# 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 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1543666'
_audit_update_record             
;
2017-12-14 deposited with the CCDC.
2017-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H40 N12 Nd4 O52'
_chemical_formula_weight         1809.56

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

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

_cell_length_a                   9.639(3)
_cell_length_b                   8.491(2)
_cell_length_c                   17.931(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.498(3)
_cell_angle_gamma                90
_cell_volume                     1455.1(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4612
_cell_measurement_theta_min      3.21
_cell_measurement_theta_max      29.15

_exptl_crystal_description       block
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_F_000             876
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    3.638
_shelx_estimated_absorpt_T_min   0.429
_shelx_estimated_absorpt_T_max   0.690
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.429
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_absorpt_special_details   'Bruker SADABS'
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX-II CCD'
_diffrn_measurement_method       'Omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6914
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.313
_diffrn_reflns_theta_max         29.301
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             1941
_reflns_number_gt                1911
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0228P)²+28.8620P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef       0.0034(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1941
_refine_ls_number_parameters     164
_refine_ls_number_restraints     104
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0376
_refine_ls_wR_factor_ref         0.0955
_refine_ls_wR_factor_gt          0.0951
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd01 Nd 0.30247(3) 0.500000 0.21259(2) 0.01682(16) Uani 1 2 d S T P . .
O002 O 0.3372(8) 0.500000 0.3526(4) 0.0427(16) Uani 1 2 d S T P . .
N003 N 0.8355(6) 0.500000 0.3511(3) 0.0218(12) Uani 1 2 d S T P . .
H00A H 0.842744 0.415741 0.380892 0.026 Uiso 0.5 1 calc R U P . .
H00B H 0.842744 0.584259 0.380892 0.026 Uiso 0.5 1 calc R U P . .
C004 C 0.6933(7) 0.500000 0.3092(5) 0.0240(14) Uani 1 2 d S T P . .
H00C H 0.687769 0.414059 0.273272 0.029 Uiso 0.5 1 calc R U P B .
H00D H 0.628051 0.476517 0.344511 0.029 Uiso 0.5 1 calc R U P . .
C005 C 0.9569(7) 0.500000 0.3091(5) 0.0259(15) Uani 1 2 d S T P . .
H00E H 0.945471 0.586960 0.273766 0.031 Uiso 0.5 1 calc R U P B .
