The crystal structures of {LnCu5}3+ (Ln = Gd, Dy and Ho) 15-metallacrown-5 complexes and a reevaluation of the isotypic EuIII analogue

Pavlishchuk, A.; Naumova, D.; Zeller, M.; Calderon Cazorla, S.; Addison, A.W.

doi:10.1107/S205698901900999X

The crystal structures of {LnCu₅}³⁺ (Ln = Gd, Dy and Ho) 15-metallacrown-5 complexes and a reevaluation of the isotypic Eu^III analogue

A. Pavlishchuk, D. Naumova, M. Zeller, S. Calderon Cazorla and A. W. Addison

The crystal structures of three new isomorphous 3d–4f 15-metallacrown-5 complexes, [LnCu₅(GlyHA)₅(CO₃)(NO₃)(H₂O)₅]·xH₂O (Ln^III = Gd (1, x = 3.5); Dy (2, x = 3.28) and Ho (3, x = 3.45)), were determined. Structural details of the previously reported isotypic Eu^III analogue were reinterpreted.

Keywords: crystal structure; lanthanide(III); hydroxamates; heteropolynuclear complex; metallacrown.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S205698901900999X/cq2031sup1.cif Contains datablocks Complex_1, Complex_2, Complex_3, global
	Structure factor file (CIF format) https://doi.org/10.1107/S205698901900999X/cq2031Complex_1sup2.hkl Contains datablock Complex_1
	Structure factor file (CIF format) https://doi.org/10.1107/S205698901900999X/cq2031Complex_2sup3.hkl Contains datablock Complex_2
	Structure factor file (CIF format) https://doi.org/10.1107/S205698901900999X/cq2031Complex_3sup4.hkl Contains datablock Complex_3

CCDC references: 1940082; 1940083; 1940084

checkCIF report

Key indicators

Structure: Complex_1

Single-crystal X-ray study
T = 150 K
Mean (C-C) = 0.004 Å
Disorder in main residue
R factor = 0.034
wR factor = 0.076
Data-to-parameter ratio = 21.8

Structure: Complex_2

Single-crystal X-ray study
T = 150 K
Mean (C-C) = 0.006 Å
Disorder in main residue
R factor = 0.031
wR factor = 0.076
Data-to-parameter ratio = 14.7

Structure: Complex_3

Single-crystal X-ray study
T = 150 K
Mean (C-C) = 0.004 Å
Disorder in main residue
R factor = 0.033
wR factor = 0.082
Data-to-parameter ratio = 21.9

checkCIF/PLATON results

No syntax errors found



Datablock: Complex_1



Alert level B
PLAT910_ALERT_3_B Missing # of FCF Reflection(s) Below Theta(Min).         11 Note

Alert level C
PLAT220_ALERT_2_C Non-Solvent  Resd 1  O   Ueq(max)/Ueq(min) Range        3.6 Ratio
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        N11 Check
PLAT314_ALERT_2_C Small Angle for H2O: Metal-O18      -H18B      .      94.39 Degree
PLAT417_ALERT_2_C Short Inter D-H..H-D       H22A     ..H23B     .       2.10 Ang.
                                                 2-x,1-y,-z  =      2_765 Check
PLAT971_ALERT_2_C Check Calcd Resid. Dens.  0.45A   From Gd1             1.73 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         35 Note
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          8 Report
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         10 Report
PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records         12 Report
PLAT175_ALERT_4_G The CIF-Embedded .res File Contains SAME Records          1 Report
PLAT178_ALERT_4_G The CIF-Embedded .res File Contains SIMU Records          1 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cu1      --O18      .        9.9 s.u.
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )         8% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  5  )       100% Note
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  5          1.50 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  N2       ..C11B             3.04 Ang.
                                                2-x,1-y,1-z  =      2_766 Check
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          5 Note
              H2 O
PLAT794_ALERT_5_G Tentative Bond Valency for Cu1       (II)      .       2.35 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu2       (II)      .       2.40 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu3       (II)      .       2.34 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu4       (II)      .       2.36 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu5       (II)      .       2.36 Info
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............        135 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         42 Note
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          1 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
   6 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  20 ALERT level G = General information/check it is not something unexpected

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  11 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   7 ALERT type 4 Improvement, methodology, query or suggestion
   6 ALERT type 5 Informative message, check




Datablock: Complex_2



Alert level B
PLAT417_ALERT_2_B Short Inter D-H..H-D       H2B      ..H23A     .       2.06 Ang.
                                                2-x,1-y,1-z  =      2_766 Check
PLAT910_ALERT_3_B Missing # of FCF Reflection(s) Below Theta(Min).         11 Note

Alert level C
PLAT220_ALERT_2_C Non-Solvent  Resd 1  O   Ueq(max)/Ueq(min) Range        3.9 Ratio
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        N11 Check
PLAT260_ALERT_2_C Large Average Ueq of Residue Including       O23      0.111 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         11 Report
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.96A   From N4             -0.69 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H2C              -0.32 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H8B              -0.36 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H10B             -0.36 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         35 Note
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          8 Report
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         12 Report
PLAT068_ALERT_1_G Reported F000 Differs from Calcd (or Missing)...     Please Check
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       7.92 Why ?
PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records         10 Report
PLAT175_ALERT_4_G The CIF-Embedded .res File Contains SAME Records          1 Report
PLAT178_ALERT_4_G The CIF-Embedded .res File Contains SIMU Records          1 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cu1      --O18      .        7.3 s.u.
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )         8% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  5  )       100% Note
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  5          0.84 Check
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          5 Note
              H2 O
PLAT794_ALERT_5_G Tentative Bond Valency for Cu1       (II)      .       2.35 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu2       (III)     .       2.67 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu3       (II)      .       2.33 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu4       (II)      .       2.36 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu5       (II)      .       2.36 Info
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............        133 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600          7 Note
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          3 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   2 ALERT level B = A potentially serious problem, consider carefully
   9 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  21 ALERT level G = General information/check it is not something unexpected

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  14 ALERT type 2 Indicator that the structure model may be wrong or deficient
   4 ALERT type 3 Indicator that the structure quality may be low
   7 ALERT type 4 Improvement, methodology, query or suggestion
   6 ALERT type 5 Informative message, check




Datablock: Complex_3



Alert level B
PLAT971_ALERT_2_B Check Calcd Resid. Dens.  0.63A   From O23             2.95 eA-3

Alert level C
PLAT214_ALERT_2_C Atom O23       (Anion/Solvent) ADP max/min Ratio        4.8 prolat
PLAT220_ALERT_2_C Non-Solvent  Resd 1  O   Ueq(max)/Ueq(min) Range        4.7 Ratio
PLAT242_ALERT_2_C Low    'MainMol' Ueq as Compared to Neighbors of        N11 Check
PLAT314_ALERT_2_C Small Angle for H2O: Metal-O18      -H18A      .      93.59 Degree
PLAT314_ALERT_2_C Small Angle for H2O: Metal-O18      -H18B      .      92.78 Degree
PLAT910_ALERT_3_C Missing # of FCF Reflection(s) Below Theta(Min).          6 Note
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         25 Report
PLAT934_ALERT_3_C Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          1 Check
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.71A   From Ho1            -2.31 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.50A   From Ho1            -2.10 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.39A   From Ho1            -1.98 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.57A   From Ho1            -1.96 eA-3
PLAT972_ALERT_2_C Check Calcd Resid. Dens.  0.49A   From Ho1            -1.89 eA-3
PLAT975_ALERT_2_C Check Calcd Resid. Dens.  0.72A   From O23             1.13 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.91A   From N4             -0.87 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.75A   From O23            -0.73 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.64A   From O22            -0.64 eA-3
PLAT976_ALERT_2_C Check Calcd Resid. Dens.  0.71A   From O22            -0.62 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H4A              -0.35 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H4D              -0.41 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H6D              -0.41 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H10C             -0.32 eA-3
PLAT977_ALERT_2_C Check Negative Difference Density on H20B             -0.40 eA-3
PLAT978_ALERT_2_C Number C-C Bonds with Positive Residual Density.          0 Info

Alert level G
PLAT002_ALERT_2_G Number of Distance or Angle Restraints on AtSite         35 Note
PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ...          9 Report
PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms ..............         12 Report
PLAT083_ALERT_2_G SHELXL Second Parameter in WGHT  Unusually Large       5.88 Why ?
PLAT154_ALERT_1_G The s.u.'s on the Cell Angles are Equal ..(Note)      0.003 Degree
PLAT172_ALERT_4_G The CIF-Embedded .res File Contains DFIX Records         10 Report
PLAT175_ALERT_4_G The CIF-Embedded .res File Contains SAME Records          1 Report
PLAT178_ALERT_4_G The CIF-Embedded .res File Contains SIMU Records          1 Report
PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X)  Cu1      --O18      .       10.3 s.u.
PLAT301_ALERT_3_G Main Residue  Disorder ..............(Resd  1  )         8% Note
PLAT302_ALERT_4_G Anion/Solvent/Minor-Residue Disorder (Resd  5  )       100% Note
PLAT304_ALERT_4_G Non-Integer Number of Atoms in ...... Resd  5          1.34 Check
PLAT432_ALERT_2_G Short Inter X...Y Contact  N2       ..C11B             3.05 Ang.
                                                2-x,1-y,1-z  =      2_766 Check
PLAT790_ALERT_4_G Centre of Gravity not Within Unit Cell: Resd.  #          5 Note
              H2 O
PLAT794_ALERT_5_G Tentative Bond Valency for Cu1       (II)      .       2.36 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu2       (II)      .       2.41 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu3       (II)      .       2.34 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu4       (II)      .       2.36 Info
PLAT794_ALERT_5_G Tentative Bond Valency for Cu5       (II)      .       2.36 Info
PLAT860_ALERT_3_G Number of Least-Squares Restraints .............        139 Note
PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L=  0.600         74 Note
PLAT933_ALERT_2_G Number of OMIT Records in Embedded .res File ...          1 Note

   0 ALERT level A = Most likely a serious problem - resolve or explain
   1 ALERT level B = A potentially serious problem, consider carefully
  24 ALERT level C = Check. Ensure it is not caused by an omission or oversight
  22 ALERT level G = General information/check it is not something unexpected

   1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
  28 ALERT type 2 Indicator that the structure model may be wrong or deficient
   5 ALERT type 3 Indicator that the structure quality may be low
   7 ALERT type 4 Improvement, methodology, query or suggestion
   6 ALERT type 5 Informative message, check

Computing details top

For all structures, data collection: APEX3 (Bruker, 2017); cell refinement: SAINT (Bruker, 2017); data reduction: SAINT (Bruker, 2017); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2018/3 (Sheldrick, 2015), SHELXLE (Hübschle et al., 2011); software used to prepare material for publication: publCIF (Westrip, 2010).

Pentaaquacarbonatopentakis(glycine hydroxamato)nitratopentacopper(II)gadolinium(III) 3.5-hydrate (Complex_1) top

Crystal data top

[Cu₅Gd(C₂H₄N₂O₂)₅(CO₃)(NO₃)(H₂O)₅]·3.5H₂O	Z = 2
M_r = 1190.49	F(000) = 1170
Triclinic, P1	D_x = 2.440 Mg m⁻³
a = 11.2057 (15) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.5054 (15) Å	Cell parameters from 9949 reflections
c = 13.2983 (10) Å	θ = 3.1–32.5°
α = 94.026 (4)°	µ = 5.35 mm⁻¹
β = 94.942 (3)°	T = 150 K
γ = 107.558 (3)°	Rod, blue
V = 1620.2 (3) Å³	0.15 × 0.10 × 0.05 mm

Data collection top

Bruker AXS D8 Quest CMOS diffractometer	12399 independent reflections
Radiation source: sealed tube X-ray source	9545 reflections with I > 2σ(I)
Triumph curved graphite crystal monochromator	R_int = 0.056
ω and phi scans	θ_max = 33.2°, θ_min = 3.1°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −17→17
T_min = 0.599, T_max = 0.747	k = −17→17
118155 measured reflections	l = −19→20

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.034	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.076	w = 1/[σ²(F_o²) + (0.0346P)² + 2.5135P] where P = (F_o² + 2F_c²)/3
S = 1.05	(Δ/σ)_max = 0.001
12399 reflections	Δρ_max = 2.06 e Å⁻³
570 parameters	Δρ_min = −1.40 e Å⁻³
135 restraints	Extinction correction: SHELXL-2018/3 (Sheldrick 2015), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00141 (15)

Special details top

Geometry. 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.

Refinement. A water molecule is partially occupied, inducing disorder for the nearby carbonate anion. The two disordered moieties were restrained to have similar geometries. Uij components of ADPs for disordered atoms closer to each other than 2.0 Angstrom were restrained to be similar. The distance of the water oxygen to one of the carbonate oxygen atoms was restrained to be at least 2.8 Angstrom for the moiety that contains the water molecule.

