# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_p140613a
_audit_block_doi                 10.5517/cc14nfqy
_database_code_depnum_ccdc_archive 'CCDC 1062330'
_audit_update_record             
;
2015-04-29 deposited with the CCDC.
2015-06-08 downloaded from the CCDC.
;
_audit_creation_date             2015-04-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.25(C64 Gd12 Mn8 N192 O16), 12(H2 O)'
_chemical_formula_sum            'C16 H24 Gd3 Mn2 N48 O16'
_chemical_formula_weight         1726.46
_chemical_melting_point          ?
_chemical_oxdiff_formula         C1GD1MN1
_chemical_oxdiff_usercomment     HHC-GD-MN
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'
Mn Mn 0.3368 0.7283 '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'

_space_group_crystal_system      cubic
_space_group_IT_number           222
_space_group_name_H-M_alt        'P n -3 n'
_space_group_name_Hall           '-P 4a 2bc 3'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y+1/2, x, z'
3 '-x+1/2, -y+1/2, z'
4 'y, -x+1/2, z'
5 'x, -z+1/2, y'
6 'x, -y+1/2, -z+1/2'
7 'x, z, -y+1/2'
8 'z, y, -x+1/2'
9 '-x+1/2, y, -z+1/2'
10 '-z+1/2, y, x'
11 'z, x, y'
12 'y, z, x'
13 '-y+1/2, -z+1/2, x'
14 'z, -x+1/2, -y+1/2'
15 '-y+1/2, z, -x+1/2'
16 '-z+1/2, -x+1/2, y'
17 '-z+1/2, x, -y+1/2'
18 'y, -z+1/2, -x+1/2'
19 'y, x, -z+1/2'
20 '-y+1/2, -x+1/2, -z+1/2'
21 '-x+1/2, z, y'
22 '-x+1/2, -z+1/2, -y+1/2'
23 'z, -y+1/2, x'
24 '-z+1/2, -y+1/2, -x+1/2'
25 '-x, -y, -z'
26 'y-1/2, -x, -z'
27 'x-1/2, y-1/2, -z'
28 '-y, x-1/2, -z'
29 '-x, z-1/2, -y'
30 '-x, y-1/2, z-1/2'
31 '-x, -z, y-1/2'
32 '-z, -y, x-1/2'
33 'x-1/2, -y, z-1/2'
34 'z-1/2, -y, -x'
35 '-z, -x, -y'
36 '-y, -z, -x'
37 'y-1/2, z-1/2, -x'
38 '-z, x-1/2, y-1/2'
39 'y-1/2, -z, x-1/2'
40 'z-1/2, x-1/2, -y'
41 'z-1/2, -x, y-1/2'
42 '-y, z-1/2, x-1/2'
43 '-y, -x, z-1/2'
44 'y-1/2, x-1/2, z-1/2'
45 'x-1/2, -z, -y'
46 'x-1/2, z-1/2, y-1/2'
47 '-z, y-1/2, -x'
48 'z-1/2, y-1/2, x-1/2'

_cell_length_a                   17.1065(12)
_cell_length_b                   17.1065(12)
_cell_length_c                   17.1065(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5005.9(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    490
_cell_measurement_temperature    130.80(14)
_cell_measurement_theta_max      24.3950
_cell_measurement_theta_min      3.3790
_exptl_absorpt_coefficient_mu    4.523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.291
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            4051
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.92
_diffrn_ambient_temperature      130.80(14)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0401191000
_diffrn_orient_matrix_UB_12      0.0009618000
_diffrn_orient_matrix_UB_13      0.0106018000
_diffrn_orient_matrix_UB_21      0.0061293000
_diffrn_orient_matrix_UB_22      0.0316029000
_diffrn_orient_matrix_UB_23      -0.0260776000
_diffrn_orient_matrix_UB_31      -0.0087172000
_diffrn_orient_matrix_UB_32      0.0267660000
_diffrn_orient_matrix_UB_33      0.0304325000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                469
_reflns_number_total             753
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         4.055
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.221
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         753
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0550
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0860P)²+37.7430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1824
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Riding coordinates:
 Gd1(O2,H2A,H2B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Gd1 Gd 0.09161(5) 0.2500 0.2500 0.0133(3) Uani 1 d . . 4 S T P
O2 O -0.18167(5) 0.5815 0.2072 0.079(4) Uani 1 d . . 1 R . .
H2A H -0.2014 0.5871 0.1616 0.119 Uiso 1 d . . 1 R . .
H2B H -0.1644 0.5350 0.2096 0.119 Uiso 1 d . . 1 R . .
C1 C 0.1106(6) 0.3894(6) 0.1106(6) 0.015(3) Uani 1 d . . 3 S T P
N3 N -0.0620(5) 0.3956(5) 0.2294(5) 0.028(2) Uani 1 d . . 1 . . .