H00F H 1.039491 0.522073 0.344542 0.031 Uiso 0.5 1 calc R U P . .
O007 O 0.9029(7) 0.2472(9) 0.2683(5) 0.0264(15) Uani 0.5 1 d . . P A -1
O009 O 0.7274(7) 0.7549(9) 0.2683(4) 0.0249(15) Uani 0.5 1 d . . P B -1
O00A O 1.0939(8) 0.3581(11) 0.2374(5) 0.0343(19) Uani 0.5 1 d . . P A -1
C00B C 0.6457(10) 0.6402(11) 0.2691(5) 0.0183(17) Uani 0.5 1 d . . P B -1
O00C O 0.5197(8) 0.6437(10) 0.2364(5) 0.0316(17) Uani 0.5 1 d . . P B -1
C00E C 0.9843(10) 0.3608(11) 0.2681(5) 0.0199(18) Uani 0.5 1 d . . P A -1
N2 N 0.3603(15) 0.718(2) 0.0969(10) 0.067(3) Uani 0.5 1 d D U P B 1
O3 O 0.4638(10) 0.6146(13) 0.1217(6) 0.050(2) Uani 0.5 1 d D U P B 1
O4 O 0.390(2) 0.838(3) 0.0509(11) 0.097(5) Uani 0.5 1 d D U P B 1
O5 O 0.2319(16) 0.712(2) 0.1149(9) 0.070(3) Uani 0.5 1 d D U P B 1
N1 N 0.1847(15) 0.717(2) 0.0963(10) 0.070(3) Uani 0.5 1 d D U P B 2
O2 O 0.3229(16) 0.712(2) 0.1144(9) 0.067(3) Uani 0.5 1 d D U P B 2
O6 O 0.133(2) 0.836(2) 0.0510(11) 0.104(5) Uani 0.5 1 d D U P B 2
O7 O 0.0942(10) 0.6121(14) 0.1215(6) 0.054(2) Uani 0.5 1 d D U P B 2
O0AA O 0.358(3) 0.936(2) 0.0414(13) 0.129(8) Uani 0.5 1 d . . P C -2
O1AA O 0.173(2) 0.921(3) 0.0434(13) 0.128(8) Uani 0.5 1 d . U P 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
Nd01 O00C 2.413(8) . ?
Nd01 O002 2.489(6) . ?
Nd01 O5 2.544(16) . ?
Nd01 O5 2.544(16) 6_565 ?
Nd01 O2 2.545(15) . ?
Nd01 O2 2.545(15) 6_565 ?
Nd01 O3 2.585(9) 6_565 ?
Nd01 O3 2.585(9) . ?
Nd01 O7 2.598(9) . ?
Nd01 O7 2.598(9) 6_565 ?
Nd01 N2 2.888(15) . ?
Nd01 N2 2.888(15) 6_565 ?
N003 C004 1.475(9) . ?
N003 C005 1.472(9) . ?
N003 H00A 0.8900 . ?
N003 H00B 0.8900 . ?
C004 C00B 1.435(10) . ?
C004 H00C 0.9700 . ?
C004 H00D 0.9700 . ?
C004 H00C 0.9700 6_565 ?
C004 H00D 0.9700 6_565 ?
C005 C00E 1.435(11) . ?
C005 H00E 0.9700 . ?
C005 H00F 0.9700 . ?
C005 H00E 0.9701 6_565 ?
C005 H00F 0.9700 6_565 ?
O007 C00E 1.243(12) . ?
O009 C00B 1.253(11) . ?
O00A C00E 1.253(12) . ?
C00B O00C 1.278(12) . ?
N2 O5 1.319(14) . ?
N2 O4 1.364(15) . ?
N2 O3 1.359(14) . ?
N1 O2 1.330(14) . ?
N1 O6 1.353(15) . ?
N1 O7 1.362(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O00C Nd01 O002 79.8(3) . . ?
O00C Nd01 O5 84.9(4) . . ?
O002 Nd01 O5 133.1(4) . . ?
O00C Nd01 O5 128.9(4) . 6_565 ?
O002 Nd01 O5 133.1(4) . 6_565 ?
O5 Nd01 O5 90.3(9) . 6_565 ?
O002 Nd01 O2 133.3(4) . . ?
O00C Nd01 O2 109.7(4) . 6_565 ?
O002 Nd01 O2 133.3(4) . 6_565 ?
O5 Nd01 O2 93.6(5) . 6_565 ?
O5 Nd01 O2 19.9(5) 6_565 6_565 ?
O00C Nd01 O3 73.9(3) . 6_565 ?
O002 Nd01 O3 128.5(3) . 6_565 ?
O5 Nd01 O3 87.8(4) . 6_565 ?
O5 Nd01 O3 55.1(4) 6_565 6_565 ?
O00C Nd01 O3 48.8(3) . . ?
O002 Nd01 O3 128.5(3) . . ?
O5 Nd01 O3 55.1(4) . . ?
O5 Nd01 O3 87.8(4) 6_565 . ?
O3 Nd01 O3 44.2(5) 6_565 . ?
O002 Nd01 O7 128.7(3) . . ?
O2 Nd01 O7 55.2(5) . . ?
