# 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_CuLuvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060773'
_audit_update_record             
;
2017-04-26 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 Cu2 Lu2 N22 O10'
_chemical_formula_weight         1530.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9931(8)
_cell_length_b                   10.7906(9)
_cell_length_c                   13.4208(7)
_cell_angle_alpha                100.423(16)
_cell_angle_beta                 91.737(16)
_cell_angle_gamma                100.596(15)
_cell_volume                     1396.01(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2973
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      26.09

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             754
_exptl_absorpt_coefficient_mu    4.331
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.3989
_exptl_absorpt_correction_T_max  0.7811
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8148
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5473
_reflns_number_gt                4482
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0561P)²+0.1269P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5473
_refine_ls_number_parameters     384
_refine_ls_number_restraints     82
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1029
_refine_ls_wR_factor_gt          0.0945
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.050
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Lu1 Lu -0.06018(2) 0.56012(2) 0.13662(2) 0.03593(11) Uani 1 1 d . . .
Cu1 Cu 0.19288(7) 0.82614(7) 0.20483(7) 0.0426(2) Uani 1 1 d . . .
C1 C -0.0765(6) 0.8510(6) 0.1245(5) 0.0405(15) Uani 1 1 d . . .
C2 C -0.2175(6) 0.7995(6) 0.1024(5) 0.0431(15) Uani 1 1 d . . .
C3 C -0.3090(7) 0.8723(7) 0.0787(6) 0.0522(18) Uani 1 1 d . . .
H3 H -0.4007 0.8353 0.0638 0.063 Uiso 1 1 calc R . .
C4 C -0.2630(8) 1.0019(7) 0.0770(6) 0.0563(19) Uani 1 1 d . . .
H4 H -0.3244 1.0513 0.0605 0.068 Uiso 1 1 calc R . .
C5 C -0.1278(8) 1.0572(7) 0.0997(6) 0.0562(19) Uani 1 1 d . . .
H5 H -0.0987 1.1439 0.0986 0.067 Uiso 1 1 calc R . .
C6 C -0.0329(7) 0.9848(6) 0.1246(6) 0.0471(16) Uani 1 1 d . . .
C7 C 0.1073(8) 1.0475(7) 0.1463(6) 0.0531(18) Uani 1 1 d . . .
H7 H 0.1285 1.1315 0.1358 0.064 Uiso 1 1 calc R . .
C8 C 0.3426(8) 1.0904(8) 0.1894(7) 0.069(2) Uani 1 1 d . . .
H8A H 0.3291 1.1761 0.1852 0.083 Uiso 1 1 calc R . .
H8B H 0.3957 1.0623 0.1334 0.083 Uiso 1 1 calc R . .
C9 C 0.4220(7) 1.0961(7) 0.2874(6) 0.0520(18) Uani 1 1 d . . .
C10 C 0.5493(8) 1.2053(8) 0.2902(7) 0.081(3) Uani 1 1 d . . .
H10A H 0.5200 1.2852 0.2901 0.121 Uiso 1 1 calc R . .
H10B H 0.5997 1.1855 0.2315 0.121 Uiso 1 1 calc R . .
H10C H 0.6065 1.2123 0.3505 0.121 Uiso 1 1 calc R . .
C11 C 0.3427(9) 1.1287(8) 0.3796(7) 0.085(3) Uani 1 1 d . . .
H11A H 0.3998 1.1363 0.4400 0.128 Uiso 1 1 calc R . .
H11B H 0.2643 1.0618 0.3783 0.128 Uiso 1 1 calc R . .
H11C H 0.3137 1.2085 0.3789 0.128 Uiso 1 1 calc R . .
C12 C 0.4738(7) 0.9729(7) 0.2859(7) 0.063(2) Uani 1 1 d . . .
H12A H 0.5223 0.9556 0.2249 0.076 Uiso 1 1 calc R . .
H12B H 0.5388 0.9850 0.3436 0.076 Uiso 1 1 calc R . .
C13 C 0.3959(7) 0.7819(7) 0.3441(6) 0.0540(19) Uani 1 1 d . . .
H13 H 0.4808 0.8065 0.3796 0.065 Uiso 1 1 calc R . .
C14 C 0.3156(7) 0.6610(7) 0.3595(6) 0.0491(17) Uani 1 1 d . . .
C15 C 0.3606(9) 0.6035(8) 0.4357(7) 0.070(2) Uani 1 1 d . . .
H15 H 0.4427 0.6420 0.4724 0.084 Uiso 1 1 calc R . .
C16 C 0.2891(10) 0.4931(9) 0.4588(7) 0.078(3) Uani 1 1 d . . .
H16 H 0.3202 0.4586 0.5118 0.093 Uiso 1 1 calc R . .
C17 C 0.1675(9) 0.4327(8) 0.4010(7) 0.065(2) Uani 1 1 d . . .
H17 H 0.1169 0.3574 0.4154 0.078 Uiso 1 1 calc R . .
C18 C 0.1238(7) 0.4847(6) 0.3237(5) 0.0431(15) Uani 1 1 d . . .
C19 C 0.1930(6) 0.6003(6) 0.3018(5) 0.0414(15) Uani 1 1 d . . .
C20 C -0.3966(7) 0.6189(8) 0.1182(7) 0.068(2) Uani 1 1 d . . .
H20A H -0.4312 0.6758 0.1702 0.101 Uiso 1 1 calc R . .
H20B H -0.4064 0.5356 0.1359 0.101 Uiso 1 1 calc R . .
H20C H -0.4469 0.6123 0.0548 0.101 Uiso 1 1 calc R . .
C21 C -0.0928(8) 0.3399(8) 0.3006(7) 0.070(2) Uani 1 1 d . . .
H21A H -0.0632 0.2596 0.2968 0.104 Uiso 1 1 calc R . .
H21B H -0.1783 0.3264 0.2618 0.104 Uiso 1 1 calc R . .
H21C H -0.1040 0.3751 0.3702 0.104 Uiso 1 1 calc R . .
C22 C 0.208(2) 0.923(3) 0.564(3) 0.116(7) Uani 0.378(10) 1 d PDU A 1
C22' C 0.0938(18) 0.8631(17) 0.4905(12) 0.094(4) Uani 0.622(10) 1 d PDU A 2
N1 N 0.2072(6) 1.0025(5) 0.1783(5) 0.0505(15) Uani 1 1 d . . .
N2 N 0.3669(5) 0.8592(5) 0.2887(5) 0.0478(14) Uani 1 1 d . . .
N3 N -0.1522(7) 0.6169(7) 0.2939(5) 0.0653(18) Uani 1 1 d . . .
N4 N -0.2112(8) 0.6877(8) 0.3324(6) 0.077(2) Uani 1 1 d U . .
N5 N -0.2640(12) 0.7693(12) 0.3741(9) 0.144(4) Uani 1 1 d U . .
N6 N 0.0823(6) 0.4433(5) 0.0406(4) 0.0464(13) Uani 1 1 d U . .
N7 N 0.1883(8) 0.4172(7) 0.0840(6) 0.0737(19) Uani 1 1 d U . .
N8 N 0.2871(11) 0.3942(11) 0.1239(8) 0.126(4) Uani 1 1 d . . .
N9 N 0.3236(6) 0.7633(6) 0.0529(5) 0.0586(16) Uani 1 1 d . . .
N10 N 0.2771(5) 0.6918(5) -0.0201(5) 0.0388(12) Uani 1 1 d . . .
N11 N 0.2316(6) 0.6205(5) -0.0954(5) 0.0521(15) Uani 1 1 d . . .
O1 O 0.0067(4) 0.7750(4) 0.1426(3) 0.0404(10) Uani 1 1 d . . .
O2 O 0.1428(4) 0.6483(4) 0.2273(3) 0.0392(10) Uani 1 1 d . . .
O3 O -0.2517(4) 0.6696(4) 0.1086(4) 0.0482(12) Uani 1 1 d . . .
O4 O 0.0087(4) 0.4290(4) 0.2599(4) 0.0460(11) Uani 1 1 d . . .
O5 O 0.071(2) 0.918(3) 0.585(2) 0.148(7) Uani 0.378(10) 1 d PDU A 1
O5' O 0.0645(12) 0.8756(13) 0.3909(11) 0.117(5) Uani 0.622(10) 1 d PDU A 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
Lu1 O1 2.278(4) . ?
Lu1 O2 2.285(4) . ?
Lu1 N11 2.316(5) 2_565 ?
Lu1 N6 2.337(5) . ?
Lu1 N3 2.352(7) . ?
Lu1 N6 2.374(6) 2_565 ?
Lu1 O3 2.480(4) . ?
Lu1 O4 2.520(5) . ?
Lu1 Cu1 3.4223(10) . ?
Cu1 O1 1.956(4) . ?
Cu1 O2 1.972(4) . ?
Cu1 N1 1.979(6) . ?
Cu1 N2 1.981(6) . ?
C1 O1 1.317(7) . ?
C1 C2 1.417(9) . ?
C1 C6 1.428(9) . ?
C2 C3 1.375(9) . ?
C2 O3 1.399(8) . ?
C3 C4 1.394(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.374(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.403(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.436(10) . ?
C7 N1 1.282(9) . ?
C7 H7 0.9300 . ?
C8 N1 1.490(8) . ?
C8 C9 1.501(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C12 1.510(11) . ?
C9 C11 1.512(10) . ?
C9 C10 1.561(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.478(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.278(9) . ?
C13 C14 1.453(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.391(11) . ?
C14 C19 1.413(9) . ?
C15 C16 1.364(12) . ?
C15 H15 0.9300 . ?
C16 C17 1.405(12) . ?
C16 H16 0.9300 . ?
C17 C18 1.362(10) . ?
C17 H17 0.9300 . ?
C18 O4 1.385(8) . ?
C18 C19 1.395(9) . ?
C19 O2 1.332(8) . ?
C20 O3 1.468(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O4 1.455(8) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.3949(11) . ?
C22' O5' 1.3953(11) . ?
N3 N4 1.114(9) . ?
N4 N5 1.174(11) . ?
N6 N7 1.293(9) . ?
N6 Lu1 2.374(6) 2_565 ?
N7 N8 1.196(11) . ?
N9 N10 1.157(8) . ?
N10 N11 1.175(8) . ?
N11 Lu1 2.316(5) 2_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Lu1 O2 65.91(15) . . ?
O1 Lu1 N11 147.78(19) . 2_565 ?
O2 Lu1 N11 145.35(19) . 2_565 ?
O1 Lu1 N6 111.44(17) . . ?
O2 Lu1 N6 80.66(18) . . ?
N11 Lu1 N6 87.6(2) 2_565 . ?
O1 Lu1 N3 86.2(2) . . ?
O2 Lu1 N3 83.3(2) . . ?
N11 Lu1 N3 90.2(2) 2_565 . ?
N6 Lu1 N3 148.3(2) . . ?
O1 Lu1 N6 82.33(17) . 2_565 ?
O2 Lu1 N6 120.48(17) . 2_565 ?
N11 Lu1 N6 82.6(2) 2_565 2_565 ?
N6 Lu1 N6 65.5(2) . 2_565 ?
N3 Lu1 N6 145.3(2) . 2_565 ?
O1 Lu1 O3 66.48(14) . . ?
O2 Lu1 O3 127.16(14) . . ?
N11 Lu1 O3 81.96(18) 2_565 . ?
N6 Lu1 O3 138.68(19) . . ?
N3 Lu1 O3 71.9(2) . . ?
N6 Lu1 O3 73.49(18) 2_565 . ?
O1 Lu1 O4 127.79(15) . . ?
O2 Lu1 O4 65.71(14) . . ?
N11 Lu1 O4 80.08(19) 2_565 . ?
N6 Lu1 O4 78.60(18) . . ?
N3 Lu1 O4 69.9(2) . . ?
N6 Lu1 O4 140.61(17) 2_565 . ?
O3 Lu1 O4 137.46(16) . . ?
O1 Lu1 Cu1 33.01(10) . . ?
O2 Lu1 Cu1 33.47(11) . . ?
N11 Lu1 Cu1 178.31(16) 2_565 . ?
N6 Lu1 Cu1 93.06(13) . . ?
N3 Lu1 Cu1 88.35(18) . . ?
N6 Lu1 Cu1 99.05(13) 2_565 . ?
O3 Lu1 Cu1 98.48(10) . . ?
O4 Lu1 Cu1 98.56(10) . . ?
O1 Cu1 O2 78.39(17) . . ?
O1 Cu1 N1 91.7(2) . . ?
O2 Cu1 N1 169.6(2) . . ?
O1 Cu1 N2 168.7(2) . . ?
O2 Cu1 N2 92.9(2) . . ?
N1 Cu1 N2 96.5(2) . . ?
O1 Cu1 Lu1 39.37(11) . . ?
O2 Cu1 Lu1 39.73(12) . . ?
N1 Cu1 Lu1 130.86(17) . . ?
N2 Cu1 Lu1 132.60(18) . . ?
O1 C1 C2 119.4(5) . . ?
O1 C1 C6 123.7(5) . . ?
C2 C1 C6 116.9(6) . . ?
C3 C2 O3 124.7(6) . . ?
C3 C2 C1 122.4(6) . . ?
O3 C2 C1 112.9(5) . . ?
C2 C3 C4 119.4(6) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 120.6(6) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 120.9(7) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.8(6) . . ?
C5 C6 C7 118.4(6) . . ?
C1 C6 C7 121.8(6) . . ?
N1 C7 C6 128.3(7) . . ?
N1 C7 H7 115.8 . . ?
C6 C7 H7 115.8 . . ?
N1 C8 C9 113.5(6) . . ?
N1 C8 H8A 108.9 . . ?
C9 C8 H8A 108.9 . . ?
N1 C8 H8B 108.9 . . ?
C9 C8 H8B 108.9 . . ?
H8A C8 H8B 107.7 . . ?
C8 C9 C12 110.3(6) . . ?
C8 C9 C11 112.8(7) . . ?
C12 C9 C11 111.9(7) . . ?
C8 C9 C10 105.2(6) . . ?
C12 C9 C10 107.2(6) . . ?
C11 C9 C10 109.1(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 114.8(6) . . ?
N2 C12 H12A 108.6 . . ?
C9 C12 H12A 108.6 . . ?
N2 C12 H12B 108.6 . . ?
C9 C12 H12B 108.6 . . ?
H12A C12 H12B 107.6 . . ?
N2 C13 C14 129.4(6) . . ?
N2 C13 H13 115.3 . . ?
C14 C13 H13 115.3 . . ?
C15 C14 C19 118.5(7) . . ?
C15 C14 C13 118.5(6) . . ?
C19 C14 C13 123.0(7) . . ?
C16 C15 C14 122.7(8) . . ?
C16 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
C15 C16 C17 118.6(8) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
C18 C17 C16 119.8(8) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 O4 123.8(6) . . ?
C17 C18 C19 122.3(7) . . ?
O4 C18 C19 113.9(6) . . ?
O2 C19 C18 119.4(6) . . ?
O2 C19 C14 122.5(6) . . ?
C18 C19 C14 118.0(6) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 N1 C8 115.3(6) . . ?
C7 N1 Cu1 124.6(5) . . ?
C8 N1 Cu1 119.9(5) . . ?
C13 N2 C12 116.3(6) . . ?
C13 N2 Cu1 122.6(5) . . ?
C12 N2 Cu1 121.0(5) . . ?
N4 N3 Lu1 139.8(7) . . ?
N3 N4 N5 174.7(12) . . ?
N7 N6 Lu1 120.1(5) . . ?
N7 N6 Lu1 122.5(5) . 2_565 ?
Lu1 N6 Lu1 114.5(2) . 2_565 ?
N8 N7 N6 179.3(10) . . ?
N9 N10 N11 178.7(7) . . ?
N10 N11 Lu1 135.4(5) . 2_565 ?
C1 O1 Cu1 127.2(4) . . ?
C1 O1 Lu1 124.0(4) . . ?
Cu1 O1 Lu1 107.62(18) . . ?
C19 O2 Cu1 126.4(4) . . ?
C19 O2 Lu1 124.1(4) . . ?
Cu1 O2 Lu1 106.80(18) . . ?
C2 O3 C20 116.3(5) . . ?
C2 O3 Lu1 116.8(3) . . ?
C20 O3 Lu1 125.7(4) . . ?
C18 O4 C21 115.4(6) . . ?
C18 O4 Lu1 116.3(4) . . ?
C21 O4 Lu1 121.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.776
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.136
####################################################################### 
# 
# 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_2-CuCevaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060761'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuCevaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Ce2 Cu2 N22 O9'
_chemical_formula_weight         1428.39

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.254(2)
_cell_length_b                   12.594(2)
_cell_length_c                   19.666(4)
_cell_angle_alpha                76.546(3)
_cell_angle_beta                 87.219(3)
_cell_angle_gamma                64.860(3)
_cell_volume                     2667.7(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3874
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      21.09

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1420
_exptl_absorpt_coefficient_mu    2.535
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.6872
_exptl_absorpt_correction_T_max  0.9054
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX SMART'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34309
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.07
_diffrn_reflns_theta_max         27.62
_reflns_number_total             12236
_reflns_number_gt                8824
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0362P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12236
_refine_ls_number_parameters     682
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.1011
_refine_ls_wR_factor_gt          0.0904
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_restrained_S_all      0.988
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.47669(2) 0.45354(2) 0.229613(15) 0.02956(8) Uani 1 1 d . . .
Ce2 Ce 0.13811(2) 0.50096(2) 0.280903(15) 0.02726(8) Uani 1 1 d . . .
Cu1 Cu 0.50294(6) 0.69286(5) 0.28431(3) 0.03526(16) Uani 1 1 d . . .
Cu2 Cu 0.06027(6) 0.32478(5) 0.19108(3) 0.03338(15) Uani 1 1 d . . .
C1 C 0.4430(4) 0.7376(5) 0.1369(3) 0.0372(12) Uani 1 1 d . . .
C2 C 0.4108(5) 0.7023(5) 0.0809(3) 0.0441(14) Uani 1 1 d . . .
C3 C 0.3776(6) 0.7789(6) 0.0168(3) 0.0604(18) Uani 1 1 d . . .
H3 H 0.3554 0.7549 -0.0195 0.073 Uiso 1 1 calc R . .
C4 C 0.3763(7) 0.8928(6) 0.0043(3) 0.071(2) Uani 1 1 d . . .
H4 H 0.3548 0.9441 -0.0401 0.085 Uiso 1 1 calc R . .
C5 C 0.4066(6) 0.9276(6) 0.0574(3) 0.0629(18) Uani 1 1 d . . .
H5 H 0.4044 1.0043 0.0493 0.075 Uiso 1 1 calc R . .
C6 C 0.4412(5) 0.8523(5) 0.1244(3) 0.0425(13) Uani 1 1 d . . .
C7 C 0.4853(5) 0.8926(5) 0.1750(3) 0.0494(15) Uani 1 1 d . . .
H7 H 0.4902 0.9660 0.1595 0.059 Uiso 1 1 calc R . .
C8 C 0.5814(5) 0.8797(5) 0.2807(3) 0.0522(16) Uani 1 1 d . . .
H8A H 0.5973 0.9438 0.2505 0.063 Uiso 1 1 calc R . .
H8B H 0.6587 0.8133 0.2983 0.063 Uiso 1 1 calc R . .
C9 C 0.5133(5) 0.9259(5) 0.3429(3) 0.0436(14) Uani 1 1 d . . .
C10 C 0.4224(6) 1.0557(5) 0.3172(4) 0.0651(19) Uani 1 1 d . . .
H10A H 0.3771 1.0841 0.3555 0.098 Uiso 1 1 calc R . .
H10B H 0.3685 1.0608 0.2815 0.098 Uiso 1 1 calc R . .
H10C H 0.4641 1.1047 0.2982 0.098 Uiso 1 1 calc R . .
C11 C 0.6069(6) 0.9162(6) 0.3948(3) 0.068(2) Uani 1 1 d . . .
H11A H 0.6539 0.9569 0.3714 0.102 Uiso 1 1 calc R . .
H11B H 0.6590 0.8327 0.4136 0.102 Uiso 1 1 calc R . .
H11C H 0.5669 0.9528 0.4321 0.102 Uiso 1 1 calc R . .
C12 C 0.4453(5) 0.8511(4) 0.3782(3) 0.0459(14) Uani 1 1 d . . .
H12A H 0.4352 0.8568 0.4266 0.055 Uiso 1 1 calc R . .
H12B H 0.3655 0.8856 0.3551 0.055 Uiso 1 1 calc R . .
C13 C 0.5456(5) 0.6418(5) 0.4331(3) 0.0399(13) Uani 1 1 d . . .
H13 H 0.5362 0.6669 0.4748 0.048 Uiso 1 1 calc R . .
C14 C 0.6029(4) 0.5143(5) 0.4377(3) 0.0343(12) Uani 1 1 d . . .
C15 C 0.6692(5) 0.4379(5) 0.4999(3) 0.0470(15) Uani 1 1 d . . .
H15 H 0.6717 0.4709 0.5371 0.056 Uiso 1 1 calc R . .
C16 C 0.7293(5) 0.3177(5) 0.5070(3) 0.0544(16) Uani 1 1 d . . .
H16 H 0.7734 0.2691 0.5486 0.065 Uiso 1 1 calc R . .
C17 C 0.7255(5) 0.2663(5) 0.4521(3) 0.0523(16) Uani 1 1 d . . .
H17 H 0.7680 0.1836 0.4567 0.063 Uiso 1 1 calc R . .
C18 C 0.6587(5) 0.3385(5) 0.3911(3) 0.0378(13) Uani 1 1 d . . .
C19 C 0.5969(4) 0.4634(4) 0.3822(3) 0.0321(11) Uani 1 1 d . . .
C20 C 0.3639(8) 0.5542(7) 0.0479(3) 0.090(3) Uani 1 1 d . . .
H20A H 0.2783 0.6029 0.0429 0.136 Uiso 1 1 calc R . .
H20B H 0.3796 0.4707 0.0637 0.136 Uiso 1 1 calc R . .
H20C H 0.3985 0.5665 0.0035 0.136 Uiso 1 1 calc R . .
C21 C 0.7318(6) 0.1773(5) 0.3312(4) 0.0661(19) Uani 1 1 d . . .
H21A H 0.8125 0.1681 0.3389 0.099 Uiso 1 1 calc R . .
H21B H 0.7233 0.1640 0.2860 0.099 Uiso 1 1 calc R . .
H21C H 0.7162 0.1196 0.3668 0.099 Uiso 1 1 calc R . .
C22 C -0.0620(4) 0.5843(4) 0.1420(3) 0.0316(11) Uani 1 1 d . . .
C23 C -0.0963(5) 0.6995(4) 0.1544(3) 0.0354(12) Uani 1 1 d . . .
C24 C -0.1993(5) 0.7958(5) 0.1223(3) 0.0475(15) Uani 1 1 d . . .
H24 H -0.2217 0.8711 0.1316 0.057 Uiso 1 1 calc R . .
C25 C -0.2699(5) 0.7802(6) 0.0759(3) 0.0562(17) Uani 1 1 d . . .
H25 H -0.3407 0.8451 0.0551 0.067 Uiso 1 1 calc R . .
C26 C -0.2372(5) 0.6721(5) 0.0606(3) 0.0501(15) Uani 1 1 d . . .
H26 H -0.2848 0.6638 0.0286 0.060 Uiso 1 1 calc R . .
C27 C -0.1319(5) 0.5720(5) 0.0924(3) 0.0393(13) Uani 1 1 d . . .
C28 C -0.0958(5) 0.4632(6) 0.0690(3) 0.0512(16) Uani 1 1 d . . .
H28 H -0.1372 0.4683 0.0291 0.061 Uiso 1 1 calc R . .
C29 C 0.0197(6) 0.2663(6) 0.0574(3) 0.0611(18) Uani 1 1 d . . .
H29A H 0.0985 0.2519 0.0392 0.073 Uiso 1 1 calc R . .
H29B H -0.0380 0.2967 0.0177 0.073 Uiso 1 1 calc R . .
C30 C 0.0233(6) 0.1480(5) 0.0985(3) 0.0532(16) Uani 1 1 d . . .
C31 C 0.0523(7) 0.0665(6) 0.0472(4) 0.086(3) Uani 1 1 d . . .
H31A H 0.1237 0.0638 0.0239 0.130 Uiso 1 1 calc R . .
H31B H -0.0142 0.0979 0.0133 0.130 Uiso 1 1 calc R . .
H31C H 0.0655 -0.0134 0.0724 0.130 Uiso 1 1 calc R . .
C32 C -0.0956(6) 0.1649(6) 0.1299(4) 0.073(2) Uani 1 1 d . . .
H32A H -0.0874 0.0910 0.1616 0.110 Uiso 1 1 calc R . .
H32B H -0.1556 0.1869 0.0933 0.110 Uiso 1 1 calc R . .
H32C H -0.1198 0.2277 0.1549 0.110 Uiso 1 1 calc R . .
C33 C 0.1254(6) 0.0893(5) 0.1544(3) 0.0602(18) Uani 1 1 d . . .
H33A H 0.1369 0.0069 0.1741 0.072 Uiso 1 1 calc R . .
H33B H 0.1991 0.0863 0.1327 0.072 Uiso 1 1 calc R . .
C34 C 0.1107(5) 0.0905(5) 0.2728(3) 0.0477(15) Uani 1 1 d . . .
H34 H 0.1195 0.0121 0.2772 0.057 Uiso 1 1 calc R . .
C35 C 0.1043(5) 0.1289(4) 0.3375(3) 0.0408(13) Uani 1 1 d . . .
C36 C 0.0927(6) 0.0554(5) 0.3997(4) 0.0574(17) Uani 1 1 d . . .
H36 H 0.0836 -0.0136 0.3981 0.069 Uiso 1 1 calc R . .
C37 C 0.0945(6) 0.0821(6) 0.4623(4) 0.0633(19) Uani 1 1 d . . .
H37 H 0.0838 0.0335 0.5031 0.076 Uiso 1 1 calc R . .
C38 C 0.1125(5) 0.1833(5) 0.4648(3) 0.0514(15) Uani 1 1 d . . .
H38 H 0.1163 0.2013 0.5077 0.062 Uiso 1 1 calc R . .
C39 C 0.1246(5) 0.2563(4) 0.4042(3) 0.0363(12) Uani 1 1 d . . .
C40 C 0.1192(4) 0.2330(4) 0.3389(3) 0.0314(11) Uani 1 1 d . . .
C41 C -0.0356(6) 0.8231(4) 0.2035(3) 0.0609(18) Uani 1 1 d . . .
H41A H -0.0407 0.8715 0.1571 0.091 Uiso 1 1 calc R . .
H41B H 0.0310 0.8175 0.2301 0.091 Uiso 1 1 calc R . .
H41C H -0.1092 0.8598 0.2259 0.091 Uiso 1 1 calc R . .
C42 C 0.1514(6) 0.3842(5) 0.4686(3) 0.0529(16) Uani 1 1 d . . .
H42A H 0.0820 0.3876 0.4945 0.079 Uiso 1 1 calc R . .
H42B H 0.1558 0.4604 0.4609 0.079 Uiso 1 1 calc R . .
H42C H 0.2231 0.3219 0.4947 0.079 Uiso 1 1 calc R . .
C43 C -0.1488(6) 0.5505(7) 0.3627(4) 0.081(2) Uani 1 1 d . . .
H43A H -0.1401 0.4767 0.3947 0.121 Uiso 1 1 calc R . .
H43B H -0.2315 0.5964 0.3454 0.121 Uiso 1 1 calc R . .
H43C H -0.1250 0.5966 0.3864 0.121 Uiso 1 1 calc R . .
N1 N 0.5184(4) 0.8387(4) 0.2385(2) 0.0412(11) Uani 1 1 d . . .
N2 N 0.5063(4) 0.7239(4) 0.3763(2) 0.0372(10) Uani 1 1 d . . .
N3 N -0.0126(4) 0.3594(4) 0.0971(2) 0.0393(11) Uani 1 1 d . . .
N4 N 0.1056(4) 0.1513(4) 0.2113(3) 0.0420(11) Uani 1 1 d . . .
N5 N 0.2587(4) 0.6264(4) 0.2415(2) 0.0395(11) Uani 1 1 d . . .
N6 N 0.2605(4) 0.7048(4) 0.2649(2) 0.0389(11) Uani 1 1 d . . .
N7 N 0.2643(4) 0.7816(4) 0.2859(3) 0.0582(14) Uani 1 1 d . . .
N8 N 0.3644(4) 0.3858(4) 0.3341(3) 0.0446(12) Uani 1 1 d . . .
N9 N 0.4042(4) 0.3071(4) 0.3831(3) 0.0393(11) Uani 1 1 d . . .
N10 N 0.4463(5) 0.2285(5) 0.4324(3) 0.0645(15) Uani 1 1 d . . .
N11 N 0.2936(4) 0.4267(5) 0.1894(3) 0.0592(6) Uani 1 1 d . . .
N12 N 0.2897(5) 0.3561(5) 0.1593(3) 0.0592(6) Uani 1 1 d . . .
N13 N 0.2819(5) 0.2893(5) 0.1301(3) 0.0592(6) Uani 1 1 d . . .
N14 N 0.5553(5) 0.2729(5) 0.1838(3) 0.0592(6) Uani 1 1 d . . .
N15 N 0.6080(5) 0.1780(5) 0.1744(3) 0.0592(6) Uani 1 1 d . . .
N16 N 0.6639(5) 0.0831(5) 0.1656(3) 0.0592(6) Uani 1 1 d . . .
N17 N 0.0758(5) 0.6394(4) 0.3605(2) 0.0497(13) Uani 1 1 d . . .
N18 N 0.0275(5) 0.7373(5) 0.3672(3) 0.0596(14) Uani 1 1 d . . .
N19 N -0.0205(7) 0.8359(6) 0.3733(4) 0.111(3) Uani 1 1 d . . .
N20 N -0.1349(4) 0.3807(4) 0.2446(3) 0.0479(12) Uani 1 1 d . . .
N21 N -0.2272(4) 0.4074(4) 0.2152(2) 0.0397(11) Uani 1 1 d . . .
N22 N -0.3176(4) 0.4331(5) 0.1849(3) 0.0537(13) Uani 1 1 d . . .
O1 O 0.4769(3) 0.6588(3) 0.19781(17) 0.0346(8) Uani 1 1 d . . .
O2 O 0.5347(3) 0.5275(3) 0.32143(17) 0.0344(8) Uani 1 1 d . . .
O3 O 0.6472(3) 0.2970(3) 0.33425(19) 0.0434(9) Uani 1 1 d . . .
O4 O 0.4164(3) 0.5875(3) 0.09767(19) 0.0459(10) Uani 1 1 d . . .
O5 O 0.0349(3) 0.4930(3) 0.17738(17) 0.0303(8) Uani 1 1 d . . .
O6 O 0.1319(3) 0.3072(3) 0.28203(17) 0.0315(8) Uani 1 1 d . . .
O7 O 0.1417(3) 0.3587(3) 0.40298(17) 0.0378(8) Uani 1 1 d . . .
O8 O -0.0179(3) 0.7056(3) 0.19955(18) 0.0392(9) Uani 1 1 d . . .
O9 O -0.0764(3) 0.5242(3) 0.30735(19) 0.0447(9) Uani 1 1 d . . .
H9 H -0.0956 0.4865 0.2852 0.067 Uiso 1 1 d R . .


_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
Ce1 N14 2.433(5) . ?
Ce1 O2 2.471(3) . ?
Ce1 O1 2.516(3) . ?
Ce1 N22 2.556(4) 1_655 ?
Ce1 N11 2.592(5) . ?
Ce1 N8 2.598(5) . ?
Ce1 N5 2.677(4) . ?
Ce1 O4 2.686(4) . ?
Ce1 O3 2.742(3) . ?
Ce1 Cu1 3.5651(8) . ?
Ce1 Ce2 4.0444(8) . ?
Ce2 O6 2.468(3) . ?
Ce2 N17 2.470(5) . ?
Ce2 O5 2.492(3) . ?
Ce2 O9 2.559(3) . ?
Ce2 N5 2.565(4) . ?
Ce2 N11 2.585(5) . ?
Ce2 O7 2.630(3) . ?
Ce2 N8 2.654(4) . ?
Ce2 O8 2.655(3) . ?
Ce2 Cu2 3.5691(8) . ?
Cu1 O2 1.911(3) . ?
Cu1 O1 1.920(3) . ?
Cu1 N1 1.931(4) . ?
Cu1 N2 1.943(4) . ?
Cu2 O6 1.955(3) . ?
Cu2 N4 1.956(4) . ?
Cu2 O5 1.959(3) . ?
Cu2 N3 1.965(4) . ?
Cu2 N20 2.448(5) . ?
C1 O1 1.318(6) . ?
C1 C6 1.399(7) . ?
C1 C2 1.408(7) . ?
C2 C3 1.355(8) . ?
C2 O4 1.379(6) . ?
C3 C4 1.390(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.346(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.436(8) . ?
C7 N1 1.267(7) . ?
C7 H7 0.9300 . ?
C8 N1 1.466(7) . ?
C8 C9 1.533(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.514(7) . ?
C9 C11 1.520(8) . ?
C9 C12 1.540(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.460(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.281(6) . ?
C13 C14 1.436(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.403(7) . ?
C14 C19 1.407(7) . ?
C15 C16 1.347(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.393(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.375(7) . ?
C17 H17 0.9300 . ?
C18 O3 1.376(6) . ?
C18 C19 1.397(7) . ?
C19 O2 1.333(5) . ?
C20 O4 1.425(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O3 1.435(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.329(5) . ?
C22 C27 1.405(7) . ?
C22 C23 1.406(7) . ?
C23 C24 1.371(7) . ?
C23 O8 1.377(6) . ?
C24 C25 1.387(8) . ?
C24 H24 0.9300 . ?
C25 C26 1.349(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.405(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.429(8) . ?
C28 N3 1.280(7) . ?
C28 H28 0.9300 . ?
C29 N3 1.463(6) . ?
C29 C30 1.504(8) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C32 1.503(8) . ?
C30 C33 1.513(8) . ?
C30 C31 1.528(7) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N4 1.462(7) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N4 1.260(7) . ?
C34 C35 1.451(8) . ?
C34 H34 0.9300 . ?
C35 C36 1.392(8) . ?
C35 C40 1.405(6) . ?
C36 C37 1.352(9) . ?
C36 H36 0.9300 . ?
C37 C38 1.395(8) . ?
C37 H37 0.9300 . ?
C38 C39 1.371(7) . ?
C38 H38 0.9300 . ?
C39 O7 1.386(6) . ?
C39 C40 1.393(7) . ?
C40 O6 1.330(5) . ?
C41 O8 1.422(5) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 O7 1.422(6) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 O9 1.380(6) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
N5 N6 1.192(5) . ?
N6 N7 1.154(6) . ?
N8 N9 1.157(6) . ?
N9 N10 1.164(6) . ?
N11 N12 1.195(6) . ?
N12 N13 1.159(6) . ?
N14 N15 1.148(6) . ?
N15 N16 1.148(6) . ?
N17 N18 1.156(6) . ?
N18 N19 1.159(7) . ?
N20 N21 1.173(6) . ?
N21 N22 1.165(6) . ?
N22 Ce1 2.556(4) 1_455 ?
O9 H9 0.8195 . ?

