#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:00:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179875 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/71/7017141.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_7017141
loop_
_publ_author_name
'Andrews, Philip C.'
'Gee, William J.'
'Junk, Peter C.'
'Maclellan, Jonathan G.'
_publ_section_title
;
 Systematic study of the formation of the lanthanoid cubane cluster motif
 mediated by steric modification of diketonate ligands.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12169
_journal_page_last               12179
_journal_paper_doi               10.1039/c1dt10580a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C96 H84 Gd4 N8 O36'
_chemical_formula_sum            'C96 H84 Gd4 N8 O36'
_chemical_formula_weight         2554.71
_chemical_name_systematic
;
?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.209(2)
_cell_length_b                   17.209(2)
_cell_length_c                   16.019(3)
_cell_measurement_reflns_used    46069
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.88
_cell_volume                     4744.0(12)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Australian synchrotron MX1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77369
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46069
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.88
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  0.9451
_exptl_absorpt_correction_T_min  0.9193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.036(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         3228
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0253P)²+8.0581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0477
_reflns_number_gt                3211
_reflns_number_total             3228
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10580a.txt
_cod_data_source_block           wge037
_cod_original_cell_volume        4744.0(13)
_cod_database_code               7017141
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+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 0.385105(9) 0.494600(10) 1.074708(10) 0.01399(7) Uani 1 1 d .
O1 O 0.50025(16) 0.42207(13) 1.06866(14) 0.0141(5) Uani 1 1 d D
O2 O 0.34435(16) 0.39416(15) 1.16043(16) 0.0209(6) Uani 1 1 d .
O3 O 0.38987(16) 0.54530(15) 1.20967(17) 0.0195(6) Uani 1 1 d .
O4 O 0.48712(19) 0.31282(18) 1.25480(19) 0.0373(8) Uani 1 1 d D
O5 O 0.4901(2) 0.2535(2) 1.3743(2) 0.0520(9) Uani 1 1 d .
O6 O 0.25744(14) 0.49147(16) 1.03496(15) 0.0201(6) Uani 1 1 d .
O7 O 0.35437(15) 0.62454(15) 1.03056(16) 0.0202(6) Uani 1 1 d .
O8 O 0.10774(17) 0.4992(2) 1.12402(17) 0.0345(7) Uani 1 1 d .
O9 O 0.1089(2) 0.3725(2) 1.1227(2) 0.0459(9) Uani 1 1 d .
N1 N 0.4566(2) 0.2738(2) 1.3098(2) 0.0298(9) Uani 1 1 d .
N2 N 0.1072(2) 0.4366(2) 1.0872(2) 0.0279(8) Uani 1 1 d .
C1 C 0.3425(2) 0.3825(2) 1.2392(2) 0.0162(8) Uani 1 1 d .
C2 C 0.3558(2) 0.4390(2) 1.2995(2) 0.0176(9) Uani 1 1 d .
C3 C 0.3793(2) 0.5152(2) 1.2808(2) 0.0181(8) Uani 1 1 d .
C4 C 0.3957(3) 0.5589(2) 1.3605(3) 0.0322(11) Uani 1 1 d .
H4A H 0.3739 0.6121 1.3582 0.039 Uiso 1 1 calc R
H4B H 0.4523 0.5623 1.3710 0.039 Uiso 1 1 calc R
C5 C 0.3553(3) 0.5102(2) 1.4279(3) 0.0365(11) Uani 1 1 d .
H5A H 0.3026 0.5309 1.4395 0.044 Uiso 1 1 calc R
H5B H 0.3857 0.5109 1.4804 0.044 Uiso 1 1 calc R
C6 C 0.3503(3) 0.4270(3) 1.3926(3) 0.0286(11) Uani 1 1 d .
H6A H 0.3938 0.3946 1.4132 0.034 Uiso 1 1 calc R
H6B H 0.3005 0.4020 1.4079 0.034 Uiso 1 1 calc R
C7 C 0.3218(2) 0.3009(2) 1.2653(2) 0.0186(9) Uani 1 1 d .
C8 C 0.3753(3) 0.2493(2) 1.2995(3) 0.0235(10) Uani 1 1 d .
C9 C 0.3559(3) 0.1744(2) 1.3233(2) 0.0288(11) Uani 1 1 d .
H9 H 0.3938 0.1408 1.3469 0.035 Uiso 1 1 calc R
C10 C 0.2792(3) 0.1493(3) 1.3117(3) 0.0313(11) Uani 1 1 d .
