#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/99/4109900.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_4109900
loop_
_publ_author_name
'Joseph P. Leonard'
'Paul Jensen'
'Thomas McCabe'
'John E. O'Brien'
'Robert D. Peacock'
'Paul E. Kruger'
'Thorfinnur Gunnlaugsson'
_publ_section_title
;
 Self-Assembly of Chiral Luminescent Lanthanide Coordination Bundles
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10986
_journal_page_last               10987
_journal_paper_doi               10.1021/ja073049e
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         '[Tb({R,R}L)3](CF3SO3)3.(12.5MeOH)'
_chemical_formula_sum            'C108.5 H131 F9 N9 O27.5 S3 Tb'
_chemical_formula_weight         2427.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           182
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_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                   22.9408(7)
_cell_length_b                   22.9408(7)
_cell_length_c                   12.9980(8)
_cell_measurement_temperature    298(2)
_cell_volume                     5924.1(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'omega 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  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            46302
_diffrn_reflns_theta_full        22.52
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       needle
_exptl_crystal_F_000             2518
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2609
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0339
_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)+(0.0636P)²+0.1959P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                2523
_reflns_number_total             2609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073049esi20070515_024822_3.cif
_cod_data_source_block           Tb.2
_cod_original_formula_sum        'C108.50 H131 F9 N9 O27.50 S3 Tb'
_cod_database_code               4109900
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'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -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
Tb1 Tb 0.3333 0.6667 0.2500 0.05211(16) Uani 1 6 d SU
N1 N 0.26963(8) 0.53927(16) 0.2500 0.0579(8) Uani 1 2 d SU
N2 N 0.3702(2) 0.5284(2) 0.0527(3) 0.0874(10) Uani 1 1 d U
H2N H 0.3529 0.4855 0.0475 0.105 Uiso 1 1 calc R
O1 O 0.36782(14) 0.61321(14) 0.12718(18) 0.0684(7) Uani 1 1 d U
C1 C 0.20131(12) 0.4026(2) 0.2500 0.0947(16) Uani 1 2 d SU
H1 H 0.1779 0.3558 0.2500 0.114 Uiso 1 2 calc SR
C2 C 0.2544(2) 0.4373(2) 0.1831(3) 0.0800(11) Uani 1 1 d U
H2 H 0.2677 0.4146 0.1381 0.096 Uiso 1 1 calc R
C3 C 0.28704(18) 0.50599(18) 0.1848(3) 0.0616(9) Uani 1 1 d U
