#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/92/4329269.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_4329269
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 Ce Cu6 N9 O30, 1.5(C4 H10 O), 3(C H4 O), 0.3(H2 O)'
_chemical_formula_sum            'C39 H87.6 Ce Cu6 N9 O34.8'
_chemical_formula_weight         1760.94
_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                   20.130(5)
_cell_length_b                   20.130(5)
_cell_length_c                   13.367(4)
_cell_measurement_reflns_used    22331
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.84
_cell_measurement_theta_min      3.04
_cell_volume                     4691(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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       ω
_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  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41589
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         36.98
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.876
_exptl_absorpt_correction_T_max  0.676
_exptl_absorpt_correction_T_min  0.506
_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    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             1790
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.792
_refine_diff_density_min         -1.270
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         7660
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0504
_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)+(0.0848P)²+6.4882P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1636
_reflns_number_gt                5964
_reflns_number_total             7660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300538q_si_001_01.cif
_cod_data_source_block           gis742a
_cod_original_formula_sum        'C39 H87.60 Ce Cu6 N9 O34.80'
_cod_database_code               4329269
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
Ce Ce 0.6667 0.3333 0.7500 0.01476(7) Uani 1 6 d S . .
Cu Cu 0.834000(18) 0.470771(19) 0.86736(3) 0.02285(9) Uani 1 1 d . . .
O1 O 0.77634(14) 0.46562(14) 0.7500 0.0191(4) Uani 1 2 d S . .
H1 H 0.7601 0.5051 0.7500 0.023 Uiso 1 2 calc SR . .
O11 O 0.76504(11) 0.35839(11) 0.87988(14) 0.0221(3) Uani 1 1 d . . .
O21 O 0.74239(15) 0.25332(13) 0.96510(19) 0.0379(6) Uani 1 1 d . . .
N11 N 0.89080(15) 0.45342(16) 0.9758(2) 0.0334(5) Uani 1 1 d . A .
H11A H 0.9362 0.4598 0.9506 0.040 Uiso 1 1 calc R . .
H11B H 0.9025 0.4895 1.0251 0.040 Uiso 1 1 calc R . .
C11 C 0.77948(17) 0.32296(17) 0.9497(2) 0.0301(6) Uani 1 1 d . A .
C21 C 0.8459(2) 0.3751(2) 1.0203(3) 0.0507(11) Uani 1 1 d . . .
C31 C 0.8872(7) 0.3397(9) 1.0593(11) 0.056(4) Uani 0.50 1 d P A 1
H31A H 0.9173 0.3686 1.1176 0.085 Uiso 0.50 1 calc PR A 1
H31B H 0.9218 0.3396 1.0077 0.085 Uiso 0.50 1 calc PR A 1
H31C H 0.8508 0.2868 1.0791 0.085 Uiso 0.50 1 calc PR A 1
C311 C 0.9075(7) 0.3416(9) 1.0164(12) 0.064(4) Uani 0.50 1 d P A 2
H31D H 0.9506 0.3718 1.0618 0.096 Uiso 0.50 1 calc PR A 2
H31E H 0.9268 0.3459 0.9481 0.096 Uiso 0.50 1 calc PR A 2
H31F H 0.8811 0.2877 1.0373 0.096 Uiso 0.50 1 calc PR A 2
C41 C 0.7976(7) 0.3861(10) 1.1219(10) 0.046(3) Uani 0.50 1 d P A 3
H41A H 0.7658 0.3363 1.1543 0.069 Uiso 0.50 1 calc PR A 3
H41B H 0.7649 0.4061 1.0984 0.069 Uiso 0.50 1 calc PR A 3
H41C H 0.8350 0.4220 1.1701 0.069 Uiso 0.50 1 calc PR A 3
C411 C 0.8204(9) 0.3763(9) 1.1125(10) 0.069(5) Uani 0.50 1 d P A 4
H41D H 0.7845 0.3238 1.1341 0.103 Uiso 0.50 1 calc PR A 4
H41E H 0.7942 0.4063 1.1119 0.103 Uiso 0.50 1 calc PR A 4
H41F H 0.8639 0.3998 1.1588 0.103 Uiso 0.50 1 calc PR A 4
O12 O 0.91681(12) 0.57423(12) 0.83453(18) 0.0319(4) Uani 1 1 d . . .
