#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:52:47 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232786 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/81/4348136.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_4348136
loop_
_publ_author_name
'Mihalcea, Ionut'
'Perfetti, Mauro'
'Pineider, Francesco'
'Tesi, Lorenzo'
'Mereacre, Valeriu'
'Wilhelm, Fabrice'
'Rogalev, Andrei'
'Anson, Christopher E.'
'Powell, Annie K.'
'Sessoli, Roberta'
_publ_section_title
;
 Spin Helicity in Chiral Lanthanide Chains.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10068
_journal_page_last               10074
_journal_paper_doi               10.1021/acs.inorgchem.6b01010
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C18 H13 Dy0.12 N4 O9 Y0.88'
_chemical_formula_weight         527.06
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'dual-space direct methods'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.1664(3)
_cell_length_b                   11.1664(3)
_cell_length_c                   26.5948(18)
_cell_measurement_reflns_used    12775
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.24
_cell_volume                     2871.8(2)
_computing_cell_refinement       'SMART-NT 5.6 (Bruker AXS Inc., 2000)'
_computing_data_collection       'SMART-NT 5.6 (Bruker AXS Inc., 2000)'
_computing_data_reduction        'SAINT+ 6.45 (Bruker AXS Inc., 2000)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART Apex'
_diffrn_measurement_method       'CCD area detector, ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            24095
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.141
_diffrn_reflns_theta_min         0.766
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    3.213
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Bruker AXS Inc., 2005)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_description       needle
_exptl_crystal_F_000             1579
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1983 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4421
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0339P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.954
_reflns_number_gt                4315
_reflns_number_total             4421
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01010_si_003.cif
_cod_data_source_block           IM-DyY-15
_cod_database_code               4348136
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.513
_shelx_estimated_absorpt_t_max   0.910
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'-x, -y, z+1/2'
'y, -x+y, z+1/6'
'x-y, x, z+5/6'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.14471(2) 0.17267(2) 0.33073(2) 0.00956(7) Uani 0.88 1 d . U P A 1
Dy1 Dy 0.14471(2) 0.17267(2) 0.33073(2) 0.00956(7) Uani 0.12 1 d . . P A 2
O1 O -0.0680(2) 0.0216(2) 0.37242(8) 0.0180(4) Uani 1 1 d . U . . .
O2 O -0.0162(2) -0.0337(2) 0.44691(8) 0.0195(5) Uani 1 1 d . . . . .
C1 C -0.0990(3) -0.0317(3) 0.41533(12) 0.0146(6) Uani 1 1 d . . . . .
C2 C -0.2494(3) -0.1034(3) 0.43060(12) 0.0161(6) Uani 1 1 d . . . . .
C3 C -0.3558(3) -0.1421(3) 0.39598(12) 0.0203(6) Uani 1 1 d . . . . .
H3A H -0.3357 -0.1236 0.3612 0.024 Uiso 1 1 calc R U . . .
C4 C -0.4916(3) -0.2081(4) 0.41282(13) 0.0232(7) Uani 1 1 d . . . . .
H4A H -0.5657 -0.2360 0.3897 0.028 Uiso 1 1 calc R U . . .
C5 C -0.5174(3) -0.2328(4) 0.46381(13) 0.0222(7) Uani 1 1 d . . . . .
H5A H -0.6104 -0.2772 0.4752 0.027 Uiso 1 1 calc R U . . .
N1 N -0.4154(3) -0.1961(3) 0.49786(11) 0.0197(5) Uani 1 1 d . . . . .
C6 C -0.2848(3) -0.1330(3) 0.48102(12) 0.0176(6) Uani 1 1 d . . . . .
H6A H -0.2125 -0.1071 0.5048 0.021 Uiso 1 1 calc R U . . .
O3 O 0.2156(2) 0.0357(2) 0.36601(8) 0.0164(5) Uani 1 1 d . U . . .
O4 O 0.1877(2) -0.1047(2) 0.43014(8) 0.0180(5) Uani 1 1 d . . . . .
C7 C 0.1963(3) -0.0760(3) 0.38437(11) 0.0134(6) Uani 1 1 d . . . . .
C8 C 0.1821(3) -0.1866(3) 0.34802(11) 0.0142(6) Uani 1 1 d . . . . .