Water H atom positions were refined and O-H and H···H distances were restrained to 0.84 (2) and 1.36 (2) Angstrom, respectively. The water H atom positions of the disordered moiety were further restrained based on hydrogen bonding considerations. Subject to these conditions the occupancy ratio refined to 0.499 (11) to 0.501 (11).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
C1	1.0282 (3)	0.3071 (3)	0.5735 (2)	0.0169 (5)
C2	1.0133 (3)	0.3907 (3)	0.6602 (2)	0.0198 (6)
H2C	1.011450	0.350005	0.723478	0.024*
H2D	1.085802	0.466751	0.669686	0.024*
C3	0.6601 (3)	0.4525 (3)	0.3876 (2)	0.0184 (5)
C4	0.5624 (3)	0.5110 (3)	0.3531 (2)	0.0237 (6)
H4C	0.492326	0.489577	0.395853	0.028*
H4D	0.600253	0.601279	0.361189	0.028*
C5	0.5301 (3)	0.2146 (3)	0.0120 (2)	0.0180 (5)
C6	0.4908 (3)	0.1751 (3)	−0.0995 (2)	0.0211 (6)
H6C	0.398256	0.136861	−0.110988	0.025*
H6D	0.513050	0.247914	−0.137828	0.025*
C7	0.8131 (3)	−0.0807 (3)	−0.0320 (2)	0.0158 (5)
C8	0.8535 (3)	−0.1924 (3)	−0.0560 (2)	0.0185 (5)
H8C	0.778171	−0.265599	−0.071359	0.022*
H8D	0.899628	−0.182227	−0.116646	0.022*
C9	1.1071 (3)	−0.0372 (3)	0.3184 (2)	0.0155 (5)
C10	1.2060 (3)	−0.0372 (3)	0.4025 (2)	0.0182 (5)
H10C	1.183398	−0.118107	0.429579	0.022*
H10D	1.288131	−0.023541	0.375327	0.022*
C11	1.0002 (9)	0.3923 (10)	0.1657 (8)	0.0187 (17)	0.499 (11)
O12	0.8812 (8)	0.3500 (10)	0.1377 (9)	0.0268 (16)	0.499 (11)
O13	1.0398 (17)	0.3359 (17)	0.2371 (11)	0.0221 (18)	0.499 (11)
O14	1.0726 (7)	0.4812 (8)	0.1298 (7)	0.0296 (16)	0.499 (11)
O23	1.3130 (8)	0.5342 (7)	0.1998 (11)	0.100 (5)	0.499 (11)
H23A	1.324 (17)	0.608 (5)	0.223 (7)	0.150*	0.499 (11)
H23B	1.242 (5)	0.491 (7)	0.171 (13)	0.150*	0.499 (11)
C11B	1.0371 (9)	0.3913 (10)	0.1761 (9)	0.0210 (18)	0.501 (11)
O12B	0.9211 (8)	0.3493 (10)	0.1322 (8)	0.0280 (16)	0.501 (11)
O13B	1.0555 (17)	0.3350 (16)	0.2552 (11)	0.0231 (19)	0.501 (11)
O14B	1.1203 (8)	0.4785 (8)	0.1474 (6)	0.0319 (18)	0.501 (11)
N1	0.9476 (2)	0.2923 (2)	0.49334 (18)	0.0184 (5)
N2	0.8943 (3)	0.4211 (3)	0.6387 (2)	0.0242 (5)
H2A	0.909529	0.503064	0.653694	0.029*
H2B	0.836962	0.381155	0.679007	0.029*
N3	0.6792 (3)	0.3745 (2)	0.32041 (19)	0.0194 (5)
N4	0.5128 (3)	0.4690 (3)	0.2453 (2)	0.0321 (7)
H4A	0.541406	0.531489	0.206441	0.038*
H4B	0.427124	0.446800	0.238524	0.038*
N5	0.6111 (2)	0.1674 (2)	0.05484 (18)	0.0177 (5)
N6	0.5532 (2)	0.0865 (2)	−0.13735 (18)	0.0190 (5)
H6A	0.585643	0.108822	−0.196056	0.023*
H6B	0.496054	0.010374	−0.150377	0.023*
N7	0.8504 (2)	−0.0252 (2)	0.05833 (18)	0.0161 (4)
N8	0.9361 (2)	−0.2106 (2)	0.03158 (19)	0.0193 (5)
H8A	1.014048	−0.203019	0.012836	0.023*
H8B	0.903608	−0.287467	0.050144	0.023*
N9	1.0599 (2)	0.0527 (2)	0.32669 (17)	0.0157 (4)
N10	1.2174 (3)	0.0598 (3)	0.4855 (2)	0.0236 (5)
H10A	1.297991	0.111081	0.495577	0.028*
H10B	1.199114	0.025111	0.543971	0.028*
N11	0.5782 (3)	0.2254 (3)	0.6118 (2)	0.0282 (6)
Cu1	1.09871 (3)	0.15598 (3)	0.45052 (3)	0.01629 (7)
Cu2	0.82345 (3)	0.37425 (3)	0.49429 (3)	0.01666 (7)
Cu3	0.56789 (4)	0.32576 (3)	0.19730 (3)	0.01924 (8)
Cu4	0.69162 (3)	0.08373 (3)	−0.03230 (3)	0.01653 (7)
Cu5	0.95028 (3)	−0.08613 (3)	0.15079 (3)	0.01552 (7)
Gd1	0.84770 (2)	0.19381 (2)	0.24301 (2)	0.01278 (4)
O1	0.9539 (2)	0.2085 (2)	0.41509 (15)	0.0205 (4)
O2	1.1140 (2)	0.2528 (2)	0.57995 (15)	0.0193 (4)
O3	0.7698 (2)	0.31983 (19)	0.35249 (15)	0.0186 (4)
O4	0.7179 (2)	0.47939 (19)	0.47886 (16)	0.0204 (4)
O5	0.6439 (2)	0.2014 (2)	0.15887 (15)	0.0208 (4)
O6	0.4844 (2)	0.2916 (2)	0.05861 (16)	0.0213 (4)
O7	0.8123 (2)	0.07808 (19)	0.07923 (15)	0.0188 (4)
O8	0.7441 (2)	−0.04598 (19)	−0.09994 (15)	0.0184 (4)
O9	0.97139 (19)	0.05463 (18)	0.24655 (15)	0.0164 (4)
O10	1.0746 (2)	−0.12244 (19)	0.24335 (15)	0.0178 (4)
O11	0.7121 (2)	0.0139 (2)	0.29536 (17)	0.0213 (4)
H11A	0.643 (3)	0.014 (4)	0.316 (3)	0.032*
H11B	0.719 (4)	−0.056 (2)	0.281 (3)	0.032*
O15	0.6328 (2)	0.2178 (2)	0.53415 (19)	0.0310 (5)
O16	0.6467 (3)	0.2508 (4)	0.6961 (2)	0.0585 (10)
O17	0.4642 (3)	0.2055 (3)	0.6078 (3)	0.0426 (7)
O18	1.2479 (2)	0.3217 (2)	0.37422 (18)	0.0241 (5)
H18A	1.266 (4)	0.378 (3)	0.421 (2)	0.036*
H18B	1.192 (3)	0.336 (4)	0.336 (3)	0.036*
O19	0.3869 (2)	0.1932 (2)	0.26751 (17)	0.0235 (5)
H19A	0.338 (3)	0.154 (4)	0.216 (2)	0.035*
H19B	0.348 (4)	0.234 (3)	0.297 (3)	0.035*
O20	0.8216 (2)	0.2497 (2)	−0.11207 (19)	0.0283 (5)
H20A	0.844 (4)	0.221 (4)	−0.165 (2)	0.042*
H20B	0.839 (4)	0.3266 (19)	−0.113 (4)	0.042*
O21	0.6426 (3)	0.6180 (2)	0.0939 (2)	0.0357 (6)
H21A	0.599 (4)	0.629 (5)	0.043 (3)	0.054*
H21B	0.685 (4)	0.572 (4)	0.075 (4)	0.054*
O22	0.8172 (4)	0.5178 (3)	0.0465 (3)	0.0538 (9)
H22A	0.824 (6)	0.514 (6)	−0.0174 (18)	0.081*
H22B	0.850 (6)	0.468 (5)	0.076 (4)	0.081*
O24	0.7763 (2)	−0.1972 (2)	0.24123 (17)	0.0213 (4)
H24A	0.805 (4)	−0.228 (4)	0.289 (2)	0.032*
H24B	0.739 (4)	−0.264 (2)	0.206 (3)	0.032*
O25	0.5128 (2)	0.0541 (2)	0.36852 (19)	0.0266 (5)
H25A	0.477 (4)	0.102 (4)	0.340 (3)	0.040*
H25B	0.541 (4)	0.095 (4)	0.425 (2)	0.040*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0204 (13)	0.0140 (12)	0.0141 (12)	0.0016 (10)	0.0034 (10)	0.0020 (9)
C2	0.0288 (15)	0.0167 (13)	0.0115 (12)	0.0042 (11)	0.0009 (11)	−0.0007 (10)
C3	0.0241 (14)	0.0139 (12)	0.0158 (12)	0.0040 (11)	0.0028 (11)	−0.0003 (10)
C4	0.0318 (17)	0.0204 (14)	0.0204 (14)	0.0120 (13)	0.0012 (12)	−0.0030 (11)
C5	0.0200 (13)	0.0194 (13)	0.0147 (12)	0.0062 (11)	0.0016 (10)	0.0022 (10)
C6	0.0246 (15)	0.0286 (15)	0.0134 (12)	0.0143 (12)	−0.0004 (11)	−0.0001 (11)
C7	0.0177 (13)	0.0158 (12)	0.0133 (12)	0.0046 (10)	0.0019 (10)	0.0000 (9)
C8	0.0252 (14)	0.0177 (13)	0.0133 (12)	0.0089 (11)	0.0009 (10)	−0.0027 (10)
C9	0.0164 (12)	0.0152 (12)	0.0142 (12)	0.0040 (10)	0.0010 (10)	0.0024 (9)
C10	0.0190 (13)	0.0186 (13)	0.0181 (13)	0.0075 (11)	−0.0003 (10)	0.0037 (10)
C11	0.019 (4)	0.021 (3)	0.016 (3)	0.006 (3)	0.003 (3)	−0.002 (2)
O12	0.019 (4)	0.027 (2)	0.030 (3)	0.000 (3)	0.002 (3)	0.011 (2)
O13	0.021 (4)	0.023 (3)	0.019 (4)	0.003 (3)	−0.001 (3)	0.005 (3)
O14	0.027 (4)	0.027 (3)	0.028 (3)	−0.003 (3)	0.003 (3)	0.006 (2)
O23	0.047 (5)	0.050 (5)	0.203 (13)	0.028 (4)	−0.018 (6)	−0.007 (6)
C11B	0.024 (4)	0.019 (2)	0.017 (3)	0.005 (3)	0.002 (3)	−0.005 (2)
O12B	0.026 (4)	0.027 (2)	0.024 (3)	−0.003 (3)	0.001 (3)	0.011 (2)
O13B	0.022 (4)	0.020 (3)	0.023 (5)	0.001 (3)	−0.005 (3)	0.001 (3)
O14B	0.036 (4)	0.026 (3)	0.020 (3)	−0.010 (3)	0.009 (3)	−0.002 (2)
N1	0.0251 (13)	0.0185 (11)	0.0115 (10)	0.0072 (10)	0.0040 (9)	−0.0032 (9)
N2	0.0282 (14)	0.0270 (13)	0.0164 (12)	0.0092 (11)	−0.0003 (10)	−0.0054 (10)
N3	0.0264 (13)	0.0174 (11)	0.0168 (11)	0.0109 (10)	0.0008 (10)	0.0010 (9)
N4	0.056 (2)	0.0267 (14)	0.0207 (13)	0.0252 (14)	−0.0001 (13)	0.0008 (11)
N5	0.0210 (12)	0.0238 (12)	0.0102 (10)	0.0106 (10)	−0.0005 (9)	−0.0003 (9)
N6	0.0215 (12)	0.0231 (12)	0.0123 (10)	0.0076 (10)	0.0003 (9)	−0.0002 (9)
N7	0.0213 (12)	0.0164 (11)	0.0131 (10)	0.0106 (9)	−0.0004 (9)	−0.0011 (8)
N8	0.0221 (12)	0.0195 (12)	0.0177 (11)	0.0098 (10)	−0.0006 (9)	−0.0011 (9)
N9	0.0177 (11)	0.0159 (11)	0.0130 (10)	0.0054 (9)	−0.0021 (8)	0.0007 (8)
N10	0.0225 (13)	0.0275 (13)	0.0199 (12)	0.0088 (11)	−0.0050 (10)	0.0003 (10)
N11	0.0271 (14)	0.0270 (14)	0.0263 (14)	0.0020 (11)	0.0040 (11)	0.0032 (11)
Cu1	0.01724 (16)	0.01941 (16)	0.01143 (15)	0.00596 (13)	−0.00150 (12)	−0.00123 (12)
Cu2	0.02216 (18)	0.01550 (16)	0.01149 (15)	0.00558 (13)	0.00110 (13)	−0.00207 (12)
Cu3	0.02855 (19)	0.01987 (17)	0.01282 (15)	0.01423 (15)	−0.00091 (14)	−0.00107 (13)
Cu4	0.01952 (17)	0.02133 (17)	0.01026 (15)	0.01014 (14)	−0.00125 (12)	−0.00179 (12)
Cu5	0.01973 (17)	0.01519 (15)	0.01250 (15)	0.00790 (13)	−0.00066 (12)	−0.00106 (12)
Gd1	0.01725 (7)	0.01235 (6)	0.00865 (6)	0.00532 (5)	−0.00028 (4)	−0.00060 (4)
O1	0.0234 (11)	0.0277 (11)	0.0114 (9)	0.0128 (9)	−0.0023 (8)	−0.0074 (8)
O2	0.0218 (10)	0.0217 (10)	0.0135 (9)	0.0064 (8)	−0.0011 (8)	0.0008 (8)
O3	0.0256 (11)	0.0203 (10)	0.0129 (9)	0.0124 (8)	0.0000 (8)	0.0001 (7)
O4	0.0254 (11)	0.0190 (10)	0.0159 (9)	0.0065 (8)	0.0025 (8)	−0.0031 (8)
O5	0.0281 (11)	0.0277 (11)	0.0102 (9)	0.0170 (9)	−0.0026 (8)	−0.0049 (8)
O6	0.0283 (11)	0.0263 (11)	0.0142 (9)	0.0169 (9)	−0.0010 (8)	0.0004 (8)
O7	0.0251 (11)	0.0193 (10)	0.0150 (9)	0.0139 (8)	−0.0021 (8)	−0.0036 (7)
O8	0.0233 (10)	0.0213 (10)	0.0119 (9)	0.0107 (8)	−0.0013 (8)	−0.0025 (7)
O9	0.0198 (10)	0.0170 (9)	0.0125 (9)	0.0083 (8)	−0.0047 (7)	−0.0016 (7)
O10	0.0209 (10)	0.0176 (9)	0.0163 (9)	0.0090 (8)	0.0005 (8)	0.0003 (7)
O11	0.0194 (10)	0.0185 (10)	0.0254 (11)	0.0043 (8)	0.0041 (9)	0.0024 (8)
O15	0.0318 (13)	0.0314 (13)	0.0280 (12)	0.0052 (10)	0.0081 (10)	0.0059 (10)
O16	0.0445 (18)	0.087 (3)	0.0234 (14)	−0.0098 (17)	0.0007 (13)	0.0051 (15)
O17	0.0271 (13)	0.0321 (14)	0.070 (2)	0.0112 (11)	0.0091 (13)	−0.0005 (14)
O18	0.0274 (12)	0.0211 (11)	0.0230 (11)	0.0090 (9)	−0.0002 (9)	−0.0060 (9)
O19	0.0230 (11)	0.0295 (12)	0.0177 (10)	0.0101 (9)	−0.0006 (8)	−0.0041 (9)
O20	0.0317 (13)	0.0248 (12)	0.0303 (13)	0.0103 (10)	0.0089 (10)	0.0017 (10)
O21	0.0499 (17)	0.0296 (13)	0.0284 (13)	0.0187 (12)	−0.0119 (12)	0.0000 (10)
O22	0.091 (3)	0.0470 (18)	0.0389 (17)	0.0372 (18)	0.0265 (18)	0.0148 (15)
O24	0.0249 (11)	0.0196 (10)	0.0181 (10)	0.0060 (9)	−0.0014 (8)	0.0027 (8)
O25	0.0262 (12)	0.0255 (12)	0.0279 (12)	0.0083 (10)	0.0031 (10)	0.0008 (9)

Geometric parameters (Å, º) top

C1—O2	1.296 (4)	N5—Cu4	1.906 (2)
C1—N1	1.303 (4)	N6—Cu4	2.005 (2)
C1—C2	1.501 (4)	N6—H6A	0.9100
C2—N2	1.488 (4)	N6—H6B	0.9100
C2—H2C	0.9900	N7—O7	1.397 (3)
C2—H2D	0.9900	N7—Cu5	1.901 (2)
C3—O4	1.295 (4)	N8—Cu5	2.022 (2)
C3—N3	1.298 (4)	N8—H8A	0.9100
C3—C4	1.505 (4)	N8—H8B	0.9100
C4—N4	1.483 (4)	N9—O9	1.398 (3)
C4—H4C	0.9900	N9—Cu1	1.898 (2)
C4—H4D	0.9900	N10—Cu1	2.016 (3)
C5—O6	1.298 (4)	N10—H10A	0.9100
C5—N5	1.302 (4)	N10—H10B	0.9100
C5—C6	1.506 (4)	N11—O17	1.223 (4)
C6—N6	1.485 (4)	N11—O15	1.255 (4)
C6—H6C	0.9900	N11—O16	1.266 (4)
C6—H6D	0.9900	Cu1—O1	1.929 (2)
C7—N7	1.292 (4)	Cu1—O2	1.949 (2)
C7—O8	1.301 (3)	Cu1—O18	2.470 (3)
C7—C8	1.509 (4)	Cu2—O3	1.929 (2)
C8—N8	1.490 (4)	Cu2—O4	1.939 (2)
C8—H8C	0.9900	Cu2—O15	2.469 (3)
C8—H8D	0.9900	Cu3—O5	1.935 (2)
C9—O10	1.294 (3)	Cu3—O6	1.952 (2)
C9—N9	1.298 (4)	Cu3—O19	2.444 (2)
C9—C10	1.506 (4)	Cu4—O7	1.938 (2)
C10—N10	1.482 (4)	Cu4—O8	1.953 (2)
C10—H10C	0.9900	Cu4—O20	2.401 (3)
C10—H10D	0.9900	Cu5—O9	1.931 (2)
C11—O14	1.252 (9)	Cu5—O10	1.939 (2)
C11—O12	1.284 (9)	Cu5—O24	2.449 (2)
C11—O13	1.307 (10)	Gd1—O11	2.359 (2)
C11—Gd1	2.733 (10)	Gd1—O3	2.381 (2)
O12—Gd1	2.317 (11)	Gd1—O7	2.408 (2)
O13—Gd1	2.288 (17)	Gd1—O9	2.414 (2)
O23—H23A	0.851 (19)	Gd1—O1	2.457 (2)
O23—H23B	0.84 (2)	Gd1—O5	2.483 (2)
C11B—O14B	1.253 (9)	O11—H11A	0.840 (19)
C11B—O13B	1.307 (10)	O11—H11B	0.838 (19)
C11B—O12B	1.310 (10)	O18—H18A	0.829 (19)
C11B—Gd1	2.857 (10)	O18—H18B	0.830 (19)
O12B—Gd1	2.396 (10)	O19—H19A	0.844 (19)
O13B—Gd1	2.388 (17)	O19—H19B	0.836 (19)
N1—O1	1.389 (3)	O20—H20A	0.847 (19)
N1—Cu2	1.902 (3)	O20—H20B	0.849 (19)
N2—Cu2	1.985 (3)	O21—H21A	0.840 (19)
N2—H2A	0.9100	O21—H21B	0.849 (19)
N2—H2B	0.9100	O22—H22A	0.86 (2)
N3—O3	1.399 (3)	O22—H22B	0.87 (2)
N3—Cu3	1.910 (3)	O24—H24A	0.833 (19)
N4—Cu3	2.010 (3)	O24—H24B	0.839 (19)
N4—H4A	0.9100	O25—H25A	0.861 (19)
N4—H4B	0.9100	O25—H25B	0.845 (19)
N5—O5	1.397 (3)

