# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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 
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data_p-31c_c_sq
_database_code_depnum_ccdc_archive 'CCDC 1515527'
_audit_update_record             
;
2017-08-18 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_audit_creation_date             2017-08-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'1(C39 H54 Gd1 N7 O3), 1(C39 H51 Gd1 N7 O3), 4(H2O)'
_chemical_formula_sum            'C78 H113 Gd2 N14 O10'
_chemical_formula_weight         1721.3385
_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'
Gd Gd -0.1653 3.9035 '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           150
_space_group_name_H-M_alt        'P 3 2 1'
_space_group_name_Hall           'P 3 2"'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'

_cell_length_a                   12.3620(18)
_cell_length_b                   12.3620(18)
_cell_length_c                   31.321(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4145.2(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2.6
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1694
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            56365
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.244
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         1.902
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'ADSC Q315r CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Australian Synchrotron'
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                34880
_reflns_number_total             56365
_reflns_special_details          
;
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       Shelxl
_computing_data_collection       'Blue Ice'
_computing_data_reduction        XDS
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         2.765
_refine_diff_density_min         -3.129
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details 
;
 Flack x determined using 1417 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         56365
_refine_ls_number_restraints     315
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0762
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0782P)²+32.7586P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.2115
_refine_special_details          ?
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 1
 0
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N3A-C2 = N3A-C13A
 1.48 with sigma of 0.02
 C14A-C13A = C2-C1
 1.52 with sigma of 0.02
 C11A-C0AA \\sim C12A-C11A
 with sigma of 0.02
 C2-C1 \\sim C14A-C13A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C13A)
Uanis(C14A) = Uanis(C1)
Uanis(C5B) = Uanis(O1B)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C1(0.6) H1A(0.6) H1B(0.6) H1C(0.6) C2(0.6) H2A(0.6) H2B(0.6)
 H11A(0.35) H11B(0.35) H11C(0.65) H11D(0.65) C12A(0.35) H12A(0.35) H12B(0.35)
 H12C(0.35) C13A(0.4) H13A(0.4) H13B(0.4) C14A(0.4) H14A(0.4) H14B(0.4)
 H14C(0.4) C0AA(0.65) H0AA(0.65) H0AB(0.65) H0AC(0.65)
 Fixed Uiso: H14A(0.07) H14B(0.07) H14C(0.07)
 Fixed X: H14A(1.04368) H14B(0.940949) H14C(0.95879)
 Fixed Y: H14A(0.63505) H14B(0.52063) H14C(0.65721)
 Fixed Z: H14A(0.20938) H14B(0.236909) H14C(0.24282)
7.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C2A(H2AA,H2AB), C2(H2A,H2B), C11A(H11A,H11B), C11A(H11C,H11D),
  C13A(H13A,H13B), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C11B(H11E,H11F), C13B(H13C,
 H13D)
7.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C5A(H5A), C6A(H6A), C8A(H8A), C3B(H3B), C6B(H6B), C8B(H8B), C9B(H9B)
7.c X=CH2 refined with riding coordinates:
 C12B(H12D,H12E)
7.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C12A(H12A,H12B,H12C), C14B(H14D,H14E,H14F), C0AA(H0AA,H0AB,
 H0AC)
;
_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
Gd1A Gd 1.3333 0.6667 0.03399(6) 0.0523(5) Uani 1 3 d S TU P . .
O1A O 1.1747(17) 0.6438(17) 0.0735(6) 0.057(4) Uani 1 1 d . U . . .
N1A N 1.3333 0.6667 -0.0560(13) 0.072(9) Uani 1 3 d S TU P . .
N2A N 1.264(2) 0.8077(19) 0.0025(6) 0.056(5) Uani 1 1 d . U . . .
N3A N 0.872(3) 0.672(3) 0.1611(8) 0.072(7) Uani 1 1 d D U . . .
C1A C 1.284(3) 0.747(3) -0.0690(8) 0.069(8) Uani 1 1 d . U . . .
H1AA H 1.1913 0.6975 -0.0698 0.082 Uiso 1 1 calc R . . . .
H1AB H 1.3132 0.7790 -0.0982 0.082 Uiso 1 1 calc R . . . .
C1 C 0.833(4) 0.483(3) 0.1980(12) 0.063(8) Uani 0.6 1 d D U . A 1
H1A H 0.8379 0.4592 0.1685 0.094 Uiso 0.6 1 calc GR . . A 1
H1B H 0.7462 0.4593 0.2045 0.094 Uiso 0.6 1 calc GR . . A 1
H1C H 0.8607 0.4402 0.2176 0.094 Uiso 0.6 1 calc GR . . A 1
C2A C 1.323(3) 0.856(3) -0.0394(8) 0.065(7) Uani 1 1 d . U . . .
H2AA H 1.4147 0.9029 -0.0365 0.078 Uiso 1 1 calc R . . . .
H2AB H 1.2956 0.9133 -0.0510 0.078 Uiso 1 1 calc R . . . .
C2 C 0.919(4) 0.629(3) 0.2032(12) 0.059(8) Uani 0.6 1 d D U . A 1
H2A H 1.0091 0.6557 0.2016 0.071 Uiso 0.6 1 calc R . . A 1
H2B H 0.9018 0.6603 0.2299 0.071 Uiso 0.6 1 calc R . . A 1
C3A C 1.187(4) 0.836(3) 0.0145(7) 0.055(7) Uani 1 1 d . U . . .
H3A H 1.1766 0.8926 -0.0029 0.066 Uiso 1 1 calc R . . . .
C4A C 1.107(2) 0.788(2) 0.0543(8) 0.050(5) Uani 1 1 d . U . . .
C5A C 1.031(3) 0.835(3) 0.0633(9) 0.061(7) Uani 1 1 d . U . . .
H5A H 1.0288 0.8917 0.0434 0.074 Uiso 1 1 calc R . . . .
C6A C 0.955(3) 0.806(2) 0.1001(8) 0.058(6) Uani 1 1 d . U . . .
H6A H 0.9087 0.8458 0.1064 0.070 Uiso 1 1 calc R . . . .
C8A C 1.033(3) 0.663(3) 0.1185(9) 0.065(7) Uani 1 1 d . U . . .
H8A H 1.0360 0.6064 0.1382 0.079 Uiso 1 1 calc R . . . .
C9A C 1.105(2) 0.697(2) 0.0822(8) 0.052(5) Uani 1 1 d . U . . .
C10A C 0.954(3) 0.714(3) 0.1267(9) 0.065(7) Uani 1 1 d . U . . .
C11A C 0.803(3) 0.736(3) 0.1733(9) 0.067(7) Uani 1 1 d D U . . .
H11A H 0.7679 0.7484 0.1465 0.080 Uiso 0.35 1 calc R . . B 1
H11B H 0.7308 0.6755 0.1906 0.080 Uiso 0.35 1 calc R . . B 1
H11C H 0.8573 0.8256 0.1663 0.080 Uiso 0.65 1 calc R . . C 2
H11D H 0.7945 0.7307 0.2048 0.080 Uiso 0.65 1 calc R . . C 2
C12A C 0.857(6) 0.856(5) 0.1965(18) 0.056(15) Uani 0.35 1 d D U . D 1
H12A H 0.9074 0.8544 0.2205 0.084 Uiso 0.35 1 calc GR . . D 1
H12B H 0.7900 0.8685 0.2073 0.084 Uiso 0.35 1 calc GR . . D 1
H12C H 0.9104 0.9243 0.1771 0.084 Uiso 0.35 1 calc GR . . D 1
C13A C 0.856(6) 0.566(6) 0.1839(19) 0.059(8) Uani 0.4 1 d D U . A 2
H13A H 0.8602 0.5072 0.1636 0.071 Uiso 0.4 1 calc R . . A 2
H13B H 0.7708 0.5235 0.1966 0.071 Uiso 0.4 1 calc R . . A 2
C14A C 0.955(7) 0.596(6) 0.221(2) 0.063(8) Uani 0.4 1 d D U . A 2
H14A H 1.0437 0.6350 0.2094 0.070 Uiso 0.4 1 d . . . E 2
H14B H 0.9409 0.5206 0.2369 0.070 Uiso 0.4 1 d . . . F 2
H14C H 0.9588 0.6572 0.2428 0.070 Uiso 0.4 1 d . . . G 2
Gd1B Gd 0.6667 0.3333 0.46625(6) 0.0305(3) Uani 1 3 d S TU P . .
O1B O 0.6441(12) 0.4718(12) 0.4254(5) 0.036(3) Uani 1 1 d . U . . .
N1B N 0.6667 0.3333 0.5537(7) 0.029(4) Uani 1 3 d S TU P . .