C9 C 0.1434(3) -0.3189(3) 0.36527(12) 0.0178(6) Uani 1 1 d . . . . .
H9A H 0.1289 -0.3391 0.4002 0.021 Uiso 1 1 calc R U . . .
C10 C 0.1261(3) -0.4213(3) 0.33158(14) 0.0211(6) Uani 1 1 d . . . . .
H10A H 0.1008 -0.5114 0.3431 0.025 Uiso 1 1 calc R U . . .
C11 C 0.1465(3) -0.3895(4) 0.28093(13) 0.0204(7) Uani 1 1 d . . . . .
H11A H 0.1336 -0.4587 0.2573 0.024 Uiso 1 1 calc R U . . .
N2 N 0.1847(3) -0.2604(3) 0.26491(10) 0.0182(5) Uani 1 1 d . . . . .
H2 H 0.192(6) -0.249(6) 0.228(2) 0.059(16) Uiso 1 1 d . . . . .
C12 C 0.2040(3) -0.1596(3) 0.29688(12) 0.0168(6) Uani 1 1 d . . . . .
H12A H 0.2327 -0.0694 0.2845 0.020 Uiso 1 1 calc R U . . .
O5 O 0.1361(2) 0.2889(2) 0.40284(8) 0.0172(4) Uani 1 1 d . U . . .
O6 O 0.2416(2) 0.2383(2) 0.46364(8) 0.0172(4) Uani 1 1 d . . . . .
C13 C 0.1818(3) 0.3002(3) 0.44677(11) 0.0146(6) Uani 1 1 d . . . . .
C14 C 0.1652(3) 0.3972(3) 0.48155(12) 0.0173(6) Uani 1 1 d . . . . .
C15 C 0.2183(3) 0.4232(3) 0.52999(12) 0.0191(6) Uani 1 1 d . . . . .
H15A H 0.2642 0.3775 0.5429 0.023 Uiso 1 1 calc R U . . .
C16 C 0.2026(4) 0.5176(4) 0.55929(13) 0.0230(7) Uani 1 1 d . . . . .
H16A H 0.2381 0.5382 0.5926 0.028 Uiso 1 1 calc R U . . .
C17 C 0.1339(4) 0.5811(4) 0.53894(13) 0.0244(7) Uani 1 1 d . . . . .
H17A H 0.1270 0.6481 0.5587 0.029 Uiso 1 1 calc R U . . .
N3 N 0.0767(3) 0.5533(3) 0.49284(12) 0.0263(6) Uani 1 1 d . . . . .
C18 C 0.0938(4) 0.4620(3) 0.46536(12) 0.0207(7) Uani 1 1 d . . . . .
H18A H 0.0543 0.4404 0.4327 0.025 Uiso 1 1 calc R U . . .
N4 N 0.3922(3) 0.4396(3) 0.33717(10) 0.0178(5) Uani 1 1 d . U . . .
O7 O 0.3876(2) 0.3330(2) 0.35605(8) 0.0176(4) Uani 1 1 d . U . . .
O8 O 0.2857(2) 0.4199(2) 0.31281(8) 0.0187(5) Uani 1 1 d . U . . .
O9 O 0.4934(3) 0.5557(2) 0.34231(10) 0.0290(6) Uani 1 1 d . . . . .
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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 '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
O3 Y1 O6 160.21(8) . 6_554
O3 Y1 O2 83.44(8) . 6_554
O6 Y1 O2 82.18(8) 6_554 6_554
O3 Y1 O5 99.26(8) . .
O6 Y1 O5 84.69(8) 6_554 .
O2 Y1 O5 144.01(8) 6_554 .
O3 Y1 O4 83.93(8) . 6_554
O6 Y1 O4 104.77(8) 6_554 6_554
O2 Y1 O4 73.38(8) 6_554 6_554
O5 Y1 O4 142.57(8) . 6_554
O3 Y1 O1 83.68(8) . .
O6 Y1 O1 78.91(8) 6_554 .
O2 Y1 O1 71.51(8) 6_554 .
O5 Y1 O1 73.14(8) . .
O4 Y1 O1 143.82(8) 6_554 .
O3 Y1 O8 127.02(8) . .
O6 Y1 O8 72.74(8) 6_554 .