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
N14 Ce1 O2 137.96(15) . . ?
N14 Ce1 O1 137.33(14) . . ?
O2 Ce1 O1 61.21(10) . . ?
N14 Ce1 N22 74.79(16) . 1_655 ?
O2 Ce1 N22 82.95(14) . 1_655 ?
O1 Ce1 N22 71.03(14) . 1_655 ?
N14 Ce1 N11 72.44(16) . . ?
O2 Ce1 N11 139.47(13) . . ?
O1 Ce1 N11 119.48(14) . . ?
N22 Ce1 N11 137.37(16) 1_655 . ?
N14 Ce1 N8 99.15(16) . . ?
O2 Ce1 N8 79.49(13) . . ?
O1 Ce1 N8 123.48(13) . . ?
N22 Ce1 N8 145.27(15) 1_655 . ?
N11 Ce1 N8 67.42(15) . . ?
N14 Ce1 N5 136.37(15) . . ?
O2 Ce1 N5 82.26(12) . . ?
O1 Ce1 N5 68.68(11) . . ?
N22 Ce1 N5 139.39(14) 1_655 . ?
N11 Ce1 N5 64.01(14) . . ?
N8 Ce1 N5 67.10(14) . . ?
N14 Ce1 O4 88.92(15) . . ?
O2 Ce1 O4 121.12(11) . . ?
O1 Ce1 O4 59.91(11) . . ?
N22 Ce1 O4 78.26(14) 1_655 . ?
N11 Ce1 O4 74.64(14) . . ?
N8 Ce1 O4 136.37(13) . . ?
N5 Ce1 O4 77.57(13) . . ?
N14 Ce1 O3 80.11(15) . . ?
O2 Ce1 O3 59.20(10) . . ?
O1 Ce1 O3 112.35(10) . . ?
N22 Ce1 O3 72.83(14) 1_655 . ?
N11 Ce1 O3 126.00(14) . . ?
N8 Ce1 O3 72.44(12) . . ?
N5 Ce1 O3 128.13(13) . . ?
O4 Ce1 O3 150.84(11) . . ?
N14 Ce1 Cu1 153.42(12) . . ?
O2 Ce1 Cu1 30.60(7) . . ?
O1 Ce1 Cu1 31.15(7) . . ?
N22 Ce1 Cu1 79.14(12) 1_655 . ?
N11 Ce1 Cu1 132.83(11) . . ?
N8 Ce1 Cu1 99.29(10) . . ?
N5 Ce1 Cu1 69.12(9) . . ?
O4 Ce1 Cu1 90.82(8) . . ?
O3 Ce1 Cu1 87.40(7) . . ?
N14 Ce1 Ce2 104.34(12) . . ?
O2 Ce1 Ce2 100.92(8) . . ?
O1 Ce1 Ce2 107.20(8) . . ?
N22 Ce1 Ce2 174.43(12) 1_655 . ?
N11 Ce1 Ce2 38.56(11) . . ?
N8 Ce1 Ce2 40.16(10) . . ?
N5 Ce1 Ce2 38.52(9) . . ?
O4 Ce1 Ce2 96.26(8) . . ?
O3 Ce1 Ce2 112.57(8) . . ?
Cu1 Ce1 Ce2 102.109(14) . . ?
O6 Ce2 N17 135.04(13) . . ?
O6 Ce2 O5 63.21(10) . . ?
N17 Ce2 O5 132.86(14) . . ?
O6 Ce2 O9 72.36(11) . . ?
N17 Ce2 O9 77.32(14) . . ?
O5 Ce2 O9 69.16(11) . . ?
O6 Ce2 N5 143.86(12) . . ?
N17 Ce2 N5 77.27(15) . . ?
O5 Ce2 N5 110.03(13) . . ?
O9 Ce2 N5 141.39(12) . . ?
O6 Ce2 N11 79.35(13) . . ?
N17 Ce2 N11 142.28(16) . . ?
O5 Ce2 N11 70.24(13) . . ?
O9 Ce2 N11 137.71(14) . . ?
N5 Ce2 N11 65.69(15) . . ?
O6 Ce2 O7 61.94(10) . . ?
N17 Ce2 O7 77.09(13) . . ?
O5 Ce2 O7 118.84(10) . . ?
O9 Ce2 O7 70.41(11) . . ?
N5 Ce2 O7 130.10(13) . . ?
N11 Ce2 O7 121.81(14) . . ?
O6 Ce2 N8 90.68(12) . . ?
N17 Ce2 N8 93.64(16) . . ?
O5 Ce2 N8 132.94(13) . . ?
O9 Ce2 N8 142.27(13) . . ?
N5 Ce2 N8 67.90(13) . . ?
N11 Ce2 N8 66.68(16) . . ?
O7 Ce2 N8 71.87(12) . . ?
O6 Ce2 O8 120.80(10) . . ?
N17 Ce2 O8 77.67(14) . . ?
O5 Ce2 O8 60.91(10) . . ?
O9 Ce2 O8 71.20(11) . . ?
N5 Ce2 O8 75.32(12) . . ?
N11 Ce2 O8 98.72(14) . . ?
O7 Ce2 O8 137.63(11) . . ?
N8 Ce2 O8 143.21(12) . . ?
O6 Ce2 Cu2 31.59(7) . . ?
N17 Ce2 Cu2 147.40(12) . . ?
O5 Ce2 Cu2 31.85(7) . . ?
O9 Ce2 Cu2 70.08(8) . . ?
N5 Ce2 Cu2 130.26(10) . . ?
N11 Ce2 Cu2 69.34(11) . . ?
O7 Ce2 Cu2 91.46(7) . . ?
N8 Ce2 Cu2 111.88(10) . . ?
O8 Ce2 Cu2 91.86(7) . . ?
O6 Ce2 Ce1 105.00(7) . . ?
N17 Ce2 Ce1 106.25(12) . . ?
O5 Ce2 Ce1 107.51(7) . . ?
O9 Ce2 Ce1 176.37(8) . . ?
N5 Ce2 Ce1 40.53(9) . . ?
N11 Ce2 Ce1 38.68(11) . . ?
O7 Ce2 Ce1 110.76(8) . . ?
N8 Ce2 Ce1 39.13(10) . . ?
O8 Ce2 Ce1 108.69(8) . . ?
Cu2 Ce2 Ce1 106.347(14) . . ?
O2 Cu1 O1 83.02(14) . . ?
O2 Cu1 N1 163.26(17) . . ?
O1 Cu1 N1 93.68(17) . . ?
O2 Cu1 N2 93.44(16) . . ?
O1 Cu1 N2 170.89(16) . . ?
N1 Cu1 N2 92.05(18) . . ?
O2 Cu1 Ce1 41.16(10) . . ?
O1 Cu1 Ce1 42.66(9) . . ?
N1 Cu1 Ce1 135.91(14) . . ?
N2 Cu1 Ce1 132.04(12) . . ?
O6 Cu2 N4 90.74(16) . . ?
O6 Cu2 O5 83.22(13) . . ?
N4 Cu2 O5 172.49(16) . . ?
O6 Cu2 N3 174.07(16) . . ?
N4 Cu2 N3 95.06(19) . . ?
O5 Cu2 N3 90.90(16) . . ?
O6 Cu2 N20 87.73(15) . . ?
N4 Cu2 N20 96.61(18) . . ?
O5 Cu2 N20 87.65(14) . . ?
N3 Cu2 N20 92.85(17) . . ?
O6 Cu2 Ce2 41.41(9) . . ?
N4 Cu2 Ce2 131.26(13) . . ?
O5 Cu2 Ce2 42.15(9) . . ?
N3 Cu2 Ce2 132.66(13) . . ?
N20 Cu2 Ce2 91.00(11) . . ?
O1 C1 C6 123.5(5) . . ?
O1 C1 C2 118.0(5) . . ?
C6 C1 C2 118.5(5) . . ?
C3 C2 O4 125.1(5) . . ?
C3 C2 C1 120.3(6) . . ?
O4 C2 C1 114.6(5) . . ?
C2 C3 C4 121.1(6) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 119.1(6) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 122.0(6) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C5 C6 C1 119.0(5) . . ?
C5 C6 C7 117.4(5) . . ?
C1 C6 C7 123.3(5) . . ?
N1 C7 C6 126.8(5) . . ?
N1 C7 H7 116.6 . . ?
C6 C7 H7 116.6 . . ?
N1 C8 C9 115.0(5) . . ?
N1 C8 H8A 108.5 . . ?
C9 C8 H8A 108.5 . . ?
N1 C8 H8B 108.5 . . ?
C9 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C10 C9 C11 110.8(5) . . ?
C10 C9 C8 109.1(5) . . ?
C11 C9 C8 106.9(5) . . ?
C10 C9 C12 108.5(5) . . ?
C11 C9 C12 109.8(5) . . ?
C8 C9 C12 111.7(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 113.8(4) . . ?
N2 C12 H12A 108.8 . . ?
C9 C12 H12A 108.8 . . ?
N2 C12 H12B 108.8 . . ?
C9 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
N2 C13 C14 125.3(5) . . ?
N2 C13 H13 117.4 . . ?
C14 C13 H13 117.4 . . ?
C15 C14 C19 118.9(5) . . ?
C15 C14 C13 118.2(5) . . ?
C19 C14 C13 122.8(5) . . ?
C16 C15 C14 121.6(6) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C17 120.1(6) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C18 C17 C16 119.7(5) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 O3 124.5(5) . . ?
C17 C18 C19 121.2(5) . . ?
O3 C18 C19 114.2(4) . . ?
O2 C19 C18 117.8(4) . . ?
O2 C19 C14 123.7(4) . . ?
C18 C19 C14 118.4(5) . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 H21A 109.5 . . ?
O3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 C27 123.4(5) . . ?
O5 C22 C23 118.5(4) . . ?
C27 C22 C23 118.1(5) . . ?
C24 C23 O8 124.6(5) . . ?
C24 C23 C22 121.0(5) . . ?
O8 C23 C22 114.4(4) . . ?
C23 C24 C25 119.7(5) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 120.9(5) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 120.7(5) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C26 C27 C22 119.4(5) . . ?
C26 C27 C28 118.0(5) . . ?
C22 C27 C28 122.4(5) . . ?
N3 C28 C27 127.0(5) . . ?
N3 C28 H28 116.5 . . ?
C27 C28 H28 116.5 . . ?
N3 C29 C30 114.8(5) . . ?
N3 C29 H29A 108.6 . . ?
C30 C29 H29A 108.6 . . ?
N3 C29 H29B 108.6 . . ?
C30 C29 H29B 108.6 . . ?
H29A C29 H29B 107.5 . . ?
C32 C30 C29 111.1(5) . . ?
C32 C30 C33 111.2(6) . . ?
C29 C30 C33 109.8(5) . . ?
C32 C30 C31 110.5(5) . . ?
C29 C30 C31 106.5(5) . . ?
C33 C30 C31 107.4(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N4 C33 C30 114.0(5) . . ?
N4 C33 H33A 108.7 . . ?
C30 C33 H33A 108.7 . . ?
N4 C33 H33B 108.7 . . ?
C30 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
N4 C34 C35 127.4(5) . . ?
N4 C34 H34 116.3 . . ?
C35 C34 H34 116.3 . . ?
C36 C35 C40 120.0(5) . . ?
C36 C35 C34 118.8(5) . . ?
C40 C35 C34 121.0(5) . . ?
C37 C36 C35 121.6(6) . . ?
C37 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
C36 C37 C38 119.2(6) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.4 . . ?
C39 C38 C37 120.0(6) . . ?
C39 C38 H38 120.0 . . ?
C37 C38 H38 120.0 . . ?
C38 C39 O7 122.9(5) . . ?
C38 C39 C40 121.9(5) . . ?
O7 C39 C40 115.2(4) . . ?
O6 C40 C39 118.9(4) . . ?
O6 C40 C35 123.8(5) . . ?
C39 C40 C35 117.3(5) . . ?
O8 C41 H41A 109.5 . . ?
O8 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O8 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O7 C42 H42A 109.5 . . ?
O7 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O7 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O9 C43 H43A 109.5 . . ?
O9 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O9 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C7 N1 C8 120.6(5) . . ?
C7 N1 Cu1 123.9(4) . . ?
C8 N1 Cu1 115.3(4) . . ?
C13 N2 C12 120.5(5) . . ?
C13 N2 Cu1 124.5(4) . . ?
C12 N2 Cu1 114.5(4) . . ?
C28 N3 C29 116.5(5) . . ?
C28 N3 Cu2 121.5(4) . . ?
C29 N3 Cu2 121.9(4) . . ?
C34 N4 C33 117.4(5) . . ?
C34 N4 Cu2 121.8(4) . . ?
C33 N4 Cu2 120.7(4) . . ?
N6 N5 Ce2 128.3(4) . . ?
N6 N5 Ce1 114.5(3) . . ?
Ce2 N5 Ce1 100.96(14) . . ?
N7 N6 N5 177.9(6) . . ?
N9 N8 Ce1 128.6(4) . . ?
N9 N8 Ce2 128.6(4) . . ?
Ce1 N8 Ce2 100.71(16) . . ?
N8 N9 N10 178.6(6) . . ?
N12 N11 Ce2 120.3(4) . . ?
N12 N11 Ce1 130.4(4) . . ?
Ce2 N11 Ce1 102.75(17) . . ?
N13 N12 N11 177.8(6) . . ?
N15 N14 Ce1 165.9(5) . . ?
N16 N15 N14 178.0(7) . . ?
N18 N17 Ce2 148.0(4) . . ?
N17 N18 N19 179.4(8) . . ?
N21 N20 Cu2 125.1(4) . . ?
N22 N21 N20 178.6(6) . . ?
N21 N22 Ce1 130.6(4) . 1_455 ?
C1 O1 Cu1 125.4(3) . . ?
C1 O1 Ce1 127.2(3) . . ?
Cu1 O1 Ce1 106.20(13) . . ?
C19 O2 Cu1 122.7(3) . . ?
C19 O2 Ce1 128.1(3) . . ?
Cu1 O2 Ce1 108.24(14) . . ?
C18 O3 C21 117.5(4) . . ?
C18 O3 Ce1 118.1(3) . . ?
C21 O3 Ce1 124.2(3) . . ?
C2 O4 C20 117.4(5) . . ?
C2 O4 Ce1 120.2(3) . . ?
C20 O4 Ce1 120.9(4) . . ?
C22 O5 Cu2 122.1(3) . . ?
C22 O5 Ce2 124.4(3) . . ?
Cu2 O5 Ce2 106.00(13) . . ?
C40 O6 Cu2 120.6(3) . . ?
C40 O6 Ce2 124.6(3) . . ?
Cu2 O6 Ce2 107.01(13) . . ?
C39 O7 C42 117.2(4) . . ?
C39 O7 Ce2 118.5(3) . . ?
C42 O7 Ce2 124.1(3) . . ?
C23 O8 C41 116.5(4) . . ?
C23 O8 Ce2 118.1(3) . . ?
C41 O8 Ce2 125.1(3) . . ?
C43 O9 Ce2 134.3(4) . . ?
C43 O9 H9 112.0 . . ?
Ce2 O9 H9 110.0 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.160
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.122
####################################################################### 
# 
# 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_3-CuPrvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060762'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuPrvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Cu2 N22 O9 Pr2'
_chemical_formula_weight         1429.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.2038(16)
_cell_length_b                   12.5702(16)
_cell_length_c                   19.689(3)
_cell_angle_alpha                76.538(2)
_cell_angle_beta                 87.325(2)
_cell_angle_gamma                65.045(2)
_cell_volume                     2658.6(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8202
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      25.96

_exptl_crystal_description       palte
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    2.664
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5673
_exptl_absorpt_correction_T_max  0.9009
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX SMART'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34437
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.07
_diffrn_reflns_theta_max         27.68
_reflns_number_total             12309
_reflns_number_gt                9896
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0392P)²+0.3335P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12309
_refine_ls_number_parameters     682
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0851
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.475399(18) 0.454300(18) 0.229911(11) 0.02725(6) Uani 1 1 d . . .
Pr2 Pr 0.138177(17) 0.500996(17) 0.280734(10) 0.02448(6) Uani 1 1 d . . .
Cu1 Cu 0.50253(4) 0.69274(4) 0.28445(2) 0.03235(11) Uani 1 1 d . . .
Cu2 Cu 0.05983(4) 0.32614(4) 0.19092(2) 0.02990(11) Uani 1 1 d . . .
C1 C 0.4425(3) 0.7361(4) 0.1375(2) 0.0341(9) Uani 1 1 d . . .
C2 C 0.4094(4) 0.7017(4) 0.0818(2) 0.0401(10) Uani 1 1 d . . .
C3 C 0.3760(5) 0.7767(5) 0.0171(3) 0.0603(14) Uani 1 1 d . . .
H3 H 0.3546 0.7517 -0.0191 0.072 Uiso 1 1 calc R . .
C4 C 0.3739(5) 0.8917(5) 0.0050(3) 0.0701(16) Uani 1 1 d . . .
H4 H 0.3511 0.9432 -0.0392 0.084 Uiso 1 1 calc R . .
C5 C 0.4050(5) 0.9279(4) 0.0577(2) 0.0570(13) Uani 1 1 d . . .
H5 H 0.4034 1.0045 0.0491 0.068 Uiso 1 1 calc R . .
C6 C 0.4394(4) 0.8523(4) 0.1247(2) 0.0390(10) Uani 1 1 d . . .
C7 C 0.4849(4) 0.8922(4) 0.1747(2) 0.0459(11) Uani 1 1 d . . .
H7 H 0.4910 0.9651 0.1589 0.055 Uiso 1 1 calc R . .
C8 C 0.5821(4) 0.8795(4) 0.2806(2) 0.0472(11) Uani 1 1 d . . .
H8A H 0.5983 0.9436 0.2504 0.057 Uiso 1 1 calc R . .
H8B H 0.6595 0.8129 0.2981 0.057 Uiso 1 1 calc R . .
C9 C 0.5140(4) 0.9255(4) 0.3426(2) 0.0412(10) Uani 1 1 d . . .
C10 C 0.4232(5) 1.0557(4) 0.3175(3) 0.0630(14) Uani 1 1 d . . .
H10A H 0.3759 1.0825 0.3555 0.094 Uiso 1 1 calc R . .
H10B H 0.3708 1.0619 0.2804 0.094 Uiso 1 1 calc R . .
H10C H 0.4654 1.1052 0.3005 0.094 Uiso 1 1 calc R . .
C11 C 0.6092(5) 0.9154(5) 0.3944(3) 0.0633(14) Uani 1 1 d . . .
H11A H 0.6567 0.9557 0.3707 0.095 Uiso 1 1 calc R . .
H11B H 0.6610 0.8318 0.4133 0.095 Uiso 1 1 calc R . .
H11C H 0.5698 0.9524 0.4316 0.095 Uiso 1 1 calc R . .
C12 C 0.4454(4) 0.8513(4) 0.3780(2) 0.0426(10) Uani 1 1 d . . .
H12A H 0.4355 0.8570 0.4263 0.051 Uiso 1 1 calc R . .
H12B H 0.3653 0.8860 0.3549 0.051 Uiso 1 1 calc R . .
C13 C 0.5458(4) 0.6418(4) 0.4327(2) 0.0362(9) Uani 1 1 d . . .
H13 H 0.5370 0.6668 0.4743 0.043 Uiso 1 1 calc R . .
C14 C 0.6029(3) 0.5131(4) 0.4373(2) 0.0328(9) Uani 1 1 d . . .
C15 C 0.6699(4) 0.4375(4) 0.4993(2) 0.0432(11) Uani 1 1 d . . .
H15 H 0.6731 0.4706 0.5363 0.052 Uiso 1 1 calc R . .
C16 C 0.7304(4) 0.3161(4) 0.5061(2) 0.0518(12) Uani 1 1 d . . .
H16 H 0.7755 0.2671 0.5474 0.062 Uiso 1 1 calc R . .
C17 C 0.7249(4) 0.2657(4) 0.4519(2) 0.0483(11) Uani 1 1 d . . .
H17 H 0.7664 0.1828 0.4567 0.058 Uiso 1 1 calc R . .
C18 C 0.6581(3) 0.3379(4) 0.3905(2) 0.0351(9) Uani 1 1 d . . .
C19 C 0.5955(3) 0.4634(3) 0.38212(19) 0.0295(8) Uani 1 1 d . . .
C20 C 0.3634(6) 0.5518(6) 0.0490(3) 0.0814(19) Uani 1 1 d . . .
H20A H 0.2775 0.6000 0.0444 0.122 Uiso 1 1 calc R . .
H20B H 0.3795 0.4681 0.0648 0.122 Uiso 1 1 calc R . .
H20C H 0.3972 0.5647 0.0045 0.122 Uiso 1 1 calc R . .
C21 C 0.7298(5) 0.1774(4) 0.3313(3) 0.0673(15) Uani 1 1 d . . .
H21A H 0.8106 0.1669 0.3409 0.101 Uiso 1 1 calc R . .
H21B H 0.7238 0.1640 0.2858 0.101 Uiso 1 1 calc R . .
H21C H 0.7113 0.1206 0.3660 0.101 Uiso 1 1 calc R . .
C22 C -0.0622(3) 0.5852(3) 0.14304(19) 0.0283(8) Uani 1 1 d . . .
C23 C -0.0962(3) 0.7004(3) 0.1549(2) 0.0316(8) Uani 1 1 d . . .
C24 C -0.1997(4) 0.7980(4) 0.1234(2) 0.0432(10) Uani 1 1 d . . .
H24 H -0.2218 0.8730 0.1332 0.052 Uiso 1 1 calc R . .
C25 C -0.2707(4) 0.7827(4) 0.0767(2) 0.0488(12) Uani 1 1 d . . .
H25 H -0.3417 0.8477 0.0559 0.059 Uiso 1 1 calc R . .
C26 C -0.2382(4) 0.6747(4) 0.0611(2) 0.0497(12) Uani 1 1 d . . .
H26 H -0.2854 0.6668 0.0286 0.060 Uiso 1 1 calc R . .
C27 C -0.1332(4) 0.5739(4) 0.0936(2) 0.0358(9) Uani 1 1 d . . .
C28 C -0.0966(4) 0.4652(4) 0.0694(2) 0.0438(11) Uani 1 1 d . . .
H28 H -0.1380 0.4712 0.0293 0.053 Uiso 1 1 calc R . .
C29 C 0.0186(5) 0.2689(4) 0.0571(2) 0.0548(13) Uani 1 1 d . . .
H29A H 0.0976 0.2545 0.0390 0.066 Uiso 1 1 calc R . .
H29B H -0.0394 0.2995 0.0174 0.066 Uiso 1 1 calc R . .
C30 C 0.0216(4) 0.1498(4) 0.0986(3) 0.0483(11) Uani 1 1 d . . .
C31 C 0.0492(6) 0.0692(5) 0.0470(3) 0.0811(19) Uani 1 1 d . . .
H31A H 0.1220 0.0647 0.0245 0.122 Uiso 1 1 calc R . .
H31B H -0.0168 0.1025 0.0124 0.122 Uiso 1 1 calc R . .
H31C H 0.0598 -0.0103 0.0717 0.122 Uiso 1 1 calc R . .
C32 C -0.0985(5) 0.1677(5) 0.1297(3) 0.0699(16) Uani 1 1 d . . .
H32A H -0.0932 0.0921 0.1580 0.105 Uiso 1 1 calc R . .
H32B H -0.1601 0.1971 0.0927 0.105 Uiso 1 1 calc R . .
H32C H -0.1188 0.2252 0.1581 0.105 Uiso 1 1 calc R . .
C33 C 0.1247(4) 0.0907(4) 0.1543(3) 0.0535(12) Uani 1 1 d . . .
H33A H 0.1364 0.0081 0.1738 0.064 Uiso 1 1 calc R . .
H33B H 0.1984 0.0882 0.1325 0.064 Uiso 1 1 calc R . .
C34 C 0.1102(4) 0.0908(4) 0.2725(3) 0.0442(11) Uani 1 1 d . . .
H34 H 0.1185 0.0124 0.2769 0.053 Uiso 1 1 calc R . .
C35 C 0.1044(4) 0.1296(3) 0.3368(2) 0.0368(9) Uani 1 1 d . . .
C36 C 0.0925(4) 0.0559(4) 0.3994(3) 0.0516(12) Uani 1 1 d . . .
H36 H 0.0823 -0.0128 0.3978 0.062 Uiso 1 1 calc R . .
C37 C 0.0953(5) 0.0820(4) 0.4614(3) 0.0568(13) Uani 1 1 d . . .
H37 H 0.0857 0.0324 0.5021 0.068 Uiso 1 1 calc R . .
C38 C 0.1125(4) 0.1835(4) 0.4646(2) 0.0475(11) Uani 1 1 d . . .
H38 H 0.1159 0.2013 0.5076 0.057 Uiso 1 1 calc R . .
C39 C 0.1245(3) 0.2569(3) 0.4042(2) 0.0329(9) Uani 1 1 d . . .
C40 C 0.1192(3) 0.2336(3) 0.3383(2) 0.0292(8) Uani 1 1 d . . .
C41 C -0.0348(5) 0.8232(4) 0.2050(3) 0.0553(13) Uani 1 1 d . . .
H41A H -0.0381 0.8716 0.1589 0.083 Uiso 1 1 calc R . .
H41B H 0.0311 0.8173 0.2327 0.083 Uiso 1 1 calc R . .
H41C H -0.1094 0.8599 0.2264 0.083 Uiso 1 1 calc R . .
C42 C 0.1514(4) 0.3854(4) 0.4681(2) 0.0489(11) Uani 1 1 d . . .
H42A H 0.0800 0.3923 0.4928 0.073 Uiso 1 1 calc R . .
H42B H 0.1594 0.4600 0.4604 0.073 Uiso 1 1 calc R . .
H42C H 0.2212 0.3214 0.4952 0.073 Uiso 1 1 calc R . .
C43 C -0.1468(5) 0.5485(5) 0.3630(3) 0.0721(17) Uani 1 1 d . . .
H43A H -0.1296 0.4743 0.3972 0.108 Uiso 1 1 calc R . .
H43B H -0.2306 0.5851 0.3471 0.108 Uiso 1 1 calc R . .
H43C H -0.1299 0.6024 0.3836 0.108 Uiso 1 1 calc R . .
N1 N 0.5179(3) 0.8387(3) 0.23832(18) 0.0390(8) Uani 1 1 d . . .
N2 N 0.5063(3) 0.7238(3) 0.37602(17) 0.0339(7) Uani 1 1 d . . .
N3 N -0.0135(3) 0.3610(3) 0.09688(17) 0.0383(8) Uani 1 1 d . . .
N4 N 0.1051(3) 0.1522(3) 0.21089(19) 0.0384(8) Uani 1 1 d . . .
N5 N 0.2590(3) 0.6263(3) 0.24204(19) 0.0364(8) Uani 1 1 d . . .
N6 N 0.2596(3) 0.7051(3) 0.26503(19) 0.0381(8) Uani 1 1 d . . .
N7 N 0.2636(4) 0.7817(3) 0.2857(2) 0.0575(11) Uani 1 1 d . . .
N8 N 0.3627(3) 0.3862(3) 0.33334(18) 0.0389(8) Uani 1 1 d . . .
N9 N 0.4044(3) 0.3072(3) 0.38294(18) 0.0356(8) Uani 1 1 d . . .
N10 N 0.4448(4) 0.2300(4) 0.4323(2) 0.0572(11) Uani 1 1 d . . .
N11 N 0.2932(3) 0.4267(4) 0.1899(2) 0.0559(4) Uani 1 1 d . . .
N12 N 0.2888(4) 0.3567(4) 0.1596(2) 0.0559(4) Uani 1 1 d . . .
N13 N 0.2807(4) 0.2916(4) 0.1296(2) 0.0559(4) Uani 1 1 d . . .
N14 N 0.5522(4) 0.2750(4) 0.1843(2) 0.0559(4) Uani 1 1 d . . .
N15 N 0.6061(4) 0.1797(4) 0.1742(2) 0.0559(4) Uani 1 1 d . . .
N16 N 0.6611(4) 0.0850(4) 0.1654(2) 0.0559(4) Uani 1 1 d . . .
N17 N 0.0772(3) 0.6374(3) 0.3600(2) 0.0474(9) Uani 1 1 d . . .
N18 N 0.0281(4) 0.7357(4) 0.3672(2) 0.0536(10) Uani 1 1 d . . .
N19 N -0.0200(6) 0.8328(5) 0.3749(3) 0.0985(19) Uani 1 1 d . . .
N20 N -0.1360(3) 0.3810(3) 0.2447(2) 0.0453(9) Uani 1 1 d . . .
N21 N -0.2289(3) 0.4089(3) 0.21580(18) 0.0367(8) Uani 1 1 d . . .
N22 N -0.3192(3) 0.4333(4) 0.1854(2) 0.0493(10) Uani 1 1 d . . .
O1 O 0.4765(2) 0.6577(2) 0.19839(13) 0.0333(6) Uani 1 1 d . . .
O2 O 0.5335(2) 0.5272(2) 0.32147(13) 0.0315(6) Uani 1 1 d . . .
O3 O 0.6460(2) 0.2974(2) 0.33309(15) 0.0389(7) Uani 1 1 d . . .
O4 O 0.4168(3) 0.5854(3) 0.09871(15) 0.0448(7) Uani 1 1 d . . .
O5 O 0.0348(2) 0.4943(2) 0.17763(13) 0.0278(5) Uani 1 1 d . . .
O6 O 0.1322(2) 0.3081(2) 0.28187(13) 0.0270(5) Uani 1 1 d . . .
O7 O 0.1421(2) 0.3594(2) 0.40225(13) 0.0345(6) Uani 1 1 d . . .
O8 O -0.0169(2) 0.7059(2) 0.20046(14) 0.0370(6) Uani 1 1 d . . .
O9 O -0.0753(2) 0.5248(3) 0.30696(15) 0.0405(7) Uani 1 1 d . . .
H9 H -0.0945 0.4871 0.2848 0.061 Uiso 1 1 d R . .


_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
Pr1 N14 2.418(4) . ?
Pr1 O2 2.456(2) . ?
Pr1 O1 2.492(2) . ?
Pr1 N22 2.542(3) 1_655 ?
Pr1 N11 2.575(4) . ?
Pr1 N8 2.587(3) . ?
Pr1 N5 2.659(3) . ?
Pr1 O4 2.664(3) . ?
Pr1 O3 2.723(3) . ?
Pr1 Cu1 3.5518(6) . ?
Pr1 Pr2 4.0166(6) . ?
Pr2 N17 2.448(4) . ?
Pr2 O6 2.451(2) . ?
Pr2 O5 2.475(2) . ?
Pr2 O9 2.537(3) . ?
Pr2 N5 2.556(3) . ?
Pr2 N11 2.574(4) . ?
Pr2 O7 2.617(3) . ?
Pr2 N8 2.626(3) . ?
Pr2 O8 2.643(3) . ?
Pr2 Cu2 3.5515(5) . ?
Cu1 O2 1.913(2) . ?
Cu1 O1 1.919(3) . ?
Cu1 N1 1.929(3) . ?
Cu1 N2 1.938(3) . ?
Cu2 O6 1.956(2) . ?
Cu2 O5 1.958(2) . ?
Cu2 N4 1.960(3) . ?
Cu2 N3 1.966(3) . ?
Cu2 N20 2.453(4) . ?
C1 O1 1.316(4) . ?
C1 C2 1.403(6) . ?
C1 C6 1.408(5) . ?
C2 C3 1.357(6) . ?
C2 O4 1.386(5) . ?
C3 C4 1.398(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.352(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.397(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.429(6) . ?
C7 N1 1.269(5) . ?
C7 H7 0.9300 . ?
C8 N1 1.473(5) . ?
C8 C9 1.532(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.516(6) . ?
C9 C11 1.526(6) . ?
C9 C12 1.536(6) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.464(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.279(5) . ?
C13 C14 1.448(5) . ?
C13 H13 0.9300 . ?
C14 C19 1.397(5) . ?
C14 C15 1.400(6) . ?
C15 C16 1.362(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.381(6) . ?
C17 H17 0.9300 . ?
C18 O3 1.379(5) . ?
C18 C19 1.404(5) . ?
C19 O2 1.330(4) . ?
C20 O4 1.431(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O3 1.430(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.320(4) . ?
C22 C27 1.402(5) . ?
C22 C23 1.403(5) . ?
C23 C24 1.377(5) . ?
C23 O8 1.382(4) . ?
C24 C25 1.390(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.349(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.409(6) . ?
C26 H26 0.9300 . ?
C27 C28 1.435(6) . ?
C28 N3 1.279(5) . ?
C28 H28 0.9300 . ?
C29 N3 1.456(5) . ?
C29 C30 1.516(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C32 1.508(7) . ?
C30 C33 1.516(6) . ?
C30 C31 1.527(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N4 1.455(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N4 1.265(5) . ?
C34 C35 1.449(6) . ?
C34 H34 0.9300 . ?
C35 C40 1.399(5) . ?
C35 C36 1.400(6) . ?
C36 C37 1.341(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.395(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.369(5) . ?
C38 H38 0.9300 . ?
C39 O7 1.384(4) . ?
C39 C40 1.405(5) . ?
C40 O6 1.327(4) . ?
C41 O8 1.421(4) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 O7 1.429(4) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 O9 1.382(5) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
N5 N6 1.183(4) . ?
N6 N7 1.150(5) . ?
N8 N9 1.169(4) . ?
N9 N10 1.154(5) . ?
N11 N12 1.190(5) . ?
N12 N13 1.152(5) . ?
N14 N15 1.158(5) . ?
N15 N16 1.145(5) . ?
N17 N18 1.164(5) . ?
N18 N19 1.154(6) . ?
N20 N21 1.168(5) . ?
N21 N22 1.165(5) . ?
N22 Pr1 2.542(3) 1_455 ?
O9 H9 0.8178 . ?

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
N14 Pr1 O2 138.12(12) . . ?
N14 Pr1 O1 137.31(11) . . ?
O2 Pr1 O1 61.45(8) . . ?
N14 Pr1 N22 74.77(13) . 1_655 ?
O2 Pr1 N22 83.27(11) . 1_655 ?
O1 Pr1 N22 71.13(11) . 1_655 ?
N14 Pr1 N11 71.96(12) . . ?
O2 Pr1 N11 139.49(10) . . ?
O1 Pr1 N11 119.75(11) . . ?
N22 Pr1 N11 137.08(12) 1_655 . ?
N14 Pr1 N8 98.86(12) . . ?
O2 Pr1 N8 79.56(10) . . ?
O1 Pr1 N8 123.77(10) . . ?
N22 Pr1 N8 145.38(12) 1_655 . ?
N11 Pr1 N8 67.15(12) . . ?
N14 Pr1 N5 136.38(12) . . ?
O2 Pr1 N5 81.98(10) . . ?
O1 Pr1 N5 68.63(9) . . ?
N22 Pr1 N5 139.46(11) 1_655 . ?
N11 Pr1 N5 64.50(11) . . ?
N8 Pr1 N5 67.10(10) . . ?
N14 Pr1 O4 88.26(12) . . ?
O2 Pr1 O4 121.75(8) . . ?
O1 Pr1 O4 60.31(8) . . ?
N22 Pr1 O4 78.01(11) 1_655 . ?
N11 Pr1 O4 74.67(11) . . ?
N8 Pr1 O4 136.43(10) . . ?
N5 Pr1 O4 78.20(10) . . ?
N14 Pr1 O3 79.86(12) . . ?
O2 Pr1 O3 59.49(8) . . ?
O1 Pr1 O3 112.56(8) . . ?
N22 Pr1 O3 72.57(11) 1_655 . ?
N11 Pr1 O3 125.71(11) . . ?
N8 Pr1 O3 72.82(9) . . ?
N5 Pr1 O3 128.37(10) . . ?
O4 Pr1 O3 150.23(9) . . ?
N14 Pr1 Cu1 153.64(9) . . ?
O2 Pr1 Cu1 30.78(6) . . ?
O1 Pr1 Cu1 31.19(6) . . ?
N22 Pr1 Cu1 79.36(9) 1_655 . ?
N11 Pr1 Cu1 133.07(9) . . ?
N8 Pr1 Cu1 99.55(8) . . ?
N5 Pr1 Cu1 68.87(7) . . ?
O4 Pr1 Cu1 91.28(6) . . ?
O3 Pr1 Cu1 87.75(6) . . ?
N14 Pr1 Pr2 104.11(9) . . ?
O2 Pr1 Pr2 100.78(6) . . ?
O1 Pr1 Pr2 107.32(6) . . ?
N22 Pr1 Pr2 174.43(9) 1_655 . ?
N11 Pr1 Pr2 38.71(8) . . ?
N8 Pr1 Pr2 39.96(7) . . ?
N5 Pr1 Pr2 38.70(7) . . ?
O4 Pr1 Pr2 96.55(6) . . ?
O3 Pr1 Pr2 112.75(6) . . ?
Cu1 Pr1 Pr2 102.125(10) . . ?
N17 Pr2 O6 134.93(10) . . ?
N17 Pr2 O5 132.90(11) . . ?
O6 Pr2 O5 63.63(8) . . ?
N17 Pr2 O9 77.11(11) . . ?
O6 Pr2 O9 72.79(8) . . ?
O5 Pr2 O9 69.37(8) . . ?
N17 Pr2 N5 77.17(11) . . ?
O6 Pr2 N5 143.85(9) . . ?
O5 Pr2 N5 109.98(10) . . ?
O9 Pr2 N5 141.11(9) . . ?
N17 Pr2 N11 142.44(12) . . ?
O6 Pr2 N11 79.10(10) . . ?
O5 Pr2 N11 70.21(10) . . ?
O9 Pr2 N11 137.86(10) . . ?
N5 Pr2 N11 65.99(11) . . ?
N17 Pr2 O7 76.73(11) . . ?
O6 Pr2 O7 62.08(8) . . ?
O5 Pr2 O7 119.32(8) . . ?
O9 Pr2 O7 70.62(9) . . ?
N5 Pr2 O7 129.72(10) . . ?
N11 Pr2 O7 121.68(11) . . ?
N17 Pr2 N8 93.64(12) . . ?
O6 Pr2 N8 90.26(9) . . ?
O5 Pr2 N8 132.90(10) . . ?
O9 Pr2 N8 142.23(10) . . ?
N5 Pr2 N8 68.03(10) . . ?
N11 Pr2 N8 66.58(12) . . ?
O7 Pr2 N8 71.62(9) . . ?
N17 Pr2 O8 77.50(11) . . ?
O6 Pr2 O8 121.40(8) . . ?
O5 Pr2 O8 61.10(8) . . ?
O9 Pr2 O8 71.19(9) . . ?
N5 Pr2 O8 75.11(9) . . ?
N11 Pr2 O8 99.03(11) . . ?
O7 Pr2 O8 137.61(9) . . ?
N8 Pr2 O8 143.13(9) . . ?
N17 Pr2 Cu2 147.51(9) . . ?
O6 Pr2 Cu2 31.82(6) . . ?
O5 Pr2 Cu2 32.03(5) . . ?
O9 Pr2 Cu2 70.40(6) . . ?
N5 Pr2 Cu2 130.33(8) . . ?
N11 Pr2 Cu2 69.14(8) . . ?
O7 Pr2 Cu2 91.80(6) . . ?
N8 Pr2 Cu2 111.68(8) . . ?
O8 Pr2 Cu2 92.23(6) . . ?
N17 Pr2 Pr1 106.22(9) . . ?
O6 Pr2 Pr1 104.85(5) . . ?
O5 Pr2 Pr1 107.43(6) . . ?
O9 Pr2 Pr1 176.58(6) . . ?
N5 Pr2 Pr1 40.57(7) . . ?
N11 Pr2 Pr1 38.73(8) . . ?
O7 Pr2 Pr1 110.66(6) . . ?
N8 Pr2 Pr1 39.25(7) . . ?
O8 Pr2 Pr1 108.56(6) . . ?
Cu2 Pr2 Pr1 106.269(11) . . ?
O2 Cu1 O1 82.55(11) . . ?
O2 Cu1 N1 163.47(14) . . ?
O1 Cu1 N1 93.73(13) . . ?
O2 Cu1 N2 93.59(12) . . ?
O1 Cu1 N2 170.88(12) . . ?
N1 Cu1 N2 92.23(14) . . ?
O2 Cu1 Pr1 41.07(7) . . ?
O1 Cu1 Pr1 42.27(7) . . ?
N1 Cu1 Pr1 135.61(10) . . ?
N2 Cu1 Pr1 132.16(9) . . ?
O6 Cu2 O5 83.13(10) . . ?
O6 Cu2 N4 90.74(12) . . ?
O5 Cu2 N4 172.40(12) . . ?
O6 Cu2 N3 174.10(12) . . ?
O5 Cu2 N3 91.03(12) . . ?
N4 Cu2 N3 95.01(14) . . ?
O6 Cu2 N20 87.73(11) . . ?
O5 Cu2 N20 87.81(11) . . ?
N4 Cu2 N20 96.46(13) . . ?
N3 Cu2 N20 92.96(13) . . ?
O6 Cu2 Pr2 41.35(7) . . ?
O5 Cu2 Pr2 42.10(7) . . ?
N4 Cu2 Pr2 131.22(10) . . ?
N3 Cu2 Pr2 132.75(10) . . ?
N20 Cu2 Pr2 91.04(8) . . ?
O1 C1 C2 118.4(4) . . ?
O1 C1 C6 123.7(4) . . ?
C2 C1 C6 117.9(4) . . ?
C3 C2 O4 124.3(4) . . ?
C3 C2 C1 121.7(4) . . ?
O4 C2 C1 114.0(3) . . ?
C2 C3 C4 119.8(5) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.0(5) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 121.2(5) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 119.4(4) . . ?
C5 C6 C7 117.2(4) . . ?
C1 C6 C7 122.9(4) . . ?
N1 C7 C6 126.9(4) . . ?
N1 C7 H7 116.6 . . ?
C6 C7 H7 116.6 . . ?
N1 C8 C9 114.7(3) . . ?
N1 C8 H8A 108.6 . . ?
C9 C8 H8A 108.6 . . ?
N1 C8 H8B 108.6 . . ?
C9 C8 H8B 108.6 . . ?
H8A C8 H8B 107.6 . . ?
C10 C9 C11 110.6(4) . . ?
C10 C9 C8 109.4(4) . . ?
C11 C9 C8 106.4(4) . . ?
C10 C9 C12 108.3(4) . . ?
C11 C9 C12 110.0(4) . . ?
C8 C9 C12 112.1(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 113.4(3) . . ?
N2 C12 H12A 108.9 . . ?
C9 C12 H12A 108.9 . . ?
N2 C12 H12B 108.9 . . ?
C9 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
N2 C13 C14 125.2(4) . . ?
N2 C13 H13 117.4 . . ?
C14 C13 H13 117.4 . . ?
C19 C14 C15 119.7(4) . . ?
C19 C14 C13 122.5(4) . . ?
C15 C14 C13 117.8(4) . . ?
C16 C15 C14 121.0(4) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.1(4) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 120.2(4) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
O3 C18 C17 125.2(4) . . ?
O3 C18 C19 114.2(3) . . ?
C17 C18 C19 120.7(4) . . ?
O2 C19 C14 124.3(3) . . ?
O2 C19 C18 117.3(3) . . ?
C14 C19 C18 118.4(3) . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 H21A 109.5 . . ?
O3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 C27 123.7(3) . . ?
O5 C22 C23 118.9(3) . . ?
C27 C22 C23 117.4(3) . . ?
C24 C23 O8 124.0(4) . . ?
C24 C23 C22 122.0(4) . . ?
O8 C23 C22 114.0(3) . . ?
C23 C24 C25 119.0(4) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C26 C25 C24 120.9(4) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 120.6(4) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C22 C27 C26 119.9(4) . . ?
C22 C27 C28 122.0(4) . . ?
C26 C27 C28 117.8(4) . . ?
N3 C28 C27 127.4(4) . . ?
N3 C28 H28 116.3 . . ?
C27 C28 H28 116.3 . . ?
N3 C29 C30 114.3(4) . . ?
N3 C29 H29A 108.7 . . ?
C30 C29 H29A 108.7 . . ?
N3 C29 H29B 108.7 . . ?
C30 C29 H29B 108.7 . . ?
H29A C29 H29B 107.6 . . ?
C32 C30 C33 111.9(4) . . ?
C32 C30 C29 110.9(4) . . ?
C33 C30 C29 109.7(4) . . ?
C32 C30 C31 110.4(4) . . ?
C33 C30 C31 107.7(4) . . ?
C29 C30 C31 106.1(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N4 C33 C30 113.8(4) . . ?
N4 C33 H33A 108.8 . . ?
C30 C33 H33A 108.8 . . ?
N4 C33 H33B 108.8 . . ?
C30 C33 H33B 108.8 . . ?
H33A C33 H33B 107.7 . . ?
N4 C34 C35 126.9(4) . . ?
N4 C34 H34 116.5 . . ?
C35 C34 H34 116.5 . . ?
C40 C35 C36 119.8(4) . . ?
C40 C35 C34 121.5(4) . . ?
C36 C35 C34 118.6(4) . . ?
C37 C36 C35 121.7(4) . . ?
C37 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
C36 C37 C38 119.9(4) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C39 C38 C37 119.5(4) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C38 C39 O7 123.7(4) . . ?
C38 C39 C40 121.9(4) . . ?
O7 C39 C40 114.4(3) . . ?
O6 C40 C35 124.0(4) . . ?
O6 C40 C39 118.8(3) . . ?
C35 C40 C39 117.2(3) . . ?
O8 C41 H41A 109.5 . . ?
O8 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O8 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O7 C42 H42A 109.5 . . ?
O7 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O7 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O9 C43 H43A 109.5 . . ?
O9 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O9 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C7 N1 C8 120.8(4) . . ?
C7 N1 Cu1 124.0(3) . . ?
C8 N1 Cu1 115.0(3) . . ?
C13 N2 C12 120.5(4) . . ?
C13 N2 Cu1 124.5(3) . . ?
C12 N2 Cu1 114.6(3) . . ?
C28 N3 C29 116.9(4) . . ?
C28 N3 Cu2 120.9(3) . . ?
C29 N3 Cu2 122.1(3) . . ?
C34 N4 C33 117.4(4) . . ?
C34 N4 Cu2 121.8(3) . . ?
C33 N4 Cu2 120.7(3) . . ?
N6 N5 Pr2 128.1(3) . . ?
N6 N5 Pr1 115.6(2) . . ?
Pr2 N5 Pr1 100.73(10) . . ?
N7 N6 N5 177.4(4) . . ?
N9 N8 Pr1 127.8(3) . . ?
N9 N8 Pr2 129.7(3) . . ?
Pr1 N8 Pr2 100.79(12) . . ?
N10 N9 N8 179.3(5) . . ?
N12 N11 Pr2 120.4(3) . . ?
N12 N11 Pr1 130.7(3) . . ?
Pr2 N11 Pr1 102.56(13) . . ?
N13 N12 N11 177.8(5) . . ?
N15 N14 Pr1 165.8(4) . . ?
N16 N15 N14 178.5(6) . . ?
N18 N17 Pr2 148.1(3) . . ?
N19 N18 N17 179.3(6) . . ?
N21 N20 Cu2 125.6(3) . . ?
N22 N21 N20 177.3(4) . . ?
N21 N22 Pr1 130.5(3) . 1_455 ?
C1 O1 Cu1 125.2(2) . . ?
C1 O1 Pr1 127.0(2) . . ?
Cu1 O1 Pr1 106.54(11) . . ?
C19 O2 Cu1 122.5(2) . . ?
C19 O2 Pr1 128.4(2) . . ?
Cu1 O2 Pr1 108.15(11) . . ?
C18 O3 C21 116.5(3) . . ?
C18 O3 Pr1 118.1(2) . . ?
C21 O3 Pr1 125.4(3) . . ?
C2 O4 C20 117.1(4) . . ?
C2 O4 Pr1 120.0(2) . . ?
C20 O4 Pr1 121.0(3) . . ?
C22 O5 Cu2 122.0(2) . . ?
C22 O5 Pr2 124.3(2) . . ?
Cu2 O5 Pr2 105.87(10) . . ?
C40 O6 Cu2 120.4(2) . . ?
C40 O6 Pr2 124.9(2) . . ?
Cu2 O6 Pr2 106.83(10) . . ?
C39 O7 C42 116.6(3) . . ?
C39 O7 Pr2 118.9(2) . . ?
C42 O7 Pr2 124.3(2) . . ?
C23 O8 C41 116.3(3) . . ?
C23 O8 Pr2 118.0(2) . . ?
C41 O8 Pr2 125.4(2) . . ?
C43 O9 Pr2 134.4(3) . . ?
C43 O9 H9 111.8 . . ?
Pr2 O9 H9 109.6 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.68
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.514
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.104
####################################################################### 
# 
# 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_CuHovaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060769'
_audit_update_record             
;
2017-04-26 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuHovaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Cu2 Ho2 N22 O9'
_chemical_formula_weight         1478.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.205(6)
_cell_length_b                   9.666(2)
_cell_length_c                   25.926(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.841(3)
_cell_angle_gamma                90.00
_cell_volume                     5234(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9975
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.63

