#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:19:13 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179104 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/66/4306695.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_4306695
loop_
_publ_author_name
'Ji-Jun Jiang'
'Sheng-Run Zheng'
'Yu Liu'
'Mei Pan'
'Wei Wang'
'Cheng-Yong Su'
_publ_section_title
;
Self-Assembly of Triple Helical and meso-Helical Cylindrical Arrays Tunable
by Bis-Tripodal Coordination Converters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10692
_journal_page_last               10699
_journal_paper_doi               10.1021/ic801516b
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C106 H90 Cl3 La N28 O12'
_chemical_formula_weight         2193.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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            6
_cell_length_a                   17.987(5)
_cell_length_b                   17.987(5)
_cell_length_c                   53.73(2)
_cell_measurement_temperature    293(2)
_cell_volume                     15054(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Smart CCD'
_diffrn_measurement_method       'ω san'
_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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            23040
_diffrn_reflns_theta_full        26.15
_diffrn_reflns_theta_max         26.15
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.8726
_exptl_absorpt_correction_T_min  0.8173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             6756
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3328
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0628
_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)+(0.1168P)²+97.5603P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.2029
_reflns_number_gt                2229
_reflns_number_total             3328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801516b_si_001_1.cif
_cod_data_source_block           meso-1
_cod_original_cell_volume        15054(9)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4306695
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
La1 La 0.0000 1.0000 0.0000 0.0330(3) Uani 1 6 d S . .
N1 N 0.0000 1.0000 -0.05262(11) 0.0324(13) Uani 1 3 d S . .
N2 N 0.0799(3) 0.9295(4) -0.02272(8) 0.0565(13) Uani 1 1 d . . .
N3 N 0.1230(4) 0.8952(4) -0.05734(9) 0.080(2) Uani 1 1 d . . .
H3A H 0.1284 0.8884 -0.0729 0.096 Uiso 1 1 calc R . .
N4 N 0.0831(5) 0.5737(5) 0.05852(11) 0.085(2) Uani 1 1 d . . .
N5 N 0.1237(5) 0.6107(5) -0.03315(10) 0.092(2) Uani 1 1 d . . .
C1 C 0.0000(6) 0.9237(5) -0.06164(11) 0.0704(19) Uani 1 1 d U . .
H1B H 0.0120 0.9285 -0.0793 0.085 Uiso 1 1 calc R . .
H1C H -0.0555 0.8730 -0.0588 0.085 Uiso 1 1 calc R . .
C2 C 0.0698(5) 0.9176(5) -0.04726(10) 0.073(2) Uani 1 1 d . . .
C3 C 0.1680(5) 0.8849(5) -0.03832(11) 0.0605(17) Uani 1 1 d . . .
C4 C 0.2233(5) 0.8534(6) -0.03854(15) 0.080(2) Uani 1 1 d . . .
H4B H 0.2397 0.8381 -0.0532 0.096 Uiso 1 1 calc R . .
C5 C 0.2522(6) 0.8460(7) -0.01614(17) 0.104(3) Uani 1 1 d . . .
H5B H 0.2907 0.8258 -0.0154 0.125 Uiso 1 1 calc R . .
C6 C 0.2274(7) 0.8668(7) 0.00588(16) 0.103(3) Uani 1 1 d . . .
H6A H 0.2502 0.8611 0.0208 0.123 Uiso 1 1 calc R . .
C7 C 0.1689(5) 0.8963(5) 0.00613(12) 0.0705(19) Uani 1 1 d . . .
H7A H 0.1506 0.9088 0.0209 0.085 Uiso 1 1 calc R . .
C8 C 0.1397(4) 0.9058(4) -0.01660(10) 0.0515(15) Uani 1 1 d . . .
C9 C 0.1021(8) 0.5384(7) 0.04153(16) 0.110(4) Uani 1 1 d U . .
H9A H 0.1171 0.4979 0.0462 0.132 Uiso 1 1 calc R . .
C10 C 0.1026(8) 0.5546(7) 0.01679(15) 0.103(3) Uani 1 1 d U . .
H10A H 0.1149 0.5233 0.0054 0.123 Uiso 1 1 calc R . .
C11 C 0.0635(7) 0.6303(7) 0.05109(14) 0.101(3) Uani 1 1 d U . .
H11A H 0.0468 0.6563 0.0631 0.121 Uiso 1 1 calc R . .
C12 C 0.0659(6) 0.6551(6) 0.02638(13) 0.093(3) Uani 1 1 d U . .
H12A H 0.0541 0.6984 0.0223 0.112 Uiso 1 1 calc R . .
C13 C 0.0856(5) 0.6151(5) 0.00861(11) 0.072(2) Uani 1 1 d U . .
C14 C 0.0919(6) 0.6397(6) -0.01768(12) 0.083(2) Uani 1 1 d U . .
H14A H 0.0726 0.6765 -0.0229 0.100 Uiso 1 1 calc R . .