O2 Y1 O8 132.56(7) 6_554 .
O5 Y1 O8 73.50(8) . .
O4 Y1 O8 75.04(8) 6_554 .
O1 Y1 O8 137.65(8) . .
O3 Y1 O7 75.40(8) . .
O6 Y1 O7 124.04(8) 6_554 .
O2 Y1 O7 140.55(8) 6_554 .
O5 Y1 O7 73.21(8) . .
O4 Y1 O7 71.60(8) 6_554 .
O1 Y1 O7 136.50(7) . .
O8 Y1 O7 51.97(7) . .
O3 Dy1 O6 160.21(8) . 6_554
O3 Dy1 O2 83.44(8) . 6_554
O6 Dy1 O2 82.18(8) 6_554 6_554
O3 Dy1 O5 99.26(8) . .
O6 Dy1 O5 84.69(8) 6_554 .
O2 Dy1 O5 144.01(8) 6_554 .
O3 Dy1 O4 83.93(8) . 6_554
O6 Dy1 O4 104.77(8) 6_554 6_554
O2 Dy1 O4 73.38(8) 6_554 6_554
O5 Dy1 O4 142.57(8) . 6_554
O3 Dy1 O1 83.68(8) . .
O6 Dy1 O1 78.91(8) 6_554 .
O2 Dy1 O1 71.51(8) 6_554 .
O5 Dy1 O1 73.14(8) . .
O4 Dy1 O1 143.82(8) 6_554 .
O3 Dy1 O8 127.02(8) . .
O6 Dy1 O8 72.74(8) 6_554 .
O2 Dy1 O8 132.56(7) 6_554 .
O5 Dy1 O8 73.50(8) . .
O4 Dy1 O8 75.04(8) 6_554 .
O1 Dy1 O8 137.65(8) . .
O3 Dy1 O7 75.40(8) . .
O6 Dy1 O7 124.04(8) 6_554 .
O2 Dy1 O7 140.55(8) 6_554 .
O5 Dy1 O7 73.21(8) . .
O4 Dy1 O7 71.60(8) 6_554 .
O1 Dy1 O7 136.50(7) . .
O8 Dy1 O7 51.97(7) . .
C1 O1 Y1 134.4(2) . .
C1 O1 Dy1 134.4(2) . .
C1 O2 Dy1 163.4(2) . 5
C1 O2 Y1 163.4(2) . 5
O1 C1 O2 125.8(3) . .
O1 C1 C2 117.8(3) . .
O2 C1 C2 116.3(3) . .
C3 C2 C6 117.9(3) . .
C3 C2 C1 122.5(3) . .
C6 C2 C1 119.6(3) . .
C4 C3 C2 119.2(3) . .
C4 C3 H3A 120.4 . .
C2 C3 H3A 120.4 . .
C5 C4 C3 119.0(3) . .
C5 C4 H4A 120.5 . .
C3 C4 H4A 120.5 . .
N1 C5 C4 122.5(3) . .
N1 C5 H5A 118.8 . .
C4 C5 H5A 118.8 . .
C6 N1 C5 117.9(3) . .
N1 C6 C2 123.5(3) . .
N1 C6 H6A 118.2 . .
C2 C6 H6A 118.2 . .
C7 O3 Y1 153.6(2) . .
C7 O3 Dy1 153.6(2) . .
C7 O4 Dy1 126.31(19) . 5
C7 O4 Y1 126.31(19) . 5
O4 C7 O3 126.0(3) . .
O4 C7 C8 116.7(3) . .
O3 C7 C8 117.3(3) . .
C12 C8 C9 118.7(3) . .
C12 C8 C7 120.9(3) . .
C9 C8 C7 120.4(3) . .
C10 C9 C8 120.2(3) . .
C10 C9 H9A 119.9 . .
C8 C9 H9A 119.9 . .
C11 C10 C9 118.7(3) . .
C11 C10 H10A 120.6 . .
C9 C10 H10A 120.6 . .
N2 C11 C10 120.3(3) . .
N2 C11 H11A 119.8 . .
C10 C11 H11A 119.8 . .
C12 N2 C11 121.9(3) . .
C12 N2 H2 123(3) . .
C11 N2 H2 115(3) . .
N2 C12 C8 120.2(3) . .
N2 C12 H12A 119.9 . .
