#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:55:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179943 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/38/7023856.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7023856
loop_
_publ_author_name
'Liu, Baolin'
'Liu, Qingxia'
'Xiao, Hongping'
'Zhang, Wu'
'Tao, Ruojie'
_publ_section_title
;
 Family of dumbbell Ni4Ln2 (Ln = Pr, Sm, Eu, Gd, Tb, Ho, Er) complexes:
 syntheses, structures, luminescent and magnetic properties.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5047
_journal_page_last               5055
_journal_paper_doi               10.1039/c3dt32935f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C60 H58 Gd2 N8 Ni4 O24, 8(H2 O)'
_chemical_formula_sum            'C60 H74 Gd2 N8 Ni4 O32'
_chemical_formula_weight         1968.61
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.7790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6620(10)
_cell_length_b                   18.1513(14)
_cell_length_c                   15.5428(12)
_cell_measurement_reflns_used    4906
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.23
_cell_volume                     3520.3(5)
_computing_cell_refinement       'APEX 2'
_computing_data_collection       'APEX 2(Bruker, 2005)'
_computing_data_reduction        'SAINT(Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL(Bruker, 2005)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17591
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    3.000
_exptl_absorpt_correction_T_max  0.6964
_exptl_absorpt_correction_T_min  0.5092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1972
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6191
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0320P)²+2.2778P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                4815
_reflns_number_total             6191
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt32935f.txt
_cod_data_source_block           1296
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               7023856
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Gd1 Gd 0.084030(13) 1.056658(9) 0.596635(11) 0.02290(5) Uani 1 1 d .
Ni1 Ni 0.16239(4) 0.89530(2) 0.71051(3) 0.02777(12) Uani 1 1 d .
Ni2 Ni 0.31503(4) 1.05075(2) 0.70923(3) 0.02627(11) Uani 1 1 d .
N1 N 0.3061(2) 0.83655(16) 0.7678(2) 0.0341(8) Uani 1 1 d .
N2 N 0.1030(3) 0.84825(16) 0.8053(2) 0.0361(8) Uani 1 1 d .
N3 N 0.3403(2) 0.99142(16) 0.82118(19) 0.0330(8) Uani 1 1 d .
N4 N 0.1473(3) 0.81625(17) 0.6172(2) 0.0446(10) Uani 1 1 d .
H4A H 0.1022 0.7807 0.6288 0.054 Uiso 1 1 calc R
H4B H 0.1215 0.8357 0.5645 0.054 Uiso 1 1 calc R
O1 O -0.2537(2) 1.05375(14) 0.54187(17) 0.0400(7) Uani 1 1 d .
O2 O -0.09007(18) 1.01693(12) 0.53170(15) 0.0272(6) Uani 1 1 d .
O3 O 0.02613(18) 0.95593(12) 0.67797(15) 0.0274(6) Uani 1 1 d .
O4 O -0.1105(3) 1.1843(2) 0.7581(2) 0.0895(12) Uani 1 1 d U
O5 O -0.0233(2) 1.13171(14) 0.66512(17) 0.0389(7) Uani 1 1 d .
O6 O 0.17261(19) 1.08119(13) 0.73789(15) 0.0300(6) Uani 1 1 d .
O7 O 0.0998(2) 1.24544(16) 0.41080(19) 0.0546(8) Uani 1 1 d .
O8 O 0.07514(19) 1.15476(13) 0.49851(16) 0.0356(7) Uani 1 1 d .
O9 O 0.25805(18) 1.10830(13) 0.59925(15) 0.0287(6) Uani 1 1 d .
O10 O 0.4508(2) 1.02890(14) 0.65800(16) 0.0362(7) Uani 1 1 d .
O11 O 0.22602(18) 0.96910(12) 0.64079(14) 0.0257(6) Uani 1 1 d D
H11 H 0.2574 0.9484 0.5926 0.031 Uiso 1 1 calc RD
C1 C 0.2899(3) 0.8137(2) 0.8563(3) 0.0418(11) Uani 1 1 d .
H1A H 0.3098 0.8537 0.8971 0.050 Uiso 1 1 calc R
H1B H 0.3355 0.7718 0.8754 0.050 Uiso 1 1 calc R
C2 C 0.1746(3) 0.7931(2) 0.8557(3) 0.0460(12) Uani 1 1 d .
H2A H 0.1604 0.7448 0.8296 0.055 Uiso 1 1 calc R
H2B H 0.1607 0.7910 0.9152 0.055 Uiso 1 1 calc R
C3 C 0.0069(3) 0.8544(2) 0.8199(3) 0.0412(11) Uani 1 1 d .
H3 H -0.0099 0.8269 0.8662 0.049 Uiso 1 1 calc R
C4 C -0.0782(3) 0.8986(2) 0.7735(2) 0.0349(10) Uani 1 1 d .
C5 C -0.1752(4) 0.8925(3) 0.8019(3) 0.0573(13) Uani 1 1 d .
H5 H -0.1802 0.8618 0.8490 0.069 Uiso 1 1 calc R
C6 C -0.2639(4) 0.9299(3) 0.7635(3) 0.0634(15) Uani 1 1 d .
H6 H -0.3281 0.9259 0.7847 0.076 Uiso 1 1 calc R
C7 C -0.2563(3) 0.9737(3) 0.6924(3) 0.0478(12) Uani 1 1 d .