C12 C 0.9388(2) 0.6055(2) 0.7500 0.0302(8) Uani 1 2 d S . .
C22 C 0.9989(3) 0.6899(3) 0.7500 0.0455(12) Uani 1 2 d S . .
H22A H 0.9923 0.7141 0.8010 0.068 Uiso 1 1 d R . .
H22C H 1.0507 0.6976 0.7500 0.068 Uiso 1 2 d SR . .
O13 O 0.90985(16) 0.41736(18) 0.7500 0.0292(6) Uani 1 2 d S . .
N13 N 0.9810(2) 0.4538(2) 0.7500 0.0363(9) Uani 1 2 d S . .
O23 O 1.0106(4) 0.4606(5) 0.8437(6) 0.0401(15) Uani 0.50 1 d P . .
O33 O 1.0239(5) 0.4862(5) 0.8118(7) 0.051(2) Uani 0.50 1 d P . .
O1M O 0.7415(3) 0.5773(3) 0.7678(18) 0.059(6) Uani 0.50 1 d P B -5
H1M H 0.6920 0.5502 0.7578 0.089 Uiso 0.50 1 d PR B -5
C1M C 0.7853(11) 0.6530(11) 0.7067(14) 0.134(7) Uiso 0.50 1 d P B -5
H1M1 H 0.7656 0.6873 0.7241 0.201 Uiso 0.50 1 calc PR B -5
H1M2 H 0.7778 0.6413 0.6350 0.201 Uiso 0.50 1 calc PR B -5
H1M3 H 0.8402 0.6781 0.7225 0.201 Uiso 0.50 1 calc PR B -5
O1E O 0.7579(12) 0.122(2) 0.2500 0.204(14) Uani 0.50 2 d SPD . 2
C1E C 0.7467(7) 0.1291(7) 0.1583(7) 0.177(14) Uani 0.50 1 d PD . 2
H1E1 H 0.7588 0.1814 0.1778 0.212 Uiso 0.50 1 d PR . 2
H1E2 H 0.6942 0.0995 0.1304 0.212 Uiso 0.50 1 d PR . 2
C2E C 0.8003(11) 0.1238(11) 0.0828(19) 0.227(18) Uani 0.50 1 d PD . 2
H2E1 H 0.7812 0.1225 0.0150 0.341 Uiso 0.50 1 calc PR . 2
H2E2 H 0.8025 0.0769 0.0949 0.341 Uiso 0.50 1 calc PR . 2
H2E3 H 0.8517 0.1685 0.0899 0.341 Uiso 0.50 1 calc PR . 2
O1W O 0.955(7) 0.934(6) 0.7500 0.15(4) Uiso 0.10 2 d SP . .
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'
Ce Ce -0.2486 2.6331 '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 Ce O1 120.0 2_655 .
O1 Ce O1 119.998(1) 2_655 3_665
O1 Ce O1 120.001(1) . 3_665
O1 Ce O11 72.37(6) 2_655 3_665
O1 Ce O11 135.53(5) . 3_665
O1 Ce O11 65.74(6) 3_665 3_665
O1 Ce O11 65.74(6) 2_655 2_655
O1 Ce O11 72.37(6) . 2_655
O1 Ce O11 135.53(5) 3_665 2_655
O11 Ce O11 76.68(7) 3_665 2_655
O1 Ce O11 72.37(6) 2_655 12_667
O1 Ce O11 135.53(5) . 12_667
O1 Ce O11 65.75(6) 3_665 12_667
O11 Ce O11 88.50(9) 3_665 12_667
O11 Ce O11 138.02(4) 2_655 12_667
O1 Ce O11 135.53(5) 2_655 .
O1 Ce O11 65.74(6) . .
O1 Ce O11 72.37(6) 3_665 .
O11 Ce O11 76.69(7) 3_665 .
O11 Ce O11 76.69(7) 2_655 .
O11 Ce O11 138.03(3) 12_667 .