N2B N 0.8032(13) 0.5402(14) 0.4984(6) 0.032(4) Uani 1 1 d . U . . .
N3B N 0.685(3) 0.797(2) 0.3345(8) 0.084(9) Uani 1 1 d . U . . .
C1B C 0.750(2) 0.4627(17) 0.5706(6) 0.035(6) Uani 1 1 d . U . . .
H1BA H 0.7829 0.4576 0.5988 0.042 Uiso 1 1 calc R . . . .
H1BB H 0.7003 0.5050 0.5745 0.042 Uiso 1 1 calc R . . . .
C2B C 0.8577(17) 0.5388(17) 0.5403(7) 0.035(4) Uani 1 1 d . U . . .
H2BA H 0.9096 0.6250 0.5512 0.042 Uiso 1 1 calc R . . . .
H2BB H 0.9111 0.5004 0.5376 0.042 Uiso 1 1 calc R . . . .
C3B C 0.829(3) 0.6515(14) 0.4839(6) 0.036(4) Uani 1 1 d . U . . .
H3B H 0.8816 0.7205 0.5016 0.044 Uiso 1 1 calc R . . . .
C5B C 0.6976(19) 0.5870(18) 0.4190(8) 0.036(3) Uani 1 1 d . U . . .
C6B C 0.662(2) 0.633(2) 0.3822(8) 0.042(5) Uani 1 1 d . U . . .
H6B H 0.5984 0.5734 0.3641 0.050 Uiso 1 1 calc R . . . .
C7B C 0.714(2) 0.758(2) 0.3715(9) 0.048(6) Uani 1 1 d . U . . .
C8B C 0.803(2) 0.8468(19) 0.4000(8) 0.046(5) Uani 1 1 d . U . . .
H8B H 0.8375 0.9334 0.3941 0.056 Uiso 1 1 calc R . . . .
C9B C 0.8392(18) 0.8103(18) 0.4358(8) 0.043(5) Uani 1 1 d . U . . .
H9B H 0.8993 0.8725 0.4542 0.051 Uiso 1 1 calc R . . . .
C10B C 0.7895(17) 0.6806(17) 0.4468(7) 0.035(4) Uani 1 1 d . U . . .
C11B C 0.567(3) 0.712(3) 0.3109(10) 0.081(8) Uani 1 1 d . U . . .
H11E H 0.5059 0.6441 0.3296 0.098 Uiso 1 1 calc R . . . .
H11F H 0.5279 0.7588 0.2992 0.098 Uiso 1 1 calc R . . . .
C12B C 0.607(5) 0.665(4) 0.2785(12) 0.124(15) Uani 1 1 d . U . . .
H12D H 0.6934 0.6900 0.2763 0.149 Uiso 1 1 calc R . . . .
H12E H 0.5493 0.6075 0.2585 0.149 Uiso 1 1 calc R . . . .
C13B C 0.740(3) 0.925(3) 0.3206(12) 0.082(10) Uani 1 1 d . U . . .
H13C H 0.7253 0.9252 0.2896 0.098 Uiso 1 1 calc R . . . .
H13D H 0.8312 0.9664 0.3251 0.098 Uiso 1 1 calc R . . . .
C14B C 0.691(3) 1.001(3) 0.3426(11) 0.088(10) Uani 1 1 d . U . . .
H14D H 0.7352 1.0867 0.3315 0.132 Uiso 1 1 calc GR . . . .
H14E H 0.7061 1.0027 0.3734 0.132 Uiso 1 1 calc GR . . . .
H14F H 0.6017 0.9636 0.3373 0.132 Uiso 1 1 calc GR . . . .
C0AA C 0.670(5) 0.696(6) 0.1547(18) 0.102(18) Uani 0.65 1 d D U . D 2
H0AA H 0.6735 0.6943 0.1235 0.152 Uiso 0.65 1 calc GR . . D 2
H0AB H 0.6447 0.7555 0.1638 0.152 Uiso 0.65 1 calc GR . . D 2
H0AC H 0.6101 0.6123 0.1653 0.152 Uiso 0.65 1 calc GR . . D 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
Gd1A O1A 2.214(18) 3_775 ?
Gd1A O1A 2.214(18) . ?
Gd1A O1A 2.214(18) 2_755 ?
Gd1A N1A 2.82(4) . ?
Gd1A N2A 2.50(2) . ?
Gd1A N2A 2.50(2) 3_775 ?
Gd1A N2A 2.50(2) 2_755 ?
O1A C9A 1.35(3) . ?
N1A C1A 1.47(3) 2_755 ?
N1A C1A 1.47(3) . ?
N1A C1A 1.47(3) 3_775 ?
N2A C2A 1.47(3) . ?
N2A C3A 1.22(3) . ?
N3A C2 1.63(4) . ?
N3A C10A 1.39(4) . ?
N3A C11A 1.48(3) . ?
N3A C13A 1.41(6) . ?
C1A H1AA 0.9900 . ?
C1A H1AB 0.9900 . ?
C1A C2A 1.50(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.58(4) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3A H3A 0.9500 . ?
C3A C4A 1.52(4) . ?
C4A C5A 1.36(4) . ?
C4A C9A 1.42(4) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.41(3) . ?
C6A H6A 0.9500 . ?
C6A C10A 1.40(4) . ?
C8A H8A 0.9500 . ?
C8A C9A 1.38(4) . ?
C8A C10A 1.42(4) . ?
C11A H11A 0.9900 . ?
C11A H11B 0.9900 . ?
C11A H11C 0.9900 . ?
C11A H11D 0.9900 . ?
C11A C12A 1.47(5) . ?
C11A C0AA 1.57(5) . ?
C12A H12A 0.9800 . ?
C12A H12B 0.9800 . ?
C12A H12C 0.9800 . ?
C13A H13A 0.9900 . ?
C13A H13B 0.9900 . ?
C13A C14A 1.59(5) . ?
C14A H14A 1.02(7) . ?
C14A H14B 0.99(7) . ?
C14A H14C 1.00(7) . ?
Gd1B O1B 2.263(13) . ?
Gd1B O1B 2.263(13) 3_665 ?
Gd1B O1B 2.263(13) 2_655 ?
Gd1B N1B 2.74(2) . ?
Gd1B N2B 2.467(15) . ?
Gd1B N2B 2.467(15) 2_655 ?
Gd1B N2B 2.467(15) 3_665 ?
O1B C5B 1.25(2) . ?
N1B C1B 1.500(19) 2_655 ?
N1B C1B 1.50(2) . ?
N1B C1B 1.500(19) 3_665 ?
N2B C2B 1.48(3) . ?
N2B C3B 1.33(2) . ?
N3B C7B 1.37(3) . ?
N3B C11B 1.50(4) . ?
N3B C13B 1.44(3) . ?
C1B H1BA 0.9900 . ?
C1B H1BB 0.9900 . ?
C1B C2B 1.52(3) . ?
C2B H2BA 0.9900 . ?
C2B H2BB 0.9900 . ?
C3B H3B 0.9500 . ?
C3B C10B 1.37(3) . ?
C5B C6B 1.45(3) . ?
C5B C10B 1.44(3) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.39(3) . ?
C7B C8B 1.41(3) . ?
C8B H8B 0.9500 . ?
C8B C9B 1.37(3) . ?
C9B H9B 0.9500 . ?
C9B C10B 1.44(3) . ?
C11B H11E 0.9900 . ?
C11B H11F 0.9900 . ?
C11B C12B 1.38(4) . ?
C12B H12D 0.9500 . ?
C12B H12E 0.9500 . ?
C13B H13C 0.9900 . ?
C13B H13D 0.9900 . ?
C13B C14B 1.51(4) . ?
C14B H14D 0.9800 . ?
C14B H14E 0.9800 . ?
C14B H14F 0.9800 . ?
C0AA H0AA 0.9800 . ?
C0AA H0AB 0.9800 . ?
C0AA H0AC 0.9800 . ?

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
O1A Gd1A O1A 91.8(6) 3_775 . ?
O1A Gd1A O1A 91.8(6) 3_775 2_755 ?
O1A Gd1A O1A 91.8(6) . 2_755 ?
O1A Gd1A N1A 124.0(5) . . ?
O1A Gd1A N1A 124.0(5) 2_755 . ?
O1A Gd1A N1A 124.0(5) 3_775 . ?
O1A Gd1A N2A 73.7(6) . . ?
O1A Gd1A N2A 88.6(7) 2_755 3_775 ?
O1A Gd1A N2A 165.5(7) . 3_775 ?
O1A Gd1A N2A 88.6(7) . 2_755 ?
O1A Gd1A N2A 73.7(6) 3_775 3_775 ?
O1A Gd1A N2A 165.5(7) 2_755 . ?
O1A Gd1A N2A 88.6(7) 3_775 . ?
