# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


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#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
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data_jc149b
_database_code_depnum_ccdc_archive 'CCDC 913544'
#TrackingRef 'jc149b.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H94 Cl1 Gd1 N8 O34 V12'
_chemical_formula_weight         2083.26
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P21212
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
_cell_length_a                   15.6592(14)
_cell_length_b                   25.175(2)
_cell_length_c                   10.2383(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4036.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6828
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      25.6
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2086
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8070
_exptl_absorpt_correction_T_max  0.9157
_exptl_absorpt_process_details   SADABS
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(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 Quasar CCD'
_diffrn_measurement_method       '\w & \p scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            17042
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.51
_diffrn_reflns_theta_max         26.00
_reflns_number_total             7447
_reflns_number_gt                6573
_reflns_threshold_expression     >2\s(I)
_computing_data_collection       Apex2
_computing_cell_refinement       Apex2
_computing_data_reduction        Apex2
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond3
_computing_publication_material  WinGX
_refine_special_details          
;
DFIX restraints were applied to some disordered C-C distnaces in the
tetrabutylammonium cations and acetonitrile solvent molecules. SQUEEZE
was used to determine the number of solvent molecules in the
crystallographic formula.
No H atoms was added to the disordered solvent molecules.
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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       none
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(11)
_refine_ls_number_reflns         7447
_refine_ls_number_parameters     434
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0391
_refine_ls_wR_factor_ref         0.1011
_refine_ls_wR_factor_gt          0.0977
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.039
_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
Gd1 Gd 0.5000 0.5000 0.03193(4) 0.02830(12) Uani 1 2 d S . .
V1 V 0.42396(6) 0.40094(4) 0.22509(9) 0.0255(2) Uani 1 1 d . . .
V2 V 0.30334(6) 0.48566(4) 0.26751(9) 0.0248(2) Uani 1 1 d . . .
V3 V 0.33159(6) 0.43534(4) 0.53277(10) 0.0228(2) Uani 1 1 d . . .
V4 V 0.47345(6) 0.62231(4) 0.53334(9) 0.0223(2) Uani 1 1 d . . .
V5 V 0.33708(6) 0.54811(4) 0.58210(9) 0.0218(2) Uani 1 1 d . . .
V6 V 0.60583(6) 0.39576(4) 0.26788(9) 0.0239(2) Uani 1 1 d . . .
Cl1 Cl 0.5000 0.5000 0.40565(19) 0.0277(4) Uani 1 2 d S . .
O1 O 0.3872(3) 0.35140(17) 0.1467(4) 0.0352(10) Uani 1 1 d . . .
O2 O 0.2106(2) 0.47183(16) 0.2138(4) 0.0320(9) Uani 1 1 d . . .
O3 O 0.2464(2) 0.40548(16) 0.5769(4) 0.0325(10) Uani 1 1 d . . .
O4 O 0.4558(3) 0.68229(15) 0.5774(4) 0.0311(10) Uani 1 1 d . . .
O5 O 0.2547(2) 0.57301(16) 0.6483(4) 0.0279(9) Uani 1 1 d . . .
O6 O 0.6460(3) 0.34158(16) 0.2163(4) 0.0341(10) Uani 1 1 d . . .
O7 O 0.5282(2) 0.41893(16) 0.1443(3) 0.0276(9) Uani 1 1 d . . .
O8 O 0.3825(2) 0.46304(16) 0.1447(3) 0.0295(9) Uani 1 1 d . . .
O9 O 0.3167(2) 0.55542(14) 0.2289(3) 0.0258(8) Uani 1 1 d . . .
O10 O 0.3408(2) 0.41858(15) 0.3485(4) 0.0259(9) Uani 1 1 d . . .
O11 O 0.4979(3) 0.37203(15) 0.3495(3) 0.0242(8) Uani 1 1 d . . .
O12 O 0.3678(2) 0.59851(14) 0.4474(3) 0.0221(8) Uani 1 1 d . . .
O13 O 0.3534(2) 0.48410(14) 0.6611(3) 0.0240(9) Uani 1 1 d . . .
O14 O 0.4159(2) 0.38951(14) 0.5704(3) 0.0247(9) Uani 1 1 d . . .
O15 O 0.4282(2) 0.58074(15) 0.6604(3) 0.0243(9) Uani 1 1 d . . .
O16 O 0.2940(2) 0.50250(15) 0.4478(3) 0.0221(8) Uani 1 1 d . . .
O17 O 0.5414(3) 0.55422(18) -0.1477(4) 0.0193(10) Uiso 0.78 1 d P . .