C8 C12 H12A 119.9 . .
C13 O5 Y1 133.6(2) . .
C13 O5 Dy1 133.6(2) . .
C13 O6 Dy1 135.5(2) . 5
C13 O6 Y1 135.5(2) . 5
O5 C13 O6 125.2(3) . .
O5 C13 C14 117.1(3) . .
O6 C13 C14 117.8(3) . .
C15 C14 C18 118.4(3) . .
C15 C14 C13 121.9(3) . .
C18 C14 C13 119.6(3) . .
C14 C15 C16 118.5(3) . .
C14 C15 H15A 120.8 . .
C16 C15 H15A 120.8 . .
C17 C16 C15 118.7(3) . .
C17 C16 H16A 120.7 . .
C15 C16 H16A 120.7 . .
N3 C17 C16 123.9(3) . .
N3 C17 H17A 118.0 . .
C16 C17 H17A 118.0 . .
C18 N3 C17 116.0(3) . .
N3 C18 C14 124.3(3) . .
N3 C18 H18A 117.8 . .
C14 C18 H18A 117.8 . .
O9 N4 O7 122.0(3) . .
O9 N4 O8 121.7(3) . .
O7 N4 O8 116.3(2) . .
O9 N4 Y1 175.8(2) . .
O7 N4 Y1 59.05(14) . .
O8 N4 Y1 57.45(14) . .
O9 N4 Dy1 175.8(2) . .
O7 N4 Dy1 59.05(14) . .
O8 N4 Dy1 57.45(14) . .
N4 O7 Y1 94.94(16) . .
N4 O7 Dy1 94.94(16) . .
N4 O8 Y1 96.54(17) . .
N4 O8 Dy1 96.54(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Y1 O3 2.249(2) .
Y1 O6 2.260(2) 6_554
Y1 O2 2.296(2) 6_554
Y1 O5 2.344(2) .
Y1 O4 2.381(2) 6_554
Y1 O1 2.389(2) .
Y1 O8 2.446(2) .
Y1 O7 2.482(2) .
Dy1 O3 2.249(2) .
Dy1 O6 2.260(2) 6_554
Dy1 O2 2.296(2) 6_554
Dy1 O5 2.344(2) .
Dy1 O4 2.381(2) 6_554
Dy1 O1 2.389(2) .
Dy1 O8 2.446(2) .
Dy1 O7 2.482(2) .
O1 C1 1.253(4) .
O2 C1 1.258(4) .
O2 Dy1 2.296(2) 5
O2 Y1 2.296(2) 5
C1 C2 1.511(4) .
C2 C3 1.390(5) .
C2 C6 1.390(4) .
C3 C4 1.388(5) .
C3 H3A 0.9500 .
C4 C5 1.385(5) .
C4 H4A 0.9500 .
C5 N1 1.349(4) .
C5 H5A 0.9500 .
N1 C6 1.340(4) .
C6 H6A 0.9500 .
O3 C7 1.254(4) .
O4 C7 1.250(4) .
O4 Dy1 2.381(2) 5
O4 Y1 2.381(2) 5
C7 C8 1.513(4) .
C8 C12 1.388(4) .
C8 C9 1.393(4) .
C9 C10 1.388(4) .
C9 H9A 0.9500 .
C10 C11 1.383(5) .
C10 H10A 0.9500 .
C11 N2 1.351(4) .
C11 H11A 0.9500 .
N2 C12 1.339(4) .
N2 H2 0.99(5) .
C12 H12A 0.9500 .
O5 C13 1.256(4) .
O6 C13 1.260(4) .
O6 Dy1 2.260(2) 5
O6 Y1 2.260(2) 5
C13 C14 1.504(4) .
C14 C15 1.387(5) .
C14 C18 1.387(5) .
C15 C16 1.391(5) .
C15 H15A 0.9500 .
C16 C17 1.388(5) .
C16 H16A 0.9500 .
C17 N3 1.345(5) .
C17 H17A 0.9500 .
N3 C18 1.343(4) .
C18 H18A 0.9500 .
N4 O9 1.229(4) .
N4 O7 1.269(3) .
N4 O8 1.273(4) .
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
N2 H2 N1 0.99(5) 1.71(5) 2.701(4) 175(5) 2_554