O2—C1—N1	123.2 (3)	O4—Cu2—O15	86.11 (9)
O2—C1—C2	121.7 (3)	N2—Cu2—O15	93.88 (11)
N1—C1—C2	115.1 (3)	N3—Cu3—O5	90.98 (10)
N2—C2—C1	109.7 (2)	N3—Cu3—O6	168.46 (11)
N2—C2—H2C	109.7	O5—Cu3—O6	85.44 (9)
C1—C2—H2C	109.7	N3—Cu3—N4	82.70 (12)
N2—C2—H2D	109.7	O5—Cu3—N4	172.15 (13)
C1—C2—H2D	109.7	O6—Cu3—N4	99.85 (11)
H2C—C2—H2D	108.2	N3—Cu3—O19	97.56 (10)
O4—C3—N3	124.2 (3)	O5—Cu3—O19	97.57 (9)
O4—C3—C4	120.7 (3)	O6—Cu3—O19	93.78 (9)
N3—C3—C4	115.1 (3)	N4—Cu3—O19	87.90 (12)
N4—C4—C3	110.7 (2)	N5—Cu4—O7	91.39 (9)
N4—C4—H4C	109.5	N5—Cu4—O8	161.67 (10)
C3—C4—H4C	109.5	O7—Cu4—O8	84.56 (8)
N4—C4—H4D	109.5	N5—Cu4—N6	83.88 (10)
C3—C4—H4D	109.5	O7—Cu4—N6	174.00 (10)
H4C—C4—H4D	108.1	O8—Cu4—N6	98.79 (9)
O6—C5—N5	124.4 (3)	N5—Cu4—O20	101.61 (10)
O6—C5—C6	120.0 (3)	O7—Cu4—O20	99.20 (9)
N5—C5—C6	115.6 (3)	O8—Cu4—O20	96.69 (9)
N6—C6—C5	111.2 (2)	N6—Cu4—O20	85.40 (10)
N6—C6—H6C	109.4	N7—Cu5—O9	89.59 (9)
C5—C6—H6C	109.4	N7—Cu5—O10	170.23 (10)
N6—C6—H6D	109.4	O9—Cu5—O10	85.57 (8)
C5—C6—H6D	109.4	N7—Cu5—N8	83.14 (10)
H6C—C6—H6D	108.0	O9—Cu5—N8	169.38 (10)
N7—C7—O8	123.8 (3)	O10—Cu5—N8	100.42 (9)
N7—C7—C8	116.0 (2)	N7—Cu5—O24	95.81 (9)
O8—C7—C8	120.2 (2)	O9—Cu5—O24	87.44 (8)
N8—C8—C7	110.4 (2)	O10—Cu5—O24	92.45 (8)
N8—C8—H8C	109.6	N8—Cu5—O24	100.96 (9)
C7—C8—H8C	109.6	O13—Gd1—O12	56.4 (3)
N8—C8—H8D	109.6	O13—Gd1—O11	153.9 (3)
C7—C8—H8D	109.6	O12—Gd1—O11	149.4 (2)
H8C—C8—H8D	108.1	O13—Gd1—O3	96.0 (6)
O10—C9—N9	123.9 (3)	O12—Gd1—O3	86.3 (3)
O10—C9—C10	120.3 (2)	O11—Gd1—O3	91.62 (8)
N9—C9—C10	115.8 (2)	O11—Gd1—O13B	147.7 (3)
N10—C10—C9	110.9 (2)	O3—Gd1—O13B	95.0 (5)
N10—C10—H10C	109.5	O11—Gd1—O12B	156.6 (2)
C9—C10—H10C	109.5	O3—Gd1—O12B	94.1 (3)
N10—C10—H10D	109.5	O13B—Gd1—O12B	54.1 (3)
C9—C10—H10D	109.5	O13—Gd1—O7	102.1 (5)
H10C—C10—H10D	108.0	O12—Gd1—O7	79.3 (3)
O14—C11—O12	123.6 (9)	O11—Gd1—O7	85.23 (8)
O14—C11—O13	122.2 (9)	O3—Gd1—O7	144.85 (7)
O12—C11—O13	114.2 (9)	O13B—Gd1—O7	106.2 (5)
O14—C11—Gd1	178.1 (8)	O12B—Gd1—O7	77.1 (3)
O12—C11—Gd1	57.7 (6)	O13—Gd1—O9	82.7 (5)
O13—C11—Gd1	56.5 (7)	O12—Gd1—O9	122.3 (2)
C11—O12—Gd1	94.3 (7)	O11—Gd1—O9	75.95 (7)
C11—O13—Gd1	95.0 (8)	O3—Gd1—O9	141.57 (7)
H23A—O23—H23B	119 (10)	O13B—Gd1—O9	79.4 (5)
O14B—C11B—O13B	123.7 (10)	O12B—Gd1—O9	111.8 (3)
O14B—C11B—O12B	123.8 (9)	O7—Gd1—O9	71.27 (6)
O13B—C11B—O12B	112.5 (9)	O13—Gd1—O1	76.8 (3)
O14B—C11B—Gd1	179.5 (9)	O12—Gd1—O1	125.7 (3)
O13B—C11B—Gd1	56.1 (7)	O11—Gd1—O1	81.98 (8)
O12B—C11B—Gd1	56.4 (5)	O3—Gd1—O1	71.71 (7)
C11B—O12B—Gd1	96.5 (7)	O13B—Gd1—O1	70.3 (3)
C11B—O13B—Gd1	96.9 (8)	O12B—Gd1—O1	121.3 (2)
C1—N1—O1	116.0 (2)	O7—Gd1—O1	141.68 (7)
C1—N1—Cu2	119.25 (19)	O9—Gd1—O1	70.62 (7)
O1—N1—Cu2	124.58 (18)	O13—Gd1—O5	125.4 (3)
C2—N2—Cu2	111.49 (18)	O12—Gd1—O5	69.6 (2)
C2—N2—H2A	109.3	O11—Gd1—O5	80.69 (8)
Cu2—N2—H2A	109.3	O3—Gd1—O5	72.08 (7)
C2—N2—H2B	109.3	O13B—Gd1—O5	131.3 (3)
Cu2—N2—H2B	109.3	O12B—Gd1—O5	79.6 (2)
H2A—N2—H2B	108.0	O7—Gd1—O5	72.87 (7)
C3—N3—O3	115.2 (2)	O9—Gd1—O5	138.36 (7)
C3—N3—Cu3	118.8 (2)	O1—Gd1—O5	139.11 (7)
O3—N3—Cu3	125.28 (18)	O13—Gd1—C11	28.5 (3)
C4—N4—Cu3	110.4 (2)	O12—Gd1—C11	27.9 (2)
C4—N4—H4A	109.6	O11—Gd1—C11	175.0 (3)
Cu3—N4—H4A	109.6	O3—Gd1—C11	92.2 (3)
C4—N4—H4B	109.6	O7—Gd1—C11	89.8 (3)
Cu3—N4—H4B	109.6	O9—Gd1—C11	102.9 (2)
H4A—N4—H4B	108.1	O1—Gd1—C11	102.3 (2)
C5—N5—O5	115.2 (2)	O5—Gd1—C11	97.4 (2)
C5—N5—Cu4	117.2 (2)	O11—Gd1—C11B	171.5 (2)
O5—N5—Cu4	126.74 (18)	O3—Gd1—C11B	95.6 (2)
C6—N6—Cu4	109.20 (18)	O13B—Gd1—C11B	27.0 (2)
C6—N6—H6A	109.8	O12B—Gd1—C11B	27.1 (2)
Cu4—N6—H6A	109.8	O7—Gd1—C11B	91.4 (2)
C6—N6—H6B	109.8	O9—Gd1—C11B	95.6 (2)
Cu4—N6—H6B	109.8	O1—Gd1—C11B	96.0 (2)
H6A—N6—H6B	108.3	O5—Gd1—C11B	105.8 (2)
C7—N7—O7	115.2 (2)	N1—O1—Cu1	107.85 (16)
C7—N7—Cu5	119.6 (2)	N1—O1—Gd1	123.02 (16)
O7—N7—Cu5	125.20 (17)	Cu1—O1—Gd1	125.67 (9)
C8—N8—Cu5	110.78 (17)	C1—O2—Cu1	107.29 (17)
C8—N8—H8A	109.5	N3—O3—Cu2	107.71 (15)
Cu5—N8—H8A	109.5	N3—O3—Gd1	123.98 (15)
C8—N8—H8B	109.5	Cu2—O3—Gd1	128.20 (10)
Cu5—N8—H8B	109.5	C3—O4—Cu2	106.89 (18)
H8A—N8—H8B	108.1	N5—O5—Cu3	107.81 (16)
C9—N9—O9	115.5 (2)	N5—O5—Gd1	120.57 (16)
C9—N9—Cu1	118.54 (19)	Cu3—O5—Gd1	123.24 (10)
O9—N9—Cu1	125.47 (17)	C5—O6—Cu3	106.60 (18)
C10—N10—Cu1	110.37 (18)	N7—O7—Cu4	107.98 (15)
C10—N10—H10A	109.6	N7—O7—Gd1	124.61 (15)
Cu1—N10—H10A	109.6	Cu4—O7—Gd1	125.52 (9)
C10—N10—H10B	109.6	C7—O8—Cu4	106.96 (17)
Cu1—N10—H10B	109.6	N9—O9—Cu5	107.74 (15)
H10A—N10—H10B	108.1	N9—O9—Gd1	125.05 (15)
O17—N11—O15	122.5 (3)	Cu5—O9—Gd1	126.68 (9)
O17—N11—O16	120.9 (3)	C9—O10—Cu5	107.26 (17)
O15—N11—O16	116.5 (3)	Gd1—O11—H11A	120 (3)
N9—Cu1—O1	89.32 (9)	Gd1—O11—H11B	122 (3)
N9—Cu1—O2	172.09 (10)	H11A—O11—H11B	115 (4)
O1—Cu1—O2	85.28 (9)	N11—O15—Cu2	124.8 (2)
N9—Cu1—N10	83.70 (10)	Cu1—O18—H18A	101 (3)
O1—Cu1—N10	165.70 (11)	Cu1—O18—H18B	94 (3)
O2—Cu1—N10	100.27 (10)	H18A—O18—H18B	104 (4)
N9—Cu1—O18	91.70 (9)	Cu3—O19—H19A	105 (3)
O1—Cu1—O18	95.08 (9)	Cu3—O19—H19B	111 (3)
O2—Cu1—O18	94.54 (8)	H19A—O19—H19B	106 (4)
N10—Cu1—O18	97.58 (10)	Cu4—O20—H20A	109 (3)
N1—Cu2—O3	90.48 (9)	Cu4—O20—H20B	140 (3)
N1—Cu2—O4	168.71 (10)	H20A—O20—H20B	108 (4)
O3—Cu2—O4	85.63 (9)	H21A—O21—H21B	110 (5)
N1—Cu2—N2	82.87 (11)	H22A—O22—H22B	111 (6)
O3—Cu2—N2	173.32 (10)	Cu5—O24—H24A	109 (3)
O4—Cu2—N2	100.83 (10)	Cu5—O24—H24B	107 (3)
N1—Cu2—O15	104.38 (10)	H24A—O24—H24B	95 (4)
O3—Cu2—O15	88.22 (9)	H25A—O25—H25B	100 (4)

O2—C1—C2—N2	−169.6 (3)	C10—C9—N9—Cu1	−9.9 (3)
N1—C1—C2—N2	9.2 (4)	C9—C10—N10—Cu1	−1.5 (3)
O4—C3—C4—N4	178.1 (3)	C9—N9—Cu1—O1	−160.3 (2)
N3—C3—C4—N4	−2.6 (4)	O9—N9—Cu1—O1	11.1 (2)
O6—C5—C6—N6	−179.6 (3)	C9—N9—Cu1—N10	7.2 (2)
N5—C5—C6—N6	0.9 (4)	O9—N9—Cu1—N10	178.6 (2)
N7—C7—C8—N8	−3.0 (4)	C9—N9—Cu1—O18	104.6 (2)
O8—C7—C8—N8	177.5 (2)	O9—N9—Cu1—O18	−84.0 (2)
O10—C9—C10—N10	−173.5 (3)	C1—N1—O1—Cu1	−6.3 (3)
N9—C9—C10—N10	7.1 (4)	Cu2—N1—O1—Cu1	178.65 (14)
O14—C11—O12—Gd1	178.3 (11)	C1—N1—O1—Gd1	−166.34 (19)
O13—C11—O12—Gd1	−3.1 (13)	Cu2—N1—O1—Gd1	18.6 (3)
O14—C11—O13—Gd1	−178.2 (10)	N1—C1—O2—Cu1	1.7 (3)
O12—C11—O13—Gd1	3.2 (13)	C2—C1—O2—Cu1	−179.6 (2)
O14B—C11B—O12B—Gd1	−179.5 (10)	C3—N3—O3—Cu2	4.8 (3)
O13B—C11B—O12B—Gd1	−1.7 (13)	Cu3—N3—O3—Cu2	−165.22 (15)
O14B—C11B—O13B—Gd1	179.5 (10)	C3—N3—O3—Gd1	−171.5 (2)
O12B—C11B—O13B—Gd1	1.7 (13)	Cu3—N3—O3—Gd1	18.4 (3)
O2—C1—N1—O1	3.2 (4)	N3—C3—O4—Cu2	−3.9 (4)
C2—C1—N1—O1	−175.5 (2)	C4—C3—O4—Cu2	175.3 (2)
O2—C1—N1—Cu2	178.5 (2)	C5—N5—O5—Cu3	−6.9 (3)
C2—C1—N1—Cu2	−0.2 (3)	Cu4—N5—O5—Cu3	161.96 (15)
C1—C2—N2—Cu2	−13.4 (3)	C5—N5—O5—Gd1	−156.0 (2)
O4—C3—N3—O3	−0.6 (4)	Cu4—N5—O5—Gd1	12.8 (3)
C4—C3—N3—O3	−179.9 (2)	N5—C5—O6—Cu3	3.2 (4)
O4—C3—N3—Cu3	170.1 (2)	C6—C5—O6—Cu3	−176.2 (2)
C4—C3—N3—Cu3	−9.1 (4)	C7—N7—O7—Cu4	9.2 (3)
C3—C4—N4—Cu3	11.8 (3)	Cu5—N7—O7—Cu4	−171.09 (14)
O6—C5—N5—O5	2.5 (4)	C7—N7—O7—Gd1	174.27 (19)
C6—C5—N5—O5	−178.0 (2)	Cu5—N7—O7—Gd1	−6.0 (3)
O6—C5—N5—Cu4	−167.4 (2)	N7—C7—O8—Cu4	−8.2 (3)
C6—C5—N5—Cu4	12.1 (4)	C8—C7—O8—Cu4	171.2 (2)
C5—C6—N6—Cu4	−12.1 (3)	C9—N9—O9—Cu5	1.1 (3)
O8—C7—N7—O7	−0.7 (4)	Cu1—N9—O9—Cu5	−170.58 (13)
C8—C7—N7—O7	179.9 (2)	C9—N9—O9—Gd1	173.21 (19)
O8—C7—N7—Cu5	179.6 (2)	Cu1—N9—O9—Gd1	1.5 (3)
C8—C7—N7—Cu5	0.2 (4)	N9—C9—O10—Cu5	1.1 (3)
C7—C8—N8—Cu5	4.2 (3)	C10—C9—O10—Cu5	−178.2 (2)
O10—C9—N9—O9	−1.6 (4)	O17—N11—O15—Cu2	131.9 (3)
C10—C9—N9—O9	177.8 (2)	O16—N11—O15—Cu2	−50.5 (4)
O10—C9—N9—Cu1	170.7 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O23—H23A···O16ⁱ	0.85 (2)	1.81 (2)	2.642 (10)	165 (10)
O23—H23B···O14	0.84 (2)	1.90 (2)	2.644 (10)	148 (5)
N2—H2A···O13ⁱ	0.91	2.17	3.00 (2)	151
N2—H2A···O13Bⁱ	0.91	2.06	2.92 (2)	157
N2—H2B···O16	0.91	2.25	3.068 (4)	150
N4—H4A···O21	0.91	2.08	2.932 (4)	155
N4—H4B···O23ⁱⁱ	0.91	1.91	2.604 (8)	132
N6—H6A···O16ⁱⁱⁱ	0.91	2.24	3.061 (4)	150
N6—H6B···N5^iv	0.91	2.53	3.268 (4)	139
N6—H6B···O5^iv	0.91	2.46	3.357 (4)	171
N8—H8A···O7^v	0.91	2.51	3.299 (4)	145
N8—H8A···O20^v	0.91	2.39	3.005 (4)	125
N8—H8B···O22^vi	0.91	2.15	3.033 (4)	163
N10—H10A···O17^vii	0.91	2.22	3.025 (4)	146
N10—H10B···O11^viii	0.91	2.41	3.192 (4)	145
O11—H11A···O25	0.84 (2)	1.84 (2)	2.662 (3)	166 (4)
O11—H11B···O24	0.84 (2)	1.98 (2)	2.798 (3)	167 (4)
O18—H18A···O4ⁱ	0.83 (2)	1.99 (2)	2.813 (3)	169 (4)
O18—H18B···O13	0.83 (2)	2.07 (2)	2.886 (14)	170 (4)
O18—H18B···O13B	0.83 (2)	1.79 (2)	2.612 (14)	169 (5)
O19—H19A···O8^iv	0.84 (2)	1.89 (2)	2.719 (3)	167 (4)
O19—H19B···O18ⁱⁱ	0.84 (2)	2.01 (2)	2.847 (3)	176 (4)
O20—H20A···O10^v	0.85 (2)	1.96 (3)	2.750 (3)	156 (5)
O20—H20B···O14^ix	0.85 (2)	2.17 (2)	2.997 (9)	165 (4)
O20—H20B···O14B^ix	0.85 (2)	2.24 (2)	3.075 (9)	169 (4)
O21—H21A···O6^x	0.84 (2)	2.00 (2)	2.813 (3)	163 (5)
O21—H21B···O22	0.85 (2)	1.83 (2)	2.650 (5)	162 (5)
O22—H22A···O14^ix	0.86 (2)	1.96 (4)	2.742 (9)	150 (6)
O22—H22A···O14B^ix	0.86 (2)	1.89 (3)	2.730 (8)	166 (6)
O22—H22B···O12	0.87 (2)	1.74 (3)	2.594 (12)	168 (6)
O22—H22B···O14	0.87 (2)	2.49 (5)	3.137 (9)	131 (5)
O22—H22B···O12B	0.87 (2)	1.94 (2)	2.803 (11)	176 (6)
O24—H24A···O2^viii	0.83 (2)	1.98 (2)	2.785 (3)	163 (4)
O24—H24B···O21^vi	0.84 (2)	1.95 (2)	2.755 (3)	161 (4)
O25—H25A···O19	0.86 (2)	1.92 (2)	2.773 (3)	173 (5)
O25—H25B···O15	0.85 (2)	1.93 (2)	2.754 (4)	166 (4)

Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) x−1, y, z; (iii) x, y, z−1; (iv) −x+1, −y, −z; (v) −x+2, −y, −z; (vi) x, y−1, z; (vii) x+1, y, z; (viii) −x+2, −y, −z+1; (ix) −x+2, −y+1, −z; (x) −x+1, −y+1, −z.

Pentaaquacarbonatopentakis(glycine hydroxamato)nitratopentacopper(II)dysprosium(III) 3.28-hydrate (Complex_2) top

Crystal data top

[Cu₅Dy(C₂H₄N₂O₂)₅(CO₃)(NO₃)(H₂O)₅]·3.28H₂O	Z = 2
M_r = 1191.77	F(000) = 1170
Triclinic, P1	D_x = 2.460 Mg m⁻³
a = 11.1083 (5) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.4991 (5) Å	Cell parameters from 9708 reflections
c = 13.2894 (6) Å	θ = 3.1–28.6°
α = 93.9235 (16)°	µ = 5.65 mm⁻¹
β = 94.7713 (17)°	T = 150 K
γ = 107.1470 (17)°	Block, blue
V = 1608.73 (13) Å³	0.25 × 0.21 × 0.11 mm

Data collection top

Bruker AXS D8 Quest CMOS diffractometer	8274 independent reflections
Radiation source: sealed tube X-ray source	6997 reflections with I > 2σ(I)
Triumph curved graphite crystal monochromator	R_int = 0.048
ω and phi scans	θ_max = 28.7°, θ_min = 3.1°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −14→14
T_min = 0.648, T_max = 0.754	k = −15→15
74286 measured reflections	l = −17→17

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.031	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.076	w = 1/[σ²(F_o²) + (0.0283P)² + 7.9239P] where P = (F_o² + 2F_c²)/3
S = 1.08	(Δ/σ)_max = 0.001
8274 reflections	Δρ_max = 0.99 e Å⁻³
564 parameters	Δρ_min = −1.26 e Å⁻³
133 restraints	Extinction correction: SHELXL-2018/3 (Sheldrick 2015), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00073 (12)

Special details top

Refinement. The structure is isotypic to its Gd analogue, AVP815, and was solved by isomorphous replacement. A water molecule is partially occupied, inducing disorder for the nearby carbonate anion. The two disordered moieties were restrained to have similar geometries. Uij components of ADPs for disordered atoms closer to each other than 2.0 Angstrom were restrained to be similar. The distance of the water oxygen to one of the carbonate oxygen atoms was restrained to be at least 2.75 Angstrom for the moiety that contains the water molecule.

