#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/92/4329276.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_4329276
loop_
_publ_author_name
'George J. Sopasis'
'Angelos B. Canaj'
'Aggelos Philippidis'
'Milosz Siczek'
'Tadeusz Lis'
'James R. O'Brien'
'Manolis M. Antonakis'
'Spiros A. Pergantis'
'Constantinos J. Milios'
_publ_section_title
;
 Heptanuclear Heterometallic [Cu6Ln] Clusters: Trapping Lanthanides into
 Copper Cages with Artificial Amino Acids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5911
_journal_page_last               5918
_journal_paper_doi               10.1021/ic300538q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety
'C30 H60 Cu6 Dy N9 O30, 1.5(C4 H10 O), 3(C H4 O)'
_chemical_formula_sum            'C39 H87 Cu6 Dy N9 O34.5'
_chemical_formula_weight         1777.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   20.116(5)
_cell_length_b                   20.116(5)
_cell_length_c                   13.338(5)
_cell_measurement_reflns_used    15628
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.56
_cell_measurement_theta_min      2.54
_cell_volume                     4674(2)
_computing_cell_refinement       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur PX with Onyx CCD'
_diffrn_measurement_method       '/f and /w'
_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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49635
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         31.56
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    2.194
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.507
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5
Analytical numeric absorption correction using a 
multifaceted crystal model based on expressions
 derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.18
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         5421
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0727P)²+7.2700P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                4186
_reflns_number_total             5421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300538q_si_001_08.cif
_cod_data_source_block           gis393a
_cod_original_formula_sum        'C39 H87 Cu6 Dy N9 O34.50'
_cod_database_code               4329276
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy Dy 0.6667 0.3333 0.7500 0.01858(10) Uani 1 6 d S . .
Cu Cu 0.83162(2) 0.46988(3) 0.86719(3) 0.02336(12) Uani 1 1 d . . .
O1 O 0.77226(19) 0.46234(19) 0.7500 0.0208(6) Uani 1 2 d S . .
H1 H 0.7551 0.5012 0.7500 0.025 Uiso 1 2 calc SR . .
O11 O 0.76215(14) 0.35699(14) 0.87834(17) 0.0227(5) Uani 1 1 d . . .
O21 O 0.74057(19) 0.25251(17) 0.9642(2) 0.0417(8) Uani 1 1 d . . .
N11 N 0.88900(19) 0.4527(2) 0.9748(2) 0.0321(7) Uani 1 1 d . A .
H11A H 0.9344 0.4593 0.9492 0.039 Uiso 1 1 calc R . .
H11B H 0.9007 0.4886 1.0245 0.039 Uiso 1 1 calc R . .
C11 C 0.7774(2) 0.3220(2) 0.9481(3) 0.0317(8) Uani 1 1 d . A .
C21 C 0.8442(3) 0.3739(3) 1.0192(3) 0.0463(12) Uani 1 1 d . . .
C31 C 0.8881(12) 0.3392(14) 1.0525(13) 0.054(5) Uani 0.50 1 d P A 1
H31A H 0.9246 0.3715 1.1042 0.081 Uiso 0.50 1 calc PR A 1
H31B H 0.9162 0.3343 0.9956 0.081 Uiso 0.50 1 calc PR A 1
H31C H 0.8534 0.2882 1.0803 0.081 Uiso 0.50 1 calc PR A 1
C311 C 0.9052(14) 0.3410(17) 1.0141(14) 0.065(6) Uani 0.50 1 d P A 2
H31D H 0.9504 0.3736 1.0551 0.098 Uiso 0.50 1 calc PR A 2
H31E H 0.9211 0.3417 0.9445 0.098 Uiso 0.50 1 calc PR A 2
H31F H 0.8801 0.2883 1.0397 0.098 Uiso 0.50 1 calc PR A 2
C41 C 0.7988(11) 0.3869(11) 1.1188(13) 0.042(3) Uani 0.50 1 d P A 3
H41A H 0.7627 0.3370 1.1481 0.062 Uiso 0.50 1 calc PR A 3
H41B H 0.7708 0.4124 1.0962 0.062 Uiso 0.50 1 calc PR A 3
H41C H 0.8369 0.4188 1.1693 0.062 Uiso 0.50 1 calc PR A 3
C411 C 0.8165(12) 0.3703(12) 1.1142(14) 0.055(5) Uani 0.50 1 d P A 4
H41D H 0.7823 0.3165 1.1327 0.083 Uiso 0.50 1 calc PR A 4
H41E H 0.7879 0.3979 1.1162 0.083 Uiso 0.50 1 calc PR A 4
H41F H 0.8594 0.3938 1.1616 0.083 Uiso 0.50 1 calc PR A 4
O12 O 0.91387(16) 0.57383(16) 0.8345(2) 0.0330(6) Uani 1 1 d . . .