H10 H 0.2652 0.0974 1.3251 0.038 Uiso 1 1 calc R
C11 C 0.2242(3) 0.2000(3) 1.2809(3) 0.0281(10) Uani 1 1 d .
H11 H 0.1716 0.1838 1.2764 0.034 Uiso 1 1 calc R
C12 C 0.2452(2) 0.2750(2) 1.2563(2) 0.0214(9) Uani 1 1 d .
H12 H 0.2072 0.3088 1.2333 0.026 Uiso 1 1 calc R
C13 C 0.2128(2) 0.5347(2) 0.9889(2) 0.0184(9) Uani 1 1 d .
C14 C 0.2261(2) 0.6132(2) 0.9733(2) 0.0186(9) Uani 1 1 d .
C15 C 0.2926(2) 0.6523(2) 0.9998(2) 0.0175(9) Uani 1 1 d .
C16 C 0.2846(2) 0.7389(2) 0.9839(2) 0.0212(9) Uani 1 1 d .
H16A H 0.3170 0.7552 0.9359 0.025 Uiso 1 1 calc R
H16B H 0.3000 0.7692 1.0337 0.025 Uiso 1 1 calc R
C17 C 0.1986(3) 0.7496(3) 0.9649(3) 0.0291(11) Uani 1 1 d .
H17A H 0.1910 0.7904 0.9221 0.035 Uiso 1 1 calc R
H17B H 0.1698 0.7645 1.0160 0.035 Uiso 1 1 calc R
C18 C 0.1702(2) 0.6704(2) 0.9323(3) 0.0269(9) Uani 1 1 d .
H18A H 0.1159 0.6602 0.9495 0.032 Uiso 1 1 calc R
H18B H 0.1737 0.6677 0.8706 0.032 Uiso 1 1 calc R
C19 C 0.1470(2) 0.4901(3) 0.9511(2) 0.0209(8) Uani 1 1 d .
C20 C 0.1021(2) 0.4378(2) 0.9957(3) 0.0225(10) Uani 1 1 d .
C21 C 0.0515(3) 0.3852(3) 0.9599(3) 0.0366(12) Uani 1 1 d .
H21 H 0.0232 0.3494 0.9931 0.044 Uiso 1 1 calc R
C22 C 0.0435(3) 0.3864(4) 0.8735(3) 0.0451(13) Uani 1 1 d .
H22 H 0.0094 0.3506 0.8470 0.054 Uiso 1 1 calc R
C23 C 0.0850(3) 0.4394(3) 0.8257(3) 0.0479(15) Uani 1 1 d .
H23 H 0.0784 0.4406 0.7669 0.057 Uiso 1 1 calc R
C24 C 0.1366(2) 0.4911(3) 0.8643(2) 0.0344(11) Uani 1 1 d .
H24 H 0.1649 0.5271 0.8313 0.041 Uiso 1 1 calc R
H1 H 0.501(3) 0.3865(18) 1.1106(15) 0.041 Uiso 1 1 d D
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'
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
O6 Gd1 O2 81.76(10) . .
O6 Gd1 O3 107.48(9) . .
O2 Gd1 O3 74.95(9) . .
O6 Gd1 O1 141.98(9) . .
O2 Gd1 O1 83.28(9) . .
O3 Gd1 O1 101.99(9) . .
O6 Gd1 O1 89.37(8) . 2_567
O2 Gd1 O1 132.80(9) . 2_567
O3 Gd1 O1 150.37(9) . 2_567
O1 Gd1 O1 75.79(9) . 2_567
O6 Gd1 O7 74.26(9) . .
O2 Gd1 O7 143.31(9) . .
O3 Gd1 O7 86.13(9) . .
O1 Gd1 O7 132.00(9) . .
O1 Gd1 O7 74.98(9) 2_567 .