Water H atom positions were refined and O-H and H···H distances were restrained to 0.84 (2) and 1.36 (2) Angstrom, respectively. The water H atom positions of the disordered moiety were further restrained based on hydrogen bonding considerations. In the final refinement cycles the partially occupied H atoms were set to ride on their carrier oxygen atom. Subject to these conditions the occupancy ratio refined to 0.280 (14) to 0.720 (14).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
C1	1.0262 (4)	0.3060 (4)	0.5723 (3)	0.0144 (7)
C2	1.0110 (4)	0.3901 (4)	0.6587 (3)	0.0179 (8)
H2C	1.008419	0.349470	0.722153	0.022*
H2D	1.084243	0.465387	0.668060	0.022*
C3	0.6572 (4)	0.4541 (4)	0.3859 (3)	0.0165 (8)
C4	0.5587 (4)	0.5142 (4)	0.3520 (3)	0.0212 (9)
H4C	0.489368	0.495117	0.396268	0.025*
H4D	0.597517	0.604064	0.358082	0.025*
C5	0.5288 (4)	0.2157 (4)	0.0107 (3)	0.0161 (8)
C6	0.4890 (4)	0.1761 (4)	−0.0999 (3)	0.0191 (8)
H6C	0.395896	0.138873	−0.110990	0.023*
H6D	0.511706	0.248396	−0.138941	0.023*
C7	0.8143 (4)	−0.0808 (4)	−0.0313 (3)	0.0137 (7)
C8	0.8543 (4)	−0.1927 (4)	−0.0548 (3)	0.0167 (8)
H8C	0.778401	−0.265253	−0.068936	0.020*
H8D	0.899991	−0.183663	−0.116018	0.020*
C9	1.1083 (4)	−0.0375 (4)	0.3189 (3)	0.0139 (7)
C10	1.2074 (4)	−0.0386 (4)	0.4026 (3)	0.0174 (8)
H10C	1.185344	−0.119834	0.429057	0.021*
H10D	1.290439	−0.024000	0.375591	0.021*
C11	0.999 (2)	0.391 (2)	0.165 (2)	0.022 (3)	0.280 (14)
O12	0.8801 (17)	0.350 (2)	0.1404 (16)	0.023 (3)	0.280 (14)
O13	1.045 (3)	0.334 (3)	0.2344 (18)	0.024 (3)	0.280 (14)
O14	1.0694 (15)	0.4834 (17)	0.1307 (14)	0.029 (4)	0.280 (14)
O23	1.3131 (16)	0.5344 (19)	0.198 (2)	0.111 (13)	0.280 (14)
H23A	1.298662	0.593330	0.230452	0.167*	0.280 (14)
H23B	1.243199	0.486108	0.171835	0.167*	0.280 (14)
C11B	1.0347 (8)	0.3924 (8)	0.1751 (7)	0.0201 (16)	0.720 (14)
O12B	0.9201 (8)	0.3484 (8)	0.1307 (6)	0.0274 (15)	0.720 (14)
O13B	1.0523 (12)	0.3364 (10)	0.2565 (6)	0.0217 (15)	0.720 (14)
O14B	1.1204 (8)	0.4780 (6)	0.1476 (5)	0.0304 (17)	0.720 (14)
N1	0.9464 (3)	0.2917 (3)	0.4929 (2)	0.0162 (7)
N2	0.8921 (4)	0.4220 (4)	0.6368 (3)	0.0227 (8)
H2A	0.907785	0.503939	0.651335	0.027*
H2B	0.834002	0.382947	0.677305	0.027*
N3	0.6771 (4)	0.3763 (3)	0.3186 (3)	0.0180 (7)
N4	0.5064 (4)	0.4693 (4)	0.2446 (3)	0.0269 (9)
H4A	0.532037	0.531124	0.204512	0.032*
H4B	0.420256	0.445419	0.239699	0.032*
N5	0.6108 (3)	0.1700 (3)	0.0538 (2)	0.0163 (7)
N6	0.5516 (3)	0.0862 (3)	−0.1372 (2)	0.0163 (7)
H6A	0.583639	0.107148	−0.196466	0.020*
H6B	0.494036	0.010417	−0.148883	0.020*
N7	0.8515 (3)	−0.0248 (3)	0.0586 (2)	0.0140 (6)
N8	0.9383 (3)	−0.2107 (3)	0.0324 (2)	0.0161 (7)
H8A	1.016697	−0.203291	0.013173	0.019*
H8B	0.906275	−0.287305	0.051533	0.019*
N9	1.0612 (3)	0.0525 (3)	0.3265 (2)	0.0140 (6)
N10	1.2167 (4)	0.0571 (4)	0.4862 (3)	0.0211 (7)
H10A	1.297672	0.107865	0.497466	0.025*
H10B	1.196810	0.021431	0.544138	0.025*
N11	0.5764 (4)	0.2266 (4)	0.6120 (3)	0.0249 (8)
Cu1	1.09805 (5)	0.15432 (4)	0.45064 (3)	0.01439 (10)
Cu2	0.82144 (5)	0.37532 (4)	0.49270 (3)	0.01460 (10)
Cu3	0.56561 (5)	0.32746 (5)	0.19608 (4)	0.01661 (11)
Cu4	0.69158 (5)	0.08435 (5)	−0.03239 (3)	0.01462 (10)
Cu5	0.95212 (5)	−0.08593 (4)	0.15104 (3)	0.01321 (10)
Dy1	0.84875 (2)	0.19510 (2)	0.24230 (2)	0.01371 (6)
O1	0.9519 (3)	0.2074 (3)	0.4149 (2)	0.0176 (6)
O2	1.1124 (3)	0.2513 (3)	0.5797 (2)	0.0169 (6)
O3	0.7689 (3)	0.3219 (3)	0.3506 (2)	0.0160 (6)
O4	0.7152 (3)	0.4811 (3)	0.4763 (2)	0.0189 (6)
O5	0.6460 (3)	0.2048 (3)	0.1576 (2)	0.0190 (6)
O6	0.4823 (3)	0.2928 (3)	0.0572 (2)	0.0191 (6)
O7	0.8131 (3)	0.0785 (3)	0.0789 (2)	0.0168 (6)
O8	0.7442 (3)	−0.0466 (3)	−0.0994 (2)	0.0158 (6)
O9	0.9731 (3)	0.0552 (3)	0.2462 (2)	0.0145 (5)
O10	1.0775 (3)	−0.1224 (3)	0.2439 (2)	0.0156 (6)
O11	0.7120 (3)	0.0153 (3)	0.2935 (2)	0.0202 (6)
H11A	0.646 (3)	0.008 (5)	0.322 (4)	0.030*
H11B	0.720 (5)	−0.054 (3)	0.284 (4)	0.030*
O15	0.6305 (3)	0.2204 (3)	0.5340 (3)	0.0289 (7)
O16	0.6442 (4)	0.2556 (5)	0.6960 (3)	0.0562 (13)
O17	0.4608 (3)	0.2031 (3)	0.6087 (3)	0.0378 (9)
O18	1.2494 (3)	0.3207 (3)	0.3755 (2)	0.0222 (6)
H18A	1.272 (5)	0.377 (4)	0.422 (3)	0.033*
H18B	1.197 (4)	0.334 (5)	0.333 (3)	0.033*
O19	0.3864 (3)	0.1929 (3)	0.2659 (2)	0.0208 (6)
H19A	0.337 (4)	0.153 (5)	0.218 (3)	0.031*
H19B	0.340 (5)	0.225 (5)	0.295 (4)	0.031*
O20	0.8193 (3)	0.2509 (3)	−0.1131 (3)	0.0244 (7)
H20A	0.848 (5)	0.225 (5)	−0.162 (3)	0.037*
H20B	0.838 (6)	0.3269 (19)	−0.105 (5)	0.037*
O21	0.6433 (4)	0.6160 (3)	0.0964 (3)	0.0301 (8)
H21A	0.606 (6)	0.639 (6)	0.048 (3)	0.045*
H21B	0.685 (5)	0.573 (5)	0.070 (5)	0.045*
O22	0.8208 (5)	0.5167 (4)	0.0461 (3)	0.0469 (11)
H22A	0.847 (7)	0.523 (7)	−0.012 (3)	0.070*
H22B	0.852 (7)	0.466 (6)	0.073 (6)	0.070*
O24	0.7778 (3)	−0.1964 (3)	0.2415 (2)	0.0181 (6)
H24A	0.806 (5)	−0.226 (5)	0.290 (3)	0.027*
H24B	0.739 (5)	−0.259 (3)	0.204 (3)	0.027*
O25	0.5139 (3)	0.0557 (3)	0.3692 (3)	0.0248 (7)
H25A	0.474 (5)	0.101 (5)	0.347 (4)	0.037*
H25B	0.538 (6)	0.097 (5)	0.425 (3)	0.037*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0170 (19)	0.0133 (18)	0.0110 (17)	0.0007 (15)	0.0037 (14)	0.0030 (14)
C2	0.024 (2)	0.0163 (19)	0.0109 (17)	0.0026 (16)	0.0017 (15)	−0.0023 (14)
C3	0.021 (2)	0.0118 (18)	0.0153 (18)	0.0030 (15)	0.0036 (15)	−0.0001 (14)
C4	0.031 (2)	0.016 (2)	0.019 (2)	0.0121 (18)	−0.0001 (17)	−0.0009 (16)
C5	0.021 (2)	0.0170 (19)	0.0109 (17)	0.0061 (16)	0.0002 (15)	0.0021 (14)
C6	0.024 (2)	0.026 (2)	0.0105 (18)	0.0138 (18)	−0.0013 (15)	−0.0009 (15)
C7	0.0146 (18)	0.0150 (18)	0.0117 (17)	0.0045 (15)	0.0026 (14)	0.0015 (14)
C8	0.022 (2)	0.0159 (19)	0.0127 (18)	0.0078 (16)	0.0009 (15)	−0.0016 (14)
C9	0.0141 (18)	0.0138 (18)	0.0132 (17)	0.0031 (14)	0.0018 (14)	0.0025 (14)
C10	0.0170 (19)	0.0191 (19)	0.0174 (19)	0.0078 (16)	0.0005 (15)	0.0011 (15)
C11	0.028 (5)	0.022 (4)	0.016 (4)	0.006 (5)	0.006 (5)	0.000 (4)
O12	0.022 (6)	0.026 (4)	0.019 (5)	0.003 (5)	0.010 (5)	0.006 (4)
O13	0.027 (5)	0.023 (4)	0.015 (5)	−0.002 (4)	0.008 (5)	0.001 (5)
O14	0.030 (7)	0.029 (6)	0.020 (6)	−0.003 (6)	0.002 (6)	0.004 (5)
O23	0.052 (13)	0.058 (13)	0.23 (4)	0.042 (11)	−0.013 (16)	−0.019 (16)
C11B	0.029 (4)	0.017 (2)	0.013 (3)	0.006 (3)	0.006 (3)	−0.002 (2)
O12B	0.031 (4)	0.026 (2)	0.022 (3)	0.001 (3)	0.007 (3)	0.0090 (19)
O13B	0.025 (3)	0.021 (2)	0.015 (4)	0.002 (2)	0.000 (3)	0.001 (3)
O14B	0.041 (4)	0.023 (3)	0.018 (3)	−0.004 (3)	0.009 (3)	−0.001 (2)
N1	0.0246 (18)	0.0153 (16)	0.0084 (15)	0.0058 (14)	0.0042 (13)	−0.0038 (12)
N2	0.027 (2)	0.026 (2)	0.0151 (17)	0.0114 (16)	−0.0011 (14)	−0.0049 (14)
N3	0.0274 (19)	0.0159 (16)	0.0140 (16)	0.0114 (14)	0.0019 (14)	0.0022 (13)
N4	0.045 (3)	0.0235 (19)	0.0176 (18)	0.0205 (18)	−0.0008 (17)	0.0010 (15)
N5	0.0189 (17)	0.0201 (17)	0.0112 (15)	0.0095 (14)	−0.0016 (13)	−0.0013 (13)
N6	0.0184 (17)	0.0213 (17)	0.0107 (15)	0.0092 (14)	0.0001 (13)	−0.0008 (13)
N7	0.0200 (17)	0.0120 (15)	0.0125 (15)	0.0088 (13)	0.0030 (13)	−0.0008 (12)
N8	0.0201 (17)	0.0165 (16)	0.0130 (15)	0.0080 (14)	0.0007 (13)	0.0002 (12)
N9	0.0139 (16)	0.0185 (16)	0.0087 (14)	0.0048 (13)	−0.0035 (12)	0.0003 (12)
N10	0.0219 (19)	0.028 (2)	0.0145 (16)	0.0113 (15)	−0.0035 (14)	0.0008 (14)
N11	0.024 (2)	0.026 (2)	0.0220 (19)	0.0033 (16)	0.0022 (15)	0.0022 (15)
Cu1	0.0158 (2)	0.0178 (2)	0.0092 (2)	0.00580 (19)	−0.00147 (17)	−0.00123 (17)
Cu2	0.0202 (2)	0.0138 (2)	0.0094 (2)	0.00534 (19)	0.00115 (18)	−0.00185 (17)
Cu3	0.0250 (3)	0.0173 (2)	0.0107 (2)	0.0125 (2)	−0.00060 (19)	−0.00092 (18)
Cu4	0.0181 (2)	0.0191 (2)	0.0083 (2)	0.00965 (19)	−0.00130 (17)	−0.00176 (17)
Cu5	0.0177 (2)	0.0126 (2)	0.0102 (2)	0.00695 (18)	−0.00060 (17)	−0.00128 (17)
Dy1	0.01860 (10)	0.01323 (9)	0.00956 (9)	0.00606 (7)	−0.00016 (6)	−0.00055 (6)
O1	0.0217 (15)	0.0213 (15)	0.0108 (13)	0.0110 (12)	−0.0017 (11)	−0.0079 (11)
O2	0.0203 (15)	0.0198 (14)	0.0106 (13)	0.0067 (12)	−0.0002 (11)	0.0003 (11)
O3	0.0210 (15)	0.0171 (14)	0.0130 (13)	0.0116 (12)	0.0002 (11)	−0.0009 (11)
O4	0.0242 (16)	0.0183 (14)	0.0143 (13)	0.0071 (12)	0.0024 (11)	−0.0016 (11)
O5	0.0279 (16)	0.0280 (16)	0.0053 (12)	0.0174 (13)	−0.0034 (11)	−0.0037 (11)
O6	0.0248 (16)	0.0220 (15)	0.0141 (13)	0.0140 (13)	−0.0017 (11)	0.0010 (11)
O7	0.0244 (15)	0.0170 (14)	0.0130 (13)	0.0145 (12)	−0.0024 (11)	−0.0041 (11)
O8	0.0198 (14)	0.0192 (14)	0.0091 (12)	0.0089 (12)	−0.0025 (10)	−0.0025 (10)
O9	0.0177 (14)	0.0164 (13)	0.0092 (12)	0.0071 (11)	−0.0055 (10)	−0.0007 (10)
O10	0.0195 (14)	0.0149 (13)	0.0136 (13)	0.0081 (11)	0.0005 (11)	−0.0012 (10)
O11	0.0186 (15)	0.0170 (14)	0.0247 (16)	0.0042 (12)	0.0051 (12)	0.0019 (12)
O15	0.0303 (18)	0.0313 (18)	0.0233 (17)	0.0047 (15)	0.0068 (14)	0.0064 (14)
O16	0.042 (2)	0.088 (4)	0.0178 (18)	−0.011 (2)	0.0019 (17)	0.003 (2)
O17	0.0249 (18)	0.0300 (19)	0.058 (3)	0.0085 (15)	0.0077 (17)	−0.0026 (17)
O18	0.0247 (17)	0.0192 (15)	0.0212 (16)	0.0075 (13)	−0.0009 (13)	−0.0087 (12)
O19	0.0212 (16)	0.0255 (16)	0.0157 (14)	0.0091 (13)	0.0000 (12)	−0.0042 (12)
O20	0.0289 (18)	0.0234 (16)	0.0233 (16)	0.0108 (14)	0.0079 (13)	0.0005 (13)
O21	0.044 (2)	0.0262 (18)	0.0204 (16)	0.0149 (16)	−0.0072 (15)	0.0016 (13)
O22	0.076 (3)	0.044 (2)	0.035 (2)	0.034 (2)	0.021 (2)	0.0123 (19)
O24	0.0230 (16)	0.0172 (14)	0.0130 (14)	0.0053 (12)	−0.0016 (11)	0.0026 (11)
O25	0.0210 (16)	0.0276 (17)	0.0270 (17)	0.0094 (13)	0.0027 (13)	0.0016 (14)

Geometric parameters (Å, º) top

C1—N1	1.289 (5)	N5—Cu4	1.904 (3)
C1—O2	1.293 (5)	N6—Cu4	2.005 (3)
C1—C2	1.503 (5)	N6—H6A	0.9100
C2—N2	1.484 (6)	N6—H6B	0.9100
C2—H2C	0.9900	N7—O7	1.393 (4)
C2—H2D	0.9900	N7—Cu5	1.899 (3)
C3—O4	1.288 (5)	N8—Cu5	2.021 (3)
C3—N3	1.299 (5)	N8—H8A	0.9100
C3—C4	1.512 (6)	N8—H8B	0.9100
C4—N4	1.492 (6)	N9—O9	1.395 (4)
C4—H4C	0.9900	N9—Cu1	1.897 (3)
C4—H4D	0.9900	N10—Cu1	2.012 (4)
C5—N5	1.293 (5)	N10—H10A	0.9100
C5—O6	1.298 (5)	N10—H10B	0.9100
C5—C6	1.499 (5)	N11—O17	1.228 (5)
C6—N6	1.486 (5)	N11—O15	1.249 (5)
C6—H6C	0.9900	N11—O16	1.260 (5)
C6—H6D	0.9900	Cu1—O1	1.931 (3)
C7—N7	1.292 (5)	Cu1—O2	1.949 (3)
C7—O8	1.301 (5)	Cu1—O18	2.476 (3)
C7—C8	1.501 (5)	Cu2—O3	1.931 (3)
C8—N8	1.491 (5)	Cu2—O4	1.939 (3)
C8—H8C	0.9900	Cu2—O15	2.464 (3)
C8—H8D	0.9900	Cu3—O5	1.941 (3)
C9—N9	1.293 (5)	Cu3—O6	1.954 (3)
C9—O10	1.295 (5)	Cu3—O19	2.430 (3)
C9—C10	1.502 (5)	Cu4—O7	1.936 (3)
C10—N10	1.484 (5)	Cu4—O8	1.956 (3)
C10—H10C	0.9900	Cu4—O20	2.400 (3)
C10—H10D	0.9900	Cu5—O9	1.932 (3)
C11—O14	1.256 (15)	Cu5—O10	1.941 (3)
C11—O12	1.275 (16)	Cu5—O24	2.440 (3)
C11—O13	1.318 (16)	Dy1—O11	2.357 (3)
C11—Dy1	2.704 (19)	Dy1—O3	2.382 (3)
O12—Dy1	2.27 (2)	Dy1—O9	2.410 (3)
O13—Dy1	2.31 (3)	Dy1—O7	2.412 (3)
O23—H23A	0.8410	Dy1—O1	2.453 (3)
O23—H23B	0.8398	Dy1—O5	2.469 (3)
C11B—O14B	1.251 (8)	O11—H11A	0.83 (2)
C11B—O12B	1.295 (9)	O11—H11B	0.82 (2)
C11B—O13B	1.326 (8)	O18—H18A	0.83 (2)
C11B—Dy1	2.834 (8)	O18—H18B	0.83 (2)
O12B—Dy1	2.380 (8)	O19—H19A	0.82 (2)
O13B—Dy1	2.347 (12)	O19—H19B	0.82 (2)
N1—O1	1.387 (4)	O20—H20A	0.82 (2)
N1—Cu2	1.907 (4)	O20—H20B	0.83 (2)
N2—Cu2	1.983 (4)	O21—H21A	0.84 (2)
N2—H2A	0.9100	O21—H21B	0.84 (2)
N2—H2B	0.9100	O22—H22A	0.85 (2)
N3—O3	1.398 (4)	O22—H22B	0.85 (2)
N3—Cu3	1.905 (4)	O24—H24A	0.83 (2)
N4—Cu3	2.017 (4)	O24—H24B	0.83 (2)
N4—H4A	0.9100	O25—H25A	0.83 (2)
N4—H4B	0.9100	O25—H25B	0.83 (2)
N5—O5	1.399 (4)