H7 H -0.3168 0.9994 0.6662 0.057 Uiso 1 1 calc R
C8 C -0.1630(3) 0.9812(2) 0.6583(2) 0.0285(9) Uani 1 1 d .
C9 C -0.1706(3) 1.0212(2) 0.5735(2) 0.0287(9) Uani 1 1 d .
C10 C -0.0677(3) 0.94574(19) 0.7020(2) 0.0275(8) Uani 1 1 d .
C11 C 0.4098(3) 0.8754(2) 0.7708(3) 0.0357(10) Uani 1 1 d .
H11A H 0.4135 0.8936 0.7127 0.043 Uiso 1 1 calc R
H11B H 0.4672 0.8400 0.7860 0.043 Uiso 1 1 calc R
C12 C 0.4297(3) 0.9390(2) 0.8337(3) 0.0409(11) Uani 1 1 d .
H12A H 0.4402 0.9204 0.8930 0.049 Uiso 1 1 calc R
H12B H 0.4948 0.9643 0.8255 0.049 Uiso 1 1 calc R
C13 C 0.2918(3) 1.0036(2) 0.8856(3) 0.0410(11) Uani 1 1 d .
H13 H 0.3224 0.9824 0.9384 0.049 Uiso 1 1 calc R
C14 C 0.1967(4) 1.0457(2) 0.8866(3) 0.0440(11) Uani 1 1 d .
C15 C 0.1558(5) 1.0466(3) 0.9646(3) 0.0701(16) Uani 1 1 d .
H15 H 0.1952 1.0245 1.0138 0.084 Uiso 1 1 calc R
C16 C 0.0604(5) 1.0789(3) 0.9713(3) 0.0836(18) Uani 1 1 d .
H16 H 0.0363 1.0798 1.0246 0.100 Uiso 1 1 calc R
C17 C -0.0001(4) 1.1099(3) 0.8983(3) 0.0620(14) Uani 1 1 d .
H17 H -0.0661 1.1307 0.9027 0.074 Uiso 1 1 calc R
C18 C 0.0350(3) 1.1111(2) 0.8184(3) 0.0393(10) Uani 1 1 d .
C19 C -0.0374(3) 1.1443(2) 0.7426(3) 0.0453(12) Uani 1 1 d .
C20 C 0.1355(3) 1.07952(19) 0.8122(2) 0.0323(10) Uani 1 1 d .
C21 C 0.3053(3) 0.7703(2) 0.7112(3) 0.0420(11) Uani 1 1 d .
H21A H 0.2658 0.7311 0.7340 0.050 Uiso 1 1 calc R
H21B H 0.3783 0.7535 0.7127 0.050 Uiso 1 1 calc R
C22 C 0.2550(3) 0.7860(2) 0.6182(3) 0.0472(12) Uani 1 1 d .
H22A H 0.2985 0.8211 0.5927 0.057 Uiso 1 1 calc R
H22B H 0.2505 0.7410 0.5842 0.057 Uiso 1 1 calc R
C23 C 0.4754(3) 1.0608(2) 0.5939(3) 0.0404(10) Uani 1 1 d .
H23 H 0.5438 1.0505 0.5829 0.048 Uiso 1 1 calc R
C24 C 0.4151(3) 1.1112(2) 0.5343(2) 0.0319(9) Uani 1 1 d .
C25 C 0.4668(3) 1.1396(2) 0.4696(3) 0.0454(11) Uani 1 1 d .
H25 H 0.5377 1.1268 0.4690 0.055 Uiso 1 1 calc R
C26 C 0.4157(4) 1.1859(3) 0.4070(3) 0.0548(13) Uani 1 1 d .
H26 H 0.4524 1.2066 0.3660 0.066 Uiso 1 1 calc R
C27 C 0.3088(3) 1.2016(2) 0.4052(3) 0.0418(11) Uani 1 1 d .
H27 H 0.2740 1.2322 0.3614 0.050 Uiso 1 1 calc R
C28 C 0.2511(3) 1.17355(19) 0.4663(2) 0.0296(9) Uani 1 1 d .
C29 C 0.1350(3) 1.19239(19) 0.4581(2) 0.0309(9) Uani 1 1 d .
C30 C 0.3059(3) 1.12961(18) 0.5353(2) 0.0250(8) Uani 1 1 d .
O1W O 0.3960(2) 1.13764(13) 0.77683(17) 0.0403(7) Uani 1 1 d .
H1WA H 0.3824 1.1640 0.8188 0.048 Uiso 1 1 d R
H1WB H 0.3852 1.1639 0.7309 0.048 Uiso 1 1 d R
O2W O 0.7173(3) 0.19172(19) 0.6333(2) 0.0759(11) Uani 1 1 d .
H2WA H 0.7142 0.1559 0.5977 0.091 Uiso 1 1 d R
H2WB H 0.7631 0.1808 0.6780 0.091 Uiso 1 1 d R
O3W O 0.9672(3) 0.3555(2) 0.4544(2) 0.0908(13) Uani 1 1 d .
H3WA H 0.9276 0.3819 0.4169 0.109 Uiso 1 1 d R
H3WB H 1.0130 0.3837 0.4843 0.109 Uiso 1 1 d R
O4W O 0.8949(4) 0.2733(2) 0.5763(3) 0.1091(16) Uani 1 1 d .