C12 C 0.9358(3) 0.6052(3) 0.7500 0.0313(11) Uani 1 2 d S . .
C22 C 0.9960(4) 0.6899(4) 0.7500 0.0477(16) Uani 1 2 d S . .
H22A H 0.9894 0.7142 0.8010 0.072 Uiso 1 1 d R . .
H22C H 1.0478 0.6976 0.7500 0.072 Uiso 1 2 d SR . .
O13 O 0.9100(2) 0.4177(2) 0.7500 0.0294(8) Uani 1 2 d S . .
N13 N 0.9810(3) 0.4555(3) 0.7500 0.0329(10) Uani 1 2 d S . .
O23 O 1.0109(7) 0.4647(7) 0.8417(9) 0.040(2) Uani 0.50 1 d P . .
O33 O 1.0240(8) 0.4882(9) 0.8149(11) 0.052(3) Uani 0.50 1 d P . .
O1M O 0.7393(4) 0.5756(4) 0.7757(5) 0.047(2) Uani 0.50 1 d P B -5
H1M H 0.6899 0.5484 0.7577 0.070 Uiso 0.50 1 d PR B -5
C1M C 0.7777(8) 0.6466(7) 0.771(7) 0.11(2) Uani 0.50 1 d P B -5
H1M1 H 0.7526 0.6654 0.7251 0.164 Uiso 0.50 1 calc PR B -5
H1M2 H 0.8292 0.6620 0.7456 0.164 Uiso 0.50 1 calc PR B -5
H1M3 H 0.7817 0.6685 0.8376 0.164 Uiso 0.50 1 calc PR B -5
O1E O 0.7521(8) 0.0924(7) 0.2500 0.075(4) Uani 0.50 2 d SPD . 2
C1E C 0.7476(8) 0.1264(8) 0.1706(15) 0.123(9) Uani 0.50 1 d PD . 2
H1E1 H 0.7843 0.1821 0.1768 0.147 Uiso 0.50 1 calc PR . 2
H1E2 H 0.6954 0.1195 0.1666 0.147 Uiso 0.50 1 calc PR . 2
C2E C 0.7637(13) 0.0984(11) 0.0766(15) 0.145(11) Uani 0.50 1 d PD . 2
H2E1 H 0.7353 0.1049 0.0214 0.218 Uiso 0.50 1 calc PR . 2
H2E2 H 0.7476 0.0439 0.0837 0.218 Uiso 0.50 1 calc PR . 2
H2E3 H 0.8188 0.1277 0.0624 0.218 Uiso 0.50 1 calc PR . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O1 Dy O1 120.000(1) 3_665 .
O1 Dy O1 119.999(1) 3_665 2_655
O1 Dy O1 120.0 . 2_655
O1 Dy O11 71.80(8) 3_665 .
O1 Dy O11 66.59(8) . .
O1 Dy O11 135.21(6) 2_655 .
