 0.0494(13) Uani 1 1 d . U . . .
H32A H 0.5483 0.2251 0.4409 0.074 Uiso 1 1 calc GR . . . .
H32B H 0.5065 0.2476 0.3167 0.074 Uiso 1 1 calc GR . . . .
H32C H 0.4996 0.1455 0.3329 0.074 Uiso 1 1 calc GR . . . .
C5 C 0.3165(3) 0.2599(3) 0.4821(4) 0.0290(9) Uani 1 1 d . U . . .
H5 H 0.2741 0.2262 0.4147 0.035 Uiso 1 1 calc R . . . .
C30 C 0.3826(4) 0.0794(4) 0.5433(5) 0.0420(11) Uani 1 1 d . U . . .
H30A H 0.3202 0.0556 0.5844 0.063 Uiso 1 1 calc GR . . . .
H30B H 0.4336 0.1075 0.6068 0.063 Uiso 1 1 calc GR . . . .
H30C H 0.3843 0.0261 0.5011 0.063 Uiso 1 1 calc GR . . . .
C28 C 0.1636(4) 0.2973(4) 0.4232(5) 0.0482(12) Uani 1 1 d . U . . .
H28A H 0.1328 0.2288 0.4430 0.072 Uiso 1 1 calc GR . . . .
H28B H 0.1976 0.3097 0.3426 0.072 Uiso 1 1 calc GR . . . .
H28C H 0.1147 0.3164 0.4171 0.072 Uiso 1 1 calc GR . . . .
O5 O 0.1147(9) 0.0592(10) 0.6461(10) 0.140(6) Uani 0.5 1 d . U . A 1
H5A H 0.1535 0.0493 0.6002 0.210 Uiso 0.5 1 d R . . A 1
H5B H 0.0637 0.0049 0.6631 0.210 Uiso 0.5 1 d R . . A 1
O7 O 0.0000 0.0000 0.301(3) 0.139(13) Uani 0.25 3 d S TU P B 2
H7A H 0.0572 0.0104 0.2847 0.208 Uiso 0.0833 1 d R . . B 2
H7B H -0.0262 0.0054 0.2323 0.208 Uiso 0.0833 1 d R . . B 2
O6 O 0.0000 0.0000 0.520(5) 0.139(13) Uani 0.25 3 d S TU P C 2
H6A H 0.0266 -0.0204 0.5738 0.208 Uiso 0.0833 1 d R . . C 2
H6B H -0.0173 0.0366 0.5588 0.208 Uiso 0.0833 1 d R . . C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 N4 2.680(6) . ?
Tb1 O1 2.188(3) 3_665 ?
Tb1 O1 2.188(3) 2_655 ?
Tb1 O1 2.188(3) . ?
Tb1 N1 2.509(3) 3_665 ?
Tb1 N1 2.509(3) . ?
Tb1 N1 2.509(3) 2_655 ?
O4 C4 1.382(5) . ?
O4 C28 1.429(6) . ?
N4 C23 1.491(5) 2_655 ?
N4 C23 1.491(5) 3_665 ?
N4 C23 1.491(5) . ?
O1 C1 1.304(5) . ?
N1 C22 1.469(5) . ?
N1 C7 1.276(5) . ?
C2 C7 1.455(5) . ?
C2 C1 1.422(5) . ?
C2 C3 1.392(6) . ?
C6 C1 1.433(5) . ?
C6 C29 1.537(6) . ?
C6 C5 1.379(6) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 C23 1.521(6) . ?
C7 H7 0.9300 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C29 C31 1.548(6) . ?
C29 C32 1.526(7) . ?
C29 C30 1.542(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.378(6) . ?
C4 C5 1.399(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C5 H5 0.9300 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
O5 H5A 0.8507 . ?
O5 H5B 0.8503 . ?
O7 H7A 0.8494 . ?
O7 H7B 0.8501 . ?
O6 H6A 0.8498 . ?
O6 H6B 0.8500 . ?

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 Tb1 N4 120.90(7) . . ?
O1 Tb1 N4 120.90(7) 3_665 . ?