O17' O 0.5000 0.5000 -0.2251(11) 0.026(2) Uiso 0.44 2 d SP . .
N1 N 0.3306(3) 0.2264(2) 0.5071(6) 0.0470(15) Uani 1 1 d . . .
N2 N 0.3629(3) 0.5407(2) -0.0610(4) 0.0374(13) Uani 1 1 d . . .
N3 N 0.7075(12) 0.3258(7) 0.8670(18) 0.032(4) Uiso 0.30 1 d P A 1
N3' N 0.7103(16) 0.3039(10) 0.911(2) 0.060(6) Uiso 0.30 1 d P B 2
N4 N 0.5373(14) 0.1110(8) 0.391(2) 0.046(5) Uiso 0.30 1 d PD . .
C1 C 0.4064(5) 0.2348(3) 0.4139(8) 0.0508(19) Uani 1 1 d . C .
H1A H 0.4097 0.2731 0.3924 0.061 Uiso 1 1 calc R . .
H1B H 0.4595 0.2253 0.4610 0.061 Uiso 1 1 calc R . .
C2 C 0.4042(5) 0.2042(3) 0.2890(9) 0.066(2) Uani 1 1 d . . .
H2A H 0.3523 0.2138 0.2390 0.079 Uiso 1 1 calc R C .
H2B H 0.4018 0.1657 0.3081 0.079 Uiso 1 1 calc R . .
C3 C 0.4835(6) 0.2164(3) 0.2076(9) 0.077(3) Uani 1 1 d . C .
H3A H 0.5350 0.2040 0.2545 0.092 Uiso 1 1 calc R . .
H3B H 0.4885 0.2553 0.1951 0.092 Uiso 1 1 calc R . .
C4 C 0.4778(7) 0.1879(5) 0.0692(10) 0.108(4) Uani 1 1 d . . .
H4A H 0.4661 0.1500 0.0817 0.163 Uiso 1 1 calc R C .
H4B H 0.5320 0.1923 0.0227 0.163 Uiso 1 1 calc R . .
H4C H 0.4316 0.2040 0.0179 0.163 Uiso 1 1 calc R . .
C5 C 0.2483(4) 0.2369(3) 0.4390(7) 0.0476(19) Uani 1 1 d . C .
H5A H 0.2013 0.2318 0.5023 0.057 Uiso 1 1 calc R . .
H5B H 0.2412 0.2101 0.3692 0.057 Uiso 1 1 calc R . .
C6 C 0.2388(4) 0.2916(3) 0.3785(8) 0.051(2) Uani 1 1 d . . .
H6A H 0.2825 0.2963 0.3096 0.061 Uiso 1 1 calc R C .
H6B H 0.2488 0.3190 0.4463 0.061 Uiso 1 1 calc R . .
C7 C 0.1498(5) 0.2997(3) 0.3190(10) 0.067(3) Uani 1 1 d . C .
H7A H 0.1400 0.2722 0.2514 0.081 Uiso 1 1 calc R . .
H7B H 0.1062 0.2948 0.3880 0.081 Uiso 1 1 calc R . .
C8 C 0.1392(5) 0.3496(4) 0.2632(12) 0.089(3) Uani 1 1 d . . .
H8A H 0.1492 0.3770 0.3293 0.133 Uiso 1 1 calc R C .
H8B H 0.0809 0.3529 0.2294 0.133 Uiso 1 1 calc R . .
H8C H 0.1800 0.3540 0.1914 0.133 Uiso 1 1 calc R . .