O1 Dy O11 71.80(8) 3_665 10_557
O1 Dy O11 66.59(8) . 10_557
O1 Dy O11 135.20(6) 2_655 10_557
O11 Dy O11 89.31(12) . 10_557
O1 Dy O11 66.59(8) 3_665 12_667
O1 Dy O11 135.21(6) . 12_667
O1 Dy O11 71.80(8) 2_655 12_667
O11 Dy O11 138.33(5) . 12_667
O11 Dy O11 76.05(9) 10_557 12_667
O1 Dy O11 66.59(8) 3_665 3_665
O1 Dy O11 135.21(6) . 3_665
O1 Dy O11 71.80(8) 2_655 3_665
O11 Dy O11 76.05(9) . 3_665
O11 Dy O11 138.33(5) 10_557 3_665
O11 Dy O11 89.31(12) 12_667 3_665
O1 Dy O11 135.21(6) 3_665 11_657
O1 Dy O11 71.80(8) . 11_657
O1 Dy O11 66.59(8) 2_655 11_657
O11 Dy O11 138.33(5) . 11_657
O11 Dy O11 76.06(9) 10_557 11_657
O11 Dy O11 76.06(9) 12_667 11_657
O11 Dy O11 138.33(5) 3_665 11_657
O1 Dy O11 135.21(6) 3_665 2_655
O1 Dy O11 71.80(8) . 2_655
O1 Dy O11 66.59(8) 2_655 2_655
O11 Dy O11 76.06(9) . 2_655
O11 Dy O11 138.33(5) 10_557 2_655
O11 Dy O11 138.33(5) 12_667 2_655
O11 Dy O11 76.06(9) 3_665 2_655
O11 Dy O11 89.31(12) 11_657 2_655
O1 Dy Cu 99.73(7) 3_665 10_557
O1 Dy Cu 32.61(4) . 10_557
O1 Dy Cu 132.33(6) 2_655 10_557
O11 Dy Cu 79.17(6) . 10_557
O11 Dy Cu 34.39(6) 10_557 10_557
O11 Dy Cu 105.35(6) 12_667 10_557
O11 Dy Cu 154.44(6) 3_665 10_557
O11 Dy Cu 66.69(6) 11_657 10_557
O11 Dy Cu 103.99(6) 2_655 10_557
O1 Dy Cu 132.33(6) 3_665 11_657
O1 Dy Cu 99.73(7) . 11_657
O1 Dy Cu 32.61(4) 2_655 11_657
O11 Dy Cu 154.45(6) . 11_657
O11 Dy Cu 105.35(6) 10_557 11_657
O11 Dy Cu 66.70(6) 12_667 11_657
O11 Dy Cu 103.99(6) 3_665 11_657
O11 Dy Cu 34.39(6) 11_657 11_657
O11 Dy Cu 79.17(6) 2_655 11_657
Cu Dy Cu 101.045(16) 10_557 11_657
O1 Dy Cu 99.73(7) 3_665 .
O1 Dy Cu 32.61(4) . .
O1 Dy Cu 132.33(6) 2_655 .
O11 Dy Cu 34.39(6) . .
O11 Dy Cu 79.17(6) 10_557 .
O11 Dy Cu 154.44(6) 12_667 .
O11 Dy Cu 105.35(6) 3_665 .
O11 Dy Cu 103.99(6) 11_657 .
O11 Dy Cu 66.69(6) 2_655 .
Cu Dy Cu 53.93(3) 10_557 .
Cu Dy Cu 127.070(7) 11_657 .
O1 Cu O12 93.62(13) . .
O1 Cu N11 165.49(14) . .
O12 Cu N11 95.31(13) . .
O1 Cu O11 85.23(12) . .
O12 Cu O11 166.17(11) . .
N11 Cu O11 83.37(12) . .
O1 Cu O21 89.59(12) . 2_655
O12 Cu O21 104.54(12) . 2_655
N11 Cu O21 99.18(14) . 2_655
O11 Cu O21 89.24(11) . 2_655
O1 Cu Dy 42.06(10) . .
O12 Cu Dy 135.42(9) . .
N11 Cu Dy 127.10(10) . .
O11 Cu Dy 43.74(7) . .
O21 Cu Dy 83.70(7) 2_655 .
Cu O1 Cu 108.48(17) 10_557 .
Cu O1 Dy 105.33(11) 10_557 .
Cu O1 Dy 105.33(11) . .
Cu O1 H1 112.4 10_557 .
Cu O1 H1 112.4 . .
Dy O1 H1 112.4 . .
C11 O11 Cu 117.0(2) . .
C11 O11 Dy 141.1(2) . .
Cu O11 Dy 101.87(10) . .
C11 O21 Cu 123.1(2) . 3_665
C21 N11 Cu 112.1(2) . .
C21 N11 H11A 109.2 . .
Cu N11 H11A 109.2 . .
C21 N11 H11B 109.2 . .
Cu N11 H11B 109.2 . .
H11A N11 H11B 107.9 . .
O21 C11 O11 125.0(3) . .
O21 C11 C21 119.1(3) . .
O11 C11 C21 115.8(3) . .
C411 C21 C31 91.2(11) . .
C411 C21 N11 115.8(10) . .
C31 C21 N11 116.3(9) . .
C411 C21 C11 109.7(10) . .
C31 C21 C11 113.4(10) . .
N11 C21 C11 109.4(3) . .
C411 C21 C311 112.2(11) . .
N11 C21 C311 103.4(9) . .
C11 C21 C311 105.7(10) . .
C31 C21 C41 109.8(10) . .
N11 C21 C41 103.3(7) . .
C11 C21 C41 103.3(7) . .
C311 C21 C41 130.7(9) . .