O1 Ce O11 65.75(6) 2_655 11_657
O1 Ce O11 72.37(6) . 11_657
O1 Ce O11 135.53(5) 3_665 11_657
O11 Ce O11 138.02(4) 3_665 11_657
O11 Ce O11 88.50(9) 2_655 11_657
O11 Ce O11 76.68(7) 12_667 11_657
O11 Ce O11 138.03(4) . 11_657
O1 Ce O11 135.53(5) 2_655 10_557
O1 Ce O11 65.75(6) . 10_557
O1 Ce O11 72.37(6) 3_665 10_557
O11 Ce O11 138.02(3) 3_665 10_557
O11 Ce O11 138.03(4) 2_655 10_557
O11 Ce O11 76.68(7) 12_667 10_557
O11 Ce O11 88.49(9) . 10_557
O11 Ce O11 76.69(7) 11_657 10_557
O1 Ce Cu 99.96(5) 2_655 12_667
O1 Ce Cu 132.24(5) . 12_667
O1 Ce Cu 32.31(3) 3_665 12_667
O11 Ce Cu 78.34(5) 3_665 12_667
O11 Ce Cu 154.06(5) 2_655 12_667
O11 Ce Cu 33.85(4) 12_667 12_667
O11 Ce Cu 104.20(5) . 12_667
O11 Ce Cu 105.72(5) 11_657 12_667
O11 Ce Cu 67.48(5) 10_557 12_667
O1 Ce Cu 32.32(3) 2_655 11_657
O1 Ce Cu 99.96(5) . 11_657
O1 Ce Cu 132.24(5) 3_665 11_657
O11 Ce Cu 104.20(5) 3_665 11_657
O11 Ce Cu 78.33(5) 2_655 11_657
O11 Ce Cu 67.48(5) 12_667 11_657
O11 Ce Cu 154.06(5) . 11_657
O11 Ce Cu 33.85(4) 11_657 11_657
O11 Ce Cu 105.72(5) 10_557 11_657
Cu Ce Cu 101.303(13) 12_667 11_657
O1 Ce Cu 132.24(5) 2_655 .
O1 Ce Cu 32.32(3) . .
O1 Ce Cu 99.96(5) 3_665 .
O11 Ce Cu 105.72(5) 3_665 .
O11 Ce Cu 67.49(5) 2_655 .
O11 Ce Cu 154.06(5) 12_667 .
O11 Ce Cu 33.85(4) . .
O11 Ce Cu 104.20(5) 11_657 .
O11 Ce Cu 78.33(5) 10_557 .
Cu Ce Cu 126.965(5) 12_667 .
Cu Ce Cu 126.966(6) 11_657 .
O1 Cu O12 92.55(10) . .
O1 Cu N11 166.56(11) . .
O12 Cu N11 95.27(11) . .
O1 Cu O11 87.02(9) . .
O12 Cu O11 165.93(9) . .
N11 Cu O11 82.74(9) . .
O1 Cu O21 89.06(9) . 2_655
O12 Cu O21 105.20(9) . 2_655
N11 Cu O21 99.38(11) . 2_655
O11 Cu O21 88.86(9) . 2_655
O1 Cu Ce 43.30(7) . .
O12 Cu Ce 135.58(7) . .
N11 Cu Ce 127.09(8) . .
O11 Cu Ce 44.34(5) . .
O21 Cu Ce 82.73(6) 2_655 .
Cu O1 Cu 109.32(12) . 10_557
Cu O1 Ce 104.39(8) . .
Cu O1 Ce 104.39(8) 10_557 .
Cu O1 H1 112.7 . .
Cu O1 H1 112.7 10_557 .
Ce O1 H1 112.7 . .
C11 O11 Cu 117.92(17) . .
C11 O11 Ce 140.13(18) . .
Cu O11 Ce 101.80(8) . .
C11 O21 Cu 124.18(19) . 3_665
C21 N11 Cu 112.29(18) . .
C21 N11 H11A 109.1 . .
Cu N11 H11A 109.1 . .
C21 N11 H11B 109.1 . .
Cu N11 H11B 109.1 . .
H11A N11 H11B 107.9 . .