O1A Gd1A N2A 165.5(7) 3_775 2_755 ?
O1A Gd1A N2A 73.7(6) 2_755 2_755 ?
N2A Gd1A N1A 66.7(5) 2_755 . ?
N2A Gd1A N1A 66.7(5) . . ?
N2A Gd1A N1A 66.7(5) 3_775 . ?
N2A Gd1A N2A 105.4(5) 2_755 3_775 ?
N2A Gd1A N2A 105.4(5) . 2_755 ?
N2A Gd1A N2A 105.4(5) . 3_775 ?
C9A O1A Gd1A 142.4(16) . . ?
C1A N1A Gd1A 106.2(19) . . ?
C1A N1A Gd1A 106.1(19) 2_755 . ?
C1A N1A Gd1A 106.1(19) 3_775 . ?
C1A N1A C1A 112.6(16) . 2_755 ?
C1A N1A C1A 112.6(16) . 3_775 ?
C1A N1A C1A 112.6(16) 2_755 3_775 ?
C2A N2A Gd1A 111.4(17) . . ?
C3A N2A Gd1A 131.4(19) . . ?
C3A N2A C2A 117(2) . . ?
C10A N3A C2 116(3) . . ?
C10A N3A C11A 120(3) . . ?
C10A N3A C13A 119(3) . . ?
C11A N3A C2 111(3) . . ?
C13A N3A C11A 121(3) . . ?
N1A C1A H1AA 109.1 . . ?
N1A C1A H1AB 109.1 . . ?
N1A C1A C2A 112(2) . . ?
H1AA C1A H1AB 107.9 . . ?
C2A C1A H1AA 109.1 . . ?
C2A C1A H1AB 109.1 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
N2A C2A C1A 108(2) . . ?
N2A C2A H2AA 110.0 . . ?
N2A C2A H2AB 110.0 . . ?
C1A C2A H2AA 110.0 . . ?
C1A C2A H2AB 110.0 . . ?
H2AA C2A H2AB 108.4 . . ?
N3A C2 H2A 112.2 . . ?
N3A C2 H2B 112.2 . . ?
C1 C2 N3A 98(3) . . ?
C1 C2 H2A 112.2 . . ?
C1 C2 H2B 112.2 . . ?
H2A C2 H2B 109.8 . . ?
N2A C3A H3A 116.7 . . ?
N2A C3A C4A 127(3) . . ?
C4A C3A H3A 116.7 . . ?
C5A C4A C3A 118(2) . . ?
C5A C4A C9A 118(2) . . ?
C9A C4A C3A 124(2) . . ?
C4A C5A H5A 117.6 . . ?
C4A C5A C6A 125(3) . . ?
C6A C5A H5A 117.6 . . ?
C5A C6A H6A 122.2 . . ?
C10A C6A C5A 116(3) . . ?
C10A C6A H6A 122.2 . . ?
C9A C8A H8A 120.0 . . ?
C9A C8A C10A 120(3) . . ?
C10A C8A H8A 120.0 . . ?
O1A C9A C4A 120(2) . . ?
O1A C9A C8A 120(2) . . ?
C8A C9A C4A 120(2) . . ?
N3A C10A C6A 119(3) . . ?
N3A C10A C8A 120(3) . . ?
C6A C10A C8A 121(3) . . ?
N3A C11A H11A 106.1 . . ?
N3A C11A H11B 106.1 . . ?
N3A C11A H11C 106.9 . . ?
N3A C11A H11D 106.9 . . ?
N3A C11A C0AA 122(3) . . ?
H11A C11A H11B 106.3 . . ?
H11C C11A H11D 106.7 . . ?
C12A C11A N3A 125(3) . . ?
C12A C11A H11A 106.1 . . ?
C12A C11A H11B 106.1 . . ?
C0AA C11A H11C 106.9 . . ?
C0AA C11A H11D 106.9 . . ?
C11A C12A H12A 109.5 . . ?
C11A C12A H12B 109.5 . . ?
C11A C12A H12C 109.5 . . ?
H12A C12A H12B 109.5 . . ?
H12A C12A H12C 109.5 . . ?
H12B C12A H12C 109.5 . . ?
N3A C13A H13A 108.6 . . ?
N3A C13A H13B 108.6 . . ?
N3A C13A C14A 115(5) . . ?
H13A C13A H13B 107.6 . . ?
C14A C13A H13A 108.6 . . ?
C14A C13A H13B 108.6 . . ?
C13A C14A H14A 112(6) . . ?
C13A C14A H14B 113(6) . . ?
C13A C14A H14C 115(6) . . ?
H14A C14A H14B 105(7) . . ?
H14A C14A H14C 105(6) . . ?
H14B C14A H14C 106(6) . . ?
O1B Gd1B O1B 91.2(6) 3_665 2_655 ?
O1B Gd1B O1B 91.2(6) 3_665 . ?
O1B Gd1B O1B 91.2(6) 2_655 . ?
O1B Gd1B N1B 124.4(4) . . ?
O1B Gd1B N1B 124.4(4) 3_665 . ?
O1B Gd1B N1B 124.4(4) 2_655 . ?
O1B Gd1B N2B 165.3(5) 2_655 . ?
O1B Gd1B N2B 89.9(5) . 2_655 ?
O1B Gd1B N2B 89.9(5) 2_655 3_665 ?
O1B Gd1B N2B 74.1(5) . . ?
O1B Gd1B N2B 74.1(5) 3_665 3_665 ?
O1B Gd1B N2B 165.3(5) 3_665 2_655 ?
O1B Gd1B N2B 89.9(5) 3_665 . ?
O1B Gd1B N2B 74.1(5) 2_655 2_655 ?
O1B Gd1B N2B 165.3(5) . 3_665 ?
N2B Gd1B N1B 65.9(4) 3_665 . ?
N2B Gd1B N1B 65.9(4) 2_655 . ?
N2B Gd1B N1B 65.9(4) . . ?
N2B Gd1B N2B 104.5(5) 3_665 2_655 ?
N2B Gd1B N2B 104.5(5) . 2_655 ?
N2B Gd1B N2B 104.5(5) 3_665 . ?
C5B O1B Gd1B 139.2(13) . . ?
C1B N1B Gd1B 110.7(11) 2_655 . ?
C1B N1B Gd1B 110.7(11) . . ?
C1B N1B Gd1B 110.7(11) 3_665 . ?
C1B N1B C1B 108.2(11) 3_665 2_655 ?
C1B N1B C1B 108.2(11) 3_665 . ?
C1B N1B C1B 108.2(11) . 2_655 ?
C2B N2B Gd1B 115.4(11) . . ?
C3B N2B Gd1B 128.2(14) . . ?
C3B N2B C2B 116.2(16) . . ?
C7B N3B C11B 121(2) . . ?
C7B N3B C13B 125(3) . . ?
C13B N3B C11B 112(3) . . ?
N1B C1B H1BA 109.4 . . ?
N1B C1B H1BB 109.4 . . ?
N1B C1B C2B 111.1(16) . . ?
H1BA C1B H1BB 108.0 . . ?
C2B C1B H1BA 109.4 . . ?
C2B C1B H1BB 109.4 . . ?
N2B C2B C1B 107.2(16) . . ?
N2B C2B H2BA 110.3 . . ?
N2B C2B H2BB 110.3 . . ?
C1B C2B H2BA 110.3 . . ?
C1B C2B H2BB 110.3 . . ?
H2BA C2B H2BB 108.5 . . ?
N2B C3B H3B 115.6 . . ?
N2B C3B C10B 128.9(18) . . ?
C10B C3B H3B 115.6 . . ?
O1B C5B C6B 119(2) . . ?
O1B C5B C10B 125.0(19) . . ?
C10B C5B C6B 116.0(18) . . ?
C5B C6B H6B 117.7 . . ?
C7B C6B C5B 125(2) . . ?
C7B C6B H6B 117.7 . . ?
N3B C7B C6B 122(2) . . ?
N3B C7B C8B 120(2) . . ?
C6B C7B C8B 117(2) . . ?
C7B C8B H8B 119.4 . . ?
C9B C8B C7B 121(2) . . ?
C9B C8B H8B 119.4 . . ?
C8B C9B H9B 118.8 . . ?
C8B C9B C10B 122(2) . . ?
C10B C9B H9B 118.8 . . ?
C3B C10B C5B 122.8(17) . . ?
C3B C10B C9B 118.8(19) . . ?
C5B C10B C9B 118(2) . . ?
N3B C11B H11E 111.2 . . ?
N3B C11B H11F 111.2 . . ?
H11E C11B H11F 109.1 . . ?
C12B C11B N3B 103(3) . . ?
C12B C11B H11E 111.2 . . ?
