#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/99/4109902.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_4109902
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         '[Sm({R,R}L)3](CF3SO3)3.(13.5MeOH)'
_chemical_formula_sum            'C109.5 H135 F9 N9 O28.5 S3 Sm'
_chemical_formula_weight         2450.79
_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                   22.8459(6)
_cell_length_b                   22.8459(6)
_cell_length_c                   12.8911(4)
_cell_measurement_temperature    153(2)
_cell_volume                     5826.9(3)
_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      153(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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0207
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            35198
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       prism
_exptl_crystal_F_000             2548
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.777
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         1826
_refine_ls_number_restraints     259
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0551
_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)+(0.0807P)²+8.5129P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1382
_reflns_number_gt                1786
_reflns_number_total             1826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073049esi20070515_024822_5.cif
_cod_data_source_block           Sm.2
_cod_original_formula_sum        'C109.50 H135 F9 N9 O28.50 S3 Sm'
_cod_database_code               4109902
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
Sm1 Sm 0.3333 0.6667 0.2500 0.0397(4) Uani 1 6 d SU
N1 N 0.26848(17) 0.5370(3) 0.2500 0.0462(18) Uani 1 2 d SU
N2 N 0.3705(4) 0.5262(4) 0.0496(5) 0.073(2) Uani 1 1 d U
H2N H 0.3531 0.4822 0.0437 0.088 Uiso 1 1 calc R
O1 O 0.3662(3) 0.6095(3) 0.1246(4) 0.0544(16) Uani 1 1 d U
C1 C 0.2000(3) 0.4001(5) 0.2500 0.086(4) Uani 1 2 d SU
H1 H 0.1760 0.3521 0.2500 0.103 Uiso 1 2 calc SR
C2 C 0.2535(4) 0.4351(4) 0.1808(7) 0.065(2) Uani 1 1 d U
H2 H 0.2666 0.4121 0.1332 0.078 Uiso 1 1 calc R
C3 C 0.2854(4) 0.5030(4) 0.1844(6) 0.0476(18) Uani 1 1 d U
C4 C 0.3440(5) 0.5488(5) 0.1172(6) 0.060(2) Uani 1 1 d U
C5 C 0.4269(8) 0.5698(7) -0.0162(6) 0.094(2) Uani 1 1 d DU
H5 H 0.4179 0.6057 -0.0424 0.113 Uiso 1 1 calc R
C6 C 0.4250(7) 0.5277(7) -0.1119(8) 0.119(5) Uani 1 1 d U
H6A H 0.3796 0.5054 -0.1422 0.178 Uiso 1 1 calc R
H6B H 0.4365 0.4935 -0.0905 0.178 Uiso 1 1 calc R
H6C H 0.4578 0.5577 -0.1636 0.178 Uiso 1 1 calc R
C7 C 0.4940(3) 0.6060(3) 0.0416(5) 0.084(3) Uani 1 1 d GDU
C8 C 0.5024(3) 0.5694(3) 0.1206(5) 0.085(3) Uani 1 1 d GDU
H8 H 0.4659 0.5264 0.1400 0.102 Uiso 1 1 calc R
C9 C 0.5642(4) 0.5956(4) 0.1712(5) 0.115(4) Uani 1 1 d GU
H9 H 0.5699 0.5706 0.2252 0.138 Uiso 1 1 calc R
C10 C 0.6176(3) 0.6585(4) 0.1429(5) 0.135(4) Uani 1 1 d GU
H10 H 0.6599 0.6764 0.1775 0.162 Uiso 1 1 calc R