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.875
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2912
_exptl_absorpt_coefficient_mu    3.868
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.3365
_exptl_absorpt_correction_T_max  0.4833
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX SMART'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32654
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.66
_reflns_number_total             6092
_reflns_number_gt                5638
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0264P)²+11.4089P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6092
_refine_ls_number_parameters     361
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0271
_refine_ls_wR_factor_ref         0.0657
_refine_ls_wR_factor_gt          0.0644
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_restrained_S_all      1.174
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ho1 Ho 0.286480(6) 0.345234(14) 0.073307(6) 0.02600(5) Uani 1 1 d . . .
Cu1 Cu 0.442512(17) 0.23584(4) 0.100696(16) 0.02850(9) Uani 1 1 d . . .
C1 C 0.40742(15) 0.5273(3) 0.06743(13) 0.0307(7) Uani 1 1 d . . .
C2 C 0.36320(16) 0.6354(3) 0.05625(14) 0.0326(7) Uani 1 1 d . . .
C3 C 0.37838(19) 0.7657(4) 0.04320(16) 0.0418(8) Uani 1 1 d . . .
H3 H 0.3482 0.8363 0.0364 0.050 Uiso 1 1 calc R . .
C4 C 0.43823(19) 0.7920(4) 0.04021(17) 0.0466(9) Uani 1 1 d . . .
H4 H 0.4480 0.8794 0.0303 0.056 Uiso 1 1 calc R . .
C5 C 0.48305(19) 0.6890(4) 0.05180(17) 0.0455(9) Uani 1 1 d . . .
H5 H 0.5234 0.7070 0.0499 0.055 Uiso 1 1 calc R . .
C6 C 0.46883(16) 0.5557(4) 0.06655(15) 0.0374(8) Uani 1 1 d . . .
C7 C 0.52012(16) 0.4572(4) 0.08169(16) 0.0412(8) Uani 1 1 d . . .
H7 H 0.5588 0.4884 0.0794 0.049 Uiso 1 1 calc R . .
C8 C 0.58255(18) 0.2623(5) 0.1112(2) 0.0539(11) Uani 1 1 d . . .
H8A H 0.6160 0.3318 0.1228 0.065 Uiso 1 1 calc R . .
H8B H 0.5850 0.2199 0.0780 0.065 Uiso 1 1 calc R . .
C9 C 0.59596(15) 0.1532(4) 0.15494(15) 0.0343(7) Uani 1 1 d . . .
C10 C 0.66365(17) 0.1006(4) 0.16427(18) 0.0470(9) Uani 1 1 d . . .
H10A H 0.6654 0.0597 0.1311 0.070 Uiso 1 1 calc R . .
H10B H 0.6748 0.0326 0.1929 0.070 Uiso 1 1 calc R . .
H10C H 0.6932 0.1765 0.1747 0.070 Uiso 1 1 calc R . .
C11 C 0.5914(2) 0.2094(5) 0.20809(17) 0.0558(11) Uani 1 1 d . . .
H11A H 0.6235 0.2792 0.2224 0.084 Uiso 1 1 calc R . .
H11B H 0.5981 0.1355 0.2342 0.084 Uiso 1 1 calc R . .
H11C H 0.5498 0.2490 0.2013 0.084 Uiso 1 1 calc R . .
C12 C 0.55029(17) 0.0326(4) 0.13384(18) 0.0436(9) Uani 1 1 d . . .
H12A H 0.5480 0.0109 0.0967 0.052 Uiso 1 1 calc R . .
H12B H 0.5670 -0.0480 0.1564 0.052 Uiso 1 1 calc R . .
C13 C 0.46166(17) -0.0288(4) 0.15749(15) 0.0379(8) Uani 1 1 d . . .
H13 H 0.4868 -0.1066 0.1708 0.046 Uiso 1 1 calc R . .
C14 C 0.40068(16) -0.0260(3) 0.16564(14) 0.0342(7) Uani 1 1 d . . .
C15 C 0.38821(19) -0.1318(4) 0.19797(16) 0.0419(8) Uani 1 1 d . . .
H15 H 0.4182 -0.2017 0.2117 0.050 Uiso 1 1 calc R . .
C16 C 0.3322(2) -0.1327(4) 0.20943(16) 0.0453(9) Uani 1 1 d . . .
H16 H 0.3242 -0.2034 0.2306 0.054 Uiso 1 1 calc R . .
C17 C 0.28751(18) -0.0282(4) 0.18950(14) 0.0384(8) Uani 1 1 d . . .
H17 H 0.2497 -0.0282 0.1975 0.046 Uiso 1 1 calc R . .
C18 C 0.29922(16) 0.0749(3) 0.15795(13) 0.0323(7) Uani 1 1 d . . .
C19 C 0.35527(15) 0.0773(3) 0.14403(12) 0.0291(6) Uani 1 1 d . . .
C20 C 0.26752(19) 0.7067(4) 0.07272(17) 0.0441(9) Uani 1 1 d . . .
H20A H 0.2935 0.7455 0.1072 0.066 Uiso 1 1 calc R . .
H20B H 0.2292 0.6684 0.0763 0.066 Uiso 1 1 calc R . .
H20C H 0.2564 0.7779 0.0453 0.066 Uiso 1 1 calc R . .
C21 C 0.2113(2) 0.2132(5) 0.1624(2) 0.0596(12) Uani 1 1 d . . .
H21A H 0.1791 0.1426 0.1519 0.089 Uiso 1 1 calc R . .
H21B H 0.1920 0.3017 0.1504 0.089 Uiso 1 1 calc R . .
H21C H 0.2311 0.2136 0.2016 0.089 Uiso 1 1 calc R . .
O5 O 0.4778(6) 0.6130(12) 0.2813(5) 0.149(4) Uani 0.50 1 d PDU . .
N1 N 0.51998(13) 0.3319(3) 0.09792(12) 0.0359(6) Uani 1 1 d . . .
N2 N 0.48570(13) 0.0623(3) 0.13426(12) 0.0342(6) Uani 1 1 d . . .
N3 N 0.31023(18) 0.4604(4) 0.15678(14) 0.0536(9) Uani 1 1 d . . .
N4 N 0.31965(15) 0.4899(3) 0.20149(13) 0.0392(7) Uani 1 1 d . . .
N5 N 0.3289(2) 0.5225(5) 0.24628(17) 0.0796(14) Uani 1 1 d . . .
N6 N 0.27153(14) 0.3537(3) -0.02157(12) 0.0354(6) Uani 1 1 d . . .
N7 N 0.30449(18) 0.4307(4) -0.04103(14) 0.0540(9) Uani 1 1 d . . .
N8 N 0.3342(2) 0.5004(6) -0.05955(19) 0.0888(16) Uani 1 1 d . . .
N9 N 0.41835(15) 0.1467(4) 0.01054(14) 0.0468(8) Uani 1 1 d . . .
N10 N 0.36907(13) 0.1129(3) -0.01911(11) 0.0310(6) Uani 1 1 d . . .
N11 N 0.31989(14) 0.0754(3) -0.05025(13) 0.0431(7) Uani 1 1 d . . .
O1 O 0.38963(10) 0.4021(2) 0.07826(10) 0.0314(5) Uani 1 1 d . . .
O2 O 0.36318(11) 0.1799(2) 0.11274(10) 0.0317(5) Uani 1 1 d . . .
O3 O 0.30293(11) 0.5989(2) 0.05683(10) 0.0353(5) Uani 1 1 d . . .
O4 O 0.25896(12) 0.1860(3) 0.13765(10) 0.0394(6) Uani 1 1 d . . .
C22 C 0.5000 0.5219(17) 0.2500 0.169(5) Uani 1 2 d SDU . .


_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
Ho1 O2 2.306(2) . ?
Ho1 O1 2.316(2) . ?
Ho1 N3 2.330(3) . ?
Ho1 N11 2.360(3) 7 ?
Ho1 N6 2.369(3) . ?
Ho1 N6 2.446(3) 7 ?
Ho1 O4 2.494(2) . ?
Ho1 O3 2.536(2) . ?
Ho1 Cu1 3.4578(9) . ?
Cu1 O1 1.959(2) . ?
Cu1 O2 1.966(2) . ?
Cu1 N1 1.978(3) . ?
Cu1 N2 1.981(3) . ?
Cu1 N9 2.375(3) . ?
C1 O1 1.332(4) . ?
C1 C2 1.396(5) . ?
C1 C6 1.399(4) . ?
C2 C3 1.375(5) . ?
C2 O3 1.389(4) . ?
C3 C4 1.381(5) . ?
C4 C5 1.367(6) . ?
C5 C6 1.410(5) . ?
C6 C7 1.433(5) . ?
C7 N1 1.282(4) . ?
C8 N1 1.476(4) . ?
C8 C9 1.502(5) . ?
C9 C11 1.516(5) . ?
C9 C12 1.520(5) . ?
C9 C10 1.526(5) . ?
C12 N2 1.466(4) . ?
C13 N2 1.281(4) . ?
C13 C14 1.440(5) . ?
C14 C19 1.395(5) . ?
C14 C15 1.408(5) . ?
C15 C16 1.374(6) . ?
C16 C17 1.387(5) . ?
C17 C18 1.369(4) . ?
C18 O4 1.382(4) . ?
C18 C19 1.409(4) . ?
C19 O2 1.330(4) . ?
C20 O3 1.447(4) . ?
C21 O4 1.435(4) . ?
O5 C22 1.3955(11) . ?
N3 N4 1.142(4) . ?
N4 N5 1.153(5) . ?
N6 N7 1.263(4) . ?
N6 Ho1 2.446(3) 7 ?
N7 N8 1.155(5) . ?
N9 N10 1.151(4) . ?
N10 N11 1.174(4) . ?
N11 Ho1 2.360(3) 7 ?
C22 O5 1.3956(11) 2_655 ?

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
O2 Ho1 O1 64.68(8) . . ?
O2 Ho1 N3 91.09(11) . . ?
O1 Ho1 N3 85.83(11) . . ?
O2 Ho1 N11 149.64(10) . 7 ?
O1 Ho1 N11 145.37(10) . 7 ?
N3 Ho1 N11 88.36(12) . 7 ?
O2 Ho1 N6 107.84(9) . . ?
O1 Ho1 N6 80.61(9) . . ?
N3 Ho1 N6 148.86(11) . . ?
N11 Ho1 N6 87.15(11) 7 . ?
O2 Ho1 N6 82.56(9) . 7 ?
O1 Ho1 N6 122.94(9) . 7 ?
N3 Ho1 N6 142.76(12) . 7 ?
N11 Ho1 N6 79.70(11) 7 7 ?
N6 Ho1 N6 66.15(12) . 7 ?
O2 Ho1 O4 65.63(8) . . ?
O1 Ho1 O4 124.87(8) . . ?
N3 Ho1 O4 72.73(12) . . ?
N11 Ho1 O4 85.34(10) 7 . ?
N6 Ho1 O4 137.40(9) . . ?
N6 Ho1 O4 71.25(10) 7 . ?
O2 Ho1 O3 128.15(8) . . ?
O1 Ho1 O3 65.40(7) . . ?
N3 Ho1 O3 72.21(11) . . ?
N11 Ho1 O3 80.32(10) 7 . ?
N6 Ho1 O3 76.66(9) . . ?
N6 Ho1 O3 138.31(9) 7 . ?
O4 Ho1 O3 142.32(8) . . ?
O2 Ho1 Cu1 32.79(5) . . ?
O1 Ho1 Cu1 32.67(6) . . ?
N3 Ho1 Cu1 93.45(9) . . ?
N11 Ho1 Cu1 177.02(8) 7 . ?
N6 Ho1 Cu1 90.08(7) . . ?
N6 Ho1 Cu1 100.17(7) 7 . ?
O4 Ho1 Cu1 97.46(6) . . ?
O3 Ho1 Cu1 97.97(5) . . ?
O1 Cu1 O2 78.10(9) . . ?
O1 Cu1 N1 92.57(11) . . ?
O2 Cu1 N1 166.44(11) . . ?
O1 Cu1 N2 167.77(10) . . ?
O2 Cu1 N2 91.35(10) . . ?
N1 Cu1 N2 96.69(12) . . ?
O1 Cu1 N9 95.34(11) . . ?
O2 Cu1 N9 98.12(11) . . ?
N1 Cu1 N9 92.48(12) . . ?
N2 Cu1 N9 92.24(12) . . ?
O1 Cu1 Ho1 39.66(6) . . ?
O2 Cu1 Ho1 39.43(6) . . ?
N1 Cu1 Ho1 132.23(8) . . ?
N2 Cu1 Ho1 130.62(8) . . ?
N9 Cu1 Ho1 91.89(8) . . ?
O1 C1 C2 119.1(3) . . ?
O1 C1 C6 122.9(3) . . ?
C2 C1 C6 118.1(3) . . ?
C3 C2 O3 123.6(3) . . ?
C3 C2 C1 121.5(3) . . ?
O3 C2 C1 114.8(3) . . ?
C2 C3 C4 120.2(3) . . ?
C5 C4 C3 119.8(3) . . ?
C4 C5 C6 120.8(3) . . ?
C1 C6 C5 119.6(3) . . ?
C1 C6 C7 123.6(3) . . ?
C5 C6 C7 116.8(3) . . ?
N1 C7 C6 128.8(3) . . ?
N1 C8 C9 115.2(3) . . ?
C8 C9 C11 112.2(3) . . ?
C8 C9 C12 109.2(3) . . ?
C11 C9 C12 111.1(3) . . ?
C8 C9 C10 106.6(3) . . ?
C11 C9 C10 109.9(3) . . ?
C12 C9 C10 107.6(3) . . ?
N2 C12 C9 112.5(3) . . ?
N2 C13 C14 128.2(3) . . ?
C19 C14 C15 119.9(3) . . ?
C19 C14 C13 122.8(3) . . ?
C15 C14 C13 117.3(3) . . ?
C16 C15 C14 120.6(3) . . ?
C15 C16 C17 120.1(3) . . ?
C18 C17 C16 119.7(3) . . ?
C17 C18 O4 124.3(3) . . ?
C17 C18 C19 121.9(3) . . ?
O4 C18 C19 113.8(3) . . ?
O2 C19 C14 123.5(3) . . ?
O2 C19 C18 118.7(3) . . ?
C14 C19 C18 117.8(3) . . ?
C7 N1 C8 113.6(3) . . ?
C7 N1 Cu1 123.7(2) . . ?
C8 N1 Cu1 122.6(2) . . ?
C13 N2 C12 115.7(3) . . ?
C13 N2 Cu1 124.9(2) . . ?
C12 N2 Cu1 119.4(2) . . ?
N4 N3 Ho1 165.5(3) . . ?
N3 N4 N5 178.5(4) . . ?
N7 N6 Ho1 122.6(2) . . ?
N7 N6 Ho1 120.9(2) . 7 ?
Ho1 N6 Ho1 113.85(12) . 7 ?
N8 N7 N6 179.0(5) . . ?
N10 N9 Cu1 127.3(3) . . ?
N9 N10 N11 177.6(4) . . ?
N10 N11 Ho1 133.7(2) . 7 ?
C1 O1 Cu1 128.12(19) . . ?
C1 O1 Ho1 124.22(19) . . ?
Cu1 O1 Ho1 107.67(9) . . ?
C19 O2 Cu1 127.8(2) . . ?
C19 O2 Ho1 123.82(19) . . ?
Cu1 O2 Ho1 107.79(9) . . ?
C2 O3 C20 116.0(3) . . ?
C2 O3 Ho1 116.23(18) . . ?
C20 O3 Ho1 121.7(2) . . ?
C18 O4 C21 116.8(3) . . ?
C18 O4 Ho1 117.43(18) . . ?
C21 O4 Ho1 124.8(2) . . ?
O5 C22 O5 101.7(16) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.66
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.092
####################################################################### 
# 
# 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_CuDyvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1540634'
_audit_update_record             
;
2017-04-26 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuDyvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 Cu2 Dy2 N22 O10'
_chemical_formula_weight         1505.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.900(3)
_cell_length_b                   10.778(3)
_cell_length_c                   13.432(4)
_cell_angle_alpha                99.895(8)
_cell_angle_beta                 91.177(7)
_cell_angle_gamma                100.921(7)
_cell_volume                     1384.2(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6541
_cell_measurement_theta_min      1.54
_cell_measurement_theta_max      27.91

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    3.501
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_T_max  0.8444
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30861
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         27.91
_reflns_number_total             6541
_reflns_number_gt                5755
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0302P)²+0.5435P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6541
_refine_ls_number_parameters     384
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0259
_refine_ls_wR_factor_ref         0.0643
_refine_ls_wR_factor_gt          0.0618
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy -0.063427(13) 0.558493(13) 0.139922(10) 0.02944(5) Uani 1 1 d . . .
Cu1 Cu 0.19316(4) 0.82901(4) 0.20652(3) 0.03663(9) Uani 1 1 d . . .
C1 C -0.0803(3) 0.8531(3) 0.1264(2) 0.0331(6) Uani 1 1 d . . .
C2 C -0.2223(3) 0.7996(3) 0.1059(2) 0.0350(7) Uani 1 1 d . . .
C3 C -0.3142(3) 0.8719(3) 0.0816(3) 0.0416(7) Uani 1 1 d . . .
H3 H -0.4069 0.8346 0.0679 0.050 Uiso 1 1 calc R . .
C4 C -0.2684(4) 1.0007(4) 0.0774(3) 0.0481(8) Uani 1 1 d . . .
H4 H -0.3302 1.0496 0.0603 0.058 Uiso 1 1 calc R . .
C5 C -0.1315(4) 1.0560(3) 0.0986(3) 0.0496(9) Uani 1 1 d . . .
H5 H -0.1018 1.1425 0.0960 0.059 Uiso 1 1 calc R . .
C6 C -0.0359(3) 0.9837(3) 0.1240(3) 0.0391(7) Uani 1 1 d . . .
C7 C 0.1059(4) 1.0480(3) 0.1449(3) 0.0452(8) Uani 1 1 d . . .
H7 H 0.1267 1.1324 0.1343 0.054 Uiso 1 1 calc R . .
C8 C 0.3429(4) 1.0899(4) 0.1848(3) 0.0552(10) Uani 1 1 d . . .
H8A H 0.3302 1.1746 0.1765 0.066 Uiso 1 1 calc R . .
H8B H 0.3974 1.0587 0.1302 0.066 Uiso 1 1 calc R . .
C9 C 0.4221(3) 1.1012(3) 0.2846(3) 0.0457(8) Uani 1 1 d . . .
C10 C 0.5490(4) 1.2089(4) 0.2867(3) 0.0677(12) Uani 1 1 d . . .
H10A H 0.5197 1.2888 0.2865 0.102 Uiso 1 1 calc R . .
H10B H 0.6005 1.1896 0.2282 0.102 Uiso 1 1 calc R . .
H10C H 0.6060 1.2156 0.3468 0.102 Uiso 1 1 calc R . .
C11 C 0.3374(5) 1.1338(4) 0.3743(4) 0.0774(15) Uani 1 1 d . . .
H11A H 0.3933 1.1460 0.4357 0.116 Uiso 1 1 calc R . .
H11B H 0.2601 1.0650 0.3741 0.116 Uiso 1 1 calc R . .
H11C H 0.3051 1.2114 0.3699 0.116 Uiso 1 1 calc R . .
C12 C 0.4751(4) 0.9784(4) 0.2880(3) 0.0553(10) Uani 1 1 d . . .
H12A H 0.5274 0.9605 0.2287 0.066 Uiso 1 1 calc R . .
H12B H 0.5377 0.9925 0.3471 0.066 Uiso 1 1 calc R . .
C13 C 0.3972(3) 0.7882(3) 0.3479(3) 0.0448(8) Uani 1 1 d . . .
H13 H 0.4817 0.8150 0.3843 0.054 Uiso 1 1 calc R . .
C14 C 0.3188(3) 0.6675(3) 0.3631(3) 0.0416(7) Uani 1 1 d . . .
C15 C 0.3657(4) 0.6103(4) 0.4400(3) 0.0557(10) Uani 1 1 d . . .
H15 H 0.4480 0.6497 0.4765 0.067 Uiso 1 1 calc R . .
C16 C 0.2943(4) 0.4993(4) 0.4627(3) 0.0644(11) Uani 1 1 d . . .
H16 H 0.3258 0.4646 0.5154 0.077 Uiso 1 1 calc R . .
C17 C 0.1736(4) 0.4378(4) 0.4063(3) 0.0529(9) Uani 1 1 d . . .
H17 H 0.1237 0.3620 0.4219 0.064 Uiso 1 1 calc R . .
C18 C 0.1275(3) 0.4878(3) 0.3283(2) 0.0380(7) Uani 1 1 d . . .
C19 C 0.1972(3) 0.6053(3) 0.3055(2) 0.0355(7) Uani 1 1 d . . .
C20 C -0.4011(3) 0.6195(4) 0.1208(3) 0.0533(9) Uani 1 1 d . . .
H20A H -0.4376 0.6733 0.1738 0.080 Uiso 1 1 calc R . .
H20B H -0.4111 0.5345 0.1359 0.080 Uiso 1 1 calc R . .
H20C H -0.4504 0.6162 0.0578 0.080 Uiso 1 1 calc R . .
C21 C -0.0847(4) 0.3360(4) 0.3028(3) 0.0591(11) Uani 1 1 d . . .
H21A H -0.0456 0.2616 0.3057 0.089 Uiso 1 1 calc R . .
H21B H -0.1667 0.3119 0.2588 0.089 Uiso 1 1 calc R . .
H21C H -0.1074 0.3716 0.3694 0.089 Uiso 1 1 calc R . .
C22 C 0.196(2) 0.9309(14) 0.5762(17) 0.218(13) Uani 0.565(9) 1 d PD A 1
C22' C 0.0930(13) 0.8668(19) 0.4826(6) 0.085(5) Uani 0.435(9) 1 d PD A 2
N1 N 0.2072(3) 1.0035(3) 0.1764(2) 0.0430(7) Uani 1 1 d . . .
N2 N 0.3671(3) 0.8643(3) 0.2913(2) 0.0403(6) Uani 1 1 d . . .
N3 N -0.1628(4) 0.6086(4) 0.2994(2) 0.0585(9) Uani 1 1 d . . .
N4 N -0.2122(4) 0.6896(4) 0.3367(3) 0.0664(10) Uani 1 1 d . . .
N5 N -0.2624(6) 0.7737(6) 0.3751(4) 0.132(2) Uani 1 1 d . . .
N6 N 0.0895(3) 0.4438(3) 0.0427(2) 0.0361(6) Uani 1 1 d . . .
N7 N 0.1930(3) 0.4191(3) 0.0844(2) 0.0509(7) Uani 1 1 d . . .
N8 N 0.2892(4) 0.3964(5) 0.1231(3) 0.0879(14) Uani 1 1 d . . .
N9 N 0.3211(3) 0.7661(3) 0.0562(2) 0.0472(7) Uani 1 1 d . . .
N10 N 0.2782(2) 0.6971(2) -0.0174(2) 0.0340(6) Uani 1 1 d . . .
N11 N 0.2368(3) 0.6289(3) -0.0948(2) 0.0456(7) Uani 1 1 d . . .
O1 O 0.0039(2) 0.77711(19) 0.14593(17) 0.0350(5) Uani 1 1 d . . .
O2 O 0.1453(2) 0.6522(2) 0.23111(16) 0.0358(5) Uani 1 1 d . . .
O3 O -0.2572(2) 0.6716(2) 0.11301(18) 0.0378(5) Uani 1 1 d . . .
O4 O 0.0134(2) 0.4302(2) 0.26429(17) 0.0398(5) Uani 1 1 d . . .
O5 O 0.0784(18) 0.8708(16) 0.5145(17) 0.258(10) Uani 0.565(9) 1 d PD A 1
O5' O 0.0629(7) 0.8786(7) 0.3831(6) 0.074(3) Uani 0.435(9) 1 d PD A 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
Dy1 O1 2.311(2) . ?
Dy1 O2 2.339(2) . ?
Dy1 N11 2.370(3) 2_565 ?
Dy1 N3 2.395(3) . ?
Dy1 N6 2.400(3) . ?
Dy1 N6 2.456(3) 2_565 ?
Dy1 O3 2.511(2) . ?
Dy1 O4 2.534(2) . ?
Dy1 Cu1 3.4580(9) . ?
Cu1 O2 1.961(2) . ?
Cu1 O1 1.967(2) . ?
Cu1 N1 1.971(3) . ?
Cu1 N2 1.982(3) . ?
Cu1 N9 2.471(3) . ?
C1 O1 1.326(3) . ?
C1 C6 1.400(4) . ?
C1 C2 1.417(4) . ?
C2 C3 1.373(4) . ?
C2 O3 1.377(4) . ?
C3 C4 1.388(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.375(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.406(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.442(5) . ?
C7 N1 1.284(4) . ?
C7 H7 0.9300 . ?
C8 N1 1.472(4) . ?
C8 C9 1.514(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C11 1.511(5) . ?
C9 C12 1.520(6) . ?
C9 C10 1.537(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.476(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.280(4) . ?
C13 C14 1.432(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.404(5) . ?
C14 C19 1.405(4) . ?
C15 C16 1.355(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.389(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.365(4) . ?
C17 H17 0.9300 . ?
C18 O4 1.382(4) . ?
C18 C19 1.408(4) . ?
C19 O2 1.330(3) . ?
C20 O3 1.442(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O4 1.439(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.3947(11) . ?
C22' O5' 1.3953(11) . ?
N3 N4 1.128(5) . ?
N4 N5 1.165(6) . ?
N6 N7 1.252(4) . ?
N6 Dy1 2.456(3) 2_565 ?
N7 N8 1.160(4) . ?
N9 N10 1.149(4) . ?
N10 N11 1.181(4) . ?
N11 Dy1 2.370(3) 2_565 ?

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 Dy1 O2 65.10(7) . . ?
O1 Dy1 N11 148.06(9) . 2_565 ?
O2 Dy1 N11 146.28(9) . 2_565 ?
O1 Dy1 N3 87.32(11) . . ?
O2 Dy1 N3 84.24(11) . . ?
N11 Dy1 N3 90.40(12) 2_565 . ?
O1 Dy1 N6 110.77(8) . . ?
O2 Dy1 N6 79.97(8) . . ?
N11 Dy1 N6 87.39(10) 2_565 . ?
N3 Dy1 N6 147.65(10) . . ?
O1 Dy1 N6 82.73(8) . 2_565 ?
O2 Dy1 N6 121.03(8) . 2_565 ?
N11 Dy1 N6 80.83(10) 2_565 2_565 ?
N3 Dy1 N6 144.55(10) . 2_565 ?
N6 Dy1 N6 66.69(10) . 2_565 ?
O1 Dy1 O3 65.53(7) . . ?
O2 Dy1 O3 125.58(7) . . ?
N11 Dy1 O3 83.47(9) 2_565 . ?
N3 Dy1 O3 72.02(10) . . ?
N6 Dy1 O3 139.46(8) . . ?
N6 Dy1 O3 72.88(8) 2_565 . ?
O1 Dy1 O4 126.23(7) . . ?
O2 Dy1 O4 64.73(7) . . ?
N11 Dy1 O4 82.16(9) 2_565 . ?
N3 Dy1 O4 69.74(10) . . ?
N6 Dy1 O4 77.99(8) . . ?
N6 Dy1 O4 141.22(8) 2_565 . ?
O3 Dy1 O4 138.85(7) . . ?
O1 Dy1 Cu1 32.83(5) . . ?
O2 Dy1 Cu1 32.90(5) . . ?
N11 Dy1 Cu1 179.10(7) 2_565 . ?
N3 Dy1 Cu1 89.82(10) . . ?
N6 Dy1 Cu1 91.97(7) . . ?
N6 Dy1 Cu1 99.49(6) 2_565 . ?
O3 Dy1 Cu1 97.42(5) . . ?
O4 Dy1 Cu1 97.10(5) . . ?
O2 Cu1 O1 79.12(8) . . ?
O2 Cu1 N1 170.19(10) . . ?
O1 Cu1 N1 91.34(10) . . ?
O2 Cu1 N2 92.33(10) . . ?
O1 Cu1 N2 167.93(11) . . ?
N1 Cu1 N2 96.75(12) . . ?
O2 Cu1 N9 92.72(10) . . ?
O1 Cu1 N9 99.51(10) . . ?
N1 Cu1 N9 91.09(11) . . ?
N2 Cu1 N9 89.31(11) . . ?
O2 Cu1 Dy1 40.37(6) . . ?
O1 Cu1 Dy1 39.57(6) . . ?
N1 Cu1 Dy1 130.49(8) . . ?
N2 Cu1 Dy1 132.69(8) . . ?
N9 Cu1 Dy1 91.75(7) . . ?
O1 C1 C6 123.3(3) . . ?
O1 C1 C2 118.6(3) . . ?
C6 C1 C2 118.1(3) . . ?
C3 C2 O3 124.4(3) . . ?
C3 C2 C1 121.5(3) . . ?
O3 C2 C1 114.1(3) . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 121.0(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.5(3) . . ?
C1 C6 C7 122.5(3) . . ?
C5 C6 C7 118.0(3) . . ?
N1 C7 C6 128.3(3) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
N1 C8 C9 113.6(3) . . ?
N1 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C11 C9 C8 112.2(4) . . ?
C11 C9 C12 111.4(4) . . ?
C8 C9 C12 109.9(3) . . ?
C11 C9 C10 109.7(3) . . ?
C8 C9 C10 106.5(3) . . ?
C12 C9 C10 107.0(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 114.8(3) . . ?
N2 C12 H12A 108.6 . . ?
C9 C12 H12A 108.6 . . ?
N2 C12 H12B 108.6 . . ?
C9 C12 H12B 108.6 . . ?
H12A C12 H12B 107.5 . . ?
N2 C13 C14 129.0(3) . . ?
N2 C13 H13 115.5 . . ?
C14 C13 H13 115.5 . . ?
C15 C14 C19 119.0(3) . . ?
C15 C14 C13 118.0(3) . . ?
C19 C14 C13 123.0(3) . . ?
C16 C15 C14 121.8(3) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C17 119.3(3) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C18 C17 C16 120.5(4) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 O4 124.8(3) . . ?
C17 C18 C19 121.2(3) . . ?
O4 C18 C19 114.0(3) . . ?
O2 C19 C14 123.2(3) . . ?
O2 C19 C18 118.8(3) . . ?
C14 C19 C18 118.0(3) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 N1 C8 115.8(3) . . ?
C7 N1 Cu1 124.7(2) . . ?
C8 N1 Cu1 119.5(2) . . ?
C13 N2 C12 115.4(3) . . ?
C13 N2 Cu1 123.2(2) . . ?
C12 N2 Cu1 121.2(2) . . ?
N4 N3 Dy1 134.7(3) . . ?
N3 N4 N5 179.6(6) . . ?
N7 N6 Dy1 120.7(2) . . ?
N7 N6 Dy1 123.5(2) . 2_565 ?
Dy1 N6 Dy1 113.32(10) . 2_565 ?
N8 N7 N6 179.8(5) . . ?
N10 N9 Cu1 127.2(2) . . ?
N9 N10 N11 177.7(3) . . ?
N10 N11 Dy1 133.9(2) . 2_565 ?
C1 O1 Cu1 127.44(19) . . ?
C1 O1 Dy1 124.16(18) . . ?
Cu1 O1 Dy1 107.61(8) . . ?
C19 O2 Cu1 126.51(18) . . ?
C19 O2 Dy1 124.31(18) . . ?
Cu1 O2 Dy1 106.72(9) . . ?
C2 O3 C20 117.1(2) . . ?
C2 O3 Dy1 117.16(16) . . ?
C20 O3 Dy1 124.9(2) . . ?
C18 O4 C21 115.4(3) . . ?
C18 O4 Dy1 117.51(18) . . ?
C21 O4 Dy1 120.7(2) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.91
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.086
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.097
####################################################################### 
# 
# 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_1-CuLavaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060760'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuLavaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Cu2 La2 N22 O9'
_chemical_formula_weight         1425.97

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P-1 '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.347(3)
_cell_length_b                   12.658(3)
_cell_length_c                   19.676(4)
_cell_angle_alpha                76.529(3)
_cell_angle_beta                 87.164(4)
_cell_angle_gamma                64.664(3)
_cell_volume                     2698.5(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4278
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      25.78

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1416
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5528
_exptl_absorpt_correction_T_max  0.8893
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18645
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         27.62
_reflns_number_total             12394
_reflns_number_gt                9174
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker ApexII'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0359P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12394
_refine_ls_number_parameters     682
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_ref         0.0905
_refine_ls_wR_factor_gt          0.0816
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
La1 La 0.47856(2) 0.45274(2) 0.229128(13) 0.02846(7) Uani 1 1 d . . .
La2 La 0.13806(2) 0.50082(2) 0.281276(12) 0.02558(7) Uani 1 1 d . . .
Cu1 Cu 0.50314(5) 0.69365(5) 0.28429(3) 0.03486(14) Uani 1 1 d . . .
Cu2 Cu 0.06134(5) 0.32310(4) 0.19134(3) 0.03088(13) Uani 1 1 d . . .
C1 C 0.4443(4) 0.7380(4) 0.1370(2) 0.0371(11) Uani 1 1 d . . .
C2 C 0.4112(5) 0.7040(4) 0.0804(2) 0.0433(12) Uani 1 1 d . . .
C3 C 0.3787(5) 0.7801(5) 0.0150(3) 0.0605(15) Uani 1 1 d . . .
H3 H 0.3586 0.7557 -0.0217 0.073 Uiso 1 1 calc R . .
C4 C 0.3761(6) 0.8940(5) 0.0039(3) 0.0709(18) Uani 1 1 d . . .
H4 H 0.3527 0.9464 -0.0401 0.085 Uiso 1 1 calc R . .
C5 C 0.4077(6) 0.9291(5) 0.0573(3) 0.0607(16) Uani 1 1 d . . .
H5 H 0.4068 1.0049 0.0491 0.073 Uiso 1 1 calc R . .
C6 C 0.4415(5) 0.8533(4) 0.1240(2) 0.0418(12) Uani 1 1 d . . .
C7 C 0.4864(5) 0.8934(5) 0.1746(3) 0.0501(13) Uani 1 1 d . . .
H7 H 0.4929 0.9655 0.1590 0.060 Uiso 1 1 calc R . .
C8 C 0.5809(5) 0.8808(5) 0.2808(3) 0.0532(14) Uani 1 1 d . . .
H8A H 0.5961 0.9449 0.2507 0.064 Uiso 1 1 calc R . .
H8B H 0.6580 0.8148 0.2985 0.064 Uiso 1 1 calc R . .
C9 C 0.5121(5) 0.9264(4) 0.3429(3) 0.0424(12) Uani 1 1 d . . .
C10 C 0.4212(5) 1.0566(4) 0.3176(3) 0.0662(17) Uani 1 1 d . . .
H10A H 0.3743 1.0835 0.3558 0.099 Uiso 1 1 calc R . .
H10B H 0.3693 1.0628 0.2807 0.099 Uiso 1 1 calc R . .
H10C H 0.4626 1.1058 0.3005 0.099 Uiso 1 1 calc R . .
C11 C 0.6058(6) 0.9165(5) 0.3944(3) 0.0679(17) Uani 1 1 d . . .
H11A H 0.6496 0.9603 0.3713 0.102 Uiso 1 1 calc R . .
H11B H 0.6602 0.8335 0.4114 0.102 Uiso 1 1 calc R . .
H11C H 0.5667 0.9495 0.4329 0.102 Uiso 1 1 calc R . .
C12 C 0.4442(5) 0.8525(4) 0.3779(3) 0.0474(13) Uani 1 1 d . . .
H12A H 0.4334 0.8584 0.4262 0.057 Uiso 1 1 calc R . .
H12B H 0.3652 0.8869 0.3545 0.057 Uiso 1 1 calc R . .
C13 C 0.5455(4) 0.6429(4) 0.4331(2) 0.0385(11) Uani 1 1 d . . .
H13 H 0.5358 0.6680 0.4747 0.046 Uiso 1 1 calc R . .
C14 C 0.6034(4) 0.5152(4) 0.4375(2) 0.0335(10) Uani 1 1 d . . .
C15 C 0.6689(4) 0.4398(5) 0.5006(2) 0.0431(12) Uani 1 1 d . . .
H15 H 0.6711 0.4729 0.5377 0.052 Uiso 1 1 calc R . .
C16 C 0.7292(5) 0.3184(5) 0.5073(3) 0.0551(14) Uani 1 1 d . . .
H16 H 0.7732 0.2698 0.5488 0.066 Uiso 1 1 calc R . .
C17 C 0.7257(5) 0.2671(4) 0.4530(3) 0.0497(13) Uani 1 1 d . . .
H17 H 0.7679 0.1846 0.4577 0.060 Uiso 1 1 calc R . .
C18 C 0.6586(4) 0.3397(4) 0.3917(2) 0.0361(10) Uani 1 1 d . . .
C19 C 0.5965(4) 0.4644(4) 0.3831(2) 0.0292(9) Uani 1 1 d . . .
C20 C 0.3625(7) 0.5570(6) 0.0474(3) 0.092(3) Uani 1 1 d . . .
H20A H 0.2771 0.6037 0.0449 0.139 Uiso 1 1 calc R . .
H20B H 0.3808 0.4731 0.0618 0.139 Uiso 1 1 calc R . .
H20C H 0.3928 0.5733 0.0021 0.139 Uiso 1 1 calc R . .
C21 C 0.7319(6) 0.1767(5) 0.3338(3) 0.0706(18) Uani 1 1 d . . .
H21A H 0.8122 0.1665 0.3419 0.106 Uiso 1 1 calc R . .
H21B H 0.7246 0.1611 0.2892 0.106 Uiso 1 1 calc R . .
H21C H 0.7145 0.1217 0.3700 0.106 Uiso 1 1 calc R . .
C22 C -0.0611(4) 0.5819(4) 0.1420(2) 0.0310(10) Uani 1 1 d . . .
C23 C -0.0956(4) 0.6976(4) 0.1536(2) 0.0337(10) Uani 1 1 d . . .
C24 C -0.1997(5) 0.7936(4) 0.1222(3) 0.0462(12) Uani 1 1 d . . .
H24 H -0.2231 0.8684 0.1322 0.055 Uiso 1 1 calc R . .
C25 C -0.2686(5) 0.7779(5) 0.0762(3) 0.0520(14) Uani 1 1 d . . .
H25 H -0.3393 0.8425 0.0557 0.062 Uiso 1 1 calc R . .
C26 C -0.2352(5) 0.6694(5) 0.0602(3) 0.0513(14) Uani 1 1 d . . .
H26 H -0.2817 0.6611 0.0278 0.062 Uiso 1 1 calc R . .
C27 C -0.1303(4) 0.5700(4) 0.0925(2) 0.0380(11) Uani 1 1 d . . .
C28 C -0.0931(5) 0.4607(5) 0.0689(2) 0.0466(13) Uani 1 1 d . . .
H28 H -0.1340 0.4662 0.0288 0.056 Uiso 1 1 calc R . .
C29 C 0.0221(6) 0.2642(5) 0.0573(3) 0.0580(16) Uani 1 1 d . . .
H29A H 0.1002 0.2501 0.0389 0.070 Uiso 1 1 calc R . .
H29B H -0.0353 0.2936 0.0177 0.070 Uiso 1 1 calc R . .
C30 C 0.0270(5) 0.1445(5) 0.0995(3) 0.0501(14) Uani 1 1 d . . .
C31 C 0.0558(6) 0.0621(6) 0.0484(3) 0.082(2) Uani 1 1 d . . .
H31A H 0.1276 0.0578 0.0255 0.123 Uiso 1 1 calc R . .
H31B H -0.0096 0.0939 0.0140 0.123 Uiso 1 1 calc R . .
H31C H 0.0676 -0.0170 0.0738 0.123 Uiso 1 1 calc R . .
C32 C -0.0930(6) 0.1617(5) 0.1301(3) 0.0736(19) Uani 1 1 d . . .
H32A H -0.0878 0.0858 0.1572 0.110 Uiso 1 1 calc R . .
H32B H -0.1537 0.1927 0.0928 0.110 Uiso 1 1 calc R . .
H32C H -0.1136 0.2173 0.1596 0.110 Uiso 1 1 calc R . .
C33 C 0.1267(5) 0.0871(5) 0.1559(3) 0.0583(15) Uani 1 1 d . . .
H33A H 0.1378 0.0052 0.1758 0.070 Uiso 1 1 calc R . .
H33B H 0.2005 0.0832 0.1347 0.070 Uiso 1 1 calc R . .
C34 C 0.1100(5) 0.0886(4) 0.2748(3) 0.0469(13) Uani 1 1 d . . .
H34 H 0.1170 0.0111 0.2796 0.056 Uiso 1 1 calc R . .
C35 C 0.1040(4) 0.1285(4) 0.3383(3) 0.0389(11) Uani 1 1 d . . .
C36 C 0.0920(5) 0.0547(4) 0.4015(3) 0.0556(15) Uani 1 1 d . . .
H36 H 0.0823 -0.0137 0.4002 0.067 Uiso 1 1 calc R . .
C37 C 0.0943(6) 0.0820(5) 0.4636(3) 0.0645(17) Uani 1 1 d . . .
H37 H 0.0838 0.0338 0.5045 0.077 Uiso 1 1 calc R . .
C38 C 0.1124(5) 0.1827(5) 0.4664(3) 0.0509(14) Uani 1 1 d . . .
H38 H 0.1169 0.2002 0.5092 0.061 Uiso 1 1 calc R . .
C39 C 0.1234(4) 0.2556(4) 0.4055(2) 0.0346(10) Uani 1 1 d . . .
C40 C 0.1187(4) 0.2319(4) 0.3400(2) 0.0303(9) Uani 1 1 d . . .
C41 C -0.0370(5) 0.8228(4) 0.2029(3) 0.0607(16) Uani 1 1 d . . .
H41A H -0.0426 0.8716 0.1566 0.091 Uiso 1 1 calc R . .
H41B H 0.0288 0.8175 0.2296 0.091 Uiso 1 1 calc R . .
H41C H -0.1103 0.8584 0.2254 0.091 Uiso 1 1 calc R . .
C42 C 0.1502(5) 0.3835(5) 0.4696(2) 0.0523(14) Uani 1 1 d . . .
H42A H 0.0789 0.3921 0.4942 0.079 Uiso 1 1 calc R . .
H42B H 0.1594 0.4569 0.4619 0.079 Uiso 1 1 calc R . .
H42C H 0.2187 0.3190 0.4970 0.079 Uiso 1 1 calc R . .
C43 C -0.1504(6) 0.5497(6) 0.3631(3) 0.081(2) Uani 1 1 d . . .
H43A H -0.1360 0.4766 0.3973 0.122 Uiso 1 1 calc R . .
H43B H -0.2329 0.5883 0.3460 0.122 Uiso 1 1 calc R . .
H43C H -0.1332 0.6024 0.3842 0.122 Uiso 1 1 calc R . .
N1 N 0.5177(4) 0.8393(3) 0.2385(2) 0.0427(10) Uani 1 1 d . . .
N2 N 0.5064(4) 0.7244(3) 0.3761(2) 0.0382(9) Uani 1 1 d . . .
N3 N -0.0110(4) 0.3576(4) 0.09638(19) 0.0396(9) Uani 1 1 d . . .
N4 N 0.1068(4) 0.1491(3) 0.2124(2) 0.0400(9) Uani 1 1 d . . .
N5 N 0.2599(3) 0.6269(3) 0.2415(2) 0.0418(10) Uani 1 1 d . . .
N6 N 0.2609(3) 0.7060(3) 0.2645(2) 0.0406(10) Uani 1 1 d . . .
N7 N 0.2659(4) 0.7814(4) 0.2860(3) 0.0579(13) Uani 1 1 d . . .
N8 N 0.3647(3) 0.3849(3) 0.3369(2) 0.0410(10) Uani 1 1 d . . .
N9 N 0.4049(4) 0.3080(4) 0.3830(2) 0.0428(10) Uani 1 1 d . . .
N10 N 0.4474(5) 0.2268(4) 0.4331(2) 0.0691(14) Uani 1 1 d . . .
N11 N 0.2961(4) 0.4235(4) 0.1889(2) 0.0590(5) Uani 1 1 d . . .
N12 N 0.2914(4) 0.3529(4) 0.1597(2) 0.0590(5) Uani 1 1 d . . .
N13 N 0.2833(4) 0.2866(4) 0.1307(2) 0.0590(5) Uani 1 1 d . . .
N14 N 0.5580(4) 0.2690(4) 0.1825(2) 0.0590(5) Uani 1 1 d . . .
N15 N 0.6122(4) 0.1736(4) 0.1746(2) 0.0590(5) Uani 1 1 d . . .
N16 N 0.6682(4) 0.0782(4) 0.1663(2) 0.0590(5) Uani 1 1 d . . .
N17 N 0.0721(4) 0.6425(4) 0.3622(2) 0.0485(11) Uani 1 1 d . . .
N18 N 0.0262(5) 0.7410(4) 0.3663(2) 0.0594(13) Uani 1 1 d . . .
N19 N -0.0188(7) 0.8396(5) 0.3726(3) 0.104(2) Uani 1 1 d . . .
N20 N -0.1340(4) 0.3795(4) 0.2443(2) 0.0480(11) Uani 1 1 d . . .
N21 N -0.2255(4) 0.4066(3) 0.2148(2) 0.0384(9) Uani 1 1 d . . .
N22 N -0.3153(4) 0.4321(4) 0.1838(2) 0.0555(12) Uani 1 1 d . . .
O1 O 0.4778(3) 0.6590(3) 0.19769(15) 0.0355(7) Uani 1 1 d . . .
O2 O 0.5356(3) 0.5284(2) 0.32190(15) 0.0345(7) Uani 1 1 d . . .
O3 O 0.6484(3) 0.2983(3) 0.33419(16) 0.0403(8) Uani 1 1 d . . .
O4 O 0.4175(3) 0.5886(3) 0.09711(16) 0.0486(9) Uani 1 1 d . . .
O5 O 0.0355(3) 0.4920(2) 0.17679(14) 0.0290(6) Uani 1 1 d . . .
O6 O 0.1315(3) 0.3051(2) 0.28302(14) 0.0295(6) Uani 1 1 d . . .
O7 O 0.1407(3) 0.3576(3) 0.40373(15) 0.0380(7) Uani 1 1 d . . .
O8 O -0.0177(3) 0.7041(2) 0.19835(16) 0.0384(7) Uani 1 1 d . . .
O9 O -0.0764(3) 0.5233(3) 0.30753(17) 0.0437(8) Uani 1 1 d . . .
H9 H -0.0956 0.4856 0.2854 0.065 Uiso 1 1 d R . .