C12B C11B H11F 111.2 . . ?
C11B C12B H12D 120.0 . . ?
C11B C12B H12E 120.0 . . ?
H12D C12B H12E 120.0 . . ?
N3B C13B H13C 108.4 . . ?
N3B C13B H13D 108.4 . . ?
N3B C13B C14B 116(3) . . ?
H13C C13B H13D 107.4 . . ?
C14B C13B H13C 108.4 . . ?
C14B C13B H13D 108.4 . . ?
C13B C14B H14D 109.5 . . ?
C13B C14B H14E 109.5 . . ?
C13B C14B H14F 109.5 . . ?
H14D C14B H14E 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
C11A C0AA H0AA 109.5 . . ?
C11A C0AA H0AB 109.5 . . ?
C11A C0AA H0AC 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 2 0 3.807
0 0 1 0.650
0 2 1 3.862
0 0 2 1.300
0 0 3 1.951
-4 4 3 7.879
0 5 3 9.755
0 5 5 10.103
0 0 10 6.515

_platon_squeeze_details          
;
TITL x_dummy   P 3 2 1      R = 0.08                                            
CELL   12.3620   12.3620   31.3210     90.00     90.00    120.00                
SPGR P321                                                                       
# Solvent Accessible Volume =       331                                         
# Electrons Found in S.A.V. =       148                                         
# Note: Atoms in Void as Cxxx and Qxxx all others                               
Q101 0.308 0.496 0.681 !       7.04 eA-3                                        
C102 0.261 0.645 0.204 !       6.30 eA-3                                        
C103 0.740 0.354 0.295 !       6.08 eA-3                                        
Q104 0.692 0.504 0.820 !       5.56 eA-3                                        
C105 0.671 0.347 0.333 !       5.39 eA-3                                        
C106 0.340 0.684 0.156 !       3.44 eA-3                                        
Q107 0.337 0.673 0.496 !       2.48 eA-3                                        
Q108 0.335 0.673 0.570 !       1.79 eA-3                                        
C109 0.284 0.769 0.693 !       1.10 eA-3                                        
Q110 0.391 0.797 0.016 !       1.00 eA-3                                        
C111 0.599 0.242 0.828 !       1.00 eA-3                                        
Q112 0.324 0.751 0.502 !       1.00 eA-3                                        
Q113 0.672 0.338 0.874 !       0.97 eA-3                                        
Q114 0.832 0.346 0.294 !       0.97 eA-3                                        
Q115 0.683 0.185 0.363 !       0.96 eA-3                                        
Q116 0.391 0.771 0.501 !       0.96 eA-3                                        
Q117 0.339 0.823 0.705 !       0.94 eA-3                                        
Q118 0.359 0.590 0.569 !       0.92 eA-3                                        
Q119 0.677 0.509 0.337 !       0.91 eA-3                                        
Q120 0.408 0.637 0.570 !       0.88 eA-3                                        
Q121 0.598 0.450 0.787 !       0.85 eA-3                                        
Q122 0.740 0.283 0.942 !       0.84 eA-3                                        
Q123 0.157 0.582 0.665 !       0.81 eA-3                                        
Q124 0.561 0.274 0.437 !       0.80 eA-3                                        
Q125 0.252 0.681 0.507 !       0.76 eA-3                                        
Q126 0.606 0.241 0.758 !       0.74 eA-3                                        
Q127 0.152 0.584 0.626 !       0.72 eA-3                                        
Q128 0.329 0.649 0.837 !       0.70 eA-3                                        
Q129 0.751 0.514 0.851 !       0.68 eA-3                                        
Q130 0.407 0.579 0.258 !       0.67 eA-3                                        
Q131 0.685 0.381 0.864 !       0.67 eA-3                                        
Q132 0.280 0.635 0.078 !       0.65 eA-3                                        
C133 0.253 0.683 0.233 !       0.64 eA-3                                        
Q134 0.543 0.812 0.172 !       0.63 eA-3                                        
Q135 0.371 0.735 0.047 !       0.63 eA-3                                        
Q136 0.138 0.464 0.712 !       0.62 eA-3                                        
Q137 0.800 0.353 0.952 !       0.61 eA-3                                        
Q138 0.190 0.523 0.221 !       0.60 eA-3                                        
Q139 0.612 0.338 0.007 !       0.60 eA-3                                        
Q140 0.429 0.189 0.307 !       0.60 eA-3                                        
Q141 0.513 0.316 0.282 !       0.57 eA-3                                        
Q142 0.861 0.011 0.701 !       0.57 eA-3                                        
Q143 0.719 0.719 0.500 !       0.57 eA-3                                        
Q144 0.340 0.663 0.766 !       0.57 eA-3                                        
Q145 0.655 0.385 0.008 !       0.56 eA-3                                        
Q146 0.641 0.095 0.312 !       0.55 eA-3                                        
Q147 0.339 0.541 0.539 !       0.55 eA-3                                        
Q148 0.377 0.189 0.289 !       0.55 eA-3                                        
Q149 0.828 0.490 0.697 !       0.53 eA-3                                        
Q150 0.925 0.716 0.592 !       0.53 eA-3                                        
Q151 0.763 0.379 0.859 !       0.52 eA-3                                        
Q152 0.595 0.776 0.156 !       0.52 eA-3                                        
Q153 0.907 0.415 0.319 !       0.51 eA-3                                        
Q154 0.328 0.657 0.325 !       0.51 eA-3                                        
Q155 0.544 0.746 0.741 !       0.51 eA-3                                        
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.333 0.667 0.691 87 39 ' '
2 0.333 0.667 0.197 77 35 ' '
3 0.667 0.333 0.309 86 39 ' '
4 0.667 0.333 0.803 76 35 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1
2 0

# start Validation Reply Form
_vrf_PLAT342_p-31c_c             
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02656 Ang.  
RESPONSE: Orientational disorder in the N, N-diethyl groups has contributed to
the low bond precision on C-C bonds.
;
_vrf_PLAT987_p-31c_c             
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: The unit cell contains two tripodal complexes of opposite
handedness with respesct to the oreientation of benzene faces.The alert BASF
/TWIN arises because of the presence of two enantiomers in the asymmetric unit.
;
####################################################################### 
# 
# 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_sandy_dy_01sept16_2nd_0ma
_database_code_depnum_ccdc_archive 'CCDC 1515528'
_audit_update_record             
;
2017-08-18 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_audit_creation_date             2017-08-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H54 Dy1 N7 O3, 3(H2 O)'
_chemical_formula_sum            'C39 H60 Dy N7 O6'
_chemical_formula_weight         885.4463
_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'
Dy Dy -0.1892 4.4098 '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           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'
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'
'-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                   12.3876(10)
_cell_length_b                   12.3876(10)
_cell_length_c                   31.693(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4211.9(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      27.189
_cell_measurement_theta_min      1.285
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.816
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1637 before and 0.0806 after correction.
The Ratio of minimum to maximum transmission is 0.8142.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1708
_exptl_crystal_preparation       'Slow evaporation from a MeOH/DCM mixture'
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.015
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.892
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            50279
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.189
_diffrn_reflns_theta_min         1.285
_diffrn_ambient_temperature      150.02
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2149
_reflns_number_total             2861
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Apex II (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.287
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2861
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0444
_refine_ls_restrained_S_all      1.331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0729P)²+3.6176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1601
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13'-C12A = C11'-C10 = C11-C10
 1.5 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H10C(0.3) H10D(0.3) H10A(0.7) H10B(0.7) C11'(0.3) H11C(0.3)
 H11B(0.3) H11A(0.3) C11(0.7) H11D(0.7) H11E(0.7) H11F(0.7) C13'(0.2) H13A(0.2)
 H13B(0.2) H13C(0.2) C13(0.8) H13D(0.8) H13E(0.8) H13F(0.8) H12D(0.2) H12C(0.2)
 H12A(0.8) H12B(0.8)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10C,H10D), C10(H10A,H10B), C12A(H12D,H12C),
 C12A(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8)
5.c Idealised Me refined as rotating group:
 C11'(H11C,H11B,H11A), C11(H11D,H11E,H11F), C13'(H13A,H13B,H13C), C13(H13D,
 H13E,H13F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy01 Dy 0.333333 0.666667 0.71513(2) 0.03579(19) Uani 1 3 d S T P . .
O002 O 0.3554(3) 0.5313(3) 0.67619(12) 0.0420(8) Uani 1 1 d . . . . .
N1 N 0.333333 0.666667 0.8025(3) 0.045(2) Uani 1 3 d S T P . .
N2 N 0.1942(4) 0.4617(4) 0.74710(14) 0.0376(9) Uani 1 1 d . . . . .
N3 N 0.3271(7) 0.2023(6) 0.5906(2) 0.075(2) Uani 1 1 d . U . . .