C11 C 0.6093(3) 0.6951(3) 0.0639(5) 0.133(4) Uani 1 1 d GU
C12 C 0.5475(3) 0.6688(3) 0.0133(4) 0.113(3) Uani 1 1 d GDU
C13 C 0.5391(5) 0.7054(4) -0.0657(5) 0.155(5) Uani 1 1 d GU
H13 H 0.4969 0.6875 -0.1003 0.186 Uiso 1 1 calc R
C14 C 0.5925(6) 0.7682(4) -0.0941(6) 0.217(8) Uani 1 1 d GU
H14 H 0.5868 0.7932 -0.1481 0.261 Uiso 1 1 calc R
C15 C 0.6543(5) 0.7945(3) -0.0435(7) 0.253(10) Uani 1 1 d GU
H15 H 0.6908 0.8374 -0.0628 0.303 Uiso 1 1 calc R
C16 C 0.6627(4) 0.7579(3) 0.0355(7) 0.204(7) Uani 1 1 d GU
H16 H 0.7049 0.7758 0.0701 0.245 Uiso 1 1 calc R
S1 S 0.3312(3) 0.3363(4) -0.0043(11) 0.126(2) Uani 0.50 1 d PDU
O2 O 0.3578(7) 0.3960(5) 0.0580(15) 0.146(8) Uani 0.50 1 d PDU
O3 O 0.3790(6) 0.3158(7) -0.0310(16) 0.138(8) Uani 0.50 1 d PDU
O4 O 0.2882(8) 0.3331(10) -0.0874(13) 0.253(12) Uani 0.50 1 d PDU
C17 C 0.2743(7) 0.2709(6) 0.0823(12) 0.184(9) Uani 0.50 1 d PDU
F1 F 0.2265(8) 0.2811(8) 0.1195(18) 0.262(13) Uani 0.50 1 d PDU
F2 F 0.2429(8) 0.2106(5) 0.0397(18) 0.239(11) Uani 0.50 1 d PDU
F3 F 0.3051(11) 0.2648(10) 0.1650(14) 0.267(11) 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'
Sm Sm -0.1638 3.4418 '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 Sm1 O1 124.3(3) 3_565 12_565
O1 Sm1 O1 80.28(18) 3_565 2_665
O1 Sm1 O1 85.3(2) 12_565 2_665
O1 Sm1 O1 85.3(2) 3_565 11
O1 Sm1 O1 80.28(18) 12_565 11
O1 Sm1 O1 148.8(3) 2_665 11
O1 Sm1 O1 148.8(3) 3_565 10_665
O1 Sm1 O1 80.28(18) 12_565 10_665
O1 Sm1 O1 124.3(3) 2_665 10_665
O1 Sm1 O1 80.28(18) 11 10_665
O1 Sm1 O1 80.28(18) 3_565 .
O1 Sm1 O1 148.8(3) 12_565 .
O1 Sm1 O1 80.28(18) 2_665 .
O1 Sm1 O1 124.3(3) 11 .
O1 Sm1 O1 85.3(2) 10_665 .
O1 Sm1 N1 62.17(13) 3_565 3_565
O1 Sm1 N1 62.17(13) 12_565 3_565
O1 Sm1 N1 74.42(13) 2_665 3_565
O1 Sm1 N1 74.42(13) 11 3_565
O1 Sm1 N1 137.35(12) 10_665 3_565
O1 Sm1 N1 137.35(12) . 3_565
O1 Sm1 N1 137.35(12) 3_565 2_665
O1 Sm1 N1 74.42(13) 12_565 2_665
O1 Sm1 N1 62.17(13) 2_665 2_665
O1 Sm1 N1 137.35(12) 11 2_665
O1 Sm1 N1 62.17(13) 10_665 2_665
O1 Sm1 N1 74.42(13) . 2_665
N1 Sm1 N1 120.000(1) 3_565 2_665
O1 Sm1 N1 74.42(13) 3_565 .
O1 Sm1 N1 137.35(12) 12_565 .
O1 Sm1 N1 137.35(12) 2_665 .
O1 Sm1 N1 62.17(13) 11 .
O1 Sm1 N1 74.42(13) 10_665 .
O1 Sm1 N1 62.17(13) . .
N1 Sm1 N1 120.000(1) 3_565 .
N1 Sm1 N1 120.000(1) 2_665 .
C3 N1 C3 119.3(8) . 11
C3 N1 Sm1 120.4(4) . .
C3 N1 Sm1 120.4(4) 11 .
C4 N2 C5 123.3(8) . .
C4 O1 Sm1 126.9(5) . .
C2 C1 C2 120.5(10) . 11
C3 C2 C1 117.0(8) . .
N1 C3 C2 123.1(8) . .
N1 C3 C4 112.3(7) . .
C2 C3 C4 124.5(8) . .
O1 C4 N2 119.4(8) . .
O1 C4 C3 117.9(7) . .
N2 C4 C3 122.7(8) . .
N2 C5 C7 113.4(6) . .
N2 C5 C6 107.5(11) . .
C7 C5 C6 115.7(8) . .
C8 C7 C12 120.0 . .
C8 C7 C5 115.8(6) . .
C12 C7 C5 123.9(6) . .
C9 C8 C7 120.0 . .
C10 C9 C8 120.0 . .
C9 C10 C11 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 128(7) 7 7
S1 S1 O2 98(5) 7 .
O3 S1 O2 38.6(9) 7 .
S1 S1 O3 44(6) 7 .
O3 S1 O3 152.2(10) 7 .
O2 S1 O3 114.6(5) . .
S1 S1 O4 147(5) 7 .
O3 S1 O4 82.1(12) 7 .
O2 S1 O4 115.1(5) . .
O3 S1 O4 114.9(5) . .
