#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/92/4329275.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_4329275
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 N9 O30 Tb, 1.5(C H4 O), 1.5 (H2 O)'
_chemical_formula_sum            'C31.5 H69 Cu6 N9 O33 Tb'
_chemical_formula_weight         1642.12
_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                   20.013(9)
_cell_length_b                   20.013(9)
_cell_length_c                   13.260(3)
_cell_measurement_reflns_used    5373
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      36.52
_cell_measurement_theta_min      3.1
_cell_volume                     4599(3)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.598
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.1415
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18505
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         36.60
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    2.180
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.456
_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    1.186
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.22
_refine_diff_density_min         -2.08
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         4691
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1913
_refine_ls_R_factor_gt           0.0980
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0967P)²+24.2268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2454
_reflns_number_gt                2507
_reflns_number_total             4691
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300538q_si_001_07.cif
_cod_data_source_block           gis736ra
_cod_original_formula_sum        'C31.50 H69 Cu6 N9 O33 Tb'
_cod_database_code               4329275
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
Tb Tb 0.6667 0.3333 0.7500 0.0280(3) Uani 1 6 d S . .
Cu Cu 0.83199(6) 0.46967(7) 0.86695(7) 0.0404(3) Uani 1 1 d . . .
O1 O 0.7726(5) 0.4629(5) 0.7500 0.038(2) Uani 1 2 d S . .
H1 H 0.7556 0.5022 0.7500 0.045 Uiso 1 2 calc SR . .
O11 O 0.7627(3) 0.3572(4) 0.8787(4) 0.0366(14) Uani 1 1 d . . .
O21 O 0.7400(4) 0.2519(4) 0.9635(5) 0.060(2) Uani 1 1 d . . .
N11 N 0.8897(5) 0.4531(5) 0.9742(5) 0.052(2) Uani 1 1 d . . .
H11A H 0.9350 0.4591 0.9481 0.062 Uiso 1 1 calc R . .
H11B H 0.9021 0.4897 1.0236 0.062 Uiso 1 1 calc R . .
C11 C 0.7779(6) 0.3206(7) 0.9479(6) 0.049(2) Uani 1 1 d . . .
C21 C 0.8448(7) 0.3746(7) 1.0203(8) 0.068(3) Uani 1 1 d . . .
C31 C 0.8967(9) 0.3388(9) 1.0355(15) 0.135(8) Uani 1 1 d . . .
H31A H 0.9377 0.3700 1.0837 0.203 Uiso 1 1 calc R . .
H31B H 0.9196 0.3373 0.9708 0.203 Uiso 1 1 calc R . .
H31C H 0.8656 0.2862 1.0617 0.203 Uiso 1 1 calc R . .
C41 C 0.8059(9) 0.3795(10) 1.1175(7) 0.121(7) Uani 1 1 d . . .
H41A H 0.7789 0.3286 1.1496 0.181 Uiso 1 1 calc R . .
H41B H 0.7688 0.3963 1.1013 0.181 Uiso 1 1 calc R . .
H41C H 0.8451 0.4166 1.1637 0.181 Uiso 1 1 calc RD . .
O12 O 0.9128(4) 0.5735(4) 0.8348(5) 0.0552(18) Uani 1 1 d . . .
C12 C 0.9361(8) 0.6066(9) 0.7500 0.052(4) Uani 1 2 d S . .
C22 C 0.9959(11) 0.6903(9) 0.7500 0.074(5) Uani 1 2 d S . .
H22A H 0.9893 0.7146 0.8010 0.111 Uiso 1 1 d R . .
H22C H 1.0477 0.6980 0.7500 0.111 Uiso 1 2 d SR . .
O13 O 0.9099(5) 0.4177(6) 0.7500 0.057(3) Uani 1 2 d S . .
N13 N 0.9819(8) 0.4542(8) 0.7500 0.060(3) Uani 1 2 d S . .
O23 O 1.0164(6) 0.4714(7) 0.8300(8) 0.120(4) Uani 1 1 d . . .