N1—C1—O2	123.5 (4)	O4—Cu2—O15	86.41 (12)
N1—C1—C2	115.2 (4)	N2—Cu2—O15	93.60 (15)
O2—C1—C2	121.2 (3)	N3—Cu3—O5	90.67 (13)
N2—C2—C1	109.7 (3)	N3—Cu3—O6	168.26 (15)
N2—C2—H2C	109.7	O5—Cu3—O6	85.39 (12)
C1—C2—H2C	109.7	N3—Cu3—N4	82.79 (15)
N2—C2—H2D	109.7	O5—Cu3—N4	171.97 (16)
C1—C2—H2D	109.7	O6—Cu3—N4	100.11 (14)
H2C—C2—H2D	108.2	N3—Cu3—O19	97.68 (13)
O4—C3—N3	124.3 (4)	O5—Cu3—O19	97.42 (12)
O4—C3—C4	120.1 (4)	O6—Cu3—O19	93.80 (12)
N3—C3—C4	115.6 (4)	N4—Cu3—O19	88.10 (15)
N4—C4—C3	110.0 (3)	N5—Cu4—O7	91.62 (13)
N4—C4—H4C	109.7	N5—Cu4—O8	161.94 (14)
C3—C4—H4C	109.7	O7—Cu4—O8	84.56 (11)
N4—C4—H4D	109.7	N5—Cu4—N6	83.78 (14)
C3—C4—H4D	109.7	O7—Cu4—N6	173.83 (14)
H4C—C4—H4D	108.2	O8—Cu4—N6	98.55 (13)
N5—C5—O6	123.9 (4)	N5—Cu4—O20	100.27 (13)
N5—C5—C6	116.2 (4)	O7—Cu4—O20	99.73 (12)
O6—C5—C6	119.9 (4)	O8—Cu4—O20	97.78 (12)
N6—C6—C5	111.0 (3)	N6—Cu4—O20	85.18 (13)
N6—C6—H6C	109.4	N7—Cu5—O9	89.53 (12)
C5—C6—H6C	109.4	N7—Cu5—O10	170.19 (14)
N6—C6—H6D	109.4	O9—Cu5—O10	85.47 (11)
C5—C6—H6D	109.4	N7—Cu5—N8	83.23 (14)
H6C—C6—H6D	108.0	O9—Cu5—N8	169.36 (13)
N7—C7—O8	123.7 (4)	O10—Cu5—N8	100.49 (13)
N7—C7—C8	116.3 (3)	N7—Cu5—O24	95.86 (13)
O8—C7—C8	120.0 (3)	O9—Cu5—O24	87.84 (11)
N8—C8—C7	110.4 (3)	O10—Cu5—O24	92.38 (11)
N8—C8—H8C	109.6	N8—Cu5—O24	100.61 (13)
C7—C8—H8C	109.6	O12—Dy1—O13	57.1 (6)
N8—C8—H8D	109.6	O12—Dy1—O11	148.9 (5)
C7—C8—H8D	109.6	O13—Dy1—O11	153.5 (6)
H8C—C8—H8D	108.1	O13B—Dy1—O11	148.4 (2)
N9—C9—O10	124.2 (4)	O13B—Dy1—O12B	54.7 (2)
N9—C9—C10	116.1 (3)	O11—Dy1—O12B	155.6 (2)
O10—C9—C10	119.6 (3)	O12—Dy1—O3	85.0 (5)
N10—C10—C9	110.6 (3)	O13—Dy1—O3	97.2 (8)
N10—C10—H10C	109.5	O13B—Dy1—O3	93.6 (3)
C9—C10—H10C	109.5	O11—Dy1—O3	92.12 (10)
N10—C10—H10D	109.5	O12B—Dy1—O3	93.8 (2)
C9—C10—H10D	109.5	O12—Dy1—O9	123.4 (5)
H10C—C10—H10D	108.1	O13—Dy1—O9	81.7 (8)
O14—C11—O12	123.4 (18)	O13B—Dy1—O9	80.7 (3)
O14—C11—O13	121.3 (19)	O11—Dy1—O9	75.78 (10)
O12—C11—O13	115.3 (18)	O12B—Dy1—O9	112.1 (2)
O14—C11—Dy1	179 (2)	O3—Dy1—O9	141.93 (9)
O12—C11—Dy1	56.8 (11)	O12—Dy1—O7	80.3 (5)
O13—C11—Dy1	58.5 (14)	O13—Dy1—O7	101.5 (7)
C11—O12—Dy1	95.2 (13)	O13B—Dy1—O7	107.8 (3)
C11—O13—Dy1	92.3 (16)	O11—Dy1—O7	84.36 (11)
H23A—O23—H23B	107.9	O12B—Dy1—O7	77.1 (2)
O14B—C11B—O12B	125.8 (7)	O3—Dy1—O7	144.46 (9)
O14B—C11B—O13B	122.3 (8)	O9—Dy1—O7	71.21 (9)
O12B—C11B—O13B	111.8 (7)	O12—Dy1—O1	126.0 (5)
O14B—C11B—Dy1	177.4 (6)	O13—Dy1—O1	77.8 (5)
O12B—C11B—Dy1	56.6 (4)	O13B—Dy1—O1	70.69 (19)
O13B—C11B—Dy1	55.3 (5)	O11—Dy1—O1	81.73 (11)
C11B—O12B—Dy1	96.4 (5)	O12B—Dy1—O1	122.6 (2)
C11B—O13B—Dy1	97.0 (6)	O3—Dy1—O1	71.77 (9)
C1—N1—O1	116.4 (3)	O9—Dy1—O1	70.83 (9)
C1—N1—Cu2	119.4 (3)	O7—Dy1—O1	141.70 (9)
O1—N1—Cu2	124.0 (3)	O12—Dy1—O5	68.7 (5)
C2—N2—Cu2	111.6 (3)	O13—Dy1—O5	125.6 (6)
C2—N2—H2A	109.3	O13B—Dy1—O5	130.3 (2)
Cu2—N2—H2A	109.3	O11—Dy1—O5	80.88 (11)
C2—N2—H2B	109.3	O12B—Dy1—O5	78.5 (2)
Cu2—N2—H2B	109.3	O3—Dy1—O5	71.92 (9)
H2A—N2—H2B	108.0	O9—Dy1—O5	138.36 (9)
C3—N3—O3	115.0 (3)	O7—Dy1—O5	72.60 (9)
C3—N3—Cu3	119.0 (3)	O1—Dy1—O5	138.84 (9)
O3—N3—Cu3	125.2 (2)	O12—Dy1—C11	28.0 (4)
C4—N4—Cu3	110.8 (3)	O13—Dy1—C11	29.1 (4)
C4—N4—H4A	109.5	O11—Dy1—C11	174.5 (7)
Cu3—N4—H4A	109.5	O3—Dy1—C11	91.8 (7)
C4—N4—H4B	109.5	O9—Dy1—C11	103.3 (6)
Cu3—N4—H4B	109.5	O7—Dy1—C11	90.2 (7)
H4A—N4—H4B	108.1	O1—Dy1—C11	103.2 (6)
C5—N5—O5	116.2 (3)	O5—Dy1—C11	96.7 (5)
C5—N5—Cu4	117.2 (3)	O13B—Dy1—C11B	27.67 (19)
O5—N5—Cu4	125.8 (2)	O11—Dy1—C11B	172.4 (2)
C6—N6—Cu4	109.1 (2)	O12B—Dy1—C11B	27.0 (2)
C6—N6—H6A	109.9	O3—Dy1—C11B	94.7 (2)
Cu4—N6—H6A	109.9	O9—Dy1—C11B	96.7 (2)
C6—N6—H6B	109.9	O7—Dy1—C11B	92.0 (2)
Cu4—N6—H6B	109.9	O1—Dy1—C11B	97.2 (2)
H6A—N6—H6B	108.3	O5—Dy1—C11B	104.4 (2)
C7—N7—O7	115.4 (3)	N1—O1—Cu1	107.4 (2)
C7—N7—Cu5	119.3 (3)	N1—O1—Dy1	123.3 (2)
O7—N7—Cu5	125.3 (2)	Cu1—O1—Dy1	125.28 (13)
C8—N8—Cu5	110.6 (2)	C1—O2—Cu1	107.0 (2)
C8—N8—H8A	109.5	N3—O3—Cu2	107.7 (2)
Cu5—N8—H8A	109.5	N3—O3—Dy1	124.3 (2)
C8—N8—H8B	109.5	Cu2—O3—Dy1	127.93 (13)
Cu5—N8—H8B	109.5	C3—O4—Cu2	107.0 (3)
H8A—N8—H8B	108.1	N5—O5—Cu3	107.2 (2)
C9—N9—O9	115.5 (3)	N5—O5—Dy1	121.8 (2)
C9—N9—Cu1	118.3 (3)	Cu3—O5—Dy1	123.95 (13)
O9—N9—Cu1	125.6 (2)	C5—O6—Cu3	106.9 (2)
C10—N10—Cu1	110.4 (2)	N7—O7—Cu4	108.0 (2)
C10—N10—H10A	109.6	N7—O7—Dy1	124.6 (2)
Cu1—N10—H10A	109.6	Cu4—O7—Dy1	125.53 (13)
C10—N10—H10B	109.6	C7—O8—Cu4	106.9 (2)
Cu1—N10—H10B	109.6	N9—O9—Cu5	107.8 (2)
H10A—N10—H10B	108.1	N9—O9—Dy1	124.9 (2)
O17—N11—O15	122.1 (4)	Cu5—O9—Dy1	126.77 (12)
O17—N11—O16	120.1 (4)	C9—O10—Cu5	107.0 (2)
O15—N11—O16	117.8 (4)	Dy1—O11—H11A	128 (4)
N9—Cu1—O1	89.39 (13)	Dy1—O11—H11B	125 (4)
N9—Cu1—O2	172.56 (14)	H11A—O11—H11B	107 (6)
O1—Cu1—O2	85.19 (12)	N11—O15—Cu2	125.3 (3)
N9—Cu1—N10	83.73 (14)	Cu1—O18—H18A	103 (4)
O1—Cu1—N10	165.35 (15)	Cu1—O18—H18B	97 (4)
O2—Cu1—N10	100.37 (13)	H18A—O18—H18B	111 (6)
N9—Cu1—O18	91.67 (12)	Cu3—O19—H19A	107 (4)
O1—Cu1—O18	95.28 (12)	Cu3—O19—H19B	117 (4)
O2—Cu1—O18	93.90 (11)	H19A—O19—H19B	101 (6)
N10—Cu1—O18	97.82 (14)	Cu4—O20—H20A	110 (4)
N1—Cu2—O3	90.66 (13)	Cu4—O20—H20B	136 (4)
N1—Cu2—O4	168.94 (14)	H20A—O20—H20B	114 (6)
O3—Cu2—O4	85.41 (12)	H21A—O21—H21B	106 (6)
N1—Cu2—N2	82.65 (15)	H22A—O22—H22B	106 (7)
O3—Cu2—N2	173.24 (14)	Cu5—O24—H24A	110 (4)
O4—Cu2—N2	101.00 (14)	Cu5—O24—H24B	106 (4)
N1—Cu2—O15	103.87 (14)	H24A—O24—H24B	101 (5)
O3—Cu2—O15	88.90 (12)	H25A—O25—H25B	95 (6)

N1—C1—C2—N2	9.0 (5)	O9—N9—Cu1—O1	11.1 (3)
O2—C1—C2—N2	−169.9 (4)	C9—N9—Cu1—N10	7.5 (3)
O4—C3—C4—N4	179.4 (4)	O9—N9—Cu1—N10	178.1 (3)
N3—C3—C4—N4	−0.7 (5)	C9—N9—Cu1—O18	105.2 (3)
N5—C5—C6—N6	1.9 (5)	O9—N9—Cu1—O18	−84.2 (3)
O6—C5—C6—N6	−178.9 (4)	C7—N7—Cu5—O9	174.1 (3)
N7—C7—C8—N8	−3.7 (5)	O7—N7—Cu5—O9	−5.5 (3)
O8—C7—C8—N8	177.5 (3)	C7—N7—Cu5—N8	1.9 (3)
N9—C9—C10—N10	8.5 (5)	O7—N7—Cu5—N8	−177.7 (3)
O10—C9—C10—N10	−173.1 (3)	C7—N7—Cu5—O24	−98.1 (3)
O14—C11—O12—Dy1	−179 (3)	O7—N7—Cu5—O24	82.2 (3)
O13—C11—O12—Dy1	−2 (3)	C1—N1—O1—Cu1	−6.8 (4)
O14—C11—O13—Dy1	179 (3)	Cu2—N1—O1—Cu1	178.22 (19)
O12—C11—O13—Dy1	2 (3)	C1—N1—O1—Dy1	−165.3 (3)
O14B—C11B—O12B—Dy1	179.0 (9)	Cu2—N1—O1—Dy1	19.7 (4)
O13B—C11B—O12B—Dy1	−1.8 (9)	N1—C1—O2—Cu1	1.8 (5)
O14B—C11B—O13B—Dy1	−178.9 (9)	C2—C1—O2—Cu1	−179.4 (3)
O12B—C11B—O13B—Dy1	1.9 (9)	C3—N3—O3—Cu2	5.3 (4)
O2—C1—N1—O1	3.6 (6)	Cu3—N3—O3—Cu2	−164.7 (2)
C2—C1—N1—O1	−175.2 (3)	C3—N3—O3—Dy1	−171.9 (3)
O2—C1—N1—Cu2	178.7 (3)	Cu3—N3—O3—Dy1	18.1 (4)
C2—C1—N1—Cu2	0.0 (5)	N3—C3—O4—Cu2	−4.7 (5)
C1—C2—N2—Cu2	−13.2 (4)	C4—C3—O4—Cu2	175.2 (3)
O4—C3—N3—O3	−0.4 (6)	C5—N5—O5—Cu3	−5.6 (4)
C4—C3—N3—O3	179.7 (3)	Cu4—N5—O5—Cu3	163.6 (2)
O4—C3—N3—Cu3	170.3 (3)	C5—N5—O5—Dy1	−157.2 (3)
C4—C3—N3—Cu3	−9.7 (5)	Cu4—N5—O5—Dy1	12.0 (4)
C3—C4—N4—Cu3	9.5 (5)	N5—C5—O6—Cu3	2.5 (5)
O6—C5—N5—O5	2.2 (6)	C6—C5—O6—Cu3	−176.5 (3)
C6—C5—N5—O5	−178.7 (3)	C7—N7—O7—Cu4	9.3 (4)
O6—C5—N5—Cu4	−168.0 (3)	Cu5—N7—O7—Cu4	−171.08 (19)
C6—C5—N5—Cu4	11.1 (5)	C7—N7—O7—Dy1	174.4 (3)
C5—C6—N6—Cu4	−12.7 (4)	Cu5—N7—O7—Dy1	−6.0 (4)
O8—C7—N7—O7	−1.1 (6)	N7—C7—O8—Cu4	−7.6 (5)
C8—C7—N7—O7	−179.8 (3)	C8—C7—O8—Cu4	171.1 (3)
O8—C7—N7—Cu5	179.3 (3)	C9—N9—O9—Cu5	1.2 (4)
C8—C7—N7—Cu5	0.5 (5)	Cu1—N9—O9—Cu5	−169.69 (19)
C7—C8—N8—Cu5	4.8 (4)	C9—N9—O9—Dy1	172.9 (3)
O10—C9—N9—O9	−0.9 (6)	Cu1—N9—O9—Dy1	2.0 (4)
C10—C9—N9—O9	177.5 (3)	N9—C9—O10—Cu5	0.1 (5)
O10—C9—N9—Cu1	170.7 (3)	C10—C9—O10—Cu5	−178.2 (3)
C10—C9—N9—Cu1	−11.0 (5)	O17—N11—O15—Cu2	134.4 (4)
C9—C10—N10—Cu1	−2.5 (4)	O16—N11—O15—Cu2	−47.2 (6)
C9—N9—Cu1—O1	−159.6 (3)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O23—H23A···O16ⁱ	0.84	1.84	2.61 (2)	150
O23—H23B···O14	0.84	1.95	2.657 (17)	141
N2—H2A···O13ⁱ	0.91	2.23	3.05 (3)	150
N2—H2A···O13Bⁱ	0.91	2.05	2.900 (11)	156
N2—H2B···O16	0.91	2.23	3.054 (6)	150
N4—H4A···O21	0.91	2.08	2.912 (6)	152
N4—H4B···O23ⁱⁱ	0.91	1.86	2.520 (16)	128
N6—H6A···O16ⁱⁱⁱ	0.91	2.29	3.091 (6)	147
N6—H6B···N5^iv	0.91	2.54	3.287 (5)	140
N6—H6B···O5^iv	0.91	2.49	3.396 (5)	171
N8—H8A···O7^v	0.91	2.48	3.262 (5)	144
N8—H8A···O20^v	0.91	2.38	2.989 (5)	124
N8—H8B···O22^vi	0.91	2.17	3.045 (6)	162
N10—H10A···O17^vii	0.91	2.20	3.005 (5)	147
N10—H10B···O11^viii	0.91	2.42	3.198 (5)	143
O11—H11A···O25	0.83 (2)	1.86 (3)	2.642 (4)	157 (6)
O11—H11B···O24	0.82 (2)	2.00 (3)	2.800 (4)	164 (6)
O18—H18A···O4ⁱ	0.83 (2)	2.01 (2)	2.821 (4)	165 (6)
O18—H18B···O13	0.83 (2)	2.05 (4)	2.87 (3)	169 (6)
O18—H18B···O13B	0.83 (2)	1.84 (3)	2.650 (10)	165 (6)
O19—H19A···O8^iv	0.82 (2)	1.91 (2)	2.710 (4)	167 (6)
O19—H19B···O18ⁱⁱ	0.82 (2)	2.01 (2)	2.827 (4)	172 (6)
O20—H20A···O10^v	0.82 (2)	1.95 (3)	2.738 (4)	160 (6)
O20—H20B···O14^ix	0.83 (2)	2.18 (3)	2.973 (18)	158 (6)
O20—H20B···O14B^ix	0.83 (2)	2.28 (3)	3.065 (7)	158 (6)
O21—H21A···O6^x	0.84 (2)	1.98 (2)	2.810 (4)	174 (7)
O21—H21B···O22	0.84 (2)	1.85 (3)	2.660 (6)	160 (7)
O22—H22A···O14^ix	0.85 (2)	1.91 (3)	2.736 (19)	166 (8)
O22—H22A···O14B^ix	0.85 (2)	1.87 (2)	2.708 (8)	171 (8)
O22—H22B···O12	0.85 (2)	1.74 (4)	2.57 (2)	165 (8)
O22—H22B···O14	0.85 (2)	2.41 (7)	3.033 (18)	130 (7)
O22—H22B···O12B	0.85 (2)	1.90 (2)	2.753 (10)	179 (9)
O24—H24A···O2^viii	0.83 (2)	1.97 (2)	2.777 (4)	165 (5)
O24—H24B···O21^vi	0.83 (2)	1.95 (2)	2.767 (5)	168 (5)
O25—H25A···O19	0.83 (2)	1.95 (2)	2.769 (5)	168 (6)
O25—H25B···O15	0.83 (2)	1.94 (3)	2.752 (5)	163 (6)

Pentaaquacarbonatopentakis(glycine hydroxamato)nitratopentacopper(II)holmium(III) 3.445-hydrate (Complex_3) top

Crystal data top

[Cu₅Ho(C₂H₄N₂O₂)₅(CO₃)(NO₃)(H₂O)₅]·3.445H₂O	Z = 2
M_r = 1197.21	F(000) = 1174.9
Triclinic, P1	D_x = 2.467 Mg m⁻³
a = 11.2027 (9) Å	Mo Kα radiation, λ = 0.71073 Å
b = 11.4955 (9) Å	Cell parameters from 9995 reflections
c = 13.2467 (10) Å	θ = 2.3–33.2°
α = 94.001 (3)°	µ = 5.77 mm⁻¹
β = 94.784 (3)°	T = 150 K
γ = 107.518 (3)°	Prism, blue
V = 1613.0 (2) Å³	0.44 × 0.42 × 0.28 mm

Data collection top

Bruker AXS D8 Quest CMOS diffractometer	12306 independent reflections
Radiation source: fine focus sealed tube X-ray source	10012 reflections with I > 2σ(I)
Triumph curved graphite crystal monochromator	R_int = 0.042
Detector resolution: 10.4167 pixels mm^-1	θ_max = 33.2°, θ_min = 2.5°
ω and phi scans	h = −17→17
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	k = −17→17
T_min = 0.548, T_max = 0.747	l = −20→20
50443 measured reflections

Refinement top

Refinement on F²	Primary atom site location: isomorphous structure methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.033	Hydrogen site location: mixed
wR(F²) = 0.082	H atoms treated by a mixture of independent and constrained refinement
S = 1.05	w = 1/[σ²(F_o²) + (0.0289P)² + 5.881P] where P = (F_o² + 2F_c²)/3
12306 reflections	(Δ/σ)_max = 0.001
563 parameters	Δρ_max = 2.80 e Å⁻³
139 restraints	Δρ_min = −2.27 e Å⁻³

Special details top

Refinement. Solved by isomorphous replacement from its Gd analogue.