H4WA H 0.9057 0.3043 0.6178 0.131 Uiso 1 1 d R
H4WB H 0.9301 0.2345 0.5933 0.131 Uiso 1 1 d R
O5W O 0.5744(3) 0.1933(2) 0.7441(3) 0.0751(13) Uani 0.75 1 d P
H5WA H 0.6073 0.1986 0.7962 0.090 Uiso 0.75 1 d PR
H5WB H 0.5707 0.2354 0.7198 0.090 Uiso 0.75 1 d PR
O6W O 0.2096(12) 0.3955(8) 0.4159(8) 0.083(5) Uani 0.25 1 d P
H6WA H 0.2280 0.4376 0.3997 0.099 Uiso 0.25 1 d PR
H6WB H 0.1910 0.3695 0.3703 0.099 Uiso 0.25 1 d PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O5 Gd1 O6 71.33(9) . .
O5 Gd1 O8 83.36(9) . .
O6 Gd1 O8 115.56(8) . .
O5 Gd1 O2 78.37(8) . .
O6 Gd1 O2 136.15(8) . .
O8 Gd1 O2 90.90(8) . .
O5 Gd1 O9 111.98(9) . .
O6 Gd1 O9 67.31(8) . .
O8 Gd1 O9 69.75(8) . .
O2 Gd1 O9 155.96(8) . .
O5 Gd1 O3 87.15(9) . .
O6 Gd1 O3 77.95(8) . .
O8 Gd1 O3 159.59(8) . .
O2 Gd1 O3 69.45(8) . .
O9 Gd1 O3 130.66(7) . .
O5 Gd1 O11 136.64(8) . .
O6 Gd1 O11 69.00(8) . .
O8 Gd1 O11 129.77(8) . .
O2 Gd1 O11 120.95(8) . .
O9 Gd1 O11 67.20(8) . .
O3 Gd1 O11 68.20(8) . .
O5 Gd1 O2 144.28(8) . 3_576
O6 Gd1 O2 143.73(8) . 3_576
O8 Gd1 O2 83.51(8) . 3_576
O2 Gd1 O2 68.78(9) . 3_576
O9 Gd1 O2 94.16(8) . 3_576
O3 Gd1 O2 93.96(8) . 3_576
O11 Gd1 O2 75.14(7) . 3_576
O5 Gd1 Gd1 112.00(6) . 3_576
O6 Gd1 Gd1 157.80(6) . 3_576
O8 Gd1 Gd1 86.58(6) . 3_576
O2 Gd1 Gd1 34.70(5) . 3_576
O9 Gd1 Gd1 126.40(6) . 3_576
O3 Gd1 Gd1 80.28(5) . 3_576
O11 Gd1 Gd1 98.78(5) . 3_576
O2 Gd1 Gd1 34.09(5) 3_576 3_576
N2 Ni1 O11 161.91(11) . .
N2 Ni1 N4 103.18(14) . .
O11 Ni1 N4 94.88(12) . .
N2 Ni1 O3 90.30(11) . .
O11 Ni1 O3 84.53(9) . .
N4 Ni1 O3 103.40(11) . .
N2 Ni1 N1 83.06(12) . .
O11 Ni1 N1 99.60(11) . .
N4 Ni1 N1 85.20(12) . .
O3 Ni1 N1 170.19(11) . .
O6 Ni2 N3 88.42(11) . .
O6 Ni2 O9 80.85(9) . .
N3 Ni2 O9 168.42(11) . .
O6 Ni2 O11 83.03(9) . .
N3 Ni2 O11 93.10(10) . .
O9 Ni2 O11 81.33(9) . .
O6 Ni2 O10 169.34(10) . .
N3 Ni2 O10 102.13(12) . .
O9 Ni2 O10 88.51(10) . .
O11 Ni2 O10 94.71(10) . .
O6 Ni2 O1W 93.66(10) . .
N3 Ni2 O1W 88.66(11) . .
O9 Ni2 O1W 96.32(10) . .
O11 Ni2 O1W 176.20(10) . .
O10 Ni2 O1W 88.20(11) . .
C1 N1 C11 111.4(3) . .
C1 N1 C21 109.5(3) . .
C11 N1 C21 108.7(3) . .
C1 N1 Ni1 106.3(2) . .
C11 N1 Ni1 117.1(2) . .
C21 N1 Ni1 103.5(2) . .
C3 N2 C2 118.7(3) . .
C3 N2 Ni1 126.3(3) . .
C2 N2 Ni1 114.4(3) . .
C13 N3 C12 118.1(3) . .
C13 N3 Ni2 123.6(3) . .
C12 N3 Ni2 117.7(2) . .
C22 N4 Ni1 106.4(2) . .
C22 N4 H4A 110.4 . .
Ni1 N4 H4A 110.4 . .
C22 N4 H4B 110.4 . .
Ni1 N4 H4B 110.4 . .
H4A N4 H4B 108.6 . .
C9 O2 Gd1 121.3(2) . .
C9 O2 Gd1 125.7(2) . 3_576
Gd1 O2 Gd1 111.22(9) . 3_576
C10 O3 Ni1 128.4(2) . .
C10 O3 Gd1 128.7(2) . .
Ni1 O3 Gd1 102.72(10) . .