C9 C 0.3438(5) 0.2647(3) 0.6206(8) 0.0513(19) Uani 1 1 d . C 1
H9A H 0.4018 0.2590 0.6565 0.062 Uiso 1 1 calc R C 1
H9B H 0.3414 0.3014 0.5864 0.062 Uiso 1 1 calc R C 1
C10 C 0.2805(9) 0.2597(6) 0.7300(13) 0.070(4) Uiso 0.753(19) 1 d P C 1
H10A H 0.2809 0.2229 0.7638 0.084 Uiso 0.753(19) 1 calc PR C 1
H10B H 0.2225 0.2676 0.6971 0.084 Uiso 0.753(19) 1 calc PR C 1
C11 C 0.3027(9) 0.2978(6) 0.8388(13) 0.067(4) Uiso 0.753(19) 1 d P C 1
H11A H 0.3611 0.2904 0.8709 0.081 Uiso 0.753(19) 1 calc PR C 1
H11B H 0.3010 0.3347 0.8058 0.081 Uiso 0.753(19) 1 calc PR C 1
C12 C 0.2429(11) 0.2917(9) 0.9424(17) 0.131(8) Uiso 0.753(19) 1 d P C 1
H12A H 0.1847 0.2935 0.9074 0.196 Uiso 0.753(19) 1 calc PR C 1
H12B H 0.2512 0.3201 1.0066 0.196 Uiso 0.753(19) 1 calc PR C 1
H12C H 0.2516 0.2571 0.9846 0.196 Uiso 0.753(19) 1 calc PR C 1
C10' C 0.2666(13) 0.2776(9) 0.714(2) 0.013(6) Uiso 0.247(19) 1 d PD C 2
C11' C 0.2995(17) 0.3162(12) 0.820(2) 0.030(7) Uiso 0.247(19) 1 d PD C 2
C12' C 0.2287(17) 0.3320(13) 0.908(3) 0.048(10) Uiso 0.247(19) 1 d PD C 2
C13 C 0.3252(5) 0.1685(3) 0.5577(9) 0.058(2) Uani 1 1 d . C .
H13A H 0.2728 0.1653 0.6113 0.070 Uiso 1 1 calc R . .
H13B H 0.3179 0.1449 0.4812 0.070 Uiso 1 1 calc R . .
C14 C 0.3994(5) 0.1477(3) 0.6375(8) 0.061(2) Uani 1 1 d . . .
H14A H 0.4528 0.1504 0.5862 0.073 Uiso 1 1 calc R C .
H14B H 0.4060 0.1694 0.7176 0.073 Uiso 1 1 calc R . .
C15 C 0.3836(6) 0.0919(3) 0.6731(10) 0.072(3) Uani 1 1 d . C .
H15A H 0.3288 0.0899 0.7213 0.087 Uiso 1 1 calc R . .
H15B H 0.3768 0.0710 0.5917 0.087 Uiso 1 1 calc R . .
C16 C 0.4485(6) 0.0674(4) 0.7508(14) 0.109(4) Uani 1 1 d . . .
H16A H 0.5031 0.0687 0.7041 0.164 Uiso 1 1 calc R C .
H16B H 0.4331 0.0303 0.7678 0.164 Uiso 1 1 calc R . .
H16C H 0.4539 0.0865 0.8339 0.164 Uiso 1 1 calc R . .
C17 C 0.2948(5) 0.5560(3) -0.0542(6) 0.052(2) Uani 1 1 d . . .
C18 C 0.2061(5) 0.5755(4) -0.0438(8) 0.085(3) Uani 1 1 d . . .
H18A H 0.1773 0.5714 -0.1282 0.127 Uiso 1 1 calc R . .
H18B H 0.2065 0.6131 -0.0191 0.127 Uiso 1 1 calc R . .
H18C H 0.1756 0.5549 0.0228 0.127 Uiso 1 1 calc R . .
C19 C 0.6389(7) 0.3194(5) 0.8972(13) 0.104(4) Uiso 1 1 d D A 1
C20 C 0.5425(5) 0.3206(3) 0.9150(8) 0.058(2) Uiso 1 1 d D A 1
C21 C 0.549(3) 0.0664(10) 0.366(4) 0.103(16) Uiso 0.30 1 d PD . .
C22 C 0.5824(18) 0.0214(11) 0.457(3) 0.068(8) Uiso 0.30 1 d PD . .
C21' C 0.553(3) 0.0738(17) 0.418(5) 0.051(11) Uiso 0.20 1 d P . .