C1 C 0.2476(5) 0.5376(6) 0.81768(19) 0.0458(13) Uani 1 1 d . . . . .
H1A H 0.214668 0.541033 0.845793 0.055 Uiso 1 1 calc R . . . .
H1B H 0.294417 0.492524 0.820637 0.055 Uiso 1 1 calc R . . . .
C2 C 0.1403(5) 0.4677(5) 0.78742(17) 0.0447(12) Uani 1 1 d . . . . .
H2A H 0.083221 0.382687 0.798138 0.054 Uiso 1 1 calc R . . . .
H2B H 0.092758 0.511864 0.784061 0.054 Uiso 1 1 calc R . . . .
C3 C 0.1678(5) 0.3532(6) 0.7340(2) 0.0421(13) Uani 1 1 d . . . . .
H3 H 0.111646 0.284834 0.751049 0.050 Uiso 1 1 calc R . . . .
C4 C 0.2127(5) 0.3225(5) 0.69682(17) 0.0388(11) Uani 1 1 d . . . . .
C5 C 0.1646(5) 0.1961(5) 0.68744(19) 0.0464(13) Uani 1 1 d . . . . .
H5 H 0.105286 0.135536 0.706137 0.056 Uiso 1 1 calc R . . . .
C6 C 0.1995(6) 0.1565(5) 0.6524(2) 0.0501(14) Uani 1 1 d . . . . .
H6 H 0.162278 0.069758 0.646848 0.060 Uiso 1 1 calc R . . . .
C7 C 0.2891(6) 0.2421(6) 0.62488(19) 0.0498(13) Uani 1 1 d . . . . .
C8 C 0.3395(5) 0.3688(5) 0.63351(17) 0.0432(12) Uani 1 1 d . . . . .
H8 H 0.399480 0.428015 0.614636 0.052 Uiso 1 1 calc R . . . .
C9 C 0.3045(5) 0.4123(4) 0.66931(17) 0.0376(11) Uani 1 1 d . . . . .
C10 C 0.2653(11) 0.0717(8) 0.5787(3) 0.103(3) Uani 1 1 d D U . . .
H10C H 0.328775 0.059090 0.564122 0.124 Uiso 0.3 1 calc R . . A 2
H10D H 0.245889 0.024072 0.605441 0.124 Uiso 0.3 1 calc R . . A 2
H10A H 0.176324 0.034395 0.586573 0.124 Uiso 0.7 1 calc R . . B 1
H10B H 0.268612 0.067922 0.547588 0.124 Uiso 0.7 1 calc R . . B 1
C11' C 0.154(2) 0.010(3) 0.5533(11) 0.120(11) Uani 0.3 1 d D U . C 2
H11C H 0.081716 -0.005589 0.570356 0.181 Uiso 0.3 1 calc GR . . C 2
H11B H 0.143141 -0.069847 0.543163 0.181 Uiso 0.3 1 calc GR . . C 2
H11A H 0.161706 0.062523 0.529176 0.181 Uiso 0.3 1 calc GR . . C 2
C11 C 0.3090(17) -0.0078(16) 0.5956(5) 0.116(5) Uani 0.7 1 d D U . C 1
H11D H 0.393413 0.020136 0.585197 0.175 Uiso 0.7 1 calc GR . . C 1
H11E H 0.253177 -0.093886 0.586583 0.175 Uiso 0.7 1 calc GR . . C 1
H11F H 0.310105 -0.003481 0.626486 0.175 Uiso 0.7 1 calc GR . . C 1
C13' C 0.558(3) 0.388(5) 0.561(2) 0.109(16) Uiso 0.2 1 d D U . D 2
H13A H 0.591823 0.389724 0.532905 0.163 Uiso 0.2 1 calc GR . . D 2
H13B H 0.604639 0.371340 0.582270 0.163 Uiso 0.2 1 calc GR . . D 2
H13C H 0.563881 0.468666 0.566689 0.163 Uiso 0.2 1 calc GR . . D 2
C13 C 0.383(2) 0.3349(19) 0.5318(4) 0.139(6) Uani 0.8 1 d . U . D 1
H13D H 0.342355 0.272120 0.509629 0.208 Uiso 0.8 1 calc GR . . D 1
H13E H 0.453300 0.410088 0.519613 0.208 Uiso 0.8 1 calc GR . . D 1
H13F H 0.323243 0.355777 0.543987 0.208 Uiso 0.8 1 calc GR . . D 1
C12A C 0.4258(13) 0.2891(10) 0.5623(4) 0.118(4) Uani 1 1 d D . . . .
H12D H 0.385011 0.331629 0.548906 0.142 Uiso 0.2 1 calc R . . D 2
H12C H 0.424232 0.231501 0.540346 0.142 Uiso 0.2 1 calc R . . D 2
H12A H 0.490035 0.359275 0.579098 0.142 Uiso 0.8 1 calc R . . D 1
H12B H 0.465887 0.245831 0.548911 0.142 Uiso 0.8 1 calc R . . D 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy01 O002 2.207(3) 3_565 ?
Dy01 O002 2.207(3) . ?
Dy01 O002 2.207(3) 2_665 ?
Dy01 N1 2.770(10) . ?
Dy01 N2 2.464(4) . ?
Dy01 N2 2.464(4) 3_565 ?
Dy01 N2 2.464(4) 2_665 ?
O002 C9 1.299(6) . ?
N1 C1 1.489(7) . ?
N1 C1 1.489(7) 2_665 ?
N1 C1 1.489(7) 3_565 ?
N2 C2 1.460(7) . ?
N2 C3 1.283(8) . ?
N3 C7 1.371(8) . ?
N3 C10 1.451(11) . ?
N3 C12A 1.463(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.512(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3 0.9500 . ?
C3 C4 1.434(8) . ?
C4 C5 1.400(7) . ?
C4 C9 1.423(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.369(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.393(9) . ?
C7 C8 1.396(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.414(7) . ?
C10 H10C 0.9900 . ?
C10 H10D 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11' 1.442(18) . ?
C10 C11 1.442(14) . ?
C11' H11C 0.9800 . ?
C11' H11B 0.9800 . ?
C11' H11A 0.9800 . ?
C11 H11D 0.9800 . ?
C11 H11E 0.9800 . ?
C11 H11F 0.9800 . ?
C13' H13A 0.9800 . ?
C13' H13B 0.9800 . ?
C13' H13C 0.9800 . ?
C13' C12A 1.47(2) . ?
C13 H13D 0.9800 . ?
C13 H13E 0.9800 . ?
C13 H13F 0.9800 . ?
C13 C12A 1.356(18) . ?
C12A H12D 0.9900 . ?
C12A H12C 0.9900 . ?
C12A H12A 0.9900 . ?
C12A H12B 0.9900 . ?

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
O002 Dy01 O002 91.77(13) 3_565 2_665 ?
O002 Dy01 O002 91.77(13) 3_565 . ?
O002 Dy01 O002 91.77(13) 2_665 . ?
O002 Dy01 N1 124.00(10) 2_665 . ?
O002 Dy01 N1 124.00(10) . . ?
O002 Dy01 N1 124.00(10) 3_565 . ?
O002 Dy01 N2 89.00(15) 2_665 3_565 ?
O002 Dy01 N2 89.01(15) . 2_665 ?
O002 Dy01 N2 74.65(14) 2_665 2_665 ?
O002 Dy01 N2 166.42(15) 2_665 . ?
O002 Dy01 N2 166.42(15) 3_565 2_665 ?
O002 Dy01 N2 166.42(15) . 3_565 ?
O002 Dy01 N2 74.65(13) 3_565 3_565 ?
O002 Dy01 N2 89.00(15) 3_565 . ?
O002 Dy01 N2 74.65(14) . . ?
N2 Dy01 N1 65.72(10) . . ?
N2 Dy01 N1 65.71(10) 3_565 . ?
N2 Dy01 N1 65.71(10) 2_665 . ?
N2 Dy01 N2 104.25(12) 3_565 2_665 ?
N2 Dy01 N2 104.26(12) 3_565 . ?
N2 Dy01 N2 104.26(12) . 2_665 ?
C9 O002 Dy01 141.4(3) . . ?
C1 N1 Dy01 108.8(4) 2_665 . ?
C1 N1 Dy01 108.8(4) . . ?
C1 N1 Dy01 108.8(4) 3_565 . ?
C1 N1 C1 110.1(4) 3_565 . ?
C1 N1 C1 110.1(4) . 2_665 ?
C1 N1 C1 110.1(4) 3_565 2_665 ?
C2 N2 Dy01 114.2(3) . . ?
C3 N2 Dy01 128.9(4) . . ?
C3 N2 C2 116.9(5) . . ?