C19 O5 Gd1 137.2(3) . .
C20 O6 Ni2 130.9(2) . .
C20 O6 Gd1 129.3(2) . .
Ni2 O6 Gd1 92.58(9) . .
C29 O8 Gd1 140.4(2) . .
C30 O9 Ni2 130.4(2) . .
C30 O9 Gd1 130.4(2) . .
Ni2 O9 Gd1 90.42(9) . .
C23 O10 Ni2 124.3(2) . .
Ni1 O11 Ni2 116.43(11) . .
Ni1 O11 Gd1 104.41(10) . .
Ni2 O11 Gd1 89.36(8) . .
Ni1 O11 H11 114.5 . .
Ni2 O11 H11 114.5 . .
Gd1 O11 H11 114.5 . .
N1 C1 C2 110.5(3) . .
N1 C1 H1A 109.5 . .
C2 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 108.1 . .
N2 C2 C1 110.0(3) . .
N2 C2 H2A 109.7 . .
C1 C2 H2A 109.7 . .
N2 C2 H2B 109.7 . .
C1 C2 H2B 109.7 . .
H2A C2 H2B 108.2 . .
N2 C3 C4 128.0(4) . .
N2 C3 H3 116.0 . .
C4 C3 H3 116.0 . .
C5 C4 C10 120.2(4) . .
C5 C4 C3 115.4(4) . .
C10 C4 C3 124.4(4) . .
C6 C5 C4 122.3(4) . .
C6 C5 H5 118.9 . .
C4 C5 H5 118.9 . .
C5 C6 C7 118.4(4) . .
C5 C6 H6 120.8 . .
C7 C6 H6 120.8 . .
C6 C7 C8 123.1(4) . .
C6 C7 H7 118.5 . .
C8 C7 H7 118.5 . .
C7 C8 C10 118.7(3) . .
C7 C8 C9 117.1(3) . .
C10 C8 C9 124.0(3) . .
O1 C9 O2 121.1(3) . .
O1 C9 C8 120.5(3) . .
O2 C9 C8 118.2(3) . .
O3 C10 C4 120.8(3) . .
O3 C10 C8 122.0(3) . .
C4 C10 C8 117.2(3) . .
N1 C11 C12 115.8(3) . .
N1 C11 H11A 108.3 . .
C12 C11 H11A 108.3 . .
N1 C11 H11B 108.3 . .
C12 C11 H11B 108.3 . .
H11A C11 H11B 107.4 . .
N3 C12 C11 111.8(3) . .
N3 C12 H12A 109.3 . .
C11 C12 H12A 109.3 . .
N3 C12 H12B 109.3 . .
C11 C12 H12B 109.3 . .
H12A C12 H12B 107.9 . .
N3 C13 C14 128.2(4) . .
N3 C13 H13 115.9 . .
C14 C13 H13 115.9 . .
C15 C14 C20 118.1(4) . .
C15 C14 C13 117.0(4) . .
C20 C14 C13 124.6(4) . .
C16 C15 C14 122.4(5) . .
C16 C15 H15 118.8 . .
C14 C15 H15 118.8 . .
C15 C16 C17 119.3(5) . .
C15 C16 H16 120.3 . .
C17 C16 H16 120.3 . .
C16 C17 C18 121.7(5) . .
C16 C17 H17 119.2 . .
C18 C17 H17 119.2 . .
C17 C18 C20 118.9(4) . .
C17 C18 C19 117.8(4) . .
C20 C18 C19 123.3(4) . .
O4 C19 O5 121.6(4) . .
O4 C19 C18 117.7(4) . .
O5 C19 C18 120.7(4) . .
O6 C20 C18 120.6(3) . .
O6 C20 C14 119.8(4) . .
C18 C20 C14 119.6(4) . .
N1 C21 C22 112.0(3) . .
N1 C21 H21A 109.2 . .
C22 C21 H21A 109.2 . .
N1 C21 H21B 109.2 . .
C22 C21 H21B 109.2 . .
H21A C21 H21B 107.9 . .
N4 C22 C21 108.8(3) . .
N4 C22 H22A 109.9 . .
C21 C22 H22A 109.9 . .
N4 C22 H22B 109.9 . .
C21 C22 H22B 109.9 . .
H22A C22 H22B 108.3 . .
O10 C23 C24 130.0(4) . .
O10 C23 H23 115.0 . .
C24 C23 H23 115.0 . .
C25 C24 C30 119.9(3) . .
C25 C24 C23 116.3(3) . .
C30 C24 C23 123.8(3) . .
C26 C25 C24 121.4(4) . .
C26 C25 H25 119.3 . .
C24 C25 H25 119.3 . .
C25 C26 C27 119.1(4) . .
C25 C26 H26 120.4 . .
C27 C26 H26 120.4 . .
C26 C27 C28 122.6(4) . .
C26 C27 H27 118.7 . .
C28 C27 H27 118.7 . .
C27 C28 C30 118.4(3) . .
C27 C28 C29 118.8(3) . .
C30 C28 C29 122.8(3) . .
O7 C29 O8 121.7(3) . .
O7 C29 C28 118.4(3) . .
O8 C29 C28 119.9(3) . .
O9 C30 C28 120.7(3) . .
O9 C30 C24 121.0(3) . .
C28 C30 C24 118.3(3) . .