O1 O 0.1576(3) 0.3424(3) 0.1576(3) 0.013(2) Uani 1 d . . 3 S T P
N2 N -0.0793(5) 0.4461(5) 0.1738(5) 0.030(2) Uani 1 d . . 1 . . .
N4 N 0.0108(5) 0.3670(5) 0.2146(5) 0.0158(19) Uani 1 d . . 1 . . .
N1 N -0.0209(5) 0.4504(5) 0.1211(5) 0.023(2) Uani 1 d . . 1 . . .
C2 C 0.0328(5) 0.4034(6) 0.1495(6) 0.017(2) Uani 1 d . . 1 . . .
Mn1 Mn 0.0000 0.5000 0.0000 0.0249(9) Uani 1 d . . 6 S T P

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Gd1 0.0128(5) 0.0136(3) 0.0136(3) 0.000 0.000 0.000
O2 0.069(7) 0.088(8) 0.081(8) 0.008(7) -0.022(7) 0.011(7)
C1 0.015(3) 0.015(3) 0.015(3) -0.006(4) 0.006(4) -0.006(4)
N3 0.022(5) 0.027(5) 0.035(6) 0.002(5) 0.005(4) 0.003(5)
O1 0.013(2) 0.013(2) 0.013(2) 0.004(3) -0.004(3) 0.004(3)
N2 0.034(5) 0.028(5) 0.028(5) 0.011(5) -0.004(5) 0.002(5)
N4 0.013(4) 0.017(4) 0.018(4) -0.003(4) 0.003(4) 0.003(4)
N1 0.019(4) 0.024(5) 0.025(5) 0.006(4) 0.011(4) 0.003(4)
C2 0.010(5) 0.016(5) 0.026(6) 0.003(5) 0.001(5) 0.002(5)
Mn1 0.0249(9) 0.0249(9) 0.0249(9) 0.0036(10) -0.0036(10) 0.0036(10)

_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
Gd1 Gd1 3.8317(13) 4 ?
Gd1 Gd1 3.8317(13) 2 ?
Gd1 Gd1 3.8317(13) 10 ?
Gd1 Gd1 3.8317(13) 8 ?
Gd1 O1 2.504(5) 2 ?
Gd1 O1 2.504(5) . ?
Gd1 O1 2.504(5) 5 ?
Gd1 O1 2.504(5) 6 ?
Gd1 N4 2.507(8) 5 ?
Gd1 N4 2.507(8) 6 ?
Gd1 N4 2.507(8) 7 ?
Gd1 N4 2.507(8) . ?
C1 O1 1.39(2) . ?
C1 C2 1.506(11) 14 ?
C1 C2 1.506(11) . ?
C1 C2 1.506(11) 13 ?
N3 N2 1.318(12) . ?
N3 N4 1.361(12) . ?
O1 Gd1 2.504(5) 4 ?
O1 Gd1 2.504(5) 10 ?
N2 N1 1.348(12) . ?
N4 C2 1.332(13) . ?
N1 C2 1.314(12) . ?
N1 Mn1 2.267(8) . ?
Mn1 N1 2.267(8) 13 ?
Mn1 N1 2.267(8) 38_565 ?
Mn1 N1 2.267(8) 25_565 ?
Mn1 N1 2.267(8) 37_565 ?
Mn1 N1 2.267(8) 14 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Gd1 Gd1 Gd1 60.0 8 4 ?
Gd1 Gd1 Gd1 60.0 2 10 ?
Gd1 Gd1 Gd1 90.0 8 10 ?
Gd1 Gd1 Gd1 90.0 4 2 ?
Gd1 Gd1 Gd1 60.0 8 2 ?
Gd1 Gd1 Gd1 60.0 4 10 ?
O1 Gd1 Gd1 40.09(13) 5 4 ?
O1 Gd1 Gd1 97.34(18) . 2 ?
O1 Gd1 Gd1 40.09(13) 6 8 ?
O1 Gd1 Gd1 40.09(13) 2 10 ?
O1 Gd1 Gd1 97.34(18) 5 2 ?
O1 Gd1 Gd1 97.34(18) 6 10 ?
O1 Gd1 Gd1 97.34(18) 2 8 ?
O1 Gd1 Gd1 97.34(18) 6 4 ?
O1 Gd1 Gd1 97.34(18) . 8 ?
O1 Gd1 Gd1 97.34(18) 5 10 ?
O1 Gd1 Gd1 40.09(13) 6 2 ?
O1 Gd1 Gd1 97.34(18) 2 4 ?
O1 Gd1 Gd1 40.09(13) 2 2 ?
O1 Gd1 Gd1 40.09(13) 5 8 ?
O1 Gd1 Gd1 40.09(13) . 10 ?
O1 Gd1 Gd1 40.09(13) . 4 ?
O1 Gd1 O1 126.4(4) 5 2 ?
O1 Gd1 O1 78.28(17) 2 . ?
O1 Gd1 O1 78.28(17) 5 . ?