S1 S1 O2 73(4) 7 7
O3 S1 O2 121.8(8) 7 7
O2 S1 O2 93.9(13) . 7
O3 S1 O2 36.2(9) . 7
O4 S1 O2 102.4(14) . 7
S1 S1 O4 28(4) 7 7
O3 S1 O4 111.6(18) 7 7
O2 S1 O4 95.4(9) . 7
O3 S1 O4 70.7(9) . 7
O4 S1 O4 139.2(12) . 7
O2 S1 O4 101.7(12) 7 7
S1 S1 C17 105(4) 7 7
O3 S1 C17 115.2(12) 7 7
O2 S1 C17 153.8(10) . 7
O3 S1 C17 91.0(10) . 7
O4 S1 C17 43.4(11) . 7
O2 S1 C17 104.8(14) 7 7
O4 S1 C17 98.5(6) 7 7
S1 S1 C17 68(4) 7 .
O3 S1 C17 93.1(11) 7 .
O2 S1 C17 103.3(4) . .
O3 S1 C17 103.3(4) . .
O4 S1 C17 103.3(4) . .
O2 S1 C17 139.0(10) 7 .
O4 S1 C17 40.5(10) 7 .
C17 S1 C17 74.3(11) 7 .
O3 O2 S1 61.3(13) 7 .
O3 O2 S1 68.9(10) 7 7
S1 O2 S1 9.0(9) . 7
O2 O3 S1 80.1(14) 7 7
O2 O3 S1 74.8(12) 7 .
S1 O3 S1 7.3(12) 7 .
O2 O3 O4 125(2) 7 7
S1 O3 O4 52.8(9) 7 7
S1 O3 O4 59.9(8) . 7
F3 O4 C17 68.2(15) 7 7
F3 O4 S1 142(2) 7 .
C17 O4 S1 81.3(13) 7 .
F3 O4 S1 138(2) 7 7
C17 O4 S1 77.2(14) 7 7
S1 O4 S1 4.4(6) . 7
F3 O4 O3 173(2) 7 7
C17 O4 O3 115.8(19) 7 7
S1 O4 O3 45.2(7) . 7
S1 O4 O3 49.4(7) 7 7
O4 C17 F2 107.6(16) 7 .
O4 C17 F1 144.6(18) 7 .
F2 C17 F1 105.7(9) . .
O4 C17 F3 54.7(15) 7 .
F2 C17 F3 105.5(9) . .
F1 C17 F3 104.9(9) . .
O4 C17 S1 55.2(6) 7 7
F2 C17 S1 113.2(12) . 7
F1 C17 S1 119.7(11) . 7
F3 C17 S1 106.6(11) . 7
O4 C17 S1 62.3(11) 7 .
F2 C17 S1 113.7(9) . .
F1 C17 S1 113.5(8) . .
F3 C17 S1 112.8(9) . .
S1 C17 S1 7.2(7) 7 .
C17 F2 F2 85.5(10) . 7
O4 F3 C17 57.1(13) 7 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sm1 O1 2.421(5) 3_565
Sm1 O1 2.421(5) 12_565
Sm1 O1 2.421(5) 2_665
Sm1 O1 2.421(5) 11
Sm1 O1 2.421(5) 10_665
Sm1 O1 2.421(5) .
Sm1 N1 2.566(7) 3_565
Sm1 N1 2.566(7) 2_665
Sm1 N1 2.566(7) .
N1 C3 1.329(8) .
N1 C3 1.329(8) 11
N2 C4 1.306(10) .
N2 C5 1.445(15) .
O1 C4 1.220(9) .
C1 C2 1.396(10) .
C1 C2 1.396(10) 11
C2 C3 1.344(11) .
C3 C4 1.495(12) .
C5 C7 1.523(15) .
C5 C6 1.552(13) .
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 0.23(2) 7
S1 O3 1.27(2) 7
S1 O2 1.4298(10) .
S1 O3 1.4298(10) .
S1 O4 1.4299(10) .
S1 O2 1.479(17) 7
S1 O4 1.63(2) 7
S1 C17 1.721(17) 7
S1 C17 1.796(8) .
O2 O3 0.91(2) 7
O2 S1 1.479(17) 7
O3 O2 0.91(2) 7
O3 S1 1.27(2) 7
O3 O4 1.78(3) 7
O4 F3 1.16(3) 7
O4 C17 1.20(3) 7
O4 S1 1.63(2) 7
O4 O3 1.78(3) 7
C17 O4 1.20(3) 7
C17 F2 1.314(9) .
C17 F1 1.315(9) .
C17 F3 1.323(9) .
C17 S1 1.721(17) 7
F2 F2 1.64(4) 7
F3 O4 1.16(3) 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 -0.010 1120.1 454.6
2 0.667 0.333 0.250 173.7 13.4
3 0.333 0.667 0.750 173.7 13.2