Ni2 O1W H1WA 132.2 . .
Ni2 O1W H1WB 90.3 . .
H1WA O1W H1WB 107.7 . .
H2WA O2W H2WB 107.7 . .
H3WA O3W H3WB 107.7 . .
H4WA O4W H4WB 107.7 . .
H5WA O5W H5WB 107.7 . .
H6WA O6W H6WB 107.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O5 2.308(3) .
Gd1 O6 2.332(2) .
Gd1 O8 2.335(2) .
Gd1 O2 2.375(2) .
Gd1 O9 2.389(2) .
Gd1 O3 2.407(2) .
Gd1 O11 2.410(2) .
Gd1 O2 2.413(2) 3_576
Gd1 Gd1 3.9511(4) 3_576
Ni1 N2 1.960(3) .
Ni1 O11 1.979(2) .
Ni1 N4 2.026(3) .
Ni1 O3 2.036(2) .
Ni1 N1 2.166(3) .
Ni2 O6 2.007(2) .
Ni2 N3 2.025(3) .
Ni2 O9 2.028(2) .
Ni2 O11 2.047(2) .
Ni2 O10 2.052(3) .
Ni2 O1W 2.068(2) .
N1 C1 1.484(5) .
N1 C11 1.485(5) .
N1 C21 1.489(5) .
N2 C3 1.280(5) .
N2 C2 1.481(5) .
N3 C13 1.279(5) .
N3 C12 1.466(5) .
N4 C22 1.468(5) .
N4 H4A 0.9000 .
N4 H4B 0.9000 .
O1 C9 1.234(4) .
O2 C9 1.301(4) .
O2 Gd1 2.413(2) 3_576
O3 C10 1.318(4) .
O4 C19 1.232(5) .
O5 C19 1.268(5) .
O6 C20 1.319(4) .
O7 C29 1.247(4) .
O8 C29 1.264(4) .
O9 C30 1.307(4) .
O10 C23 1.237(5) .
O11 H11 0.9800 .
C1 C2 1.505(6) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.435(5) .
C3 H3 0.9300 .
C4 C5 1.378(6) .
C4 C10 1.428(5) .
C5 C6 1.360(6) .
C5 H5 0.9300 .
C6 C7 1.378(6) .
C6 H6 0.9300 .
C7 C8 1.382(5) .
C7 H7 0.9300 .
C8 C10 1.432(5) .
C8 C9 1.494(5) .
C11 C12 1.506(5) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C13 C14 1.428(6) .
C13 H13 0.9300 .
C14 C15 1.397(6) .
C14 C20 1.418(5) .
C15 C16 1.362(8) .
C15 H15 0.9300 .
C16 C17 1.377(7) .
C16 H16 0.9300 .
C17 C18 1.389(6) .
C17 H17 0.9300 .
C18 C20 1.414(6) .
C18 C19 1.492(6) .
C21 C22 1.504(5) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 C24 1.427(5) .
C23 H23 0.9300 .
C24 C25 1.388(5) .
C24 C30 1.426(5) .
C25 C26 1.362(6) .
C25 H25 0.9300 .
C26 C27 1.378(6) .
C26 H26 0.9300 .
C27 C28 1.390(5) .
C27 H27 0.9300 .
C28 C30 1.419(5) .
C28 C29 1.494(5) .
O1W H1WA 0.8500 .
O1W H1WB 0.8500 .
O2W H2WA 0.8500 .
O2W H2WB 0.8501 .
O3W H3WA 0.8499 .
O3W H3WB 0.8500 .
O4W H4WA 0.8500 .
O4W H4WB 0.8499 .
O5W H5WA 0.8500 .
O5W H5WB 0.8500 .
O6W H6WA 0.8500 .
O6W H6WB 0.8500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6W H6WB O5W 0.85 2.52 3.332(13) 160.5 4_565
O5W H5WA O7 0.85 2.07 2.787(5) 142.0 4_676
O4W H4WB O5 0.85 2.20 3.015(5) 159.9 1_645
O3W H3WA O1W 0.85 2.17 2.757(4) 125.6 4_675
O2W H2WB O4 0.85 1.85 2.664(5) 158.9 1_645
O2W H2WA O1 0.85 2.12 2.933(4) 161.1 1_645
O1W H1WB O9 0.85 2.58 3.052(3) 115.9 .
O1W H1WA O3W 0.85 2.23 2.757(4) 120.6 4_576
O11 H11 O1 0.98 2.08 2.948(3) 146.2 3_576
N4 H4B O8 0.90 2.52 3.118(4) 124.2 3_576
N4 H4A O7 0.90 2.57 3.281(4) 136.3 3_576
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N2 Ni1 N1 C1 -16.0(2) . .
O11 Ni1 N1 C1 145.9(2) . .
N4 Ni1 N1 C1 -120.0(2) . .
N2 Ni1 N1 C11 -141.2(3) . .
O11 Ni1 N1 C11 20.7(3) . .
N4 Ni1 N1 C11 114.9(3) . .
N2 Ni1 N1 C21 99.3(2) . .
O11 Ni1 N1 C21 -98.8(2) . .
N4 Ni1 N1 C21 -4.7(2) . .
O11 Ni1 N2 C3 81.4(5) . .
N4 Ni1 N2 C3 -95.6(3) . .