O1 Tb1 N4 120.90(7) 2_655 . ?
O1 Tb1 O1 95.99(10) 2_655 . ?
O1 Tb1 O1 95.99(10) . 3_665 ?
O1 Tb1 O1 95.99(10) 2_655 3_665 ?
O1 Tb1 N1 86.72(11) 2_655 3_665 ?
O1 Tb1 N1 167.01(11) 2_655 . ?
O1 Tb1 N1 167.01(11) . 3_665 ?
O1 Tb1 N1 86.72(11) 3_665 . ?
O1 Tb1 N1 71.07(10) 2_655 2_655 ?
O1 Tb1 N1 71.07(10) . . ?
O1 Tb1 N1 71.07(10) 3_665 3_665 ?
O1 Tb1 N1 86.72(11) . 2_655 ?
O1 Tb1 N1 167.02(11) 3_665 2_655 ?
N1 Tb1 N4 67.37(7) 3_665 . ?
N1 Tb1 N4 67.37(7) 2_655 . ?
N1 Tb1 N4 67.37(7) . . ?
N1 Tb1 N1 106.14(8) 3_665 . ?
N1 Tb1 N1 106.14(8) 2_655 . ?
N1 Tb1 N1 106.14(8) 2_655 3_665 ?
C4 O4 C28 116.9(4) . . ?
C23 N4 Tb1 109.9(3) . . ?
C23 N4 Tb1 109.9(3) 2_655 . ?
C23 N4 Tb1 109.9(3) 3_665 . ?
C23 N4 C23 109.1(3) 2_655 3_665 ?
C23 N4 C23 109.1(3) 3_665 . ?
C23 N4 C23 109.1(3) 2_655 . ?
C1 O1 Tb1 145.8(3) . . ?
C22 N1 Tb1 112.2(2) . . ?
C7 N1 Tb1 130.4(3) . . ?
C7 N1 C22 117.4(3) . . ?
C1 C2 C7 121.8(3) . . ?
C3 C2 C7 116.7(4) . . ?
C3 C2 C1 121.2(4) . . ?
C1 C6 C29 119.1(4) . . ?
C5 C6 C1 119.5(4) . . ?
C5 C6 C29 121.4(4) . . ?
N1 C22 H22A 110.3 . . ?
N1 C22 H22B 110.3 . . ?
N1 C22 C23 107.3(3) . . ?
H22A C22 H22B 108.5 . . ?
C23 C22 H22A 110.3 . . ?
C23 C22 H22B 110.3 . . ?
N1 C7 C2 127.1(4) . . ?
N1 C7 H7 116.5 . . ?
C2 C7 H7 116.5 . . ?
N4 C23 C22 110.5(3) . . ?
N4 C23 H23A 109.6 . . ?
N4 C23 H23B 109.6 . . ?
C22 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
O1 C1 C2 121.0(3) . . ?
O1 C1 C6 121.7(4) . . ?
C2 C1 C6 117.2(4) . . ?
C6 C29 C31 111.3(4) . . ?
C6 C29 C30 108.5(3) . . ?
C32 C29 C6 111.2(4) . . ?
C32 C29 C31 108.3(4) . . ?
C32 C29 C30 110.5(4) . . ?
C30 C29 C31 107.0(4) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 C2 120.8(4) . . ?
C4 C3 H3 119.6 . . ?
O4 C4 C5 124.4(4) . . ?
C3 C4 O4 116.8(4) . . ?
C3 C4 C5 118.8(4) . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C6 C5 C4 122.3(4) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O4 C28 H28A 109.5 . . ?
O4 C28 H28B 109.5 . . ?
O4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H5A O5 H5B 109.5 . . ?
H7A O7 H7B 109.5 . . ?
H6A O6 H6B 109.6 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C23 H23B O4 0.97 2.51 3.416(6) 155.7 4
O5 H5B O5 0.85 1.89 2.71(2) 162.5 3
O7 H7B O6 0.85 2.25 2.92(7) 135.4 4_554
O6 H6A O7 0.85 2.45 2.92(7) 115.6 4

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