N4' N 0.509(3) 0.0932(16) 0.364(4) 0.062(10) Uiso 0.20 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Gd1 0.0309(2) 0.0416(2) 0.01239(18) 0.000 0.000 0.0122(2)
V1 0.0272(5) 0.0338(5) 0.0154(4) -0.0051(4) -0.0032(4) 0.0053(4)
V2 0.0225(4) 0.0368(6) 0.0151(4) -0.0022(4) -0.0034(4) 0.0055(4)
V3 0.0245(5) 0.0282(5) 0.0156(4) -0.0009(4) 0.0008(5) 0.0007(4)
V4 0.0277(5) 0.0235(5) 0.0158(4) 0.0002(4) 0.0014(4) 0.0032(4)
V5 0.0235(5) 0.0277(5) 0.0141(4) 0.0009(4) 0.0014(4) 0.0039(4)
V6 0.0273(5) 0.0311(5) 0.0135(4) -0.0036(4) -0.0010(4) 0.0092(4)
Cl1 0.0262(9) 0.0303(10) 0.0266(9) 0.000 0.000 0.0050(10)
O1 0.039(2) 0.042(3) 0.024(2) -0.0109(19) -0.005(2) 0.003(2)
O2 0.0247(19) 0.048(2) 0.023(2) -0.0073(19) -0.0059(19) 0.0033(19)
O3 0.029(2) 0.039(2) 0.029(2) -0.0014(19) 0.0016(19) -0.0020(19)
O4 0.038(2) 0.030(2) 0.025(2) 0.0016(18) 0.0014(19) 0.0068(19)
O5 0.028(2) 0.037(2) 0.019(2) -0.0007(18) 0.0036(18) 0.0049(19)
O6 0.043(2) 0.039(2) 0.0206(19) -0.0073(19) 0.001(2) 0.017(2)
O7 0.033(2) 0.038(2) 0.0120(18) 0.0015(16) 0.0002(17) 0.0090(19)
O8 0.031(2) 0.040(2) 0.0174(19) -0.0028(17) -0.0038(18) 0.012(2)
O9 0.0275(19) 0.037(2) 0.0130(17) 0.0008(17) -0.0041(17) 0.0073(18)
O10 0.030(2) 0.032(2) 0.0164(19) -0.0054(16) -0.0048(18) 0.0025(19)
O11 0.0268(18) 0.034(2) 0.0115(16) -0.0014(15) -0.0002(19) 0.000(2)
O12 0.0267(19) 0.0260(19) 0.0134(19) 0.0016(15) 0.0027(16) 0.0064(17)
O13 0.033(2) 0.026(2) 0.0135(17) 0.0010(15) -0.0043(17) 0.0014(18)
O14 0.033(2) 0.027(2) 0.0143(18) 0.0005(15) 0.0006(17) 0.0015(18)
O15 0.032(2) 0.026(2) 0.0146(18) -0.0027(16) -0.0005(18) 0.0005(19)
O16 0.0250(18) 0.0275(18) 0.0138(17) 0.0003(17) -0.0029(14) 0.0075(18)
N1 0.042(3) 0.039(3) 0.059(4) -0.008(3) 0.000(3) -0.012(3)
N2 0.040(3) 0.057(4) 0.015(3) 0.005(2) -0.003(2) 0.017(3)
C1 0.040(4) 0.049(4) 0.063(5) -0.004(4) 0.001(4) -0.016(4)
C2 0.045(4) 0.066(5) 0.086(6) -0.023(5) 0.011(5) -0.001(4)
C3 0.081(6) 0.058(5) 0.091(7) -0.021(5) 0.023(6) -0.001(5)
C4 0.103(9) 0.112(9) 0.110(9) -0.018(8) 0.044(8) 0.006(8)
C5 0.028(3) 0.053(4) 0.062(5) -0.014(4) -0.002(3) -0.012(3)
C6 0.028(3) 0.058(5) 0.066(5) -0.010(4) 0.004(4) -0.014(4)
C7 0.054(5) 0.046(5) 0.102(7) -0.003(5) 0.006(5) 0.000(4)
C8 0.045(5) 0.104(8) 0.117(9) 0.011(7) 0.003(6) -0.001(5)
C9 0.045(4) 0.046(4) 0.063(5) -0.013(4) 0.004(4) -0.013(4)
C13 0.047(4) 0.042(4) 0.085(7) -0.006(4) -0.008(4) -0.020(4)
C14 0.063(5) 0.051(5) 0.070(6) -0.005(4) 0.009(5) -0.023(4)
C15 0.064(5) 0.057(5) 0.096(7) 0.010(5) 0.002(5) -0.023(5)
C16 0.072(6) 0.072(7) 0.184(13) 0.013(8) 0.037(8) -0.008(6)
C17 0.057(5) 0.075(5) 0.024(4) 0.003(3) 0.005(3) 0.025(4)
C18 0.055(5) 0.152(9) 0.048(5) 0.018(6) 0.011(4) 0.048(6)
_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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 O8 2.363(4) 2_665 ?
Gd1 O8 2.363(4) . ?
Gd1 O17 2.381(5) 2_665 ?
Gd1 O17 2.381(5) . ?
Gd1 O7 2.384(4) 2_665 ?
Gd1 O7 2.384(4) . ?
Gd1 N2 2.561(5) . ?
Gd1 N2 2.561(5) 2_665 ?
Gd1 O17' 2.632(11) . ?
Gd1 V1 3.3982(11) 2_665 ?