C15 C 0.1306(6) 0.6383(6) -0.05872(12) 0.088(3) Uani 1 1 d U . .
C16 C 0.2022(7) 0.6516(10) -0.07074(15) 0.130(4) Uani 1 1 d U . .
H16A H 0.2418 0.6413 -0.0626 0.156 Uiso 1 1 calc R . .
C17 C 0.0752(6) 0.6545(6) -0.07069(11) 0.081(2) Uani 1 1 d U . .
H17A H 0.0279 0.6498 -0.0622 0.098 Uiso 1 1 calc R . .
Cl1 Cl 0.1453(2) 0.3333 0.0833 0.0986(10) Uani 1 2 d S . .
O1 O 0.1394(8) 0.3954(7) 0.07011(17) 0.186(4) Uani 1 1 d U . .
O2 O 0.1720(6) 0.2877(5) 0.06650(13) 0.127(2) Uani 1 1 d U . .
N1W N 0.3333 0.6667 0.0432(5) 0.182(9) Uani 1 3 d SU . .
C1W C 0.3333 0.6667 0.0220(4) 0.126(7) Uani 1 3 d S . .
C2W C 0.3333 0.6667 -0.0045(4) 0.113(6) Uani 1 3 d SU . .
H2W1 H 0.3638 0.6391 -0.0105 0.169 Uiso 0.33 1 calc PR . .
H2W2 H 0.3609 0.7247 -0.0105 0.169 Uiso 0.33 1 calc PR . .
H2W3 H 0.2753 0.6362 -0.0105 0.169 Uiso 0.33 1 calc PR . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
La La -0.2871 2.4523 '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
_geom_angle_publ_flag
N2 La1 N2 100.37(12) 21_665 19_575 ?
N2 La1 N2 180.00(16) 21_665 3_465 ?
N2 La1 N2 79.63(12) 19_575 3_465 ?
N2 La1 N2 100.37(12) 21_665 20_455 ?
N2 La1 N2 100.37(12) 19_575 20_455 ?
N2 La1 N2 79.63(12) 3_465 20_455 ?
N2 La1 N2 79.63(12) 21_665 2_675 ?
N2 La1 N2 79.63(12) 19_575 2_675 ?
N2 La1 N2 100.37(12) 3_465 2_675 ?
N2 La1 N2 180.00(16) 20_455 2_675 ?
N2 La1 N2 79.63(12) 21_665 . ?
N2 La1 N2 180.00(16) 19_575 . ?
N2 La1 N2 100.37(12) 3_465 . ?
N2 La1 N2 79.63(12) 20_455 . ?
N2 La1 N2 100.37(12) 2_675 . ?
N2 La1 N1 62.49(9) 21_665 19_575 ?
N2 La1 N1 62.49(9) 19_575 19_575 ?
N2 La1 N1 117.51(9) 3_465 19_575 ?
N2 La1 N1 62.49(9) 20_455 19_575 ?
N2 La1 N1 117.51(9) 2_675 19_575 ?
N2 La1 N1 117.51(9) . 19_575 ?
N2 La1 N1 117.51(10) 21_665 . ?
N2 La1 N1 117.51(9) 19_575 . ?
N2 La1 N1 62.49(9) 3_465 . ?
N2 La1 N1 117.51(9) 20_455 . ?
N2 La1 N1 62.49(9) 2_675 . ?
N2 La1 N1 62.49(9) . . ?
N1 La1 N1 180.0 19_575 . ?
C1 N1 C1 109.5(3) 2_675 . ?
C1 N1 C1 109.5(3) 2_675 3_465 ?
C1 N1 C1 109.5(3) . 3_465 ?
C1 N1 La1 109.5(3) 2_675 . ?
C1 N1 La1 109.5(3) . . ?
C1 N1 La1 109.5(3) 3_465 . ?
C2 N2 C8 104.5(5) . . ?
C2 N2 La1 118.1(4) . . ?
C8 N2 La1 137.1(4) . . ?
C2 N3 C3 107.5(5) . . ?
C2 N3 H3A 126.3 . . ?
C3 N3 H3A 126.3 . . ?
C9 N4 C11 115.1(7) . . ?
C14 N5 C15 117.6(7) . . ?
N1 C1 C2 106.7(5) . . ?
N1 C1 H1B 110.4 . . ?
C2 C1 H1B 110.4 . . ?
N1 C1 H1C 110.4 . . ?
C2 C1 H1C 110.4 . . ?
H1B C1 H1C 108.6 . . ?
N3 C2 N2 113.1(6) . . ?
N3 C2 C1 124.1(5) . . ?
N2 C2 C1 122.7(5) . . ?
N3 C3 C4 130.5(6) . . ?
N3 C3 C8 105.5(5) . . ?
C4 C3 C8 123.8(6) . . ?
C5 C4 C3 115.5(7) . . ?
C5 C4 H4B 122.2 . . ?
C3 C4 H4B 122.2 . . ?
C4 C5 C6 123.2(7) . . ?
C4 C5 H5B 118.4 . . ?