C7 N3 C10 121.4(7) . . ?
C7 N3 C12A 122.2(7) . . ?
C10 N3 C12A 116.3(6) . . ?
N1 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
N1 C1 C2 111.2(5) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
N2 C2 C1 106.9(4) . . ?
N2 C2 H2A 110.3 . . ?
N2 C2 H2B 110.3 . . ?
C1 C2 H2A 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N2 C3 H3 116.1 . . ?
N2 C3 C4 127.9(6) . . ?
C4 C3 H3 116.1 . . ?
C5 C4 C3 117.8(5) . . ?
C5 C4 C9 118.1(5) . . ?
C9 C4 C3 124.1(5) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 C4 122.6(5) . . ?
C6 C5 H5 118.7 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.6(5) . . ?
C7 C6 H6 119.7 . . ?
N3 C7 C6 120.6(6) . . ?
N3 C7 C8 121.3(6) . . ?
C6 C7 C8 118.1(5) . . ?
C7 C8 H8 118.8 . . ?
C7 C8 C9 122.4(5) . . ?
C9 C8 H8 118.8 . . ?
O002 C9 C4 121.9(5) . . ?
O002 C9 C8 119.9(5) . . ?
C8 C9 C4 118.1(4) . . ?
N3 C10 H10C 106.2 . . ?
N3 C10 H10D 106.2 . . ?
N3 C10 H10A 107.4 . . ?
N3 C10 H10B 107.4 . . ?
H10C C10 H10D 106.3 . . ?
H10A C10 H10B 106.9 . . ?
C11' C10 N3 124.7(16) . . ?
C11' C10 H10C 106.2 . . ?
C11' C10 H10D 106.2 . . ?
C11 C10 N3 119.7(12) . . ?
C11 C10 H10A 107.4 . . ?
C11 C10 H10B 107.4 . . ?
C10 C11' H11C 109.5 . . ?
C10 C11' H11B 109.5 . . ?
C10 C11' H11A 109.5 . . ?
H11C C11' H11B 109.5 . . ?
H11C C11' H11A 109.5 . . ?
H11B C11' H11A 109.5 . . ?
C10 C11 H11D 109.5 . . ?
C10 C11 H11E 109.5 . . ?
C10 C11 H11F 109.5 . . ?
H11D C11 H11E 109.5 . . ?
H11D C11 H11F 109.5 . . ?
H11E C11 H11F 109.5 . . ?
H13A C13' H13B 109.5 . . ?
H13A C13' H13C 109.5 . . ?
H13B C13' H13C 109.5 . . ?
C12A C13' H13A 109.5 . . ?
C12A C13' H13B 109.5 . . ?
C12A C13' H13C 109.5 . . ?
H13D C13 H13E 109.5 . . ?
H13D C13 H13F 109.5 . . ?
H13E C13 H13F 109.5 . . ?
C12A C13 H13D 109.5 . . ?
C12A C13 H13E 109.5 . . ?
C12A C13 H13F 109.5 . . ?
N3 C12A C13' 143(3) . . ?
N3 C12A H12D 101.1 . . ?
N3 C12A H12C 101.1 . . ?
N3 C12A H12A 109.0 . . ?
N3 C12A H12B 109.0 . . ?
C13' C12A H12D 101.1 . . ?
C13' C12A H12C 101.1 . . ?
C13 C12A N3 112.8(14) . . ?
C13 C12A H12A 109.0 . . ?
C13 C12A H12B 109.0 . . ?
H12D C12A H12C 104.5 . . ?
H12A C12A H12B 107.8 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.333 0.667 0.561 96.4 49.1 ?
2 0.333 0.667 0.061 96.4 49.1 ?
3 0.667 0.333 0.939 96.4 48.7 ?
4 0.667 0.333 0.439 96.4 48.6 ?

_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_FL177_a
_database_code_depnum_ccdc_archive 'CCDC 1515525'
_audit_update_record             
;
2017-08-18 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_audit_creation_date             2016-11-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_formula_moiety         'C39 H57 N7 O3'
_chemical_formula_sum            'C39 H57 N7 O3'
_chemical_formula_weight         671.93
_chemical_absolute_configuration unk
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_H-M_alt        'R 3 c'
_space_group_name_Hall           ' R 3 -2"c'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x+y,y,z+1/2
5 x,x-y,z+1/2
6 -y,-x,z+1/2
7 x+1/3,y+2/3,z+2/3
8 -y+1/3,x-y+2/3,z+2/3
9 -x+y+1/3,-x+2/3,z+2/3
10 -x+y+1/3,y+2/3,z+7/6
11 x+1/3,x-y+2/3,z+7/6
12 -y+1/3,-x+2/3,z+7/6
13 x+2/3,y+1/3,z+1/3
14 -y+2/3,x-y+1/3,z+1/3
15 -x+y+2/3,-x+1/3,z+1/3
16 -x+y+2/3,y+1/3,z+5/6
17 x+2/3,x-y+1/3,z+5/6
18 -y+2/3,-x+1/3,z+5/6

_symmetry_Int_Tables_number      161
_cell_length_a                   13.6115(19)
_cell_length_b                   13.6115(19)
_cell_length_c                   35.291(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5662.5(16)
_cell_formula_units_Z            6
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    33332
_cell_measurement_theta_max      31.81
_cell_measurement_theta_min      2.88
_exptl_crystal_description       hexagonal
_exptl_crystal_colour            'clear yellow'

_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_density_diffrn    1.1822
_exptl_crystal_F_000             2184.8532
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            33332
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         31.81
_diffrn_reflns_theta_min         2.88
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.9857
_diffrn_measured_fraction_theta_max 0.8499
_diffrn_measurement_device_type  'ADSC Q315r CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Australian Synchrotron'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_reflns_Friedel_coverage         0.846
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              51
_reflns_limit_l_min              -51
_reflns_number_gt                3564
_reflns_number_total             3668
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.5053
_refine_diff_density_min         -0.3478
_refine_diff_density_rms         0.0549
_refine_ls_abs_structure_details 
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.0(8)
_refine_ls_d_res_high            0.6741
_refine_ls_d_res_low             7.0635
_refine_ls_goodness_of_fit_ref   1.2796
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3668
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      1.2794
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1383
_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
2. Restrained distances
 O1-H1
 0.87 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C10(H10a,H10b), C12(H12a,H12b)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C8(H8)
3.c Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C13(H13a,H13b,H13c)
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
O1 O 0.27676(8) 0.35995(7) 0.45616(2) 0.01866(18) Uani 1.000000 1 D . .
H1 H 0.318(2) 0.4155(16) 0.4406(6) 0.056(7) Uiso 1.000000 1 D . .
C1 C 0.37807(10) 0.59436(10) 0.35923(3) 0.0198(2) Uani 1.000000 1 . . .
H1a H 0.31534(10) 0.51477(10) 0.35787(3) 0.0237(3) Uiso 1.000000 1 R . .
H1b H 0.41022(10) 0.61772(10) 0.33347(3) 0.0237(3) Uiso 1.000000 1 R . .
N1 N 0.333333333333 0.666666666667 0.37186(4) 0.0163(3) Uani 1.000000 3 S T P
N2 N 0.41933(9) 0.53989(9) 0.42073(3) 0.0190(2) Uani 1.000000 1 . . .
C2 C 0.46985(11) 0.60150(11) 0.38593(3) 0.0213(2) Uani 1.000000 1 . . .
H2a H 0.51220(11) 0.56901(11) 0.37334(3) 0.0256(3) Uiso 1.000000 1 R . .
H2b H 0.52408(11) 0.68196(11) 0.39189(3) 0.0256(3) Uiso 1.000000 1 R . .
N3 N 0.28105(9) 0.35662(9) 0.59114(3) 0.0214(2) Uani 1.000000 1 . . .
C3 C 0.45094(10) 0.59186(10) 0.45256(4) 0.0189(2) Uani 1.000000 1 . . .
H3 H 0.50589(10) 0.67038(10) 0.45284(4) 0.0226(3) Uiso 1.000000 1 R . .
C5 C 0.31926(9) 0.41838(9) 0.48869(3) 0.0149(2) Uani 1.000000 1 . . .
C4 C 0.40487(10) 0.53369(10) 0.48809(3) 0.0167(2) Uani 1.000000 1 . . .
C6 C 0.27514(9) 0.36179(9) 0.52269(3) 0.0165(2) Uani 1.000000 1 . . .
H6 H 0.21492(9) 0.28531(9) 0.52228(3) 0.0198(2) Uiso 1.000000 1 R . .
C7 C 0.31811(10) 0.41584(10) 0.55772(3) 0.0171(2) Uani 1.000000 1 . . .