O3 Ni1 N2 C3 8.3(3) . .
N1 Ni1 N2 C3 -179.0(3) . .
O11 Ni1 N2 C2 -107.4(4) . .
N4 Ni1 N2 C2 75.7(3) . .
O3 Ni1 N2 C2 179.5(3) . .
N1 Ni1 N2 C2 -7.7(3) . .
O6 Ni2 N3 C13 -21.5(3) . .
O9 Ni2 N3 C13 -43.6(7) . .
O11 Ni2 N3 C13 -104.4(3) . .
O10 Ni2 N3 C13 160.1(3) . .
O1W Ni2 N3 C13 72.2(3) . .
O6 Ni2 N3 C12 167.7(3) . .
O9 Ni2 N3 C12 145.6(5) . .
O11 Ni2 N3 C12 84.7(2) . .
O10 Ni2 N3 C12 -10.8(3) . .
O1W Ni2 N3 C12 -98.6(3) . .
N2 Ni1 N4 C22 -104.8(3) . .
O11 Ni1 N4 C22 76.2(3) . .
O3 Ni1 N4 C22 161.7(2) . .
N1 Ni1 N4 C22 -23.1(3) . .
O5 Gd1 O2 C9 -28.8(2) . .
O6 Gd1 O2 C9 17.9(3) . .
O8 Gd1 O2 C9 -111.8(3) . .
O9 Gd1 O2 C9 -147.3(2) . .
O3 Gd1 O2 C9 62.5(2) . .
O11 Gd1 O2 C9 109.1(2) . .
O2 Gd1 O2 C9 165.5(3) 3_576 .
Gd1 Gd1 O2 C9 165.5(3) 3_576 .
O5 Gd1 O2 Gd1 165.71(11) . 3_576
O6 Gd1 O2 Gd1 -147.60(9) . 3_576
O8 Gd1 O2 Gd1 82.68(10) . 3_576
O9 Gd1 O2 Gd1 47.2(2) . 3_576
O3 Gd1 O2 Gd1 -102.98(10) . 3_576
O11 Gd1 O2 Gd1 -56.38(12) . 3_576
O2 Gd1 O2 Gd1 0.001(1) 3_576 3_576
N2 Ni1 O3 C10 -15.2(3) . .
O11 Ni1 O3 C10 -177.8(3) . .
N4 Ni1 O3 C10 88.4(3) . .
N2 Ni1 O3 Gd1 159.65(11) . .
O11 Ni1 O3 Gd1 -2.99(9) . .
N4 Ni1 O3 Gd1 -96.72(12) . .
O5 Gd1 O3 C10 34.0(3) . .
O6 Gd1 O3 C10 105.5(3) . .
O8 Gd1 O3 C10 -28.3(4) . .
O2 Gd1 O3 C10 -44.7(2) . .
O9 Gd1 O3 C10 150.8(2) . .
O11 Gd1 O3 C10 177.5(3) . .
O2 Gd1 O3 C10 -110.3(3) 3_576 .
Gd1 Gd1 O3 C10 -78.9(3) 3_576 .
O5 Gd1 O3 Ni1 -140.87(10) . .
O6 Gd1 O3 Ni1 -69.36(10) . .
O8 Gd1 O3 Ni1 156.9(2) . .
O2 Gd1 O3 Ni1 140.48(11) . .
O9 Gd1 O3 Ni1 -24.04(14) . .
O11 Gd1 O3 Ni1 2.63(8) . .
O2 Gd1 O3 Ni1 74.90(9) 3_576 .
Gd1 Gd1 O3 Ni1 106.23(8) 3_576 .
O6 Gd1 O5 C19 -27.5(4) . .
O8 Gd1 O5 C19 -147.4(4) . .
O2 Gd1 O5 C19 120.3(4) . .
O9 Gd1 O5 C19 -82.4(4) . .
O3 Gd1 O5 C19 50.7(4) . .
O11 Gd1 O5 C19 -2.9(4) . .
O2 Gd1 O5 C19 143.5(3) 3_576 .
Gd1 Gd1 O5 C19 129.0(4) 3_576 .
N3 Ni2 O6 C20 17.9(3) . .
O9 Ni2 O6 C20 -166.5(3) . .
O11 Ni2 O6 C20 111.2(3) . .
O10 Ni2 O6 C20 -170.5(5) . .
O1W Ni2 O6 C20 -70.7(3) . .
N3 Ni2 O6 Gd1 -133.63(10) . .
O9 Ni2 O6 Gd1 41.99(9) . .
O11 Ni2 O6 Gd1 -40.31(8) . .
O10 Ni2 O6 Gd1 38.0(6) . .
O1W Ni2 O6 Gd1 137.81(9) . .
O5 Gd1 O6 C20 45.6(3) . .
O8 Gd1 O6 C20 118.3(3) . .
O2 Gd1 O6 C20 -3.2(3) . .
O9 Gd1 O6 C20 170.3(3) . .
O3 Gd1 O6 C20 -45.4(3) . .
O11 Gd1 O6 C20 -116.5(3) . .
O2 Gd1 O6 C20 -125.6(3) 3_576 .
Gd1 Gd1 O6 C20 -57.0(4) 3_576 .
O5 Gd1 O6 Ni2 -162.15(11) . .
O8 Gd1 O6 Ni2 -89.43(10) . .