Gd1 V1 3.3982(11) . ?
V1 O1 1.591(4) . ?
V1 O10 1.868(4) . ?
V1 O11 1.869(4) . ?
V1 O8 1.882(4) . ?
V1 O7 1.886(4) . ?
V1 V2 2.8819(13) . ?
V1 V6 2.8844(14) . ?
V2 O2 1.591(4) . ?
V2 O9 1.812(4) . ?
V2 O8 1.855(4) . ?
V2 O16 1.900(3) . ?
V2 O10 1.971(4) . ?
V2 V3 3.0293(14) . ?
V3 O3 1.597(4) . ?
V3 O14 1.796(4) . ?
V3 O13 1.830(4) . ?
V3 O10 1.939(4) . ?
V3 O16 1.990(4) . ?
V3 V5 2.8848(14) . ?
V4 O4 1.600(4) . ?
V4 O14 1.798(4) 2_665 ?
V4 O15 1.814(4) . ?
V4 O11 1.940(3) 2_665 ?
V4 O12 1.967(4) . ?
V4 V5 2.8809(13) . ?
V4 V6 3.0224(14) 2_665 ?
V5 O5 1.586(4) . ?
V5 O13 1.821(4) . ?
V5 O15 1.831(4) . ?
V5 O16 1.913(4) . ?
V5 O12 1.935(4) . ?
V6 O6 1.592(4) . ?
V6 O9 1.772(4) 2_665 ?
V6 O7 1.849(4) . ?
V6 O12 1.889(3) 2_665 ?
V6 O11 1.978(4) . ?
V6 V4 3.0224(14) 2_665 ?
O9 V6 1.772(4) 2_665 ?
O11 V4 1.940(3) 2_665 ?
O12 V6 1.889(3) 2_665 ?
O14 V4 1.798(4) 2_665 ?
O17 O17' 1.707(7) . ?
O17' O17 1.707(7) 2_665 ?
N1 C5 1.490(8) . ?
N1 C9 1.524(9) . ?
N1 C1 1.537(9) . ?
N1 C13 1.548(9) . ?
N2 C17 1.137(8) . ?
N3 C19 1.13(2) . ?
N4 N4' 0.68(4) . ?
N4 C21' 1.01(4) . ?
N4 C21 1.163(19) . ?
C1 C2 1.494(11) . ?
C2 C3 1.526(11) . ?
C3 C4 1.591(12) . ?
C5 C6 1.517(10) . ?
C6 C7 1.535(10) . ?
C7 C8 1.390(12) . ?
C9 C10 1.501(15) . ?
C10 C11 1.509(16) . ?
C11 C12 1.423(19) . ?
C10' C11' 1.544(18) . ?
C11' C12' 1.483(19) . ?
C13 C14 1.514(11) . ?
C14 C15 1.473(10) . ?
C15 C16 1.431(13) . ?
C17 C18 1.478(10) . ?
C19 C20 1.522(11) . ?
C21 C21' 0.56(6) . ?
C21 N4' 0.92(5) . ?
C21 C22 1.556(19) . ?
C22 C21' 1.45(5) . ?
C21' N4' 1.00(5) . ?
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
O8 Gd1 O8 121.51(18) 2_665 . ?
O8 Gd1 O17 144.64(14) 2_665 2_665 ?
O8 Gd1 O17 86.53(14) . 2_665 ?
O8 Gd1 O17 86.53(14) 2_665 . ?
O8 Gd1 O17 144.64(14) . . ?
O17 Gd1 O17 78.8(2) 2_665 . ?
O8 Gd1 O7 64.63(13) 2_665 2_665 ?
O8 Gd1 O7 87.54(13) . 2_665 ?
O17 Gd1 O7 144.39(14) 2_665 2_665 ?
O17 Gd1 O7 86.12(14) . 2_665 ?
O8 Gd1 O7 87.54(13) 2_665 . ?
O8 Gd1 O7 64.63(13) . . ?
O17 Gd1 O7 86.12(14) 2_665 . ?
O17 Gd1 O7 144.39(14) . . ?
O7 Gd1 O7 122.32(17) 2_665 . ?
O8 Gd1 N2 132.58(16) 2_665 . ?
O8 Gd1 N2 71.73(15) . . ?
O17 Gd1 N2 73.36(16) 2_665 . ?
O17 Gd1 N2 73.27(16) . . ?
O7 Gd1 N2 71.44(15) 2_665 . ?
O7 Gd1 N2 132.59(16) . . ?