C9 C 0.44413(10) 0.58840(10) 0.52323(3) 0.0204(2) Uani 1.000000 1 . . .
H9 H 0.50058(10) 0.66642(10) 0.52357(3) 0.0244(3) Uiso 1.000000 1 R . .
C8 C 0.40326(10) 0.53234(10) 0.55725(3) 0.0198(2) Uani 1.000000 1 . . .
H8 H 0.43222(10) 0.57185(10) 0.58044(3) 0.0237(3) Uiso 1.000000 1 R . .
C10 C 0.32029(10) 0.41285(11) 0.62792(3) 0.0220(2) Uani 1.000000 1 . . .
H10a H 0.30810(10) 0.35501(11) 0.64721(3) 0.0264(3) Uiso 1.000000 1 R . .
H10b H 0.40288(10) 0.46674(11) 0.62641(3) 0.0264(3) Uiso 1.000000 1 R . .
C11 C 0.26123(12) 0.47686(13) 0.64094(4) 0.0302(3) Uani 1.000000 1 . . .
H11a H 0.2755(10) 0.5366(8) 0.6226(2) 0.0453(4) Uiso 1.000000 1 GR . .
H11b H 0.17941(18) 0.4241(2) 0.6428(4) 0.0453(4) Uiso 1.000000 1 GR . .
H11c H 0.2908(9) 0.5111(10) 0.66579(18) 0.0453(4) Uiso 1.000000 1 GR . .
C12 C 0.19420(11) 0.23649(10) 0.59104(4) 0.0249(2) Uani 1.000000 1 . . .
H12a H 0.21046(11) 0.19838(10) 0.57008(4) 0.0299(3) Uiso 1.000000 1 R . .
H12b H 0.19937(11) 0.20184(10) 0.61507(4) 0.0299(3) Uiso 1.000000 1 R . .
C13 C 0.07379(11) 0.21428(13) 0.58659(4) 0.0313(3) Uani 1.000000 1 . . .
H13a H 0.0680(3) 0.2498(10) 0.5632(2) 0.0469(4) Uiso 1.000000 1 GR . .
H13b H 0.02112(16) 0.13232(13) 0.5854(4) 0.0469(4) Uiso 1.000000 1 GR . .
H13c H 0.0545(4) 0.2464(10) 0.6083(2) 0.0469(4) Uiso 1.000000 1 GR . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 H1 0.876(10) . ?
O1 C5 1.3511(13) . ?
C1 H1a 0.9900 . ?
C1 H1b 0.9900 . ?
C1 N1 1.4619(12) 2_665 ?
C1 C2 1.5285(18) . ?
N2 C2 1.4519(15) . ?
N2 C3 1.2817(17) . ?
C2 H2a 0.9900 . ?
C2 H2b 0.9900 . ?
N3 C7 1.3741(15) . ?
N3 C10 1.4654(15) . ?
N3 C12 1.4623(16) . ?
C3 H3 0.9500 . ?
C3 C4 1.4479(16) . ?
C5 C4 1.4116(15) . ?
C5 C6 1.3897(15) . ?
C4 C9 1.4071(16) . ?
C6 H6 0.9500 . ?
C6 C7 1.4077(15) . ?
C7 C8 1.4214(16) . ?
C9 H9 0.9500 . ?
C9 C8 1.3814(15) . ?
C8 H8 0.9500 . ?
C10 H10a 0.9900 . ?
C10 H10b 0.9900 . ?
C10 C11 1.5221(18) . ?
C11 H11a 0.9800 . ?
C11 H11b 0.9800 . ?
C11 H11c 0.9800 . ?
C12 H12a 0.9900 . ?
C12 H12b 0.9900 . ?
C12 C13 1.519(2) . ?
C13 H13a 0.9800 . ?
C13 H13b 0.9800 . ?
C13 H13c 0.9800 . ?

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
C5 O1 H1 97.2(17) . . ?
H1b C1 H1a 107.9 . . ?
N1 C1 H1a 109.25(5) 2_665 . ?
N1 C1 H1b 109.25(7) 2_665 . ?
C2 C1 H1a 109.25(6) . . ?
C2 C1 H1b 109.25(6) . . ?
C2 C1 N1 111.82(10) . 2_665 ?
C1 N1 C1 111.14(7) . 3_565 ?
C1 N1 C1 111.14(6) 2_665 3_565 ?
C1 N1 C1 111.14(7) 2_665 . ?
C3 N2 C2 119.42(11) . . ?
N2 C2 C1 110.41(10) . . ?
H2a C2 C1 109.57(6) . . ?
H2a C2 N2 109.57(6) . . ?
H2b C2 C1 109.57(6) . . ?
H2b C2 N2 109.57(7) . . ?
H2b C2 H2a 108.1 . . ?
C10 N3 C7 121.53(10) . . ?
C12 N3 C7 120.54(10) . . ?
C12 N3 C10 117.77(10) . . ?
H3 C3 N2 119.23(7) . . ?
C4 C3 N2 121.55(11) . . ?
C4 C3 H3 119.23(6) . . ?
C4 C5 O1 120.95(10) . . ?
C6 C5 O1 117.92(10) . . ?
C6 C5 C4 121.12(10) . . ?
C5 C4 C3 120.80(10) . . ?
C9 C4 C3 121.86(11) . . ?
C9 C4 C5 117.33(10) . . ?
H6 C6 C5 119.43(6) . . ?
C7 C6 C5 121.14(10) . . ?
C7 C6 H6 119.43(6) . . ?
C6 C7 N3 120.83(10) . . ?
C8 C7 N3 121.33(11) . . ?
C8 C7 C6 117.81(10) . . ?
H9 C9 C4 118.93(7) . . ?
C8 C9 C4 122.14(11) . . ?
C8 C9 H9 118.93(7) . . ?
C9 C8 C7 120.34(10) . . ?
H8 C8 C7 119.83(7) . . ?
H8 C8 C9 119.83(7) . . ?
H10a C10 N3 108.74(6) . . ?
H10b C10 N3 108.74(6) . . ?
H10b C10 H10a 107.6 . . ?
C11 C10 N3 114.04(10) . . ?
C11 C10 H10a 108.74(7) . . ?
C11 C10 H10b 108.74(7) . . ?
H11a C11 C10 109.5 . . ?
H11b C11 C10 109.5 . . ?
H11b C11 H11a 109.5 . . ?
H11c C11 C10 109.5 . . ?
H11c C11 H11a 109.5 . . ?
H11c C11 H11b 109.5 . . ?
H12a C12 N3 108.68(7) . . ?
H12b C12 N3 108.68(7) . . ?
H12b C12 H12a 107.6 . . ?
C13 C12 N3 114.30(12) . . ?
C13 C12 H12a 108.68(8) . . ?
C13 C12 H12b 108.68(7) . . ?
H13a C13 C12 109.5 . . ?
H13b C13 C12 109.5 . . ?
H13b C13 H13a 109.5 . . ?
H13c C13 C12 109.5 . . ?
H13c C13 H13a 109.5 . . ?
H13c C13 H13b 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O1 H1 1 0.8700 0.0100 -0.0058
####################################################################### 
# 
# 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_p-3c1_a
_database_code_depnum_ccdc_archive 'CCDC 1515526'
_audit_update_record             
;
2017-08-18 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_audit_creation_date             2017-08-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '1(C39 H54 Eu1 N7 O3), 1.5(H2O)'
_chemical_formula_sum            'C39 H57 Eu N7 O4.5'
_chemical_formula_weight         847.88
_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           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'
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'
'-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                   12.3525(17)
_cell_length_b                   12.3525(17)
_cell_length_c                   31.422(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4152.2(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2824
_cell_measurement_temperature    100
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2.6
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1696
_exptl_crystal_preparation       'slow evaporation from MeOH and DCM mixture'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            54585
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         1.904
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'ADSC Q315r CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_source                   'MX1 Australian Synchrotron'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2264
_reflns_number_total             2831
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'ShelXL least squares'
_computing_data_collection       'Blue Ice'
_computing_data_reduction        XDS
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.039
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2831
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0608
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0407P)²+22.0586P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1438
_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
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C12(H12A,H12B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C8(H8)
3.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_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
Eu1 Eu 0.333333 0.666667 0.28508(2) 0.04404(19) Uani 1 3 d S TU P . .
O1 O 0.3553(4) 0.5277(4) 0.32469(14) 0.0487(10) Uani 1 1 d . U . . .
C1 C 0.2504(6) 0.5366(6) 0.1815(2) 0.0531(15) Uani 1 1 d . U . . .
H1A H 0.299806 0.494017 0.178459 0.064 Uiso 1 1 calc R . . . .
H1B H 0.217231 0.539343 0.153031 0.064 Uiso 1 1 calc R . . . .