O21 C11 O11 125.0(3) . .
O21 C11 C21 119.8(3) . .
O11 C11 C21 115.1(3) . .
C411 C21 C31 89.9(11) . .
C411 C21 N11 112.4(8) . .
C31 C21 N11 118.2(6) . .
C411 C21 C11 111.5(7) . .
C31 C21 C11 113.9(7) . .
N11 C21 C11 109.6(3) . .
C411 C21 C311 113.7(10) . .
N11 C21 C311 103.4(6) . .
C11 C21 C311 105.7(6) . .
C31 C21 C41 106.1(8) . .
N11 C21 C41 104.9(7) . .
C11 C21 C41 102.4(5) . .
C311 C21 C41 130.0(8) . .
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 129.2(2) . .
O12 C12 O12 127.2(4) . 10_557
O12 C12 C22 116.38(19) . .
O12 C12 C22 116.38(19) 10_557 .
C12 C22 H22A 111.2 . .
C12 C22 H22C 111.8 . .
H22A C22 H22C 110.8 . .
O33 N13 O33 93.2(9) 10_557 .
O33 N13 O13 131.5(5) 10_557 .
O33 N13 O13 131.5(5) . .
O33 N13 O23 116.1(6) 10_557 .
O13 N13 O23 112.1(3) . .
O33 N13 O23 116.1(6) . 10_557
O13 N13 O23 112.1(3) . 10_557
O23 N13 O23 133.3(7) . 10_557
O33 O23 N13 55.6(13) . .
O23 O33 N13 97.7(15) . .
O23 O33 O33 133.7(16) . 10_557
C1M O1M H1M 116.2 . .
C1E O1E C1E 151(3) . 10_556
O1E C1E C2E 117.6(18) . .
O1E C1E H1E1 84.3 . .
C2E C1E H1E1 116.4 . .
O1E C1E H1E2 119.5 . .
C2E C1E H1E2 106.8 . .
H1E1 C1E H1E2 111.1 . .
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
Ce O1 2.467(2) 2_655
Ce O1 2.467(2) .
Ce O1 2.467(2) 3_665
Ce O11 2.4882(19) 3_665
Ce O11 2.4882(18) 2_655
Ce O11 2.4882(19) 12_667
Ce O11 2.4882(18) .
Ce O11 2.4882(18) 11_657
Ce O11 2.4883(19) 10_557
Ce Cu 3.4846(8) 12_667
Ce Cu 3.4846(8) 11_657
Ce Cu 3.4846(8) .
Cu O1 1.9231(15) .
Cu O12 1.959(2) .
Cu N11 1.982(3) .
Cu O11 1.983(2) .
Cu O21 2.362(2) 2_655
O1 Cu 1.9231(15) 10_557
O1 H1 1.0000 .
O11 C11 1.292(3) .
O21 C11 1.232(4) .
O21 Cu 2.362(2) 3_665
N11 C21 1.494(5) .
N11 H11A 0.9200 .
N11 H11B 0.9200 .
C11 C21 1.541(4) .
C21 C411 1.340(13) .
C21 C31 1.437(14) .
C21 C311 1.682(15) .
C21 C41 1.748(11) .
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 1.261(3) .
C12 O12 1.261(3) 10_557
C12 C22 1.514(6) .
C22 H22A 0.8868 .
C22 H22C 0.9730 .
O13 N13 1.240(4) .
N13 O33 1.136(10) 10_557
N13 O33 1.136(10) .
N13 O23 1.365(8) .
N13 O23 1.365(8) 10_557
O23 O33 0.619(9) .
O33 O33 1.651(19) 10_557
O1M C1M 1.56(2) .
O1M H1M 0.8744 .
C1M H1M1 0.9800 .
C1M H1M2 0.9800 .
C1M H1M3 0.9800 .
O1E C1E 1.267(10) .
O1E C1E 1.267(10) 10_556
C1E C2E 1.519(17) .
C1E H1E1 0.9900 .
C1E H1E2 0.9900 .
C2E H2E1 0.9800 .
C2E H2E2 0.9800 .
C2E H2E3 0.9800 .