O8 Gd1 N2 71.73(15) 2_665 2_665 ?
O8 Gd1 N2 132.58(16) . 2_665 ?
O17 Gd1 N2 73.27(16) 2_665 2_665 ?
O17 Gd1 N2 73.36(16) . 2_665 ?
O7 Gd1 N2 132.59(16) 2_665 2_665 ?
O7 Gd1 N2 71.44(15) . 2_665 ?
N2 Gd1 N2 136.4(2) . 2_665 ?
O8 Gd1 O17' 119.25(9) 2_665 . ?
O8 Gd1 O17' 119.25(9) . . ?
O17 Gd1 O17' 39.41(11) 2_665 . ?
O17 Gd1 O17' 39.41(11) . . ?
O7 Gd1 O17' 118.84(9) 2_665 . ?
O7 Gd1 O17' 118.84(9) . . ?
N2 Gd1 O17' 68.18(11) . . ?
N2 Gd1 O17' 68.18(11) 2_665 . ?
O8 Gd1 V1 32.21(9) 2_665 2_665 ?
O8 Gd1 V1 106.11(10) . 2_665 ?
O17 Gd1 V1 165.00(11) 2_665 2_665 ?
O17 Gd1 V1 86.18(11) . 2_665 ?
O7 Gd1 V1 32.43(9) 2_665 2_665 ?
O7 Gd1 V1 106.41(9) . 2_665 ?
N2 Gd1 V1 102.51(13) . 2_665 ?
N2 Gd1 V1 102.47(12) 2_665 2_665 ?
O17' Gd1 V1 125.589(17) . 2_665 ?
O8 Gd1 V1 106.11(10) 2_665 . ?
O8 Gd1 V1 32.21(9) . . ?
O17 Gd1 V1 86.18(11) 2_665 . ?
O17 Gd1 V1 165.00(11) . . ?
O7 Gd1 V1 106.41(9) 2_665 . ?
O7 Gd1 V1 32.43(9) . . ?
N2 Gd1 V1 102.47(12) . . ?
N2 Gd1 V1 102.51(13) 2_665 . ?
O17' Gd1 V1 125.589(17) . . ?
V1 Gd1 V1 108.82(3) 2_665 . ?
O1 V1 O10 106.01(19) . . ?
O1 V1 O11 105.21(19) . . ?
O10 V1 O11 93.61(16) . . ?
O1 V1 O8 107.8(2) . . ?
O10 V1 O8 81.84(17) . . ?
O11 V1 O8 146.64(17) . . ?
O1 V1 O7 106.2(2) . . ?
O10 V1 O7 147.50(18) . . ?
O11 V1 O7 81.75(16) . . ?
O8 V1 O7 84.68(17) . . ?
O1 V1 V2 114.80(16) . . ?
O10 V1 V2 42.72(12) . . ?
O11 V1 V2 126.26(12) . . ?
O8 V1 V2 39.21(11) . . ?
O7 V1 V2 117.13(13) . . ?
O1 V1 V6 113.45(16) . . ?
O10 V1 V6 126.60(12) . . ?
O11 V1 V6 42.89(12) . . ?
O8 V1 V6 116.40(13) . . ?
O7 V1 V6 38.98(11) . . ?
V2 V1 V6 131.13(4) . . ?
O1 V1 Gd1 114.11(16) . . ?
O10 V1 Gd1 117.62(12) . . ?
O11 V1 Gd1 117.75(13) . . ?
O8 V1 Gd1 42.00(12) . . ?
O7 V1 Gd1 42.69(12) . . ?
V2 V1 Gd1 76.95(3) . . ?
V6 V1 Gd1 77.03(3) . . ?
O2 V2 O9 104.04(19) . . ?
O2 V2 O8 107.96(19) . . ?
O9 V2 O8 94.15(17) . . ?
O2 V2 O16 108.34(19) . . ?
O9 V2 O16 90.26(17) . . ?
O8 V2 O16 141.10(16) . . ?
O2 V2 O10 103.27(19) . . ?
O9 V2 O10 152.57(16) . . ?
O8 V2 O10 79.81(16) . . ?
O16 V2 O10 78.76(15) . . ?
O2 V2 V1 112.59(15) . . ?
O9 V2 V1 127.47(12) . . ?
O8 V2 V1 39.89(12) . . ?
O16 V2 V1 111.21(11) . . ?
O10 V2 V1 40.01(11) . . ?
O2 V2 V3 110.58(15) . . ?
O9 V2 V3 125.72(12) . . ?