O1W O 0.7425(9) 0.5786(10) 0.7714(15) 0.077(7) Uani 0.25 1 d P A -1
O1M O 0.7425(9) 0.5786(10) 0.7714(15) 0.077(7) Uani 0.25 1 d PD B -1
H1M H 0.6983 0.5532 0.7969 0.116 Uiso 0.25 1 calc PR B -1
C1M C 0.772(4) 0.6566(18) 0.791(6) 0.15(3) Uiso 0.25 1 d PD B -1
H1M1 H 0.8272 0.6811 0.8048 0.222 Uiso 0.25 1 calc PR B -1
H1M2 H 0.7453 0.6628 0.8489 0.222 Uiso 0.25 1 calc PR B -1
H1M3 H 0.7637 0.6811 0.7314 0.222 Uiso 0.25 1 calc PR B -1
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'
Tb Tb -0.1723 4.1537 '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 Tb O1 120.000(1) . 2_655
O1 Tb O1 120.000(2) . 3_665
O1 Tb O1 120.000(2) 2_655 3_665
O1 Tb O11 66.5(2) . .
O1 Tb O11 135.31(13) 2_655 .
O1 Tb O11 71.8(2) 3_665 .
O1 Tb O11 135.31(14) . 12_667
O1 Tb O11 71.8(2) 2_655 12_667
O1 Tb O11 66.5(2) 3_665 12_667
O11 Tb O11 138.25(10) . 12_667
O1 Tb O11 71.8(2) . 2_655
O1 Tb O11 66.5(2) 2_655 2_655
O1 Tb O11 135.31(13) 3_665 2_655
O11 Tb O11 76.2(2) . 2_655
O11 Tb O11 138.25(10) 12_667 2_655
O1 Tb O11 71.8(2) . 11_657
O1 Tb O11 66.5(2) 2_655 11_657
O1 Tb O11 135.31(13) 3_665 11_657
O11 Tb O11 138.25(10) . 11_657
O11 Tb O11 76.2(2) 12_667 11_657
O11 Tb O11 89.1(3) 2_655 11_657
O1 Tb O11 135.31(14) . 3_665
O1 Tb O11 71.8(2) 2_655 3_665
O1 Tb O11 66.5(2) 3_665 3_665
O11 Tb O11 76.2(2) . 3_665
O11 Tb O11 89.1(3) 12_667 3_665
O11 Tb O11 76.2(2) 2_655 3_665
O11 Tb O11 138.25(10) 11_657 3_665
O1 Tb O11 66.5(2) . 10_557
O1 Tb O11 135.31(13) 2_655 10_557
O1 Tb O11 71.8(2) 3_665 10_557
O11 Tb O11 89.1(3) . 10_557
O11 Tb O11 76.2(2) 12_667 10_557
O11 Tb O11 138.25(10) 2_655 10_557
O11 Tb O11 76.2(2) 11_657 10_557
O11 Tb O11 138.25(10) 3_665 10_557
O1 Tb Cu 32.68(12) . .
O1 Tb Cu 132.58(17) 2_655 .
O1 Tb Cu 99.50(19) 3_665 .
O11 Tb Cu 34.24(15) . .
O11 Tb Cu 154.29(14) 12_667 .
O11 Tb Cu 66.95(15) 2_655 .
O11 Tb Cu 104.05(14) 11_657 .
O11 Tb Cu 105.47(14) 3_665 .
O11 Tb Cu 78.91(14) 10_557 .
O1 Tb Cu 132.58(17) . 12_667
O1 Tb Cu 99.50(19) 2_655 12_667
O1 Tb Cu 32.68(12) 3_665 12_667
O11 Tb Cu 104.05(14) . 12_667
O11 Tb Cu 34.24(14) 12_667 12_667
O11 Tb Cu 154.29(14) 2_655 12_667
O11 Tb Cu 105.47(14) 11_657 12_667
O11 Tb Cu 78.91(14) 3_665 12_667
O11 Tb Cu 66.95(15) 10_557 12_667
Cu Tb Cu 127.026(10) . 12_667
O1 Tb Cu 99.50(19) . 11_657
O1 Tb Cu 32.68(12) 2_655 11_657
O1 Tb Cu 132.58(17) 3_665 11_657
O11 Tb Cu 154.30(14) . 11_657
O11 Tb Cu 66.95(15) 12_667 11_657
O11 Tb Cu 78.91(14) 2_655 11_657
O11 Tb Cu 34.24(15) 11_657 11_657
O11 Tb Cu 104.05(14) 3_665 11_657
O11 Tb Cu 105.47(14) 10_557 11_657
Cu Tb Cu 127.025(11) . 11_657
Cu Tb Cu 101.16(3) 12_667 11_657
O1 Cu O12 93.1(3) . .