A water molecule is partially occupied, inducing disorder for the nearby carbonate anion. The two disordered moieties were restrained to have similar geometries. Uij components of ADPs for disordered atoms closer to each other than 2.0 Angstrom were restrained to be similar. The distance of the water oxygen to one of the carbonate oxygen atoms was restrained to be at least 2.8 Angstrom for the moiety that contains the water molecule.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
C1	1.0280 (3)	0.3079 (3)	0.5731 (2)	0.0118 (5)
C2	1.0125 (3)	0.3910 (3)	0.6604 (2)	0.0141 (6)
H2C	1.009297	0.349401	0.723592	0.017*
H2D	1.085438	0.466647	0.670787	0.017*
C3	0.6597 (3)	0.4528 (3)	0.3871 (2)	0.0138 (5)
C4	0.5618 (3)	0.5118 (3)	0.3530 (3)	0.0177 (6)
H4C	0.491688	0.490089	0.395941	0.021*
H4D	0.599580	0.602076	0.361106	0.021*
C5	0.5303 (3)	0.2146 (3)	0.0111 (2)	0.0123 (5)
C6	0.4901 (3)	0.1750 (3)	−0.1003 (2)	0.0173 (6)
H6C	0.397531	0.136935	−0.111278	0.021*
H6D	0.512297	0.247545	−0.139250	0.021*
C7	0.8131 (3)	−0.0808 (3)	−0.0328 (2)	0.0114 (5)
C8	0.8533 (3)	−0.1924 (3)	−0.0563 (2)	0.0140 (5)
H8C	0.778056	−0.265608	−0.070891	0.017*
H8D	0.898930	−0.182788	−0.117611	0.017*
C9	1.1067 (3)	−0.0368 (3)	0.3181 (2)	0.0098 (5)
C10	1.2053 (3)	−0.0372 (3)	0.4021 (2)	0.0139 (5)
H10C	1.182002	−0.117768	0.429942	0.017*
H10D	1.287142	−0.024697	0.374459	0.017*
C11	0.9971 (13)	0.3886 (16)	0.1665 (14)	0.022 (2)	0.445 (11)
O12	0.8827 (10)	0.3498 (14)	0.1383 (12)	0.0236 (19)	0.445 (11)
O13	1.042 (3)	0.334 (2)	0.2371 (15)	0.024 (2)	0.445 (11)
O14	1.0681 (9)	0.4809 (11)	0.1285 (9)	0.030 (2)	0.445 (11)
O23	1.2942 (11)	0.5207 (9)	0.1960 (8)	0.082 (4)	0.445 (11)
H23A	1.308337	0.590634	0.233418	0.122*	0.445 (11)
H23B	1.233023	0.460780	0.173402	0.122*	0.445 (11)
C11B	1.0297 (10)	0.3906 (11)	0.1741 (10)	0.0202 (19)	0.555 (11)
O12B	0.9181 (9)	0.3477 (11)	0.1319 (10)	0.0282 (19)	0.555 (11)
O13B	1.050 (2)	0.3358 (17)	0.2541 (11)	0.0225 (19)	0.555 (11)
O14B	1.1139 (8)	0.4780 (8)	0.1452 (6)	0.0272 (17)	0.555 (11)
N1	0.9480 (3)	0.2936 (2)	0.49315 (19)	0.0136 (5)
N2	0.8953 (3)	0.4226 (3)	0.6386 (2)	0.0216 (6)
H2A	0.911575	0.504772	0.653058	0.026*
H2B	0.837833	0.383792	0.679653	0.026*
N3	0.6791 (3)	0.3750 (2)	0.3201 (2)	0.0138 (5)
N4	0.5131 (4)	0.4698 (3)	0.2452 (2)	0.0255 (7)
H4A	0.542034	0.532305	0.206181	0.031*
H4B	0.427458	0.447852	0.238332	0.031*
N5	0.6111 (3)	0.1682 (2)	0.05439 (19)	0.0122 (5)
N6	0.5523 (3)	0.0857 (3)	−0.13800 (19)	0.0136 (5)
H6A	0.584500	0.107440	−0.197228	0.016*
H6B	0.495105	0.009616	−0.150397	0.016*
N7	0.8501 (3)	−0.0247 (2)	0.05795 (19)	0.0109 (4)
N8	0.9364 (3)	−0.2099 (2)	0.0309 (2)	0.0141 (5)
H8A	1.014323	−0.201893	0.011654	0.017*
H8B	0.904566	−0.286957	0.049667	0.017*
N9	1.0597 (2)	0.0533 (2)	0.32597 (19)	0.0110 (4)
N10	1.2179 (3)	0.0612 (3)	0.4850 (2)	0.0185 (5)
H10A	1.298457	0.112497	0.494020	0.022*
H10B	1.200453	0.027405	0.544288	0.022*
N11	0.5792 (3)	0.2265 (3)	0.6124 (2)	0.0229 (6)
Cu1	1.09880 (4)	0.15681 (3)	0.44997 (3)	0.01166 (7)
Cu2	0.82339 (4)	0.37481 (3)	0.49405 (3)	0.01165 (7)
Cu3	0.56785 (4)	0.32620 (4)	0.19698 (3)	0.01405 (8)
Cu4	0.69119 (4)	0.08365 (4)	−0.03271 (3)	0.01185 (7)
Cu5	0.95011 (4)	−0.08588 (3)	0.15039 (3)	0.01067 (7)
Ho1	0.84737 (2)	0.19371 (2)	0.24296 (2)	0.01295 (4)
O1	0.9539 (2)	0.2094 (2)	0.41456 (17)	0.0171 (5)
O2	1.1136 (2)	0.2531 (2)	0.57996 (16)	0.0139 (4)
O3	0.7699 (2)	0.3202 (2)	0.35211 (16)	0.0136 (4)
O4	0.7177 (2)	0.4801 (2)	0.47858 (17)	0.0150 (4)
O5	0.6451 (2)	0.2021 (2)	0.15826 (16)	0.0159 (4)
O6	0.4839 (2)	0.2914 (2)	0.05838 (17)	0.0159 (4)
O7	0.8119 (2)	0.0781 (2)	0.07896 (17)	0.0143 (4)
O8	0.7438 (2)	−0.0459 (2)	−0.10037 (16)	0.0142 (4)
O9	0.9714 (2)	0.0553 (2)	0.24613 (16)	0.0120 (4)
O10	1.0747 (2)	−0.1222 (2)	0.24305 (17)	0.0126 (4)
O11	0.7125 (2)	0.0137 (2)	0.2961 (2)	0.0176 (5)
H11A	0.647 (3)	0.013 (4)	0.320 (4)	0.026*
H11B	0.718 (5)	−0.054 (2)	0.280 (4)	0.026*
O15	0.6333 (3)	0.2185 (3)	0.5342 (2)	0.0257 (6)
O16	0.6461 (4)	0.2526 (4)	0.6963 (2)	0.0562 (12)
O17	0.4642 (3)	0.2061 (3)	0.6079 (3)	0.0366 (7)
O18	1.2491 (3)	0.3228 (2)	0.3739 (2)	0.0212 (5)
H18A	1.265 (5)	0.370 (4)	0.426 (2)	0.032*
H18B	1.193 (4)	0.332 (5)	0.333 (3)	0.032*
O19	0.3874 (2)	0.1934 (2)	0.26731 (19)	0.0187 (5)
H19A	0.343 (4)	0.151 (4)	0.218 (3)	0.028*
H19B	0.343 (4)	0.226 (4)	0.298 (3)	0.028*
O20	0.8212 (3)	0.2497 (2)	−0.1135 (2)	0.0225 (5)
H20A	0.839 (5)	0.217 (4)	−0.165 (3)	0.034*
H20B	0.841 (5)	0.3242 (18)	−0.108 (4)	0.034*
O21	0.6432 (3)	0.6168 (3)	0.0936 (2)	0.0311 (7)
H21A	0.597 (5)	0.617 (5)	0.042 (3)	0.047*
H21B	0.677 (5)	0.568 (4)	0.071 (4)	0.047*
O22	0.8170 (5)	0.5170 (4)	0.0460 (3)	0.0501 (10)
H22A	0.845 (7)	0.518 (7)	−0.013 (3)	0.075*
H22B	0.843 (7)	0.460 (5)	0.070 (5)	0.075*
O24	0.7767 (2)	−0.1977 (2)	0.24108 (19)	0.0173 (5)
H24A	0.801 (4)	−0.226 (4)	0.290 (3)	0.026*
H24B	0.737 (4)	−0.256 (3)	0.201 (3)	0.026*
O25	0.5129 (3)	0.0538 (2)	0.3694 (2)	0.0218 (5)
H25A	0.477 (4)	0.094 (4)	0.338 (4)	0.033*
H25B	0.540 (5)	0.094 (4)	0.425 (2)	0.033*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
C1	0.0147 (13)	0.0115 (12)	0.0078 (11)	0.0018 (10)	0.0012 (10)	0.0010 (9)
C2	0.0204 (15)	0.0121 (13)	0.0079 (12)	0.0028 (11)	0.0018 (11)	−0.0008 (10)
C3	0.0203 (15)	0.0086 (12)	0.0119 (13)	0.0034 (11)	0.0032 (11)	−0.0004 (10)
C4	0.0232 (16)	0.0141 (14)	0.0159 (14)	0.0078 (12)	−0.0007 (12)	−0.0035 (11)
C5	0.0152 (14)	0.0140 (13)	0.0081 (12)	0.0052 (11)	−0.0004 (10)	0.0010 (9)
C6	0.0209 (16)	0.0243 (16)	0.0093 (12)	0.0126 (13)	−0.0024 (11)	−0.0001 (11)
C7	0.0139 (13)	0.0129 (12)	0.0081 (12)	0.0053 (11)	0.0013 (10)	−0.0002 (9)
C8	0.0200 (15)	0.0124 (13)	0.0100 (12)	0.0068 (11)	0.0005 (11)	−0.0033 (10)
C9	0.0093 (12)	0.0113 (12)	0.0087 (11)	0.0028 (10)	0.0011 (9)	0.0015 (9)
C10	0.0138 (13)	0.0144 (13)	0.0146 (13)	0.0059 (11)	0.0001 (11)	0.0029 (10)
C11	0.025 (5)	0.024 (3)	0.017 (3)	0.009 (4)	0.005 (4)	−0.003 (3)
O12	0.022 (4)	0.026 (3)	0.022 (3)	0.004 (4)	0.003 (4)	0.008 (3)
O13	0.026 (4)	0.022 (3)	0.021 (5)	0.001 (3)	0.004 (4)	0.001 (4)
O14	0.027 (5)	0.029 (4)	0.030 (4)	0.000 (4)	0.005 (4)	0.005 (3)
O23	0.145 (10)	0.061 (6)	0.075 (7)	0.088 (7)	0.012 (7)	0.002 (5)
C11B	0.030 (4)	0.016 (2)	0.014 (3)	0.004 (3)	0.007 (3)	−0.003 (2)
O12B	0.032 (5)	0.021 (2)	0.026 (3)	−0.003 (4)	0.009 (4)	0.006 (2)
O13B	0.025 (4)	0.019 (3)	0.018 (4)	−0.002 (2)	0.001 (3)	0.002 (3)
O14B	0.032 (4)	0.021 (3)	0.019 (3)	−0.007 (3)	0.011 (3)	0.000 (2)
N1	0.0176 (12)	0.0149 (12)	0.0083 (11)	0.0056 (10)	0.0029 (9)	−0.0040 (9)
N2	0.0274 (16)	0.0282 (15)	0.0106 (12)	0.0139 (13)	−0.0014 (11)	−0.0083 (11)
N3	0.0199 (13)	0.0131 (11)	0.0095 (11)	0.0081 (10)	−0.0011 (9)	−0.0014 (9)
N4	0.046 (2)	0.0207 (14)	0.0164 (13)	0.0227 (15)	−0.0035 (13)	−0.0010 (11)
N5	0.0145 (12)	0.0167 (12)	0.0066 (10)	0.0080 (10)	−0.0024 (9)	−0.0014 (8)
N6	0.0163 (12)	0.0169 (12)	0.0076 (10)	0.0059 (10)	0.0004 (9)	−0.0004 (9)
N7	0.0153 (12)	0.0104 (10)	0.0088 (10)	0.0073 (9)	0.0004 (9)	−0.0012 (8)
N8	0.0170 (12)	0.0130 (11)	0.0130 (11)	0.0072 (10)	−0.0011 (9)	−0.0026 (9)
N9	0.0118 (11)	0.0115 (11)	0.0087 (10)	0.0035 (9)	−0.0031 (8)	−0.0011 (8)
N10	0.0191 (14)	0.0213 (14)	0.0147 (12)	0.0081 (11)	−0.0050 (10)	−0.0014 (10)
N11	0.0229 (15)	0.0218 (14)	0.0209 (14)	0.0027 (12)	0.0021 (12)	0.0007 (11)
Cu1	0.01256 (17)	0.01432 (17)	0.00767 (15)	0.00496 (14)	−0.00191 (12)	−0.00186 (12)
Cu2	0.01622 (18)	0.01112 (16)	0.00713 (15)	0.00445 (14)	0.00047 (13)	−0.00241 (12)
Cu3	0.0221 (2)	0.01470 (17)	0.00826 (16)	0.01148 (15)	−0.00165 (14)	−0.00181 (12)
Cu4	0.01516 (17)	0.01590 (17)	0.00609 (15)	0.00853 (14)	−0.00143 (12)	−0.00185 (12)
Cu5	0.01450 (17)	0.00999 (15)	0.00826 (15)	0.00602 (13)	−0.00087 (12)	−0.00170 (12)
Ho1	0.01760 (7)	0.01211 (6)	0.00911 (6)	0.00536 (5)	−0.00014 (5)	−0.00060 (4)
O1	0.0202 (11)	0.0247 (12)	0.0085 (9)	0.0135 (10)	−0.0027 (8)	−0.0079 (8)
O2	0.0158 (10)	0.0164 (10)	0.0085 (9)	0.0050 (9)	−0.0018 (8)	−0.0016 (8)
O3	0.0185 (11)	0.0150 (10)	0.0096 (9)	0.0102 (9)	−0.0013 (8)	−0.0016 (8)
O4	0.0214 (11)	0.0133 (10)	0.0101 (9)	0.0064 (9)	0.0003 (8)	−0.0037 (8)
O5	0.0229 (12)	0.0225 (11)	0.0050 (9)	0.0140 (10)	−0.0042 (8)	−0.0049 (8)
O6	0.0222 (12)	0.0193 (11)	0.0101 (10)	0.0135 (9)	−0.0016 (8)	−0.0018 (8)
O7	0.0211 (11)	0.0143 (10)	0.0106 (9)	0.0128 (9)	−0.0033 (8)	−0.0046 (8)
O8	0.0203 (11)	0.0162 (10)	0.0079 (9)	0.0098 (9)	−0.0016 (8)	−0.0023 (7)
O9	0.0159 (10)	0.0135 (10)	0.0070 (9)	0.0076 (8)	−0.0055 (7)	−0.0012 (7)
O10	0.0152 (10)	0.0116 (9)	0.0114 (9)	0.0056 (8)	0.0001 (8)	−0.0003 (7)
O11	0.0150 (11)	0.0137 (10)	0.0236 (12)	0.0037 (9)	0.0030 (9)	0.0003 (9)
O15	0.0262 (14)	0.0257 (13)	0.0224 (13)	0.0025 (11)	0.0059 (11)	0.0047 (10)
O16	0.039 (2)	0.086 (3)	0.0181 (15)	−0.0168 (19)	0.0004 (14)	0.0038 (17)
O17	0.0214 (14)	0.0286 (15)	0.059 (2)	0.0074 (12)	0.0086 (14)	−0.0025 (14)
O18	0.0242 (13)	0.0197 (12)	0.0194 (12)	0.0088 (10)	0.0004 (10)	−0.0062 (9)
O19	0.0176 (12)	0.0233 (12)	0.0142 (11)	0.0071 (10)	−0.0017 (9)	−0.0041 (9)
O20	0.0257 (13)	0.0200 (12)	0.0240 (13)	0.0097 (11)	0.0079 (10)	0.0001 (10)
O21	0.0443 (19)	0.0255 (14)	0.0248 (14)	0.0174 (13)	−0.0118 (13)	0.0005 (11)
O22	0.087 (3)	0.043 (2)	0.0364 (19)	0.037 (2)	0.026 (2)	0.0151 (16)
O24	0.0195 (12)	0.0172 (11)	0.0146 (11)	0.0050 (9)	−0.0019 (9)	0.0040 (8)
O25	0.0198 (12)	0.0216 (12)	0.0241 (13)	0.0072 (10)	0.0019 (10)	−0.0004 (10)