O2 Gd1 O6 Ni2 149.05(9) . .
O9 Gd1 O6 Ni2 -37.44(8) . .
O3 Gd1 O6 Ni2 106.79(9) . .
O11 Gd1 O6 Ni2 35.74(8) . .
O2 Gd1 O6 Ni2 26.67(18) 3_576 .
Gd1 Gd1 O6 Ni2 95.23(16) 3_576 .
O5 Gd1 O8 C29 135.2(4) . .
O6 Gd1 O8 C29 69.6(4) . .
O2 Gd1 O8 C29 -146.6(4) . .
O9 Gd1 O8 C29 18.8(3) . .
O3 Gd1 O8 C29 -162.0(3) . .
O11 Gd1 O8 C29 -13.6(4) . .
O2 Gd1 O8 C29 -78.1(4) 3_576 .
Gd1 Gd1 O8 C29 -112.2(4) 3_576 .
O6 Ni2 O9 C30 170.1(3) . .
N3 Ni2 O9 C30 -167.5(5) . .
O11 Ni2 O9 C30 -105.6(3) . .
O10 Ni2 O9 C30 -10.6(3) . .
O1W Ni2 O9 C30 77.4(3) . .
O6 Ni2 O9 Gd1 -40.74(8) . .
N3 Ni2 O9 Gd1 -18.4(6) . .
O11 Ni2 O9 Gd1 43.53(8) . .
O10 Ni2 O9 Gd1 138.52(9) . .
O1W Ni2 O9 Gd1 -133.45(9) . .
O5 Gd1 O9 C30 -116.8(3) . .
O6 Gd1 O9 C30 -173.9(3) . .
O8 Gd1 O9 C30 -43.2(3) . .
O2 Gd1 O9 C30 -5.0(4) . .
O3 Gd1 O9 C30 137.2(3) . .
O11 Gd1 O9 C30 110.3(3) . .
O2 Gd1 O9 C30 38.3(3) 3_576 .
Gd1 Gd1 O9 C30 26.3(3) 3_576 .
O5 Gd1 O9 Ni2 94.05(10) . .
O6 Gd1 O9 Ni2 36.94(8) . .
O8 Gd1 O9 Ni2 167.68(11) . .
O2 Gd1 O9 Ni2 -154.14(15) . .
O3 Gd1 O9 Ni2 -11.97(13) . .
O11 Gd1 O9 Ni2 -38.85(8) . .
O2 Gd1 O9 Ni2 -110.82(9) 3_576 .
Gd1 Gd1 O9 Ni2 -122.87(6) 3_576 .
O6 Ni2 O10 C23 17.4(7) . .
N3 Ni2 O10 C23 -171.2(3) . .
O9 Ni2 O10 C23 13.5(3) . .
O11 Ni2 O10 C23 94.6(3) . .
O1W Ni2 O10 C23 -82.9(3) . .
N2 Ni1 O11 Ni2 25.6(4) . .
N4 Ni1 O11 Ni2 -157.37(13) . .
O3 Ni1 O11 Ni2 99.60(12) . .
N1 Ni1 O11 Ni2 -71.42(14) . .
N2 Ni1 O11 Gd1 -71.0(4) . .
N4 Ni1 O11 Gd1 106.04(11) . .
O3 Ni1 O11 Gd1 3.00(9) . .
N1 Ni1 O11 Gd1 -168.02(10) . .
O6 Ni2 O11 Ni1 -67.09(12) . .
N3 Ni2 O11 Ni1 20.93(14) . .
O9 Ni2 O11 Ni1 -148.85(13) . .
O10 Ni2 O11 Ni1 123.38(12) . .
O6 Ni2 O11 Gd1 38.71(8) . .
N3 Ni2 O11 Gd1 126.74(11) . .
O9 Ni2 O11 Gd1 -43.04(8) . .
O10 Ni2 O11 Gd1 -130.81(9) . .
O5 Gd1 O11 Ni1 57.18(15) . .
O6 Gd1 O11 Ni1 82.27(10) . .
O8 Gd1 O11 Ni1 -171.37(9) . .
O2 Gd1 O11 Ni1 -49.83(12) . .
O9 Gd1 O11 Ni1 155.60(12) . .
O3 Gd1 O11 Ni1 -2.72(8) . .
O2 Gd1 O11 Ni1 -103.27(10) 3_576 .
Gd1 Gd1 O11 Ni1 -78.50(8) 3_576 .
O5 Gd1 O11 Ni2 -59.99(14) . .
O6 Gd1 O11 Ni2 -34.90(8) . .
O8 Gd1 O11 Ni2 71.46(12) . .
O2 Gd1 O11 Ni2 -167.01(7) . .
O9 Gd1 O11 Ni2 38.43(8) . .
O3 Gd1 O11 Ni2 -119.90(10) . .
O2 Gd1 O11 Ni2 139.56(10) 3_576 .
Gd1 Gd1 O11 Ni2 164.33(6) 3_576 .
C11 N1 C1 C2 164.9(3) . .
C21 N1 C1 C2 -74.9(4) . .
Ni1 N1 C1 C2 36.3(3) . .
C3 N2 C2 C1 -157.9(4) . .
Ni1 N2 C2 C1 30.1(4) . .
N1 C1 C2 N2 -44.3(4) . .