O6 Gd1 O1 141.16(9) . 3_665
O2 Gd1 O1 134.96(9) . 3_665
O3 Gd1 O1 77.80(8) . 3_665
O1 Gd1 O1 68.15(9) . 3_665
O1 Gd1 O1 74.00(9) 2_567 3_665
O7 Gd1 O1 67.65(9) . 3_665
O6 Gd1 O7 76.56(9) . 4_657
O2 Gd1 O7 73.22(8) . 4_657
O3 Gd1 O7 146.94(8) . 4_657
O1 Gd1 O7 65.68(8) . 4_657
O1 Gd1 O7 59.65(8) 2_567 4_657
O7 Gd1 O7 125.49(3) . 4_657
O1 Gd1 O7 120.24(7) 3_665 4_657
O6 Gd1 Gd1 108.88(6) . 2_567
O2 Gd1 Gd1 163.66(7) . 2_567
O3 Gd1 Gd1 111.97(7) . 2_567
O1 Gd1 Gd1 80.79(6) . 2_567
O1 Gd1 Gd1 38.45(6) 2_567 2_567
O7 Gd1 Gd1 53.03(6) . 2_567
O1 Gd1 Gd1 39.69(5) 3_665 2_567
O7 Gd1 Gd1 96.73(5) 4_657 2_567
O6 Gd1 Gd1 110.29(6) . 4_657
O2 Gd1 Gd1 100.00(7) . 4_657
O3 Gd1 Gd1 140.70(7) . 4_657
O1 Gd1 Gd1 39.24(5) . 4_657
O1 Gd1 Gd1 40.82(6) 2_567 4_657
O7 Gd1 Gd1 114.10(6) . 4_657
O1 Gd1 Gd1 79.66(5) 3_665 4_657
O7 Gd1 Gd1 40.65(5) 4_657 4_657
Gd1 Gd1 Gd1 65.019(9) 2_567 4_657
O6 Gd1 Gd1 163.79(6) . 3_665
O2 Gd1 Gd1 109.72(7) . 3_665
O3 Gd1 Gd1 86.98(7) . 3_665
O1 Gd1 Gd1 34.97(6) . 3_665
O1 Gd1 Gd1 74.44(5) 2_567 3_665
O7 Gd1 Gd1 100.14(6) . 3_665
O1 Gd1 Gd1 33.39(6) 3_665 3_665
O7 Gd1 Gd1 95.43(5) 4_657 3_665
Gd1 Gd1 Gd1 57.491(5) 2_567 3_665
Gd1 Gd1 Gd1 57.491(4) 4_657 3_665
Gd1 O1 Gd1 102.31(9) . 4_657
Gd1 O1 Gd1 111.64(9) . 3_665
Gd1 O1 Gd1 99.49(9) 4_657 3_665
Gd1 O1 H1 110(3) . .
Gd1 O1 H1 122(2) 4_657 .
Gd1 O1 H1 111(4) 3_665 .
C1 O2 Gd1 135.3(2) . .
C3 O3 Gd1 132.6(2) . .
C13 O6 Gd1 135.4(2) . .
C15 O7 Gd1 130.6(2) . .
C15 O7 Gd1 119.1(2) . 2_567
Gd1 O7 Gd1 86.32(8) . 2_567
O4 N1 O5 123.7(4) . .
O4 N1 C8 118.9(4) . .
O5 N1 C8 117.3(4) . .
O8 N2 O9 124.0(4) . .
O8 N2 C20 117.9(4) . .
O9 N2 C20 118.1(4) . .
O2 C1 C2 124.9(4) . .
O2 C1 C7 115.3(3) . .
C2 C1 C7 119.8(3) . .
C1 C2 C3 123.5(4) . .
C1 C2 C6 125.6(4) . .
C3 C2 C6 110.9(4) . .
O3 C3 C2 128.1(4) . .
O3 C3 C4 122.1(3) . .
C2 C3 C4 109.8(3) . .
C3 C4 C5 103.8(3) . .
C3 C4 H4A 111.0 . .
C5 C4 H4A 111.0 . .
C3 C4 H4B 111.0 . .
C5 C4 H4B 111.0 . .
H4A C4 H4B 109.0 . .
C4 C5 C6 105.9(4) . .
C4 C5 H5A 110.6 . .
C6 C5 H5A 110.6 . .
C4 C5 H5B 110.6 . .
C6 C5 H5B 110.6 . .
H5A C5 H5B 108.7 . .
C2 C6 C5 103.5(4) . .
C2 C6 H6A 111.1 . .
C5 C6 H6A 111.1 . .
C2 C6 H6B 111.1 . .
C5 C6 H6B 111.1 . .
H6A C6 H6B 109.0 . .
C8 C7 C12 117.5(4) . .
C8 C7 C1 123.2(4) . .
C12 C7 C1 119.3(4) . .
C9 C8 C7 122.8(4) . .
C9 C8 N1 117.7(4) . .
C7 C8 N1 119.4(4) . .
C8 C9 C10 118.5(4) . .
C8 C9 H9 120.7 . .