O1 Cu N11 166.2(4) . .
O12 Cu N11 95.4(3) . .
O1 Cu O11 85.8(3) . .
O12 Cu O11 167.0(3) . .
N11 Cu O11 83.5(3) . .
O1 Cu O21 89.1(3) . 2_655
O12 Cu O21 103.7(3) . 2_655
N11 Cu O21 99.4(3) . 2_655
O11 Cu O21 89.2(3) . 2_655
O1 Cu Tb 42.3(2) . .
O12 Cu Tb 135.2(2) . .
N11 Cu Tb 127.4(2) . .
O11 Cu Tb 43.96(15) . .
O21 Cu Tb 83.52(18) 2_655 .
Cu O1 Cu 107.9(4) . 10_557
Cu O1 Tb 105.0(3) . .
Cu O1 Tb 105.0(3) 10_557 .
Cu O1 H1 112.8 . .
Cu O1 H1 112.8 10_557 .
Tb O1 H1 112.8 . .
C11 O11 Cu 118.0(6) . .
C11 O11 Tb 140.1(6) . .
Cu O11 Tb 101.8(2) . .
C11 O21 Cu 124.1(6) . 3_665
C21 N11 Cu 112.3(6) . .
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 124.8(9) . .
O21 C11 C21 120.9(8) . .
O11 C11 C21 113.9(9) . .
N11 C21 C41 109.5(11) . .
N11 C21 C31 110.6(11) . .
C41 C21 C31 113.6(12) . .
N11 C21 C11 109.4(8) . .
C41 C21 C11 105.9(10) . .
C31 C21 C11 107.6(10) . .
C21 C31 H31A 109.5 . .
C21 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C21 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C21 C41 H41A 109.5 . .
C21 C41 H41B 109.5 . .
H41A C41 H41B 109.5 . .
C21 C41 H41C 109.5 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C12 O12 Cu 130.3(8) . .
O12 C12 O12 124.6(14) . 10_557
O12 C12 C22 117.7(7) . .
O12 C12 C22 117.7(7) 10_557 .
C12 C22 H22A 111.1 . .
C12 C22 H22C 112.0 . .
H22A C22 H22C 110.9 . .
O23 N13 O23 121.2(17) 10_557 .
O23 N13 O13 119.4(8) 10_557 .
O23 N13 O13 119.4(8) . .
H1M1 C1M H1M2 109.5 . .
H1M1 C1M H1M3 109.5 . .
H1M2 C1M H1M3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb O1 2.392(8) .
Tb O1 2.392(8) 2_655
Tb O1 2.392(8) 3_665
Tb O11 2.433(5) .
Tb O11 2.433(5) 12_667
Tb O11 2.433(5) 2_655
Tb O11 2.433(5) 11_657
Tb O11 2.433(5) 3_665
Tb O11 2.433(5) 10_557
Tb Cu 3.4306(16) .
Tb Cu 3.4306(16) 12_667
Tb Cu 3.4306(16) 11_657
Cu O1 1.918(5) .
Cu O12 1.938(7) .
Cu N11 1.962(7) .
Cu O11 1.972(6) .
Cu O21 2.284(7) 2_655
O1 Cu 1.918(5) 10_557
O1 H1 1.0000 .
O11 C11 1.300(11) .
O21 C11 1.211(12) .
O21 Cu 2.284(7) 3_665
N11 C21 1.494(14) .
N11 H11A 0.9200 .
N11 H11B 0.9200 .
C11 C21 1.562(13) .
C21 C41 1.534(18) .
C21 C31 1.542(19) .
C31 H31A 0.9800 .
C31 H31B 0.9800 .
C31 H31C 0.9800 .
C41 H41A 0.9800 .
C41 H41B 0.9800 .
C41 H41C 0.9800 .
O12 C12 1.269(10) .
C12 O12 1.269(10) 10_557
C12 C22 1.49(2) .
C22 H22A 0.8805 .
C22 H22C 0.9672 .
O13 N13 1.248(15) .
N13 O23 1.218(11) 10_557
N13 O23 1.218(11) .
C1M H1M1 0.9800 .
C1M H1M2 0.9800 .
C1M H1M3 0.9800 .