C4 C 0.3449(2) 0.5523(2) 0.1187(3) 0.0667(9) Uani 1 1 d U
C5 C 0.4271(3) 0.5723(3) -0.0129(3) 0.1007(11) Uani 1 1 d DU
H5 H 0.4188 0.6081 -0.0366 0.121 Uiso 1 1 calc R
C6 C 0.4271(4) 0.5335(4) -0.1104(4) 0.139(3) Uani 1 1 d U
H6A H 0.3860 0.5188 -0.1478 0.208 Uiso 1 1 calc R
H6B H 0.4306 0.4950 -0.0906 0.208 Uiso 1 1 calc R
H6C H 0.4646 0.5624 -0.1532 0.208 Uiso 1 1 calc R
C7 C 0.49344(15) 0.60673(16) 0.0425(3) 0.1016(14) Uani 1 1 d GDU
C8 C 0.50165(19) 0.57009(16) 0.1207(3) 0.1126(15) Uani 1 1 d GDU
H8 H 0.4658 0.5285 0.1399 0.135 Uiso 1 1 calc R
C9 C 0.5634(2) 0.5957(2) 0.1701(3) 0.143(2) Uani 1 1 d GU
H9 H 0.5689 0.5712 0.2224 0.172 Uiso 1 1 calc R
C10 C 0.61691(18) 0.6579(2) 0.1414(3) 0.169(3) Uani 1 1 d GU
H10 H 0.6582 0.6750 0.1745 0.202 Uiso 1 1 calc R
C11 C 0.60871(16) 0.69455(17) 0.0633(3) 0.166(3) Uani 1 1 d GU
C12 C 0.54697(18) 0.66897(15) 0.0138(2) 0.1290(19) Uani 1 1 d GDU
C13 C 0.5388(3) 0.7056(2) -0.0643(3) 0.183(3) Uani 1 1 d GU
H13 H 0.4974 0.6885 -0.0974 0.220 Uiso 1 1 calc R
C14 C 0.5923(4) 0.7678(2) -0.0930(4) 0.256(6) Uani 1 1 d GU
H14 H 0.5868 0.7924 -0.1453 0.308 Uiso 1 1 calc R
C15 C 0.6540(3) 0.79342(18) -0.0436(5) 0.308(8) Uani 1 1 d GU
H15 H 0.6898 0.8351 -0.0628 0.369 Uiso 1 1 calc R
C16 C 0.6622(2) 0.7568(2) 0.0346(4) 0.250(5) Uani 1 1 d GU
H16 H 0.7035 0.7739 0.0676 0.300 Uiso 1 1 calc R
S1 S 0.3363(3) 0.3426(2) -0.0150(8) 0.161(2) Uani 0.50 1 d PDU
O2 O 0.3586(5) 0.3985(4) 0.0536(10) 0.189(6) Uani 0.50 1 d PDU
O3 O 0.3857(4) 0.3234(5) -0.0347(11) 0.172(6) Uani 0.50 1 d PDU
O4 O 0.2970(7) 0.3415(7) -0.1010(9) 0.347(12) Uani 0.50 1 d PDU
C17 C 0.2750(5) 0.2731(4) 0.0626(10) 0.238(7) Uani 0.50 1 d PDU
F1 F 0.2272(6) 0.2820(6) 0.0981(14) 0.358(12) Uani 0.50 1 d PDU
F2 F 0.2466(5) 0.2165(4) 0.0124(16) 0.320(10) Uani 0.50 1 d PDU
F3 F 0.3029(9) 0.2627(9) 0.1440(12) 0.373(10) Uani 0.50 1 d PDU
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 Tb1 O1 126.92(14) 12_565 3_565
O1 Tb1 O1 85.37(12) 12_565 2_665
O1 Tb1 O1 79.81(9) 3_565 2_665
O1 Tb1 O1 79.81(9) 12_565 11
O1 Tb1 O1 85.37(12) 3_565 11
O1 Tb1 O1 146.49(14) 2_665 11
O1 Tb1 O1 79.81(9) 12_565 10_665
O1 Tb1 O1 146.49(14) 3_565 10_665
O1 Tb1 O1 126.92(14) 2_665 10_665
O1 Tb1 O1 79.81(9) 11 10_665
O1 Tb1 O1 146.49(14) 12_565 .
O1 Tb1 O1 79.81(9) 3_565 .
O1 Tb1 O1 79.81(9) 2_665 .
O1 Tb1 O1 126.92(14) 11 .
O1 Tb1 O1 85.37(12) 10_665 .
O1 Tb1 N1 63.46(7) 12_565 3_565
O1 Tb1 N1 63.46(7) 3_565 3_565
O1 Tb1 N1 73.25(7) 2_665 3_565
O1 Tb1 N1 73.25(7) 11 3_565
O1 Tb1 N1 137.32(6) 10_665 3_565
O1 Tb1 N1 137.32(6) . 3_565
O1 Tb1 N1 137.32(6) 12_565 .
O1 Tb1 N1 73.25(7) 3_565 .
O1 Tb1 N1 137.32(6) 2_665 .
O1 Tb1 N1 63.46(7) 11 .
O1 Tb1 N1 73.25(7) 10_665 .
O1 Tb1 N1 63.46(7) . .
N1 Tb1 N1 120.0 3_565 .