O2 Nd01 O7 87.0(4) 6_565 . ?
O00C Nd01 O7 151.4(3) . 6_565 ?
O002 Nd01 O7 128.7(3) . 6_565 ?
O5 Nd01 O7 73.2(5) . 6_565 ?
O5 Nd01 O7 36.1(5) 6_565 6_565 ?
O2 Nd01 O7 87.0(4) . 6_565 ?
O2 Nd01 O7 55.2(5) 6_565 6_565 ?
O3 Nd01 O7 86.8(4) 6_565 6_565 ?
O3 Nd01 O7 102.7(3) . 6_565 ?
O7 Nd01 O7 43.0(5) . 6_565 ?
O00C Nd01 N2 63.8(4) . . ?
O002 Nd01 N2 135.3(4) . . ?
O5 Nd01 N2 27.2(3) . . ?
O5 Nd01 N2 91.1(7) 6_565 . ?
O3 Nd01 N2 66.4(4) 6_565 . ?
O3 Nd01 N2 28.1(3) . . ?
O00C Nd01 N2 101.9(3) . 6_565 ?
O002 Nd01 N2 135.3(4) . 6_565 ?
O5 Nd01 N2 91.1(7) . 6_565 ?
O5 Nd01 N2 27.2(3) 6_565 6_565 ?
O3 Nd01 N2 28.1(3) 6_565 6_565 ?
O3 Nd01 N2 66.4(4) . 6_565 ?
N2 Nd01 N2 79.7(7) . 6_565 ?
C004 N003 C005 119.1(6) . . ?
C004 N003 H00A 107.5 . . ?
C005 N003 H00A 107.5 . . ?
C004 N003 H00B 107.5 . . ?
C005 N003 H00B 107.5 . . ?
H00A N003 H00B 107.0 . . ?
C00B C004 N003 118.1(5) . . ?
C00B C004 H00C 107.8 . . ?
N003 C004 H00C 107.8 . . ?
C00B C004 H00D 107.8 . . ?
N003 C004 H00D 107.8 . . ?
H00C C004 H00D 107.1 . . ?
C00B C004 H00C 19.4(5) . 6_565 ?
N003 C004 H00C 107.8(2) . 6_565 ?
H00C C004 H00C 97.6 . 6_565 ?
H00D C004 H00C 127.2 . 6_565 ?
C00B C004 H00D 88.0(5) . 6_565 ?
N003 C004 H00D 107.8(4) . 6_565 ?
H00C C004 H00D 127.2 . 6_565 ?
H00D C004 H00D 23.7 . 6_565 ?
H00C C004 H00D 107.1 6_565 6_565 ?
C00E C005 N003 118.3(5) . . ?
C00E C005 H00E 107.7 . . ?
N003 C005 H00E 107.7 . . ?
C00E C005 H00F 107.7 . . ?
N003 C005 H00F 107.7 . . ?
H00E C005 H00F 107.1 . . ?
C00E C005 H00E 18.3(5) . 6_565 ?
N003 C005 H00E 107.7(2) . 6_565 ?
H00E C005 H00E 99.1 . 6_565 ?
H00F C005 H00E 126.0 . 6_565 ?
C00E C005 H00F 89.2(5) . 6_565 ?
N003 C005 H00F 107.7(4) . 6_565 ?
H00E C005 H00F 126.0 . 6_565 ?
H00F C005 H00F 22.3 . 6_565 ?
H00E C005 H00F 107.1 6_565 6_565 ?
C00E O007 H00E 23.7(5) . 6_565 ?
O009 C00B O00C 122.5(9) . . ?
O009 C00B C004 119.3(8) . . ?
O00C C00B C004 118.1(8) . . ?
O009 C00B H00C 100.3(12) . 6_565 ?
O00C C00B H00C 130.4(13) . 6_565 ?
C004 C00B H00C 31.8(7) . 6_565 ?
C00B O00C Nd01 145.1(7) . . ?
O007 C00E O00A 123.7(10) . . ?
O007 C00E C005 118.6(8) . . ?
O00A C00E C005 117.6(8) . . ?
O007 C00E H00E 99.5(12) . 6_565 ?
O00A C00E H00E 132.1(14) . 6_565 ?
C005 C00E H00E 30.7(8) . 6_565 ?
O5 N2 O4 116.9(14) . . ?
O5 N2 O3 124.7(13) . . ?
O4 N2 O3 118.4(12) . . ?
O5 N2 Nd01 61.7(9) . . ?
O4 N2 Nd01 171.2(13) . . ?
O3 N2 Nd01 63.5(7) . . ?
N2 O3 Nd01 88.4(7) . . ?
N2 O5 Nd01 91.1(10) . . ?
O2 N1 O6 116.4(14) . . ?
O2 N1 O7 124.5(13) . . ?
O6 N1 O7 119.1(13) . . ?
O2 N1 Nd01 61.4(8) . . ?
O6 N1 Nd01 170.5(13) . . ?
O7 N1 Nd01 63.6(7) . . ?
N1 O2 Nd01 91.3(9) . . ?
N1 O7 Nd01 88.3(7) . . ?

_refine_diff_density_max         1.689
_refine_diff_density_min         -1.993
_refine_diff_density_rms         0.173