N1 N 0.333333 0.666667 0.1968(3) 0.0506(19) Uani 1 3 d S TU P . .
N2 N 0.1948(4) 0.4574(5) 0.25247(16) 0.0445(11) Uani 1 1 d . U . . .
C2 C 0.1428(6) 0.4628(6) 0.2114(2) 0.0539(15) Uani 1 1 d . U . . .
H2A H 0.091944 0.503904 0.214478 0.065 Uiso 1 1 calc R . . . .
H2B H 0.088594 0.377378 0.200203 0.065 Uiso 1 1 calc R . . . .
C3 C 0.1685(6) 0.3481(6) 0.2661(2) 0.0521(14) Uani 1 1 d . U . . .
H3 H 0.113419 0.279351 0.248754 0.063 Uiso 1 1 calc R . . . .
N3 N 0.3235(8) 0.1982(7) 0.4126(2) 0.088(2) Uani 1 1 d . U . . .
C5 C 0.3042(5) 0.4085(6) 0.3318(2) 0.0451(13) Uani 1 1 d . U . . .
C4 C 0.2122(5) 0.3179(6) 0.3041(2) 0.0455(13) Uani 1 1 d . U . . .
C7 C 0.2867(7) 0.2389(7) 0.3776(2) 0.0574(16) Uani 1 1 d . U . . .
C6 C 0.3384(6) 0.3658(6) 0.3682(2) 0.0544(15) Uani 1 1 d . U . . .
H6 H 0.398729 0.425541 0.387105 0.065 Uiso 1 1 calc R . . . .
C9 C 0.1635(6) 0.1907(6) 0.3137(2) 0.0568(16) Uani 1 1 d . U . . .
H9 H 0.105307 0.129813 0.294576 0.068 Uiso 1 1 calc R . . . .
C8 C 0.1968(6) 0.1514(6) 0.3495(2) 0.0601(17) Uani 1 1 d . U . . .
H8 H 0.158967 0.064538 0.355423 0.072 Uiso 1 1 calc R . . . .
C10 C 0.4371(14) 0.2906(11) 0.4392(3) 0.121(4) Uani 1 1 d . U . . .
H10A H 0.478441 0.248082 0.452511 0.146 Uiso 1 1 calc R . . . .
H10B H 0.498691 0.360397 0.421410 0.146 Uiso 1 1 calc R . . . .
C11 C 0.3883(18) 0.3327(16) 0.4693(4) 0.167(6) Uani 1 1 d . U . . .
H11A H 0.337979 0.363884 0.455558 0.251 Uiso 1 1 calc GR . . . .
H11B H 0.456258 0.400538 0.485463 0.251 Uiso 1 1 calc GR . . . .
H11C H 0.335394 0.264201 0.488680 0.251 Uiso 1 1 calc GR . . . .
C12 C 0.2598(11) 0.0665(9) 0.4257(3) 0.096(3) Uani 1 1 d . U . . .
H12A H 0.170070 0.027934 0.418304 0.115 Uiso 1 1 calc R . . . .
H12B H 0.265829 0.062799 0.456979 0.115 Uiso 1 1 calc R . . . .
C13 C 0.3114(14) -0.0106(13) 0.4055(4) 0.143(5) Uani 1 1 d . U . . .
H13A H 0.269527 -0.094675 0.417894 0.215 Uiso 1 1 calc GR . . . .
H13B H 0.401432 0.029740 0.410887 0.215 Uiso 1 1 calc GR . . . .
H13C H 0.296310 -0.016524 0.374736 0.215 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.244(4) 3_565 ?
Eu1 O1 2.244(4) 2_665 ?
Eu1 O1 2.244(4) . ?
Eu1 N1 2.772(9) . ?
Eu1 N2 2.497(5) 3_565 ?
Eu1 N2 2.497(5) . ?
Eu1 N2 2.497(5) 2_665 ?
O1 C5 1.299(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 N1 1.489(7) . ?
C1 C2 1.507(9) . ?
N2 C2 1.458(8) . ?
N2 C3 1.293(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3 0.9500 . ?
C3 C4 1.434(9) . ?
N3 C7 1.376(9) . ?
N3 C10 1.540(14) . ?
N3 C12 1.467(11) . ?
C5 C4 1.425(8) . ?
C5 C6 1.411(9) . ?
C4 C9 1.405(8) . ?
C7 C6 1.397(9) . ?
C7 C8 1.408(10) . ?
C6 H6 0.9500 . ?
C9 H9 0.9500 . ?
C9 C8 1.368(10) . ?
C8 H8 0.9500 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.357(16) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.524(15) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

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 O1 92.21(16) 3_565 2_665 ?
O1 Eu1 O1 92.21(16) 3_565 . ?
O1 Eu1 O1 92.21(16) 2_665 . ?
O1 Eu1 N1 123.69(11) 2_665 . ?
O1 Eu1 N1 123.69(11) . . ?
O1 Eu1 N1 123.69(11) 3_565 . ?
O1 Eu1 N2 89.75(16) 2_665 3_565 ?
O1 Eu1 N2 73.61(15) 2_665 2_665 ?
O1 Eu1 N2 165.76(16) 3_565 2_665 ?
O1 Eu1 N2 165.76(16) 2_665 . ?
O1 Eu1 N2 73.61(15) . . ?
O1 Eu1 N2 165.76(16) . 3_565 ?
O1 Eu1 N2 73.61(15) 3_565 3_565 ?
O1 Eu1 N2 89.75(16) 3_565 . ?
O1 Eu1 N2 89.75(16) . 2_665 ?
N2 Eu1 N1 65.78(12) 3_565 . ?
N2 Eu1 N1 65.78(12) 2_665 . ?
N2 Eu1 N1 65.78(12) . . ?
N2 Eu1 N2 104.33(14) 3_565 . ?
N2 Eu1 N2 104.33(14) 3_565 2_665 ?
N2 Eu1 N2 104.33(14) . 2_665 ?
C5 O1 Eu1 141.9(4) . . ?
H1A C1 H1B 107.9 . . ?
N1 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
N1 C1 C2 111.9(6) . . ?
C2 C1 H1A 109.2 . . ?
C2 C1 H1B 109.2 . . ?
C1 N1 Eu1 108.9(4) 3_565 . ?
C1 N1 Eu1 108.9(4) . . ?
C1 N1 Eu1 109.0(4) 2_665 . ?
C1 N1 C1 110.0(4) 3_565 . ?
C1 N1 C1 110.0(4) 3_565 2_665 ?
C1 N1 C1 110.0(4) . 2_665 ?
C2 N2 Eu1 113.9(4) . . ?
C3 N2 Eu1 129.0(4) . . ?
C3 N2 C2 117.0(5) . . ?
C1 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
N2 C2 C1 107.8(5) . . ?
N2 C2 H2A 110.2 . . ?
N2 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
N2 C3 H3 116.0 . . ?
N2 C3 C4 128.0(6) . . ?
C4 C3 H3 116.0 . . ?
C7 N3 C10 120.5(7) . . ?
C7 N3 C12 122.4(8) . . ?
C12 N3 C10 117.0(7) . . ?
O1 C5 C4 122.0(6) . . ?
O1 C5 C6 119.8(6) . . ?
C6 C5 C4 118.2(6) . . ?
C5 C4 C3 124.1(6) . . ?
C9 C4 C3 117.6(6) . . ?
C9 C4 C5 118.3(6) . . ?
N3 C7 C6 122.0(7) . . ?
N3 C7 C8 119.9(7) . . ?
C6 C7 C8 118.1(6) . . ?
C5 C6 H6 118.8 . . ?
C7 C6 C5 122.5(6) . . ?
C7 C6 H6 118.8 . . ?
C4 C9 H9 118.7 . . ?
C8 C9 C4 122.5(7) . . ?
C8 C9 H9 118.7 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.3(6) . . ?
C9 C8 H8 119.8 . . ?
N3 C10 H10A 110.9 . . ?
N3 C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
C11 C10 N3 104.4(14) . . ?
C11 C10 H10A 110.9 . . ?
C11 C10 H10B 110.9 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 H12A 108.6 . . ?
N3 C12 H12B 108.6 . . ?
N3 C12 C13 114.6(10) . . ?
H12A C12 H12B 107.6 . . ?
C13 C12 H12A 108.6 . . ?
C13 C12 H12B 108.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 72.4 7.1 ?
2 0.000 0.000 0.500 72.4 7.1 ?
3 0.333 0.667 0.447 102.9 30.5 ?
4 0.333 0.667 0.947 102.9 30.6 ?
5 0.667 0.333 0.553 102.9 30.9 ?
6 0.667 0.333 0.053 102.9 30.9 ?

_olex2_submission_special_instructions 'No special instructions were received'