C6 C5 H5B 118.4 . . ?
C7 C6 C5 121.2(7) . . ?
C7 C6 H6A 119.4 . . ?
C5 C6 H6A 119.4 . . ?
C8 C7 C6 116.6(7) . . ?
C8 C7 H7A 121.7 . . ?
C6 C7 H7A 121.7 . . ?
C7 C8 N2 131.0(6) . . ?
C7 C8 C3 119.7(6) . . ?
N2 C8 C3 109.2(5) . . ?
N4 C9 C10 125.3(9) . . ?
N4 C9 H9A 117.3 . . ?
C10 C9 H9A 117.3 . . ?
C13 C10 C9 120.9(8) . . ?
C13 C10 H10A 119.6 . . ?
C9 C10 H10A 119.6 . . ?
N4 C11 C12 124.6(8) . . ?
N4 C11 H11A 117.7 . . ?
C12 C11 H11A 117.7 . . ?
C13 C12 C11 118.5(8) . . ?
C13 C12 H12A 120.7 . . ?
C11 C12 H12A 120.7 . . ?
C12 C13 C10 115.4(7) . . ?
C12 C13 C14 121.4(7) . . ?
C10 C13 C14 123.1(7) . . ?
N5 C14 C13 119.4(8) . . ?
N5 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
C17 C15 C16 118.7(8) . . ?
C17 C15 N5 126.0(7) . . ?
C16 C15 N5 115.2(8) . . ?
C15 C16 C16 120.2(5) . 11_564 ?
C15 C16 H16A 119.9 . . ?
C16 C16 H16A 119.9 11_564 . ?
C15 C17 C17 121.0(4) . 11_564 ?
C15 C17 H17A 119.5 . . ?
C17 C17 H17A 119.5 11_564 . ?
O1 Cl1 O1 122.0(11) 17_554 . ?
O1 Cl1 O2 108.6(5) 17_554 17_554 ?
O1 Cl1 O2 105.9(6) . 17_554 ?
O1 Cl1 O2 105.9(6) 17_554 . ?
O1 Cl1 O2 108.6(5) . . ?
O2 Cl1 O2 104.5(7) 17_554 . ?
N1W C1W C2W 180.000(2) . . ?
C1W C2W H2W1 109.5 . . ?
C1W C2W H2W2 109.5 . . ?
H2W1 C2W H2W2 109.5 . . ?
C1W C2W H2W3 109.5 . . ?
H2W1 C2W H2W3 109.5 . . ?
H2W2 C2W H2W3 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
La1 N2 2.643(5) 21_665 ?
La1 N2 2.643(5) 19_575 ?
La1 N2 2.643(5) 3_465 ?
La1 N2 2.643(5) 20_455 ?
La1 N2 2.643(5) 2_675 ?
La1 N2 2.643(5) . ?
La1 N1 2.827(6) 19_575 ?
La1 N1 2.827(6) . ?
N1 C1 1.455(7) 2_675 ?
N1 C1 1.455(7) . ?
N1 C1 1.455(7) 3_465 ?
N2 C2 1.333(7) . ?
N2 C8 1.379(8) . ?
N3 C2 1.325(8) . ?
N3 C3 1.371(8) . ?
N3 H3A 0.8600 . ?
N4 C9 1.253(12) . ?
N4 C11 1.295(12) . ?
N5 C14 1.262(9) . ?
N5 C15 1.445(9) . ?
C1 C2 1.525(10) . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C3 C4 1.369(9) . ?
C3 C8 1.398(8) . ?
C4 C5 1.344(11) . ?
C4 H4B 0.9300 . ?
C5 C6 1.381(12) . ?
C5 H5B 0.9300 . ?
C6 C7 1.395(11) . ?
C6 H6A 0.9300 . ?
C7 C8 1.374(8) . ?
C7 H7A 0.9300 . ?
C9 C10 1.360(11) . ?
C9 H9A 0.9300 . ?
C10 C13 1.344(11) . ?
C10 H10A 0.9300 . ?
C11 C12 1.395(11) . ?
C11 H11A 0.9300 . ?
C12 C13 1.346(10) . ?
C12 H12A 0.9300 . ?
C13 C14 1.468(9) . ?
C14 H14A 0.9300 . ?
C15 C17 1.336(11) . ?
C15 C16 1.350(12) . ?
C16 C16 1.432(17) 11_564 ?
C16 H16A 0.9300 . ?
C17 C17 1.410(12) 11_564 ?
C17 H17A 0.9300 . ?
Cl1 O1 1.371(9) 17_554 ?
Cl1 O1 1.371(9) . ?
Cl1 O2 1.454(8) 17_554 ?
Cl1 O2 1.454(8) . ?
N1W C1W 1.14(3) . ?
C1W C2W 1.43(3) . ?
C2W H2W1 0.9600 . ?
C2W H2W2 0.9600 . ?
C2W H2W3 0.9600 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3A N4 0.86 1.95 2.783(7) 164.4 29_455