_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
La1 N14 2.483(4) . ?
La1 O2 2.503(3) . ?
La1 O1 2.535(3) . ?
La1 N22 2.580(4) 1_655 ?
La1 N11 2.620(5) . ?
La1 N8 2.665(4) . ?
La1 O4 2.697(3) . ?
La1 N5 2.702(4) . ?
La1 O3 2.744(3) . ?
La1 Cu1 3.5967(8) . ?
La1 La2 4.0954(9) . ?
La2 O6 2.505(3) . ?
La2 O5 2.516(3) . ?
La2 N17 2.524(4) . ?
La2 O9 2.579(3) . ?
La2 N5 2.603(3) . ?
La2 N11 2.629(4) . ?
La2 O7 2.648(3) . ?
La2 O8 2.665(3) . ?
La2 N8 2.687(4) . ?
La2 Cu2 3.5964(7) . ?
Cu1 O2 1.917(3) . ?
Cu1 O1 1.927(3) . ?
Cu1 N1 1.933(4) . ?
Cu1 N2 1.940(4) . ?
Cu2 O6 1.962(3) . ?
Cu2 N4 1.970(4) . ?
Cu2 O5 1.974(3) . ?
Cu2 N3 1.983(4) . ?
Cu2 N20 2.457(4) . ?
C1 O1 1.318(5) . ?
C1 C6 1.407(6) . ?
C1 C2 1.419(6) . ?
C2 C3 1.374(7) . ?
C2 O4 1.389(5) . ?
C3 C4 1.394(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.365(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.445(7) . ?
C7 N1 1.273(6) . ?
C7 H7 0.9300 . ?
C8 N1 1.482(6) . ?
C8 C9 1.533(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.521(7) . ?
C9 C11 1.522(7) . ?
C9 C12 1.538(6) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.475(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.282(6) . ?
C13 C14 1.445(6) . ?
C13 H13 0.9300 . ?
C14 C19 1.393(6) . ?
C14 C15 1.412(6) . ?
C15 C16 1.367(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.384(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.384(6) . ?
C17 H17 0.9300 . ?
C18 O3 1.386(5) . ?
C18 C19 1.400(6) . ?
C19 O2 1.336(5) . ?
C20 O4 1.435(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O3 1.442(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.320(5) . ?
C22 C27 1.400(6) . ?
C22 C23 1.411(6) . ?
C23 O8 1.377(5) . ?
C23 C24 1.379(6) . ?
C24 C25 1.373(7) . ?
C24 H24 0.9300 . ?
C25 C26 1.365(7) . ?
C25 H25 0.9300 . ?
C26 C27 1.407(7) . ?
C26 H26 0.9300 . ?
C27 C28 1.441(6) . ?
C28 N3 1.271(6) . ?
C28 H28 0.9300 . ?
C29 N3 1.462(5) . ?
C29 C30 1.525(7) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C33 1.507(8) . ?
C30 C32 1.518(8) . ?
C30 C31 1.537(6) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N4 1.458(6) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N4 1.278(6) . ?
C34 C35 1.441(7) . ?
C34 H34 0.9300 . ?
C35 C40 1.403(5) . ?
C35 C36 1.414(7) . ?
C36 C37 1.349(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.399(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.371(6) . ?
C38 H38 0.9300 . ?
C39 O7 1.389(5) . ?
C39 C40 1.400(6) . ?
C40 O6 1.328(5) . ?
C41 O8 1.440(5) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 O7 1.431(5) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 O9 1.397(6) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
N5 N6 1.196(5) . ?
N6 N7 1.155(5) . ?
N8 N9 1.112(5) . ?
N9 N10 1.192(6) . ?
N11 N12 1.191(5) . ?
N12 N13 1.159(5) . ?
N14 N15 1.148(5) . ?
N15 N16 1.153(5) . ?
N17 N18 1.149(5) . ?
N18 N19 1.163(6) . ?
N20 N21 1.172(5) . ?
N21 N22 1.171(6) . ?
N22 La1 2.580(4) 1_455 ?
O9 H9 0.8227 . ?

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
N14 La1 O2 138.39(14) . . ?
N14 La1 O1 137.78(12) . . ?
O2 La1 O1 60.78(9) . . ?
N14 La1 N22 75.01(14) . 1_655 ?
O2 La1 N22 83.16(12) . 1_655 ?
O1 La1 N22 71.18(12) . 1_655 ?
N14 La1 N11 71.75(14) . . ?
O2 La1 N11 139.48(12) . . ?
O1 La1 N11 120.10(13) . . ?
N22 La1 N11 137.19(14) 1_655 . ?
N14 La1 N8 99.44(13) . . ?
O2 La1 N8 78.95(11) . . ?
O1 La1 N8 122.74(10) . . ?
N22 La1 N8 145.19(14) 1_655 . ?
N11 La1 N8 67.67(14) . . ?
N14 La1 O4 89.46(14) . . ?
O2 La1 O4 120.47(9) . . ?
O1 La1 O4 59.69(9) . . ?
N22 La1 O4 78.28(13) 1_655 . ?
N11 La1 O4 75.21(13) . . ?
N8 La1 O4 136.48(12) . . ?
N14 La1 N5 136.35(13) . . ?
O2 La1 N5 81.77(11) . . ?
O1 La1 N5 68.44(10) . . ?
N22 La1 N5 139.30(13) 1_655 . ?
N11 La1 N5 64.68(12) . . ?
N8 La1 N5 66.89(12) . . ?
O4 La1 N5 77.35(12) . . ?
N14 La1 O3 80.68(13) . . ?
O2 La1 O3 58.97(9) . . ?
O1 La1 O3 111.75(9) . . ?
N22 La1 O3 72.84(13) 1_655 . ?
N11 La1 O3 125.88(12) . . ?
N8 La1 O3 72.36(11) . . ?
O4 La1 O3 151.00(10) . . ?
N5 La1 O3 127.67(11) . . ?
N14 La1 Cu1 153.82(11) . . ?
O2 La1 Cu1 30.42(6) . . ?
O1 La1 Cu1 30.88(7) . . ?
N22 La1 Cu1 79.31(10) 1_655 . ?
N11 La1 Cu1 133.18(10) . . ?
N8 La1 Cu1 98.67(9) . . ?
O4 La1 Cu1 90.32(7) . . ?
N5 La1 Cu1 68.77(8) . . ?
O3 La1 Cu1 86.99(6) . . ?
N14 La1 La2 104.14(10) . . ?
O2 La1 La2 100.69(7) . . ?
O1 La1 La2 107.04(7) . . ?
N22 La1 La2 174.41(11) 1_655 . ?
N11 La1 La2 38.80(9) . . ?
N8 La1 La2 40.27(9) . . ?
O4 La1 La2 96.22(8) . . ?
N5 La1 La2 38.60(7) . . ?
O3 La1 La2 112.60(7) . . ?
Cu1 La1 La2 101.915(13) . . ?
O6 La2 O5 63.15(9) . . ?
O6 La2 N17 134.54(11) . . ?
O5 La2 N17 132.55(12) . . ?
O6 La2 O9 71.76(9) . . ?
O5 La2 O9 69.04(9) . . ?
N17 La2 O9 77.14(12) . . ?
O6 La2 N5 144.08(11) . . ?
O5 La2 N5 110.18(11) . . ?
N17 La2 N5 77.64(13) . . ?
O9 La2 N5 141.82(11) . . ?
O6 La2 N11 79.32(11) . . ?
O5 La2 N11 70.19(12) . . ?
N17 La2 N11 142.93(13) . . ?
O9 La2 N11 137.39(12) . . ?
N5 La2 N11 65.95(13) . . ?
O6 La2 O7 61.33(9) . . ?
O5 La2 O7 118.32(9) . . ?
N17 La2 O7 77.42(11) . . ?
O9 La2 O7 70.09(10) . . ?
N5 La2 O7 130.40(11) . . ?
N11 La2 O7 121.32(13) . . ?
O6 La2 O8 120.22(9) . . ?
O5 La2 O8 60.44(9) . . ?
N17 La2 O8 78.00(12) . . ?
O9 La2 O8 71.34(10) . . ?
N5 La2 O8 75.72(11) . . ?
N11 La2 O8 98.66(13) . . ?
O7 La2 O8 137.82(10) . . ?
O6 La2 N8 90.95(10) . . ?
O5 La2 N8 133.44(11) . . ?
N17 La2 N8 93.54(14) . . ?
O9 La2 N8 141.65(11) . . ?
N5 La2 N8 67.97(12) . . ?
N11 La2 N8 67.21(14) . . ?
O7 La2 N8 71.59(11) . . ?
O8 La2 N8 143.68(10) . . ?
O6 La2 Cu2 31.53(6) . . ?
O5 La2 Cu2 31.87(6) . . ?
N17 La2 Cu2 146.90(10) . . ?
O9 La2 Cu2 69.76(7) . . ?
N5 La2 Cu2 130.40(9) . . ?
N11 La2 Cu2 69.21(9) . . ?
O7 La2 Cu2 90.88(6) . . ?
O8 La2 Cu2 91.40(6) . . ?
N8 La2 Cu2 112.19(8) . . ?
O6 La2 La1 105.29(7) . . ?
O5 La2 La1 107.30(6) . . ?
N17 La2 La1 106.82(10) . . ?
O9 La2 La1 175.99(7) . . ?
N5 La2 La1 40.36(8) . . ?
N11 La2 La1 38.63(10) . . ?
O7 La2 La1 111.12(7) . . ?
O8 La2 La1 108.55(7) . . ?
N8 La2 La1 39.88(9) . . ?
Cu2 La2 La1 106.284(14) . . ?
O2 Cu1 O1 83.07(12) . . ?
O2 Cu1 N1 163.35(16) . . ?
O1 Cu1 N1 93.87(15) . . ?
O2 Cu1 N2 93.20(14) . . ?
O1 Cu1 N2 170.95(14) . . ?
N1 Cu1 N2 92.01(16) . . ?
O2 Cu1 La1 41.38(9) . . ?
O1 Cu1 La1 42.48(8) . . ?
N1 Cu1 La1 135.93(12) . . ?
N2 Cu1 La1 132.06(10) . . ?
O6 Cu2 N4 90.22(14) . . ?
O6 Cu2 O5 83.82(11) . . ?
N4 Cu2 O5 172.59(15) . . ?
O6 Cu2 N3 174.38(13) . . ?
N4 Cu2 N3 95.31(16) . . ?
O5 Cu2 N3 90.59(14) . . ?
O6 Cu2 N20 87.60(13) . . ?
N4 Cu2 N20 96.35(15) . . ?
O5 Cu2 N20 87.82(12) . . ?
N3 Cu2 N20 92.75(16) . . ?
O6 Cu2 La2 41.88(7) . . ?
N4 Cu2 La2 131.19(12) . . ?
O5 Cu2 La2 42.30(8) . . ?
N3 Cu2 La2 132.50(11) . . ?
N20 Cu2 La2 91.21(10) . . ?
O1 C1 C6 124.4(4) . . ?
O1 C1 C2 118.0(4) . . ?
C6 C1 C2 117.6(4) . . ?
C3 C2 O4 124.4(5) . . ?
C3 C2 C1 121.4(5) . . ?
O4 C2 C1 114.1(4) . . ?
C2 C3 C4 119.6(5) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.1(5) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 120.0(5) . . ?
C5 C6 C7 116.6(4) . . ?
C1 C6 C7 123.0(4) . . ?
N1 C7 C6 126.1(4) . . ?
N1 C7 H7 116.9 . . ?
C6 C7 H7 116.9 . . ?
N1 C8 C9 114.2(4) . . ?
N1 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10 C9 C11 110.6(4) . . ?
C10 C9 C8 109.5(4) . . ?
C11 C9 C8 105.9(4) . . ?
C10 C9 C12 108.2(4) . . ?
C11 C9 C12 110.4(4) . . ?
C8 C9 C12 112.3(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 113.3(4) . . ?
N2 C12 H12A 108.9 . . ?
C9 C12 H12A 108.9 . . ?
N2 C12 H12B 108.9 . . ?
C9 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
N2 C13 C14 124.9(4) . . ?
N2 C13 H13 117.6 . . ?
C14 C13 H13 117.6 . . ?
C19 C14 C15 119.5(4) . . ?
C19 C14 C13 123.1(4) . . ?
C15 C14 C13 117.3(4) . . ?
C16 C15 C14 120.3(5) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C15 C16 C17 120.8(5) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 119.4(5) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 O3 124.4(4) . . ?
C17 C18 C19 121.2(4) . . ?
O3 C18 C19 114.4(4) . . ?
O2 C19 C14 123.7(4) . . ?
O2 C19 C18 117.5(4) . . ?
C14 C19 C18 118.8(4) . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 H21A 109.5 . . ?
O3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 C27 123.8(4) . . ?
O5 C22 C23 118.6(4) . . ?
C27 C22 C23 117.6(4) . . ?
O8 C23 C24 124.4(4) . . ?
O8 C23 C22 114.2(4) . . ?
C24 C23 C22 121.4(4) . . ?
C25 C24 C23 119.5(5) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C26 C25 C24 121.2(5) . . ?
C26 C25 H25 119.4 . . ?
C24 C25 H25 119.4 . . ?
C25 C26 C27 120.0(5) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C22 C27 C26 120.1(4) . . ?
C22 C27 C28 122.1(4) . . ?
C26 C27 C28 117.6(4) . . ?
N3 C28 C27 127.6(4) . . ?
N3 C28 H28 116.2 . . ?
C27 C28 H28 116.2 . . ?
N3 C29 C30 114.9(4) . . ?
N3 C29 H29A 108.5 . . ?
C30 C29 H29A 108.5 . . ?
N3 C29 H29B 108.5 . . ?
C30 C29 H29B 108.5 . . ?
H29A C29 H29B 107.5 . . ?
C33 C30 C32 111.3(5) . . ?
C33 C30 C29 110.4(4) . . ?
C32 C30 C29 110.7(5) . . ?
C33 C30 C31 108.1(5) . . ?
C32 C30 C31 109.5(5) . . ?
C29 C30 C31 106.7(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N4 C33 C30 114.8(4) . . ?
N4 C33 H33A 108.6 . . ?
C30 C33 H33A 108.6 . . ?
N4 C33 H33B 108.6 . . ?
C30 C33 H33B 108.6 . . ?
H33A C33 H33B 107.6 . . ?
N4 C34 C35 126.5(4) . . ?
N4 C34 H34 116.7 . . ?
C35 C34 H34 116.7 . . ?
C40 C35 C36 119.6(4) . . ?
C40 C35 C34 122.4(4) . . ?
C36 C35 C34 117.8(4) . . ?
C37 C36 C35 121.1(5) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C36 C37 C38 120.0(5) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C39 C38 C37 119.6(5) . . ?
C39 C38 H38 120.2 . . ?
C37 C38 H38 120.2 . . ?
C38 C39 O7 123.1(4) . . ?
C38 C39 C40 122.2(4) . . ?
O7 C39 C40 114.7(4) . . ?
O6 C40 C39 119.2(4) . . ?
O6 C40 C35 123.2(4) . . ?
C39 C40 C35 117.5(4) . . ?
O8 C41 H41A 109.5 . . ?
O8 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O8 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O7 C42 H42A 109.5 . . ?
O7 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O7 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O9 C43 H43A 109.5 . . ?
O9 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O9 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C7 N1 C8 119.6(4) . . ?
C7 N1 Cu1 124.6(3) . . ?
C8 N1 Cu1 115.5(3) . . ?
C13 N2 C12 120.4(4) . . ?
C13 N2 Cu1 124.8(3) . . ?
C12 N2 Cu1 114.4(3) . . ?
C28 N3 C29 117.5(4) . . ?
C28 N3 Cu2 120.9(3) . . ?
C29 N3 Cu2 121.5(3) . . ?
C34 N4 C33 117.5(4) . . ?
C34 N4 Cu2 121.8(3) . . ?
C33 N4 Cu2 120.4(3) . . ?
N6 N5 La2 128.4(3) . . ?
N6 N5 La1 115.0(3) . . ?
La2 N5 La1 101.04(12) . . ?
N7 N6 N5 177.6(5) . . ?
N9 N8 La1 127.2(3) . . ?
N9 N8 La2 130.2(3) . . ?
La1 N8 La2 99.85(14) . . ?
N8 N9 N10 178.9(5) . . ?
N12 N11 La1 131.5(4) . . ?
N12 N11 La2 119.5(4) . . ?
La1 N11 La2 102.57(14) . . ?
N13 N12 N11 178.0(6) . . ?
N15 N14 La1 164.1(4) . . ?
N14 N15 N16 178.8(6) . . ?
N18 N17 La2 146.1(4) . . ?
N17 N18 N19 177.9(7) . . ?
N21 N20 Cu2 125.3(3) . . ?
N22 N21 N20 178.1(5) . . ?
N21 N22 La1 130.0(4) . 1_455 ?
C1 O1 Cu1 124.8(3) . . ?
C1 O1 La1 127.4(3) . . ?
Cu1 O1 La1 106.64(12) . . ?
C19 O2 Cu1 123.1(2) . . ?
C19 O2 La1 127.8(2) . . ?
Cu1 O2 La1 108.20(12) . . ?
C18 O3 C21 116.3(4) . . ?
C18 O3 La1 118.5(2) . . ?
C21 O3 La1 125.1(3) . . ?
C2 O4 C20 117.0(4) . . ?
C2 O4 La1 120.6(3) . . ?
C20 O4 La1 120.6(3) . . ?
C22 O5 Cu2 121.8(3) . . ?
C22 O5 La2 124.3(2) . . ?
Cu2 O5 La2 105.84(12) . . ?
C40 O6 Cu2 121.2(2) . . ?
C40 O6 La2 124.6(2) . . ?
Cu2 O6 La2 106.59(11) . . ?
C39 O7 C42 116.9(3) . . ?
C39 O7 La2 119.3(2) . . ?
C42 O7 La2 123.6(2) . . ?
C23 O8 C41 116.6(4) . . ?
C23 O8 La2 118.4(2) . . ?
C41 O8 La2 124.5(3) . . ?
C43 O9 La2 134.7(3) . . ?
C43 O9 H9 111.2 . . ?
La2 O9 H9 110.5 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.050
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.113
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_CuErvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060770'
_audit_update_record             
;
2017-04-26 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuErvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Cu2 Er2 N22 O9'
_chemical_formula_weight         1482.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.177(6)
_cell_length_b                   9.669(2)
_cell_length_c                   25.894(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.798(3)
_cell_angle_gamma                90.00
_cell_volume                     5224(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9621
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.50

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2920
_exptl_absorpt_coefficient_mu    4.059
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.4688
_exptl_absorpt_correction_T_max  0.8545
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX SMART'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32568
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.67
_diffrn_reflns_theta_max         27.62
_reflns_number_total             6050
_reflns_number_gt                5394
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0297P)²+8.5301P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6050
_refine_ls_number_parameters     361
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0703
_refine_ls_wR_factor_gt          0.0680
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_restrained_S_all      1.132
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Er1 Er 0.286617(7) 0.345268(16) 0.073247(6) 0.02602(6) Uani 1 1 d . . .
Cu1 Cu 0.442235(19) 0.23623(4) 0.100471(18) 0.02858(10) Uani 1 1 d . . .
C1 C 0.40709(17) 0.5276(4) 0.06758(15) 0.0311(8) Uani 1 1 d . . .
C2 C 0.36270(18) 0.6352(4) 0.05634(16) 0.0326(8) Uani 1 1 d . . .
C3 C 0.3776(2) 0.7658(4) 0.04336(18) 0.0415(9) Uani 1 1 d . . .
H3 H 0.3473 0.8361 0.0364 0.050 Uiso 1 1 calc R . .
C4 C 0.4379(2) 0.7925(4) 0.04059(19) 0.0470(11) Uani 1 1 d . . .
H4 H 0.4478 0.8801 0.0310 0.056 Uiso 1 1 calc R . .
C5 C 0.4826(2) 0.6896(4) 0.05207(19) 0.0464(11) Uani 1 1 d . . .
H5 H 0.5230 0.7079 0.0503 0.056 Uiso 1 1 calc R . .
C6 C 0.46853(18) 0.5562(4) 0.06656(17) 0.0365(8) Uani 1 1 d . . .
C7 C 0.51956(18) 0.4580(4) 0.08150(17) 0.0404(9) Uani 1 1 d . . .
H7 H 0.5582 0.4893 0.0792 0.049 Uiso 1 1 calc R . .
C8 C 0.5822(2) 0.2625(5) 0.1108(2) 0.0528(12) Uani 1 1 d . . .
H8A H 0.6157 0.3320 0.1221 0.063 Uiso 1 1 calc R . .
H8B H 0.5843 0.2198 0.0775 0.063 Uiso 1 1 calc R . .
C9 C 0.59586(17) 0.1539(4) 0.15480(16) 0.0347(8) Uani 1 1 d . . .
C10 C 0.66364(19) 0.1016(5) 0.1641(2) 0.0473(10) Uani 1 1 d . . .
H10A H 0.6651 0.0579 0.1312 0.071 Uiso 1 1 calc R . .
H10B H 0.6755 0.0360 0.1936 0.071 Uiso 1 1 calc R . .
H10C H 0.6930 0.1781 0.1732 0.071 Uiso 1 1 calc R . .
C11 C 0.5916(2) 0.2110(5) 0.20772(19) 0.0544(12) Uani 1 1 d . . .
H11A H 0.6234 0.2818 0.2215 0.082 Uiso 1 1 calc R . .
H11B H 0.5990 0.1380 0.2343 0.082 Uiso 1 1 calc R . .
H11C H 0.5498 0.2497 0.2011 0.082 Uiso 1 1 calc R . .
C12 C 0.55019(18) 0.0335(4) 0.1341(2) 0.0437(10) Uani 1 1 d . . .
H12A H 0.5479 0.0111 0.0969 0.052 Uiso 1 1 calc R . .
H12B H 0.5669 -0.0467 0.1569 0.052 Uiso 1 1 calc R . .
C13 C 0.46157(18) -0.0277(4) 0.15763(17) 0.0384(9) Uani 1 1 d . . .
H13 H 0.4868 -0.1053 0.1711 0.046 Uiso 1 1 calc R . .
C14 C 0.40061(18) -0.0251(4) 0.16564(16) 0.0343(8) Uani 1 1 d . . .
C15 C 0.3881(2) -0.1305(4) 0.19810(18) 0.0429(10) Uani 1 1 d . . .
H15 H 0.4181 -0.2002 0.2120 0.051 Uiso 1 1 calc R . .
C16 C 0.3318(2) -0.1312(4) 0.20945(18) 0.0437(10) Uani 1 1 d . . .
H16 H 0.3239 -0.2017 0.2307 0.052 Uiso 1 1 calc R . .
C17 C 0.2870(2) -0.0273(4) 0.18938(16) 0.0388(9) Uani 1 1 d . . .
H17 H 0.2491 -0.0275 0.1972 0.047 Uiso 1 1 calc R . .
C18 C 0.29914(18) 0.0762(4) 0.15775(14) 0.0318(8) Uani 1 1 d . . .
C19 C 0.35507(17) 0.0787(4) 0.14394(14) 0.0286(7) Uani 1 1 d . . .
C20 C 0.2670(2) 0.7059(4) 0.07273(19) 0.0435(10) Uani 1 1 d . . .
H20A H 0.2934 0.7460 0.1068 0.065 Uiso 1 1 calc R . .
H20B H 0.2292 0.6669 0.0771 0.065 Uiso 1 1 calc R . .
H20C H 0.2549 0.7762 0.0449 0.065 Uiso 1 1 calc R . .
C21 C 0.2108(2) 0.2150(5) 0.1622(2) 0.0595(14) Uani 1 1 d . . .
H21A H 0.1783 0.1448 0.1513 0.089 Uiso 1 1 calc R . .
H21B H 0.1918 0.3038 0.1502 0.089 Uiso 1 1 calc R . .
H21C H 0.2303 0.2148 0.2014 0.089 Uiso 1 1 calc R . .
O5 O 0.4778(7) 0.6126(12) 0.2809(6) 0.150(4) Uani 0.50 1 d PDU . .
N1 N 0.51965(14) 0.3324(3) 0.09771(14) 0.0358(7) Uani 1 1 d . . .
N2 N 0.48554(14) 0.0633(3) 0.13431(13) 0.0332(7) Uani 1 1 d . . .
N3 N 0.3108(2) 0.4598(4) 0.15652(16) 0.0542(10) Uani 1 1 d . . .
N4 N 0.31981(16) 0.4903(3) 0.20114(14) 0.0380(7) Uani 1 1 d . . .
N5 N 0.3288(3) 0.5238(5) 0.24572(19) 0.0792(15) Uani 1 1 d . . .
N6 N 0.27142(15) 0.3528(3) -0.02143(13) 0.0333(7) Uani 1 1 d . . .
N7 N 0.30442(19) 0.4289(4) -0.04071(16) 0.0531(10) Uani 1 1 d . . .
N8 N 0.3347(3) 0.4985(6) -0.0591(2) 0.0858(17) Uani 1 1 d . . .
N9 N 0.41798(17) 0.1470(4) 0.01015(15) 0.0458(9) Uani 1 1 d . . .
N10 N 0.36869(15) 0.1133(3) -0.01926(13) 0.0310(7) Uani 1 1 d . . .
N11 N 0.31889(16) 0.0767(4) -0.05052(15) 0.0426(8) Uani 1 1 d . . .
O1 O 0.38926(11) 0.4024(2) 0.07825(11) 0.0309(5) Uani 1 1 d . . .
O2 O 0.36289(12) 0.1805(2) 0.11241(11) 0.0312(6) Uani 1 1 d . . .
O3 O 0.30247(12) 0.5986(3) 0.05674(11) 0.0346(6) Uani 1 1 d . . .
O4 O 0.25877(13) 0.1875(3) 0.13755(12) 0.0384(6) Uani 1 1 d . . .
C22 C 0.5000 0.5202(17) 0.2500 0.167(5) Uani 1 2 d SDU . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Er1 O2 2.295(2) . ?
Er1 O1 2.303(2) . ?
Er1 N3 2.319(4) . ?
Er1 N11 2.336(3) 7 ?
Er1 N6 2.360(3) . ?
Er1 N6 2.440(3) 7 ?
Er1 O4 2.486(3) . ?
Er1 O3 2.531(3) . ?
Er1 Cu1 3.4453(9) . ?
Cu1 O1 1.958(2) . ?
Cu1 O2 1.962(2) . ?
Cu1 N1 1.975(3) . ?
Cu1 N2 1.978(3) . ?
Cu1 N9 2.377(4) . ?
C1 O1 1.331(4) . ?
C1 C2 1.394(5) . ?
C1 C6 1.399(5) . ?
C2 C3 1.376(5) . ?
C2 O3 1.385(4) . ?
C3 C4 1.387(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.364(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.407(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.427(5) . ?
C7 N1 1.285(5) . ?
C7 H7 0.9300 . ?
C8 N1 1.475(5) . ?
C8 C9 1.504(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C11 1.510(6) . ?
C9 C12 1.516(5) . ?
C9 C10 1.526(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.464(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.281(5) . ?
C13 C14 1.436(5) . ?
C13 H13 0.9300 . ?
C14 C19 1.400(5) . ?
C14 C15 1.407(5) . ?
C15 C16 1.374(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.384(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.376(5) . ?
C17 H17 0.9300 . ?
C18 O4 1.384(4) . ?
C18 C19 1.403(5) . ?
C19 O2 1.327(4) . ?
C20 O3 1.445(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O4 1.438(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
O5 C22 1.3955(11) . ?
N3 N4 1.143(5) . ?
N4 N5 1.150(5) . ?
N6 N7 1.254(5) . ?
N6 Er1 2.440(3) 7 ?
N7 N8 1.161(5) . ?
N9 N10 1.148(5) . ?
N10 N11 1.181(4) . ?
N11 Er1 2.336(3) 7 ?
C22 O5 1.3955(11) 2_655 ?