O8 V2 V3 112.43(12) . . ?
O16 V2 V3 39.94(11) . . ?
O10 V2 V3 38.82(11) . . ?
V1 V2 V3 74.33(3) . . ?
O3 V3 O14 104.56(19) . . ?
O3 V3 O13 105.57(19) . . ?
O14 V3 O13 98.03(17) . . ?
O3 V3 O10 103.61(19) . . ?
O14 V3 O10 90.82(16) . . ?
O13 V3 O10 146.17(17) . . ?
O3 V3 O16 106.06(18) . . ?
O14 V3 O16 148.98(16) . . ?
O13 V3 O16 78.39(15) . . ?
O10 V3 O16 77.39(15) . . ?
O3 V3 V5 116.02(15) . . ?
O14 V3 V5 124.95(13) . . ?
O13 V3 V5 37.69(11) . . ?
O10 V3 V5 112.48(12) . . ?
O16 V3 V5 41.34(10) . . ?
O3 V3 V2 109.18(15) . . ?
O14 V3 V2 124.65(12) . . ?
O13 V3 V2 112.97(12) . . ?
O10 V3 V2 39.60(12) . . ?
O16 V3 V2 37.80(9) . . ?
V5 V3 V2 75.50(3) . . ?
O4 V4 O14 105.27(19) . 2_665 ?
O4 V4 O15 105.92(19) . . ?
O14 V4 O15 97.45(17) 2_665 . ?
O4 V4 O11 104.16(18) . 2_665 ?
O14 V4 O11 89.65(17) 2_665 2_665 ?
O15 V4 O11 145.95(17) . 2_665 ?
O4 V4 O12 105.55(18) . . ?
O14 V4 O12 148.67(17) 2_665 . ?
O15 V4 O12 79.41(16) . . ?
O11 V4 O12 77.48(15) 2_665 . ?
O4 V4 V5 115.77(15) . . ?
O14 V4 V5 124.76(13) 2_665 . ?
O15 V4 V5 37.99(12) . . ?
O11 V4 V5 112.79(12) 2_665 . ?
O12 V4 V5 41.98(10) . . ?
O4 V4 V6 108.95(15) . 2_665 ?
O14 V4 V6 124.10(12) 2_665 2_665 ?
O15 V4 V6 113.43(12) . 2_665 ?
O11 V4 V6 39.99(12) 2_665 2_665 ?
O12 V4 V6 37.49(10) . 2_665 ?
V5 V4 V6 75.74(3) . 2_665 ?
O5 V5 O13 105.91(19) . . ?
O5 V5 O15 105.60(19) . . ?
O13 V5 O15 95.36(17) . . ?
O5 V5 O16 104.93(18) . . ?
O13 V5 O16 80.64(16) . . ?
O15 V5 O16 149.12(16) . . ?
O5 V5 O12 104.33(18) . . ?
O13 V5 O12 149.54(17) . . ?
O15 V5 O12 79.87(16) . . ?
O16 V5 O12 88.24(15) . . ?
O5 V5 V4 114.86(15) . . ?
O13 V5 V4 123.15(13) . . ?
O15 V5 V4 37.58(12) . . ?
O16 V5 V4 121.71(11) . . ?
O12 V5 V4 42.85(11) . . ?
O5 V5 V3 116.08(15) . . ?
O13 V5 V3 37.91(11) . . ?
O15 V5 V3 122.79(13) . . ?
O16 V5 V3 43.39(11) . . ?
O12 V5 V3 121.88(11) . . ?
V4 V5 V3 129.04(4) . . ?
O6 V6 O9 104.41(19) . 2_665 ?
O6 V6 O7 107.62(19) . . ?
O9 V6 O7 94.40(18) 2_665 . ?
O6 V6 O12 107.57(19) . 2_665 ?
O9 V6 O12 90.95(17) 2_665 2_665 ?
O7 V6 O12 141.76(16) . 2_665 ?
O6 V6 O11 102.68(19) . . ?
O9 V6 O11 152.78(17) 2_665 . ?
O7 V6 O11 79.79(16) . . ?
O12 V6 O11 78.39(15) 2_665 . ?
O6 V6 V1 112.25(16) . . ?
O9 V6 V1 127.59(12) 2_665 . ?
O7 V6 V1 39.90(12) . . ?
O12 V6 V1 111.10(12) 2_665 . ?
O11 V6 V1 40.00(11) . . ?
O6 V6 V4 109.39(16) . 2_665 ?
O9 V6 V4 126.01(13) 2_665 2_665 ?