O1 Tb1 N1 73.25(7) 12_565 2_665
O1 Tb1 N1 137.32(6) 3_565 2_665
O1 Tb1 N1 63.46(7) 2_665 2_665
O1 Tb1 N1 137.32(6) 11 2_665
O1 Tb1 N1 63.46(7) 10_665 2_665
O1 Tb1 N1 73.25(7) . 2_665
N1 Tb1 N1 120.0 3_565 2_665
N1 Tb1 N1 120.0 . 2_665
C3 N1 C3 120.3(4) . 11
C3 N1 Tb1 119.8(2) . .
C3 N1 Tb1 119.8(2) 11 .
C4 N2 C5 121.9(4) . .
C4 O1 Tb1 125.8(2) . .
C2 C1 C2 120.0(5) 11 .
C3 C2 C1 118.2(4) . .
N1 C3 C2 121.7(4) . .
N1 C3 C4 112.1(3) . .
C2 C3 C4 126.3(3) . .
O1 C4 N2 120.8(4) . .
O1 C4 C3 118.7(3) . .
N2 C4 C3 120.5(4) . .
N2 C5 C7 113.8(3) . .
N2 C5 C6 109.7(5) . .
C7 C5 C6 113.8(4) . .
C8 C7 C12 120.0 . .
C8 C7 C5 116.1(3) . .
C12 C7 C5 123.6(3) . .
C7 C8 C9 120.0 . .
C8 C9 C10 120.0 . .
C11 C10 C9 120.0 . .
C12 C11 C10 120.0 . .
C12 C11 C16 120.0 . .
C10 C11 C16 120.0 . .
C13 C12 C11 120.0 . .
C13 C12 C7 120.0 . .
C11 C12 C7 120.0 . .
C12 C13 C14 120.0 . .
C13 C14 C15 120.0 . .
C16 C15 C14 120.0 . .
C15 C16 C11 120.0 . .
S1 S1 O3 92(2) 7 7
S1 S1 O2 87.0(15) 7 7
O3 S1 O2 124.3(6) 7 7
S1 S1 O2 74.2(15) 7 .
O3 S1 O2 31.3(6) 7 .
O2 S1 O2 97.4(9) 7 .
S1 S1 O3 68.7(18) 7 .
O3 S1 O3 145.1(8) 7 .
O2 S1 O3 30.9(7) 7 .
O2 S1 O3 113.9(4) . .
S1 S1 O4 161.0(6) 7 .
O3 S1 O4 91.1(9) 7 .
O2 S1 O4 106.2(11) 7 .
O2 S1 O4 116.3(5) . .
O3 S1 O4 116.4(5) . .
S1 S1 C17 107.0(8) 7 7
O3 S1 C17 117.9(9) 7 7
O2 S1 C17 115.3(9) 7 7
O2 S1 C17 147.3(9) . 7
O3 S1 C17 96.0(7) . 7
O4 S1 C17 55.3(10) . 7
S1 S1 C17 58.9(6) 7 .
O3 S1 C17 91.2(7) 7 .
O2 S1 C17 132.9(8) 7 .
O2 S1 C17 102.4(4) . .
O3 S1 C17 102.4(4) . .
O4 S1 C17 102.4(4) . .
C17 S1 C17 56.2(9) 7 .
S1 S1 O4 14.4(5) 7 7
O3 S1 O4 97.2(11) 7 7
O2 S1 O4 95.5(9) 7 7
O2 S1 O4 84.5(6) . 7
O3 S1 O4 72.0(6) . 7
O4 S1 O4 146.8(10) . 7
C17 S1 O4 92.9(5) 7 7
C17 S1 O4 45.6(8) . 7
O3 O2 S1 78.4(8) 7 7
O3 O2 S1 67.3(11) 7 .
S1 O2 S1 18.8(8) 7 .
O2 O3 S1 81.4(11) 7 7
O2 O3 S1 70.7(10) 7 .
S1 O3 S1 18.8(8) 7 .
F3 O4 C17 62.8(11) 7 7
F3 O4 S1 131.1(17) 7 .
C17 O4 S1 69.3(8) 7 .
F3 O4 S1 127.3(17) 7 7
C17 O4 S1 65.1(8) 7 7
S1 O4 S1 4.6(2) . 7
F1 C17 F2 107.1(8) . .