Geometric parameters (Å, º) top

C1—N1	1.296 (4)	N5—Cu4	1.903 (3)
C1—O2	1.297 (4)	N6—Cu4	2.008 (3)
C1—C2	1.503 (4)	N6—H6A	0.9100
C2—N2	1.475 (5)	N6—H6B	0.9100
C2—H2C	0.9900	N7—O7	1.391 (3)
C2—H2D	0.9900	N7—Cu5	1.902 (3)
C3—N3	1.294 (4)	N8—Cu5	2.019 (3)
C3—O4	1.297 (4)	N8—H8A	0.9100
C3—C4	1.508 (5)	N8—H8B	0.9100
C4—N4	1.478 (4)	N9—O9	1.393 (3)
C4—H4C	0.9900	N9—Cu1	1.897 (2)
C4—H4D	0.9900	N10—Cu1	2.013 (3)
C5—N5	1.296 (4)	N10—H10A	0.9100
C5—O6	1.302 (4)	N10—H10B	0.9100
C5—C6	1.504 (4)	N11—O17	1.234 (4)
C6—N6	1.485 (4)	N11—O16	1.252 (5)
C6—H6C	0.9900	N11—O15	1.253 (4)
C6—H6D	0.9900	Cu1—O1	1.930 (2)
C7—N7	1.296 (4)	Cu1—O2	1.948 (2)
C7—O8	1.299 (4)	Cu1—O18	2.471 (3)
C7—C8	1.504 (4)	Cu2—O3	1.926 (2)
C8—N8	1.485 (4)	Cu2—O4	1.940 (2)
C8—H8C	0.9900	Cu2—O15	2.463 (3)
C8—H8D	0.9900	Cu3—O5	1.939 (2)
C9—O10	1.294 (3)	Cu3—O6	1.949 (2)
C9—N9	1.297 (4)	Cu3—O19	2.437 (3)
C9—C10	1.502 (4)	Cu4—O7	1.937 (2)
C10—N10	1.487 (4)	Cu4—O8	1.949 (2)
C10—H10C	0.9900	Cu4—O20	2.405 (3)
C10—H10D	0.9900	Cu5—O9	1.931 (2)
C11—O12	1.239 (11)	Cu5—O10	1.941 (2)
C11—O14	1.283 (12)	Cu5—O24	2.443 (3)
C11—O13	1.305 (13)	Ho1—O11	2.358 (2)
C11—Ho1	2.683 (14)	Ho1—O3	2.374 (2)
O12—Ho1	2.304 (16)	Ho1—O7	2.404 (2)
O13—Ho1	2.30 (3)	Ho1—O9	2.407 (2)
O23—H23A	0.8779	Ho1—O1	2.446 (2)
O23—H23B	0.8290	Ho1—O5	2.475 (2)
C11B—O14B	1.261 (9)	O11—H11A	0.817 (19)
C11B—O12B	1.262 (10)	O11—H11B	0.813 (19)
C11B—O13B	1.309 (10)	O18—H18A	0.821 (19)
C11B—Ho1	2.817 (10)	O18—H18B	0.834 (19)
O12B—Ho1	2.374 (12)	O19—H19A	0.820 (19)
O13B—Ho1	2.35 (2)	O19—H19B	0.826 (19)
N1—O1	1.391 (3)	O20—H20A	0.824 (19)
N1—Cu2	1.898 (3)	O20—H20B	0.814 (19)
N2—Cu2	1.987 (3)	O21—H21A	0.822 (19)
N2—H2A	0.9100	O21—H21B	0.827 (19)
N2—H2B	0.9100	O22—H22A	0.87 (2)
N3—O3	1.400 (3)	O22—H22B	0.86 (2)
N3—Cu3	1.908 (3)	O24—H24A	0.810 (19)
N4—Cu3	2.010 (3)	O24—H24B	0.820 (19)
N4—H4A	0.9100	O25—H25A	0.817 (19)
N4—H4B	0.9100	O25—H25B	0.826 (19)
N5—O5	1.392 (3)

N1—C1—O2	123.5 (3)	O4—Cu2—O15	86.17 (10)
N1—C1—C2	115.0 (3)	N2—Cu2—O15	94.35 (12)
O2—C1—C2	121.5 (3)	N3—Cu3—O5	90.80 (10)
N2—C2—C1	109.7 (3)	N3—Cu3—O6	168.64 (12)
N2—C2—H2C	109.7	O5—Cu3—O6	85.53 (9)
C1—C2—H2C	109.7	N3—Cu3—N4	82.62 (12)
N2—C2—H2D	109.7	O5—Cu3—N4	171.72 (13)
C1—C2—H2D	109.7	O6—Cu3—N4	99.97 (11)
H2C—C2—H2D	108.2	N3—Cu3—O19	97.77 (10)
N3—C3—O4	124.0 (3)	O5—Cu3—O19	97.72 (10)
N3—C3—C4	115.6 (3)	O6—Cu3—O19	93.38 (10)
O4—C3—C4	120.4 (3)	N4—Cu3—O19	88.20 (13)
N4—C4—C3	110.2 (3)	N5—Cu4—O7	91.47 (10)
N4—C4—H4C	109.6	N5—Cu4—O8	162.00 (11)
C3—C4—H4C	109.6	O7—Cu4—O8	84.51 (9)
N4—C4—H4D	109.6	N5—Cu4—N6	83.87 (11)
C3—C4—H4D	109.6	O7—Cu4—N6	173.92 (11)
H4C—C4—H4D	108.1	O8—Cu4—N6	98.74 (10)
N5—C5—O6	123.9 (3)	N5—Cu4—O20	101.33 (10)
N5—C5—C6	116.3 (3)	O7—Cu4—O20	99.21 (10)
O6—C5—C6	119.8 (3)	O8—Cu4—O20	96.64 (9)
N6—C6—C5	110.8 (3)	N6—Cu4—O20	85.56 (11)
N6—C6—H6C	109.5	N7—Cu5—O9	89.41 (10)
C5—C6—H6C	109.5	N7—Cu5—O10	170.18 (10)
N6—C6—H6D	109.5	O9—Cu5—O10	85.63 (9)
C5—C6—H6D	109.5	N7—Cu5—N8	83.25 (11)
H6C—C6—H6D	108.1	O9—Cu5—N8	169.11 (11)
N7—C7—O8	123.2 (3)	O10—Cu5—N8	100.38 (10)
N7—C7—C8	116.1 (3)	N7—Cu5—O24	95.87 (10)
O8—C7—C8	120.7 (3)	O9—Cu5—O24	87.88 (9)
N8—C8—C7	110.6 (2)	O10—Cu5—O24	92.41 (9)
N8—C8—H8C	109.5	N8—Cu5—O24	100.83 (10)
C7—C8—H8C	109.5	O13—Ho1—O12	56.5 (4)
N8—C8—H8D	109.5	O13—Ho1—O11	152.9 (5)
C7—C8—H8D	109.5	O12—Ho1—O11	150.1 (3)
H8C—C8—H8D	108.1	O13B—Ho1—O11	148.4 (3)
O10—C9—N9	124.0 (3)	O13—Ho1—O3	96.3 (8)
O10—C9—C10	120.0 (3)	O12—Ho1—O3	86.1 (3)
N9—C9—C10	116.1 (3)	O13B—Ho1—O3	94.1 (6)
N10—C10—C9	110.9 (3)	O11—Ho1—O3	91.94 (8)
N10—C10—H10C	109.5	O13B—Ho1—O12B	53.9 (3)
C9—C10—H10C	109.5	O11—Ho1—O12B	156.3 (3)
N10—C10—H10D	109.5	O3—Ho1—O12B	93.6 (3)
C9—C10—H10D	109.5	O13—Ho1—O7	102.0 (6)
H10C—C10—H10D	108.1	O12—Ho1—O7	79.5 (4)
O12—C11—O14	120.4 (12)	O13B—Ho1—O7	106.6 (5)
O12—C11—O13	117.9 (14)	O11—Ho1—O7	85.22 (8)
O14—C11—O13	121.7 (13)	O3—Ho1—O7	144.68 (8)
O12—C11—Ho1	59.0 (8)	O12B—Ho1—O7	77.0 (3)
O14—C11—Ho1	179.1 (14)	O13—Ho1—O9	81.6 (7)
O13—C11—Ho1	58.9 (12)	O12—Ho1—O9	121.8 (3)
C11—O12—Ho1	93.5 (9)	O13B—Ho1—O9	80.2 (5)
C11—O13—Ho1	92.0 (13)	O11—Ho1—O9	76.01 (8)
H23A—O23—H23B	137.8	O3—Ho1—O9	141.82 (7)
O14B—C11B—O12B	124.9 (10)	O12B—Ho1—O9	112.0 (3)
O14B—C11B—O13B	122.2 (10)	O7—Ho1—O9	71.34 (7)
O12B—C11B—O13B	112.9 (10)	O13—Ho1—O1	76.1 (4)
O14B—C11B—Ho1	178.2 (8)	O12—Ho1—O1	124.9 (4)
O12B—C11B—Ho1	56.8 (6)	O13B—Ho1—O1	70.4 (3)
O13B—C11B—Ho1	56.1 (9)	O11—Ho1—O1	82.19 (9)
C11B—O12B—Ho1	96.8 (7)	O3—Ho1—O1	71.84 (7)
C11B—O13B—Ho1	96.4 (9)	O12B—Ho1—O1	121.4 (3)
C1—N1—O1	116.0 (3)	O7—Ho1—O1	141.85 (8)
C1—N1—Cu2	119.6 (2)	O9—Ho1—O1	70.69 (7)
O1—N1—Cu2	124.2 (2)	O13—Ho1—O5	125.9 (5)
C2—N2—Cu2	111.84 (19)	O12—Ho1—O5	69.8 (3)
C2—N2—H2A	109.2	O13B—Ho1—O5	130.1 (4)
Cu2—N2—H2A	109.2	O11—Ho1—O5	81.21 (9)
C2—N2—H2B	109.2	O3—Ho1—O5	72.17 (7)
Cu2—N2—H2B	109.2	O12B—Ho1—O5	78.7 (3)
H2A—N2—H2B	107.9	O7—Ho1—O5	72.61 (7)
C3—N3—O3	115.4 (3)	O9—Ho1—O5	138.51 (7)
C3—N3—Cu3	118.6 (2)	O1—Ho1—O5	139.56 (7)
O3—N3—Cu3	125.27 (18)	O13—Ho1—C11	29.1 (3)
C4—N4—Cu3	110.7 (2)	O12—Ho1—C11	27.5 (3)
C4—N4—H4A	109.5	O11—Ho1—C11	175.1 (4)
Cu3—N4—H4A	109.5	O3—Ho1—C11	91.9 (4)
C4—N4—H4B	109.5	O7—Ho1—C11	89.9 (4)
Cu3—N4—H4B	109.5	O9—Ho1—C11	102.7 (4)
H4A—N4—H4B	108.1	O1—Ho1—C11	101.9 (4)
C5—N5—O5	116.0 (2)	O5—Ho1—C11	97.1 (3)
C5—N5—Cu4	117.0 (2)	O13B—Ho1—C11B	27.5 (2)
O5—N5—Cu4	126.14 (19)	O11—Ho1—C11B	172.5 (3)
C6—N6—Cu4	109.22 (19)	O3—Ho1—C11B	94.7 (3)
C6—N6—H6A	109.8	O12B—Ho1—C11B	26.4 (3)
Cu4—N6—H6A	109.8	O7—Ho1—C11B	91.3 (3)
C6—N6—H6B	109.8	O9—Ho1—C11B	96.6 (3)
Cu4—N6—H6B	109.8	O1—Ho1—C11B	96.6 (3)
H6A—N6—H6B	108.3	O5—Ho1—C11B	104.1 (3)
C7—N7—O7	115.5 (2)	N1—O1—Cu1	107.69 (18)
C7—N7—Cu5	119.1 (2)	N1—O1—Ho1	123.14 (18)
O7—N7—Cu5	125.31 (18)	Cu1—O1—Ho1	125.76 (10)
C8—N8—Cu5	110.78 (19)	C1—O2—Cu1	107.06 (18)
C8—N8—H8A	109.5	N3—O3—Cu2	107.65 (16)
Cu5—N8—H8A	109.5	N3—O3—Ho1	124.14 (16)
C8—N8—H8B	109.5	Cu2—O3—Ho1	128.11 (11)
Cu5—N8—H8B	109.5	C3—O4—Cu2	106.88 (19)
H8A—N8—H8B	108.1	N5—O5—Cu3	107.34 (17)
C9—N9—O9	115.8 (2)	N5—O5—Ho1	121.38 (17)
C9—N9—Cu1	118.3 (2)	Cu3—O5—Ho1	123.44 (10)
O9—N9—Cu1	125.40 (19)	C5—O6—Cu3	106.62 (19)
C10—N10—Cu1	110.2 (2)	N7—O7—Cu4	107.95 (16)
C10—N10—H10A	109.6	N7—O7—Ho1	124.58 (17)
Cu1—N10—H10A	109.6	Cu4—O7—Ho1	125.63 (10)
C10—N10—H10B	109.6	C7—O8—Cu4	107.32 (18)
Cu1—N10—H10B	109.6	N9—O9—Cu5	107.61 (16)
H10A—N10—H10B	108.1	N9—O9—Ho1	125.18 (16)
O17—N11—O16	120.7 (4)	Cu5—O9—Ho1	126.63 (10)
O17—N11—O15	121.9 (3)	C9—O10—Cu5	107.02 (19)
O16—N11—O15	117.4 (3)	Ho1—O11—H11A	122 (3)
N9—Cu1—O1	89.22 (10)	Ho1—O11—H11B	122 (3)
N9—Cu1—O2	171.80 (11)	H11A—O11—H11B	114 (5)
O1—Cu1—O2	85.31 (9)	N11—O15—Cu2	124.4 (2)
N9—Cu1—N10	83.88 (11)	Cu1—O18—H18A	93 (4)
O1—Cu1—N10	165.90 (12)	Cu1—O18—H18B	93 (4)
O2—Cu1—N10	100.11 (11)	H18A—O18—H18B	114 (5)
N9—Cu1—O18	92.05 (10)	Cu3—O19—H19A	104 (3)
O1—Cu1—O18	95.36 (10)	Cu3—O19—H19B	118 (3)
O2—Cu1—O18	94.54 (9)	H19A—O19—H19B	108 (5)
N10—Cu1—O18	97.16 (11)	Cu4—O20—H20A	105 (4)
N1—Cu2—O3	90.61 (10)	Cu4—O20—H20B	137 (4)
N1—Cu2—O4	168.51 (11)	H20A—O20—H20B	116 (5)
O3—Cu2—O4	85.63 (9)	H21A—O21—H21B	99 (6)
N1—Cu2—N2	82.56 (12)	H22A—O22—H22B	100 (6)
O3—Cu2—N2	173.12 (11)	Cu5—O24—H24A	112 (3)
O4—Cu2—N2	100.93 (11)	Cu5—O24—H24B	104 (3)
N1—Cu2—O15	104.57 (11)	H24A—O24—H24B	106 (5)
O3—Cu2—O15	88.10 (10)	H25A—O25—H25B	105 (5)