O7 V6 V4 113.15(12) . 2_665 ?
O12 V6 V4 39.32(11) 2_665 2_665 ?
O11 V6 V4 39.07(10) . 2_665 ?
V1 V6 V4 74.80(3) . 2_665 ?
V6 O7 V1 101.12(17) . . ?
V6 O7 Gd1 136.2(2) . . ?
V1 O7 Gd1 104.87(16) . . ?
V2 O8 V1 100.90(18) . . ?
V2 O8 Gd1 136.9(2) . . ?
V1 O8 Gd1 105.79(17) . . ?
V6 O9 V2 134.6(2) 2_665 . ?
V1 O10 V3 139.6(2) . . ?
V1 O10 V2 97.27(17) . . ?
V3 O10 V2 101.58(17) . . ?
V1 O11 V4 140.9(2) . 2_665 ?
V1 O11 V6 97.10(16) . . ?
V4 O11 V6 100.94(18) 2_665 . ?
V6 O12 V5 142.9(2) 2_665 . ?
V6 O12 V4 103.19(17) 2_665 . ?
V5 O12 V4 95.18(15) . . ?
V5 O13 V3 104.40(18) . . ?
V3 O14 V4 140.3(2) . 2_665 ?
V4 O15 V5 104.43(18) . . ?
V2 O16 V5 143.6(2) . . ?
V2 O16 V3 102.26(17) . . ?
V5 O16 V3 95.27(14) . . ?
O17' O17 Gd1 78.3(4) . . ?
O17 O17' O17 124.7(7) 2_665 . ?
O17 O17' Gd1 62.3(4) 2_665 . ?
O17 O17' Gd1 62.3(4) . . ?
C5 N1 C9 111.2(6) . . ?
C5 N1 C1 110.6(6) . . ?
C9 N1 C1 106.3(5) . . ?
C5 N1 C13 106.1(5) . . ?
C9 N1 C13 110.4(6) . . ?
C1 N1 C13 112.3(6) . . ?
C17 N2 Gd1 154.1(5) . . ?
N4' N4 C21' 70(4) . . ?
N4' N4 C21 52(4) . . ?
C21' N4 C21 29(3) . . ?
C2 C1 N1 116.3(6) . . ?
C1 C2 C3 110.2(7) . . ?
C2 C3 C4 110.5(8) . . ?
N1 C5 C6 116.0(6) . . ?
C5 C6 C7 111.8(6) . . ?
C8 C7 C6 113.0(7) . . ?
C10 C9 N1 115.3(7) . . ?
C9 C10 C11 110.2(10) . . ?
C12 C11 C10 109.3(13) . . ?
C12' C11' C10' 110(2) . . ?
C14 C13 N1 117.6(6) . . ?
C15 C14 C13 109.5(7) . . ?
C16 C15 C14 115.4(8) . . ?
N2 C17 C18 179.2(9) . . ?
N3 C19 C20 166.8(17) . . ?
C21' C21 N4' 82(6) . . ?
C21' C21 N4 60(5) . . ?
N4' C21 N4 36(3) . . ?
C21' C21 C22 69(6) . . ?
N4' C21 C22 141(5) . . ?
N4 C21 C22 129(3) . . ?
C21' C22 C21 21(2) . . ?
C21 C21' N4' 65(6) . . ?
C21 C21' N4 91(6) . . ?
N4' C21' N4 40(3) . . ?
C21 C21' C22 90(6) . . ?
N4' C21' C22 144(5) . . ?
N4 C21' C22 176(5) . . ?
N4 N4' C21 92(5) . . ?
N4 N4' C21' 70(5) . . ?
C21 N4' C21' 34(4) . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 -0.081 130 12 ' '
2 0.500 1.000 0.080 130 12 ' '
_platon_squeeze_details          
;
Summary and Remarks : N = NOTE, W = WARNING, E = ERROR
#===============================================================================
N: No S.U.'s (esd) on observed/calculated parameters.
N: DISORDERED structure - ATOMS with Pop. .LT. 1.0 are not moved or as a group.
W: Unit cell contains non-integral number of atoms (please check).
#-------------------------------------------------------------------------------
N: Number of Isotropic Non-H Atoms ....................................... 6
N: Number of moved primary input atoms: .................................. 9
N: Total Potential Solvent Accessible Void Vol .................. 262.7 Ang^3
N: Electron Count / Cell = 24 - To be included in D(calc), F000 & Mol.Wght.
#===============================================================================
;
_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.49
_refine_diff_density_rms         0.10