C10 C9 H9 120.7 . .
C11 C10 C9 119.9(4) . .
C11 C10 H10 120.0 . .
C9 C10 H10 120.0 . .
C10 C11 C12 120.5(4) . .
C10 C11 H11 119.8 . .
C12 C11 H11 119.8 . .
C7 C12 C11 120.6(4) . .
C7 C12 H12 119.7 . .
C11 C12 H12 119.7 . .
O6 C13 C14 124.1(4) . .
O6 C13 C19 112.6(3) . .
C14 C13 C19 123.3(4) . .
C13 C14 C15 123.3(4) . .
C13 C14 C18 126.8(4) . .
C15 C14 C18 109.7(4) . .
O7 C15 C14 128.7(4) . .
O7 C15 C16 120.9(4) . .
C14 C15 C16 110.4(3) . .
C15 C16 C17 103.9(3) . .
C15 C16 H16A 111.0 . .
C17 C16 H16A 111.0 . .
C15 C16 H16B 111.0 . .
C17 C16 H16B 111.0 . .
H16A C16 H16B 109.0 . .
C16 C17 C18 105.6(3) . .
C16 C17 H17A 110.6 . .
C18 C17 H17A 110.6 . .
C16 C17 H17B 110.6 . .
C18 C17 H17B 110.6 . .
H17A C17 H17B 108.7 . .
C14 C18 C17 103.0(3) . .
C14 C18 H18A 111.2 . .
C17 C18 H18A 111.2 . .
C14 C18 H18B 111.2 . .
C17 C18 H18B 111.2 . .
H18A C18 H18B 109.1 . .
C20 C19 C24 116.6(4) . .
C20 C19 C13 123.2(3) . .
C24 C19 C13 119.4(4) . .
C21 C20 C19 124.3(4) . .
C21 C20 N2 116.4(4) . .
C19 C20 N2 119.4(3) . .
C20 C21 C22 117.9(5) . .
C20 C21 H21 121.1 . .
C22 C21 H21 121.1 . .
C23 C22 C21 120.4(5) . .
C23 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
C22 C23 C24 120.0(5) . .
C22 C23 H23 120.0 . .
C24 C23 H23 120.0 . .
C23 C24 C19 120.7(5) . .
C23 C24 H24 119.6 . .
C19 C24 H24 119.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 O6 2.288(2) .
Gd1 O2 2.316(3) .
Gd1 O3 2.333(3) .
Gd1 O1 2.344(3) .
Gd1 O1 2.385(2) 2_567
Gd1 O7 2.404(3) .
Gd1 O1 2.441(3) 3_665
Gd1 O7 2.949(3) 4_657
Gd1 Gd1 3.6830(5) 2_567
Gd1 Gd1 3.6830(5) 4_657
Gd1 Gd1 3.9588(7) 3_665
O1 Gd1 2.385(2) 4_657
O1 Gd1 2.441(3) 3_665
O1 H1 0.909(9) .
O2 C1 1.278(5) .
O3 C3 1.264(5) .
O4 N1 1.227(5) .
O5 N1 1.234(5) .
O6 C13 1.299(5) .
O7 C15 1.265(5) .
O7 Gd1 2.949(3) 2_567
O8 N2 1.227(5) .
O9 N2 1.241(5) .
N1 C8 1.470(6) .
N2 C20 1.469(6) .
C1 C2 1.390(5) .
C1 C7 1.509(5) .
C2 C3 1.406(6) .
C2 C6 1.507(6) .
C3 C4 1.508(6) .
C4 C5 1.534(6) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.543(6) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.391(6) .
C7 C12 1.398(6) .
C8 C9 1.385(6) .
C9 C10 1.401(7) .
C9 H9 0.9500 .
C10 C11 1.379(7) .
C10 H10 0.9500 .
C11 C12 1.399(6) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.392(6) .
C13 C19 1.496(6) .
C14 C15 1.394(6) .
C14 C18 1.526(5) .
C15 C16 1.518(5) .
C16 C17 1.523(6) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.538(7) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C20 1.384(6) .
C19 C24 1.402(5) .
C20 C21 1.380(6) .
C21 C22 1.390(7) .
C21 H21 0.9500 .
C22 C23 1.389(8) .
C22 H22 0.9500 .
C23 C24 1.401(7) .
C23 H23 0.9500 .
C24 H24 0.9500 .
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
O1 H1 O4 0.909(9) 2.646(9) 3.532(4) 165(3)