N1—C1—C2—N2	8.4 (4)	C9—N9—Cu1—N10	7.6 (2)
O2—C1—C2—N2	−169.9 (3)	O9—N9—Cu1—N10	178.8 (2)
N3—C3—C4—N4	−2.7 (4)	C9—N9—Cu1—O18	104.6 (2)
O4—C3—C4—N4	177.8 (3)	O9—N9—Cu1—O18	−84.2 (2)
N5—C5—C6—N6	1.1 (4)	C1—N1—Cu2—O3	173.7 (2)
O6—C5—C6—N6	−178.8 (3)	O1—N1—Cu2—O3	−12.2 (2)
N7—C7—C8—N8	−3.6 (4)	C1—N1—Cu2—O4	103.0 (5)
O8—C7—C8—N8	177.4 (3)	O1—N1—Cu2—O4	−82.9 (6)
O10—C9—C10—N10	−174.3 (3)	C1—N1—Cu2—N2	−5.5 (3)
N9—C9—C10—N10	6.7 (4)	O1—N1—Cu2—N2	168.6 (3)
O14—C11—O12—Ho1	179.1 (16)	C1—N1—Cu2—O15	−98.1 (2)
O13—C11—O12—Ho1	−2.4 (19)	O1—N1—Cu2—O15	76.0 (2)
O12—C11—O13—Ho1	2.4 (19)	C1—N1—O1—Cu1	−6.7 (3)
O14—C11—O13—Ho1	−179.2 (16)	Cu2—N1—O1—Cu1	178.98 (15)
O14B—C11B—O12B—Ho1	179.6 (12)	C1—N1—O1—Ho1	−166.9 (2)
O13B—C11B—O12B—Ho1	−1.4 (14)	Cu2—N1—O1—Ho1	18.8 (3)
O14B—C11B—O13B—Ho1	−179.5 (12)	N1—C1—O2—Cu1	2.0 (4)
O12B—C11B—O13B—Ho1	1.4 (14)	C2—C1—O2—Cu1	−179.9 (2)
O2—C1—N1—O1	3.3 (4)	C3—N3—O3—Cu2	4.8 (3)
C2—C1—N1—O1	−174.9 (2)	Cu3—N3—O3—Cu2	−165.17 (16)
O2—C1—N1—Cu2	177.9 (2)	C3—N3—O3—Ho1	−171.8 (2)
C2—C1—N1—Cu2	−0.3 (4)	Cu3—N3—O3—Ho1	18.3 (3)
C1—C2—N2—Cu2	−12.2 (3)	N3—C3—O4—Cu2	−4.1 (4)
O4—C3—N3—O3	−0.4 (5)	C4—C3—O4—Cu2	175.3 (2)
C4—C3—N3—O3	−179.8 (3)	C5—N5—O5—Cu3	−6.4 (3)
O4—C3—N3—Cu3	170.2 (2)	Cu4—N5—O5—Cu3	162.64 (16)
C4—C3—N3—Cu3	−9.2 (4)	C5—N5—O5—Ho1	−156.4 (2)
C3—C4—N4—Cu3	12.1 (4)	Cu4—N5—O5—Ho1	12.6 (3)
O6—C5—N5—O5	1.8 (5)	N5—C5—O6—Cu3	3.7 (4)
C6—C5—N5—O5	−178.0 (3)	C6—C5—O6—Cu3	−176.4 (2)
O6—C5—N5—Cu4	−168.2 (2)	C7—N7—O7—Cu4	9.1 (3)
C6—C5—N5—Cu4	11.9 (4)	Cu5—N7—O7—Cu4	−171.06 (15)
C5—C6—N6—Cu4	−12.2 (3)	C7—N7—O7—Ho1	174.4 (2)
O8—C7—N7—O7	−0.8 (4)	Cu5—N7—O7—Ho1	−5.8 (3)
C8—C7—N7—O7	−179.8 (3)	N7—C7—O8—Cu4	−8.0 (4)
O8—C7—N7—Cu5	179.4 (2)	C8—C7—O8—Cu4	171.0 (2)
C8—C7—N7—Cu5	0.4 (4)	C9—N9—O9—Cu5	0.9 (3)
C7—C8—N8—Cu5	4.8 (3)	Cu1—N9—O9—Cu5	−170.52 (14)
O10—C9—N9—O9	−1.0 (4)	C9—N9—O9—Ho1	172.60 (19)
C10—C9—N9—O9	177.9 (2)	Cu1—N9—O9—Ho1	1.2 (3)
O10—C9—N9—Cu1	171.0 (2)	N9—C9—O10—Cu5	0.6 (3)
C10—C9—N9—Cu1	−10.0 (3)	C10—C9—O10—Cu5	−178.3 (2)
C9—C10—N10—Cu1	−0.8 (3)	O17—N11—O15—Cu2	132.2 (3)
C9—N9—Cu1—O1	−160.1 (2)	O16—N11—O15—Cu2	−50.0 (5)
O9—N9—Cu1—O1	11.1 (2)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O23—H23A···O16ⁱ	0.88	1.87	2.747 (11)	173
O23—H23B···O14	0.83	1.98	2.509 (13)	121
N2—H2A···O13ⁱ	0.91	2.17	3.00 (3)	150
N2—H2A···O13Bⁱ	0.91	2.05	2.90 (2)	155
N2—H2B···O16	0.91	2.26	3.078 (5)	149
N4—H4A···O21	0.91	2.07	2.914 (5)	154
N4—H4B···O23ⁱⁱ	0.91	1.98	2.726 (10)	138
N6—H6A···O16ⁱⁱⁱ	0.91	2.25	3.060 (5)	149
N6—H6B···N5^iv	0.91	2.52	3.267 (4)	139
N6—H6B···O5^iv	0.91	2.46	3.359 (4)	171
N8—H8A···O7^v	0.91	2.49	3.285 (4)	146
N8—H8A···O20^v	0.91	2.41	3.017 (4)	124
N8—H8B···O22^vi	0.91	2.17	3.048 (5)	163
N10—H10A···O17^vii	0.91	2.23	3.024 (4)	145
N10—H10B···O11^viii	0.91	2.39	3.183 (4)	146
O11—H11A···O25	0.82 (2)	1.86 (2)	2.660 (4)	165 (5)
O11—H11B···O24	0.81 (2)	2.00 (2)	2.801 (4)	166 (5)
O18—H18A···O4ⁱ	0.82 (2)	2.01 (3)	2.801 (3)	160 (5)
O18—H18B···O13	0.83 (2)	2.04 (3)	2.87 (2)	173 (5)
O18—H18B···O13B	0.83 (2)	1.84 (3)	2.671 (18)	171 (5)
O19—H19A···O8^iv	0.82 (2)	1.90 (2)	2.713 (3)	174 (5)
O19—H19B···O18ⁱⁱ	0.83 (2)	2.02 (2)	2.840 (4)	174 (5)
O20—H20A···O10^v	0.82 (2)	1.96 (3)	2.732 (3)	156 (5)
O20—H20B···O14^ix	0.81 (2)	2.21 (3)	2.997 (12)	162 (5)
O20—H20B···O14B^ix	0.81 (2)	2.27 (3)	3.060 (9)	163 (5)
O21—H21A···O6^x	0.82 (2)	2.07 (3)	2.813 (4)	151 (6)
O21—H21B···O22	0.83 (2)	1.87 (3)	2.638 (5)	154 (6)
O22—H22A···O14^ix	0.87 (2)	1.88 (3)	2.736 (12)	170 (7)
O22—H22A···O14B^ix	0.87 (2)	1.84 (2)	2.709 (9)	173 (7)
O22—H22B···O12	0.86 (2)	1.74 (3)	2.600 (16)	170 (7)
O22—H22B···O14	0.86 (2)	2.51 (6)	3.088 (11)	125 (6)
O22—H22B···O12B	0.86 (2)	1.93 (3)	2.791 (14)	173 (7)
O24—H24A···O2^viii	0.81 (2)	1.99 (2)	2.781 (3)	166 (5)
O24—H24B···O21^vi	0.82 (2)	1.94 (2)	2.759 (4)	174 (5)
O25—H25A···O19	0.82 (2)	1.96 (2)	2.779 (4)	177 (5)
O25—H25B···O15	0.83 (2)	1.95 (2)	2.751 (4)	165 (5)

Comparison of single crystal data and structure refinement details for complexes 1–3 with those of their earlier reported Eu^III analogue (CCDC127569, Stemmler et al., 1999) top

	CCDC127569	Complex 1	Complex 2	Complex 3
Formula	[EuCu₅(GlyHA)₅(CO₃)(NO₃)(H₂O)₅]·3.5H₂O	[GdCu₅(GlyHA)₅(CO₃)(NO₃)(H₂O)₅]·3.5(H₂O)	[DyCu₅(GlyHA)₅(CO₃)(NO₃)(H₂O)₅]·3.28(H₂O)	[HoCu₅(GlyHA)₅(CO₃)(NO₃)(H₂O)₅]·3.445(H₂O)
M (g mol^-1)	1186.17	1190.49	1191.77	1197.21
Crystal system	Triclinic	Triclinic	Triclinic	Triclinic
Space group	P1	P1	P1	P1
a (Å)	11.163 (5)	11.2057 (15)	11.1083 (5)	11.2027 (9)
b (Å)	11.524 (4)	11.5054 (15)	11.4991 (5)	11.4955 (9)
c (Å)	13.323 (4)	13.2983 (10)	13.2894 (6)	13.2467 (10)
α (°)	93.85 (3)	94.026 (4)	93.9235 (16)	94.001 (3)
β (°)	94.79 (3)	94.942 (3)	94.7713 (17)	94.784 (3)
γ (°)	107.14 (3)	107.558 (3)	107.1470 (17)	107.518 (3)
Volume (Å³)	1624.5 (10)	1620.2 (3)	1608.73 (13)	1613.0 (2)
Z	2	2	2	2
T (K)	293 (2)	150 (2)	150 (2)	150 (2)
Range of data collection	2.53 °<2θ < 26.03°	3.091° < 2θ <33.234°	3.091° <2θ <28.693°	2.544° <2θ <33.243°
ρ_calc (g cm^-3)	2.425	2.440	2.460	2.467
Absorption coefficient (mm^-1)	5.229	5.353	5.651	5.773
F(000)	1168	1170	1170	1174.9
Collected reflections	6344	118155	74286	50443
Reflections unique	6344	12399	8274	12306
R_int	0.1272	0.0560	0.0483	0.0417
Goodness-of-fit on F²	1.114	1.050	1.084	1.053
R₁([I>2σ(I)]^a	0.1230	0.0343	0.0307	0.0334
wR₂[I>2σ(I)]^b	0.2979	0.0681	0.0709	0.0769

Notes: (a) R₁ = Σ||F_o| - |F_c||/Σ|F_o|, (b) wR₂= {Σ[w(F_o² - F_c²)²]/Σ[w(F_o²)²]}^1/2

Selected bond lengths (Å) for complex 1 top

Cu1—O1	1.929 (2)	Cu2—O3	1.929 (2)	Cu3—O5	1.935 (2)
Cu1—O2	1.949 (2)	Cu2—O4	1.939 (2)	Cu3—O6	1.952 (2)
Cu1—N9	1.898 (2)	Cu2—N1	1.902 (3)	Cu3—N3	1.910 (3)
Cu1—N10	2.016 (3)	Cu2—N2	1.985 (3)	Cu3—N4	2.010 (3)
Cu1—O18w	2.470 (3)	Cu2—O15_(NO3)	2.469 (3)	Cu3—O19w	2.444 (2)
Cu4—O7	1.938 (2)	Cu5—O9	1.931 (2)	Gd1—O1	2.457 (2)
Cu4—O8	1.953 (2)	Cu5—O10	1.939 (2)	Gd1—O3	2.381 (2)
Cu4—N5	1.906 (2)	Cu5—N7	1.901 (2)	Gd1—O5	2.483 (2)
Cu4—N6	2.005 (2)	Cu5—N8	2.022 (2)	Gd1—O7	2.408 (2)
Cu4—O20w	2.401 (3)	Cu5—O24w	2.449 (2)	Gd1—O9	2.414 (2)
C11—O12	1.284 (9)	C11B—O12B	1.310 (10)	Gd1—O11w	2.359 (2)
C11—O13	1.307 (10)	C11B—O13B	1.307 (10)	Gd1—O12	2.317 (11)
C11—O14	1.252 (9)	C11B—O14B	1.253 (9)	Gd1—O13	2.288 (17)
Gd1—O12B	2.396 (10)	Gd1—O13B	2.388 (17)

Selected bond lengths (Å) for complex 2 top

Cu1—O1	1.931 (3)	Cu2—O3	1.931 (3)	Cu3—O5	1.941 (3)
Cu1—O2	1.949 (3)	Cu2—O4	1.939 (3)	Cu3—O6	1.954 (3)
Cu1—N9	1.897 (3)	Cu2—N1	1.907 (4)	Cu3—N3	1.905 (4)
Cu1—N10	2.012 (4)	Cu2—N2	1.983 (4)	Cu3—N4	2.017 (4)
Cu1—O18w	2.476 (3)	Cu2—O15_(NO3)	2.464 (3)	Cu3—O19w	2.430 (3)
Cu4—O7	1.936 (3)	Cu5—O9	1.932 (3)	Dy1—O1	2.453 (3)
Cu4—O8	1.956 (3)	Cu5—O10	1.941 (3)	Dy1—O3	2.382 (3)
Cu4—N5	1.904 (3)	Cu5—N7	1.899 (3)	Dy1—O5	2.469 (3)
Cu4—N6	2.005 (3)	Cu5—N8	2.021 (3)	Dy1—O7	2.412 (3)
Cu4—O20w	2.400 (3)	Cu5—O24w	2.440 (3)	Dy1—O9	2.410 (3)
C11—O12	1.275 (16)	C11B—O12B	1.295 (9)	Dy1—O11w	2.357 (3)
C11—O13	1.318 (16)	C11B—O13B	1.326 (8)	Dy1—O12	2.27 (2)
C11—O14	1.256 (15)	C11B—O14B	1.251 (8)	Dy1—O13	2.31 (3)
Dy1—O12B	2.380 (8)	Dy1—O13B	2.347 (12)

Selected bond lengths (Å) for complex 3 top

Cu1—O1	1.930 (2)	Cu2—O3	1.926 (2)	Cu3—O5	1.939 (2)
Cu1—O2	1.948 (2)	Cu2—O4	1.940 (2)	Cu3—O6	1.949 (2)
Cu1—N9	1.897 (2)	Cu2—N1	1.898 (3)	Cu3—N3	1.908 (3)
Cu1—N10	2.013 (3)	Cu2–N2	1.987 (3)	Cu3—N4	2.010 (3)
Cu1—O18w	2.471 (3)	Cu2—O15_(NO3)	2.463 (3)	Cu3—O19w	2.437 (3)
Cu4—O7	1.937 (2)	Cu5—O9	1.931 (2)	Ho1—O1	2.446 (2)
Cu4—O8	1.949 (2)	Cu5—O10	1.941 (2)	Ho1—O3	2.374 (2)
Cu4—N5	1.903 (3)	Cu5—N7	1.902 (3)	Ho1—O5	2.475 (2)
Cu4—N6	2.008 (3)	Cu5—N8	2.019 (3)	Ho1—O7	2.404 (2)
Cu4—O20w	2.405 (3)	Cu5—O24w	2.443 (3)	Ho1—O9	2.407 (2)
C11—O12	1.239 (11)	C11B—O12B	1.262 (10)	Ho1—O11w	2.358 (2)
C11—O13	1.305 (13)	C11B—O13B	1.309 (10)	Ho1—O12	2.304 (16)
C11—O14	1.283 (12)	C11B—O14B	1.261 (9)	Ho1—O13	2.30 (3)
Ho1—O12B	2.374 (12)	Ho1—O13B	2.35 (2)

Selected angles (°) for complex 1 top

O1—Cu1—O2	85.28 (9)	O3—Cu2—O4	85.63 (9)	O5—Cu3—O6	85.44 (9)
N9—Cu1—O1	89.32 (9)	N1—Cu2—O3	90.48 (9)	N3—Cu3—O5	90.98 (10)
O2—Cu1—N10	100.27 (10)	O4—Cu2—N2	100.83 (10)	O6—Cu3—N4	99.85 (11)-
N9–Cu1—N10	83.70 (10)	N1—Cu2—N2	82.87 (11)	N3—Cu3—N4	82.70 (12)
O7—Cu4—O8	84.56 (8)	O9—Cu5—O10	85.57 (8)	O3—Gd1—O1	71.71 (7)
N5—Cu4—O7	91.39 (9)	N7—Cu5—O9	89.59 (9)	O3—Gd1—O5	72.08 (7)
O8—Cu4—N6	98.79 (9)	O10—Cu5—N8	100.42 (9)	O7—Gd1—O5	72.87 (7)
N5—Cu4—N6	83.88 (10)	N7—Cu5—N8	83.14 (10)	O7—Gd1—O9	71.27 (6)
O13—Gd1—O12	56.4 (3)	O13B–Gd1–O12B	54.1 (3)	O9—Gd1—O1	70.62 (7)

Selected angles (°) for complex 2 top

O1—Cu1—O2	85.19 (12)	O3—Cu2—O4	85.41 (12)	O5–Cu3—O6	85.39 (12)
O1—Cu1—N9	89.39 (13)	O3—Cu2—N1	90.66 (13)	O5—Cu3—N3	90.67 (13)
O2—Cu1—N10	100.37 (13)	O4—Cu2—N2	101.00 (14)	O6—Cu3—N4	100.11 (14)
N9—Cu1—N10	83.73 (14)	N1—Cu2—N2	82.65 (15)	N3—Cu3—N4	82.79 (15)
O7—Cu4—O8	84.56 (11)	O9—Cu5—O10	85.47 (11)	O1—Dy1—O3	71.77 (9)
O7—Cu4—N5	91.62 (13)	O9—Cu5—N7	89.53 (12)	O3—Dy1—O5	71.92 (9)
O8—Cu4—N6	98.55 (13)	O10—Cu5—N8	100.49 (13)	O5—Dy1—O7	72.60 (9)
N5—Cu4—N6	83.78 (14)	N7—Cu5—N8	83.23 (14)	O7—Dy1—O9	71.21 (9)
O12—Dy1—O13	57.1 (6)	O12B–Dy1—O13B	54.7 (2)	O9—Dy1—O1	70.83 (9)

Selected angles (°) for complex 3 top

O1—Cu1—O2	85.31 (9)	O3—Cu2—O4	85.63 (9)	O5—Cu3—O6	85.53 (9)
O1—Cu1—N9	89.22 (10)	O3—Cu2—N1	90.61 (10)	O5—Cu3—N3	90.80 (10)
O2—Cu1—N10	100.11 (11)	O4–Cu2—N2	100.93 (11)	O6—Cu3—N4	99.97 (11)
N9—Cu1—N10	83.88 (11)	N1—Cu2—N2	82.56 (12)	N3—Cu3—N4	82.62 (12)
O7—Cu4—O8	84.51 (9)	O9—Cu5—O10	85.63 (9)	O1—Ho1—O3	71.84 (7)
O7—Cu4—N5	91.47 (10)	O9—Cu5—N7	89.41 (10)	O3—Ho1—O5	72.17 (7)
O8—Cu4—N6	98.74 (10)	O10—Cu5—N8	100.38 (10)	O5—Ho1—O7	72.61 (7)
N5—Cu4—N6	83.87 (11)	N7—Cu5—N8	83.25 (11)	O7—Ho1—O9	71.34 (7)
O12—Ho1—O13	56.5 (4)	O12B—Ho1—O13B	53.9 (3)	O9—Ho1—O1	70.69 (7)

Comparison of selected characteristics of 1–3 with the earlier reported Eu^III analogue (CCDC127569; Stemmler et al., 1999) top

	CCDC127569	Complex 1	Complex 2	Complex 3
	EuCu₅	GdCu₅	DyCu₅	HoCu₅
Range of Ln···Cu separations (Å)	3.890 (2)–3.911 (3)	3.8699 (5)–3.9097 (5)	3.8715 (5)–3.9016 (6)	3.8670 (5)–3.9021 (5)
Range of Cu···Cu separations (Å)	4.575 (3)–4.589 (3)	4.5677 (7)–4.5846 (7)	4.5645 (7)–4.5797 (8)	4.5583 (7)–4.5808 (7)
Range of Ln—O_equat (Å)	2.406 (11)–2.493 (11)	2.381 (2)–2.484 (2)	2.382 (3)–2.469 (3)	2.374 (2)–2.475 (2)
Range of Ln—O_carbonate (Å)	2.369 (13)–2.392 (15)	2.288 (17)–2.396 (10)	2.27 (2)–2.380 (8)	2.30 (3)–2.374 (12)
Range of Cu—O_equat (Å)	1.901 (11)–1.972 (10)	1.929 (2)–1.953 (2)	1.931 (3)–1.956 (4)	1.929 (2)–1.953 (2)
Range of Cu—N_equat (Å)	1.886 (14)–2.022 (13)	1.898 (2)–2.022 (2)	1.898 (3)–2.022 (3)	1.898 (2)–2.022 (2)
Range of τ values (Addison et al., 1984) for pentacoordinate Cu^II ions	0.00–0.20	0.01–0.20	0.01–0.20	0.02–0.20
Ln^III coordination number	8	8	8	8
Average deviation of non-hydrogen atoms from Cu₅ plane (Å)	0.179	0.188	0.183	0.186
Largest deviation among non-hydrogen atoms from Cu₅ plane (Å)	0.605	0.606	0.602	0.597
Deviation of Ln^III ion from Cu₅ plane (Å)	0.351	0.337	0.354	0.330

Continuous shape calculations for octacoordinated Ln³⁺ ions in 1–3 obtained using Shape2.1 software (Casanova et al., 2005) top

	Complex 1	Complex 2	Complex 3
OP-8	31.930	31.846	31.915
HPY-8	22.627	22.698	22.560
HBPY-8	16.081	16.114	16.307
CU-8	12.990	12.970	12.794
SAPR-8	3.769	3.759	3.770
TDD-8	1.805	1.743	1.763
JGBF-8	12.037	12.418	12.302
JETBPY-8	27.751	27.478	27.602

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