C21 C31 H31A 109.5 . .
C21 C31 H31B 109.5 . .
C21 C31 H31C 109.5 . .
C21 C311 H31D 109.5 . .
C21 C311 H31E 109.5 . .
H31D C311 H31E 109.5 . .
C21 C311 H31F 109.5 . .
H31D C311 H31F 109.5 . .
H31E C311 H31F 109.5 . .
C21 C41 H41A 109.5 . .
C21 C41 H41B 109.5 . .
C21 C41 H41C 109.5 . .
C21 C411 H41D 109.5 . .
C21 C411 H41E 109.5 . .
C21 C411 H41F 109.5 . .
C12 O12 Cu 129.1(3) . .
O12 C12 O12 127.1(5) . 10_557
O12 C12 C22 116.5(3) . .
O12 C12 C22 116.5(3) 10_557 .
C12 C22 H22A 111.3 . .
C12 C22 H22C 111.7 . .
H22A C22 H22C 110.9 . .
O33 N13 O33 95.9(12) 10_557 .
O33 N13 O13 130.4(7) 10_557 .
O33 N13 O13 130.4(7) . .
O33 N13 O23 116.6(8) 10_557 .
O13 N13 O23 112.7(5) . .
O33 N13 O23 116.6(8) . 10_557
O13 N13 O23 112.7(5) . 10_557
O23 N13 O23 133.0(12) . 10_557
O33 O23 N13 61(3) . .
O23 O33 N13 96(3) . .
O23 O33 O33 131(3) . 10_557
C1M O1M H1M 123.3 . .
C1E O1E C1E 111(2) 10_556 .
O1E C1E C2E 114.1(13) . .
O1E C1E H1E1 108.7 . .
C2E C1E H1E1 108.7 . .
O1E C1E H1E2 108.7 . .
C2E C1E H1E2 108.7 . .
H1E1 C1E H1E2 107.6 . .
C1E C2E H2E1 109.5 . .
C1E C2E H2E2 109.5 . .
H2E1 C2E H2E2 109.5 . .
C1E C2E H2E3 109.5 . .
H2E1 C2E H2E3 109.5 . .
H2E2 C2E H2E3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Dy O1 2.395(3) 3_665
Dy O1 2.395(3) .
Dy O1 2.395(3) 2_655
Dy O11 2.436(2) .
Dy O11 2.436(2) 10_557
Dy O11 2.436(2) 12_667
Dy O11 2.436(2) 3_665
Dy O11 2.436(2) 11_657
Dy O11 2.436(2) 2_655
Dy Cu 3.4473(8) 10_557
Dy Cu 3.4473(8) 11_657
Dy Cu 3.4473(8) .
Cu O1 1.926(2) .
Cu O12 1.960(3) .
Cu N11 1.978(3) .
Cu O11 1.990(3) .
Cu O21 2.300(3) 2_655
O1 Cu 1.926(2) 10_557
O1 H1 1.0000 .
O11 C11 1.293(4) .
O21 C11 1.229(5) .
O21 Cu 2.300(3) 3_665
N11 C21 1.499(6) .
N11 H11A 0.9200 .
N11 H11B 0.9200 .
C11 C21 1.547(5) .
C21 C411 1.372(19) .
C21 C31 1.44(2) .
C21 C311 1.66(3) .
C21 C41 1.704(16) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C311 H31D 0.9800 .
C311 H31E 0.9800 .
C311 H31F 0.9800 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
C411 H41D 0.9800 .
C411 H41E 0.9800 .
C411 H41F 0.9800 .
O12 C12 1.260(4) .
C12 O12 1.260(4) 10_557
C12 C22 1.518(8) .
C22 H22A 0.8855 .
C22 H22C 0.9724 .
O13 N13 1.238(6) .
N13 O33 1.167(17) 10_557
N13 O33 1.167(17) .
N13 O23 1.334(13) .
N13 O23 1.334(12) 10_557
O23 O33 0.543(14) .
O33 O33 1.73(3) 10_557
O1M C1M 1.241(14) .
O1M H1M 0.8962 .
C1M H1M1 0.9800 .
C1M H1M2 0.9800 .
C1M H1M3 0.9800 .
O1E C1E 1.288(14) 10_556
O1E C1E 1.288(14) .
C1E C2E 1.476(17) .
C1E H1E1 0.9900 .
C1E H1E2 0.9900 .
C2E H2E1 0.9800 .
C2E H2E2 0.9800 .
C2E H2E3 0.9800 .