F1 C17 F3 105.6(9) . .
F2 C17 F3 105.6(8) . .
F1 C17 O4 129.8(14) . 7
F2 C17 O4 117.8(12) . 7
F3 C17 O4 42.9(10) . 7
F1 C17 F2 69.1(10) . 7
F2 C17 F2 51.4(10) . 7
F3 C17 F2 148.7(12) . 7
O4 C17 F2 159.9(15) 7 7
F1 C17 S1 119.9(10) . 7
F2 C17 S1 118.6(10) . 7
F3 C17 S1 97.7(10) . 7
O4 C17 S1 55.4(4) 7 7
F2 C17 S1 111.7(13) 7 7
F1 C17 C17 108.3(11) . 7
F2 C17 C17 61.2(9) . 7
F3 C17 C17 146.0(12) . 7
O4 C17 C17 112.2(10) 7 7
F2 C17 C17 48.6(8) 7 7
S1 C17 C17 67.8(7) 7 7
F1 C17 S1 113.8(7) . .
F2 C17 S1 112.3(8) . .
F3 C17 S1 111.8(8) . .
O4 C17 S1 69.3(8) 7 .
F2 C17 S1 97.9(10) 7 .
S1 C17 S1 14.1(6) 7 .
C17 C17 S1 56.0(4) 7 .
C17 F1 F2 62.0(7) . 7
F2 F2 C17 73.4(10) 7 .
F2 F2 C17 55.1(12) 7 7
C17 F2 C17 70.1(9) . 7
F2 F2 F1 94(2) 7 7
C17 F2 F1 109.4(9) . 7
C17 F2 F1 48.9(9) 7 7
O4 F3 C17 74.4(12) 7 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Tb1 O1 2.377(2) 12_565
Tb1 O1 2.377(2) 3_565
Tb1 O1 2.377(2) 2_665
Tb1 O1 2.377(2) 11
Tb1 O1 2.377(2) 10_665
Tb1 O1 2.377(2) .
Tb1 N1 2.531(3) 3_565
Tb1 N1 2.531(3) .
Tb1 N1 2.531(3) 2_665
N1 C3 1.329(4) .
N1 C3 1.329(4) 11
N2 C4 1.300(5) .
N2 C5 1.460(7) .
O1 C4 1.228(4) .
C1 C2 1.380(5) 11
C1 C2 1.380(5) .
C2 C3 1.365(5) .
C3 C4 1.490(5) .
C5 C7 1.502(7) .
C5 C6 1.549(7) .
C7 C8 1.3900 .
C7 C12 1.3900 .
C8 C9 1.3900 .
C9 C10 1.3900 .
C10 C11 1.3900 .
C11 C12 1.3900 .
C11 C16 1.3900 .
C12 C13 1.3900 .
C13 C14 1.3900 .
C14 C15 1.3900 .
C15 C16 1.3900 .
S1 S1 0.46(2) 7
S1 O3 1.333(14) 7
S1 O2 1.377(12) 7
S1 O2 1.4294(10) .
S1 O3 1.4295(10) .
S1 O4 1.4296(10) .
S1 C17 1.625(9) 7
S1 C17 1.815(7) .
S1 O4 1.872(19) 7
O2 O3 0.750(15) 7
O2 S1 1.377(12) 7
O3 O2 0.750(15) 7
O3 S1 1.333(14) 7
O4 F3 1.01(2) 7
O4 C17 1.43(2) 7
O4 S1 1.872(19) 7
C17 F1 1.296(9) .
C17 F2 1.300(9) .
C17 F3 1.319(9) .
C17 O4 1.43(2) 7
C17 F2 1.52(2) 7
C17 S1 1.625(9) 7
C17 C17 1.63(3) 7
F1 F2 1.61(3) 7
F2 F2 1.24(3) 7
F2 C17 1.52(2) 7
F2 F1 1.61(3) 7
F3 O4 1.01(2) 7
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 -0.011 1175.2 440.1
2 0.667 0.333 0.250 174.0 3.8
3 0.333 0.667 0.750 174.0 5.3