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
O2 Er1 O1 64.86(8) . . ?
O2 Er1 N3 90.98(12) . . ?
O1 Er1 N3 85.45(12) . . ?
O2 Er1 N11 149.43(11) . 7 ?
O1 Er1 N11 145.41(11) . 7 ?
N3 Er1 N11 88.63(13) . 7 ?
O2 Er1 N6 107.75(10) . . ?
O1 Er1 N6 80.89(10) . . ?
N3 Er1 N6 149.08(12) . . ?
N11 Er1 N6 87.13(12) 7 . ?
O2 Er1 N6 82.57(10) . 7 ?
O1 Er1 N6 123.12(10) . 7 ?
N3 Er1 N6 142.98(13) . 7 ?
N11 Er1 N6 79.53(11) 7 7 ?
N6 Er1 N6 65.78(13) . 7 ?
O2 Er1 O4 65.86(8) . . ?
O1 Er1 O4 125.07(9) . . ?
N3 Er1 O4 72.64(12) . . ?
N11 Er1 O4 84.96(11) 7 . ?
N6 Er1 O4 137.25(10) . . ?
N6 Er1 O4 71.47(10) 7 . ?
O2 Er1 O3 128.51(8) . . ?
O1 Er1 O3 65.55(8) . . ?
N3 Er1 O3 72.16(12) . . ?
N11 Er1 O3 80.18(11) 7 . ?
N6 Er1 O3 76.93(10) . . ?
N6 Er1 O3 138.08(10) 7 . ?
O4 Er1 O3 141.94(9) . . ?
O2 Er1 Cu1 32.84(6) . . ?
O1 Er1 Cu1 32.80(6) . . ?
N3 Er1 Cu1 93.21(10) . . ?
N11 Er1 Cu1 177.12(9) 7 . ?
N6 Er1 Cu1 90.15(8) . . ?
N6 Er1 Cu1 100.23(8) 7 . ?
O4 Er1 Cu1 97.70(6) . . ?
O3 Er1 Cu1 98.27(6) . . ?
O1 Cu1 O2 77.93(10) . . ?
O1 Cu1 N1 92.61(12) . . ?
O2 Cu1 N1 166.39(13) . . ?
O1 Cu1 N2 167.48(12) . . ?
O2 Cu1 N2 91.42(11) . . ?
N1 Cu1 N2 96.68(13) . . ?
O1 Cu1 N9 95.48(12) . . ?
O2 Cu1 N9 97.99(12) . . ?
N1 Cu1 N9 92.59(13) . . ?
N2 Cu1 N9 92.47(13) . . ?
O1 Cu1 Er1 39.57(7) . . ?
O2 Cu1 Er1 39.36(7) . . ?
N1 Cu1 Er1 132.17(9) . . ?
N2 Cu1 Er1 130.65(9) . . ?
N9 Cu1 Er1 91.87(9) . . ?
O1 C1 C2 118.9(3) . . ?
O1 C1 C6 123.0(3) . . ?
C2 C1 C6 118.1(3) . . ?
C3 C2 O3 123.3(3) . . ?
C3 C2 C1 121.6(4) . . ?
O3 C2 C1 115.0(3) . . ?
C2 C3 C4 120.0(4) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 119.6(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C1 C6 C5 119.4(4) . . ?
C1 C6 C7 123.4(3) . . ?
C5 C6 C7 117.1(4) . . ?
N1 C7 C6 129.1(3) . . ?
N1 C7 H7 115.4 . . ?
C6 C7 H7 115.4 . . ?
N1 C8 C9 115.2(3) . . ?
N1 C8 H8A 108.5 . . ?
C9 C8 H8A 108.5 . . ?
N1 C8 H8B 108.5 . . ?
C9 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C8 C9 C11 112.0(4) . . ?
C8 C9 C12 109.2(4) . . ?
C11 C9 C12 111.3(4) . . ?
C8 C9 C10 106.6(3) . . ?
C11 C9 C10 109.8(3) . . ?
C12 C9 C10 107.8(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 112.6(3) . . ?
N2 C12 H12A 109.1 . . ?
C9 C12 H12A 109.1 . . ?
N2 C12 H12B 109.1 . . ?
C9 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
N2 C13 C14 128.1(4) . . ?
N2 C13 H13 115.9 . . ?
C14 C13 H13 115.9 . . ?
C19 C14 C15 119.8(4) . . ?
C19 C14 C13 122.8(3) . . ?
C15 C14 C13 117.4(4) . . ?
C16 C15 C14 120.6(4) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C15 C16 C17 120.3(4) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 119.4(4) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C17 C18 O4 124.0(3) . . ?
C17 C18 C19 122.1(4) . . ?
O4 C18 C19 113.9(3) . . ?
O2 C19 C14 123.5(3) . . ?
O2 C19 C18 118.7(3) . . ?
C14 C19 C18 117.7(3) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 N1 C8 113.9(3) . . ?
C7 N1 Cu1 123.5(3) . . ?
C8 N1 Cu1 122.5(3) . . ?
C13 N2 C12 115.5(3) . . ?
C13 N2 Cu1 125.0(3) . . ?
C12 N2 Cu1 119.6(2) . . ?
N4 N3 Er1 165.9(4) . . ?
N3 N4 N5 178.6(5) . . ?
N7 N6 Er1 122.3(3) . . ?
N7 N6 Er1 120.8(3) . 7 ?
Er1 N6 Er1 114.22(13) . 7 ?
N8 N7 N6 179.2(5) . . ?
N10 N9 Cu1 127.1(3) . . ?
N9 N10 N11 177.9(4) . . ?
N10 N11 Er1 134.4(3) . 7 ?
C1 O1 Cu1 128.0(2) . . ?
C1 O1 Er1 124.3(2) . . ?
Cu1 O1 Er1 107.63(10) . . ?
C19 O2 Cu1 127.7(2) . . ?
C19 O2 Er1 123.8(2) . . ?
Cu1 O2 Er1 107.81(10) . . ?
C2 O3 C20 116.0(3) . . ?
C2 O3 Er1 116.0(2) . . ?
C20 O3 Er1 121.8(2) . . ?
C18 O4 C21 117.2(3) . . ?
C18 O4 Er1 117.0(2) . . ?
C21 O4 Er1 124.9(3) . . ?
O5 C22 O5 100.4(17) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.101
####################################################################### 
# 
# 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_CuEuvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060765'
_audit_update_record             
;
2017-04-26 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuEuvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Cu2 Eu2 N22 O9'
_chemical_formula_weight         1452.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.254(3)
_cell_length_b                   9.6647(11)
_cell_length_c                   26.110(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.7290(10)
_cell_angle_gamma                90.00
_cell_volume                     5285.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9945
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2880
_exptl_absorpt_coefficient_mu    3.209
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5130
_exptl_absorpt_correction_T_max  0.6621
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX SMART'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32930
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         27.60
_reflns_number_total             6115
_reflns_number_gt                5565
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0241P)²+9.9204P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6115
_refine_ls_number_parameters     361
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0263
_refine_ls_wR_factor_ref         0.0606
_refine_ls_wR_factor_gt          0.0591
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.113
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.286979(6) 0.350457(14) 0.074893(5) 0.02453(5) Uani 1 1 d . . .
Cu1 Cu 0.444152(15) 0.23916(4) 0.101913(14) 0.02798(8) Uani 1 1 d . G .
C1 C 0.40960(13) 0.5311(3) 0.06833(11) 0.0283(6) Uani 1 1 d . . .
C2 C 0.36553(14) 0.6398(3) 0.05688(12) 0.0309(6) Uani 1 1 d . H .
C3 C 0.38071(16) 0.7694(3) 0.04339(14) 0.0393(7) Uani 1 1 d . . .
H3 H 0.3508 0.8404 0.0365 0.047 Uiso 1 1 calc R H .
C4 C 0.44095(17) 0.7939(3) 0.04014(15) 0.0458(8) Uani 1 1 d . H .
H4 H 0.4510 0.8806 0.0298 0.055 Uiso 1 1 calc R . .
C5 C 0.48509(17) 0.6907(4) 0.05211(15) 0.0440(8) Uani 1 1 d . . .
H5 H 0.5256 0.7081 0.0506 0.053 Uiso 1 1 calc R H .
C6 C 0.47054(14) 0.5581(3) 0.06676(13) 0.0348(6) Uani 1 1 d . G .
C7 C 0.52155(14) 0.4592(3) 0.08211(14) 0.0398(7) Uani 1 1 d . . .
H7 H 0.5602 0.4899 0.0798 0.048 Uiso 1 1 calc R A 1
C8 C 0.58354(16) 0.2649(4) 0.11125(18) 0.0539(10) Uani 1 1 d . . .
H8A H 0.6169 0.3343 0.1228 0.065 Uiso 1 1 calc R B 1
H8B H 0.5858 0.2229 0.0782 0.065 Uiso 1 1 calc R B 1
C9 C 0.59686(14) 0.1553(3) 0.15463(13) 0.0325(6) Uani 1 1 d . G .
C10 C 0.66461(15) 0.1028(4) 0.16378(16) 0.0458(8) Uani 1 1 d . . .
H10A H 0.6671 0.0670 0.1303 0.069 Uiso 1 1 calc R G .
H10B H 0.6749 0.0309 0.1907 0.069 Uiso 1 1 calc R . .
H10C H 0.6943 0.1777 0.1761 0.069 Uiso 1 1 calc R . .
C11 C 0.59254(17) 0.2103(5) 0.20780(15) 0.0553(10) Uani 1 1 d . . .
H11A H 0.6247 0.2796 0.2222 0.083 Uiso 1 1 calc R G .
H11B H 0.5990 0.1358 0.2334 0.083 Uiso 1 1 calc R . .
H11C H 0.5511 0.2502 0.2014 0.083 Uiso 1 1 calc R . .
C12 C 0.55146(15) 0.0349(4) 0.13407(16) 0.0440(8) Uani 1 1 d . . .
H12A H 0.5490 0.0127 0.0972 0.053 Uiso 1 1 calc R C 1
H12B H 0.5681 -0.0456 0.1566 0.053 Uiso 1 1 calc R C 1
C13 C 0.46361(15) -0.0265(3) 0.15800(13) 0.0367(7) Uani 1 1 d . . .
H13 H 0.4889 -0.1039 0.1711 0.044 Uiso 1 1 calc R D 1
C14 C 0.40270(14) -0.0243(3) 0.16643(12) 0.0331(6) Uani 1 1 d . G .
C15 C 0.39018(17) -0.1302(3) 0.19814(14) 0.0412(8) Uani 1 1 d . . .
H15 H 0.4202 -0.2000 0.2116 0.049 Uiso 1 1 calc R G .
C16 C 0.33470(18) -0.1327(3) 0.20969(14) 0.0439(8) Uani 1 1 d . G .
H16 H 0.3268 -0.2043 0.2304 0.053 Uiso 1 1 calc R . .
C17 C 0.29032(16) -0.0282(3) 0.19048(13) 0.0374(7) Uani 1 1 d . . .
H17 H 0.2526 -0.0292 0.1984 0.045 Uiso 1 1 calc R G .
C18 C 0.30192(14) 0.0767(3) 0.15975(11) 0.0299(6) Uani 1 1 d . G .
C19 C 0.35775(13) 0.0801(3) 0.14591(11) 0.0276(6) Uani 1 1 d . . .
C20 C 0.26978(17) 0.7137(3) 0.07217(15) 0.0422(8) Uani 1 1 d . . .
H20A H 0.2948 0.7527 0.1066 0.063 Uiso 1 1 calc R E 1
H20B H 0.2309 0.6765 0.0747 0.063 Uiso 1 1 calc R E 1
H20C H 0.2599 0.7844 0.0447 0.063 Uiso 1 1 calc R E 1
C21 C 0.21372(18) 0.2128(4) 0.16434(16) 0.0507(9) Uani 1 1 d . . .
H21A H 0.1832 0.1387 0.1553 0.076 Uiso 1 1 calc R F 1
H21B H 0.1924 0.2985 0.1508 0.076 Uiso 1 1 calc R F 1
H21C H 0.2333 0.2183 0.2032 0.076 Uiso 1 1 calc R F 1
N1 N 0.52130(12) 0.3345(3) 0.09853(11) 0.0351(6) Uani 1 1 d . G 1
N2 N 0.48698(11) 0.0653(3) 0.13475(11) 0.0336(5) Uani 1 1 d . G 1
N3 N 0.30951(16) 0.4700(3) 0.15870(12) 0.0502(7) Uani 1 1 d . H 1
N4 N 0.31943(14) 0.4953(3) 0.20327(12) 0.0400(6) Uani 1 1 d . H 1
N5 N 0.3295(2) 0.5250(4) 0.24854(14) 0.0779(12) Uani 1 1 d . H 1
N6 N 0.27239(12) 0.3566(2) -0.02259(10) 0.0324(5) Uani 1 1 d . . 1
N7 N 0.30397(13) 0.4308(3) -0.04122(11) 0.0397(6) Uani 1 1 d . I 1
N8 N 0.33299(18) 0.5005(4) -0.05946(14) 0.0686(11) Uani 1 1 d . I 1
N9 N 0.41876(14) 0.1486(3) 0.01274(12) 0.0463(7) Uani 1 1 d . G 1
N10 N 0.37037(12) 0.1126(3) -0.01754(10) 0.0312(5) Uani 1 1 d . G 1
N11 N 0.32223(13) 0.0736(3) -0.04909(12) 0.0426(7) Uani 1 1 d . . 1
O1 O 0.39199(9) 0.4068(2) 0.07980(8) 0.0308(4) Uani 1 1 d . G 1
O2 O 0.36561(9) 0.1834(2) 0.11522(8) 0.0308(4) Uani 1 1 d . G 1
O3 O 0.30551(10) 0.6048(2) 0.05789(9) 0.0332(5) Uani 1 1 d . H 1
O4 O 0.26165(10) 0.1876(2) 0.14017(8) 0.0337(5) Uani 1 1 d . G 1
C22 C 0.5000 0.5158(14) 0.2500 0.169(5) Uani 1 2 d SDU . 1
O5 O 0.4787(6) 0.6107(10) 0.2804(5) 0.150(4) Uani 0.50 1 d PDU J 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
Eu1 O2 2.352(2) . ?
Eu1 O1 2.3605(19) . ?
Eu1 N3 2.374(3) . ?
Eu1 N11 2.407(3) 7 ?
Eu1 N6 2.455(2) . ?
Eu1 O4 2.520(2) . ?
Eu1 N6 2.529(2) 7 ?
Eu1 O3 2.556(2) . ?
Eu1 Cu1 3.4961(5) . ?
Eu1 Eu1 4.1746(5) 7 ?
Cu1 O1 1.963(2) . ?
Cu1 O2 1.9688(19) . ?
Cu1 N1 1.977(2) . ?
Cu1 N2 1.979(3) . ?
Cu1 N9 2.370(3) . ?
C1 O1 1.328(3) . ?
C1 C6 1.395(4) . ?
C1 C2 1.399(4) . ?
C2 C3 1.374(4) . ?
C2 O3 1.387(3) . ?
C3 C4 1.392(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.361(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.406(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.434(4) . ?
C7 N1 1.279(4) . ?
C7 H7 0.9300 . ?
C8 N1 1.473(4) . ?
C8 C9 1.506(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C12 1.516(4) . ?
C9 C11 1.519(5) . ?
C9 C10 1.531(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.471(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.280(4) . ?
C13 C14 1.445(4) . ?
C13 H13 0.9300 . ?
C14 C19 1.394(4) . ?
C14 C15 1.402(4) . ?
C15 C16 1.366(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.383(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.371(4) . ?
C17 H17 0.9300 . ?
C18 O4 1.380(4) . ?
C18 C19 1.406(4) . ?
C19 O2 1.328(3) . ?
C20 O3 1.442(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O4 1.432(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
N3 N4 1.135(4) . ?
N4 N5 1.162(4) . ?
N6 N7 1.215(3) . ?
N6 Eu1 2.529(2) 7 ?
N7 N8 1.143(4) . ?
N9 N10 1.153(4) . ?
N10 N11 1.172(4) . ?
N11 Eu1 2.407(3) 7 ?
C22 O5 1.3955(10) . ?
C22 O5 1.3955(10) 2_655 ?

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
O2 Eu1 O1 63.95(7) . . ?
O2 Eu1 N3 91.60(10) . . ?
O1 Eu1 N3 86.59(9) . . ?
O2 Eu1 N11 149.64(9) . 7 ?
O1 Eu1 N11 146.33(9) . 7 ?
N3 Eu1 N11 89.34(10) . 7 ?
O2 Eu1 N6 107.38(8) . . ?
O1 Eu1 N6 80.37(8) . . ?
N3 Eu1 N6 148.94(9) . . ?
N11 Eu1 N6 86.26(9) 7 . ?
O2 Eu1 O4 64.59(7) . . ?
O1 Eu1 O4 123.43(7) . . ?
N3 Eu1 O4 72.93(9) . . ?
N11 Eu1 O4 86.83(9) 7 . ?
N6 Eu1 O4 137.28(8) . . ?
O2 Eu1 N6 82.68(8) . 7 ?
O1 Eu1 N6 122.61(8) . 7 ?
N3 Eu1 N6 142.40(9) . 7 ?
N11 Eu1 N6 78.25(9) 7 7 ?
N6 Eu1 N6 66.24(9) . 7 ?
O4 Eu1 N6 71.07(7) . 7 ?
O2 Eu1 O3 126.77(7) . . ?
O1 Eu1 O3 64.70(7) . . ?
N3 Eu1 O3 72.28(9) . . ?
N11 Eu1 O3 82.23(8) 7 . ?
N6 Eu1 O3 76.67(7) . . ?
O4 Eu1 O3 143.55(7) . . ?
N6 Eu1 O3 138.82(8) 7 . ?
O2 Eu1 Cu1 32.45(5) . . ?
O1 Eu1 Cu1 32.37(5) . . ?
N3 Eu1 Cu1 94.48(8) . . ?
N11 Eu1 Cu1 175.67(7) 7 . ?
N6 Eu1 Cu1 89.42(6) . . ?
O4 Eu1 Cu1 96.21(5) . . ?
N6 Eu1 Cu1 99.80(6) 7 . ?
O3 Eu1 Cu1 97.00(5) . . ?
O2 Eu1 Eu1 95.65(5) . 7 ?
O1 Eu1 Eu1 103.19(5) . 7 ?
N3 Eu1 Eu1 169.68(8) . 7 ?
N11 Eu1 Eu1 80.69(7) 7 7 ?
N6 Eu1 Eu1 33.68(5) . 7 ?
O4 Eu1 Eu1 103.63(5) . 7 ?
N6 Eu1 Eu1 32.57(6) 7 7 ?
O3 Eu1 Eu1 108.68(5) . 7 ?
Cu1 Eu1 Eu1 95.574(8) . 7 ?
O1 Cu1 O2 78.80(8) . . ?
O1 Cu1 N1 92.19(9) . . ?
O2 Cu1 N1 166.35(10) . . ?
O1 Cu1 N2 168.20(9) . . ?
O2 Cu1 N2 91.00(9) . . ?
N1 Cu1 N2 96.72(10) . . ?
O1 Cu1 N9 95.44(10) . . ?
O2 Cu1 N9 98.09(10) . . ?
N1 Cu1 N9 92.92(11) . . ?
N2 Cu1 N9 91.84(11) . . ?
O1 Cu1 Eu1 40.07(6) . . ?
O2 Cu1 Eu1 39.87(6) . . ?
N1 Cu1 Eu1 132.25(8) . . ?
N2 Cu1 Eu1 130.65(7) . . ?
N9 Cu1 Eu1 91.43(7) . . ?
O1 C1 C6 122.7(3) . . ?
O1 C1 C2 119.2(2) . . ?
C6 C1 C2 118.1(3) . . ?
C3 C2 O3 123.3(3) . . ?
C3 C2 C1 121.6(3) . . ?
O3 C2 C1 115.0(2) . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.6(3) . . ?
C1 C6 C7 123.5(3) . . ?
C5 C6 C7 116.8(3) . . ?
N1 C7 C6 129.0(3) . . ?
N1 C7 H7 115.5 . . ?
C6 C7 H7 115.5 . . ?
N1 C8 C9 115.0(3) . . ?
N1 C8 H8A 108.5 . . ?
C9 C8 H8A 108.5 . . ?
N1 C8 H8B 108.5 . . ?
C9 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C8 C9 C12 109.6(3) . . ?
C8 C9 C11 112.6(3) . . ?
C12 C9 C11 110.6(3) . . ?
C8 C9 C10 106.5(3) . . ?
C12 C9 C10 107.7(3) . . ?
C11 C9 C10 109.6(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 112.2(3) . . ?
N2 C12 H12A 109.2 . . ?
C9 C12 H12A 109.2 . . ?
N2 C12 H12B 109.2 . . ?
C9 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
N2 C13 C14 127.9(3) . . ?
N2 C13 H13 116.0 . . ?
C14 C13 H13 116.0 . . ?
C19 C14 C15 119.7(3) . . ?
C19 C14 C13 122.7(3) . . ?
C15 C14 C13 117.6(3) . . ?
C16 C15 C14 121.2(3) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 119.7(3) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 120.0(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 O4 124.4(3) . . ?
C17 C18 C19 121.7(3) . . ?
O4 C18 C19 114.0(2) . . ?
O2 C19 C14 123.5(3) . . ?
O2 C19 C18 118.7(3) . . ?
C14 C19 C18 117.7(3) . . ?
C7 N1 C8 113.3(3) . . ?
C7 N1 Cu1 123.8(2) . . ?
C8 N1 Cu1 122.8(2) . . ?
C13 N2 C12 114.9(3) . . ?
C13 N2 Cu1 125.5(2) . . ?
C12 N2 Cu1 119.6(2) . . ?
N4 N3 Eu1 163.1(3) . . ?
N3 N4 N5 178.1(4) . . ?
N7 N6 Eu1 122.5(2) . . ?
N7 N6 Eu1 121.2(2) . 7 ?
Eu1 N6 Eu1 113.75(9) . 7 ?
N8 N7 N6 179.0(4) . . ?
N10 N9 Cu1 130.0(2) . . ?
N9 N10 N11 177.9(3) . . ?
N10 N11 Eu1 134.1(2) . 7 ?
C1 O1 Cu1 128.48(17) . . ?
C1 O1 Eu1 123.95(17) . . ?
Cu1 O1 Eu1 107.56(8) . . ?
C19 O2 Cu1 128.16(18) . . ?
C19 O2 Eu1 123.81(17) . . ?
Cu1 O2 Eu1 107.68(8) . . ?
C2 O3 C20 116.5(2) . . ?
C2 O3 Eu1 116.77(16) . . ?
C20 O3 Eu1 121.44(19) . . ?
C18 O4 C21 117.2(2) . . ?
C18 O4 Eu1 118.05(16) . . ?
C21 O4 Eu1 124.16(19) . . ?
O5 C22 O5 97.8(13) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.083
####################################################################### 
# 
# 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_8-CuTbvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060767'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 Cu2 N22 O10 Tb2'
_chemical_formula_weight         1498.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.941(3)
_cell_length_b                   10.887(3)
_cell_length_c                   13.544(4)
_cell_angle_alpha                99.761(4)
_cell_angle_beta                 90.893(5)
_cell_angle_gamma                101.172(5)
_cell_volume                     1415.6(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2759
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      23.90

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             742
_exptl_absorpt_coefficient_mu    3.282
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.4198
_exptl_absorpt_correction_T_max  0.7349
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8501
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0574
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.53
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5532
_reflns_number_gt                4573
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0599P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5532
_refine_ls_number_parameters     364
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.1054
_refine_ls_wR_factor_gt          0.0999
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb -0.06459(3) 0.55879(2) 0.140638(19) 0.03210(11) Uani 1 1 d . . .
Cu1 Cu 0.19224(7) 0.83075(7) 0.20594(5) 0.03962(18) Uani 1 1 d . . .
C1 C -0.0839(6) 0.8523(5) 0.1266(4) 0.0345(12) Uani 1 1 d . . .
C2 C -0.2231(6) 0.8003(5) 0.1073(4) 0.0368(13) Uani 1 1 d . . .
C3 C -0.3155(7) 0.8714(6) 0.0832(4) 0.0471(15) Uani 1 1 d . . .
H3 H -0.4078 0.8341 0.0701 0.056 Uiso 1 1 calc R . .
C4 C -0.2699(7) 0.9994(7) 0.0785(5) 0.0521(17) Uani 1 1 d . . .
H4 H -0.3319 1.0477 0.0622 0.062 Uiso 1 1 calc R . .
C5 C -0.1341(8) 1.0543(7) 0.0980(5) 0.0524(17) Uani 1 1 d . . .
H5 H -0.1050 1.1397 0.0938 0.063 Uiso 1 1 calc R . .
C6 C -0.0368(6) 0.9848(6) 0.1242(4) 0.0427(14) Uani 1 1 d . . .
C7 C 0.1049(7) 1.0478(6) 0.1433(5) 0.0480(15) Uani 1 1 d . . .
H7 H 0.1259 1.1309 0.1316 0.058 Uiso 1 1 calc R . .
C8 C 0.3414(7) 1.0892(7) 0.1825(6) 0.0602(19) Uani 1 1 d . . .
H8A H 0.3293 1.1722 0.1713 0.072 Uiso 1 1 calc R . .
H8B H 0.3964 1.0563 0.1297 0.072 Uiso 1 1 calc R . .
C9 C 0.4199(7) 1.1054(6) 0.2830(5) 0.0519(17) Uani 1 1 d . . .
C10 C 0.5444(8) 1.2125(8) 0.2849(6) 0.074(2) Uani 1 1 d . . .
H10A H 0.5143 1.2903 0.2812 0.111 Uiso 1 1 calc R . .
H10B H 0.5986 1.1923 0.2286 0.111 Uiso 1 1 calc R . .
H10C H 0.5988 1.2224 0.3459 0.111 Uiso 1 1 calc R . .
C11 C 0.3326(10) 1.1370(8) 0.3701(6) 0.086(3) Uani 1 1 d . . .
H11A H 0.3840 1.1428 0.4319 0.129 Uiso 1 1 calc R . .
H11B H 0.2517 1.0715 0.3662 0.129 Uiso 1 1 calc R . .
H11C H 0.3065 1.2169 0.3677 0.129 Uiso 1 1 calc R . .
C12 C 0.4727(7) 0.9848(7) 0.2886(5) 0.0584(18) Uani 1 1 d . . .
H12A H 0.5274 0.9678 0.2310 0.070 Uiso 1 1 calc R . .
H12B H 0.5332 1.0003 0.3481 0.070 Uiso 1 1 calc R . .
C13 C 0.3968(7) 0.7930(7) 0.3481(5) 0.0524(17) Uani 1 1 d . . .
H13 H 0.4804 0.8204 0.3846 0.063 Uiso 1 1 calc R . .
C14 C 0.3177(7) 0.6710(6) 0.3627(5) 0.0469(15) Uani 1 1 d . . .
C15 C 0.3654(8) 0.6151(7) 0.4400(5) 0.066(2) Uani 1 1 d . . .
H15 H 0.4465 0.6552 0.4766 0.079 Uiso 1 1 calc R . .
C16 C 0.2943(9) 0.5037(8) 0.4616(5) 0.071(2) Uani 1 1 d . . .
H16 H 0.3266 0.4690 0.5132 0.085 Uiso 1 1 calc R . .
C17 C 0.1745(8) 0.4418(7) 0.4074(5) 0.0576(18) Uani 1 1 d . . .
H17 H 0.1253 0.3669 0.4240 0.069 Uiso 1 1 calc R . .
C18 C 0.1269(7) 0.4904(6) 0.3284(4) 0.0427(14) Uani 1 1 d . . .
C19 C 0.1960(6) 0.6087(6) 0.3059(4) 0.0391(13) Uani 1 1 d . . .
C20 C -0.4028(7) 0.6187(7) 0.1214(6) 0.0567(18) Uani 1 1 d . . .
H20A H -0.4399 0.6704 0.1745 0.085 Uiso 1 1 calc R . .
H20B H -0.4126 0.5339 0.1352 0.085 Uiso 1 1 calc R . .
H20C H -0.4513 0.6166 0.0591 0.085 Uiso 1 1 calc R . .
C21 C -0.0812(8) 0.3357(7) 0.3032(6) 0.069(2) Uani 1 1 d . . .
H21A H -0.0413 0.2620 0.3023 0.103 Uiso 1 1 calc R . .
H21B H -0.1646 0.3130 0.2619 0.103 Uiso 1 1 calc R . .
H21C H -0.1009 0.3678 0.3707 0.103 Uiso 1 1 calc R . .
C22 C 0.218(2) 0.929(3) 0.561(2) 0.151(10) Uiso 0.565(13) 1 d PD A 1
C22' C 0.0969(18) 0.8640(17) 0.4860(10) 0.059(5) Uiso 0.435(13) 1 d PD A 2
N1 N 0.2062(5) 1.0043(5) 0.1746(4) 0.0454(12) Uani 1 1 d . . .
N2 N 0.3661(5) 0.8684(5) 0.2912(4) 0.0431(12) Uani 1 1 d . . .
N3 N -0.1642(7) 0.6074(7) 0.2999(4) 0.0660(18) Uani 1 1 d . . .
N4 N -0.2157(7) 0.6869(8) 0.3383(5) 0.075(2) Uani 1 1 d . . .
N5 N -0.2651(12) 0.7709(12) 0.3775(7) 0.148(5) Uani 1 1 d . . .
N6 N 0.0915(5) 0.4445(5) 0.0423(3) 0.0390(11) Uani 1 1 d . . .
N7 N 0.1926(6) 0.4202(5) 0.0834(4) 0.0473(13) Uani 1 1 d . . .
N8 N 0.2855(8) 0.3972(8) 0.1212(5) 0.088(2) Uani 1 1 d . . .
N9 N 0.3199(6) 0.7677(5) 0.0567(4) 0.0531(14) Uani 1 1 d . . .
N10 N 0.2775(5) 0.6988(5) -0.0177(4) 0.0381(11) Uani 1 1 d . . .
N11 N 0.2375(6) 0.6310(5) -0.0937(4) 0.0489(13) Uani 1 1 d . . .
O1 O 0.0034(4) 0.7783(4) 0.1457(3) 0.0393(9) Uani 1 1 d . . .
O2 O 0.1441(4) 0.6550(4) 0.2319(3) 0.0381(9) Uani 1 1 d . . .
O3 O -0.2586(4) 0.6720(4) 0.1145(3) 0.0387(9) Uani 1 1 d . . .
O4 O 0.0139(4) 0.4322(4) 0.2651(3) 0.0435(10) Uani 1 1 d . . .
O5 O 0.076(2) 0.894(3) 0.553(3) 0.285(15) Uiso 0.565(13) 1 d PD A 1
O5' O 0.0656(15) 0.8747(15) 0.3874(9) 0.094(6) Uiso 0.435(13) 1 d PD A 2


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.343(4) . ?
Tb1 O2 2.360(4) . ?
Tb1 N11 2.403(5) 2_565 ?
Tb1 N3 2.407(6) . ?
Tb1 N6 2.446(4) . ?
Tb1 N6 2.482(5) 2_565 ?
Tb1 O3 2.532(4) . ?
Tb1 O4 2.553(4) . ?
Tb1 Cu1 3.4901(10) . ?
Cu1 O2 1.973(4) . ?
Cu1 O1 1.974(4) . ?
Cu1 N1 1.985(5) . ?
Cu1 N2 1.998(5) . ?
Cu1 N9 2.474(6) . ?
C1 O1 1.343(6) . ?
C1 C2 1.393(8) . ?
C1 C6 1.434(8) . ?
C2 C3 1.379(8) . ?
C2 O3 1.393(7) . ?
C3 C4 1.392(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.368(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.414(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.441(9) . ?
C7 N1 1.289(8) . ?
C7 H7 0.9300 . ?
C8 N1 1.467(8) . ?
C8 C9 1.525(10) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C11 1.507(10) . ?
C9 C12 1.518(10) . ?
C9 C10 1.525(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.492(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.290(8) . ?
C13 C14 1.453(10) . ?
C13 H13 0.9300 . ?
C14 C19 1.411(8) . ?
C14 C15 1.416(9) . ?
C15 C16 1.360(11) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.386(8) . ?
C17 H17 0.9300 . ?
C18 O4 1.382(7) . ?
C18 C19 1.421(8) . ?
C19 O2 1.334(6) . ?
C20 O3 1.449(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O4 1.441(8) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.3949(12) . ?
C22' O5' 1.3952(11) . ?
N3 N4 1.144(8) . ?
N4 N5 1.174(10) . ?
N6 N7 1.235(6) . ?
N6 Tb1 2.482(5) 2_565 ?
N7 N8 1.138(7) . ?
N9 N10 1.167(7) . ?
N10 N11 1.174(7) . ?
N11 Tb1 2.403(5) 2_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O2 64.69(13) . . ?
O1 Tb1 N11 148.25(17) . 2_565 ?
O2 Tb1 N11 146.67(17) . 2_565 ?
O1 Tb1 N3 87.65(19) . . ?
O2 Tb1 N3 83.8(2) . . ?
N11 Tb1 N3 91.2(2) 2_565 . ?
O1 Tb1 N6 110.50(16) . . ?
O2 Tb1 N6 80.38(15) . . ?
N11 Tb1 N6 86.71(17) 2_565 . ?
N3 Tb1 N6 147.47(18) . . ?
O1 Tb1 N6 82.84(15) . 2_565 ?
O2 Tb1 N6 121.44(15) . 2_565 ?
N11 Tb1 N6 79.88(17) 2_565 2_565 ?
N3 Tb1 N6 144.63(19) . 2_565 ?
N6 Tb1 N6 66.72(18) . 2_565 ?
O1 Tb1 O3 65.24(13) . . ?
O2 Tb1 O3 124.67(13) . . ?
N11 Tb1 O3 84.23(16) 2_565 . ?
N3 Tb1 O3 72.11(17) . . ?
N6 Tb1 O3 139.63(14) . . ?
N6 Tb1 O3 72.97(14) 2_565 . ?
O1 Tb1 O4 126.03(13) . . ?
O2 Tb1 O4 64.68(13) . . ?
N11 Tb1 O4 82.66(16) 2_565 . ?
N3 Tb1 O4 69.60(18) . . ?
N6 Tb1 O4 77.95(14) . . ?
N6 Tb1 O4 141.19(14) 2_565 . ?
O3 Tb1 O4 139.06(13) . . ?
O1 Tb1 Cu1 32.62(9) . . ?
O2 Tb1 Cu1 32.73(9) . . ?
N11 Tb1 Cu1 178.65(13) 2_565 . ?
N3 Tb1 Cu1 89.87(18) . . ?
N6 Tb1 Cu1 91.94(12) . . ?
N6 Tb1 Cu1 99.68(12) 2_565 . ?
O3 Tb1 Cu1 96.87(9) . . ?
O4 Tb1 Cu1 96.97(9) . . ?
O2 Cu1 O1 79.21(15) . . ?
O2 Cu1 N1 170.12(19) . . ?
O1 Cu1 N1 91.21(19) . . ?
O2 Cu1 N2 92.58(19) . . ?
O1 Cu1 N2 167.96(19) . . ?
N1 Cu1 N2 96.5(2) . . ?
O2 Cu1 N9 92.76(18) . . ?
O1 Cu1 N9 99.24(17) . . ?
N1 Cu1 N9 91.2(2) . . ?
N2 Cu1 N9 89.86(19) . . ?
O2 Cu1 Tb1 40.30(11) . . ?
O1 Cu1 Tb1 39.78(11) . . ?
N1 Cu1 Tb1 130.56(15) . . ?
N2 Cu1 Tb1 132.86(16) . . ?
N9 Cu1 Tb1 91.40(13) . . ?
O1 C1 C2 120.0(5) . . ?
O1 C1 C6 121.4(5) . . ?
C2 C1 C6 118.6(5) . . ?
C3 C2 C1 122.0(6) . . ?
C3 C2 O3 124.0(5) . . ?
C1 C2 O3 114.0(5) . . ?
C2 C3 C4 119.7(6) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.1(6) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 121.8(6) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 117.8(6) . . ?
C5 C6 C7 119.2(6) . . ?
C1 C6 C7 123.0(5) . . ?
N1 C7 C6 128.6(6) . . ?
N1 C7 H7 115.7 . . ?
C6 C7 H7 115.7 . . ?
N1 C8 C9 114.4(6) . . ?
N1 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C11 C9 C12 111.2(7) . . ?
C11 C9 C10 110.0(6) . . ?
C12 C9 C10 107.4(6) . . ?
C11 C9 C8 111.9(7) . . ?
C12 C9 C8 108.9(5) . . ?
C10 C9 C8 107.3(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 116.0(6) . . ?
N2 C12 H12A 108.3 . . ?
C9 C12 H12A 108.3 . . ?
N2 C12 H12B 108.3 . . ?
C9 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
N2 C13 C14 128.4(6) . . ?
N2 C13 H13 115.8 . . ?
C14 C13 H13 115.8 . . ?
C19 C14 C15 119.4(6) . . ?
C19 C14 C13 123.5(6) . . ?
C15 C14 C13 117.1(6) . . ?
C16 C15 C14 121.0(7) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.5(7) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C18 120.5(7) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
O4 C18 C17 125.3(6) . . ?
O4 C18 C19 114.1(5) . . ?
C17 C18 C19 120.6(6) . . ?
O2 C19 C14 123.1(5) . . ?
O2 C19 C18 118.9(5) . . ?
C14 C19 C18 118.0(5) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 N1 C8 116.2(5) . . ?
C7 N1 Cu1 124.7(4) . . ?
C8 N1 Cu1 119.1(4) . . ?
C13 N2 C12 115.7(5) . . ?
C13 N2 Cu1 123.2(4) . . ?
C12 N2 Cu1 121.0(4) . . ?
N4 N3 Tb1 135.6(6) . . ?
N3 N4 N5 178.0(11) . . ?
N7 N6 Tb1 120.5(4) . . ?
N7 N6 Tb1 123.9(4) . 2_565 ?
Tb1 N6 Tb1 113.28(18) . 2_565 ?
N8 N7 N6 179.6(8) . . ?
N10 N9 Cu1 128.0(4) . . ?
N9 N10 N11 178.3(6) . . ?
N10 N11 Tb1 134.7(4) . 2_565 ?
C1 O1 Cu1 128.3(3) . . ?
C1 O1 Tb1 123.1(3) . . ?
Cu1 O1 Tb1 107.60(16) . . ?
C19 O2 Cu1 126.8(4) . . ?
C19 O2 Tb1 124.1(3) . . ?
Cu1 O2 Tb1 106.97(15) . . ?
C2 O3 C20 117.5(4) . . ?
C2 O3 Tb1 117.3(3) . . ?
C20 O3 Tb1 124.6(3) . . ?
C18 O4 C21 115.0(5) . . ?
C18 O4 Tb1 117.6(3) . . ?
C21 O4 Tb1 121.6(4) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.581
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.133
####################################################################### 
# 
# 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_CuTmvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060771'
_audit_update_record             
;
2017-04-26 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuTmvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Cu2 N22 O9 Tm2'
_chemical_formula_weight         1486.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.168(4)
_cell_length_b                   9.6653(16)
_cell_length_c                   25.841(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.811(2)
_cell_angle_gamma                90.00
_cell_volume                     5209.1(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9992
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.58

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2928
_exptl_absorpt_coefficient_mu    4.255
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.3096
_exptl_absorpt_correction_T_max  0.5147
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX SMART'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32402
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         27.60
_reflns_number_total             6029
_reflns_number_gt                5703
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0310P)²+21.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6029
_refine_ls_number_parameters     361
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0757
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_restrained_S_all      1.191
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tm1 Tm 0.286317(7) 0.342831(17) 0.072637(6) 0.02646(6) Uani 1 1 d . . .
Cu1 Cu 0.44180(2) 0.23447(5) 0.100292(19) 0.02858(11) Uani 1 1 d . . .
C1 C 0.40642(19) 0.5255(4) 0.06700(16) 0.0313(8) Uani 1 1 d . . .
C2 C 0.3621(2) 0.6334(4) 0.05581(18) 0.0343(9) Uani 1 1 d . . .
C3 C 0.3776(2) 0.7643(4) 0.0431(2) 0.0434(10) Uani 1 1 d . . .
H3 H 0.3475 0.8350 0.0364 0.052 Uiso 1 1 calc R . .
C4 C 0.4374(2) 0.7911(5) 0.0403(2) 0.0477(11) Uani 1 1 d . . .
H4 H 0.4473 0.8787 0.0305 0.057 Uiso 1 1 calc R . .
C5 C 0.4821(2) 0.6883(5) 0.0518(2) 0.0458(11) Uani 1 1 d . . .
H5 H 0.5226 0.7067 0.0502 0.055 Uiso 1 1 calc R . .
C6 C 0.4680(2) 0.5543(4) 0.06621(18) 0.0369(9) Uani 1 1 d . . .
C7 C 0.5194(2) 0.4561(5) 0.08152(19) 0.0408(10) Uani 1 1 d . . .
H7 H 0.5581 0.4876 0.0794 0.049 Uiso 1 1 calc R . .
C8 C 0.5819(2) 0.2611(6) 0.1108(2) 0.0533(13) Uani 1 1 d . . .
H8A H 0.6156 0.3303 0.1222 0.064 Uiso 1 1 calc R . .
H8B H 0.5840 0.2183 0.0774 0.064 Uiso 1 1 calc R . .
C9 C 0.59561(19) 0.1514(4) 0.15517(17) 0.0343(9) Uani 1 1 d . . .
C10 C 0.6633(2) 0.0999(5) 0.1642(2) 0.0474(11) Uani 1 1 d . . .
H10A H 0.6648 0.0568 0.1311 0.071 Uiso 1 1 calc R . .
H10B H 0.6754 0.0338 0.1937 0.071 Uiso 1 1 calc R . .
H10C H 0.6926 0.1766 0.1734 0.071 Uiso 1 1 calc R . .
C11 C 0.5909(2) 0.2081(6) 0.2081(2) 0.0560(14) Uani 1 1 d . . .
H11A H 0.6210 0.2825 0.2210 0.084 Uiso 1 1 calc R . .
H11B H 0.6006 0.1361 0.2353 0.084 Uiso 1 1 calc R . .
H11C H 0.5483 0.2417 0.2018 0.084 Uiso 1 1 calc R . .
C12 C 0.5498(2) 0.0318(5) 0.1339(2) 0.0437(10) Uani 1 1 d . . .
H12A H 0.5475 0.0102 0.0966 0.052 Uiso 1 1 calc R . .
H12B H 0.5664 -0.0491 0.1565 0.052 Uiso 1 1 calc R . .
C13 C 0.4609(2) -0.0299(5) 0.15738(19) 0.0396(9) Uani 1 1 d . . .
H13 H 0.4861 -0.1076 0.1708 0.048 Uiso 1 1 calc R . .
C14 C 0.3998(2) -0.0271(4) 0.16518(17) 0.0345(8) Uani 1 1 d . . .
C15 C 0.3870(2) -0.1326(5) 0.1977(2) 0.0431(10) Uani 1 1 d . . .
H15 H 0.4168 -0.2030 0.2112 0.052 Uiso 1 1 calc R . .
C16 C 0.3309(2) -0.1330(5) 0.2097(2) 0.0454(11) Uani 1 1 d . . .
H16 H 0.3231 -0.2027 0.2314 0.054 Uiso 1 1 calc R . .
C17 C 0.2864(2) -0.0291(5) 0.18916(17) 0.0390(9) Uani 1 1 d . . .
H17 H 0.2484 -0.0289 0.1970 0.047 Uiso 1 1 calc R . .
C18 C 0.2981(2) 0.0743(4) 0.15717(16) 0.0331(8) Uani 1 1 d . . .
C19 C 0.35444(19) 0.0766(4) 0.14345(15) 0.0296(8) Uani 1 1 d . . .
C20 C 0.2671(2) 0.7044(5) 0.0732(2) 0.0445(10) Uani 1 1 d . . .
H20A H 0.2939 0.7431 0.1075 0.067 Uiso 1 1 calc R . .
H20B H 0.2292 0.6661 0.0776 0.067 Uiso 1 1 calc R . .
H20C H 0.2553 0.7755 0.0456 0.067 Uiso 1 1 calc R . .
C21 C 0.2102(3) 0.2131(7) 0.1618(3) 0.0651(17) Uani 1 1 d . . .
H21A H 0.1769 0.1447 0.1504 0.098 Uiso 1 1 calc R . .
H21B H 0.1922 0.3031 0.1507 0.098 Uiso 1 1 calc R . .
H21C H 0.2299 0.2106 0.2011 0.098 Uiso 1 1 calc R . .
N1 N 0.51941(16) 0.3317(4) 0.09765(15) 0.0364(8) Uani 1 1 d . . .
N2 N 0.48514(16) 0.0613(3) 0.13423(15) 0.0345(7) Uani 1 1 d . . .
N3 N 0.3108(2) 0.4551(5) 0.15587(17) 0.0563(11) Uani 1 1 d . . .
N4 N 0.31967(18) 0.4872(4) 0.20044(15) 0.0387(8) Uani 1 1 d . . .
N5 N 0.3284(3) 0.5206(6) 0.2450(2) 0.0775(16) Uani 1 1 d . . .
N6 N 0.27103(18) 0.3528(4) -0.02106(15) 0.0367(8) Uani 1 1 d . . .
N7 N 0.3044(2) 0.4312(5) -0.04107(19) 0.0612(12) Uani 1 1 d . . .
N8 N 0.3348(3) 0.5001(8) -0.0597(3) 0.097(2) Uani 1 1 d . . .
N9 N 0.41799(19) 0.1457(4) 0.00977(17) 0.0470(10) Uani 1 1 d . . .
N10 N 0.36846(16) 0.1138(3) -0.01972(14) 0.0307(7) Uani 1 1 d . . .
N11 N 0.31858(17) 0.0781(4) -0.05090(16) 0.0432(9) Uani 1 1 d . . .
O1 O 0.38879(12) 0.4002(3) 0.07777(12) 0.0317(6) Uani 1 1 d . . .
O2 O 0.36229(13) 0.1785(3) 0.11191(11) 0.0316(6) Uani 1 1 d . . .
O3 O 0.30169(14) 0.5967(3) 0.05637(13) 0.0356(6) Uani 1 1 d . . .
O4 O 0.25776(15) 0.1845(3) 0.13671(13) 0.0428(7) Uani 1 1 d . . .
C22 C 0.5000 0.519(2) 0.2500 0.170(6) Uani 1 2 d SDU . .
O5 O 0.4785(8) 0.6108(15) 0.2816(7) 0.153(5) Uani 0.50 1 d PDU . .


_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
Tm1 O2 2.287(3) . ?
Tm1 O1 2.298(3) . ?
Tm1 N3 2.304(4) . ?
Tm1 N11 2.329(4) 7 ?
Tm1 N6 2.330(4) . ?
Tm1 N6 2.412(3) 7 ?
Tm1 O4 2.489(3) . ?
Tm1 O3 2.532(3) . ?
Tm1 Cu1 3.4379(7) . ?
Cu1 O1 1.955(3) . ?
Cu1 O2 1.962(3) . ?
Cu1 N2 1.980(3) . ?
Cu1 N1 1.982(3) . ?
Cu1 N9 2.377(4) . ?
C1 O1 1.331(5) . ?
C1 C2 1.394(6) . ?
C1 C6 1.399(6) . ?
C2 C3 1.380(6) . ?
C2 O3 1.389(5) . ?
C3 C4 1.377(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.363(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.412(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.432(6) . ?
C7 N1 1.272(6) . ?
C7 H7 0.9300 . ?
C8 N1 1.478(6) . ?
C8 C9 1.516(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C11 1.510(6) . ?
C9 C12 1.514(6) . ?
C9 C10 1.523(6) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.464(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.281(5) . ?
C13 C14 1.437(6) . ?
C13 H13 0.9300 . ?
C14 C19 1.396(6) . ?
C14 C15 1.409(6) . ?
C15 C16 1.380(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.381(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.376(6) . ?
C17 H17 0.9300 . ?
C18 O4 1.377(5) . ?
C18 C19 1.409(5) . ?
C19 O2 1.327(5) . ?
C20 O3 1.443(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O4 1.438(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
N3 N4 1.143(5) . ?
N4 N5 1.147(6) . ?
N6 N7 1.284(6) . ?
N6 Tm1 2.412(3) 7 ?
N7 N8 1.162(7) . ?
N9 N10 1.147(5) . ?
N10 N11 1.178(5) . ?
N11 Tm1 2.329(4) 7 ?
C22 O5 1.3952(10) 2_655 ?
C22 O5 1.3952(10) . ?