C2 N2 C3 C4 -173.6(4) . .
Ni1 N2 C3 C4 -2.7(6) . .
N2 C3 C4 C5 177.9(4) . .
N2 C3 C4 C10 -1.4(7) . .
C10 C4 C5 C6 0.6(7) . .
C3 C4 C5 C6 -178.7(4) . .
C4 C5 C6 C7 1.6(8) . .
C5 C6 C7 C8 0.2(7) . .
C6 C7 C8 C10 -4.2(6) . .
C6 C7 C8 C9 171.0(4) . .
Gd1 O2 C9 O1 125.2(3) . .
Gd1 O2 C9 O1 -71.5(4) 3_576 .
Gd1 O2 C9 C8 -58.8(4) . .
Gd1 O2 C9 C8 104.5(3) 3_576 .
C7 C8 C9 O1 9.0(5) . .
C10 C8 C9 O1 -176.2(3) . .
C7 C8 C9 O2 -167.0(3) . .
C10 C8 C9 O2 7.8(5) . .
Ni1 O3 C10 C4 15.6(5) . .
Gd1 O3 C10 C4 -158.0(2) . .
Ni1 O3 C10 C8 -164.7(2) . .
Gd1 O3 C10 C8 21.8(4) . .
C5 C4 C10 O3 175.3(4) . .
C3 C4 C10 O3 -5.4(6) . .
C5 C4 C10 C8 -4.4(5) . .
C3 C4 C10 C8 174.8(3) . .
C7 C8 C10 O3 -173.7(3) . .
C9 C8 C10 O3 11.6(5) . .
C7 C8 C10 C4 6.1(5) . .
C9 C8 C10 C4 -168.7(3) . .
C1 N1 C11 C12 -52.4(4) . .
C21 N1 C11 C12 -173.1(3) . .
Ni1 N1 C11 C12 70.1(4) . .
C13 N3 C12 C11 120.5(4) . .
Ni2 N3 C12 C11 -68.1(4) . .
N1 C11 C12 N3 -51.9(4) . .
C12 N3 C13 C14 -172.8(4) . .
Ni2 N3 C13 C14 16.4(6) . .
N3 C13 C14 C15 175.9(4) . .
N3 C13 C14 C20 3.0(7) . .
C20 C14 C15 C16 -0.2(7) . .
C13 C14 C15 C16 -173.6(5) . .
C14 C15 C16 C17 1.9(9) . .
C15 C16 C17 C18 -1.8(8) . .
C16 C17 C18 C20 0.0(7) . .
C16 C17 C18 C19 178.5(5) . .
Gd1 O5 C19 O4 -172.9(3) . .
Gd1 O5 C19 C18 7.3(6) . .
C17 C18 C19 O4 17.4(6) . .
C20 C18 C19 O4 -164.2(4) . .
C17 C18 C19 O5 -162.9(4) . .
C20 C18 C19 O5 15.5(6) . .
Ni2 O6 C20 C18 173.6(2) . .
Gd1 O6 C20 C18 -44.4(4) . .
Ni2 O6 C20 C14 -6.5(5) . .
Gd1 O6 C20 C14 135.5(3) . .
C17 C18 C20 O6 -178.4(4) . .
C19 C18 C20 O6 3.2(6) . .
C17 C18 C20 C14 1.7(6) . .
C19 C18 C20 C14 -176.7(4) . .
C15 C14 C20 O6 178.5(4) . .
C13 C14 C20 O6 -8.7(6) . .
C15 C14 C20 C18 -1.6(6) . .
C13 C14 C20 C18 171.3(4) . .
C1 N1 C21 C22 145.0(3) . .
C11 N1 C21 C22 -93.1(4) . .
Ni1 N1 C21 C22 32.0(4) . .
Ni1 N4 C22 C21 47.1(4) . .
N1 C21 C22 N4 -55.0(4) . .
Ni2 O10 C23 C24 -8.8(6) . .
O10 C23 C24 C25 178.2(4) . .
O10 C23 C24 C30 -5.3(7) . .
C30 C24 C25 C26 0.8(6) . .
C23 C24 C25 C26 177.4(4) . .
C24 C25 C26 C27 -3.5(7) . .
C25 C26 C27 C28 1.7(7) . .
C26 C27 C28 C30 2.8(6) . .
C26 C27 C28 C29 -178.7(4) . .
Gd1 O8 C29 O7 -177.2(2) . .
Gd1 O8 C29 C28 2.8(6) . .
C27 C28 C29 O7 -16.8(5) . .
C30 C28 C29 O7 161.6(3) . .
C27 C28 C29 O8 163.1(3) . .
C30 C28 C29 O8 -18.5(5) . .
Ni2 O9 C30 C28 -176.4(2) . .
Gd1 O9 C30 C28 46.0(4) . .
Ni2 O9 C30 C24 1.9(5) . .
Gd1 O9 C30 C24 -135.8(3) . .
C27 C28 C30 O9 172.9(3) . .
C29 C28 C30 O9 -5.5(5) . .
C27 C28 C30 C24 -5.3(5) . .
C29 C28 C30 C24 176.3(3) . .
C25 C24 C30 O9 -174.6(3) . .
C23 C24 C30 O9 9.0(5) . .
C25 C24 C30 C28 3.7(5) . .
C23 C24 C30 C28 -172.7(3) . .