O1 Gd1 O1 78.28(17) 2 6 ?
O1 Gd1 O1 78.28(17) 5 6 ?
O1 Gd1 O1 126.4(4) . 6 ?
O1 Gd1 N4 65.9(3) 5 5 ?
O1 Gd1 N4 65.9(3) 2 7 ?
O1 Gd1 N4 154.8(2) 5 7 ?
O1 Gd1 N4 126.9(2) . 5 ?
O1 Gd1 N4 126.9(2) 5 6 ?
O1 Gd1 N4 84.1(2) . 7 ?
O1 Gd1 N4 84.1(2) 5 . ?
O1 Gd1 N4 126.9(2) 2 . ?
O1 Gd1 N4 154.8(2) 6 . ?
O1 Gd1 N4 126.9(2) 6 7 ?
O1 Gd1 N4 154.8(2) 2 5 ?
O1 Gd1 N4 65.9(3) . . ?
O1 Gd1 N4 84.1(2) 6 5 ?
O1 Gd1 N4 154.8(2) . 6 ?
O1 Gd1 N4 65.9(3) 6 6 ?
O1 Gd1 N4 84.1(2) 2 6 ?
N4 Gd1 Gd1 124.09(19) 7 4 ?
N4 Gd1 Gd1 162.67(18) . 2 ?
N4 Gd1 Gd1 79.93(19) . 4 ?
N4 Gd1 Gd1 162.67(18) 7 8 ?
N4 Gd1 Gd1 102.67(18) 5 4 ?
N4 Gd1 Gd1 162.67(18) 5 10 ?
N4 Gd1 Gd1 102.67(18) 7 2 ?
N4 Gd1 Gd1 162.67(18) 6 4 ?
N4 Gd1 Gd1 124.09(19) 6 10 ?
N4 Gd1 Gd1 79.93(19) 7 10 ?
N4 Gd1 Gd1 102.67(18) . 10 ?
N4 Gd1 Gd1 79.93(19) 6 2 ?
N4 Gd1 Gd1 124.09(19) . 8 ?
N4 Gd1 Gd1 79.93(19) 5 8 ?
N4 Gd1 Gd1 102.67(18) 6 8 ?
N4 Gd1 Gd1 124.09(19) 5 2 ?
N4 Gd1 N4 72.30(18) 7 6 ?
N4 Gd1 N4 72.30(18) 5 . ?
N4 Gd1 N4 113.1(4) 6 . ?
N4 Gd1 N4 113.1(4) 7 5 ?
N4 Gd1 N4 72.30(18) 7 . ?
N4 Gd1 N4 72.30(18) 6 5 ?
O1 C1 C2 110.3(7) . 13 ?
O1 C1 C2 110.3(7) . 14 ?
O1 C1 C2 110.3(7) . . ?
C2 C1 C2 108.6(8) 13 . ?
C2 C1 C2 108.6(8) 13 14 ?
C2 C1 C2 108.6(8) 14 . ?
N2 N3 N4 107.9(8) . . ?
Gd1 O1 Gd1 99.8(3) 10 . ?
Gd1 O1 Gd1 99.8(3) 4 10 ?
Gd1 O1 Gd1 99.8(3) 4 . ?
C1 O1 Gd1 118.0(2) . 10 ?
C1 O1 Gd1 118.0(2) . . ?
C1 O1 Gd1 118.0(2) . 4 ?
N3 N2 N1 110.6(8) . . ?
N3 N4 Gd1 138.3(6) . . ?
C2 N4 Gd1 114.8(6) . . ?
C2 N4 N3 104.2(8) . . ?
N2 N1 Mn1 138.5(7) . . ?
C2 N1 N2 103.8(8) . . ?
C2 N1 Mn1 117.1(7) . . ?
N4 C2 C1 123.0(10) . . ?
N1 C2 C1 123.5(10) . . ?
N1 C2 N4 113.4(9) . . ?
N1 Mn1 N1 98.0(3) 25_565 13 ?
N1 Mn1 N1 82.0(3) 14 . ?
N1 Mn1 N1 82.0(3) 37_565 25_565 ?
N1 Mn1 N1 98.0(3) 38_565 . ?
N1 Mn1 N1 98.0(3) 14 25_565 ?
N1 Mn1 N1 82.0(3) 38_565 37_565 ?
N1 Mn1 N1 180.0 38_565 14 ?
N1 Mn1 N1 82.0(3) 14 13 ?
N1 Mn1 N1 98.0(3) 37_565 . ?
N1 Mn1 N1 180.0(4) 37_565 13 ?
N1 Mn1 N1 82.0(3) 38_565 25_565 ?
N1 Mn1 N1 82.0(3) . 13 ?
N1 Mn1 N1 180.0(4) . 25_565 ?
N1 Mn1 N1 98.0(3) 37_565 14 ?
N1 Mn1 N1 98.0(3) 38_565 13 ?