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
O2 Tm1 O1 64.98(9) . . ?
O2 Tm1 N3 90.48(14) . . ?
O1 Tm1 N3 85.27(14) . . ?
O2 Tm1 N11 149.32(12) . 7 ?
O1 Tm1 N11 145.25(13) . 7 ?
N3 Tm1 N11 88.29(15) . 7 ?
O2 Tm1 N6 108.39(11) . . ?
O1 Tm1 N6 80.96(11) . . ?
N3 Tm1 N6 148.87(15) . . ?
N11 Tm1 N6 87.37(14) 7 . ?
O2 Tm1 N6 82.63(12) . 7 ?
O1 Tm1 N6 123.12(11) . 7 ?
N3 Tm1 N6 142.96(15) . 7 ?
N11 Tm1 N6 80.08(13) 7 7 ?
N6 Tm1 N6 66.07(15) . 7 ?
O2 Tm1 O4 65.97(10) . . ?
O1 Tm1 O4 125.39(10) . . ?
N3 Tm1 O4 72.60(15) . . ?
N11 Tm1 O4 84.49(13) 7 . ?
N6 Tm1 O4 137.42(12) . . ?
N6 Tm1 O4 71.36(12) 7 . ?
O2 Tm1 O3 128.79(9) . . ?
O1 Tm1 O3 65.79(9) . . ?
N3 Tm1 O3 72.31(14) . . ?
N11 Tm1 O3 79.71(12) 7 . ?
N6 Tm1 O3 76.58(11) . . ?
N6 Tm1 O3 138.01(11) 7 . ?
O4 Tm1 O3 141.74(10) . . ?
O2 Tm1 Cu1 32.92(6) . . ?
O1 Tm1 Cu1 32.82(7) . . ?
N3 Tm1 Cu1 92.73(12) . . ?
N11 Tm1 Cu1 177.58(11) 7 . ?
N6 Tm1 Cu1 90.63(9) . . ?
N6 Tm1 Cu1 100.35(9) 7 . ?
O4 Tm1 Cu1 97.90(7) . . ?
O3 Tm1 Cu1 98.51(6) . . ?
O1 Cu1 O2 77.93(11) . . ?
O1 Cu1 N2 167.61(13) . . ?
O2 Cu1 N2 91.45(13) . . ?
O1 Cu1 N1 92.43(13) . . ?
O2 Cu1 N1 166.31(14) . . ?
N2 Cu1 N1 96.87(14) . . ?
O1 Cu1 N9 95.28(13) . . ?
O2 Cu1 N9 98.03(13) . . ?
N2 Cu1 N9 92.50(15) . . ?
N1 Cu1 N9 92.47(15) . . ?
O1 Cu1 Tm1 39.58(8) . . ?
O2 Cu1 Tm1 39.32(8) . . ?
N2 Cu1 Tm1 130.64(10) . . ?
N1 Cu1 Tm1 132.00(10) . . ?
N9 Cu1 Tm1 91.88(10) . . ?
O1 C1 C2 119.2(3) . . ?
O1 C1 C6 122.7(4) . . ?
C2 C1 C6 118.1(4) . . ?
C3 C2 O3 123.7(4) . . ?
C3 C2 C1 121.3(4) . . ?
O3 C2 C1 114.9(3) . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.4(4) . . ?
C1 C6 C7 123.6(4) . . ?
C5 C6 C7 116.9(4) . . ?
N1 C7 C6 128.9(4) . . ?
N1 C7 H7 115.6 . . ?
C6 C7 H7 115.6 . . ?
N1 C8 C9 115.4(4) . . ?
N1 C8 H8A 108.4 . . ?
C9 C8 H8A 108.4 . . ?
N1 C8 H8B 108.4 . . ?
C9 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
C11 C9 C12 111.2(4) . . ?
C11 C9 C8 112.0(4) . . ?
C12 C9 C8 108.8(4) . . ?
C11 C9 C10 110.3(4) . . ?
C12 C9 C10 108.1(4) . . ?
C8 C9 C10 106.2(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 112.7(4) . . ?
N2 C12 H12A 109.0 . . ?
C9 C12 H12A 109.0 . . ?
N2 C12 H12B 109.0 . . ?
C9 C12 H12B 109.0 . . ?
H12A C12 H12B 107.8 . . ?
N2 C13 C14 128.2(4) . . ?
N2 C13 H13 115.9 . . ?
C14 C13 H13 115.9 . . ?
C19 C14 C15 119.8(4) . . ?
C19 C14 C13 122.8(4) . . ?
C15 C14 C13 117.4(4) . . ?
C16 C15 C14 120.9(4) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 119.5(4) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 120.1(4) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 O4 124.2(4) . . ?
C17 C18 C19 121.8(4) . . ?
O4 C18 C19 114.0(3) . . ?
O2 C19 C14 123.6(4) . . ?
O2 C19 C18 118.6(3) . . ?
C14 C19 C18 117.8(4) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 N1 C8 114.0(4) . . ?
C7 N1 Cu1 123.8(3) . . ?
C8 N1 Cu1 122.0(3) . . ?
C13 N2 C12 115.7(4) . . ?
C13 N2 Cu1 124.8(3) . . ?
C12 N2 Cu1 119.4(3) . . ?
N4 N3 Tm1 166.9(4) . . ?
N3 N4 N5 179.4(6) . . ?
N7 N6 Tm1 122.8(3) . . ?
N7 N6 Tm1 120.5(3) . 7 ?
Tm1 N6 Tm1 113.93(15) . 7 ?
N8 N7 N6 178.7(7) . . ?
N10 N9 Cu1 126.5(3) . . ?
N9 N10 N11 177.8(4) . . ?
N10 N11 Tm1 134.3(3) . 7 ?
C1 O1 Cu1 128.2(2) . . ?
C1 O1 Tm1 124.2(2) . . ?
Cu1 O1 Tm1 107.61(12) . . ?
C19 O2 Cu1 127.6(2) . . ?
C19 O2 Tm1 123.9(2) . . ?
Cu1 O2 Tm1 107.77(11) . . ?
C2 O3 C20 115.5(3) . . ?
C2 O3 Tm1 115.7(2) . . ?
C20 O3 Tm1 122.3(3) . . ?
C18 O4 C21 117.1(3) . . ?
C18 O4 Tm1 116.9(2) . . ?
C21 O4 Tm1 124.9(3) . . ?
O5 C22 O5 101(2) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.60
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.103
####################################################################### 
# 
# 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_4-CuNdvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060763'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuNdvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Cu2 N22 Nd2 O9'
_chemical_formula_weight         1436.63

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.179(2)
_cell_length_b                   12.571(2)
_cell_length_c                   19.723(3)
_cell_angle_alpha                76.538(2)
_cell_angle_beta                 87.492(2)
_cell_angle_gamma                65.094(2)
_cell_volume                     2658.3(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9970
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      27.58

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1428
_exptl_absorpt_coefficient_mu    2.785
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.4022
_exptl_absorpt_correction_T_max  0.8968
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX SMART'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            34487
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.06
_diffrn_reflns_theta_max         27.74
_reflns_number_total             12393
_reflns_number_gt                10537
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0376P)²+1.7677P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12393
_refine_ls_number_parameters     682
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0833
_refine_ls_wR_factor_gt          0.0786
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nd1 Nd 0.473343(15) 0.455491(16) 0.230434(9) 0.02762(5) Uani 1 1 d . . .
Nd2 Nd 0.137479(15) 0.501268(15) 0.280698(9) 0.02444(5) Uani 1 1 d . . .
Cu1 Cu 0.50149(4) 0.69285(4) 0.28472(2) 0.03286(10) Uani 1 1 d . . .
Cu2 Cu 0.05848(4) 0.32796(4) 0.19065(2) 0.02997(10) Uani 1 1 d . . .
C1 C 0.4409(3) 0.7360(3) 0.13814(18) 0.0346(8) Uani 1 1 d . . .
C2 C 0.4088(3) 0.6998(4) 0.08261(19) 0.0401(8) Uani 1 1 d . . .
C3 C 0.3753(5) 0.7763(4) 0.0172(2) 0.0606(12) Uani 1 1 d . . .
H3 H 0.3542 0.7513 -0.0191 0.073 Uiso 1 1 calc R . .
C4 C 0.3729(5) 0.8905(5) 0.0051(2) 0.0711(15) Uani 1 1 d . . .
H4 H 0.3505 0.9417 -0.0393 0.085 Uiso 1 1 calc R . .
C5 C 0.4030(4) 0.9277(4) 0.0578(2) 0.0582(12) Uani 1 1 d . . .
H5 H 0.4001 1.0048 0.0493 0.070 Uiso 1 1 calc R . .
C6 C 0.4384(3) 0.8523(3) 0.1248(2) 0.0405(9) Uani 1 1 d . . .
C7 C 0.4840(4) 0.8928(4) 0.1750(2) 0.0483(10) Uani 1 1 d . . .
H7 H 0.4902 0.9656 0.1592 0.058 Uiso 1 1 calc R . .
C8 C 0.5822(4) 0.8794(4) 0.2807(2) 0.0476(10) Uani 1 1 d . . .
H8A H 0.5980 0.9436 0.2504 0.057 Uiso 1 1 calc R . .
H8B H 0.6599 0.8129 0.2981 0.057 Uiso 1 1 calc R . .
C9 C 0.5143(4) 0.9253(3) 0.3427(2) 0.0416(9) Uani 1 1 d . . .
C10 C 0.4235(5) 1.0562(4) 0.3180(3) 0.0653(13) Uani 1 1 d . . .
H10A H 0.3752 1.0819 0.3558 0.098 Uiso 1 1 calc R . .
H10B H 0.3719 1.0634 0.2801 0.098 Uiso 1 1 calc R . .
H10C H 0.4661 1.1058 0.3023 0.098 Uiso 1 1 calc R . .
C11 C 0.6096(5) 0.9152(5) 0.3941(3) 0.0634(13) Uani 1 1 d . . .
H11A H 0.6594 0.9524 0.3701 0.095 Uiso 1 1 calc R . .
H11B H 0.6593 0.8316 0.4146 0.095 Uiso 1 1 calc R . .
H11C H 0.5703 0.9552 0.4302 0.095 Uiso 1 1 calc R . .
C12 C 0.4455(4) 0.8511(3) 0.3783(2) 0.0441(9) Uani 1 1 d . . .
H12A H 0.4363 0.8566 0.4266 0.053 Uiso 1 1 calc R . .
H12B H 0.3650 0.8860 0.3555 0.053 Uiso 1 1 calc R . .
C13 C 0.5454(3) 0.6412(3) 0.43266(19) 0.0361(8) Uani 1 1 d . . .
H13 H 0.5361 0.6661 0.4742 0.043 Uiso 1 1 calc R . .
C14 C 0.6030(3) 0.5129(3) 0.43722(18) 0.0330(7) Uani 1 1 d . . .
C15 C 0.6701(3) 0.4363(4) 0.4991(2) 0.0432(9) Uani 1 1 d . . .
H15 H 0.6731 0.4686 0.5364 0.052 Uiso 1 1 calc R . .
C16 C 0.7310(4) 0.3149(4) 0.5053(2) 0.0536(11) Uani 1 1 d . . .
H16 H 0.7770 0.2656 0.5463 0.064 Uiso 1 1 calc R . .
C17 C 0.7244(4) 0.2650(4) 0.4508(2) 0.0510(11) Uani 1 1 d . . .
H17 H 0.7660 0.1822 0.4552 0.061 Uiso 1 1 calc R . .
C18 C 0.6567(3) 0.3376(3) 0.39022(19) 0.0356(8) Uani 1 1 d . . .
C19 C 0.5949(3) 0.4632(3) 0.38202(18) 0.0310(7) Uani 1 1 d . . .
C20 C 0.3648(6) 0.5491(5) 0.0500(3) 0.0792(17) Uani 1 1 d . . .
H20A H 0.2784 0.5949 0.0457 0.119 Uiso 1 1 calc R . .
H20B H 0.3839 0.4647 0.0651 0.119 Uiso 1 1 calc R . .
H20C H 0.3978 0.5645 0.0056 0.119 Uiso 1 1 calc R . .
C21 C 0.7293(5) 0.1775(4) 0.3304(3) 0.0686(14) Uani 1 1 d . . .
H21A H 0.8102 0.1680 0.3392 0.103 Uiso 1 1 calc R . .
H21B H 0.7221 0.1640 0.2851 0.103 Uiso 1 1 calc R . .
H21C H 0.7122 0.1201 0.3654 0.103 Uiso 1 1 calc R . .
C22 C -0.0640(3) 0.5878(3) 0.14368(17) 0.0294(7) Uani 1 1 d . . .
C23 C -0.0971(3) 0.7023(3) 0.15641(18) 0.0333(7) Uani 1 1 d . . .
C24 C -0.2006(4) 0.7997(4) 0.1248(2) 0.0455(9) Uani 1 1 d . . .
H24 H -0.2225 0.8745 0.1348 0.055 Uiso 1 1 calc R . .
C25 C -0.2724(4) 0.7856(4) 0.0778(2) 0.0517(11) Uani 1 1 d . . .
H25 H -0.3434 0.8510 0.0572 0.062 Uiso 1 1 calc R . .
C26 C -0.2401(4) 0.6781(4) 0.0616(2) 0.0485(10) Uani 1 1 d . . .
H26 H -0.2878 0.6709 0.0289 0.058 Uiso 1 1 calc R . .
C27 C -0.1353(3) 0.5772(3) 0.09364(19) 0.0374(8) Uani 1 1 d . . .
C28 C -0.0991(4) 0.4686(4) 0.0695(2) 0.0446(9) Uani 1 1 d . . .
H28 H -0.1413 0.4750 0.0294 0.054 Uiso 1 1 calc R . .
C29 C 0.0155(5) 0.2724(4) 0.0566(2) 0.0568(12) Uani 1 1 d . . .
H29A H 0.0944 0.2581 0.0384 0.068 Uiso 1 1 calc R . .
H29B H -0.0430 0.3032 0.0171 0.068 Uiso 1 1 calc R . .
C30 C 0.0189(4) 0.1530(4) 0.0978(2) 0.0505(10) Uani 1 1 d . . .
C31 C 0.0465(6) 0.0719(5) 0.0464(3) 0.0832(18) Uani 1 1 d . . .
H31A H 0.1215 0.0642 0.0256 0.125 Uiso 1 1 calc R . .
H31B H -0.0179 0.1070 0.0106 0.125 Uiso 1 1 calc R . .
H31C H 0.0533 -0.0064 0.0708 0.125 Uiso 1 1 calc R . .
C32 C -0.1016(5) 0.1707(5) 0.1288(3) 0.0706(15) Uani 1 1 d . . .
H32A H -0.0948 0.0960 0.1591 0.106 Uiso 1 1 calc R . .
H32B H -0.1625 0.1959 0.0919 0.106 Uiso 1 1 calc R . .
H32C H -0.1240 0.2313 0.1551 0.106 Uiso 1 1 calc R . .
C33 C 0.1226(4) 0.0927(4) 0.1534(2) 0.0557(12) Uani 1 1 d . . .
H33A H 0.1337 0.0103 0.1728 0.067 Uiso 1 1 calc R . .
H33B H 0.1965 0.0898 0.1317 0.067 Uiso 1 1 calc R . .
C34 C 0.1089(4) 0.0918(3) 0.2722(2) 0.0441(9) Uani 1 1 d . . .
H34 H 0.1170 0.0135 0.2766 0.053 Uiso 1 1 calc R . .
C35 C 0.1036(3) 0.1304(3) 0.3361(2) 0.0398(9) Uani 1 1 d . . .
C36 C 0.0920(4) 0.0558(4) 0.3987(2) 0.0528(11) Uani 1 1 d . . .
H36 H 0.0818 -0.0129 0.3972 0.063 Uiso 1 1 calc R . .
C37 C 0.0953(4) 0.0820(4) 0.4605(2) 0.0583(12) Uani 1 1 d . . .
H37 H 0.0862 0.0323 0.5012 0.070 Uiso 1 1 calc R . .
C38 C 0.1126(4) 0.1839(4) 0.4638(2) 0.0476(10) Uani 1 1 d . . .
H38 H 0.1156 0.2017 0.5067 0.057 Uiso 1 1 calc R . .
C39 C 0.1249(3) 0.2578(3) 0.40348(18) 0.0328(7) Uani 1 1 d . . .
C40 C 0.1193(3) 0.2343(3) 0.33799(18) 0.0293(7) Uani 1 1 d . . .
C41 C -0.0348(4) 0.8245(3) 0.2064(3) 0.0567(12) Uani 1 1 d . . .
H41A H -0.0367 0.8727 0.1605 0.085 Uiso 1 1 calc R . .
H41B H 0.0308 0.8180 0.2348 0.085 Uiso 1 1 calc R . .
H41C H -0.1101 0.8620 0.2271 0.085 Uiso 1 1 calc R . .
C42 C 0.1515(4) 0.3853(4) 0.46765(19) 0.0480(10) Uani 1 1 d . . .
H42A H 0.0803 0.3913 0.4924 0.072 Uiso 1 1 calc R . .
H42B H 0.1588 0.4602 0.4602 0.072 Uiso 1 1 calc R . .
H42C H 0.2218 0.3215 0.4946 0.072 Uiso 1 1 calc R . .
C43 C -0.1470(4) 0.5481(5) 0.3631(3) 0.0709(15) Uani 1 1 d . . .
H43A H -0.1246 0.4752 0.3991 0.106 Uiso 1 1 calc R . .
H43B H -0.2306 0.5778 0.3478 0.106 Uiso 1 1 calc R . .
H43C H -0.1357 0.6077 0.3811 0.106 Uiso 1 1 calc R . .
N1 N 0.5169(3) 0.8386(3) 0.23908(17) 0.0415(7) Uani 1 1 d . . .
N2 N 0.5062(3) 0.7230(3) 0.37631(15) 0.0335(6) Uani 1 1 d . . .
N3 N -0.0160(3) 0.3645(3) 0.09634(16) 0.0389(7) Uani 1 1 d . . .
N4 N 0.1034(3) 0.1543(3) 0.21008(18) 0.0397(7) Uani 1 1 d . . .
N5 N 0.2584(3) 0.6257(3) 0.24262(17) 0.0370(7) Uani 1 1 d . . .
N6 N 0.2588(3) 0.7046(3) 0.26558(18) 0.0382(7) Uani 1 1 d . . .
N7 N 0.2623(3) 0.7819(3) 0.2864(2) 0.0573(10) Uani 1 1 d . . .
N8 N 0.3610(3) 0.3867(3) 0.33315(17) 0.0397(7) Uani 1 1 d . . .
N9 N 0.4030(3) 0.3081(3) 0.38293(16) 0.0364(7) Uani 1 1 d . . .
N10 N 0.4435(4) 0.2308(4) 0.4321(2) 0.0602(10) Uani 1 1 d . . .
N11 N 0.2909(3) 0.4288(4) 0.1899(2) 0.0565(4) Uani 1 1 d . . .
N12 N 0.2867(3) 0.3591(4) 0.1596(2) 0.0565(4) Uani 1 1 d . . .
N13 N 0.2794(3) 0.2934(4) 0.1296(2) 0.0565(4) Uani 1 1 d . . .
N14 N 0.5499(3) 0.2774(4) 0.1852(2) 0.0565(4) Uani 1 1 d . . .
N15 N 0.6036(3) 0.1817(4) 0.1748(2) 0.0565(4) Uani 1 1 d . . .
N16 N 0.6575(3) 0.0876(4) 0.1654(2) 0.0565(4) Uani 1 1 d . . .
N17 N 0.0783(3) 0.6362(3) 0.35973(18) 0.0474(8) Uani 1 1 d . . .
N18 N 0.0281(4) 0.7335(3) 0.36803(18) 0.0539(9) Uani 1 1 d . . .
N19 N -0.0206(6) 0.8302(4) 0.3767(3) 0.0981(18) Uani 1 1 d . . .
N20 N -0.1374(3) 0.3823(3) 0.24440(19) 0.0463(8) Uani 1 1 d . . .
N21 N -0.2308(3) 0.4097(3) 0.21601(16) 0.0360(7) Uani 1 1 d . . .
N22 N -0.3217(3) 0.4347(4) 0.1866(2) 0.0520(9) Uani 1 1 d . . .
O1 O 0.4754(2) 0.6576(2) 0.19897(12) 0.0345(5) Uani 1 1 d . . .
O2 O 0.5314(2) 0.5276(2) 0.32157(12) 0.0331(5) Uani 1 1 d . . .
O3 O 0.6442(2) 0.2979(2) 0.33249(14) 0.0410(6) Uani 1 1 d . . .
O4 O 0.4162(3) 0.5840(3) 0.10009(13) 0.0441(6) Uani 1 1 d . . .
O5 O 0.03302(19) 0.49626(19) 0.17827(12) 0.0286(5) Uani 1 1 d . . .
O6 O 0.1320(2) 0.30932(19) 0.28151(12) 0.0280(5) Uani 1 1 d . . .
O7 O 0.1419(2) 0.3598(2) 0.40190(12) 0.0355(5) Uani 1 1 d . . .
O8 O -0.0176(2) 0.7068(2) 0.20169(13) 0.0367(6) Uani 1 1 d . . .
O9 O -0.0746(2) 0.5244(2) 0.30685(13) 0.0394(6) Uani 1 1 d . . .
H9 H -0.0938 0.4867 0.2847 0.059 Uiso 1 1 d R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nd1 N14 2.403(4) . ?
Nd1 O2 2.442(2) . ?
Nd1 O1 2.482(2) . ?
Nd1 N22 2.532(3) 1_655 ?
Nd1 N11 2.568(4) . ?
Nd1 N8 2.581(3) . ?
Nd1 N5 2.638(3) . ?
Nd1 O4 2.642(3) . ?
Nd1 O3 2.710(3) . ?
Nd1 Cu1 3.5423(7) . ?
Nd1 Nd2 3.9966(7) . ?
Nd2 N17 2.435(3) . ?
Nd2 O6 2.438(2) . ?
Nd2 O5 2.461(2) . ?
Nd2 O9 2.518(2) . ?
Nd2 N5 2.545(3) . ?
Nd2 N11 2.561(4) . ?
Nd2 N8 2.608(3) . ?
Nd2 O7 2.613(2) . ?
Nd2 O8 2.635(2) . ?
Nd2 Cu2 3.5415(6) . ?
Cu1 O2 1.913(2) . ?
Cu1 O1 1.916(2) . ?
Cu1 N1 1.927(3) . ?
Cu1 N2 1.938(3) . ?
Cu2 N4 1.958(3) . ?
Cu2 O6 1.958(2) . ?
Cu2 O5 1.961(2) . ?
Cu2 N3 1.973(3) . ?
Cu2 N20 2.454(3) . ?
C1 O1 1.316(4) . ?
C1 C2 1.407(5) . ?
C1 C6 1.411(5) . ?
C2 C3 1.377(5) . ?
C2 O4 1.381(5) . ?
C3 C4 1.387(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.356(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.397(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.437(6) . ?
C7 N1 1.279(5) . ?
C7 H7 0.9300 . ?
C8 N1 1.471(5) . ?
C8 C9 1.533(6) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.519(6) . ?
C9 C11 1.519(6) . ?
C9 C12 1.539(5) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.471(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.273(5) . ?
C13 C14 1.444(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.400(5) . ?
C14 C19 1.401(5) . ?
C15 C16 1.364(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.387(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.373(5) . ?
C17 H17 0.9300 . ?
C18 O3 1.383(4) . ?
C18 C19 1.406(5) . ?
C19 O2 1.334(4) . ?
C20 O4 1.430(5) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O3 1.439(5) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.321(4) . ?
C22 C23 1.403(5) . ?
C22 C27 1.407(5) . ?
C23 O8 1.373(4) . ?
C23 C24 1.375(5) . ?
C24 C25 1.390(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.351(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.405(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.436(5) . ?
C28 N3 1.276(5) . ?
C28 H28 0.9300 . ?
C29 N3 1.457(5) . ?
C29 C30 1.516(6) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C32 1.512(6) . ?
C30 C33 1.516(6) . ?
C30 C31 1.531(5) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 N4 1.460(5) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 N4 1.280(5) . ?
C34 C35 1.441(6) . ?
C34 H34 0.9300 . ?
C35 C40 1.406(5) . ?
C35 C36 1.409(6) . ?
C36 C37 1.341(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.399(6) . ?
C37 H37 0.9300 . ?
C38 C39 1.374(5) . ?
C38 H38 0.9300 . ?
C39 O7 1.377(4) . ?
C39 C40 1.401(5) . ?
C40 O6 1.332(4) . ?
C41 O8 1.429(4) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 O7 1.427(4) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 O9 1.394(5) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
N5 N6 1.184(4) . ?
N6 N7 1.156(4) . ?
N8 N9 1.170(4) . ?
N9 N10 1.152(5) . ?
N11 N12 1.188(5) . ?
N12 N13 1.154(5) . ?
N14 N15 1.166(5) . ?
N15 N16 1.141(5) . ?
N17 N18 1.162(5) . ?
N18 N19 1.157(5) . ?
N20 N21 1.167(4) . ?
N21 N22 1.157(4) . ?
N22 Nd1 2.532(3) 1_455 ?
O9 H9 0.8177 . ?

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
N14 Nd1 O2 138.04(11) . . ?
N14 Nd1 O1 137.09(11) . . ?
O2 Nd1 O1 61.56(8) . . ?
N14 Nd1 N22 74.78(12) . 1_655 ?
O2 Nd1 N22 83.24(10) . 1_655 ?
O1 Nd1 N22 70.87(10) . 1_655 ?
N14 Nd1 N11 72.10(12) . . ?
O2 Nd1 N11 139.49(10) . . ?
O1 Nd1 N11 119.70(11) . . ?
N22 Nd1 N11 137.09(12) 1_655 . ?
N14 Nd1 N8 98.68(12) . . ?
O2 Nd1 N8 79.66(9) . . ?
O1 Nd1 N8 124.18(9) . . ?
N22 Nd1 N8 145.31(11) 1_655 . ?
N11 Nd1 N8 67.21(11) . . ?
N14 Nd1 N5 136.46(11) . . ?
O2 Nd1 N5 81.91(9) . . ?
O1 Nd1 N5 68.97(8) . . ?
N22 Nd1 N5 139.57(11) 1_655 . ?
N11 Nd1 N5 64.41(10) . . ?
N8 Nd1 N5 67.06(9) . . ?
N14 Nd1 O4 87.79(12) . . ?
O2 Nd1 O4 122.18(8) . . ?
O1 Nd1 O4 60.62(8) . . ?
N22 Nd1 O4 77.80(11) 1_655 . ?
N11 Nd1 O4 74.44(11) . . ?
N8 Nd1 O4 136.65(9) . . ?
N5 Nd1 O4 78.84(9) . . ?
N14 Nd1 O3 79.34(11) . . ?
O2 Nd1 O3 59.90(8) . . ?
O1 Nd1 O3 112.79(8) . . ?
N22 Nd1 O3 72.38(11) 1_655 . ?
N11 Nd1 O3 125.71(11) . . ?
N8 Nd1 O3 72.93(9) . . ?
N5 Nd1 O3 128.61(9) . . ?
O4 Nd1 O3 149.68(8) . . ?
N14 Nd1 Cu1 153.44(9) . . ?
O2 Nd1 Cu1 30.85(5) . . ?
O1 Nd1 Cu1 31.23(5) . . ?
N22 Nd1 Cu1 79.15(9) 1_655 . ?
N11 Nd1 Cu1 133.08(8) . . ?
N8 Nd1 Cu1 99.86(7) . . ?
N5 Nd1 Cu1 69.02(6) . . ?
O4 Nd1 Cu1 91.64(6) . . ?
O3 Nd1 Cu1 88.12(5) . . ?
N14 Nd1 Nd2 104.09(9) . . ?
O2 Nd1 Nd2 100.74(6) . . ?
O1 Nd1 Nd2 107.66(6) . . ?
N22 Nd1 Nd2 174.56(9) 1_655 . ?
N11 Nd1 Nd2 38.75(8) . . ?
N8 Nd1 Nd2 39.88(7) . . ?
N5 Nd1 Nd2 38.70(6) . . ?
O4 Nd1 Nd2 96.88(6) . . ?
O3 Nd1 Nd2 112.78(6) . . ?
Cu1 Nd1 Nd2 102.339(10) . . ?
N17 Nd2 O6 135.17(10) . . ?
N17 Nd2 O5 132.82(10) . . ?
O6 Nd2 O5 63.91(7) . . ?
N17 Nd2 O9 77.36(10) . . ?
O6 Nd2 O9 72.93(8) . . ?
O5 Nd2 O9 69.28(8) . . ?
N17 Nd2 N5 76.99(11) . . ?
O6 Nd2 N5 143.61(9) . . ?
O5 Nd2 N5 110.03(9) . . ?
O9 Nd2 N5 141.29(9) . . ?
N17 Nd2 N11 142.15(11) . . ?
O6 Nd2 N11 79.10(10) . . ?
O5 Nd2 N11 70.30(10) . . ?
O9 Nd2 N11 137.84(10) . . ?
N5 Nd2 N11 65.85(11) . . ?
N17 Nd2 N8 93.35(11) . . ?
O6 Nd2 N8 90.03(9) . . ?
O5 Nd2 N8 133.26(9) . . ?
O9 Nd2 N8 141.97(9) . . ?
N5 Nd2 N8 68.03(10) . . ?
N11 Nd2 N8 66.91(12) . . ?
N17 Nd2 O7 76.59(10) . . ?
O6 Nd2 O7 62.29(7) . . ?
O5 Nd2 O7 119.55(7) . . ?
O9 Nd2 O7 70.51(8) . . ?
N5 Nd2 O7 129.50(9) . . ?
N11 Nd2 O7 122.06(11) . . ?
N8 Nd2 O7 71.46(9) . . ?
N17 Nd2 O8 77.17(10) . . ?
O6 Nd2 O8 121.95(7) . . ?
O5 Nd2 O8 61.30(7) . . ?
O9 Nd2 O8 71.35(8) . . ?
N5 Nd2 O8 75.02(9) . . ?
N11 Nd2 O8 99.05(11) . . ?
N8 Nd2 O8 143.03(9) . . ?
O7 Nd2 O8 137.37(8) . . ?
N17 Nd2 Cu2 147.81(8) . . ?
O6 Nd2 Cu2 31.96(5) . . ?
O5 Nd2 Cu2 32.18(5) . . ?
O9 Nd2 Cu2 70.46(6) . . ?
N5 Nd2 Cu2 130.26(7) . . ?
N11 Nd2 Cu2 69.10(8) . . ?
N8 Nd2 Cu2 111.71(7) . . ?
O7 Nd2 Cu2 92.08(5) . . ?
O8 Nd2 Cu2 92.62(5) . . ?
N17 Nd2 Nd1 105.87(8) . . ?
O6 Nd2 Nd1 104.74(5) . . ?
O5 Nd2 Nd1 107.67(5) . . ?
O9 Nd2 Nd1 176.71(6) . . ?
N5 Nd2 Nd1 40.39(7) . . ?
N11 Nd2 Nd1 38.88(8) . . ?
N8 Nd2 Nd1 39.39(7) . . ?
O7 Nd2 Nd1 110.66(6) . . ?
O8 Nd2 Nd1 108.50(6) . . ?
Cu2 Nd2 Nd1 106.315(10) . . ?
O2 Cu1 O1 82.29(10) . . ?
O2 Cu1 N1 163.82(13) . . ?
O1 Cu1 N1 94.04(12) . . ?
O2 Cu1 N2 93.47(11) . . ?
O1 Cu1 N2 170.94(11) . . ?
N1 Cu1 N2 92.19(13) . . ?
O2 Cu1 Nd1 40.88(7) . . ?
O1 Cu1 Nd1 42.18(7) . . ?
N1 Cu1 Nd1 135.85(10) . . ?
N2 Cu1 Nd1 131.96(8) . . ?
N4 Cu2 O6 90.93(11) . . ?
N4 Cu2 O5 172.52(11) . . ?
O6 Cu2 O5 82.83(9) . . ?
N4 Cu2 N3 95.13(13) . . ?
O6 Cu2 N3 173.76(11) . . ?
O5 Cu2 N3 91.02(11) . . ?
N4 Cu2 N20 96.37(12) . . ?
O6 Cu2 N20 87.88(10) . . ?
O5 Cu2 N20 87.55(10) . . ?
N3 Cu2 N20 92.93(12) . . ?
N4 Cu2 Nd2 131.34(10) . . ?
O6 Cu2 Nd2 41.23(6) . . ?
O5 Cu2 Nd2 41.94(6) . . ?
N3 Cu2 Nd2 132.54(9) . . ?
N20 Cu2 Nd2 91.03(8) . . ?
O1 C1 C2 117.8(3) . . ?
O1 C1 C6 123.9(3) . . ?
C2 C1 C6 118.2(3) . . ?
C3 C2 O4 125.0(4) . . ?
C3 C2 C1 120.7(4) . . ?
O4 C2 C1 114.2(3) . . ?
C2 C3 C4 120.2(4) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 119.4(4) . . ?
C5 C6 C7 117.4(4) . . ?
C1 C6 C7 122.8(3) . . ?
N1 C7 C6 126.6(4) . . ?
N1 C7 H7 116.7 . . ?
C6 C7 H7 116.7 . . ?
N1 C8 C9 114.3(3) . . ?
N1 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10 C9 C11 110.2(4) . . ?
C10 C9 C8 109.7(4) . . ?
C11 C9 C8 106.5(4) . . ?
C10 C9 C12 108.4(4) . . ?
C11 C9 C12 109.9(4) . . ?
C8 C9 C12 112.2(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 113.5(3) . . ?
N2 C12 H12A 108.9 . . ?
C9 C12 H12A 108.9 . . ?
N2 C12 H12B 108.9 . . ?
C9 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
N2 C13 C14 125.3(3) . . ?
N2 C13 H13 117.4 . . ?
C14 C13 H13 117.4 . . ?
C15 C14 C19 119.2(3) . . ?
C15 C14 C13 118.3(3) . . ?
C19 C14 C13 122.4(3) . . ?
C16 C15 C14 121.0(4) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C17 120.1(4) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 120.1(4) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 O3 125.1(3) . . ?
C17 C18 C19 120.8(4) . . ?
O3 C18 C19 114.1(3) . . ?
O2 C19 C14 124.1(3) . . ?
O2 C19 C18 117.2(3) . . ?
C14 C19 C18 118.6(3) . . ?
O4 C20 H20A 109.5 . . ?
O4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C21 H21A 109.5 . . ?
O3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 C23 118.6(3) . . ?
O5 C22 C27 123.5(3) . . ?
C23 C22 C27 117.9(3) . . ?
O8 C23 C24 124.5(3) . . ?
O8 C23 C22 114.2(3) . . ?
C24 C23 C22 121.3(3) . . ?
C23 C24 C25 119.5(4) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C26 C25 C24 120.8(4) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 120.6(4) . . ?
C25 C26 H26 119.7 . . ?
C27 C26 H26 119.7 . . ?
C26 C27 C22 119.7(4) . . ?
C26 C27 C28 118.1(3) . . ?
C22 C27 C28 122.0(3) . . ?
N3 C28 C27 127.7(3) . . ?
N3 C28 H28 116.1 . . ?
C27 C28 H28 116.1 . . ?
N3 C29 C30 114.7(3) . . ?
N3 C29 H29A 108.6 . . ?
C30 C29 H29A 108.6 . . ?
N3 C29 H29B 108.6 . . ?
C30 C29 H29B 108.6 . . ?
H29A C29 H29B 107.6 . . ?
C32 C30 C33 111.9(4) . . ?
C32 C30 C29 110.7(4) . . ?
C33 C30 C29 110.1(4) . . ?
C32 C30 C31 110.3(4) . . ?
C33 C30 C31 107.1(4) . . ?
C29 C30 C31 106.6(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N4 C33 C30 113.5(3) . . ?
N4 C33 H33A 108.9 . . ?
C30 C33 H33A 108.9 . . ?
N4 C33 H33B 108.9 . . ?
C30 C33 H33B 108.9 . . ?
H33A C33 H33B 107.7 . . ?
N4 C34 C35 126.7(3) . . ?
N4 C34 H34 116.7 . . ?
C35 C34 H34 116.7 . . ?
C40 C35 C36 119.7(4) . . ?
C40 C35 C34 121.9(3) . . ?
C36 C35 C34 118.2(4) . . ?
C37 C36 C35 121.2(4) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C36 C37 C38 120.1(4) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C39 C38 C37 119.8(4) . . ?
C39 C38 H38 120.1 . . ?
C37 C38 H38 120.1 . . ?
C38 C39 O7 123.7(3) . . ?
C38 C39 C40 121.5(3) . . ?
O7 C39 C40 114.9(3) . . ?
O6 C40 C39 118.5(3) . . ?
O6 C40 C35 123.8(3) . . ?
C39 C40 C35 117.7(3) . . ?
O8 C41 H41A 109.5 . . ?
O8 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O8 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O7 C42 H42A 109.5 . . ?
O7 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O7 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O9 C43 H43A 109.5 . . ?
O9 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O9 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C7 N1 C8 120.2(3) . . ?
C7 N1 Cu1 124.0(3) . . ?
C8 N1 Cu1 115.5(3) . . ?
C13 N2 C12 120.4(3) . . ?
C13 N2 Cu1 124.6(3) . . ?
C12 N2 Cu1 114.5(2) . . ?
C28 N3 C29 117.3(3) . . ?
C28 N3 Cu2 120.8(3) . . ?
C29 N3 Cu2 121.7(3) . . ?
C34 N4 C33 117.2(3) . . ?
C34 N4 Cu2 121.7(3) . . ?
C33 N4 Cu2 121.0(3) . . ?
N6 N5 Nd2 128.1(2) . . ?
N6 N5 Nd1 115.8(2) . . ?
Nd2 N5 Nd1 100.91(10) . . ?
N7 N6 N5 177.6(4) . . ?
N9 N8 Nd1 127.8(2) . . ?
N9 N8 Nd2 130.0(2) . . ?
Nd1 N8 Nd2 100.73(11) . . ?
N10 N9 N8 179.5(4) . . ?
N12 N11 Nd2 120.6(3) . . ?
N12 N11 Nd1 130.5(3) . . ?
Nd2 N11 Nd1 102.37(12) . . ?
N13 N12 N11 178.2(5) . . ?
N15 N14 Nd1 166.3(4) . . ?
N16 N15 N14 178.9(5) . . ?
N18 N17 Nd2 148.9(3) . . ?
N19 N18 N17 179.2(6) . . ?
N21 N20 Cu2 126.0(3) . . ?
N22 N21 N20 178.0(4) . . ?
N21 N22 Nd1 131.5(3) . 1_455 ?
C1 O1 Cu1 125.2(2) . . ?
C1 O1 Nd1 126.8(2) . . ?
Cu1 O1 Nd1 106.60(10) . . ?
C19 O2 Cu1 122.2(2) . . ?
C19 O2 Nd1 128.4(2) . . ?
Cu1 O2 Nd1 108.26(10) . . ?
C18 O3 C21 116.2(3) . . ?
C18 O3 Nd1 117.9(2) . . ?
C21 O3 Nd1 125.7(3) . . ?
C2 O4 C20 116.9(3) . . ?
C2 O4 Nd1 120.2(2) . . ?
C20 O4 Nd1 121.3(3) . . ?
C22 O5 Cu2 122.3(2) . . ?
C22 O5 Nd2 124.4(2) . . ?
Cu2 O5 Nd2 105.89(9) . . ?
C40 O6 Cu2 120.3(2) . . ?
C40 O6 Nd2 124.9(2) . . ?
Cu2 O6 Nd2 106.81(9) . . ?
C39 O7 C42 116.7(3) . . ?
C39 O7 Nd2 118.60(19) . . ?
C42 O7 Nd2 124.5(2) . . ?
C23 O8 C41 116.2(3) . . ?
C23 O8 Nd2 117.81(19) . . ?
C41 O8 Nd2 125.6(2) . . ?
C43 O9 Nd2 134.7(3) . . ?
C43 O9 H9 111.6 . . ?
Nd2 O9 H9 109.4 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.74
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.573
_refine_diff_density_min         -1.129
_refine_diff_density_rms         0.105
####################################################################### 
# 
# 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_CuYbvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060772'
_audit_update_record             
;
2017-04-26 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuYbvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 Cu2 N22 O10 Yb2'
_chemical_formula_weight         1526.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.986(4)
_cell_length_b                   10.816(4)
_cell_length_c                   13.393(5)
_cell_angle_alpha                100.436(6)
_cell_angle_beta                 91.137(6)
_cell_angle_gamma                100.644(6)
_cell_volume                     1395.9(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4283
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      26.79

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_exptl_absorpt_coefficient_mu    4.145
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.3248
_exptl_absorpt_correction_T_max  0.7327
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9079
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         27.00
_reflns_number_total             6031
_reflns_number_gt                5328
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0552P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6031
_refine_ls_number_parameters     384
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0888
_refine_ls_wR_factor_gt          0.0859
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb -0.060463(17) 0.559793(16) 0.136714(13) 0.03673(8) Uani 1 1 d . . .
Cu1 Cu 0.19343(5) 0.82591(5) 0.20514(4) 0.04317(14) Uani 1 1 d . . .
C1 C -0.0774(4) 0.8520(4) 0.1245(3) 0.0407(9) Uani 1 1 d . . .
C2 C -0.2174(4) 0.7988(5) 0.1032(3) 0.0439(10) Uani 1 1 d . . .
C3 C -0.3083(5) 0.8718(5) 0.0789(4) 0.0543(12) Uani 1 1 d . . .
H3 H -0.3996 0.8342 0.0633 0.065 Uiso 1 1 calc R . .
C4 C -0.2643(6) 1.0011(5) 0.0775(4) 0.0609(14) Uani 1 1 d . . .
H4 H -0.3259 1.0502 0.0613 0.073 Uiso 1 1 calc R . .
C5 C -0.1273(6) 1.0567(5) 0.1006(4) 0.0573(13) Uani 1 1 d . . .
H5 H -0.0978 1.1432 0.0996 0.069 Uiso 1 1 calc R . .
C6 C -0.0334(5) 0.9839(5) 0.1253(4) 0.0479(11) Uani 1 1 d . . .
C7 C 0.1067(6) 1.0483(5) 0.1479(4) 0.0554(12) Uani 1 1 d . . .
H7 H 0.1265 1.1331 0.1396 0.067 Uiso 1 1 calc R . .
C8 C 0.3434(6) 1.0887(6) 0.1883(5) 0.0675(15) Uani 1 1 d . . .
H8A H 0.3305 1.1742 0.1834 0.081 Uiso 1 1 calc R . .
H8B H 0.3963 1.0597 0.1318 0.081 Uiso 1 1 calc R . .
C9 C 0.4238(5) 1.0956(5) 0.2862(4) 0.0563(13) Uani 1 1 d . . .
C10 C 0.5513(6) 1.2036(6) 0.2901(5) 0.0797(19) Uani 1 1 d . . .
H10A H 0.5226 1.2833 0.2891 0.120 Uiso 1 1 calc R . .
H10B H 0.6039 1.1834 0.2322 0.120 Uiso 1 1 calc R . .
H10C H 0.6061 1.2106 0.3513 0.120 Uiso 1 1 calc R . .
C11 C 0.3442(8) 1.1287(7) 0.3795(6) 0.095(3) Uani 1 1 d . . .
H11A H 0.3971 1.1259 0.4394 0.143 Uiso 1 1 calc R . .
H11B H 0.2599 1.0680 0.3747 0.143 Uiso 1 1 calc R . .
H11C H 0.3251 1.2132 0.3833 0.143 Uiso 1 1 calc R . .
C12 C 0.4737(5) 0.9719(6) 0.2861(5) 0.0665(15) Uani 1 1 d . . .
H12A H 0.5235 0.9539 0.2254 0.080 Uiso 1 1 calc R . .
H12B H 0.5374 0.9843 0.3442 0.080 Uiso 1 1 calc R . .
C13 C 0.3964(5) 0.7820(5) 0.3446(4) 0.0544(12) Uani 1 1 d . . .
H13 H 0.4808 0.8070 0.3804 0.065 Uiso 1 1 calc R . .
C14 C 0.3165(5) 0.6607(5) 0.3592(4) 0.0518(11) Uani 1 1 d . . .
C15 C 0.3624(6) 0.6032(6) 0.4366(4) 0.0676(15) Uani 1 1 d . . .
H15 H 0.4438 0.6420 0.4736 0.081 Uiso 1 1 calc R . .
C16 C 0.2901(7) 0.4919(6) 0.4585(5) 0.0781(18) Uani 1 1 d . . .
H16 H 0.3213 0.4559 0.5104 0.094 Uiso 1 1 calc R . .
C17 C 0.1685(6) 0.4332(6) 0.4017(4) 0.0640(14) Uani 1 1 d . . .
H17 H 0.1177 0.3584 0.4167 0.077 Uiso 1 1 calc R . .
C18 C 0.1236(5) 0.4850(5) 0.3242(4) 0.0478(10) Uani 1 1 d . . .
C19 C 0.1938(4) 0.6001(4) 0.3018(3) 0.0435(10) Uani 1 1 d . . .
C20 C -0.3976(5) 0.6205(6) 0.1182(5) 0.0697(16) Uani 1 1 d . . .
H20A H -0.4315 0.6745 0.1729 0.105 Uiso 1 1 calc R . .
H20B H -0.4089 0.5351 0.1318 0.105 Uiso 1 1 calc R . .
H20C H -0.4475 0.6192 0.0559 0.105 Uiso 1 1 calc R . .
C21 C -0.0905(6) 0.3386(6) 0.3016(5) 0.0718(17) Uani 1 1 d . . .
H21A H -0.0546 0.2626 0.3039 0.108 Uiso 1 1 calc R . .
H21B H -0.1731 0.3168 0.2590 0.108 Uiso 1 1 calc R . .
H21C H -0.1096 0.3764 0.3691 0.108 Uiso 1 1 calc R . .
C22 C 0.188(2) 0.930(2) 0.5791(18) 0.160(7) Uani 0.540(12) 1 d PDU A 1
C22' C 0.096(3) 0.858(4) 0.4804(13) 0.122(6) Uani 0.460(12) 1 d PDU A 2
N1 N 0.2085(4) 1.0029(4) 0.1784(3) 0.0514(10) Uani 1 1 d . . .
N2 N 0.3668(4) 0.8590(4) 0.2894(3) 0.0482(9) Uani 1 1 d . . .
N3 N -0.1544(5) 0.6145(5) 0.2939(4) 0.0693(13) Uani 1 1 d . . .
N4 N -0.2112(6) 0.6898(6) 0.3339(4) 0.0807(16) Uani 1 1 d . . .
N5 N -0.2662(11) 0.7653(11) 0.3732(6) 0.179(5) Uani 1 1 d . . .
N6 N 0.0831(4) 0.4441(4) 0.0414(3) 0.0486(9) Uani 1 1 d U . .
N7 N 0.1905(6) 0.4166(5) 0.0843(4) 0.0746(13) Uani 1 1 d U . .
N8 N 0.2884(9) 0.3933(10) 0.1243(6) 0.140(3) Uani 1 1 d . . .
N9 N 0.3237(4) 0.7637(4) 0.0537(3) 0.0575(11) Uani 1 1 d . . .
N10 N 0.2771(4) 0.6922(3) -0.0190(3) 0.0412(8) Uani 1 1 d . . .
N11 N 0.2320(4) 0.6211(4) -0.0946(3) 0.0548(10) Uani 1 1 d . . .
O1 O 0.0060(3) 0.7750(3) 0.1430(2) 0.0420(7) Uani 1 1 d . . .
O2 O 0.1433(3) 0.6485(3) 0.2276(2) 0.0414(7) Uani 1 1 d . . .
O3 O -0.2524(3) 0.6703(3) 0.1089(3) 0.0503(8) Uani 1 1 d . . .
O4 O 0.0091(3) 0.4294(3) 0.2606(2) 0.0493(8) Uani 1 1 d . . .
O5 O 0.078(2) 0.873(3) 0.5100(16) 0.181(6) Uani 0.540(12) 1 d PDU A 1
O5' O 0.0637(10) 0.8747(10) 0.3825(8) 0.084(4) Uani 0.460(12) 1 d PDU A 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
Yb1 O1 2.285(3) . ?
Yb1 O2 2.302(3) . ?
Yb1 N11 2.324(4) 2_565 ?
Yb1 N6 2.326(4) . ?
Yb1 N3 2.343(5) . ?
Yb1 N6 2.383(4) 2_565 ?
Yb1 O3 2.494(3) . ?
Yb1 O4 2.527(3) . ?
Yb1 Cu1 3.4364(11) . ?
Yb1 Yb1 3.9469(14) 2_565 ?
Cu1 O2 1.970(3) . ?
Cu1 O1 1.973(3) . ?
Cu1 N2 1.986(4) . ?
Cu1 N1 1.989(4) . ?
C1 O1 1.330(5) . ?
C1 C6 1.412(6) . ?
C1 C2 1.412(6) . ?
C2 C3 1.378(6) . ?
C2 O3 1.386(6) . ?
C3 C4 1.391(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(8) . ?
C4 H4 0.9300 . ?
C5 C6 1.402(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.442(7) . ?
C7 N1 1.297(7) . ?
C7 H7 0.9300 . ?
C8 N1 1.476(6) . ?
C8 C9 1.507(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C12 1.511(8) . ?
C9 C11 1.517(8) . ?
C9 C10 1.553(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.474(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.279(7) . ?
C13 C14 1.451(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.411(7) . ?
C14 C19 1.416(6) . ?
C15 C16 1.368(9) . ?
C15 H15 0.9300 . ?
C16 C17 1.401(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.370(7) . ?
C17 H17 0.9300 . ?
C18 O4 1.384(6) . ?
C18 C19 1.397(7) . ?
C19 O2 1.336(5) . ?
C20 O3 1.466(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O4 1.454(6) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 O5 1.3948(11) . ?
C22' O5' 1.3951(12) . ?
N3 N4 1.139(7) . ?
N4 N5 1.126(9) . ?
N6 N7 1.313(7) . ?
N6 Yb1 2.383(4) 2_565 ?
N7 N8 1.194(8) . ?
N9 N10 1.157(5) . ?
N10 N11 1.179(5) . ?
N11 Yb1 2.324(4) 2_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Yb1 O2 65.92(11) . . ?
O1 Yb1 N11 147.56(14) . 2_565 ?
O2 Yb1 N11 145.64(14) . 2_565 ?
O1 Yb1 N6 111.64(13) . . ?
O2 Yb1 N6 80.39(13) . . ?
N11 Yb1 N6 87.59(15) 2_565 . ?
O1 Yb1 N3 86.36(16) . . ?
O2 Yb1 N3 83.55(16) . . ?
N11 Yb1 N3 90.26(18) 2_565 . ?
N6 Yb1 N3 147.88(16) . . ?
O1 Yb1 N6 82.69(12) . 2_565 ?
O2 Yb1 N6 120.94(12) . 2_565 ?
N11 Yb1 N6 81.82(14) 2_565 2_565 ?
N6 Yb1 N6 66.11(17) . 2_565 ?
N3 Yb1 N6 145.06(17) . 2_565 ?
O1 Yb1 O3 66.16(10) . . ?
O2 Yb1 O3 126.98(11) . . ?
N11 Yb1 O3 82.10(14) 2_565 . ?
N6 Yb1 O3 138.95(13) . . ?
N3 Yb1 O3 72.10(15) . . ?
N6 Yb1 O3 73.11(13) 2_565 . ?
O1 Yb1 O4 127.43(11) . . ?
O2 Yb1 O4 65.37(10) . . ?
N11 Yb1 O4 80.74(13) 2_565 . ?
N6 Yb1 O4 78.25(13) . . ?
N3 Yb1 O4 69.79(15) . . ?
N6 Yb1 O4 140.74(13) 2_565 . ?
O3 Yb1 O4 137.85(11) . . ?
O1 Yb1 Cu1 33.23(7) . . ?
O2 Yb1 Cu1 33.28(8) . . ?
N11 Yb1 Cu1 178.57(11) 2_565 . ?
N6 Yb1 Cu1 92.88(10) . . ?
N3 Yb1 Cu1 88.63(14) . . ?
N6 Yb1 Cu1 99.60(10) 2_565 . ?
O3 Yb1 Cu1 98.41(8) . . ?
O4 Yb1 Cu1 98.03(8) . . ?
O1 Yb1 Yb1 98.08(8) . 2_565 ?
O2 Yb1 Yb1 102.25(8) . 2_565 ?
N11 Yb1 Yb1 83.64(11) 2_565 2_565 ?
N6 Yb1 Yb1 33.51(10) . 2_565 ?
N3 Yb1 Yb1 173.76(14) . 2_565 ?
N6 Yb1 Yb1 32.60(10) 2_565 2_565 ?
O3 Yb1 Yb1 105.60(8) . 2_565 ?
O4 Yb1 Yb1 110.34(8) . 2_565 ?
Cu1 Yb1 Yb1 97.49(2) . 2_565 ?
O2 Cu1 O1 78.54(12) . . ?
O2 Cu1 N2 92.85(15) . . ?
O1 Cu1 N2 168.54(15) . . ?
O2 Cu1 N1 169.81(15) . . ?
O1 Cu1 N1 91.73(15) . . ?
N2 Cu1 N1 96.38(17) . . ?
O2 Cu1 Yb1 39.88(8) . . ?
O1 Cu1 Yb1 39.40(8) . . ?
N2 Cu1 Yb1 132.71(12) . . ?
N1 Cu1 Yb1 130.84(12) . . ?
O1 C1 C6 123.5(4) . . ?
O1 C1 C2 118.2(4) . . ?
C6 C1 C2 118.3(4) . . ?
C3 C2 O3 124.4(4) . . ?
C3 C2 C1 121.2(5) . . ?
O3 C2 C1 114.3(4) . . ?
C2 C3 C4 120.4(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 119.6(5) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 120.8(5) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.6(4) . . ?
C5 C6 C7 117.5(4) . . ?
C1 C6 C7 122.8(4) . . ?
N1 C7 C6 128.3(5) . . ?
N1 C7 H7 115.9 . . ?
C6 C7 H7 115.9 . . ?
N1 C8 C9 114.1(4) . . ?
N1 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C8 C9 C12 110.4(5) . . ?
C8 C9 C11 112.7(6) . . ?
C12 C9 C11 110.9(6) . . ?
C8 C9 C10 106.7(5) . . ?
C12 C9 C10 107.6(5) . . ?
C11 C9 C10 108.3(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 115.6(4) . . ?
N2 C12 H12A 108.4 . . ?
C9 C12 H12A 108.4 . . ?
N2 C12 H12B 108.4 . . ?
C9 C12 H12B 108.4 . . ?
H12A C12 H12B 107.5 . . ?
N2 C13 C14 128.9(4) . . ?
N2 C13 H13 115.5 . . ?
C14 C13 H13 115.5 . . ?
C15 C14 C19 118.9(5) . . ?
C15 C14 C13 117.8(5) . . ?
C19 C14 C13 123.3(4) . . ?
C16 C15 C14 121.7(5) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C15 C16 C17 118.9(5) . . ?
C15 C16 H16 120.6 . . ?
C17 C16 H16 120.6 . . ?
C18 C17 C16 120.7(5) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 O4 124.4(5) . . ?
C17 C18 C19 121.5(5) . . ?
O4 C18 C19 114.1(4) . . ?
O2 C19 C18 119.1(4) . . ?
O2 C19 C14 122.6(4) . . ?
C18 C19 C14 118.3(4) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 N1 C8 116.2(4) . . ?
C7 N1 Cu1 124.1(3) . . ?
C8 N1 Cu1 119.7(4) . . ?
C13 N2 C12 115.9(4) . . ?
C13 N2 Cu1 123.1(3) . . ?
C12 N2 Cu1 120.9(4) . . ?
N4 N3 Yb1 138.9(5) . . ?
N5 N4 N3 179.2(11) . . ?
N7 N6 Yb1 121.0(3) . . ?
N7 N6 Yb1 122.4(3) . 2_565 ?
Yb1 N6 Yb1 113.89(17) . 2_565 ?
N8 N7 N6 179.0(7) . . ?
N9 N10 N11 178.3(5) . . ?
N10 N11 Yb1 135.8(3) . 2_565 ?
C1 O1 Cu1 127.2(3) . . ?
C1 O1 Yb1 124.4(3) . . ?
Cu1 O1 Yb1 107.38(12) . . ?
C19 O2 Cu1 126.4(3) . . ?
C19 O2 Yb1 124.3(3) . . ?
Cu1 O2 Yb1 106.84(13) . . ?
C2 O3 C20 116.3(4) . . ?
C2 O3 Yb1 116.5(2) . . ?
C20 O3 Yb1 126.0(3) . . ?
C18 O4 C21 114.8(4) . . ?
C18 O4 Yb1 116.6(3) . . ?
C21 O4 Yb1 121.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_CuSmvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060764'
_audit_update_record             
;
2017-04-26 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuSmvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Cu2 N22 O14 Sm2'
_chemical_formula_weight         1609.06

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'
Cu Cu 0.3201 1.2651 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c '

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

_cell_length_a                   15.427(2)
_cell_length_b                   13.0451(17)
_cell_length_c                   34.166(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.601(8)
_cell_angle_gamma                90.00
_cell_volume                     6392.9(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5911
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      24.72

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3232
_exptl_absorpt_coefficient_mu    2.543
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.3352
_exptl_absorpt_correction_T_max  0.7501
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41203
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.00
_reflns_number_total             11012
_reflns_number_gt                7966
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0345P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11012
_refine_ls_number_parameters     797
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0855
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.67914(2) -0.76440(2) -0.043853(8) 0.03628(9) Uani 1 1 d . . .
Sm2 Sm 0.56977(2) -0.64062(2) -0.157410(8) 0.03490(9) Uani 1 1 d . . .
Cu1 Cu 0.78854(5) -0.56294(5) 0.02709(2) 0.04422(18) Uani 1 1 d . . .
Cu2 Cu 0.47609(5) -0.39105(5) -0.15462(2) 0.04023(17) Uani 1 1 d . . .
O1 O 0.8221(3) -0.6722(3) -0.00415(10) 0.0410(9) Uani 1 1 d . . .
O2 O 0.6670(2) -0.6333(2) 0.00283(10) 0.0361(8) Uani 1 1 d . . .
O3 O 0.8370(3) -0.8430(3) -0.03947(12) 0.0546(11) Uani 1 1 d . . .
O4 O 0.5445(3) -0.7827(3) -0.01343(10) 0.0443(9) Uani 1 1 d . . .
O5 O 0.5913(2) -0.4566(2) -0.15294(10) 0.0361(8) Uani 1 1 d . . .
O6 O 0.4362(2) -0.5355(2) -0.16223(10) 0.0385(9) Uani 1 1 d . . .
O7 O 0.7161(3) -0.5739(3) -0.16626(12) 0.0503(10) Uani 1 1 d . . .
O8 O 0.4098(3) -0.7225(3) -0.19371(11) 0.0485(10) Uani 1 1 d . . .
O9 O 0.7494(3) -0.8372(3) 0.02875(11) 0.0593(12) Uani 1 1 d . . .
H9 H 0.7724 -0.7887 0.0492 0.089 Uiso 1 1 d R . .
O10 O 0.5062(3) -0.5632(3) -0.22896(10) 0.0583(11) Uani 1 1 d . . .
H10 H 0.4872 -0.5171 -0.2284 0.087 Uiso 1 1 d R . .
N1 N 0.6822(3) -0.6036(4) -0.08466(13) 0.0489(13) Uani 1 1 d . . .
N2 N 0.7238(4) -0.5300(4) -0.06857(15) 0.0593(10) Uani 1 1 d . . .
N3 N 0.7638(4) -0.4592(4) -0.05184(15) 0.0593(10) Uani 1 1 d . . .
N4 N 0.6668(3) -0.7954(4) -0.11972(13) 0.0490(13) Uani 1 1 d . . .
N5 N 0.6490(4) -0.8792(4) -0.13529(15) 0.0633(16) Uani 1 1 d . . .
N6 N 0.6324(6) -0.9600(4) -0.14970(18) 0.104(3) Uani 1 1 d . . .
N7 N 0.5203(4) -0.7179(4) -0.10003(14) 0.0514(13) Uani 1 1 d . . .
N8 N 0.4426(5) -0.7443(4) -0.10446(14) 0.0509(13) Uani 1 1 d . . .
N9 N 0.3676(5) -0.7677(5) -0.10854(18) 0.0779(18) Uani 1 1 d . . .
N10 N 0.6407(4) -0.9423(4) -0.05361(15) 0.0597(14) Uani 1 1 d . . .
N11 N 0.6629(3) -1.0289(4) -0.04619(16) 0.0516(13) Uani 1 1 d . . .
N12 N 0.6849(4) -1.1127(5) -0.0390(2) 0.090(2) Uani 1 1 d . . .
N13 N 0.5904(4) -0.7573(4) -0.21020(14) 0.0605(15) Uani 1 1 d . . .
N14 N 0.5762(3) -0.8121(3) -0.23890(13) 0.0448(12) Uani 1 1 d . . .
N15 N 0.5621(4) -0.8661(4) -0.26762(14) 0.0617(15) Uani 1 1 d . . .
N16 N 0.8219(4) -0.6798(4) 0.08693(17) 0.0620(14) Uani 1 1 d U . .
N17 N 0.8733(5) -0.6817(5) 0.1164(2) 0.0795(16) Uani 1 1 d U . .
N18 N 0.9319(6) -0.6813(7) 0.1535(3) 0.127(3) Uani 1 1 d U . .
N19 N 0.9165(4) -0.5045(4) 0.04699(14) 0.0519(13) Uani 1 1 d . . .
N20 N 0.7312(4) -0.4475(3) 0.04541(13) 0.0494(13) Uani 1 1 d . . .
N21 N 0.5366(4) -0.2552(3) -0.14034(13) 0.0428(12) Uani 1 1 d . . .
N22 N 0.3552(3) -0.3476(3) -0.15330(14) 0.0447(12) Uani 1 1 d . . .
C1 C 0.9073(4) -0.7100(4) 0.00701(16) 0.0433(14) Uani 1 1 d . . .
C2 C 0.9198(5) -0.8034(5) -0.01119(18) 0.0528(16) Uani 1 1 d . . .
C3 C 1.0075(5) -0.8474(5) -0.0008(2) 0.0680(19) Uani 1 1 d . . .
H3 H 1.0139 -0.9090 -0.0131 0.082 Uiso 1 1 calc R . .
C4 C 1.0843(5) -0.8005(6) 0.0275(2) 0.075(2) Uani 1 1 d . . .
H4 H 1.1429 -0.8301 0.0346 0.090 Uiso 1 1 calc R . .
C5 C 1.0742(5) -0.7102(6) 0.0452(2) 0.070(2) Uani 1 1 d . . .
H5 H 1.1266 -0.6789 0.0646 0.084 Uiso 1 1 calc R . .
C6 C 0.9871(4) -0.6628(5) 0.03505(17) 0.0483(15) Uani 1 1 d . . .
C7 C 0.9867(5) -0.5596(5) 0.05034(18) 0.0571(17) Uani 1 1 d . . .
H7 H 1.0448 -0.5301 0.0643 0.069 Uiso 1 1 calc R . .
C8 C 0.9355(5) -0.3949(5) 0.0588(2) 0.071(2) Uani 1 1 d . . .
H8A H 0.9264 -0.3559 0.0334 0.085 Uiso 1 1 calc R . .
H8B H 1.0006 -0.3884 0.0769 0.085 Uiso 1 1 calc R . .
C9 C 0.8771(5) -0.3465(5) 0.0810(2) 0.068(2) Uani 1 1 d . . .
C10 C 0.8925(6) -0.4011(6) 0.1226(2) 0.092(3) Uani 1 1 d . . .
H10A H 0.8524 -0.3717 0.1354 0.138 Uiso 1 1 calc R . .
H10B H 0.9563 -0.3934 0.1411 0.138 Uiso 1 1 calc R . .
H10C H 0.8783 -0.4727 0.1173 0.138 Uiso 1 1 calc R . .
C11 C 0.9089(6) -0.2338(5) 0.0891(3) 0.103(3) Uani 1 1 d . . .
H11A H 0.9024 -0.2014 0.0630 0.154 Uiso 1 1 calc R . .
H11B H 0.9729 -0.2313 0.1078 0.154 Uiso 1 1 calc R . .
H11C H 0.8710 -0.1984 0.1017 0.154 Uiso 1 1 calc R . .
C12 C 0.7757(5) -0.3464(5) 0.0528(2) 0.0645(19) Uani 1 1 d . . .
H12A H 0.7421 -0.3023 0.0652 0.077 Uiso 1 1 calc R . .
H12B H 0.7699 -0.3170 0.0259 0.077 Uiso 1 1 calc R . .
C13 C 0.6549(5) -0.4560(4) 0.05261(16) 0.0479(15) Uani 1 1 d . . .
H13 H 0.6377 -0.3994 0.0647 0.057 Uiso 1 1 calc R . .
C14 C 0.5940(4) -0.5427(4) 0.04407(15) 0.0422(14) Uani 1 1 d . . .
C15 C 0.5191(5) -0.5384(5) 0.05814(16) 0.0506(16) Uani 1 1 d . . .
H15 H 0.5138 -0.4821 0.0738 0.061 Uiso 1 1 calc R . .
C16 C 0.4544(5) -0.6142(5) 0.04946(17) 0.0531(16) Uani 1 1 d . . .
H16 H 0.4057 -0.6102 0.0593 0.064 Uiso 1 1 calc R . .
C17 C 0.4621(4) -0.6978(4) 0.02572(16) 0.0486(15) Uani 1 1 d . . .
H17 H 0.4183 -0.7503 0.0197 0.058 Uiso 1 1 calc R . .
C18 C 0.5343(4) -0.7036(4) 0.01095(15) 0.0395(14) Uani 1 1 d . . .
C19 C 0.6014(4) -0.6255(4) 0.01939(15) 0.0361(13) Uani 1 1 d . . .
C20 C 0.8462(5) -0.9288(5) -0.0637(2) 0.074(2) Uani 1 1 d . . .
H20A H 0.8809 -0.9087 -0.0807 0.111 Uiso 1 1 calc R . .
H20B H 0.7854 -0.9520 -0.0816 0.111 Uiso 1 1 calc R . .
H20C H 0.8784 -0.9832 -0.0451 0.111 Uiso 1 1 calc R . .
C21 C 0.4877(5) -0.8707(4) -0.0169(2) 0.070(2) Uani 1 1 d . . .
H21A H 0.5006 -0.8995 0.0105 0.104 Uiso 1 1 calc R . .
H21B H 0.5009 -0.9207 -0.0346 0.104 Uiso 1 1 calc R . .
H21C H 0.4232 -0.8514 -0.0290 0.104 Uiso 1 1 calc R . .
C22 C 0.6638(4) -0.4106(4) -0.15703(15) 0.0385(13) Uani 1 1 d . . .
C23 C 0.7315(4) -0.4689(5) -0.16460(16) 0.0477(15) Uani 1 1 d . . .
C24 C 0.8076(5) -0.4266(6) -0.1697(2) 0.0638(18) Uani 1 1 d . . .
H24 H 0.8507 -0.4682 -0.1752 0.077 Uiso 1 1 calc R . .
C25 C 0.8201(5) -0.3215(6) -0.1668(2) 0.076(2) Uani 1 1 d . . .
H25 H 0.8718 -0.2918 -0.1701 0.091 Uiso 1 1 calc R . .
C26 C 0.7562(5) -0.2622(5) -0.1589(2) 0.0655(19) Uani 1 1 d . . .
H26 H 0.7652 -0.1916 -0.1566 0.079 Uiso 1 1 calc R . .
C27 C 0.6764(4) -0.3040(4) -0.15395(17) 0.0460(15) Uani 1 1 d . . .
C28 C 0.6162(5) -0.2368(4) -0.14270(17) 0.0499(16) Uani 1 1 d . . .
H28 H 0.6379 -0.1701 -0.1361 0.060 Uiso 1 1 calc R . .
C29 C 0.4959(5) -0.1696(4) -0.12473(19) 0.0605(18) Uani 1 1 d . . .
H29A H 0.5236 -0.1063 -0.1294 0.073 Uiso 1 1 calc R . .
H29B H 0.5134 -0.1777 -0.0946 0.073 Uiso 1 1 calc R . .
C30 C 0.3906(5) -0.1591(4) -0.14444(19) 0.0613(18) Uani 1 1 d . . .
C31 C 0.3645(6) -0.0658(5) -0.1233(2) 0.090(3) Uani 1 1 d . . .
H31A H 0.3860 -0.0767 -0.0934 0.135 Uiso 1 1 calc R . .
H31B H 0.2980 -0.0574 -0.1343 0.135 Uiso 1 1 calc R . .
H31C H 0.3932 -0.0053 -0.1290 0.135 Uiso 1 1 calc R . .
C32 C 0.3551(5) -0.1440(5) -0.19189(18) 0.071(2) Uani 1 1 d . . .
H32A H 0.3855 -0.0858 -0.1984 0.106 Uiso 1 1 calc R . .
H32B H 0.2890 -0.1325 -0.2023 0.106 Uiso 1 1 calc R . .
H32C H 0.3683 -0.2041 -0.2049 0.106 Uiso 1 1 calc R . .
C33 C 0.3435(5) -0.2514(4) -0.13334(19) 0.0603(18) Uani 1 1 d . . .
H33A H 0.3688 -0.2604 -0.1030 0.072 Uiso 1 1 calc R . .
H33B H 0.2774 -0.2372 -0.1417 0.072 Uiso 1 1 calc R . .
C34 C 0.2810(5) -0.4017(5) -0.16971(18) 0.0546(16) Uani 1 1 d . . .
H34 H 0.2262 -0.3730 -0.1693 0.066 Uiso 1 1 calc R . .
C35 C 0.2729(4) -0.5017(5) -0.18860(18) 0.0497(15) Uani 1 1 d . . .
C36 C 0.1819(5) -0.5365(6) -0.2117(2) 0.075(2) Uani 1 1 d . . .
H36 H 0.1311 -0.4945 -0.2148 0.090 Uiso 1 1 calc R . .
C37 C 0.1682(6) -0.6315(6) -0.2294(3) 0.090(3) Uani 1 1 d . . .
H37 H 0.1080 -0.6533 -0.2452 0.108 Uiso 1 1 calc R . .
C38 C 0.2429(5) -0.6960(5) -0.2243(2) 0.0677(19) Uani 1 1 d . . .
H38 H 0.2330 -0.7609 -0.2364 0.081 Uiso 1 1 calc R . .
C39 C 0.3312(4) -0.6634(4) -0.20131(17) 0.0468(15) Uani 1 1 d . . .
C40 C 0.3488(4) -0.5643(4) -0.18350(16) 0.0391(13) Uani 1 1 d . . .
C41 C 0.7890(5) -0.6401(6) -0.1671(3) 0.097(3) Uani 1 1 d . . .
H41A H 0.7940 -0.6364 -0.1942 0.146 Uiso 1 1 calc R . .
H41B H 0.7751 -0.7093 -0.1618 0.146 Uiso 1 1 calc R . .
H41C H 0.8468 -0.6193 -0.1458 0.146 Uiso 1 1 calc R . .
C42 C 0.3958(5) -0.8291(5) -0.2037(2) 0.074(2) Uani 1 1 d . . .
H42A H 0.3528 -0.8567 -0.1920 0.111 Uiso 1 1 calc R . .
H42B H 0.4543 -0.8646 -0.1920 0.111 Uiso 1 1 calc R . .
H42C H 0.3710 -0.8376 -0.2337 0.111 Uiso 1 1 calc R . .
C43 C 0.7730(7) -0.9334(6) 0.0470(2) 0.114(3) Uani 1 1 d . . .
H43A H 0.8029 -0.9262 0.0770 0.171 Uiso 1 1 calc R . .
H43B H 0.8148 -0.9665 0.0360 0.171 Uiso 1 1 calc R . .
H43C H 0.7177 -0.9741 0.0407 0.171 Uiso 1 1 calc R . .
C44 C 0.4452(5) -0.6030(5) -0.26804(17) 0.073(2) Uani 1 1 d . . .
H44A H 0.4609 -0.5744 -0.2905 0.110 Uiso 1 1 calc R . .
H44B H 0.3821 -0.5854 -0.2720 0.110 Uiso 1 1 calc R . .
H44C H 0.4513 -0.6763 -0.2680 0.110 Uiso 1 1 calc R . .
O11 O -0.0084(11) -0.1004(9) -0.1287(7) 0.416(14) Uani 1 1 d . . .
C45 C 0.0039(13) -0.0087(15) -0.1217(8) 0.297(11) Uani 1 1 d . . .
O12 O -0.0849(19) -0.4507(18) -0.3062(8) 0.468(14) Uani 1 1 d . . .
C46 C -0.110(3) -0.436(3) -0.2694(18) 0.61(4) Uani 1 1 d . . .
O13 O 0.0786(10) -0.1988(17) -0.2238(6) 0.391(13) Uani 1 1 d . . .
C47 C 0.0887(18) -0.219(3) -0.2604(8) 0.368(19) Uani 1 1 d . . .
C48 C 0.2018(9) -0.4210(13) -0.3030(6) 0.227(9) Uani 1 1 d . . .
O14 O 0.1195(9) -0.3758(10) -0.3243(4) 0.267(6) Uani 1 1 d . . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 N10 2.389(5) . ?
Sm1 O2 2.393(3) . ?
Sm1 O1 2.438(4) . ?
Sm1 O9 2.500(4) . ?
Sm1 N1 2.528(4) . ?
Sm1 N4 2.560(4) . ?
Sm1 N7 2.568(5) . ?
Sm1 O3 2.596(4) . ?
Sm1 O4 2.653(4) . ?
Sm1 Cu1 3.5523(8) . ?
Sm1 Sm2 3.9607(6) . ?
Sm2 O5 2.420(3) . ?
Sm2 O6 2.429(3) . ?
Sm2 N13 2.469(5) . ?
Sm2 O10 2.488(3) . ?
Sm2 N1 2.499(4) . ?
Sm2 O7 2.539(4) . ?
Sm2 O8 2.552(4) . ?
Sm2 N7 2.558(5) . ?
Sm2 N4 2.560(4) . ?
Sm2 Cu2 3.5775(8) . ?
Cu1 O1 1.961(3) . ?
Cu1 N20 1.962(5) . ?
Cu1 O2 1.975(3) . ?
Cu1 N19 1.988(5) . ?
Cu1 N16 2.449(5) . ?
Cu2 O5 1.955(3) . ?
Cu2 N22 1.965(5) . ?
Cu2 O6 1.970(3) . ?
Cu2 N21 1.978(4) . ?
O1 C1 1.323(6) . ?
O2 C19 1.332(6) . ?
O3 C2 1.386(7) . ?
O3 C20 1.429(6) . ?
O4 C18 1.371(6) . ?
O4 C21 1.422(6) . ?
O5 C22 1.321(6) . ?
O6 C40 1.329(6) . ?
O7 C23 1.388(6) . ?
O7 C41 1.426(7) . ?
O8 C39 1.379(7) . ?
O8 C42 1.428(6) . ?
O9 C43 1.389(7) . ?
O9 H9 0.9124 . ?
O10 C44 1.419(7) . ?
O10 H10 0.6732 . ?
N1 N2 1.174(6) . ?
N2 N3 1.140(6) . ?
N4 N5 1.203(6) . ?
N5 N6 1.152(7) . ?
N7 N8 1.201(7) . ?
N8 N9 1.155(7) . ?
N10 N11 1.180(6) . ?
N11 N12 1.145(7) . ?
N13 N14 1.167(6) . ?
N14 N15 1.162(6) . ?
N16 N17 1.027(7) . ?
N17 N18 1.258(9) . ?
N19 C7 1.269(7) . ?
N19 C8 1.485(7) . ?
N20 C13 1.292(7) . ?
N20 C12 1.465(7) . ?
N21 C28 1.282(7) . ?
N21 C29 1.474(7) . ?
N22 C34 1.285(7) . ?
N22 C33 1.471(7) . ?
C1 C6 1.394(8) . ?
C1 C2 1.412(8) . ?
C2 C3 1.390(9) . ?
C3 C4 1.368(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.359(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.402(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.445(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.511(9) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C12 1.505(9) . ?
C9 C10 1.529(9) . ?
C9 C11 1.543(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.430(7) . ?
C13 H13 0.9300 . ?
C14 C19 1.400(7) . ?
C14 C15 1.407(8) . ?
C15 C16 1.358(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.391(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.383(7) . ?
C17 H17 0.9300 . ?
C18 C19 1.406(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.391(8) . ?
C22 C27 1.403(7) . ?
C23 C24 1.365(8) . ?
C24 C25 1.383(9) . ?
C24 H24 0.9300 . ?
C25 C26 1.356(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.411(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.429(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.519(9) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C32 1.521(8) . ?
C30 C33 1.524(8) . ?
C30 C31 1.543(8) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 C35 1.440(8) . ?
C34 H34 0.9300 . ?
C35 C40 1.385(8) . ?
C35 C36 1.408(9) . ?
C36 C37 1.362(9) . ?
C36 H36 0.9300 . ?
C37 C38 1.385(10) . ?
C37 H37 0.9300 . ?
C38 C39 1.366(8) . ?
C38 H38 0.9300 . ?
C39 C40 1.412(7) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
O11 C45 1.221(17) . ?
O12 C46 1.46(4) . ?
O13 C47 1.34(3) . ?
C48 O14 1.345(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
N10 Sm1 O2 135.34(14) . . ?
N10 Sm1 O1 133.18(16) . . ?
O2 Sm1 O1 63.47(11) . . ?
N10 Sm1 O9 76.35(15) . . ?
O2 Sm1 O9 73.86(12) . . ?
O1 Sm1 O9 70.27(12) . . ?
N10 Sm1 N1 141.55(15) . . ?
O2 Sm1 N1 78.26(13) . . ?
O1 Sm1 N1 72.60(13) . . ?
O9 Sm1 N1 140.62(14) . . ?
N10 Sm1 N4 77.49(15) . . ?
O2 Sm1 N4 142.45(13) . . ?
O1 Sm1 N4 110.86(14) . . ?
O9 Sm1 N4 142.00(14) . . ?
N1 Sm1 N4 65.30(14) . . ?
N10 Sm1 N7 90.33(17) . . ?
O2 Sm1 N7 92.40(14) . . ?
O1 Sm1 N7 135.87(14) . . ?
O9 Sm1 N7 141.02(15) . . ?
N1 Sm1 N7 66.30(15) . . ?
N4 Sm1 N7 65.52(15) . . ?
N10 Sm1 O3 78.69(16) . . ?
O2 Sm1 O3 123.09(12) . . ?
O1 Sm1 O3 61.68(12) . . ?
O9 Sm1 O3 74.79(13) . . ?
N1 Sm1 O3 98.74(14) . . ?
N4 Sm1 O3 73.42(13) . . ?
N7 Sm1 O3 138.90(14) . . ?
N10 Sm1 O4 77.12(14) . . ?
O2 Sm1 O4 62.51(11) . . ?
O1 Sm1 O4 120.29(11) . . ?
O9 Sm1 O4 72.14(13) . . ?
N1 Sm1 O4 117.83(14) . . ?
N4 Sm1 O4 127.24(14) . . ?
N7 Sm1 O4 69.20(14) . . ?
O3 Sm1 O4 142.65(12) . . ?
N10 Sm1 Cu1 147.72(12) . . ?
O2 Sm1 Cu1 31.83(8) . . ?
O1 Sm1 Cu1 31.82(8) . . ?
O9 Sm1 Cu1 71.37(9) . . ?
N1 Sm1 Cu1 70.24(10) . . ?
N4 Sm1 Cu1 130.32(11) . . ?
N7 Sm1 Cu1 114.71(11) . . ?
O3 Sm1 Cu1 93.03(9) . . ?
O4 Sm1 Cu1 92.47(7) . . ?
N10 Sm1 Sm2 105.37(12) . . ?
O2 Sm1 Sm2 104.59(8) . . ?
O1 Sm1 Sm2 108.40(8) . . ?
O9 Sm1 Sm2 178.27(9) . . ?
N1 Sm1 Sm2 37.76(10) . . ?
N4 Sm1 Sm2 39.32(10) . . ?
N7 Sm1 Sm2 39.31(11) . . ?
O3 Sm1 Sm2 105.66(8) . . ?
O4 Sm1 Sm2 107.93(8) . . ?
Cu1 Sm1 Sm2 106.906(16) . . ?
O5 Sm2 O6 62.48(11) . . ?
O5 Sm2 N13 127.29(14) . . ?
O6 Sm2 N13 129.26(15) . . ?
O5 Sm2 O10 69.81(11) . . ?
O6 Sm2 O10 71.75(12) . . ?
N13 Sm2 O10 69.06(14) . . ?
O5 Sm2 N1 73.55(13) . . ?
O6 Sm2 N1 102.66(14) . . ?
N13 Sm2 N1 128.08(17) . . ?
O10 Sm2 N1 140.98(14) . . ?
O5 Sm2 O7 63.91(12) . . ?
O6 Sm2 O7 124.57(12) . . ?
N13 Sm2 O7 76.39(15) . . ?
O10 Sm2 O7 77.88(13) . . ?
N1 Sm2 O7 74.36(14) . . ?
O5 Sm2 O8 122.12(12) . . ?
O6 Sm2 O8 63.86(12) . . ?
N13 Sm2 O8 75.44(16) . . ?
O10 Sm2 O8 74.44(13) . . ?
N1 Sm2 O8 139.20(13) . . ?
O7 Sm2 O8 145.93(12) . . ?
O5 Sm2 N7 114.52(13) . . ?
O6 Sm2 N7 77.84(14) . . ?
N13 Sm2 N7 118.19(16) . . ?
O10 Sm2 N7 142.37(16) . . ?
N1 Sm2 N7 66.88(16) . . ?
O7 Sm2 N7 139.07(15) . . ?
O8 Sm2 N7 72.53(15) . . ?
O5 Sm2 N4 135.15(14) . . ?
O6 Sm2 N4 143.45(13) . . ?
N13 Sm2 N4 70.88(15) . . ?
O10 Sm2 N4 139.47(13) . . ?
N1 Sm2 N4 65.72(15) . . ?
O7 Sm2 N4 87.09(14) . . ?
O8 Sm2 N4 101.30(14) . . ?
N7 Sm2 N4 65.68(15) . . ?
O5 Sm2 Cu2 31.05(8) . . ?
O6 Sm2 Cu2 31.50(8) . . ?
N13 Sm2 Cu2 137.95(11) . . ?
O10 Sm2 Cu2 68.89(8) . . ?
N1 Sm2 Cu2 86.39(11) . . ?
O7 Sm2 Cu2 94.41(9) . . ?
O8 Sm2 Cu2 93.80(9) . . ?
N7 Sm2 Cu2 95.78(11) . . ?
N4 Sm2 Cu2 150.61(10) . . ?
O5 Sm2 Sm1 110.08(8) . . ?
O6 Sm2 Sm1 109.96(7) . . ?
N13 Sm2 Sm1 109.96(11) . . ?
O10 Sm2 Sm1 178.10(10) . . ?
N1 Sm2 Sm1 38.28(10) . . ?
O7 Sm2 Sm1 100.34(9) . . ?
O8 Sm2 Sm1 107.00(8) . . ?
N7 Sm2 Sm1 39.50(12) . . ?
N4 Sm2 Sm1 39.33(9) . . ?
Cu2 Sm2 Sm1 112.059(13) . . ?
O1 Cu1 N20 166.36(17) . . ?
O1 Cu1 O2 80.43(14) . . ?
N20 Cu1 O2 91.17(18) . . ?
O1 Cu1 N19 92.14(19) . . ?
N20 Cu1 N19 96.0(2) . . ?
O2 Cu1 N19 172.53(18) . . ?
O1 Cu1 N16 89.15(16) . . ?
N20 Cu1 N16 101.10(18) . . ?
O2 Cu1 N16 86.34(16) . . ?
N19 Cu1 N16 94.4(2) . . ?
O1 Cu1 Sm1 40.98(11) . . ?
N20 Cu1 Sm1 128.95(15) . . ?
O2 Cu1 Sm1 39.71(9) . . ?
N19 Cu1 Sm1 132.82(15) . . ?
N16 Cu1 Sm1 90.57(13) . . ?
O5 Cu2 N22 170.37(16) . . ?
O5 Cu2 O6 79.72(14) . . ?
N22 Cu2 O6 91.49(18) . . ?
O5 Cu2 N21 92.46(18) . . ?
N22 Cu2 N21 95.9(2) . . ?
O6 Cu2 N21 170.23(18) . . ?
O5 Cu2 Sm2 39.69(10) . . ?
N22 Cu2 Sm2 131.22(14) . . ?
O6 Cu2 Sm2 40.13(10) . . ?
N21 Cu2 Sm2 131.51(15) . . ?
C1 O1 Cu1 123.2(3) . . ?
C1 O1 Sm1 125.2(3) . . ?
Cu1 O1 Sm1 107.20(16) . . ?
C19 O2 Cu1 122.6(3) . . ?
C19 O2 Sm1 126.6(3) . . ?
Cu1 O2 Sm1 108.46(15) . . ?
C2 O3 C20 115.7(5) . . ?
C2 O3 Sm1 119.8(3) . . ?
C20 O3 Sm1 124.5(4) . . ?
C18 O4 C21 116.9(4) . . ?
C18 O4 Sm1 116.9(3) . . ?
C21 O4 Sm1 125.9(3) . . ?
C22 O5 Cu2 126.4(3) . . ?
C22 O5 Sm2 123.1(3) . . ?
Cu2 O5 Sm2 109.27(15) . . ?
C40 O6 Cu2 123.2(3) . . ?
C40 O6 Sm2 122.8(3) . . ?
Cu2 O6 Sm2 108.38(15) . . ?
C23 O7 C41 118.3(5) . . ?
C23 O7 Sm2 118.7(3) . . ?
C41 O7 Sm2 122.4(4) . . ?
C39 O8 C42 117.0(5) . . ?
C39 O8 Sm2 118.9(3) . . ?
C42 O8 Sm2 123.9(4) . . ?
C43 O9 Sm1 137.3(4) . . ?
C43 O9 H9 108.6 . . ?
Sm1 O9 H9 113.6 . . ?
C44 O10 Sm2 131.4(4) . . ?
C44 O10 H10 102.0 . . ?
Sm2 O10 H10 110.7 . . ?
N2 N1 Sm2 133.1(4) . . ?
N2 N1 Sm1 122.6(4) . . ?
Sm2 N1 Sm1 103.96(17) . . ?
N3 N2 N1 177.9(6) . . ?
N5 N4 Sm2 119.9(4) . . ?
N5 N4 Sm1 120.7(4) . . ?
Sm2 N4 Sm1 101.35(15) . . ?
N6 N5 N4 179.1(6) . . ?
N8 N7 Sm2 125.6(4) . . ?
N8 N7 Sm1 131.2(4) . . ?
Sm2 N7 Sm1 101.2(2) . . ?
N9 N8 N7 178.6(7) . . ?
N11 N10 Sm1 149.5(5) . . ?
N12 N11 N10 179.7(7) . . ?
N14 N13 Sm2 163.0(5) . . ?
N15 N14 N13 179.5(6) . . ?
N17 N16 Cu1 133.0(6) . . ?
N16 N17 N18 175.6(8) . . ?
C7 N19 C8 116.4(5) . . ?
C7 N19 Cu1 121.3(4) . . ?
C8 N19 Cu1 122.3(4) . . ?
C13 N20 C12 116.5(5) . . ?
C13 N20 Cu1 123.0(4) . . ?
C12 N20 Cu1 120.5(4) . . ?
C28 N21 C29 115.2(5) . . ?
C28 N21 Cu2 121.9(4) . . ?
C29 N21 Cu2 122.8(4) . . ?
C34 N22 C33 115.4(5) . . ?
C34 N22 Cu2 122.1(4) . . ?
C33 N22 Cu2 122.4(4) . . ?
O1 C1 C6 124.5(5) . . ?
O1 C1 C2 118.4(5) . . ?
C6 C1 C2 117.1(6) . . ?
O3 C2 C3 125.7(6) . . ?
O3 C2 C1 112.9(5) . . ?
C3 C2 C1 121.4(6) . . ?
C4 C3 C2 120.3(7) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 119.4(7) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 121.9(7) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C5 119.9(6) . . ?
C1 C6 C7 122.7(6) . . ?
C5 C6 C7 116.9(6) . . ?
N19 C7 C6 127.8(6) . . ?
N19 C7 H7 116.1 . . ?
C6 C7 H7 116.1 . . ?
N19 C8 C9 116.4(5) . . ?
N19 C8 H8A 108.2 . . ?
C9 C8 H8A 108.2 . . ?
N19 C8 H8B 108.2 . . ?
C9 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?
C12 C9 C8 110.6(5) . . ?
C12 C9 C10 111.3(6) . . ?
C8 C9 C10 110.7(6) . . ?
C12 C9 C11 107.5(6) . . ?
C8 C9 C11 106.3(6) . . ?
C10 C9 C11 110.3(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N20 C12 C9 114.9(5) . . ?
N20 C12 H12A 108.5 . . ?
C9 C12 H12A 108.5 . . ?
N20 C12 H12B 108.5 . . ?
C9 C12 H12B 108.5 . . ?
H12A C12 H12B 107.5 . . ?
N20 C13 C14 127.2(5) . . ?
N20 C13 H13 116.4 . . ?
C14 C13 H13 116.4 . . ?
C19 C14 C15 119.7(5) . . ?
C19 C14 C13 122.7(5) . . ?
C15 C14 C13 117.3(5) . . ?
C16 C15 C14 121.8(5) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C17 119.0(6) . . ?
C15 C16 H16 120.5 . . ?
C17 C16 H16 120.5 . . ?
C18 C17 C16 120.6(6) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
O4 C18 C17 123.5(5) . . ?
O4 C18 C19 115.4(5) . . ?
C17 C18 C19 121.1(5) . . ?
O2 C19 C14 123.9(5) . . ?
O2 C19 C18 118.3(5) . . ?
C14 C19 C18 117.8(5) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 C23 119.6(5) . . ?
O5 C22 C27 122.8(5) . . ?
C23 C22 C27 117.5(5) . . ?
C24 C23 O7 122.5(6) . . ?
C24 C23 C22 122.8(6) . . ?
O7 C23 C22 114.7(5) . . ?
C23 C24 C25 119.7(6) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C26 C25 C24 119.1(6) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C25 C26 C27 122.2(6) . . ?
C25 C26 H26 118.9 . . ?
C27 C26 H26 118.9 . . ?
C22 C27 C26 118.5(6) . . ?
C22 C27 C28 122.8(5) . . ?
C26 C27 C28 118.5(6) . . ?
N21 C28 C27 129.4(5) . . ?
N21 C28 H28 115.3 . . ?
C27 C28 H28 115.3 . . ?
N21 C29 C30 115.9(5) . . ?
N21 C29 H29A 108.3 . . ?
C30 C29 H29A 108.3 . . ?
N21 C29 H29B 108.3 . . ?
C30 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
C29 C30 C32 113.1(6) . . ?
C29 C30 C33 110.4(5) . . ?
C32 C30 C33 110.5(6) . . ?
C29 C30 C31 106.6(6) . . ?
C32 C30 C31 110.0(5) . . ?
C33 C30 C31 106.0(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N22 C33 C30 114.0(5) . . ?
N22 C33 H33A 108.7 . . ?
C30 C33 H33A 108.7 . . ?
N22 C33 H33B 108.7 . . ?
C30 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
N22 C34 C35 127.6(6) . . ?
N22 C34 H34 116.2 . . ?
C35 C34 H34 116.2 . . ?
C40 C35 C36 120.1(6) . . ?
C40 C35 C34 123.2(6) . . ?
C36 C35 C34 116.6(6) . . ?
C37 C36 C35 120.2(7) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C36 C37 C38 120.7(7) . . ?
C36 C37 H37 119.6 . . ?
C38 C37 H37 119.6 . . ?
C39 C38 C37 119.4(7) . . ?
C39 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
C38 C39 O8 123.8(6) . . ?
C38 C39 C40 121.7(6) . . ?
O8 C39 C40 114.5(5) . . ?
O6 C40 C35 122.8(5) . . ?
O6 C40 C39 119.3(5) . . ?
C35 C40 C39 117.8(5) . . ?
O7 C41 H41A 109.5 . . ?
O7 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O7 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O8 C42 H42A 109.5 . . ?
O8 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O8 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O9 C43 H43A 109.5 . . ?
O9 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O9 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O10 C44 H44A 109.5 . . ?
O10 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
O10 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.979
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.101
####################################################################### 
# 
# 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_CuGdvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060766'
_audit_update_record             
;
2017-04-26 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuGdvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43 H52 Cu2 Gd2 N22 O9'
_chemical_formula_weight         1462.65

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   22.246(5)
_cell_length_b                   9.670(2)
_cell_length_c                   26.064(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.768(3)
_cell_angle_gamma                90.00
_cell_volume                     5276(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9895
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.64

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2888
_exptl_absorpt_coefficient_mu    3.352
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5001
_exptl_absorpt_correction_T_max  0.6512
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX SMART'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            32954
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         27.64
_reflns_number_total             6130
_reflns_number_gt                5636
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0277P)²+9.9515P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6130
_refine_ls_number_parameters     353
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0645
_refine_ls_wR_factor_gt          0.0631
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.286879(6) 0.349335(14) 0.074547(6) 0.02536(5) Uani 1 1 d . . .
Cu1 Cu 0.443794(16) 0.23853(4) 0.101570(15) 0.02870(9) Uani 1 1 d . . .
C1 C 0.40911(14) 0.5301(3) 0.06817(12) 0.0298(6) Uani 1 1 d . . .
C2 C 0.36481(15) 0.6381(3) 0.05675(13) 0.0322(6) Uani 1 1 d . . .
C3 C 0.38008(17) 0.7687(3) 0.04342(14) 0.0405(8) Uani 1 1 d . . .
H3 H 0.3502 0.8396 0.0367 0.049 Uiso 1 1 calc R . .
C4 C 0.44026(18) 0.7939(4) 0.04008(16) 0.0474(9) Uani 1 1 d . . .
H4 H 0.4502 0.8806 0.0298 0.057 Uiso 1 1 calc R . .
C5 C 0.48446(18) 0.6906(4) 0.05205(16) 0.0459(8) Uani 1 1 d . . .
H5 H 0.5249 0.7082 0.0504 0.055 Uiso 1 1 calc R . .
C6 C 0.47023(15) 0.5583(3) 0.06676(13) 0.0359(7) Uani 1 1 d . . .
C7 C 0.52123(15) 0.4591(4) 0.08213(15) 0.0409(8) Uani 1 1 d . . .
H7 H 0.5599 0.4899 0.0800 0.049 Uiso 1 1 calc R . .
C8 C 0.58347(17) 0.2645(4) 0.11128(19) 0.0552(11) Uani 1 1 d . . .
H8A H 0.6169 0.3338 0.1230 0.066 Uiso 1 1 calc R . .
H8B H 0.5859 0.2226 0.0782 0.066 Uiso 1 1 calc R . .
C9 C 0.59658(15) 0.1549(3) 0.15463(14) 0.0348(7) Uani 1 1 d . . .
C10 C 0.66467(16) 0.1030(4) 0.16404(17) 0.0479(9) Uani 1 1 d . . .
H10A H 0.6669 0.0642 0.1308 0.072 Uiso 1 1 calc R . .
H10B H 0.6756 0.0335 0.1920 0.072 Uiso 1 1 calc R . .
H10C H 0.6941 0.1788 0.1752 0.072 Uiso 1 1 calc R . .
C11 C 0.59229(18) 0.2099(5) 0.20789(16) 0.0558(10) Uani 1 1 d . . .
H11A H 0.6240 0.2804 0.2220 0.084 Uiso 1 1 calc R . .
H11B H 0.5996 0.1358 0.2338 0.084 Uiso 1 1 calc R . .
H11C H 0.5506 0.2481 0.2015 0.084 Uiso 1 1 calc R . .
C12 C 0.55112(16) 0.0347(4) 0.13399(17) 0.0446(8) Uani 1 1 d . . .
H12A H 0.5487 0.0127 0.0970 0.054 Uiso 1 1 calc R . .
H12B H 0.5678 -0.0458 0.1565 0.054 Uiso 1 1 calc R . .
C13 C 0.46325(16) -0.0269(3) 0.15790(14) 0.0381(7) Uani 1 1 d . . .
H13 H 0.4885 -0.1044 0.1710 0.046 Uiso 1 1 calc R . .
C14 C 0.40259(15) -0.0242(3) 0.16621(13) 0.0350(7) Uani 1 1 d . . .
C15 C 0.38985(18) -0.1301(3) 0.19796(15) 0.0413(8) Uani 1 1 d . . .
H15 H 0.4197 -0.2002 0.2113 0.050 Uiso 1 1 calc R . .
C16 C 0.33425(19) -0.1322(4) 0.20974(15) 0.0447(8) Uani 1 1 d . . .
H16 H 0.3264 -0.2036 0.2305 0.054 Uiso 1 1 calc R . .
C17 C 0.28983(17) -0.0276(3) 0.19058(13) 0.0389(7) Uani 1 1 d . . .
H17 H 0.2523 -0.0279 0.1988 0.047 Uiso 1 1 calc R . .
C18 C 0.30142(15) 0.0767(3) 0.15931(12) 0.0308(6) Uani 1 1 d . . .
C19 C 0.35733(14) 0.0795(3) 0.14546(12) 0.0286(6) Uani 1 1 d . . .
C20 C 0.26935(18) 0.7121(4) 0.07231(15) 0.0433(8) Uani 1 1 d . . .
H20A H 0.2941 0.7491 0.1072 0.065 Uiso 1 1 calc R . .
H20B H 0.2299 0.6757 0.0740 0.065 Uiso 1 1 calc R . .
H20C H 0.2604 0.7840 0.0454 0.065 Uiso 1 1 calc R . .
C21 C 0.21317(19) 0.2135(4) 0.16399(17) 0.0533(10) Uani 1 1 d . . .
H21A H 0.1826 0.1395 0.1550 0.080 Uiso 1 1 calc R . .
H21B H 0.1919 0.2992 0.1504 0.080 Uiso 1 1 calc R . .
H21C H 0.2329 0.2191 0.2029 0.080 Uiso 1 1 calc R . .
N1 N 0.52095(12) 0.3343(3) 0.09834(12) 0.0359(6) Uani 1 1 d . . .
N2 N 0.48665(12) 0.0650(3) 0.13462(11) 0.0340(6) Uani 1 1 d . . .
N3 N 0.30982(17) 0.4685(3) 0.15849(13) 0.0517(8) Uani 1 1 d . . .
N4 N 0.31967(14) 0.4947(3) 0.20303(12) 0.0401(6) Uani 1 1 d . . .
N5 N 0.3293(2) 0.5256(5) 0.24801(15) 0.0800(13) Uani 1 1 d . . .
N6 N 0.27249(13) 0.3558(3) -0.02258(11) 0.0327(6) Uani 1 1 d . . .
N7 N 0.30416(14) 0.4304(3) -0.04139(12) 0.0426(7) Uani 1 1 d . . .
N8 N 0.3331(2) 0.5002(4) -0.05928(15) 0.0723(12) Uani 1 1 d . . .
N9 N 0.41854(15) 0.1484(3) 0.01223(13) 0.0465(7) Uani 1 1 d . . .
N10 N 0.36989(12) 0.1125(3) -0.01804(11) 0.0317(5) Uani 1 1 d . . .
N11 N 0.32185(13) 0.0739(3) -0.04937(12) 0.0430(7) Uani 1 1 d . . .
O1 O 0.39145(9) 0.4061(2) 0.07934(9) 0.0318(5) Uani 1 1 d . . .
O2 O 0.36514(10) 0.1827(2) 0.11470(9) 0.0313(4) Uani 1 1 d . . .
O3 O 0.30475(10) 0.6031(2) 0.05770(9) 0.0341(5) Uani 1 1 d . . .
O4 O 0.26108(10) 0.1878(2) 0.13963(9) 0.0351(5) Uani 1 1 d . . .
C22 C 0.5000 -0.4806(15) 0.2500 0.171(5) Uiso 1 2 d SDU . .
O5 O 0.4784(6) -0.3895(11) 0.2815(5) 0.149(4) Uiso 0.50 1 d PDU . .


_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 O2 2.343(2) . ?
Gd1 O1 2.352(2) . ?
Gd1 N3 2.371(3) . ?
Gd1 N11 2.400(3) 7 ?
Gd1 N6 2.443(3) . ?
Gd1 N6 2.510(2) 7 ?
Gd1 O4 2.511(2) . ?
Gd1 O3 2.547(2) . ?
Gd1 Cu1 3.4880(8) . ?
Cu1 O1 1.965(2) . ?
Cu1 O2 1.969(2) . ?
Cu1 N1 1.977(3) . ?
Cu1 N2 1.978(3) . ?
Cu1 N9 2.369(3) . ?
C1 O1 1.325(3) . ?
C1 C2 1.397(4) . ?
C1 C6 1.399(4) . ?
C2 C3 1.382(4) . ?
C2 O3 1.387(4) . ?
C3 C4 1.392(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.362(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.402(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.435(5) . ?
C7 N1 1.280(4) . ?
C7 H7 0.9300 . ?
C8 N1 1.479(4) . ?
C8 C9 1.504(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C12 1.515(5) . ?
C9 C11 1.519(5) . ?
C9 C10 1.534(4) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 N2 1.469(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N2 1.281(4) . ?
C13 C14 1.437(5) . ?
C13 H13 0.9300 . ?
C14 C19 1.395(4) . ?
C14 C15 1.405(4) . ?
C15 C16 1.372(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.384(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.375(4) . ?
C17 H17 0.9300 . ?
C18 O4 1.383(4) . ?
C18 C19 1.408(4) . ?
C19 O2 1.327(3) . ?
C20 O3 1.442(4) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 O4 1.435(4) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
N3 N4 1.135(4) . ?
N4 N5 1.157(4) . ?
N6 N7 1.221(4) . ?
N6 Gd1 2.511(2) 7 ?
N7 N8 1.137(4) . ?
N9 N10 1.156(4) . ?
N10 N11 1.165(4) . ?
N11 Gd1 2.400(3) 7 ?
C22 O5 1.3954(10) 2_655 ?
C22 O5 1.3955(10) . ?

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
O2 Gd1 O1 64.20(7) . . ?
O2 Gd1 N3 91.52(10) . . ?
O1 Gd1 N3 86.40(10) . . ?
O2 Gd1 N11 149.64(9) . 7 ?
O1 Gd1 N11 146.05(9) . 7 ?
N3 Gd1 N11 89.11(11) . 7 ?
O2 Gd1 N6 107.31(8) . . ?
O1 Gd1 N6 80.20(8) . . ?
N3 Gd1 N6 148.87(10) . . ?
N11 Gd1 N6 86.68(10) 7 . ?
O2 Gd1 N6 82.73(8) . 7 ?
O1 Gd1 N6 122.92(8) . 7 ?
N3 Gd1 N6 142.34(10) . 7 ?
N11 Gd1 N6 78.42(9) 7 7 ?
N6 Gd1 N6 66.44(10) . 7 ?
O2 Gd1 O4 64.89(7) . . ?
O1 Gd1 O4 123.87(7) . . ?
N3 Gd1 O4 72.89(10) . . ?
N11 Gd1 O4 86.43(9) 7 . ?
N6 Gd1 O4 137.41(8) . . ?
N6 Gd1 O4 71.00(8) 7 . ?
O2 Gd1 O3 127.14(7) . . ?
O1 Gd1 O3 64.85(7) . . ?
N3 Gd1 O3 72.15(10) . . ?
N11 Gd1 O3 81.74(9) 7 . ?
N6 Gd1 O3 76.72(8) . . ?
N6 Gd1 O3 138.79(8) 7 . ?
O4 Gd1 O3 143.15(7) . . ?
O2 Gd1 Cu1 32.53(5) . . ?
O1 Gd1 Cu1 32.51(5) . . ?
N3 Gd1 Cu1 94.28(8) . . ?
N11 Gd1 Cu1 176.02(7) 7 . ?
N6 Gd1 Cu1 89.34(6) . . ?
N6 Gd1 Cu1 100.03(6) 7 . ?
O4 Gd1 Cu1 96.56(5) . . ?
O3 Gd1 Cu1 97.29(5) . . ?
O1 Cu1 O2 78.74(8) . . ?
O1 Cu1 N1 92.16(10) . . ?
O2 Cu1 N1 166.28(11) . . ?
O1 Cu1 N2 168.09(10) . . ?
O2 Cu1 N2 90.99(10) . . ?
N1 Cu1 N2 96.79(11) . . ?
O1 Cu1 N9 95.38(10) . . ?
O2 Cu1 N9 98.09(10) . . ?
N1 Cu1 N9 92.93(11) . . ?
N2 Cu1 N9 92.01(11) . . ?
O1 Cu1 Gd1 40.04(6) . . ?
O2 Cu1 Gd1 39.81(6) . . ?
N1 Cu1 Gd1 132.19(8) . . ?
N2 Cu1 Gd1 130.60(7) . . ?
N9 Cu1 Gd1 91.50(8) . . ?
O1 C1 C2 118.9(3) . . ?
O1 C1 C6 123.0(3) . . ?
C2 C1 C6 118.1(3) . . ?
C3 C2 O3 123.2(3) . . ?
C3 C2 C1 121.4(3) . . ?
O3 C2 C1 115.3(3) . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 121.3(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 119.7(3) . . ?
C1 C6 C7 123.1(3) . . ?
C5 C6 C7 117.1(3) . . ?
N1 C7 C6 129.1(3) . . ?
N1 C7 H7 115.5 . . ?
C6 C7 H7 115.5 . . ?
N1 C8 C9 114.9(3) . . ?
N1 C8 H8A 108.5 . . ?
C9 C8 H8A 108.5 . . ?
N1 C8 H8B 108.5 . . ?
C9 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
C8 C9 C12 109.7(3) . . ?
C8 C9 C11 112.5(3) . . ?
C12 C9 C11 110.6(3) . . ?
C8 C9 C10 106.3(3) . . ?
C12 C9 C10 108.1(3) . . ?
C11 C9 C10 109.4(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 112.3(3) . . ?
N2 C12 H12A 109.1 . . ?
C9 C12 H12A 109.1 . . ?
N2 C12 H12B 109.1 . . ?
C9 C12 H12B 109.1 . . ?
H12A C12 H12B 107.9 . . ?
N2 C13 C14 127.7(3) . . ?
N2 C13 H13 116.1 . . ?
C14 C13 H13 116.1 . . ?
C19 C14 C15 119.3(3) . . ?
C19 C14 C13 123.1(3) . . ?
C15 C14 C13 117.6(3) . . ?
C16 C15 C14 121.3(3) . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C15 C16 C17 119.8(3) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C18 C17 C16 119.7(3) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 O4 124.2(3) . . ?
C17 C18 C19 121.7(3) . . ?
O4 C18 C19 114.1(2) . . ?
O2 C19 C14 123.4(3) . . ?
O2 C19 C18 118.5(3) . . ?
C14 C19 C18 118.1(3) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 N1 C8 113.4(3) . . ?
C7 N1 Cu1 123.9(2) . . ?
C8 N1 Cu1 122.7(2) . . ?
C13 N2 C12 114.9(3) . . ?
C13 N2 Cu1 125.5(2) . . ?
C12 N2 Cu1 119.5(2) . . ?
N4 N3 Gd1 163.7(3) . . ?
N3 N4 N5 177.9(4) . . ?
N7 N6 Gd1 122.7(2) . . ?
N7 N6 Gd1 121.3(2) . 7 ?
Gd1 N6 Gd1 113.56(10) . 7 ?
N8 N7 N6 179.4(4) . . ?
N10 N9 Cu1 129.6(3) . . ?
N9 N10 N11 177.9(3) . . ?
N10 N11 Gd1 133.9(2) . 7 ?
C1 O1 Cu1 128.40(18) . . ?
C1 O1 Gd1 124.14(18) . . ?
Cu1 O1 Gd1 107.45(9) . . ?
C19 O2 Cu1 128.09(19) . . ?
C19 O2 Gd1 123.86(18) . . ?
Cu1 O2 Gd1 107.66(9) . . ?
C2 O3 C20 116.2(3) . . ?
C2 O3 Gd1 116.49(17) . . ?
C20 O3 Gd1 121.9(2) . . ?
C18 O4 C21 117.2(2) . . ?
C18 O4 Gd1 117.78(16) . . ?
C21 O4 Gd1 124.4(2) . . ?
O5 C22 O5 101.7(14) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.64
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.086
####################################################################### 
# 
# 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_9-CuDyvaldmpnN3
_database_code_depnum_ccdc_archive 'CCDC 1060768'
_audit_update_record             
;
2015-04-21 deposited with the CCDC.
2017-05-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            CuDyvaldmpnN3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 Cu2 Dy2 N22 O10'
_chemical_formula_weight         1505.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.900(3)
_cell_length_b                   10.778(3)
_cell_length_c                   13.432(4)
_cell_angle_alpha                99.895(8)
_cell_angle_beta                 91.177(7)
_cell_angle_gamma                100.921(7)
_cell_volume                     1384.2(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6541
_cell_measurement_theta_min      1.54
_cell_measurement_theta_max      27.91

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             744
_exptl_absorpt_coefficient_mu    3.501
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.5714
_exptl_absorpt_correction_T_max  0.8444
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30861
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         27.91
_reflns_number_total             6541
_reflns_number_gt                5755
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex Duo'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0344P)²+0.6152P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6541
_refine_ls_number_parameters     361
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0667
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.436574(14) 0.558493(13) 0.139922(11) 0.02941(6) Uani 1 1 d . . .
Cu1 Cu 0.69316(4) 0.82901(4) 0.20651(3) 0.03658(10) Uani 1 1 d . . .
C1 C 0.4198(3) 0.8534(3) 0.1264(2) 0.0329(7) Uani 1 1 d . . .
C2 C 0.2777(3) 0.7996(3) 0.1059(3) 0.0351(7) Uani 1 1 d . . .
C3 C 0.1858(3) 0.8718(4) 0.0815(3) 0.0415(8) Uani 1 1 d . . .
H3 H 0.0911 0.8337 0.0674 0.050 Uiso 1 1 calc R . .
C4 C 0.2316(4) 1.0005(4) 0.0774(3) 0.0478(9) Uani 1 1 d . . .
H4A H 0.1684 1.0506 0.0600 0.057 Uiso 1 1 calc R . .
C5 C 0.3683(4) 1.0557(4) 0.0985(3) 0.0495(9) Uani 1 1 d . . .
H5A H 0.3987 1.1440 0.0956 0.059 Uiso 1 1 calc R . .
C6 C 0.4640(4) 0.9838(3) 0.1242(3) 0.0390(7) Uani 1 1 d . . .
C7 C 0.6057(4) 1.0484(3) 0.1446(3) 0.0458(9) Uani 1 1 d . . .
H7A H 0.6268 1.1345 0.1334 0.055 Uiso 1 1 calc R . .
C8 C 0.8431(4) 1.0897(4) 0.1848(3) 0.0552(10) Uani 1 1 d . . .
H8A H 0.8299 1.1762 0.1762 0.066 Uiso 1 1 calc R . .
H8B H 0.8987 1.0580 0.1291 0.066 Uiso 1 1 calc R . .
C9 C 0.9223(4) 1.1011(4) 0.2847(3) 0.0458(9) Uani 1 1 d . . .
C10 C 1.0490(4) 1.2089(5) 0.2868(4) 0.0679(13) Uani 1 1 d . . .
H10A H 1.0189 1.2901 0.2849 0.102 Uiso 1 1 calc R . .
H10B H 1.1027 1.1882 0.2279 0.102 Uiso 1 1 calc R . .
H10C H 1.1061 1.2172 0.3490 0.102 Uiso 1 1 calc R . .
C11 C 0.8375(5) 1.1340(5) 0.3741(4) 0.0767(16) Uani 1 1 d . . .
H11A H 0.8042 1.2130 0.3693 0.115 Uiso 1 1 calc R . .
H11B H 0.8945 1.1470 0.4370 0.115 Uiso 1 1 calc R . .
H11C H 0.7587 1.0636 0.3742 0.115 Uiso 1 1 calc R . .
C12 C 0.9750(4) 0.9784(4) 0.2881(4) 0.0557(11) Uani 1 1 d . . .
H12A H 1.0285 0.9600 0.2277 0.067 Uiso 1 1 calc R . .
H12B H 1.0389 0.9928 0.3485 0.067 Uiso 1 1 calc R . .
C13 C 0.8971(4) 0.7883(4) 0.3479(3) 0.0443(8) Uani 1 1 d . . .
H13A H 0.9835 0.8157 0.3849 0.053 Uiso 1 1 calc R . .
C14 C 0.8188(4) 0.6676(3) 0.3630(3) 0.0419(8) Uani 1 1 d . . .
C15 C 0.8657(4) 0.6103(4) 0.4401(3) 0.0559(11) Uani 1 1 d . . .
H15A H 0.9497 0.6505 0.4775 0.067 Uiso 1 1 calc R . .
C16 C 0.7944(5) 0.4991(5) 0.4625(4) 0.0646(12) Uani 1 1 d . . .
H16A H 0.8267 0.4634 0.5161 0.078 Uiso 1 1 calc R . .
C17 C 0.6735(4) 0.4379(4) 0.4063(3) 0.0533(10) Uani 1 1 d . . .
H17 H 0.6225 0.3605 0.4223 0.064 Uiso 1 1 calc R . .
C18 C 0.6274(3) 0.4878(3) 0.3282(3) 0.0382(7) Uani 1 1 d . . .
C19 C 0.6972(3) 0.6053(3) 0.3054(3) 0.0358(7) Uani 1 1 d . . .
C20 C 0.0989(3) 0.6194(4) 0.1206(4) 0.0532(10) Uani 1 1 d . . .
H20A H 0.0873 0.5282 0.1253 0.080 Uiso 1 1 calc R . .
H20B H 0.0463 0.6284 0.0605 0.080 Uiso 1 1 calc R . .
H20C H 0.0652 0.6659 0.1812 0.080 Uiso 1 1 calc R . .
C21 C 0.4149(4) 0.3360(4) 0.3028(3) 0.0586(11) Uani 1 1 d . . .
H21A H 0.3382 0.3006 0.2524 0.088 Uiso 1 1 calc R . .
H21B H 0.3799 0.3767 0.3653 0.088 Uiso 1 1 calc R . .
H21C H 0.4596 0.2667 0.3170 0.088 Uiso 1 1 calc R . .
C22 C 0.6739(15) 0.9243(12) 0.5697(9) 0.240(6) Uani 1 1 d DU . .
N1 N 0.7078(3) 1.0034(3) 0.1763(2) 0.0429(7) Uani 1 1 d . . .
N2 N 0.8667(3) 0.8643(3) 0.2914(2) 0.0400(7) Uani 1 1 d . . .
N3 N 0.3373(4) 0.6088(4) 0.2993(3) 0.0583(9) Uani 1 1 d . . .
N4 N 0.2877(4) 0.6895(5) 0.3367(3) 0.0662(11) Uani 1 1 d . . .
N5 N 0.2366(7) 0.7724(7) 0.3752(5) 0.132(2) Uani 1 1 d . . .
N6 N 0.4105(3) 0.5563(3) -0.0426(2) 0.0362(6) Uani 1 1 d . . .
N7 N 0.3069(3) 0.5810(3) -0.0844(2) 0.0507(8) Uani 1 1 d . . .
N8 N 0.2108(5) 0.6036(5) -0.1231(4) 0.0887(15) Uani 1 1 d . . .
N9 N 0.8211(3) 0.7662(3) 0.0563(3) 0.0473(7) Uani 1 1 d . . .
N10 N 0.7780(3) 0.6970(3) -0.0174(2) 0.0341(6) Uani 1 1 d . . .
N11 N 0.7368(3) 0.6290(3) -0.0949(2) 0.0457(7) Uani 1 1 d . . .
O1 O 0.5039(2) 0.7771(2) 0.14583(18) 0.0349(5) Uani 1 1 d . . .
O2 O 0.6454(2) 0.6521(2) 0.23117(17) 0.0358(5) Uani 1 1 d . . .
O3 O 0.2425(2) 0.6715(2) 0.11288(19) 0.0378(5) Uani 1 1 d . . .
O4 O 0.5135(2) 0.4303(2) 0.26413(18) 0.0400(5) Uani 1 1 d . . .
O5 O 0.5856(9) 0.8607(9) 0.4868(7) 0.120(3) Uiso 0.598(9) 1 d PDU A 1
O5' O 0.5622(8) 0.8790(8) 0.3823(6) 0.066(3) Uiso 0.402(9) 1 d P A 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
Dy1 O1 2.311(2) . ?
Dy1 O2 2.340(2) . ?
Dy1 N11 2.370(3) 2_665 ?
Dy1 N3 2.395(3) . ?
Dy1 N6 2.401(3) 2_665 ?
Dy1 N6 2.456(3) . ?
Dy1 O3 2.513(2) . ?
Dy1 O4 2.532(2) . ?
Dy1 Cu1 3.4579(9) . ?
Cu1 O2 1.962(2) . ?
Cu1 O1 1.967(2) . ?
Cu1 N1 1.970(3) . ?
Cu1 N2 1.980(3) . ?
Cu1 N9 2.468(3) . ?
C1 O1 1.327(4) . ?
C1 C6 1.396(5) . ?
C1 C2 1.419(4) . ?
C2 C3 1.373(5) . ?
C2 O3 1.378(4) . ?
C3 C4 1.386(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.405(5) . ?
C5 H5A 0.9500 . ?
C6 C7 1.441(5) . ?
C7 N1 1.295(5) . ?
C7 H7A 0.9500 . ?
C8 N1 1.469(4) . ?
C8 C9 1.515(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C11 1.510(6) . ?
C9 C12 1.519(6) . ?
C9 C10 1.536(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 N2 1.478(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 N2 1.278(5) . ?
C13 C14 1.431(5) . ?
C13 H13A 0.9500 . ?
C14 C19 1.406(5) . ?
C14 C15 1.407(5) . ?
C15 C16 1.355(6) . ?
C15 H15A 0.9500 . ?
C16 C17 1.389(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.365(5) . ?
C17 H17 0.9500 . ?
C18 O4 1.381(4) . ?
C18 C19 1.409(5) . ?
C19 O2 1.328(4) . ?
C20 O3 1.439(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 O4 1.443(4) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 O5 1.3947(11) . ?
N3 N4 1.128(5) . ?
N4 N5 1.160(6) . ?
N6 N7 1.253(4) . ?
N6 Dy1 2.401(3) 2_665 ?
N7 N8 1.160(5) . ?
N9 N10 1.152(4) . ?
N10 N11 1.181(4) . ?
N11 Dy1 2.370(3) 2_665 ?

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 Dy1 O2 65.14(8) . . ?
O1 Dy1 N11 148.08(10) . 2_665 ?
O2 Dy1 N11 146.21(10) . 2_665 ?
O1 Dy1 N3 87.32(12) . . ?
O2 Dy1 N3 84.23(12) . . ?
N11 Dy1 N3 90.39(13) 2_665 . ?
O1 Dy1 N6 110.77(9) . 2_665 ?
O2 Dy1 N6 79.97(9) . 2_665 ?
N11 Dy1 N6 87.38(11) 2_665 2_665 ?
N3 Dy1 N6 147.67(11) . 2_665 ?
O1 Dy1 N6 82.67(9) . . ?
O2 Dy1 N6 121.03(9) . . ?
N11 Dy1 N6 80.89(10) 2_665 . ?
N3 Dy1 N6 144.51(11) . . ?
N6 Dy1 N6 66.70(11) 2_665 . ?
O1 Dy1 O3 65.57(7) . . ?
O2 Dy1 O3 125.65(8) . . ?
N11 Dy1 O3 83.45(10) 2_665 . ?
N3 Dy1 O3 72.02(10) . . ?
N6 Dy1 O3 139.43(9) 2_665 . ?
N6 Dy1 O3 72.83(9) . . ?
O1 Dy1 O4 126.26(8) . . ?
O2 Dy1 O4 64.69(8) . . ?
N11 Dy1 O4 82.12(9) 2_665 . ?
N3 Dy1 O4 69.81(11) . . ?
N6 Dy1 O4 77.94(9) 2_665 . ?
N6 Dy1 O4 141.22(9) . . ?
O3 Dy1 O4 138.89(8) . . ?
O1 Dy1 Cu1 32.84(5) . . ?
O2 Dy1 Cu1 32.93(5) . . ?
N11 Dy1 Cu1 179.07(8) 2_665 . ?
N3 Dy1 Cu1 89.79(10) . . ?
N6 Dy1 Cu1 91.98(7) 2_665 . ?
N6 Dy1 Cu1 99.47(7) . . ?
O3 Dy1 Cu1 97.47(6) . . ?
O4 Dy1 Cu1 97.09(6) . . ?
O2 Cu1 O1 79.17(9) . . ?
O2 Cu1 N1 170.38(11) . . ?
O1 Cu1 N1 91.46(11) . . ?
O2 Cu1 N2 92.27(11) . . ?
O1 Cu1 N2 167.89(11) . . ?
N1 Cu1 N2 96.66(12) . . ?
O2 Cu1 N9 92.73(11) . . ?
O1 Cu1 N9 99.49(10) . . ?
N1 Cu1 N9 90.97(12) . . ?
N2 Cu1 N9 89.37(12) . . ?
O2 Cu1 Dy1 40.41(6) . . ?
O1 Cu1 Dy1 39.58(6) . . ?
N1 Cu1 Dy1 130.61(9) . . ?
N2 Cu1 Dy1 132.67(9) . . ?
N9 Cu1 Dy1 91.76(8) . . ?
O1 C1 C6 123.4(3) . . ?
O1 C1 C2 118.4(3) . . ?
C6 C1 C2 118.2(3) . . ?
C3 C2 O3 124.3(3) . . ?
C3 C2 C1 121.5(3) . . ?
O3 C2 C1 114.2(3) . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.0(3) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C4 C5 C6 121.2(3) . . ?
C4 C5 H5A 119.4 . . ?
C6 C5 H5A 119.4 . . ?
C1 C6 C5 119.4(3) . . ?
C1 C6 C7 122.8(3) . . ?
C5 C6 C7 117.8(3) . . ?
N1 C7 C6 127.9(3) . . ?
N1 C7 H7A 116.1 . . ?
C6 C7 H7A 116.1 . . ?
N1 C8 C9 113.6(3) . . ?
N1 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
N1 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C11 C9 C8 112.1(4) . . ?
C11 C9 C12 111.5(4) . . ?
C8 C9 C12 109.8(3) . . ?
C11 C9 C10 109.6(3) . . ?
C8 C9 C10 106.4(3) . . ?
C12 C9 C10 107.1(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 C9 114.8(3) . . ?
N2 C12 H12A 108.6 . . ?
C9 C12 H12A 108.6 . . ?
N2 C12 H12B 108.6 . . ?
C9 C12 H12B 108.6 . . ?
H12A C12 H12B 107.5 . . ?
N2 C13 C14 128.9(3) . . ?
N2 C13 H13A 115.5 . . ?
C14 C13 H13A 115.5 . . ?
C19 C14 C15 118.9(3) . . ?
C19 C14 C13 123.1(3) . . ?
C15 C14 C13 118.0(3) . . ?
C16 C15 C14 121.7(4) . . ?
C16 C15 H15A 119.1 . . ?
C14 C15 H15A 119.1 . . ?
C15 C16 C17 119.4(4) . . ?
C15 C16 H16A 120.3 . . ?
C17 C16 H16A 120.3 . . ?
C18 C17 C16 120.6(4) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 O4 125.0(3) . . ?
C17 C18 C19 121.1(3) . . ?
O4 C18 C19 113.9(3) . . ?
O2 C19 C14 123.1(3) . . ?
O2 C19 C18 118.8(3) . . ?
C14 C19 C18 118.1(3) . . ?
O3 C20 H20A 109.5 . . ?
O3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C7 N1 C8 115.6(3) . . ?
C7 N1 Cu1 124.6(2) . . ?
C8 N1 Cu1 119.7(3) . . ?
C13 N2 C12 115.2(3) . . ?
C13 N2 Cu1 123.4(2) . . ?
C12 N2 Cu1 121.3(2) . . ?
N4 N3 Dy1 134.9(3) . . ?
N3 N4 N5 179.9(7) . . ?
N7 N6 Dy1 120.6(2) . 2_665 ?
N7 N6 Dy1 123.5(2) . . ?
Dy1 N6 Dy1 113.30(11) 2_665 . ?
N8 N7 N6 179.9(5) . . ?
N10 N9 Cu1 127.3(2) . . ?
N9 N10 N11 177.6(4) . . ?
N10 N11 Dy1 133.8(2) . 2_665 ?
C1 O1 Cu1 127.3(2) . . ?
C1 O1 Dy1 124.29(19) . . ?
Cu1 O1 Dy1 107.58(9) . . ?
C19 O2 Cu1 126.6(2) . . ?
C19 O2 Dy1 124.3(2) . . ?
Cu1 O2 Dy1 106.66(9) . . ?
C2 O3 C20 117.3(3) . . ?
C2 O3 Dy1 117.02(17) . . ?
C20 O3 Dy1 124.9(2) . . ?
C18 O4 C21 115.3(3) . . ?
C18 O4 Dy1 117.58(19) . . ?
C21 O4 Dy1 120.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.91
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.101
